#------------------------------------------------------------------------------ #$Date: 2019-10-07 12:55:59 +0300 (Mon, 07 Oct 2019) $ #$Revision: 219132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234429.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_7234429 loop_ _publ_author_name 'Xuan Zhang' 'Haomiao Xie' 'Maria Ballesteros-Rivas' 'Zhao-Xi Wang' 'Kim R. Dunbar' _publ_section_title ; Structural distortions of the spin-crossover material [Co(pyterpy)2](TCNQ)2 mediated by supramolecular interactions ; _journal_name_full 'Journal of Materials Chemistry C' _journal_page_first 9292 _journal_page_last 9298 _journal_paper_doi 10.1039/C5TC01851J _journal_volume 3 _journal_year 2015 _chemical_formula_moiety 'C40 H28 Co N8, 2(C12 H4 N4), C3 H7 N O, C H4 O' _chemical_formula_sum 'C68 H47 Co N17 O2' _chemical_formula_weight 1193.15 _chemical_name_common Co(pyterpy)2(TCNQ)2_DMF_MeOH _chemical_name_systematic ; Cobalt(II) bis-(4?-(4???-pyridyl)- 2,2?:6?,2??-terpyridine) tetracyanoquinodimethane N,N-dimethyl formamide methanol ; _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 _atom_sites_solution_primary direct _cell_angle_alpha 74.249(7) _cell_angle_beta 81.736(8) _cell_angle_gamma 85.755(7) _cell_formula_units_Z 2 _cell_length_a 8.911(5) _cell_length_b 13.921(8) _cell_length_c 24.708(15) _cell_measurement_reflns_used 8222 _cell_measurement_temperature 110.15 _cell_measurement_theta_max 26.23 _cell_measurement_theta_min 2.31 _cell_volume 2917(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 110.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_unetI/netI 0.0935 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 30512 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 1.521 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0804 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.8618. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.358 _exptl_crystal_description needle _exptl_crystal_F_000 1234 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.988 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.080 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 797 _refine_ls_number_reflns 11425 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0508 _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^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1228 _refine_ls_wR_factor_ref 0.1379 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8274 _reflns_number_total 11425 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-9292.cif _cod_data_source_block 5-110K _cod_database_code 7234429 _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 0.972 _shelx_estimated_absorpt_t_min 0.916 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40), C57(H57), C58(H58), C60(H60), C61(H61), C45(H45), C46(H46), C48(H48), C49(H49), C65(H65) 2.b Idealised Me refined as rotating group: C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C) 2.c Idealised tetrahedral OH refined as rotating group: O2(H2A) ; _shelx_res_file ; TITL P-1_a.res in P-1 REM Old TITL P-1 in P-1 REM SHELXT solution in P-1 REM R1 0.167, Rweak 0.006, Alpha 0.053, Orientation as input REM Formula found by SHELXT: C72 Co N14 O CELL 0.71073 8.9107 13.9213 24.7078 74.249 81.736 85.755 ZERR 2 0.0053 0.0082 0.0146 0.007 0.008 0.007 LATT 1 SFAC C H Co N O UNIT 136 94 2 34 4 L.S. 10 PLAN 1 SIZE 0.08 0.13 0.25 TEMP -163 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.063600 FVAR 0.32503 CO1 3 0.124367 0.683110 0.236198 11.00000 0.01853 0.01192 = 0.01025 0.00095 -0.00334 -0.00157 N1 4 0.112358 0.610703 0.316676 11.00000 0.01700 0.01565 = 0.01577 -0.00180 -0.00161 -0.00155 N2 4 0.337072 0.726088 0.260997 11.00000 0.02326 0.01768 = 0.01833 -0.00037 -0.00370 -0.00433 N3 4 -0.096930 0.610971 0.252452 11.00000 0.02632 0.01896 = 0.02124 -0.00261 -0.01034 0.00018 N4 4 0.158730 0.750783 0.158412 11.00000 0.01811 0.01502 = 0.01476 -0.00238 -0.00252 -0.00058 N5 4 0.236956 0.572109 0.206692 11.00000 0.01953 0.01727 = 0.01844 0.00151 -0.00591 -0.00261 N6 4 0.027610 0.817336 0.238888 11.00000 0.02045 0.02129 = 0.01589 -0.00258 -0.00239 -0.00585 N7 4 0.159945 0.276053 0.588060 11.00000 0.03629 0.03129 = 0.01716 0.00424 -0.00120 -0.00295 N8 4 0.446848 1.027915 -0.116380 11.00000 0.04418 0.02119 = 0.02128 -0.00177 0.00451 -0.00627 C1 1 0.226007 0.615796 0.346901 11.00000 0.01879 0.01747 = 0.01721 -0.00626 -0.00323 -0.00056 C2 1 0.235482 0.552370 0.400254 11.00000 0.02484 0.02481 = 0.01750 -0.00235 -0.00822 -0.00448 AFIX 43 H2 2 0.315566 0.558136 0.420619 11.00000 -1.20000 AFIX 0 C3 1 0.127898 0.480130 0.424146 11.00000 0.02208 0.01645 = 0.01545 -0.00281 -0.00221 0.00072 C4 1 0.010230 0.476858 0.392880 11.00000 0.02287 0.01721 = 0.01950 -0.00234 -0.00425 -0.00436 AFIX 43 H4 2 -0.065882 0.428994 0.408009 11.00000 -1.20000 AFIX 0 C5 1 0.004089 0.542883 0.340094 11.00000 0.01684 0.01979 = 0.01851 -0.00608 -0.00095 -0.00164 C6 1 -0.117881 0.546025 0.304038 11.00000 0.02339 0.02021 = 0.01974 -0.00436 -0.00584 -0.00181 C7 1 -0.245890 0.488625 0.322846 11.00000 0.03100 0.03798 = 0.02818 0.00038 -0.01024 -0.01312 AFIX 43 H7 2 -0.258375 0.443300 0.359518 11.00000 -1.20000 AFIX 0 C8 1 -0.355086 0.499517 0.286402 11.00000 0.02943 0.04711 = 0.03912 -0.00601 -0.01198 -0.01415 AFIX 43 H8 2 -0.443093 0.460729 0.297797 11.00000 -1.20000 AFIX 0 C9 1 -0.335006 0.567052 0.233505 11.00000 0.03324 0.03638 = 0.03467 -0.00829 -0.02027 -0.00190 AFIX 43 H9 2 -0.409180 0.576303 0.208328 11.00000 -1.20000 AFIX 0 C10 1 -0.204523 0.620501 0.218353 11.00000 0.03476 0.02404 = 0.02285 -0.00447 -0.01413 0.00007 AFIX 43 H10 2 -0.189999 0.666434 0.181912 11.00000 -1.20000 AFIX 0 C11 1 0.442262 0.790231 0.231038 11.00000 0.02914 0.02136 = 0.01875 0.00020 0.00073 -0.00682 AFIX 43 H11 2 0.440081 0.815837 0.191378 11.00000 -1.20000 AFIX 0 C12 1 0.554484 0.820886 0.255566 11.00000 0.02701 0.02544 = 0.02694 -0.00110 0.00113 -0.01166 AFIX 43 H12 2 0.628732 0.865435 0.232842 11.00000 -1.20000 AFIX 0 C13 1 0.556990 0.785967 0.313263 11.00000 0.02868 0.03268 = 0.03103 -0.00491 -0.01012 -0.01160 AFIX 43 H13 2 0.632098 0.806430 0.331035 11.00000 -1.20000 AFIX 0 C14 1 0.447282 0.720232 0.344802 11.00000 0.02920 0.02959 = 0.01619 0.00026 -0.00709 -0.00791 AFIX 43 H14 2 0.444509 0.696151 0.384766 11.00000 -1.20000 AFIX 0 C15 1 0.342063 0.690284 0.317226 11.00000 0.01976 0.01972 = 0.01935 -0.00255 -0.00359 -0.00239 C16 1 0.138832 0.408766 0.480451 11.00000 0.02182 0.02006 = 0.01690 -0.00119 -0.00360 0.00055 C17 1 0.235267 0.424925 0.516677 11.00000 0.02968 0.02272 = 0.02094 -0.00224 -0.00672 -0.00390 AFIX 43 H17 2 0.296479 0.481796 0.505484 11.00000 -1.20000 AFIX 0 C18 1 0.240717 0.357542 0.568814 11.00000 0.03146 0.03234 = 0.01953 -0.00428 -0.00734 0.00106 AFIX 43 H18 2 0.307055 0.370321 0.592707 11.00000 -1.20000 AFIX 0 C19 1 0.067419 0.261239 0.552900 11.00000 0.04723 0.03862 = 0.03153 0.01047 -0.01263 -0.01901 AFIX 43 H19 2 0.007696 0.203664 0.565340 11.00000 -1.20000 AFIX 0 C20 1 0.053478 0.323731 0.500237 11.00000 0.04260 0.03717 = 0.02796 0.00828 -0.01569 -0.01825 AFIX 43 H20 2 -0.014157 0.308963 0.477413 11.00000 -1.20000 AFIX 0 C21 1 0.243518 0.704220 0.122490 11.00000 0.01731 0.01629 = 0.01653 -0.00277 -0.00593 -0.00385 C22 1 0.290578 0.755752 0.066900 11.00000 0.01897 0.01920 = 0.01455 -0.00348 -0.00297 -0.00243 AFIX 43 H22 2 0.348423 0.722160 0.041691 11.00000 -1.20000 AFIX 0 C23 1 0.252392 0.857385 0.048195 11.00000 0.02102 0.01735 = 0.01527 -0.00308 -0.00455 -0.00103 C24 1 0.162986 0.903517 0.085694 11.00000 0.02021 0.01425 = 0.01857 -0.00107 -0.00474 0.00034 AFIX 43 H24 2 0.132869 0.972074 0.073598 11.00000 -1.20000 AFIX 0 C25 1 0.118262 0.848469 0.140890 11.00000 0.01808 0.01488 = 0.02008 -0.00384 -0.00570 0.00000 C26 1 0.037995 0.886368 0.187177 11.00000 0.02012 0.01948 = 0.01641 -0.00292 -0.00411 -0.00383 C27 1 -0.019221 0.983456 0.181465 11.00000 0.03011 0.02084 = 0.02161 -0.00344 -0.00399 -0.00026 AFIX 43 H27 2 -0.011607 1.030435 0.145304 11.00000 -1.20000 AFIX 0 C28 1 -0.088204 1.011111 0.229683 11.00000 0.03334 0.02349 = 0.02889 -0.01156 -0.00014 0.00042 AFIX 43 H28 2 -0.127259 1.077424 0.226833 11.00000 -1.20000 AFIX 0 C29 1 -0.098960 0.940921 0.281544 11.00000 0.02598 0.03219 = 0.02622 -0.01605 0.00303 -0.00333 AFIX 43 H29 2 -0.146394 0.958150 0.314776 11.00000 -1.20000 AFIX 0 C30 1 -0.039783 0.845105 0.284544 11.00000 0.02550 0.02954 = 0.01629 -0.00454 0.00050 -0.00721 AFIX 43 H30 2 -0.047310 0.797225 0.320398 11.00000 -1.20000 AFIX 0 C31 1 0.276477 0.479646 0.236774 11.00000 0.02361 0.01951 = 0.02156 0.00168 -0.00520 -0.00336 AFIX 43 H31 2 0.238962 0.458461 0.275956 11.00000 -1.20000 AFIX 0 C32 1 0.370023 0.414687 0.212298 11.00000 0.02572 0.01490 = 0.02664 0.00018 -0.00755 -0.00116 AFIX 43 H32 2 0.397024 0.350234 0.234490 11.00000 -1.20000 AFIX 0 C33 1 0.423265 0.444666 0.155511 11.00000 0.02648 0.01915 = 0.02685 -0.00808 -0.00967 0.00009 AFIX 43 H33 2 0.488523 0.401367 0.138140 11.00000 -1.20000 AFIX 0 C34 1 0.381007 0.538601 0.123757 11.00000 0.02206 0.01886 = 0.02102 -0.00564 -0.00713 -0.00161 AFIX 43 H34 2 0.415388 0.560232 0.084321 11.00000 -1.20000 AFIX 0 C35 1 0.287638 0.600234 0.150727 11.00000 0.01862 0.01600 = 0.01739 -0.00222 -0.00762 -0.00301 C36 1 0.318065 0.915898 -0.009017 11.00000 0.02669 0.01646 = 0.01411 -0.00457 -0.00404 -0.00271 C37 1 0.464785 0.895055 -0.031717 11.00000 0.02724 0.01893 = 0.02295 -0.00376 -0.00147 -0.00086 AFIX 43 H37 2 0.524669 0.842271 -0.011025 11.00000 -1.20000 AFIX 0 C38 1 0.522642 0.951691 -0.084549 11.00000 0.03386 0.02371 = 0.02969 -0.00654 0.00407 -0.00545 AFIX 43 H38 2 0.622861 0.935615 -0.099365 11.00000 -1.20000 AFIX 0 C39 1 0.306916 1.047991 -0.093820 11.00000 0.04129 0.01783 = 0.01915 -0.00087 -0.00614 -0.00147 AFIX 43 H39 2 0.250799 1.102216 -0.115200 11.00000 -1.20000 AFIX 0 C40 1 0.237849 0.995530 -0.041585 11.00000 0.02827 0.01941 = 0.01715 -0.00358 -0.00377 -0.00056 AFIX 43 H40 2 0.137306 1.013297 -0.027986 11.00000 -1.20000 AFIX 0 N13 4 0.949385 0.857570 -0.039258 11.00000 0.03602 0.01906 = 0.03315 -0.00554 -0.00461 0.00031 N14 4 0.609473 0.716324 0.102451 11.00000 0.02478 0.02520 = 0.02909 -0.00513 -0.00591 0.00208 N15 4 1.497213 0.354397 0.021755 11.00000 0.02950 0.02400 = 0.03026 -0.00657 -0.00532 0.00190 N16 4 1.161030 0.187025 0.155917 11.00000 0.04348 0.02704 = 0.03321 0.00346 -0.00463 -0.00221 C53 1 0.858430 0.700472 0.037618 11.00000 0.02096 0.01761 = 0.01827 -0.00577 -0.00430 0.00078 C54 1 0.720696 0.709825 0.072463 11.00000 0.02637 0.01372 = 0.02193 -0.00340 -0.01288 0.00057 C55 1 0.908093 0.787046 -0.004883 11.00000 0.02284 0.01780 = 0.02308 -0.00747 -0.00590 0.00251 C56 1 0.948657 0.611117 0.047462 11.00000 0.02266 0.01724 = 0.01719 -0.00568 -0.00746 -0.00155 C57 1 0.902606 0.524426 0.092162 11.00000 0.02050 0.02263 = 0.01765 -0.00586 -0.00180 -0.00185 AFIX 43 H57 2 0.808856 0.526613 0.115669 11.00000 -1.20000 AFIX 0 C58 1 0.992015 0.438692 0.101339 11.00000 0.02583 0.01841 = 0.01515 -0.00026 -0.00423 -0.00264 AFIX 43 H58 2 0.959132 0.382215 0.131079 11.00000 -1.20000 AFIX 0 C59 1 1.132868 0.432755 0.067211 11.00000 0.02154 0.01789 = 0.01712 -0.00560 -0.00709 -0.00084 C60 1 1.178424 0.518764 0.023221 11.00000 0.01827 0.01983 = 0.01968 -0.00647 -0.00339 -0.00230 AFIX 43 H60 2 1.272532 0.516802 -0.000113 11.00000 -1.20000 AFIX 0 C61 1 1.089104 0.604240 0.013930 11.00000 0.02399 0.01666 = 0.01819 -0.00178 -0.00489 -0.00405 AFIX 43 H61 2 1.122447 0.660493 -0.015883 11.00000 -1.20000 AFIX 0 C62 1 1.229602 0.346029 0.076829 11.00000 0.02345 0.01817 = 0.01774 -0.00397 -0.00447 -0.00135 C63 1 1.376188 0.348486 0.046302 11.00000 0.02567 0.01523 = 0.01790 -0.00367 -0.00558 0.00154 C64 1 1.191310 0.258405 0.120705 11.00000 0.02442 0.02409 = 0.02151 -0.00603 -0.00613 0.00424 N9 4 0.613508 1.184250 0.288000 11.00000 0.08526 0.04745 = 0.03306 -0.00110 -0.01313 -0.00739 N10 4 0.893701 1.237900 0.406282 11.00000 0.06010 0.04648 = 0.04837 -0.01105 0.00036 -0.02406 N11 4 0.354384 0.643380 0.513376 11.00000 0.05943 0.03592 = 0.07255 -0.01655 -0.01361 -0.01554 N12 4 0.639857 0.679211 0.635151 11.00000 0.05140 0.03060 = 0.04057 -0.00119 -0.00616 -0.00156 C41 1 0.704342 1.124531 0.386233 11.00000 0.03538 0.02536 = 0.02723 -0.00405 -0.00194 -0.00632 C42 1 0.807974 1.186547 0.397690 11.00000 0.04418 0.02907 = 0.02977 -0.00489 0.00399 -0.00746 C43 1 0.653384 1.157886 0.331892 11.00000 0.04882 0.02676 = 0.02883 -0.00421 0.00033 -0.00510 C44 1 0.662644 1.031834 0.424644 11.00000 0.02963 0.02307 = 0.02622 -0.00672 0.00083 -0.00250 C45 1 0.561144 0.969768 0.411694 11.00000 0.03756 0.02780 = 0.02443 -0.00756 -0.00810 -0.00096 AFIX 43 H45 2 0.522273 0.990273 0.376315 11.00000 -1.20000 AFIX 0 C46 1 0.518239 0.881478 0.448854 11.00000 0.03483 0.02473 = 0.03348 -0.01094 -0.00741 -0.00403 AFIX 43 H46 2 0.448800 0.842204 0.439178 11.00000 -1.20000 AFIX 0 C47 1 0.576170 0.846727 0.502419 11.00000 0.02884 0.01961 = 0.02841 -0.00852 -0.00179 -0.00026 C48 1 0.679350 0.908304 0.514609 11.00000 0.04071 0.02797 = 0.02313 -0.00541 -0.00779 -0.00415 AFIX 43 H48 2 0.720947 0.887128 0.549435 11.00000 -1.20000 AFIX 0 C49 1 0.720429 0.997274 0.477549 11.00000 0.03556 0.02737 = 0.02847 -0.00956 -0.00467 -0.00970 AFIX 43 H49 2 0.789094 1.036960 0.487307 11.00000 -1.20000 AFIX 0 C50 1 0.532224 0.755362 0.540599 11.00000 0.03224 0.02113 = 0.02837 -0.00655 -0.00015 -0.00172 C51 1 0.592435 0.715015 0.592865 11.00000 0.03873 0.01800 = 0.03212 -0.00288 0.00146 -0.00259 C52 1 0.433587 0.693136 0.526089 11.00000 0.03814 0.02302 = 0.04177 -0.00644 -0.00249 -0.00336 O1 5 -0.184831 0.089505 0.615209 11.00000 0.07582 0.06388 = 0.13950 0.03794 -0.04253 -0.03394 N17 4 -0.209043 -0.057025 0.680969 11.00000 0.06426 0.04489 = 0.05851 -0.00364 -0.01820 -0.01274 C65 1 -0.155586 0.000690 0.628065 11.00000 0.05526 0.07445 = 0.05243 0.00843 -0.02030 -0.02873 AFIX 43 H65 2 -0.095590 -0.029257 0.601577 11.00000 -1.20000 AFIX 0 C66 1 -0.299577 -0.016275 0.726270 11.00000 0.06699 0.04521 = 0.11294 -0.03247 0.01715 0.00413 AFIX 137 H66A 2 -0.242679 -0.028033 0.758730 11.00000 -1.50000 H66B 2 -0.396367 -0.049765 0.738395 11.00000 -1.50000 H66C 2 -0.318927 0.055640 0.711328 11.00000 -1.50000 AFIX 0 C67 1 -0.178872 -0.165259 0.696747 11.00000 0.11295 0.04537 = 0.07397 -0.01300 -0.00493 -0.00899 AFIX 137 H67A 2 -0.118386 -0.184965 0.664846 11.00000 -1.50000 H67B 2 -0.275219 -0.199436 0.706307 11.00000 -1.50000 H67C 2 -0.122825 -0.183783 0.729644 11.00000 -1.50000 AFIX 0 O2 5 0.706535 1.273263 0.168281 11.00000 0.09489 0.06381 = 0.04466 -0.01054 0.01278 -0.00522 AFIX 147 H2A 2 0.692576 1.243519 0.202964 11.00000 -1.50000 AFIX 0 C68 1 0.693250 1.207575 0.137017 11.00000 0.15879 0.05133 = 0.05978 -0.02146 -0.06214 0.03031 AFIX 137 H68A 2 0.652294 1.243123 0.101944 11.00000 -1.50000 H68B 2 0.624627 1.154971 0.159026 11.00000 -1.50000 H68C 2 0.793315 1.177592 0.127694 11.00000 -1.50000 AFIX 0 HKLF 4 REM P-1_a.res in P-1 REM R1 = 0.0508 for 8274 Fo > 4sig(Fo) and 0.0759 for all 11425 data REM 797 parameters refined using 0 restraints END WGHT 0.0636 0.0000 REM Highest difference peak 0.988, deepest hole -0.676, 1-sigma level 0.080 Q1 1 -0.3911 -0.0740 0.7509 11.00000 0.05 0.76 ; _shelx_res_checksum 68651 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 0.12437(4) 0.68311(2) 0.23620(2) 0.01413(11) Uani 1 1 d . . . . . N1 N 0.1124(2) 0.61070(14) 0.31668(8) 0.0166(4) Uani 1 1 d . . . . . N2 N 0.3371(2) 0.72609(14) 0.26100(9) 0.0203(5) Uani 1 1 d . . . . . N3 N -0.0969(2) 0.61097(14) 0.25245(9) 0.0220(5) Uani 1 1 d . . . . . N4 N 0.1587(2) 0.75078(14) 0.15841(8) 0.0162(4) Uani 1 1 d . . . . . N5 N 0.2370(2) 0.57211(14) 0.20669(9) 0.0192(5) Uani 1 1 d . . . . . N6 N 0.0276(2) 0.81734(14) 0.23889(9) 0.0194(5) Uani 1 1 d . . . . . N7 N 0.1599(3) 0.27605(16) 0.58806(9) 0.0305(6) Uani 1 1 d . . . . . N8 N 0.4468(3) 1.02792(15) -0.11638(10) 0.0303(6) Uani 1 1 d . . . . . C1 C 0.2260(3) 0.61580(17) 0.34690(10) 0.0174(5) Uani 1 1 d . . . . . C2 C 0.2355(3) 0.55237(18) 0.40025(11) 0.0223(6) Uani 1 1 d . . . . . H2 H 0.3156 0.5581 0.4206 0.027 Uiso 1 1 calc R . . . . C3 C 0.1279(3) 0.48013(17) 0.42415(10) 0.0184(5) Uani 1 1 d . . . . . C4 C 0.0102(3) 0.47686(17) 0.39288(10) 0.0200(6) Uani 1 1 d . . . . . H4 H -0.0659 0.4290 0.4080 0.024 Uiso 1 1 calc R . . . . C5 C 0.0041(3) 0.54288(17) 0.34009(11) 0.0183(5) Uani 1 1 d . . . . . C6 C -0.1179(3) 0.54603(17) 0.30404(11) 0.0209(6) Uani 1 1 d . . . . . C7 C -0.2459(3) 0.4886(2) 0.32285(12) 0.0329(7) Uani 1 1 d . . . . . H7 H -0.2584 0.4433 0.3595 0.040 Uiso 1 1 calc R . . . . C8 C -0.3551(3) 0.4995(2) 0.28640(13) 0.0382(8) Uani 1 1 d . . . . . H8 H -0.4431 0.4607 0.2978 0.046 Uiso 1 1 calc R . . . . C9 C -0.3350(3) 0.5671(2) 0.23351(13) 0.0333(7) Uani 1 1 d . . . . . H9 H -0.4092 0.5763 0.2083 0.040 Uiso 1 1 calc R . . . . C10 C -0.2045(3) 0.62050(18) 0.21835(12) 0.0266(6) Uani 1 1 d . . . . . H10 H -0.1900 0.6664 0.1819 0.032 Uiso 1 1 calc R . . . . C11 C 0.4423(3) 0.79023(18) 0.23104(11) 0.0242(6) Uani 1 1 d . . . . . H11 H 0.4401 0.8158 0.1914 0.029 Uiso 1 1 calc R . . . . C12 C 0.5545(3) 0.82089(19) 0.25557(12) 0.0275(6) Uani 1 1 d . . . . . H12 H 0.6287 0.8654 0.2328 0.033 Uiso 1 1 calc R . . . . C13 C 0.5570(3) 0.78597(19) 0.31326(12) 0.0303(7) Uani 1 1 d . . . . . H13 H 0.6321 0.8064 0.3310 0.036 Uiso 1 1 calc R . . . . C14 C 0.4473(3) 0.72023(19) 0.34480(11) 0.0255(6) Uani 1 1 d . . . . . H14 H 0.4445 0.6962 0.3848 0.031 Uiso 1 1 calc R . . . . C15 C 0.3421(3) 0.69028(17) 0.31723(11) 0.0199(6) Uani 1 1 d . . . . . C16 C 0.1388(3) 0.40877(17) 0.48045(11) 0.0203(6) Uani 1 1 d . . . . . C17 C 0.2353(3) 0.42492(18) 0.51668(11) 0.0246(6) Uani 1 1 d . . . . . H17 H 0.2965 0.4818 0.5055 0.030 Uiso 1 1 calc R . . . . C18 C 0.2407(3) 0.35754(19) 0.56881(12) 0.0280(6) Uani 1 1 d . . . . . H18 H 0.3071 0.3703 0.5927 0.034 Uiso 1 1 calc R . . . . C19 C 0.0674(4) 0.2612(2) 0.55290(13) 0.0413(8) Uani 1 1 d . . . . . H19 H 0.0077 0.2037 0.5653 0.050 Uiso 1 1 calc R . . . . C20 C 0.0535(3) 0.3237(2) 0.50024(13) 0.0372(8) Uani 1 1 d . . . . . H20 H -0.0142 0.3090 0.4774 0.045 Uiso 1 1 calc R . . . . C21 C 0.2435(3) 0.70422(16) 0.12249(10) 0.0165(5) Uani 1 1 d . . . . . C22 C 0.2906(3) 0.75575(17) 0.06690(10) 0.0176(5) Uani 1 1 d . . . . . H22 H 0.3484 0.7222 0.0417 0.021 Uiso 1 1 calc R . . . . C23 C 0.2524(3) 0.85738(17) 0.04819(10) 0.0179(5) Uani 1 1 d . . . . . C24 C 0.1630(3) 0.90352(17) 0.08569(10) 0.0181(5) Uani 1 1 d . . . . . H24 H 0.1329 0.9721 0.0736 0.022 Uiso 1 1 calc R . . . . C25 C 0.1183(3) 0.84847(16) 0.14089(11) 0.0175(5) Uani 1 1 d . . . . . C26 C 0.0380(3) 0.88637(17) 0.18718(10) 0.0187(5) Uani 1 1 d . . . . . C27 C -0.0192(3) 0.98346(18) 0.18146(11) 0.0246(6) Uani 1 1 d . . . . . H27 H -0.0116 1.0304 0.1453 0.029 Uiso 1 1 calc R . . . . C28 C -0.0882(3) 1.01111(19) 0.22968(12) 0.0281(6) Uani 1 1 d . . . . . H28 H -0.1273 1.0774 0.2268 0.034 Uiso 1 1 calc R . . . . C29 C -0.0990(3) 0.94092(19) 0.28154(12) 0.0270(6) Uani 1 1 d . . . . . H29 H -0.1464 0.9582 0.3148 0.032 Uiso 1 1 calc R . . . . C30 C -0.0398(3) 0.84510(19) 0.28454(11) 0.0241(6) Uani 1 1 d . . . . . H30 H -0.0473 0.7972 0.3204 0.029 Uiso 1 1 calc R . . . . C31 C 0.2765(3) 0.47965(17) 0.23677(11) 0.0226(6) Uani 1 1 d . . . . . H31 H 0.2390 0.4585 0.2760 0.027 Uiso 1 1 calc R . . . . C32 C 0.3700(3) 0.41469(18) 0.21230(11) 0.0231(6) Uani 1 1 d . . . . . H32 H 0.3970 0.3502 0.2345 0.028 Uiso 1 1 calc R . . . . C33 C 0.4233(3) 0.44467(18) 0.15551(11) 0.0232(6) Uani 1 1 d . . . . . H33 H 0.4885 0.4014 0.1381 0.028 Uiso 1 1 calc R . . . . C34 C 0.3810(3) 0.53860(17) 0.12376(11) 0.0201(6) Uani 1 1 d . . . . . H34 H 0.4154 0.5602 0.0843 0.024 Uiso 1 1 calc R . . . . C35 C 0.2876(3) 0.60023(16) 0.15073(10) 0.0171(5) Uani 1 1 d . . . . . C36 C 0.3181(3) 0.91590(17) -0.00902(10) 0.0187(5) Uani 1 1 d . . . . . C37 C 0.4648(3) 0.89505(18) -0.03172(11) 0.0236(6) Uani 1 1 d . . . . . H37 H 0.5247 0.8423 -0.0110 0.028 Uiso 1 1 calc R . . . . C38 C 0.5226(3) 0.95169(19) -0.08455(12) 0.0298(7) Uani 1 1 d . . . . . H38 H 0.6229 0.9356 -0.0994 0.036 Uiso 1 1 calc R . . . . C39 C 0.3069(3) 1.04799(18) -0.09382(11) 0.0266(6) Uani 1 1 d . . . . . H39 H 0.2508 1.1022 -0.1152 0.032 Uiso 1 1 calc R . . . . C40 C 0.2378(3) 0.99553(17) -0.04158(11) 0.0218(6) Uani 1 1 d . . . . . H40 H 0.1373 1.0133 -0.0280 0.026 Uiso 1 1 calc R . . . . N13 N 0.9494(3) 0.85757(15) -0.03926(10) 0.0297(6) Uani 1 1 d . . . . . N14 N 0.6095(3) 0.71632(15) 0.10245(10) 0.0267(5) Uani 1 1 d . . . . . N15 N 1.4972(3) 0.35440(15) 0.02176(10) 0.0280(5) Uani 1 1 d . . . . . N16 N 1.1610(3) 0.18703(17) 0.15592(11) 0.0368(6) Uani 1 1 d . . . . . C53 C 0.8584(3) 0.70047(17) 0.03762(10) 0.0186(5) Uani 1 1 d . . . . . C54 C 0.7207(3) 0.70983(17) 0.07246(11) 0.0200(6) Uani 1 1 d . . . . . C55 C 0.9081(3) 0.78705(18) -0.00488(11) 0.0207(6) Uani 1 1 d . . . . . C56 C 0.9487(3) 0.61112(17) 0.04746(10) 0.0183(5) Uani 1 1 d . . . . . C57 C 0.9026(3) 0.52443(17) 0.09216(11) 0.0202(6) Uani 1 1 d . . . . . H57 H 0.8089 0.5266 0.1157 0.024 Uiso 1 1 calc R . . . . C58 C 0.9920(3) 0.43869(17) 0.10134(10) 0.0204(6) Uani 1 1 d . . . . . H58 H 0.9591 0.3822 0.1311 0.024 Uiso 1 1 calc R . . . . C59 C 1.1329(3) 0.43275(17) 0.06721(10) 0.0182(5) Uani 1 1 d . . . . . C60 C 1.1784(3) 0.51876(17) 0.02322(11) 0.0188(5) Uani 1 1 d . . . . . H60 H 1.2725 0.5168 -0.0001 0.023 Uiso 1 1 calc R . . . . C61 C 1.0891(3) 0.60424(17) 0.01393(11) 0.0198(6) Uani 1 1 d . . . . . H61 H 1.1224 0.6605 -0.0159 0.024 Uiso 1 1 calc R . . . . C62 C 1.2296(3) 0.34603(17) 0.07683(11) 0.0197(6) Uani 1 1 d . . . . . C63 C 1.3762(3) 0.34849(17) 0.04630(11) 0.0196(6) Uani 1 1 d . . . . . C64 C 1.1913(3) 0.25841(19) 0.12071(11) 0.0233(6) Uani 1 1 d . . . . . N9 N 0.6135(4) 1.1843(2) 0.28800(12) 0.0563(8) Uani 1 1 d . . . . . N10 N 0.8937(3) 1.2379(2) 0.40628(12) 0.0515(8) Uani 1 1 d . . . . . N11 N 0.3544(3) 0.64338(19) 0.51338(14) 0.0543(8) Uani 1 1 d . . . . . N12 N 0.6399(3) 0.67921(18) 0.63515(12) 0.0424(7) Uani 1 1 d . . . . . C41 C 0.7043(3) 1.12453(19) 0.38623(12) 0.0298(7) Uani 1 1 d . . . . . C42 C 0.8080(4) 1.1865(2) 0.39769(13) 0.0355(7) Uani 1 1 d . . . . . C43 C 0.6534(4) 1.1579(2) 0.33189(13) 0.0358(7) Uani 1 1 d . . . . . C44 C 0.6626(3) 1.03183(19) 0.42464(12) 0.0266(6) Uani 1 1 d . . . . . C45 C 0.5611(3) 0.96977(19) 0.41169(12) 0.0294(7) Uani 1 1 d . . . . . H45 H 0.5223 0.9903 0.3763 0.035 Uiso 1 1 calc R . . . . C46 C 0.5182(3) 0.88148(19) 0.44885(12) 0.0299(7) Uani 1 1 d . . . . . H46 H 0.4488 0.8422 0.4392 0.036 Uiso 1 1 calc R . . . . C47 C 0.5762(3) 0.84673(18) 0.50242(12) 0.0254(6) Uani 1 1 d . . . . . C48 C 0.6794(3) 0.90830(19) 0.51461(12) 0.0303(7) Uani 1 1 d . . . . . H48 H 0.7209 0.8871 0.5494 0.036 Uiso 1 1 calc R . . . . C49 C 0.7204(3) 0.99727(19) 0.47755(12) 0.0295(7) Uani 1 1 d . . . . . H49 H 0.7891 1.0370 0.4873 0.035 Uiso 1 1 calc R . . . . C50 C 0.5322(3) 0.75536(18) 0.54060(12) 0.0276(6) Uani 1 1 d . . . . . C51 C 0.5924(3) 0.71502(19) 0.59286(13) 0.0309(7) Uani 1 1 d . . . . . C52 C 0.4336(3) 0.6931(2) 0.52609(13) 0.0349(7) Uani 1 1 d . . . . . O1 O -0.1848(3) 0.0895(2) 0.61521(16) 0.1013(13) Uani 1 1 d . . . . . N17 N -0.2090(4) -0.0570(2) 0.68097(14) 0.0563(8) Uani 1 1 d . . . . . C65 C -0.1556(4) 0.0007(3) 0.62807(17) 0.0630(12) Uani 1 1 d . . . . . H65 H -0.0956 -0.0293 0.6016 0.076 Uiso 1 1 calc R . . . . C66 C -0.2996(5) -0.0163(3) 0.7263(2) 0.0760(13) Uani 1 1 d . . . . . H66A H -0.2427 -0.0280 0.7587 0.114 Uiso 1 1 calc GR . . . . H66B H -0.3964 -0.0498 0.7384 0.114 Uiso 1 1 calc GR . . . . H66C H -0.3189 0.0556 0.7113 0.114 Uiso 1 1 calc GR . . . . C67 C -0.1789(5) -0.1653(3) 0.69675(19) 0.0784(13) Uani 1 1 d . . . . . H67A H -0.1184 -0.1850 0.6648 0.118 Uiso 1 1 calc GR . . . . H67B H -0.2752 -0.1994 0.7063 0.118 Uiso 1 1 calc GR . . . . H67C H -0.1228 -0.1838 0.7296 0.118 Uiso 1 1 calc GR . . . . O2 O 0.7065(4) 1.27326(19) 0.16828(11) 0.0706(8) Uani 1 1 d . . . . . H2A H 0.6926 1.2435 0.2030 0.106 Uiso 1 1 calc GR . . . . C68 C 0.6932(6) 1.2076(3) 0.13702(17) 0.0855(17) Uani 1 1 d . . . . . H68A H 0.6523 1.2431 0.1019 0.128 Uiso 1 1 calc GR . . . . H68B H 0.6246 1.1550 0.1590 0.128 Uiso 1 1 calc GR . . . . H68C H 0.7933 1.1776 0.1277 0.128 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 Co1 0.0185(2) 0.01192(17) 0.01025(18) 0.00095(12) -0.00334(14) -0.00157(13) N1 0.0170(11) 0.0156(10) 0.0158(11) -0.0018(8) -0.0016(9) -0.0016(8) N2 0.0233(12) 0.0177(10) 0.0183(12) -0.0004(9) -0.0037(10) -0.0043(9) N3 0.0263(12) 0.0190(11) 0.0212(12) -0.0026(9) -0.0103(10) 0.0002(9) N4 0.0181(11) 0.0150(10) 0.0148(11) -0.0024(8) -0.0025(9) -0.0006(8) N5 0.0195(11) 0.0173(10) 0.0184(12) 0.0015(8) -0.0059(10) -0.0026(8) N6 0.0205(12) 0.0213(11) 0.0159(11) -0.0026(9) -0.0024(9) -0.0058(9) N7 0.0363(14) 0.0313(13) 0.0172(12) 0.0042(10) -0.0012(11) -0.0030(11) N8 0.0442(16) 0.0212(12) 0.0213(13) -0.0018(10) 0.0045(12) -0.0063(10) C1 0.0188(13) 0.0175(12) 0.0172(13) -0.0063(10) -0.0032(11) -0.0006(10) C2 0.0248(15) 0.0248(13) 0.0175(14) -0.0023(11) -0.0082(12) -0.0045(11) C3 0.0221(14) 0.0164(12) 0.0155(13) -0.0028(10) -0.0022(11) 0.0007(10) C4 0.0229(14) 0.0172(12) 0.0195(14) -0.0023(10) -0.0042(12) -0.0044(10) C5 0.0168(13) 0.0198(12) 0.0185(13) -0.0061(10) -0.0010(11) -0.0016(10) C6 0.0234(14) 0.0202(13) 0.0197(14) -0.0044(10) -0.0058(12) -0.0018(10) C7 0.0310(17) 0.0380(16) 0.0282(17) 0.0004(13) -0.0102(14) -0.0131(13) C8 0.0294(17) 0.0471(18) 0.0391(19) -0.0060(15) -0.0120(15) -0.0141(14) C9 0.0332(17) 0.0364(16) 0.0347(18) -0.0083(13) -0.0203(15) -0.0019(13) C10 0.0348(16) 0.0240(14) 0.0229(15) -0.0045(11) -0.0141(13) 0.0001(12) C11 0.0291(15) 0.0214(13) 0.0188(14) 0.0002(11) 0.0007(12) -0.0068(11) C12 0.0270(15) 0.0254(14) 0.0269(16) -0.0011(12) 0.0011(13) -0.0117(12) C13 0.0287(16) 0.0327(15) 0.0310(17) -0.0049(12) -0.0101(14) -0.0116(12) C14 0.0292(16) 0.0296(14) 0.0162(14) 0.0003(11) -0.0071(12) -0.0079(12) C15 0.0198(14) 0.0197(12) 0.0194(14) -0.0026(10) -0.0036(11) -0.0024(10) C16 0.0218(14) 0.0201(13) 0.0169(13) -0.0012(10) -0.0036(11) 0.0006(10) C17 0.0297(15) 0.0227(13) 0.0209(14) -0.0022(11) -0.0067(13) -0.0039(11) C18 0.0315(16) 0.0323(15) 0.0195(15) -0.0043(12) -0.0073(13) 0.0011(12) C19 0.047(2) 0.0386(17) 0.0315(18) 0.0105(14) -0.0126(16) -0.0190(15) C20 0.0426(19) 0.0372(17) 0.0280(17) 0.0083(13) -0.0157(15) -0.0183(14) C21 0.0173(13) 0.0163(12) 0.0165(13) -0.0028(10) -0.0059(11) -0.0038(10) C22 0.0190(13) 0.0192(12) 0.0145(13) -0.0035(10) -0.0030(11) -0.0024(10) C23 0.0210(14) 0.0174(12) 0.0153(13) -0.0031(10) -0.0046(11) -0.0010(10) C24 0.0202(14) 0.0142(12) 0.0186(14) -0.0011(10) -0.0047(11) 0.0003(10) C25 0.0181(13) 0.0149(12) 0.0201(14) -0.0038(10) -0.0057(11) 0.0000(10) C26 0.0201(14) 0.0195(12) 0.0164(13) -0.0029(10) -0.0041(11) -0.0038(10) C27 0.0301(16) 0.0208(13) 0.0216(14) -0.0034(11) -0.0040(13) -0.0003(11) C28 0.0333(17) 0.0235(14) 0.0289(16) -0.0116(12) -0.0001(13) 0.0004(12) C29 0.0260(15) 0.0322(15) 0.0262(16) -0.0161(12) 0.0030(13) -0.0033(12) C30 0.0255(15) 0.0295(14) 0.0163(14) -0.0045(11) 0.0005(12) -0.0072(11) C31 0.0236(14) 0.0195(13) 0.0216(14) 0.0017(11) -0.0052(12) -0.0034(11) C32 0.0257(15) 0.0149(12) 0.0266(15) 0.0002(11) -0.0075(13) -0.0012(10) C33 0.0265(15) 0.0191(13) 0.0268(15) -0.0081(11) -0.0097(13) 0.0001(11) C34 0.0221(14) 0.0189(12) 0.0210(14) -0.0056(10) -0.0071(12) -0.0016(10) C35 0.0186(13) 0.0160(12) 0.0174(13) -0.0022(10) -0.0076(11) -0.0030(10) C36 0.0267(15) 0.0165(12) 0.0141(13) -0.0046(10) -0.0040(11) -0.0027(10) C37 0.0272(15) 0.0189(13) 0.0230(15) -0.0038(11) -0.0015(12) -0.0009(11) C38 0.0339(17) 0.0237(14) 0.0297(16) -0.0065(12) 0.0041(14) -0.0055(12) C39 0.0413(18) 0.0178(13) 0.0191(14) -0.0009(11) -0.0061(13) -0.0015(12) C40 0.0283(15) 0.0194(13) 0.0171(14) -0.0036(10) -0.0038(12) -0.0006(11) N13 0.0360(14) 0.0191(12) 0.0331(14) -0.0055(10) -0.0046(12) 0.0003(10) N14 0.0248(13) 0.0252(12) 0.0291(14) -0.0051(10) -0.0059(12) 0.0021(10) N15 0.0295(14) 0.0240(12) 0.0303(14) -0.0066(10) -0.0053(12) 0.0019(10) N16 0.0435(16) 0.0270(13) 0.0332(15) 0.0035(11) -0.0046(13) -0.0022(11) C53 0.0210(14) 0.0176(12) 0.0183(13) -0.0058(10) -0.0043(11) 0.0008(10) C54 0.0264(16) 0.0137(12) 0.0219(14) -0.0034(10) -0.0129(13) 0.0006(10) C55 0.0228(14) 0.0178(13) 0.0231(14) -0.0075(11) -0.0059(12) 0.0025(10) C56 0.0227(14) 0.0172(12) 0.0172(13) -0.0057(10) -0.0075(11) -0.0016(10) C57 0.0205(14) 0.0226(13) 0.0176(13) -0.0059(10) -0.0018(11) -0.0019(10) C58 0.0258(15) 0.0184(12) 0.0152(13) -0.0003(10) -0.0042(12) -0.0026(10) C59 0.0215(14) 0.0179(12) 0.0171(13) -0.0056(10) -0.0071(11) -0.0008(10) C60 0.0183(13) 0.0198(12) 0.0197(14) -0.0065(10) -0.0034(11) -0.0023(10) C61 0.0240(14) 0.0167(12) 0.0182(13) -0.0018(10) -0.0049(12) -0.0041(10) C62 0.0234(14) 0.0182(12) 0.0177(13) -0.0040(10) -0.0045(12) -0.0014(10) C63 0.0257(16) 0.0152(12) 0.0179(14) -0.0037(10) -0.0056(12) 0.0015(10) C64 0.0244(15) 0.0241(14) 0.0215(15) -0.0060(12) -0.0061(12) 0.0042(11) N9 0.085(2) 0.0474(17) 0.0331(18) -0.0011(13) -0.0131(17) -0.0074(16) N10 0.060(2) 0.0465(17) 0.0484(19) -0.0110(14) 0.0004(16) -0.0241(15) N11 0.059(2) 0.0359(15) 0.073(2) -0.0166(15) -0.0136(17) -0.0155(14) N12 0.0514(18) 0.0306(14) 0.0406(17) -0.0012(12) -0.0062(14) -0.0016(12) C41 0.0354(17) 0.0254(14) 0.0272(16) -0.0041(12) -0.0019(14) -0.0063(12) C42 0.0442(19) 0.0291(16) 0.0298(17) -0.0049(13) 0.0040(15) -0.0075(14) C43 0.049(2) 0.0268(15) 0.0288(18) -0.0042(13) 0.0003(15) -0.0051(13) C44 0.0296(16) 0.0231(14) 0.0262(15) -0.0067(11) 0.0008(13) -0.0025(11) C45 0.0376(17) 0.0278(14) 0.0244(15) -0.0076(12) -0.0081(14) -0.0010(12) C46 0.0348(17) 0.0247(14) 0.0335(17) -0.0109(12) -0.0074(14) -0.0040(12) C47 0.0288(15) 0.0196(13) 0.0284(16) -0.0085(11) -0.0018(13) -0.0003(11) C48 0.0407(18) 0.0280(15) 0.0231(15) -0.0054(12) -0.0078(14) -0.0041(13) C49 0.0356(17) 0.0274(15) 0.0285(16) -0.0096(12) -0.0047(14) -0.0097(12) C50 0.0322(16) 0.0211(13) 0.0284(16) -0.0066(12) -0.0002(13) -0.0017(12) C51 0.0387(18) 0.0180(13) 0.0321(17) -0.0029(12) 0.0015(15) -0.0026(12) C52 0.0381(18) 0.0230(14) 0.0418(19) -0.0064(13) -0.0025(15) -0.0034(13) O1 0.076(2) 0.0639(19) 0.139(3) 0.0379(19) -0.043(2) -0.0339(16) N17 0.064(2) 0.0449(17) 0.059(2) -0.0036(15) -0.0182(18) -0.0127(15) C65 0.055(2) 0.074(3) 0.052(3) 0.008(2) -0.020(2) -0.029(2) C66 0.067(3) 0.045(2) 0.113(4) -0.032(2) 0.017(3) 0.0041(19) C67 0.113(4) 0.045(2) 0.074(3) -0.013(2) -0.005(3) -0.009(2) O2 0.095(2) 0.0638(17) 0.0447(16) -0.0105(13) 0.0128(17) -0.0052(15) C68 0.159(5) 0.051(2) 0.060(3) -0.021(2) -0.062(3) 0.030(3) 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' Co Co 0.3494 0.9721 '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' 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 N1 Co1 N2 77.47(8) . . N1 Co1 N3 77.30(8) . . N1 Co1 N5 95.76(9) . . N1 Co1 N6 102.68(9) . . N3 Co1 N2 154.63(8) . . N4 Co1 N1 173.86(8) . . N4 Co1 N2 97.33(8) . . N4 Co1 N3 108.01(8) . . N4 Co1 N5 81.00(9) . . N4 Co1 N6 80.40(9) . . N5 Co1 N2 91.61(8) . . N5 Co1 N3 93.50(9) . . N6 Co1 N2 89.84(8) . . N6 Co1 N3 93.10(9) . . N6 Co1 N5 161.37(9) . . C1 N1 Co1 120.21(16) . . C5 N1 Co1 120.09(16) . . C5 N1 C1 118.8(2) . . C11 N2 Co1 130.14(17) . . C11 N2 C15 117.9(2) . . C15 N2 Co1 111.22(16) . . C6 N3 Co1 112.01(15) . . C10 N3 Co1 129.72(18) . . C10 N3 C6 118.2(2) . . C21 N4 Co1 118.77(16) . . C25 N4 Co1 119.88(17) . . C25 N4 C21 120.6(2) . . C31 N5 Co1 127.88(19) . . C35 N5 Co1 113.50(15) . . C35 N5 C31 118.3(2) . . C26 N6 Co1 113.76(17) . . C30 N6 Co1 127.54(17) . . C30 N6 C26 118.7(2) . . C18 N7 C19 115.5(2) . . C39 N8 C38 115.8(2) . . N1 C1 C2 121.8(2) . . N1 C1 C15 115.1(2) . . C2 C1 C15 123.1(2) . . C1 C2 H2 119.9 . . C1 C2 C3 120.1(2) . . C3 C2 H2 119.9 . . C2 C3 C4 117.4(2) . . C2 C3 C16 121.1(2) . . C4 C3 C16 121.4(2) . . C3 C4 H4 119.8 . . C5 C4 C3 120.4(2) . . C5 C4 H4 119.8 . . N1 C5 C4 121.4(2) . . N1 C5 C6 114.3(2) . . C4 C5 C6 124.2(2) . . N3 C6 C5 114.8(2) . . N3 C6 C7 122.4(2) . . C7 C6 C5 122.8(2) . . C6 C7 H7 121.0 . . C6 C7 C8 118.1(3) . . C8 C7 H7 121.0 . . C7 C8 H8 120.1 . . C9 C8 C7 119.8(3) . . C9 C8 H8 120.1 . . C8 C9 H9 120.9 . . C10 C9 C8 118.2(2) . . C10 C9 H9 120.9 . . N3 C10 C9 123.3(3) . . N3 C10 H10 118.3 . . C9 C10 H10 118.3 . . N2 C11 H11 118.7 . . N2 C11 C12 122.7(2) . . C12 C11 H11 118.7 . . C11 C12 H12 120.4 . . C13 C12 C11 119.3(2) . . C13 C12 H12 120.4 . . C12 C13 H13 120.8 . . C12 C13 C14 118.5(2) . . C14 C13 H13 120.8 . . C13 C14 H14 120.5 . . C15 C14 C13 119.1(2) . . C15 C14 H14 120.5 . . N2 C15 C1 114.5(2) . . N2 C15 C14 122.6(2) . . C14 C15 C1 122.9(2) . . C17 C16 C3 121.1(2) . . C20 C16 C3 122.4(2) . . C20 C16 C17 116.5(2) . . C16 C17 H17 120.4 . . C18 C17 C16 119.3(2) . . C18 C17 H17 120.4 . . N7 C18 C17 124.7(2) . . N7 C18 H18 117.7 . . C17 C18 H18 117.7 . . N7 C19 H19 117.8 . . N7 C19 C20 124.3(3) . . C20 C19 H19 117.8 . . C16 C20 H20 120.2 . . C19 C20 C16 119.6(3) . . C19 C20 H20 120.2 . . N4 C21 C22 120.7(2) . . N4 C21 C35 112.6(2) . . C22 C21 C35 126.4(2) . . C21 C22 H22 120.2 . . C21 C22 C23 119.6(2) . . C23 C22 H22 120.2 . . C22 C23 C36 119.8(2) . . C24 C23 C22 118.7(2) . . C24 C23 C36 121.2(2) . . C23 C24 H24 120.3 . . C25 C24 C23 119.4(2) . . C25 C24 H24 120.3 . . N4 C25 C24 120.9(2) . . N4 C25 C26 112.0(2) . . C24 C25 C26 126.9(2) . . N6 C26 C25 113.7(2) . . N6 C26 C27 121.5(2) . . C27 C26 C25 124.8(2) . . C26 C27 H27 120.5 . . C26 C27 C28 119.0(2) . . C28 C27 H27 120.5 . . C27 C28 H28 120.4 . . C29 C28 C27 119.2(2) . . C29 C28 H28 120.4 . . C28 C29 H29 120.4 . . C28 C29 C30 119.2(3) . . C30 C29 H29 120.4 . . N6 C30 C29 122.5(2) . . N6 C30 H30 118.7 . . C29 C30 H30 118.7 . . N5 C31 H31 119.0 . . N5 C31 C32 122.1(3) . . C32 C31 H31 119.0 . . C31 C32 H32 120.4 . . C33 C32 C31 119.2(2) . . C33 C32 H32 120.4 . . C32 C33 H33 120.3 . . C32 C33 C34 119.5(3) . . C34 C33 H33 120.3 . . C33 C34 H34 120.7 . . C35 C34 C33 118.6(2) . . C35 C34 H34 120.7 . . N5 C35 C21 113.8(2) . . N5 C35 C34 122.3(2) . . C34 C35 C21 123.7(2) . . C37 C36 C23 120.9(2) . . C37 C36 C40 117.0(2) . . C40 C36 C23 122.0(2) . . C36 C37 H37 120.3 . . C38 C37 C36 119.4(2) . . C38 C37 H37 120.3 . . N8 C38 C37 124.3(3) . . N8 C38 H38 117.9 . . C37 C38 H38 117.9 . . N8 C39 H39 117.7 . . N8 C39 C40 124.6(2) . . C40 C39 H39 117.7 . . C36 C40 H40 120.5 . . C39 C40 C36 119.0(3) . . C39 C40 H40 120.5 . . C54 C53 C55 117.0(2) . . C56 C53 C54 121.5(2) . . C56 C53 C55 121.3(2) . . N14 C54 C53 178.1(3) . . N13 C55 C53 179.5(3) . . C53 C56 C57 121.7(2) . . C61 C56 C53 120.9(2) . . C61 C56 C57 117.4(2) . . C56 C57 H57 119.6 . . C58 C57 C56 120.9(2) . . C58 C57 H57 119.6 . . C57 C58 H58 119.4 . . C57 C58 C59 121.1(2) . . C59 C58 H58 119.4 . . C58 C59 C60 117.8(2) . . C62 C59 C58 122.3(2) . . C62 C59 C60 119.8(2) . . C59 C60 H60 119.5 . . C61 C60 C59 121.1(2) . . C61 C60 H60 119.5 . . C56 C61 H61 119.2 . . C60 C61 C56 121.7(2) . . C60 C61 H61 119.2 . . C59 C62 C64 122.4(2) . . C63 C62 C59 119.8(2) . . C63 C62 C64 117.5(2) . . N15 C63 C62 177.0(3) . . N16 C64 C62 179.4(3) . . C42 C41 C43 115.6(2) . . C42 C41 C44 122.1(3) . . C44 C41 C43 122.1(2) . . N10 C42 C41 179.0(3) . . N9 C43 C41 179.4(4) . . C41 C44 C45 121.1(2) . . C41 C44 C49 121.5(2) . . C45 C44 C49 117.4(2) . . C44 C45 H45 119.3 . . C46 C45 C44 121.5(3) . . C46 C45 H45 119.3 . . C45 C46 H46 119.4 . . C45 C46 C47 121.1(2) . . C47 C46 H46 119.4 . . C48 C47 C46 117.0(2) . . C50 C47 C46 121.0(2) . . C50 C47 C48 122.0(2) . . C47 C48 H48 119.2 . . C49 C48 C47 121.6(3) . . C49 C48 H48 119.2 . . C44 C49 H49 119.3 . . C48 C49 C44 121.4(2) . . C48 C49 H49 119.3 . . C47 C50 C51 123.2(2) . . C47 C50 C52 120.6(3) . . C52 C50 C51 115.9(2) . . N12 C51 C50 177.7(3) . . N11 C52 C50 178.9(3) . . C65 N17 C66 123.9(3) . . C65 N17 C67 120.9(4) . . C67 N17 C66 115.2(3) . . O1 C65 N17 120.1(5) . . O1 C65 H65 120.0 . . N17 C65 H65 120.0 . . N17 C66 H66A 109.5 . . N17 C66 H66B 109.5 . . N17 C66 H66C 109.5 . . H66A C66 H66B 109.5 . . H66A C66 H66C 109.5 . . H66B C66 H66C 109.5 . . N17 C67 H67A 109.5 . . N17 C67 H67B 109.5 . . N17 C67 H67C 109.5 . . H67A C67 H67B 109.5 . . H67A C67 H67C 109.5 . . H67B C67 H67C 109.5 . . C68 O2 H2A 109.5 . . O2 C68 H68A 109.5 . . O2 C68 H68B 109.5 . . O2 C68 H68C 109.5 . . H68A C68 H68B 109.5 . . H68A C68 H68C 109.5 . . H68B C68 H68C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 N1 1.962(2) . Co1 N2 2.242(2) . Co1 N3 2.215(2) . Co1 N4 1.888(2) . Co1 N5 2.024(2) . Co1 N6 2.013(2) . N1 C1 1.358(3) . N1 C5 1.355(3) . N2 C11 1.338(3) . N2 C15 1.349(3) . N3 C6 1.345(3) . N3 C10 1.341(3) . N4 C21 1.351(3) . N4 C25 1.349(3) . N5 C31 1.350(3) . N5 C35 1.350(3) . N6 C26 1.370(3) . N6 C30 1.338(3) . N7 C18 1.327(3) . N7 C19 1.344(4) . N8 C38 1.339(3) . N8 C39 1.333(4) . C1 C2 1.383(3) . C1 C15 1.487(3) . C2 H2 0.9500 . C2 C3 1.392(3) . C3 C4 1.399(3) . C3 C16 1.485(3) . C4 H4 0.9500 . C4 C5 1.382(3) . C5 C6 1.492(3) . C6 C7 1.392(4) . C7 H7 0.9500 . C7 C8 1.392(4) . C8 H8 0.9500 . C8 C9 1.384(4) . C9 H9 0.9500 . C9 C10 1.377(4) . C10 H10 0.9500 . C11 H11 0.9500 . C11 C12 1.388(3) . C12 H12 0.9500 . C12 C13 1.379(4) . C13 H13 0.9500 . C13 C14 1.388(4) . C14 H14 0.9500 . C14 C15 1.383(3) . C16 C17 1.396(3) . C16 C20 1.390(4) . C17 H17 0.9500 . C17 C18 1.377(3) . C18 H18 0.9500 . C19 H19 0.9500 . C19 C20 1.372(4) . C20 H20 0.9500 . C21 C22 1.386(3) . C21 C35 1.478(3) . C22 H22 0.9500 . C22 C23 1.396(3) . C23 C24 1.393(3) . C23 C36 1.487(3) . C24 H24 0.9500 . C24 C25 1.388(3) . C25 C26 1.461(4) . C26 C27 1.386(3) . C27 H27 0.9500 . C27 C28 1.396(4) . C28 H28 0.9500 . C28 C29 1.380(4) . C29 H29 0.9500 . C29 C30 1.384(4) . C30 H30 0.9500 . C31 H31 0.9500 . C31 C32 1.385(4) . C32 H32 0.9500 . C32 C33 1.374(4) . C33 H33 0.9500 . C33 C34 1.387(3) . C34 H34 0.9500 . C34 C35 1.385(3) . C36 C37 1.389(4) . C36 C40 1.397(3) . C37 H37 0.9500 . C37 C38 1.378(4) . C38 H38 0.9500 . C39 H39 0.9500 . C39 C40 1.380(4) . C40 H40 0.9500 . N13 C55 1.154(3) . N14 C54 1.163(3) . N15 C63 1.156(3) . N16 C64 1.149(3) . C53 C54 1.413(4) . C53 C55 1.418(3) . C53 C56 1.413(3) . C56 C57 1.437(3) . C56 C61 1.410(4) . C57 H57 0.9500 . C57 C58 1.369(3) . C58 H58 0.9500 . C58 C59 1.418(4) . C59 C60 1.421(3) . C59 C62 1.416(3) . C60 H60 0.9500 . C60 C61 1.366(3) . C61 H61 0.9500 . C62 C63 1.409(4) . C62 C64 1.420(3) . N9 C43 1.146(4) . N10 C42 1.162(4) . N11 C52 1.154(4) . N12 C51 1.154(4) . C41 C42 1.416(4) . C41 C43 1.425(4) . C41 C44 1.417(4) . C44 C45 1.420(4) . C44 C49 1.421(4) . C45 H45 0.9500 . C45 C46 1.362(4) . C46 H46 0.9500 . C46 C47 1.437(4) . C47 C48 1.417(4) . C47 C50 1.406(4) . C48 H48 0.9500 . C48 C49 1.364(4) . C49 H49 0.9500 . C50 C51 1.425(4) . C50 C52 1.422(4) . O1 C65 1.208(5) . N17 C65 1.374(5) . N17 C66 1.498(5) . N17 C67 1.465(4) . C65 H65 0.9500 . C66 H66A 0.9800 . C66 H66B 0.9800 . C66 H66C 0.9800 . C67 H67A 0.9800 . C67 H67B 0.9800 . C67 H67C 0.9800 . O2 H2A 0.8400 . O2 C68 1.369(4) . C68 H68A 0.9800 . C68 H68B 0.9800 . C68 H68C 0.9800 .