# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Robert LaDuca' _publ_contact_author_email LADUCA@MSU.EDU _publ_section_title ; Pendant Arm Position Control of Topology in Cobalt Phenylenediacetate Coordination Polymers Containing Long-Spanning Dipyridyl Ligands: Rectangular Grid, Primitive Cubic, and 5-Connected Archimedean Layered Net Topologies ; loop_ _publ_author_name 'Robert LaDuca' 'Karyn M. Blake' 'Lindsey L. Johnston' 'Joseph A. Nettleman' 'Ronald M Supkowski' # Attachment 'co13phda4bpmpfinal.cif' data_p21n _database_code_depnum_ccdc_archive 'CCDC 714971' #TrackingRef 'co13phda4bpmpfinal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 Co N4 O4' _chemical_formula_weight 519.45 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.057(4) _cell_length_b 9.896(2) _cell_length_c 16.909(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.425(3) _cell_angle_gamma 90.00 _cell_volume 2428.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26545 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max .45 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6942 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26545 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5641 _reflns_number_gt 4352 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0355P)^2^+1.7760P] 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 5641 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.633092(18) 0.41963(3) 0.547223(15) 0.01699(8) Uani 1 1 d . . . C1 C 0.64205(15) 0.2392(2) 0.69645(12) 0.0221(4) Uani 1 1 d . . . H1 H 0.6453 0.1707 0.6580 0.027 Uiso 1 1 calc R . . C2 C 0.64770(15) 0.2013(2) 0.77601(12) 0.0243(5) Uani 1 1 d . . . H2 H 0.6562 0.1089 0.7915 0.029 Uiso 1 1 calc R . . C3 C 0.64093(15) 0.2978(2) 0.83352(12) 0.0229(5) Uani 1 1 d . . . C4 C 0.63026(19) 0.4306(2) 0.80682(13) 0.0362(6) Uani 1 1 d . . . H4 H 0.6250 0.5009 0.8436 0.043 Uiso 1 1 calc R . . C5 C 0.62736(19) 0.4601(2) 0.72646(13) 0.0340(6) Uani 1 1 d . . . H5 H 0.6215 0.5522 0.7100 0.041 Uiso 1 1 calc R . . C6 C 0.64381(19) 0.2538(2) 0.91944(13) 0.0324(6) Uani 1 1 d . . . H6A H 0.5941 0.1868 0.9164 0.039 Uiso 1 1 calc R . . H6B H 0.7032 0.2075 0.9432 0.039 Uiso 1 1 calc R . . C7 C 0.71977(14) 0.4355(2) 1.00735(12) 0.0229(4) Uani 1 1 d . . . H7A H 0.7404 0.4747 0.9613 0.027 Uiso 1 1 calc R . . H7B H 0.7680 0.3725 1.0376 0.027 Uiso 1 1 calc R . . C8 C 0.60589(17) 0.3052(2) 1.04482(13) 0.0312(5) Uani 1 1 d . . . H8A H 0.6535 0.2408 1.0744 0.037 Uiso 1 1 calc R . . H8B H 0.5475 0.2548 1.0244 0.037 Uiso 1 1 calc R . . C9 C 0.70636(15) 0.5466(2) 1.06383(12) 0.0224(4) Uani 1 1 d . . . H9A H 0.7645 0.5977 1.0838 0.027 Uiso 1 1 calc R . . H9B H 0.6585 0.6099 1.0334 0.027 Uiso 1 1 calc R . . C10 C 0.59307(15) 0.4149(2) 1.10331(13) 0.0273(5) Uani 1 1 d . . . H10A H 0.5433 0.4769 1.0746 0.033 Uiso 1 1 calc R . . H10B H 0.5748 0.3736 1.1500 0.033 Uiso 1 1 calc R . . C11 C 0.66710(18) 0.6006(2) 1.18791(13) 0.0289(5) Uani 1 1 d . . . H11A H 0.6125 0.6545 1.1597 0.035 Uiso 1 1 calc R . . H11B H 0.7216 0.6606 1.1978 0.035 Uiso 1 1 calc R . . C12 C 0.6875(3) 0.4067(3) 1.38441(16) 0.0620(10) Uani 1 1 d . . . H12 H 0.7178 0.3274 1.4097 0.074 Uiso 1 1 calc R . . C13 C 0.6971(3) 0.4412(3) 1.30810(16) 0.0628(11) Uani 1 1 d . . . H13 H 0.7330 0.3859 1.2825 0.075 Uiso 1 1 calc R . . C14 C 0.65554(15) 0.5540(2) 1.26940(12) 0.0221(4) Uani 1 1 d . . . C15 C 0.60530(19) 0.6278(3) 1.31001(14) 0.0401(6) Uani 1 1 d . . . H15 H 0.5743 0.7073 1.2857 0.048 Uiso 1 1 calc R . . C16 C 0.59946(18) 0.5869(3) 1.38665(14) 0.0398(6) Uani 1 1 d . . . H16 H 0.5648 0.6416 1.4138 0.048 Uiso 1 1 calc R . . C21 C 0.45675(13) 0.1233(2) 0.33752(12) 0.0196(4) Uani 1 1 d . . . C22 C 0.41363(14) 0.1648(2) 0.25821(12) 0.0192(4) Uani 1 1 d . . . H22 H 0.3572 0.2132 0.2483 0.023 Uiso 1 1 calc R . . C23 C 0.45065(14) 0.1376(2) 0.19269(12) 0.0203(4) Uani 1 1 d . . . C24 C 0.53262(15) 0.0662(2) 0.20771(13) 0.0267(5) Uani 1 1 d . . . H24 H 0.5588 0.0462 0.1638 0.032 Uiso 1 1 calc R . . C25 C 0.57693(16) 0.0235(3) 0.28698(14) 0.0317(5) Uani 1 1 d . . . H25 H 0.6331 -0.0254 0.2969 0.038 Uiso 1 1 calc R . . C26 C 0.53916(15) 0.0523(2) 0.35083(13) 0.0283(5) Uani 1 1 d . . . H26 H 0.5698 0.0231 0.4047 0.034 Uiso 1 1 calc R . . C27 C 0.41587(14) 0.1576(2) 0.40778(12) 0.0226(4) Uani 1 1 d . . . H27A H 0.4272 0.0822 0.4477 0.027 Uiso 1 1 calc R . . H27B H 0.3484 0.1694 0.3865 0.027 Uiso 1 1 calc R . . C28 C 0.45829(14) 0.2868(2) 0.45068(11) 0.0189(4) Uani 1 1 d . . . C29 C 0.40139(14) 0.1856(2) 0.10745(12) 0.0244(5) Uani 1 1 d . . . H29A H 0.4301 0.1428 0.0674 0.029 Uiso 1 1 calc R . . H29B H 0.4094 0.2846 0.1044 0.029 Uiso 1 1 calc R . . C30 C 0.29918(14) 0.1531(2) 0.08379(11) 0.0193(4) Uani 1 1 d . . . N1 N 0.63225(12) 0.36758(18) 0.67048(10) 0.0208(4) Uani 1 1 d . . . N2 N 0.63359(12) 0.36225(18) 0.97532(10) 0.0230(4) Uani 1 1 d . . . N3 N 0.67854(12) 0.49077(17) 1.13391(10) 0.0203(4) Uani 1 1 d . . . N4 N 0.63872(12) 0.47735(18) 1.42466(10) 0.0230(4) Uani 1 1 d . . . O1 O 0.27516(10) 0.03254(15) 0.09017(9) 0.0244(3) Uani 1 1 d . . . O2 O 0.24097(10) 0.24357(15) 0.05697(8) 0.0238(3) Uani 1 1 d . . . O3 O 0.53646(10) 0.27665(14) 0.50061(8) 0.0226(3) Uani 1 1 d . . . O4 O 0.41303(11) 0.39386(15) 0.43257(9) 0.0299(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 0.02004(15) 0.01975(14) 0.01027(13) -0.00003(11) 0.00244(10) 0.00093(11) C1 0.0314(12) 0.0212(10) 0.0154(10) -0.0026(8) 0.0090(8) -0.0002(9) C2 0.0375(13) 0.0181(10) 0.0188(10) 0.0001(8) 0.0100(9) -0.0033(9) C3 0.0304(12) 0.0254(11) 0.0137(10) -0.0004(8) 0.0072(9) -0.0008(9) C4 0.0713(18) 0.0229(12) 0.0145(10) -0.0019(9) 0.0119(11) 0.0116(12) C5 0.0650(17) 0.0200(11) 0.0160(11) 0.0015(9) 0.0092(11) 0.0084(11) C6 0.0625(17) 0.0223(11) 0.0159(10) -0.0011(9) 0.0164(10) -0.0023(11) C7 0.0275(11) 0.0282(11) 0.0164(10) 0.0025(8) 0.0120(8) 0.0008(9) C8 0.0441(14) 0.0343(13) 0.0198(11) -0.0041(10) 0.0167(10) -0.0149(11) C9 0.0295(12) 0.0245(11) 0.0150(10) 0.0020(8) 0.0094(8) -0.0024(9) C10 0.0299(12) 0.0379(13) 0.0174(10) -0.0019(9) 0.0121(9) -0.0049(10) C11 0.0502(15) 0.0229(11) 0.0169(10) 0.0012(9) 0.0148(10) 0.0026(10) C12 0.134(3) 0.0345(15) 0.0271(14) 0.0132(12) 0.0383(17) 0.0425(18) C13 0.129(3) 0.0449(17) 0.0285(14) 0.0156(12) 0.0453(17) 0.0528(19) C14 0.0307(12) 0.0215(11) 0.0143(10) -0.0013(8) 0.0060(8) -0.0008(9) C15 0.0593(17) 0.0407(14) 0.0245(12) 0.0134(11) 0.0186(12) 0.0254(13) C16 0.0503(16) 0.0526(16) 0.0225(12) 0.0117(11) 0.0199(11) 0.0265(13) C21 0.0182(10) 0.0205(10) 0.0188(10) -0.0026(8) 0.0030(8) -0.0040(8) C22 0.0170(10) 0.0190(10) 0.0206(10) -0.0025(8) 0.0031(8) -0.0005(8) C23 0.0184(10) 0.0219(10) 0.0196(10) 0.0002(8) 0.0031(8) -0.0038(8) C24 0.0250(11) 0.0332(12) 0.0236(11) -0.0043(9) 0.0095(9) 0.0015(9) C25 0.0266(12) 0.0391(13) 0.0283(12) -0.0013(10) 0.0052(10) 0.0131(10) C26 0.0271(12) 0.0341(13) 0.0205(11) 0.0009(9) 0.0004(9) 0.0053(10) C27 0.0198(11) 0.0292(12) 0.0185(10) 0.0005(9) 0.0047(8) -0.0036(9) C28 0.0257(11) 0.0236(11) 0.0102(9) 0.0019(8) 0.0093(8) 0.0026(8) C29 0.0226(11) 0.0324(12) 0.0189(10) 0.0049(9) 0.0068(9) -0.0030(9) C30 0.0246(11) 0.0253(11) 0.0082(9) 0.0000(8) 0.0048(8) -0.0009(9) N1 0.0279(10) 0.0213(9) 0.0123(8) -0.0019(7) 0.0040(7) 0.0011(7) N2 0.0330(10) 0.0257(9) 0.0132(8) -0.0019(7) 0.0111(7) -0.0030(8) N3 0.0290(10) 0.0214(9) 0.0127(8) 0.0002(7) 0.0092(7) -0.0003(7) N4 0.0281(10) 0.0256(9) 0.0148(8) 0.0007(7) 0.0048(7) -0.0016(8) O1 0.0235(8) 0.0220(8) 0.0254(8) 0.0004(6) 0.0024(6) -0.0020(6) O2 0.0248(8) 0.0254(8) 0.0216(7) 0.0071(6) 0.0072(6) 0.0022(6) O3 0.0231(8) 0.0237(8) 0.0182(7) -0.0005(6) 0.0007(6) -0.0006(6) O4 0.0426(10) 0.0281(9) 0.0192(8) 0.0051(6) 0.0083(7) 0.0164(7) _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 2.0323(15) . ? Co1 O4 2.0327(15) 3_666 ? Co1 O1 2.1215(15) 4_666 ? Co1 N1 2.1502(17) . ? Co1 N4 2.1730(17) 1_554 ? Co1 O2 2.2654(15) 4_666 ? C1 N1 1.339(3) . ? C1 C2 1.377(3) . ? C2 C3 1.386(3) . ? C3 C4 1.385(3) . ? C3 C6 1.506(3) . ? C4 C5 1.379(3) . ? C5 N1 1.333(3) . ? C6 N2 1.465(3) . ? C7 N2 1.459(3) . ? C7 C9 1.504(3) . ? C8 N2 1.461(3) . ? C8 C10 1.515(3) . ? C9 N3 1.466(2) . ? C10 N3 1.461(3) . ? C11 N3 1.459(3) . ? C11 C14 1.507(3) . ? C12 N4 1.326(3) . ? C12 C13 1.379(3) . ? C13 C14 1.359(3) . ? C14 C15 1.362(3) . ? C15 C16 1.382(3) . ? C16 N4 1.318(3) . ? C21 C22 1.388(3) . ? C21 C26 1.392(3) . ? C21 C27 1.515(3) . ? C22 C23 1.393(3) . ? C23 C24 1.386(3) . ? C23 C29 1.512(3) . ? C24 C25 1.394(3) . ? C25 C26 1.377(3) . ? C27 C28 1.524(3) . ? C28 O4 1.253(2) . ? C28 O3 1.257(2) . ? C29 C30 1.518(3) . ? C30 O2 1.250(2) . ? C30 O1 1.260(2) . ? C30 Co1 2.516(2) 4_565 ? N4 Co1 2.1730(17) 1_556 ? O1 Co1 2.1215(15) 4_565 ? O2 Co1 2.2654(15) 4_565 ? O4 Co1 2.0327(15) 3_666 ? 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 O4 117.13(7) . 3_666 ? O3 Co1 O1 147.22(6) . 4_666 ? O4 Co1 O1 95.64(6) 3_666 4_666 ? O3 Co1 N1 91.20(6) . . ? O4 Co1 N1 87.95(6) 3_666 . ? O1 Co1 N1 89.26(6) 4_666 . ? O3 Co1 N4 91.07(6) . 1_554 ? O4 Co1 N4 91.34(6) 3_666 1_554 ? O1 Co1 N4 88.64(6) 4_666 1_554 ? N1 Co1 N4 177.70(7) . 1_554 ? O3 Co1 O2 87.56(6) . 4_666 ? O4 Co1 O2 154.90(6) 3_666 4_666 ? O1 Co1 O2 59.73(6) 4_666 4_666 ? N1 Co1 O2 87.00(6) . 4_666 ? N4 Co1 O2 92.73(6) 1_554 4_666 ? N1 C1 C2 123.46(19) . . ? C1 C2 C3 120.0(2) . . ? C4 C3 C2 116.68(19) . . ? C4 C3 C6 124.06(19) . . ? C2 C3 C6 119.25(19) . . ? C5 C4 C3 119.5(2) . . ? N1 C5 C4 124.1(2) . . ? N2 C6 C3 115.40(18) . . ? N2 C7 C9 110.02(17) . . ? N2 C8 C10 111.19(19) . . ? N3 C9 C7 110.71(17) . . ? N3 C10 C8 110.26(18) . . ? N3 C11 C14 113.96(18) . . ? N4 C12 C13 124.1(2) . . ? C14 C13 C12 120.3(2) . . ? C13 C14 C15 116.4(2) . . ? C13 C14 C11 122.8(2) . . ? C15 C14 C11 120.8(2) . . ? C14 C15 C16 119.9(2) . . ? N4 C16 C15 124.5(2) . . ? C22 C21 C26 118.27(19) . . ? C22 C21 C27 120.57(18) . . ? C26 C21 C27 121.15(18) . . ? C21 C22 C23 121.88(19) . . ? C24 C23 C22 118.58(19) . . ? C24 C23 C29 121.49(19) . . ? C22 C23 C29 119.92(18) . . ? C23 C24 C25 120.4(2) . . ? C26 C25 C24 120.0(2) . . ? C25 C26 C21 120.9(2) . . ? C21 C27 C28 110.78(16) . . ? O4 C28 O3 125.70(19) . . ? O4 C28 C27 117.46(18) . . ? O3 C28 C27 116.84(18) . . ? C23 C29 C30 113.00(17) . . ? O2 C30 O1 121.30(19) . . ? O2 C30 C29 120.52(18) . . ? O1 C30 C29 118.16(18) . . ? O2 C30 Co1 63.95(11) . 4_565 ? O1 C30 Co1 57.37(10) . 4_565 ? C29 C30 Co1 175.53(15) . 4_565 ? C5 N1 C1 116.17(18) . . ? C5 N1 Co1 122.63(15) . . ? C1 N1 Co1 121.09(13) . . ? C7 N2 C8 108.03(16) . . ? C7 N2 C6 111.60(17) . . ? C8 N2 C6 109.69(17) . . ? C11 N3 C10 111.41(17) . . ? C11 N3 C9 109.40(16) . . ? C10 N3 C9 108.77(16) . . ? C16 N4 C12 114.9(2) . . ? C16 N4 Co1 123.73(15) . 1_556 ? C12 N4 Co1 121.22(16) . 1_556 ? C30 O1 Co1 92.62(12) . 4_565 ? C30 O2 Co1 86.33(12) . 4_565 ? C28 O3 Co1 130.59(14) . . ? C28 O4 Co1 156.15(14) . 3_666 ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.460 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.065 # Attachment '0co14phda4bpmpfinal.cif' data_twin5 _database_code_depnum_ccdc_archive 'CCDC 752667' #TrackingRef '0co14phda4bpmpfinal.cif' _audit_update_record ; 2009-10-19 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 Co N4 O8' _chemical_formula_weight 587.49 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.6877(10) _cell_length_b 10.5913(18) _cell_length_c 12.901(2) _cell_angle_alpha 87.320(3) _cell_angle_beta 79.649(3) _cell_angle_gamma 81.610(3) _cell_volume 756.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15050 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 26.26 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 307 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7593 _exptl_absorpt_correction_T_max 0.9494 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15050 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.26 _reflns_number_total 5032 _reflns_number_gt 4673 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.1200P)^2^+0.9895P] 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 5032 _refine_ls_number_parameters 188 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1863 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _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 0.0000 1.0000 0.5000 0.01671(19) Uani 1 2 d S . . O1 O 0.2171(4) 0.8708(2) 0.58558(18) 0.0208(5) Uani 1 1 d . . . O2 O -0.0619(5) 0.7691(3) 0.6860(2) 0.0374(7) Uani 1 1 d . . . O3 O 0.3230(4) 1.0596(2) 0.4138(2) 0.0258(5) Uani 1 1 d D . . H3A H 0.453(5) 1.092(3) 0.421(3) 0.031 Uiso 1 1 d D . . H3B H 0.254(6) 1.122(3) 0.373(3) 0.031 Uiso 1 1 d D . . N1 N 0.0365(5) 0.8605(3) 0.3816(2) 0.0230(6) Uani 1 1 d . . . N2 N 0.3484(6) 0.5277(3) 0.0996(3) 0.0331(7) Uani 1 1 d . . . C1 C 0.2364(7) 0.7732(4) 0.3643(3) 0.0304(9) Uani 1 1 d . . . H1 H 0.3619 0.7793 0.4027 0.036 Uiso 1 1 calc R . . C2 C 0.2684(7) 0.6755(4) 0.2940(3) 0.0304(8) Uani 1 1 d . . . H2 H 0.4146 0.6177 0.2842 0.036 Uiso 1 1 calc R . . C3 C 0.0919(7) 0.6612(4) 0.2383(3) 0.0312(8) Uani 1 1 d . . . C4 C -0.1139(8) 0.7490(5) 0.2560(4) 0.0562(15) Uani 1 1 d . . . H4 H -0.2423 0.7428 0.2194 0.067 Uiso 1 1 calc R . . C5 C -0.1359(7) 0.8465(5) 0.3265(4) 0.0454(11) Uani 1 1 d . . . C6 C 0.1147(8) 0.5475(4) 0.1703(4) 0.0466(12) Uani 1 1 d . . . H6 H -0.0076 0.4946 0.1728 0.056 Uiso 1 1 calc R . . C7 C 0.3645(7) 0.6224(4) 0.0149(3) 0.0382(10) Uani 1 1 d . . . H7A H 0.3378 0.7087 0.0449 0.046 Uiso 1 1 calc R . . H7B H 0.2370 0.6174 -0.0272 0.046 Uiso 1 1 calc R . . C8 C 0.3904(7) 0.3989(4) 0.0557(3) 0.0374(9) Uani 1 1 d . . . H8A H 0.2630 0.3896 0.0145 0.045 Uiso 1 1 calc R . . H8B H 0.3832 0.3342 0.1136 0.045 Uiso 1 1 calc R . . C11 C 0.1521(6) 0.7821(3) 0.6481(3) 0.0218(7) Uani 1 1 d . . . C12 C 0.3516(7) 0.6781(3) 0.6745(3) 0.0288(8) Uani 1 1 d . . . H12A H 0.4913 0.7178 0.6867 0.035 Uiso 1 1 calc R . . H12B H 0.2909 0.6313 0.7398 0.035 Uiso 1 1 calc R . . C13 C 0.4300(6) 0.5861(3) 0.5839(3) 0.0268(7) Uani 1 1 d . . . C14 C 0.2760(6) 0.5038(3) 0.5623(3) 0.0290(8) Uani 1 1 d . . . H14 H 0.1204 0.5060 0.6045 0.035 Uiso 1 1 calc R . . C15 C 0.6550(6) 0.5812(3) 0.5197(3) 0.0307(9) Uani 1 1 d . . . H15 H 0.7630 0.6370 0.5321 0.037 Uiso 1 1 calc R . . O1W O 0.169(11) 1.009(2) 0.054(3) 0.30(4) Uiso 0.25 1 d P A 1 O1WA O 0.358(16) 1.0522(14) 0.069(2) 0.35(5) Uiso 0.25 1 d P B 2 O1WB O 0.382(15) 0.9896(19) -0.0539(16) 0.37(5) Uiso 0.25 1 d P C 3 O1WC O 0.508(14) 0.990(3) -0.102(2) 0.31(4) Uiso 0.25 1 d P D 4 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 0.0137(3) 0.0155(3) 0.0200(3) -0.0035(3) -0.0020(3) 0.0008(2) O1 0.0175(12) 0.0182(11) 0.0259(12) -0.0002(9) -0.0048(9) 0.0009(9) O2 0.0231(15) 0.0406(16) 0.0478(17) 0.0170(13) -0.0075(12) -0.0064(12) O3 0.0161(13) 0.0293(13) 0.0320(14) 0.0042(10) -0.0045(10) -0.0048(10) N1 0.0197(15) 0.0235(15) 0.0249(15) -0.0053(12) -0.0045(11) 0.0022(11) N2 0.0319(18) 0.0356(18) 0.0292(17) -0.0170(13) -0.0004(13) 0.0031(14) C1 0.031(2) 0.033(2) 0.0269(19) -0.0109(15) -0.0109(15) 0.0092(16) C2 0.035(2) 0.0238(17) 0.0280(18) -0.0044(14) -0.0057(15) 0.0115(15) C3 0.030(2) 0.033(2) 0.0285(19) -0.0122(16) 0.0025(15) -0.0028(16) C4 0.030(2) 0.076(4) 0.066(3) -0.046(3) -0.019(2) 0.013(2) C5 0.028(2) 0.059(3) 0.051(3) -0.030(2) -0.0148(18) 0.0113(19) C6 0.036(2) 0.051(3) 0.050(3) -0.033(2) 0.0123(19) -0.010(2) C7 0.037(2) 0.037(2) 0.037(2) -0.0167(17) -0.0072(17) 0.0105(18) C8 0.039(2) 0.035(2) 0.036(2) -0.0172(17) -0.0032(17) 0.0003(17) C11 0.0228(19) 0.0206(17) 0.0235(18) -0.0013(13) -0.0093(13) -0.0018(14) C12 0.029(2) 0.0227(17) 0.038(2) 0.0057(15) -0.0161(16) -0.0016(15) C13 0.0242(18) 0.0161(15) 0.042(2) 0.0037(14) -0.0158(15) 0.0020(14) C14 0.0201(18) 0.0198(17) 0.047(2) 0.0035(15) -0.0088(15) -0.0005(14) C15 0.0228(18) 0.0167(15) 0.056(3) 0.0026(15) -0.0168(17) -0.0031(13) _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 O1 2.115(2) . ? Co1 O1 2.115(2) 2_576 ? Co1 O3 2.133(2) . ? Co1 O3 2.133(2) 2_576 ? Co1 N1 2.137(3) . ? Co1 N1 2.137(3) 2_576 ? O1 C11 1.262(4) . ? O2 C11 1.252(4) . ? O3 H3A 0.882(18) . ? O3 H3B 0.911(18) . ? N1 C5 1.339(5) . ? N1 C1 1.349(4) . ? N2 C7 1.448(6) . ? N2 C6 1.464(5) . ? N2 C8 1.472(5) . ? C1 C2 1.379(5) . ? C1 H1 0.9500 . ? C2 C3 1.364(6) . ? C2 H2 0.9500 . ? C3 C4 1.376(5) . ? C3 C6 1.500(5) . ? C4 C5 1.385(6) . ? C4 H4 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.515(6) 2_665 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C7 1.515(6) 2_665 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C11 C12 1.535(5) . ? C12 C13 1.519(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.389(5) . ? C13 C14 1.392(5) . ? C14 C15 1.385(5) 2_666 ? C14 H14 0.9500 . ? C15 C14 1.385(5) 2_666 ? C15 H15 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 O1 180.000(1) . 2_576 ? O1 Co1 O3 88.15(9) . . ? O1 Co1 O3 91.85(9) 2_576 . ? O1 Co1 O3 91.85(9) . 2_576 ? O1 Co1 O3 88.15(9) 2_576 2_576 ? O3 Co1 O3 180.00(7) . 2_576 ? O1 Co1 N1 89.91(10) . . ? O1 Co1 N1 90.08(10) 2_576 . ? O3 Co1 N1 86.77(11) . . ? O3 Co1 N1 93.23(11) 2_576 . ? O1 Co1 N1 90.09(10) . 2_576 ? O1 Co1 N1 89.91(10) 2_576 2_576 ? O3 Co1 N1 93.23(11) . 2_576 ? O3 Co1 N1 86.77(11) 2_576 2_576 ? N1 Co1 N1 180.000(1) . 2_576 ? C11 O1 Co1 127.6(2) . . ? Co1 O3 H3A 143(3) . . ? Co1 O3 H3B 98(3) . . ? H3A O3 H3B 100(3) . . ? C5 N1 C1 115.8(3) . . ? C5 N1 Co1 124.3(2) . . ? C1 N1 Co1 119.8(2) . . ? C7 N2 C6 111.9(3) . . ? C7 N2 C8 109.8(3) . . ? C6 N2 C8 110.0(3) . . ? N1 C1 C2 123.6(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 116.5(4) . . ? C2 C3 C6 120.7(4) . . ? C4 C3 C6 122.6(4) . . ? C3 C4 C5 120.8(4) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 122.9(4) . . ? N2 C6 C3 111.8(3) . . ? N2 C6 H6 124.1 . . ? C3 C6 H6 124.1 . . ? N2 C7 C8 110.7(3) . 2_665 ? N2 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 2_665 . ? N2 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 2_665 . ? H7A C7 H7B 108.1 . . ? N2 C8 C7 109.8(3) . 2_665 ? N2 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 2_665 . ? N2 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 2_665 . ? H8A C8 H8B 108.2 . . ? O2 C11 O1 125.3(3) . . ? O2 C11 C12 117.6(3) . . ? O1 C11 C12 117.0(3) . . ? C13 C12 C11 109.6(3) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C15 C13 C14 117.7(4) . . ? C15 C13 C12 121.7(3) . . ? C14 C13 C12 120.6(3) . . ? C15 C14 C13 121.3(4) 2_666 . ? C15 C14 H14 119.3 2_666 . ? C13 C14 H14 119.3 . . ? C14 C15 C13 121.0(3) 2_666 . ? C14 C15 H15 119.5 2_666 . ? C13 C15 H15 119.5 . . ? 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 O1 Co1 O1 C11 -140(100) 2_576 . . . ? O3 Co1 O1 C11 -169.5(3) . . . . ? O3 Co1 O1 C11 10.5(3) 2_576 . . . ? N1 Co1 O1 C11 -82.7(3) . . . . ? N1 Co1 O1 C11 97.3(3) 2_576 . . . ? O1 Co1 N1 C5 146.1(4) . . . . ? O1 Co1 N1 C5 -33.9(4) 2_576 . . . ? O3 Co1 N1 C5 -125.8(4) . . . . ? O3 Co1 N1 C5 54.2(4) 2_576 . . . ? N1 Co1 N1 C5 -74(33) 2_576 . . . ? O1 Co1 N1 C1 -28.8(3) . . . . ? O1 Co1 N1 C1 151.2(3) 2_576 . . . ? O3 Co1 N1 C1 59.4(3) . . . . ? O3 Co1 N1 C1 -120.6(3) 2_576 . . . ? N1 Co1 N1 C1 111(33) 2_576 . . . ? C5 N1 C1 C2 0.8(6) . . . . ? Co1 N1 C1 C2 176.1(3) . . . . ? N1 C1 C2 C3 -1.1(6) . . . . ? C1 C2 C3 C4 0.5(6) . . . . ? C1 C2 C3 C6 -173.6(4) . . . . ? C2 C3 C4 C5 0.4(8) . . . . ? C6 C3 C4 C5 174.3(5) . . . . ? C1 N1 C5 C4 0.1(7) . . . . ? Co1 N1 C5 C4 -174.9(4) . . . . ? C3 C4 C5 N1 -0.7(9) . . . . ? C7 N2 C6 C3 -72.7(5) . . . . ? C8 N2 C6 C3 164.9(4) . . . . ? C2 C3 C6 N2 -50.2(6) . . . . ? C4 C3 C6 N2 136.0(5) . . . . ? C6 N2 C7 C8 178.9(3) . . . 2_665 ? C8 N2 C7 C8 -58.6(5) . . . 2_665 ? C7 N2 C8 C7 58.0(5) . . . 2_665 ? C6 N2 C8 C7 -178.4(4) . . . 2_665 ? Co1 O1 C11 O2 -14.1(5) . . . . ? Co1 O1 C11 C12 162.3(2) . . . . ? O2 C11 C12 C13 98.7(4) . . . . ? O1 C11 C12 C13 -78.0(4) . . . . ? C11 C12 C13 C15 110.1(4) . . . . ? C11 C12 C13 C14 -69.5(4) . . . . ? C15 C13 C14 C15 0.8(6) . . . 2_666 ? C12 C13 C14 C15 -179.6(3) . . . 2_666 ? C14 C13 C15 C14 -0.8(6) . . . 2_666 ? C12 C13 C15 C14 179.6(3) . . . 2_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O1 0.882(18) 1.96(2) 2.820(3) 166(4) 2_676 O3 H3B O2 0.911(18) 1.72(2) 2.615(4) 166(4) 2_576 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.963 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.145 # Attachment '0co12phda4bpmpfinal.cif' data_c2c _database_code_depnum_ccdc_archive 'CCDC 752668' #TrackingRef '0co12phda4bpmpfinal.cif' # start Validation Reply Form _vrf_CHEMW03_c2c ; PROBLEM: _The ratio of given/expected molecular weight as calculated from the _atom_site*(or type) data lies outside the range 0.90 <> 1.10 RESPONSE: Solvent atom electron density accounted for using SQUEEZE ; # end Validation Reply Form # start Validation Reply Form _vrf_PLAT306_c2c ; PROBLEM: _Isolated Oxygen Atom (H-atoms Missing ?) RESPONSE: Solvent atom electron density accounted for using SQUEEZE ; # end Validation Reply Form # start Validation Reply Form _vrf_PLAT043_c2c ; PROBLEM: _Check Reported Molecular Weight RESPONSE: Solvent atom electron density accounted for using SQUEEZE ; # end Validation Reply Form _audit_update_record ; 2009-10-19 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H75 Cl Co N8 O21' _chemical_formula_weight 1122.47 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 33.323(2) _cell_length_b 9.3186(6) _cell_length_c 37.814(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.8500(10) _cell_angle_gamma 90.00 _cell_volume 11238.0(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10313 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 25.38 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3816 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8469 _exptl_absorpt_correction_T_max 0.9585 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10313 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.38 _reflns_number_total 10313 _reflns_number_gt 6614 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.1397P)^2^+67.6513P] 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 10313 _refine_ls_number_parameters 603 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.3048 _refine_ls_wR_factor_gt 0.2909 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.90103(2) 0.03022(10) 0.17084(2) 0.0404(3) Uani 1 1 d . . . Cl1 Cl 0.85748(7) 0.1251(3) 0.41758(7) 0.0806(7) Uani 1 1 d . . . O2 O 0.89781(13) 0.2464(5) 0.18120(11) 0.0423(10) Uani 1 1 d . C . O3 O 0.90252(12) 0.8108(5) 0.15993(12) 0.0425(10) Uani 1 1 d . . . O5 O 0.96882(13) 0.0245(5) 0.18277(12) 0.0507(11) Uani 1 1 d . . . O6 O 0.8881(4) 0.0170(10) 0.4338(3) 0.157(4) Uani 1 1 d . B . N1 N 0.90067(16) -0.0216(6) 0.22663(15) 0.0457(13) Uani 1 1 d . . . N2 N 0.87975(18) -0.2314(6) 0.34424(15) 0.0501(14) Uani 1 1 d . . . N3 N 0.82186(15) -0.3789(6) 0.37564(14) 0.0425(13) Uani 1 1 d . . . N4 N 0.66610(16) -0.4830(6) 0.34807(15) 0.0452(13) Uani 1 1 d . . . N5 N 0.90245(15) 0.0798(6) 0.11548(14) 0.0395(12) Uani 1 1 d . . . N6 N 0.97274(17) 0.0841(6) 0.01441(14) 0.0477(14) Uani 1 1 d . . . N7 N 0.84042(17) -0.3398(6) 0.48695(16) 0.0469(13) Uani 1 1 d D . . H7N H 0.848(2) -0.427(4) 0.4810(19) 0.056 Uiso 1 1 d D . . N8 N 0.75666(14) 0.0986(5) 0.50543(14) 0.0355(11) Uani 1 1 d . . . C1 C 0.8705(2) 0.5472(6) 0.13732(18) 0.0454(16) Uani 1 1 d . . . C2 C 0.8431(2) 0.5695(8) 0.10274(19) 0.0552(18) Uani 1 1 d . . . H2 H 0.8539 0.5975 0.0831 0.066 Uiso 1 1 calc R . . C3 C 0.8008(3) 0.5525(7) 0.0959(2) 0.061(2) Uani 1 1 d . . . H3 H 0.7827 0.5651 0.0716 0.073 Uiso 1 1 calc R . . C4 C 0.7845(2) 0.5182(8) 0.1235(3) 0.063(2) Uani 1 1 d . . . H4 H 0.7550 0.5125 0.1189 0.075 Uiso 1 1 calc R . . C5 C 0.8113(2) 0.4907(7) 0.1591(2) 0.059(2) Uani 1 1 d . . . H5 H 0.7998 0.4639 0.1784 0.071 Uiso 1 1 calc R . . C6 C 0.85442(19) 0.5025(6) 0.16629(19) 0.0458(16) Uani 1 1 d . . . C7 C 0.9166(2) 0.5726(9) 0.1433(2) 0.0575(19) Uani 1 1 d . A . H7A H 0.9230 0.5601 0.1195 0.069 Uiso 1 1 calc R . . H7B H 0.9328 0.5000 0.1608 0.069 Uiso 1 1 calc R . . C8 C 0.93061(19) 0.7242(9) 0.1586(2) 0.061(2) Uani 1 1 d . . . C9 C 0.8836(3) 0.4736(8) 0.20405(19) 0.061(2) Uani 1 1 d . C . H9A H 0.8670 0.4699 0.2219 0.073 Uiso 1 1 calc R . . H9B H 0.9034 0.5549 0.2112 0.073 Uiso 1 1 calc R . . C10 C 0.9085(2) 0.3358(8) 0.20720(18) 0.0546(19) Uani 1 1 d . . . C11 C 0.8751(3) 0.0463(9) 0.2425(2) 0.065(2) Uani 1 1 d . . . H11 H 0.8567 0.1166 0.2283 0.078 Uiso 1 1 calc R . . C12 C 0.8734(2) 0.0220(8) 0.2776(2) 0.0564(18) Uani 1 1 d . . . H12 H 0.8533 0.0698 0.2867 0.068 Uiso 1 1 calc R . . C13 C 0.9009(2) -0.0714(7) 0.29909(19) 0.0470(16) Uani 1 1 d . . . C14 C 0.9278(2) -0.1478(7) 0.2825(2) 0.0518(17) Uani 1 1 d . . . H14 H 0.9467 -0.2186 0.2960 0.062 Uiso 1 1 calc R . . C15 C 0.9258(2) -0.1166(7) 0.24689(18) 0.0435(15) Uani 1 1 d . . . H15 H 0.9440 -0.1674 0.2360 0.052 Uiso 1 1 calc R . . C16 C 0.9033(2) -0.1021(7) 0.3386(2) 0.0544(18) Uani 1 1 d . . . H16A H 0.9332 -0.1143 0.3528 0.065 Uiso 1 1 calc R . . H16B H 0.8925 -0.0178 0.3488 0.065 Uiso 1 1 calc R . . C17 C 0.8333(2) -0.2112(8) 0.32946(19) 0.0503(17) Uani 1 1 d . . . H17A H 0.8257 -0.1914 0.3026 0.060 Uiso 1 1 calc R . . H17B H 0.8246 -0.1277 0.3417 0.060 Uiso 1 1 calc R . . C18 C 0.8105(2) -0.3431(8) 0.3362(2) 0.0564(19) Uani 1 1 d . . . H18A H 0.7799 -0.3268 0.3268 0.068 Uiso 1 1 calc R . . H18B H 0.8176 -0.4248 0.3223 0.068 Uiso 1 1 calc R . . C19 C 0.89031(19) -0.2698(8) 0.3845(2) 0.0543(19) Uani 1 1 d . . . H19A H 0.8828 -0.1890 0.3983 0.065 Uiso 1 1 calc R . . H19B H 0.9209 -0.2863 0.3943 0.065 Uiso 1 1 calc R . . C20 C 0.8672(2) -0.4026(8) 0.3900(2) 0.0563(19) Uani 1 1 d . . . H20A H 0.8754 -0.4846 0.3770 0.068 Uiso 1 1 calc R . . H20B H 0.8746 -0.4262 0.4166 0.068 Uiso 1 1 calc R . . C21 C 0.8008(2) -0.5109(8) 0.3826(2) 0.059(2) Uani 1 1 d . . . H21A H 0.8100 -0.5321 0.4094 0.070 Uiso 1 1 calc R . . H21B H 0.8095 -0.5920 0.3696 0.070 Uiso 1 1 calc R . . C22 C 0.6897(2) -0.3705(8) 0.36272(18) 0.0486(16) Uani 1 1 d . . . H22 H 0.6762 -0.2830 0.3653 0.058 Uiso 1 1 calc R . . C23 C 0.7322(2) -0.3756(8) 0.37408(19) 0.0535(18) Uani 1 1 d . . . H23 H 0.7477 -0.2935 0.3851 0.064 Uiso 1 1 calc R . . C24 C 0.7529(2) -0.4993(8) 0.3697(2) 0.0519(18) Uani 1 1 d . . . C25 C 0.7291(2) -0.6124(8) 0.3558(2) 0.061(2) Uani 1 1 d . . . H25 H 0.7424 -0.7012 0.3540 0.073 Uiso 1 1 calc R . . C26 C 0.6859(2) -0.6058(8) 0.3437(2) 0.0590(19) Uani 1 1 d . . . H26 H 0.6701 -0.6870 0.3324 0.071 Uiso 1 1 calc R . . C31 C 0.92209(19) 0.2004(8) 0.10954(18) 0.0479(16) Uani 1 1 d . . . H31 H 0.9296 0.2711 0.1284 0.058 Uiso 1 1 calc R . . C32 C 0.93161(19) 0.2235(7) 0.07673(18) 0.0442(15) Uani 1 1 d . . . H32 H 0.9463 0.3074 0.0735 0.053 Uiso 1 1 calc R . . C33 C 0.91944(18) 0.1231(7) 0.04877(16) 0.0401(15) Uani 1 1 d . . . C34 C 0.89776(18) 0.0053(6) 0.05410(17) 0.0374(14) Uani 1 1 d . . . H34 H 0.8885 -0.0644 0.0352 0.045 Uiso 1 1 calc R . . C35 C 0.88956(18) -0.0105(7) 0.08757(16) 0.0393(14) Uani 1 1 d . . . H35 H 0.8736 -0.0915 0.0908 0.047 Uiso 1 1 calc R . . C36 C 0.93001(19) 0.1458(8) 0.01210(19) 0.0515(18) Uani 1 1 d . . . H36A H 0.9085 0.0986 -0.0082 0.062 Uiso 1 1 calc R . . H36B H 0.9298 0.2497 0.0066 0.062 Uiso 1 1 calc R . . C37 C 0.9732(2) -0.0707(7) 0.01796(19) 0.0461(16) Uani 1 1 d . . . H37A H 0.9517 -0.1129 -0.0033 0.055 Uiso 1 1 calc R . . H37B H 0.9663 -0.0977 0.0408 0.055 Uiso 1 1 calc R . . C38 C 1.0159(2) -0.1305(8) 0.01922(19) 0.0560(19) Uani 1 1 d . . . H38A H 1.0372 -0.0953 0.0416 0.067 Uiso 1 1 calc R . . H38B H 1.0154 -0.2366 0.0203 0.067 Uiso 1 1 calc R . . C41 C 0.83684(19) -0.3441(7) 0.52179(19) 0.0455(16) Uani 1 1 d . . . H41 H 0.8511 -0.4188 0.5376 0.055 Uiso 1 1 calc R . . C42 C 0.81464(19) -0.2505(7) 0.53542(17) 0.0405(14) Uani 1 1 d . . . H42 H 0.8124 -0.2610 0.5598 0.049 Uiso 1 1 calc R . . C43 C 0.79473(17) -0.1364(6) 0.51281(17) 0.0374(14) Uani 1 1 d . . . C44 C 0.79761(18) -0.1310(7) 0.47743(16) 0.0413(15) Uani 1 1 d . . . H44 H 0.7835 -0.0575 0.4611 0.050 Uiso 1 1 calc R . . C45 C 0.8208(2) -0.2309(7) 0.46556(18) 0.0431(15) Uani 1 1 d . . . H45 H 0.8231 -0.2230 0.4412 0.052 Uiso 1 1 calc R . . C46 C 0.7704(2) -0.0311(7) 0.52845(18) 0.0452(15) Uani 1 1 d . . . H46A H 0.7454 -0.0800 0.5317 0.054 Uiso 1 1 calc R . . H46B H 0.7880 -0.0008 0.5532 0.054 Uiso 1 1 calc R . . C47 C 0.79123(17) 0.1956(7) 0.50738(18) 0.0414(15) Uani 1 1 d . . . H47A H 0.8130 0.1455 0.4990 0.050 Uiso 1 1 calc R . . H47B H 0.8039 0.2262 0.5333 0.050 Uiso 1 1 calc R . . C48 C 0.77600(16) 0.3263(6) 0.48330(17) 0.0353(13) Uani 1 1 d . . . H48A H 0.7998 0.3921 0.4852 0.042 Uiso 1 1 calc R . . H48B H 0.7649 0.2959 0.4572 0.042 Uiso 1 1 calc R . . O4 O 0.9682(4) 0.7226(15) 0.1769(4) 0.057(3) Uani 0.50 1 d P A 1 O7 O 0.8272(4) 0.030(2) 0.3981(6) 0.112(6) Uani 0.50 1 d P B 1 O8 O 0.8797(4) 0.241(3) 0.4099(8) 0.140(12) Uani 0.50 1 d P B 1 O9 O 0.8441(16) 0.151(2) 0.4456(14) 0.35(3) Uani 0.50 1 d P B 1 O1 O 0.9400(10) 0.322(2) 0.2344(8) 0.056(5) Uani 0.50 1 d P C 1 O4A O 0.9680(4) 0.7750(16) 0.1577(4) 0.065(4) Uani 0.50 1 d P A 2 O7A O 0.8297(15) 0.097(3) 0.3785(9) 0.27(2) Uani 0.50 1 d P B 2 O8A O 0.8772(13) 0.199(4) 0.4006(13) 0.28(3) Uani 0.50 1 d P B 2 O9A O 0.8357(8) 0.2142(15) 0.4375(6) 0.124(7) Uani 0.50 1 d P B 2 O1A O 0.9334(13) 0.311(4) 0.2411(10) 0.115(16) Uani 0.50 1 d P C 2 O1W O 1.0000 0.1328(10) 0.2500 0.091(3) Uani 1 2 d S . . 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 0.0330(4) 0.0478(5) 0.0397(5) -0.0020(4) 0.0097(3) 0.0066(4) Cl1 0.0760(14) 0.0791(16) 0.1011(18) -0.0120(13) 0.0487(14) -0.0190(12) O2 0.046(2) 0.041(2) 0.035(2) -0.0011(19) 0.0044(18) 0.0166(19) O3 0.036(2) 0.040(2) 0.051(3) -0.007(2) 0.0114(19) -0.0007(19) O5 0.035(2) 0.066(3) 0.046(3) -0.006(2) 0.0044(19) 0.002(2) O6 0.209(11) 0.105(7) 0.145(8) 0.013(6) 0.031(7) 0.052(7) N1 0.041(3) 0.048(3) 0.051(3) -0.005(3) 0.018(2) 0.005(3) N2 0.058(3) 0.048(3) 0.050(3) 0.014(3) 0.025(3) -0.010(3) N3 0.032(3) 0.053(3) 0.042(3) 0.013(2) 0.010(2) -0.003(2) N4 0.043(3) 0.043(3) 0.056(3) 0.005(3) 0.024(3) -0.007(3) N5 0.030(3) 0.042(3) 0.046(3) -0.004(2) 0.011(2) 0.003(2) N6 0.046(3) 0.062(4) 0.041(3) 0.015(3) 0.021(2) 0.021(3) N7 0.041(3) 0.041(3) 0.057(4) 0.002(3) 0.012(3) 0.000(3) N8 0.029(2) 0.028(2) 0.049(3) 0.002(2) 0.012(2) -0.002(2) C1 0.054(4) 0.023(3) 0.052(4) -0.013(3) 0.004(3) 0.011(3) C2 0.060(5) 0.052(4) 0.042(4) -0.010(3) -0.003(3) -0.005(3) C3 0.074(5) 0.020(3) 0.066(5) -0.002(3) -0.018(4) 0.005(3) C4 0.031(3) 0.049(4) 0.094(6) -0.005(4) -0.006(4) -0.001(3) C5 0.064(5) 0.032(4) 0.085(6) 0.005(3) 0.028(4) 0.014(3) C6 0.038(3) 0.030(3) 0.061(4) -0.009(3) 0.001(3) 0.011(3) C7 0.042(4) 0.068(5) 0.057(4) -0.026(4) 0.007(3) 0.000(3) C8 0.026(3) 0.081(5) 0.072(5) -0.039(4) 0.008(3) 0.013(3) C9 0.073(5) 0.059(4) 0.044(4) -0.004(3) 0.006(3) 0.040(4) C10 0.062(5) 0.067(5) 0.032(4) 0.001(3) 0.010(3) 0.027(4) C11 0.072(5) 0.062(5) 0.072(5) 0.012(4) 0.039(4) 0.025(4) C12 0.055(4) 0.057(4) 0.063(5) 0.004(4) 0.026(4) 0.016(4) C13 0.053(4) 0.036(3) 0.058(4) -0.007(3) 0.026(3) -0.010(3) C14 0.059(4) 0.040(4) 0.060(4) 0.008(3) 0.024(4) 0.001(3) C15 0.047(4) 0.032(3) 0.055(4) 0.003(3) 0.021(3) 0.000(3) C16 0.065(5) 0.039(4) 0.061(4) 0.010(3) 0.021(4) -0.004(3) C17 0.055(4) 0.050(4) 0.044(4) 0.012(3) 0.010(3) -0.005(3) C18 0.048(4) 0.063(5) 0.057(4) 0.015(4) 0.014(3) -0.012(3) C19 0.031(3) 0.068(5) 0.063(4) 0.024(4) 0.012(3) -0.007(3) C20 0.046(4) 0.047(4) 0.079(5) 0.037(4) 0.022(4) 0.006(3) C21 0.040(4) 0.063(5) 0.074(5) 0.028(4) 0.018(3) 0.012(3) C22 0.040(4) 0.054(4) 0.050(4) 0.002(3) 0.011(3) 0.001(3) C23 0.039(4) 0.062(5) 0.050(4) 0.005(3) 0.000(3) -0.013(3) C24 0.045(4) 0.053(4) 0.065(4) 0.023(4) 0.028(3) 0.001(3) C25 0.045(4) 0.037(4) 0.106(6) 0.017(4) 0.028(4) -0.002(3) C26 0.043(4) 0.054(5) 0.085(5) -0.006(4) 0.025(4) -0.001(3) C31 0.037(3) 0.057(4) 0.049(4) -0.010(3) 0.013(3) 0.005(3) C32 0.035(3) 0.046(4) 0.054(4) 0.006(3) 0.015(3) 0.011(3) C33 0.039(3) 0.045(4) 0.035(3) 0.001(3) 0.009(3) 0.024(3) C34 0.037(3) 0.023(3) 0.050(4) -0.009(3) 0.009(3) 0.005(2) C35 0.032(3) 0.043(4) 0.043(3) -0.011(3) 0.011(3) 0.000(3) C36 0.035(3) 0.071(5) 0.053(4) 0.009(4) 0.019(3) 0.013(3) C37 0.057(4) 0.041(4) 0.052(4) 0.013(3) 0.034(3) 0.017(3) C38 0.061(4) 0.063(5) 0.052(4) 0.016(3) 0.030(4) 0.028(4) C41 0.036(3) 0.040(4) 0.052(4) 0.006(3) 0.000(3) -0.008(3) C42 0.040(3) 0.038(3) 0.041(3) -0.006(3) 0.007(3) -0.006(3) C43 0.029(3) 0.034(3) 0.047(4) -0.005(3) 0.009(3) -0.011(2) C44 0.036(3) 0.053(4) 0.034(3) 0.002(3) 0.009(3) -0.014(3) C45 0.048(4) 0.036(3) 0.046(4) 0.005(3) 0.016(3) -0.013(3) C46 0.041(3) 0.048(4) 0.047(4) 0.012(3) 0.014(3) -0.011(3) C47 0.025(3) 0.046(4) 0.052(4) -0.009(3) 0.010(3) -0.009(3) C48 0.022(3) 0.030(3) 0.051(4) -0.005(3) 0.006(2) -0.008(2) O4 0.034(6) 0.053(8) 0.077(10) -0.024(6) 0.007(7) 0.004(5) O7 0.056(8) 0.135(17) 0.134(16) -0.028(12) 0.010(9) -0.042(9) O8 0.029(6) 0.086(12) 0.30(3) 0.078(15) 0.046(11) 0.004(7) O9 0.60(7) 0.033(11) 0.67(8) 0.02(2) 0.58(7) 0.01(2) O1 0.063(11) 0.063(9) 0.025(8) -0.021(6) -0.014(8) 0.042(7) O4A 0.036(6) 0.063(9) 0.096(11) -0.036(8) 0.018(8) 0.003(6) O7A 0.42(5) 0.11(2) 0.16(3) -0.017(17) -0.12(3) -0.03(2) O8A 0.39(5) 0.19(3) 0.43(5) 0.18(3) 0.39(5) 0.14(3) O9A 0.232(19) 0.027(8) 0.183(15) 0.006(9) 0.169(15) 0.035(11) O1A 0.085(16) 0.19(3) 0.054(16) -0.002(12) -0.004(11) 0.085(15) O1W 0.085(6) 0.086(6) 0.081(6) 0.000 -0.006(5) 0.000 _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 O2 2.061(4) . ? Co1 O3 2.090(4) 1_545 ? Co1 N4 2.145(5) 4_655 ? Co1 N5 2.158(5) . ? Co1 N1 2.168(5) . ? Co1 O5 2.172(4) . ? Cl1 O8A 1.25(2) . ? Cl1 O9 1.28(3) . ? Cl1 O8 1.382(19) . ? Cl1 O7 1.384(16) . ? Cl1 O6 1.438(9) . ? Cl1 O9A 1.449(14) . ? Cl1 O7A 1.52(2) . ? O2 C10 1.258(8) . ? O3 C8 1.247(7) . ? O3 Co1 2.090(4) 1_565 ? N1 C15 1.305(8) . ? N1 C11 1.334(9) . ? N2 C16 1.487(8) . ? N2 C17 1.499(9) . ? N2 C19 1.501(8) . ? N3 C20 1.465(8) . ? N3 C18 1.468(8) . ? N3 C21 1.477(9) . ? N4 C22 1.331(8) . ? N4 C26 1.354(9) . ? N4 Co1 2.146(5) 4_645 ? N5 C35 1.321(8) . ? N5 C31 1.351(9) . ? N6 C37 1.448(9) . ? N6 C38 1.492(8) 5_755 ? N6 C36 1.514(8) . ? N7 C45 1.344(8) . ? N7 C41 1.358(9) . ? N7 H7N 0.90(2) . ? N8 C47 1.449(7) . ? N8 C48 1.458(7) 7_656 ? N8 C46 1.482(8) . ? C1 C2 1.376(9) . ? C1 C6 1.413(10) . ? C1 C7 1.506(10) . ? C2 C3 1.367(11) . ? C2 H2 0.9500 . ? C3 C4 1.344(12) . ? C3 H3 0.9500 . ? C4 C5 1.408(11) . ? C4 H4 0.9500 . ? C5 C6 1.388(10) . ? C5 H5 0.9500 . ? C6 C9 1.500(9) . ? C7 C8 1.547(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.243(14) . ? C8 O4A 1.342(15) . ? C9 C10 1.516(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O1 1.24(3) . ? C10 O1A 1.33(3) . ? C11 C12 1.364(10) . ? C11 H11 0.9500 . ? C12 C13 1.352(10) . ? C12 H12 0.9500 . ? C13 C14 1.426(9) . ? C13 C16 1.500(10) . ? C14 C15 1.361(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.503(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.505(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C24 1.530(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.355(9) . ? C22 H22 0.9500 . ? C23 C24 1.379(10) . ? C23 H23 0.9500 . ? C24 C25 1.333(10) . ? C25 C26 1.380(10) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.384(9) . ? C31 H31 0.9500 . ? C32 C33 1.381(9) . ? C32 H32 0.9500 . ? C33 C34 1.361(9) . ? C33 C36 1.541(9) . ? C34 C35 1.378(8) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.515(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N6 1.492(8) 5_755 ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C41 C42 1.340(9) . ? C41 H41 0.9500 . ? C42 C43 1.405(9) . ? C42 H42 0.9500 . ? C43 C44 1.370(8) . ? C43 C46 1.498(9) . ? C44 C45 1.366(9) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.517(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 N8 1.458(7) 7_656 ? C48 H48A 0.9900 . ? C48 H48B 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 O2 Co1 O3 178.45(16) . 1_545 ? O2 Co1 N4 90.73(18) . 4_655 ? O3 Co1 N4 87.73(18) 1_545 4_655 ? O2 Co1 N5 89.55(18) . . ? O3 Co1 N5 90.55(18) 1_545 . ? N4 Co1 N5 90.17(19) 4_655 . ? O2 Co1 N1 90.99(19) . . ? O3 Co1 N1 88.94(19) 1_545 . ? N4 Co1 N1 90.7(2) 4_655 . ? N5 Co1 N1 178.98(19) . . ? O2 Co1 O5 95.33(18) . . ? O3 Co1 O5 86.22(17) 1_545 . ? N4 Co1 O5 171.44(18) 4_655 . ? N5 Co1 O5 83.85(17) . . ? N1 Co1 O5 95.23(18) . . ? O8A Cl1 O9 133(2) . . ? O8A Cl1 O8 22(3) . . ? O9 Cl1 O8 111.2(18) . . ? O8A Cl1 O7 119(3) . . ? O9 Cl1 O7 101(2) . . ? O8 Cl1 O7 137.6(15) . . ? O8A Cl1 O6 101.0(17) . . ? O9 Cl1 O6 99(2) . . ? O8 Cl1 O6 106.1(9) . . ? O7 Cl1 O6 95.6(10) . . ? O8A Cl1 O9A 111.6(19) . . ? O9 Cl1 O9A 28.4(17) . . ? O8 Cl1 O9A 92.4(14) . . ? O7 Cl1 O9A 104.1(12) . . ? O6 Cl1 O9A 125.5(10) . . ? O8A Cl1 O7A 82(3) . . ? O9 Cl1 O7A 125(3) . . ? O8 Cl1 O7A 98(2) . . ? O7 Cl1 O7A 39.6(15) . . ? O6 Cl1 O7A 116.9(14) . . ? O9A Cl1 O7A 110(2) . . ? C10 O2 Co1 140.9(4) . . ? C8 O3 Co1 134.6(4) . 1_565 ? C15 N1 C11 116.3(6) . . ? C15 N1 Co1 122.6(4) . . ? C11 N1 Co1 121.1(5) . . ? C16 N2 C17 112.1(5) . . ? C16 N2 C19 111.1(5) . . ? C17 N2 C19 108.7(5) . . ? C20 N3 C18 110.2(5) . . ? C20 N3 C21 107.5(5) . . ? C18 N3 C21 112.0(5) . . ? C22 N4 C26 117.8(6) . . ? C22 N4 Co1 121.8(4) . 4_645 ? C26 N4 Co1 120.3(5) . 4_645 ? C35 N5 C31 117.3(5) . . ? C35 N5 Co1 123.0(4) . . ? C31 N5 Co1 119.2(4) . . ? C37 N6 C38 111.6(5) . 5_755 ? C37 N6 C36 111.7(5) . . ? C38 N6 C36 107.8(5) 5_755 . ? C45 N7 C41 116.2(6) . . ? C45 N7 H7N 131(5) . . ? C41 N7 H7N 109(5) . . ? C47 N8 C48 109.6(5) . 7_656 ? C47 N8 C46 111.9(5) . . ? C48 N8 C46 110.5(5) 7_656 . ? C2 C1 C6 119.1(7) . . ? C2 C1 C7 119.0(7) . . ? C6 C1 C7 121.9(6) . . ? C3 C2 C1 121.7(8) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 120.4(7) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.0(7) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.3(8) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 118.4(6) . . ? C5 C6 C9 121.3(7) . . ? C1 C6 C9 120.3(6) . . ? C1 C7 C8 112.6(5) . . ? C1 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C1 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? O4 C8 O3 129.3(9) . . ? O4 C8 O4A 39.3(7) . . ? O3 C8 O4A 119.0(9) . . ? O4 C8 C7 110.1(8) . . ? O3 C8 C7 117.2(6) . . ? O4A C8 C7 119.6(8) . . ? C6 C9 C10 114.6(6) . . ? C6 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? C6 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? O1 C10 O2 123.8(11) . . ? O1 C10 O1A 17(4) . . ? O2 C10 O1A 126.3(16) . . ? O1 C10 C9 117.8(10) . . ? O2 C10 C9 118.3(6) . . ? O1A C10 C9 113.6(15) . . ? N1 C11 C12 124.8(7) . . ? N1 C11 H11 117.6 . . ? C12 C11 H11 117.6 . . ? C13 C12 C11 118.7(7) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 117.4(6) . . ? C12 C13 C16 123.6(6) . . ? C14 C13 C16 118.9(6) . . ? C15 C14 C13 118.2(6) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? N1 C15 C14 124.4(6) . . ? N1 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? N2 C16 C13 114.8(6) . . ? N2 C16 H16A 108.6 . . ? C13 C16 H16A 108.6 . . ? N2 C16 H16B 108.6 . . ? C13 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? N2 C17 C18 110.6(5) . . ? N2 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N3 C18 C17 111.3(6) . . ? N3 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? N3 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N2 C19 C20 111.0(6) . . ? N2 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N2 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N3 C20 C19 109.8(5) . . ? N3 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? N3 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? N3 C21 C24 113.0(5) . . ? N3 C21 H21A 109.0 . . ? C24 C21 H21A 109.0 . . ? N3 C21 H21B 109.0 . . ? C24 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N4 C22 C23 122.8(7) . . ? N4 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 116.5(6) . . ? C25 C24 C21 121.1(7) . . ? C23 C24 C21 122.2(7) . . ? C24 C25 C26 122.7(7) . . ? C24 C25 H25 118.7 . . ? C26 C25 H25 118.7 . . ? N4 C26 C25 119.7(7) . . ? N4 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? N5 C31 C32 121.8(6) . . ? N5 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C33 C32 C31 119.2(6) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 118.9(6) . . ? C34 C33 C36 120.9(6) . . ? C32 C33 C36 120.2(6) . . ? C33 C34 C35 118.5(5) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? N5 C35 C34 124.1(6) . . ? N5 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? N6 C36 C33 110.6(5) . . ? N6 C36 H36A 109.5 . . ? C33 C36 H36A 109.5 . . ? N6 C36 H36B 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? N6 C37 C38 110.8(6) . . ? N6 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? N6 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? N6 C38 C37 109.5(5) 5_755 . ? N6 C38 H38A 109.8 5_755 . ? C37 C38 H38A 109.8 . . ? N6 C38 H38B 109.8 5_755 . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? C42 C41 N7 124.6(6) . . ? C42 C41 H41 117.7 . . ? N7 C41 H41 117.7 . . ? C41 C42 C43 118.4(6) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C44 C43 C42 117.9(6) . . ? C44 C43 C46 124.1(6) . . ? C42 C43 C46 118.0(6) . . ? C45 C44 C43 120.2(6) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? N7 C45 C44 122.7(6) . . ? N7 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? N8 C46 C43 114.4(5) . . ? N8 C46 H46A 108.7 . . ? C43 C46 H46A 108.7 . . ? N8 C46 H46B 108.7 . . ? C43 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? N8 C47 C48 110.3(5) . . ? N8 C47 H47A 109.6 . . ? C48 C47 H47A 109.6 . . ? N8 C47 H47B 109.6 . . ? C48 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? N8 C48 C47 111.0(5) 7_656 . ? N8 C48 H48A 109.4 7_656 . ? C47 C48 H48A 109.4 . . ? N8 C48 H48B 109.4 7_656 . ? C47 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? 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 O2 C10 117(6) 1_545 . . . ? N4 Co1 O2 C10 120.6(7) 4_655 . . . ? N5 Co1 O2 C10 -149.2(7) . . . . ? N1 Co1 O2 C10 29.9(7) . . . . ? O5 Co1 O2 C10 -65.4(7) . . . . ? O2 Co1 N1 C15 -135.7(5) . . . . ? O3 Co1 N1 C15 45.9(5) 1_545 . . . ? N4 Co1 N1 C15 133.6(5) 4_655 . . . ? N5 Co1 N1 C15 -14(13) . . . . ? O5 Co1 N1 C15 -40.2(5) . . . . ? O2 Co1 N1 C11 42.4(6) . . . . ? O3 Co1 N1 C11 -136.1(6) 1_545 . . . ? N4 Co1 N1 C11 -48.4(6) 4_655 . . . ? N5 Co1 N1 C11 164(12) . . . . ? O5 Co1 N1 C11 137.8(6) . . . . ? O2 Co1 N5 C35 -154.5(5) . . . . ? O3 Co1 N5 C35 24.0(5) 1_545 . . . ? N4 Co1 N5 C35 -63.8(5) 4_655 . . . ? N1 Co1 N5 C35 84(12) . . . . ? O5 Co1 N5 C35 110.1(5) . . . . ? O2 Co1 N5 C31 34.1(4) . . . . ? O3 Co1 N5 C31 -147.4(4) 1_545 . . . ? N4 Co1 N5 C31 124.9(4) 4_655 . . . ? N1 Co1 N5 C31 -88(12) . . . . ? O5 Co1 N5 C31 -61.3(4) . . . . ? C6 C1 C2 C3 1.4(10) . . . . ? C7 C1 C2 C3 -177.9(6) . . . . ? C1 C2 C3 C4 2.4(10) . . . . ? C2 C3 C4 C5 -4.0(11) . . . . ? C3 C4 C5 C6 1.7(11) . . . . ? C4 C5 C6 C1 2.1(9) . . . . ? C4 C5 C6 C9 -180.0(6) . . . . ? C2 C1 C6 C5 -3.6(9) . . . . ? C7 C1 C6 C5 175.7(6) . . . . ? C2 C1 C6 C9 178.4(6) . . . . ? C7 C1 C6 C9 -2.3(9) . . . . ? C2 C1 C7 C8 95.5(8) . . . . ? C6 C1 C7 C8 -83.8(8) . . . . ? Co1 O3 C8 O4 32.6(16) 1_565 . . . ? Co1 O3 C8 O4A -13.8(13) 1_565 . . . ? Co1 O3 C8 C7 -170.6(5) 1_565 . . . ? C1 C7 C8 O4 152.6(9) . . . . ? C1 C7 C8 O3 -8.5(11) . . . . ? C1 C7 C8 O4A -165.1(10) . . . . ? C5 C6 C9 C10 108.4(8) . . . . ? C1 C6 C9 C10 -73.6(9) . . . . ? Co1 O2 C10 O1 30(2) . . . . ? Co1 O2 C10 O1A 9(3) . . . . ? Co1 O2 C10 C9 -155.0(6) . . . . ? C6 C9 C10 O1 163(2) . . . . ? C6 C9 C10 O2 -12.8(11) . . . . ? C6 C9 C10 O1A -178(2) . . . . ? C15 N1 C11 C12 -0.7(12) . . . . ? Co1 N1 C11 C12 -178.8(6) . . . . ? N1 C11 C12 C13 3.8(13) . . . . ? C11 C12 C13 C14 -5.0(11) . . . . ? C11 C12 C13 C16 177.3(7) . . . . ? C12 C13 C14 C15 3.5(10) . . . . ? C16 C13 C14 C15 -178.7(6) . . . . ? C11 N1 C15 C14 -1.0(10) . . . . ? Co1 N1 C15 C14 177.1(5) . . . . ? C13 C14 C15 N1 -0.4(10) . . . . ? C17 N2 C16 C13 -68.7(8) . . . . ? C19 N2 C16 C13 169.3(6) . . . . ? C12 C13 C16 N2 96.2(8) . . . . ? C14 C13 C16 N2 -81.5(8) . . . . ? C16 N2 C17 C18 -179.2(6) . . . . ? C19 N2 C17 C18 -55.9(7) . . . . ? C20 N3 C18 C17 -58.7(8) . . . . ? C21 N3 C18 C17 -178.3(6) . . . . ? N2 C17 C18 N3 57.5(8) . . . . ? C16 N2 C19 C20 -178.7(6) . . . . ? C17 N2 C19 C20 57.4(7) . . . . ? C18 N3 C20 C19 59.1(8) . . . . ? C21 N3 C20 C19 -178.7(6) . . . . ? N2 C19 C20 N3 -59.4(8) . . . . ? C20 N3 C21 C24 178.5(6) . . . . ? C18 N3 C21 C24 -60.4(8) . . . . ? C26 N4 C22 C23 -1.6(10) . . . . ? Co1 N4 C22 C23 -178.5(5) 4_645 . . . ? N4 C22 C23 C24 2.0(11) . . . . ? C22 C23 C24 C25 -3.3(10) . . . . ? C22 C23 C24 C21 -179.2(6) . . . . ? N3 C21 C24 C25 145.0(7) . . . . ? N3 C21 C24 C23 -39.3(10) . . . . ? C23 C24 C25 C26 4.4(12) . . . . ? C21 C24 C25 C26 -179.7(7) . . . . ? C22 N4 C26 C25 2.6(10) . . . . ? Co1 N4 C26 C25 179.5(6) 4_645 . . . ? C24 C25 C26 N4 -4.2(12) . . . . ? C35 N5 C31 C32 -5.3(9) . . . . ? Co1 N5 C31 C32 166.5(5) . . . . ? N5 C31 C32 C33 2.3(9) . . . . ? C31 C32 C33 C34 1.1(8) . . . . ? C31 C32 C33 C36 -179.5(5) . . . . ? C32 C33 C34 C35 -1.3(8) . . . . ? C36 C33 C34 C35 179.3(5) . . . . ? C31 N5 C35 C34 5.2(9) . . . . ? Co1 N5 C35 C34 -166.3(4) . . . . ? C33 C34 C35 N5 -2.0(9) . . . . ? C37 N6 C36 C33 66.3(7) . . . . ? C38 N6 C36 C33 -170.7(6) 5_755 . . . ? C34 C33 C36 N6 -92.5(7) . . . . ? C32 C33 C36 N6 88.1(7) . . . . ? C38 N6 C37 C38 57.7(8) 5_755 . . . ? C36 N6 C37 C38 178.5(5) . . . . ? N6 C37 C38 N6 -56.5(8) . . . 5_755 ? C45 N7 C41 C42 1.6(9) . . . . ? N7 C41 C42 C43 -2.3(9) . . . . ? C41 C42 C43 C44 2.8(8) . . . . ? C41 C42 C43 C46 -179.2(5) . . . . ? C42 C43 C44 C45 -2.8(8) . . . . ? C46 C43 C44 C45 179.4(5) . . . . ? C41 N7 C45 C44 -1.4(9) . . . . ? C43 C44 C45 N7 2.1(9) . . . . ? C47 N8 C46 C43 -73.7(7) . . . . ? C48 N8 C46 C43 163.9(5) 7_656 . . . ? C44 C43 C46 N8 -12.2(8) . . . . ? C42 C43 C46 N8 170.0(5) . . . . ? C48 N8 C47 C48 -57.5(7) 7_656 . . . ? C46 N8 C47 C48 179.6(5) . . . . ? N8 C47 C48 N8 58.3(7) . . . 7_656 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 0.508 -0.003 3307 1156 ' ' _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.507 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.099