#------------------------------------------------------------------------------ #$Date: 2019-10-07 12:55:59 +0300 (Mon, 07 Oct 2019) $ #$Revision: 219132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234433.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_7234433 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), C2 H3 N, C H4 O' _chemical_formula_sum 'C67 H43 Co N17 O' _chemical_formula_weight 1161.11 _chemical_name_common Co(pyterpy)2(TCNQ)2_MeCN_MeOH _chemical_name_systematic ; Cobalt(II) bis-(4?-(4???-pyridyl)- 2,2?:6?,2??-terpyridine) tetracyanoquinodimethane acetonitrile 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 76.313(4) _cell_angle_beta 81.950(4) _cell_angle_gamma 87.007(4) _cell_formula_units_Z 2 _cell_length_a 8.939(3) _cell_length_b 13.632(5) _cell_length_c 24.204(8) _cell_measurement_reflns_used 6741 _cell_measurement_temperature 110.15 _cell_measurement_theta_max 26.09 _cell_measurement_theta_min 2.30 _cell_volume 2836.9(17) _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 0.907 _diffrn_measured_fraction_theta_max 0.997 _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 0.1068 _diffrn_reflns_av_unetI/netI 0.0951 _diffrn_reflns_Laue_measured_fraction_full 0.907 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 26219 _diffrn_reflns_point_group_measured_fraction_full 0.907 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.405 _diffrn_reflns_theta_min 1.538 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.365 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0860 before and 0.0520 after correction. The Ratio of minimum to maximum transmission is 0.8928. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.359 _exptl_crystal_description plate _exptl_crystal_F_000 1198 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.502 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 778 _refine_ls_number_reflns 9330 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0502 _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^)+(0.0390P)^2^+1.0912P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1186 _refine_ls_wR_factor_ref 0.1254 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7146 _reflns_number_total 9330 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-9292.cif _cod_data_source_block p-1_a _cod_original_cell_volume 2836.8(16) _cod_database_code 7234433 _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 0.993 _shelx_estimated_absorpt_t_min 0.880 _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) 2.b Idealised Me refined as rotating group: C66(H66A,H66B,H66C), C67(H67A,H67B,H67C) 2.c Idealised tetrahedral OH refined as rotating group: O1(H1) ; _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 0.105, Rweak 0.009, Alpha 0.045, Orientation as input REM Formula found by SHELXT: C70 N15 Co CELL 0.71073 8.9389 13.6323 24.2035 76.313 81.95 87.007 ZERR 2 0.003 0.0045 0.008 0.004 0.004 0.004 LATT 1 SFAC C H Co N O UNIT 134 86 2 34 2 L.S. 10 PLAN 10 SIZE 0.02 0.16 0.36 TEMP -163 BOND $H LIST 6 fmap 2 acta OMIT 2 6 4 OMIT -2 5 4 REM REM REM WGHT 0.039000 1.091200 FVAR 0.27721 CO1 3 0.121458 0.690461 0.239164 11.00000 0.01624 0.01060 = 0.00795 -0.00029 -0.00077 -0.00361 N1 4 0.156258 0.753109 0.161564 11.00000 0.01099 0.01451 = 0.01286 -0.00701 -0.00561 -0.00132 N2 4 0.021747 0.823479 0.242328 11.00000 0.01379 0.01592 = 0.00754 0.00151 -0.00082 -0.00658 N3 4 0.232722 0.577245 0.211181 11.00000 0.01497 0.01115 = 0.00966 0.00043 -0.00223 -0.00489 N4 4 0.109099 0.621955 0.319104 11.00000 0.00951 0.01485 = 0.01418 -0.00756 0.00050 -0.00260 N5 4 0.325822 0.742706 0.263094 11.00000 0.01582 0.01307 = 0.01060 0.00108 -0.00024 -0.00459 N6 4 -0.095769 0.617134 0.254618 11.00000 0.01696 0.01232 = 0.01013 -0.00192 -0.00241 -0.00132 N7 4 0.449255 1.019414 -0.117272 11.00000 0.04093 0.01631 = 0.01783 -0.00317 0.00441 -0.00561 N8 4 0.181458 0.279226 0.586258 11.00000 0.02610 0.02176 = 0.01462 -0.00154 0.00116 -0.00191 C1 1 0.243141 0.705232 0.125196 11.00000 0.01218 0.01321 = 0.01332 -0.00397 -0.00360 -0.00537 C2 1 0.291679 0.754862 0.068879 11.00000 0.01507 0.01316 = 0.01009 -0.00416 -0.00029 -0.00311 AFIX 43 H2 2 0.350889 0.719846 0.043630 11.00000 -1.20000 AFIX 0 C3 1 0.253013 0.855820 0.049856 11.00000 0.01382 0.01362 = 0.01188 -0.00194 -0.00327 -0.00245 C4 1 0.160724 0.904829 0.087322 11.00000 0.01565 0.01063 = 0.01315 -0.00021 -0.00404 -0.00184 AFIX 43 H4 2 0.129586 0.973245 0.074706 11.00000 -1.20000 AFIX 0 C5 1 0.115571 0.851523 0.143275 11.00000 0.01384 0.01281 = 0.01135 -0.00248 -0.00273 -0.00308 C6 1 0.034001 0.892655 0.190439 11.00000 0.01442 0.01420 = 0.01274 -0.00144 -0.00083 -0.00488 C7 1 -0.021317 0.989928 0.185213 11.00000 0.02081 0.01649 = 0.01484 -0.00135 0.00005 -0.00265 AFIX 43 H7 2 -0.012235 1.036056 0.148780 11.00000 -1.20000 AFIX 0 C8 1 -0.090927 1.020314 0.233897 11.00000 0.01881 0.01350 = 0.02460 -0.00620 0.00080 -0.00064 AFIX 43 H8 2 -0.127963 1.087631 0.231296 11.00000 -1.20000 AFIX 0 C9 1 -0.104957 0.950613 0.285963 11.00000 0.01887 0.02100 = 0.01454 -0.00690 0.00264 -0.00347 AFIX 43 H9 2 -0.153907 0.968955 0.319614 11.00000 -1.20000 AFIX 0 C10 1 -0.046752 0.853530 0.288547 11.00000 0.01747 0.02015 = 0.01033 -0.00228 0.00128 -0.00824 AFIX 43 H10 2 -0.055874 0.806372 0.324630 11.00000 -1.20000 AFIX 0 C11 1 0.269735 0.484924 0.241271 11.00000 0.01968 0.01406 = 0.01221 0.00090 -0.00336 -0.00635 AFIX 43 H11 2 0.230126 0.465627 0.280722 11.00000 -1.20000 AFIX 0 C12 1 0.362690 0.416551 0.217647 11.00000 0.02489 0.00959 = 0.01764 -0.00113 -0.00577 -0.00202 AFIX 43 H12 2 0.386274 0.352280 0.240523 11.00000 -1.20000 AFIX 0 C13 1 0.420563 0.443734 0.160026 11.00000 0.02074 0.01417 = 0.01876 -0.00818 -0.00539 0.00011 AFIX 43 H13 2 0.486099 0.398930 0.142900 11.00000 -1.20000 AFIX 0 C14 1 0.381063 0.537494 0.127846 11.00000 0.01591 0.01322 = 0.01407 -0.00425 -0.00191 -0.00336 AFIX 43 H14 2 0.418134 0.557147 0.088161 11.00000 -1.20000 AFIX 0 C15 1 0.287398 0.602248 0.153836 11.00000 0.01338 0.01176 = 0.01093 -0.00189 -0.00385 -0.00585 C16 1 0.318382 0.912775 -0.008110 11.00000 0.02023 0.01244 = 0.01117 -0.00410 0.00050 -0.00507 C17 1 0.465566 0.891704 -0.030566 11.00000 0.02181 0.01448 = 0.01729 -0.00326 0.00088 -0.00495 AFIX 43 H17 2 0.524956 0.840861 -0.009008 11.00000 -1.20000 AFIX 0 C18 1 0.524647 0.945671 -0.084725 11.00000 0.02564 0.01687 = 0.02325 -0.00690 0.00928 -0.00646 AFIX 43 H18 2 0.624486 0.929236 -0.099522 11.00000 -1.20000 AFIX 0 C19 1 0.308392 1.039722 -0.094900 11.00000 0.03570 0.01380 = 0.01401 0.00139 -0.00433 -0.00348 AFIX 43 H19 2 0.252583 1.091973 -0.117133 11.00000 -1.20000 AFIX 0 C20 1 0.238783 0.989873 -0.041716 11.00000 0.02430 0.01023 = 0.01396 -0.00219 -0.00154 -0.00203 AFIX 43 H20 2 0.138479 1.007753 -0.028248 11.00000 -1.20000 AFIX 0 C21 1 0.222954 0.629848 0.349451 11.00000 0.01325 0.01424 = 0.01122 -0.00330 0.00084 -0.00419 C22 1 0.235120 0.565945 0.402328 11.00000 0.01737 0.01926 = 0.01184 -0.00162 -0.00342 -0.00632 AFIX 43 H22 2 0.314784 0.574341 0.422887 11.00000 -1.20000 AFIX 0 C23 1 0.131844 0.489451 0.425739 11.00000 0.01878 0.01271 = 0.00849 -0.00151 0.00068 -0.00062 C24 1 0.013230 0.482917 0.394672 11.00000 0.01571 0.01016 = 0.01546 0.00020 0.00166 -0.00486 AFIX 43 H24 2 -0.060949 0.432639 0.409470 11.00000 -1.20000 AFIX 0 C25 1 0.004348 0.549837 0.342398 11.00000 0.01436 0.01250 = 0.00945 -0.00221 0.00206 -0.00281 C26 1 -0.118212 0.551802 0.306630 11.00000 0.01577 0.01478 = 0.01362 -0.00041 -0.00067 -0.00362 C27 1 -0.246879 0.494197 0.324597 11.00000 0.02536 0.03272 = 0.01877 0.00480 -0.00627 -0.01402 AFIX 43 H27 2 -0.258474 0.447146 0.360714 11.00000 -1.20000 AFIX 0 C28 1 -0.358588 0.506509 0.288833 11.00000 0.02238 0.03609 = 0.02709 0.00062 -0.00389 -0.01628 AFIX 43 H28 2 -0.448203 0.468322 0.300235 11.00000 -1.20000 AFIX 0 C29 1 -0.337387 0.575100 0.236456 11.00000 0.02205 0.03365 = 0.01903 -0.00275 -0.00890 -0.00866 AFIX 43 H29 2 -0.412841 0.585427 0.211531 11.00000 -1.20000 AFIX 0 C30 1 -0.204999 0.628466 0.220814 11.00000 0.02038 0.01708 = 0.01345 -0.00054 -0.00443 -0.00381 AFIX 43 H30 2 -0.190802 0.675127 0.184598 11.00000 -1.20000 AFIX 0 C31 1 0.424377 0.813027 0.232647 11.00000 0.02017 0.01830 = 0.01075 0.00050 0.00178 -0.00697 AFIX 43 H31 2 0.420261 0.837100 0.192698 11.00000 -1.20000 AFIX 0 C32 1 0.531789 0.851654 0.257478 11.00000 0.02186 0.02508 = 0.02006 -0.00037 0.00039 -0.01368 AFIX 43 H32 2 0.601680 0.899976 0.234723 11.00000 -1.20000 AFIX 0 C33 1 0.535493 0.818709 0.315858 11.00000 0.02532 0.02696 = 0.02007 -0.00244 -0.00406 -0.01333 AFIX 43 H33 2 0.607031 0.844775 0.333942 11.00000 -1.20000 AFIX 0 C34 1 0.433722 0.747398 0.347465 11.00000 0.02166 0.01980 = 0.01498 -0.00051 -0.00450 -0.00889 AFIX 43 H34 2 0.433305 0.724555 0.387736 11.00000 -1.20000 AFIX 0 C35 1 0.332453 0.709537 0.319999 11.00000 0.01403 0.01082 = 0.01171 0.00029 0.00005 -0.00175 C36 1 0.148571 0.416054 0.480823 11.00000 0.01764 0.01370 = 0.00919 -0.00191 0.00225 -0.00059 C37 1 0.257615 0.428205 0.514526 11.00000 0.02152 0.01748 = 0.01326 0.00024 -0.00090 -0.00499 AFIX 43 H37 2 0.324021 0.483619 0.502264 11.00000 -1.20000 AFIX 0 C38 1 0.268398 0.359433 0.565642 11.00000 0.02429 0.02522 = 0.01384 -0.00259 -0.00379 -0.00005 AFIX 43 H38 2 0.343247 0.369977 0.587786 11.00000 -1.20000 AFIX 0 C39 1 0.077606 0.267422 0.553611 11.00000 0.03343 0.01969 = 0.01545 0.00321 0.00009 -0.01023 AFIX 43 H39 2 0.013945 0.210677 0.566848 11.00000 -1.20000 AFIX 0 C40 1 0.057083 0.332743 0.501724 11.00000 0.02342 0.02552 = 0.01418 0.00041 -0.00395 -0.00754 AFIX 43 H40 2 -0.019146 0.320523 0.480622 11.00000 -1.20000 AFIX 0 N13 4 0.344784 0.328686 0.360873 11.00000 0.03137 0.02516 = 0.02538 0.00135 -0.00205 -0.00414 N14 4 0.676422 0.341202 0.474702 11.00000 0.03470 0.02019 = 0.03409 -0.00353 -0.00348 -0.00817 N15 4 0.032987 -0.218840 0.596368 11.00000 0.03794 0.03294 = 0.03792 -0.00546 0.00080 -0.01604 N16 4 0.377373 -0.187573 0.701495 11.00000 0.04816 0.03266 = 0.02397 -0.00047 -0.00303 -0.00605 C53 1 0.464516 0.241846 0.451536 11.00000 0.02005 0.01224 = 0.01702 -0.00363 -0.00071 -0.00177 C54 1 0.397066 0.289207 0.401613 11.00000 0.02167 0.01163 = 0.02186 -0.00197 0.00334 -0.00338 C55 1 0.582550 0.296562 0.463559 11.00000 0.02623 0.01424 = 0.02034 -0.00057 0.00197 -0.00209 C56 1 0.412017 0.151778 0.489788 11.00000 0.01736 0.01508 = 0.01722 -0.00604 0.00087 -0.00161 C57 1 0.282026 0.102323 0.483175 11.00000 0.01960 0.01618 = 0.01915 -0.00445 -0.00196 0.00042 AFIX 43 H57 2 0.227764 0.130553 0.451881 11.00000 -1.20000 AFIX 0 C58 1 0.233436 0.015374 0.520673 11.00000 0.01931 0.01751 = 0.01811 -0.00466 -0.00167 -0.00554 AFIX 43 H58 2 0.146427 -0.015882 0.514708 11.00000 -1.20000 AFIX 0 C59 1 0.309477 -0.030091 0.568648 11.00000 0.01953 0.01755 = 0.01762 -0.00852 0.00416 -0.00391 C60 1 0.438386 0.019957 0.575479 11.00000 0.02035 0.01998 = 0.01568 -0.00415 -0.00337 0.00129 AFIX 43 H60 2 0.491547 -0.007681 0.607163 11.00000 -1.20000 AFIX 0 C61 1 0.488087 0.106659 0.537808 11.00000 0.01868 0.01573 = 0.02120 -0.00838 -0.00223 -0.00197 AFIX 43 H61 2 0.575383 0.137712 0.543688 11.00000 -1.20000 AFIX 0 C62 1 0.260745 -0.120657 0.607700 11.00000 0.02326 0.01680 = 0.01489 -0.00282 0.00273 -0.00527 C63 1 0.135321 -0.175220 0.601382 11.00000 0.02787 0.01947 = 0.02014 -0.00117 0.00354 -0.00494 C64 1 0.326397 -0.158724 0.658966 11.00000 0.02988 0.01842 = 0.01780 -0.00283 0.00783 -0.00964 N9 4 0.609344 0.720050 0.104861 11.00000 0.02298 0.01806 = 0.02109 -0.00155 -0.00343 -0.00040 N10 4 0.946314 0.857154 -0.042499 11.00000 0.03126 0.01388 = 0.02252 -0.00220 -0.00238 -0.00052 N11 4 1.166023 0.196332 0.163581 11.00000 0.03386 0.02521 = 0.02880 0.00047 -0.00511 -0.00507 N12 4 1.495017 0.357863 0.022496 11.00000 0.02430 0.02079 = 0.02313 -0.00672 -0.00026 -0.00338 C41 1 0.856153 0.703396 0.038245 11.00000 0.02017 0.01224 = 0.01483 -0.00330 -0.00212 -0.00272 C42 1 0.718526 0.713825 0.074012 11.00000 0.02210 0.01067 = 0.01772 -0.00299 -0.00829 -0.00095 C43 1 0.904036 0.788182 -0.006288 11.00000 0.01790 0.01613 = 0.01879 -0.00801 -0.00433 0.00143 C44 1 0.946697 0.613753 0.048296 11.00000 0.01894 0.01293 = 0.01447 -0.00589 -0.00454 -0.00389 C45 1 0.902145 0.528445 0.093881 11.00000 0.01591 0.01717 = 0.01403 -0.00576 0.00108 -0.00325 AFIX 43 H45 2 0.808909 0.531210 0.117774 11.00000 -1.20000 AFIX 0 C46 1 0.990771 0.443238 0.103738 11.00000 0.02004 0.01280 = 0.01236 -0.00077 -0.00242 -0.00250 AFIX 43 H46 2 0.958127 0.387782 0.134329 11.00000 -1.20000 AFIX 0 C47 1 1.131468 0.435908 0.068970 11.00000 0.01722 0.01436 = 0.01497 -0.00583 -0.00428 -0.00447 C48 1 1.175052 0.521165 0.023503 11.00000 0.01650 0.01409 = 0.01379 -0.00352 -0.00039 -0.00446 AFIX 43 H48 2 1.267869 0.518532 -0.000655 11.00000 -1.20000 AFIX 0 C49 1 1.086461 0.606189 0.014008 11.00000 0.01870 0.01420 = 0.01142 -0.00311 -0.00065 -0.00667 AFIX 43 H49 2 1.119397 0.661822 -0.016420 11.00000 -1.20000 AFIX 0 C50 1 1.227686 0.349632 0.079335 11.00000 0.01587 0.01544 = 0.01215 -0.00364 0.00048 -0.00527 C51 1 1.193454 0.265047 0.125651 11.00000 0.02013 0.01609 = 0.02266 -0.00757 -0.00562 0.00157 C52 1 1.374810 0.351707 0.047626 11.00000 0.02247 0.01054 = 0.01667 -0.00480 -0.00573 -0.00081 N17 4 1.179961 -0.057898 0.380399 11.00000 0.06399 0.05594 = 0.05862 0.00008 -0.02035 -0.02285 C65 1 1.203334 0.017580 0.348154 11.00000 0.03621 0.04563 = 0.03567 -0.00842 -0.01254 -0.01227 C66 1 1.234263 0.113361 0.307084 11.00000 0.05375 0.05147 = 0.03851 -0.00151 -0.00926 -0.01635 AFIX 137 H66A 2 1.197662 0.111845 0.270980 11.00000 -1.50000 H66B 2 1.343386 0.124535 0.300083 11.00000 -1.50000 H66C 2 1.182578 0.168233 0.322520 11.00000 -1.50000 AFIX 0 O1 5 0.707185 0.281434 0.176528 11.00000 0.08790 0.07933 = 0.04857 -0.00781 -0.00128 -0.00953 AFIX 147 H1 2 0.681282 0.257360 0.211674 11.00000 -1.50000 AFIX 0 C67 1 0.678315 0.210965 0.145170 11.00000 0.21130 0.08123 = 0.08996 -0.05706 -0.10430 0.06745 AFIX 137 H67A 2 0.697587 0.241872 0.104013 11.00000 -1.50000 H67B 2 0.572612 0.190587 0.155321 11.00000 -1.50000 H67C 2 0.744696 0.151497 0.154399 11.00000 -1.50000 AFIX 0 HKLF 4 REM P-1_a.res in P-1 REM R1 = 0.0502 for 7146 Fo > 4sig(Fo) and 0.0676 for all 9330 data REM 778 parameters refined using 0 restraints END WGHT 0.0390 1.0818 REM Highest difference peak 0.502, deepest hole -0.511, 1-sigma level 0.066 Q1 1 -0.0040 0.6904 0.2496 11.00000 0.05 0.50 Q2 1 0.2551 0.6735 0.2289 11.00000 0.05 0.49 Q3 1 0.0449 0.7629 0.2342 11.00000 0.05 0.49 Q4 1 0.1382 0.7033 0.1908 11.00000 0.05 0.43 Q5 1 0.1957 0.6041 0.2490 11.00000 0.05 0.43 Q6 1 0.0944 0.6813 0.2912 11.00000 0.05 0.40 Q7 1 0.0893 0.8675 0.2210 11.00000 0.05 0.34 Q8 1 0.2771 0.6543 0.1381 11.00000 0.05 0.33 Q9 1 0.2160 0.7375 0.1522 11.00000 0.05 0.31 Q10 1 0.1349 0.6402 0.3377 11.00000 0.05 0.31 ; _shelx_res_checksum 6538 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 0.12146(4) 0.69046(3) 0.23916(2) 0.01187(12) Uani 1 1 d . . . . . N1 N 0.1563(2) 0.75311(18) 0.16156(10) 0.0117(5) Uani 1 1 d . . . . . N2 N 0.0217(2) 0.82348(18) 0.24233(9) 0.0130(5) Uani 1 1 d . . . . . N3 N 0.2327(3) 0.57725(18) 0.21118(10) 0.0122(5) Uani 1 1 d . . . . . N4 N 0.1091(2) 0.62195(18) 0.31910(10) 0.0123(5) Uani 1 1 d . . . . . N5 N 0.3258(3) 0.74271(18) 0.26309(10) 0.0138(5) Uani 1 1 d . . . . . N6 N -0.0958(3) 0.61713(18) 0.25462(10) 0.0132(5) Uani 1 1 d . . . . . N7 N 0.4493(3) 1.0194(2) -0.11727(11) 0.0258(7) Uani 1 1 d . . . . . N8 N 0.1815(3) 0.2792(2) 0.58626(10) 0.0216(6) Uani 1 1 d . . . . . C1 C 0.2431(3) 0.7052(2) 0.12520(12) 0.0124(6) Uani 1 1 d . . . . . C2 C 0.2917(3) 0.7549(2) 0.06888(12) 0.0126(6) Uani 1 1 d . . . . . H2 H 0.3509 0.7198 0.0436 0.015 Uiso 1 1 calc R . . . . C3 C 0.2530(3) 0.8558(2) 0.04986(12) 0.0130(6) Uani 1 1 d . . . . . C4 C 0.1607(3) 0.9048(2) 0.08732(12) 0.0133(6) Uani 1 1 d . . . . . H4 H 0.1296 0.9732 0.0747 0.016 Uiso 1 1 calc R . . . . C5 C 0.1156(3) 0.8515(2) 0.14328(12) 0.0125(6) Uani 1 1 d . . . . . C6 C 0.0340(3) 0.8927(2) 0.19044(12) 0.0140(7) Uani 1 1 d . . . . . C7 C -0.0213(3) 0.9899(2) 0.18521(13) 0.0179(7) Uani 1 1 d . . . . . H7 H -0.0122 1.0361 0.1488 0.022 Uiso 1 1 calc R . . . . C8 C -0.0909(3) 1.0203(2) 0.23390(13) 0.0190(7) Uani 1 1 d . . . . . H8 H -0.1280 1.0876 0.2313 0.023 Uiso 1 1 calc R . . . . C9 C -0.1050(3) 0.9506(2) 0.28596(13) 0.0180(7) Uani 1 1 d . . . . . H9 H -0.1539 0.9690 0.3196 0.022 Uiso 1 1 calc R . . . . C10 C -0.0468(3) 0.8535(2) 0.28855(12) 0.0162(7) Uani 1 1 d . . . . . H10 H -0.0559 0.8064 0.3246 0.019 Uiso 1 1 calc R . . . . C11 C 0.2697(3) 0.4849(2) 0.24127(13) 0.0156(7) Uani 1 1 d . . . . . H11 H 0.2301 0.4656 0.2807 0.019 Uiso 1 1 calc R . . . . C12 C 0.3627(3) 0.4166(2) 0.21765(13) 0.0174(7) Uani 1 1 d . . . . . H12 H 0.3863 0.3523 0.2405 0.021 Uiso 1 1 calc R . . . . C13 C 0.4206(3) 0.4437(2) 0.16003(13) 0.0169(7) Uani 1 1 d . . . . . H13 H 0.4861 0.3989 0.1429 0.020 Uiso 1 1 calc R . . . . C14 C 0.3811(3) 0.5375(2) 0.12785(12) 0.0141(7) Uani 1 1 d . . . . . H14 H 0.4181 0.5571 0.0882 0.017 Uiso 1 1 calc R . . . . C15 C 0.2874(3) 0.6022(2) 0.15384(12) 0.0117(6) Uani 1 1 d . . . . . C16 C 0.3184(3) 0.9128(2) -0.00811(12) 0.0145(7) Uani 1 1 d . . . . . C17 C 0.4656(3) 0.8917(2) -0.03057(13) 0.0181(7) Uani 1 1 d . . . . . H17 H 0.5250 0.8409 -0.0090 0.022 Uiso 1 1 calc R . . . . C18 C 0.5246(4) 0.9457(2) -0.08472(13) 0.0225(8) Uani 1 1 d . . . . . H18 H 0.6245 0.9292 -0.0995 0.027 Uiso 1 1 calc R . . . . C19 C 0.3084(4) 1.0397(2) -0.09490(13) 0.0217(7) Uani 1 1 d . . . . . H19 H 0.2526 1.0920 -0.1171 0.026 Uiso 1 1 calc R . . . . C20 C 0.2388(3) 0.9899(2) -0.04172(12) 0.0163(7) Uani 1 1 d . . . . . H20 H 0.1385 1.0078 -0.0282 0.020 Uiso 1 1 calc R . . . . C21 C 0.2230(3) 0.6298(2) 0.34945(12) 0.0129(6) Uani 1 1 d . . . . . C22 C 0.2351(3) 0.5659(2) 0.40233(12) 0.0161(7) Uani 1 1 d . . . . . H22 H 0.3148 0.5743 0.4229 0.019 Uiso 1 1 calc R . . . . C23 C 0.1318(3) 0.4895(2) 0.42574(12) 0.0137(7) Uani 1 1 d . . . . . C24 C 0.0132(3) 0.4829(2) 0.39467(12) 0.0145(7) Uani 1 1 d . . . . . H24 H -0.0609 0.4326 0.4095 0.017 Uiso 1 1 calc R . . . . C25 C 0.0043(3) 0.5498(2) 0.34240(12) 0.0124(6) Uani 1 1 d . . . . . C26 C -0.1182(3) 0.5518(2) 0.30663(12) 0.0152(7) Uani 1 1 d . . . . . C27 C -0.2469(3) 0.4942(3) 0.32460(14) 0.0266(8) Uani 1 1 d . . . . . H27 H -0.2585 0.4471 0.3607 0.032 Uiso 1 1 calc R . . . . C28 C -0.3586(4) 0.5065(3) 0.28883(14) 0.0292(8) Uani 1 1 d . . . . . H28 H -0.4482 0.4683 0.3002 0.035 Uiso 1 1 calc R . . . . C29 C -0.3374(3) 0.5751(3) 0.23646(13) 0.0246(8) Uani 1 1 d . . . . . H29 H -0.4128 0.5854 0.2115 0.029 Uiso 1 1 calc R . . . . C30 C -0.2050(3) 0.6285(2) 0.22081(13) 0.0171(7) Uani 1 1 d . . . . . H30 H -0.1908 0.6751 0.1846 0.021 Uiso 1 1 calc R . . . . C31 C 0.4244(3) 0.8130(2) 0.23265(13) 0.0172(7) Uani 1 1 d . . . . . H31 H 0.4203 0.8371 0.1927 0.021 Uiso 1 1 calc R . . . . C32 C 0.5318(3) 0.8517(2) 0.25748(13) 0.0230(8) Uani 1 1 d . . . . . H32 H 0.6017 0.9000 0.2347 0.028 Uiso 1 1 calc R . . . . C33 C 0.5355(4) 0.8187(3) 0.31586(13) 0.0241(8) Uani 1 1 d . . . . . H33 H 0.6070 0.8448 0.3339 0.029 Uiso 1 1 calc R . . . . C34 C 0.4337(3) 0.7474(2) 0.34747(13) 0.0189(7) Uani 1 1 d . . . . . H34 H 0.4333 0.7246 0.3877 0.023 Uiso 1 1 calc R . . . . C35 C 0.3325(3) 0.7095(2) 0.32000(12) 0.0128(6) Uani 1 1 d . . . . . C36 C 0.1486(3) 0.4161(2) 0.48082(12) 0.0140(7) Uani 1 1 d . . . . . C37 C 0.2576(3) 0.4282(2) 0.51453(12) 0.0180(7) Uani 1 1 d . . . . . H37 H 0.3240 0.4836 0.5023 0.022 Uiso 1 1 calc R . . . . C38 C 0.2684(3) 0.3594(2) 0.56564(13) 0.0213(7) Uani 1 1 d . . . . . H38 H 0.3432 0.3700 0.5878 0.026 Uiso 1 1 calc R . . . . C39 C 0.0776(4) 0.2674(2) 0.55361(13) 0.0241(8) Uani 1 1 d . . . . . H39 H 0.0139 0.2107 0.5668 0.029 Uiso 1 1 calc R . . . . C40 C 0.0571(3) 0.3327(2) 0.50172(13) 0.0215(7) Uani 1 1 d . . . . . H40 H -0.0191 0.3205 0.4806 0.026 Uiso 1 1 calc R . . . . N13 N 0.3448(3) 0.3287(2) 0.36087(12) 0.0286(7) Uani 1 1 d . . . . . N14 N 0.6764(3) 0.3412(2) 0.47470(12) 0.0300(7) Uani 1 1 d . . . . . N15 N 0.0330(3) -0.2188(2) 0.59637(13) 0.0367(8) Uani 1 1 d . . . . . N16 N 0.3774(3) -0.1876(2) 0.70149(13) 0.0359(8) Uani 1 1 d . . . . . C53 C 0.4645(3) 0.2418(2) 0.45154(13) 0.0165(7) Uani 1 1 d . . . . . C54 C 0.3971(3) 0.2892(2) 0.40161(14) 0.0192(7) Uani 1 1 d . . . . . C55 C 0.5826(4) 0.2966(2) 0.46356(13) 0.0213(7) Uani 1 1 d . . . . . C56 C 0.4120(3) 0.1518(2) 0.48979(13) 0.0164(7) Uani 1 1 d . . . . . C57 C 0.2820(3) 0.1023(2) 0.48318(13) 0.0183(7) Uani 1 1 d . . . . . H57 H 0.2278 0.1306 0.4519 0.022 Uiso 1 1 calc R . . . . C58 C 0.2334(3) 0.0154(2) 0.52067(12) 0.0181(7) Uani 1 1 d . . . . . H58 H 0.1464 -0.0159 0.5147 0.022 Uiso 1 1 calc R . . . . C59 C 0.3095(3) -0.0301(2) 0.56865(13) 0.0180(7) Uani 1 1 d . . . . . C60 C 0.4384(3) 0.0200(2) 0.57548(13) 0.0186(7) Uani 1 1 d . . . . . H60 H 0.4915 -0.0077 0.6072 0.022 Uiso 1 1 calc R . . . . C61 C 0.4881(3) 0.1067(2) 0.53781(13) 0.0178(7) Uani 1 1 d . . . . . H61 H 0.5754 0.1377 0.5437 0.021 Uiso 1 1 calc R . . . . C62 C 0.2607(3) -0.1207(2) 0.60770(13) 0.0188(7) Uani 1 1 d . . . . . C63 C 0.1353(4) -0.1752(3) 0.60138(13) 0.0236(8) Uani 1 1 d . . . . . C64 C 0.3264(4) -0.1587(2) 0.65897(14) 0.0230(8) Uani 1 1 d . . . . . N9 N 0.6093(3) 0.7201(2) 0.10486(11) 0.0212(6) Uani 1 1 d . . . . . N10 N 0.9463(3) 0.8572(2) -0.04250(11) 0.0230(6) Uani 1 1 d . . . . . N11 N 1.1660(3) 0.1963(2) 0.16358(12) 0.0302(7) Uani 1 1 d . . . . . N12 N 1.4950(3) 0.3579(2) 0.02250(11) 0.0226(6) Uani 1 1 d . . . . . C41 C 0.8562(3) 0.7034(2) 0.03824(12) 0.0157(7) Uani 1 1 d . . . . . C42 C 0.7185(3) 0.7138(2) 0.07401(13) 0.0163(7) Uani 1 1 d . . . . . C43 C 0.9040(3) 0.7882(2) -0.00629(13) 0.0168(7) Uani 1 1 d . . . . . C44 C 0.9467(3) 0.6138(2) 0.04830(12) 0.0146(7) Uani 1 1 d . . . . . C45 C 0.9021(3) 0.5284(2) 0.09388(12) 0.0155(7) Uani 1 1 d . . . . . H45 H 0.8089 0.5312 0.1178 0.019 Uiso 1 1 calc R . . . . C46 C 0.9908(3) 0.4432(2) 0.10374(12) 0.0153(7) Uani 1 1 d . . . . . H46 H 0.9581 0.3878 0.1343 0.018 Uiso 1 1 calc R . . . . C47 C 1.1315(3) 0.4359(2) 0.06897(12) 0.0147(7) Uani 1 1 d . . . . . C48 C 1.1751(3) 0.5212(2) 0.02350(12) 0.0148(7) Uani 1 1 d . . . . . H48 H 1.2679 0.5185 -0.0007 0.018 Uiso 1 1 calc R . . . . C49 C 1.0865(3) 0.6062(2) 0.01401(12) 0.0147(7) Uani 1 1 d . . . . . H49 H 1.1194 0.6618 -0.0164 0.018 Uiso 1 1 calc R . . . . C50 C 1.2277(3) 0.3496(2) 0.07934(12) 0.0145(7) Uani 1 1 d . . . . . C51 C 1.1935(3) 0.2650(2) 0.12565(14) 0.0189(7) Uani 1 1 d . . . . . C52 C 1.3748(4) 0.3517(2) 0.04763(13) 0.0160(7) Uani 1 1 d . . . . . N17 N 1.1800(4) -0.0579(3) 0.38040(16) 0.0598(11) Uani 1 1 d . . . . . C65 C 1.2033(4) 0.0176(3) 0.34815(17) 0.0382(10) Uani 1 1 d . . . . . C66 C 1.2343(5) 0.1134(3) 0.30708(17) 0.0485(11) Uani 1 1 d . . . . . H66A H 1.1977 0.1118 0.2710 0.073 Uiso 1 1 calc GR . . . . H66B H 1.3434 0.1245 0.3001 0.073 Uiso 1 1 calc GR . . . . H66C H 1.1826 0.1682 0.3225 0.073 Uiso 1 1 calc GR . . . . O1 O 0.7072(4) 0.2814(3) 0.17653(13) 0.0736(10) Uani 1 1 d . . . . . H1 H 0.6813 0.2574 0.2117 0.110 Uiso 1 1 calc GR . . . . C67 C 0.6783(8) 0.2110(4) 0.1452(2) 0.116(3) Uani 1 1 d . . . . . H67A H 0.6976 0.2419 0.1040 0.173 Uiso 1 1 calc GR . . . . H67B H 0.5726 0.1906 0.1553 0.173 Uiso 1 1 calc GR . . . . H67C H 0.7447 0.1515 0.1544 0.173 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 0.0162(2) 0.0106(2) 0.0079(2) -0.00029(16) -0.00077(16) -0.00361(16) N1 0.0110(12) 0.0145(14) 0.0129(13) -0.0070(11) -0.0056(10) -0.0013(10) N2 0.0138(13) 0.0159(14) 0.0075(12) 0.0015(11) -0.0008(10) -0.0066(11) N3 0.0150(13) 0.0111(13) 0.0097(13) 0.0004(11) -0.0022(10) -0.0049(10) N4 0.0095(12) 0.0149(14) 0.0142(13) -0.0076(11) 0.0005(10) -0.0026(10) N5 0.0158(13) 0.0131(14) 0.0106(13) 0.0011(11) -0.0002(10) -0.0046(11) N6 0.0170(13) 0.0123(14) 0.0101(13) -0.0019(11) -0.0024(10) -0.0013(11) N7 0.0409(18) 0.0163(15) 0.0178(15) -0.0032(12) 0.0044(13) -0.0056(13) N8 0.0261(15) 0.0218(16) 0.0146(14) -0.0015(12) 0.0012(12) -0.0019(12) C1 0.0122(15) 0.0132(16) 0.0133(15) -0.0040(13) -0.0036(12) -0.0054(12) C2 0.0151(15) 0.0132(16) 0.0101(15) -0.0042(13) -0.0003(12) -0.0031(12) C3 0.0138(15) 0.0136(17) 0.0119(15) -0.0019(13) -0.0033(12) -0.0025(13) C4 0.0157(16) 0.0106(16) 0.0132(16) -0.0002(13) -0.0040(12) -0.0018(12) C5 0.0138(15) 0.0128(17) 0.0113(15) -0.0025(13) -0.0027(12) -0.0031(12) C6 0.0144(16) 0.0142(17) 0.0127(16) -0.0014(13) -0.0008(12) -0.0049(13) C7 0.0208(17) 0.0165(18) 0.0148(16) -0.0013(14) 0.0000(13) -0.0027(14) C8 0.0188(17) 0.0135(17) 0.0246(18) -0.0062(14) 0.0008(14) -0.0006(13) C9 0.0189(17) 0.0210(18) 0.0145(16) -0.0069(14) 0.0026(13) -0.0035(14) C10 0.0175(16) 0.0201(18) 0.0103(15) -0.0023(13) 0.0013(12) -0.0082(13) C11 0.0197(17) 0.0141(17) 0.0122(16) 0.0009(13) -0.0034(13) -0.0064(13) C12 0.0249(18) 0.0096(16) 0.0176(17) -0.0011(13) -0.0058(13) -0.0020(13) C13 0.0207(17) 0.0142(17) 0.0188(17) -0.0082(14) -0.0054(13) 0.0001(13) C14 0.0159(16) 0.0132(16) 0.0141(16) -0.0042(13) -0.0019(12) -0.0034(13) C15 0.0134(15) 0.0118(16) 0.0109(15) -0.0019(13) -0.0039(12) -0.0058(12) C16 0.0202(17) 0.0124(16) 0.0112(15) -0.0041(13) 0.0005(13) -0.0051(13) C17 0.0218(17) 0.0145(17) 0.0173(17) -0.0033(14) 0.0009(13) -0.0050(14) C18 0.0256(18) 0.0169(18) 0.0233(18) -0.0069(15) 0.0093(15) -0.0065(15) C19 0.036(2) 0.0138(17) 0.0140(17) 0.0014(14) -0.0043(15) -0.0035(15) C20 0.0243(17) 0.0102(16) 0.0140(16) -0.0022(13) -0.0015(13) -0.0020(13) C21 0.0133(15) 0.0142(16) 0.0112(15) -0.0033(13) 0.0008(12) -0.0042(12) C22 0.0174(16) 0.0193(17) 0.0118(16) -0.0016(13) -0.0034(12) -0.0063(13) C23 0.0188(16) 0.0127(16) 0.0085(15) -0.0015(13) 0.0007(12) -0.0006(13) C24 0.0157(16) 0.0102(16) 0.0155(16) 0.0002(13) 0.0017(12) -0.0049(12) C25 0.0144(15) 0.0125(16) 0.0094(15) -0.0022(12) 0.0021(12) -0.0028(12) C26 0.0158(16) 0.0148(17) 0.0136(16) -0.0004(13) -0.0007(12) -0.0036(13) C27 0.0254(19) 0.033(2) 0.0188(18) 0.0048(15) -0.0063(14) -0.0140(16) C28 0.0224(18) 0.036(2) 0.027(2) 0.0006(17) -0.0039(15) -0.0163(16) C29 0.0220(18) 0.034(2) 0.0190(18) -0.0027(16) -0.0089(14) -0.0087(15) C30 0.0204(17) 0.0171(17) 0.0135(16) -0.0005(13) -0.0044(13) -0.0038(14) C31 0.0202(17) 0.0183(18) 0.0107(15) 0.0005(13) 0.0018(13) -0.0070(14) C32 0.0219(18) 0.0251(19) 0.0201(18) -0.0004(15) 0.0004(14) -0.0137(15) C33 0.0253(18) 0.027(2) 0.0201(18) -0.0024(15) -0.0041(14) -0.0133(15) C34 0.0217(17) 0.0198(18) 0.0150(16) -0.0005(14) -0.0045(13) -0.0089(14) C35 0.0140(15) 0.0108(16) 0.0117(16) 0.0003(13) 0.0001(12) -0.0017(12) C36 0.0176(16) 0.0137(16) 0.0092(15) -0.0019(13) 0.0022(12) -0.0006(13) C37 0.0215(17) 0.0175(17) 0.0133(16) 0.0002(13) -0.0009(13) -0.0050(14) C38 0.0243(18) 0.0252(19) 0.0138(17) -0.0026(15) -0.0038(14) 0.0000(15) C39 0.033(2) 0.0197(19) 0.0154(17) 0.0032(14) 0.0001(15) -0.0102(15) C40 0.0234(18) 0.0255(19) 0.0142(17) 0.0004(14) -0.0040(13) -0.0075(15) N13 0.0314(17) 0.0252(17) 0.0254(17) 0.0014(14) -0.0021(13) -0.0041(13) N14 0.0347(17) 0.0202(16) 0.0341(18) -0.0035(14) -0.0035(14) -0.0082(14) N15 0.0379(19) 0.0329(19) 0.0379(19) -0.0055(15) 0.0008(15) -0.0160(16) N16 0.048(2) 0.0327(19) 0.0240(17) -0.0005(15) -0.0030(15) -0.0061(15) C53 0.0201(17) 0.0122(16) 0.0170(16) -0.0036(13) -0.0007(13) -0.0018(13) C54 0.0217(18) 0.0116(17) 0.0219(18) -0.0020(14) 0.0033(14) -0.0034(14) C55 0.0262(19) 0.0142(18) 0.0203(18) -0.0006(14) 0.0020(14) -0.0021(15) C56 0.0174(16) 0.0151(17) 0.0172(16) -0.0060(14) 0.0009(13) -0.0016(13) C57 0.0196(17) 0.0162(18) 0.0191(17) -0.0045(14) -0.0020(13) 0.0004(13) C58 0.0193(17) 0.0175(18) 0.0181(17) -0.0047(14) -0.0017(13) -0.0055(14) C59 0.0195(17) 0.0175(18) 0.0176(17) -0.0085(14) 0.0042(13) -0.0039(14) C60 0.0204(17) 0.0200(18) 0.0157(16) -0.0041(14) -0.0034(13) 0.0013(14) C61 0.0187(17) 0.0157(17) 0.0212(17) -0.0084(14) -0.0022(13) -0.0020(13) C62 0.0233(17) 0.0168(18) 0.0149(16) -0.0028(14) 0.0027(13) -0.0053(14) C63 0.0279(19) 0.0195(19) 0.0201(18) -0.0012(15) 0.0035(14) -0.0049(16) C64 0.0299(19) 0.0184(19) 0.0178(18) -0.0028(15) 0.0078(15) -0.0096(15) N9 0.0230(15) 0.0181(15) 0.0211(15) -0.0015(12) -0.0034(12) -0.0004(12) N10 0.0313(16) 0.0139(15) 0.0225(15) -0.0022(13) -0.0024(12) -0.0005(12) N11 0.0339(17) 0.0252(17) 0.0288(17) 0.0005(15) -0.0051(13) -0.0051(14) N12 0.0243(16) 0.0208(16) 0.0231(15) -0.0067(12) -0.0003(13) -0.0034(12) C41 0.0202(17) 0.0122(16) 0.0148(16) -0.0033(13) -0.0021(13) -0.0027(13) C42 0.0221(18) 0.0107(16) 0.0177(17) -0.0030(13) -0.0083(15) -0.0010(13) C43 0.0179(17) 0.0161(18) 0.0188(17) -0.0080(15) -0.0043(13) 0.0014(14) C44 0.0189(16) 0.0129(16) 0.0145(16) -0.0059(13) -0.0045(13) -0.0039(13) C45 0.0159(16) 0.0172(17) 0.0140(16) -0.0058(13) 0.0011(12) -0.0032(13) C46 0.0200(17) 0.0128(17) 0.0124(16) -0.0008(13) -0.0024(13) -0.0025(13) C47 0.0172(16) 0.0144(17) 0.0150(16) -0.0058(13) -0.0043(13) -0.0045(13) C48 0.0165(16) 0.0141(17) 0.0138(16) -0.0035(13) -0.0004(12) -0.0045(13) C49 0.0187(16) 0.0142(17) 0.0114(15) -0.0031(13) -0.0007(12) -0.0067(13) C50 0.0159(16) 0.0154(17) 0.0121(15) -0.0036(13) 0.0005(12) -0.0053(13) C51 0.0201(17) 0.0161(18) 0.0227(18) -0.0076(16) -0.0056(14) 0.0016(14) C52 0.0225(18) 0.0105(16) 0.0167(16) -0.0048(13) -0.0057(14) -0.0008(13) N17 0.064(3) 0.056(3) 0.059(3) 0.000(2) -0.020(2) -0.023(2) C65 0.036(2) 0.046(3) 0.036(2) -0.008(2) -0.0125(18) -0.012(2) C66 0.054(3) 0.051(3) 0.039(2) -0.002(2) -0.009(2) -0.016(2) O1 0.088(2) 0.079(3) 0.049(2) -0.0078(19) -0.0013(19) -0.010(2) C67 0.211(7) 0.081(4) 0.090(4) -0.057(4) -0.104(5) 0.067(5) 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 81.23(10) . . N1 Co1 N3 81.62(10) . . N1 Co1 N4 173.63(10) . . N1 Co1 N5 96.66(9) . . N1 Co1 N6 107.50(9) . . N2 Co1 N3 162.85(9) . . N2 Co1 N5 89.26(9) . . N2 Co1 N6 91.53(9) . . N3 Co1 N5 92.66(9) . . N3 Co1 N6 93.67(9) . . N4 Co1 N2 102.67(10) . . N4 Co1 N3 94.40(10) . . N4 Co1 N5 78.49(9) . . N4 Co1 N6 77.62(9) . . N6 Co1 N5 155.67(9) . . C1 N1 Co1 119.3(2) . . C1 N1 C5 119.9(2) . . C5 N1 Co1 119.96(19) . . C6 N2 Co1 114.12(19) . . C10 N2 Co1 127.9(2) . . C10 N2 C6 117.9(3) . . C11 N3 Co1 129.1(2) . . C11 N3 C15 117.3(2) . . C15 N3 Co1 113.49(18) . . C21 N4 Co1 119.97(18) . . C21 N4 C25 118.3(2) . . C25 N4 Co1 120.39(18) . . C31 N5 Co1 129.58(19) . . C31 N5 C35 118.2(2) . . C35 N5 Co1 111.15(17) . . C26 N6 Co1 112.38(18) . . C30 N6 Co1 129.4(2) . . C30 N6 C26 118.2(2) . . C18 N7 C19 116.1(3) . . C38 N8 C39 115.6(3) . . N1 C1 C2 121.2(3) . . N1 C1 C15 112.3(2) . . C2 C1 C15 126.3(3) . . C1 C2 H2 120.3 . . C3 C2 C1 119.5(3) . . C3 C2 H2 120.3 . . C2 C3 C4 119.2(3) . . C2 C3 C16 119.9(3) . . C4 C3 C16 120.7(3) . . C3 C4 H4 120.6 . . C5 C4 C3 118.9(3) . . C5 C4 H4 120.6 . . N1 C5 C4 121.3(3) . . N1 C5 C6 111.7(2) . . C4 C5 C6 126.8(3) . . N2 C6 C5 112.7(3) . . C7 C6 N2 122.0(3) . . C7 C6 C5 125.2(3) . . C6 C7 H7 120.3 . . C6 C7 C8 119.4(3) . . C8 C7 H7 120.3 . . C7 C8 H8 120.6 . . C9 C8 C7 118.7(3) . . C9 C8 H8 120.6 . . C8 C9 H9 120.4 . . C8 C9 C10 119.2(3) . . C10 C9 H9 120.4 . . N2 C10 C9 122.8(3) . . N2 C10 H10 118.6 . . C9 C10 H10 118.6 . . N3 C11 H11 118.3 . . N3 C11 C12 123.4(3) . . C12 C11 H11 118.3 . . C11 C12 H12 120.6 . . C13 C12 C11 118.8(3) . . C13 C12 H12 120.6 . . C12 C13 H13 120.6 . . C12 C13 C14 118.8(3) . . C14 C13 H13 120.6 . . C13 C14 H14 120.2 . . C15 C14 C13 119.7(3) . . C15 C14 H14 120.2 . . N3 C15 C1 113.0(2) . . N3 C15 C14 122.0(3) . . C14 C15 C1 124.9(3) . . C17 C16 C3 120.3(3) . . C17 C16 C20 117.1(3) . . C20 C16 C3 122.6(3) . . C16 C17 H17 120.3 . . C18 C17 C16 119.4(3) . . C18 C17 H17 120.3 . . N7 C18 C17 123.9(3) . . N7 C18 H18 118.1 . . C17 C18 H18 118.1 . . N7 C19 H19 117.7 . . N7 C19 C20 124.5(3) . . C20 C19 H19 117.7 . . C16 C20 H20 120.5 . . C19 C20 C16 118.9(3) . . C19 C20 H20 120.5 . . N4 C21 C22 121.7(3) . . N4 C21 C35 114.1(2) . . C22 C21 C35 124.2(3) . . C21 C22 H22 119.7 . . C21 C22 C23 120.6(3) . . C23 C22 H22 119.7 . . C22 C23 C24 117.3(3) . . C22 C23 C36 121.4(3) . . C24 C23 C36 121.3(3) . . C23 C24 H24 120.1 . . C25 C24 C23 119.9(3) . . C25 C24 H24 120.1 . . N4 C25 C24 122.2(3) . . N4 C25 C26 113.3(2) . . C24 C25 C26 124.5(3) . . N6 C26 C25 114.1(2) . . N6 C26 C27 122.1(3) . . C27 C26 C25 123.7(3) . . C26 C27 H27 120.6 . . C26 C27 C28 118.8(3) . . C28 C27 H27 120.6 . . C27 C28 H28 120.5 . . C29 C28 C27 119.0(3) . . C29 C28 H28 120.5 . . C28 C29 H29 120.5 . . C28 C29 C30 119.1(3) . . C30 C29 H29 120.5 . . N6 C30 C29 122.7(3) . . N6 C30 H30 118.7 . . C29 C30 H30 118.7 . . N5 C31 H31 118.8 . . N5 C31 C32 122.4(3) . . C32 C31 H31 118.8 . . C31 C32 H32 120.5 . . C33 C32 C31 118.9(3) . . C33 C32 H32 120.5 . . C32 C33 H33 120.5 . . C34 C33 C32 119.0(3) . . C34 C33 H33 120.5 . . C33 C34 H34 120.3 . . C33 C34 C35 119.4(3) . . C35 C34 H34 120.3 . . N5 C35 C21 114.2(2) . . N5 C35 C34 122.1(3) . . C34 C35 C21 123.7(3) . . C37 C36 C23 121.3(3) . . C40 C36 C23 122.3(3) . . C40 C36 C37 116.4(3) . . C36 C37 H37 120.2 . . C38 C37 C36 119.6(3) . . C38 C37 H37 120.2 . . N8 C38 C37 124.7(3) . . N8 C38 H38 117.7 . . C37 C38 H38 117.7 . . N8 C39 H39 117.9 . . N8 C39 C40 124.2(3) . . C40 C39 H39 117.9 . . C36 C40 H40 120.2 . . C39 C40 C36 119.6(3) . . C39 C40 H40 120.2 . . C55 C53 C54 115.3(3) . . C56 C53 C54 123.6(3) . . C56 C53 C55 120.9(3) . . N13 C54 C53 178.7(3) . . N14 C55 C53 178.2(3) . . C53 C56 C57 122.5(3) . . C53 C56 C61 120.6(3) . . C57 C56 C61 116.9(3) . . C56 C57 H57 119.3 . . C58 C57 C56 121.5(3) . . C58 C57 H57 119.3 . . C57 C58 H58 119.1 . . C57 C58 C59 121.8(3) . . C59 C58 H58 119.1 . . C60 C59 C58 116.6(3) . . C62 C59 C58 122.4(3) . . C62 C59 C60 121.0(3) . . C59 C60 H60 119.1 . . C61 C60 C59 121.8(3) . . C61 C60 H60 119.1 . . C56 C61 H61 119.3 . . C60 C61 C56 121.5(3) . . C60 C61 H61 119.3 . . C59 C62 C63 122.9(3) . . C59 C62 C64 121.7(3) . . C64 C62 C63 115.2(3) . . N15 C63 C62 179.5(4) . . N16 C64 C62 177.9(4) . . C43 C41 C42 117.4(3) . . C43 C41 C44 120.9(3) . . C44 C41 C42 121.6(3) . . N9 C42 C41 177.3(3) . . N10 C43 C41 178.6(3) . . C41 C44 C45 121.7(3) . . C49 C44 C41 121.0(3) . . C49 C44 C45 117.3(3) . . C44 C45 H45 119.3 . . C46 C45 C44 121.3(3) . . C46 C45 H45 119.3 . . C45 C46 H46 119.4 . . C45 C46 C47 121.2(3) . . C47 C46 H46 119.4 . . C46 C47 C48 117.2(3) . . C50 C47 C46 122.3(3) . . C50 C47 C48 120.5(3) . . C47 C48 H48 119.3 . . C49 C48 C47 121.4(3) . . C49 C48 H48 119.3 . . C44 C49 H49 119.2 . . C48 C49 C44 121.6(3) . . C48 C49 H49 119.2 . . C47 C50 C51 122.8(3) . . C47 C50 C52 119.6(3) . . C51 C50 C52 117.1(3) . . N11 C51 C50 179.6(4) . . N12 C52 C50 176.7(3) . . N17 C65 C66 179.6(5) . . C65 C66 H66A 109.5 . . C65 C66 H66B 109.5 . . C65 C66 H66C 109.5 . . H66A C66 H66B 109.5 . . H66A C66 H66C 109.5 . . H66B C66 H66C 109.5 . . C67 O1 H1 109.5 . . O1 C67 H67A 109.5 . . O1 C67 H67B 109.5 . . O1 C67 H67C 109.5 . . H67A C67 H67B 109.5 . . H67A C67 H67C 109.5 . . H67B C67 H67C 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 1.860(2) . Co1 N2 1.992(3) . Co1 N3 1.994(2) . Co1 N4 1.930(2) . Co1 N5 2.193(2) . Co1 N6 2.175(2) . N1 C1 1.353(4) . N1 C5 1.357(4) . N2 C6 1.375(4) . N2 C10 1.339(4) . N3 C11 1.347(4) . N3 C15 1.373(3) . N4 C21 1.358(4) . N4 C25 1.359(3) . N5 C31 1.345(3) . N5 C35 1.353(3) . N6 C26 1.355(4) . N6 C30 1.340(4) . N7 C18 1.337(4) . N7 C19 1.341(4) . N8 C38 1.331(4) . N8 C39 1.339(4) . C1 C2 1.390(4) . C1 C15 1.472(4) . C2 H2 0.9500 . C2 C3 1.386(4) . C3 C4 1.403(4) . C3 C16 1.488(4) . C4 H4 0.9500 . C4 C5 1.392(4) . C5 C6 1.475(4) . C6 C7 1.374(4) . C7 H7 0.9500 . C7 C8 1.395(4) . C8 H8 0.9500 . C8 C9 1.381(4) . C9 H9 0.9500 . C9 C10 1.387(4) . C10 H10 0.9500 . C11 H11 0.9500 . C11 C12 1.387(4) . C12 H12 0.9500 . C12 C13 1.387(4) . C13 H13 0.9500 . C13 C14 1.387(4) . C14 H14 0.9500 . C14 C15 1.384(4) . C16 C17 1.394(4) . C16 C20 1.397(4) . C17 H17 0.9500 . C17 C18 1.389(4) . C18 H18 0.9500 . C19 H19 0.9500 . C19 C20 1.383(4) . C20 H20 0.9500 . C21 C22 1.382(4) . C21 C35 1.482(4) . C22 H22 0.9500 . C22 C23 1.391(4) . C23 C24 1.401(4) . C23 C36 1.487(4) . C24 H24 0.9500 . C24 C25 1.383(4) . C25 C26 1.484(4) . C26 C27 1.386(4) . C27 H27 0.9500 . C27 C28 1.389(4) . C28 H28 0.9500 . C28 C29 1.381(4) . C29 H29 0.9500 . C29 C30 1.381(4) . C30 H30 0.9500 . C31 H31 0.9500 . C31 C32 1.387(4) . C32 H32 0.9500 . C32 C33 1.382(4) . C33 H33 0.9500 . C33 C34 1.380(4) . C34 H34 0.9500 . C34 C35 1.381(4) . C36 C37 1.395(4) . C36 C40 1.387(4) . C37 H37 0.9500 . C37 C38 1.376(4) . C38 H38 0.9500 . C39 H39 0.9500 . C39 C40 1.386(4) . C40 H40 0.9500 . N13 C54 1.154(4) . N14 C55 1.158(4) . N15 C63 1.152(4) . N16 C64 1.159(4) . C53 C54 1.426(4) . C53 C55 1.423(4) . C53 C56 1.409(4) . C56 C57 1.420(4) . C56 C61 1.425(4) . C57 H57 0.9500 . C57 C58 1.361(4) . C58 H58 0.9500 . C58 C59 1.425(4) . C59 C60 1.418(4) . C59 C62 1.413(4) . C60 H60 0.9500 . C60 C61 1.363(4) . C61 H61 0.9500 . C62 C63 1.422(4) . C62 C64 1.422(5) . N9 C42 1.155(4) . N10 C43 1.162(4) . N11 C51 1.155(4) . N12 C52 1.155(4) . C41 C42 1.423(4) . C41 C43 1.419(4) . C41 C44 1.421(4) . C44 C45 1.431(4) . C44 C49 1.413(4) . C45 H45 0.9500 . C45 C46 1.364(4) . C46 H46 0.9500 . C46 C47 1.425(4) . C47 C48 1.427(4) . C47 C50 1.415(4) . C48 H48 0.9500 . C48 C49 1.361(4) . C49 H49 0.9500 . C50 C51 1.417(4) . C50 C52 1.425(4) . N17 C65 1.144(5) . C65 C66 1.455(5) . C66 H66A 0.9800 . C66 H66B 0.9800 . C66 H66C 0.9800 . O1 H1 0.8400 . O1 C67 1.411(6) . C67 H67A 0.9800 . C67 H67B 0.9800 . C67 H67C 0.9800 .