#------------------------------------------------------------------------------ #$Date: 2019-10-07 12:55:59 +0300 (Mon, 07 Oct 2019) $ #$Revision: 219132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234432.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_7234432 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, C0.61 O0.25, 2(C12 H4 N4), C3 H7 N O' _chemical_formula_sum 'C67.61 H43 Co N17 O1.25' _chemical_formula_weight 1172.44 _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 105.759(6) _cell_angle_beta 95.448(6) _cell_angle_gamma 94.088(6) _cell_formula_units_Z 2 _cell_length_a 8.986(4) _cell_length_b 13.909(6) _cell_length_c 24.825(11) _cell_measurement_reflns_used 5855 _cell_measurement_temperature 300.15 _cell_measurement_theta_max 21.90 _cell_measurement_theta_min 2.29 _cell_volume 2957(2) _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 300.15 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _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 0.0424 _diffrn_reflns_av_unetI/netI 0.0584 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _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 33075 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.733 _diffrn_reflns_theta_min 1.529 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0820 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.9194. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.317 _exptl_crystal_description needle _exptl_crystal_F_000 1209 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.201 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.046 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 797 _refine_ls_number_reflns 12505 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0475 _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^)+(0.0467P)^2^+0.3909P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.1195 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8014 _reflns_number_total 12505 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-9292.cif _cod_data_source_block 8-300K _cod_database_code 7234432 _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 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), C45(H45), C46(H46), C48(H48), C49(H49), C57(H57), C58(H58), C60(H60), C61(H61), C65(H65) 2.b Idealised Me refined as rotating group: C66(H66A,H66B,H66C), C67(H67A,H67B,H67C) ; _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 0.178, Rweak 0.011, Alpha 0.061, Orientation as input REM Formula found by SHELXT: C69 N12 O2 Co CELL 0.71073 8.986 13.9093 24.825 105.759 95.448 94.088 ZERR 2 0.004 0.0063 0.0111 0.006 0.006 0.006 LATT 1 SFAC C H Co N O UNIT 135.22 86 2 34 2.5 L.S. 10 PLAN 20 SIZE 0.08 0.13 0.25 TEMP 27 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.046700 0.390900 FVAR 0.36953 CO1 3 0.130585 0.586279 0.763482 11.00000 0.04351 0.04614 = 0.02617 0.01720 0.00456 0.01081 N1 4 0.119047 0.579899 0.682917 11.00000 0.04177 0.04502 = 0.03392 0.01550 0.00476 0.01451 N2 4 0.336405 0.517536 0.738427 11.00000 0.05115 0.05839 = 0.03122 0.02033 0.00425 0.01718 N3 4 -0.086118 0.642902 0.747145 11.00000 0.05353 0.05867 = 0.03683 0.02181 0.01209 0.01538 N4 4 0.166184 0.595818 0.842258 11.00000 0.04029 0.04110 = 0.03142 0.01472 0.00358 0.00667 N5 4 0.243523 0.727349 0.793206 11.00000 0.05125 0.05542 = 0.03669 0.02525 0.00786 0.01289 N6 4 0.030067 0.450399 0.764201 11.00000 0.04888 0.05427 = 0.02954 0.01205 -0.00269 0.01321 N7 4 0.155357 0.633493 0.408908 11.00000 0.08388 0.10091 = 0.03723 0.03172 0.00330 0.01403 N8 4 0.445810 0.587709 1.115933 11.00000 0.11083 0.07718 = 0.04634 0.02903 -0.01699 0.00044 C1 1 0.230353 0.543908 0.652797 11.00000 0.04297 0.04709 = 0.03219 0.01370 0.00520 0.01243 C2 1 0.236411 0.552359 0.598956 11.00000 0.04629 0.06128 = 0.03574 0.01716 0.00865 0.02005 AFIX 43 H2 2 0.313160 0.525886 0.578730 11.00000 -1.20000 AFIX 0 C3 1 0.129644 0.599765 0.574659 11.00000 0.04722 0.04798 = 0.03070 0.01398 0.00150 0.00922 C4 1 0.015815 0.636162 0.606363 11.00000 0.04827 0.05267 = 0.03555 0.01830 0.00341 0.01724 AFIX 43 H4 2 -0.058082 0.668510 0.591541 11.00000 -1.20000 AFIX 0 C5 1 0.011817 0.624626 0.659498 11.00000 0.03992 0.04836 = 0.03267 0.01446 0.00247 0.01148 C6 1 -0.107344 0.657518 0.695700 11.00000 0.04614 0.05537 = 0.03865 0.01900 0.00977 0.01788 C7 1 -0.231750 0.697515 0.678306 11.00000 0.06740 0.09841 = 0.04958 0.03699 0.01660 0.04345 AFIX 43 H7 2 -0.243377 0.707626 0.642682 11.00000 -1.20000 AFIX 0 C8 1 -0.340061 0.722735 0.714390 11.00000 0.06563 0.11978 = 0.06958 0.03977 0.02250 0.05367 AFIX 43 H8 2 -0.424960 0.750585 0.703509 11.00000 -1.20000 AFIX 0 C9 1 -0.320261 0.706056 0.766282 11.00000 0.06545 0.09527 = 0.06472 0.03191 0.03258 0.03660 AFIX 43 H9 2 -0.392502 0.720907 0.790947 11.00000 -1.20000 AFIX 0 C10 1 -0.192327 0.667148 0.781249 11.00000 0.06770 0.07352 = 0.04714 0.02730 0.02324 0.02258 AFIX 43 H10 2 -0.178574 0.657081 0.816849 11.00000 -1.20000 AFIX 0 C11 1 0.439230 0.481861 0.768620 11.00000 0.05955 0.07303 = 0.04109 0.02706 0.00413 0.02276 AFIX 43 H11 2 0.435116 0.494117 0.807161 11.00000 -1.20000 AFIX 0 C12 1 0.550034 0.428107 0.744958 11.00000 0.06071 0.09552 = 0.05474 0.03563 0.00455 0.03867 AFIX 43 H12 2 0.620787 0.405389 0.767172 11.00000 -1.20000 AFIX 0 C13 1 0.555057 0.408281 0.687965 11.00000 0.06768 0.10167 = 0.05800 0.03631 0.01990 0.04739 AFIX 43 H13 2 0.628524 0.371063 0.670964 11.00000 -1.20000 AFIX 0 C14 1 0.450661 0.443890 0.656314 11.00000 0.06269 0.09007 = 0.04042 0.02706 0.01404 0.04069 AFIX 43 H14 2 0.451882 0.430681 0.617579 11.00000 -1.20000 AFIX 0 C15 1 0.344524 0.499214 0.682588 11.00000 0.04362 0.05410 = 0.03681 0.01955 0.00543 0.01501 C16 1 0.137516 0.612248 0.517595 11.00000 0.05000 0.05353 = 0.03000 0.01507 0.00135 0.00710 C17 1 0.058764 0.679260 0.498197 11.00000 0.09446 0.10950 = 0.04453 0.04228 0.01978 0.05273 AFIX 43 H17 2 -0.001935 0.719553 0.521127 11.00000 -1.20000 AFIX 0 C18 1 0.070094 0.686568 0.444447 11.00000 0.11810 0.12741 = 0.05663 0.05492 0.01742 0.05849 AFIX 43 H18 2 0.014038 0.731905 0.432166 11.00000 -1.20000 AFIX 0 C19 1 0.230385 0.570173 0.428466 11.00000 0.07267 0.08395 = 0.03813 0.01664 0.01445 0.01053 AFIX 43 H19 2 0.291226 0.531398 0.404840 11.00000 -1.20000 AFIX 0 C20 1 0.226125 0.556683 0.481026 11.00000 0.06148 0.06535 = 0.03572 0.01777 0.00753 0.01583 AFIX 43 H20 2 0.282754 0.510264 0.491939 11.00000 -1.20000 AFIX 0 C21 1 0.124965 0.516648 0.860578 11.00000 0.04054 0.04608 = 0.03023 0.01533 0.00554 0.00779 C22 1 0.169037 0.516030 0.915364 11.00000 0.05109 0.04590 = 0.03186 0.01819 0.00356 0.00248 AFIX 43 H22 2 0.138588 0.461203 0.927763 11.00000 -1.20000 AFIX 0 C23 1 0.259029 0.597606 0.951901 11.00000 0.04743 0.04640 = 0.02923 0.01522 0.00517 0.00818 C24 1 0.297282 0.679580 0.932387 11.00000 0.04949 0.04413 = 0.03213 0.01282 0.00393 0.00482 AFIX 43 H24 2 0.353801 0.736309 0.956346 11.00000 -1.20000 AFIX 0 C25 1 0.250946 0.676422 0.877200 11.00000 0.04215 0.04386 = 0.03084 0.01587 0.00845 0.01259 C26 1 0.294724 0.752940 0.849065 11.00000 0.04284 0.04479 = 0.03277 0.01484 0.00843 0.01363 C27 1 0.385610 0.839904 0.875294 11.00000 0.05480 0.04574 = 0.04224 0.01238 0.00997 0.00849 AFIX 43 H27 2 0.419084 0.855698 0.913578 11.00000 -1.20000 AFIX 0 C28 1 0.426626 0.903663 0.843913 11.00000 0.06520 0.04378 = 0.06242 0.01791 0.01809 0.00515 AFIX 43 H28 2 0.488856 0.962659 0.860783 11.00000 -1.20000 AFIX 0 C29 1 0.374291 0.878824 0.787394 11.00000 0.07322 0.05339 = 0.06193 0.03234 0.01862 0.01294 AFIX 43 H29 2 0.400383 0.920676 0.765526 11.00000 -1.20000 AFIX 0 C30 1 0.283218 0.791404 0.764094 11.00000 0.06787 0.06098 = 0.04214 0.02906 0.00989 0.01450 AFIX 43 H30 2 0.246906 0.775549 0.726056 11.00000 -1.20000 AFIX 0 C31 1 -0.041390 0.377764 0.720298 11.00000 0.06233 0.06344 = 0.03861 0.00862 -0.00864 0.01556 AFIX 43 H31 2 -0.049980 0.388738 0.684861 11.00000 -1.20000 AFIX 0 C32 1 -0.102148 0.288228 0.725478 11.00000 0.07274 0.05558 = 0.05944 0.00384 -0.01906 0.00553 AFIX 43 H32 2 -0.150894 0.239430 0.694103 11.00000 -1.20000 AFIX 0 C33 1 -0.090269 0.271361 0.777485 11.00000 0.07871 0.04937 = 0.06970 0.01680 -0.01243 -0.00514 AFIX 43 H33 2 -0.131104 0.210915 0.781773 11.00000 -1.20000 AFIX 0 C34 1 -0.017181 0.344784 0.823543 11.00000 0.06982 0.05194 = 0.04801 0.02154 -0.00732 -0.00027 AFIX 43 H34 2 -0.007622 0.334479 0.859138 11.00000 -1.20000 AFIX 0 C35 1 0.041022 0.433250 0.815671 11.00000 0.04508 0.04570 = 0.03405 0.01517 -0.00012 0.00742 C36 1 0.321087 0.594787 1.008993 11.00000 0.05917 0.04619 = 0.03002 0.01367 0.00040 0.00774 C37 1 0.243078 0.546397 1.041149 11.00000 0.07151 0.05743 = 0.03510 0.01967 0.00355 0.00435 AFIX 43 H37 2 0.146665 0.514933 1.027753 11.00000 -1.20000 AFIX 0 C38 1 0.309812 0.545346 1.093220 11.00000 0.10262 0.07259 = 0.03937 0.02803 0.00970 0.00971 AFIX 43 H38 2 0.254957 0.512290 1.113988 11.00000 -1.20000 AFIX 0 C39 1 0.520463 0.633227 1.084581 11.00000 0.09066 0.07368 = 0.06325 0.02814 -0.02818 -0.00463 AFIX 43 H39 2 0.616825 0.663658 1.099150 11.00000 -1.20000 AFIX 0 C40 1 0.464483 0.638401 1.031714 11.00000 0.07034 0.06516 = 0.04841 0.02758 -0.00843 -0.00178 AFIX 43 H40 2 0.522724 0.670903 1.011636 11.00000 -1.20000 AFIX 0 O2 5 0.713803 0.057810 0.828542 0.24853 0.16341 0.16615 = 0.12979 0.06967 0.00624 0.03087 N9 4 0.621066 0.028781 0.713127 11.00000 0.17078 0.14397 = 0.07066 0.03855 0.01548 0.03358 N10 4 0.890126 -0.144369 0.593249 11.00000 0.11765 0.09760 = 0.11197 0.04078 -0.00373 0.04919 N11 4 0.361940 0.344983 0.485242 11.00000 0.13930 0.08990 = 0.17684 0.06066 0.01377 0.05648 N12 4 0.637927 0.184013 0.364719 11.00000 0.11861 0.11291 = 0.08077 0.05159 0.00486 -0.00140 C41 1 0.807311 -0.085436 0.602094 11.00000 0.09210 0.07120 = 0.07284 0.03201 -0.01004 0.01927 C42 1 0.659081 0.010853 0.668895 11.00000 0.10840 0.08126 = 0.06738 0.03094 -0.00448 0.01919 C43 1 0.706940 -0.010861 0.614239 11.00000 0.08026 0.06493 = 0.05724 0.02454 -0.00439 0.01627 C44 1 0.664783 0.043328 0.575553 11.00000 0.06754 0.05223 = 0.05403 0.01813 -0.00182 0.01122 C45 1 0.565575 0.118835 0.588319 11.00000 0.08019 0.05970 = 0.05860 0.01649 0.01015 0.01883 AFIX 43 H45 2 0.528649 0.133601 0.623083 11.00000 -1.20000 AFIX 0 C46 1 0.523249 0.169938 0.551263 11.00000 0.07630 0.05638 = 0.06701 0.01986 0.01002 0.02174 AFIX 43 H46 2 0.457414 0.218767 0.560989 11.00000 -1.20000 AFIX 0 C47 1 0.576977 0.150784 0.497854 11.00000 0.06577 0.04385 = 0.06490 0.02102 -0.00344 0.00804 C48 1 0.676176 0.076135 0.485335 11.00000 0.08381 0.06238 = 0.05710 0.02211 0.01164 0.02114 AFIX 43 H48 2 0.714723 0.062030 0.450880 11.00000 -1.20000 AFIX 0 C49 1 0.716727 0.024308 0.522540 11.00000 0.08473 0.05812 = 0.06237 0.02266 0.01117 0.02790 AFIX 43 H49 2 0.781034 -0.025422 0.512553 11.00000 -1.20000 AFIX 0 C50 1 0.534171 0.204265 0.459003 11.00000 0.06847 0.05431 = 0.07502 0.02897 -0.00231 0.00661 C51 1 0.438313 0.282414 0.473062 11.00000 0.09432 0.06591 = 0.10281 0.04223 -0.00748 0.01654 C52 1 0.592224 0.191381 0.406879 11.00000 0.08251 0.06847 = 0.07755 0.04099 -0.00549 0.00019 C68 1 0.666649 0.144755 0.853795 0.60837 0.47195 0.31856 = 0.35433 0.16172 0.26932 0.12091 N13 4 1.495319 1.122384 0.977148 11.00000 0.06507 0.06447 = 0.07697 0.01968 -0.00763 -0.00232 N14 4 1.161751 1.158198 0.845273 11.00000 0.11405 0.10597 = 0.08583 0.06191 0.00532 0.01175 N15 4 0.949221 0.678866 1.038099 11.00000 0.08878 0.06451 = 0.07609 0.03939 0.00497 0.00470 N16 4 0.620259 0.687455 0.898003 11.00000 0.05693 0.07746 = 0.06840 0.02876 0.00768 0.00303 C53 1 1.376790 1.104874 0.953294 11.00000 0.05979 0.04225 = 0.05042 0.01365 0.00450 0.00378 C54 1 1.193808 1.122651 0.880367 11.00000 0.06377 0.06162 = 0.05823 0.02815 0.00941 0.00326 C55 1 1.232045 1.077378 0.923586 11.00000 0.04960 0.05111 = 0.04595 0.01881 0.00490 0.00651 C56 1 1.137279 1.000185 0.933288 11.00000 0.04633 0.04509 = 0.03773 0.01257 0.00685 0.00779 C57 1 1.000013 0.961300 0.899275 11.00000 0.05371 0.05184 = 0.04075 0.02017 0.00138 0.00452 AFIX 43 H57 2 0.969407 0.988133 0.870056 11.00000 -1.20000 AFIX 0 C58 1 0.911914 0.885530 0.908409 11.00000 0.05040 0.05213 = 0.03904 0.01476 -0.00204 0.00415 AFIX 43 H58 2 0.821909 0.861335 0.885290 11.00000 -1.20000 AFIX 0 C59 1 0.953999 0.842125 0.952586 11.00000 0.05038 0.04346 = 0.03920 0.01451 0.00850 0.01069 C60 1 1.091647 0.881200 0.986125 11.00000 0.05491 0.04766 = 0.04181 0.01972 0.00259 0.01130 AFIX 43 H60 2 1.123067 0.854356 1.015252 11.00000 -1.20000 AFIX 0 C61 1 1.179041 0.956852 0.976894 11.00000 0.04748 0.04728 = 0.04257 0.01325 0.00150 0.00903 AFIX 43 H61 2 1.269186 0.980990 0.999930 11.00000 -1.20000 AFIX 0 C62 1 0.863014 0.762765 0.962311 11.00000 0.05298 0.04630 = 0.04625 0.01838 0.00839 0.00834 C63 1 0.910072 0.716773 1.004234 11.00000 0.05748 0.04430 = 0.05483 0.01949 0.00822 0.00334 C64 1 0.728534 0.721091 0.927594 11.00000 0.05204 0.05045 = 0.05080 0.02162 0.01505 0.00967 O1 5 -0.196741 0.781459 0.378300 11.00000 0.23814 0.45286 = 0.34554 0.29757 0.11436 0.17853 N17 4 -0.208410 0.872219 0.317697 11.00000 0.14287 0.14852 = 0.12727 0.05838 0.03340 0.05640 C65 1 -0.158896 0.861799 0.367018 11.00000 0.22729 0.36511 = 0.19843 0.18510 0.09872 0.18457 AFIX 43 H65 2 -0.096792 0.913060 0.393198 11.00000 -1.20000 AFIX 0 C66 1 -0.167796 0.964236 0.303559 11.00000 0.28616 0.12979 = 0.19904 0.07291 -0.00862 0.00524 AFIX 137 H66A 2 -0.106397 0.950531 0.273282 11.00000 -1.50000 H66B 2 -0.112830 1.012238 0.335926 11.00000 -1.50000 H66C 2 -0.257233 0.990953 0.292094 11.00000 -1.50000 AFIX 0 C67 1 -0.306627 0.794701 0.273659 11.00000 0.17837 0.18707 = 0.19222 0.01710 0.02983 -0.03743 AFIX 137 H67A 2 -0.322435 0.735460 0.285995 11.00000 -1.50000 H67B 2 -0.259867 0.778653 0.239551 11.00000 -1.50000 H67C 2 -0.401475 0.819561 0.266781 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad_a.res in P-1 REM R1 = 0.0475 for 8014 Fo > 4sig(Fo) and 0.0871 for all 12505 data REM 797 parameters refined using 0 restraints END WGHT 0.0467 0.3909 REM Highest difference peak 0.201, deepest hole -0.299, 1-sigma level 0.046 Q1 1 0.0215 0.6406 0.7488 11.00000 0.05 0.20 Q2 1 0.4108 0.3273 0.4515 11.00000 0.05 0.20 Q3 1 -0.4246 1.0378 0.3357 11.00000 0.05 0.18 Q4 1 0.6784 0.0227 0.4323 11.00000 0.05 0.17 Q5 1 0.0581 0.7755 0.5265 11.00000 0.05 0.17 Q6 1 -0.3815 0.2413 0.7104 11.00000 0.05 0.16 Q7 1 -0.0775 0.6803 0.5168 11.00000 0.05 0.16 Q8 1 0.0931 0.5469 0.7115 11.00000 0.05 0.16 Q9 1 0.8754 0.9722 0.9116 11.00000 0.05 0.16 Q10 1 1.4675 1.0611 0.9387 11.00000 0.05 0.16 Q11 1 0.5621 0.0182 0.7542 11.00000 0.05 0.16 Q12 1 0.7464 -0.0402 0.8296 11.00000 0.05 0.16 Q13 1 0.1714 0.5588 0.8018 11.00000 0.05 0.16 Q14 1 0.5793 0.0441 0.7639 11.00000 0.05 0.15 Q15 1 0.8201 0.0782 0.6569 11.00000 0.05 0.15 Q16 1 -0.0016 0.7579 0.7793 11.00000 0.05 0.15 Q17 1 0.2431 0.5186 0.7416 11.00000 0.05 0.15 Q18 1 -0.2657 0.6590 0.6314 11.00000 0.05 0.15 Q19 1 0.3777 0.5202 0.8319 11.00000 0.05 0.15 Q20 1 0.6067 -0.0472 0.5873 11.00000 0.05 0.15 ; _shelx_res_checksum 45071 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 0.13058(3) 0.58628(2) 0.76348(2) 0.03687(10) Uani 1 1 d . . . . . N1 N 0.1190(2) 0.57990(14) 0.68292(7) 0.0388(4) Uani 1 1 d . . . . . N2 N 0.3364(2) 0.51754(15) 0.73843(8) 0.0448(5) Uani 1 1 d . . . . . N3 N -0.0861(2) 0.64290(15) 0.74715(8) 0.0471(5) Uani 1 1 d . . . . . N4 N 0.1662(2) 0.59582(14) 0.84226(7) 0.0366(4) Uani 1 1 d . . . . . N5 N 0.2435(2) 0.72735(15) 0.79321(8) 0.0448(5) Uani 1 1 d . . . . . N6 N 0.0301(2) 0.45040(15) 0.76420(8) 0.0443(5) Uani 1 1 d . . . . . N7 N 0.1554(3) 0.6335(2) 0.40891(9) 0.0716(7) Uani 1 1 d . . . . . N8 N 0.4458(3) 0.5877(2) 1.11593(10) 0.0780(8) Uani 1 1 d . . . . . C1 C 0.2304(3) 0.54391(17) 0.65280(9) 0.0398(5) Uani 1 1 d . . . . . C2 C 0.2364(3) 0.55236(18) 0.59896(9) 0.0461(6) Uani 1 1 d . . . . . H2 H 0.3132 0.5259 0.5787 0.055 Uiso 1 1 calc R . . . . C3 C 0.1296(3) 0.59977(17) 0.57466(9) 0.0414(6) Uani 1 1 d . . . . . C4 C 0.0158(3) 0.63616(18) 0.60636(9) 0.0438(6) Uani 1 1 d . . . . . H4 H -0.0581 0.6685 0.5915 0.053 Uiso 1 1 calc R . . . . C5 C 0.0118(2) 0.62463(17) 0.65950(9) 0.0395(5) Uani 1 1 d . . . . . C6 C -0.1073(3) 0.65752(18) 0.69570(10) 0.0446(6) Uani 1 1 d . . . . . C7 C -0.2318(3) 0.6975(2) 0.67831(11) 0.0662(8) Uani 1 1 d . . . . . H7 H -0.2434 0.7076 0.6427 0.079 Uiso 1 1 calc R . . . . C8 C -0.3401(3) 0.7227(3) 0.71439(13) 0.0792(10) Uani 1 1 d . . . . . H8 H -0.4250 0.7506 0.7035 0.095 Uiso 1 1 calc R . . . . C9 C -0.3203(3) 0.7061(2) 0.76628(12) 0.0702(9) Uani 1 1 d . . . . . H9 H -0.3925 0.7209 0.7909 0.084 Uiso 1 1 calc R . . . . C10 C -0.1923(3) 0.6671(2) 0.78125(11) 0.0589(7) Uani 1 1 d . . . . . H10 H -0.1786 0.6571 0.8168 0.071 Uiso 1 1 calc R . . . . C11 C 0.4392(3) 0.4819(2) 0.76862(11) 0.0550(7) Uani 1 1 d . . . . . H11 H 0.4351 0.4941 0.8072 0.066 Uiso 1 1 calc R . . . . C12 C 0.5500(3) 0.4281(2) 0.74496(11) 0.0661(8) Uani 1 1 d . . . . . H12 H 0.6208 0.4054 0.7672 0.079 Uiso 1 1 calc R . . . . C13 C 0.5551(3) 0.4083(2) 0.68797(12) 0.0703(9) Uani 1 1 d . . . . . H13 H 0.6285 0.3711 0.6710 0.084 Uiso 1 1 calc R . . . . C14 C 0.4507(3) 0.4439(2) 0.65631(11) 0.0605(8) Uani 1 1 d . . . . . H14 H 0.4519 0.4307 0.6176 0.073 Uiso 1 1 calc R . . . . C15 C 0.3445(3) 0.49921(18) 0.68259(9) 0.0430(6) Uani 1 1 d . . . . . C16 C 0.1375(3) 0.61225(18) 0.51759(9) 0.0440(6) Uani 1 1 d . . . . . C17 C 0.0588(4) 0.6793(2) 0.49820(11) 0.0758(10) Uani 1 1 d . . . . . H17 H -0.0019 0.7196 0.5211 0.091 Uiso 1 1 calc R . . . . C18 C 0.0701(4) 0.6866(3) 0.44445(13) 0.0922(12) Uani 1 1 d . . . . . H18 H 0.0140 0.7319 0.4322 0.111 Uiso 1 1 calc R . . . . C19 C 0.2304(3) 0.5702(2) 0.42847(11) 0.0644(8) Uani 1 1 d . . . . . H19 H 0.2912 0.5314 0.4048 0.077 Uiso 1 1 calc R . . . . C20 C 0.2261(3) 0.5567(2) 0.48103(10) 0.0529(7) Uani 1 1 d . . . . . H20 H 0.2828 0.5103 0.4919 0.063 Uiso 1 1 calc R . . . . C21 C 0.1250(2) 0.51665(17) 0.86058(9) 0.0378(5) Uani 1 1 d . . . . . C22 C 0.1690(3) 0.51603(18) 0.91536(9) 0.0417(6) Uani 1 1 d . . . . . H22 H 0.1386 0.4612 0.9278 0.050 Uiso 1 1 calc R . . . . C23 C 0.2590(3) 0.59761(17) 0.95190(9) 0.0399(5) Uani 1 1 d . . . . . C24 C 0.2973(3) 0.67958(17) 0.93239(9) 0.0416(6) Uani 1 1 d . . . . . H24 H 0.3538 0.7363 0.9563 0.050 Uiso 1 1 calc R . . . . C25 C 0.2509(2) 0.67642(17) 0.87720(9) 0.0372(5) Uani 1 1 d . . . . . C26 C 0.2947(3) 0.75294(17) 0.84907(9) 0.0386(5) Uani 1 1 d . . . . . C27 C 0.3856(3) 0.83990(18) 0.87529(10) 0.0471(6) Uani 1 1 d . . . . . H27 H 0.4191 0.8557 0.9136 0.057 Uiso 1 1 calc R . . . . C28 C 0.4266(3) 0.90366(19) 0.84391(12) 0.0559(7) Uani 1 1 d . . . . . H28 H 0.4889 0.9627 0.8608 0.067 Uiso 1 1 calc R . . . . C29 C 0.3743(3) 0.8788(2) 0.78739(12) 0.0586(7) Uani 1 1 d . . . . . H29 H 0.4004 0.9207 0.7655 0.070 Uiso 1 1 calc R . . . . C30 C 0.2832(3) 0.7914(2) 0.76409(11) 0.0535(7) Uani 1 1 d . . . . . H30 H 0.2469 0.7755 0.7261 0.064 Uiso 1 1 calc R . . . . C31 C -0.0414(3) 0.3778(2) 0.72030(11) 0.0564(7) Uani 1 1 d . . . . . H31 H -0.0500 0.3887 0.6849 0.068 Uiso 1 1 calc R . . . . C32 C -0.1021(3) 0.2882(2) 0.72548(12) 0.0669(8) Uani 1 1 d . . . . . H32 H -0.1509 0.2394 0.6941 0.080 Uiso 1 1 calc R . . . . C33 C -0.0903(3) 0.2714(2) 0.77748(13) 0.0679(8) Uani 1 1 d . . . . . H33 H -0.1311 0.2109 0.7818 0.081 Uiso 1 1 calc R . . . . C34 C -0.0172(3) 0.34478(19) 0.82354(11) 0.0564(7) Uani 1 1 d . . . . . H34 H -0.0076 0.3345 0.8591 0.068 Uiso 1 1 calc R . . . . C35 C 0.0410(3) 0.43325(18) 0.81567(9) 0.0410(6) Uani 1 1 d . . . . . C36 C 0.3211(3) 0.59479(18) 1.00899(9) 0.0447(6) Uani 1 1 d . . . . . C37 C 0.2431(3) 0.54640(19) 1.04115(10) 0.0537(7) Uani 1 1 d . . . . . H37 H 0.1467 0.5149 1.0278 0.064 Uiso 1 1 calc R . . . . C38 C 0.3098(4) 0.5453(2) 1.09322(11) 0.0690(8) Uani 1 1 d . . . . . H38 H 0.2550 0.5123 1.1140 0.083 Uiso 1 1 calc R . . . . C39 C 0.5205(4) 0.6332(2) 1.08458(13) 0.0772(9) Uani 1 1 d . . . . . H39 H 0.6168 0.6637 1.0992 0.093 Uiso 1 1 calc R . . . . C40 C 0.4645(3) 0.6384(2) 1.03171(11) 0.0605(7) Uani 1 1 d . . . . . H40 H 0.5227 0.6709 1.0116 0.073 Uiso 1 1 calc R . . . . O2 O 0.7138(19) 0.0578(16) 0.8285(7) 0.148(10) Uani 0.249(16) 1 d . . . . . N9 N 0.6211(4) 0.0288(3) 0.71313(14) 0.1258(13) Uani 1 1 d . . . . . N10 N 0.8901(4) -0.1444(2) 0.59325(13) 0.1061(11) Uani 1 1 d . . . . . N11 N 0.3619(4) 0.3450(2) 0.48524(16) 0.1288(13) Uani 1 1 d . . . . . N12 N 0.6379(4) 0.1840(2) 0.36472(13) 0.1004(10) Uani 1 1 d . . . . . C41 C 0.8073(4) -0.0854(3) 0.60209(13) 0.0772(9) Uani 1 1 d . . . . . C42 C 0.6591(4) 0.0109(3) 0.66889(16) 0.0842(10) Uani 1 1 d . . . . . C43 C 0.7069(3) -0.0109(2) 0.61424(12) 0.0664(8) Uani 1 1 d . . . . . C44 C 0.6648(3) 0.0433(2) 0.57555(11) 0.0576(7) Uani 1 1 d . . . . . C45 C 0.5656(3) 0.1188(2) 0.58832(12) 0.0655(8) Uani 1 1 d . . . . . H45 H 0.5286 0.1336 0.6231 0.079 Uiso 1 1 calc R . . . . C46 C 0.5232(3) 0.1699(2) 0.55126(12) 0.0652(8) Uani 1 1 d . . . . . H46 H 0.4574 0.2188 0.5610 0.078 Uiso 1 1 calc R . . . . C47 C 0.5770(3) 0.15078(19) 0.49785(12) 0.0577(7) Uani 1 1 d . . . . . C48 C 0.6762(3) 0.0761(2) 0.48534(12) 0.0658(8) Uani 1 1 d . . . . . H48 H 0.7147 0.0620 0.4509 0.079 Uiso 1 1 calc R . . . . C49 C 0.7167(3) 0.0243(2) 0.52254(12) 0.0661(8) Uani 1 1 d . . . . . H49 H 0.7810 -0.0254 0.5126 0.079 Uiso 1 1 calc R . . . . C50 C 0.5342(3) 0.2043(2) 0.45900(13) 0.0645(8) Uani 1 1 d . . . . . C51 C 0.4383(4) 0.2824(3) 0.47306(15) 0.0849(10) Uani 1 1 d . . . . . C52 C 0.5922(4) 0.1914(2) 0.40688(16) 0.0735(9) Uani 1 1 d . . . . . C68 C 0.667(2) 0.145(2) 0.8538(8) 0.349(15) Uani 0.61(3) 1 d . . . . . N13 N 1.4953(3) 1.12238(18) 0.97715(11) 0.0704(7) Uani 1 1 d . . . . . N14 N 1.1618(3) 1.1582(2) 0.84527(12) 0.0954(9) Uani 1 1 d . . . . . N15 N 0.9492(3) 0.67887(18) 1.03810(11) 0.0730(7) Uani 1 1 d . . . . . N16 N 0.6203(3) 0.68745(18) 0.89800(10) 0.0661(7) Uani 1 1 d . . . . . C53 C 1.3768(3) 1.10487(18) 0.95329(11) 0.0509(6) Uani 1 1 d . . . . . C54 C 1.1938(3) 1.1227(2) 0.88037(12) 0.0590(7) Uani 1 1 d . . . . . C55 C 1.2320(3) 1.07738(18) 0.92359(10) 0.0478(6) Uani 1 1 d . . . . . C56 C 1.1373(3) 1.00019(17) 0.93329(10) 0.0426(6) Uani 1 1 d . . . . . C57 C 1.0000(3) 0.96130(18) 0.89928(10) 0.0477(6) Uani 1 1 d . . . . . H57 H 0.9694 0.9881 0.8701 0.057 Uiso 1 1 calc R . . . . C58 C 0.9119(3) 0.88553(18) 0.90841(10) 0.0473(6) Uani 1 1 d . . . . . H58 H 0.8219 0.8613 0.8853 0.057 Uiso 1 1 calc R . . . . C59 C 0.9540(3) 0.84212(17) 0.95259(10) 0.0433(6) Uani 1 1 d . . . . . C60 C 1.0916(3) 0.88120(18) 0.98612(10) 0.0466(6) Uani 1 1 d . . . . . H60 H 1.1231 0.8544 1.0153 0.056 Uiso 1 1 calc R . . . . C61 C 1.1790(3) 0.95685(18) 0.97689(10) 0.0457(6) Uani 1 1 d . . . . . H61 H 1.2692 0.9810 0.9999 0.055 Uiso 1 1 calc R . . . . C62 C 0.8630(3) 0.76276(18) 0.96231(10) 0.0471(6) Uani 1 1 d . . . . . C63 C 0.9101(3) 0.71677(19) 1.00423(11) 0.0511(6) Uani 1 1 d . . . . . C64 C 0.7285(3) 0.72109(19) 0.92759(11) 0.0488(6) Uani 1 1 d . . . . . O1 O -0.1967(7) 0.7815(6) 0.3783(3) 0.296(4) Uani 1 1 d . . . . . N17 N -0.2084(5) 0.8722(4) 0.3177(2) 0.1324(13) Uani 1 1 d . . . . . C65 C -0.1589(9) 0.8618(7) 0.3670(3) 0.230(5) Uani 1 1 d . . . . . H65 H -0.0968 0.9131 0.3932 0.276 Uiso 1 1 calc R . . . . C66 C -0.1678(7) 0.9642(4) 0.3036(3) 0.203(3) Uani 1 1 d . . . . . H66A H -0.1064 0.9505 0.2733 0.304 Uiso 1 1 calc GR . . . . H66B H -0.1128 1.0122 0.3359 0.304 Uiso 1 1 calc GR . . . . H66C H -0.2572 0.9910 0.2921 0.304 Uiso 1 1 calc GR . . . . C67 C -0.3066(7) 0.7947(5) 0.2737(3) 0.195(3) Uani 1 1 d . . . . . H67A H -0.3224 0.7355 0.2860 0.293 Uiso 1 1 calc GR . . . . H67B H -0.2599 0.7787 0.2396 0.293 Uiso 1 1 calc GR . . . . H67C H -0.4015 0.8196 0.2668 0.293 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 0.0435(2) 0.0461(2) 0.02617(17) 0.01720(14) 0.00456(13) 0.01081(14) N1 0.0418(11) 0.0450(11) 0.0339(10) 0.0155(9) 0.0048(9) 0.0145(9) N2 0.0511(12) 0.0584(13) 0.0312(11) 0.0203(10) 0.0042(9) 0.0172(10) N3 0.0535(13) 0.0587(13) 0.0368(11) 0.0218(10) 0.0121(10) 0.0154(10) N4 0.0403(11) 0.0411(11) 0.0314(10) 0.0147(9) 0.0036(8) 0.0067(9) N5 0.0513(12) 0.0554(13) 0.0367(11) 0.0253(10) 0.0079(9) 0.0129(10) N6 0.0489(12) 0.0543(13) 0.0295(10) 0.0121(9) -0.0027(9) 0.0132(10) N7 0.0839(18) 0.101(2) 0.0372(13) 0.0317(14) 0.0033(13) 0.0140(16) N8 0.111(2) 0.0772(18) 0.0463(15) 0.0290(13) -0.0170(15) 0.0004(16) C1 0.0430(14) 0.0471(14) 0.0322(12) 0.0137(11) 0.0052(10) 0.0124(11) C2 0.0463(15) 0.0613(16) 0.0357(13) 0.0172(12) 0.0086(11) 0.0201(12) C3 0.0472(14) 0.0480(14) 0.0307(12) 0.0140(11) 0.0015(11) 0.0092(11) C4 0.0483(15) 0.0527(15) 0.0356(13) 0.0183(11) 0.0034(11) 0.0172(12) C5 0.0399(13) 0.0484(14) 0.0327(12) 0.0145(11) 0.0025(10) 0.0115(11) C6 0.0461(15) 0.0554(16) 0.0387(14) 0.0190(12) 0.0098(11) 0.0179(12) C7 0.0674(19) 0.098(2) 0.0496(16) 0.0370(16) 0.0166(14) 0.0435(17) C8 0.066(2) 0.120(3) 0.070(2) 0.040(2) 0.0225(17) 0.0537(19) C9 0.065(2) 0.095(2) 0.065(2) 0.0319(17) 0.0326(16) 0.0366(17) C10 0.0677(19) 0.0735(19) 0.0471(16) 0.0273(14) 0.0232(14) 0.0226(15) C11 0.0595(17) 0.0730(19) 0.0411(15) 0.0271(14) 0.0041(13) 0.0228(15) C12 0.0607(18) 0.096(2) 0.0547(18) 0.0356(16) 0.0046(14) 0.0387(17) C13 0.068(2) 0.102(2) 0.0580(18) 0.0363(17) 0.0199(15) 0.0474(18) C14 0.0627(18) 0.090(2) 0.0404(15) 0.0271(14) 0.0140(13) 0.0407(16) C15 0.0436(14) 0.0541(15) 0.0368(13) 0.0195(12) 0.0054(11) 0.0150(12) C16 0.0500(15) 0.0535(15) 0.0300(12) 0.0151(11) 0.0014(11) 0.0071(12) C17 0.094(2) 0.110(3) 0.0445(17) 0.0423(17) 0.0198(16) 0.053(2) C18 0.118(3) 0.127(3) 0.057(2) 0.055(2) 0.017(2) 0.058(3) C19 0.073(2) 0.084(2) 0.0381(15) 0.0166(15) 0.0145(14) 0.0105(17) C20 0.0615(17) 0.0654(18) 0.0357(14) 0.0178(13) 0.0075(12) 0.0158(14) C21 0.0405(13) 0.0461(14) 0.0302(12) 0.0153(11) 0.0055(10) 0.0078(11) C22 0.0511(15) 0.0459(14) 0.0319(13) 0.0182(11) 0.0036(11) 0.0025(12) C23 0.0474(14) 0.0464(14) 0.0292(12) 0.0152(11) 0.0052(10) 0.0082(11) C24 0.0495(15) 0.0441(14) 0.0321(13) 0.0128(11) 0.0039(11) 0.0048(11) C25 0.0422(13) 0.0439(14) 0.0308(12) 0.0159(11) 0.0084(10) 0.0126(11) C26 0.0428(14) 0.0448(14) 0.0328(13) 0.0148(11) 0.0084(10) 0.0136(11) C27 0.0548(16) 0.0457(15) 0.0422(14) 0.0124(12) 0.0100(12) 0.0085(12) C28 0.0652(18) 0.0438(15) 0.0624(18) 0.0179(13) 0.0181(14) 0.0052(13) C29 0.073(2) 0.0534(17) 0.0619(19) 0.0323(15) 0.0186(15) 0.0129(15) C30 0.0679(18) 0.0610(18) 0.0421(15) 0.0291(14) 0.0099(13) 0.0145(15) C31 0.0623(18) 0.0634(19) 0.0386(15) 0.0086(14) -0.0086(13) 0.0156(15) C32 0.073(2) 0.0556(19) 0.0594(19) 0.0038(15) -0.0191(15) 0.0055(15) C33 0.079(2) 0.0494(17) 0.070(2) 0.0168(15) -0.0124(16) -0.0051(15) C34 0.0698(19) 0.0519(16) 0.0480(16) 0.0215(13) -0.0073(13) -0.0003(14) C35 0.0451(14) 0.0457(14) 0.0341(13) 0.0152(11) -0.0001(11) 0.0074(11) C36 0.0592(17) 0.0462(14) 0.0300(13) 0.0137(11) 0.0004(11) 0.0077(12) C37 0.0715(19) 0.0574(17) 0.0351(14) 0.0197(12) 0.0035(13) 0.0043(14) C38 0.103(3) 0.073(2) 0.0394(16) 0.0280(15) 0.0097(16) 0.0097(19) C39 0.091(2) 0.074(2) 0.063(2) 0.0281(17) -0.0282(18) -0.0046(18) C40 0.070(2) 0.0652(18) 0.0484(16) 0.0276(14) -0.0084(14) -0.0018(15) O2 0.163(15) 0.166(18) 0.130(14) 0.070(12) 0.006(9) 0.031(10) N9 0.171(4) 0.144(3) 0.071(2) 0.039(2) 0.015(2) 0.034(3) N10 0.118(3) 0.098(2) 0.112(3) 0.041(2) -0.004(2) 0.049(2) N11 0.139(3) 0.090(2) 0.177(4) 0.061(2) 0.014(3) 0.056(2) N12 0.119(3) 0.113(3) 0.081(2) 0.052(2) 0.0049(19) -0.0014(19) C41 0.092(3) 0.071(2) 0.073(2) 0.0320(18) -0.0100(18) 0.019(2) C42 0.108(3) 0.081(2) 0.067(2) 0.031(2) -0.004(2) 0.019(2) C43 0.080(2) 0.0649(19) 0.0572(19) 0.0245(15) -0.0044(16) 0.0163(16) C44 0.0675(19) 0.0522(17) 0.0540(17) 0.0181(14) -0.0018(14) 0.0112(14) C45 0.080(2) 0.0597(18) 0.0586(18) 0.0165(15) 0.0102(16) 0.0188(16) C46 0.076(2) 0.0564(18) 0.067(2) 0.0199(15) 0.0100(16) 0.0217(15) C47 0.0658(18) 0.0438(15) 0.0649(19) 0.0210(14) -0.0034(15) 0.0080(14) C48 0.084(2) 0.0624(19) 0.0571(18) 0.0221(15) 0.0116(16) 0.0211(16) C49 0.085(2) 0.0581(18) 0.0624(19) 0.0227(15) 0.0112(16) 0.0279(16) C50 0.068(2) 0.0543(18) 0.075(2) 0.0290(16) -0.0023(16) 0.0066(15) C51 0.094(3) 0.066(2) 0.103(3) 0.042(2) -0.007(2) 0.017(2) C52 0.083(2) 0.068(2) 0.078(2) 0.0410(19) -0.0055(19) 0.0002(17) C68 0.47(3) 0.32(3) 0.35(2) 0.162(19) 0.27(2) 0.12(2) N13 0.0651(17) 0.0645(16) 0.0770(18) 0.0197(13) -0.0076(14) -0.0023(13) N14 0.114(2) 0.106(2) 0.086(2) 0.0619(19) 0.0053(17) 0.0117(18) N15 0.0888(19) 0.0645(16) 0.0761(18) 0.0394(14) 0.0050(14) 0.0047(14) N16 0.0569(16) 0.0775(18) 0.0684(17) 0.0288(14) 0.0077(13) 0.0030(13) C53 0.0598(18) 0.0422(15) 0.0504(16) 0.0137(12) 0.0045(14) 0.0038(13) C54 0.0638(19) 0.0616(18) 0.0582(18) 0.0281(15) 0.0094(14) 0.0033(14) C55 0.0496(16) 0.0511(16) 0.0460(15) 0.0188(12) 0.0049(12) 0.0065(12) C56 0.0463(15) 0.0451(14) 0.0377(13) 0.0126(11) 0.0069(11) 0.0078(12) C57 0.0537(16) 0.0518(16) 0.0408(14) 0.0202(12) 0.0014(12) 0.0045(13) C58 0.0504(15) 0.0521(16) 0.0390(14) 0.0148(12) -0.0020(11) 0.0041(12) C59 0.0504(15) 0.0435(14) 0.0392(14) 0.0145(11) 0.0085(11) 0.0107(12) C60 0.0549(16) 0.0477(15) 0.0418(14) 0.0197(12) 0.0026(12) 0.0113(12) C61 0.0475(15) 0.0473(15) 0.0426(14) 0.0132(12) 0.0015(11) 0.0090(12) C62 0.0530(16) 0.0463(15) 0.0462(15) 0.0184(12) 0.0084(12) 0.0083(12) C63 0.0575(17) 0.0443(15) 0.0548(17) 0.0195(13) 0.0082(13) 0.0033(13) C64 0.0520(17) 0.0505(16) 0.0508(16) 0.0216(13) 0.0150(14) 0.0097(13) O1 0.238(6) 0.453(10) 0.346(8) 0.298(8) 0.114(5) 0.179(6) N17 0.143(4) 0.149(4) 0.127(3) 0.058(3) 0.033(3) 0.056(3) C65 0.227(8) 0.365(13) 0.198(7) 0.185(8) 0.099(6) 0.185(9) C66 0.286(8) 0.130(5) 0.199(6) 0.073(5) -0.009(6) 0.005(5) C67 0.178(6) 0.187(6) 0.192(6) 0.017(5) 0.030(5) -0.037(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 77.35(7) . . N1 Co1 N3 76.89(7) . . N1 Co1 N5 96.40(8) . . N1 Co1 N6 104.27(8) . . N3 Co1 N2 154.03(7) . . N4 Co1 N1 173.44(8) . . N4 Co1 N2 97.35(7) . . N4 Co1 N3 108.57(7) . . N4 Co1 N5 79.84(8) . . N4 Co1 N6 79.44(8) . . N5 Co1 N2 92.46(8) . . N5 Co1 N3 93.57(8) . . N6 Co1 N2 90.74(8) . . N6 Co1 N3 92.46(8) . . N6 Co1 N5 159.28(7) . . C1 N1 Co1 120.06(14) . . C1 N1 C5 119.02(19) . . C5 N1 Co1 120.22(15) . . C11 N2 Co1 129.44(16) . . C11 N2 C15 117.8(2) . . C15 N2 Co1 112.17(14) . . C6 N3 Co1 112.72(15) . . C10 N3 Co1 129.28(17) . . C10 N3 C6 117.9(2) . . C21 N4 Co1 119.73(15) . . C21 N4 C25 120.37(18) . . C25 N4 Co1 119.23(14) . . C26 N5 Co1 113.72(15) . . C30 N5 Co1 128.53(18) . . C30 N5 C26 117.5(2) . . C31 N6 Co1 127.65(17) . . C31 N6 C35 117.9(2) . . C35 N6 Co1 114.49(15) . . C19 N7 C18 114.7(2) . . C38 N8 C39 115.4(2) . . N1 C1 C2 121.1(2) . . N1 C1 C15 115.00(19) . . C2 C1 C15 123.9(2) . . C1 C2 H2 119.6 . . C1 C2 C3 120.8(2) . . C3 C2 H2 119.6 . . C2 C3 C4 117.2(2) . . C2 C3 C16 121.4(2) . . C4 C3 C16 121.5(2) . . C3 C4 H4 119.8 . . C5 C4 C3 120.4(2) . . C5 C4 H4 119.8 . . N1 C5 C4 121.5(2) . . N1 C5 C6 114.05(19) . . C4 C5 C6 124.5(2) . . N3 C6 C5 114.7(2) . . N3 C6 C7 122.0(2) . . C7 C6 C5 123.3(2) . . C6 C7 H7 120.4 . . C6 C7 C8 119.2(2) . . C8 C7 H7 120.4 . . C7 C8 H8 120.5 . . C9 C8 C7 119.0(3) . . C9 C8 H8 120.5 . . C8 C9 H9 120.6 . . C10 C9 C8 118.8(3) . . C10 C9 H9 120.6 . . N3 C10 C9 123.1(2) . . N3 C10 H10 118.4 . . C9 C10 H10 118.4 . . N2 C11 H11 118.7 . . N2 C11 C12 122.6(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 120.3 . . C14 C13 C12 119.3(3) . . C14 C13 H13 120.3 . . C13 C14 H14 120.5 . . C15 C14 C13 119.0(2) . . C15 C14 H14 120.5 . . N2 C15 C1 114.4(2) . . N2 C15 C14 122.2(2) . . C14 C15 C1 123.4(2) . . C17 C16 C3 122.4(2) . . C17 C16 C20 116.2(2) . . C20 C16 C3 121.3(2) . . C16 C17 H17 120.2 . . C16 C17 C18 119.5(3) . . C18 C17 H17 120.2 . . N7 C18 C17 124.7(3) . . N7 C18 H18 117.7 . . C17 C18 H18 117.7 . . N7 C19 H19 117.4 . . N7 C19 C20 125.1(3) . . C20 C19 H19 117.4 . . C16 C20 H20 120.2 . . C19 C20 C16 119.7(2) . . C19 C20 H20 120.2 . . N4 C21 C22 120.8(2) . . N4 C21 C35 112.70(19) . . C22 C21 C35 126.4(2) . . C21 C22 H22 120.1 . . C21 C22 C23 119.8(2) . . C23 C22 H22 120.1 . . C22 C23 C36 121.0(2) . . C24 C23 C22 118.3(2) . . C24 C23 C36 120.6(2) . . C23 C24 H24 120.2 . . C25 C24 C23 119.7(2) . . C25 C24 H24 120.2 . . N4 C25 C24 121.0(2) . . N4 C25 C26 113.07(19) . . C24 C25 C26 125.8(2) . . N5 C26 C25 113.8(2) . . N5 C26 C27 122.2(2) . . C27 C26 C25 123.9(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 119.3(3) . . C29 C28 H28 120.4 . . C28 C29 H29 120.7 . . C30 C29 C28 118.7(2) . . C30 C29 H29 120.7 . . N5 C30 C29 123.4(2) . . N5 C30 H30 118.3 . . C29 C30 H30 118.3 . . N6 C31 H31 118.6 . . N6 C31 C32 122.7(2) . . C32 C31 H31 118.6 . . C31 C32 H32 120.4 . . C31 C32 C33 119.1(3) . . C33 C32 H32 120.4 . . C32 C33 H33 120.2 . . C32 C33 C34 119.5(3) . . C34 C33 H33 120.2 . . C33 C34 H34 120.7 . . C35 C34 C33 118.6(2) . . C35 C34 H34 120.7 . . N6 C35 C21 113.4(2) . . N6 C35 C34 122.2(2) . . C34 C35 C21 124.4(2) . . C37 C36 C23 122.8(2) . . C40 C36 C23 120.5(2) . . C40 C36 C37 116.7(2) . . C36 C37 H37 120.4 . . C38 C37 C36 119.2(3) . . C38 C37 H37 120.4 . . N8 C38 C37 125.0(3) . . N8 C38 H38 117.5 . . C37 C38 H38 117.5 . . N8 C39 H39 117.8 . . N8 C39 C40 124.4(3) . . C40 C39 H39 117.8 . . C36 C40 C39 119.4(3) . . C36 C40 H40 120.3 . . C39 C40 H40 120.3 . . N10 C41 C43 178.6(4) . . N9 C42 C43 179.6(5) . . C41 C43 C42 116.1(3) . . C41 C43 C44 121.6(3) . . C44 C43 C42 122.2(3) . . C43 C44 C45 121.3(3) . . C49 C44 C43 122.0(3) . . C49 C44 C45 116.6(2) . . C44 C45 H45 119.2 . . C46 C45 C44 121.6(3) . . C46 C45 H45 119.2 . . C45 C46 H46 119.3 . . C45 C46 C47 121.4(3) . . C47 C46 H46 119.3 . . C48 C47 C46 116.9(2) . . C48 C47 C50 121.3(3) . . C50 C47 C46 121.9(3) . . C47 C48 H48 119.4 . . C49 C48 C47 121.3(3) . . C49 C48 H48 119.4 . . C44 C49 H49 119.0 . . C48 C49 C44 122.1(3) . . C48 C49 H49 119.0 . . C47 C50 C51 120.7(3) . . C47 C50 C52 123.4(3) . . C52 C50 C51 115.7(3) . . N11 C51 C50 178.9(4) . . N12 C52 C50 177.8(4) . . N13 C53 C55 176.7(3) . . N14 C54 C55 179.2(4) . . C53 C55 C54 117.1(2) . . C53 C55 C56 120.3(2) . . C56 C55 C54 122.3(2) . . C55 C56 C57 121.9(2) . . C55 C56 C61 120.7(2) . . C61 C56 C57 117.3(2) . . C56 C57 H57 119.4 . . C58 C57 C56 121.1(2) . . C58 C57 H57 119.4 . . C57 C58 H58 119.3 . . C57 C58 C59 121.5(2) . . C59 C58 H58 119.3 . . C60 C59 C58 116.9(2) . . C60 C59 C62 121.2(2) . . C62 C59 C58 121.9(2) . . C59 C60 H60 119.3 . . C61 C60 C59 121.4(2) . . C61 C60 H60 119.3 . . C56 C61 H61 119.1 . . C60 C61 C56 121.8(2) . . C60 C61 H61 119.1 . . C63 C62 C59 121.2(2) . . C64 C62 C59 121.3(2) . . C64 C62 C63 117.3(2) . . N15 C63 C62 179.4(3) . . N16 C64 C62 178.2(3) . . C65 N17 C66 120.3(7) . . C65 N17 C67 124.1(6) . . C66 N17 C67 115.6(5) . . O1 C65 N17 118.9(10) . . O1 C65 H65 120.6 . . N17 C65 H65 120.6 . . 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 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 N1 1.9702(19) . Co1 N2 2.207(2) . Co1 N3 2.195(2) . Co1 N4 1.9180(19) . Co1 N5 2.052(2) . Co1 N6 2.041(2) . N1 C1 1.349(3) . N1 C5 1.352(3) . N2 C11 1.341(3) . N2 C15 1.350(3) . N3 C6 1.345(3) . N3 C10 1.336(3) . N4 C21 1.343(3) . N4 C25 1.347(3) . N5 C26 1.360(3) . N5 C30 1.340(3) . N6 C31 1.341(3) . N6 C35 1.358(3) . N7 C18 1.329(4) . N7 C19 1.312(3) . N8 C38 1.321(4) . N8 C39 1.328(4) . C1 C2 1.379(3) . C1 C15 1.477(3) . C2 H2 0.9300 . C2 C3 1.384(3) . C3 C4 1.390(3) . C3 C16 1.481(3) . C4 H4 0.9300 . C4 C5 1.375(3) . C5 C6 1.481(3) . C6 C7 1.369(3) . C7 H7 0.9300 . C7 C8 1.384(4) . C8 H8 0.9300 . C8 C9 1.367(4) . C9 H9 0.9300 . C9 C10 1.367(4) . C10 H10 0.9300 . C11 H11 0.9300 . C11 C12 1.369(3) . C12 H12 0.9300 . C12 C13 1.372(4) . C13 H13 0.9300 . C13 C14 1.371(3) . C14 H14 0.9300 . C14 C15 1.370(3) . C16 C17 1.369(3) . C16 C20 1.378(3) . C17 H17 0.9300 . C17 C18 1.378(4) . C18 H18 0.9300 . C19 H19 0.9300 . C19 C20 1.371(3) . C20 H20 0.9300 . C21 C22 1.382(3) . C21 C35 1.473(3) . C22 H22 0.9300 . C22 C23 1.391(3) . C23 C24 1.389(3) . C23 C36 1.485(3) . C24 H24 0.9300 . C24 C25 1.382(3) . C25 C26 1.474(3) . C26 C27 1.373(3) . C27 H27 0.9300 . C27 C28 1.383(3) . C28 H28 0.9300 . C28 C29 1.377(4) . C29 H29 0.9300 . C29 C30 1.367(4) . C30 H30 0.9300 . C31 H31 0.9300 . C31 C32 1.367(4) . C32 H32 0.9300 . C32 C33 1.369(4) . C33 H33 0.9300 . C33 C34 1.382(4) . C34 H34 0.9300 . C34 C35 1.373(3) . C36 C37 1.383(3) . C36 C40 1.382(4) . C37 H37 0.9300 . C37 C38 1.377(3) . C38 H38 0.9300 . C39 H39 0.9300 . C39 C40 1.383(4) . C40 H40 0.9300 . O2 C68 1.322(19) . N9 C42 1.149(4) . N10 C41 1.138(4) . N11 C51 1.141(4) . N12 C52 1.142(4) . C41 C43 1.413(4) . C42 C43 1.423(5) . C43 C44 1.414(4) . C44 C45 1.416(4) . C44 C49 1.402(4) . C45 H45 0.9300 . C45 C46 1.350(4) . C46 H46 0.9300 . C46 C47 1.418(4) . C47 C48 1.407(4) . C47 C50 1.411(4) . C48 H48 0.9300 . C48 C49 1.357(4) . C49 H49 0.9300 . C50 C51 1.425(4) . C50 C52 1.412(4) . N13 C53 1.144(3) . N14 C54 1.137(3) . N15 C63 1.149(3) . N16 C64 1.148(3) . C53 C55 1.406(4) . C54 C55 1.412(4) . C55 C56 1.409(3) . C56 C57 1.409(3) . C56 C61 1.409(3) . C57 H57 0.9300 . C57 C58 1.354(3) . C58 H58 0.9300 . C58 C59 1.423(3) . C59 C60 1.408(3) . C59 C62 1.414(3) . C60 H60 0.9300 . C60 C61 1.350(3) . C61 H61 0.9300 . C62 C63 1.410(3) . C62 C64 1.404(4) . O1 C65 1.256(10) . N17 C65 1.312(7) . N17 C66 1.448(6) . N17 C67 1.476(6) . 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 .