#------------------------------------------------------------------------------ #$Date: 2021-04-05 16:49:32 +0300 (Mon, 05 Apr 2021) $ #$Revision: 263610 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/00/1560076.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_1560076 loop_ _publ_author_name 'Diment, Wilfred T.' 'St\"o\&ser, Tim' 'Kerr, Ryan W. F.' 'Phanopoulos, Andreas' 'Durr, Christopher B.' 'Williams, Charlotte K.' _publ_section_title ; Ortho-vanillin derived Al(iii) and Co(iii) catalyst systems for switchable catalysis using \e-decalactone, phthalic anhydride and cyclohexene oxide ; _journal_issue 5 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 1737 _journal_page_last 1745 _journal_paper_doi 10.1039/D0CY02164D _journal_volume 11 _journal_year 2021 _chemical_formula_moiety 'C23 H27 Co N2 O6' _chemical_formula_sum 'C23 H27 Co N2 O6' _chemical_formula_weight 486.39 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-10-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-11-02 deposited with the CCDC. 2020-12-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.7450(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.99960(10) _cell_length_b 12.8364(2) _cell_length_c 19.0472(3) _cell_measurement_reflns_used 5906 _cell_measurement_temperature 150.00(16) _cell_measurement_theta_max 76.0760 _cell_measurement_theta_min 4.1230 _cell_volume 2185.15(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _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_environment N~2~ _diffrn_ambient_temperature 150.00(16) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4102 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.992 _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 -88.00 41.00 1.00 1.00 -- -42.66 0.00 -60.00 129 2 \w -15.00 23.00 1.00 1.00 -- -42.66 38.00 150.00 38 3 \w 82.00 129.00 1.00 1.00 -- 42.66 178.00-150.00 47 4 \w 43.00 69.00 1.00 5.00 -- 111.00 -30.00 -60.00 26 5 \w 143.00 169.00 1.00 5.00 -- 111.00 125.00-120.00 26 6 \w 31.00 70.00 1.00 5.00 -- 111.00 -95.00 90.00 39 7 \w 94.00 136.00 1.00 5.00 -- 111.00 125.00-120.00 42 8 \w 143.00 173.00 1.00 5.00 -- 111.00 125.00-180.00 30 9 \w 62.00 90.00 1.00 5.00 -- 111.00 -45.00 120.00 28 10 \w 87.00 152.00 1.00 5.00 -- 111.00 45.00-180.00 65 11 \w 45.00 95.00 1.00 5.00 -- 111.00 -45.00 60.00 50 12 \w 44.00 91.00 1.00 5.00 -- 111.00 -45.00 -60.00 47 13 \w 94.00 130.00 1.00 5.00 -- 111.00 125.00-180.00 36 14 \w 75.00 100.00 1.00 5.00 -- 111.00 -95.00 90.00 25 15 \w 76.00 105.00 1.00 5.00 -- 111.00 -95.00 -90.00 29 16 \w 61.00 86.00 1.00 5.00 -- 111.00 -61.00 120.00 25 17 \w 89.00 129.00 1.00 5.00 -- 111.00 -61.00 120.00 40 18 \w 65.00 116.00 1.00 5.00 -- 111.00-125.00 -60.00 51 19 \w 81.00 112.00 1.00 5.00 -- 111.00 77.00 30.00 31 20 \w 140.00 178.00 1.00 5.00 -- 111.00 77.00 30.00 38 21 \w 40.00 89.00 1.00 5.00 -- 111.00 -30.00 150.00 49 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0206755000 _diffrn_orient_matrix_UB_12 -0.0076989000 _diffrn_orient_matrix_UB_13 -0.0790104000 _diffrn_orient_matrix_UB_21 -0.0856226000 _diffrn_orient_matrix_UB_22 -0.1041334000 _diffrn_orient_matrix_UB_23 -0.0051134000 _diffrn_orient_matrix_UB_31 -0.1481238000 _diffrn_orient_matrix_UB_32 0.0591115000 _diffrn_orient_matrix_UB_33 -0.0192828000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 12050 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.271 _diffrn_reflns_theta_min 4.162 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.527 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.50275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark brown' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.478 _exptl_crystal_description block _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.386 _exptl_crystal_size_mid 0.223 _exptl_crystal_size_min 0.191 _refine_diff_density_max 0.336 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 4529 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0337 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.5446P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.0830 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4158 _reflns_number_total 4529 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cy02164d2.cif _cod_data_source_block 027ap19 _cod_depositor_comments 'Adding full bibliography for 1560075--1560077.cif.' _cod_database_code 1560076 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C25 H35 N2 O6 Co1' _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. ; _shelx_estimated_absorpt_t_max 0.369 _shelx_estimated_absorpt_t_min 0.187 _reflns_odcompleteness_completeness 99.89 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C00E(H00A,H00C), C00H(H00D,H00E) 2.b Aromatic/amide H refined with riding coordinates: C00B(H00B), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00N(H00N), C00O(H00O), C00R(H00R) 2.c Idealised Me refined as rotating group: C00S(H00F,H00G,H00H), C00T(H00M,H00P,H00Q), C00U(H00S,H00T,H00U), C00V(H00V, H00W,H00X), C00W(H00Y,H,HA) ; _shelx_res_file ; TITL 027ap19_a.res in P2(1)/c 027ap19.res created by SHELXL-2018/3 at 17:56:36 on 23-Oct-2020 REM Old TITL 027AP19 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.094, Rweak 0.057, Alpha 0.050 REM 0.538 for 216 systematic absences, Orientation as input REM Formula found by SHELXT: C23 N2 O6 Co CELL 1.54184 8.9996 12.8364 19.0472 90 96.745 90 ZERR 4 0.0001 0.0002 0.0003 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Co N O UNIT 92 108 4 8 24 L.S. 30 PLAN 10 SIZE 0.191 0.223 0.386 BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.044300 0.544600 FVAR 0.53567 CO01 3 0.565470 0.493357 0.660301 11.00000 0.01055 0.01199 = 0.00613 0.00020 0.00224 0.00083 O002 5 0.433543 0.426732 0.723769 11.00000 0.01477 0.01866 = 0.00999 0.00177 0.00273 -0.00070 O003 5 0.602406 0.356188 0.630665 11.00000 0.01552 0.01501 = 0.01376 -0.00043 0.00548 -0.00017 O004 5 0.357780 0.481109 0.617999 11.00000 0.01438 0.02200 = 0.00919 0.00061 0.00093 -0.00008 O005 5 0.751882 0.487977 0.716364 11.00000 0.01249 0.02274 = 0.00991 -0.00030 0.00184 0.00240 O006 5 0.699370 0.164762 0.645382 11.00000 0.02500 0.01322 = 0.02260 0.00234 0.01099 0.00204 O007 5 0.958447 0.383361 0.809840 11.00000 0.01255 0.02780 = 0.02242 0.00190 0.00053 0.00170 N008 4 0.525971 0.626137 0.700143 11.00000 0.01275 0.01583 = 0.01070 0.00026 0.00403 0.00109 N009 4 0.641548 0.554131 0.580121 11.00000 0.01291 0.01290 = 0.00821 -0.00043 0.00047 -0.00101 C00A 1 0.719214 0.333045 0.599593 11.00000 0.01234 0.01615 = 0.00904 -0.00149 -0.00019 -0.00115 C00B 1 0.567188 0.647725 0.765446 11.00000 0.01707 0.01628 = 0.01264 -0.00166 0.00631 -0.00137 AFIX 43 H00B 2 0.533479 0.709666 0.783356 11.00000 -1.20000 AFIX 0 C00C 1 0.791514 0.402782 0.557214 11.00000 0.01318 0.01541 = 0.01067 -0.00135 0.00118 -0.00098 C00D 1 0.327449 0.435139 0.673835 11.00000 0.01565 0.01982 = 0.01240 -0.00186 0.00384 -0.00128 C00E 1 0.456737 0.708626 0.654640 11.00000 0.01455 0.01675 = 0.01472 0.00061 0.00373 0.00416 AFIX 23 H00A 2 0.438004 0.768769 0.683153 11.00000 -1.20000 H00C 2 0.361530 0.684492 0.631102 11.00000 -1.20000 AFIX 0 C00F 1 0.753879 0.506003 0.784292 11.00000 0.01320 0.01928 = 0.01037 0.00018 0.00231 -0.00442 C00G 1 0.662530 0.581711 0.812609 11.00000 0.01656 0.01975 = 0.01054 -0.00104 0.00178 -0.00437 C00H 1 0.571545 0.649368 0.548118 11.00000 0.01869 0.01556 = 0.00956 0.00104 0.00136 0.00177 AFIX 23 H00D 2 0.471911 0.632005 0.526127 11.00000 -1.20000 H00E 2 0.629001 0.672484 0.511008 11.00000 -1.20000 AFIX 0 C00I 1 0.773564 0.546436 0.932048 11.00000 0.02399 0.03036 = 0.00886 -0.00070 0.00097 -0.00940 AFIX 43 H00I 2 0.779728 0.558628 0.980433 11.00000 -1.20000 AFIX 0 C00J 1 0.735301 0.506972 0.545252 11.00000 0.01328 0.01659 = 0.00928 -0.00065 0.00157 -0.00360 AFIX 43 H00J 2 0.770368 0.543941 0.508565 11.00000 -1.20000 AFIX 0 C00K 1 0.907008 0.368354 0.518480 11.00000 0.01818 0.02035 = 0.01709 -0.00192 0.00752 -0.00401 AFIX 43 H00K 2 0.948101 0.414101 0.488177 11.00000 -1.20000 AFIX 0 C00L 1 0.893310 0.198172 0.569534 11.00000 0.01917 0.01593 = 0.02311 -0.00227 0.00579 0.00285 AFIX 43 H00L 2 0.930487 0.130728 0.575308 11.00000 -1.20000 AFIX 0 C00M 1 0.559098 0.739923 0.599212 11.00000 0.01553 0.01360 = 0.01192 0.00091 0.00123 0.00231 C00N 1 0.958697 0.268182 0.525292 11.00000 0.01805 0.02213 = 0.02509 -0.00385 0.01143 0.00162 AFIX 43 H00N 2 1.036683 0.246466 0.500797 11.00000 -1.20000 AFIX 0 C00O 1 0.675250 0.601888 0.885742 11.00000 0.02192 0.02186 = 0.01291 -0.00293 0.00520 -0.00614 AFIX 43 H00O 2 0.616353 0.653385 0.902865 11.00000 -1.20000 AFIX 0 C00P 1 0.774604 0.228647 0.604411 11.00000 0.01699 0.01568 = 0.01311 -0.00052 0.00255 -0.00070 C00Q 1 0.857398 0.451847 0.833485 11.00000 0.01283 0.02292 = 0.01447 0.00259 0.00097 -0.00337 C00R 1 0.864641 0.471019 0.905143 11.00000 0.01813 0.02868 = 0.01266 0.00519 -0.00208 -0.00598 AFIX 43 H00R 2 0.931344 0.433122 0.936270 11.00000 -1.20000 AFIX 0 C00S 1 0.482355 0.830820 0.557372 11.00000 0.02639 0.01758 = 0.01871 0.00368 0.00224 0.00603 AFIX 137 H00F 2 0.384036 0.809963 0.537272 11.00000 -1.50000 H00G 2 0.540180 0.850458 0.520221 11.00000 -1.50000 H00H 2 0.474730 0.889032 0.588388 11.00000 -1.50000 AFIX 0 C00T 1 0.713882 0.772154 0.634158 11.00000 0.01692 0.01830 = 0.01845 -0.00147 0.00159 -0.00174 AFIX 137 H00M 2 0.703578 0.826436 0.667919 11.00000 -1.50000 H00P 2 0.772658 0.797099 0.598728 11.00000 -1.50000 H00Q 2 0.762612 0.713170 0.657774 11.00000 -1.50000 AFIX 0 C00U 1 0.893928 0.287751 0.782406 11.00000 0.02108 0.02612 = 0.03173 0.00073 0.00702 0.00130 AFIX 137 H00S 2 0.804098 0.302282 0.751580 11.00000 -1.50000 H00T 2 0.870516 0.244575 0.820767 11.00000 -1.50000 H00U 2 0.963860 0.252213 0.756454 11.00000 -1.50000 AFIX 0 C00V 1 0.174958 0.392821 0.679570 11.00000 0.01888 0.04989 = 0.01949 0.00151 0.00274 -0.01075 AFIX 137 H00V 2 0.103826 0.426205 0.645290 11.00000 -1.50000 H00W 2 0.148602 0.405898 0.726167 11.00000 -1.50000 H00X 2 0.174318 0.319129 0.670945 11.00000 -1.50000 AFIX 0 C00W 1 0.743982 0.058691 0.649608 11.00000 0.04725 0.01630 = 0.04376 0.00827 0.02844 0.00758 AFIX 137 H00Y 2 0.737992 0.029800 0.602872 11.00000 -1.50000 H 2 0.679050 0.020591 0.676871 11.00000 -1.50000 HA 2 0.845082 0.053927 0.671940 11.00000 -1.50000 AFIX 0 HKLF 4 REM 027ap19_a.res in P2(1)/c REM wR2 = 0.0830, GooF = S = 1.072, Restrained GooF = 1.072 for all data REM R1 = 0.0337 for 4158 Fo > 4sig(Fo) and 0.0375 for all 4529 data REM 294 parameters refined using 0 restraints END WGHT 0.0443 0.5446 REM Highest difference peak 0.336, deepest hole -0.570, 1-sigma level 0.077 Q1 1 0.1328 0.4531 0.6829 11.00000 0.05 0.34 Q2 1 0.0845 0.5193 0.6636 11.00000 0.05 0.30 Q3 1 0.8445 0.3849 0.5381 11.00000 0.05 0.25 Q4 1 0.1187 0.3730 0.6322 11.00000 0.05 0.25 Q5 1 0.5098 0.7224 0.6269 11.00000 0.05 0.25 Q6 1 0.2459 0.4202 0.6826 11.00000 0.05 0.24 Q7 1 0.6187 0.6174 0.7855 11.00000 0.05 0.23 Q8 1 0.7624 0.5177 0.4794 11.00000 0.05 0.23 Q9 1 0.7568 0.3719 0.5776 11.00000 0.05 0.23 Q10 1 0.1761 0.4196 0.5844 11.00000 0.05 0.22 ; _shelx_res_checksum 12456 _olex2_submission_original_sample_id 027AP19 _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 1.484 _oxdiff_exptl_absorpt_empirical_full_min 0.767 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Co01 Co 0.56547(2) 0.49336(2) 0.66030(2) 0.00946(8) Uani 1 1 d . . . . . O002 O 0.43354(12) 0.42673(9) 0.72377(6) 0.0144(2) Uani 1 1 d . . . . . O003 O 0.60241(12) 0.35619(9) 0.63067(6) 0.0145(2) Uani 1 1 d . . . . . O004 O 0.35778(13) 0.48111(10) 0.61800(6) 0.0152(2) Uani 1 1 d . . . . . O005 O 0.75188(13) 0.48798(9) 0.71636(6) 0.0150(2) Uani 1 1 d . . . . . O006 O 0.69937(14) 0.16476(10) 0.64538(7) 0.0196(2) Uani 1 1 d . . . . . O007 O 0.95845(13) 0.38336(11) 0.80984(7) 0.0210(3) Uani 1 1 d . . . . . N008 N 0.52597(14) 0.62614(11) 0.70014(7) 0.0129(3) Uani 1 1 d . . . . . N009 N 0.64155(14) 0.55413(10) 0.58012(6) 0.0114(2) Uani 1 1 d . . . . . C00A C 0.71921(16) 0.33304(13) 0.59959(8) 0.0126(3) Uani 1 1 d . . . . . C00B C 0.56719(18) 0.64773(13) 0.76545(8) 0.0150(3) Uani 1 1 d . . . . . H00B H 0.533479 0.709666 0.783356 0.018 Uiso 1 1 calc R . . . . C00C C 0.79151(17) 0.40278(13) 0.55721(8) 0.0131(3) Uani 1 1 d . . . . . C00D C 0.32745(17) 0.43514(13) 0.67383(8) 0.0158(3) Uani 1 1 d . . . . . C00E C 0.45674(17) 0.70863(13) 0.65464(8) 0.0152(3) Uani 1 1 d . . . . . H00A H 0.438004 0.768769 0.683153 0.018 Uiso 1 1 calc R . . . . H00C H 0.361530 0.684492 0.631102 0.018 Uiso 1 1 calc R . . . . C00F C 0.75388(18) 0.50600(13) 0.78429(9) 0.0142(3) Uani 1 1 d . . . . . C00G C 0.66253(18) 0.58171(13) 0.81261(8) 0.0156(3) Uani 1 1 d . . . . . C00H C 0.57154(18) 0.64937(13) 0.54812(8) 0.0146(3) Uani 1 1 d . . . . . H00D H 0.471911 0.632005 0.526127 0.018 Uiso 1 1 calc R . . . . H00E H 0.629001 0.672484 0.511008 0.018 Uiso 1 1 calc R . . . . C00I C 0.77356(19) 0.54644(15) 0.93205(9) 0.0211(3) Uani 1 1 d . . . . . H00I H 0.779728 0.558628 0.980433 0.025 Uiso 1 1 calc R . . . . C00J C 0.73530(18) 0.50697(12) 0.54525(8) 0.0130(3) Uani 1 1 d . . . . . H00J H 0.770368 0.543941 0.508565 0.016 Uiso 1 1 calc R . . . . C00K C 0.90701(18) 0.36835(14) 0.51848(9) 0.0181(3) Uani 1 1 d . . . . . H00K H 0.948101 0.414101 0.488177 0.022 Uiso 1 1 calc R . . . . C00L C 0.89331(19) 0.19817(13) 0.56953(9) 0.0191(3) Uani 1 1 d . . . . . H00L H 0.930487 0.130728 0.575308 0.023 Uiso 1 1 calc R . . . . C00M C 0.55910(17) 0.73992(13) 0.59921(8) 0.0137(3) Uani 1 1 d . . . . . C00N C 0.95870(19) 0.26818(14) 0.52529(10) 0.0211(3) Uani 1 1 d . . . . . H00N H 1.036683 0.246466 0.500797 0.025 Uiso 1 1 calc R . . . . C00O C 0.67525(19) 0.60189(14) 0.88574(9) 0.0186(3) Uani 1 1 d . . . . . H00O H 0.616353 0.653385 0.902865 0.022 Uiso 1 1 calc R . . . . C00P C 0.77460(18) 0.22865(13) 0.60441(8) 0.0152(3) Uani 1 1 d . . . . . C00Q C 0.85740(17) 0.45185(14) 0.83348(9) 0.0168(3) Uani 1 1 d . . . . . C00R C 0.86464(19) 0.47102(15) 0.90514(9) 0.0201(3) Uani 1 1 d . . . . . H00R H 0.931344 0.433122 0.936270 0.024 Uiso 1 1 calc R . . . . C00S C 0.4824(2) 0.83082(14) 0.55737(9) 0.0209(3) Uani 1 1 d . . . . . H00F H 0.384036 0.809963 0.537272 0.031 Uiso 1 1 calc GR . . . . H00G H 0.540180 0.850458 0.520221 0.031 Uiso 1 1 calc GR . . . . H00H H 0.474730 0.889032 0.588388 0.031 Uiso 1 1 calc GR . . . . C00T C 0.71388(18) 0.77215(14) 0.63416(9) 0.0179(3) Uani 1 1 d . . . . . H00M H 0.703578 0.826436 0.667919 0.027 Uiso 1 1 calc GR . . . . H00P H 0.772658 0.797099 0.598728 0.027 Uiso 1 1 calc GR . . . . H00Q H 0.762612 0.713170 0.657774 0.027 Uiso 1 1 calc GR . . . . C00U C 0.8939(2) 0.28775(16) 0.78241(11) 0.0260(4) Uani 1 1 d . . . . . H00S H 0.804098 0.302282 0.751580 0.039 Uiso 1 1 calc GR . . . . H00T H 0.870516 0.244575 0.820767 0.039 Uiso 1 1 calc GR . . . . H00U H 0.963860 0.252213 0.756454 0.039 Uiso 1 1 calc GR . . . . C00V C 0.1750(2) 0.39282(19) 0.67957(10) 0.0294(4) Uani 1 1 d . . . . . H00V H 0.103826 0.426205 0.645290 0.044 Uiso 1 1 calc GR . . . . H00W H 0.148602 0.405898 0.726167 0.044 Uiso 1 1 calc GR . . . . H00X H 0.174318 0.319129 0.670945 0.044 Uiso 1 1 calc GR . . . . C00W C 0.7440(3) 0.05869(15) 0.64961(13) 0.0339(5) Uani 1 1 d . . . . . H00Y H 0.737992 0.029800 0.602872 0.051 Uiso 1 1 calc GR . . . . H H 0.679050 0.020591 0.676871 0.051 Uiso 1 1 calc GR . . . . HA H 0.845082 0.053927 0.671940 0.051 Uiso 1 1 calc GR . . . . 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 Co01 0.01055(13) 0.01199(13) 0.00613(12) 0.00020(8) 0.00224(9) 0.00083(8) O002 0.0148(5) 0.0187(6) 0.0100(5) 0.0018(4) 0.0027(4) -0.0007(4) O003 0.0155(5) 0.0150(5) 0.0138(5) -0.0004(4) 0.0055(4) -0.0002(4) O004 0.0144(5) 0.0220(6) 0.0092(5) 0.0006(4) 0.0009(4) -0.0001(4) O005 0.0125(5) 0.0227(6) 0.0099(5) -0.0003(4) 0.0018(4) 0.0024(4) O006 0.0250(6) 0.0132(6) 0.0226(6) 0.0023(5) 0.0110(5) 0.0020(5) O007 0.0126(5) 0.0278(7) 0.0224(6) 0.0019(5) 0.0005(4) 0.0017(5) N008 0.0128(6) 0.0158(6) 0.0107(6) 0.0003(5) 0.0040(4) 0.0011(5) N009 0.0129(6) 0.0129(6) 0.0082(5) -0.0004(5) 0.0005(4) -0.0010(5) C00A 0.0123(7) 0.0161(7) 0.0090(6) -0.0015(6) -0.0002(5) -0.0011(6) C00B 0.0171(7) 0.0163(7) 0.0126(7) -0.0017(6) 0.0063(5) -0.0014(6) C00C 0.0132(6) 0.0154(7) 0.0107(6) -0.0014(6) 0.0012(5) -0.0010(6) C00D 0.0157(7) 0.0198(8) 0.0124(7) -0.0019(6) 0.0038(5) -0.0013(6) C00E 0.0145(7) 0.0167(7) 0.0147(7) 0.0006(6) 0.0037(5) 0.0042(6) C00F 0.0132(7) 0.0193(8) 0.0104(7) 0.0002(6) 0.0023(6) -0.0044(5) C00G 0.0166(7) 0.0197(8) 0.0105(7) -0.0010(6) 0.0018(5) -0.0044(6) C00H 0.0187(7) 0.0156(7) 0.0096(6) 0.0010(6) 0.0014(5) 0.0018(6) C00I 0.0240(8) 0.0304(9) 0.0089(7) -0.0007(7) 0.0010(6) -0.0094(7) C00J 0.0133(7) 0.0166(8) 0.0093(7) -0.0007(5) 0.0016(5) -0.0036(5) C00K 0.0182(7) 0.0204(8) 0.0171(7) -0.0019(6) 0.0075(6) -0.0040(6) C00L 0.0192(8) 0.0159(8) 0.0231(8) -0.0023(6) 0.0058(6) 0.0028(6) C00M 0.0155(7) 0.0136(7) 0.0119(7) 0.0009(6) 0.0012(5) 0.0023(6) C00N 0.0180(8) 0.0221(9) 0.0251(8) -0.0039(7) 0.0114(6) 0.0016(6) C00O 0.0219(8) 0.0219(8) 0.0129(7) -0.0029(6) 0.0052(6) -0.0061(6) C00P 0.0170(7) 0.0157(8) 0.0131(7) -0.0005(6) 0.0025(5) -0.0007(6) C00Q 0.0128(7) 0.0229(8) 0.0145(7) 0.0026(6) 0.0010(5) -0.0034(6) C00R 0.0181(8) 0.0287(9) 0.0127(7) 0.0052(7) -0.0021(6) -0.0060(7) C00S 0.0264(8) 0.0176(8) 0.0187(8) 0.0037(6) 0.0022(6) 0.0060(7) C00T 0.0169(7) 0.0183(8) 0.0185(7) -0.0015(6) 0.0016(6) -0.0017(6) C00U 0.0211(8) 0.0261(9) 0.0317(10) 0.0007(8) 0.0070(7) 0.0013(7) C00V 0.0189(8) 0.0499(13) 0.0195(8) 0.0015(8) 0.0027(7) -0.0108(8) C00W 0.0472(12) 0.0163(9) 0.0438(12) 0.0083(8) 0.0284(10) 0.0076(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O002 Co01 C00D 33.31(5) . . ? O003 Co01 O002 85.37(5) . . ? O003 Co01 O004 89.72(5) . . ? O003 Co01 N008 173.83(5) . . ? O003 Co01 N009 92.84(5) . . ? O003 Co01 C00D 85.98(5) . . ? O004 Co01 O002 66.71(5) . . ? O004 Co01 C00D 33.43(5) . . ? O005 Co01 O002 101.29(5) . . ? O005 Co01 O003 87.65(5) . . ? O005 Co01 O004 167.90(5) . . ? O005 Co01 N008 90.14(5) . . ? O005 Co01 N009 95.12(5) . . ? O005 Co01 C00D 134.52(6) . . ? N008 Co01 O002 89.43(5) . . ? N008 Co01 O004 91.26(5) . . ? N008 Co01 C00D 91.49(6) . . ? N009 Co01 O002 163.39(5) . . ? N009 Co01 O004 96.80(5) . . ? N009 Co01 N008 93.09(6) . . ? N009 Co01 C00D 130.13(6) . . ? C00D O002 Co01 87.60(9) . . ? C00A O003 Co01 121.92(10) . . ? C00D O004 Co01 88.93(9) . . ? C00F O005 Co01 117.46(10) . . ? C00P O006 C00W 116.92(13) . . ? C00Q O007 C00U 114.31(13) . . ? C00B N008 Co01 121.94(12) . . ? C00B N008 C00E 118.18(14) . . ? C00E N008 Co01 119.73(10) . . ? C00H N009 Co01 119.54(10) . . ? C00J N009 Co01 122.63(11) . . ? C00J N009 C00H 116.85(13) . . ? O003 C00A C00C 124.48(15) . . ? O003 C00A C00P 118.67(14) . . ? C00C C00A C00P 116.74(14) . . ? N008 C00B C00G 123.98(15) . . ? C00A C00C C00J 120.14(14) . . ? C00A C00C C00K 121.04(15) . . ? C00K C00C C00J 118.31(15) . . ? O002 C00D Co01 59.08(8) . . ? O002 C00D O004 116.65(14) . . ? O002 C00D C00V 122.08(15) . . ? O004 C00D Co01 57.64(8) . . ? O004 C00D C00V 121.27(15) . . ? C00V C00D Co01 176.74(14) . . ? N008 C00E C00M 110.45(12) . . ? O005 C00F C00G 123.63(15) . . ? O005 C00F C00Q 119.68(15) . . ? C00G C00F C00Q 116.61(15) . . ? C00F C00G C00B 119.62(14) . . ? C00O C00G C00B 118.77(15) . . ? C00O C00G C00F 121.22(16) . . ? N009 C00H C00M 115.29(12) . . ? C00O C00I C00R 118.88(15) . . ? N009 C00J C00C 126.60(15) . . ? C00N C00K C00C 120.44(15) . . ? C00P C00L C00N 120.62(16) . . ? C00H C00M C00E 109.50(13) . . ? C00H C00M C00S 108.09(13) . . ? C00H C00M C00T 110.60(13) . . ? C00S C00M C00E 106.69(13) . . ? C00T C00M C00E 111.18(13) . . ? C00T C00M C00S 110.65(14) . . ? C00K C00N C00L 119.70(15) . . ? C00I C00O C00G 120.77(17) . . ? O006 C00P C00A 114.04(14) . . ? O006 C00P C00L 124.69(15) . . ? C00L C00P C00A 121.28(15) . . ? O007 C00Q C00F 120.18(15) . . ? O007 C00Q C00R 118.71(15) . . ? C00R C00Q C00F 121.01(16) . . ? C00Q C00R C00I 121.46(16) . . ? 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 Co01 O002 1.9849(11) . ? Co01 O003 1.8904(12) . ? Co01 O004 1.9529(11) . ? Co01 O005 1.8812(12) . ? Co01 N008 1.9159(14) . ? Co01 N009 1.9119(13) . ? Co01 C00D 2.3115(16) . ? O002 C00D 1.271(2) . ? O003 C00A 1.2999(19) . ? O004 C00D 1.274(2) . ? O005 C00F 1.312(2) . ? O006 C00P 1.365(2) . ? O006 C00W 1.419(2) . ? O007 C00Q 1.378(2) . ? O007 C00U 1.430(2) . ? N008 C00B 1.286(2) . ? N008 C00E 1.461(2) . ? N009 C00H 1.474(2) . ? N009 C00J 1.285(2) . ? C00A C00C 1.414(2) . ? C00A C00P 1.429(2) . ? C00B C00G 1.442(2) . ? C00C C00J 1.439(2) . ? C00C C00K 1.414(2) . ? C00D C00V 1.492(2) . ? C00E C00M 1.534(2) . ? C00F C00G 1.420(2) . ? C00F C00Q 1.423(2) . ? C00G C00O 1.408(2) . ? C00H C00M 1.529(2) . ? C00I C00O 1.373(3) . ? C00I C00R 1.404(3) . ? C00K C00N 1.368(3) . ? C00L C00N 1.407(3) . ? C00L C00P 1.379(2) . ? C00M C00S 1.531(2) . ? C00M C00T 1.529(2) . ? C00Q C00R 1.381(2) . ?