#------------------------------------------------------------------------------ #$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000395.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_4000395 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C28 H62 Co3 N6 O31 P4' _chemical_formula_weight 1279.51 _space_group_IT_number 13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/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 106.8330(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 14.8651(14) _cell_length_b 7.5694(7) _cell_length_c 22.796(2) _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 2455.1(4) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Siemens Smart CCD' _diffrn_measurement_method 'narrow frame method' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 7145 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_min 2.66 _diffrn_standards_decay_% <1.0% _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_type SADABS _exptl_absorpt_process_details ? _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description brick _exptl_crystal_F_000 1322 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 327 _refine_ls_number_reflns 4268 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_gt 0.0625 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+4.1075P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1342 _refine_ls_wR_factor_ref 0.1636 _reflns_number_gt 2607 _reflns_number_total 4268 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M P2/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 4000395 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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 Co1 Co 0.0000 -0.05424(16) 0.7500 0.0269(3) Uani 1 2 d S . . Co2 Co -0.29523(6) 0.22187(12) 0.58450(4) 0.0284(3) Uani 1 1 d . . . P1 P -0.35865(12) -0.1616(3) 0.55148(8) 0.0340(5) Uani 1 1 d . . . P2 P -0.38109(13) 0.4055(3) 0.68101(8) 0.0381(5) Uani 1 1 d . . . N1 N 0.0025(4) -0.0420(7) 0.6560(2) 0.0279(13) Uani 1 1 d . . . N2 N -0.1905(4) 0.3449(7) 0.5514(2) 0.0280(13) Uani 1 1 d . . . N3 N -0.3785(3) 0.0714(7) 0.6364(2) 0.0300(13) Uani 1 1 d . . . C1 C -0.4419(5) 0.2002(10) 0.6534(3) 0.0382(18) Uani 1 1 d . . . H1A H -0.4657 0.1497 0.6850 0.046 Uiso 1 1 calc R . . H1B H -0.4950 0.2242 0.6179 0.046 Uiso 1 1 calc R . . C2 C -0.3105(4) -0.0093(9) 0.6909(3) 0.0316(16) Uani 1 1 d . . . H2A H -0.3232 -0.1350 0.6913 0.038 Uiso 1 1 calc R . . H2B H -0.3200 0.0417 0.7277 0.038 Uiso 1 1 calc R . . C3 C -0.2098(4) 0.0166(9) 0.6923(3) 0.0272(15) Uani 1 1 d . . . C4 C -0.4320(5) -0.0684(9) 0.5949(3) 0.0358(17) Uani 1 1 d . . . H4A H -0.4885 -0.0183 0.5671 0.043 Uiso 1 1 calc R . . H4B H -0.4505 -0.1603 0.6187 0.043 Uiso 1 1 calc R . . C10 C -0.0708(5) -0.0919(9) 0.5498(3) 0.0312(16) Uani 1 1 d . . . H10A H -0.1217 -0.1387 0.5199 0.037 Uiso 1 1 calc R . . C11 C -0.0670(5) -0.1064(9) 0.6106(3) 0.0305(16) Uani 1 1 d . . . H11A H -0.1158 -0.1646 0.6204 0.037 Uiso 1 1 calc R . . C12 C 0.0709(5) 0.0423(10) 0.6397(3) 0.0375(18) Uani 1 1 d . . . H12A H 0.1199 0.0914 0.6705 0.045 Uiso 1 1 calc R . . C13 C 0.0728(4) 0.0602(10) 0.5800(3) 0.0340(17) Uani 1 1 d . . . H13A H 0.1226 0.1184 0.5714 0.041 Uiso 1 1 calc R . . C14 C 0.0005(4) -0.0082(8) 0.5329(3) 0.0265(15) Uani 1 1 d . . . C20 C -0.1109(5) 0.4056(11) 0.5895(3) 0.046(2) Uani 1 1 d . . . H20A H -0.1058 0.4051 0.6312 0.055 Uiso 1 1 calc R . . C21 C -0.1222(5) 0.4078(10) 0.4704(3) 0.0387(19) Uani 1 1 d . . . H21A H -0.1291 0.4066 0.4285 0.046 Uiso 1 1 calc R . . C22 C -0.0361(5) 0.4686(10) 0.5722(3) 0.0384(18) Uani 1 1 d . . . H22A H 0.0168 0.5113 0.6015 0.046 Uiso 1 1 calc R . . C23 C -0.1955(4) 0.3481(10) 0.4925(3) 0.0356(17) Uani 1 1 d . . . H23A H -0.2504 0.3088 0.4643 0.043 Uiso 1 1 calc R . . C24 C -0.0398(4) 0.4683(8) 0.5107(3) 0.0245(14) Uani 1 1 d . . . O1 O -0.1905(3) 0.1281(6) 0.65694(19) 0.0349(12) Uani 1 1 d . . . O2 O -0.1485(3) -0.0728(6) 0.73047(18) 0.0326(11) Uani 1 1 d . . . O11 O -0.4170(3) -0.2806(6) 0.5027(2) 0.0405(12) Uani 1 1 d . . . O12 O -0.3133(3) -0.0060(6) 0.53011(19) 0.0357(12) Uani 1 1 d . . . O13 O -0.2772(3) -0.2650(6) 0.5985(2) 0.0385(12) Uani 1 1 d . . . H13B H -0.2982 -0.3563 0.6088 0.058 Uiso 1 1 calc R . . O21 O -0.3181(3) 0.3707(7) 0.7482(2) 0.0504(14) Uani 1 1 d . . . H21B H -0.3444 0.4094 0.7726 0.076 Uiso 1 1 calc R . . O22 O -0.4524(3) 0.5451(7) 0.6787(2) 0.0471(13) Uani 1 1 d . . . O23 O -0.3135(3) 0.4353(6) 0.6428(2) 0.0438(13) Uani 1 1 d . . . O1W O 0.0000 0.2266(9) 0.7500 0.081(3) Uani 1 2 d S . . O2W O 0.0000 -0.3296(9) 0.7500 0.057(2) Uani 1 2 d S . . O3W O -0.3997(3) 0.3465(6) 0.5143(2) 0.0404(12) Uani 1 1 d . . . O4W O -0.3622(4) 0.4622(8) 0.8478(2) 0.0600(16) Uani 1 1 d . . . O5W O -0.5000 0.7966(10) 0.7500 0.061(2) Uani 1 2 d S . . O6W O -0.2976(4) 0.1401(10) 0.9127(3) 0.080(2) Uani 1 1 d . . . O7W O -0.3238(5) 0.8416(11) 0.8406(3) 0.101(2) Uani 1 1 d . . . O8W O -0.1274(7) 0.4342(13) 0.7476(5) 0.152(4) Uani 1 1 d . . . O9W O -0.1667(5) 0.6504(12) 0.8096(3) 0.136(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 0.0348(7) 0.0289(7) 0.0167(6) 0.000 0.0069(5) 0.000 Co2 0.0219(5) 0.0420(6) 0.0224(4) 0.0007(4) 0.0082(4) -0.0079(5) P1 0.0272(10) 0.0461(12) 0.0292(9) -0.0060(8) 0.0089(8) -0.0122(9) P2 0.0329(11) 0.0517(13) 0.0346(10) -0.0121(9) 0.0173(9) -0.0088(10) N1 0.035(3) 0.029(3) 0.021(3) -0.002(2) 0.010(2) -0.011(3) N2 0.026(3) 0.036(3) 0.023(3) 0.005(2) 0.008(2) -0.001(3) N3 0.022(3) 0.046(4) 0.022(3) -0.005(3) 0.007(2) -0.009(3) C1 0.023(4) 0.064(5) 0.031(4) -0.009(4) 0.013(3) -0.009(4) C2 0.030(4) 0.039(4) 0.025(3) -0.003(3) 0.006(3) -0.013(3) C3 0.030(4) 0.034(4) 0.019(3) 0.002(3) 0.008(3) -0.008(3) C4 0.034(4) 0.046(5) 0.030(4) -0.003(3) 0.013(3) -0.014(4) C10 0.032(4) 0.043(4) 0.021(3) -0.004(3) 0.011(3) -0.006(3) C11 0.030(4) 0.036(4) 0.028(3) -0.006(3) 0.013(3) -0.007(3) C12 0.035(4) 0.052(5) 0.021(3) 0.003(3) 0.001(3) -0.010(4) C13 0.023(3) 0.054(5) 0.024(3) 0.003(3) 0.006(3) -0.008(4) C14 0.028(4) 0.030(4) 0.020(3) 0.001(3) 0.004(3) 0.005(3) C20 0.039(4) 0.076(6) 0.026(4) 0.002(4) 0.016(3) -0.014(4) C21 0.031(4) 0.064(5) 0.024(3) -0.003(3) 0.013(3) -0.017(4) C22 0.030(4) 0.065(5) 0.021(3) 0.001(3) 0.009(3) -0.024(4) C23 0.019(3) 0.059(5) 0.026(3) 0.004(3) 0.002(3) -0.016(4) C24 0.023(3) 0.024(3) 0.026(3) 0.001(3) 0.007(3) -0.004(3) O1 0.027(3) 0.048(3) 0.026(2) 0.008(2) 0.004(2) -0.010(2) O2 0.037(3) 0.037(3) 0.024(2) 0.004(2) 0.011(2) -0.005(2) O11 0.031(3) 0.052(3) 0.038(3) -0.014(2) 0.009(2) -0.010(3) O12 0.035(3) 0.048(3) 0.030(2) -0.003(2) 0.018(2) -0.009(2) O13 0.028(3) 0.047(3) 0.040(3) 0.002(2) 0.010(2) -0.009(2) O21 0.035(3) 0.076(4) 0.038(3) -0.018(3) 0.009(2) 0.001(3) O22 0.044(3) 0.052(3) 0.052(3) -0.009(3) 0.024(3) -0.003(3) O23 0.046(3) 0.044(3) 0.054(3) -0.016(3) 0.034(3) -0.019(3) O1W 0.184(10) 0.027(4) 0.031(4) 0.000 0.030(5) 0.000 O2W 0.100(7) 0.026(4) 0.059(5) 0.000 0.045(5) 0.000 O3W 0.026(3) 0.047(3) 0.043(3) -0.007(2) 0.002(2) -0.001(2) O4W 0.055(3) 0.078(4) 0.047(3) -0.005(3) 0.017(3) 0.002(3) O5W 0.068(6) 0.059(5) 0.060(5) 0.000 0.028(4) 0.000 O6W 0.065(4) 0.129(6) 0.053(4) -0.003(4) 0.027(3) 0.006(4) O7W 0.095(5) 0.110(6) 0.090(5) -0.013(5) 0.016(4) -0.009(5) O8W 0.119(7) 0.148(9) 0.187(10) -0.030(8) 0.040(7) -0.015(7) O9W 0.086(5) 0.185(9) 0.101(6) 0.084(6) -0.029(4) -0.072(6)