#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000474.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_4000474 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _publ_section_title ; Assembly of Hybrid Inorganic-Organic Materials from Octahedral Nb6 Clusters and Metal Complexes ; loop_ _publ_author_name 'Huajun Zhou' 'Cynthia S. Day ' 'Abdessadek Lachgar' _chemical_formula_sum 'C24 H56 Cl12 N10 Nb6 O2' _chemical_formula_weight 1499.65 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 14.086(3) _cell_length_b 20.057(4) _cell_length_c 20.938(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5915(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3966 _cell_measurement_theta_min 3.893 _cell_measurement_theta_max 22.705 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ; Data were corrected for absorption effects using the multiscan technique (SADABS). The ratio of minimum to maximum apparent transmission was 0.79. ; _diffrn_ambient_temperature 193(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 'Bruker SMART APEX 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 25560 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3521 _reflns_number_gt 2647 _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^)+(0.0640P)^2^+7.7140P] 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 3521 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 Nb1 Nb 0.0000 0.05760(3) 0.41787(3) 0.04018(17) Uani 1 2 d S . . Nb2 Nb 0.10399(3) 0.06036(2) 0.539108(19) 0.03939(15) Uani 1 1 d . . . Cl1 Cl 0.12381(9) 0.13859(6) 0.44897(6) 0.0509(3) Uani 1 1 d . . . Cl2 Cl 0.12184(9) -0.00346(7) 0.35770(5) 0.0528(3) Uani 1 1 d . . . Cl3 Cl 0.24476(12) 0.0000 0.5000 0.0480(4) Uani 1 2 d S . . Cl4 Cl 0.0000 0.14213(9) 0.59267(9) 0.0524(4) Uani 1 2 d S . . C1 C 0.0000 0.1197(4) 0.3265(4) 0.0559(19) Uani 1 2 d S . . C2 C 0.2178(4) 0.1278(3) 0.5821(3) 0.0596(14) Uani 1 1 d . . . C3 C 0.5000 0.0905(4) 0.5102(5) 0.089(3) Uani 1 2 d S . . H3A H 0.5000 0.0675 0.4689 0.133 Uiso 1 2 calc SR . . H3B H 0.4432 0.0778 0.5343 0.133 Uiso 0.50 1 calc PR . . H3C H 0.5568 0.0778 0.5343 0.133 Uiso 0.50 1 calc PR . . C4 C 0.5000 0.1995(5) 0.5626(5) 0.080(3) Uani 1 2 d S . . H4A H 0.5573 0.1877 0.5866 0.119 Uiso 0.50 1 calc PR . . H4B H 0.4437 0.1867 0.5872 0.119 Uiso 0.50 1 calc PR . . H4C H 0.4990 0.2477 0.5551 0.119 Uiso 1 2 calc SR . . C5 C 0.4127(5) 0.1829(4) 0.4632(3) 0.087(2) Uani 1 1 d . . . H5A H 0.4122 0.1599 0.4218 0.130 Uiso 1 1 calc R . . H5B H 0.4127 0.2312 0.4562 0.130 Uiso 1 1 calc R . . H5C H 0.3562 0.1702 0.4876 0.130 Uiso 1 1 calc R . . C6 C 0.2526(5) 0.3050(3) 0.6921(3) 0.0761(18) Uani 1 1 d . . . H6A H 0.3091 0.3335 0.6932 0.114 Uiso 1 1 calc R . . H6B H 0.1956 0.3329 0.6905 0.114 Uiso 1 1 calc R . . H6C H 0.2550 0.2765 0.6540 0.114 Uiso 1 1 calc R . . C7 C 0.1632(4) 0.2193(3) 0.7478(3) 0.0665(15) Uani 1 1 d . . . H7A H 0.1610 0.1912 0.7860 0.100 Uiso 1 1 calc R . . H7B H 0.1656 0.1910 0.7097 0.100 Uiso 1 1 calc R . . H7C H 0.1063 0.2474 0.7462 0.100 Uiso 1 1 calc R . . O1 O 0.4347(12) 0.0944(9) 0.3384(8) 0.170(6) Uiso 0.50 1 d P . . N1 N 0.0000 0.1487(4) 0.2800(3) 0.072(2) Uani 1 2 d S . . N2 N 0.2749(4) 0.1601(3) 0.6037(3) 0.0839(17) Uani 1 1 d . . . N3 N 0.5000 0.1634(3) 0.4996(3) 0.0627(17) Uani 1 2 d S . . N4 N 0.2500 0.2628(3) 0.7500 0.0560(15) Uani 1 2 d S . . C8 C 0.3712(15) 0.0128(10) 0.3237(11) 0.126(6) 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 Nb1 0.0437(3) 0.0433(3) 0.0336(3) 0.0044(2) 0.000 0.000 Nb2 0.0417(3) 0.0416(2) 0.0349(2) -0.00350(17) -0.00087(16) -0.00302(17) Cl1 0.0538(7) 0.0461(7) 0.0526(7) 0.0066(5) 0.0017(6) -0.0093(5) Cl2 0.0521(7) 0.0716(8) 0.0346(6) 0.0018(5) 0.0071(5) 0.0055(6) Cl3 0.0403(8) 0.0584(10) 0.0454(9) -0.0049(7) 0.000 0.000 Cl4 0.0581(10) 0.0473(9) 0.0519(10) -0.0153(8) 0.000 0.000 C1 0.050(4) 0.068(5) 0.050(4) 0.020(4) 0.000 0.000 C2 0.057(3) 0.067(3) 0.054(3) -0.017(3) 0.005(3) -0.013(3) C3 0.124(9) 0.046(5) 0.095(7) 0.009(5) 0.000 0.000 C4 0.064(5) 0.074(6) 0.101(7) -0.024(5) 0.000 0.000 C5 0.075(5) 0.099(6) 0.087(5) 0.016(4) -0.016(4) -0.005(4) C6 0.092(5) 0.076(4) 0.060(4) 0.010(3) -0.004(3) -0.005(4) C7 0.059(4) 0.081(4) 0.059(3) -0.007(3) 0.006(3) -0.008(3) N1 0.069(5) 0.086(5) 0.062(4) 0.029(4) 0.000 0.000 N2 0.076(4) 0.101(4) 0.074(3) -0.035(3) 0.007(3) -0.039(3) N3 0.062(4) 0.050(4) 0.077(5) 0.012(3) 0.000 0.000 N4 0.058(4) 0.063(4) 0.047(3) 0.000 0.001(3) 0.000