# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email sunwy@nju.edu.cn _publ_author_name 'Wei-Yin Sun' data_1 _database_code_depnum_ccdc_archive 'CCDC 893711' #TrackingRef 'CE-ART-09-2012-026533.cif' _audit_creation_date 2012-10-08 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _chemical_name_systematic ; [Co(L)(PIN)]-dioxane-H2O ; _chemical_name_common (Co(L)(PIN))-dioxane-H2O _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Co N4 O8' _chemical_formula_sum 'C28 H26 Co N4 O8' _chemical_formula_weight 605.46 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.512(5) _cell_length_b 9.9435(19) _cell_length_c 26.994(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.945(11) _cell_angle_gamma 90.00 _cell_volume 5386.5(19) _cell_formula_units_Z 8 _cell_measurement_temperature 200 _cell_measurement_reflns_used 18404 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9211 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; [Co(L)(PIN)]-dioxane-H2O ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 22979 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6168 _reflns_number_gt 5265 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+13.2259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6168 _refine_ls_number_parameters 570 _refine_ls_number_restraints 297 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.858933(13) 0.95292(3) 0.322870(10) 0.01410(9) Uani 1 1 d . . . O1 O 0.44636(8) 0.58228(16) 0.33040(7) 0.0274(4) Uani 1 1 d . . . O2 O 0.34999(8) 0.68255(16) 0.32354(7) 0.0295(4) Uani 1 1 d . . . O3 O 0.43096(8) 1.30175(15) 0.32680(6) 0.0263(4) Uani 1 1 d . . . O4 O 0.33802(9) 1.18598(19) 0.31581(8) 0.0383(5) Uani 1 1 d . . . O5 O 0.53431(12) 0.3062(2) 0.41060(9) 0.0507(6) Uani 1 1 d . . . H25 H 0.5016(19) 0.311(4) 0.3865(15) 0.061 Uiso 1 1 d . . . H26 H 0.5329(19) 0.245(4) 0.4284(14) 0.061 Uiso 1 1 d . . . O6 O 0.7171(3) 0.2783(7) 0.4502(2) 0.120(2) Uani 0.724(9) 1 d PDU . . O6B O 0.7689(12) 0.252(2) 0.4560(8) 0.129(5) Uani 0.276(9) 1 d PDU . . O7 O 0.5733(12) 1.081(3) 0.4798(8) 0.119(5) Uani 0.196(8) 1 d PDU . . O7B O 0.5387(7) 1.0997(15) 0.4820(6) 0.104(4) Uani 0.390(9) 1 d PDU . . O7C O 0.5130(7) 1.0979(14) 0.4708(5) 0.108(4) Uani 0.413(9) 1 d PDU . . O20 O 0.79152(16) 0.8446(3) 0.56798(9) 0.0970(13) Uani 1 1 d . . . N11 N 0.75247(8) 0.95726(18) 0.31690(7) 0.0182(4) Uani 1 1 d . . . N20 N 0.87888(16) 0.9731(3) 0.55970(13) 0.0246(10) Uani 0.667(8) 1 d P . . H8 H 0.9133 1.0174 0.5770 0.030 Uiso 0.667(8) 1 calc PR . . N20B N 0.8737(3) 0.9931(7) 0.5933(3) 0.030(2) Uani 0.333(8) 1 d P . . H8B H 0.9033 1.0461 0.5840 0.036 Uiso 0.333(8) 1 calc PR . . N21 N 0.84886(9) 1.03959(19) 0.74218(7) 0.0199(4) Uani 1 1 d U . . N31 N 0.86879(10) 0.9398(2) 0.40368(7) 0.0234(4) Uani 1 1 d U . . C1 C 0.54371(10) 0.9506(2) 0.32046(8) 0.0179(4) Uani 1 1 d . . . C2 C 0.51226(10) 0.8274(2) 0.32361(8) 0.0190(4) Uani 1 1 d . . . H1 H 0.5370 0.7464 0.3245 0.023 Uiso 1 1 calc R . . C3 C 0.44497(10) 0.8222(2) 0.32551(8) 0.0181(4) Uani 1 1 d . . . C4 C 0.40872(10) 0.9398(2) 0.32442(8) 0.0188(4) Uani 1 1 d . . . H2 H 0.3628 0.9358 0.3255 0.023 Uiso 1 1 calc R . . C5 C 0.43901(10) 1.0642(2) 0.32178(8) 0.0181(4) Uani 1 1 d . . . C6 C 0.50638(10) 1.0688(2) 0.31944(8) 0.0183(4) Uani 1 1 d . . . H3 H 0.5272 1.1533 0.3171 0.022 Uiso 1 1 calc R . . C12 C 0.71283(10) 0.8550(2) 0.29721(8) 0.0193(4) Uani 1 1 d . . . H4 H 0.7320 0.7822 0.2824 0.023 Uiso 1 1 calc R . . C13 C 0.64562(10) 0.8500(2) 0.29734(8) 0.0195(4) Uani 1 1 d . . . H5 H 0.6198 0.7749 0.2830 0.023 Uiso 1 1 calc R . . C14 C 0.61559(10) 0.9550(2) 0.31851(8) 0.0183(4) Uani 1 1 d . . . C15 C 0.65633(11) 1.0630(2) 0.33789(10) 0.0267(5) Uani 1 1 d . . . H6 H 0.6381 1.1381 0.3521 0.032 Uiso 1 1 calc R . . C16 C 0.72334(11) 1.0606(2) 0.33637(10) 0.0267(5) Uani 1 1 d . . . H7 H 0.7501 1.1354 0.3497 0.032 Uiso 1 1 calc R . . C20 C 0.8328(2) 0.9275(5) 0.58550(19) 0.0340(12) Uani 0.667(8) 1 d P . . C20B C 0.8410(5) 0.9066(10) 0.5593(4) 0.043(3) Uani 0.333(8) 1 d P . . C22 C 0.7900(4) 0.9981(14) 0.7110(3) 0.0180(14) Uani 0.667(8) 1 d PDU . . H9 H 0.7515 0.9887 0.7252 0.022 Uiso 0.667(8) 1 calc PR . . C23 C 0.7844(3) 0.9696(9) 0.6600(3) 0.0254(12) Uani 0.667(8) 1 d PDU . . H10 H 0.7425 0.9457 0.6396 0.030 Uiso 0.667(8) 1 calc PR . . C24 C 0.8401(4) 0.9760(6) 0.6392(2) 0.0231(12) Uani 0.667(8) 1 d PDU . . C25 C 0.8992(3) 1.0134(6) 0.6697(3) 0.0259(13) Uani 0.667(8) 1 d PDU . . H11 H 0.9388 1.0180 0.6567 0.031 Uiso 0.667(8) 1 calc PR . . C26 C 0.9003(4) 1.0446(10) 0.7203(3) 0.0253(17) Uani 0.667(8) 1 d PDU . . H12 H 0.9418 1.0716 0.7406 0.030 Uiso 0.667(8) 1 calc PR . . C22B C 0.8032(9) 1.005(3) 0.7079(7) 0.029(3) Uani 0.333(8) 1 d PDU . . H9B H 0.7609 0.9938 0.7165 0.034 Uiso 0.333(8) 1 calc PR . . C23B C 0.8061(6) 0.9799(18) 0.6582(5) 0.025(3) Uani 0.333(8) 1 d PDU . . H10B H 0.7685 0.9457 0.6351 0.031 Uiso 0.333(8) 1 calc PR . . C24B C 0.8640(6) 1.0055(12) 0.6431(4) 0.016(2) Uani 0.333(8) 1 d PDU . . C25B C 0.9159(6) 1.0541(12) 0.6784(4) 0.018(2) Uani 0.333(8) 1 d PDU . . H11B H 0.9565 1.0767 0.6687 0.022 Uiso 0.333(8) 1 calc PR . . C26B C 0.9102(8) 1.071(2) 0.7283(5) 0.018(3) Uani 0.333(8) 1 d PDU . . H12B H 0.9468 1.1034 0.7528 0.021 Uiso 0.333(8) 1 calc PR . . C31 C 0.41162(11) 0.6876(2) 0.32676(8) 0.0204(4) Uani 1 1 d . . . C32 C 0.8335(7) 0.8662(15) 0.4263(3) 0.0292(19) Uani 0.667(8) 1 d PDU . . H13 H 0.8045 0.8040 0.4060 0.035 Uiso 0.667(8) 1 calc PR . . C33 C 0.8332(4) 0.8673(8) 0.4775(3) 0.0275(13) Uani 0.667(8) 1 d PDU . . H14 H 0.8045 0.8096 0.4912 0.033 Uiso 0.667(8) 1 calc PR . . C34 C 0.8759(3) 0.9553(6) 0.5081(2) 0.0208(11) Uani 0.667(8) 1 d PDU . . C35 C 0.9184(3) 1.0316(8) 0.4856(2) 0.0281(12) Uani 0.667(8) 1 d PDU . . H15 H 0.9501 1.0895 0.5057 0.034 Uiso 0.667(8) 1 calc PR . . C36 C 0.9147(5) 1.0235(12) 0.4342(3) 0.0250(14) Uani 0.667(8) 1 d PDU . . H16 H 0.9441 1.0761 0.4192 0.030 Uiso 0.667(8) 1 calc PR . . C32B C 0.8238(15) 0.844(3) 0.4197(6) 0.024(3) Uani 0.333(8) 1 d PDU . . H13B H 0.7964 0.7885 0.3950 0.028 Uiso 0.333(8) 1 calc PR . . C33B C 0.8199(10) 0.8307(17) 0.4702(6) 0.035(3) Uani 0.333(8) 1 d PDU . . H14B H 0.7924 0.7635 0.4802 0.042 Uiso 0.333(8) 1 calc PR . . C34B C 0.8560(6) 0.9152(13) 0.5052(4) 0.024(2) Uani 0.333(8) 1 d PDU . . C35B C 0.8974(7) 1.0063(15) 0.4903(5) 0.034(3) Uani 0.333(8) 1 d PDU . . H15B H 0.9229 1.0672 0.5137 0.040 Uiso 0.333(8) 1 calc PR . . C36B C 0.9011(12) 1.007(3) 0.4391(6) 0.033(3) Uani 0.333(8) 1 d PDU . . H16B H 0.9329 1.0667 0.4303 0.039 Uiso 0.333(8) 1 calc PR . . C51 C 0.39900(11) 1.1909(2) 0.32108(8) 0.0219(5) Uani 1 1 d . . . C61 C 0.6987(6) 0.1537(14) 0.4751(5) 0.140(4) Uani 0.724(9) 1 d PDU . . H17 H 0.7262 0.0770 0.4681 0.168 Uiso 0.724(9) 1 calc PR . . H18 H 0.6512 0.1315 0.4619 0.168 Uiso 0.724(9) 1 calc PR . . C61B C 0.7070(15) 0.195(5) 0.4687(14) 0.131(6) Uani 0.276(9) 1 d PDU . . H17B H 0.6834 0.1330 0.4423 0.158 Uiso 0.276(9) 1 calc PR . . H18B H 0.6760 0.2656 0.4758 0.158 Uiso 0.276(9) 1 calc PR . . C62 C 0.7110(5) 0.1812(15) 0.5322(5) 0.150(4) Uani 0.724(9) 1 d PDU . . H19 H 0.6814 0.2541 0.5392 0.180 Uiso 0.724(9) 1 calc PR . . H20 H 0.7016 0.0993 0.5504 0.180 Uiso 0.724(9) 1 calc PR . . C62B C 0.7420(16) 0.122(2) 0.5164(10) 0.137(6) Uani 0.276(9) 1 d PDU . . H19B H 0.7177 0.0425 0.5253 0.165 Uiso 0.276(9) 1 calc PR . . H20B H 0.7894 0.1009 0.5174 0.165 Uiso 0.276(9) 1 calc PR . . C71 C 0.5039(15) 1.003(4) 0.4555(12) 0.113(5) Uani 0.196(8) 1 d PDU . . H21 H 0.4780 1.0782 0.4368 0.136 Uiso 0.196(8) 1 calc PR . . H22 H 0.5185 0.9499 0.4288 0.136 Uiso 0.196(8) 1 calc PR . . C71B C 0.5297(12) 0.9427(14) 0.4643(6) 0.103(4) Uani 0.390(9) 1 d PDU . . H21B H 0.4848 0.9231 0.4438 0.124 Uiso 0.390(9) 1 calc PR . . H22B H 0.5645 0.9121 0.4464 0.124 Uiso 0.390(9) 1 calc PR . . C71C C 0.5595(8) 0.9618(15) 0.4782(8) 0.116(5) Uani 0.413(9) 1 d PDU . . H21C H 0.5848 0.9485 0.4511 0.139 Uiso 0.413(9) 1 calc PR . . H22C H 0.5894 0.9552 0.5120 0.139 Uiso 0.413(9) 1 calc PR . . C72 C 0.4479(14) 0.916(2) 0.4656(7) 0.076(5) Uani 0.196(8) 1 d PDU . . H23 H 0.4596 0.8214 0.4593 0.091 Uiso 0.196(8) 1 calc PR . . H24 H 0.4077 0.9382 0.4398 0.091 Uiso 0.196(8) 1 calc PR . . C72B C 0.5395(7) 0.8881(16) 0.5175(5) 0.100(4) Uani 0.390(9) 1 d PDU . . H23B H 0.5679 0.9463 0.5430 0.121 Uiso 0.390(9) 1 calc PR . . H24B H 0.5561 0.7943 0.5206 0.121 Uiso 0.390(9) 1 calc PR . . C72C C 0.4982(9) 0.8745(14) 0.4725(5) 0.098(3) Uani 0.413(9) 1 d PDU . . H23C H 0.5074 0.7788 0.4664 0.117 Uiso 0.413(9) 1 calc PR . . H24C H 0.4609 0.9076 0.4460 0.117 Uiso 0.413(9) 1 calc PR . . 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 0.01117(14) 0.01433(14) 0.01747(15) -0.00038(11) 0.00455(10) -0.00067(11) O1 0.0233(8) 0.0158(7) 0.0442(10) -0.0020(7) 0.0101(7) -0.0030(6) O2 0.0194(8) 0.0203(8) 0.0510(11) -0.0013(7) 0.0123(8) -0.0050(6) O3 0.0289(9) 0.0145(7) 0.0333(9) -0.0022(6) 0.0016(7) 0.0054(6) O4 0.0179(8) 0.0360(10) 0.0610(13) -0.0009(9) 0.0082(8) 0.0110(8) O5 0.0538(14) 0.0446(13) 0.0429(13) 0.0026(10) -0.0148(10) -0.0199(11) O6 0.103(4) 0.137(5) 0.108(4) -0.006(4) -0.011(3) 0.053(4) O6B 0.113(7) 0.141(8) 0.123(7) 0.001(7) 0.000(6) 0.044(7) O7 0.128(8) 0.105(6) 0.120(7) 0.029(6) 0.020(6) -0.019(7) O7B 0.113(8) 0.090(5) 0.110(6) 0.030(4) 0.031(6) -0.025(6) O7C 0.114(7) 0.088(5) 0.116(6) 0.048(4) 0.011(6) -0.031(5) O20 0.130(3) 0.135(3) 0.0382(13) -0.0404(15) 0.0462(15) -0.108(2) N11 0.0133(8) 0.0194(9) 0.0231(9) -0.0014(7) 0.0066(7) -0.0004(7) N20 0.0278(17) 0.0298(18) 0.018(2) -0.0035(12) 0.0089(12) -0.0064(14) N20B 0.034(4) 0.040(4) 0.020(4) -0.003(3) 0.012(3) -0.009(3) N21 0.0193(9) 0.0228(9) 0.0192(9) 0.0002(7) 0.0074(7) 0.0010(8) N31 0.0237(10) 0.0286(10) 0.0177(9) -0.0023(8) 0.0037(7) 0.0006(8) C1 0.0132(9) 0.0168(9) 0.0245(10) -0.0012(8) 0.0060(8) -0.0010(8) C2 0.0150(10) 0.0145(9) 0.0284(11) -0.0006(8) 0.0065(8) 0.0014(8) C3 0.0147(10) 0.0151(10) 0.0249(11) -0.0022(8) 0.0053(8) -0.0028(8) C4 0.0111(9) 0.0199(10) 0.0258(11) -0.0022(8) 0.0042(8) -0.0019(8) C5 0.0145(10) 0.0174(10) 0.0217(10) -0.0031(8) 0.0025(8) 0.0014(8) C6 0.0167(10) 0.0136(9) 0.0250(11) -0.0013(8) 0.0049(8) -0.0012(8) C12 0.0161(10) 0.0181(10) 0.0243(11) -0.0018(8) 0.0060(8) 0.0013(8) C13 0.0145(10) 0.0177(10) 0.0264(11) -0.0017(8) 0.0044(8) -0.0003(8) C14 0.0132(9) 0.0170(9) 0.0253(11) 0.0020(8) 0.0056(8) 0.0004(8) C15 0.0195(11) 0.0194(11) 0.0445(14) -0.0087(10) 0.0142(10) -0.0009(9) C16 0.0187(11) 0.0213(11) 0.0425(14) -0.0082(10) 0.0115(10) -0.0049(9) C20 0.039(3) 0.042(2) 0.023(2) -0.0073(18) 0.0134(18) -0.017(2) C20B 0.062(7) 0.044(5) 0.028(5) -0.004(4) 0.023(5) -0.019(5) C22 0.014(3) 0.026(3) 0.016(2) -0.0025(19) 0.0058(17) -0.007(3) C23 0.021(3) 0.036(3) 0.020(2) -0.0046(16) 0.006(2) -0.013(3) C24 0.021(3) 0.027(3) 0.023(2) -0.0016(17) 0.007(2) -0.006(2) C25 0.024(3) 0.028(3) 0.030(3) -0.002(2) 0.015(3) -0.005(2) C26 0.015(3) 0.032(4) 0.026(3) -0.001(2) 0.000(2) -0.005(2) C22B 0.020(6) 0.032(6) 0.040(5) 0.002(4) 0.021(4) -0.009(6) C23B 0.013(5) 0.039(5) 0.022(4) -0.003(3) 0.001(4) -0.015(5) C24B 0.009(5) 0.026(5) 0.012(4) -0.004(3) 0.000(4) -0.003(4) C25B 0.014(5) 0.027(6) 0.014(4) 0.005(4) 0.006(3) -0.002(4) C26B 0.011(5) 0.033(7) 0.011(4) -0.003(4) 0.008(4) -0.006(4) C31 0.0201(11) 0.0188(10) 0.0241(11) -0.0031(8) 0.0087(9) -0.0059(9) C32 0.032(4) 0.031(5) 0.023(3) -0.008(2) 0.001(3) -0.011(3) C33 0.037(4) 0.027(4) 0.021(3) -0.006(2) 0.010(3) -0.015(2) C34 0.020(3) 0.024(3) 0.019(2) -0.006(2) 0.003(2) -0.005(2) C35 0.020(3) 0.042(3) 0.022(2) -0.007(2) 0.004(2) -0.010(2) C36 0.022(4) 0.033(4) 0.019(2) -0.004(2) 0.0040(19) -0.012(2) C32B 0.030(8) 0.033(9) 0.009(4) -0.006(4) 0.008(5) -0.019(4) C33B 0.048(8) 0.035(8) 0.021(5) -0.016(4) 0.009(5) -0.026(5) C34B 0.027(6) 0.028(6) 0.017(4) -0.011(4) 0.002(4) -0.019(4) C35B 0.027(8) 0.047(7) 0.026(5) -0.015(5) 0.001(5) -0.023(5) C36B 0.027(9) 0.037(7) 0.039(6) 0.000(5) 0.017(4) -0.017(5) C51 0.0216(11) 0.0217(11) 0.0220(11) -0.0014(8) 0.0038(9) 0.0077(9) C61 0.134(6) 0.139(8) 0.124(6) 0.012(6) -0.024(5) 0.019(6) C61B 0.132(8) 0.128(10) 0.120(8) 0.007(8) -0.006(7) -0.001(8) C62 0.144(8) 0.134(7) 0.164(8) -0.011(6) 0.013(6) 0.043(6) C62B 0.142(9) 0.127(9) 0.139(9) -0.016(7) 0.021(7) 0.044(7) C71 0.123(8) 0.107(8) 0.109(8) -0.005(6) 0.024(6) -0.010(6) C71B 0.114(8) 0.101(7) 0.099(7) -0.010(6) 0.032(6) -0.011(6) C71C 0.131(8) 0.100(7) 0.116(7) 0.001(6) 0.024(6) -0.010(6) C72 0.100(8) 0.069(7) 0.060(7) -0.005(6) 0.021(6) -0.008(7) C72B 0.111(7) 0.094(6) 0.102(6) 0.026(6) 0.033(6) 0.022(6) C72C 0.124(7) 0.078(5) 0.093(6) 0.003(5) 0.026(5) -0.016(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.0949(16) 3_545 ? Co1 N21 2.1462(18) 6_575 ? Co1 N31 2.1525(19) . ? Co1 N11 2.1566(18) . ? Co1 O1 2.1820(16) 3 ? Co1 O2 2.2911(17) 3 ? O1 C31 1.259(3) . ? O1 Co1 2.1820(16) 3_445 ? O2 C31 1.250(3) . ? O2 Co1 2.2911(17) 3_445 ? O3 C51 1.275(3) . ? O3 Co1 2.0949(16) 3_455 ? O4 C51 1.230(3) . ? O5 H25 0.83(4) . ? O5 H26 0.78(4) . ? O6 C61 1.495(9) . ? O6 C62 1.506(9) 7_656 ? O6B C62B 1.494(11) 7_656 ? O6B C61B 1.495(11) . ? O7 C72 1.620(11) 5_676 ? O7 C71 1.635(11) . ? O7B C72B 1.613(10) 5_676 ? O7B C71B 1.632(10) . ? O7C C72C 1.619(10) 5_676 ? O7C C71C 1.644(10) . ? O20 C20 1.206(5) . ? O20 C20B 1.250(10) . ? N11 C12 1.341(3) . ? N11 C16 1.348(3) . ? N20 C20 1.363(6) . ? N20 C34 1.393(6) . ? N20 H8 0.8800 . ? N20B C20B 1.334(14) . ? N20B C24B 1.402(12) . ? N20B H8B 0.8800 . ? N21 C22B 1.223(19) . ? N21 C26 1.312(9) . ? N21 C22 1.385(7) . ? N21 C26B 1.420(15) . ? N21 Co1 2.1462(18) 6_576 ? N31 C36B 1.239(19) . ? N31 C32 1.270(10) . ? N31 C36 1.391(8) . ? N31 C32B 1.456(17) . ? C1 C2 1.395(3) . ? C1 C6 1.399(3) . ? C1 C14 1.487(3) . ? C2 C3 1.393(3) . ? C2 H1 0.9500 . ? C3 C4 1.383(3) . ? C3 C31 1.507(3) . ? C4 C5 1.393(3) . ? C4 H2 0.9500 . ? C5 C6 1.397(3) . ? C5 C51 1.502(3) . ? C6 H3 0.9500 . ? C12 C13 1.380(3) . ? C12 H4 0.9500 . ? C13 C14 1.393(3) . ? C13 H5 0.9500 . ? C14 C15 1.395(3) . ? C15 C16 1.384(3) . ? C15 H6 0.9500 . ? C16 H7 0.9500 . ? C20 C24 1.506(8) . ? C20B C34B 1.554(16) . ? C22 C23 1.387(7) . ? C22 H9 0.9500 . ? C23 C24 1.375(6) . ? C23 H10 0.9500 . ? C24 C25 1.369(7) . ? C25 C26 1.396(8) . ? C25 H11 0.9500 . ? C26 H12 0.9500 . ? C22B C23B 1.378(14) . ? C22B H9B 0.9500 . ? C23B C24B 1.358(11) . ? C23B H10B 0.9500 . ? C24B C25B 1.361(10) . ? C25B C26B 1.386(12) . ? C25B H11B 0.9500 . ? C26B H12B 0.9500 . ? C32 C33 1.384(8) . ? C32 H13 0.9500 . ? C33 C34 1.385(7) . ? C33 H14 0.9500 . ? C34 C35 1.387(7) . ? C35 C36 1.377(7) . ? C35 H15 0.9500 . ? C36 H16 0.9500 . ? C32B C33B 1.387(13) . ? C32B H13B 0.9500 . ? C33B C34B 1.363(10) . ? C33B H14B 0.9500 . ? C34B C35B 1.359(12) . ? C35B C36B 1.400(14) . ? C35B H15B 0.9500 . ? C36B H16B 0.9500 . ? C61 C62 1.535(15) . ? C61 H17 0.9900 . ? C61 H18 0.9900 . ? C61B C62B 1.52(2) . ? C61B H17B 0.9900 . ? C61B H18B 0.9900 . ? C62 O6 1.506(9) 7_656 ? C62 H19 0.9900 . ? C62 H20 0.9900 . ? C62B O6B 1.494(11) 7_656 ? C62B H19B 0.9900 . ? C62B H20B 0.9900 . ? C71 C72 1.512(15) . ? C71 H21 0.9900 . ? C71 H22 0.9900 . ? C71B C72B 1.510(14) . ? C71B H21B 0.9900 . ? C71B H22B 0.9900 . ? C71C C72C 1.510(14) . ? C71C H21C 0.9900 . ? C71C H22C 0.9900 . ? C72 O7 1.620(11) 5_676 ? C72 H23 0.9900 . ? C72 H24 0.9900 . ? C72B O7B 1.613(10) 5_676 ? C72B H23B 0.9900 . ? C72B H24B 0.9900 . ? C72C O7C 1.619(10) 5_676 ? C72C H23C 0.9900 . ? C72C H24C 0.9900 . ? 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 _geom_angle_publ_flag O3 Co1 N21 89.71(7) 3_545 6_575 ? O3 Co1 N31 89.31(7) 3_545 . ? N21 Co1 N31 178.51(7) 6_575 . ? O3 Co1 N11 135.30(7) 3_545 . ? N21 Co1 N11 92.31(7) 6_575 . ? N31 Co1 N11 87.60(7) . . ? O3 Co1 O1 82.00(7) 3_545 3 ? N21 Co1 O1 88.78(7) 6_575 3 ? N31 Co1 O1 92.20(7) . 3 ? N11 Co1 O1 142.67(7) . 3 ? O3 Co1 O2 140.49(6) 3_545 3 ? N21 Co1 O2 88.99(7) 6_575 3 ? N31 Co1 O2 92.48(7) . 3 ? N11 Co1 O2 84.21(6) . 3 ? O1 Co1 O2 58.49(6) 3 3 ? C31 O1 Co1 92.42(13) . 3_445 ? C31 O2 Co1 87.67(13) . 3_445 ? C51 O3 Co1 105.92(14) . 3_455 ? H25 O5 H26 113(4) . . ? C61 O6 C62 113.7(8) . 7_656 ? C62B O6B C61B 89(3) 7_656 . ? C72 O7 C71 89.9(18) 5_676 . ? C72B O7B C71B 91.2(14) 5_676 . ? C72C O7C C71C 102.5(12) 5_676 . ? C20 O20 C20B 37.4(5) . . ? C12 N11 C16 116.81(18) . . ? C12 N11 Co1 122.39(14) . . ? C16 N11 Co1 120.64(14) . . ? C20 N20 C34 125.3(5) . . ? C20 N20 H8 117.4 . . ? C34 N20 H8 117.4 . . ? C20B N20B C24B 124.5(9) . . ? C20B N20B H8B 117.8 . . ? C24B N20B H8B 117.8 . . ? C22B N21 C26 103.4(8) . . ? C22B N21 C22 11.6(9) . . ? C26 N21 C22 114.8(4) . . ? C22B N21 C26B 116.3(9) . . ? C26 N21 C26B 15.0(7) . . ? C22 N21 C26B 127.9(6) . . ? C22B N21 Co1 132.5(8) . 6_576 ? C26 N21 Co1 122.5(4) . 6_576 ? C22 N21 Co1 121.0(3) . 6_576 ? C26B N21 Co1 110.9(5) . 6_576 ? C36B N31 C32 101.8(7) . . ? C36B N31 C36 14.9(7) . . ? C32 N31 C36 116.3(5) . . ? C36B N31 C32B 113.2(8) . . ? C32 N31 C32B 11.4(8) . . ? C36 N31 C32B 127.6(7) . . ? C36B N31 Co1 132.3(7) . . ? C32 N31 Co1 125.3(4) . . ? C36 N31 Co1 118.2(3) . . ? C32B N31 Co1 114.1(6) . . ? C2 C1 C6 118.70(19) . . ? C2 C1 C14 120.13(19) . . ? C6 C1 C14 121.17(18) . . ? C3 C2 C1 120.61(19) . . ? C3 C2 H1 119.7 . . ? C1 C2 H1 119.7 . . ? C4 C3 C2 120.02(19) . . ? C4 C3 C31 120.47(19) . . ? C2 C3 C31 119.47(19) . . ? C3 C4 C5 120.57(19) . . ? C3 C4 H2 119.7 . . ? C5 C4 H2 119.7 . . ? C4 C5 C6 119.15(19) . . ? C4 C5 C51 119.82(19) . . ? C6 C5 C51 121.03(19) . . ? C5 C6 C1 120.95(19) . . ? C5 C6 H3 119.5 . . ? C1 C6 H3 119.5 . . ? N11 C12 C13 123.37(19) . . ? N11 C12 H4 118.3 . . ? C13 C12 H4 118.3 . . ? C12 C13 C14 120.0(2) . . ? C12 C13 H5 120.0 . . ? C14 C13 H5 120.0 . . ? C13 C14 C15 116.71(19) . . ? C13 C14 C1 121.24(19) . . ? C15 C14 C1 122.05(19) . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H6 120.1 . . ? C14 C15 H6 120.1 . . ? N11 C16 C15 123.2(2) . . ? N11 C16 H7 118.4 . . ? C15 C16 H7 118.4 . . ? O20 C20 N20 122.1(5) . . ? O20 C20 C24 121.3(4) . . ? N20 C20 C24 116.3(4) . . ? O20 C20B N20B 120.0(10) . . ? O20 C20B C34B 121.9(9) . . ? N20B C20B C34B 116.3(9) . . ? N21 C22 C23 123.1(5) . . ? N21 C22 H9 118.5 . . ? C23 C22 H9 118.5 . . ? C24 C23 C22 119.4(5) . . ? C24 C23 H10 120.3 . . ? C22 C23 H10 120.3 . . ? C25 C24 C23 118.3(5) . . ? C25 C24 C20 124.5(5) . . ? C23 C24 C20 116.9(5) . . ? C24 C25 C26 118.8(6) . . ? C24 C25 H11 120.6 . . ? C26 C25 H11 120.6 . . ? N21 C26 C25 125.4(6) . . ? N21 C26 H12 117.3 . . ? C25 C26 H12 117.3 . . ? N21 C22B C23B 127.4(13) . . ? N21 C22B H9B 116.3 . . ? C23B C22B H9B 116.3 . . ? C24B C23B C22B 118.4(11) . . ? C24B C23B H10B 120.8 . . ? C22B C23B H10B 120.8 . . ? C23B C24B C25B 117.5(9) . . ? C23B C24B N20B 125.2(10) . . ? C25B C24B N20B 117.2(10) . . ? C24B C25B C26B 120.9(10) . . ? C24B C25B H11B 119.6 . . ? C26B C25B H11B 119.6 . . ? C25B C26B N21 119.2(10) . . ? C25B C26B H12B 120.4 . . ? N21 C26B H12B 120.4 . . ? O2 C31 O1 121.3(2) . . ? O2 C31 C3 119.5(2) . . ? O1 C31 C3 119.24(19) . . ? N31 C32 C33 126.6(6) . . ? N31 C32 H13 116.7 . . ? C33 C32 H13 116.7 . . ? C32 C33 C34 117.8(6) . . ? C32 C33 H14 121.1 . . ? C34 C33 H14 121.1 . . ? C33 C34 C35 117.5(5) . . ? C33 C34 N20 124.6(6) . . ? C35 C34 N20 117.8(6) . . ? C36 C35 C34 120.0(5) . . ? C36 C35 H15 120.0 . . ? C34 C35 H15 120.0 . . ? C35 C36 N31 121.4(5) . . ? C35 C36 H16 119.3 . . ? N31 C36 H16 119.3 . . ? C33B C32B N31 121.4(12) . . ? C33B C32B H13B 119.3 . . ? N31 C32B H13B 119.3 . . ? C34B C33B C32B 119.5(12) . . ? C34B C33B H14B 120.2 . . ? C32B C33B H14B 120.2 . . ? C35B C34B C33B 119.2(10) . . ? C35B C34B C20B 124.9(10) . . ? C33B C34B C20B 115.7(11) . . ? C34B C35B C36B 117.3(11) . . ? C34B C35B H15B 121.3 . . ? C36B C35B H15B 121.3 . . ? N31 C36B C35B 129.2(12) . . ? N31 C36B H16B 115.4 . . ? C35B C36B H16B 115.4 . . ? O4 C51 O3 122.3(2) . . ? O4 C51 C5 120.5(2) . . ? O3 C51 C5 117.22(19) . . ? O6 C61 C62 107.4(10) . . ? O6 C61 H17 110.2 . . ? C62 C61 H17 110.2 . . ? O6 C61 H18 110.2 . . ? C62 C61 H18 110.2 . . ? H17 C61 H18 108.5 . . ? O6B C61B C62B 96(2) . . ? O6B C61B H17B 112.6 . . ? C62B C61B H17B 112.6 . . ? O6B C61B H18B 112.6 . . ? C62B C61B H18B 112.6 . . ? H17B C61B H18B 110.1 . . ? O6 C62 C61 108.2(10) 7_656 . ? O6 C62 H19 110.0 7_656 . ? C61 C62 H19 110.0 . . ? O6 C62 H20 110.0 7_656 . ? C61 C62 H20 110.0 . . ? H19 C62 H20 108.4 . . ? O6B C62B C61B 86(2) 7_656 . ? O6B C62B H19B 114.3 7_656 . ? C61B C62B H19B 114.3 . . ? O6B C62B H20B 114.3 7_656 . ? C61B C62B H20B 114.3 . . ? H19B C62B H20B 111.5 . . ? C72 C71 O7 146(3) . . ? C72 C71 H21 100.2 . . ? O7 C71 H21 100.2 . . ? C72 C71 H22 100.2 . . ? O7 C71 H22 100.2 . . ? H21 C71 H22 104.2 . . ? C72B C71B O7B 94.7(13) . . ? C72B C71B H21B 112.8 . . ? O7B C71B H21B 112.8 . . ? C72B C71B H22B 112.8 . . ? O7B C71B H22B 112.8 . . ? H21B C71B H22B 110.2 . . ? C72C C71C O7C 90.6(11) . . ? C72C C71C H21C 113.5 . . ? O7C C71C H21C 113.5 . . ? C72C C71C H22C 113.5 . . ? O7C C71C H22C 113.5 . . ? H21C C71C H22C 110.8 . . ? C71 C72 O7 121(2) . 5_676 ? C71 C72 H23 107.1 . . ? O7 C72 H23 107.1 5_676 . ? C71 C72 H24 107.1 . . ? O7 C72 H24 107.1 5_676 . ? H23 C72 H24 106.8 . . ? C71B C72B O7B 92.5(13) . 5_676 ? C71B C72B H23B 113.2 . . ? O7B C72B H23B 113.2 5_676 . ? C71B C72B H24B 113.2 . . ? O7B C72B H24B 113.2 5_676 . ? H23B C72B H24B 110.6 . . ? C71C C72C O7C 94.8(12) . 5_676 ? C71C C72C H23C 112.8 . . ? O7C C72C H23C 112.8 5_676 . ? C71C C72C H24C 112.8 . . ? O7C C72C H24C 112.8 5_676 . ? H23C C72C H24C 110.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co1 N11 C12 -24.3(2) 3_545 . . . ? N21 Co1 N11 C12 67.67(17) 6_575 . . . ? N31 Co1 N11 C12 -110.84(17) . . . . ? O1 Co1 N11 C12 158.68(15) 3 . . . ? O2 Co1 N11 C12 156.42(17) 3 . . . ? O3 Co1 N11 C16 151.01(17) 3_545 . . . ? N21 Co1 N11 C16 -117.06(18) 6_575 . . . ? N31 Co1 N11 C16 64.42(18) . . . . ? O1 Co1 N11 C16 -26.1(2) 3 . . . ? O2 Co1 N11 C16 -28.31(18) 3 . . . ? O3 Co1 N31 C36B 97(2) 3_545 . . . ? N21 Co1 N31 C36B 146(3) 6_575 . . . ? N11 Co1 N31 C36B -127(2) . . . . ? O1 Co1 N31 C36B 15(2) 3 . . . ? O2 Co1 N31 C36B -43(2) 3 . . . ? O3 Co1 N31 C32 -92.5(10) 3_545 . . . ? N21 Co1 N31 C32 -44(3) 6_575 . . . ? N11 Co1 N31 C32 42.9(10) . . . . ? O1 Co1 N31 C32 -174.4(10) 3 . . . ? O2 Co1 N31 C32 127.0(10) 3 . . . ? O3 Co1 N31 C36 91.4(7) 3_545 . . . ? N21 Co1 N31 C36 140(3) 6_575 . . . ? N11 Co1 N31 C36 -133.3(7) . . . . ? O1 Co1 N31 C36 9.4(7) 3 . . . ? O2 Co1 N31 C36 -49.2(7) 3 . . . ? O3 Co1 N31 C32B -90.2(17) 3_545 . . . ? N21 Co1 N31 C32B -41(3) 6_575 . . . ? N11 Co1 N31 C32B 45.2(17) . . . . ? O1 Co1 N31 C32B -172.1(17) 3 . . . ? O2 Co1 N31 C32B 129.3(17) 3 . . . ? C6 C1 C2 C3 0.2(3) . . . . ? C14 C1 C2 C3 179.9(2) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C1 C2 C3 C31 177.5(2) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C31 C3 C4 C5 -178.1(2) . . . . ? C3 C4 C5 C6 1.0(3) . . . . ? C3 C4 C5 C51 -179.5(2) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C51 C5 C6 C1 179.54(19) . . . . ? C2 C1 C6 C5 0.3(3) . . . . ? C14 C1 C6 C5 -179.4(2) . . . . ? C16 N11 C12 C13 -1.7(3) . . . . ? Co1 N11 C12 C13 173.69(16) . . . . ? N11 C12 C13 C14 0.2(3) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C12 C13 C14 C1 -178.3(2) . . . . ? C2 C1 C14 C13 29.5(3) . . . . ? C6 C1 C14 C13 -150.9(2) . . . . ? C2 C1 C14 C15 -150.1(2) . . . . ? C6 C1 C14 C15 29.5(3) . . . . ? C13 C14 C15 C16 -1.3(3) . . . . ? C1 C14 C15 C16 178.3(2) . . . . ? C12 N11 C16 C15 1.7(4) . . . . ? Co1 N11 C16 C15 -173.80(19) . . . . ? C14 C15 C16 N11 -0.2(4) . . . . ? C20B O20 C20 N20 3.7(8) . . . . ? C20B O20 C20 C24 -170.4(11) . . . . ? C34 N20 C20 O20 14.9(7) . . . . ? C34 N20 C20 C24 -170.8(4) . . . . ? C20 O20 C20B N20B 1.6(6) . . . . ? C20 O20 C20B C34B -162.6(16) . . . . ? C24B N20B C20B O20 11.3(15) . . . . ? C24B N20B C20B C34B 176.3(9) . . . . ? C22B N21 C22 C23 6(10) . . . . ? C26 N21 C22 C23 -2.8(16) . . . . ? C26B N21 C22 C23 6(2) . . . . ? Co1 N21 C22 C23 -168.6(9) 6_576 . . . ? N21 C22 C23 C24 3.2(17) . . . . ? C22 C23 C24 C25 -1.3(13) . . . . ? C22 C23 C24 C20 172.6(9) . . . . ? O20 C20 C24 C25 146.9(6) . . . . ? N20 C20 C24 C25 -27.4(8) . . . . ? O20 C20 C24 C23 -26.5(9) . . . . ? N20 C20 C24 C23 159.1(6) . . . . ? C23 C24 C25 C26 -0.7(10) . . . . ? C20 C24 C25 C26 -174.0(7) . . . . ? C22B N21 C26 C25 -1(2) . . . . ? C22 N21 C26 C25 0.7(14) . . . . ? C26B N21 C26 C25 -152(6) . . . . ? Co1 N21 C26 C25 166.3(7) 6_576 . . . ? C24 C25 C26 N21 1.0(13) . . . . ? C26 N21 C22B C23B -1(4) . . . . ? C22 N21 C22B C23B -173(14) . . . . ? C26B N21 C22B C23B 7(4) . . . . ? Co1 N21 C22B C23B -166.6(19) 6_576 . . . ? N21 C22B C23B C24B -6(4) . . . . ? C22B C23B C24B C25B 0(3) . . . . ? C22B C23B C24B N20B -176.0(19) . . . . ? C20B N20B C24B C23B -29.5(18) . . . . ? C20B N20B C24B C25B 154.3(10) . . . . ? C23B C24B C25B C26B 3(2) . . . . ? N20B C24B C25B C26B 179.2(14) . . . . ? C24B C25B C26B N21 -1(2) . . . . ? C22B N21 C26B C25B -3(3) . . . . ? C26 N21 C26B C25B 28(4) . . . . ? C22 N21 C26B C25B -3(2) . . . . ? Co1 N21 C26B C25B 171.5(13) 6_576 . . . ? Co1 O2 C31 O1 -3.4(2) 3_445 . . . ? Co1 O2 C31 C3 175.75(18) 3_445 . . . ? Co1 O1 C31 O2 3.5(2) 3_445 . . . ? Co1 O1 C31 C3 -175.59(17) 3_445 . . . ? C4 C3 C31 O2 4.5(3) . . . . ? C2 C3 C31 O2 -173.1(2) . . . . ? C4 C3 C31 O1 -176.3(2) . . . . ? C2 C3 C31 O1 6.0(3) . . . . ? C36B N31 C32 C33 1(2) . . . . ? C36 N31 C32 C33 5(2) . . . . ? C32B N31 C32 C33 178(13) . . . . ? Co1 N31 C32 C33 -171.7(11) . . . . ? N31 C32 C33 C34 -1(2) . . . . ? C32 C33 C34 C35 -3.0(13) . . . . ? C32 C33 C34 N20 176.5(10) . . . . ? C20 N20 C34 C33 -13.2(8) . . . . ? C20 N20 C34 C35 166.4(5) . . . . ? C33 C34 C35 C36 3.4(12) . . . . ? N20 C34 C35 C36 -176.2(8) . . . . ? C34 C35 C36 N31 0.1(16) . . . . ? C36B N31 C36 C35 10(7) . . . . ? C32 N31 C36 C35 -4.0(17) . . . . ? C32B N31 C36 C35 -6(2) . . . . ? Co1 N31 C36 C35 172.6(8) . . . . ? C36B N31 C32B C33B -1(4) . . . . ? C32 N31 C32B C33B -4(9) . . . . ? C36 N31 C32B C33B 4(4) . . . . ? Co1 N31 C32B C33B -175(2) . . . . ? N31 C32B C33B C34B 4(4) . . . . ? C32B C33B C34B C35B -3(3) . . . . ? C32B C33B C34B C20B 172(2) . . . . ? O20 C20B C34B C35B 162.4(12) . . . . ? N20B C20B C34B C35B -2.3(18) . . . . ? O20 C20B C34B C33B -12.3(18) . . . . ? N20B C20B C34B C33B -177.0(13) . . . . ? C33B C34B C35B C36B -1(3) . . . . ? C20B C34B C35B C36B -175.1(18) . . . . ? C32 N31 C36B C35B -3(3) . . . . ? C36 N31 C36B C35B -170(11) . . . . ? C32B N31 C36B C35B -4(4) . . . . ? Co1 N31 C36B C35B 168.9(18) . . . . ? C34B C35B C36B N31 4(4) . . . . ? Co1 O3 C51 O4 -1.5(3) 3_455 . . . ? Co1 O3 C51 C5 179.38(15) 3_455 . . . ? C4 C5 C51 O4 -10.1(3) . . . . ? C6 C5 C51 O4 169.5(2) . . . . ? C4 C5 C51 O3 169.1(2) . . . . ? C6 C5 C51 O3 -11.4(3) . . . . ? C62 O6 C61 C62 60.2(14) 7_656 . . . ? C62B O6B C61B C62B -94(3) 7_656 . . . ? O6 C61 C62 O6 -56.8(14) . . . 7_656 ? O6B C61B C62B O6B 91(3) . . . 7_656 ? C72 O7 C71 C72 -23(7) 5_676 . . . ? C72B O7B C71B C72B -87.4(14) 5_676 . . . ? C72C O7C C71C C72C 84.9(13) 5_676 . . . ? O7 C71 C72 O7 27(8) . . . 5_676 ? O7B C71B C72B O7B 88.6(15) . . . 5_676 ? O7C C71C C72C O7C -77.4(12) . . . 5_676 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.610 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.110 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 893712' #TrackingRef 'CE-ART-09-2012-026533.cif' _audit_creation_date 2011-05-01 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Co(L)(DPE)]-1/2(DPE) ; _chemical_name_common (Co(L)(DPE))-1/2(DPE) _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 Co N4 O4' _chemical_formula_sum 'C31 H22 Co N4 O4' _chemical_formula_weight 573.46 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.570(4) _cell_length_b 9.901(2) _cell_length_c 27.211(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.526(9) _cell_angle_gamma 90.00 _cell_volume 5255(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200 _cell_measurement_reflns_used 18579 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.57 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type none _exptl_special_details ; [Co(L)(DPE)]-1/2(DPE) ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 21649 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5956 _reflns_number_gt 5042 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+5.1330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5956 _refine_ls_number_parameters 397 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.136103(13) 0.55592(3) 0.174277(10) 0.01758(10) Uani 1 1 d . . . O1 O 0.54672(8) 0.18749(15) 0.16198(7) 0.0303(4) Uani 1 1 d . . . O2 O 0.64398(8) 0.28787(18) 0.16952(7) 0.0382(4) Uani 1 1 d . . . O3 O 0.55904(9) 0.90961(15) 0.16669(7) 0.0304(4) Uani 1 1 d . . . O4 O 0.65603(9) 0.79903(19) 0.18086(7) 0.0393(4) Uani 1 1 d . . . N11 N 0.24673(9) 0.56251(17) 0.18840(7) 0.0230(4) Uani 1 1 d . . . N21 N 0.14946(9) 0.56574(17) 0.25629(7) 0.0211(4) Uani 1 1 d . . . N31 N 0.12319(10) 0.46750(19) 0.59299(7) 0.0276(4) Uani 1 1 d . . . N41 N 0.4476(7) 0.6486(9) 0.5055(3) 0.127(4) Uani 0.50 1 d P . . N41B N 0.3779(11) 0.5571(16) 0.4985(6) 0.175(6) Uani 0.50 1 d P . . C1 C 0.45285(10) 0.55480(19) 0.17935(8) 0.0217(4) Uani 1 1 d . . . C2 C 0.48375(11) 0.4316(2) 0.17466(9) 0.0227(4) Uani 1 1 d . . . H1 H 0.4598 0.3496 0.1748 0.027 Uiso 1 1 calc R . . C3 C 0.54935(10) 0.4275(2) 0.16979(8) 0.0215(4) Uani 1 1 d . . . C4 C 0.58520(10) 0.5471(2) 0.17027(8) 0.0220(4) Uani 1 1 d . . . H2 H 0.6303 0.5442 0.1680 0.026 Uiso 1 1 calc R . . C5 C 0.55505(10) 0.6711(2) 0.17406(8) 0.0218(4) Uani 1 1 d . . . C6 C 0.48921(10) 0.6742(2) 0.17883(8) 0.0226(4) Uani 1 1 d . . . H3 H 0.4689 0.7586 0.1818 0.027 Uiso 1 1 calc R . . C12 C 0.28748(11) 0.4546(2) 0.20378(9) 0.0245(4) Uani 1 1 d . . . H4 H 0.2698 0.3785 0.2166 0.029 Uiso 1 1 calc R . . C13 C 0.35429(11) 0.4480(2) 0.20196(9) 0.0244(4) Uani 1 1 d . . . H5 H 0.3806 0.3682 0.2128 0.029 Uiso 1 1 calc R . . C14 C 0.38266(11) 0.5588(2) 0.18414(9) 0.0223(4) Uani 1 1 d . . . C15 C 0.34104(12) 0.6726(2) 0.17031(10) 0.0332(5) Uani 1 1 d . . . H6 H 0.3580 0.7518 0.1589 0.040 Uiso 1 1 calc R . . C16 C 0.27482(11) 0.6709(2) 0.17312(10) 0.0319(5) Uani 1 1 d . . . H7 H 0.2479 0.7504 0.1638 0.038 Uiso 1 1 calc R . . C20 C 0.15691(13) 0.5587(3) 0.41579(9) 0.0342(5) Uani 1 1 d . . . H8 H 0.1976 0.5902 0.4410 0.041 Uiso 1 1 calc R . . C22 C 0.20794(11) 0.5883(2) 0.29484(9) 0.0278(5) Uani 1 1 d . . . H9 H 0.2485 0.6047 0.2862 0.033 Uiso 1 1 calc R . . C23 C 0.21202(12) 0.5890(3) 0.34678(9) 0.0335(5) Uani 1 1 d . . . H10 H 0.2547 0.6054 0.3727 0.040 Uiso 1 1 calc R . . C24 C 0.15338(12) 0.5655(2) 0.36092(8) 0.0265(5) Uani 1 1 d . . . C25 C 0.09198(12) 0.5470(2) 0.32068(9) 0.0305(5) Uani 1 1 d . . . H11 H 0.0502 0.5347 0.3280 0.037 Uiso 1 1 calc R . . C26 C 0.09257(11) 0.5470(2) 0.27011(9) 0.0300(5) Uani 1 1 d . . . H12 H 0.0503 0.5329 0.2434 0.036 Uiso 1 1 calc R . . C30 C 0.10677(14) 0.5111(3) 0.43261(9) 0.0366(5) Uani 1 1 d . . . H13 H 0.0654 0.4824 0.4074 0.044 Uiso 1 1 calc R . . C31 C 0.58180(11) 0.2933(2) 0.16645(8) 0.0239(4) Uani 1 1 d . . . C32 C 0.07850(13) 0.3950(3) 0.55580(9) 0.0347(5) Uani 1 1 d . . . H14 H 0.0506 0.3310 0.5657 0.042 Uiso 1 1 calc R . . C33 C 0.07090(14) 0.4086(3) 0.50335(10) 0.0385(6) Uani 1 1 d . . . H15 H 0.0381 0.3556 0.4784 0.046 Uiso 1 1 calc R . . C34 C 0.11175(13) 0.5006(3) 0.48772(9) 0.0340(5) Uani 1 1 d . . . C35 C 0.15697(16) 0.5783(3) 0.52636(10) 0.0424(6) Uani 1 1 d . . . H16 H 0.1849 0.6443 0.5175 0.051 Uiso 1 1 calc R . . C36 C 0.16105(15) 0.5593(3) 0.57750(10) 0.0389(6) Uani 1 1 d . . . H17 H 0.1922 0.6136 0.6031 0.047 Uiso 1 1 calc R . . C40 C 0.2901(4) 0.3303(8) 0.4907(3) 0.1255(19) Uani 0.50 1 d PU . . H18 H 0.2757 0.2957 0.4563 0.151 Uiso 0.50 1 calc PR . . C42 C 0.4176(7) 0.6275(13) 0.5418(5) 0.116(3) Uani 0.50 1 d PU . . H19 H 0.4345 0.6791 0.5726 0.139 Uiso 0.50 1 calc PR . . C43 C 0.3601(4) 0.5317(8) 0.5393(2) 0.127(2) Uani 0.50 1 d PU . . H20 H 0.3353 0.5326 0.5633 0.153 Uiso 0.50 1 calc PR . . C44 C 0.3465(7) 0.4391(15) 0.4970(4) 0.106(3) Uani 0.50 1 d PU . . C45 C 0.3675(4) 0.4614(8) 0.4588(2) 0.1208(19) Uani 0.50 1 d PU . . H21 H 0.3492 0.4120 0.4276 0.145 Uiso 0.50 1 calc PR . . C46 C 0.4230(7) 0.5695(12) 0.4635(4) 0.115(3) Uani 0.50 1 d PU . . H22 H 0.4407 0.5807 0.4354 0.138 Uiso 0.50 1 calc PR . . C40B C 0.2443(8) 0.2290(15) 0.4815(4) 0.110(3) Uani 0.50 1 d PU . . H18B H 0.2343 0.1919 0.4478 0.132 Uiso 0.50 1 calc PR . . C42B C 0.3601(4) 0.5317(8) 0.5393(2) 0.127(2) Uani 0.50 1 d PU . . H19B H 0.3802 0.5791 0.5708 0.153 Uiso 0.50 1 calc PR . . C43B C 0.3088(7) 0.4293(13) 0.5352(4) 0.111(3) Uani 0.50 1 d PU . . H20B H 0.2865 0.4241 0.5608 0.133 Uiso 0.50 1 calc PR . . C44B C 0.2901(4) 0.3303(8) 0.4907(3) 0.1255(19) Uani 0.50 1 d PU . . C45B C 0.3172(8) 0.3606(15) 0.4533(5) 0.126(3) Uani 0.50 1 d PU . . H21B H 0.3019 0.3119 0.4216 0.151 Uiso 0.50 1 calc PR . . C46B C 0.3675(4) 0.4614(8) 0.4588(2) 0.1208(19) Uani 0.50 1 d PU . . H22B H 0.3940 0.4644 0.4359 0.145 Uiso 0.50 1 calc PR . . C51 C 0.59319(11) 0.8011(2) 0.17392(8) 0.0258(4) Uani 1 1 d . . . 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 0.01573(15) 0.01723(15) 0.02340(16) -0.00070(10) 0.01135(11) -0.00060(10) O1 0.0347(9) 0.0185(7) 0.0426(9) 0.0007(6) 0.0194(7) 0.0038(7) O2 0.0247(8) 0.0307(9) 0.0645(12) -0.0029(8) 0.0220(8) 0.0077(7) O3 0.0372(9) 0.0176(7) 0.0419(9) -0.0018(6) 0.0204(8) -0.0059(7) O4 0.0224(8) 0.0427(10) 0.0539(11) 0.0073(8) 0.0135(7) -0.0120(8) N11 0.0201(8) 0.0207(8) 0.0331(9) -0.0019(7) 0.0151(7) -0.0008(7) N21 0.0182(8) 0.0236(8) 0.0248(9) 0.0002(7) 0.0112(7) 0.0000(7) N31 0.0295(10) 0.0309(9) 0.0267(9) 0.0031(8) 0.0147(8) 0.0038(8) N41 0.211(12) 0.084(6) 0.052(4) -0.006(4) -0.005(6) 0.057(7) N41B 0.27(2) 0.146(13) 0.107(10) 0.048(9) 0.055(12) 0.063(12) C1 0.0176(9) 0.0190(9) 0.0324(11) 0.0008(8) 0.0133(8) 0.0008(8) C2 0.0202(10) 0.0175(9) 0.0330(11) 0.0004(8) 0.0124(8) -0.0027(8) C3 0.0186(9) 0.0195(9) 0.0289(10) 0.0003(8) 0.0111(8) 0.0038(8) C4 0.0142(9) 0.0240(10) 0.0305(11) 0.0009(8) 0.0110(8) 0.0007(8) C5 0.0181(9) 0.0188(9) 0.0302(10) 0.0012(8) 0.0102(8) -0.0011(8) C6 0.0197(9) 0.0157(9) 0.0362(11) -0.0001(8) 0.0141(8) -0.0002(8) C12 0.0211(10) 0.0228(10) 0.0334(11) 0.0029(8) 0.0141(8) -0.0013(8) C13 0.0202(10) 0.0195(10) 0.0368(12) 0.0032(8) 0.0135(9) 0.0017(8) C14 0.0185(9) 0.0194(9) 0.0335(11) -0.0022(8) 0.0146(8) -0.0011(8) C15 0.0263(11) 0.0194(10) 0.0632(16) 0.0076(10) 0.0275(11) 0.0015(9) C16 0.0236(11) 0.0206(10) 0.0585(15) 0.0054(10) 0.0229(10) 0.0030(9) C20 0.0346(12) 0.0456(14) 0.0233(11) 0.0006(10) 0.0105(9) 0.0015(11) C22 0.0196(10) 0.0370(12) 0.0290(11) -0.0017(9) 0.0109(8) -0.0024(9) C23 0.0240(11) 0.0492(14) 0.0273(11) -0.0037(10) 0.0081(9) -0.0057(11) C24 0.0271(11) 0.0310(11) 0.0230(10) 0.0010(8) 0.0101(9) 0.0020(9) C25 0.0250(11) 0.0431(13) 0.0281(11) 0.0033(9) 0.0153(9) 0.0002(10) C26 0.0191(10) 0.0490(14) 0.0239(10) 0.0001(9) 0.0094(8) -0.0011(10) C30 0.0389(13) 0.0472(14) 0.0266(11) 0.0025(11) 0.0147(10) 0.0013(12) C31 0.0251(10) 0.0232(10) 0.0258(10) 0.0004(8) 0.0117(8) 0.0060(9) C32 0.0319(12) 0.0458(14) 0.0296(12) 0.0044(10) 0.0144(10) -0.0019(11) C33 0.0350(13) 0.0544(16) 0.0277(12) 0.0000(11) 0.0120(10) -0.0066(12) C34 0.0375(13) 0.0423(13) 0.0274(11) 0.0064(10) 0.0176(10) 0.0082(11) C35 0.0604(18) 0.0409(14) 0.0329(13) 0.0022(11) 0.0246(13) -0.0123(13) C36 0.0539(16) 0.0370(13) 0.0308(12) -0.0019(10) 0.0206(12) -0.0097(12) C40 0.124(4) 0.137(4) 0.105(4) 0.028(3) 0.021(3) 0.072(3) C42 0.133(7) 0.109(6) 0.086(6) 0.005(5) 0.006(6) 0.055(5) C43 0.160(5) 0.149(4) 0.074(3) 0.019(3) 0.039(3) 0.047(3) C44 0.126(6) 0.112(6) 0.072(5) 0.013(4) 0.020(5) 0.074(4) C45 0.142(4) 0.143(5) 0.075(3) 0.011(3) 0.029(3) 0.065(3) C46 0.148(7) 0.125(7) 0.066(5) -0.012(5) 0.026(5) 0.050(5) C40B 0.154(7) 0.125(6) 0.057(4) 0.006(4) 0.041(5) 0.088(4) C42B 0.160(5) 0.149(4) 0.074(3) 0.019(3) 0.039(3) 0.047(3) C43B 0.129(7) 0.140(7) 0.067(5) 0.027(4) 0.035(5) 0.061(5) C44B 0.124(4) 0.137(4) 0.105(4) 0.028(3) 0.021(3) 0.072(3) C45B 0.140(7) 0.146(7) 0.089(6) 0.003(6) 0.034(5) 0.071(5) C46B 0.142(4) 0.143(5) 0.075(3) 0.011(3) 0.029(3) 0.065(3) C51 0.0264(10) 0.0252(11) 0.0278(10) -0.0005(8) 0.0116(8) -0.0084(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.1086(16) 3_445 ? Co1 N31 2.155(2) 6_565 ? Co1 N21 2.1625(19) . ? Co1 N11 2.1850(18) . ? Co1 O1 2.1906(16) 3_455 ? Co1 O2 2.3089(19) 3_455 ? O1 C31 1.256(3) . ? O1 Co1 2.1905(16) 3_545 ? O2 C31 1.256(2) . ? O2 Co1 2.3089(18) 3_545 ? O3 C51 1.264(3) . ? O3 Co1 2.1086(16) 3 ? O4 C51 1.246(3) . ? N11 C12 1.341(3) . ? N11 C16 1.346(3) . ? N21 C22 1.340(3) . ? N21 C26 1.351(3) . ? N31 C32 1.339(3) . ? N31 C36 1.348(3) . ? N31 Co1 2.155(2) 6_566 ? N41 C42 1.338(19) . ? N41 C46 1.344(14) . ? C1 C2 1.400(3) . ? C1 C6 1.401(3) . ? C1 C14 1.491(3) . ? C2 C3 1.398(3) . ? C2 H1 0.9500 . ? C3 C4 1.393(3) . ? C3 C31 1.503(3) . ? C4 C5 1.394(3) . ? C4 H2 0.9500 . ? C5 C6 1.401(3) . ? C5 C51 1.508(3) . ? C6 H3 0.9500 . ? C12 C13 1.392(3) . ? C12 H4 0.9500 . ? C13 C14 1.400(3) . ? C13 H5 0.9500 . ? C14 C15 1.393(3) . ? C15 C16 1.388(3) . ? C15 H6 0.9500 . ? C16 H7 0.9500 . ? C20 C30 1.340(4) . ? C20 C24 1.473(3) . ? C20 H8 0.9500 . ? C22 C23 1.389(3) . ? C22 H9 0.9500 . ? C23 C24 1.397(3) . ? C23 H10 0.9500 . ? C24 C25 1.396(3) . ? C25 C26 1.380(3) . ? C25 H11 0.9500 . ? C26 H12 0.9500 . ? C30 C34 1.474(3) . ? C30 H13 0.9500 . ? C32 C33 1.392(3) . ? C32 H14 0.9500 . ? C33 C34 1.394(4) . ? C33 H15 0.9500 . ? C34 C35 1.394(4) . ? C35 C36 1.380(4) . ? C35 H16 0.9500 . ? C36 H17 0.9500 . ? C40 C40B 1.324(18) 7_556 ? C40 C44 1.553(18) . ? C40 H18 0.9500 . ? C42 C43 1.500(16) . ? C42 H19 0.9500 . ? C43 C44 1.428(14) . ? C43 H20 0.9500 . ? C44 C45 1.263(15) . ? C45 C46 1.541(16) . ? C45 H21 0.9500 . ? C46 H22 0.9500 . ? C40B C40 1.325(18) 7_556 ? C40B H18B 0.9500 . ? C43B H20B 0.9500 . ? C45B H21B 0.9500 . ? 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 _geom_angle_publ_flag O3 Co1 N31 88.97(7) 3_445 6_565 ? O3 Co1 N21 88.68(7) 3_445 . ? N31 Co1 N21 176.40(7) 6_565 . ? O3 Co1 N11 138.27(6) 3_445 . ? N31 Co1 N11 88.03(7) 6_565 . ? N21 Co1 N11 91.91(7) . . ? O3 Co1 O1 79.93(6) 3_445 3_455 ? N31 Co1 O1 94.79(7) 6_565 3_455 ? N21 Co1 O1 87.48(6) . 3_455 ? N11 Co1 O1 141.79(6) . 3_455 ? O3 Co1 O2 137.88(6) 3_445 3_455 ? N31 Co1 O2 92.15(7) 6_565 3_455 ? N21 Co1 O2 91.43(6) . 3_455 ? N11 Co1 O2 83.83(6) . 3_455 ? O1 Co1 O2 58.01(6) 3_455 3_455 ? C31 O1 Co1 93.02(13) . 3_545 ? C31 O2 Co1 87.58(13) . 3_545 ? C51 O3 Co1 101.83(13) . 3 ? C12 N11 C16 116.41(18) . . ? C12 N11 Co1 122.96(13) . . ? C16 N11 Co1 119.67(14) . . ? C22 N21 C26 116.54(18) . . ? C22 N21 Co1 127.11(14) . . ? C26 N21 Co1 116.35(14) . . ? C32 N31 C36 116.8(2) . . ? C32 N31 Co1 123.30(15) . 6_566 ? C36 N31 Co1 119.89(17) . 6_566 ? C42 N41 C46 113.5(14) . . ? C2 C1 C6 118.35(18) . . ? C2 C1 C14 120.75(17) . . ? C6 C1 C14 120.90(17) . . ? C3 C2 C1 120.90(18) . . ? C3 C2 H1 119.5 . . ? C1 C2 H1 119.5 . . ? C4 C3 C2 119.92(18) . . ? C4 C3 C31 120.56(18) . . ? C2 C3 C31 119.46(18) . . ? C3 C4 C5 120.18(18) . . ? C3 C4 H2 119.9 . . ? C5 C4 H2 119.9 . . ? C4 C5 C6 119.44(18) . . ? C4 C5 C51 120.50(18) . . ? C6 C5 C51 120.05(18) . . ? C1 C6 C5 121.17(18) . . ? C1 C6 H3 119.4 . . ? C5 C6 H3 119.4 . . ? N11 C12 C13 123.55(19) . . ? N11 C12 H4 118.2 . . ? C13 C12 H4 118.2 . . ? C12 C13 C14 120.03(19) . . ? C12 C13 H5 120.0 . . ? C14 C13 H5 120.0 . . ? C15 C14 C13 116.07(19) . . ? C15 C14 C1 121.81(18) . . ? C13 C14 C1 122.11(18) . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H6 119.8 . . ? C14 C15 H6 119.8 . . ? N11 C16 C15 123.5(2) . . ? N11 C16 H7 118.2 . . ? C15 C16 H7 118.2 . . ? C30 C20 C24 124.5(2) . . ? C30 C20 H8 117.7 . . ? C24 C20 H8 117.7 . . ? N21 C22 C23 123.1(2) . . ? N21 C22 H9 118.4 . . ? C23 C22 H9 118.4 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H10 120.0 . . ? C24 C23 H10 120.0 . . ? C25 C24 C23 116.8(2) . . ? C25 C24 C20 122.0(2) . . ? C23 C24 C20 121.2(2) . . ? C26 C25 C24 119.3(2) . . ? C26 C25 H11 120.3 . . ? C24 C25 H11 120.3 . . ? N21 C26 C25 124.1(2) . . ? N21 C26 H12 118.0 . . ? C25 C26 H12 118.0 . . ? C20 C30 C34 124.1(2) . . ? C20 C30 H13 118.0 . . ? C34 C30 H13 118.0 . . ? O1 C31 O2 120.85(19) . . ? O1 C31 C3 119.41(18) . . ? O2 C31 C3 119.72(19) . . ? N31 C32 C33 123.3(2) . . ? N31 C32 H14 118.3 . . ? C33 C32 H14 118.3 . . ? C32 C33 C34 119.6(2) . . ? C32 C33 H15 120.2 . . ? C34 C33 H15 120.2 . . ? C35 C34 C33 116.9(2) . . ? C35 C34 C30 122.8(2) . . ? C33 C34 C30 120.2(2) . . ? C36 C35 C34 119.8(2) . . ? C36 C35 H16 120.1 . . ? C34 C35 H16 120.1 . . ? N31 C36 C35 123.5(2) . . ? N31 C36 H17 118.3 . . ? C35 C36 H17 118.3 . . ? C40B C40 C44 139.5(11) 7_556 . ? C40B C40 H18 110.3 7_556 . ? C44 C40 H18 110.3 . . ? N41 C42 C43 127.4(11) . . ? N41 C42 H19 116.3 . . ? C43 C42 H19 116.3 . . ? C44 C43 C42 113.1(10) . . ? C44 C43 H20 123.4 . . ? C42 C43 H20 123.4 . . ? C45 C44 C43 121.2(15) . . ? C45 C44 C40 118.0(11) . . ? C43 C44 C40 118.8(11) . . ? C44 C45 C46 119.5(11) . . ? C44 C45 H21 120.3 . . ? C46 C45 H21 120.3 . . ? N41 C46 C45 122.9(12) . . ? N41 C46 H22 118.5 . . ? C45 C46 H22 118.5 . . ? C40 C40B H18B 113.0 7_556 . ? O4 C51 O3 122.44(19) . . ? O4 C51 C5 120.1(2) . . ? O3 C51 C5 117.50(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co1 N11 C12 -11.6(2) 3_445 . . . ? N31 Co1 N11 C12 -97.83(18) 6_565 . . . ? N21 Co1 N11 C12 78.56(18) . . . . ? O1 Co1 N11 C12 166.93(15) 3_455 . . . ? O2 Co1 N11 C12 169.79(18) 3_455 . . . ? O3 Co1 N11 C16 156.77(16) 3_445 . . . ? N31 Co1 N11 C16 70.53(18) 6_565 . . . ? N21 Co1 N11 C16 -113.07(18) . . . . ? O1 Co1 N11 C16 -24.7(2) 3_455 . . . ? O2 Co1 N11 C16 -21.84(17) 3_455 . . . ? O3 Co1 N21 C22 146.56(18) 3_445 . . . ? N11 Co1 N21 C22 8.31(18) . . . . ? O1 Co1 N21 C22 -133.46(18) 3_455 . . . ? O2 Co1 N21 C22 -75.57(18) 3_455 . . . ? O3 Co1 N21 C26 -33.43(16) 3_445 . . . ? N11 Co1 N21 C26 -171.69(16) . . . . ? O1 Co1 N21 C26 46.55(16) 3_455 . . . ? O2 Co1 N21 C26 104.44(16) 3_455 . . . ? C6 C1 C2 C3 0.2(3) . . . . ? C14 C1 C2 C3 179.5(2) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C1 C2 C3 C31 178.2(2) . . . . ? C2 C3 C4 C5 -1.9(3) . . . . ? C31 C3 C4 C5 -179.16(19) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? C3 C4 C5 C51 -179.21(19) . . . . ? C2 C1 C6 C5 -0.4(3) . . . . ? C14 C1 C6 C5 -179.7(2) . . . . ? C4 C5 C6 C1 -0.6(3) . . . . ? C51 C5 C6 C1 -179.66(19) . . . . ? C16 N11 C12 C13 -3.5(3) . . . . ? Co1 N11 C12 C13 165.24(17) . . . . ? N11 C12 C13 C14 1.1(4) . . . . ? C12 C13 C14 C15 1.6(3) . . . . ? C12 C13 C14 C1 -177.4(2) . . . . ? C2 C1 C14 C15 -156.3(2) . . . . ? C6 C1 C14 C15 23.0(3) . . . . ? C2 C1 C14 C13 22.6(3) . . . . ? C6 C1 C14 C13 -158.1(2) . . . . ? C13 C14 C15 C16 -1.8(4) . . . . ? C1 C14 C15 C16 177.2(2) . . . . ? C12 N11 C16 C15 3.3(4) . . . . ? Co1 N11 C16 C15 -165.8(2) . . . . ? C14 C15 C16 N11 -0.7(4) . . . . ? C26 N21 C22 C23 1.9(3) . . . . ? Co1 N21 C22 C23 -178.04(18) . . . . ? N21 C22 C23 C24 -0.1(4) . . . . ? C22 C23 C24 C25 -2.3(4) . . . . ? C22 C23 C24 C20 176.8(2) . . . . ? C30 C20 C24 C25 12.7(4) . . . . ? C30 C20 C24 C23 -166.3(3) . . . . ? C23 C24 C25 C26 2.7(3) . . . . ? C20 C24 C25 C26 -176.4(2) . . . . ? C22 N21 C26 C25 -1.4(3) . . . . ? Co1 N21 C26 C25 178.55(19) . . . . ? C24 C25 C26 N21 -0.9(4) . . . . ? C24 C20 C30 C34 177.9(2) . . . . ? Co1 O1 C31 O2 7.6(2) 3_545 . . . ? Co1 O1 C31 C3 -170.54(17) 3_545 . . . ? Co1 O2 C31 O1 -7.2(2) 3_545 . . . ? Co1 O2 C31 C3 170.93(17) 3_545 . . . ? C4 C3 C31 O1 -174.5(2) . . . . ? C2 C3 C31 O1 8.3(3) . . . . ? C4 C3 C31 O2 7.4(3) . . . . ? C2 C3 C31 O2 -169.9(2) . . . . ? C36 N31 C32 C33 1.3(4) . . . . ? Co1 N31 C32 C33 -179.0(2) 6_566 . . . ? N31 C32 C33 C34 0.7(4) . . . . ? C32 C33 C34 C35 -2.3(4) . . . . ? C32 C33 C34 C30 176.9(2) . . . . ? C20 C30 C34 C35 22.7(4) . . . . ? C20 C30 C34 C33 -156.4(3) . . . . ? C33 C34 C35 C36 1.9(4) . . . . ? C30 C34 C35 C36 -177.3(3) . . . . ? C32 N31 C36 C35 -1.7(4) . . . . ? Co1 N31 C36 C35 178.5(2) 6_566 . . . ? C34 C35 C36 N31 0.2(4) . . . . ? C46 N41 C42 C43 -2.1(15) . . . . ? N41 C42 C43 C44 11.8(14) . . . . ? C42 C43 C44 C45 -18.2(12) . . . . ? C42 C43 C44 C40 177.8(7) . . . . ? C40B C40 C44 C45 176.6(8) 7_556 . . . ? C40B C40 C44 C43 -18.9(14) 7_556 . . . ? C43 C44 C45 C46 15.4(13) . . . . ? C40 C44 C45 C46 179.5(7) . . . . ? C42 N41 C46 C45 -2.2(14) . . . . ? C44 C45 C46 N41 -4.5(14) . . . . ? Co1 O3 C51 O4 -2.9(3) 3 . . . ? Co1 O3 C51 C5 176.99(15) 3 . . . ? C4 C5 C51 O4 -14.4(3) . . . . ? C6 C5 C51 O4 164.6(2) . . . . ? C4 C5 C51 O3 165.8(2) . . . . ? C6 C5 C51 O3 -15.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.616 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.122 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 893713' #TrackingRef 'CE-ART-09-2012-026533.cif' _audit_creation_date 2012-10-08 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _chemical_name_systematic ; [Co(L)(BPE)]-4(H2O) ; _chemical_name_common (Co(L)(BPE))-4(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C25 H27 Co N3 O8' _chemical_formula_sum 'C25 H27 Co N3 O8' _chemical_formula_weight 556.43 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' '-x+1/2, -y+1/2, z+1' 'x+1/2, y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' '-x+1, -y, z+1' 'x+1/2, y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' '-x+1, -y+1/2, z+1/2' _cell_length_a 52.349(8) _cell_length_b 20.421(4) _cell_length_c 9.9111(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10595(3) _cell_formula_units_Z 16 _cell_measurement_temperature 200 _cell_measurement_reflns_used 23245 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4624 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8727 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_special_details ; [Co(L)(BPE)]-4(H2O) ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 25291 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -66 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5829 _reflns_number_gt 5359 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(10) _refine_ls_number_reflns 5829 _refine_ls_number_parameters 383 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.461795(5) 0.339565(11) 0.16536(2) 0.01904(8) Uani 1 1 d . . . O1 O 0.45939(4) 0.41590(11) 0.30966(19) 0.0371(5) Uani 1 1 d . . . O2 O 0.46488(4) 0.32349(11) 0.4159(3) 0.0469(5) Uani 1 1 d . . . O3 O 0.45887(4) 0.41970(10) 1.02899(19) 0.0366(5) Uani 1 1 d . . . O4 O 0.46125(4) 0.32708(11) 0.9258(3) 0.0489(6) Uani 1 1 d . . . O5 O 0.3661(6) 0.4308(15) 0.697(3) 0.183(9) Uani 0.291(14) 1 d PU . . O5B O 0.3883(4) 0.4188(10) 0.572(2) 0.212(8) Uani 0.414(15) 1 d PU . . O5C O 0.3911(5) 0.4553(11) 0.679(3) 0.194(7) Uani 0.296(13) 1 d PU . . O6 O 0.3780(3) 0.5428(14) 0.448(3) 0.285(9) Uani 0.489(10) 1 d PDU . . O6B O 0.3707(5) 0.6199(16) 0.464(2) 0.285(9) Uani 0.511(10) 1 d PU . . O7 O 0.41140(19) 0.4856(5) 0.3107(12) 0.135(4) Uani 0.489(10) 1 d PU . . O7B O 0.3983(3) 0.4724(8) 0.422(2) 0.219(7) Uani 0.511(10) 1 d PU . . O8 O 0.3413(3) 0.5370(7) 0.512(2) 0.228(8) Uani 0.489(10) 1 d PDU . . O8B O 0.3635(4) 0.4846(12) 0.601(2) 0.287(10) Uani 0.511(10) 1 d PU . . N11 N 0.46447(3) 0.73447(7) 0.6633(2) 0.0228(3) Uani 1 1 d . . . N21 N 0.50245(3) 0.35057(8) 0.1577(2) 0.0241(3) Uani 1 1 d . . . N31 N 0.67086(3) 0.42118(9) -0.0703(2) 0.0299(4) Uani 1 1 d . . . C1 C 0.46417(3) 0.52428(9) 0.6659(3) 0.0204(3) Uani 1 1 d . . . C2 C 0.46423(4) 0.48859(11) 0.5451(2) 0.0233(4) Uani 1 1 d . . . H1 H 0.4650 0.5109 0.4612 0.028 Uiso 1 1 calc R . . C3 C 0.46317(4) 0.42070(12) 0.5478(3) 0.0232(5) Uani 1 1 d . . . C4 C 0.46226(4) 0.38771(9) 0.6687(3) 0.0233(4) Uani 1 1 d . . . H2 H 0.4618 0.3412 0.6699 0.028 Uiso 1 1 calc R . . C5 C 0.46204(4) 0.42282(12) 0.7900(3) 0.0217(5) Uani 1 1 d . . . C6 C 0.46314(4) 0.49027(11) 0.7876(2) 0.0207(4) Uani 1 1 d . . . H3 H 0.4632 0.5139 0.8702 0.025 Uiso 1 1 calc R . . C12 C 0.45481(6) 0.69967(11) 0.5606(3) 0.0390(6) Uani 1 1 d . . . H4 H 0.4479 0.7226 0.4857 0.047 Uiso 1 1 calc R . . C13 C 0.45444(6) 0.63236(12) 0.5586(3) 0.0413(6) Uani 1 1 d . . . H5 H 0.4471 0.6101 0.4837 0.050 Uiso 1 1 calc R . . C14 C 0.46458(4) 0.59674(9) 0.6645(3) 0.0231(4) Uani 1 1 d . . . C15 C 0.47466(4) 0.63277(10) 0.7708(2) 0.0237(4) Uani 1 1 d . . . H6 H 0.4817 0.6110 0.8469 0.028 Uiso 1 1 calc R . . C16 C 0.47438(4) 0.70063(10) 0.7656(2) 0.0229(4) Uani 1 1 d . . . H7 H 0.4817 0.7242 0.8387 0.027 Uiso 1 1 calc R . . C31 C 0.46248(4) 0.38401(12) 0.4165(3) 0.0294(5) Uani 1 1 d . . . C51 C 0.46058(4) 0.38675(12) 0.9219(3) 0.0297(5) Uani 1 1 d . . . C20 C 0.58331(5) 0.38646(16) 0.1143(4) 0.0514(7) Uani 1 1 d . . . H8 H 0.5899 0.4096 0.1949 0.062 Uiso 1 1 calc R . . H9 H 0.5922 0.3439 0.1079 0.062 Uiso 1 1 calc R . . C22 C 0.51239(5) 0.41039(10) 0.1766(3) 0.0344(5) Uani 1 1 d . . . H10 H 0.5011 0.4451 0.1997 0.041 Uiso 1 1 calc R . . C23 C 0.53805(5) 0.42423(12) 0.1643(4) 0.0391(5) Uani 1 1 d . . . H11 H 0.5441 0.4676 0.1777 0.047 Uiso 1 1 calc R . . C24 C 0.55503(4) 0.37428(13) 0.1322(3) 0.0368(6) Uani 1 1 d . . . C25 C 0.54484(5) 0.31281(13) 0.1116(3) 0.0394(6) Uani 1 1 d . . . H12 H 0.5557 0.2772 0.0892 0.047 Uiso 1 1 calc R . . C26 C 0.51879(4) 0.30309(11) 0.1236(3) 0.0325(5) Uani 1 1 d . . . H13 H 0.5122 0.2605 0.1067 0.039 Uiso 1 1 calc R . . C30 C 0.58925(5) 0.42629(17) -0.0090(4) 0.0546(8) Uani 1 1 d . . . H14 H 0.5830 0.4716 0.0037 0.065 Uiso 1 1 calc R . . H15 H 0.5803 0.4073 -0.0880 0.065 Uiso 1 1 calc R . . C32 C 0.66043(5) 0.45726(14) 0.0256(3) 0.0448(6) Uani 1 1 d . . . H16 H 0.6714 0.4818 0.0827 0.054 Uiso 1 1 calc R . . C33 C 0.63421(5) 0.46122(17) 0.0474(4) 0.0551(8) Uani 1 1 d . . . H17 H 0.6277 0.4872 0.1192 0.066 Uiso 1 1 calc R . . C34 C 0.61766(5) 0.42742(15) -0.0351(3) 0.0450(6) Uani 1 1 d . . . C35 C 0.62842(6) 0.39156(19) -0.1360(4) 0.0584(8) Uani 1 1 d . . . H18 H 0.6179 0.3681 -0.1971 0.070 Uiso 1 1 calc R . . C36 C 0.65480(5) 0.38918(16) -0.1499(4) 0.0516(7) Uani 1 1 d . . . H19 H 0.6617 0.3632 -0.2204 0.062 Uiso 1 1 calc R . . 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 0.02701(12) 0.01172(11) 0.01840(12) 0.00029(10) 0.00298(11) 0.00035(9) O1 0.0477(10) 0.0464(12) 0.0172(9) -0.0121(8) 0.0033(8) 0.0035(8) O2 0.0664(12) 0.0246(8) 0.0499(13) -0.0217(11) 0.0003(11) 0.0054(8) O3 0.0491(11) 0.0420(11) 0.0187(10) 0.0060(8) 0.0020(8) -0.0069(8) O4 0.0787(15) 0.0265(9) 0.0416(13) 0.0131(10) 0.0097(10) 0.0033(8) O5 0.202(15) 0.158(13) 0.191(14) -0.041(12) -0.024(12) -0.006(12) O5B 0.211(12) 0.219(13) 0.208(13) -0.065(11) -0.079(11) -0.032(10) O5C 0.180(12) 0.186(12) 0.216(12) -0.082(11) -0.032(11) 0.021(10) O6 0.267(14) 0.323(17) 0.264(15) -0.003(14) 0.009(12) 0.006(13) O6B 0.282(14) 0.349(17) 0.224(14) -0.005(14) 0.022(11) 0.006(14) O7 0.133(7) 0.126(7) 0.146(8) -0.002(6) -0.034(6) 0.067(6) O7B 0.191(11) 0.208(11) 0.259(15) -0.006(12) -0.044(11) -0.011(9) O8 0.281(14) 0.182(12) 0.222(14) -0.062(10) -0.062(12) -0.001(10) O8B 0.341(17) 0.272(16) 0.248(15) -0.142(13) -0.109(13) -0.027(14) N11 0.0334(8) 0.0139(7) 0.0210(7) -0.0013(9) -0.0003(8) -0.0008(6) N21 0.0297(7) 0.0196(8) 0.0231(8) 0.0002(8) 0.0036(9) -0.0018(6) N31 0.0265(8) 0.0256(9) 0.0377(11) -0.0003(9) 0.0041(9) -0.0005(6) C1 0.0297(8) 0.0143(8) 0.0173(8) -0.0005(9) 0.0011(8) 0.0001(7) C2 0.0349(11) 0.0203(11) 0.0148(10) 0.0019(8) 0.0011(8) -0.0013(8) C3 0.0307(11) 0.0203(11) 0.0187(11) -0.0030(9) -0.0007(9) 0.0013(8) C4 0.0314(9) 0.0144(8) 0.0241(9) 0.0002(10) 0.0012(8) 0.0022(7) C5 0.0277(11) 0.0171(10) 0.0204(11) 0.0035(9) 0.0011(8) 0.0026(8) C6 0.0281(10) 0.0164(10) 0.0174(10) 0.0006(8) 0.0030(7) 0.0012(7) C12 0.0754(17) 0.0160(11) 0.0258(11) 0.0032(9) -0.0158(12) -0.0010(11) C13 0.0789(18) 0.0178(11) 0.0273(12) -0.0005(9) -0.0186(13) -0.0056(12) C14 0.0340(10) 0.0143(8) 0.0210(9) 0.0036(11) 0.0026(10) -0.0011(7) C15 0.0339(11) 0.0161(9) 0.0210(10) 0.0012(8) -0.0049(8) 0.0017(8) C16 0.0304(10) 0.0157(9) 0.0225(9) -0.0012(8) -0.0025(8) -0.0001(8) C31 0.0323(10) 0.0308(12) 0.0251(11) -0.0107(12) 0.0004(10) 0.0006(7) C51 0.0317(10) 0.0298(12) 0.0275(12) 0.0161(12) 0.0033(10) 0.0012(7) C20 0.0319(12) 0.0602(18) 0.0622(19) 0.0178(15) 0.0005(12) -0.0042(12) C22 0.0345(11) 0.0237(11) 0.0449(14) -0.0040(11) 0.0046(11) -0.0025(8) C23 0.0373(11) 0.0293(10) 0.0505(14) -0.0012(17) 0.0019(11) -0.0109(10) C24 0.0304(11) 0.0428(14) 0.0372(14) 0.0082(10) 0.0001(9) -0.0029(10) C25 0.0352(12) 0.0323(13) 0.0507(15) 0.0051(12) 0.0106(11) 0.0061(10) C26 0.0343(11) 0.0229(10) 0.0401(13) 0.0015(9) 0.0097(10) 0.0000(9) C30 0.0311(13) 0.069(2) 0.063(2) 0.0171(16) 0.0055(13) 0.0021(13) C32 0.0332(12) 0.0483(16) 0.0529(16) -0.0138(13) 0.0075(11) -0.0030(11) C33 0.0384(14) 0.065(2) 0.062(2) -0.0150(15) 0.0149(14) 0.0031(13) C34 0.0326(12) 0.0489(16) 0.0535(16) 0.0159(13) 0.0038(12) 0.0003(11) C35 0.0381(14) 0.076(2) 0.061(2) -0.0131(17) 0.0013(14) -0.0147(15) C36 0.0335(12) 0.0644(19) 0.0569(18) -0.0253(15) 0.0040(12) -0.0058(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.119(2) . ? Co1 O3 2.128(2) 1_554 ? Co1 N21 2.1414(17) . ? Co1 N11 2.1508(16) 5_544 ? Co1 N31 2.1589(17) 15_455 ? Co1 O4 2.388(3) 1_554 ? O1 C31 1.253(4) . ? O2 C31 1.242(3) . ? O3 C51 1.260(4) . ? O3 Co1 2.128(2) 1_556 ? O4 C51 1.220(3) . ? O4 Co1 2.388(3) 1_556 ? O5 O5C 1.41(3) . ? O5 O6B 1.43(3) 14_545 ? O5 O8B 1.46(3) . ? O5 O5B 1.72(4) . ? O5B O5C 1.30(3) . ? O5B O6B 1.79(3) 14_545 ? O5C O8B 1.74(3) . ? O6 O6B 1.63(3) . ? O6 O7B 1.81(3) . ? O6B O5 1.43(3) 10_554 ? O6B O5B 1.79(3) 10_554 ? O7 O7B 1.32(2) . ? O8 O8B 1.81(3) . ? N11 C16 1.332(3) . ? N11 C12 1.340(3) . ? N11 Co1 2.1508(16) 5 ? N21 C26 1.337(3) . ? N21 C22 1.341(3) . ? N31 C32 1.320(3) . ? N31 C36 1.325(3) . ? N31 Co1 2.1589(17) 7_554 ? C1 C6 1.393(3) . ? C1 C2 1.401(3) . ? C1 C14 1.480(2) . ? C2 C3 1.388(4) . ? C2 H1 0.9500 . ? C3 C4 1.376(4) . ? C3 C31 1.502(4) . ? C4 C5 1.399(4) . ? C4 H2 0.9500 . ? C5 C6 1.379(4) . ? C5 C51 1.503(3) . ? C6 H3 0.9500 . ? C12 C13 1.375(3) . ? C12 H4 0.9500 . ? C13 C14 1.383(4) . ? C13 H5 0.9500 . ? C14 C15 1.389(4) . ? C15 C16 1.387(3) . ? C15 H6 0.9500 . ? C16 H7 0.9500 . ? C20 C30 1.501(4) . ? C20 C24 1.512(3) . ? C20 H8 0.9900 . ? C20 H9 0.9900 . ? C22 C23 1.379(4) . ? C22 H10 0.9500 . ? C23 C24 1.390(4) . ? C23 H11 0.9500 . ? C24 C25 1.379(4) . ? C25 C26 1.383(3) . ? C25 H12 0.9500 . ? C26 H13 0.9500 . ? C30 C34 1.510(4) . ? C30 H14 0.9900 . ? C30 H15 0.9900 . ? C32 C33 1.392(4) . ? C32 H16 0.9500 . ? C33 C34 1.377(4) . ? C33 H17 0.9500 . ? C34 C35 1.361(5) . ? C35 C36 1.388(4) . ? C35 H18 0.9500 . ? C36 H19 0.9500 . ? 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 _geom_angle_publ_flag O1 Co1 O3 81.87(7) . 1_554 ? O1 Co1 N21 90.33(7) . . ? O3 Co1 N21 88.18(7) 1_554 . ? O1 Co1 N11 138.09(8) . 5_544 ? O3 Co1 N11 140.01(8) 1_554 5_544 ? N21 Co1 N11 92.28(6) . 5_544 ? O1 Co1 N31 88.35(8) . 15_455 ? O3 Co1 N31 92.79(8) 1_554 15_455 ? N21 Co1 N31 178.24(10) . 15_455 ? N11 Co1 N31 87.92(6) 5_544 15_455 ? O1 Co1 O4 138.49(8) . 1_554 ? O3 Co1 O4 56.62(8) 1_554 1_554 ? N21 Co1 O4 89.30(8) . 1_554 ? N11 Co1 O4 83.39(8) 5_544 1_554 ? N31 Co1 O4 92.46(8) 15_455 1_554 ? C31 O1 Co1 100.37(17) . . ? C51 O3 Co1 96.84(16) . 1_556 ? C51 O4 Co1 85.69(18) . 1_556 ? O5C O5 O6B 83(2) . 14_545 ? O5C O5 O8B 74(2) . . ? O6B O5 O8B 141(3) 14_545 . ? O5C O5 O5B 47.8(14) . . ? O6B O5 O5B 68.5(16) 14_545 . ? O8B O5 O5B 72.3(18) . . ? O5C O5B O5 53.6(16) . . ? O5C O5B O6B 73(2) . 14_545 ? O5 O5B O6B 48.1(13) . 14_545 ? O5B O5C O5 78.6(19) . . ? O5B O5C O8B 75.3(16) . . ? O5 O5C O8B 54.1(16) . . ? O6B O6 O7B 156.9(17) . . ? O5 O6B O6 136(2) 10_554 . ? O5 O6B O5B 63.3(17) 10_554 10_554 ? O6 O6B O5B 121.7(19) . 10_554 ? O7 O7B O6 105.3(15) . . ? O5 O8B O5C 51.4(14) . . ? O5 O8B O8 145(2) . . ? O5C O8B O8 162(2) . . ? C16 N11 C12 116.73(17) . . ? C16 N11 Co1 122.41(15) . 5 ? C12 N11 Co1 120.77(16) . 5 ? C26 N21 C22 116.61(19) . . ? C26 N21 Co1 124.68(15) . . ? C22 N21 Co1 118.44(14) . . ? C32 N31 C36 116.2(2) . . ? C32 N31 Co1 120.97(17) . 7_554 ? C36 N31 Co1 122.71(17) . 7_554 ? C6 C1 C2 118.71(16) . . ? C6 C1 C14 120.5(2) . . ? C2 C1 C14 120.8(2) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H1 119.9 . . ? C1 C2 H1 119.9 . . ? C4 C3 C2 120.5(2) . . ? C4 C3 C31 120.6(2) . . ? C2 C3 C31 118.9(2) . . ? C3 C4 C5 119.84(16) . . ? C3 C4 H2 120.1 . . ? C5 C4 H2 120.1 . . ? C6 C5 C4 119.8(2) . . ? C6 C5 C51 120.4(2) . . ? C4 C5 C51 119.8(2) . . ? C5 C6 C1 121.0(2) . . ? C5 C6 H3 119.5 . . ? C1 C6 H3 119.5 . . ? N11 C12 C13 123.1(2) . . ? N11 C12 H4 118.4 . . ? C13 C12 H4 118.4 . . ? C12 C13 C14 120.6(2) . . ? C12 C13 H5 119.7 . . ? C14 C13 H5 119.7 . . ? C13 C14 C15 116.29(18) . . ? C13 C14 C1 121.8(2) . . ? C15 C14 C1 121.9(2) . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H6 120.1 . . ? C14 C15 H6 120.1 . . ? N11 C16 C15 123.5(2) . . ? N11 C16 H7 118.3 . . ? C15 C16 H7 118.3 . . ? O2 C31 O1 121.8(2) . . ? O2 C31 C3 119.9(3) . . ? O1 C31 C3 118.4(2) . . ? O4 C51 O3 120.6(3) . . ? O4 C51 C5 121.0(3) . . ? O3 C51 C5 118.3(2) . . ? C30 C20 C24 112.8(2) . . ? C30 C20 H8 109.0 . . ? C24 C20 H8 109.0 . . ? C30 C20 H9 109.0 . . ? C24 C20 H9 109.0 . . ? H8 C20 H9 107.8 . . ? N21 C22 C23 123.5(2) . . ? N21 C22 H10 118.2 . . ? C23 C22 H10 118.2 . . ? C22 C23 C24 119.5(2) . . ? C22 C23 H11 120.2 . . ? C24 C23 H11 120.2 . . ? C25 C24 C23 117.1(2) . . ? C25 C24 C20 120.7(2) . . ? C23 C24 C20 122.2(2) . . ? C24 C25 C26 119.9(2) . . ? C24 C25 H12 120.0 . . ? C26 C25 H12 120.0 . . ? N21 C26 C25 123.3(2) . . ? N21 C26 H13 118.4 . . ? C25 C26 H13 118.4 . . ? C20 C30 C34 110.6(2) . . ? C20 C30 H14 109.5 . . ? C34 C30 H14 109.5 . . ? C20 C30 H15 109.5 . . ? C34 C30 H15 109.5 . . ? H14 C30 H15 108.1 . . ? N31 C32 C33 123.5(3) . . ? N31 C32 H16 118.2 . . ? C33 C32 H16 118.2 . . ? C34 C33 C32 119.9(3) . . ? C34 C33 H17 120.0 . . ? C32 C33 H17 120.0 . . ? C35 C34 C33 116.4(2) . . ? C35 C34 C30 121.7(3) . . ? C33 C34 C30 121.7(3) . . ? C34 C35 C36 120.2(3) . . ? C34 C35 H18 119.9 . . ? C36 C35 H18 119.9 . . ? N31 C36 C35 123.7(3) . . ? N31 C36 H19 118.2 . . ? C35 C36 H19 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co1 O1 C31 -175.50(15) 1_554 . . . ? N21 Co1 O1 C31 -87.39(15) . . . . ? N11 Co1 O1 C31 6.40(19) 5_544 . . . ? N31 Co1 O1 C31 91.44(15) 15_455 . . . ? O4 Co1 O1 C31 -176.71(13) 1_554 . . . ? O6B O5 O5B O5C -100(2) 14_545 . . . ? O8B O5 O5B O5C 84.8(19) . . . . ? O5C O5 O5B O6B 100(2) . . . 14_545 ? O8B O5 O5B O6B -175(2) . . . 14_545 ? O6B O5B O5C O5 -49.9(16) 14_545 . . . ? O5 O5B O5C O8B -55.6(16) . . . . ? O6B O5B O5C O8B -105.5(16) 14_545 . . . ? O6B O5 O5C O5B 67.3(18) 14_545 . . . ? O8B O5 O5C O5B -80.0(17) . . . . ? O6B O5 O5C O8B 147(2) 14_545 . . . ? O5B O5 O5C O8B 80.0(17) . . . . ? O7B O6 O6B O5 7(8) . . . 10_554 ? O7B O6 O6B O5B 90(5) . . . 10_554 ? O6B O6 O7B O7 -51(6) . . . . ? O6B O5 O8B O5C -57(4) 14_545 . . . ? O5B O5 O8B O5C -50.0(13) . . . . ? O5C O5 O8B O8 -170(2) . . . . ? O6B O5 O8B O8 133(4) 14_545 . . . ? O5B O5 O8B O8 140(2) . . . . ? O5B O5C O8B O5 86(2) . . . . ? O5B O5C O8B O8 -112(5) . . . . ? O5 O5C O8B O8 161(5) . . . . ? O1 Co1 N21 C26 154.0(2) . . . . ? O3 Co1 N21 C26 -124.1(2) 1_554 . . . ? N11 Co1 N21 C26 15.8(2) 5_544 . . . ? N31 Co1 N21 C26 112(2) 15_455 . . . ? O4 Co1 N21 C26 -67.5(2) 1_554 . . . ? O1 Co1 N21 C22 -32.18(19) . . . . ? O3 Co1 N21 C22 49.68(19) 1_554 . . . ? N11 Co1 N21 C22 -170.34(19) 5_544 . . . ? N31 Co1 N21 C22 -74(2) 15_455 . . . ? O4 Co1 N21 C22 106.30(19) 1_554 . . . ? C6 C1 C2 C3 0.3(3) . . . . ? C14 C1 C2 C3 -178.33(19) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? C1 C2 C3 C31 178.21(18) . . . . ? C2 C3 C4 C5 0.9(3) . . . . ? C31 C3 C4 C5 -177.81(18) . . . . ? C3 C4 C5 C6 -1.0(3) . . . . ? C3 C4 C5 C51 178.93(19) . . . . ? C4 C5 C6 C1 0.8(3) . . . . ? C51 C5 C6 C1 -179.15(18) . . . . ? C2 C1 C6 C5 -0.4(3) . . . . ? C14 C1 C6 C5 178.19(18) . . . . ? C16 N11 C12 C13 1.1(4) . . . . ? Co1 N11 C12 C13 -175.4(2) 5 . . . ? N11 C12 C13 C14 -0.8(5) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? C12 C13 C14 C1 179.2(2) . . . . ? C6 C1 C14 C13 -150.5(3) . . . . ? C2 C1 C14 C13 28.1(3) . . . . ? C6 C1 C14 C15 28.1(3) . . . . ? C2 C1 C14 C15 -153.3(2) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? C1 C14 C15 C16 -179.3(2) . . . . ? C12 N11 C16 C15 -1.2(3) . . . . ? Co1 N11 C16 C15 175.24(16) 5 . . . ? C14 C15 C16 N11 1.1(3) . . . . ? Co1 O1 C31 O2 -2.6(2) . . . . ? Co1 O1 C31 C3 177.59(16) . . . . ? C4 C3 C31 O2 -10.6(3) . . . . ? C2 C3 C31 O2 170.7(2) . . . . ? C4 C3 C31 O1 169.2(2) . . . . ? C2 C3 C31 O1 -9.5(3) . . . . ? Co1 O4 C51 O3 -4.6(2) 1_556 . . . ? Co1 O4 C51 C5 174.78(18) 1_556 . . . ? Co1 O3 C51 O4 5.1(2) 1_556 . . . ? Co1 O3 C51 C5 -174.21(16) 1_556 . . . ? C6 C5 C51 O4 -175.2(2) . . . . ? C4 C5 C51 O4 4.8(3) . . . . ? C6 C5 C51 O3 4.1(3) . . . . ? C4 C5 C51 O3 -175.8(2) . . . . ? C26 N21 C22 C23 -0.8(4) . . . . ? Co1 N21 C22 C23 -175.2(3) . . . . ? N21 C22 C23 C24 -0.8(5) . . . . ? C22 C23 C24 C25 1.3(5) . . . . ? C22 C23 C24 C20 178.7(3) . . . . ? C30 C20 C24 C25 108.7(3) . . . . ? C30 C20 C24 C23 -68.5(4) . . . . ? C23 C24 C25 C26 -0.2(4) . . . . ? C20 C24 C25 C26 -177.6(3) . . . . ? C22 N21 C26 C25 2.0(4) . . . . ? Co1 N21 C26 C25 175.9(2) . . . . ? C24 C25 C26 N21 -1.5(4) . . . . ? C24 C20 C30 C34 -170.5(3) . . . . ? C36 N31 C32 C33 1.8(5) . . . . ? Co1 N31 C32 C33 -173.9(3) 7_554 . . . ? N31 C32 C33 C34 -1.4(5) . . . . ? C32 C33 C34 C35 -0.3(5) . . . . ? C32 C33 C34 C30 175.4(3) . . . . ? C20 C30 C34 C35 105.1(4) . . . . ? C20 C30 C34 C33 -70.4(4) . . . . ? C33 C34 C35 C36 1.4(5) . . . . ? C30 C34 C35 C36 -174.3(3) . . . . ? C32 N31 C36 C35 -0.6(5) . . . . ? Co1 N31 C36 C35 175.0(3) 7_554 . . . ? C34 C35 C36 N31 -1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.510 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.109 #====END