#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100964.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100964 _chemical_formula_moiety '(C72 H72 Cl4 Mn8 N12 O12) 4+, 4 (Cl O4) -' _chemical_formula_sum 'C72 H72 Cl8 Mn8 N12 O28' _chemical_formula_weight 2276.54 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' 'Mn' 'Mn' 0.3368 0.7283 '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 11.643(6) _cell_length_b 11.702(6) _cell_length_c 17.890(9) _cell_angle_alpha 72.939(11) _cell_angle_beta 74.285(9) _cell_angle_gamma 70.911(19) _cell_volume 2160.4(18) _cell_formula_units_Z 1 _cell_measurement_temperature 112(2) _cell_measurement_reflns_used 2559 _cell_measurement_theta_min 2.284 _cell_measurement_theta_max 24.619 _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max .12 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.6210 _exptl_absorpt_correction_T_max 0.8679 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 112(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 '3-circle diffractometer with fixed chi of 54.74 degrees' _diffrn_measurement_device_type 'Bruker' _diffrn_measurement_method 'phi and omega scans' _diffrn_measurement_details ; 0.3 degree frames were measured with a counting time of 10.2 seconds each. ; _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 22.4 _diffrn_detector_details ; The detector was operated in 4x4 "binning" mode. ; _diffrn_standards_number 72 _diffrn_standards_interval_time 218 _diffrn_standards_decay_% 5.2 _diffrn_reflns_number 7106 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.1181 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.50 _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.882 _reflns_number_total 7106 _reflns_number_gt 4162 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [\s^2^(Fo^2^)+(0.06Fo^2^)^2^]^-1^ ; _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 7106 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1670 _refine_ls_R_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.2320 _refine_ls_wR_factor_gt 0.2148 _refine_ls_goodness_of_fit_ref 1.586 _refine_ls_restrained_S_all 1.586 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.631 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.180 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 Mn1 Mn 0.54580(14) 0.12057(17) 0.48705(10) 0.0218(4) Uani 1 1 d . . . Mn2 Mn 0.43949(15) 0.08337(18) 0.34478(10) 0.0243(5) Uani 1 1 d . . . Mn3 Mn 0.61957(13) 0.04435(17) -0.00564(10) 0.0211(4) Uani 1 1 d . . . Mn4 Mn 0.41035(14) 0.05166(18) 0.15485(10) 0.0247(5) Uani 1 1 d . . . Cl5 Cl 0.5024(3) 0.1816(3) 0.20424(17) 0.0322(7) Uani 1 1 d . . . Cl6 Cl 0.3156(2) -0.0157(3) 0.29411(17) 0.0319(8) Uani 1 1 d . . . O7 O 0.4893(6) 0.1081(8) 0.5962(5) 0.035(2) Uani 1 1 d . . . C8 C 0.4242(11) 0.2197(13) 0.6256(9) 0.043(4) Uani 1 1 d . . . C9 C 0.3984(11) 0.3252(14) 0.5570(9) 0.041(4) Uani 1 1 d . . . C10 C 0.3236(14) 0.4405(15) 0.5656(11) 0.063(5) Uani 1 1 d . . . C11 C 0.3086(16) 0.5336(16) 0.4970(13) 0.077(6) Uani 1 1 d . . . C12 C 0.3691(14) 0.5117(15) 0.4195(12) 0.065(5) Uani 1 1 d . . . C13 C 0.4387(12) 0.3943(14) 0.4166(10) 0.048(4) Uani 1 1 d . . . N14 N 0.4527(8) 0.3030(10) 0.4829(7) 0.035(3) Uani 1 1 d . . . O15 O 0.5814(6) 0.1334(8) 0.3770(5) 0.030(2) Uani 1 1 d . . . C16 C 0.6980(9) 0.1446(13) 0.3300(7) 0.032(3) Uani 1 1 d . . . C17 C 0.7814(10) 0.1492(11) 0.3795(7) 0.026(3) Uani 1 1 d . . . C18 C 0.9035(10) 0.1501(12) 0.3480(7) 0.030(3) Uani 1 1 d . . . C19 C 0.9746(10) 0.1527(13) 0.3968(7) 0.035(3) Uani 1 1 d . . . C20 C 0.9252(10) 0.1533(12) 0.4762(8) 0.034(3) Uani 1 1 d . . . C21 C 0.8012(10) 0.1529(12) 0.5024(8) 0.033(3) Uani 1 1 d . . . N22 N 0.7319(8) 0.1521(9) 0.4544(6) 0.028(2) Uani 1 1 d . . . O23 O 0.3855(6) 0.0615(7) 0.4775(4) 0.0200(17) Uani 1 1 d . . . C24 C 0.2637(8) 0.1289(10) 0.5072(6) 0.017(2) Uani 1 1 d . . . C25 C 0.2197(9) 0.2414(11) 0.4445(7) 0.024(3) Uani 1 1 d . . . C26 C 0.1130(10) 0.3373(12) 0.4653(8) 0.034(3) Uani 1 1 d . . . C27 C 0.0711(12) 0.4342(13) 0.4052(9) 0.045(4) Uani 1 1 d . . . C28 C 0.1342(13) 0.4380(13) 0.3272(8) 0.047(4) Uani 1 1 d . . . C29 C 0.2366(14) 0.3426(15) 0.3107(8) 0.053(4) Uani 1 1 d . . . N30 N 0.2787(8) 0.2445(9) 0.3689(5) 0.026(2) Uani 1 1 d . . . O31 O 0.6396(6) 0.0834(7) -0.1167(5) 0.0262(19) Uani 1 1 d . . . C32 C 0.6488(10) 0.2047(12) -0.1629(7) 0.031(3) Uani 1 1 d . . . C33 C 0.6533(9) 0.2846(13) -0.1114(8) 0.030(3) Uani 1 1 d . . . C34 C 0.6548(10) 0.4088(12) -0.1437(8) 0.036(3) Uani 1 1 d . . . C35 C 0.6525(11) 0.4733(14) -0.0917(8) 0.042(4) Uani 1 1 d . . . C36 C 0.6523(10) 0.4213(12) -0.0120(8) 0.035(3) Uani 1 1 d . . . C37 C 0.6516(9) 0.2984(11) 0.0145(7) 0.023(3) Uani 1 1 d . . . N38 N 0.6521(7) 0.2297(9) -0.0341(5) 0.022(2) Uani 1 1 d . . . O39 O 0.6023(6) -0.0177(8) 0.1046(4) 0.0260(19) Uani 1 1 d . . . C40 C 0.7095(9) -0.0858(13) 0.1385(7) 0.035(3) Uani 1 1 d . . . C41 C 0.8185(10) -0.1110(13) 0.0734(9) 0.037(3) Uani 1 1 d . . . C42 C 0.9328(11) -0.1854(14) 0.0896(9) 0.046(4) Uani 1 1 d . . . C43 C 1.0299(13) -0.1997(19) 0.0241(12) 0.074(6) Uani 1 1 d . . . C44 C 1.0131(11) -0.1351(16) -0.0516(11) 0.054(4) Uani 1 1 d . . . C45 C 0.8950(10) -0.0613(13) -0.0614(8) 0.040(4) Uani 1 1 d . . . N46 N 0.7994(7) -0.0515(10) 0.0004(6) 0.028(2) Uani 1 1 d . . . O47 O 0.4392(6) 0.1135(7) 0.0215(4) 0.0204(17) Uani 1 1 d . . . C48 C 0.3677(9) 0.2352(11) -0.0094(7) 0.024(3) Uani 1 1 d . . . C49 C 0.2581(9) 0.2770(11) 0.0505(7) 0.022(3) Uani 1 1 d . . . C50 C 0.1664(9) 0.3864(13) 0.0303(8) 0.034(3) Uani 1 1 d . . . C51 C 0.0647(11) 0.4252(14) 0.0885(9) 0.045(4) Uani 1 1 d . . . C52 C 0.0560(10) 0.3555(13) 0.1634(8) 0.038(3) Uani 1 1 d . . . C53 C 0.1503(10) 0.2498(13) 0.1795(7) 0.036(3) Uani 1 1 d . . . N54 N 0.2470(7) 0.2124(9) 0.1252(5) 0.024(2) Uani 1 1 d . . . Cl55 Cl 0.9814(3) 0.8165(4) 0.2897(2) 0.0442(9) Uani 1 1 d . . . O56 O 1.0755(8) 0.7465(12) 0.2415(7) 0.074(4) Uani 1 1 d . . . O57 O 1.0166(12) 0.8245(14) 0.3559(7) 0.093(5) Uani 1 1 d . . . O58 O 0.8855(13) 0.759(2) 0.3170(9) 0.154(9) Uani 1 1 d . . . O59 O 0.9423(19) 0.9356(14) 0.2423(8) 0.160(9) Uani 1 1 d . . . Cl60 Cl 0.3089(3) 0.4774(4) 0.7844(2) 0.0461(9) Uani 1 1 d . . . O61 O 0.2482(8) 0.5730(9) 0.7246(6) 0.057(3) Uani 1 1 d . . . O62 O 0.3306(14) 0.5184(15) 0.8408(8) 0.111(5) Uani 1 1 d . . . O63 O 0.2216(13) 0.4067(13) 0.8299(7) 0.097(4) Uani 1 1 d . . . O64 O 0.4112(13) 0.410(2) 0.7462(8) 0.178(11) Uani 1 1 d . . . H8A H 0.4755 0.2356 0.6555 0.052 Uiso 1 1 calc R . . H8B H 0.3456 0.2096 0.6621 0.052 Uiso 1 1 calc R . . H10 H 0.2833 0.4561 0.6168 0.075 Uiso 1 1 calc R . . H11 H 0.2569 0.6139 0.5017 0.092 Uiso 1 1 calc R . . H12 H 0.3610 0.5758 0.3726 0.078 Uiso 1 1 calc R . . H13 H 0.4791 0.3756 0.3661 0.058 Uiso 1 1 calc R . . H16A H 0.6861 0.2211 0.2872 0.038 Uiso 1 1 calc R . . H16B H 0.7376 0.0730 0.3045 0.038 Uiso 1 1 calc R . . H18 H 0.9374 0.1490 0.2935 0.036 Uiso 1 1 calc R . . H19 H 1.0585 0.1541 0.3760 0.041 Uiso 1 1 calc R . . H20 H 0.9734 0.1539 0.5112 0.041 Uiso 1 1 calc R . . H21 H 0.7646 0.1533 0.5567 0.040 Uiso 1 1 calc R . . H24A H 0.2633 0.1549 0.5552 0.020 Uiso 1 1 calc R . . H24B H 0.2069 0.0752 0.5225 0.020 Uiso 1 1 calc R . . H26 H 0.0719 0.3344 0.5193 0.041 Uiso 1 1 calc R . . H27 H -0.0012 0.4985 0.4170 0.054 Uiso 1 1 calc R . . H28 H 0.1071 0.5059 0.2855 0.056 Uiso 1 1 calc R . . H29 H 0.2792 0.3451 0.2571 0.064 Uiso 1 1 calc R . . H32A H 0.5765 0.2458 -0.1893 0.038 Uiso 1 1 calc R . . H32B H 0.7245 0.1961 -0.2049 0.038 Uiso 1 1 calc R . . H34 H 0.6572 0.4453 -0.1989 0.044 Uiso 1 1 calc R . . H35 H 0.6510 0.5585 -0.1110 0.051 Uiso 1 1 calc R . . H36 H 0.6527 0.4681 0.0232 0.042 Uiso 1 1 calc R . . H37 H 0.6507 0.2607 0.0694 0.028 Uiso 1 1 calc R . . H40A H 0.6968 -0.1651 0.1741 0.042 Uiso 1 1 calc R . . H40B H 0.7239 -0.0374 0.1704 0.042 Uiso 1 1 calc R . . H42 H 0.9446 -0.2248 0.1425 0.056 Uiso 1 1 calc R . . H43 H 1.1084 -0.2547 0.0320 0.089 Uiso 1 1 calc R . . H44 H 1.0801 -0.1408 -0.0959 0.065 Uiso 1 1 calc R . . H45 H 0.8816 -0.0165 -0.1134 0.048 Uiso 1 1 calc R . . H48A H 0.3408 0.2352 -0.0573 0.028 Uiso 1 1 calc R . . H48B H 0.4197 0.2938 -0.0254 0.028 Uiso 1 1 calc R . . H50 H 0.1732 0.4344 -0.0229 0.041 Uiso 1 1 calc R . . H51 H 0.0024 0.4999 0.0754 0.054 Uiso 1 1 calc R . . H52 H -0.0131 0.3786 0.2040 0.046 Uiso 1 1 calc R . . H53 H 0.1456 0.2012 0.2326 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0169(8) 0.0150(11) 0.0382(11) -0.0084(8) -0.0027(7) -0.0105(7) Mn2 0.0255(9) 0.0202(12) 0.0303(10) -0.0090(8) -0.0045(7) -0.0080(8) Mn3 0.0145(8) 0.0174(11) 0.0373(11) -0.0093(8) -0.0030(7) -0.0109(7) Mn4 0.0212(8) 0.0252(12) 0.0301(10) -0.0100(8) -0.0028(7) -0.0077(8) Cl5 0.0414(16) 0.029(2) 0.0332(17) -0.0115(14) -0.0016(13) -0.0189(14) Cl6 0.0278(14) 0.045(2) 0.0309(16) -0.0109(15) -0.0040(12) -0.0193(14) O7 0.027(4) 0.032(6) 0.056(6) -0.030(5) -0.024(4) 0.008(4) C8 0.037(7) 0.029(9) 0.078(11) -0.029(8) -0.019(7) -0.006(6) C9 0.037(7) 0.035(10) 0.071(10) -0.027(8) -0.023(7) -0.011(6) C10 0.068(10) 0.020(10) 0.107(14) -0.025(10) -0.029(10) -0.002(8) C11 0.084(12) 0.012(10) 0.143(19) -0.026(11) -0.045(13) 0.001(8) C12 0.065(10) 0.017(10) 0.111(15) -0.002(10) -0.027(10) -0.011(8) C13 0.051(8) 0.027(10) 0.079(11) -0.013(9) -0.018(8) -0.021(7) N14 0.026(5) 0.023(7) 0.063(8) -0.008(6) -0.012(5) -0.016(5) O15 0.026(4) 0.033(6) 0.038(5) -0.013(4) -0.002(3) -0.016(4) C16 0.019(5) 0.052(10) 0.031(7) -0.013(7) -0.001(5) -0.018(6) C17 0.030(6) 0.016(7) 0.034(7) -0.005(6) -0.003(5) -0.013(5) C18 0.029(6) 0.024(8) 0.036(7) 0.000(6) 0.003(5) -0.019(6) C19 0.021(6) 0.038(9) 0.041(8) -0.004(7) -0.004(5) -0.010(6) C20 0.036(7) 0.017(8) 0.049(8) 0.000(6) -0.019(6) -0.005(6) C21 0.033(6) 0.020(8) 0.054(9) -0.007(6) -0.011(6) -0.015(6) N22 0.028(5) 0.014(6) 0.045(7) -0.007(5) -0.010(5) -0.010(4) O23 0.016(3) 0.009(5) 0.038(5) -0.010(4) -0.002(3) -0.005(3) C24 0.015(5) 0.011(6) 0.032(6) -0.011(5) -0.003(4) -0.008(4) C25 0.023(5) 0.015(7) 0.039(7) -0.015(6) -0.002(5) -0.006(5) C26 0.036(6) 0.013(8) 0.048(8) -0.008(6) -0.004(6) -0.003(6) C27 0.044(7) 0.015(8) 0.070(10) -0.010(7) -0.005(7) -0.005(6) C28 0.066(9) 0.017(9) 0.041(8) -0.006(7) -0.005(7) 0.003(7) C29 0.073(10) 0.042(11) 0.036(8) -0.010(8) -0.015(7) 0.000(8) N30 0.036(5) 0.013(6) 0.028(6) -0.002(5) -0.001(4) -0.011(4) O31 0.028(4) 0.011(5) 0.045(5) -0.009(4) -0.001(4) -0.013(3) C32 0.030(6) 0.024(8) 0.043(8) -0.011(6) 0.002(5) -0.014(6) C33 0.014(5) 0.032(9) 0.049(8) -0.015(7) -0.003(5) -0.009(5) C34 0.037(7) 0.020(8) 0.049(8) -0.005(7) -0.006(6) -0.008(6) C35 0.048(8) 0.029(9) 0.058(10) -0.020(8) -0.001(7) -0.021(7) C36 0.034(6) 0.034(9) 0.049(9) -0.025(7) 0.010(6) -0.027(6) C37 0.022(5) 0.018(7) 0.039(7) -0.017(6) 0.002(5) -0.015(5) N38 0.017(4) 0.017(6) 0.032(6) -0.008(5) -0.001(4) -0.007(4) O39 0.019(4) 0.027(5) 0.035(5) -0.006(4) -0.006(3) -0.010(4) C40 0.028(6) 0.032(9) 0.044(8) -0.013(7) -0.013(6) 0.001(6) C41 0.031(6) 0.031(9) 0.068(10) -0.021(8) -0.025(7) -0.011(6) C42 0.030(7) 0.042(10) 0.080(11) -0.031(8) -0.025(7) 0.000(6) C43 0.038(9) 0.076(16) 0.123(17) -0.034(13) -0.033(10) -0.011(9) C44 0.027(7) 0.057(12) 0.087(13) -0.030(10) 0.000(7) -0.020(7) C45 0.021(6) 0.043(10) 0.061(9) -0.020(8) -0.002(6) -0.013(6) N46 0.020(5) 0.033(7) 0.048(7) -0.019(6) -0.006(5) -0.020(5) O47 0.019(3) 0.016(5) 0.028(4) -0.005(4) 0.000(3) -0.011(3) C48 0.026(6) 0.010(7) 0.034(7) 0.002(5) -0.007(5) -0.008(5) C49 0.013(5) 0.024(8) 0.037(7) -0.006(6) -0.007(5) -0.013(5) C50 0.021(6) 0.033(9) 0.049(8) -0.010(7) -0.011(6) -0.007(6) C51 0.031(7) 0.038(10) 0.066(10) -0.022(8) -0.008(7) 0.000(6) C52 0.027(6) 0.033(9) 0.051(9) -0.008(7) 0.004(6) -0.015(6) C53 0.029(6) 0.041(10) 0.033(7) 0.001(6) -0.003(6) -0.012(6) N54 0.023(5) 0.026(7) 0.025(5) -0.005(5) -0.008(4) -0.007(4) Cl55 0.0429(18) 0.047(3) 0.045(2) -0.0155(18) 0.0003(16) -0.0177(17) O56 0.043(6) 0.078(10) 0.103(9) -0.046(8) 0.010(6) -0.016(6) O57 0.127(10) 0.119(13) 0.074(8) 0.002(8) -0.035(7) -0.095(10) O58 0.117(10) 0.29(3) 0.134(13) -0.132(15) 0.076(9) -0.172(14) O59 0.30(2) 0.048(12) 0.077(10) -0.035(8) -0.053(12) 0.058(12) Cl60 0.052(2) 0.041(3) 0.043(2) -0.0049(18) -0.0087(16) -0.0137(18) O61 0.066(6) 0.024(7) 0.069(7) 0.010(5) -0.031(5) 0.002(5) O62 0.165(13) 0.111(14) 0.100(10) -0.024(10) -0.067(10) -0.059(11) O63 0.152(12) 0.060(10) 0.095(9) 0.019(8) -0.031(8) -0.076(9) O64 0.113(11) 0.24(2) 0.084(11) -0.053(13) -0.017(9) 0.097(13) _cod_database_code 1100964