#------------------------------------------------------------------------------ #$Date: 2017-06-27 04:40:36 +0300 (Tue, 27 Jun 2017) $ #$Revision: 198150 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/85/7228545.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_7228545 loop_ _publ_author_name 'Xiong, Ying' 'Liu, Guo Cheng' 'Wang, Xiuli' 'Zhang, Juwen' 'Lin, Hongyan' 'Sha, Xiao Ting' _publ_section_title ; Polycarboxylates-directed pyridyl-amide-based CoII complexes: fluorescent recognition of Fe3+ and Fe3+-functionalized composite materials for enhancing photocatalytic activities ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE00800G _journal_year 2017 _chemical_formula_sum 'C78 H74 Cl0 Co3 N12 O26' _chemical_formula_weight 1772.28 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-04-05 deposited with the CCDC. 2017-06-26 downloaded from the CCDC. ; _cell_angle_alpha 84.5680(10) _cell_angle_beta 87.8930(10) _cell_angle_gamma 79.8920(10) _cell_formula_units_Z 1 _cell_length_a 10.1876(5) _cell_length_b 10.6755(5) _cell_length_c 17.3180(8) _cell_measurement_reflns_used 5229 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.256 _cell_measurement_theta_min 1.181 _cell_volume 1845.52(15) _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 13758 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.256 _diffrn_reflns_theta_min 1.181 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_description BLOCK _exptl_crystal_F_000 915 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.110 _exptl_transmission_factor_max 0.999 _exptl_transmission_factor_min 0.994 _refine_diff_density_max 0.600 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 538 _refine_ls_number_reflns 9095 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0396 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+1.2021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1091 _refine_ls_wR_factor_ref 0.1221 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7278 _reflns_number_total 9095 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce00800g2.cif _cod_data_source_block 6 _cod_database_code 7228545 _shelx_shelxl_version_number 2014/7 _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_min 0.894 _shelx_estimated_absorpt_t_max 0.921 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 10.1876 10.6755 17.3180 84.568 87.893 79.892 ZERR 1.00 0.0005 0.0005 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H N O CL CO UNIT 78 74 12 26 0 3 MERG 2 ACTA FMAP 2 PLAN 5 SIZE 0.15 0.13 0.11 LIST 1 DFIX 3.2 0.01 O3W O8 L.S. 4 WGHT 0.068800 1.202100 FVAR 0.12828 CO1 6 -0.500000 0.500000 0.500000 10.50000 0.01899 0.01746 = 0.02289 -0.00019 -0.00067 -0.00606 O1 4 -0.459885 0.681730 0.487707 11.00000 0.02425 0.02079 = 0.03285 -0.00120 0.00293 -0.00954 N1 3 -0.477306 0.485736 0.626058 11.00000 0.02394 0.02444 = 0.02606 -0.00254 -0.00289 -0.00711 C1 1 -0.361185 0.733256 0.464286 11.00000 0.02153 0.02181 = 0.01847 -0.00359 -0.00064 -0.00730 O1W 4 0.041182 1.216733 0.471370 11.00000 0.03592 0.06511 = 0.03479 -0.00277 -0.00551 -0.02365 AFIX 3 H1WA 2 0.093382 1.251363 0.496322 11.00000 -1.20000 H1WB 2 -0.006588 1.179723 0.504310 11.00000 -1.20000 AFIX 0 CO2 6 0.044239 1.204757 0.351711 11.00000 0.01510 0.02363 = 0.02956 -0.00129 -0.00008 -0.00652 O2 4 -0.241447 0.677664 0.465567 11.00000 0.02026 0.02342 = 0.04109 -0.00047 -0.00466 -0.00324 N2 3 -0.309098 0.484818 0.899599 11.00000 0.02653 0.03485 = 0.02856 -0.01064 -0.00503 -0.00235 AFIX 43 H2A 2 -0.247517 0.433637 0.877542 11.00000 -1.20000 AFIX 0 C2 1 -0.394616 0.870487 0.430686 11.00000 0.01656 0.02080 = 0.01952 -0.00232 0.00001 -0.00513 O2W 4 -0.292288 0.428791 0.478885 11.00000 0.02622 0.02794 = 0.04529 -0.00275 0.00342 -0.00436 AFIX 3 H2WA 2 -0.250998 0.491461 0.470095 11.00000 -1.20000 H2WB 2 -0.276599 0.383362 0.440756 11.00000 -1.20000 AFIX 0 O3W 4 0.398549 0.760166 -0.182186 11.00000 0.34168 0.18123 = 0.17125 -0.00279 -0.01130 0.11313 N3 3 0.066400 1.185785 0.228650 11.00000 0.02740 0.03191 = 0.03015 -0.00297 0.00194 -0.01042 O3 4 -0.107658 1.103048 0.364721 11.00000 0.01714 0.02993 = 0.04445 -0.00091 0.00100 -0.00994 C3 1 -0.527682 0.921804 0.415847 11.00000 0.01664 0.02373 = 0.02461 -0.00327 -0.00009 -0.00748 AFIX 43 H3A 2 -0.592662 0.870910 0.426273 11.00000 -1.20000 AFIX 0 O4W 4 0.170321 0.810568 0.446025 11.00000 0.05627 0.06614 = 0.10555 0.01361 0.00795 -0.02050 AFIX 3 H4WA 2 0.232271 0.762808 0.423125 11.00000 -1.20000 H4WB 2 0.194411 0.882488 0.447925 11.00000 -1.20000 AFIX 0 C4 1 -0.564685 1.048040 0.385667 11.00000 0.01322 0.02581 = 0.02192 -0.00341 -0.00058 -0.00381 O4 4 -0.265757 1.274326 0.352712 11.00000 0.03590 0.02458 = 0.09326 0.00622 0.00655 -0.01109 N4 3 0.249742 1.158144 -0.047351 11.00000 0.03220 0.04325 = 0.03589 -0.01461 0.00738 -0.01484 AFIX 43 H4A 2 0.284676 1.220456 -0.034122 11.00000 -1.20000 AFIX 0 O5 4 -0.746597 1.219732 0.360728 11.00000 0.01950 0.02648 = 0.04295 -0.00202 -0.00319 -0.00164 N5 3 0.898934 1.154325 -0.254120 11.00000 0.03534 0.02619 = 0.03634 -0.01027 0.00961 -0.00830 AFIX 43 H5A 2 0.862107 1.109060 -0.282585 11.00000 -1.20000 AFIX 0 C5 1 -0.709002 1.100766 0.370908 11.00000 0.01656 0.02994 = 0.02521 -0.00159 -0.00056 -0.00348 O6 4 -0.791805 1.026170 0.367419 11.00000 0.01701 0.03250 = 0.04736 -0.00144 -0.00459 -0.00798 C6 1 -0.467046 1.124219 0.370578 11.00000 0.01950 0.02118 = 0.02467 -0.00029 0.00188 -0.00376 AFIX 43 H6A 2 -0.491396 1.209490 0.351997 11.00000 -1.20000 AFIX 0 O7 4 -0.356677 0.624651 0.991385 11.00000 0.03087 0.04140 = 0.03777 -0.01764 0.00230 -0.00701 C7 1 -0.332769 1.073188 0.383214 11.00000 0.01652 0.02095 = 0.02330 -0.00336 0.00293 -0.00738 O8 4 0.271788 0.993419 -0.120625 11.00000 0.05124 0.07145 = 0.08723 -0.05269 0.02860 -0.03501 C8 1 -0.228182 1.157314 0.365391 11.00000 0.02056 0.02272 = 0.03072 -0.00194 0.00310 -0.00809 O9 4 0.885039 1.265722 -0.149759 11.00000 0.03206 0.04433 = 0.03963 -0.01675 0.00421 -0.01232 C9 1 -0.297562 0.946510 0.413390 11.00000 0.01475 0.02149 = 0.02223 -0.00333 0.00053 -0.00410 AFIX 43 H9A 2 -0.208353 0.912352 0.422075 11.00000 -1.20000 AFIX 0 N9 3 -0.011461 1.409752 0.333596 11.00000 0.02325 0.02727 = 0.03395 -0.00178 0.00157 -0.00612 C10 1 -0.384001 0.540376 0.655016 11.00000 0.02987 0.03639 = 0.02992 0.00006 -0.00070 -0.01558 AFIX 43 H10A 2 -0.327175 0.577864 0.620409 11.00000 -1.20000 AFIX 0 C11 1 -0.557017 0.433172 0.677759 11.00000 0.03383 0.03990 = 0.03003 -0.00393 -0.00308 -0.02098 AFIX 43 H11A 2 -0.622366 0.393500 0.659311 11.00000 -1.20000 AFIX 0 C12 1 -0.547766 0.434486 0.756867 11.00000 0.03159 0.04272 = 0.02674 -0.00203 0.00035 -0.01712 AFIX 43 H12A 2 -0.606274 0.396874 0.790219 11.00000 -1.20000 AFIX 0 C13 1 -0.366962 0.544457 0.733487 11.00000 0.03434 0.04127 = 0.03331 -0.00341 -0.00522 -0.02032 AFIX 43 H13A 2 -0.299061 0.582424 0.750443 11.00000 -1.20000 AFIX 0 C14 1 -0.451003 0.492025 0.786656 11.00000 0.02413 0.02607 = 0.02682 -0.00403 -0.00429 -0.00292 C15 1 -0.445294 0.500247 0.872717 11.00000 0.02576 0.04668 = 0.02653 -0.00930 -0.00256 -0.00642 AFIX 23 H15A 2 -0.493889 0.582492 0.885473 11.00000 -1.20000 H15B 2 -0.488877 0.434499 0.899752 11.00000 -1.20000 AFIX 0 C16 1 -0.276597 0.547262 0.957193 11.00000 0.02956 0.02857 = 0.02240 -0.00409 0.00022 -0.00814 C17 1 -0.132726 0.519927 0.978499 11.00000 0.02749 0.02679 = 0.02585 -0.00699 -0.00128 -0.00631 C18 1 -0.031101 0.503894 0.922423 11.00000 0.03270 0.04298 = 0.02089 -0.00646 -0.00232 -0.00759 AFIX 43 H18A 2 -0.051854 0.506689 0.870371 11.00000 -1.20000 AFIX 0 C19 1 0.100533 0.483838 0.944198 11.00000 0.03141 0.04505 = 0.02513 -0.01051 0.00232 -0.00725 AFIX 43 H19A 2 0.168154 0.472764 0.906629 11.00000 -1.20000 AFIX 0 C20 1 -0.034482 1.173006 0.184104 11.00000 0.02553 0.04699 = 0.03515 -0.00775 0.00481 -0.01256 AFIX 43 H20A 2 -0.118180 1.172457 0.207325 11.00000 -1.20000 AFIX 0 C21 1 0.186498 1.181852 0.193475 11.00000 0.02633 0.03733 = 0.03074 0.00007 -0.00220 -0.01035 AFIX 43 H21A 2 0.258129 1.190587 0.223099 11.00000 -1.20000 AFIX 0 C22 1 0.209399 1.165571 0.115839 11.00000 0.02289 0.03738 = 0.03566 -0.00260 0.00484 -0.00605 AFIX 43 H22A 2 0.295105 1.160896 0.094585 11.00000 -1.20000 AFIX 0 C23 1 -0.020303 1.160661 0.105711 11.00000 0.02681 0.04524 = 0.03586 -0.01013 0.00057 -0.01271 AFIX 43 H23A 2 -0.094076 1.155303 0.076914 11.00000 -1.20000 AFIX 0 C24 1 0.104071 1.156219 0.069689 11.00000 0.02949 0.02667 = 0.03227 -0.00616 0.00322 -0.00712 C25 1 0.119092 1.142002 -0.016042 11.00000 0.03051 0.05553 = 0.03532 -0.01474 0.00527 -0.01539 AFIX 23 H25A 2 0.103157 1.057920 -0.025620 11.00000 -1.20000 H25B 2 0.051887 1.204733 -0.043157 11.00000 -1.20000 AFIX 0 C26 1 0.317782 1.078973 -0.096272 11.00000 0.03454 0.04238 = 0.03641 -0.01232 0.00628 -0.01343 C27 1 0.453904 1.105578 -0.120173 11.00000 0.03158 0.02944 = 0.03525 -0.00960 0.00486 -0.00843 C28 1 0.497149 1.095222 -0.196934 11.00000 0.03477 0.04407 = 0.03359 -0.01804 0.00201 -0.01140 AFIX 43 H28A 2 0.443183 1.068816 -0.232133 11.00000 -1.20000 AFIX 0 C29 1 0.620175 1.124147 -0.220844 11.00000 0.03429 0.03992 = 0.02867 -0.01151 0.00515 -0.00829 AFIX 43 H29A 2 0.647473 1.119331 -0.272476 11.00000 -1.20000 AFIX 0 C30 1 0.703792 1.160522 -0.168174 11.00000 0.02776 0.02516 = 0.02941 -0.00706 0.00448 -0.00379 C31 1 0.537723 1.140827 -0.067105 11.00000 0.03445 0.03584 = 0.02824 -0.00599 0.00348 -0.00831 AFIX 43 H31A 2 0.509939 1.146874 -0.015630 11.00000 -1.20000 AFIX 0 C32 1 0.661482 1.166644 -0.090912 11.00000 0.03170 0.03364 = 0.02833 -0.00696 -0.00079 -0.00781 AFIX 43 H32A 2 0.717459 1.188406 -0.055043 11.00000 -1.20000 AFIX 0 C33 1 0.836009 1.196860 -0.190247 11.00000 0.02924 0.02275 = 0.03119 -0.00370 0.00170 -0.00325 C34 1 1.030807 1.184898 -0.275624 11.00000 0.03238 0.02556 = 0.04712 -0.00559 0.01341 -0.00178 AFIX 23 H34A 2 1.066905 1.137795 -0.319081 11.00000 -1.20000 H34B 2 1.090083 1.157547 -0.232374 11.00000 -1.20000 AFIX 0 C36 1 -0.090652 1.473756 0.277754 11.00000 0.03116 0.03358 = 0.03589 -0.00040 -0.00292 -0.00987 AFIX 43 H36A 2 -0.141134 1.428722 0.250559 11.00000 -1.20000 AFIX 0 C37 1 -0.100822 1.603857 0.258650 11.00000 0.03207 0.03031 = 0.03710 0.00255 -0.00087 -0.00300 AFIX 43 H37A 2 -0.157622 1.644371 0.219595 11.00000 -1.20000 AFIX 0 C38 1 -0.026622 1.673715 0.297564 11.00000 0.02583 0.02571 = 0.03683 -0.00492 0.01099 -0.00279 C39 1 0.050800 1.608451 0.356936 11.00000 0.04033 0.03226 = 0.04578 -0.00773 -0.00695 -0.01061 AFIX 43 H39A 2 0.100357 1.651833 0.385862 11.00000 -1.20000 AFIX 0 C40 1 0.055043 1.478944 0.373615 11.00000 0.03118 0.03302 = 0.04179 -0.00005 -0.00710 -0.00518 AFIX 43 H40A 2 0.106687 1.437594 0.414719 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P-1 REM R1 = 0.0396 for 7278 Fo > 4sig(Fo) and 0.0541 for all 9095 data REM 538 parameters refined using 1 restraints END WGHT 0.0649 0.9677 REM Highest difference peak 0.600, deepest hole -0.814, 1-sigma level 0.095 Q1 1 -0.2681 1.2452 0.3006 11.00000 0.05 0.58 Q2 1 -0.2019 0.5273 0.9725 11.00000 0.05 0.41 Q3 1 0.3207 0.9527 -0.0970 11.00000 0.05 0.39 Q4 1 0.3843 1.0989 -0.1040 11.00000 0.05 0.38 Q5 1 -0.4357 0.4771 0.8297 11.00000 0.05 0.35 ; _shelx_res_checksum 71748 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 Co1 Co -0.5000 0.5000 0.5000 0.01953(10) Uani 1 2 d S . P O1 O -0.45988(15) 0.68173(14) 0.48771(9) 0.0254(3) Uani 1 1 d . . . N1 N -0.47731(18) 0.48574(18) 0.62606(11) 0.0244(4) Uani 1 1 d . . . C1 C -0.3612(2) 0.7333(2) 0.46429(12) 0.0201(4) Uani 1 1 d . . . O1W O 0.04118(19) 1.2167(2) 0.47137(11) 0.0435(5) Uani 1 1 d . . . H1WA H 0.0934 1.2514 0.4963 0.052 Uiso 1 1 d R U . H1WB H -0.0066 1.1797 0.5043 0.052 Uiso 1 1 d R U . Co2 Co 0.04424(3) 1.20476(3) 0.35171(2) 0.02246(9) Uani 1 1 d . . . O2 O -0.24145(15) 0.67766(15) 0.46557(10) 0.0284(3) Uani 1 1 d . . . N2 N -0.3091(2) 0.4848(2) 0.89960(11) 0.0297(4) Uani 1 1 d . . . H2A H -0.2475 0.4336 0.8775 0.036 Uiso 1 1 calc R U . C2 C -0.39462(19) 0.87049(19) 0.43069(11) 0.0187(4) Uani 1 1 d . . . O2W O -0.29229(16) 0.42879(16) 0.47888(11) 0.0333(4) Uani 1 1 d . . . H2WA H -0.2510 0.4915 0.4701 0.040 Uiso 1 1 d R U . H2WB H -0.2766 0.3834 0.4408 0.040 Uiso 1 1 d R U . O3W O 0.3985(9) 0.7602(6) -0.1822(4) 0.251(4) Uani 1 1 d D . . N3 N 0.0664(2) 1.1858(2) 0.22865(12) 0.0292(4) Uani 1 1 d . . . O3 O -0.10766(15) 1.10305(16) 0.36472(10) 0.0300(4) Uani 1 1 d . . . C3 C -0.5277(2) 0.9218(2) 0.41585(12) 0.0211(4) Uani 1 1 d . . . H3A H -0.5927 0.8709 0.4263 0.025 Uiso 1 1 calc R U . O4W O 0.1703(3) 0.8106(3) 0.44603(18) 0.0764(8) Uani 1 1 d . . . H4WA H 0.2323 0.7628 0.4231 0.092 Uiso 1 1 d R U . H4WB H 0.1944 0.8825 0.4479 0.092 Uiso 1 1 d R U . C4 C -0.56469(19) 1.0480(2) 0.38567(12) 0.0202(4) Uani 1 1 d . . . O4 O -0.2658(2) 1.27433(18) 0.35271(15) 0.0515(6) Uani 1 1 d . . . N4 N 0.2497(2) 1.1581(2) -0.04735(13) 0.0356(5) Uani 1 1 d . . . H4A H 0.2847 1.2205 -0.0341 0.043 Uiso 1 1 calc R U . O5 O -0.74660(15) 1.21973(16) 0.36073(10) 0.0299(4) Uani 1 1 d . . . N5 N 0.8989(2) 1.15433(19) -0.25412(12) 0.0320(4) Uani 1 1 d . . . H5A H 0.8621 1.1091 -0.2826 0.038 Uiso 1 1 calc R U . C5 C -0.7090(2) 1.1008(2) 0.37091(13) 0.0240(4) Uani 1 1 d . . . O6 O -0.79181(15) 1.02617(16) 0.36742(11) 0.0319(4) Uani 1 1 d . . . C6 C -0.4670(2) 1.1242(2) 0.37058(12) 0.0219(4) Uani 1 1 d . . . H6A H -0.4914 1.2095 0.3520 0.026 Uiso 1 1 calc R U . O7 O -0.35668(17) 0.62465(18) 0.99139(11) 0.0358(4) Uani 1 1 d . . . C7 C -0.3328(2) 1.0732(2) 0.38321(12) 0.0197(4) Uani 1 1 d . . . O8 O 0.2718(2) 0.9934(2) -0.12062(16) 0.0648(7) Uani 1 1 d D . . C8 C -0.2282(2) 1.1573(2) 0.36539(13) 0.0243(4) Uani 1 1 d . . . O9 O 0.88504(18) 1.26572(18) -0.14976(11) 0.0373(4) Uani 1 1 d . . . C9 C -0.2976(2) 0.94651(19) 0.41339(12) 0.0193(4) Uani 1 1 d . . . H9A H -0.2084 0.9124 0.4221 0.023 Uiso 1 1 calc R U . N9 N -0.01146(19) 1.40975(19) 0.33360(12) 0.0281(4) Uani 1 1 d . . . C10 C -0.3840(2) 0.5404(2) 0.65502(14) 0.0311(5) Uani 1 1 d . . . H10A H -0.3272 0.5779 0.6204 0.037 Uiso 1 1 calc R U . C11 C -0.5570(3) 0.4332(2) 0.67776(14) 0.0327(5) Uani 1 1 d . . . H11A H -0.6224 0.3935 0.6593 0.039 Uiso 1 1 calc R U . C12 C -0.5478(2) 0.4345(3) 0.75687(14) 0.0325(5) Uani 1 1 d . . . H12A H -0.6063 0.3969 0.7902 0.039 Uiso 1 1 calc R U . C13 C -0.3670(3) 0.5445(3) 0.73349(15) 0.0345(5) Uani 1 1 d . . . H13A H -0.2991 0.5824 0.7504 0.041 Uiso 1 1 calc R U . C14 C -0.4510(2) 0.4920(2) 0.78666(13) 0.0256(4) Uani 1 1 d . . . C15 C -0.4453(2) 0.5002(3) 0.87272(14) 0.0325(5) Uani 1 1 d . . . H15A H -0.4939 0.5825 0.8855 0.039 Uiso 1 1 calc R U . H15B H -0.4889 0.4345 0.8998 0.039 Uiso 1 1 calc R U . C16 C -0.2766(2) 0.5473(2) 0.95719(13) 0.0264(5) Uani 1 1 d . . . C17 C -0.1327(2) 0.5199(2) 0.97850(13) 0.0262(4) Uani 1 1 d . . . C18 C -0.0311(2) 0.5039(3) 0.92242(14) 0.0318(5) Uani 1 1 d . . . H18A H -0.0519 0.5067 0.8704 0.038 Uiso 1 1 calc R U . C19 C 0.1005(3) 0.4838(3) 0.94420(14) 0.0334(5) Uani 1 1 d . . . H19A H 0.1682 0.4728 0.9066 0.040 Uiso 1 1 calc R U . C20 C -0.0345(2) 1.1730(3) 0.18410(15) 0.0350(5) Uani 1 1 d . . . H20A H -0.1182 1.1725 0.2073 0.042 Uiso 1 1 calc R U . C21 C 0.1865(2) 1.1819(2) 0.19347(14) 0.0310(5) Uani 1 1 d . . . H21A H 0.2581 1.1906 0.2231 0.037 Uiso 1 1 calc R U . C22 C 0.2094(2) 1.1656(2) 0.11584(15) 0.0321(5) Uani 1 1 d . . . H22A H 0.2951 1.1609 0.0946 0.038 Uiso 1 1 calc R U . C23 C -0.0203(2) 1.1607(3) 0.10571(15) 0.0348(5) Uani 1 1 d . . . H23A H -0.0941 1.1553 0.0769 0.042 Uiso 1 1 calc R U . C24 C 0.1041(2) 1.1562(2) 0.06969(14) 0.0291(5) Uani 1 1 d . . . C25 C 0.1191(3) 1.1420(3) -0.01604(16) 0.0389(6) Uani 1 1 d . . . H25A H 0.1032 1.0579 -0.0256 0.047 Uiso 1 1 calc R U . H25B H 0.0519 1.2047 -0.0432 0.047 Uiso 1 1 calc R U . C26 C 0.3178(3) 1.0790(3) -0.09627(16) 0.0366(6) Uani 1 1 d . . . C27 C 0.4539(2) 1.1056(2) -0.12017(15) 0.0314(5) Uani 1 1 d . . . C28 C 0.4971(3) 1.0952(3) -0.19693(15) 0.0360(6) Uani 1 1 d . . . H28A H 0.4432 1.0688 -0.2321 0.043 Uiso 1 1 calc R U . C29 C 0.6202(3) 1.1241(3) -0.22084(15) 0.0337(5) Uani 1 1 d . . . H29A H 0.6475 1.1193 -0.2725 0.040 Uiso 1 1 calc R U . C30 C 0.7038(2) 1.1605(2) -0.16817(14) 0.0274(5) Uani 1 1 d . . . C31 C 0.5377(3) 1.1408(2) -0.06710(15) 0.0325(5) Uani 1 1 d . . . H31A H 0.5099 1.1469 -0.0156 0.039 Uiso 1 1 calc R U . C32 C 0.6615(2) 1.1666(2) -0.09091(14) 0.0307(5) Uani 1 1 d . . . H32A H 0.7175 1.1884 -0.0550 0.037 Uiso 1 1 calc R U . C33 C 0.8360(2) 1.1969(2) -0.19025(14) 0.0279(5) Uani 1 1 d . . . C34 C 1.0308(3) 1.1849(2) -0.27562(17) 0.0356(6) Uani 1 1 d . . . H34A H 1.0669 1.1378 -0.3191 0.043 Uiso 1 1 calc R U . H34B H 1.0901 1.1575 -0.2324 0.043 Uiso 1 1 calc R U . C36 C -0.0907(2) 1.4738(2) 0.27775(15) 0.0331(5) Uani 1 1 d . . . H36A H -0.1411 1.4287 0.2506 0.040 Uiso 1 1 calc R U . C37 C -0.1008(3) 1.6039(2) 0.25865(15) 0.0338(5) Uani 1 1 d . . . H37A H -0.1576 1.6444 0.2196 0.041 Uiso 1 1 calc R U . C38 C -0.0266(2) 1.6737(2) 0.29756(14) 0.0298(5) Uani 1 1 d . . . C39 C 0.0508(3) 1.6085(3) 0.35694(17) 0.0385(6) Uani 1 1 d . . . H39A H 0.1004 1.6518 0.3859 0.046 Uiso 1 1 calc R U . C40 C 0.0550(3) 1.4789(2) 0.37361(16) 0.0354(5) Uani 1 1 d . . . H40A H 0.1067 1.4376 0.4147 0.043 Uiso 1 1 calc R U . 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 0.01899(19) 0.01746(19) 0.0229(2) -0.00019(14) -0.00067(15) -0.00606(14) O1 0.0242(7) 0.0208(7) 0.0328(8) -0.0012(6) 0.0029(6) -0.0095(6) N1 0.0239(9) 0.0244(9) 0.0261(9) -0.0025(7) -0.0029(7) -0.0071(7) C1 0.0215(9) 0.0218(10) 0.0185(9) -0.0036(7) -0.0006(7) -0.0073(8) O1W 0.0359(10) 0.0651(14) 0.0348(10) -0.0028(9) -0.0055(8) -0.0237(9) Co2 0.01510(14) 0.02363(16) 0.02956(17) -0.00129(11) -0.00008(11) -0.00652(11) O2 0.0203(7) 0.0234(8) 0.0411(9) -0.0005(7) -0.0047(7) -0.0032(6) N2 0.0265(10) 0.0349(11) 0.0286(10) -0.0106(8) -0.0050(8) -0.0024(8) C2 0.0166(9) 0.0208(10) 0.0195(10) -0.0023(7) 0.0000(7) -0.0051(7) O2W 0.0262(8) 0.0279(9) 0.0453(10) -0.0028(7) 0.0034(7) -0.0044(7) O3W 0.342(10) 0.181(6) 0.171(6) -0.003(5) -0.011(6) 0.113(6) N3 0.0274(10) 0.0319(10) 0.0301(10) -0.0030(8) 0.0019(8) -0.0104(8) O3 0.0171(7) 0.0299(9) 0.0445(10) -0.0009(7) 0.0010(7) -0.0099(6) C3 0.0166(9) 0.0237(10) 0.0246(10) -0.0033(8) -0.0001(8) -0.0075(8) O4W 0.0563(15) 0.0661(17) 0.106(2) 0.0136(15) 0.0080(15) -0.0205(13) C4 0.0132(9) 0.0258(10) 0.0219(10) -0.0034(8) -0.0006(7) -0.0038(8) O4 0.0359(10) 0.0246(9) 0.0933(17) 0.0062(10) 0.0065(10) -0.0111(8) N4 0.0322(11) 0.0432(13) 0.0359(12) -0.0146(9) 0.0074(9) -0.0148(9) O5 0.0195(7) 0.0265(8) 0.0429(10) -0.0020(7) -0.0032(7) -0.0016(6) N5 0.0353(11) 0.0262(10) 0.0363(11) -0.0103(8) 0.0096(9) -0.0083(8) C5 0.0166(9) 0.0299(11) 0.0252(11) -0.0016(8) -0.0006(8) -0.0035(8) O6 0.0170(7) 0.0325(9) 0.0474(10) -0.0014(7) -0.0046(7) -0.0080(6) C6 0.0195(10) 0.0212(10) 0.0247(10) -0.0003(8) 0.0019(8) -0.0038(8) O7 0.0309(9) 0.0414(10) 0.0378(10) -0.0176(8) 0.0023(7) -0.0070(8) C7 0.0165(9) 0.0209(10) 0.0233(10) -0.0034(8) 0.0029(7) -0.0074(7) O8 0.0512(13) 0.0715(16) 0.0872(18) -0.0527(14) 0.0286(12) -0.0350(12) C8 0.0206(10) 0.0227(10) 0.0307(11) -0.0019(8) 0.0031(8) -0.0081(8) O9 0.0321(9) 0.0443(11) 0.0396(10) -0.0167(8) 0.0042(7) -0.0123(8) C9 0.0148(9) 0.0215(10) 0.0222(10) -0.0033(8) 0.0005(7) -0.0041(7) N9 0.0232(9) 0.0273(10) 0.0340(11) -0.0018(8) 0.0016(8) -0.0061(8) C10 0.0299(12) 0.0364(13) 0.0299(12) 0.0001(10) -0.0007(9) -0.0156(10) C11 0.0338(12) 0.0399(14) 0.0300(12) -0.0039(10) -0.0031(10) -0.0210(11) C12 0.0316(12) 0.0427(14) 0.0267(12) -0.0020(10) 0.0003(9) -0.0171(11) C13 0.0343(13) 0.0413(14) 0.0333(13) -0.0034(10) -0.0052(10) -0.0203(11) C14 0.0241(10) 0.0261(11) 0.0268(11) -0.0040(9) -0.0043(8) -0.0029(8) C15 0.0258(11) 0.0467(15) 0.0265(12) -0.0093(10) -0.0026(9) -0.0064(10) C16 0.0296(11) 0.0286(11) 0.0224(11) -0.0041(9) 0.0002(8) -0.0081(9) C17 0.0275(11) 0.0268(11) 0.0258(11) -0.0070(9) -0.0013(9) -0.0063(9) C18 0.0327(12) 0.0430(14) 0.0209(11) -0.0065(10) -0.0023(9) -0.0076(10) C19 0.0314(12) 0.0451(15) 0.0251(12) -0.0105(10) 0.0023(9) -0.0072(11) C20 0.0255(11) 0.0470(15) 0.0352(13) -0.0078(11) 0.0048(10) -0.0126(11) C21 0.0263(11) 0.0373(13) 0.0307(12) 0.0001(10) -0.0022(9) -0.0103(10) C22 0.0229(11) 0.0374(13) 0.0357(13) -0.0026(10) 0.0048(9) -0.0060(9) C23 0.0268(12) 0.0452(15) 0.0359(13) -0.0101(11) 0.0006(10) -0.0127(10) C24 0.0295(11) 0.0267(11) 0.0323(12) -0.0062(9) 0.0032(9) -0.0071(9) C25 0.0305(13) 0.0555(17) 0.0353(14) -0.0147(12) 0.0053(10) -0.0154(12) C26 0.0345(13) 0.0424(15) 0.0364(14) -0.0123(11) 0.0063(10) -0.0134(11) C27 0.0316(12) 0.0294(12) 0.0353(13) -0.0096(10) 0.0049(10) -0.0084(10) C28 0.0348(13) 0.0441(15) 0.0336(13) -0.0180(11) 0.0020(10) -0.0114(11) C29 0.0343(13) 0.0399(14) 0.0287(12) -0.0115(10) 0.0052(10) -0.0083(11) C30 0.0278(11) 0.0252(11) 0.0294(12) -0.0071(9) 0.0045(9) -0.0038(9) C31 0.0345(13) 0.0358(13) 0.0282(12) -0.0060(10) 0.0035(10) -0.0083(10) C32 0.0317(12) 0.0336(13) 0.0283(12) -0.0070(9) -0.0008(9) -0.0078(10) C33 0.0292(11) 0.0228(11) 0.0312(12) -0.0037(9) 0.0017(9) -0.0032(9) C34 0.0324(13) 0.0256(12) 0.0471(15) -0.0056(10) 0.0134(11) -0.0018(10) C36 0.0312(12) 0.0336(13) 0.0359(13) -0.0004(10) -0.0029(10) -0.0099(10) C37 0.0321(12) 0.0303(13) 0.0371(13) 0.0025(10) -0.0009(10) -0.0030(10) C38 0.0258(11) 0.0257(11) 0.0368(13) -0.0049(9) 0.0110(9) -0.0028(9) C39 0.0403(14) 0.0323(13) 0.0458(15) -0.0077(11) -0.0069(12) -0.0106(11) C40 0.0312(12) 0.0330(13) 0.0418(14) 0.0000(11) -0.0071(10) -0.0052(10) 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' 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' Cl Cl 0.1484 0.1585 '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' 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 O1 Co1 O1 180.0 . 2_466 O1 Co1 O2W 90.78(6) . 2_466 O1 Co1 O2W 89.22(6) 2_466 2_466 O1 Co1 O2W 89.22(6) . . O1 Co1 O2W 90.78(6) 2_466 . O2W Co1 O2W 180.0 2_466 . O1 Co1 N1 92.09(7) . . O1 Co1 N1 87.92(7) 2_466 . O2W Co1 N1 86.76(7) 2_466 . O2W Co1 N1 93.23(7) . . O1 Co1 N1 87.91(7) . 2_466 O1 Co1 N1 92.09(7) 2_466 2_466 O2W Co1 N1 93.23(7) 2_466 2_466 O2W Co1 N1 86.77(7) . 2_466 N1 Co1 N1 180.0 . 2_466 C1 O1 Co1 135.64(14) . . C10 N1 C11 116.2(2) . . C10 N1 Co1 119.00(16) . . C11 N1 Co1 124.62(15) . . O2 C1 O1 124.9(2) . . O2 C1 C2 119.61(18) . . O1 C1 C2 115.50(18) . . O3 Co2 O1W 89.74(7) . . O3 Co2 N9 116.55(7) . . O1W Co2 N9 89.93(8) . . O3 Co2 N3 93.39(7) . . O1W Co2 N3 174.84(8) . . N9 Co2 N3 92.33(8) . . O3 Co2 O5 151.38(7) . 1_655 O1W Co2 O5 83.43(7) . 1_655 N9 Co2 O5 91.29(7) . 1_655 N3 Co2 O5 91.88(7) . 1_655 O3 Co2 O6 93.96(6) . 1_655 O1W Co2 O6 89.14(7) . 1_655 N9 Co2 O6 149.48(7) . 1_655 N3 Co2 O6 86.55(7) . 1_655 O5 Co2 O6 58.30(6) 1_655 1_655 C16 N2 C15 122.3(2) . . C9 C2 C3 119.18(19) . . C9 C2 C1 122.46(18) . . C3 C2 C1 118.35(18) . . C20 N3 C21 116.5(2) . . C20 N3 Co2 123.24(16) . . C21 N3 Co2 120.17(16) . . C8 O3 Co2 121.71(15) . . C4 C3 C2 120.94(19) . . C3 C4 C6 119.34(19) . . C3 C4 C5 119.65(18) . . C6 C4 C5 121.01(19) . . C26 N4 C25 122.1(2) . . C5 O5 Co2 93.69(13) . 1_455 C33 N5 C34 119.9(2) . . O5 C5 O6 120.2(2) . . O5 C5 C4 119.52(19) . . O6 C5 C4 120.3(2) . . C5 O6 Co2 87.64(13) . 1_455 C4 C6 C7 120.39(19) . . C9 C7 C6 119.44(18) . . C9 C7 C8 121.08(18) . . C6 C7 C8 119.47(19) . . O4 C8 O3 124.2(2) . . O4 C8 C7 118.4(2) . . O3 C8 C7 117.33(19) . . C2 C9 C7 120.67(18) . . C36 N9 C40 116.6(2) . . C36 N9 Co2 125.74(17) . . C40 N9 Co2 116.76(16) . . N1 C10 C13 123.8(2) . . N1 C11 C12 123.7(2) . . C11 C12 C14 119.9(2) . . C14 C13 C10 119.8(2) . . C13 C14 C12 116.6(2) . . C13 C14 C15 123.2(2) . . C12 C14 C15 120.1(2) . . N2 C15 C14 112.46(19) . . O7 C16 N2 123.9(2) . . O7 C16 C17 120.3(2) . . N2 C16 C17 115.8(2) . . C19 C17 C18 119.5(2) 2_567 . C19 C17 C16 118.8(2) 2_567 . C18 C17 C16 121.7(2) . . C19 C18 C17 119.9(2) . . C18 C19 C17 120.6(2) . 2_567 N3 C20 C23 123.2(2) . . N3 C21 C22 123.6(2) . . C21 C22 C24 119.6(2) . . C20 C23 C24 120.0(2) . . C22 C24 C23 117.0(2) . . C22 C24 C25 123.2(2) . . C23 C24 C25 119.7(2) . . N4 C25 C24 113.2(2) . . O8 C26 N4 122.5(2) . . O8 C26 C27 122.3(2) . . N4 C26 C27 115.2(2) . . C28 C27 C31 119.5(2) . . C28 C27 C26 119.2(2) . . C31 C27 C26 121.3(2) . . C29 C28 C27 120.1(2) . . C28 C29 C30 120.6(2) . . C32 C30 C29 118.9(2) . . C32 C30 C33 117.5(2) . . C29 C30 C33 123.6(2) . . C32 C31 C27 120.1(2) . . C31 C32 C30 120.8(2) . . O9 C33 N5 121.2(2) . . O9 C33 C30 120.0(2) . . N5 C33 C30 118.8(2) . . N5 C34 C38 112.5(2) . 2_685 N9 C36 C37 123.0(2) . . C38 C37 C36 120.1(2) . . C39 C38 C37 116.7(2) . . C39 C38 C34 121.9(2) . 2_685 C37 C38 C34 121.4(2) . 2_685 C38 C39 C40 120.2(2) . . N9 C40 C39 123.3(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 O1 2.0420(15) . Co1 O1 2.0420(15) 2_466 Co1 O2W 2.1495(16) 2_466 Co1 O2W 2.1495(16) . Co1 N1 2.1919(19) . Co1 N1 2.1919(19) 2_466 O1 C1 1.265(2) . N1 C10 1.334(3) . N1 C11 1.337(3) . C1 O2 1.259(3) . C1 C2 1.510(3) . O1W Co2 2.0870(19) . Co2 O3 2.0352(15) . Co2 N9 2.158(2) . Co2 N3 2.160(2) . Co2 O5 2.1770(16) 1_655 Co2 O6 2.3057(17) 1_655 N2 C16 1.333(3) . N2 C15 1.457(3) . C2 C9 1.393(3) . C2 C3 1.394(3) . N3 C20 1.341(3) . N3 C21 1.342(3) . O3 C8 1.263(3) . C3 C4 1.391(3) . C4 C6 1.394(3) . C4 C5 1.501(3) . O4 C8 1.242(3) . N4 C26 1.341(3) . N4 C25 1.451(3) . O5 C5 1.258(3) . O5 Co2 2.1770(16) 1_455 N5 C33 1.335(3) . N5 C34 1.464(3) . C5 O6 1.264(3) . O6 Co2 2.3057(17) 1_455 C6 C7 1.398(3) . O7 C16 1.233(3) . C7 C9 1.393(3) . C7 C8 1.515(3) . O8 C26 1.212(3) . O9 C33 1.238(3) . N9 C36 1.339(3) . N9 C40 1.339(3) . C10 C13 1.382(3) . C11 C12 1.378(3) . C12 C14 1.388(3) . C13 C14 1.381(3) . C14 C15 1.505(3) . C16 C17 1.496(3) . C17 C19 1.385(3) 2_567 C17 C18 1.393(3) . C18 C19 1.381(3) . C19 C17 1.385(3) 2_567 C20 C23 1.376(4) . C21 C22 1.378(3) . C22 C24 1.384(3) . C23 C24 1.387(3) . C24 C25 1.506(3) . C26 C27 1.500(3) . C27 C28 1.393(3) . C27 C31 1.397(3) . C28 C29 1.382(4) . C29 C30 1.396(3) . C30 C32 1.395(3) . C30 C33 1.493(3) . C31 C32 1.378(3) . C34 C38 1.515(3) 2_685 C36 C37 1.384(3) . C37 C38 1.383(4) . C38 C39 1.377(4) . C38 C34 1.515(3) 2_685 C39 C40 1.379(4) .