#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000196.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_4000196 _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_formula_sum 'Cl14.36 Nb6 O4.64 Rb1.76 Ti2' _chemical_formula_weight 1386.87 _symmetry_cell_setting Monoclinic _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.503(3) _cell_length_b 8.8162(11) _cell_length_c 15.710(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.207(10) _cell_angle_gamma 90.00 _cell_volume 2672.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2545 _exptl_absorpt_coefficient_mu 7.673 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4533 _exptl_absorpt_correction_T_max 0.606 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4087 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.32 _reflns_number_total 3363 _reflns_number_gt 2394 _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^)+(0.0375P)^2^+2.6679P] 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 SHELXL _refine_ls_extinction_coef 0.00014(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3363 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.49971(3) 0.12697(7) 0.10931(4) 0.01704(13) Uani 1 1 d . . . Nb2 Nb 0.58320(3) -0.11441(7) 0.10015(4) 0.02102(15) Uani 1 1 d . . . Nb3 Nb 0.43179(3) -0.14051(7) 0.01985(4) 0.02288(15) Uani 1 1 d . . . Rb1 Rb 0.6665(2) 0.4103(2) 0.33203(14) 0.0551(9) Uani 0.577(8) 1 d P . . Rb2 Rb 0.7060(4) 0.4309(5) 0.3444(3) 0.0448(16) Uani 0.302(8) 1 d P . . Ti1 Ti 0.36317(6) -0.07369(15) 0.17056(8) 0.0229(3) Uani 1 1 d . . . Cl1 Cl 0.5000 0.2845(3) 0.2500 0.0273(5) Uani 1 2 d S . . Cl2 Cl 0.40334(10) 0.3012(2) 0.00902(12) 0.0285(4) Uani 1 1 d . . . Cl3 Cl 0.57969(10) 0.3314(2) 0.10356(13) 0.0333(4) Uani 1 1 d . . . Cl4 Cl 0.51785(11) -0.3105(2) 0.14097(14) 0.0363(4) Uani 1 1 d . . . Cl5 Cl 0.68909(11) -0.2278(3) 0.24559(13) 0.0423(5) Uani 1 1 d . . . Cl6 Cl 0.34642(13) -0.2878(3) 0.06648(17) 0.0526(7) Uani 1 1 d . . . Cl7 Cl 0.27258(11) 0.0828(3) 0.09028(17) 0.0504(6) Uani 1 1 d . . . Cl8 Cl 0.32814(14) 0.9639(3) 0.90652(17) 0.0423(10) Uani 0.683(14) 1 d P . . O8 O 0.32814(14) 0.9639(3) 0.90652(17) 0.0423(10) Uani 0.317(14) 1 d P . . O1 O 0.4311(2) -0.0091(5) 0.1238(3) 0.0208(10) Uani 1 1 d . . . O2 O 0.4187(2) 0.0129(5) 0.2937(3) 0.0235(10) 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 Nb1 0.0193(3) 0.0200(3) 0.0142(3) 0.0003(2) 0.0097(2) 0.0016(2) Nb2 0.0236(3) 0.0264(3) 0.0141(3) 0.0026(2) 0.0093(2) 0.0074(3) Nb3 0.0284(3) 0.0257(3) 0.0215(3) -0.0048(2) 0.0174(3) -0.0056(3) Rb1 0.054(2) 0.0477(11) 0.0582(12) -0.0083(8) 0.0199(10) -0.0166(9) Rb2 0.040(3) 0.0421(19) 0.056(2) -0.0093(15) 0.0253(19) -0.0003(18) Ti1 0.0220(6) 0.0328(7) 0.0167(6) -0.0048(5) 0.0111(5) -0.0055(5) Cl1 0.0430(14) 0.0225(11) 0.0236(11) 0.000 0.0213(11) 0.000 Cl2 0.0348(9) 0.0301(9) 0.0236(8) 0.0043(7) 0.0157(7) 0.0142(8) Cl3 0.0455(11) 0.0319(9) 0.0345(10) -0.0134(8) 0.0286(9) -0.0141(8) Cl4 0.0525(12) 0.0283(9) 0.0398(10) 0.0128(8) 0.0309(10) 0.0089(9) Cl5 0.0452(12) 0.0582(13) 0.0239(9) 0.0085(9) 0.0156(8) 0.0325(10) Cl6 0.0746(16) 0.0487(13) 0.0642(14) -0.0305(11) 0.0577(13) -0.0372(12) Cl7 0.0326(11) 0.0583(14) 0.0490(13) 0.0023(11) 0.0077(9) 0.0109(10) Cl8 0.0432(17) 0.0594(19) 0.0278(14) 0.0013(12) 0.0189(12) 0.0057(13) O8 0.0432(17) 0.0594(19) 0.0278(14) 0.0013(12) 0.0189(12) 0.0057(13) O1 0.024(2) 0.026(2) 0.018(2) -0.0015(19) 0.014(2) 0.002(2) O2 0.020(2) 0.034(3) 0.016(2) -0.004(2) 0.0070(19) -0.004(2)