#------------------------------------------------------------------------------ #$Date: 2022-09-24 00:52:57 +0300 (Sat, 24 Sep 2022) $ #$Revision: 278129 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/13/07/7130758.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7130758 loop_ _publ_author_name 'Mathoni\`ere, Corine' 'Mitcov, Dmitri' 'Koumousi, Evangelia' 'Amorin Rosario, Daniel' 'Dechambenoit, Pierre' 'Sadaf, Jafri Fatima' 'Sainctavit, Philippe' 'Cartier dit Moulin, Christophe' 'Trzop, Elzbieta' 'Toupet, Loic' 'Collet, Eric' 'Arrio, Marie-Anne' 'Rogalev, Andrei' 'Wilhelm, Fabrice' 'Clerac, Rodolphe' _publ_section_title ; Metal-to-metal electron transfer in a cyanido-bridged {Fe2Co2} square complex followed by X-ray diffraction and absorption techniques ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D2CC04246K _journal_year 2022 _chemical_formula_moiety 'C42 H46 B Co Fe N13, C F3 O3 S, C3 H7 N O, 0.5(H2 O)' _chemical_formula_sum 'C46 H54 B Co F3 Fe N14 O4.5 S' _chemical_formula_weight 1089.68 _chemical_melting_point ? _chemical_properties_physical Light-sensitive,Photo-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2022-06-29 deposited with the CCDC. 2022-09-22 downloaded from the CCDC. ; _cell_angle_alpha 69.953(7) _cell_angle_beta 87.972(7) _cell_angle_gamma 71.580(7) _cell_formula_units_Z 2 _cell_length_a 13.2457(11) _cell_length_b 13.8227(9) _cell_length_c 14.7690(12) _cell_measurement_reflns_used 1609 _cell_measurement_temperature 80.0 _cell_measurement_theta_max 21.5680 _cell_measurement_theta_min 3.1190 _cell_volume 2402.0(4) _computing_cell_refinement 'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.33.5 (Oxford Diffraction Ltd., 2008)' _computing_data_reduction 'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 80.0 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1852 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -104.00 -32.00 1.00 60.00 -- -21.92 179.00-180.00 72 2 \w -48.00 51.00 1.00 60.00 -- -21.92 38.00-150.00 99 3 \w -24.00 16.00 1.00 60.00 -- -21.92 -88.00 164.00 40 4 \w -87.00 9.00 1.00 60.00 -- -21.92 -38.00 30.00 96 5 \w -83.00 11.00 1.00 60.00 -- -21.92 -77.00 -30.00 94 6 \w 78.00 103.00 1.00 60.00 -- 23.80 179.00-180.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0171023000 _diffrn_orient_matrix_UB_12 0.0539566000 _diffrn_orient_matrix_UB_13 -0.0338488000 _diffrn_orient_matrix_UB_21 0.0364542000 _diffrn_orient_matrix_UB_22 -0.0167244000 _diffrn_orient_matrix_UB_23 -0.0323112000 _diffrn_orient_matrix_UB_31 -0.0398208000 _diffrn_orient_matrix_UB_32 -0.0119106000 _diffrn_orient_matrix_UB_33 -0.0210119000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1112 _diffrn_reflns_av_unetI/netI 0.2351 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16164 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.831 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_meas ? _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_F_000 1130 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.069 _exptl_crystal_size_min 0.027 _refine_diff_density_max 0.556 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 661 _refine_ls_number_reflns 8442 _refine_ls_number_restraints 84 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.1937 _refine_ls_R_factor_gt 0.0818 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1152 _refine_ls_wR_factor_ref 0.1649 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3812 _reflns_number_total 8442 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mebipy80Kdark CELL 0.71073 13.2457 13.8227 14.769 69.953 87.972 71.58 ZERR 2 0.0011 0.0009 0.0012 0.007 0.007 0.007 LATT 1 SFAC C H B Co F Fe N O S UNIT 92 108 2 2 6 2 28 9 2 EQIV $1 1-X,1-Y,1-Z ISOR 0.005 0.01 C32 C33 C36 C31 C34 C35 C43 C46 C40 C39 C42 C38 C37 C3 L.S. 6 0 0 PLAN 10 TEMP -193.15 HTAB O5 N8_$1 BOND $H CONF list 4 fmap 2 53 acta OMIT -4 50 WGHT 0.021900 FVAR 0.44151 CO1 4 0.733601 0.375255 0.406107 11.00000 0.02511 0.01253 = 0.02980 -0.00282 0.00335 -0.00493 FE1 6 0.454959 0.257827 0.594636 11.00000 0.02389 0.01494 = 0.02599 -0.00275 0.00273 -0.00621 S1 9 0.021649 0.178894 0.157959 11.00000 0.04304 0.03048 = 0.04921 -0.01656 0.01871 -0.01696 F1 5 -0.064676 0.033918 0.162323 11.00000 0.09806 0.06060 = 0.08352 -0.00657 0.00046 -0.05619 F2 5 0.017650 0.083617 0.035297 11.00000 0.08542 0.04257 = 0.05055 -0.01440 -0.01557 -0.01918 F3 5 -0.136261 0.188086 0.050429 11.00000 0.03918 0.09820 = 0.06945 -0.00106 -0.01691 -0.01312 O1 8 0.360626 0.339130 1.053196 11.00000 0.06318 0.02978 = 0.04291 -0.00271 -0.00246 -0.02332 O2 8 0.120080 0.092007 0.197049 11.00000 0.03519 0.06548 = 0.06079 -0.03025 -0.00192 -0.00253 O3 8 0.032877 0.271123 0.080147 11.00000 0.11216 0.04783 = 0.05940 -0.01813 0.04906 -0.05150 O4 8 -0.051613 0.203821 0.225989 11.00000 0.04917 0.03039 = 0.05783 -0.00422 0.02615 -0.00142 O5 8 0.670213 0.560754 0.788773 10.50000 0.16070 0.07483 = 0.09944 -0.00467 0.01871 -0.04987 AFIX 3 H5D 2 0.680243 0.588944 0.728123 10.50000 -1.50000 H5E 2 0.664563 0.611934 0.812093 10.50000 -1.50000 AFIX 0 N1 7 0.363420 0.175379 0.682297 11.00000 0.02548 0.01752 = 0.02515 -0.00760 0.00352 -0.00933 N2 7 0.418348 0.072733 0.745145 11.00000 0.02611 0.01225 = 0.02750 -0.00124 -0.00108 -0.00112 N3 7 0.551827 0.218369 0.713974 11.00000 0.03519 0.00734 = 0.02301 0.00231 -0.00621 -0.00353 N4 7 0.579653 0.113080 0.780036 11.00000 0.02611 0.01794 = 0.02690 -0.00560 0.00223 -0.00404 N5 7 0.540692 0.113329 0.578277 11.00000 0.02626 0.01011 = 0.02626 -0.00036 -0.00288 -0.00447 N6 7 0.579256 0.022630 0.661398 11.00000 0.02907 0.02406 = 0.02976 -0.01168 0.00309 -0.01186 N7 7 0.326799 0.473139 0.612294 11.00000 0.01167 0.01325 = 0.03323 0.00082 0.00054 0.00198 N8 7 0.295535 0.341646 0.417544 11.00000 0.02919 0.02585 = 0.02854 -0.01120 -0.00007 -0.01000 N9 7 0.610823 0.350144 0.464583 11.00000 0.02353 0.01727 = 0.02733 -0.00829 0.00297 -0.00651 N10 7 0.797998 0.339885 0.533164 11.00000 0.02401 0.01670 = 0.03182 -0.00453 0.00249 -0.00963 N11 7 0.796886 0.219244 0.435596 11.00000 0.01704 0.01512 = 0.02822 -0.00262 0.00352 -0.00458 N12 7 0.857371 0.400557 0.339608 11.00000 0.03334 0.01218 = 0.04315 -0.00656 0.00292 -0.00553 N13 7 0.679797 0.398778 0.277288 11.00000 0.03607 0.00866 = 0.03701 -0.00372 0.00801 -0.00582 N14 7 0.296310 0.296022 0.937492 11.00000 0.03884 0.02479 = 0.03737 -0.00642 0.01538 -0.01114 C1 1 0.173659 0.290942 0.627175 11.00000 0.02353 0.03685 = 0.03879 -0.01197 0.00395 -0.01150 AFIX 137 H1A 2 0.191005 0.354444 0.628211 11.00000 -1.50000 H1B 2 0.105128 0.291614 0.654693 11.00000 -1.50000 H1C 2 0.168793 0.293431 0.560309 11.00000 -1.50000 AFIX 0 C2 1 0.260064 0.188181 0.686234 11.00000 0.02326 0.02663 = 0.04008 -0.02078 0.00447 -0.00661 C3 1 0.246816 0.093230 0.751846 11.00000 0.02819 0.01712 = 0.02922 -0.00396 0.00601 -0.01315 AFIX 43 H3 2 0.181155 0.080331 0.768718 11.00000 -1.20000 AFIX 0 C4 1 0.345087 0.024057 0.786193 11.00000 0.03762 0.01555 = 0.02829 -0.00381 0.00538 -0.01280 C5 1 0.379681 -0.092771 0.860001 11.00000 0.05266 0.02864 = 0.03639 -0.01654 0.02287 -0.01689 AFIX 137 H5A 2 0.430286 -0.141580 0.832053 11.00000 -1.50000 H5B 2 0.316878 -0.116406 0.876315 11.00000 -1.50000 H5C 2 0.413917 -0.094747 0.918649 11.00000 -1.50000 AFIX 0 C6 1 0.583529 0.389823 0.701806 11.00000 0.02890 0.02069 = 0.04896 -0.01413 -0.00306 -0.01064 AFIX 137 H6A 2 0.594985 0.405260 0.633062 11.00000 -1.50000 H6B 2 0.634132 0.410527 0.732030 11.00000 -1.50000 H6C 2 0.510397 0.431597 0.708497 11.00000 -1.50000 AFIX 0 C7 1 0.600491 0.270464 0.750567 11.00000 0.02491 0.01736 = 0.02396 -0.01213 0.00433 -0.00314 C8 1 0.658901 0.201283 0.837085 11.00000 0.02440 0.02596 = 0.02735 -0.01074 -0.00755 -0.00664 AFIX 43 H8 2 0.700427 0.218501 0.876701 11.00000 -1.20000 AFIX 0 C9 1 0.644630 0.102617 0.854048 11.00000 0.02411 0.02939 = 0.02384 -0.00295 -0.00475 -0.00366 C10 1 0.688350 -0.004157 0.937205 11.00000 0.04675 0.02681 = 0.02956 -0.01031 -0.00376 -0.00242 AFIX 137 H10A 2 0.629151 -0.028719 0.966447 11.00000 -1.50000 H10B 2 0.728443 0.005974 0.985835 11.00000 -1.50000 H10C 2 0.735774 -0.058880 0.913193 11.00000 -1.50000 AFIX 0 C11 1 0.551143 0.152253 0.400639 11.00000 0.02357 0.02423 = 0.02171 -0.01115 0.00444 -0.00865 AFIX 137 H11A 2 0.477012 0.200550 0.390883 11.00000 -1.50000 H11B 2 0.560920 0.107767 0.359662 11.00000 -1.50000 H11C 2 0.599149 0.195977 0.383367 11.00000 -1.50000 AFIX 0 C12 1 0.576137 0.079571 0.504618 11.00000 0.02424 0.02395 = 0.02915 -0.01029 0.00506 -0.01114 C13 1 0.636864 -0.032417 0.539563 11.00000 0.00859 0.02182 = 0.04068 -0.01420 -0.00274 -0.00150 AFIX 43 H13 2 0.669810 -0.076447 0.502575 11.00000 -1.20000 AFIX 0 C14 1 0.637858 -0.063609 0.638330 11.00000 0.02597 0.02508 = 0.02998 -0.01015 0.00401 -0.00637 C15 1 0.689918 -0.173711 0.714209 11.00000 0.03906 0.01065 = 0.02900 -0.00084 -0.00532 -0.00456 AFIX 137 H15A 2 0.743954 -0.169084 0.754750 11.00000 -1.50000 H15B 2 0.723949 -0.226420 0.682711 11.00000 -1.50000 H15C 2 0.635714 -0.197249 0.754524 11.00000 -1.50000 AFIX 0 C16 1 0.377361 0.389669 0.607229 11.00000 0.02326 0.01545 = 0.01686 0.00309 0.00039 -0.00408 C17 1 0.358529 0.304153 0.484384 11.00000 0.02863 0.01096 = 0.04133 -0.01207 0.00000 -0.00646 C18 1 0.548072 0.318962 0.514779 11.00000 0.02283 0.00813 = 0.03262 -0.00801 -0.01083 0.00156 C19 1 0.802174 0.407817 0.577155 11.00000 0.03004 0.01669 = 0.03410 0.00088 -0.00826 -0.01364 AFIX 43 H19 2 0.772801 0.483732 0.542468 11.00000 -1.20000 AFIX 0 C20 1 0.845530 0.375586 0.667954 11.00000 0.02791 0.03560 = 0.03560 -0.01338 0.00109 -0.01769 AFIX 43 H20 2 0.850571 0.428256 0.693760 11.00000 -1.20000 AFIX 0 C21 1 0.883383 0.264547 0.724823 11.00000 0.01944 0.03032 = 0.03133 -0.00001 -0.00426 -0.00386 C22 1 0.875939 0.192806 0.680729 11.00000 0.02545 0.02454 = 0.03140 0.00249 -0.00173 -0.00439 AFIX 43 H22 2 0.900160 0.116738 0.715898 11.00000 -1.20000 AFIX 0 C23 1 0.834035 0.230730 0.587100 11.00000 0.00848 0.01572 = 0.03369 0.00231 -0.00402 -0.00086 C24 1 0.931287 0.226879 0.825596 11.00000 0.04924 0.04644 = 0.03660 -0.00430 -0.00844 -0.02009 AFIX 137 H24A 2 0.931763 0.152216 0.860105 11.00000 -1.50000 H24B 2 0.889003 0.274726 0.858799 11.00000 -1.50000 H24C 2 1.004635 0.228893 0.824232 11.00000 -1.50000 AFIX 0 C25 1 0.831379 0.162462 0.530314 11.00000 0.02033 0.01699 = 0.03097 0.00243 0.00358 -0.00742 C26 1 0.867184 0.050230 0.567227 11.00000 0.01813 0.01208 = 0.04678 0.00444 -0.00576 -0.00301 AFIX 43 H26 2 0.888600 0.012969 0.634205 11.00000 -1.20000 AFIX 0 C27 1 0.871913 -0.008763 0.505717 11.00000 0.01783 0.01665 = 0.05322 -0.01006 0.00130 -0.00947 C28 1 0.840665 0.049547 0.409277 11.00000 0.02916 0.01788 = 0.03371 -0.01103 0.00711 -0.00901 AFIX 43 H28 2 0.845126 0.012992 0.364545 11.00000 -1.20000 AFIX 0 C29 1 0.802542 0.162419 0.378115 11.00000 0.02170 0.01837 = 0.03603 -0.00670 -0.00385 -0.00788 AFIX 43 H29 2 0.779117 0.201256 0.311674 11.00000 -1.20000 AFIX 0 C30 1 0.910308 -0.132625 0.545649 11.00000 0.03185 0.01487 = 0.06033 -0.00097 -0.00755 -0.00086 AFIX 137 H30A 2 0.852346 -0.158297 0.576595 11.00000 -1.50000 H30B 2 0.971318 -0.158996 0.593354 11.00000 -1.50000 H30C 2 0.931983 -0.160335 0.492709 11.00000 -1.50000 AFIX 0 C31 1 0.947214 0.398552 0.381514 11.00000 0.03235 0.03113 = 0.05010 -0.01338 0.00766 -0.01284 AFIX 43 H31 2 0.953686 0.383478 0.449216 11.00000 -1.20000 AFIX 0 C32 1 1.032277 0.418898 0.324816 11.00000 0.04584 0.04220 = 0.06410 -0.02238 0.01213 -0.01822 AFIX 43 H32 2 1.096690 0.414758 0.354549 11.00000 -1.20000 AFIX 0 C33 1 1.020549 0.443746 0.229832 11.00000 0.04404 0.03947 = 0.06148 -0.01713 0.02123 -0.01855 C34 1 0.930604 0.445124 0.188086 11.00000 0.05733 0.03286 = 0.04890 -0.01324 0.01994 -0.01529 AFIX 43 H34 2 0.923908 0.461799 0.120151 11.00000 -1.20000 AFIX 0 C35 1 0.847068 0.422408 0.243178 11.00000 0.04298 0.02138 = 0.03917 -0.01245 0.01215 -0.00627 C36 1 1.111017 0.465264 0.164191 11.00000 0.10009 0.08119 = 0.11826 -0.05763 0.05784 -0.05096 AFIX 137 H36A 2 1.136459 0.408646 0.135290 11.00000 -1.50000 H36B 2 1.170166 0.464112 0.203009 11.00000 -1.50000 H36C 2 1.083542 0.536619 0.112832 11.00000 -1.50000 AFIX 0 C37 1 0.751281 0.413899 0.209092 11.00000 0.03959 0.01996 = 0.03879 -0.00862 0.00668 -0.00611 C38 1 0.729371 0.412339 0.118634 11.00000 0.05158 0.02893 = 0.03777 -0.00618 0.01188 -0.00424 AFIX 43 H38 2 0.778619 0.423644 0.070944 11.00000 -1.20000 AFIX 0 C39 1 0.639110 0.395034 0.096131 11.00000 0.04756 0.02333 = 0.03217 -0.00869 -0.00261 0.00417 C40 1 0.566866 0.383450 0.164292 11.00000 0.04035 0.02520 = 0.03682 -0.00662 -0.00695 -0.00156 AFIX 43 H40 2 0.502257 0.373371 0.150252 11.00000 -1.20000 AFIX 0 C41 1 0.588932 0.386578 0.253467 11.00000 0.04144 0.00890 = 0.03892 -0.00417 -0.00864 -0.00324 AFIX 43 H41 2 0.537779 0.379828 0.299967 11.00000 -1.20000 AFIX 0 C42 1 0.621517 0.385620 -0.000979 11.00000 0.07634 0.04515 = 0.04830 -0.02260 -0.00661 0.01029 AFIX 137 H42A 2 0.675031 0.319932 -0.005268 11.00000 -1.50000 H42B 2 0.628221 0.449735 -0.052906 11.00000 -1.50000 H42C 2 0.549929 0.381108 -0.007529 11.00000 -1.50000 AFIX 0 C43 1 0.294557 0.313457 1.019167 11.00000 0.04747 0.02663 = 0.03398 -0.00877 0.01488 -0.01100 AFIX 43 H43 2 0.235611 0.305306 1.056053 11.00000 -1.20000 AFIX 0 C44 1 0.386884 0.296674 0.879089 11.00000 0.04804 0.04543 = 0.03080 -0.00115 0.01059 -0.00784 AFIX 137 H44A 2 0.436297 0.321655 0.905968 11.00000 -1.50000 H44B 2 0.361718 0.345875 0.812581 11.00000 -1.50000 H44C 2 0.423719 0.222932 0.879332 11.00000 -1.50000 AFIX 0 C45 1 0.213566 0.266949 0.901930 11.00000 0.08262 0.02697 = 0.02986 0.00296 0.00801 -0.02425 AFIX 137 H45A 2 0.162619 0.255653 0.951053 11.00000 -1.50000 H45B 2 0.245913 0.199786 0.888047 11.00000 -1.50000 H45C 2 0.176240 0.325757 0.842654 11.00000 -1.50000 AFIX 0 C46 1 -0.044517 0.122536 0.100216 11.00000 0.03297 0.03618 = 0.03517 0.00317 0.00428 -0.01232 B1 3 0.540327 0.031487 0.756678 11.00000 0.04111 0.01269 = 0.02108 0.00653 -0.00509 -0.00905 AFIX 13 H1 2 0.566573 -0.041253 0.809429 11.00000 -1.20000 AFIX 0 HKLF 4 REM mebipy80Kdark REM R1 = 0.0818 for 3812 Fo > 4sig(Fo) and 0.1937 for all 8442 data REM 661 parameters refined using 84 restraints END WGHT 0.0219 0.0000 REM Highest difference peak 0.556, deepest hole -0.491, 1-sigma level 0.105 Q1 1 -0.0615 0.1529 0.1651 11.00000 0.05 0.56 Q2 1 0.5380 0.2147 0.5766 11.00000 0.05 0.52 Q3 1 0.8167 0.3359 0.3789 11.00000 0.05 0.52 Q4 1 0.9191 0.0126 0.4013 11.00000 0.05 0.51 Q5 1 1.0022 0.4607 0.1748 11.00000 0.05 0.51 Q6 1 0.6591 0.4249 0.4354 11.00000 0.05 0.50 Q7 1 0.6450 0.3852 0.3849 11.00000 0.05 0.48 Q8 1 0.8911 0.4592 0.1515 11.00000 0.05 0.47 Q9 1 0.8329 0.3593 0.4224 11.00000 0.05 0.47 Q10 1 0.4526 0.3155 0.6419 11.00000 0.05 0.46 REM The information below was added by Olex2. REM REM R1 = 0.0818 for 3812 Fo > 4sig(Fo) and 0.1937 for all 20520 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.56, deepest hole -0.49 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1937 REM R1_gt = 0.0818 REM wR_ref = 0.1649 REM GOOF = 1.001 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 20520 REM Reflections_gt = 3812 REM Parameters = n/a REM Hole = -0.49 REM Peak = 0.56 REM Flack = n/a ; _cod_data_source_file d2cc04246k2.cif _cod_data_source_block mebipy80Kdark _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'not measured' was changed to '?' -- the value is undefined or not given. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 2402.0(3) _cod_original_formula_sum 'C46 H54 B Co F3 Fe N14 O4.50 S' _cod_database_code 7130758 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula C46H53BCoF3FeN14O4.4S _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.87 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 3. Others Fixed Sof: O5(0.5) H5D(0.5) H5E(0.5) 4.a Riding coordinates: O5(H5D,H5E) 4.b Ternary CH refined with riding coordinates: B1(H1) 4.c Aromatic/amide H refined with riding coordinates: C3(H3), C8(H8), C13(H13), C19(H19), C20(H20), C22(H22), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C38(H38), C40(H40), C41(H41), C43(H43) 4.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C30(H30A,H30B, H30C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A, H45B,H45C) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.090 _oxdiff_exptl_absorpt_empirical_full_min 0.895 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.73360(8) 0.37526(8) 0.40611(8) 0.0241(3) Uani 1 1 d . . . . . Fe1 Fe 0.45496(8) 0.25783(9) 0.59464(8) 0.0229(3) Uani 1 1 d . . . . . S1 S 0.02165(18) 0.17889(18) 0.15796(19) 0.0393(6) Uani 1 1 d . . . . . F1 F -0.0647(4) 0.0339(4) 0.1623(4) 0.078(2) Uani 1 1 d . . . . . F2 F 0.0177(4) 0.0836(4) 0.0353(4) 0.0599(17) Uani 1 1 d . . . . . F3 F -0.1363(4) 0.1881(5) 0.0504(4) 0.078(2) Uani 1 1 d . . . . . O1 O 0.3606(5) 0.3391(4) 1.0532(4) 0.0458(18) Uani 1 1 d . . . . . O2 O 0.1201(4) 0.0920(5) 0.1970(5) 0.0549(19) Uani 1 1 d . . . . . O3 O 0.0329(5) 0.2711(5) 0.0801(5) 0.068(2) Uani 1 1 d . . . . . O4 O -0.0516(4) 0.2038(4) 0.2260(5) 0.0523(19) Uani 1 1 d . . . . . O5 O 0.6702(12) 0.5608(12) 0.7888(12) 0.116(7) Uani 0.5 1 d . . P . . H5D H 0.680243 0.588944 0.728123 0.174 Uiso 0.5 1 d R . P . . H5E H 0.664563 0.611934 0.812093 0.174 Uiso 0.5 1 d R . P . . N1 N 0.3634(5) 0.1754(5) 0.6823(5) 0.0221(16) Uani 1 1 d . . . . . N2 N 0.4183(4) 0.0727(5) 0.7451(5) 0.0247(17) Uani 1 1 d . . . . . N3 N 0.5518(5) 0.2184(5) 0.7140(5) 0.0246(17) Uani 1 1 d . . . . . N4 N 0.5797(5) 0.1131(5) 0.7800(5) 0.0250(17) Uani 1 1 d . . . . . N5 N 0.5407(4) 0.1133(5) 0.5783(5) 0.0227(17) Uani 1 1 d . . . . . N6 N 0.5793(5) 0.0226(5) 0.6614(5) 0.0262(17) Uani 1 1 d . . . . . N7 N 0.3268(4) 0.4731(5) 0.6123(5) 0.0233(17) Uani 1 1 d . . . . . N8 N 0.2955(5) 0.3416(5) 0.4175(5) 0.0271(17) Uani 1 1 d . . . . . N9 N 0.6108(5) 0.3501(5) 0.4646(5) 0.0226(16) Uani 1 1 d . . . . . N10 N 0.7980(4) 0.3399(5) 0.5332(5) 0.0245(17) Uani 1 1 d . . . . . N11 N 0.7969(4) 0.2192(5) 0.4356(5) 0.0217(16) Uani 1 1 d . . . . . N12 N 0.8574(5) 0.4006(5) 0.3396(5) 0.0309(18) Uani 1 1 d . . . . . N13 N 0.6798(5) 0.3988(5) 0.2773(5) 0.0289(18) Uani 1 1 d . . . . . N14 N 0.2963(5) 0.2960(5) 0.9375(5) 0.0350(19) Uani 1 1 d . . . . . C1 C 0.1737(5) 0.2909(6) 0.6272(6) 0.033(2) Uani 1 1 d . . . . . H1A H 0.191005 0.354444 0.628211 0.050 Uiso 1 1 calc GR . . . . H1B H 0.105128 0.291614 0.654693 0.050 Uiso 1 1 calc GR . . . . H1C H 0.168793 0.293431 0.560309 0.050 Uiso 1 1 calc GR . . . . C2 C 0.2601(6) 0.1882(6) 0.6862(6) 0.028(2) Uani 1 1 d . . . . . C3 C 0.2468(6) 0.0932(6) 0.7518(6) 0.025(2) Uani 1 1 d . U . . . H3 H 0.181155 0.080331 0.768718 0.030 Uiso 1 1 calc R . . . . C4 C 0.3451(6) 0.0241(6) 0.7862(6) 0.027(2) Uani 1 1 d . . . . . C5 C 0.3797(6) -0.0928(6) 0.8600(6) 0.037(2) Uani 1 1 d . . . . . H5A H 0.430286 -0.141580 0.832053 0.056 Uiso 1 1 calc GR . . . . H5B H 0.316878 -0.116406 0.876315 0.056 Uiso 1 1 calc GR . . . . H5C H 0.413917 -0.094747 0.918649 0.056 Uiso 1 1 calc GR . . . . C6 C 0.5835(6) 0.3898(5) 0.7018(6) 0.031(2) Uani 1 1 d . . . . . H6A H 0.594985 0.405260 0.633062 0.047 Uiso 1 1 calc GR . . . . H6B H 0.634132 0.410527 0.732030 0.047 Uiso 1 1 calc GR . . . . H6C H 0.510397 0.431597 0.708497 0.047 Uiso 1 1 calc GR . . . . C7 C 0.6005(6) 0.2705(6) 0.7506(6) 0.0217(19) Uani 1 1 d . . . . . C8 C 0.6589(6) 0.2013(6) 0.8371(6) 0.026(2) Uani 1 1 d . . . . . H8 H 0.700427 0.218501 0.876701 0.031 Uiso 1 1 calc R . . . . C9 C 0.6446(6) 0.1026(6) 0.8540(6) 0.029(2) Uani 1 1 d . . . . . C10 C 0.6884(6) -0.0042(6) 0.9372(6) 0.036(2) Uani 1 1 d . . . . . H10A H 0.629151 -0.028719 0.966447 0.055 Uiso 1 1 calc GR . . . . H10B H 0.728443 0.005974 0.985835 0.055 Uiso 1 1 calc GR . . . . H10C H 0.735774 -0.058880 0.913193 0.055 Uiso 1 1 calc GR . . . . C11 C 0.5511(5) 0.1523(6) 0.4006(5) 0.0222(19) Uani 1 1 d . . . . . H11A H 0.477012 0.200550 0.390883 0.033 Uiso 1 1 calc GR . . . . H11B H 0.560920 0.107767 0.359662 0.033 Uiso 1 1 calc GR . . . . H11C H 0.599149 0.195977 0.383367 0.033 Uiso 1 1 calc GR . . . . C12 C 0.5761(6) 0.0796(6) 0.5046(6) 0.025(2) Uani 1 1 d . . . . . C13 C 0.6369(5) -0.0324(6) 0.5396(6) 0.024(2) Uani 1 1 d . . . . . H13 H 0.669810 -0.076447 0.502575 0.028 Uiso 1 1 calc R . . . . C14 C 0.6379(6) -0.0636(6) 0.6383(6) 0.027(2) Uani 1 1 d . . . . . C15 C 0.6899(6) -0.1737(5) 0.7142(6) 0.029(2) Uani 1 1 d . . . . . H15A H 0.743954 -0.169084 0.754750 0.043 Uiso 1 1 calc GR . . . . H15B H 0.723949 -0.226420 0.682711 0.043 Uiso 1 1 calc GR . . . . H15C H 0.635714 -0.197249 0.754524 0.043 Uiso 1 1 calc GR . . . . C16 C 0.3774(6) 0.3897(6) 0.6072(6) 0.021(2) Uani 1 1 d . . . . . C17 C 0.3585(6) 0.3042(6) 0.4844(6) 0.026(2) Uani 1 1 d . . . . . C18 C 0.5481(6) 0.3190(5) 0.5148(6) 0.022(2) Uani 1 1 d . . . . . C19 C 0.8022(6) 0.4078(6) 0.5772(6) 0.028(2) Uani 1 1 d . . . . . H19 H 0.772801 0.483732 0.542468 0.033 Uiso 1 1 calc R . . . . C20 C 0.8455(6) 0.3756(6) 0.6680(6) 0.031(2) Uani 1 1 d . . . . . H20 H 0.850571 0.428256 0.693760 0.037 Uiso 1 1 calc R . . . . C21 C 0.8834(6) 0.2645(7) 0.7248(6) 0.031(2) Uani 1 1 d . . . . . C22 C 0.8759(6) 0.1928(6) 0.6807(6) 0.031(2) Uani 1 1 d . . . . . H22 H 0.900160 0.116738 0.715898 0.038 Uiso 1 1 calc R . . . . C23 C 0.8340(5) 0.2307(6) 0.5871(6) 0.023(2) Uani 1 1 d . . . . . C24 C 0.9313(6) 0.2269(7) 0.8256(6) 0.045(3) Uani 1 1 d . . . . . H24A H 0.931763 0.152216 0.860105 0.068 Uiso 1 1 calc GR . . . . H24B H 0.889003 0.274726 0.858799 0.068 Uiso 1 1 calc GR . . . . H24C H 1.004635 0.228893 0.824232 0.068 Uiso 1 1 calc GR . . . . C25 C 0.8314(5) 0.1625(6) 0.5303(6) 0.025(2) Uani 1 1 d . . . . . C26 C 0.8672(5) 0.0502(6) 0.5672(6) 0.030(2) Uani 1 1 d . . . . . H26 H 0.888600 0.012969 0.634205 0.036 Uiso 1 1 calc R . . . . C27 C 0.8719(6) -0.0088(6) 0.5057(7) 0.029(2) Uani 1 1 d . . . . . C28 C 0.8407(5) 0.0495(6) 0.4093(6) 0.026(2) Uani 1 1 d . . . . . H28 H 0.845126 0.012992 0.364545 0.031 Uiso 1 1 calc R . . . . C29 C 0.8025(5) 0.1624(6) 0.3781(6) 0.026(2) Uani 1 1 d . . . . . H29 H 0.779117 0.201256 0.311674 0.031 Uiso 1 1 calc R . . . . C30 C 0.9103(6) -0.1326(6) 0.5456(6) 0.040(3) Uani 1 1 d . . . . . H30A H 0.852346 -0.158297 0.576595 0.061 Uiso 1 1 calc GR . . . . H30B H 0.971318 -0.158996 0.593354 0.061 Uiso 1 1 calc GR . . . . H30C H 0.931983 -0.160335 0.492709 0.061 Uiso 1 1 calc GR . . . . C31 C 0.9472(6) 0.3986(6) 0.3815(7) 0.038(2) Uani 1 1 d . U . . . H31 H 0.953686 0.383478 0.449216 0.045 Uiso 1 1 calc R . . . . C32 C 1.0323(7) 0.4189(7) 0.3248(8) 0.049(3) Uani 1 1 d . U . . . H32 H 1.096690 0.414758 0.354549 0.059 Uiso 1 1 calc R . . . . C33 C 1.0205(7) 0.4437(7) 0.2298(8) 0.048(3) Uani 1 1 d . U . . . C34 C 0.9306(7) 0.4451(7) 0.1881(7) 0.047(3) Uani 1 1 d . U . . . H34 H 0.923908 0.461799 0.120151 0.056 Uiso 1 1 calc R . . . . C35 C 0.8471(7) 0.4224(6) 0.2432(7) 0.035(2) Uani 1 1 d . U . . . C36 C 1.1110(8) 0.4653(8) 0.1642(9) 0.089(4) Uani 1 1 d . U . . . H36A H 1.136459 0.408646 0.135290 0.134 Uiso 1 1 calc GR . . . . H36B H 1.170166 0.464112 0.203009 0.134 Uiso 1 1 calc GR . . . . H36C H 1.083542 0.536619 0.112832 0.134 Uiso 1 1 calc GR . . . . C37 C 0.7513(7) 0.4139(6) 0.2091(7) 0.034(2) Uani 1 1 d . U . . . C38 C 0.7294(7) 0.4123(6) 0.1186(7) 0.043(2) Uani 1 1 d . U . . . H38 H 0.778619 0.423644 0.070944 0.052 Uiso 1 1 calc R . . . . C39 C 0.6391(7) 0.3950(6) 0.0961(7) 0.038(2) Uani 1 1 d . U . . . C40 C 0.5669(7) 0.3835(6) 0.1643(7) 0.037(2) Uani 1 1 d . U . . . H40 H 0.502257 0.373371 0.150252 0.045 Uiso 1 1 calc R . . . . C41 C 0.5889(6) 0.3866(6) 0.2535(6) 0.032(2) Uani 1 1 d . . . . . H41 H 0.537779 0.379828 0.299967 0.038 Uiso 1 1 calc R . . . . C42 C 0.6215(7) 0.3856(7) -0.0010(7) 0.062(3) Uani 1 1 d . U . . . H42A H 0.675031 0.319932 -0.005268 0.093 Uiso 1 1 calc GR . . . . H42B H 0.628221 0.449735 -0.052906 0.093 Uiso 1 1 calc GR . . . . H42C H 0.549929 0.381108 -0.007529 0.093 Uiso 1 1 calc GR . . . . C43 C 0.2946(7) 0.3135(6) 1.0192(7) 0.037(2) Uani 1 1 d . U . . . H43 H 0.235611 0.305306 1.056053 0.045 Uiso 1 1 calc R . . . . C44 C 0.3869(6) 0.2967(7) 0.8791(6) 0.047(3) Uani 1 1 d . . . . . H44A H 0.436297 0.321655 0.905968 0.070 Uiso 1 1 calc GR . . . . H44B H 0.361718 0.345875 0.812581 0.070 Uiso 1 1 calc GR . . . . H44C H 0.423719 0.222932 0.879332 0.070 Uiso 1 1 calc GR . . . . C45 C 0.2136(7) 0.2669(7) 0.9019(6) 0.048(3) Uani 1 1 d . . . . . H45A H 0.162619 0.255653 0.951053 0.073 Uiso 1 1 calc GR . . . . H45B H 0.245913 0.199786 0.888047 0.073 Uiso 1 1 calc GR . . . . H45C H 0.176240 0.325757 0.842654 0.073 Uiso 1 1 calc GR . . . . C46 C -0.0445(7) 0.1225(7) 0.1002(7) 0.039(2) Uani 1 1 d . U . . . B1 B 0.5403(7) 0.0315(7) 0.7567(7) 0.028(3) Uani 1 1 d . . . . . H1 H 0.566573 -0.041253 0.809429 0.034 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0251(6) 0.0125(6) 0.0298(8) -0.0028(5) 0.0033(5) -0.0049(5) Fe1 0.0239(7) 0.0149(6) 0.0260(8) -0.0028(5) 0.0027(5) -0.0062(5) S1 0.0430(15) 0.0305(14) 0.0492(18) -0.0166(12) 0.0187(13) -0.0170(11) F1 0.098(4) 0.061(4) 0.084(5) -0.007(4) 0.000(4) -0.056(4) F2 0.085(4) 0.043(3) 0.051(4) -0.014(3) -0.016(3) -0.019(3) F3 0.039(3) 0.098(5) 0.069(5) -0.001(4) -0.017(3) -0.013(3) O1 0.063(4) 0.030(4) 0.043(4) -0.003(3) -0.002(3) -0.023(3) O2 0.035(4) 0.065(5) 0.061(5) -0.030(4) -0.002(3) -0.003(3) O3 0.112(6) 0.048(4) 0.059(5) -0.018(4) 0.049(4) -0.052(4) O4 0.049(4) 0.030(4) 0.058(5) -0.004(3) 0.026(3) -0.001(3) O5 0.161(16) 0.075(12) 0.099(16) -0.005(11) 0.019(13) -0.050(11) N1 0.025(4) 0.018(4) 0.025(4) -0.008(3) 0.004(3) -0.009(3) N2 0.026(4) 0.012(4) 0.028(4) -0.001(3) -0.001(3) -0.001(3) N3 0.035(4) 0.007(3) 0.023(4) 0.002(3) -0.006(3) -0.004(3) N4 0.026(4) 0.018(4) 0.027(5) -0.006(3) 0.002(3) -0.004(3) N5 0.026(4) 0.010(4) 0.026(5) 0.000(3) -0.003(3) -0.004(3) N6 0.029(4) 0.024(4) 0.030(5) -0.012(4) 0.003(3) -0.012(3) N7 0.012(3) 0.013(4) 0.033(5) 0.001(3) 0.001(3) 0.002(3) N8 0.029(4) 0.026(4) 0.029(5) -0.011(3) 0.000(3) -0.010(3) N9 0.024(4) 0.017(4) 0.027(5) -0.008(3) 0.003(3) -0.007(3) N10 0.024(4) 0.017(4) 0.032(5) -0.005(3) 0.002(3) -0.010(3) N11 0.017(4) 0.015(4) 0.028(5) -0.003(3) 0.004(3) -0.005(3) N12 0.033(4) 0.012(4) 0.043(5) -0.007(3) 0.003(4) -0.006(3) N13 0.036(4) 0.009(4) 0.037(5) -0.004(3) 0.008(4) -0.006(3) N14 0.039(5) 0.025(4) 0.037(5) -0.006(4) 0.015(4) -0.011(3) C1 0.024(5) 0.037(5) 0.039(6) -0.012(5) 0.004(4) -0.012(4) C2 0.023(5) 0.027(5) 0.040(6) -0.021(4) 0.004(4) -0.007(4) C3 0.028(4) 0.017(3) 0.029(4) -0.004(3) 0.006(3) -0.013(3) C4 0.038(5) 0.016(5) 0.028(6) -0.004(4) 0.005(4) -0.013(4) C5 0.053(6) 0.029(5) 0.036(6) -0.017(5) 0.023(5) -0.017(4) C6 0.029(5) 0.021(5) 0.049(7) -0.014(4) -0.003(4) -0.011(4) C7 0.025(5) 0.017(4) 0.024(5) -0.012(4) 0.004(4) -0.003(3) C8 0.024(5) 0.026(5) 0.027(5) -0.011(4) -0.008(4) -0.007(4) C9 0.024(5) 0.029(5) 0.024(5) -0.003(4) -0.005(4) -0.004(4) C10 0.047(5) 0.027(5) 0.030(6) -0.010(4) -0.004(4) -0.002(4) C11 0.024(4) 0.024(5) 0.022(5) -0.011(4) 0.004(4) -0.009(3) C12 0.024(5) 0.024(5) 0.029(6) -0.010(4) 0.005(4) -0.011(4) C13 0.009(4) 0.022(5) 0.041(6) -0.014(4) -0.003(4) -0.001(3) C14 0.026(5) 0.025(5) 0.030(6) -0.010(4) 0.004(4) -0.006(4) C15 0.039(5) 0.011(4) 0.029(6) -0.001(4) -0.005(4) -0.005(4) C16 0.023(5) 0.015(5) 0.017(5) 0.003(4) 0.000(4) -0.004(4) C17 0.029(5) 0.011(4) 0.041(6) -0.012(4) 0.000(4) -0.006(4) C18 0.023(5) 0.008(4) 0.033(6) -0.008(4) -0.011(4) 0.002(3) C19 0.030(5) 0.017(5) 0.034(6) 0.001(4) -0.008(4) -0.014(4) C20 0.028(5) 0.036(6) 0.036(6) -0.013(4) 0.001(4) -0.018(4) C21 0.019(5) 0.030(5) 0.031(6) 0.000(4) -0.004(4) -0.004(4) C22 0.025(5) 0.025(5) 0.031(6) 0.002(4) -0.002(4) -0.004(4) C23 0.008(4) 0.016(5) 0.034(6) 0.002(4) -0.004(4) -0.001(3) C24 0.049(6) 0.046(6) 0.037(6) -0.004(5) -0.008(5) -0.020(5) C25 0.020(4) 0.017(5) 0.031(6) 0.002(4) 0.004(4) -0.007(3) C26 0.018(4) 0.012(4) 0.047(6) 0.004(4) -0.006(4) -0.003(3) C27 0.018(5) 0.017(5) 0.053(7) -0.010(5) 0.001(4) -0.009(4) C28 0.029(5) 0.018(5) 0.034(6) -0.011(4) 0.007(4) -0.009(4) C29 0.022(5) 0.018(5) 0.036(6) -0.007(4) -0.004(4) -0.008(4) C30 0.032(5) 0.015(5) 0.060(7) -0.001(5) -0.008(5) -0.001(4) C31 0.032(4) 0.031(4) 0.050(5) -0.013(3) 0.008(3) -0.013(3) C32 0.046(4) 0.042(4) 0.064(5) -0.022(4) 0.012(4) -0.018(3) C33 0.044(4) 0.039(4) 0.061(5) -0.017(4) 0.021(4) -0.019(3) C34 0.057(4) 0.033(4) 0.049(5) -0.013(3) 0.020(4) -0.015(3) C35 0.043(4) 0.021(4) 0.039(4) -0.012(3) 0.012(3) -0.006(3) C36 0.100(7) 0.081(7) 0.118(9) -0.058(6) 0.058(6) -0.051(6) C37 0.040(4) 0.020(4) 0.039(4) -0.009(3) 0.007(3) -0.006(3) C38 0.052(4) 0.029(4) 0.038(4) -0.006(3) 0.012(4) -0.004(3) C39 0.048(4) 0.023(4) 0.032(4) -0.009(3) -0.003(3) 0.004(3) C40 0.040(4) 0.025(4) 0.037(4) -0.007(3) -0.007(3) -0.002(3) C41 0.041(6) 0.009(4) 0.039(6) -0.004(4) -0.009(5) -0.003(4) C42 0.076(6) 0.045(6) 0.048(6) -0.023(5) -0.007(5) 0.010(5) C43 0.047(4) 0.027(4) 0.034(4) -0.009(3) 0.015(4) -0.011(3) C44 0.048(6) 0.045(6) 0.031(6) -0.001(5) 0.011(5) -0.008(5) C45 0.083(7) 0.027(5) 0.030(6) 0.003(5) 0.008(5) -0.024(5) C46 0.033(4) 0.036(4) 0.035(4) 0.003(3) 0.004(3) -0.012(3) B1 0.041(6) 0.013(5) 0.021(6) 0.007(4) -0.005(5) -0.009(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -16 -12 -11 0.0585 15 0 9 0.0416 16 11 11 0.0616 3 -16 -1 0.1004 18 1 -2 0.0272 -18 -1 2 0.0002 0 -15 -17 0.0815 -4 0 19 0.0332 4 0 -19 0.0332 -10 1 -14 0.0087 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Co1 N10 93.0(3) 2_666 . ? N7 Co1 N11 175.5(3) 2_666 . ? N7 Co1 N12 90.6(2) 2_666 . ? N7 Co1 N13 91.9(3) 2_666 . ? N9 Co1 N7 90.1(3) . 2_666 ? N9 Co1 N10 88.3(3) . . ? N9 Co1 N11 88.6(2) . . ? N9 Co1 N12 176.9(3) . . ? N9 Co1 N13 94.3(3) . . ? N10 Co1 N11 82.6(3) . . ? N10 Co1 N12 94.7(3) . . ? N10 Co1 N13 174.4(3) . . ? N11 Co1 N12 90.9(2) . . ? N13 Co1 N11 92.6(3) . . ? N13 Co1 N12 82.7(3) . . ? N1 Fe1 N5 87.1(2) . . ? N3 Fe1 N1 88.0(2) . . ? N3 Fe1 N5 89.8(2) . . ? C16 Fe1 N1 93.6(3) . . ? C16 Fe1 N3 90.9(3) . . ? C16 Fe1 N5 179.0(3) . . ? C16 Fe1 C17 85.0(3) . . ? C16 Fe1 C18 92.4(3) . . ? C17 Fe1 N1 92.1(3) . . ? C17 Fe1 N3 175.9(3) . . ? C17 Fe1 N5 94.3(3) . . ? C18 Fe1 N1 174.0(3) . . ? C18 Fe1 N3 91.1(3) . . ? C18 Fe1 N5 87.0(3) . . ? C18 Fe1 C17 89.3(3) . . ? O2 S1 O3 114.5(4) . . ? O2 S1 C46 102.6(4) . . ? O3 S1 C46 103.1(4) . . ? O4 S1 O2 116.3(4) . . ? O4 S1 O3 115.6(4) . . ? O4 S1 C46 101.7(4) . . ? H5D O5 H5E 104.5 . . ? N2 N1 Fe1 115.6(4) . . ? C2 N1 Fe1 135.9(5) . . ? C2 N1 N2 107.7(6) . . ? N1 N2 B1 120.9(6) . . ? C4 N2 N1 107.6(6) . . ? C4 N2 B1 131.5(6) . . ? N4 N3 Fe1 118.5(5) . . ? C7 N3 Fe1 136.1(5) . . ? C7 N3 N4 105.4(6) . . ? N3 N4 B1 118.1(6) . . ? C9 N4 N3 109.7(6) . . ? C9 N4 B1 132.1(6) . . ? N6 N5 Fe1 117.7(5) . . ? C12 N5 Fe1 136.6(5) . . ? C12 N5 N6 105.6(6) . . ? N5 N6 B1 118.0(7) . . ? C14 N6 N5 110.2(7) . . ? C14 N6 B1 131.3(7) . . ? C16 N7 Co1 164.6(7) . 2_666 ? C18 N9 Co1 167.2(6) . . ? C19 N10 Co1 127.9(5) . . ? C19 N10 C23 116.9(7) . . ? C23 N10 Co1 114.8(5) . . ? C25 N11 Co1 113.7(6) . . ? C29 N11 Co1 128.7(5) . . ? C29 N11 C25 117.3(6) . . ? C31 N12 Co1 125.6(6) . . ? C31 N12 C35 120.4(7) . . ? C35 N12 Co1 114.0(5) . . ? C37 N13 Co1 113.9(5) . . ? C41 N13 Co1 126.5(6) . . ? C41 N13 C37 118.9(8) . . ? C43 N14 C44 121.4(8) . . ? C43 N14 C45 123.3(8) . . ? C45 N14 C44 115.1(8) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C2 C1 123.5(7) . . ? N1 C2 C3 109.1(6) . . ? C3 C2 C1 127.4(7) . . ? C2 C3 H3 126.8 . . ? C4 C3 C2 106.3(6) . . ? C4 C3 H3 126.8 . . ? N2 C4 C5 121.2(7) . . ? C3 C4 N2 109.2(6) . . ? C3 C4 C5 129.5(7) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? N3 C7 C6 121.2(7) . . ? N3 C7 C8 110.9(6) . . ? C8 C7 C6 127.8(7) . . ? C7 C8 H8 127.0 . . ? C9 C8 C7 105.9(6) . . ? C9 C8 H8 127.0 . . ? N4 C9 C8 108.1(6) . . ? N4 C9 C10 121.5(7) . . ? C8 C9 C10 130.4(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? N5 C12 C11 123.3(7) . . ? N5 C12 C13 110.4(7) . . ? C13 C12 C11 126.2(8) . . ? C12 C13 H13 127.4 . . ? C14 C13 C12 105.1(8) . . ? C14 C13 H13 127.4 . . ? N6 C14 C13 108.6(7) . . ? N6 C14 C15 122.0(8) . . ? C13 C14 C15 129.3(8) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 Fe1 177.7(7) . . ? N8 C17 Fe1 173.9(7) . . ? N9 C18 Fe1 175.2(7) . . ? N10 C19 H19 118.1 . . ? N10 C19 C20 123.9(7) . . ? C20 C19 H19 118.1 . . ? C19 C20 H20 119.8 . . ? C19 C20 C21 120.4(8) . . ? C21 C20 H20 119.8 . . ? C20 C21 C24 121.4(8) . . ? C22 C21 C20 116.1(8) . . ? C22 C21 C24 122.4(7) . . ? C21 C22 H22 119.7 . . ? C23 C22 C21 120.5(7) . . ? C23 C22 H22 119.7 . . ? N10 C23 C25 112.6(7) . . ? C22 C23 N10 122.0(8) . . ? C22 C23 C25 125.2(7) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 C23 114.2(6) . . ? N11 C25 C26 122.1(8) . . ? C26 C25 C23 123.6(8) . . ? C25 C26 H26 120.1 . . ? C25 C26 C27 119.9(8) . . ? C27 C26 H26 120.1 . . ? C26 C27 C30 120.4(8) . . ? C28 C27 C26 117.5(7) . . ? C28 C27 C30 122.1(8) . . ? C27 C28 H28 120.4 . . ? C27 C28 C29 119.2(8) . . ? C29 C28 H28 120.4 . . ? N11 C29 C28 123.9(8) . . ? N11 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N12 C31 H31 119.8 . . ? N12 C31 C32 120.3(9) . . ? C32 C31 H31 119.8 . . ? C31 C32 H32 120.4 . . ? C33 C32 C31 119.2(9) . . ? C33 C32 H32 120.4 . . ? C32 C33 C34 120.4(9) . . ? C32 C33 C36 121.6(9) . . ? C34 C33 C36 117.9(10) . . ? C33 C34 H34 119.4 . . ? C33 C34 C35 121.2(10) . . ? C35 C34 H34 119.4 . . ? N12 C35 C34 118.5(8) . . ? N12 C35 C37 114.7(8) . . ? C34 C35 C37 126.7(9) . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N13 C37 C35 114.2(8) . . ? N13 C37 C38 119.0(8) . . ? C38 C37 C35 126.6(9) . . ? C37 C38 H38 119.1 . . ? C39 C38 C37 121.9(9) . . ? C39 C38 H38 119.1 . . ? C38 C39 C40 118.3(9) . . ? C38 C39 C42 120.5(9) . . ? C40 C39 C42 121.2(9) . . ? C39 C40 H40 120.4 . . ? C39 C40 C41 119.2(8) . . ? C41 C40 H40 120.4 . . ? N13 C41 C40 122.6(9) . . ? N13 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 C43 N14 127.0(9) . . ? O1 C43 H43 116.5 . . ? N14 C43 H43 116.5 . . ? N14 C44 H44A 109.5 . . ? N14 C44 H44B 109.5 . . ? N14 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N14 C45 H45A 109.5 . . ? N14 C45 H45B 109.5 . . ? N14 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? F1 C46 S1 112.5(7) . . ? F1 C46 F2 103.8(8) . . ? F2 C46 S1 111.4(6) . . ? F3 C46 S1 116.4(7) . . ? F3 C46 F1 106.4(6) . . ? F3 C46 F2 105.4(8) . . ? N2 B1 H1 110.2 . . ? N4 B1 N2 109.1(7) . . ? N4 B1 H1 110.2 . . ? N6 B1 N2 107.6(6) . . ? N6 B1 N4 109.5(6) . . ? N6 B1 H1 110.2 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 1.916(6) 2_666 ? Co1 N9 1.888(6) . ? Co1 N10 1.926(6) . ? Co1 N11 1.945(6) . ? Co1 N12 1.946(7) . ? Co1 N13 1.939(7) . ? Fe1 N1 2.048(6) . ? Fe1 N3 2.027(6) . ? Fe1 N5 2.053(6) . ? Fe1 C16 1.857(8) . ? Fe1 C17 1.900(8) . ? Fe1 C18 1.870(8) . ? S1 O2 1.437(6) . ? S1 O3 1.439(6) . ? S1 O4 1.424(6) . ? S1 C46 1.744(10) . ? F1 C46 1.354(9) . ? F2 C46 1.380(11) . ? F3 C46 1.323(8) . ? O1 C43 1.222(9) . ? O5 H5D 0.8700 . ? O5 H5E 0.8697 . ? N1 N2 1.377(7) . ? N1 C2 1.326(8) . ? N2 C4 1.361(8) . ? N2 B1 1.528(10) . ? N3 N4 1.385(7) . ? N3 C7 1.346(9) . ? N4 C9 1.355(9) . ? N4 B1 1.521(10) . ? N5 N6 1.387(8) . ? N5 C12 1.340(10) . ? N6 C14 1.347(10) . ? N6 B1 1.513(12) . ? N7 C16 1.163(9) . ? N8 C17 1.172(8) . ? N9 C18 1.179(9) . ? N10 C19 1.327(9) . ? N10 C23 1.374(8) . ? N11 C25 1.359(9) . ? N11 C29 1.326(10) . ? N12 C31 1.349(9) . ? N12 C35 1.353(10) . ? N13 C37 1.367(10) . ? N13 C41 1.342(8) . ? N14 C43 1.307(11) . ? N14 C44 1.453(10) . ? N14 C45 1.450(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.511(9) . ? C2 C3 1.398(9) . ? C3 H3 0.9500 . ? C3 C4 1.339(9) . ? C4 C5 1.538(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6 C7 1.501(9) . ? C7 C8 1.382(9) . ? C8 H8 0.9500 . ? C8 C9 1.373(9) . ? C9 C10 1.513(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 C12 1.498(10) . ? C12 C13 1.416(9) . ? C13 H13 0.9500 . ? C13 C14 1.371(11) . ? C14 C15 1.507(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C19 H19 0.9500 . ? C19 C20 1.345(10) . ? C20 H20 0.9500 . ? C20 C21 1.404(10) . ? C21 C22 1.388(11) . ? C21 C24 1.488(10) . ? C22 H22 0.9500 . ? C22 C23 1.367(10) . ? C23 C25 1.470(11) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.379(9) . ? C26 H26 0.9500 . ? C26 C27 1.402(11) . ? C27 C28 1.376(10) . ? C27 C30 1.522(9) . ? C28 H28 0.9500 . ? C28 C29 1.388(9) . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C31 C32 1.422(11) . ? C32 H32 0.9500 . ? C32 C33 1.327(13) . ? C33 C34 1.353(11) . ? C33 C36 1.552(13) . ? C34 H34 0.9500 . ? C34 C35 1.402(11) . ? C35 C37 1.434(10) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.386(12) . ? C38 H38 0.9500 . ? C38 C39 1.364(10) . ? C39 C40 1.369(12) . ? C39 C42 1.516(12) . ? C40 H40 0.9500 . ? C40 C41 1.377(11) . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? B1 H1 1.0000 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5 H5D N8 0.87 2.09 2.963(17) 179.3 2_666 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co1 N10 C19 C20 177.4(6) . . . . ? Co1 N10 C23 C22 -176.1(6) . . . . ? Co1 N10 C23 C25 9.3(8) . . . . ? Co1 N11 C25 C23 -11.7(8) . . . . ? Co1 N11 C25 C26 172.4(5) . . . . ? Co1 N11 C29 C28 -173.6(5) . . . . ? Co1 N12 C31 C32 -179.7(6) . . . . ? Co1 N12 C35 C34 178.1(6) . . . . ? Co1 N12 C35 C37 -5.0(9) . . . . ? Co1 N13 C37 C35 -7.0(8) . . . . ? Co1 N13 C37 C38 168.8(6) . . . . ? Co1 N13 C41 C40 -166.6(6) . . . . ? Fe1 N1 N2 C4 -170.7(5) . . . . ? Fe1 N1 N2 B1 7.9(9) . . . . ? Fe1 N1 C2 C1 -11.4(13) . . . . ? Fe1 N1 C2 C3 168.4(6) . . . . ? Fe1 N3 N4 C9 179.8(5) . . . . ? Fe1 N3 N4 B1 3.0(9) . . . . ? Fe1 N3 C7 C6 3.4(12) . . . . ? Fe1 N3 C7 C8 -179.9(6) . . . . ? Fe1 N5 N6 C14 -176.9(5) . . . . ? Fe1 N5 N6 B1 10.1(8) . . . . ? Fe1 N5 C12 C11 -3.9(11) . . . . ? Fe1 N5 C12 C13 177.3(5) . . . . ? O2 S1 C46 F1 61.8(8) . . . . ? O2 S1 C46 F2 -54.3(7) . . . . ? O2 S1 C46 F3 -175.1(7) . . . . ? O3 S1 C46 F1 -179.0(7) . . . . ? O3 S1 C46 F2 64.9(7) . . . . ? O3 S1 C46 F3 -55.9(8) . . . . ? O4 S1 C46 F1 -58.9(7) . . . . ? O4 S1 C46 F2 -175.0(6) . . . . ? O4 S1 C46 F3 64.2(7) . . . . ? N1 N2 C4 C3 -0.7(9) . . . . ? N1 N2 C4 C5 179.5(7) . . . . ? N1 N2 B1 N4 53.5(10) . . . . ? N1 N2 B1 N6 -65.2(9) . . . . ? N1 C2 C3 C4 -0.2(10) . . . . ? N2 N1 C2 C1 180.0(8) . . . . ? N2 N1 C2 C3 -0.2(9) . . . . ? N3 N4 C9 C8 0.5(9) . . . . ? N3 N4 C9 C10 -179.7(7) . . . . ? N3 N4 B1 N2 -59.7(9) . . . . ? N3 N4 B1 N6 57.9(9) . . . . ? N3 C7 C8 C9 -0.3(9) . . . . ? N4 N3 C7 C6 -176.1(7) . . . . ? N4 N3 C7 C8 0.6(9) . . . . ? N5 N6 C14 C13 -1.6(8) . . . . ? N5 N6 C14 C15 -179.9(6) . . . . ? N5 N6 B1 N2 52.8(8) . . . . ? N5 N6 B1 N4 -65.6(8) . . . . ? N5 C12 C13 C14 -1.2(8) . . . . ? N6 N5 C12 C11 179.1(6) . . . . ? N6 N5 C12 C13 0.3(8) . . . . ? N7 Co1 N9 C18 -130(3) 2_666 . . . ? N10 Co1 N9 C18 -36(3) . . . . ? N10 C19 C20 C21 -4.4(13) . . . . ? N10 C23 C25 N11 1.7(9) . . . . ? N10 C23 C25 C26 177.5(6) . . . . ? N11 Co1 N9 C18 46(3) . . . . ? N11 C25 C26 C27 2.0(11) . . . . ? N12 C31 C32 C33 2.4(13) . . . . ? N12 C35 C37 N13 7.9(10) . . . . ? N12 C35 C37 C38 -167.5(8) . . . . ? N13 Co1 N9 C18 139(3) . . . . ? N13 C37 C38 C39 -0.7(13) . . . . ? C1 C2 C3 C4 179.6(8) . . . . ? C2 N1 N2 C4 0.5(9) . . . . ? C2 N1 N2 B1 179.1(7) . . . . ? C2 C3 C4 N2 0.5(10) . . . . ? C2 C3 C4 C5 -179.6(9) . . . . ? C4 N2 B1 N4 -128.3(9) . . . . ? C4 N2 B1 N6 112.9(9) . . . . ? C6 C7 C8 C9 176.1(8) . . . . ? C7 N3 N4 C9 -0.6(9) . . . . ? C7 N3 N4 B1 -177.4(7) . . . . ? C7 C8 C9 N4 -0.1(9) . . . . ? C7 C8 C9 C10 -179.9(9) . . . . ? C9 N4 B1 N2 124.5(9) . . . . ? C9 N4 B1 N6 -118.0(9) . . . . ? C11 C12 C13 C14 -179.9(7) . . . . ? C12 N5 N6 C14 0.8(8) . . . . ? C12 N5 N6 B1 -172.2(6) . . . . ? C12 C13 C14 N6 1.7(8) . . . . ? C12 C13 C14 C15 179.9(7) . . . . ? C14 N6 B1 N2 -118.3(8) . . . . ? C14 N6 B1 N4 123.2(8) . . . . ? C19 N10 C23 C22 -2.3(11) . . . . ? C19 N10 C23 C25 -176.9(6) . . . . ? C19 C20 C21 C22 1.9(12) . . . . ? C19 C20 C21 C24 -179.8(8) . . . . ? C20 C21 C22 C23 0.2(12) . . . . ? C21 C22 C23 N10 0.0(12) . . . . ? C21 C22 C23 C25 174.0(7) . . . . ? C22 C23 C25 N11 -172.8(7) . . . . ? C22 C23 C25 C26 3.1(12) . . . . ? C23 N10 C19 C20 4.5(12) . . . . ? C23 C25 C26 C27 -173.5(7) . . . . ? C24 C21 C22 C23 -178.2(7) . . . . ? C25 N11 C29 C28 0.4(11) . . . . ? C25 C26 C27 C28 0.5(11) . . . . ? C25 C26 C27 C30 -179.4(6) . . . . ? C26 C27 C28 C29 -2.4(11) . . . . ? C27 C28 C29 N11 2.0(11) . . . . ? C29 N11 C25 C23 173.5(6) . . . . ? C29 N11 C25 C26 -2.5(10) . . . . ? C30 C27 C28 C29 177.5(6) . . . . ? C31 N12 C35 C34 -1.4(11) . . . . ? C31 N12 C35 C37 175.5(7) . . . . ? C31 C32 C33 C34 -2.8(14) . . . . ? C31 C32 C33 C36 -179.1(8) . . . . ? C32 C33 C34 C35 1.1(14) . . . . ? C33 C34 C35 N12 1.0(13) . . . . ? C33 C34 C35 C37 -175.4(8) . . . . ? C34 C35 C37 N13 -175.5(8) . . . . ? C34 C35 C37 C38 9.1(14) . . . . ? C35 N12 C31 C32 -0.3(11) . . . . ? C35 C37 C38 C39 174.5(8) . . . . ? C36 C33 C34 C35 177.6(8) . . . . ? C37 N13 C41 C40 3.2(11) . . . . ? C37 C38 C39 C40 2.7(12) . . . . ? C37 C38 C39 C42 -175.5(8) . . . . ? C38 C39 C40 C41 -1.8(12) . . . . ? C39 C40 C41 N13 -1.2(12) . . . . ? C41 N13 C37 C35 -178.0(6) . . . . ? C41 N13 C37 C38 -2.2(11) . . . . ? C42 C39 C40 C41 176.4(7) . . . . ? C44 N14 C43 O1 5.5(14) . . . . ? C45 N14 C43 O1 -179.3(8) . . . . ? B1 N2 C4 C3 -179.0(8) . . . . ? B1 N2 C4 C5 1.1(14) . . . . ? B1 N4 C9 C8 176.6(8) . . . . ? B1 N4 C9 C10 -3.6(14) . . . . ? B1 N6 C14 C13 170.1(7) . . . . ? B1 N6 C14 C15 -8.2(12) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 2 1.82 5.72 0 0 -2 10.28 9.25 0 0 3 257.54 35.67 0 0 -3 262.36 35.81 0 0 4 783.38 69.26 0 0 5 1588.11 109.95 0 0 6 1007.13 96.46 0 0 7 270.53 56.96 0 0 8 -13.03 19.48 0 0 9 645.44 98.36 0 0 10 180.88 56.66 0 0 11 484.98 95.82 0 0 12 315.79 81.35 0 0 13 69.27 46.57 0 0 14 51.39 43.32 0 0 15 186.92 74.82 0 0 16 102.3 54.21 0 0 16 138.36 63.9 0 0 17 59.21 52.75 0 0 17 41.43 43.85 0 0 18 -16.68 35.37 0 0 18 -16.51 35.12 0 -1 17 197.51 84.39 0 -1 17 77.33 47.15 0 -1 16 51.19 48.42 0 -1 16 -13.58 24.19 0 -1 15 -68.64 58.9 0 -1 15 -8.77 30.44 0 -1 14 86.31 58.08 0 -1 14 72.42 44.48 0 -1 13 8.01 29.72 0 -1 13 47.78 36.72 0 -1 12 -31.41 30.17 0 -1 11 22.38 28.35 0 -1 10 388.35 84.54 0 -1 9 83.54 38.74 0 -1 8 -4.9 17.5 0 -1 7 -9.8 21.93 0 -1 6 1222.59 110.53 0 -1 5 1.87 22.38 0 -1 4 60.99 26.51 0 -1 3 70.64 23.56 0 -1 3 41.24 9.21 0 -1 2 1054.46 54.88 0 -1 2 1046.27 41.2 0 -1 2 1070.24 65.4 0 1 -2 1057.94 64.91 0 1 2 1132.54 55.62 0 1 3 2101.19 92.97 0 -1 -3 2447.08 101.05 0 -1 -4 601.61 31.63 0 1 4 626.83 59.58 0 1 5 384.61 52.54 0 1 6 3.15 16.44 0 1 7 181.85 45.36 0 1 8 -3.12 19.86 0 1 9 29.12 23.19 0 1 10 320.64 72.2 0 1 11 -6.07 23.27 0 1 12 41.19 37.16 0 1 13 42.61 47.4 0 1 14 35.45 41.84 0 1 15 87.95 49.13 0 1 16 -122.31 63.83 0 1 17 -28.53 39.15 0 1 18 -24.65 39.22 0 1 18 -47.91 52.35 0 1 19 114.81 63.74 0 -2 17 -131.81 83.21 0 -2 16 -1.57 29.8 0 -2 16 81.3 57.48 0 -2 15 -26.49 37.22 0 -2 15 118.52 64.22 0 -2 14 127.89 54.88 0 -2 14 182.73 77.09 0 -2 13 133.81 54.56 0 -2 13 134.84 62.04 0 -2 12 -8.53 19.06 0 -2 12 -26.82 34.57 0 -2 11 86.62 39.87 0 -2 11 121.86 56.66 0 -2 10 281.2 62.23 0 -2 10 480.56 95.8 0 -2 9 413.57 74.42 0 -2 9 570.2 98.45 0 -2 8 53.77 30.18 0 -2 8 50.9 33.46 0 -2 7 19.28 21.56 0 -2 7 34.45 28.8 0 -2 6 436.69 60.6 0 -2 6 388.17 32.98 0 -2 6 327.72 62.54 0 -2 5 100.93 29.45 0 -2 5 113.71 38.54 0 -2 5 123.28 20.55 0 -2 4 590.58 58.76 0 -2 4 618.43 44.53 0 -2 4 654.87 73.6 0 -2 3 70.66 23.13 0 -2 3 93.47 28.58 0 -2 3 50.81 17.21 0 -2 2 100.32 23.53 0 2 -2 73.41 20.96 0 -2 2 198.74 38.62 0 -2 2 108.31 23.44 0 -2 2 95.05 28.72 0 -2 1 842.12 51.55 0 2 -1 801.4 49.55 0 -2 1 839.96 59.02 0 2 -1 737.71 55.62 0 -2 0 1079.77 53.87 0 2 0 1194.92 57.52 0 2 0 1130.18 61.85 0 -2 0 1131.39 60.92 0 2 1 2316.88 84.21 0 -2 -1 2149.87 78.29 0 2 1 2320.81 83.73 0 -2 -1 2201.71 81.99 0 -2 -2 1655.71 75.71 0 2 2 1650.68 75.5 0 2 3 1277.12 74.2 0 -2 -3 1268.72 74.48 0 2 3 1159.14 71.95 0 2 4 23.79 16.22 0 -2 -5 589.53 45.47 0 2 5 599.54 65.19 0 2 6 295.9 51.17 0 -2 -6 233.96 28.75 0 -2 -7 1182.96 60.24 0 2 7 1235.22 110.03 0 -2 -8 81.06 15.94 0 2 8 61.89 29.32 0 2 9 16.86 21.8 0 2 10 -3.48 16.28 0 2 11 -31.54 28.94 0 2 12 86.03 45.66 0 2 13 89.08 50.17 0 2 14 -42.22 38.49 0 2 15 -114.96 67.65 0 2 16 -31.72 46.08 0 2 17 7.07 32.67 0 2 18 -22.68 50.91 0 -3 17 27.44 50.76 0 -3 16 59.28 48.14 0 -3 15 52.03 51.33 0 -3 14 167.25 77.82 0 -3 14 123.42 56.16 0 -3 13 71.57 50.89 0 -3 13 -8.11 22.71 0 -3 12 1.8 30.25 0 -3 12 35.39 36.41 0 -3 11 25.77 27.07 0 -3 11 56.17 32.44 0 -3 10 -4.48 25.7 0 -3 10 31.18 28.83 0 -3 9 226.07 66.16 0 -3 9 170.98 48.92 0 -3 8 599.41 83.57 0 -3 8 743.97 110.71 0 -3 7 520.27 72.82 0 -3 7 474.45 45.83 0 -3 7 494.85 86.35 0 -3 6 51.34 26.61 0 -3 6 16.44 11.22 0 -3 6 1.33 15.5 0 -3 5 19.52 17.38 0 -3 5 -5.89 15.09 0 -3 5 1.09 9.39 0 -3 4 109.82 31.02 0 -3 4 146.48 40.79 0 -3 4 75.38 29.17 0 -3 4 55.22 18.36 0 3 -3 1847.83 67.73 0 -3 3 2013.91 107.62 0 -3 3 2128.18 103.1 0 -3 3 1975.53 123.94 0 -3 3 2019.48 71.93 0 -3 2 1925.47 97.19 0 3 -2 1991.96 98.13 0 -3 2 1899.94 98.27 0 -3 2 1859.03 112.44 0 3 -1 2637.32 107.69 0 -3 1 2638.88 108.09 0 -3 1 2684.39 124.06 0 3 0 1088.69 67.02 0 -3 0 1004.74 64.2 0 -3 0 1125.72 75.53 0 -3 -1 8568.96 191.5 0 3 1 9686.54 201.87 0 -3 -1 9176.96 204.15 0 3 2 3350.98 125.23 0 -3 -2 3270.31 123.39 0 -3 -3 856.13 66.67 0 -3 -4 749.41 68.07 0 3 4 672.27 65.41 0 3 5 320.6 51.63 0 3 6 733.22 80.36 0 3 7 27.7 21.05 0 3 8 256 54.77 0 3 9 169.95 47.18 0 -3 -9 153.01 27.57 0 3 10 42.07 27.01 0 -3 -10 34.51 13.3 0 3 11 241.57 67.11 0 3 12 131.8 57.09 0 3 13 494.67 99.98 0 3 14 147.67 63.54 0 3 15 63.87 58.51 0 3 16 49.18 43.33 0 3 17 221 83.79 0 3 18 128.62 74.37 0 -4 16 -13.18 32.17 0 -4 16 95.37 60.09 0 -4 15 -37.19 45.89 0 -4 15 -21.71 33.66 0 -4 14 46.13 50.08 0 -4 14 88.16 62.53 0 -4 13 24.08 35.85 0 -4 13 16.33 34.75 0 -4 12 0.33 22.7 0 -4 12 -24.93 33.87 0 -4 12 -63.22 47.36 0 -4 11 81.38 40.26 0 -4 11 32.47 33.67 0 -4 11 42.89 38.85 0 -4 10 15.15 24.32 0 -4 10 -10.37 22.32 0 -4 10 26.98 27.72 0 -4 9 147.45 47.93 0 -4 9 22.16 28.47 0 -4 9 175.91 59.51 0 -4 8 52.3 34.11 0 -4 8 31.87 22.54 0 -4 8 57.15 36.77 0 -4 7 48.89 32 0 -4 7 89.39 40.34 0 -4 7 83.01 34.93 0 -4 6 33.53 26.72 0 4 -6 19.3 14.64 0 -4 6 5.01 24.41 0 -4 6 12.73 17.77 0 -4 5 114.01 39.28 0 4 -5 136.42 25.29 0 -4 5 129.48 25.02 0 -4 5 131.5 35.57 0 -4 4 157.43 47.03 0 -4 4 200.91 41.94 0 -4 4 177.48 24.69 0 4 -4 180.62 23.86 0 -4 3 186.45 19.18 0 -4 3 179.03 42.29 0 -4 3 204.72 39.1 0 -4 2 168.61 39.43 0 -4 2 260.02 43.15 0 -4 1 726.43 74.26 0 -4 1 737.91 66.04 0 -4 0 1464.38 99.12 0 -4 0 1404.1 87.4 0 -4 -1 3181.34 140.28 0 -4 -1 3139.9 133.72 0 -4 -2 166 35.19 0 -4 -3 665.75 65.99 0 -4 -4 417.11 55.34 0 -4 -5 56.06 26.83 0 4 5 23.55 17.22 0 4 6 3.24 15.92 0 4 7 1208.2 112.23 0 4 8 163.16 43.95 0 4 9 28.59 22.07 0 4 10 1.39 20.08 0 4 11 57.04 33.14 0 4 12 20.05 28.35 0 4 13 -35.88 35.66 0 4 14 -22.5 30.89 0 4 15 20.1 31.32 0 4 16 4.28 34.39 0 4 17 81.12 57.81 0 4 18 69.69 59.68 0 4 19 -12.24 39.11 0 -5 16 60.97 54.55 0 -5 15 -30.21 49.04 0 -5 14 46.87 43.63 0 -5 13 88.69 61.3 0 -5 12 176.56 71.23 0 -5 12 149.07 56.65 0 -5 11 14.6 29.17 0 -5 11 -5.23 26.58 0 -5 10 -21 34.46 0 -5 10 3.24 24.74 0 -5 9 61.36 42.04 0 -5 9 35.55 27.16 0 5 -8 1685.88 113.42 0 -5 8 1718.88 153.79 0 -5 8 1558.94 169.63 0 -5 7 1571.41 138.53 0 5 -7 1467.88 95.22 0 -5 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66.13 53.69 -16 -8 3 27.96 44.49 -16 -8 2 145.79 79.96 -16 -8 1 28.37 42.12 -16 -8 0 73.75 55.5 -16 -8 -1 151.19 77.98 -16 -8 -2 66.19 54.47 -16 -8 -3 131.74 63.3 -16 -8 -4 90.77 65.12 -16 -8 -5 34.68 42.22 -16 -8 -6 48.99 53.36 -16 -8 -7 128 76.79 16 8 9 101.41 66.29 16 8 10 -57.75 54.69 16 8 10 44.56 51.67 16 9 -5 -121.68 78.97 -16 -9 4 -26.96 35.29 16 9 -4 65.27 62.09 -16 -9 3 50.37 50.19 16 9 -3 66.97 55.84 -16 -9 2 -13.01 32.02 -16 -9 1 114.37 67.78 -16 -9 0 -16.6 33.37 -16 -9 -1 58.83 63.36 -16 -9 -2 46.93 44.82 -16 -9 -3 117.46 74.79 -16 -9 -4 55.92 49 -16 -9 -5 -19.27 38.41 -16 -9 -6 -1.75 42.31 16 9 6 16.67 42.96 -16 -9 -7 8.44 32.48 16 9 7 -12.1 41.03 16 9 8 127.23 76.91 16 9 9 31.18 38.53 16 9 10 -4.03 42.44 16 10 -3 -126.52 83.84 -16 -10 2 40.33 43.95 16 10 -2 6.54 39.76 -16 -10 1 34.07 52.4 16 10 -1 -123.18 79.74 -16 -10 0 5.43 44.98 16 10 0 18.66 35.43 -16 -10 -1 76.97 55.1 16 10 1 62.92 54.33 -16 -10 -2 159.66 77.4 16 10 2 153.66 81.89 -16 -10 -3 184.68 92.28 16 10 3 85.93 68.62 -16 -10 -4 245.47 96.02 16 10 4 68.2 63.31 -16 -10 -5 85.39 67.71 16 10 5 30.89 34.39 -16 -10 -6 39.84 40.2 16 10 6 -5.07 38.73 16 10 7 88.37 70.5 16 10 8 13.63 38.95 16 10 9 35.15 43.29 16 10 10 -107.48 73.08 -16 -11 0 17.32 41.09 16 11 0 57.45 54.05 -16 -11 -1 81.95 69.88 16 11 1 78.58 70.3 -16 -11 -2 -42.61 56.22 16 11 2 38.47 55.13 -16 -11 -3 91.77 58.38 16 11 3 111.94 74.74 -16 -11 -4 48.75 51.99 16 11 4 7.6 28.86 -16 -11 -5 5.12 40.1 16 11 5 37.74 52.83 16 11 6 32.89 43.41 16 11 7 -61.34 63.33 -16 -12 -2 4.28 31.64 -16 -12 -3 -62.5 58.99 -16 -12 -4 46.18 49.28 17 -1 -1 32.72 49.15 17 0 0 -6.44 34.83 17 0 1 23.56 41.15 17 1 1 -2.41 44.01 17 1 2 -7.67 41.87 17 1 3 256.67 104.99 17 2 3 -103.19 74.82 17 2 4 10.55 46.26 17 3 4 -153.85 79.59 17 3 5 -36.82 65.04 -17 -4 2 39.35 56.88 -17 -4 1 64.31 55.87 -17 -4 0 103.73 70.18 -17 -4 -1 -7.5 48.85 17 4 5 -87.88 67.96 17 4 6 21.36 50.72 -17 -5 3 -2.63 40.27 -17 -5 2 -67.74 55.16 -17 -5 1 -36.31 52.4 -17 -5 0 112.04 84.53 -17 -5 -1 69.41 55 -17 -5 -2 50.53 55.49 17 5 7 49.4 50.23 -17 -6 4 120.12 70.07 -17 -6 3 41.18 52.52 -17 -6 2 108.74 73.49 -17 -6 1 62.49 60.96 -17 -6 0 -26.08 40.34 -17 -6 -1 91.89 68.95 -17 -6 -2 142.4 78.24 -17 -6 -3 102.33 74.05 17 6 8 10.23 50.81 -17 -7 4 28.52 55.87 -17 -7 3 -4.5 50.73 -17 -7 2 23.99 42.68 -17 -7 1 44.51 47.01 -17 -7 0 42.09 45.36 -17 -7 -1 22.93 51.44 -17 -7 -2 6.94 39.77 -17 -7 -3 -46.46 58.56 -17 -8 4 -75.84 65.98 -17 -8 3 82.79 77.32 -17 -8 2 -73.41 65.78 -17 -8 1 -1.69 43.11 -17 -8 0 44.4 46.12 -17 -8 -1 23.74 43.51 -17 -8 -2 -53.62 58.55 -17 -8 -3 68.69 58.74 -17 -9 4 -4.15 38.93 -17 -9 3 -0.47 26.98 -17 -9 2 34.79 50.8 -17 -9 1 34.47 52.3 -17 -9 0 52.25 53.64 -17 -9 -1 -0.28 39.79 -17 -9 -2 223.31 98.14 -17 -9 -3 134.23 78.58 -17 -10 2 -47.47 48.32 -17 -10 1 15.32 32.95 -17 -10 0 44.88 44.76 -17 -10 -1 -1.66 42.14 -17 -10 -2 117.91 71.32 -17 -10 -3 -11.92 30.98 -17 -11 0 67.32 58.28 -17 -11 -1 -89.89 60.35 -17 -11 -2 46.18 47.23 -17 -11 -3 -4.32 29.83 -17 -12 -2 36.19 52.45 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -15.6916 -12.0545 -11.0138 -0.0093 -0.0146 0.9999 14.9327 -0.4826 8.6855 -0.5754 0.2718 -0.7714 15.7720 11.0967 11.3280 -0.0544 0.0233 -0.9982 3.0537 -16.4726 -1.2630 -0.8983 0.4276 0.1011 17.9231 0.7370 -1.7877 -0.2062 0.6988 -0.6849 -17.9231 -0.7370 1.7877 0.2062 -0.6988 0.6849 0.4259 -15.0797 -17.0339 -0.2444 0.8181 0.5206 -4.0989 -0.1434 19.2906 -0.5906 -0.7703 -0.2404 4.0989 0.1434 -19.2906 0.5906 0.7703 0.2404 -10.4473 1.0155 -14.1153 0.7113 0.0583 0.7005