#------------------------------------------------------------------------------ #$Date: 2019-10-07 12:55:59 +0300 (Mon, 07 Oct 2019) $ #$Revision: 219132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234430.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_7234430 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 74.116(9) _cell_angle_beta 82.082(10) _cell_angle_gamma 85.910(10) _cell_formula_units_Z 2 _cell_length_a 8.941(7) _cell_length_b 13.990(11) _cell_length_c 24.828(19) _cell_measurement_reflns_used 9783 _cell_measurement_temperature 150.15 _cell_measurement_theta_max 27.06 _cell_measurement_theta_min 2.30 _cell_volume 2957(4) _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 150.15 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.983 _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 0.0428 _diffrn_reflns_av_unetI/netI 0.0538 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 31031 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.732 _diffrn_reflns_theta_min 1.514 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.353 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0903 before and 0.0544 after correction. The Ratio of minimum to maximum transmission is 0.8272. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.340 _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 0.671 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.072 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 797 _refine_ls_number_reflns 12363 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0461 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.4876P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1388 _refine_ls_wR_factor_ref 0.1560 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9792 _reflns_number_total 12363 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-9292.cif _cod_data_source_block 6-150K _cod_database_code 7234430 _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 0.917 _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 sad_a.res in P-1 REM Old TITL sad in P-1 REM SHELXT solution in P-1 REM R1 0.116, Rweak 0.005, Alpha 0.057, Orientation as input REM Formula found by SHELXT: C72 Co N14 O CELL 0.71073 8.9413 13.9905 24.8277 74.116 82.082 85.91 ZERR 2 0.0071 0.011 0.0194 0.009 0.01 0.01 LATT 1 SFAC C H Co N O UNIT 136 94 2 34 4 L.S. 10 PLAN 20 SIZE 0.08 0.13 0.25 TEMP 23 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.090000 0.487600 FVAR 0.34681 CO1 3 0.874403 0.318064 0.763682 11.00000 0.02022 0.01309 = 0.01022 0.00174 -0.00213 -0.00185 N1 4 0.886640 0.390927 0.683103 11.00000 0.01921 0.01836 = 0.01601 -0.00344 -0.00317 -0.00337 N2 4 0.661586 0.275068 0.739187 11.00000 0.02179 0.02077 = 0.01889 -0.00045 -0.00235 -0.00403 N3 4 1.095706 0.390586 0.747553 11.00000 0.02928 0.02037 = 0.02114 -0.00178 -0.01007 -0.00024 N4 4 0.839740 0.250487 0.841686 11.00000 0.01873 0.01674 = 0.01544 -0.00229 -0.00397 -0.00240 N5 4 0.971912 0.183596 0.761272 11.00000 0.02414 0.02242 = 0.01762 -0.00172 -0.00006 -0.00425 N6 4 0.762202 0.429360 0.792869 11.00000 0.01874 0.01767 = 0.02086 0.00143 -0.00419 -0.00359 N7 4 0.840922 0.724795 0.411496 11.00000 0.04624 0.03486 = 0.01974 0.00511 -0.00366 -0.00186 N8 4 0.553132 -0.027567 1.116153 11.00000 0.05685 0.02724 = 0.02205 -0.00115 0.00604 -0.00849 C1 1 0.773328 0.385359 0.653258 11.00000 0.02495 0.01947 = 0.01739 -0.00193 -0.00261 -0.00202 C2 1 0.764822 0.448966 0.599331 11.00000 0.02617 0.02564 = 0.01739 -0.00085 -0.00514 -0.00473 AFIX 43 H2 2 0.687263 0.443081 0.579160 11.00000 -1.20000 AFIX 0 C3 1 0.871928 0.521011 0.575742 11.00000 0.02493 0.01959 = 0.01485 -0.00194 -0.00355 -0.00080 C4 1 0.989907 0.524910 0.606845 11.00000 0.02295 0.01887 = 0.01913 -0.00200 -0.00238 -0.00456 AFIX 43 H4 2 1.064355 0.571428 0.592107 11.00000 -1.20000 AFIX 0 C5 1 0.994842 0.458674 0.659934 11.00000 0.01823 0.01958 = 0.01717 -0.00241 -0.00018 -0.00232 C6 1 1.116121 0.456101 0.695780 11.00000 0.02414 0.02279 = 0.01984 -0.00140 -0.00480 -0.00292 C7 1 1.244132 0.513646 0.677486 11.00000 0.03205 0.03920 = 0.02716 0.00203 -0.00993 -0.01399 AFIX 43 H7 2 1.256124 0.558194 0.641832 11.00000 -1.20000 AFIX 0 C8 1 1.353060 0.502774 0.713784 11.00000 0.02746 0.04533 = 0.04441 -0.00230 -0.01203 -0.01459 AFIX 43 H8 2 1.438642 0.540857 0.702814 11.00000 -1.20000 AFIX 0 C9 1 1.333651 0.434906 0.766439 11.00000 0.03199 0.03689 = 0.04006 -0.00659 -0.01892 -0.00210 AFIX 43 H9 2 1.406194 0.425898 0.791037 11.00000 -1.20000 AFIX 0 C10 1 1.203202 0.380787 0.781477 11.00000 0.03628 0.02691 = 0.02701 -0.00235 -0.01588 -0.00147 AFIX 43 H10 2 1.189746 0.335475 0.816857 11.00000 -1.20000 AFIX 0 C11 1 0.556819 0.210456 0.769209 11.00000 0.03348 0.02414 = 0.02035 0.00100 -0.00102 -0.00679 AFIX 43 H11 2 0.559505 0.185362 0.807847 11.00000 -1.20000 AFIX 0 C12 1 0.444846 0.179800 0.744727 11.00000 0.02824 0.02975 = 0.03115 0.00001 0.00011 -0.01421 AFIX 43 H12 2 0.372348 0.136396 0.766766 11.00000 -1.20000 AFIX 0 C13 1 0.442788 0.214953 0.686822 11.00000 0.03172 0.03527 = 0.03142 -0.00354 -0.00862 -0.01351 AFIX 43 H13 2 0.369868 0.194607 0.669397 11.00000 -1.20000 AFIX 0 C14 1 0.551511 0.281100 0.655255 11.00000 0.03037 0.03216 = 0.02075 -0.00062 -0.00512 -0.00904 AFIX 43 H14 2 0.553285 0.304903 0.616343 11.00000 -1.20000 AFIX 0 C15 1 0.657237 0.310962 0.682789 11.00000 0.02095 0.02200 = 0.01774 -0.00262 -0.00467 -0.00303 C16 1 0.861976 0.592152 0.518978 11.00000 0.02595 0.02230 = 0.01445 0.00015 -0.00065 -0.00025 C17 1 0.945208 0.677814 0.499991 11.00000 0.04654 0.03888 = 0.02647 0.00738 -0.01317 -0.01818 AFIX 43 H17 2 1.009385 0.692860 0.522760 11.00000 -1.20000 AFIX 0 C18 1 0.931679 0.740786 0.446677 11.00000 0.05452 0.04259 = 0.03006 0.01426 -0.00686 -0.02330 AFIX 43 H18 2 0.988983 0.797381 0.434690 11.00000 -1.20000 AFIX 0 C19 1 0.761747 0.642942 0.430401 11.00000 0.03726 0.03462 = 0.01940 -0.00327 -0.00889 0.00199 AFIX 43 H19 2 0.698243 0.629904 0.406774 11.00000 -1.20000 AFIX 0 C20 1 0.766804 0.575212 0.482984 11.00000 0.03489 0.02549 = 0.01973 -0.00108 -0.00663 -0.00338 AFIX 43 H20 2 0.707504 0.519547 0.493862 11.00000 -1.20000 AFIX 0 C21 1 0.755651 0.296883 0.877397 11.00000 0.01811 0.01748 = 0.01812 -0.00238 -0.00524 -0.00250 C22 1 0.708040 0.244890 0.933143 11.00000 0.02396 0.01901 = 0.01712 -0.00367 -0.00265 0.00003 AFIX 43 H22 2 0.651537 0.277357 0.957627 11.00000 -1.20000 AFIX 0 C23 1 0.746375 0.143421 0.951684 11.00000 0.02297 0.01892 = 0.01592 -0.00129 -0.00426 -0.00225 C24 1 0.836288 0.097477 0.914431 11.00000 0.02438 0.01850 = 0.01626 -0.00246 -0.00617 0.00120 AFIX 43 H24 2 0.866247 0.030802 0.926437 11.00000 -1.20000 AFIX 0 C25 1 0.880527 0.152412 0.859241 11.00000 0.02026 0.01737 = 0.01768 -0.00254 -0.00456 -0.00007 C26 1 0.961545 0.114063 0.812803 11.00000 0.02192 0.02087 = 0.01627 -0.00343 -0.00347 -0.00337 C27 1 1.018445 0.017332 0.818983 11.00000 0.03221 0.02286 = 0.02246 -0.00395 -0.00288 0.00034 AFIX 43 H27 2 1.010646 -0.028388 0.854286 11.00000 -1.20000 AFIX 0 C28 1 1.087846 -0.010244 0.771105 11.00000 0.03511 0.02558 = 0.03667 -0.01394 0.00086 0.00239 AFIX 43 H28 2 1.126327 -0.074776 0.774118 11.00000 -1.20000 AFIX 0 C29 1 1.098458 0.059816 0.719196 11.00000 0.03078 0.03676 = 0.02796 -0.01590 0.00654 -0.00592 AFIX 43 H29 2 1.144962 0.043023 0.686986 11.00000 -1.20000 AFIX 0 C30 1 1.038584 0.155882 0.715776 11.00000 0.02715 0.02999 = 0.02096 -0.00610 0.00385 -0.00844 AFIX 43 H30 2 1.045094 0.202362 0.680735 11.00000 -1.20000 AFIX 0 C31 1 0.723472 0.522104 0.763290 11.00000 0.03103 0.01919 = 0.02250 0.00145 -0.00776 -0.00344 AFIX 43 H31 2 0.760868 0.543231 0.725263 11.00000 -1.20000 AFIX 0 C32 1 0.630564 0.587001 0.787141 11.00000 0.03162 0.01502 = 0.03361 0.00146 -0.01013 -0.00134 AFIX 43 H32 2 0.604733 0.649855 0.765317 11.00000 -1.20000 AFIX 0 C33 1 0.576553 0.556859 0.844104 11.00000 0.03230 0.01919 = 0.03269 -0.00967 -0.00987 0.00326 AFIX 43 H33 2 0.512986 0.598977 0.860872 11.00000 -1.20000 AFIX 0 C34 1 0.618757 0.462653 0.875891 11.00000 0.02890 0.02035 = 0.02109 -0.00611 -0.00684 -0.00267 AFIX 43 H34 2 0.585574 0.441384 0.914291 11.00000 -1.20000 AFIX 0 C35 1 0.711690 0.401016 0.848938 11.00000 0.02099 0.01689 = 0.01941 -0.00343 -0.00612 -0.00361 C36 1 0.681495 0.084552 1.009075 11.00000 0.02848 0.01636 = 0.01685 -0.00244 -0.00203 -0.00425 C37 1 0.535118 0.105532 1.031620 11.00000 0.03195 0.02090 = 0.02424 -0.00258 0.00303 -0.00163 AFIX 43 H37 2 0.476887 0.157202 1.011425 11.00000 -1.20000 AFIX 0 C38 1 0.477107 0.048340 1.084653 11.00000 0.04303 0.02728 = 0.03103 -0.00600 0.00981 -0.00641 AFIX 43 H38 2 0.379584 0.063825 1.099069 11.00000 -1.20000 AFIX 0 C39 1 0.692577 -0.047653 1.093809 11.00000 0.05551 0.02100 = 0.01908 0.00193 -0.00498 -0.00327 AFIX 43 H39 2 0.747355 -0.100447 1.114792 11.00000 -1.20000 AFIX 0 C40 1 0.761486 0.004827 1.041407 11.00000 0.03326 0.02188 = 0.01906 -0.00266 -0.00575 -0.00046 AFIX 43 H40 2 0.859022 -0.012777 1.028099 11.00000 -1.20000 AFIX 0 N13 4 0.050926 0.142047 1.039696 11.00000 0.04454 0.01822 = 0.03568 -0.00291 -0.00312 0.00049 N14 4 0.388528 0.284755 0.897392 11.00000 0.02901 0.02899 = 0.03265 -0.00477 -0.00440 0.00296 N15 4 -0.498207 0.645232 0.978339 11.00000 0.03330 0.02880 = 0.03448 -0.00957 0.00042 0.00252 N16 4 -0.160713 0.812639 0.843521 11.00000 0.05230 0.02797 = 0.04215 0.00382 -0.00578 -0.00236 C53 1 -0.230487 0.653904 0.923131 11.00000 0.02724 0.01934 = 0.02091 -0.00400 -0.00389 -0.00121 C54 1 -0.376934 0.651671 0.953598 11.00000 0.03239 0.01709 = 0.02415 -0.00571 -0.00646 0.00340 C55 1 -0.192288 0.741215 0.879035 11.00000 0.03027 0.02190 = 0.02817 -0.00428 -0.00717 0.00245 C56 1 -0.133527 0.566961 0.932869 11.00000 0.02432 0.01911 = 0.01741 -0.00483 -0.00476 -0.00275 C57 1 0.007341 0.561005 0.898550 11.00000 0.02649 0.02094 = 0.01817 -0.00082 -0.00229 -0.00275 AFIX 43 H57 2 0.039196 0.615958 0.869442 11.00000 -1.20000 AFIX 0 C58 1 0.095678 0.475711 0.907956 11.00000 0.02511 0.02290 = 0.01820 -0.00631 -0.00075 -0.00274 AFIX 43 H58 2 0.186756 0.473644 0.885075 11.00000 -1.20000 AFIX 0 C59 1 0.050747 0.389100 0.952488 11.00000 0.02813 0.01703 = 0.01975 -0.00564 -0.00653 -0.00070 C60 1 -0.089432 0.395863 0.986418 11.00000 0.02851 0.01709 = 0.01863 -0.00145 -0.00245 -0.00463 AFIX 43 H60 2 -0.121264 0.341081 1.015651 11.00000 -1.20000 AFIX 0 C61 1 -0.178420 0.480976 0.977064 11.00000 0.02143 0.02124 = 0.02065 -0.00557 -0.00081 -0.00298 AFIX 43 H61 2 -0.269679 0.482875 0.999867 11.00000 -1.20000 AFIX 0 C62 1 0.141458 0.299456 0.962433 11.00000 0.02570 0.01890 = 0.02236 -0.00484 -0.00492 -0.00062 C63 1 0.091437 0.212827 1.005211 11.00000 0.02742 0.01880 = 0.02723 -0.00865 -0.00627 0.00260 C64 1 0.278157 0.290461 0.927488 11.00000 0.02908 0.01561 = 0.02555 -0.00215 -0.00816 0.00168 N9 4 0.387833 -0.184474 0.712923 11.00000 0.08872 0.05355 = 0.03495 0.00056 -0.01012 -0.01045 N10 4 0.107985 -0.239389 0.594832 11.00000 0.06382 0.04564 = 0.05708 -0.01200 0.00496 -0.02657 N11 4 0.643457 0.357844 0.485472 11.00000 0.07279 0.03745 = 0.08279 -0.01679 -0.01308 -0.01985 N12 4 0.358149 0.320017 0.364828 11.00000 0.06074 0.03680 = 0.03714 0.00103 -0.00616 0.00023 C41 1 0.193140 -0.188043 0.603149 11.00000 0.04905 0.02685 = 0.03753 -0.00407 0.00855 -0.00944 C42 1 0.347209 -0.158429 0.668675 11.00000 0.05235 0.03119 = 0.03245 -0.00516 0.00424 -0.00667 C43 1 0.295770 -0.125593 0.614704 11.00000 0.04377 0.02602 = 0.02873 -0.00651 0.00117 -0.00582 C44 1 0.337625 -0.032659 0.575880 11.00000 0.03145 0.02353 = 0.02991 -0.00911 0.00416 -0.00426 C45 1 0.438085 0.030113 0.588715 11.00000 0.03903 0.02910 = 0.02962 -0.00843 -0.00577 -0.00331 AFIX 43 H45 2 0.475603 0.010826 0.623364 11.00000 -1.20000 AFIX 0 C46 1 0.480866 0.118462 0.551130 11.00000 0.03517 0.02538 = 0.03798 -0.01028 -0.00493 -0.00554 AFIX 43 H46 2 0.548804 0.156880 0.560454 11.00000 -1.20000 AFIX 0 C47 1 0.423623 0.152550 0.498258 11.00000 0.03279 0.02098 = 0.03048 -0.00894 0.00048 -0.00263 C48 1 0.320667 0.090531 0.485799 11.00000 0.04457 0.02843 = 0.02792 -0.00750 -0.00614 -0.00456 AFIX 43 H48 2 0.280156 0.110910 0.451748 11.00000 -1.20000 AFIX 0 C49 1 0.280353 0.001608 0.522994 11.00000 0.04101 0.02908 = 0.02986 -0.01026 -0.00555 -0.01059 AFIX 43 H49 2 0.213781 -0.037403 0.513425 11.00000 -1.20000 AFIX 0 C50 1 0.467200 0.244492 0.459314 11.00000 0.03781 0.02131 = 0.03415 -0.00781 0.00172 -0.00118 C51 1 0.565009 0.307476 0.473414 11.00000 0.04092 0.02292 = 0.04907 -0.00586 0.00152 -0.00610 C52 1 0.405860 0.284523 0.407086 11.00000 0.03922 0.02152 = 0.03811 -0.00517 0.00307 -0.00203 O1 5 1.186792 0.910409 0.384965 11.00000 0.09932 0.08756 = 0.15547 0.04822 -0.05489 -0.04252 N17 4 1.208305 1.057175 0.318956 11.00000 0.06719 0.04910 = 0.06052 -0.00885 -0.01264 -0.01232 C65 1 1.158935 0.999889 0.369803 11.00000 0.07128 0.08491 = 0.06301 0.01786 -0.02607 -0.03771 AFIX 43 H65 2 1.100114 1.029556 0.395131 11.00000 -1.20000 AFIX 0 C66 1 1.177624 1.164742 0.303372 11.00000 0.11597 0.05407 = 0.08082 -0.01909 0.01257 -0.00850 AFIX 137 H66A 2 1.270351 1.198392 0.298669 11.00000 -1.50000 H66B 2 1.108639 1.182447 0.332597 11.00000 -1.50000 H66C 2 1.133752 1.183954 0.268625 11.00000 -1.50000 AFIX 0 C67 1 1.301579 1.016639 0.275702 11.00000 0.06718 0.06070 = 0.09948 -0.02774 -0.00921 0.00899 AFIX 137 H67A 2 1.397767 1.047379 0.266196 11.00000 -1.50000 H67B 2 1.251056 1.030141 0.242570 11.00000 -1.50000 H67C 2 1.316430 0.946099 0.290279 11.00000 -1.50000 AFIX 0 O2 5 0.292761 -0.272927 0.831614 11.00000 0.12557 0.09259 = 0.06925 -0.01318 0.01354 -0.01677 AFIX 147 H2A 2 0.319268 -0.247750 0.798023 11.00000 -1.50000 AFIX 0 C68 1 0.311073 -0.206470 0.862005 11.00000 0.21383 0.07592 = 0.08465 -0.03363 -0.08830 0.03753 AFIX 137 H68A 2 0.408615 -0.177959 0.849977 11.00000 -1.50000 H68B 2 0.303429 -0.240493 0.901456 11.00000 -1.50000 H68C 2 0.233926 -0.154677 0.855747 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad_a.res in P-1 REM R1 = 0.0461 for 9792 Fo > 4sig(Fo) and 0.0607 for all 12363 data REM 797 parameters refined using 0 restraints END WGHT 0.0900 0.4876 REM Highest difference peak 0.671, deepest hole -0.661, 1-sigma level 0.072 Q1 1 1.2985 1.0051 0.2278 11.00000 0.05 0.67 Q2 1 0.8400 0.2646 0.7719 11.00000 0.05 0.49 Q3 1 0.9204 0.3768 0.7527 11.00000 0.05 0.46 Q4 1 1.2475 0.9343 0.3434 11.00000 0.05 0.44 Q5 1 0.4388 -0.2357 0.8363 11.00000 0.05 0.44 Q6 1 0.7715 0.3584 0.7627 11.00000 0.05 0.37 Q7 1 0.9252 0.3175 0.7312 11.00000 0.05 0.37 Q8 1 0.9675 0.2733 0.7678 11.00000 0.05 0.35 Q9 1 0.9368 0.1261 0.8430 11.00000 0.05 0.35 Q10 1 0.8480 0.2999 0.8021 11.00000 0.05 0.35 Q11 1 0.9017 0.3470 0.7219 11.00000 0.05 0.33 Q12 1 0.8692 0.2844 0.8108 11.00000 0.05 0.32 Q13 1 0.8690 0.5546 0.5459 11.00000 0.05 0.30 Q14 1 0.8758 0.2004 0.8505 11.00000 0.05 0.29 Q15 1 0.7480 0.4188 0.8206 11.00000 0.05 0.29 Q16 1 -0.1707 0.6181 0.9274 11.00000 0.05 0.29 Q17 1 0.7087 0.4565 0.7788 11.00000 0.05 0.28 Q18 1 0.7211 0.3623 0.8629 11.00000 0.05 0.27 Q19 1 0.4160 -0.0978 1.1247 11.00000 0.05 0.25 Q20 1 0.3594 0.2799 0.9309 11.00000 0.05 0.25 ; _shelx_res_checksum 23608 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 0.87440(3) 0.31806(2) 0.76368(2) 0.01539(10) Uani 1 1 d . . . . . N1 N 0.8866(2) 0.39093(13) 0.68310(7) 0.0179(4) Uani 1 1 d . . . . . N2 N 0.6616(2) 0.27507(13) 0.73919(8) 0.0213(4) Uani 1 1 d . . . . . N3 N 1.0957(2) 0.39059(13) 0.74755(8) 0.0237(4) Uani 1 1 d . . . . . N4 N 0.8397(2) 0.25049(12) 0.84169(7) 0.0171(4) Uani 1 1 d . . . . . N5 N 0.9719(2) 0.18360(14) 0.76127(8) 0.0222(4) Uani 1 1 d . . . . . N6 N 0.7622(2) 0.42936(13) 0.79287(8) 0.0201(4) Uani 1 1 d . . . . . N7 N 0.8409(3) 0.72479(16) 0.41150(9) 0.0361(5) Uani 1 1 d . . . . . N8 N 0.5531(3) -0.02757(15) 1.11615(9) 0.0372(5) Uani 1 1 d . . . . . C1 C 0.7733(3) 0.38536(16) 0.65326(9) 0.0211(5) Uani 1 1 d . . . . . C2 C 0.7648(3) 0.44897(16) 0.59933(9) 0.0236(5) Uani 1 1 d . . . . . H2 H 0.6873 0.4431 0.5792 0.028 Uiso 1 1 calc R . . . . C3 C 0.8719(3) 0.52101(15) 0.57574(9) 0.0202(4) Uani 1 1 d . . . . . C4 C 0.9899(3) 0.52491(15) 0.60684(9) 0.0208(5) Uani 1 1 d . . . . . H4 H 1.0644 0.5714 0.5921 0.025 Uiso 1 1 calc R . . . . C5 C 0.9948(2) 0.45867(15) 0.65993(9) 0.0189(4) Uani 1 1 d . . . . . C6 C 1.1161(3) 0.45610(16) 0.69578(9) 0.0228(5) Uani 1 1 d . . . . . C7 C 1.2441(3) 0.51365(19) 0.67749(11) 0.0337(6) Uani 1 1 d . . . . . H7 H 1.2561 0.5582 0.6418 0.040 Uiso 1 1 calc R . . . . C8 C 1.3531(3) 0.5028(2) 0.71378(12) 0.0396(7) Uani 1 1 d . . . . . H8 H 1.4386 0.5409 0.7028 0.048 Uiso 1 1 calc R . . . . C9 C 1.3337(3) 0.43491(19) 0.76644(12) 0.0356(6) Uani 1 1 d . . . . . H9 H 1.4062 0.4259 0.7910 0.043 Uiso 1 1 calc R . . . . C10 C 1.2032(3) 0.38079(18) 0.78148(10) 0.0298(5) Uani 1 1 d . . . . . H10 H 1.1897 0.3355 0.8169 0.036 Uiso 1 1 calc R . . . . C11 C 0.5568(3) 0.21046(17) 0.76921(10) 0.0273(5) Uani 1 1 d . . . . . H11 H 0.5595 0.1854 0.8078 0.033 Uiso 1 1 calc R . . . . C12 C 0.4448(3) 0.17980(18) 0.74473(11) 0.0310(6) Uani 1 1 d . . . . . H12 H 0.3723 0.1364 0.7668 0.037 Uiso 1 1 calc R . . . . C13 C 0.4428(3) 0.21495(19) 0.68682(11) 0.0328(6) Uani 1 1 d . . . . . H13 H 0.3699 0.1946 0.6694 0.039 Uiso 1 1 calc R . . . . C14 C 0.5515(3) 0.28110(18) 0.65526(10) 0.0285(5) Uani 1 1 d . . . . . H14 H 0.5533 0.3049 0.6163 0.034 Uiso 1 1 calc R . . . . C15 C 0.6572(2) 0.31096(16) 0.68279(9) 0.0204(4) Uani 1 1 d . . . . . C16 C 0.8620(3) 0.59215(16) 0.51898(9) 0.0221(5) Uani 1 1 d . . . . . C17 C 0.9452(3) 0.6778(2) 0.49999(11) 0.0388(7) Uani 1 1 d . . . . . H17 H 1.0094 0.6929 0.5228 0.047 Uiso 1 1 calc R . . . . C18 C 0.9317(4) 0.7408(2) 0.44668(12) 0.0459(8) Uani 1 1 d . . . . . H18 H 0.9890 0.7974 0.4347 0.055 Uiso 1 1 calc R . . . . C19 C 0.7617(3) 0.64294(18) 0.43040(10) 0.0308(6) Uani 1 1 d . . . . . H19 H 0.6982 0.6299 0.4068 0.037 Uiso 1 1 calc R . . . . C20 C 0.7668(3) 0.57521(17) 0.48298(10) 0.0273(5) Uani 1 1 d . . . . . H20 H 0.7075 0.5195 0.4939 0.033 Uiso 1 1 calc R . . . . C21 C 0.7557(2) 0.29688(15) 0.87740(9) 0.0180(4) Uani 1 1 d . . . . . C22 C 0.7080(3) 0.24489(15) 0.93314(9) 0.0203(4) Uani 1 1 d . . . . . H22 H 0.6515 0.2774 0.9576 0.024 Uiso 1 1 calc R . . . . C23 C 0.7464(2) 0.14342(15) 0.95168(9) 0.0197(4) Uani 1 1 d . . . . . C24 C 0.8363(3) 0.09748(16) 0.91443(9) 0.0199(4) Uani 1 1 d . . . . . H24 H 0.8662 0.0308 0.9264 0.024 Uiso 1 1 calc R . . . . C25 C 0.8805(2) 0.15241(15) 0.85924(9) 0.0187(4) Uani 1 1 d . . . . . C26 C 0.9615(2) 0.11406(16) 0.81280(9) 0.0198(4) Uani 1 1 d . . . . . C27 C 1.0184(3) 0.01733(17) 0.81898(10) 0.0264(5) Uani 1 1 d . . . . . H27 H 1.0106 -0.0284 0.8543 0.032 Uiso 1 1 calc R . . . . C28 C 1.0878(3) -0.01024(18) 0.77111(11) 0.0320(6) Uani 1 1 d . . . . . H28 H 1.1263 -0.0748 0.7741 0.038 Uiso 1 1 calc R . . . . C29 C 1.0985(3) 0.05982(19) 0.71920(11) 0.0311(6) Uani 1 1 d . . . . . H29 H 1.1450 0.0430 0.6870 0.037 Uiso 1 1 calc R . . . . C30 C 1.0386(3) 0.15588(18) 0.71578(10) 0.0265(5) Uani 1 1 d . . . . . H30 H 1.0451 0.2024 0.6807 0.032 Uiso 1 1 calc R . . . . C31 C 0.7235(3) 0.52210(16) 0.76329(10) 0.0251(5) Uani 1 1 d . . . . . H31 H 0.7609 0.5432 0.7253 0.030 Uiso 1 1 calc R . . . . C32 C 0.6306(3) 0.58700(16) 0.78714(10) 0.0277(5) Uani 1 1 d . . . . . H32 H 0.6047 0.6499 0.7653 0.033 Uiso 1 1 calc R . . . . C33 C 0.5766(3) 0.55686(16) 0.84410(10) 0.0272(5) Uani 1 1 d . . . . . H33 H 0.5130 0.5990 0.8609 0.033 Uiso 1 1 calc R . . . . C34 C 0.6188(3) 0.46265(16) 0.87589(10) 0.0229(5) Uani 1 1 d . . . . . H34 H 0.5856 0.4414 0.9143 0.027 Uiso 1 1 calc R . . . . C35 C 0.7117(2) 0.40102(15) 0.84894(9) 0.0189(4) Uani 1 1 d . . . . . C36 C 0.6815(3) 0.08455(15) 1.00908(9) 0.0209(5) Uani 1 1 d . . . . . C37 C 0.5351(3) 0.10553(17) 1.03162(10) 0.0270(5) Uani 1 1 d . . . . . H37 H 0.4769 0.1572 1.0114 0.032 Uiso 1 1 calc R . . . . C38 C 0.4771(3) 0.04834(18) 1.08465(11) 0.0353(6) Uani 1 1 d . . . . . H38 H 0.3796 0.0638 1.0991 0.042 Uiso 1 1 calc R . . . . C39 C 0.6926(3) -0.04765(17) 1.09381(10) 0.0332(6) Uani 1 1 d . . . . . H39 H 0.7474 -0.1004 1.1148 0.040 Uiso 1 1 calc R . . . . C40 C 0.7615(3) 0.00483(16) 1.04141(9) 0.0251(5) Uani 1 1 d . . . . . H40 H 0.8590 -0.0128 1.0281 0.030 Uiso 1 1 calc R . . . . N13 N 0.0509(3) 0.14205(14) 1.03970(9) 0.0339(5) Uani 1 1 d . . . . . N14 N 0.3885(2) 0.28476(15) 0.89739(9) 0.0310(5) Uani 1 1 d . . . . . N15 N -0.4982(3) 0.64523(15) 0.97834(9) 0.0326(5) Uani 1 1 d . . . . . N16 N -0.1607(3) 0.81264(16) 0.84352(10) 0.0434(6) Uani 1 1 d . . . . . C53 C -0.2305(3) 0.65390(16) 0.92313(9) 0.0227(5) Uani 1 1 d . . . . . C54 C -0.3769(3) 0.65167(16) 0.95360(10) 0.0244(5) Uani 1 1 d . . . . . C55 C -0.1923(3) 0.74121(17) 0.87903(10) 0.0271(5) Uani 1 1 d . . . . . C56 C -0.1335(3) 0.56696(15) 0.93287(9) 0.0200(4) Uani 1 1 d . . . . . C57 C 0.0073(3) 0.56100(16) 0.89855(9) 0.0227(5) Uani 1 1 d . . . . . H57 H 0.0392 0.6160 0.8694 0.027 Uiso 1 1 calc R . . . . C58 C 0.0957(3) 0.47571(16) 0.90796(9) 0.0220(5) Uani 1 1 d . . . . . H58 H 0.1868 0.4736 0.8851 0.026 Uiso 1 1 calc R . . . . C59 C 0.0507(3) 0.38910(15) 0.95249(9) 0.0211(5) Uani 1 1 d . . . . . C60 C -0.0894(3) 0.39586(16) 0.98642(9) 0.0219(5) Uani 1 1 d . . . . . H60 H -0.1213 0.3411 1.0157 0.026 Uiso 1 1 calc R . . . . C61 C -0.1784(3) 0.48098(16) 0.97706(9) 0.0212(5) Uani 1 1 d . . . . . H61 H -0.2697 0.4829 0.9999 0.025 Uiso 1 1 calc R . . . . C62 C 0.1415(3) 0.29946(16) 0.96243(9) 0.0223(5) Uani 1 1 d . . . . . C63 C 0.0914(3) 0.21283(16) 1.00521(10) 0.0239(5) Uani 1 1 d . . . . . C64 C 0.2782(3) 0.29046(15) 0.92749(10) 0.0237(5) Uani 1 1 d . . . . . N9 N 0.3878(4) -0.1845(2) 0.71292(11) 0.0609(8) Uani 1 1 d . . . . . N10 N 0.1080(3) -0.2394(2) 0.59483(12) 0.0558(7) Uani 1 1 d . . . . . N11 N 0.6435(4) 0.35784(19) 0.48547(14) 0.0630(8) Uani 1 1 d . . . . . N12 N 0.3581(3) 0.32002(18) 0.36483(10) 0.0471(6) Uani 1 1 d . . . . . C41 C 0.1931(3) -0.18804(19) 0.60315(12) 0.0397(7) Uani 1 1 d . . . . . C42 C 0.3472(3) -0.1584(2) 0.66868(12) 0.0400(7) Uani 1 1 d . . . . . C43 C 0.2958(3) -0.12559(18) 0.61470(11) 0.0333(6) Uani 1 1 d . . . . . C44 C 0.3376(3) -0.03266(17) 0.57588(10) 0.0285(5) Uani 1 1 d . . . . . C45 C 0.4381(3) 0.03011(18) 0.58872(11) 0.0322(6) Uani 1 1 d . . . . . H45 H 0.4756 0.0108 0.6234 0.039 Uiso 1 1 calc R . . . . C46 C 0.4809(3) 0.11846(18) 0.55113(11) 0.0322(6) Uani 1 1 d . . . . . H46 H 0.5488 0.1569 0.5605 0.039 Uiso 1 1 calc R . . . . C47 C 0.4236(3) 0.15255(17) 0.49826(10) 0.0280(5) Uani 1 1 d . . . . . C48 C 0.3207(3) 0.09053(18) 0.48580(11) 0.0333(6) Uani 1 1 d . . . . . H48 H 0.2802 0.1109 0.4517 0.040 Uiso 1 1 calc R . . . . C49 C 0.2804(3) 0.00161(18) 0.52299(11) 0.0323(6) Uani 1 1 d . . . . . H49 H 0.2138 -0.0374 0.5134 0.039 Uiso 1 1 calc R . . . . C50 C 0.4672(3) 0.24449(17) 0.45931(11) 0.0316(6) Uani 1 1 d . . . . . C51 C 0.5650(3) 0.30748(19) 0.47341(12) 0.0388(6) Uani 1 1 d . . . . . C52 C 0.4059(3) 0.28452(18) 0.40709(12) 0.0342(6) Uani 1 1 d . . . . . O1 O 1.1868(4) 0.9104(3) 0.38496(18) 0.1244(16) Uani 1 1 d . . . . . N17 N 1.2083(4) 1.0572(2) 0.31896(13) 0.0591(8) Uani 1 1 d . . . . . C65 C 1.1589(5) 0.9999(3) 0.36980(17) 0.0771(13) Uani 1 1 d . . . . . H65 H 1.1001 1.0296 0.3951 0.092 Uiso 1 1 calc R . . . . C66 C 1.1776(6) 1.1647(3) 0.30337(19) 0.0855(14) Uani 1 1 d . . . . . H66A H 1.2704 1.1984 0.2987 0.128 Uiso 1 1 calc GR . . . . H66B H 1.1086 1.1824 0.3326 0.128 Uiso 1 1 calc GR . . . . H66C H 1.1338 1.1840 0.2686 0.128 Uiso 1 1 calc GR . . . . C67 C 1.3016(5) 1.0166(3) 0.27570(19) 0.0752(12) Uani 1 1 d . . . . . H67A H 1.3978 1.0474 0.2662 0.113 Uiso 1 1 calc GR . . . . H67B H 1.2511 1.0301 0.2426 0.113 Uiso 1 1 calc GR . . . . H67C H 1.3164 0.9461 0.2903 0.113 Uiso 1 1 calc GR . . . . O2 O 0.2928(5) -0.2729(2) 0.83161(13) 0.0993(10) Uani 1 1 d . . . . . H2A H 0.3193 -0.2478 0.7980 0.149 Uiso 1 1 calc GR . . . . C68 C 0.3111(8) -0.2065(4) 0.8620(2) 0.118(2) Uani 1 1 d . . . . . H68A H 0.4086 -0.1780 0.8500 0.177 Uiso 1 1 calc GR . . . . H68B H 0.3034 -0.2405 0.9015 0.177 Uiso 1 1 calc GR . . . . H68C H 0.2339 -0.1547 0.8557 0.177 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 0.02022(17) 0.01309(15) 0.01022(15) 0.00174(10) -0.00213(11) -0.00185(11) N1 0.0192(9) 0.0184(9) 0.0160(9) -0.0034(7) -0.0032(7) -0.0034(7) N2 0.0218(10) 0.0208(9) 0.0189(9) -0.0004(7) -0.0023(8) -0.0040(7) N3 0.0293(11) 0.0204(9) 0.0211(10) -0.0018(7) -0.0101(8) -0.0002(8) N4 0.0187(9) 0.0167(8) 0.0154(9) -0.0023(7) -0.0040(7) -0.0024(7) N5 0.0241(10) 0.0224(9) 0.0176(9) -0.0017(7) -0.0001(8) -0.0043(7) N6 0.0187(9) 0.0177(9) 0.0209(9) 0.0014(7) -0.0042(7) -0.0036(7) N7 0.0462(14) 0.0349(12) 0.0197(10) 0.0051(9) -0.0037(9) -0.0019(10) N8 0.0568(16) 0.0272(11) 0.0220(11) -0.0011(9) 0.0060(10) -0.0085(10) C1 0.0249(12) 0.0195(10) 0.0174(10) -0.0019(8) -0.0026(9) -0.0020(9) C2 0.0262(12) 0.0256(11) 0.0174(11) -0.0009(9) -0.0051(9) -0.0047(9) C3 0.0249(12) 0.0196(10) 0.0149(10) -0.0019(8) -0.0035(9) -0.0008(9) C4 0.0230(12) 0.0189(10) 0.0191(11) -0.0020(8) -0.0024(9) -0.0046(8) C5 0.0182(11) 0.0196(10) 0.0172(10) -0.0024(8) -0.0002(8) -0.0023(8) C6 0.0241(12) 0.0228(11) 0.0198(11) -0.0014(9) -0.0048(9) -0.0029(9) C7 0.0321(14) 0.0392(14) 0.0272(13) 0.0020(11) -0.0099(11) -0.0140(11) C8 0.0275(14) 0.0453(16) 0.0444(16) -0.0023(13) -0.0120(12) -0.0146(12) C9 0.0320(14) 0.0369(14) 0.0401(15) -0.0066(12) -0.0189(12) -0.0021(11) C10 0.0363(14) 0.0269(12) 0.0270(12) -0.0024(10) -0.0159(11) -0.0015(10) C11 0.0335(14) 0.0241(12) 0.0203(11) 0.0010(9) -0.0010(10) -0.0068(10) C12 0.0282(13) 0.0297(12) 0.0312(13) 0.0000(10) 0.0001(10) -0.0142(10) C13 0.0317(14) 0.0353(13) 0.0314(13) -0.0035(11) -0.0086(11) -0.0135(11) C14 0.0304(13) 0.0322(13) 0.0207(11) -0.0006(10) -0.0051(10) -0.0090(10) C15 0.0210(11) 0.0220(11) 0.0177(10) -0.0026(8) -0.0047(9) -0.0030(9) C16 0.0259(12) 0.0223(11) 0.0145(10) 0.0002(8) -0.0006(9) -0.0002(9) C17 0.0465(17) 0.0389(15) 0.0265(13) 0.0074(11) -0.0132(12) -0.0182(12) C18 0.0545(19) 0.0426(16) 0.0301(14) 0.0143(12) -0.0069(13) -0.0233(14) C19 0.0373(14) 0.0346(13) 0.0194(11) -0.0033(10) -0.0089(10) 0.0020(11) C20 0.0349(14) 0.0255(12) 0.0197(11) -0.0011(9) -0.0066(10) -0.0034(10) C21 0.0181(11) 0.0175(10) 0.0181(10) -0.0024(8) -0.0052(8) -0.0025(8) C22 0.0240(12) 0.0190(10) 0.0171(10) -0.0037(8) -0.0026(9) 0.0000(8) C23 0.0230(11) 0.0189(10) 0.0159(10) -0.0013(8) -0.0043(9) -0.0022(8) C24 0.0244(12) 0.0185(10) 0.0163(10) -0.0025(8) -0.0062(9) 0.0012(8) C25 0.0203(11) 0.0174(10) 0.0177(10) -0.0025(8) -0.0046(8) -0.0001(8) C26 0.0219(11) 0.0209(10) 0.0163(10) -0.0034(8) -0.0035(8) -0.0034(8) C27 0.0322(13) 0.0229(11) 0.0225(11) -0.0039(9) -0.0029(10) 0.0003(9) C28 0.0351(14) 0.0256(12) 0.0367(14) -0.0139(11) 0.0009(11) 0.0024(10) C29 0.0308(14) 0.0368(14) 0.0280(13) -0.0159(11) 0.0065(10) -0.0059(11) C30 0.0272(13) 0.0300(12) 0.0210(11) -0.0061(9) 0.0038(9) -0.0084(10) C31 0.0310(13) 0.0192(11) 0.0225(11) 0.0014(9) -0.0078(10) -0.0034(9) C32 0.0316(13) 0.0150(10) 0.0336(13) 0.0015(9) -0.0101(11) -0.0013(9) C33 0.0323(13) 0.0192(11) 0.0327(13) -0.0097(10) -0.0099(11) 0.0033(9) C34 0.0289(12) 0.0204(11) 0.0211(11) -0.0061(9) -0.0068(9) -0.0027(9) C35 0.0210(11) 0.0169(10) 0.0194(10) -0.0034(8) -0.0061(9) -0.0036(8) C36 0.0285(12) 0.0164(10) 0.0168(10) -0.0024(8) -0.0020(9) -0.0042(8) C37 0.0320(13) 0.0209(11) 0.0242(12) -0.0026(9) 0.0030(10) -0.0016(9) C38 0.0430(16) 0.0273(13) 0.0310(14) -0.0060(11) 0.0098(12) -0.0064(11) C39 0.0555(18) 0.0210(12) 0.0191(12) 0.0019(9) -0.0050(11) -0.0033(11) C40 0.0333(13) 0.0219(11) 0.0191(11) -0.0027(9) -0.0058(10) -0.0005(9) N13 0.0445(14) 0.0182(10) 0.0357(12) -0.0029(9) -0.0031(10) 0.0005(9) N14 0.0290(12) 0.0290(11) 0.0326(12) -0.0048(9) -0.0044(10) 0.0030(9) N15 0.0333(13) 0.0288(11) 0.0345(12) -0.0096(9) 0.0004(10) 0.0025(9) N16 0.0523(16) 0.0280(12) 0.0421(14) 0.0038(10) -0.0058(11) -0.0024(10) C53 0.0272(12) 0.0193(10) 0.0209(11) -0.0040(9) -0.0039(9) -0.0012(9) C54 0.0324(14) 0.0171(10) 0.0242(12) -0.0057(9) -0.0065(10) 0.0034(9) C55 0.0303(13) 0.0219(11) 0.0282(12) -0.0043(10) -0.0072(10) 0.0025(9) C56 0.0243(12) 0.0191(10) 0.0174(10) -0.0048(8) -0.0048(9) -0.0027(8) C57 0.0265(12) 0.0209(11) 0.0182(11) -0.0008(9) -0.0023(9) -0.0028(9) C58 0.0251(12) 0.0229(11) 0.0182(11) -0.0063(9) -0.0008(9) -0.0027(9) C59 0.0281(12) 0.0170(10) 0.0197(11) -0.0056(8) -0.0065(9) -0.0007(9) C60 0.0285(12) 0.0171(10) 0.0186(11) -0.0014(8) -0.0025(9) -0.0046(9) C61 0.0214(11) 0.0212(11) 0.0206(11) -0.0056(9) -0.0008(9) -0.0030(9) C62 0.0257(12) 0.0189(10) 0.0224(11) -0.0048(9) -0.0049(9) -0.0006(9) C63 0.0274(12) 0.0188(11) 0.0272(12) -0.0087(9) -0.0063(10) 0.0026(9) C64 0.0291(13) 0.0156(10) 0.0256(12) -0.0021(9) -0.0082(10) 0.0017(9) N9 0.089(2) 0.0536(16) 0.0350(15) 0.0006(12) -0.0101(15) -0.0104(15) N10 0.0638(19) 0.0456(15) 0.0571(17) -0.0120(13) 0.0050(14) -0.0266(14) N11 0.073(2) 0.0374(14) 0.083(2) -0.0168(14) -0.0131(17) -0.0199(14) N12 0.0607(17) 0.0368(13) 0.0371(14) 0.0010(11) -0.0062(12) 0.0002(12) C41 0.0491(18) 0.0268(13) 0.0375(15) -0.0041(11) 0.0085(13) -0.0094(12) C42 0.0524(18) 0.0312(14) 0.0325(15) -0.0052(11) 0.0042(13) -0.0067(12) C43 0.0438(16) 0.0260(12) 0.0287(13) -0.0065(10) 0.0012(11) -0.0058(11) C44 0.0315(13) 0.0235(12) 0.0299(13) -0.0091(10) 0.0042(10) -0.0043(10) C45 0.0390(15) 0.0291(13) 0.0296(13) -0.0084(10) -0.0058(11) -0.0033(11) C46 0.0352(14) 0.0254(12) 0.0380(14) -0.0103(11) -0.0049(11) -0.0055(10) C47 0.0328(14) 0.0210(11) 0.0305(13) -0.0089(10) 0.0005(10) -0.0026(9) C48 0.0446(16) 0.0284(13) 0.0279(13) -0.0075(10) -0.0061(11) -0.0046(11) C49 0.0410(15) 0.0291(13) 0.0299(13) -0.0103(10) -0.0056(11) -0.0106(11) C50 0.0378(15) 0.0213(11) 0.0342(14) -0.0078(10) 0.0017(11) -0.0012(10) C51 0.0409(16) 0.0229(12) 0.0491(17) -0.0059(12) 0.0015(13) -0.0061(11) C52 0.0392(15) 0.0215(12) 0.0381(15) -0.0052(11) 0.0031(12) -0.0020(10) O1 0.099(3) 0.088(2) 0.155(4) 0.048(2) -0.055(2) -0.043(2) N17 0.067(2) 0.0491(16) 0.0605(18) -0.0089(14) -0.0126(15) -0.0123(14) C65 0.071(3) 0.085(3) 0.063(2) 0.018(2) -0.026(2) -0.038(2) C66 0.116(4) 0.054(2) 0.081(3) -0.019(2) 0.013(3) -0.009(2) C67 0.067(3) 0.061(2) 0.099(3) -0.028(2) -0.009(2) 0.0090(19) O2 0.126(3) 0.093(2) 0.069(2) -0.0132(18) 0.014(2) -0.017(2) C68 0.214(7) 0.076(3) 0.085(3) -0.034(3) -0.088(4) 0.038(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 77.91(7) . . N1 Co1 N3 77.03(7) . . N1 Co1 N5 102.72(8) . . N1 Co1 N6 95.65(8) . . N3 Co1 N2 154.82(7) . . N4 Co1 N1 173.83(7) . . N4 Co1 N2 97.01(8) . . N4 Co1 N3 108.15(7) . . N4 Co1 N5 80.62(8) . . N4 Co1 N6 80.87(8) . . N5 Co1 N2 90.09(8) . . N5 Co1 N3 93.01(9) . . N5 Co1 N6 161.48(8) . . N6 Co1 N2 91.52(8) . . N6 Co1 N3 93.35(9) . . C1 N1 Co1 119.67(15) . . C1 N1 C5 119.33(18) . . C5 N1 Co1 120.15(14) . . C11 N2 Co1 130.16(16) . . C11 N2 C15 118.34(19) . . C15 N2 Co1 110.66(14) . . C6 N3 Co1 112.00(14) . . C10 N3 Co1 129.65(17) . . C10 N3 C6 118.3(2) . . C21 N4 Co1 119.01(14) . . C21 N4 C25 120.82(18) . . C25 N4 Co1 119.48(14) . . C26 N5 Co1 114.04(15) . . C30 N5 Co1 127.54(16) . . C30 N5 C26 118.4(2) . . C31 N6 Co1 128.53(17) . . C31 N6 C35 117.86(19) . . C35 N6 Co1 113.39(14) . . C19 N7 C18 115.8(2) . . C39 N8 C38 116.1(2) . . N1 C1 C2 121.1(2) . . N1 C1 C15 115.52(19) . . C2 C1 C15 123.3(2) . . C1 C2 H2 119.9 . . C3 C2 C1 120.3(2) . . C3 C2 H2 119.9 . . C2 C3 C4 117.9(2) . . C2 C3 C16 121.2(2) . . C4 C3 C16 120.9(2) . . C3 C4 H4 120.2 . . C5 C4 C3 119.6(2) . . C5 C4 H4 120.2 . . N1 C5 C4 121.7(2) . . N1 C5 C6 114.67(18) . . C4 C5 C6 123.6(2) . . N3 C6 C5 114.7(2) . . N3 C6 C7 122.0(2) . . C7 C6 C5 123.3(2) . . C6 C7 H7 120.8 . . C8 C7 C6 118.5(2) . . C8 C7 H7 120.8 . . C7 C8 H8 120.1 . . C9 C8 C7 119.7(2) . . C9 C8 H8 120.1 . . C8 C9 H9 120.9 . . C8 C9 C10 118.3(2) . . C10 C9 H9 120.9 . . N3 C10 C9 123.2(2) . . N3 C10 H10 118.4 . . C9 C10 H10 118.4 . . N2 C11 H11 118.7 . . N2 C11 C12 122.5(2) . . C12 C11 H11 118.7 . . C11 C12 H12 120.5 . . C11 C12 C13 119.0(2) . . C13 C12 H12 120.5 . . C12 C13 H13 120.5 . . C12 C13 C14 119.0(2) . . C14 C13 H13 120.5 . . C13 C14 H14 120.5 . . C15 C14 C13 118.9(2) . . C15 C14 H14 120.5 . . N2 C15 C1 114.74(19) . . N2 C15 C14 122.2(2) . . C14 C15 C1 123.1(2) . . C17 C16 C3 122.1(2) . . C17 C16 C20 117.1(2) . . C20 C16 C3 120.8(2) . . C16 C17 H17 120.3 . . C18 C17 C16 119.4(2) . . C18 C17 H17 120.3 . . N7 C18 C17 123.9(3) . . N7 C18 H18 118.0 . . C17 C18 H18 118.0 . . N7 C19 H19 117.6 . . N7 C19 C20 124.8(2) . . C20 C19 H19 117.6 . . C16 C20 C19 118.9(2) . . C16 C20 H20 120.5 . . C19 C20 H20 120.5 . . N4 C21 C22 120.74(19) . . N4 C21 C35 112.55(19) . . C22 C21 C35 126.5(2) . . C21 C22 H22 120.4 . . C21 C22 C23 119.3(2) . . C23 C22 H22 120.4 . . C22 C23 C24 119.0(2) . . C22 C23 C36 119.66(19) . . C24 C23 C36 121.18(19) . . C23 C24 H24 120.2 . . C25 C24 C23 119.5(2) . . C25 C24 H24 120.2 . . N4 C25 C24 120.60(19) . . N4 C25 C26 112.38(18) . . C24 C25 C26 126.83(19) . . N5 C26 C25 113.29(19) . . N5 C26 C27 122.1(2) . . C27 C26 C25 124.6(2) . . C26 C27 H27 120.6 . . C26 C27 C28 118.8(2) . . C28 C27 H27 120.6 . . C27 C28 H28 120.4 . . C29 C28 C27 119.2(2) . . C29 C28 H28 120.4 . . C28 C29 H29 120.4 . . C28 C29 C30 119.3(2) . . C30 C29 H29 120.4 . . N5 C30 C29 122.3(2) . . N5 C30 H30 118.8 . . C29 C30 H30 118.8 . . N6 C31 H31 118.6 . . N6 C31 C32 122.9(2) . . C32 C31 H31 118.6 . . C31 C32 H32 120.5 . . C31 C32 C33 119.0(2) . . C33 C32 H32 120.5 . . C32 C33 H33 120.4 . . C32 C33 C34 119.2(2) . . C34 C33 H33 120.4 . . C33 C34 H34 120.7 . . C35 C34 C33 118.6(2) . . C35 C34 H34 120.7 . . N6 C35 C21 113.92(19) . . N6 C35 C34 122.40(19) . . C34 C35 C21 123.5(2) . . C37 C36 C23 120.7(2) . . C37 C36 C40 117.2(2) . . C40 C36 C23 122.1(2) . . C36 C37 H37 120.3 . . C38 C37 C36 119.3(2) . . C38 C37 H37 120.3 . . N8 C38 C37 124.0(3) . . N8 C38 H38 118.0 . . C37 C38 H38 118.0 . . N8 C39 H39 117.7 . . N8 C39 C40 124.6(2) . . C40 C39 H39 117.7 . . C36 C40 H40 120.6 . . C39 C40 C36 118.8(2) . . C39 C40 H40 120.6 . . C54 C53 C55 117.5(2) . . C54 C53 C56 120.0(2) . . C55 C53 C56 122.2(2) . . N15 C54 C53 176.7(2) . . N16 C55 C53 179.4(3) . . C53 C56 C57 122.3(2) . . C53 C56 C61 119.9(2) . . C61 C56 C57 117.81(19) . . C56 C57 H57 119.5 . . C58 C57 C56 120.9(2) . . C58 C57 H57 119.5 . . C57 C58 H58 119.3 . . C57 C58 C59 121.4(2) . . C59 C58 H58 119.3 . . C60 C59 C58 117.28(19) . . C60 C59 C62 120.9(2) . . C62 C59 C58 121.8(2) . . C59 C60 H60 119.2 . . C61 C60 C59 121.6(2) . . C61 C60 H60 119.2 . . C56 C61 H61 119.5 . . C60 C61 C56 121.1(2) . . C60 C61 H61 119.5 . . C59 C62 C63 120.9(2) . . C64 C62 C59 121.4(2) . . C64 C62 C63 117.48(19) . . N13 C63 C62 179.5(2) . . N14 C64 C62 178.0(2) . . N10 C41 C43 178.6(3) . . N9 C42 C43 179.2(3) . . C41 C43 C42 115.7(2) . . C41 C43 C44 122.0(2) . . C42 C43 C44 122.1(2) . . C45 C44 C43 121.3(2) . . C49 C44 C43 121.7(2) . . C49 C44 C45 117.0(2) . . C44 C45 H45 119.3 . . C46 C45 C44 121.5(2) . . C46 C45 H45 119.3 . . C45 C46 H46 119.3 . . C45 C46 C47 121.4(2) . . C47 C46 H46 119.3 . . C46 C47 C48 117.1(2) . . C46 C47 C50 121.5(2) . . C50 C47 C48 121.4(2) . . C47 C48 H48 119.4 . . C49 C48 C47 121.3(2) . . C49 C48 H48 119.4 . . C44 C49 H49 119.1 . . C48 C49 C44 121.7(2) . . C48 C49 H49 119.1 . . C47 C50 C52 123.5(2) . . C51 C50 C47 120.6(2) . . C51 C50 C52 115.6(2) . . N11 C51 C50 179.2(3) . . N12 C52 C50 177.6(3) . . C65 N17 C66 121.7(4) . . C65 N17 C67 122.2(4) . . C66 N17 C67 116.1(3) . . O1 C65 N17 123.5(5) . . O1 C65 H65 118.2 . . N17 C65 H65 118.2 . . 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 1.973(2) . Co1 N2 2.244(2) . Co1 N3 2.225(2) . Co1 N4 1.901(2) . Co1 N5 2.029(2) . Co1 N6 2.037(2) . N1 C1 1.353(3) . N1 C5 1.358(3) . N2 C11 1.345(3) . N2 C15 1.357(3) . N3 C6 1.356(3) . N3 C10 1.339(3) . N4 C21 1.354(3) . N4 C25 1.360(3) . N5 C26 1.375(3) . N5 C30 1.343(3) . N6 C31 1.352(3) . N6 C35 1.360(3) . N7 C18 1.342(4) . N7 C19 1.328(3) . N8 C38 1.338(3) . N8 C39 1.336(4) . C1 C2 1.399(3) . C1 C15 1.492(3) . C2 H2 0.9300 . C2 C3 1.391(3) . C3 C4 1.403(3) . C3 C16 1.496(3) . C4 H4 0.9300 . C4 C5 1.393(3) . C5 C6 1.487(3) . C6 C7 1.397(3) . C7 H7 0.9300 . C7 C8 1.389(4) . C8 H8 0.9300 . C8 C9 1.386(4) . C9 H9 0.9300 . C9 C10 1.387(4) . C10 H10 0.9300 . C11 H11 0.9300 . C11 C12 1.388(4) . C12 H12 0.9300 . C12 C13 1.389(4) . C13 H13 0.9300 . C13 C14 1.392(3) . C14 H14 0.9300 . C14 C15 1.388(3) . C16 C17 1.391(4) . C16 C20 1.390(3) . C17 H17 0.9300 . C17 C18 1.390(4) . C18 H18 0.9300 . C19 H19 0.9300 . C19 C20 1.392(3) . C20 H20 0.9300 . C21 C22 1.399(3) . C21 C35 1.486(3) . C22 H22 0.9300 . C22 C23 1.400(3) . C23 C24 1.401(3) . C23 C36 1.498(3) . C24 H24 0.9300 . C24 C25 1.394(3) . C25 C26 1.482(3) . C26 C27 1.387(3) . C27 H27 0.9300 . C27 C28 1.400(4) . C28 H28 0.9300 . C28 C29 1.385(4) . C29 H29 0.9300 . C29 C30 1.396(4) . C30 H30 0.9300 . C31 H31 0.9300 . C31 C32 1.384(3) . C32 H32 0.9300 . C32 C33 1.388(4) . C33 H33 0.9300 . C33 C34 1.394(3) . C34 H34 0.9300 . C34 C35 1.394(3) . C36 C37 1.395(3) . C36 C40 1.398(3) . C37 H37 0.9300 . C37 C38 1.392(3) . C38 H38 0.9300 . C39 H39 0.9300 . C39 C40 1.390(3) . C40 H40 0.9300 . N13 C63 1.160(3) . N14 C64 1.165(3) . N15 C54 1.167(3) . N16 C55 1.160(3) . C53 C54 1.417(4) . C53 C55 1.425(3) . C53 C56 1.427(3) . C56 C57 1.431(3) . C56 C61 1.427(3) . C57 H57 0.9300 . C57 C58 1.366(3) . C58 H58 0.9300 . C58 C59 1.437(3) . C59 C60 1.423(3) . C59 C62 1.426(3) . C60 H60 0.9300 . C60 C61 1.367(3) . C61 H61 0.9300 . C62 C63 1.428(3) . C62 C64 1.417(3) . N9 C42 1.159(4) . N10 C41 1.158(4) . N11 C51 1.150(4) . N12 C52 1.156(4) . C41 C43 1.418(4) . C42 C43 1.422(4) . C43 C44 1.430(3) . C44 C45 1.423(4) . C44 C49 1.422(4) . C45 H45 0.9300 . C45 C46 1.372(4) . C46 H46 0.9300 . C46 C47 1.421(4) . C47 C48 1.427(4) . C47 C50 1.424(3) . C48 H48 0.9300 . C48 C49 1.369(4) . C49 H49 0.9300 . C50 C51 1.424(4) . C50 C52 1.432(4) . O1 C65 1.222(5) . N17 C65 1.332(5) . N17 C66 1.463(5) . N17 C67 1.480(5) . C65 H65 0.9300 . C66 H66A 0.9600 . C66 H66B 0.9600 . C66 H66C 0.9600 . C67 H67A 0.9600 . C67 H67B 0.9600 . C67 H67C 0.9600 . O2 H2A 0.8200 . O2 C68 1.379(5) . C68 H68A 0.9600 . C68 H68B 0.9600 . C68 H68C 0.9600 .