Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cai, Ji-Wen' 'Liu, Hong-Ke' 'Liu, Jun' 'Yu, Xiao-Lan' 'Zhang, Hua-Xin' _publ_contact_author_name 'Dr Hong-Ke Liu' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 CHINA ; _publ_contact_author_email 'HONGKE_LIU@YAHOO.COM' _publ_section_title ; Synthesis and Crystal Structures of Silver(I), Palladium(II), Zinc(II) and Cobalt(II) Complexes of Ditoptic Ligand 1,3-bis(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene ; data_Compound 1 _database_code_CSD 172860 #data_[Ag2(bitmb)2](PF6)2 (CH3CN)2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H46 Ag2 F12 N10 P2' _chemical_formula_weight 1148.51 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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 8.799(2) _cell_length_b 9.907(2) _cell_length_c 13.853(3) _cell_angle_alpha 98.37(3) _cell_angle_beta 101.74(3) _cell_angle_gamma 102.62(3) _cell_volume 1130.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6383 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 27.24 _reflns_number_total 4748 _reflns_number_observed 3157 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1564P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4742 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_obs 0.0757 _refine_ls_wR_factor_all 0.2532 _refine_ls_wR_factor_obs 0.2062 _refine_ls_goodness_of_fit_all 1.001 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.199 _refine_ls_shift/esd_mean 0.023 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.00010(7) -0.54988(6) 0.21746(4) 0.0567(3) Uani 1 d . . N4 N -0.1933(8) -0.4545(7) 0.1947(4) 0.0532(14) Uani 1 d . . N2 N -0.3552(6) -0.3169(6) 0.2170(4) 0.0450(12) Uani 1 d . . C14 C -0.4318(7) -0.2082(7) 0.4494(5) 0.0457(15) Uani 1 d . . C13 C -0.3763(10) -0.3604(9) 0.1151(5) 0.060(2) Uani 1 d . . H13A H -0.4536(10) -0.3397(9) 0.0635(5) 0.080 Uiso 1 d R . C12 C -0.2612(8) -0.0028(7) 0.5682(5) 0.049(2) Uani 1 d . . C11 C -0.3800(7) -0.1273(7) 0.5479(5) 0.0463(15) Uani 1 d . . C10 C -0.3732(8) -0.1562(7) 0.3718(5) 0.0437(14) Uani 1 d . . C9 C -0.2543(8) -0.0319(7) 0.3917(5) 0.0477(15) Uani 1 d . . C8 C -0.1966(8) 0.0424(7) 0.4915(6) 0.053(2) Uani 1 d . . H8A H -0.1119(8) 0.1276(7) 0.5073(6) 0.080 Uiso 1 d R . C7 C -0.2436(8) -0.3760(8) 0.2620(5) 0.049(2) Uani 1 d . . H7A H -0.2029(8) -0.3610(8) 0.3335(5) 0.080 Uiso 1 d R . C4 C -0.4492(9) -0.2306(8) 0.2632(5) 0.056(2) Uani 1 d . . H4A H -0.5522(9) -0.2912(8) 0.2599(5) 0.080 Uiso 1 d R . H4B H -0.4660(9) -0.1611(8) 0.2235(5) 0.080 Uiso 1 d R . C1 C -0.2797(11) -0.4454(10) 0.1021(5) 0.067(2) Uani 1 d . . H1A H -0.2677(11) -0.4876(10) 0.0381(5) 0.080 Uiso 1 d R . C17 C -0.5512(11) -0.3507(8) 0.4281(7) 0.068(2) Uani 1 d . . H17A H -0.5754(11) -0.3934(8) 0.3581(7) 0.080 Uiso 1 d R . H17B H -0.5040(11) -0.4095(8) 0.4679(7) 0.080 Uiso 1 d R . H17C H -0.6483(11) -0.3402(8) 0.4462(7) 0.080 Uiso 1 d R . C16 C -0.1991(11) 0.0895(9) 0.6731(6) 0.071(2) Uani 1 d . . H16A H -0.2528(11) 0.0447(9) 0.7183(6) 0.080 Uiso 1 d R . H16B H -0.0854(11) 0.1027(9) 0.6962(6) 0.080 Uiso 1 d R . H16C H -0.2222(11) 0.1795(9) 0.6709(6) 0.080 Uiso 1 d R . C15 C -0.1865(11) 0.0270(10) 0.3107(7) 0.069(2) Uani 1 d . . H15A H -0.2382(11) -0.0370(10) 0.2478(7) 0.080 Uiso 1 d R . H15B H -0.2073(11) 0.1175(10) 0.3073(7) 0.080 Uiso 1 d R . H15C H -0.0728(11) 0.0365(10) 0.3243(7) 0.080 Uiso 1 d R . P1 P 0.0000 -0.5000 0.5000 0.0457(5) Uani 1 d S . P2 P -0.5000 0.0000 0.0000 0.0751(9) Uani 1 d S . F3 F 0.0645(6) -0.4073(5) 0.4242(3) 0.0700(12) Uani 1 d . . F2 F -0.1437(8) -0.4285(8) 0.4971(5) 0.110(2) Uani 1 d . . F9 F -0.5492(10) -0.0116(8) 0.1036(4) 0.111(2) Uani 1 d . . F1 F 0.1057(9) -0.3840(6) 0.5934(4) 0.102(2) Uani 1 d . . F8 F -0.3481(10) -0.0554(10) 0.0372(6) 0.126(3) Uani 1 d . . F7 F -0.5988(12) -0.1576(7) -0.0452(6) 0.130(3) Uani 1 d . . N1 N -0.3729(7) -0.2508(6) 0.6942(4) 0.0487(13) Uani 1 d . . C3 C -0.2386(9) -0.2879(8) 0.6898(5) 0.051(2) Uani 1 d . . H3A H -0.1761(9) -0.2637(8) 0.6426(5) 0.080 Uiso 1 d R . C2 C -0.4616(9) -0.1705(9) 0.6306(6) 0.059(2) Uani 1 d . . H2A H -0.5691(9) -0.2263(9) 0.5995(6) 0.080 Uiso 1 d R . H2B H -0.4675(9) -0.0872(9) 0.6733(6) 0.080 Uiso 1 d R . N3 N 0.1956(7) -0.6452(6) 0.2386(4) 0.0493(13) Uani 1 d . . C6 C 0.3108(10) -0.6374(9) 0.1847(5) 0.059(2) Uani 1 d . . H6A H 0.3054(10) -0.6000(9) 0.1243(5) 0.080 Uiso 1 d R . C5 C -0.4216(10) -0.3002(9) 0.7736(5) 0.062(2) Uani 1 d . . H5A H -0.5169(10) -0.2934(9) 0.7955(5) 0.080 Uiso 1 d R . N1W N -0.1616(13) -0.6366(11) -0.0942(7) 0.098(3) Uani 1 d . . C2W C -0.1081(14) -0.7210(12) -0.0682(7) 0.081(3) Uani 1 d . . C1W C -0.0433(15) -0.8374(13) -0.0355(10) 0.102(3) Uani 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 Ag1 0.0578(4) 0.0684(4) 0.0551(4) 0.0118(3) 0.0116(2) 0.0414(3) N4 0.059(3) 0.067(4) 0.045(3) 0.016(3) 0.012(2) 0.037(3) N2 0.040(3) 0.051(3) 0.045(3) 0.009(2) 0.002(2) 0.023(2) C14 0.034(3) 0.041(3) 0.068(4) 0.015(3) 0.010(3) 0.021(3) C13 0.064(5) 0.082(5) 0.046(3) 0.018(3) 0.010(3) 0.042(4) C12 0.046(4) 0.047(4) 0.056(4) 0.003(3) 0.005(3) 0.027(3) C11 0.037(3) 0.054(4) 0.057(4) 0.017(3) 0.009(3) 0.029(3) C10 0.041(3) 0.041(3) 0.053(3) 0.008(3) 0.007(3) 0.024(3) C9 0.039(3) 0.050(4) 0.064(4) 0.019(3) 0.014(3) 0.024(3) C8 0.041(4) 0.044(4) 0.074(4) 0.009(3) 0.008(3) 0.015(3) C7 0.052(4) 0.059(4) 0.044(3) 0.010(3) 0.006(3) 0.032(3) C4 0.046(4) 0.065(4) 0.060(4) 0.005(3) 0.001(3) 0.033(3) C1 0.077(5) 0.094(6) 0.041(3) 0.013(4) 0.014(3) 0.048(5) C17 0.062(5) 0.047(4) 0.089(6) 0.014(4) 0.013(4) 0.005(4) C16 0.075(5) 0.070(5) 0.060(4) -0.004(4) -0.005(4) 0.035(4) C15 0.061(5) 0.069(5) 0.089(6) 0.028(4) 0.034(4) 0.021(4) P1 0.0473(13) 0.0508(14) 0.0443(11) 0.0112(10) 0.0127(10) 0.0211(11) P2 0.109(3) 0.069(2) 0.062(2) 0.0267(15) 0.023(2) 0.041(2) F3 0.071(3) 0.077(3) 0.067(3) 0.027(2) 0.023(2) 0.015(2) F2 0.117(5) 0.168(6) 0.109(4) 0.073(4) 0.060(4) 0.106(5) F9 0.146(6) 0.131(5) 0.080(4) 0.050(4) 0.043(4) 0.053(5) F1 0.132(5) 0.080(4) 0.063(3) 0.004(3) 0.003(3) -0.015(4) F8 0.126(6) 0.172(7) 0.120(5) 0.079(5) 0.037(4) 0.083(5) F7 0.174(8) 0.080(4) 0.136(6) 0.001(4) 0.066(5) 0.017(4) N1 0.047(3) 0.061(3) 0.049(3) 0.014(3) 0.017(2) 0.029(3) C3 0.052(4) 0.059(4) 0.058(4) 0.021(3) 0.022(3) 0.031(3) C2 0.049(4) 0.084(5) 0.066(4) 0.031(4) 0.022(3) 0.044(4) N3 0.043(3) 0.062(4) 0.052(3) 0.016(3) 0.012(2) 0.030(3) C6 0.070(5) 0.070(5) 0.051(4) 0.021(3) 0.025(3) 0.034(4) C5 0.065(5) 0.082(6) 0.056(4) 0.022(4) 0.028(4) 0.035(4) N1W 0.113(7) 0.099(7) 0.100(6) 0.029(5) 0.038(5) 0.047(6) C2W 0.090(7) 0.085(7) 0.071(5) 0.011(5) 0.020(5) 0.029(6) C1W 0.095(8) 0.096(8) 0.119(8) 0.024(7) 0.010(7) 0.046(6) _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 Ag1 N4 2.112(6) . ? Ag1 N3 2.126(5) . ? N4 C7 1.333(8) . ? N4 C1 1.377(9) . ? N2 C7 1.344(8) . ? N2 C13 1.377(9) . ? N2 C4 1.479(8) . ? C14 C10 1.399(10) . ? C14 C11 1.408(10) . ? C14 C17 1.513(11) . ? C13 C1 1.340(11) . ? C12 C11 1.381(11) . ? C12 C8 1.387(10) . ? C12 C16 1.523(10) . ? C11 C2 1.535(10) . ? C10 C9 1.382(10) . ? C10 C4 1.518(9) . ? C9 C8 1.402(10) . ? C9 C15 1.504(10) . ? P1 F1 1.572(5) 2_546 ? P1 F1 1.572(5) . ? P1 F2 1.575(5) . ? P1 F2 1.575(5) 2_546 ? P1 F3 1.601(4) . ? P1 F3 1.601(4) 2_546 ? P2 F7 1.577(7) . ? P2 F7 1.577(7) 2_455 ? P2 F8 1.574(7) . ? P2 F8 1.574(7) 2_455 ? P2 F9 1.594(6) 2_455 ? P2 F9 1.594(6) . ? N1 C3 1.322(8) . ? N1 C5 1.375(9) . ? N1 C2 1.488(8) . ? C3 N3 1.309(9) 2_546 ? N3 C3 1.309(9) 2_546 ? N3 C6 1.372(9) . ? C6 C5 1.344(11) 2_546 ? C5 C6 1.344(11) 2_546 ? N1W C2W 1.114(13) . ? C2W C1W 1.48(2) . ? 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 N4 Ag1 N3 179.2(2) . . ? C7 N4 C1 105.5(6) . . ? C7 N4 Ag1 129.1(4) . . ? C1 N4 Ag1 124.9(5) . . ? C7 N2 C13 106.2(5) . . ? C7 N2 C4 128.9(5) . . ? C13 N2 C4 124.7(5) . . ? C10 C14 C11 119.9(6) . . ? C10 C14 C17 120.4(7) . . ? C11 C14 C17 119.7(7) . . ? C1 C13 N2 107.6(6) . . ? C11 C12 C8 120.0(6) . . ? C11 C12 C16 121.9(7) . . ? C8 C12 C16 118.1(7) . . ? C12 C11 C14 119.2(6) . . ? C12 C11 C2 119.9(6) . . ? C14 C11 C2 120.8(6) . . ? C9 C10 C14 120.9(6) . . ? C9 C10 C4 119.0(6) . . ? C14 C10 C4 119.9(6) . . ? C10 C9 C8 118.1(6) . . ? C10 C9 C15 122.7(7) . . ? C8 C9 C15 119.2(7) . . ? C12 C8 C9 121.6(6) . . ? N4 C7 N2 111.4(6) . . ? N2 C4 C10 115.3(5) . . ? C13 C1 N4 109.3(6) . . ? F1 P1 F1 180.0 2_546 . ? F1 P1 F2 89.4(4) 2_546 . ? F1 P1 F2 90.6(4) . . ? F1 P1 F2 90.6(4) 2_546 2_546 ? F1 P1 F2 89.4(4) . 2_546 ? F2 P1 F2 180.000(2) . 2_546 ? F1 P1 F3 88.8(3) 2_546 . ? F1 P1 F3 91.2(3) . . ? F2 P1 F3 90.3(3) . . ? F2 P1 F3 89.7(3) 2_546 . ? F1 P1 F3 91.2(3) 2_546 2_546 ? F1 P1 F3 88.8(3) . 2_546 ? F2 P1 F3 89.7(3) . 2_546 ? F2 P1 F3 90.3(3) 2_546 2_546 ? F3 P1 F3 180.0 . 2_546 ? F7 P2 F7 180.0 . 2_455 ? F7 P2 F8 88.8(5) . . ? F7 P2 F8 91.2(5) 2_455 . ? F7 P2 F8 91.2(5) . 2_455 ? F7 P2 F8 88.8(5) 2_455 2_455 ? F8 P2 F8 180.0 . 2_455 ? F7 P2 F9 90.0(4) . 2_455 ? F7 P2 F9 90.0(4) 2_455 2_455 ? F8 P2 F9 89.7(4) . 2_455 ? F8 P2 F9 90.3(4) 2_455 2_455 ? F7 P2 F9 90.0(4) . . ? F7 P2 F9 90.0(4) 2_455 . ? F8 P2 F9 90.3(4) . . ? F8 P2 F9 89.7(4) 2_455 . ? F9 P2 F9 180.0 2_455 . ? C3 N1 C5 106.6(6) . . ? C3 N1 C2 130.1(6) . . ? C5 N1 C2 123.4(6) . . ? N1 C3 N3 111.9(6) . 2_546 ? N1 C2 C11 112.5(5) . . ? C3 N3 C6 106.1(5) 2_546 . ? C3 N3 Ag1 127.4(5) 2_546 . ? C6 N3 Ag1 126.3(5) . . ? C5 C6 N3 108.5(6) 2_546 . ? C6 C5 N1 106.9(7) 2_546 . ? N1W C2W C1W 177.7(13) . . ? _refine_diff_density_max 2.075 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.186 #===END data_[Pd2(bitmb)4]Cl4.cif _database_code_CSD 154826 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cai, Ji-Wen' 'Liu, Hong-Ke' 'Liu, Jun' 'Yu, Xiao-Lan' 'Zhang, Hua-Xin' _publ_contact_author_name 'Dr Hong-Ke Liu' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 CHINA ; _publ_contact_author_email 'HONGKE_LIU@YAHOO.COM' _publ_section_title ; Synthesis and Crystal Structures of Silver(I), Palladium(II), Zinc(II) and Cobalt(II) Complexes of Ditoptic Ligand 1,3-bis(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene ; #data_[Pd2(bitmb)4]Cl4 8H2O 1.5 CH3CN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H100 Cl4 N17.50 O8 Pd2' _chemical_formula_weight 1681.79 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7708(15) _cell_length_b 14.3618(19) _cell_length_c 14.4184(19) _cell_angle_alpha 96.710(2) _cell_angle_beta 113.302(2) _cell_angle_gamma 94.745(2) _cell_volume 2201.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 873 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 15867 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 6.82 _diffrn_reflns_theta_max 30.06 _reflns_number_total 12124 _reflns_number_gt 6036 _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^)+(0.0948P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12124 _refine_ls_number_parameters 440 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1352 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.2030 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.003 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 Pd1 Pd 0.681173(15) 0.950269(11) 1.430666(12) 0.05159(5) Uani 1 1 d . . . N1 N 0.65326(17) 0.88394(13) 1.29159(14) 0.0624(6) Uani 1 1 d . . . N2 N 0.65749(19) 0.86101(16) 1.14058(15) 0.0731(7) Uani 1 1 d . . . N3 N 0.70567(16) 0.82854(13) 1.48675(14) 0.0591(6) Uani 1 1 d . . . N4 N 0.76601(17) 0.69190(13) 1.51828(16) 0.0685(6) Uani 1 1 d . . . N5 N 0.70725(16) 1.01940(13) 1.56918(13) 0.0562(5) Uani 1 1 d . . . N6 N 1.21651(17) 0.93756(16) 1.26548(15) 0.0727(7) Uani 1 1 d . . . N7 N 0.64502(16) 1.07027(12) 1.37222(14) 0.0563(6) Uani 1 1 d . . . N8 N 1.33859(17) 0.78200(13) 1.64908(16) 0.0662(6) Uani 1 1 d . . . C1 C 0.5774(3) 0.79945(19) 1.2384(2) 0.0787(9) Uani 1 1 d . . . H1A H 0.5318 0.7578 1.2632 0.080 Uiso 1 1 d R . . C2 C 0.5779(3) 0.7869(2) 1.1450(2) 0.0974(12) Uani 1 1 d . . . H2A H 0.5301 0.7362 1.0900 0.080 Uiso 1 1 d R . . C3 C 0.6997(2) 0.91827(18) 1.22992(17) 0.0644(8) Uani 1 1 d . . . H3A H 0.7562 0.9761 1.2477 0.080 Uiso 1 1 d R . . C4 C 0.6832(3) 0.8774(3) 1.0510(2) 0.0952(12) Uani 1 1 d . . . H4A H 0.6932 0.8181 1.0188 0.080 Uiso 1 1 d R . . H4B H 0.6129 0.9002 1.0025 0.080 Uiso 1 1 d R . . C5 C 0.7984(2) 0.9455(2) 1.07869(17) 0.0756(9) Uani 1 1 d . . . C6 C 0.7938(3) 1.0415(2) 1.07464(19) 0.0895(11) Uani 1 1 d . . . C7 C 0.9031(3) 1.1015(2) 1.1003(2) 0.0898(11) Uani 1 1 d . . . H7A H 0.8995 1.1679 1.0995 0.080 Uiso 1 1 d R . . C8 C 1.0167(3) 1.0705(3) 1.12805(19) 0.0892(11) Uani 1 1 d . . . C9 C 1.0229(2) 0.9764(2) 1.13097(17) 0.0825(10) Uani 1 1 d . . . C10 C 0.9156(3) 0.9121(2) 1.11098(18) 0.0825(9) Uani 1 1 d . . . C11 C 0.6707(3) 1.0822(3) 1.0439(3) 0.1167(13) Uani 1 1 d . . . H11A H 0.6864 1.1491 1.0456 0.080 Uiso 1 1 d R . . H11B H 0.6342 1.0706 1.0911 0.080 Uiso 1 1 d R . . H11C H 0.6142 1.0526 0.9759 0.080 Uiso 1 1 d R . . C12 C 0.9210(3) 0.8068(3) 1.1196(3) 0.1119(14) Uani 1 1 d . . . H12A H 1.0060 0.7948 1.1426 0.080 Uiso 1 1 d R . . H12B H 0.8719 0.7686 1.0541 0.080 Uiso 1 1 d R . . H12C H 0.8882 0.7913 1.1681 0.080 Uiso 1 1 d R . . C13 C 1.1321(4) 1.1432(3) 1.1548(3) 0.1233(16) Uani 1 1 d . . . H13A H 1.2043 1.1110 1.1722 0.080 Uiso 1 1 d R . . H13B H 1.1427 1.1904 1.2116 0.080 Uiso 1 1 d R . . H13C H 1.1222 1.1731 1.0964 0.080 Uiso 1 1 d R . . C14 C 0.6484(2) 0.79137(19) 1.5433(2) 0.0748(8) Uani 1 1 d . . . H14A H 0.5918 0.8217 1.5656 0.080 Uiso 1 1 d R . . C15 C 0.6854(3) 0.7063(2) 1.5628(2) 0.0917(10) Uani 1 1 d . . . H15A H 0.6589 0.6644 1.5999 0.080 Uiso 1 1 d R . . C16 C 0.7777(2) 0.76617(15) 1.47457(19) 0.0632(7) Uani 1 1 d . . . H16A H 0.8309 0.7741 1.4391 0.080 Uiso 1 1 d R . . C17 C 0.8243(2) 0.60401(17) 1.5158(3) 0.0925(11) Uani 1 1 d . . . H17A H 0.8469 0.5826 1.5806 0.080 Uiso 1 1 d R . . H17B H 0.7638 0.5557 1.4641 0.080 Uiso 1 1 d R . . C18 C 1.0545(2) 0.64954(15) 1.5710(2) 0.0682(8) Uani 1 1 d . . . C19 C 1.1612(2) 0.65505(15) 1.5495(2) 0.0727(9) Uani 1 1 d . . . C20 C 1.1492(2) 0.63364(17) 1.4505(2) 0.0783(9) Uani 1 1 d . . . C21 C 1.0297(3) 0.60676(19) 1.3727(2) 0.0851(10) Uani 1 1 d . . . H21A H 1.0210 0.5913 1.3034 0.080 Uiso 1 1 d R . . C22 C 0.9245(3) 0.59837(17) 1.3915(2) 0.0796(10) Uani 1 1 d . . . C23 C 0.9383(2) 0.61833(15) 1.4934(2) 0.0687(8) Uani 1 1 d . . . C24 C 0.7991(3) 0.5686(2) 1.3046(3) 0.1213(17) Uani 1 1 d . . . H24A H 0.7352 0.5668 1.3303 0.080 Uiso 1 1 d R . . H24B H 0.7965 0.5069 1.2695 0.080 Uiso 1 1 d R . . H24C H 0.7851 0.6134 1.2581 0.080 Uiso 1 1 d R . . C25 C 1.2581(3) 0.6420(3) 1.4176(3) 0.1116(14) Uani 1 1 d . . . H25A H 1.3345 0.6625 1.4774 0.080 Uiso 1 1 d R . . H25B H 1.2463 0.6874 1.3718 0.080 Uiso 1 1 d R . . H25C H 1.2624 0.5816 1.3838 0.080 Uiso 1 1 d R . . C26 C 1.0661(3) 0.6772(2) 1.6777(2) 0.0993(12) Uani 1 1 d . . . H26A H 0.9847 0.6688 1.6785 0.080 Uiso 1 1 d R . . H26B H 1.1015 0.7427 1.7001 0.080 Uiso 1 1 d R . . H26C H 1.1190 0.6395 1.7229 0.080 Uiso 1 1 d R . . C27 C 1.1451(3) 0.9342(3) 1.1552(2) 0.1011(12) Uani 1 1 d . . . H27A H 1.1278 0.8704 1.1195 0.080 Uiso 1 1 d R . . H27B H 1.1955 0.9711 1.1303 0.080 Uiso 1 1 d R . . C28 C 1.3136(2) 0.8882(2) 1.3067(2) 0.0763(9) Uani 1 1 d . . . H28A H 1.3424 0.8433 1.2692 0.080 Uiso 1 1 d R . . C29 C 0.6405(2) 1.08513(18) 1.59078(19) 0.0677(8) Uani 1 1 d . . . H29A H 0.5722 1.1092 1.5415 0.080 Uiso 1 1 d R . . C30 C 0.7922(2) 1.00748(19) 1.65756(17) 0.0679(7) Uani 1 1 d . . . H30A H 0.8528 0.9648 1.6657 0.080 Uiso 1 1 d R . . C31 C 1.2897(3) 0.68129(17) 1.6357(3) 0.0877(11) Uani 1 1 d . . . H31A H 1.2844 0.6694 1.6982 0.080 Uiso 1 1 d R . . H31B H 1.3462 0.6422 1.6233 0.080 Uiso 1 1 d R . . C32 C 1.4545(3) 0.82435(19) 1.7168(2) 0.0818(10) Uani 1 1 d . . . H32A H 1.5181 0.7945 1.7636 0.080 Uiso 1 1 d R . . C33 C 0.5365(2) 1.08314(18) 1.29557(19) 0.0724(9) Uani 1 1 d . . . H33A H 0.4663 1.0352 1.2561 0.080 Uiso 1 1 d R . . C34 C 0.7192(2) 1.15255(16) 1.40486(19) 0.0655(8) Uani 1 1 d . . . H34A H 0.8019 1.1635 1.4586 0.080 Uiso 1 1 d R . . Cl1 Cl 1.0378(3) 0.9303(2) 0.6283(2) 0.1790(11) Uiso 0.50 1 d P . . Cl1' Cl 1.0222(2) 0.9571(2) 0.5653(2) 0.1499(8) Uiso 0.50 1 d P . . Cl2 Cl 1.5065(2) 0.51808(19) 0.61759(19) 0.2526(9) Uiso 1 1 d . . . O1W O 1.2266(5) 0.7005(4) 1.1189(4) 0.243(2) Uiso 1 1 d . . . O2W O 1.6320(6) 0.6678(5) 0.8498(5) 0.278(3) Uiso 1 1 d . . . O3W O 1.4084(8) 0.5994(6) 1.2267(6) 0.195(3) Uiso 0.50 1 d P . . O3W' O 1.8459(8) 0.5695(7) 0.7846(7) 0.206(3) Uiso 0.50 1 d P . . O4W O 1.0025(4) 1.1560(3) 1.6052(3) 0.1005(13) Uiso 0.50 1 d P . . O4W' O 1.0121(10) 1.0842(9) 1.5621(8) 0.233(4) Uiso 0.50 1 d P . . N1W N 1.4912(4) 0.6555(7) 0.8964(6) 0.263(4) Uiso 0.75 1 d PD . . C1W C 1.2874(5) 0.6424(11) 0.9259(6) 0.300 Uiso 0.75 1 d PD . . C2W C 1.3927(3) 0.6540(4) 0.9005(3) 0.134(2) Uani 0.75 1 d PDU . . 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 Pd1 0.05313(7) 0.04435(7) 0.05744(8) 0.01184(6) 0.02055(6) 0.01357(6) N1 0.0611(9) 0.0555(10) 0.0658(10) 0.0053(8) 0.0219(8) 0.0093(8) N2 0.0686(11) 0.0799(13) 0.0591(10) -0.0034(10) 0.0175(9) 0.0121(10) N3 0.0610(8) 0.0531(9) 0.0705(9) 0.0158(8) 0.0317(7) 0.0154(8) N4 0.0675(9) 0.0501(9) 0.0994(12) 0.0304(9) 0.0392(9) 0.0179(8) N5 0.0540(8) 0.0555(9) 0.0599(9) 0.0121(8) 0.0215(7) 0.0173(7) N6 0.0624(9) 0.0969(14) 0.0633(10) 0.0051(10) 0.0300(8) 0.0243(10) N7 0.0570(9) 0.0441(9) 0.0635(9) 0.0124(8) 0.0179(8) 0.0136(7) N8 0.0596(9) 0.0493(9) 0.0858(12) 0.0215(9) 0.0209(9) 0.0178(8) C1 0.0815(15) 0.0638(15) 0.0808(15) -0.0001(13) 0.0277(12) 0.0009(13) C2 0.097(2) 0.0845(19) 0.0791(18) -0.0218(15) 0.0145(16) 0.0022(17) C3 0.0664(12) 0.0632(14) 0.0535(11) 0.0022(11) 0.0169(10) 0.0045(11) C4 0.0856(17) 0.131(2) 0.0584(14) 0.0029(15) 0.0204(13) 0.0230(17) C5 0.0735(13) 0.1066(19) 0.0484(11) 0.0084(12) 0.0250(9) 0.0281(13) C6 0.0875(16) 0.126(2) 0.0612(13) 0.0244(15) 0.0313(12) 0.0333(16) C7 0.0986(17) 0.105(2) 0.0694(14) 0.0244(14) 0.0337(13) 0.0261(16) C8 0.0917(16) 0.124(2) 0.0515(12) 0.0105(14) 0.0300(11) 0.0163(17) C9 0.0715(13) 0.132(2) 0.0442(11) 0.0074(13) 0.0233(10) 0.0250(15) C10 0.0983(16) 0.1006(19) 0.0476(11) 0.0011(12) 0.0285(11) 0.0308(15) C11 0.1071(18) 0.149(3) 0.110(2) 0.0419(19) 0.0469(16) 0.0612(18) C12 0.114(2) 0.133(3) 0.0801(18) 0.0088(19) 0.0301(16) 0.037(2) C13 0.112(2) 0.171(4) 0.0790(18) 0.023(2) 0.0338(17) 0.003(2) C14 0.0728(11) 0.0745(14) 0.0991(14) 0.0341(12) 0.0500(10) 0.0252(11) C15 0.0946(15) 0.0813(16) 0.1280(17) 0.0535(13) 0.0629(13) 0.0267(13) C16 0.0656(11) 0.0461(11) 0.0865(13) 0.0197(10) 0.0368(10) 0.0118(9) C17 0.0861(15) 0.0477(12) 0.156(2) 0.0391(13) 0.0545(15) 0.0214(11) C18 0.0802(13) 0.0427(10) 0.0885(14) 0.0223(10) 0.0362(11) 0.0213(10) C19 0.0775(13) 0.0384(10) 0.1005(16) 0.0233(11) 0.0292(12) 0.0199(10) C20 0.0876(13) 0.0453(11) 0.1153(17) 0.0171(12) 0.0519(12) 0.0225(10) C21 0.1077(17) 0.0572(14) 0.0921(16) 0.0045(13) 0.0433(14) 0.0187(13) C22 0.0780(15) 0.0467(12) 0.1031(18) 0.0091(12) 0.0249(14) 0.0162(11) C23 0.0694(12) 0.0397(10) 0.0996(16) 0.0164(11) 0.0341(11) 0.0175(9) C24 0.101(2) 0.0719(19) 0.143(3) 0.000(2) 0.004(2) 0.0154(17) C25 0.0993(18) 0.093(2) 0.150(3) 0.014(2) 0.0584(17) 0.0249(16) C26 0.1089(18) 0.0833(18) 0.113(2) 0.0214(16) 0.0481(16) 0.0296(16) C27 0.0852(15) 0.163(3) 0.0553(13) 0.0016(16) 0.0305(11) 0.0347(18) C28 0.0710(12) 0.0818(16) 0.0842(14) 0.0071(13) 0.0387(10) 0.0272(11) C29 0.0614(11) 0.0687(13) 0.0721(13) 0.0068(11) 0.0241(10) 0.0267(10) C30 0.0649(10) 0.0903(15) 0.0588(11) 0.0156(11) 0.0300(9) 0.0373(10) C31 0.0765(15) 0.0484(12) 0.128(2) 0.0273(13) 0.0269(15) 0.0136(11) C32 0.0730(15) 0.0704(14) 0.0869(16) 0.0340(12) 0.0089(13) 0.0217(12) C33 0.0617(13) 0.0633(13) 0.0736(14) 0.0218(11) 0.0057(12) 0.0063(11) C34 0.0564(11) 0.0540(12) 0.0805(14) 0.0198(11) 0.0179(10) 0.0168(9) C2W 0.133(4) 0.141(4) 0.060(2) -0.023(3) -0.019(3) 0.011(3) _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 Pd1 N1 2.004(2) . ? Pd1 N3 2.0056(19) . ? Pd1 N7 2.0096(18) . ? Pd1 N5 2.0174(19) . ? N1 C3 1.333(4) . ? N1 C1 1.386(3) . ? N2 C3 1.327(3) . ? N2 C2 1.383(4) . ? N2 C4 1.478(4) . ? N3 C16 1.326(3) . ? N3 C14 1.372(4) . ? N4 C16 1.325(3) . ? N4 C15 1.355(4) . ? N4 C17 1.489(3) . ? N5 C30 1.313(3) . ? N5 C29 1.361(3) . ? N6 C30 1.328(3) 2_778 ? N6 C28 1.362(3) . ? N6 C27 1.468(3) . ? N7 C34 1.325(3) . ? N7 C33 1.363(3) . ? N8 C34 1.345(3) 2_778 ? N8 C32 1.362(3) . ? N8 C31 1.473(3) . ? C1 C2 1.340(5) . ? C4 C5 1.488(4) . ? C5 C6 1.391(4) . ? C5 C10 1.416(4) . ? C6 C7 1.379(4) . ? C6 C11 1.527(5) . ? C7 C8 1.365(5) . ? C8 C9 1.364(5) . ? C8 C13 1.530(5) . ? C9 C10 1.410(4) . ? C9 C27 1.535(4) . ? C10 C12 1.537(5) . ? C14 C15 1.355(4) . ? C17 C23 1.503(4) . ? C18 C23 1.376(3) . ? C18 C19 1.407(4) . ? C18 C26 1.492(4) . ? C19 C20 1.371(4) . ? C19 C31 1.512(3) . ? C20 C21 1.395(4) . ? C20 C25 1.534(5) . ? C21 C22 1.367(5) . ? C22 C23 1.405(4) . ? C22 C24 1.496(4) . ? C28 C29 1.351(4) 2_778 ? C29 C28 1.351(4) 2_778 ? C30 N6 1.328(3) 2_778 ? C32 C33 1.362(4) 2_778 ? C33 C32 1.362(4) 2_778 ? C34 N8 1.345(3) 2_778 ? Cl1 Cl1' 0.985(4) . ? Cl1' O4W' 1.733(12) 2_777 ? Cl1' O4W' 1.843(13) 1_554 ? Cl1' Cl1' 2.282(6) 2_776 ? O4W O4W' 1.179(13) . ? O4W' Cl1' 1.733(12) 2_777 ? O4W' Cl1' 1.843(13) 1_556 ? N1W C2W 1.183(6) . ? C1W C2W 1.426(7) . ? 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 N1 Pd1 N3 90.88(8) . . ? N1 Pd1 N7 89.09(8) . . ? N3 Pd1 N7 176.37(8) . . ? N1 Pd1 N5 178.70(8) . . ? N3 Pd1 N5 90.33(8) . . ? N7 Pd1 N5 89.68(8) . . ? C3 N1 C1 107.1(2) . . ? C3 N1 Pd1 124.82(15) . . ? C1 N1 Pd1 127.9(2) . . ? C3 N2 C2 106.9(2) . . ? C3 N2 C4 126.3(2) . . ? C2 N2 C4 126.7(2) . . ? C16 N3 C14 105.8(2) . . ? C16 N3 Pd1 127.25(18) . . ? C14 N3 Pd1 126.93(17) . . ? C16 N4 C15 108.5(2) . . ? C16 N4 C17 127.1(3) . . ? C15 N4 C17 124.3(2) . . ? C30 N5 C29 106.3(2) . . ? C30 N5 Pd1 125.84(17) . . ? C29 N5 Pd1 127.85(14) . . ? C30 N6 C28 107.3(2) 2_778 . ? C30 N6 C27 128.2(2) 2_778 . ? C28 N6 C27 124.3(2) . . ? C34 N7 C33 107.54(19) . . ? C34 N7 Pd1 126.33(14) . . ? C33 N7 Pd1 126.03(15) . . ? C34 N8 C32 107.7(2) 2_778 . ? C34 N8 C31 127.06(19) 2_778 . ? C32 N8 C31 125.2(2) . . ? C2 C1 N1 107.3(3) . . ? C1 C2 N2 108.2(2) . . ? N2 C3 N1 110.5(2) . . ? N2 C4 C5 112.9(2) . . ? C6 C5 C10 119.1(3) . . ? C6 C5 C4 121.6(3) . . ? C10 C5 C4 119.3(3) . . ? C7 C6 C5 119.3(3) . . ? C7 C6 C11 119.2(3) . . ? C5 C6 C11 121.5(3) . . ? C8 C7 C6 122.7(3) . . ? C9 C8 C7 118.9(3) . . ? C9 C8 C13 122.7(3) . . ? C7 C8 C13 118.4(3) . . ? C8 C9 C10 121.2(3) . . ? C8 C9 C27 122.6(3) . . ? C10 C9 C27 116.2(3) . . ? C9 C10 C5 118.6(3) . . ? C9 C10 C12 122.4(3) . . ? C5 C10 C12 119.0(3) . . ? C15 C14 N3 109.1(3) . . ? C14 C15 N4 106.1(3) . . ? N4 C16 N3 110.5(2) . . ? N4 C17 C23 112.6(2) . . ? C23 C18 C19 120.0(3) . . ? C23 C18 C26 119.5(3) . . ? C19 C18 C26 120.5(2) . . ? C20 C19 C18 120.1(2) . . ? C20 C19 C31 119.8(3) . . ? C18 C19 C31 120.0(3) . . ? C19 C20 C21 118.6(3) . . ? C19 C20 C25 124.6(2) . . ? C21 C20 C25 116.7(3) . . ? C22 C21 C20 122.7(3) . . ? C21 C22 C23 118.2(2) . . ? C21 C22 C24 120.0(3) . . ? C23 C22 C24 121.8(3) . . ? C18 C23 C22 120.2(3) . . ? C18 C23 C17 121.0(3) . . ? C22 C23 C17 118.8(2) . . ? N6 C27 C9 112.4(2) . . ? C29 C28 N6 106.4(2) 2_778 . ? C28 C29 N5 108.9(2) 2_778 . ? N5 C30 N6 111.1(2) . 2_778 ? N8 C31 C19 112.1(2) . . ? N8 C32 C33 106.9(2) . 2_778 ? C32 C33 N7 108.1(2) 2_778 . ? N7 C34 N8 109.67(18) . 2_778 ? Cl1 Cl1' O4W' 137.6(5) . 2_777 ? Cl1 Cl1' O4W' 121.5(5) . 1_554 ? O4W' Cl1' O4W' 100.8(5) 2_777 1_554 ? Cl1 Cl1' Cl1' 169.3(4) . 2_776 ? O4W' Cl1' Cl1' 52.5(4) 2_777 2_776 ? O4W' Cl1' Cl1' 48.3(4) 1_554 2_776 ? O4W O4W' Cl1' 133.2(9) . 2_777 ? O4W O4W' Cl1' 145.7(10) . 1_556 ? Cl1' O4W' Cl1' 79.2(5) 2_777 1_556 ? N1W C2W C1W 166.7(8) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.846 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.093 #===END data_Complex 3 _database_code_CSD 171467 #Data of [Zn(bitmb)(CH3COO)(C2H5OH)](OH) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 N4 O4 Zn' _chemical_formula_weight 466.15 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.960(2) _cell_length_b 12.150(2) _cell_length_c 15.710(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2282.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8214 _exptl_absorpt_correction_T_max 0.9331 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 12253 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.35 _reflns_number_total 2443 _reflns_number_gt 1723 _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^)+(0.2198P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2443 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2770 _refine_ls_wR_factor_gt 0.2518 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Zn1 Zn 0.14449(6) 0.2500 0.18011(5) 0.0604(4) Uani 1 2 d S . . N1 N 0.2428(3) 0.1151(3) 0.1759(2) 0.0626(10) Uani 1 1 d . . . C8 C 0.6339(5) -0.2500 0.1107(5) 0.0677(18) Uani 1 2 d S . . N2 N 0.3808(4) 0.0020(4) 0.2046(4) 0.0788(13) Uani 1 1 d . . . C5 C 0.5213(4) -0.1495(4) 0.2084(4) 0.0705(13) Uani 1 1 d . . . C6 C 0.4799(6) -0.2500 0.2420(5) 0.080(2) Uani 1 2 d S . . C7 C 0.5967(4) -0.1513(4) 0.1426(4) 0.0695(13) Uani 1 1 d . . . C1 C 0.3311(4) 0.0946(4) 0.2244(4) 0.0657(12) Uani 1 1 d . . . H1A H 0.3552 0.1410 0.2678 0.079 Uiso 1 1 calc R . . C9 C 0.3927(11) -0.2500 0.3114(9) 0.156(6) Uani 1 2 d S . . H9A H 0.3758 -0.3245 0.3273 0.235 Uiso 0.50 1 calc PR . . H9B H 0.3261 -0.2146 0.2911 0.235 Uiso 0.50 1 calc PR . . H9C H 0.4207 -0.2109 0.3601 0.235 Uiso 0.50 1 calc PR . . C4 C 0.4818(6) -0.0420(6) 0.2458(5) 0.116(3) Uani 1 1 d . . . H4A H 0.4667 -0.0526 0.3059 0.139 Uiso 1 1 calc R . . H4B H 0.5414 0.0118 0.2409 0.139 Uiso 1 1 calc R . . C3 C 0.3179(7) -0.0440(7) 0.1401(6) 0.129(4) Uani 1 1 d . . . H3A H 0.3304 -0.1119 0.1144 0.155 Uiso 1 1 calc R . . C10 C 0.6428(6) -0.0460(7) 0.1031(7) 0.137(4) Uani 1 1 d . . . H10A H 0.6097 0.0167 0.1305 0.206 Uiso 1 1 calc R . . H10B H 0.6253 -0.0445 0.0435 0.206 Uiso 1 1 calc R . . H10C H 0.7225 -0.0438 0.1105 0.206 Uiso 1 1 calc R . . C2 C 0.2346(5) 0.0277(5) 0.1210(4) 0.095(2) Uani 1 1 d . . . H2A H 0.1814 0.0191 0.0782 0.114 Uiso 1 1 calc R . . O2 O 0.0299(10) 0.2500 0.4303(6) 0.166(4) Uani 1 2 d S . . O1 O 0.0465(4) 0.2500 0.2808(4) 0.0761(13) Uani 1 2 d S . . C14 C 0.2031(5) 0.2500 0.3545(4) 0.0591(14) Uani 1 2 d S . . C12 C 0.1010(9) 0.2500 0.3501(5) 0.075(2) Uani 1 2 d S . . O3 O 0.0270(10) 0.2117(6) 0.0745(5) 0.121(4) Uani 0.50 1 d P . . OW1 O 0.6126(13) -0.2500 0.4966(11) 0.234(7) Uani 1 2 d S . . C15 C -0.0100(10) 0.1281(12) 0.0940(8) 0.089(3) Uani 0.50 1 d P . . C16 C -0.040(2) -0.0041(16) 0.0491(13) 0.150(7) Uiso 0.50 1 d P . . 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 Zn1 0.0484(6) 0.0437(5) 0.0891(7) 0.000 0.0008(3) 0.000 N1 0.050(2) 0.047(2) 0.091(3) -0.0098(17) 0.0003(17) 0.0002(16) C8 0.049(4) 0.068(4) 0.086(4) 0.000 -0.012(3) 0.000 N2 0.062(2) 0.058(3) 0.117(3) -0.030(3) -0.021(2) 0.015(2) C5 0.050(2) 0.051(3) 0.110(3) -0.014(3) -0.019(3) 0.0108(19) C6 0.050(4) 0.101(6) 0.091(5) 0.000 -0.002(3) 0.000 C7 0.054(3) 0.049(2) 0.106(4) 0.010(2) -0.023(3) -0.007(2) C1 0.054(2) 0.046(2) 0.097(4) -0.012(2) -0.002(2) 0.0009(19) C9 0.064(6) 0.239(17) 0.167(12) 0.000 0.040(7) 0.000 C4 0.090(4) 0.083(4) 0.173(6) -0.058(4) -0.060(4) 0.040(3) C3 0.108(5) 0.113(6) 0.167(7) -0.088(6) -0.063(5) 0.058(5) C10 0.126(7) 0.080(5) 0.206(9) 0.062(6) -0.054(6) -0.040(4) C2 0.072(3) 0.091(4) 0.122(5) -0.044(4) -0.029(3) 0.026(3) O2 0.200(10) 0.127(6) 0.171(8) 0.000 0.086(8) 0.000 O1 0.058(3) 0.075(3) 0.096(4) 0.000 0.007(3) 0.000 C14 0.040(3) 0.066(4) 0.072(4) 0.000 0.002(3) 0.000 C12 0.103(6) 0.034(3) 0.088(5) 0.000 0.013(5) 0.000 O3 0.201(11) 0.069(6) 0.095(5) -0.031(4) 0.044(6) -0.019(5) OW1 0.178(11) 0.246(14) 0.279(16) 0.000 0.128(12) 0.000 C15 0.079(7) 0.092(8) 0.096(8) 0.026(6) -0.002(6) 0.031(6) _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 Zn1 O1 1.968(6) . ? Zn1 N1 2.018(4) 7_565 ? Zn1 N1 2.018(4) . ? Zn1 O3 2.223(11) . ? Zn1 O3 2.223(11) 7_565 ? N1 C1 1.325(6) . ? N1 C2 1.372(6) . ? C8 C7 1.374(6) . ? C8 C7 1.374(6) 7 ? N2 C1 1.310(6) . ? N2 C3 1.380(8) . ? N2 C4 1.472(7) . ? C5 C7 1.373(8) . ? C5 C6 1.419(7) . ? C5 C4 1.508(7) . ? C6 C5 1.419(7) 7 ? C6 C9 1.509(13) . ? C7 C10 1.525(8) . ? C3 C2 1.358(9) . ? O2 C12 1.520(11) . ? O1 C12 1.269(11) . ? C14 C12 1.223(12) . ? O3 O3 0.930(16) 7_565 ? O3 C15 1.149(14) . ? C15 C16 1.79(2) . ? C16 C16 1.81(4) 5 ? 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 Zn1 N1 111.92(13) . 7_565 ? O1 Zn1 N1 111.92(13) . . ? N1 Zn1 N1 108.6(2) 7_565 . ? O1 Zn1 O3 102.9(3) . . ? N1 Zn1 O3 120.9(3) 7_565 . ? N1 Zn1 O3 100.0(3) . . ? O1 Zn1 O3 102.9(3) . 7_565 ? N1 Zn1 O3 100.0(3) 7_565 7_565 ? N1 Zn1 O3 120.9(3) . 7_565 ? O3 Zn1 O3 24.1(4) . 7_565 ? C1 N1 C2 105.9(4) . . ? C1 N1 Zn1 126.7(3) . . ? C2 N1 Zn1 127.4(3) . . ? C7 C8 C7 121.6(7) . 7 ? C1 N2 C3 106.0(5) . . ? C1 N2 C4 125.5(5) . . ? C3 N2 C4 128.5(5) . . ? C7 C5 C6 119.7(5) . . ? C7 C5 C4 120.8(6) . . ? C6 C5 C4 119.4(6) . . ? C5 C6 C5 118.7(7) 7 . ? C5 C6 C9 120.7(3) 7 . ? C5 C6 C9 120.7(3) . . ? C5 C7 C8 120.1(5) . . ? C5 C7 C10 122.1(6) . . ? C8 C7 C10 117.8(6) . . ? N2 C1 N1 112.7(5) . . ? N2 C4 C5 113.6(5) . . ? C2 C3 N2 107.6(5) . . ? C3 C2 N1 107.7(5) . . ? C12 O1 Zn1 112.5(5) . . ? C14 C12 O1 124.2(8) . . ? C14 C12 O2 120.7(9) . . ? O1 C12 O2 115.1(9) . . ? O3 O3 C15 152.1(8) 7_565 . ? O3 O3 Zn1 77.9(2) 7_565 . ? C15 O3 Zn1 103.3(9) . . ? O3 C15 C16 139.9(12) . . ? C15 C16 C16 100.4(16) . 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 Zn1 N1 C1 -73.5(4) . . . . ? N1 Zn1 N1 C1 50.5(5) 7_565 . . . ? O3 Zn1 N1 C1 178.1(5) . . . . ? O3 Zn1 N1 C1 165.1(5) 7_565 . . . ? O1 Zn1 N1 C2 108.7(5) . . . . ? N1 Zn1 N1 C2 -127.3(4) 7_565 . . . ? O3 Zn1 N1 C2 0.3(5) . . . . ? O3 Zn1 N1 C2 -12.7(6) 7_565 . . . ? C7 C5 C6 C5 2.4(10) . . . 7 ? C4 C5 C6 C5 -177.5(4) . . . 7 ? C7 C5 C6 C9 -177.0(7) . . . . ? C4 C5 C6 C9 3.1(10) . . . . ? C6 C5 C7 C8 -1.5(8) . . . . ? C4 C5 C7 C8 178.4(5) . . . . ? C6 C5 C7 C10 179.1(6) . . . . ? C4 C5 C7 C10 -1.0(8) . . . . ? C7 C8 C7 C5 0.5(10) 7 . . . ? C7 C8 C7 C10 180.0(5) 7 . . . ? C3 N2 C1 N1 -2.3(8) . . . . ? C4 N2 C1 N1 178.8(6) . . . . ? C2 N1 C1 N2 0.6(6) . . . . ? Zn1 N1 C1 N2 -177.5(4) . . . . ? C1 N2 C4 C5 -178.9(6) . . . . ? C3 N2 C4 C5 2.5(13) . . . . ? C7 C5 C4 N2 90.6(7) . . . . ? C6 C5 C4 N2 -89.5(8) . . . . ? C1 N2 C3 C2 3.0(11) . . . . ? C4 N2 C3 C2 -178.2(7) . . . . ? N2 C3 C2 N1 -2.7(11) . . . . ? C1 N1 C2 C3 1.3(8) . . . . ? Zn1 N1 C2 C3 179.5(6) . . . . ? N1 Zn1 O1 C12 -61.08(13) 7_565 . . . ? N1 Zn1 O1 C12 61.08(13) . . . . ? O3 Zn1 O1 C12 167.6(2) . . . . ? O3 Zn1 O1 C12 -167.6(2) 7_565 . . . ? Zn1 O1 C12 C14 0.000(1) . . . . ? Zn1 O1 C12 O2 180.000(1) . . . . ? O1 Zn1 O3 O3 92.80(9) . . . 7_565 ? N1 Zn1 O3 O3 -32.88(16) 7_565 . . 7_565 ? N1 Zn1 O3 O3 -151.78(15) . . . 7_565 ? O1 Zn1 O3 C15 -58.6(8) . . . . ? N1 Zn1 O3 C15 175.7(7) 7_565 . . . ? N1 Zn1 O3 C15 56.8(9) . . . . ? O3 Zn1 O3 C15 -151.4(8) 7_565 . . . ? O3 O3 C15 C16 137.3(16) 7_565 . . . ? Zn1 O3 C15 C16 -133.5(17) . . . . ? O3 C15 C16 C16 14(3) . . . 5 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.199 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.126 #===END data_Compound 4 _database_code_CSD 172861 #data_[Co(bitmb)2(CH3CN)2] (ClO4)2 (C2H5OH)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H58 Cl2 Co N10 O10' _chemical_formula_weight 992.82 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.430(2) _cell_length_b 11.790(2) _cell_length_c 11.820(2) _cell_angle_alpha 84.90(3) _cell_angle_beta 87.80(3) _cell_angle_gamma 65.80(3) _cell_volume 1447.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 445 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8172 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5819 _reflns_number_gt 3799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1927P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5819 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2749 _refine_ls_wR_factor_gt 0.2510 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 Co Co 0.0000 0.0000 0.0000 0.0395(3) Uani 1 2 d S . . N7 N 0.1527(3) -0.0952(3) 0.1173(3) 0.0465(8) Uani 1 1 d . . . N8 N 0.2912(3) -0.2387(3) 0.2343(3) 0.0495(9) Uani 1 1 d . . . N2 N -0.0804(3) 0.1406(3) 0.1146(3) 0.0461(8) Uani 1 1 d . . . N1 N -0.1542(3) 0.3204(3) 0.1893(3) 0.0483(9) Uani 1 1 d . . . C31 C 0.1850(4) -0.2056(4) 0.1704(4) 0.0499(10) Uani 1 1 d . . . H31A H 0.1384 -0.2568 0.1657 0.080 Uiso 1 1 d R . . C6 C -0.4202(4) 0.5498(3) 0.2563(3) 0.0408(9) Uani 1 1 d . . . C9 C -0.3543(5) 0.5955(4) 0.4642(4) 0.0535(11) Uani 1 1 d . . . H9A H -0.3319 0.6105 0.5372 0.080 Uiso 1 1 d R . . C7 C -0.2911(4) 0.5120(3) 0.2827(3) 0.0408(9) Uani 1 1 d . . . C13 C -0.1089(4) 0.2600(4) 0.0968(4) 0.0489(10) Uani 1 1 d . . . H13A H -0.0990 0.3013 0.0257 0.080 Uiso 1 1 d R . . C5 C -0.5138(4) 0.6098(4) 0.3357(4) 0.0437(9) Uani 1 1 d . . . H5A H -0.6028 0.6333 0.3195 0.080 Uiso 1 1 d R . . C4 C -0.4806(4) 0.6357(4) 0.4386(4) 0.0487(10) Uani 1 1 d . . . C8 C -0.2578(4) 0.5329(4) 0.3889(4) 0.0502(10) Uani 1 1 d . . . C10 C -0.1881(4) 0.4541(4) 0.1970(4) 0.0528(11) Uani 1 1 d . . . H10A H -0.2164 0.4948 0.1228 0.080 Uiso 1 1 d R . . H10B H -0.1133 0.4666 0.2150 0.080 Uiso 1 1 d R . . C3 C -0.1192(5) 0.4937(6) 0.4226(5) 0.0844(18) Uani 1 1 d . . . H3A H -0.1206 0.5127 0.5001 0.080 Uiso 1 1 d R . . H3B H -0.0700 0.4060 0.4171 0.080 Uiso 1 1 d R . . H3C H -0.0809 0.5400 0.3756 0.080 Uiso 1 1 d R . . C12 C -0.1039(6) 0.1232(5) 0.2267(5) 0.0726(17) Uani 1 1 d . . . C2 C -0.4565(5) 0.5236(5) 0.1428(4) 0.0674(14) Uani 1 1 d . . . H2A H -0.3808 0.4824 0.0986 0.080 Uiso 1 1 d R . . H2B H -0.5031 0.4718 0.1541 0.080 Uiso 1 1 d R . . H2C H -0.5096 0.6017 0.1034 0.080 Uiso 1 1 d R . . C32 C 0.2412(5) -0.0523(5) 0.1499(5) 0.0673(14) Uani 1 1 d . . . H32A H 0.2454 0.0255 0.1241 0.080 Uiso 1 1 d R . . C11 C -0.1482(6) 0.2324(5) 0.2742(4) 0.0694(15) Uani 1 1 d . . . H11A H -0.1746 0.2503 0.3510 0.080 Uiso 1 1 d R . . C1 C -0.5800(6) 0.7025(5) 0.5281(5) 0.0789(17) Uani 1 1 d . . . H1A H -0.6662 0.7282 0.5017 0.080 Uiso 1 1 d R . . H1B H -0.5663 0.6462 0.5951 0.080 Uiso 1 1 d R . . H1C H -0.5669 0.7743 0.5457 0.080 Uiso 1 1 d R . . C33 C 0.3264(5) -0.1418(5) 0.2225(5) 0.0718(16) Uani 1 1 d . . . H33A H 0.3963 -0.1362 0.2605 0.080 Uiso 1 1 d R . . C34 C 0.3436(4) -0.3558(5) 0.3087(5) 0.0615(13) Uani 1 1 d . . . H34A H 0.2982 -0.4070 0.2987 0.080 Uiso 1 1 d R . . H34B H 0.4324 -0.4002 0.2898 0.080 Uiso 1 1 d R . . H34C H 0.3364 -0.3359 0.3864 0.080 Uiso 1 1 d R . . Cl1 Cl -0.18437(15) 0.56795(16) -0.16613(13) 0.0791(5) Uani 1 1 d . . . O4 O -0.2633(9) 0.6097(9) -0.2602(9) 0.198(3) Uiso 1 1 d . A . O1A O -0.0792(11) 0.4453(11) -0.1518(11) 0.114(3) Uiso 0.50 1 d P A 1 O1B O -0.1116(18) 0.4771(17) -0.2446(17) 0.185(6) Uiso 0.50 1 d P A 2 O3 O -0.2723(7) 0.5534(10) -0.0927(6) 0.204(4) Uani 1 1 d . A . O2 O -0.1392(8) 0.6526(8) -0.1485(10) 0.219(5) Uani 1 1 d . A . C14 C -0.2185(10) -0.2463(8) 0.1555(10) 0.142(4) Uani 1 1 d . . . C15 C -0.1532(5) -0.1633(4) 0.1136(5) 0.0633(13) Uani 1 1 d . . . N4 N -0.1031(4) -0.1060(3) 0.0813(3) 0.0507(9) Uani 1 1 d . . . O5 O -0.003(2) 0.183(2) 0.5665(19) 0.228(8) Uiso 0.50 1 d P . . C18 C 0.127(3) 0.150(3) 0.522(3) 0.198(11) Uiso 0.50 1 d P . . H12 H -0.095(5) 0.064(5) 0.256(4) 0.062(16) Uiso 1 1 d . . . O6 O -0.4411(17) 0.1784(16) 0.1079(16) 0.180(6) Uiso 0.50 1 d P . . C16 C 0.215(3) 0.146(3) 0.428(2) 0.182(9) Uiso 0.50 1 d P . . H16A H 0.3009 0.1156 0.4564 0.274 Uiso 0.50 1 calc PR . . H16B H 0.1913 0.2286 0.3914 0.274 Uiso 0.50 1 calc PR . . H16C H 0.2109 0.0918 0.3735 0.274 Uiso 0.50 1 calc PR . . C17 C -0.459(3) 0.103(3) 0.207(3) 0.185(10) Uiso 0.50 1 d P . . C19 C -0.442(3) -0.017(3) 0.311(3) 0.238(14) Uiso 0.50 1 d P . . H19A H -0.5147 0.0101 0.3613 0.358 Uiso 0.50 1 calc PR . . H19B H -0.3651 -0.0383 0.3531 0.358 Uiso 0.50 1 calc PR . . H19C H -0.4383 -0.0885 0.2752 0.358 Uiso 0.50 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 Co 0.0385(4) 0.0277(4) 0.0438(5) 0.0013(3) -0.0028(3) -0.0055(3) N7 0.0404(18) 0.0349(17) 0.057(2) 0.0053(15) -0.0113(16) -0.0084(14) N8 0.0389(18) 0.0432(19) 0.057(2) 0.0102(16) -0.0091(16) -0.0095(15) N2 0.0473(19) 0.0339(17) 0.049(2) -0.0036(15) 0.0028(16) -0.0082(14) N1 0.050(2) 0.0360(18) 0.055(2) -0.0081(15) 0.0140(16) -0.0132(15) C31 0.039(2) 0.045(2) 0.057(3) 0.003(2) -0.0111(19) -0.0091(18) C6 0.045(2) 0.037(2) 0.038(2) -0.0005(16) -0.0070(17) -0.0137(17) C9 0.065(3) 0.055(3) 0.040(2) -0.0071(19) -0.009(2) -0.022(2) C7 0.041(2) 0.0330(19) 0.044(2) -0.0035(16) 0.0006(17) -0.0106(16) C13 0.055(2) 0.037(2) 0.048(2) -0.0064(18) 0.0043(19) -0.0115(18) C5 0.0338(19) 0.038(2) 0.050(2) 0.0068(17) -0.0090(17) -0.0062(16) C4 0.055(2) 0.039(2) 0.041(2) -0.0030(17) 0.0051(19) -0.0078(18) C8 0.043(2) 0.051(2) 0.057(3) -0.002(2) -0.009(2) -0.0189(19) C10 0.056(3) 0.036(2) 0.067(3) -0.014(2) 0.018(2) -0.0190(19) C3 0.056(3) 0.109(5) 0.083(4) -0.002(4) -0.027(3) -0.027(3) C12 0.099(4) 0.039(3) 0.064(3) 0.001(2) 0.021(3) -0.016(3) C2 0.071(3) 0.080(4) 0.056(3) -0.012(3) -0.012(2) -0.033(3) C32 0.066(3) 0.053(3) 0.082(4) 0.023(3) -0.030(3) -0.027(2) C11 0.093(4) 0.049(3) 0.053(3) -0.006(2) 0.018(3) -0.017(3) C1 0.081(4) 0.059(3) 0.078(4) -0.017(3) 0.025(3) -0.009(3) C33 0.057(3) 0.067(3) 0.092(4) 0.024(3) -0.030(3) -0.030(3) C34 0.030(2) 0.061(3) 0.080(3) 0.023(2) -0.014(2) -0.0099(19) Cl1 0.0797(10) 0.1011(12) 0.0700(9) -0.0039(8) 0.0056(7) -0.0515(9) O3 0.136(6) 0.330(12) 0.141(6) 0.051(7) 0.036(5) -0.107(7) O2 0.159(7) 0.152(6) 0.384(15) -0.078(8) -0.049(8) -0.086(5) C14 0.143(8) 0.104(6) 0.206(10) 0.011(6) 0.055(7) -0.086(6) C15 0.069(3) 0.044(2) 0.078(3) 0.002(2) 0.003(3) -0.025(2) N4 0.053(2) 0.0392(18) 0.058(2) 0.0018(17) -0.0004(17) -0.0190(17) _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 Co N2 2.117(3) . ? Co N2 2.117(3) 2 ? Co N7 2.129(3) . ? Co N7 2.129(3) 2 ? Co N4 2.187(4) 2 ? Co N4 2.187(4) . ? N7 C31 1.305(5) . ? N7 C32 1.383(6) . ? N8 C31 1.351(5) . ? N8 C33 1.353(6) . ? N8 C34 1.478(5) . ? N2 C13 1.308(5) . ? N2 C12 1.356(7) . ? N1 C13 1.327(5) . ? N1 C11 1.360(6) . ? N1 C10 1.472(5) . ? C6 C7 1.394(5) . ? C6 C5 1.395(6) . ? C6 C2 1.513(6) . ? C9 C4 1.359(6) . ? C9 C8 1.388(7) . ? C7 C8 1.396(6) . ? C7 C10 1.500(6) . ? C5 C4 1.384(6) . ? C5 C34 1.548(5) 1_465 ? C4 C1 1.533(6) . ? C8 C3 1.516(6) . ? C12 C11 1.342(7) . ? C32 C33 1.364(6) . ? C34 C5 1.548(5) 1_645 ? Cl1 O2 1.331(6) . ? Cl1 O3 1.357(6) . ? Cl1 O4 1.381(10) . ? Cl1 O1B 1.44(2) . ? Cl1 O1A 1.453(12) . ? O4 O1B 1.80(2) . ? C14 C15 1.498(8) . ? C15 N4 1.089(6) . ? O5 C18 1.46(3) . ? C18 C16 1.47(4) . ? O6 C17 1.46(3) . ? C17 C19 1.75(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co N2 180.00(19) . 2 ? N2 Co N7 88.29(13) . . ? N2 Co N7 91.71(13) 2 . ? N2 Co N7 91.71(13) . 2 ? N2 Co N7 88.29(13) 2 2 ? N7 Co N7 180.0(3) . 2 ? N2 Co N4 88.50(14) . 2 ? N2 Co N4 91.50(14) 2 2 ? N7 Co N4 90.98(14) . 2 ? N7 Co N4 89.02(14) 2 2 ? N2 Co N4 91.50(14) . . ? N2 Co N4 88.50(14) 2 . ? N7 Co N4 89.02(14) . . ? N7 Co N4 90.98(14) 2 . ? N4 Co N4 180.0(3) 2 . ? C31 N7 C32 105.9(3) . . ? C31 N7 Co 128.1(3) . . ? C32 N7 Co 126.0(3) . . ? C31 N8 C33 106.8(4) . . ? C31 N8 C34 122.9(4) . . ? C33 N8 C34 130.1(4) . . ? C13 N2 C12 104.8(4) . . ? C13 N2 Co 128.5(3) . . ? C12 N2 Co 126.5(3) . . ? C13 N1 C11 106.4(4) . . ? C13 N1 C10 124.8(4) . . ? C11 N1 C10 128.4(4) . . ? N7 C31 N8 111.8(4) . . ? C7 C6 C5 119.4(4) . . ? C7 C6 C2 119.5(4) . . ? C5 C6 C2 121.0(4) . . ? C4 C9 C8 122.1(4) . . ? C6 C7 C8 119.4(4) . . ? C6 C7 C10 120.9(4) . . ? C8 C7 C10 119.7(4) . . ? N2 C13 N1 112.3(4) . . ? C4 C5 C6 120.9(4) . . ? C4 C5 C34 119.9(4) . 1_465 ? C6 C5 C34 119.1(4) . 1_465 ? C9 C4 C5 118.8(4) . . ? C9 C4 C1 118.2(4) . . ? C5 C4 C1 122.9(4) . . ? C9 C8 C7 119.2(4) . . ? C9 C8 C3 118.9(4) . . ? C7 C8 C3 121.8(4) . . ? N1 C10 C7 113.6(4) . . ? C11 C12 N2 110.1(5) . . ? C33 C32 N7 108.4(4) . . ? C12 C11 N1 106.2(5) . . ? N8 C33 C32 107.1(4) . . ? N8 C34 C5 110.1(4) . 1_645 ? O2 Cl1 O3 118.9(7) . . ? O2 Cl1 O4 108.7(6) . . ? O3 Cl1 O4 96.6(5) . . ? O2 Cl1 O1B 115.7(8) . . ? O3 Cl1 O1B 123.4(9) . . ? O4 Cl1 O1B 79.0(8) . . ? O2 Cl1 O1A 108.1(6) . . ? O3 Cl1 O1A 101.2(7) . . ? O4 Cl1 O1A 123.7(6) . . ? O1B Cl1 O1A 46.8(7) . . ? Cl1 O4 O1B 52.0(7) . . ? Cl1 O1B O4 48.9(7) . . ? N4 C15 C14 177.7(7) . . ? C15 N4 Co 174.1(4) . . ? C16 C18 O5 151(3) . . ? O6 C17 C19 165(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.842 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.100 #===END