#------------------------------------------------------------------------------ #$Date: 2019-11-24 08:09:53 +0200 (Sun, 24 Nov 2019) $ #$Revision: 237245 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/80/4088071.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_4088071 loop_ _publ_author_name 'Belli, Roman G.' 'Burton, Krista M. E.' 'Rufh, Stephanie A.' 'McDonald, Robert' 'Rosenberg, Lisa' _publ_section_title ; Inner- and Outer-Sphere Roles of Ruthenium Phosphido Complexes in the Hydrophosphination of Alkenes ; _journal_issue 23 _journal_name_full Organometallics _journal_page_first 5637 _journal_paper_doi 10.1021/acs.organomet.5b00835 _journal_volume 34 _journal_year 2015 _chemical_formula_moiety 'C52 H42 N P2 Ru, C24 B F20, 2.5(C6 H6)' _chemical_formula_sum 'C91 H57 B F20 N P2 Ru' _chemical_formula_weight 1718.19 _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 geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 104.6950(4) _cell_angle_beta 107.8349(4) _cell_angle_gamma 108.4208(4) _cell_formula_units_Z 2 _cell_length_a 16.0400(6) _cell_length_b 16.8124(6) _cell_length_c 16.8412(6) _cell_measurement_reflns_used 9994 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 26.12 _cell_measurement_theta_min 2.30 _cell_volume 3780.4(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_unetI/netI 0.0380 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 35924 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.437 _diffrn_reflns_theta_min 1.385 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9187 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.509 _exptl_crystal_description fragment _exptl_crystal_F_000 1738 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.216 _exptl_crystal_size_min 0.151 _refine_diff_density_max 0.793 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1000 _refine_ls_number_reflns 18521 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0377 _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^)+(0.0413P)^2^+1.4346P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.0970 _reflns_Friedel_coverage 0.000 _reflns_number_gt 15091 _reflns_number_total 18521 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file om5b00835_si_001.cif _cod_data_source_block 6 _cod_database_code 4088071 _shelx_shelxl_version_number 2014/7 _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_min 0.921 _shelx_estimated_absorpt_t_max 0.949 _shelx_res_file ; vic1527.res created by SHELXL-2014/7 TITL vic1527 in P-1 CELL 0.71073 16.0400 16.8124 16.8412 104.6950 107.8349 108.4208 ZERR 2.00 0.0006 0.0006 0.0006 0.0004 0.0004 0.0004 LATT 1 SFAC C H B N F P RU UNIT 182 114 2 2 40 4 2 SIZE 0.151 0.216 0.24 TEMP -80 L.S. 4 ACTA CONF 2.4 MPLA 5 C1 C2 C3 C3A C7A RU MPLA 3 C1 C2 C3 RU MPLA 4 C1 C3 C3A C7A RU MPLA 6 C3A > C7A RU WGHT 0.041300 1.434600 FVAR 0.11610 RU 7 0.336692 0.073043 0.310836 11.00000 0.02486 0.02159 = 0.02235 0.00868 0.00920 0.00786 P1 6 0.347568 0.217966 0.332012 11.00000 0.02647 0.02210 = 0.02419 0.00918 0.01020 0.00846 P2 6 0.457841 0.080811 0.256894 11.00000 0.02795 0.02320 = 0.02785 0.00903 0.01302 0.00883 N 4 0.229367 0.009281 0.182305 11.00000 0.03090 0.02560 = 0.02887 0.01232 0.01145 0.01079 C1 1 0.250999 0.023981 0.383926 11.00000 0.03606 0.03186 = 0.03253 0.01705 0.01971 0.01565 AFIX 13 H1 2 0.184868 0.020333 0.373665 11.00000 -1.20000 AFIX 0 C2 1 0.339875 0.099402 0.445840 11.00000 0.04685 0.03031 = 0.02483 0.01265 0.01772 0.01477 AFIX 13 H2 2 0.346622 0.157797 0.487165 11.00000 -1.20000 AFIX 0 C3 1 0.417798 0.077569 0.443373 11.00000 0.03242 0.03305 = 0.02504 0.01459 0.00778 0.00748 AFIX 13 H3 2 0.488097 0.117329 0.482996 11.00000 -1.20000 AFIX 0 C3A 1 0.376173 -0.018541 0.386832 11.00000 0.03093 0.03428 = 0.02932 0.02026 0.01306 0.01282 C4 1 0.417383 -0.080545 0.368737 11.00000 0.03298 0.04443 = 0.04418 0.02996 0.01845 0.02030 AFIX 43 H4 2 0.485681 -0.060210 0.392463 11.00000 -1.20000 AFIX 0 C5 1 0.356599 -0.170249 0.316375 11.00000 0.05072 0.04106 = 0.05588 0.03022 0.03178 0.02981 AFIX 43 H5 2 0.383500 -0.212621 0.305767 11.00000 -1.20000 AFIX 0 C6 1 0.254926 -0.201501 0.277688 11.00000 0.04706 0.02560 = 0.04963 0.01604 0.02406 0.01248 AFIX 43 H6 2 0.215099 -0.264172 0.241014 11.00000 -1.20000 AFIX 0 C7 1 0.212654 -0.143608 0.291851 11.00000 0.03294 0.02948 = 0.03814 0.01497 0.01526 0.00883 AFIX 43 H7 2 0.144299 -0.164887 0.263708 11.00000 -1.20000 AFIX 0 C7A 1 0.273148 -0.050877 0.349589 11.00000 0.03132 0.02967 = 0.03079 0.01732 0.01510 0.01238 C10 1 0.169903 -0.037853 0.111356 11.00000 0.03196 0.02858 = 0.03174 0.01300 0.01180 0.01235 C11 1 0.100455 -0.095281 0.019805 11.00000 0.02763 0.03014 = 0.02697 0.00761 0.00589 0.00889 C12 1 0.067403 -0.189008 -0.009449 11.00000 0.04531 0.03537 = 0.03273 0.01454 0.00633 0.01381 AFIX 43 H12 2 0.087081 -0.215784 0.031944 11.00000 -1.20000 AFIX 0 C13 1 0.005919 -0.242917 -0.098840 11.00000 0.05016 0.02933 = 0.03930 0.00828 0.00656 0.01049 AFIX 43 H13 2 -0.016920 -0.307124 -0.119117 11.00000 -1.20000 AFIX 0 C14 1 -0.022752 -0.204308 -0.159176 11.00000 0.04320 0.04067 = 0.02901 0.00722 0.00186 0.01068 AFIX 43 H14 2 -0.065042 -0.241918 -0.220831 11.00000 -1.20000 AFIX 0 C15 1 0.009831 -0.111391 -0.130163 11.00000 0.05318 0.04157 = 0.03649 0.01768 0.00217 0.01445 AFIX 43 H15 2 -0.009887 -0.084987 -0.171921 11.00000 -1.20000 AFIX 0 C16 1 0.071113 -0.056329 -0.040539 11.00000 0.04726 0.03069 = 0.03681 0.01265 0.00515 0.01127 AFIX 43 H16 2 0.093001 0.007783 -0.020392 11.00000 -1.20000 AFIX 0 C21 1 0.270006 0.244222 0.385565 11.00000 0.03249 0.02593 = 0.02659 0.01198 0.01420 0.01347 C22 1 0.175768 0.177721 0.351803 11.00000 0.03173 0.02783 = 0.03126 0.01094 0.01247 0.01248 AFIX 43 H22 2 0.156560 0.120056 0.306955 11.00000 -1.20000 AFIX 0 C23 1 0.109781 0.194108 0.382347 11.00000 0.03461 0.03786 = 0.04639 0.02130 0.01954 0.01624 AFIX 43 H23 2 0.045481 0.148329 0.357733 11.00000 -1.20000 AFIX 0 C24 1 0.137250 0.276915 0.448563 11.00000 0.05342 0.04614 = 0.05802 0.02590 0.03723 0.02910 AFIX 43 H24 2 0.092445 0.287909 0.470686 11.00000 -1.20000 AFIX 0 C25 1 0.230149 0.343769 0.482564 11.00000 0.06009 0.03330 = 0.05563 0.01075 0.03438 0.02220 AFIX 43 H25 2 0.249025 0.400952 0.528009 11.00000 -1.20000 AFIX 0 C26 1 0.296278 0.328222 0.450964 11.00000 0.04216 0.02662 = 0.04110 0.00861 0.01944 0.01201 AFIX 43 H26 2 0.359691 0.375104 0.474075 11.00000 -1.20000 AFIX 0 C31 1 0.309508 0.259084 0.241635 11.00000 0.03331 0.03007 = 0.03044 0.01564 0.01629 0.01585 C32 1 0.243168 0.198897 0.154451 11.00000 0.04529 0.03305 = 0.03345 0.01527 0.01368 0.01856 AFIX 43 H32 2 0.220335 0.135292 0.139955 11.00000 -1.20000 AFIX 0 C33 1 0.209533 0.230190 0.087893 11.00000 0.05606 0.04608 = 0.03212 0.01729 0.01196 0.02537 AFIX 43 H33 2 0.164290 0.188038 0.028379 11.00000 -1.20000 AFIX 0 C34 1 0.241671 0.322088 0.108094 11.00000 0.05624 0.05021 = 0.04310 0.03127 0.02408 0.03086 AFIX 43 H34 2 0.219890 0.343520 0.062288 11.00000 -1.20000 AFIX 0 C35 1 0.305336 0.382748 0.194683 11.00000 0.05835 0.03536 = 0.05284 0.02721 0.02242 0.02263 AFIX 43 H35 2 0.326372 0.446203 0.208949 11.00000 -1.20000 AFIX 0 C36 1 0.339209 0.352037 0.261564 11.00000 0.04829 0.03055 = 0.03839 0.01532 0.01252 0.01438 AFIX 43 H36 2 0.382933 0.394628 0.321342 11.00000 -1.20000 AFIX 0 C41 1 0.470132 0.305599 0.407877 11.00000 0.02872 0.02198 = 0.03318 0.00814 0.01039 0.01001 C42 1 0.507557 0.324306 0.500716 11.00000 0.03780 0.03170 = 0.03615 0.01196 0.01127 0.01140 AFIX 43 H42 2 0.467474 0.294239 0.525234 11.00000 -1.20000 AFIX 0 C43 1 0.602734 0.386418 0.557180 11.00000 0.04553 0.03844 = 0.03731 0.00975 0.00144 0.01317 AFIX 43 H43 2 0.627137 0.399256 0.620212 11.00000 -1.20000 AFIX 0 C44 1 0.662474 0.429890 0.522079 11.00000 0.03170 0.03269 = 0.06133 0.01304 0.00303 0.00725 AFIX 43 H44 2 0.727404 0.472937 0.560921 11.00000 -1.20000 AFIX 0 C45 1 0.626842 0.410107 0.430373 11.00000 0.03384 0.02892 = 0.06017 0.01699 0.01595 0.00816 AFIX 43 H45 2 0.667980 0.438683 0.405912 11.00000 -1.20000 AFIX 0 C46 1 0.531692 0.349001 0.373630 11.00000 0.03356 0.02571 = 0.04125 0.01093 0.01492 0.00976 AFIX 43 H46 2 0.508029 0.336466 0.310663 11.00000 -1.20000 AFIX 0 C51 1 0.571422 0.096444 0.342656 11.00000 0.02823 0.02951 = 0.03617 0.01374 0.01533 0.01064 C52 1 0.622437 0.176048 0.420953 11.00000 0.03357 0.03396 = 0.03910 0.01058 0.01317 0.01058 AFIX 43 H52 2 0.598125 0.220849 0.428228 11.00000 -1.20000 AFIX 0 C53 1 0.708057 0.190623 0.488216 11.00000 0.03545 0.04873 = 0.03707 0.01115 0.00854 0.00747 AFIX 43 H53 2 0.742603 0.245432 0.540762 11.00000 -1.20000 AFIX 0 C54 1 0.742854 0.125012 0.478409 11.00000 0.03464 0.07023 = 0.04553 0.02840 0.01371 0.02194 AFIX 43 H54 2 0.801313 0.134659 0.524517 11.00000 -1.20000 AFIX 0 C55 1 0.693164 0.045657 0.402067 11.00000 0.04378 0.05918 = 0.05587 0.02948 0.02399 0.03110 AFIX 43 H55 2 0.717155 0.000563 0.395949 11.00000 -1.20000 AFIX 0 C56 1 0.608021 0.031406 0.333978 11.00000 0.03761 0.03881 = 0.04342 0.01629 0.01906 0.01769 AFIX 43 H56 2 0.574559 -0.023098 0.281141 11.00000 -1.20000 AFIX 0 C61 1 0.425032 -0.024456 0.163659 11.00000 0.03484 0.02821 = 0.02779 0.00973 0.01336 0.01312 C62 1 0.347359 -0.104153 0.144938 11.00000 0.03490 0.03106 = 0.03280 0.01204 0.01510 0.01338 AFIX 43 H62 2 0.309643 -0.103259 0.178734 11.00000 -1.20000 AFIX 0 C63 1 0.324645 -0.185087 0.077040 11.00000 0.04294 0.02843 = 0.04291 0.00877 0.01642 0.01013 AFIX 43 H63 2 0.271608 -0.239229 0.064773 11.00000 -1.20000 AFIX 0 C64 1 0.378809 -0.187076 0.027431 11.00000 0.05752 0.03411 = 0.04066 0.00241 0.02177 0.01885 AFIX 43 H64 2 0.363051 -0.242447 -0.018978 11.00000 -1.20000 AFIX 0 C65 1 0.456183 -0.108193 0.045431 11.00000 0.06106 0.04403 = 0.04680 0.01413 0.03498 0.02559 AFIX 43 H65 2 0.493756 -0.109534 0.011530 11.00000 -1.20000 AFIX 0 C66 1 0.478934 -0.027326 0.112755 11.00000 0.04725 0.03454 = 0.04172 0.01236 0.02614 0.01411 AFIX 43 H66 2 0.531740 0.026676 0.124358 11.00000 -1.20000 AFIX 0 C71 1 0.500088 0.165472 0.210601 11.00000 0.04212 0.02382 = 0.03671 0.01263 0.02539 0.01280 C72 1 0.430633 0.171952 0.142523 11.00000 0.05120 0.03657 = 0.04254 0.01925 0.02799 0.02212 AFIX 43 H72 2 0.364307 0.131820 0.120543 11.00000 -1.20000 AFIX 0 C73 1 0.456670 0.236310 0.106001 11.00000 0.07864 0.04574 = 0.05256 0.03036 0.04143 0.03660 AFIX 43 H73 2 0.408281 0.240813 0.060235 11.00000 -1.20000 AFIX 0 C74 1 0.553044 0.293604 0.136476 11.00000 0.08814 0.03269 = 0.06508 0.02679 0.05762 0.02949 AFIX 43 H74 2 0.571165 0.338231 0.112314 11.00000 -1.20000 AFIX 0 C75 1 0.622735 0.285964 0.201842 11.00000 0.06273 0.03230 = 0.06429 0.01777 0.04380 0.01008 AFIX 43 H75 2 0.689142 0.324475 0.221554 11.00000 -1.20000 AFIX 0 C76 1 0.597217 0.222486 0.239528 11.00000 0.04515 0.03469 = 0.05216 0.01686 0.02923 0.01168 AFIX 43 H76 2 0.646027 0.218059 0.284950 11.00000 -1.20000 AFIX 0 F82 5 0.090633 0.303941 0.635986 11.00000 0.05702 0.03443 = 0.03523 0.01401 0.02401 0.01570 F83 5 0.010866 0.127133 0.535891 11.00000 0.07060 0.04285 = 0.04555 -0.00254 0.02629 0.01441 F84 5 -0.031279 0.002878 0.611609 11.00000 0.06331 0.02271 = 0.09450 0.00561 0.04223 0.01068 F85 5 0.004789 0.061714 0.790311 11.00000 0.06524 0.03664 = 0.09376 0.04112 0.04419 0.02262 F86 5 0.085048 0.237197 0.891890 11.00000 0.04957 0.04166 = 0.04636 0.02784 0.02071 0.01946 F92 5 0.310593 0.538899 1.005284 11.00000 0.03120 0.04290 = 0.03662 0.00386 0.01002 0.00802 F93 5 0.294894 0.599869 1.158358 11.00000 0.06246 0.05813 = 0.03367 -0.00197 0.01075 0.02107 F94 5 0.124297 0.529808 1.170323 11.00000 0.09617 0.07707 = 0.04925 0.02245 0.05008 0.04827 F95 5 -0.035124 0.395906 1.021141 11.00000 0.05940 0.05549 = 0.07328 0.03926 0.05060 0.03487 F96 5 -0.022773 0.334136 0.865553 11.00000 0.03058 0.03977 = 0.04777 0.01793 0.01741 0.01094 F102 5 -0.064456 0.316860 0.680998 11.00000 0.02915 0.02859 = 0.04647 0.01177 0.00635 0.00624 F103 5 -0.151363 0.414705 0.627900 11.00000 0.03639 0.05635 = 0.05395 0.01695 0.00300 0.02264 F104 5 -0.054908 0.598056 0.686167 11.00000 0.07056 0.05714 = 0.07011 0.03228 0.02459 0.04610 F105 5 0.136094 0.682300 0.805935 11.00000 0.06264 0.02685 = 0.08778 0.02184 0.02908 0.02034 F106 5 0.225130 0.587354 0.866628 11.00000 0.03235 0.02702 = 0.04928 0.00934 0.01221 0.00661 F112 5 0.284989 0.349551 0.935762 11.00000 0.04179 0.05308 = 0.04201 0.02958 0.02135 0.02433 F113 5 0.465169 0.385394 0.954216 11.00000 0.03787 0.06119 = 0.04374 0.02058 0.01036 0.02740 F114 5 0.537477 0.471519 0.855990 11.00000 0.02909 0.05868 = 0.07065 0.02335 0.02469 0.01774 F115 5 0.420546 0.512178 0.733913 11.00000 0.04936 0.05142 = 0.06542 0.03307 0.04030 0.02157 F116 5 0.243215 0.482445 0.717938 11.00000 0.03991 0.04129 = 0.04374 0.02625 0.02177 0.02017 C81 1 0.090498 0.281700 0.769524 11.00000 0.02418 0.02675 = 0.03343 0.01153 0.01133 0.00948 C82 1 0.070203 0.246477 0.677810 11.00000 0.03294 0.02751 = 0.03955 0.01321 0.01747 0.01203 C83 1 0.029415 0.155028 0.624078 11.00000 0.03756 0.03326 = 0.04350 0.00568 0.01785 0.01313 C84 1 0.007977 0.092438 0.662351 11.00000 0.03559 0.02111 = 0.06555 0.00727 0.02428 0.00940 C85 1 0.026861 0.122351 0.751897 11.00000 0.03554 0.03013 = 0.06826 0.02568 0.02729 0.01558 C86 1 0.068146 0.215049 0.803947 11.00000 0.02840 0.03251 = 0.04008 0.01788 0.01515 0.01445 C91 1 0.145512 0.429278 0.926606 11.00000 0.03197 0.03062 = 0.03017 0.01423 0.01386 0.01557 C92 1 0.222859 0.498691 1.004395 11.00000 0.03308 0.03376 = 0.03354 0.01372 0.01447 0.01527 C93 1 0.216717 0.532428 1.085243 11.00000 0.04845 0.03823 = 0.03035 0.00844 0.01210 0.02122 C94 1 0.130487 0.497265 1.091666 11.00000 0.06636 0.04527 = 0.03574 0.01978 0.03047 0.03517 C95 1 0.050996 0.429802 1.016712 11.00000 0.04714 0.03975 = 0.05358 0.02864 0.03415 0.02747 C96 1 0.059966 0.398546 0.937356 11.00000 0.03504 0.02990 = 0.03575 0.01715 0.01635 0.01537 C101 1 0.087585 0.445791 0.775594 11.00000 0.02912 0.02682 = 0.02690 0.01130 0.01436 0.01091 C102 1 -0.009163 0.407770 0.714721 11.00000 0.03051 0.02896 = 0.03180 0.01274 0.01418 0.01157 C103 1 -0.056794 0.456921 0.684820 11.00000 0.03239 0.04310 = 0.03208 0.01462 0.01154 0.01977 C104 1 -0.008883 0.549449 0.714873 11.00000 0.04734 0.04271 = 0.04579 0.02357 0.02262 0.03029 C105 1 0.086895 0.591592 0.775047 11.00000 0.04625 0.02520 = 0.04756 0.01429 0.02424 0.01689 C106 1 0.131328 0.539971 0.804141 11.00000 0.02898 0.02748 = 0.03333 0.01010 0.01485 0.00970 C111 1 0.255007 0.417948 0.829767 11.00000 0.02692 0.02330 = 0.02761 0.00678 0.01053 0.00815 C112 1 0.316582 0.392716 0.885708 11.00000 0.03266 0.03001 = 0.02788 0.00974 0.01286 0.01204 C113 1 0.409855 0.409563 0.895969 11.00000 0.03248 0.03365 = 0.03202 0.00832 0.00942 0.01636 C114 1 0.446404 0.452339 0.846692 11.00000 0.02543 0.03207 = 0.04489 0.00729 0.01460 0.00967 C115 1 0.387811 0.474438 0.786792 11.00000 0.03601 0.03014 = 0.04247 0.01455 0.02236 0.01121 C116 1 0.294823 0.457548 0.779180 11.00000 0.03161 0.02478 = 0.03341 0.01134 0.01365 0.01117 B 3 0.145079 0.393337 0.824775 11.00000 0.02450 0.02401 = 0.02694 0.00966 0.01040 0.00725 C11S 1 0.461439 0.278739 0.709739 11.00000 0.05394 0.06967 = 0.05584 0.01924 0.02848 0.03088 AFIX 43 H11S 2 0.521275 0.312036 0.709232 11.00000 -1.20000 AFIX 0 C12S 1 0.459023 0.231701 0.765396 11.00000 0.05671 0.06644 = 0.06504 0.02359 0.02378 0.03685 AFIX 43 H12S 2 0.517102 0.232161 0.803167 11.00000 -1.20000 AFIX 0 C13S 1 0.372843 0.184138 0.766410 11.00000 0.07790 0.07139 = 0.10338 0.05203 0.04833 0.04558 AFIX 43 H13S 2 0.370852 0.151618 0.804933 11.00000 -1.20000 AFIX 0 C14S 1 0.288649 0.183728 0.710970 11.00000 0.05381 0.07562 = 0.12860 0.05431 0.04042 0.03212 AFIX 43 H14S 2 0.228730 0.150874 0.711590 11.00000 -1.20000 AFIX 0 C15S 1 0.291122 0.230414 0.655155 11.00000 0.05678 0.07123 = 0.06708 0.01628 0.01655 0.03747 AFIX 43 H15S 2 0.233139 0.229818 0.617022 11.00000 -1.20000 AFIX 0 C16S 1 0.377289 0.277692 0.654710 11.00000 0.07640 0.07518 = 0.04638 0.02127 0.03538 0.04719 AFIX 43 H16S 2 0.379243 0.310148 0.616127 11.00000 -1.20000 AFIX 66 PART 1 C21S 1 0.826058 0.048241 0.257884 10.50000 0.06465 AFIX 43 H21S 2 0.861683 0.052611 0.316685 10.50000 -1.20000 AFIX 65 C22S 1 0.804656 0.119795 0.247067 10.50000 0.08717 AFIX 43 H22S 2 0.825654 0.173068 0.298475 10.50000 -1.20000 AFIX 65 C23S 1 0.752530 0.113402 0.161033 10.50000 0.06436 AFIX 43 H23S 2 0.737903 0.162306 0.153641 10.50000 -1.20000 AFIX 65 C24S 1 0.721807 0.035456 0.085816 10.50000 0.05530 AFIX 43 H24S 2 0.686182 0.031087 0.027016 10.50000 -1.20000 AFIX 65 C25S 1 0.743209 -0.036098 0.096632 10.50000 0.05723 AFIX 43 H25S 2 0.722211 -0.089371 0.045224 10.50000 -1.20000 AFIX 65 C26S 1 0.795334 -0.029707 0.182665 10.50000 0.05300 AFIX 43 H26S 2 0.809962 -0.078611 0.190057 10.50000 -1.20000 AFIX 66 PART 2 C31S 1 0.838533 0.100855 0.287327 10.50000 0.06553 AFIX 43 H31S 2 0.876331 0.128230 0.350930 10.50000 -1.20000 AFIX 65 C32S 1 0.800543 0.149067 0.242769 10.50000 0.07187 AFIX 43 H32S 2 0.812376 0.209393 0.275919 10.50000 -1.20000 AFIX 65 C33S 1 0.745238 0.109013 0.149708 10.50000 0.08386 AFIX 43 H33S 2 0.719274 0.141964 0.119255 10.50000 -1.20000 AFIX 65 C34S 1 0.727923 0.020748 0.101204 10.50000 0.10230 AFIX 43 H34S 2 0.690125 -0.006627 0.037601 10.50000 -1.20000 AFIX 65 C35S 1 0.765913 -0.027465 0.145761 10.50000 0.10383 AFIX 43 H35S 2 0.754079 -0.087790 0.112611 10.50000 -1.20000 AFIX 65 C36S 1 0.821218 0.012588 0.238822 10.50000 0.06897 AFIX 43 H36S 2 0.847182 -0.020364 0.269275 10.50000 -1.20000 AFIX 66 PART -1 C41S 1 -0.082117 0.456179 0.454850 10.50000 0.06131 AFIX 43 H41S 2 -0.148345 0.414150 0.421247 10.50000 -1.20000 AFIX 65 C42S 1 -0.053132 0.545911 0.462351 10.50000 0.04729 AFIX 43 H42S 2 -0.099549 0.565211 0.433875 10.50000 -1.20000 AFIX 65 C43S 1 0.043769 0.607406 0.511517 10.50000 0.07081 AFIX 43 H43S 2 0.063578 0.668734 0.516644 10.50000 -1.20000 AFIX 65 C44S 1 0.111685 0.579169 0.553182 10.50000 0.07903 AFIX 43 H44S 2 0.177912 0.621198 0.586785 10.50000 -1.20000 AFIX 65 C45S 1 0.082701 0.489437 0.545682 10.50000 0.06427 AFIX 43 H45S 2 0.129119 0.470139 0.574158 10.50000 -1.20000 AFIX 65 C46S 1 -0.014199 0.427942 0.496516 10.50000 0.06999 AFIX 43 H46S 2 -0.034009 0.366614 0.491390 10.50000 -1.20000 PART 0 AFIX 0 HKLF 4 REM vic1527 in P-1 REM R1 = 0.0377 for 15091 Fo > 4sig(Fo) and 0.0486 for all 18521 data REM 1000 parameters refined using 0 restraints END WGHT 0.0413 1.4346 REM 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