#------------------------------------------------------------------------------ #$Date: 2019-10-07 12:55:59 +0300 (Mon, 07 Oct 2019) $ #$Revision: 219132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234431.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_7234431 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 74.006(11) _cell_angle_beta 81.940(11) _cell_angle_gamma 85.735(12) _cell_formula_units_Z 2 _cell_length_a 8.981(3) _cell_length_b 13.924(4) _cell_length_c 24.722(8) _cell_measurement_reflns_used 8769 _cell_measurement_temperature 180.15 _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 2.29 _cell_volume 2940.4(16) _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 180.15 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.989 _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 0.0718 _diffrn_reflns_av_unetI/netI 0.0736 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 25859 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 1.535 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.355 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0574 before and 0.0427 after correction. The Ratio of minimum to maximum transmission is 0.9230. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.348 _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 0.644 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.073 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 797 _refine_ls_number_reflns 11436 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0446 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1187 _refine_ls_wR_factor_ref 0.1287 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9057 _reflns_number_total 11436 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file J-Mater-Chem-C-2015-3-9292.cif _cod_data_source_block 7-180K _cod_database_code 7234431 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.972 _shelx_estimated_absorpt_t_min 0.916 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40), C57(H57), C58(H58), C60(H60), C61(H61), C45(H45), C46(H46), C48(H48), C49(H49), C65(H65) 2.b Idealised Me refined as rotating group: C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C) 2.c Idealised tetrahedral OH refined as rotating group: O2(H2A) ; _shelx_res_file ; TITL P-1_a.res in P-1 REM Old TITL P-1 in P-1 REM SHELXT solution in P-1 REM R1 0.126, Rweak 0.007, Alpha 0.068, Orientation as input REM Formula found by SHELXT: C72 Co N14 O CELL 0.71073 8.9813 13.9236 24.7216 74.006 81.94 85.735 ZERR 2 0.0029 0.0044 0.0076 0.011 0.011 0.012 LATT 1 SFAC C H Co N O UNIT 136 94 2 34 4 L.S. 10 PLAN 1 SIZE 0.08 0.13 0.25 TEMP -93 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.061300 FVAR 0.33210 CO1 3 0.127875 0.681538 0.236055 11.00000 0.02510 0.01699 = 0.01196 0.00318 -0.00261 -0.00225 N1 4 0.115223 0.609115 0.316440 11.00000 0.02524 0.02146 = 0.01884 -0.00142 -0.00251 -0.00340 N2 4 0.339365 0.724550 0.260709 11.00000 0.03019 0.02511 = 0.01962 0.00307 -0.00223 -0.00653 N3 4 -0.092034 0.608688 0.252174 11.00000 0.03293 0.02500 = 0.02432 0.00033 -0.00929 -0.00321 N4 4 0.162250 0.749439 0.158348 11.00000 0.02402 0.01833 = 0.01777 -0.00110 -0.00435 -0.00073 N5 4 0.239611 0.570817 0.206837 11.00000 0.02864 0.02177 = 0.02091 0.00426 -0.00551 -0.00339 N6 4 0.030826 0.815521 0.238175 11.00000 0.02831 0.02708 = 0.01758 -0.00058 0.00014 -0.00709 N7 4 0.157474 0.277594 0.588661 11.00000 0.05397 0.04098 = 0.02335 0.00802 -0.00414 -0.00482 N8 4 0.445087 1.028205 -0.115969 11.00000 0.06412 0.03149 = 0.02708 0.00051 0.00874 -0.00872 C1 1 0.228349 0.614263 0.346594 11.00000 0.02681 0.02382 = 0.01900 -0.00134 -0.00412 -0.00268 C2 1 0.236206 0.551109 0.400170 11.00000 0.02984 0.03234 = 0.01964 0.00031 -0.00609 -0.00781 AFIX 43 H2 2 0.315624 0.556507 0.420700 11.00000 -1.20000 AFIX 0 C3 1 0.128492 0.479627 0.424255 11.00000 0.03044 0.02068 = 0.01936 -0.00088 -0.00151 -0.00164 C4 1 0.012419 0.475719 0.392991 11.00000 0.02910 0.02340 = 0.02125 -0.00074 -0.00102 -0.00599 AFIX 43 H4 2 -0.063239 0.428001 0.408225 11.00000 -1.20000 AFIX 0 C5 1 0.007410 0.541239 0.339854 11.00000 0.02582 0.02429 = 0.02064 -0.00307 -0.00187 -0.00414 C6 1 -0.113216 0.544339 0.303750 11.00000 0.03030 0.02739 = 0.02405 -0.00243 -0.00580 -0.00530 C7 1 -0.240304 0.486911 0.322063 11.00000 0.04308 0.05015 = 0.03357 0.00732 -0.01340 -0.02081 AFIX 43 H7 2 -0.252478 0.441125 0.358682 11.00000 -1.20000 AFIX 0 C8 1 -0.348635 0.497837 0.285852 11.00000 0.04100 0.06546 = 0.04863 -0.00232 -0.01659 -0.02168 AFIX 43 H8 2 -0.436232 0.459382 0.297349 11.00000 -1.20000 AFIX 0 C9 1 -0.328379 0.564683 0.233219 11.00000 0.04064 0.05229 = 0.04085 -0.00653 -0.02200 -0.00608 AFIX 43 H9 2 -0.401629 0.574019 0.207808 11.00000 -1.20000 AFIX 0 C10 1 -0.198390 0.617961 0.218293 11.00000 0.04143 0.03330 = 0.03228 -0.00114 -0.01808 -0.00272 AFIX 43 H10 2 -0.183913 0.663884 0.181764 11.00000 -1.20000 AFIX 0 C11 1 0.443633 0.788498 0.230871 11.00000 0.03937 0.03004 = 0.02225 0.00499 -0.00047 -0.01046 AFIX 43 H11 2 0.440938 0.814568 0.191220 11.00000 -1.20000 AFIX 0 C12 1 0.555942 0.818572 0.255316 11.00000 0.03649 0.03967 = 0.03384 0.00242 -0.00009 -0.01800 AFIX 43 H12 2 0.629966 0.862791 0.232573 11.00000 -1.20000 AFIX 0 C13 1 0.558306 0.783531 0.312643 11.00000 0.03991 0.04642 = 0.03740 -0.00130 -0.01033 -0.01902 AFIX 43 H13 2 0.632991 0.803776 0.330450 11.00000 -1.20000 AFIX 0 C14 1 0.449584 0.717884 0.344270 11.00000 0.03841 0.04098 = 0.02460 0.00203 -0.00887 -0.01348 AFIX 43 H14 2 0.447785 0.693398 0.384215 11.00000 -1.20000 AFIX 0 C15 1 0.343646 0.688423 0.316953 11.00000 0.02761 0.02297 = 0.02162 0.00184 -0.00366 -0.00314 C16 1 0.138348 0.409006 0.480823 11.00000 0.03080 0.02585 = 0.01970 0.00002 -0.00283 -0.00218 C17 1 0.053247 0.324429 0.500697 11.00000 0.06074 0.04724 = 0.03028 0.01362 -0.01613 -0.02464 AFIX 43 H17 2 -0.013651 0.309450 0.477842 11.00000 -1.20000 AFIX 0 C18 1 0.066722 0.262667 0.553693 11.00000 0.07049 0.05249 = 0.03607 0.01666 -0.01474 -0.02786 AFIX 43 H18 2 0.007217 0.205202 0.566390 11.00000 -1.20000 AFIX 0 C19 1 0.238185 0.358498 0.569090 11.00000 0.04521 0.04361 = 0.02312 -0.00081 -0.00998 -0.00080 AFIX 43 H19 2 0.304227 0.371318 0.592922 11.00000 -1.20000 AFIX 0 C20 1 0.233254 0.425100 0.516880 11.00000 0.04007 0.03333 = 0.02284 0.00026 -0.00675 -0.00601 AFIX 43 H20 2 0.294342 0.481816 0.505486 11.00000 -1.20000 AFIX 0 C21 1 0.121651 0.847401 0.140647 11.00000 0.02621 0.01850 = 0.02020 -0.00026 -0.00609 -0.00072 C22 1 0.164908 0.902261 0.085914 11.00000 0.03058 0.01859 = 0.02070 0.00147 -0.00431 0.00034 AFIX 43 H22 2 0.133805 0.970691 0.073711 11.00000 -1.20000 AFIX 0 C23 1 0.255201 0.856608 0.048214 11.00000 0.02815 0.02310 = 0.01808 -0.00103 -0.00355 -0.00305 C24 1 0.293020 0.755381 0.066999 11.00000 0.02635 0.02330 = 0.01949 -0.00360 -0.00346 -0.00111 AFIX 43 H24 2 0.350332 0.721896 0.041870 11.00000 -1.20000 AFIX 0 C25 1 0.246672 0.703457 0.122632 11.00000 0.02473 0.01850 = 0.02110 -0.00037 -0.00555 -0.00351 C26 1 0.290359 0.599570 0.150731 11.00000 0.02561 0.01967 = 0.02023 -0.00044 -0.00644 -0.00398 C27 1 0.382685 0.537898 0.123817 11.00000 0.03216 0.02464 = 0.02674 -0.00648 -0.00651 -0.00023 AFIX 43 H27 2 0.416572 0.559742 0.084388 11.00000 -1.20000 AFIX 0 C28 1 0.424315 0.444167 0.155478 11.00000 0.03760 0.02412 = 0.03318 -0.00730 -0.01127 0.00217 AFIX 43 H28 2 0.488623 0.400857 0.138127 11.00000 -1.20000 AFIX 0 C29 1 0.372284 0.413920 0.212146 11.00000 0.04004 0.01920 = 0.04129 0.00014 -0.01346 0.00024 AFIX 43 H29 2 0.399787 0.349433 0.234382 11.00000 -1.20000 AFIX 0 C30 1 0.279344 0.478305 0.236576 11.00000 0.03627 0.02199 = 0.02517 0.00617 -0.00585 -0.00437 AFIX 43 H30 2 0.242236 0.456476 0.275721 11.00000 -1.20000 AFIX 0 C31 1 -0.037358 0.843250 0.283644 11.00000 0.03644 0.03523 = 0.02018 -0.00623 0.00134 -0.00775 AFIX 43 H31 2 -0.045099 0.795119 0.319515 11.00000 -1.20000 AFIX 0 C32 1 -0.096647 0.938408 0.280634 11.00000 0.04111 0.04067 = 0.02931 -0.01532 0.00527 -0.00346 AFIX 43 H32 2 -0.144364 0.955221 0.313786 11.00000 -1.20000 AFIX 0 C33 1 -0.085773 1.008800 0.228904 11.00000 0.04417 0.03137 = 0.03978 -0.01247 0.00175 0.00133 AFIX 43 H33 2 -0.125056 1.075070 0.225890 11.00000 -1.20000 AFIX 0 C34 1 -0.016224 0.981431 0.180951 11.00000 0.03887 0.02714 = 0.02630 -0.00292 -0.00085 0.00175 AFIX 43 H34 2 -0.008291 1.028502 0.144718 11.00000 -1.20000 AFIX 0 C35 1 0.040628 0.885093 0.187085 11.00000 0.02557 0.02205 = 0.02004 -0.00212 -0.00081 -0.00293 C36 1 0.318502 0.915787 -0.008916 11.00000 0.03622 0.02157 = 0.01846 -0.00136 -0.00335 -0.00431 C37 1 0.238858 0.994971 -0.041202 11.00000 0.04033 0.02583 = 0.02040 -0.00174 -0.00436 -0.00048 AFIX 43 H37 2 0.139366 1.012750 -0.027529 11.00000 -1.20000 AFIX 0 C38 1 0.306526 1.047397 -0.093444 11.00000 0.06135 0.02469 = 0.02301 0.00355 -0.00523 -0.00313 AFIX 43 H38 2 0.250038 1.101260 -0.114985 11.00000 -1.20000 AFIX 0 C39 1 0.521245 0.952294 -0.084440 11.00000 0.04874 0.03409 = 0.03430 -0.00850 0.01094 -0.00735 AFIX 43 H39 2 0.620455 0.936405 -0.099366 11.00000 -1.20000 AFIX 0 C40 1 0.464573 0.895656 -0.031576 11.00000 0.03756 0.02576 = 0.02676 -0.00209 0.00150 -0.00356 AFIX 43 H40 2 0.524655 0.843216 -0.010699 11.00000 -1.20000 AFIX 0 N13 4 0.949834 0.857883 -0.039086 11.00000 0.05252 0.02591 = 0.04275 -0.00305 -0.00397 0.00064 N14 4 0.613376 0.714319 0.102209 11.00000 0.03453 0.03674 = 0.03942 -0.00584 -0.00542 0.00308 N15 4 1.495769 0.354785 0.021260 11.00000 0.03868 0.03633 = 0.03969 -0.01145 -0.00119 0.00217 N16 4 1.161505 0.187315 0.155147 11.00000 0.06347 0.03698 = 0.04517 0.00812 -0.00393 -0.00372 C53 1 0.860941 0.700130 0.037467 11.00000 0.03187 0.02349 = 0.02597 -0.00376 -0.00570 -0.00002 C54 1 0.909151 0.787200 -0.004718 11.00000 0.03618 0.02294 = 0.03084 -0.00640 -0.00729 0.00327 C55 1 0.723370 0.708712 0.072496 11.00000 0.03425 0.02225 = 0.02811 -0.00309 -0.01236 0.00035 C56 1 0.950435 0.611092 0.047156 11.00000 0.03034 0.02272 = 0.02226 -0.00457 -0.00813 -0.00123 C57 1 0.905456 0.523922 0.091697 11.00000 0.02936 0.02576 = 0.02289 -0.00356 0.00037 -0.00212 AFIX 43 H57 2 0.812497 0.525704 0.115132 11.00000 -1.20000 AFIX 0 C58 1 0.993831 0.438937 0.100832 11.00000 0.03402 0.02395 = 0.02031 0.00040 -0.00339 -0.00331 AFIX 43 H58 2 0.961257 0.382208 0.130505 11.00000 -1.20000 AFIX 0 C59 1 1.134272 0.433039 0.066886 11.00000 0.02967 0.02379 = 0.02161 -0.00463 -0.00694 -0.00103 C60 1 1.178645 0.519529 0.022994 11.00000 0.02716 0.02627 = 0.02260 -0.00427 -0.00131 -0.00324 AFIX 43 H60 2 1.271924 0.517928 -0.000278 11.00000 -1.20000 AFIX 0 C61 1 1.090037 0.604690 0.013640 11.00000 0.03161 0.02183 = 0.02309 -0.00123 -0.00273 -0.00487 AFIX 43 H61 2 1.122802 0.661218 -0.016141 11.00000 -1.20000 AFIX 0 C62 1 1.229927 0.346619 0.076396 11.00000 0.03217 0.02219 = 0.02623 -0.00200 -0.00519 -0.00135 C63 1 1.375991 0.348950 0.045919 11.00000 0.03592 0.02056 = 0.02605 -0.00476 -0.00795 0.00165 C64 1 1.191954 0.258877 0.120021 11.00000 0.03691 0.02874 = 0.03099 -0.00401 -0.00603 0.00322 N9 4 0.619947 1.183826 0.288513 11.00000 0.12219 0.06592 = 0.04003 0.00213 -0.01523 -0.01355 N10 4 0.894237 1.237261 0.407392 11.00000 0.08561 0.06148 = 0.06198 -0.01075 0.00349 -0.03693 N11 4 0.357158 0.642590 0.514013 11.00000 0.08691 0.04748 = 0.10376 -0.01979 -0.01559 -0.02522 N12 4 0.638888 0.679376 0.635715 11.00000 0.07471 0.04701 = 0.04823 0.00151 -0.00476 0.00078 C41 1 0.706928 1.124596 0.386851 11.00000 0.05325 0.03314 = 0.03383 -0.00570 0.00444 -0.01000 C42 1 0.809115 1.186313 0.398763 11.00000 0.06353 0.03686 = 0.04010 -0.00548 0.00812 -0.01423 C43 1 0.657750 1.157663 0.332580 11.00000 0.07235 0.03814 = 0.03612 -0.00270 0.00354 -0.01076 C44 1 0.664722 1.031800 0.425196 11.00000 0.04335 0.03328 = 0.03099 -0.00857 0.00238 -0.00537 C45 1 0.563771 0.969546 0.412544 11.00000 0.05240 0.03590 = 0.03485 -0.00666 -0.00929 -0.00552 AFIX 43 H45 2 0.524817 0.990260 0.377162 11.00000 -1.20000 AFIX 0 C46 1 0.521128 0.881003 0.449640 11.00000 0.04906 0.03339 = 0.04551 -0.01302 -0.00920 -0.00699 AFIX 43 H46 2 0.452895 0.841635 0.439713 11.00000 -1.20000 AFIX 0 C47 1 0.576983 0.846598 0.502888 11.00000 0.04160 0.02569 = 0.03619 -0.00802 0.00214 -0.00320 C48 1 0.679722 0.907847 0.515305 11.00000 0.05732 0.03397 = 0.03249 -0.00437 -0.00913 -0.00972 AFIX 43 H48 2 0.720697 0.886482 0.550274 11.00000 -1.20000 AFIX 0 C49 1 0.720813 0.996598 0.478153 11.00000 0.05432 0.03726 = 0.03587 -0.00804 -0.00515 -0.01479 AFIX 43 H49 2 0.789046 1.035989 0.488062 11.00000 -1.20000 AFIX 0 C50 1 0.532881 0.754834 0.541196 11.00000 0.04496 0.02719 = 0.04197 -0.00714 -0.00004 -0.00389 C51 1 0.435353 0.692526 0.526871 11.00000 0.05855 0.02947 = 0.05938 -0.00773 -0.00079 -0.00706 C52 1 0.592150 0.715009 0.593437 11.00000 0.05400 0.02586 = 0.04660 -0.00176 0.00239 -0.00420 O1 5 -0.189624 0.091895 0.617578 11.00000 0.11463 0.10026 = 0.17433 0.05679 -0.05020 -0.05503 N17 4 -0.211928 -0.055593 0.681565 11.00000 0.08430 0.06454 = 0.07778 -0.00699 -0.02056 -0.01715 C65 1 -0.159296 0.004510 0.629443 11.00000 0.09625 0.10973 = 0.07483 0.02163 -0.03082 -0.05330 AFIX 43 H65 2 -0.098317 -0.023696 0.602651 11.00000 -1.20000 AFIX 0 C66 1 -0.304194 -0.018702 0.727559 11.00000 0.09393 0.07452 = 0.13553 -0.03836 0.01155 0.00919 AFIX 137 H66A 2 -0.245864 -0.027600 0.759369 11.00000 -1.50000 H66B 2 -0.396033 -0.056702 0.740542 11.00000 -1.50000 H66C 2 -0.331133 0.052366 0.712896 11.00000 -1.50000 AFIX 0 C67 1 -0.177553 -0.163172 0.696508 11.00000 0.15596 0.06867 = 0.11148 -0.02130 -0.00340 -0.01127 AFIX 137 H67A 2 -0.127060 -0.182219 0.662991 11.00000 -1.50000 H67B 2 -0.271139 -0.199083 0.710171 11.00000 -1.50000 H67C 2 -0.111398 -0.180389 0.726387 11.00000 -1.50000 AFIX 0 O2 5 0.708252 1.272332 0.169097 11.00000 0.12525 0.08436 = 0.06232 -0.01028 0.01031 -0.00938 AFIX 147 H2A 2 0.701643 1.241464 0.203662 11.00000 -1.50000 AFIX 0 C68 1 0.690197 1.208160 0.138439 11.00000 0.18602 0.07427 = 0.07045 -0.02205 -0.06978 0.02533 AFIX 137 H68A 2 0.715238 1.241031 0.097981 11.00000 -1.50000 H68B 2 0.585427 1.188011 0.145768 11.00000 -1.50000 H68C 2 0.756839 1.148929 0.149348 11.00000 -1.50000 AFIX 0 HKLF 4 REM P-1_a.res in P-1 REM R1 = 0.0446 for 9057 Fo > 4sig(Fo) and 0.0580 for all 11436 data REM 797 parameters refined using 0 restraints END WGHT 0.0613 0.0000 REM Highest difference peak 0.644, deepest hole -0.481, 1-sigma level 0.073 Q1 1 0.5806 1.2359 0.1694 11.00000 0.05 0.64 ; _shelx_res_checksum 36967 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 0.12787(3) 0.68154(2) 0.23606(2) 0.01933(9) Uani 1 1 d . . . . . N1 N 0.11522(19) 0.60912(12) 0.31644(7) 0.0225(4) Uani 1 1 d . . . . . N2 N 0.3394(2) 0.72455(13) 0.26071(7) 0.0266(4) Uani 1 1 d . . . . . N3 N -0.0920(2) 0.60869(13) 0.25217(8) 0.0281(4) Uani 1 1 d . . . . . N4 N 0.16225(19) 0.74944(12) 0.15835(7) 0.0206(4) Uani 1 1 d . . . . . N5 N 0.2396(2) 0.57082(13) 0.20684(7) 0.0254(4) Uani 1 1 d . . . . . N6 N 0.0308(2) 0.81552(13) 0.23817(7) 0.0254(4) Uani 1 1 d . . . . . N7 N 0.1575(3) 0.27759(15) 0.58866(8) 0.0427(5) Uani 1 1 d . . . . . N8 N 0.4451(3) 1.02820(15) -0.11597(9) 0.0436(5) Uani 1 1 d . . . . . C1 C 0.2283(2) 0.61426(15) 0.34659(9) 0.0239(5) Uani 1 1 d . . . . . C2 C 0.2362(2) 0.55111(16) 0.40017(9) 0.0281(5) Uani 1 1 d . . . . . H2 H 0.3156 0.5565 0.4207 0.034 Uiso 1 1 calc R . . . . C3 C 0.1285(2) 0.47963(15) 0.42426(9) 0.0245(5) Uani 1 1 d . . . . . C4 C 0.0124(2) 0.47572(16) 0.39299(9) 0.0256(5) Uani 1 1 d . . . . . H4 H -0.0632 0.4280 0.4082 0.031 Uiso 1 1 calc R . . . . C5 C 0.0074(2) 0.54124(15) 0.33985(9) 0.0241(5) Uani 1 1 d . . . . . C6 C -0.1132(2) 0.54434(16) 0.30375(9) 0.0277(5) Uani 1 1 d . . . . . C7 C -0.2403(3) 0.4869(2) 0.32206(11) 0.0441(7) Uani 1 1 d . . . . . H7 H -0.2525 0.4411 0.3587 0.053 Uiso 1 1 calc R . . . . C8 C -0.3486(3) 0.4978(2) 0.28585(12) 0.0522(8) Uani 1 1 d . . . . . H8 H -0.4362 0.4594 0.2973 0.063 Uiso 1 1 calc R . . . . C9 C -0.3284(3) 0.5647(2) 0.23322(11) 0.0439(7) Uani 1 1 d . . . . . H9 H -0.4016 0.5740 0.2078 0.053 Uiso 1 1 calc R . . . . C10 C -0.1984(3) 0.61796(17) 0.21829(10) 0.0358(6) Uani 1 1 d . . . . . H10 H -0.1839 0.6639 0.1818 0.043 Uiso 1 1 calc R . . . . C11 C 0.4436(3) 0.78850(17) 0.23087(10) 0.0328(5) Uani 1 1 d . . . . . H11 H 0.4409 0.8146 0.1912 0.039 Uiso 1 1 calc R . . . . C12 C 0.5559(3) 0.81857(18) 0.25532(10) 0.0387(6) Uani 1 1 d . . . . . H12 H 0.6300 0.8628 0.2326 0.046 Uiso 1 1 calc R . . . . C13 C 0.5583(3) 0.78353(19) 0.31264(11) 0.0418(6) Uani 1 1 d . . . . . H13 H 0.6330 0.8038 0.3305 0.050 Uiso 1 1 calc R . . . . C14 C 0.4496(3) 0.71788(18) 0.34427(10) 0.0357(6) Uani 1 1 d . . . . . H14 H 0.4478 0.6934 0.3842 0.043 Uiso 1 1 calc R . . . . C15 C 0.3436(2) 0.68842(15) 0.31695(9) 0.0255(5) Uani 1 1 d . . . . . C16 C 0.1383(2) 0.40901(16) 0.48082(9) 0.0267(5) Uani 1 1 d . . . . . C17 C 0.0532(3) 0.3244(2) 0.50070(11) 0.0487(7) Uani 1 1 d . . . . . H17 H -0.0137 0.3095 0.4778 0.058 Uiso 1 1 calc R . . . . C18 C 0.0667(4) 0.2627(2) 0.55369(12) 0.0566(8) Uani 1 1 d . . . . . H18 H 0.0072 0.2052 0.5664 0.068 Uiso 1 1 calc R . . . . C19 C 0.2382(3) 0.35850(19) 0.56909(10) 0.0384(6) Uani 1 1 d . . . . . H19 H 0.3042 0.3713 0.5929 0.046 Uiso 1 1 calc R . . . . C20 C 0.2333(3) 0.42510(17) 0.51688(10) 0.0331(5) Uani 1 1 d . . . . . H20 H 0.2943 0.4818 0.5055 0.040 Uiso 1 1 calc R . . . . C21 C 0.1217(2) 0.84740(15) 0.14065(9) 0.0223(5) Uani 1 1 d . . . . . C22 C 0.1649(2) 0.90226(15) 0.08591(9) 0.0246(5) Uani 1 1 d . . . . . H22 H 0.1338 0.9707 0.0737 0.030 Uiso 1 1 calc R . . . . C23 C 0.2552(2) 0.85661(15) 0.04821(9) 0.0238(5) Uani 1 1 d . . . . . C24 C 0.2930(2) 0.75538(15) 0.06700(9) 0.0234(5) Uani 1 1 d . . . . . H24 H 0.3503 0.7219 0.0419 0.028 Uiso 1 1 calc R . . . . C25 C 0.2467(2) 0.70346(15) 0.12263(9) 0.0220(4) Uani 1 1 d . . . . . C26 C 0.2904(2) 0.59957(15) 0.15073(9) 0.0223(5) Uani 1 1 d . . . . . C27 C 0.3827(2) 0.53790(16) 0.12382(10) 0.0277(5) Uani 1 1 d . . . . . H27 H 0.4166 0.5597 0.0844 0.033 Uiso 1 1 calc R . . . . C28 C 0.4243(3) 0.44417(16) 0.15548(10) 0.0312(5) Uani 1 1 d . . . . . H28 H 0.4886 0.4009 0.1381 0.037 Uiso 1 1 calc R . . . . C29 C 0.3723(3) 0.41392(17) 0.21215(11) 0.0344(6) Uani 1 1 d . . . . . H29 H 0.3998 0.3494 0.2344 0.041 Uiso 1 1 calc R . . . . C30 C 0.2793(3) 0.47830(16) 0.23658(10) 0.0299(5) Uani 1 1 d . . . . . H30 H 0.2422 0.4565 0.2757 0.036 Uiso 1 1 calc R . . . . C31 C -0.0374(3) 0.84325(17) 0.28364(10) 0.0310(5) Uani 1 1 d . . . . . H31 H -0.0451 0.7951 0.3195 0.037 Uiso 1 1 calc R . . . . C32 C -0.0966(3) 0.93841(18) 0.28063(10) 0.0367(6) Uani 1 1 d . . . . . H32 H -0.1444 0.9552 0.3138 0.044 Uiso 1 1 calc R . . . . C33 C -0.0858(3) 1.00880(19) 0.22890(11) 0.0387(6) Uani 1 1 d . . . . . H33 H -0.1251 1.0751 0.2259 0.046 Uiso 1 1 calc R . . . . C34 C -0.0162(3) 0.98143(17) 0.18095(10) 0.0321(5) Uani 1 1 d . . . . . H34 H -0.0083 1.0285 0.1447 0.039 Uiso 1 1 calc R . . . . C35 C 0.0406(2) 0.88509(15) 0.18709(9) 0.0234(5) Uani 1 1 d . . . . . C36 C 0.3185(3) 0.91579(15) -0.00892(9) 0.0261(5) Uani 1 1 d . . . . . C37 C 0.2389(3) 0.99497(16) -0.04120(9) 0.0297(5) Uani 1 1 d . . . . . H37 H 0.1394 1.0128 -0.0275 0.036 Uiso 1 1 calc R . . . . C38 C 0.3065(3) 1.04740(17) -0.09344(10) 0.0383(6) Uani 1 1 d . . . . . H38 H 0.2500 1.1013 -0.1150 0.046 Uiso 1 1 calc R . . . . C39 C 0.5212(3) 0.95229(18) -0.08444(10) 0.0405(6) Uani 1 1 d . . . . . H39 H 0.6205 0.9364 -0.0994 0.049 Uiso 1 1 calc R . . . . C40 C 0.4646(3) 0.89566(17) -0.03158(10) 0.0314(5) Uani 1 1 d . . . . . H40 H 0.5247 0.8432 -0.0107 0.038 Uiso 1 1 calc R . . . . N13 N 0.9498(3) 0.85788(15) -0.03909(9) 0.0419(5) Uani 1 1 d . . . . . N14 N 0.6134(2) 0.71432(15) 0.10221(9) 0.0379(5) Uani 1 1 d . . . . . N15 N 1.4958(2) 0.35478(15) 0.02126(9) 0.0385(5) Uani 1 1 d . . . . . N16 N 1.1615(3) 0.18731(17) 0.15515(10) 0.0526(6) Uani 1 1 d . . . . . C53 C 0.8609(2) 0.70013(16) 0.03747(9) 0.0275(5) Uani 1 1 d . . . . . C54 C 0.9092(3) 0.78720(17) -0.00472(10) 0.0301(5) Uani 1 1 d . . . . . C55 C 0.7234(3) 0.70871(16) 0.07250(10) 0.0282(5) Uani 1 1 d . . . . . C56 C 0.9504(2) 0.61109(15) 0.04716(9) 0.0249(5) Uani 1 1 d . . . . . C57 C 0.9055(2) 0.52392(15) 0.09170(9) 0.0269(5) Uani 1 1 d . . . . . H57 H 0.8125 0.5257 0.1151 0.032 Uiso 1 1 calc R . . . . C58 C 0.9938(2) 0.43894(16) 0.10083(9) 0.0272(5) Uani 1 1 d . . . . . H58 H 0.9613 0.3822 0.1305 0.033 Uiso 1 1 calc R . . . . C59 C 1.1343(2) 0.43304(15) 0.06689(9) 0.0250(5) Uani 1 1 d . . . . . C60 C 1.1786(2) 0.51953(15) 0.02299(9) 0.0259(5) Uani 1 1 d . . . . . H60 H 1.2719 0.5179 -0.0003 0.031 Uiso 1 1 calc R . . . . C61 C 1.0900(2) 0.60469(16) 0.01364(9) 0.0263(5) Uani 1 1 d . . . . . H61 H 1.1228 0.6612 -0.0161 0.032 Uiso 1 1 calc R . . . . C62 C 1.2299(3) 0.34662(16) 0.07640(9) 0.0276(5) Uani 1 1 d . . . . . C63 C 1.3760(3) 0.34895(16) 0.04592(10) 0.0275(5) Uani 1 1 d . . . . . C64 C 1.1920(3) 0.25888(17) 0.12002(10) 0.0331(5) Uani 1 1 d . . . . . N9 N 0.6199(4) 1.1838(2) 0.28851(12) 0.0783(9) Uani 1 1 d . . . . . N10 N 0.8942(3) 1.2373(2) 0.40739(12) 0.0703(8) Uani 1 1 d . . . . . N11 N 0.3572(4) 0.64259(19) 0.51401(14) 0.0779(9) Uani 1 1 d . . . . . N12 N 0.6389(3) 0.67938(18) 0.63572(11) 0.0600(7) Uani 1 1 d . . . . . C41 C 0.7069(3) 1.12460(18) 0.38685(11) 0.0413(6) Uani 1 1 d . . . . . C42 C 0.8091(3) 1.1863(2) 0.39876(12) 0.0486(7) Uani 1 1 d . . . . . C43 C 0.6578(4) 1.1577(2) 0.33258(12) 0.0509(7) Uani 1 1 d . . . . . C44 C 0.6647(3) 1.03180(18) 0.42520(10) 0.0364(6) Uani 1 1 d . . . . . C45 C 0.5638(3) 0.96955(18) 0.41254(11) 0.0410(6) Uani 1 1 d . . . . . H45 H 0.5248 0.9903 0.3772 0.049 Uiso 1 1 calc R . . . . C46 C 0.5211(3) 0.88100(18) 0.44964(11) 0.0416(6) Uani 1 1 d . . . . . H46 H 0.4529 0.8416 0.4397 0.050 Uiso 1 1 calc R . . . . C47 C 0.5770(3) 0.84660(17) 0.50289(11) 0.0351(6) Uani 1 1 d . . . . . C48 C 0.6797(3) 0.90785(18) 0.51530(11) 0.0414(6) Uani 1 1 d . . . . . H48 H 0.7207 0.8865 0.5503 0.050 Uiso 1 1 calc R . . . . C49 C 0.7208(3) 0.99660(19) 0.47815(11) 0.0422(6) Uani 1 1 d . . . . . H49 H 0.7890 1.0360 0.4881 0.051 Uiso 1 1 calc R . . . . C50 C 0.5329(3) 0.75483(18) 0.54120(11) 0.0389(6) Uani 1 1 d . . . . . C51 C 0.4354(3) 0.69253(19) 0.52687(13) 0.0503(7) Uani 1 1 d . . . . . C52 C 0.5921(3) 0.71501(19) 0.59344(12) 0.0445(7) Uani 1 1 d . . . . . O1 O -0.1896(4) 0.0919(3) 0.61758(17) 0.1427(16) Uani 1 1 d . . . . . N17 N -0.2119(4) -0.0556(2) 0.68157(14) 0.0762(9) Uani 1 1 d . . . . . C65 C -0.1593(5) 0.0045(4) 0.62944(18) 0.0983(15) Uani 1 1 d . . . . . H65 H -0.0983 -0.0237 0.6027 0.118 Uiso 1 1 calc R . . . . C66 C -0.3042(5) -0.0187(3) 0.7276(2) 0.1025(14) Uani 1 1 d . . . . . H66A H -0.2459 -0.0276 0.7594 0.154 Uiso 1 1 calc GR . . . . H66B H -0.3960 -0.0567 0.7405 0.154 Uiso 1 1 calc GR . . . . H66C H -0.3311 0.0524 0.7129 0.154 Uiso 1 1 calc GR . . . . C67 C -0.1776(6) -0.1632(3) 0.6965(2) 0.1136(16) Uani 1 1 d . . . . . H67A H -0.1271 -0.1822 0.6630 0.170 Uiso 1 1 calc GR . . . . H67B H -0.2711 -0.1991 0.7102 0.170 Uiso 1 1 calc GR . . . . H67C H -0.1114 -0.1804 0.7264 0.170 Uiso 1 1 calc GR . . . . O2 O 0.7083(4) 1.2723(2) 0.16910(11) 0.0944(8) Uani 1 1 d . . . . . H2A H 0.7016 1.2415 0.2037 0.142 Uiso 1 1 calc GR . . . . C68 C 0.6902(6) 1.2082(3) 0.13844(16) 0.1060(17) Uani 1 1 d . . . . . H68A H 0.7152 1.2410 0.0980 0.159 Uiso 1 1 calc GR . . . . H68B H 0.5854 1.1880 0.1458 0.159 Uiso 1 1 calc GR . . . . H68C H 0.7568 1.1489 0.1493 0.159 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 0.02510(16) 0.01699(16) 0.01196(15) 0.00318(11) -0.00261(11) -0.00225(11) N1 0.0252(9) 0.0215(9) 0.0188(9) -0.0014(7) -0.0025(7) -0.0034(7) N2 0.0302(10) 0.0251(10) 0.0196(10) 0.0031(8) -0.0022(8) -0.0065(8) N3 0.0329(10) 0.0250(10) 0.0243(10) 0.0003(8) -0.0093(8) -0.0032(8) N4 0.0240(9) 0.0183(9) 0.0178(9) -0.0011(7) -0.0043(7) -0.0007(7) N5 0.0286(10) 0.0218(9) 0.0209(10) 0.0043(8) -0.0055(8) -0.0034(7) N6 0.0283(10) 0.0271(10) 0.0176(9) -0.0006(8) 0.0001(7) -0.0071(8) N7 0.0540(14) 0.0410(13) 0.0234(11) 0.0080(9) -0.0041(10) -0.0048(11) N8 0.0641(15) 0.0315(12) 0.0271(12) 0.0005(9) 0.0087(11) -0.0087(10) C1 0.0268(11) 0.0238(11) 0.0190(11) -0.0013(9) -0.0041(9) -0.0027(9) C2 0.0298(12) 0.0323(13) 0.0196(11) 0.0003(10) -0.0061(9) -0.0078(10) C3 0.0304(12) 0.0207(11) 0.0194(11) -0.0009(9) -0.0015(9) -0.0016(9) C4 0.0291(12) 0.0234(11) 0.0212(11) -0.0007(9) -0.0010(9) -0.0060(9) C5 0.0258(11) 0.0243(11) 0.0206(11) -0.0031(9) -0.0019(9) -0.0041(9) C6 0.0303(12) 0.0274(12) 0.0240(12) -0.0024(10) -0.0058(9) -0.0053(9) C7 0.0431(15) 0.0501(16) 0.0336(15) 0.0073(12) -0.0134(12) -0.0208(12) C8 0.0410(16) 0.0655(19) 0.0486(18) -0.0023(15) -0.0166(14) -0.0217(14) C9 0.0406(15) 0.0523(17) 0.0408(16) -0.0065(13) -0.0220(13) -0.0061(12) C10 0.0414(14) 0.0333(13) 0.0323(14) -0.0011(11) -0.0181(11) -0.0027(11) C11 0.0394(13) 0.0300(13) 0.0222(12) 0.0050(10) -0.0005(10) -0.0105(10) C12 0.0365(14) 0.0397(14) 0.0338(14) 0.0024(11) -0.0001(11) -0.0180(11) C13 0.0399(14) 0.0464(16) 0.0374(15) -0.0013(12) -0.0103(12) -0.0190(12) C14 0.0384(14) 0.0410(14) 0.0246(13) 0.0020(11) -0.0089(11) -0.0135(11) C15 0.0276(11) 0.0230(11) 0.0216(12) 0.0018(9) -0.0037(9) -0.0031(9) C16 0.0308(12) 0.0259(12) 0.0197(11) 0.0000(9) -0.0028(9) -0.0022(9) C17 0.0607(18) 0.0472(16) 0.0303(15) 0.0136(12) -0.0161(13) -0.0246(14) C18 0.070(2) 0.0525(18) 0.0361(16) 0.0167(13) -0.0147(15) -0.0279(15) C19 0.0452(15) 0.0436(15) 0.0231(13) -0.0008(11) -0.0100(11) -0.0008(12) C20 0.0401(14) 0.0333(13) 0.0228(12) 0.0003(10) -0.0067(10) -0.0060(10) C21 0.0262(11) 0.0185(11) 0.0202(11) -0.0003(9) -0.0061(9) -0.0007(8) C22 0.0306(12) 0.0186(11) 0.0207(11) 0.0015(9) -0.0043(9) 0.0003(9) C23 0.0282(11) 0.0231(11) 0.0181(11) -0.0010(9) -0.0036(9) -0.0030(9) C24 0.0263(11) 0.0233(11) 0.0195(11) -0.0036(9) -0.0035(9) -0.0011(9) C25 0.0247(11) 0.0185(11) 0.0211(11) -0.0004(9) -0.0055(9) -0.0035(8) C26 0.0256(11) 0.0197(11) 0.0202(11) -0.0004(9) -0.0064(9) -0.0040(8) C27 0.0322(12) 0.0246(12) 0.0267(12) -0.0065(10) -0.0065(10) -0.0002(9) C28 0.0376(13) 0.0241(12) 0.0332(14) -0.0073(10) -0.0113(11) 0.0022(10) C29 0.0400(14) 0.0192(12) 0.0413(15) 0.0001(11) -0.0135(12) 0.0002(10) C30 0.0363(13) 0.0220(12) 0.0252(12) 0.0062(9) -0.0059(10) -0.0044(10) C31 0.0364(13) 0.0352(13) 0.0202(12) -0.0062(10) 0.0013(10) -0.0078(10) C32 0.0411(14) 0.0407(15) 0.0293(14) -0.0153(12) 0.0053(11) -0.0035(11) C33 0.0442(15) 0.0314(14) 0.0398(15) -0.0125(12) 0.0017(12) 0.0013(11) C34 0.0389(13) 0.0271(13) 0.0263(13) -0.0029(10) -0.0008(10) 0.0017(10) C35 0.0256(11) 0.0220(11) 0.0200(11) -0.0021(9) -0.0008(9) -0.0029(9) C36 0.0362(12) 0.0216(11) 0.0185(11) -0.0014(9) -0.0033(9) -0.0043(9) C37 0.0403(13) 0.0258(12) 0.0204(12) -0.0017(10) -0.0044(10) -0.0005(10) C38 0.0614(18) 0.0247(13) 0.0230(13) 0.0036(10) -0.0052(12) -0.0031(12) C39 0.0487(16) 0.0341(14) 0.0343(15) -0.0085(12) 0.0109(12) -0.0073(12) C40 0.0376(13) 0.0258(12) 0.0268(13) -0.0021(10) 0.0015(10) -0.0036(10) N13 0.0525(14) 0.0259(11) 0.0427(14) -0.0031(10) -0.0040(11) 0.0006(10) N14 0.0345(12) 0.0367(12) 0.0394(13) -0.0058(10) -0.0054(10) 0.0031(9) N15 0.0387(12) 0.0363(12) 0.0397(13) -0.0114(10) -0.0012(10) 0.0022(9) N16 0.0635(16) 0.0370(13) 0.0452(15) 0.0081(11) -0.0039(12) -0.0037(11) C53 0.0319(12) 0.0235(12) 0.0260(12) -0.0038(10) -0.0057(10) 0.0000(9) C54 0.0362(13) 0.0229(12) 0.0308(13) -0.0064(10) -0.0073(10) 0.0033(10) C55 0.0343(13) 0.0223(12) 0.0281(13) -0.0031(10) -0.0124(11) 0.0003(10) C56 0.0303(12) 0.0227(11) 0.0223(12) -0.0046(9) -0.0081(9) -0.0012(9) C57 0.0294(12) 0.0258(12) 0.0229(12) -0.0036(9) 0.0004(9) -0.0021(9) C58 0.0340(12) 0.0239(12) 0.0203(12) 0.0004(9) -0.0034(9) -0.0033(9) C59 0.0297(12) 0.0238(11) 0.0216(12) -0.0046(9) -0.0069(9) -0.0010(9) C60 0.0272(11) 0.0263(12) 0.0226(12) -0.0043(9) -0.0013(9) -0.0032(9) C61 0.0316(12) 0.0218(11) 0.0231(12) -0.0012(9) -0.0027(9) -0.0049(9) C62 0.0322(12) 0.0222(11) 0.0262(12) -0.0020(9) -0.0052(10) -0.0013(9) C63 0.0359(13) 0.0206(11) 0.0260(12) -0.0048(9) -0.0079(10) 0.0016(9) C64 0.0369(13) 0.0287(13) 0.0310(14) -0.0040(11) -0.0060(11) 0.0032(10) N9 0.122(3) 0.0659(19) 0.0400(17) 0.0021(14) -0.0152(17) -0.0136(17) N10 0.086(2) 0.0615(17) 0.0620(18) -0.0108(14) 0.0035(15) -0.0369(16) N11 0.087(2) 0.0475(16) 0.104(3) -0.0198(16) -0.0156(18) -0.0252(15) N12 0.0747(18) 0.0470(15) 0.0482(16) 0.0015(12) -0.0048(14) 0.0008(13) C41 0.0533(16) 0.0331(14) 0.0338(15) -0.0057(11) 0.0044(12) -0.0100(12) C42 0.0635(19) 0.0369(15) 0.0401(16) -0.0055(13) 0.0081(14) -0.0142(14) C43 0.072(2) 0.0381(16) 0.0361(17) -0.0027(13) 0.0035(15) -0.0108(14) C44 0.0433(14) 0.0333(14) 0.0310(14) -0.0086(11) 0.0024(11) -0.0054(11) C45 0.0524(16) 0.0359(14) 0.0349(15) -0.0067(12) -0.0093(12) -0.0055(12) C46 0.0491(16) 0.0334(14) 0.0455(16) -0.0130(12) -0.0092(13) -0.0070(12) C47 0.0416(14) 0.0257(13) 0.0362(14) -0.0080(11) 0.0021(11) -0.0032(10) C48 0.0573(17) 0.0340(14) 0.0325(14) -0.0044(11) -0.0091(12) -0.0097(12) C49 0.0543(17) 0.0373(15) 0.0359(15) -0.0080(12) -0.0051(13) -0.0148(12) C50 0.0450(15) 0.0272(13) 0.0420(15) -0.0071(11) 0.0000(12) -0.0039(11) C51 0.0585(18) 0.0295(15) 0.059(2) -0.0077(13) -0.0008(15) -0.0071(13) C52 0.0540(17) 0.0259(14) 0.0466(18) -0.0018(12) 0.0024(14) -0.0042(12) O1 0.115(3) 0.100(2) 0.174(4) 0.057(2) -0.050(2) -0.055(2) N17 0.084(2) 0.065(2) 0.078(2) -0.0070(17) -0.0206(18) -0.0171(16) C65 0.096(3) 0.110(4) 0.075(3) 0.022(3) -0.031(2) -0.053(3) C66 0.094(3) 0.075(3) 0.136(4) -0.038(3) 0.012(3) 0.009(2) C67 0.156(5) 0.069(3) 0.111(4) -0.021(3) -0.003(3) -0.011(3) O2 0.125(2) 0.0844(19) 0.0623(17) -0.0103(15) 0.0103(18) -0.0094(17) C68 0.186(5) 0.074(3) 0.070(3) -0.022(2) -0.070(3) 0.025(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N1 Co1 N2 77.87(7) . . N1 Co1 N3 77.07(7) . . N1 Co1 N5 95.94(7) . . N1 Co1 N6 102.71(7) . . N3 Co1 N2 154.84(7) . . N4 Co1 N1 173.97(7) . . N4 Co1 N2 96.98(7) . . N4 Co1 N3 108.16(7) . . N4 Co1 N5 80.92(7) . . N4 Co1 N6 80.30(7) . . N5 Co1 N2 91.45(7) . . N5 Co1 N3 93.40(7) . . N6 Co1 N2 90.26(7) . . N6 Co1 N3 92.96(7) . . N6 Co1 N5 161.21(7) . . C1 N1 Co1 119.78(14) . . C5 N1 Co1 120.21(13) . . C5 N1 C1 119.14(17) . . C11 N2 Co1 130.41(15) . . C11 N2 C15 118.14(18) . . C15 N2 Co1 110.70(13) . . C6 N3 Co1 112.11(13) . . C10 N3 Co1 129.92(16) . . C10 N3 C6 117.9(2) . . C21 N4 Co1 119.80(14) . . C25 N4 Co1 118.95(13) . . C25 N4 C21 120.53(18) . . C26 N5 Co1 113.41(13) . . C30 N5 Co1 128.34(16) . . C30 N5 C26 118.0(2) . . C31 N6 Co1 127.58(15) . . C31 N6 C35 117.90(19) . . C35 N6 Co1 114.50(14) . . C19 N7 C18 115.5(2) . . C38 N8 C39 115.9(2) . . N1 C1 C2 121.18(19) . . N1 C1 C15 115.39(18) . . C2 C1 C15 123.38(18) . . C1 C2 H2 119.8 . . C1 C2 C3 120.39(19) . . C3 C2 H2 119.8 . . C2 C3 C4 117.78(19) . . C2 C3 C16 121.04(19) . . C4 C3 C16 121.17(19) . . C3 C4 H4 120.0 . . C5 C4 C3 120.0(2) . . C5 C4 H4 120.0 . . N1 C5 C4 121.46(18) . . N1 C5 C6 114.48(18) . . C4 C5 C6 124.06(19) . . N3 C6 C5 114.72(19) . . N3 C6 C7 122.06(19) . . C7 C6 C5 123.2(2) . . C6 C7 H7 120.6 . . C8 C7 C6 118.7(2) . . C8 C7 H7 120.6 . . C7 C8 H8 120.3 . . C9 C8 C7 119.4(2) . . C9 C8 H8 120.3 . . C8 C9 H9 121.0 . . C8 C9 C10 118.0(2) . . C10 C9 H9 121.0 . . N3 C10 C9 123.8(2) . . N3 C10 H10 118.1 . . C9 C10 H10 118.1 . . N2 C11 H11 118.6 . . N2 C11 C12 122.8(2) . . C12 C11 H11 118.6 . . C11 C12 H12 120.5 . . C13 C12 C11 119.0(2) . . C13 C12 H12 120.5 . . C12 C13 H13 120.6 . . C12 C13 C14 118.8(2) . . C14 C13 H13 120.6 . . C13 C14 H14 120.4 . . C15 C14 C13 119.3(2) . . C15 C14 H14 120.4 . . N2 C15 C1 114.81(18) . . N2 C15 C14 121.9(2) . . C14 C15 C1 123.2(2) . . C17 C16 C3 122.2(2) . . C17 C16 C20 116.6(2) . . C20 C16 C3 121.2(2) . . C16 C17 H17 120.4 . . C18 C17 C16 119.3(2) . . C18 C17 H17 120.4 . . N7 C18 C17 124.6(3) . . N7 C18 H18 117.7 . . C17 C18 H18 117.7 . . N7 C19 H19 117.7 . . N7 C19 C20 124.6(2) . . C20 C19 H19 117.7 . . C16 C20 H20 120.3 . . C19 C20 C16 119.4(2) . . C19 C20 H20 120.3 . . N4 C21 C22 120.9(2) . . N4 C21 C35 112.00(18) . . C22 C21 C35 126.89(19) . . C21 C22 H22 120.2 . . C21 C22 C23 119.64(19) . . C23 C22 H22 120.2 . . C22 C23 C36 121.18(19) . . C24 C23 C22 118.38(19) . . C24 C23 C36 120.3(2) . . C23 C24 H24 120.2 . . C25 C24 C23 119.7(2) . . C25 C24 H24 120.2 . . N4 C25 C24 120.80(19) . . N4 C25 C26 112.67(18) . . C24 C25 C26 126.3(2) . . N5 C26 C25 113.76(19) . . N5 C26 C27 122.30(19) . . C27 C26 C25 123.8(2) . . C26 C27 H27 120.7 . . C28 C27 C26 118.6(2) . . C28 C27 H27 120.7 . . C27 C28 H28 120.2 . . C29 C28 C27 119.6(2) . . C29 C28 H28 120.2 . . 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 118.9 . . C29 C30 H30 118.9 . . N6 C31 H31 118.5 . . N6 C31 C32 122.9(2) . . C32 C31 H31 118.5 . . C31 C32 H32 120.5 . . C33 C32 C31 119.0(2) . . C33 C32 H32 120.5 . . C32 C33 H33 120.5 . . C32 C33 C34 119.0(2) . . C34 C33 H33 120.5 . . C33 C34 H34 120.6 . . C35 C34 C33 118.8(2) . . C35 C34 H34 120.6 . . N6 C35 C21 113.20(18) . . N6 C35 C34 122.3(2) . . C34 C35 C21 124.46(19) . . C37 C36 C23 122.3(2) . . C37 C36 C40 117.0(2) . . C40 C36 C23 120.62(19) . . C36 C37 H37 120.6 . . C38 C37 C36 118.8(2) . . C38 C37 H37 120.6 . . N8 C38 C37 124.8(2) . . N8 C38 H38 117.6 . . C37 C38 H38 117.6 . . N8 C39 H39 118.1 . . N8 C39 C40 123.9(2) . . C40 C39 H39 118.1 . . C36 C40 H40 120.2 . . C39 C40 C36 119.5(2) . . C39 C40 H40 120.2 . . C54 C53 C55 116.96(19) . . C56 C53 C54 121.5(2) . . C56 C53 C55 121.4(2) . . N13 C54 C53 179.4(3) . . N14 C55 C53 178.2(2) . . C53 C56 C57 121.7(2) . . C53 C56 C61 121.0(2) . . C61 C56 C57 117.29(19) . . C56 C57 H57 119.5 . . C58 C57 C56 121.0(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 117.45(19) . . C62 C59 C58 122.6(2) . . C62 C59 C60 120.0(2) . . C59 C60 H60 119.4 . . C61 C60 C59 121.2(2) . . C61 C60 H60 119.4 . . C56 C61 H61 119.2 . . C60 C61 C56 121.6(2) . . C60 C61 H61 119.2 . . C59 C62 C63 120.1(2) . . C59 C62 C64 122.2(2) . . C64 C62 C63 117.4(2) . . N15 C63 C62 177.2(2) . . N16 C64 C62 179.5(3) . . C42 C41 C43 115.9(2) . . C42 C41 C44 122.1(2) . . C43 C41 C44 121.9(2) . . N10 C42 C41 178.6(3) . . N9 C43 C41 179.0(4) . . C41 C44 C45 121.8(2) . . C49 C44 C41 121.6(2) . . C49 C44 C45 116.6(2) . . C44 C45 H45 119.0 . . C46 C45 C44 122.0(2) . . C46 C45 H45 119.0 . . C45 C46 H46 119.5 . . C45 C46 C47 121.1(2) . . C47 C46 H46 119.5 . . C48 C47 C46 117.1(2) . . C50 C47 C46 121.0(2) . . C50 C47 C48 121.9(2) . . C47 C48 H48 119.3 . . C49 C48 C47 121.4(2) . . C49 C48 H48 119.3 . . C44 C49 H49 119.1 . . C48 C49 C44 121.8(2) . . C48 C49 H49 119.1 . . C47 C50 C51 121.0(2) . . C47 C50 C52 122.9(2) . . C52 C50 C51 115.9(2) . . N11 C51 C50 178.5(3) . . N12 C52 C50 177.5(3) . . C65 N17 C66 124.3(4) . . C65 N17 C67 121.0(4) . . C67 N17 C66 114.7(3) . . O1 C65 N17 120.3(5) . . O1 C65 H65 119.8 . . N17 C65 H65 119.8 . . 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 1.9566(18) . Co1 N2 2.2434(18) . Co1 N3 2.2233(19) . Co1 N4 1.8857(18) . Co1 N5 2.0213(19) . Co1 N6 2.0104(19) . N1 C1 1.359(3) . N1 C5 1.358(3) . N2 C11 1.335(3) . N2 C15 1.347(3) . N3 C6 1.339(3) . N3 C10 1.333(3) . N4 C21 1.352(3) . N4 C25 1.348(3) . N5 C26 1.355(3) . N5 C30 1.346(3) . N6 C31 1.341(3) . N6 C35 1.360(3) . N7 C18 1.333(3) . N7 C19 1.323(3) . N8 C38 1.330(3) . N8 C39 1.334(3) . C1 C2 1.381(3) . C1 C15 1.485(3) . C2 H2 0.9500 . C2 C3 1.391(3) . C3 C4 1.395(3) . C3 C16 1.481(3) . C4 H4 0.9500 . C4 C5 1.382(3) . C5 C6 1.488(3) . C6 C7 1.392(3) . C7 H7 0.9500 . C7 C8 1.385(3) . C8 H8 0.9500 . C8 C9 1.373(4) . C9 H9 0.9500 . C9 C10 1.381(4) . C10 H10 0.9500 . C11 H11 0.9500 . C11 C12 1.390(3) . C12 H12 0.9500 . C12 C13 1.369(3) . C13 H13 0.9500 . C13 C14 1.387(3) . C14 H14 0.9500 . C14 C15 1.386(3) . C16 C17 1.386(3) . C16 C20 1.387(3) . C17 H17 0.9500 . C17 C18 1.371(3) . C18 H18 0.9500 . C19 H19 0.9500 . C19 C20 1.370(3) . C20 H20 0.9500 . C21 C22 1.376(3) . C21 C35 1.471(3) . C22 H22 0.9500 . C22 C23 1.403(3) . C23 C24 1.389(3) . C23 C36 1.483(3) . C24 H24 0.9500 . C24 C25 1.387(3) . C25 C26 1.472(3) . C26 C27 1.386(3) . C27 H27 0.9500 . C27 C28 1.379(3) . C28 H28 0.9500 . C28 C29 1.371(3) . C29 H29 0.9500 . C29 C30 1.382(3) . C30 H30 0.9500 . C31 H31 0.9500 . C31 C32 1.377(3) . C32 H32 0.9500 . C32 C33 1.376(3) . C33 H33 0.9500 . C33 C34 1.395(3) . C34 H34 0.9500 . C34 C35 1.375(3) . C36 C37 1.386(3) . C36 C40 1.393(3) . C37 H37 0.9500 . C37 C38 1.377(3) . C38 H38 0.9500 . C39 H39 0.9500 . C39 C40 1.376(3) . C40 H40 0.9500 . N13 C54 1.153(3) . N14 C55 1.157(3) . N15 C63 1.156(3) . N16 C64 1.148(3) . C53 C54 1.414(3) . C53 C55 1.423(3) . C53 C56 1.408(3) . C56 C57 1.435(3) . C56 C61 1.414(3) . C57 H57 0.9500 . C57 C58 1.358(3) . C58 H58 0.9500 . C58 C59 1.424(3) . C59 C60 1.420(3) . C59 C62 1.410(3) . C60 H60 0.9500 . C60 C61 1.361(3) . C61 H61 0.9500 . C62 C63 1.416(3) . C62 C64 1.416(3) . N9 C43 1.141(4) . N10 C42 1.159(3) . N11 C51 1.155(3) . N12 C52 1.149(3) . C41 C42 1.414(4) . C41 C43 1.415(4) . C41 C44 1.417(3) . C44 C45 1.420(3) . C44 C49 1.415(3) . C45 H45 0.9500 . C45 C46 1.362(3) . C46 H46 0.9500 . C46 C47 1.420(3) . C47 C48 1.419(3) . C47 C50 1.411(3) . C48 H48 0.9500 . C48 C49 1.362(3) . C49 H49 0.9500 . C50 C51 1.419(4) . C50 C52 1.419(4) . O1 C65 1.190(5) . N17 C65 1.370(5) . N17 C66 1.496(5) . N17 C67 1.461(4) . C65 H65 0.9500 . C66 H66A 0.9800 . C66 H66B 0.9800 . C66 H66C 0.9800 . C67 H67A 0.9800 . C67 H67B 0.9800 . C67 H67C 0.9800 . O2 H2A 0.8400 . O2 C68 1.352(4) . C68 H68A 0.9800 . C68 H68B 0.9800 . C68 H68C 0.9800 .