#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000285.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_4000285 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'C4 H18 Co2 N2 O14 P4' _chemical_formula_weight 559.94 _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4635(13) _cell_length_b 7.7205(18) _cell_length_c 9.976(2) _cell_angle_alpha 71.198(4) _cell_angle_beta 82.385(4) _cell_angle_gamma 87.920(5) _cell_volume 394.82(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 808 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.53 _exptl_crystal_description 'needle' _exptl_crystal_colour 'purple red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 282 _exptl_absorpt_coefficient_mu 2.586 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_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 'Siemens SMART CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 2423 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1692 _reflns_number_gt 1349 _reflns_threshold_expression >2sigma(I) _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^)+(0.0227P)^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 1692 _refine_ls_number_parameters 136 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.32661(8) 0.36145(7) 0.63245(5) 0.01382(15) Uani 1 1 d . . . P1 P 0.78609(17) 0.14085(13) 0.74886(10) 0.0134(2) Uani 1 1 d . . . P2 P 0.78276(17) 0.54148(12) 0.70721(10) 0.0128(2) Uani 1 1 d . . . O1 O 0.6050(4) 0.1608(3) 0.6428(2) 0.0161(6) Uani 1 1 d . . . O2 O 1.0554(4) 0.1573(3) 0.6897(3) 0.0183(6) Uani 1 1 d . . . O3 O 0.7378(5) -0.0477(3) 0.8726(3) 0.0189(6) Uani 1 1 d . . . H3 H 0.729(7) -0.117(6) 0.837(4) 0.026 Uiso 1 1 d . . . O4 O 0.6250(4) 0.5562(3) 0.5872(2) 0.0145(5) Uani 1 1 d . . . O5 O 1.0579(4) 0.5370(3) 0.6630(3) 0.0174(6) Uani 1 1 d . . . O6 O 0.7126(4) 0.6866(3) 0.7765(3) 0.0189(6) Uani 1 1 d . . . O7 O 0.4257(4) 0.3119(3) 0.8538(3) 0.0163(6) Uani 1 1 d D . . H7 H 0.374(6) 0.216(3) 0.929(2) 0.023 Uiso 1 1 d D . . C1 C 0.7947(6) 0.2857(5) 0.9772(4) 0.0199(9) Uani 1 1 d . . . H1A H 0.7486 0.1659 1.0413 0.030 Uiso 1 1 calc R . . H1B H 0.7263 0.3762 1.0183 0.030 Uiso 1 1 calc R . . H1C H 0.9714 0.2970 0.9610 0.030 Uiso 1 1 calc R . . C2 C 0.6965(6) 0.3142(5) 0.8365(4) 0.0131(8) Uani 1 1 d . . . N1 N 1.2946(6) 0.8523(5) 0.6397(4) 0.0211(8) Uani 1 1 d . . . H11 H 1.434(7) 0.824(5) 0.691(4) 0.029 Uiso 1 1 d . . . H12 H 1.324(7) 0.861(5) 0.555(4) 0.029 Uiso 1 1 d . . . H13 H 1.168(7) 0.760(5) 0.660(4) 0.029 Uiso 1 1 d . . . H14 H 1.221(6) 0.968(5) 0.650(4) 0.029 Uiso 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 0.0118(3) 0.0143(3) 0.0151(3) -0.0046(2) -0.0006(2) -0.00059(19) P1 0.0130(5) 0.0116(5) 0.0156(5) -0.0050(4) -0.0006(4) -0.0009(4) P2 0.0123(5) 0.0115(5) 0.0152(5) -0.0050(4) -0.0023(4) 0.0000(4) O1 0.0144(13) 0.0183(14) 0.0182(14) -0.0091(11) -0.0036(11) 0.0020(10) O2 0.0121(13) 0.0156(14) 0.0281(15) -0.0105(12) 0.0037(11) -0.0016(10) O3 0.0282(16) 0.0115(14) 0.0181(14) -0.0060(11) -0.0028(12) -0.0018(11) O4 0.0124(13) 0.0172(14) 0.0135(12) -0.0042(11) -0.0008(10) -0.0031(10) O5 0.0126(13) 0.0131(14) 0.0260(14) -0.0063(11) -0.0006(11) 0.0001(10) O6 0.0203(15) 0.0165(14) 0.0222(14) -0.0091(12) -0.0043(11) 0.0019(11) O7 0.0120(13) 0.0182(15) 0.0167(14) -0.0037(11) 0.0005(11) -0.0003(11) C1 0.019(2) 0.024(2) 0.0159(19) -0.0059(17) -0.0017(16) -0.0008(16) C2 0.0073(18) 0.017(2) 0.0151(18) -0.0069(16) 0.0036(15) -0.0009(14) N1 0.0166(19) 0.0210(19) 0.029(2) -0.0127(17) -0.0040(16) 0.0004(14) _cod_database_code 4000285