#------------------------------------------------------------------------------ #$Date: 2011-01-03 12:48:23 +0000 (Mon, 03 Jan 2011) $ #$Revision: 5312 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000476.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_4000476 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C58 H84 Cl12 Mn2 N12 Nb6 O8' _chemical_formula_weight 2170.11 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 93.648(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.2271(11) _cell_length_b 21.8002(18) _cell_length_c 13.7809(10) _cell_measurement_reflns_used 48 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 12.51 _cell_measurement_theta_min 3.41 _cell_volume 3965.7(5) _diffrn_ambient_temperature 213(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 12795 _diffrn_reflns_theta_max 29.35 _diffrn_reflns_theta_min 2.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_T_max 0.6412 _exptl_absorpt_correction_T_min 0.4576 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ? _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'blcok shape' _exptl_crystal_F_000 2160 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_ls_extinction_coef 0.00049(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXTL-PC _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 469 _refine_ls_number_reflns 10883 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0378 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+4.5592P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.0862 _reflns_number_gt 8327 _reflns_number_total 10883 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M P2(1)/c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4000476 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Nb1 Nb 0.10072(2) 0.057072(13) 0.43539(2) 0.01779(7) Uani 1 1 d . . . Nb2 Nb -0.11146(2) 0.066819(13) 0.48260(2) 0.01739(7) Uani 1 1 d . . . Nb3 Nb 0.04592(2) 0.036376(13) 0.63544(2) 0.01764(7) Uani 1 1 d . . . Cl1 Cl 0.17268(7) 0.10996(4) 0.58227(6) 0.02623(18) Uani 1 1 d . . . Cl2 Cl -0.18099(7) 0.03733(4) 0.32049(6) 0.02573(17) Uani 1 1 d . . . Cl3 Cl -0.01181(7) 0.14665(4) 0.40529(6) 0.02416(17) Uani 1 1 d . . . Cl4 Cl 0.25052(6) -0.01079(4) 0.44648(7) 0.02558(17) Uani 1 1 d . . . Cl5 Cl 0.06681(7) 0.02373(4) 0.26515(6) 0.02432(17) Uani 1 1 d . . . Cl6 Cl -0.07911(7) 0.12040(4) 0.63932(6) 0.02459(17) Uani 1 1 d . . . N1 N 0.2596(3) 0.15333(18) 0.3225(3) 0.0411(9) Uani 1 1 d . . . N2 N -0.3010(2) 0.17416(15) 0.4460(2) 0.0302(7) Uani 1 1 d . . . N3 N 0.1355(3) 0.09341(19) 0.8562(3) 0.0439(9) Uani 1 1 d . . . C1 C 0.2087(3) 0.12036(18) 0.3614(3) 0.0274(8) Uani 1 1 d . . . C2 C -0.2370(3) 0.13952(16) 0.4606(3) 0.0241(7) Uani 1 1 d . . . C3 C 0.1020(3) 0.07523(18) 0.7830(3) 0.0282(8) Uani 1 1 d . . . Mn1 Mn -0.44642(4) 0.21438(2) 0.37168(4) 0.02233(11) Uani 1 1 d . . . O1 O -0.3836(2) 0.28025(12) 0.3110(2) 0.0293(6) Uani 1 1 d . . . O2 O -0.4358(2) 0.15888(12) 0.26834(19) 0.0296(6) Uani 1 1 d . . . N4 N -0.4718(2) 0.26614(14) 0.4867(2) 0.0254(6) Uani 1 1 d . . . N5 N -0.5253(2) 0.15402(14) 0.4447(2) 0.0253(6) Uani 1 1 d . . . C4 C -0.3765(3) 0.33842(17) 0.3361(3) 0.0276(8) Uani 1 1 d . . . C5 C -0.3255(3) 0.37931(19) 0.2771(3) 0.0369(9) Uani 1 1 d . . . H5 H -0.2992 0.3647 0.2197 0.044 Uiso 1 1 calc R . . C6 C -0.3134(4) 0.4400(2) 0.3014(4) 0.0450(11) Uani 1 1 d . . . H6 H -0.2771 0.4658 0.2615 0.054 Uiso 1 1 calc R . . C7 C -0.3540(4) 0.4641(2) 0.3844(4) 0.0499(13) Uani 1 1 d . . . H7 H -0.3459 0.5058 0.4002 0.060 Uiso 1 1 calc R . . C8 C -0.4054(4) 0.42614(19) 0.4417(3) 0.0397(10) Uani 1 1 d . . . H8 H -0.4346 0.4425 0.4966 0.048 Uiso 1 1 calc R . . C9 C -0.4166(3) 0.36268(17) 0.4218(3) 0.0288(8) Uani 1 1 d . . . C10 C -0.4614(3) 0.32465(18) 0.4922(3) 0.0301(8) Uani 1 1 d . . . H10 H -0.4851 0.3442 0.5471 0.036 Uiso 1 1 calc R . . C11 C -0.5105(3) 0.23136(19) 0.5685(3) 0.0337(9) Uani 1 1 d . . . H11A H -0.5487 0.2585 0.6096 0.040 Uiso 1 1 calc R . . H11B H -0.4543 0.2133 0.6084 0.040 Uiso 1 1 calc R . . C12 C -0.5785(3) 0.18170(19) 0.5248(3) 0.0337(9) Uani 1 1 d . . . H12A H -0.5916 0.1507 0.5739 0.040 Uiso 1 1 calc R . . H12B H -0.6434 0.1991 0.5001 0.040 Uiso 1 1 calc R . . C13 C -0.5331(3) 0.09672(18) 0.4253(3) 0.0308(8) Uani 1 1 d . . . H13 H -0.5729 0.0729 0.4651 0.037 Uiso 1 1 calc R . . C14 C -0.4866(3) 0.06599(18) 0.3482(3) 0.0314(8) Uani 1 1 d . . . C15 C -0.4893(4) 0.00140(19) 0.3460(4) 0.0408(10) Uani 1 1 d . . . H15 H -0.5227 -0.0198 0.3940 0.049 Uiso 1 1 calc R . . C16 C -0.4442(4) -0.0312(2) 0.2754(4) 0.0468(12) Uani 1 1 d . . . H16 H -0.4444 -0.0743 0.2764 0.056 Uiso 1 1 calc R . . C17 C -0.3985(3) 0.0001(2) 0.2029(3) 0.0413(11) Uani 1 1 d . . . H17 H -0.3684 -0.0220 0.1537 0.050 Uiso 1 1 calc R . . C18 C -0.3964(3) 0.0631(2) 0.2016(3) 0.0351(9) Uani 1 1 d . . . H18 H -0.3652 0.0832 0.1511 0.042 Uiso 1 1 calc R . . C19 C -0.4395(3) 0.09822(18) 0.2739(3) 0.0288(8) Uani 1 1 d . . . O3 O -0.6016(2) 0.24313(13) 0.2976(2) 0.0325(6) Uani 1 1 d . . . H3O H -0.635(4) 0.217(2) 0.298(4) 0.039 Uiso 1 1 d . . . C20 C -0.6570(4) 0.2988(2) 0.2983(4) 0.0513(13) Uani 1 1 d . . . H20A H -0.6878 0.3067 0.2337 0.077 Uiso 1 1 calc R . . H20B H -0.6117 0.3322 0.3175 0.077 Uiso 1 1 calc R . . H20C H -0.7095 0.2955 0.3440 0.077 Uiso 1 1 calc R . . N6 N -0.0862(3) 0.16969(14) 0.0596(2) 0.0289(7) Uani 1 1 d . . . C21 C -0.1601(4) 0.2209(2) 0.0768(4) 0.0428(14) Uani 0.836(6) 1 d P . . C22 C -0.2142(4) 0.2160(3) 0.1709(5) 0.0682(18) Uani 1 1 d . . . C23 C -0.1443(4) 0.1095(2) 0.0473(4) 0.0416(13) Uani 0.836(6) 1 d P . . C24 C -0.0843(5) 0.0549(2) 0.0162(5) 0.0625(16) Uani 1 1 d . . . C25 C -0.0058(4) 0.1635(3) 0.1449(4) 0.0428(14) Uani 0.836(6) 1 d P . . C26 C 0.0531(4) 0.2219(2) 0.1707(4) 0.0506(12) Uani 1 1 d . . . C27 C -0.0297(4) 0.1860(3) -0.0303(4) 0.0394(13) Uani 0.836(6) 1 d P . . C28 C -0.0973(5) 0.1867(3) -0.1239(3) 0.0591(15) Uani 1 1 d . . . C21' C -0.160(2) 0.1692(14) 0.148(2) 0.044(7) Uiso 0.164(6) 1 d P . . C23' C -0.040(2) 0.1038(15) 0.048(2) 0.048(8) Uiso 0.164(6) 1 d P . . C25' C -0.0085(19) 0.2220(11) 0.0697(18) 0.031(5) Uiso 0.164(6) 1 d P . . C27' C -0.161(2) 0.1845(12) -0.0341(19) 0.036(6) Uiso 0.164(6) 1 d P . . O4 O 0.3102(4) 0.3971(2) 0.4935(3) 0.0640(17) Uani 0.850(9) 1 d P A 1 C29 C 0.2808(5) 0.3696(3) 0.5757(5) 0.083(2) Uani 1 1 d . . . H29A H 0.2131 0.3832 0.5885 0.125 Uiso 0.850(9) 1 calc PR A 1 H29B H 0.3274 0.3806 0.6301 0.125 Uiso 1 1 calc R A 1 H29C H 0.2808 0.3255 0.5671 0.125 Uiso 1 1 calc R A 1 O4' O 0.212(2) 0.4047(13) 0.550(2) 0.068(10) Uiso 0.150(9) 1 d P A 2 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 Nb1 0.01646(13) 0.01819(13) 0.01866(14) 0.00124(11) 0.00066(10) -0.00130(11) Nb2 0.01596(13) 0.01760(13) 0.01844(14) 0.00037(11) -0.00023(10) 0.00182(11) Nb3 0.01737(14) 0.01857(13) 0.01672(13) -0.00070(11) -0.00103(10) 0.00001(11) Cl1 0.0258(4) 0.0265(4) 0.0260(4) -0.0025(3) -0.0011(3) -0.0083(3) Cl2 0.0234(4) 0.0291(4) 0.0236(4) -0.0011(3) -0.0069(3) 0.0052(3) Cl3 0.0266(4) 0.0192(4) 0.0268(4) 0.0046(3) 0.0024(3) 0.0011(3) Cl4 0.0170(4) 0.0282(4) 0.0319(4) 0.0028(3) 0.0044(3) 0.0011(3) Cl5 0.0268(4) 0.0278(4) 0.0185(4) 0.0018(3) 0.0027(3) -0.0016(3) Cl6 0.0284(4) 0.0222(4) 0.0230(4) -0.0044(3) -0.0002(3) 0.0053(3) N1 0.0345(19) 0.048(2) 0.040(2) 0.0108(17) -0.0004(16) -0.0137(17) N2 0.0246(16) 0.0282(16) 0.0375(18) -0.0004(14) -0.0013(14) 0.0040(13) N3 0.048(2) 0.050(2) 0.0327(19) -0.0104(17) -0.0033(17) -0.0040(19) C1 0.0220(17) 0.0323(19) 0.0277(18) 0.0056(15) -0.0003(14) -0.0033(15) C2 0.0230(17) 0.0239(16) 0.0254(17) -0.0025(14) 0.0006(14) -0.0002(14) C3 0.0267(18) 0.0304(18) 0.0275(19) -0.0026(15) 0.0025(15) -0.0006(15) Mn1 0.0210(3) 0.0228(3) 0.0235(3) 0.0014(2) 0.0039(2) 0.0010(2) O1 0.0306(14) 0.0257(13) 0.0328(14) 0.0026(11) 0.0105(12) -0.0003(11) O2 0.0351(15) 0.0276(13) 0.0265(13) -0.0024(11) 0.0046(11) 0.0003(11) N4 0.0218(15) 0.0306(16) 0.0240(15) 0.0011(12) 0.0036(12) 0.0010(12) N5 0.0235(15) 0.0266(15) 0.0261(15) 0.0055(12) 0.0033(12) -0.0001(12) C4 0.0202(17) 0.0284(18) 0.034(2) 0.0024(15) -0.0012(15) 0.0009(14) C5 0.034(2) 0.035(2) 0.043(2) 0.0065(18) 0.0057(18) -0.0057(17) C6 0.049(3) 0.038(2) 0.047(3) 0.015(2) -0.003(2) -0.015(2) C7 0.071(4) 0.027(2) 0.050(3) 0.005(2) -0.012(3) -0.010(2) C8 0.052(3) 0.029(2) 0.037(2) -0.0029(18) -0.006(2) -0.0002(19) C9 0.031(2) 0.0254(17) 0.0296(19) 0.0007(15) -0.0014(16) -0.0013(15) C10 0.0283(19) 0.034(2) 0.0279(19) -0.0055(16) 0.0025(15) 0.0017(16) C11 0.039(2) 0.036(2) 0.0264(19) 0.0027(16) 0.0094(17) -0.0026(18) C12 0.032(2) 0.038(2) 0.032(2) 0.0040(17) 0.0091(17) -0.0051(17) C13 0.029(2) 0.0314(19) 0.031(2) 0.0067(16) -0.0026(16) -0.0044(16) C14 0.0277(19) 0.0293(19) 0.036(2) 0.0006(16) -0.0082(16) -0.0025(15) C15 0.045(3) 0.027(2) 0.049(3) 0.0028(19) -0.007(2) -0.0050(18) C16 0.053(3) 0.031(2) 0.055(3) -0.009(2) -0.011(2) 0.003(2) C17 0.037(2) 0.037(2) 0.049(3) -0.018(2) -0.011(2) 0.0076(18) C18 0.028(2) 0.041(2) 0.035(2) -0.0084(18) -0.0036(16) 0.0031(17) C19 0.0237(18) 0.0291(18) 0.032(2) -0.0021(15) -0.0089(15) 0.0012(15) O3 0.0241(14) 0.0284(14) 0.0447(17) 0.0073(13) -0.0001(12) -0.0037(11) C20 0.051(3) 0.036(2) 0.064(3) 0.005(2) -0.013(3) 0.011(2) N6 0.0357(18) 0.0275(15) 0.0240(15) 0.0022(13) 0.0044(13) 0.0062(14) C21 0.040(3) 0.032(3) 0.056(4) -0.012(2) -0.001(3) 0.012(2) C22 0.050(3) 0.087(4) 0.071(4) -0.035(3) 0.027(3) -0.003(3) C23 0.045(3) 0.028(2) 0.052(3) -0.001(2) 0.012(3) -0.005(2) C24 0.082(4) 0.033(2) 0.071(4) -0.008(2) -0.006(3) 0.012(3) C25 0.048(3) 0.051(3) 0.028(3) 0.006(2) -0.007(2) 0.010(3) C26 0.046(3) 0.057(3) 0.046(3) -0.008(2) -0.014(2) 0.001(2) C27 0.046(3) 0.045(3) 0.027(2) 0.006(2) 0.007(2) -0.005(2) C28 0.079(4) 0.075(4) 0.022(2) 0.002(2) -0.006(2) -0.007(3) O4 0.056(3) 0.090(4) 0.046(3) -0.007(2) 0.005(2) -0.013(3) C29 0.067(4) 0.096(5) 0.086(5) 0.035(4) 0.005(4) 0.003(4)