#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/19/2011900.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011900 loop_ _publ_author_name 'Tillinski, Ralf' 'N\"ather, Christian' 'Bensch, Wolfgang' _publ_section_title ; RbCu~2~VS~4~ ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 333 _journal_page_last 334 _journal_paper_doi 10.1107/S0108270100019442 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'Rb Cu2 V S4' _chemical_formula_sum 'Cu2 Rb S4 V' _chemical_formula_weight 391.73 _chemical_name_common Rubidiumdicoppervanadiumtetrasulfide _chemical_name_systematic Rubidiumdicoppervanadiumtetrasulfide _space_group_IT_number 40 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'A 2 -2a' _symmetry_space_group_name_H-M 'A m a 2' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.382(3) _cell_length_b 18.187(11) _cell_length_c 5.413(2) _cell_measurement_reflns_used 10 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24 _cell_measurement_theta_min 13 _cell_volume 726.7(6) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1991)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1991)' _computing_publication_material 'CIFTAB in SHELXL93' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.0 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device 'STOE AED-II four-circle' _diffrn_measurement_method \w--\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .055 _diffrn_reflns_av_sigmaI/netI .0608 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 1230 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.24 _diffrn_standards_decay_% negligible _diffrn_standards_interval_time 'every 2 h' _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 14.744 _exptl_absorpt_correction_T_max .345 _exptl_absorpt_correction_T_min .290 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(XEMP in SHELXTL/PC; Siemens, 1990)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 728 _exptl_crystal_size_max .08 _exptl_crystal_size_mid .075 _exptl_crystal_size_min .07 _refine_diff_density_max .949 _refine_diff_density_min -.659 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 46 _refine_ls_number_reflns 628 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.038 _refine_ls_restrained_S_obs 1.079 _refine_ls_R_factor_all .058 _refine_ls_R_factor_gt .033 _refine_ls_shift/esd_max <0.001 _refine_ls_shift/esd_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .078 _reflns_number_observed 483 _reflns_number_total 628 _reflns_observed_criterion I>2\s(I) _cod_data_source_file sk1402.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17 times). '_geom_bond_publ_flag' value 'N' changed to 'n' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (29 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17 times). '_geom_bond_publ_flag' value 'N' changed to 'n' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (29 times). '_geom_angle_publ_flag' value 'Y' changed to 'y' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (14 times). '_geom_angle_publ_flag' value 'N' changed to 'n' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (206 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011900 _cod_database_fobs_code 2011900 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y, z' '-x+1/2, y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V .0132(12) .0164(12) .013(2) .000 .000 .000(2) Cu1 .0150(7) .0242(9) .0249(10) -.0039(8) .000 .000 Cu2 .0224(10) .0252(11) .0136(12) .000 .000 .0029(14) S1 .041(2) .016(2) .017(2) .000 .000 .004(3) S2 .0152(10) .0265(11) .0164(13) .0031(9) -.001(3) -.0014(13) S3 .0162(14) .0157(15) .015(2) .000 .000 -.001(3) Rb .0336(8) .0271(7) .0274(8) .000 .000 .0048(13) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol V .2500 .10888(13) .6036(7) .0143(6) Uani d S 1 . V Cu1 .0000 .0000 .6253(4) .0214(5) Uani d S 1 . Cu Cu2 .2500 .10573(10) .1029(4) .0204(6) Uani d S 1 . Cu S1 .2500 .2040(2) .3668(17) .0248(9) Uani d S 1 . S S2 .0076(3) .10917(14) .8357(7) .0194(5) Uani d . 1 . S S3 .2500 .0076(2) .3709(8) .0157(7) Uani d S 1 . S Rb .7500 .18224(8) .3550(6) .0294(4) Uani d S 1 . Rb loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rb Rb -.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V .3005 .5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 V S2 . 4 109.88(14) y S1 V S2 . . 109.88(14) n S2 V S2 4 . 109.9(3) y S1 V S3 . . 109.1(2) y S2 V S3 4 . 109.05(12) y S2 V S3 . . 109.05(12) n S1 V Cu2 . 1_556 127.7(2) n S2 V Cu2 4 1_556 54.94(14) n S2 V Cu2 . 1_556 54.94(14) n S3 V Cu2 . 1_556 123.2(2) n S1 V Cu1 . . 127.81(14) n S2 V Cu1 4 . 122.3(2) n S2 V Cu1 . . 54.51(8) n S3 V Cu1 . . 54.63(9) n Cu2 V Cu1 1_556 . 86.63(10) n S1 V Cu1 . 3 127.81(13) n S2 V Cu1 4 3 54.51(8) n S2 V Cu1 . 3 122.3(2) n S3 V Cu1 . 3 54.63(9) n Cu2 V Cu1 1_556 3 86.63(10) n Cu1 V Cu1 . 3 85.87(8) n S1 V Cu2 . . 54.7(2) n S2 V Cu2 4 . 125.07(14) n S2 V Cu2 . . 125.07(14) n S3 V Cu2 . . 54.43(12) n Cu2 V Cu2 1_556 . 177.58(14) n Cu1 V Cu2 . . 91.60(11) n Cu1 V Cu2 3 . 91.60(11) n S1 V Rb . 6_655 56.2(2) n S2 V Rb 4 6_655 78.70(11) n S2 V Rb . 6_655 78.70(11) n S3 V Rb . 6_655 165.3(2) n Cu2 V Rb 1_556 6_655 71.51(10) n Cu1 V Rb . 6_655 132.33(8) n Cu1 V Rb 3 6_655 132.33(8) n Cu2 V Rb . 6_655 110.91(11) n S1 V Rb . 1_455 63.16(5) n S2 V Rb 4 1_455 156.0(2) n S2 V Rb . 1_455 57.15(10) n S3 V Rb . 1_455 94.72(9) n Cu2 V Rb 1_556 1_455 109.34(8) n Cu1 V Rb . 1_455 69.09(5) n Cu1 V Rb 3 1_455 148.76(10) n Cu2 V Rb . 1_455 71.49(7) n Rb V Rb 6_655 1_455 78.85(4) n S1 V Rb . . 63.16(5) n S2 V Rb 4 . 57.15(10) n S2 V Rb . . 156.0(2) n S3 V Rb . . 94.72(9) n Cu2 V Rb 1_556 . 109.34(8) n Cu1 V Rb . . 148.76(10) n Cu1 V Rb 3 . 69.09(5) n Cu2 V Rb . . 71.49(7) n Rb V Rb 6_655 . 78.85(4) n Rb V Rb 1_455 . 125.64(11) n S2 Cu1 S2 . 2 120.4(2) y S2 Cu1 S3 . 2 111.61(10) y S2 Cu1 S3 2 2 103.03(11) y S2 Cu1 S3 . . 103.03(11) n S2 Cu1 S3 2 . 111.61(10) n S3 Cu1 S3 2 . 106.7(2) y S2 Cu1 V . . 51.02(11) n S2 Cu1 V 2 . 132.23(9) n S3 Cu1 V 2 . 124.24(14) n S3 Cu1 V . . 52.09(10) n S2 Cu1 V . 2 132.23(9) n S2 Cu1 V 2 2 51.02(11) n S3 Cu1 V 2 2 52.09(10) n S3 Cu1 V . 2 124.24(14) n V Cu1 V . 2 175.0(2) y S2 Cu1 Rb . 2_655 151.01(6) n S2 Cu1 Rb 2 2_655 58.89(9) n S3 Cu1 Rb 2 2_655 95.72(10) n S3 Cu1 Rb . 2_655 58.04(9) n V Cu1 Rb . 2_655 105.72(6) n V Cu1 Rb 2 2_655 72.41(6) n S2 Cu1 Rb . 1_455 58.89(9) n S2 Cu1 Rb 2 1_455 151.01(6) n S3 Cu1 Rb 2 1_455 58.04(9) n S3 Cu1 Rb . 1_455 95.72(10) n V Cu1 Rb . 1_455 72.41(6) n V Cu1 Rb 2 1_455 105.72(6) n Rb Cu1 Rb 2_655 1_455 137.81(11) n S1 Cu2 S3 . . 102.3(2) y S1 Cu2 S2 . 1_554 111.79(13) y S3 Cu2 S2 . 1_554 114.67(12) y S1 Cu2 S2 . 4_554 111.79(13) n S3 Cu2 S2 . 4_554 114.67(12) n S2 Cu2 S2 1_554 4_554 102.0(2) y S1 Cu2 V . 1_554 127.4(2) n S3 Cu2 V . 1_554 130.30(15) n S2 Cu2 V 1_554 1_554 51.02(11) n S2 Cu2 V 4_554 1_554 51.02(10) n S1 Cu2 V . . 50.2(2) n S3 Cu2 V . . 52.12(12) n S2 Cu2 V 1_554 . 128.89(10) n S2 Cu2 V 4_554 . 128.89(10) n V Cu2 V 1_554 . 177.58(14) y S1 Cu2 Rb . 6_654 57.8(2) n S3 Cu2 Rb . 6_654 160.11(13) n S2 Cu2 Rb 1_554 6_654 76.57(10) n S2 Cu2 Rb 4_554 6_654 76.57(10) n V Cu2 Rb 1_554 6_654 69.60(9) n V Cu2 Rb . 6_654 107.99(9) n S1 Cu2 Rb . . 62.32(4) n S3 Cu2 Rb . . 93.02(7) n S2 Cu2 Rb 1_554 . 152.10(13) n S2 Cu2 Rb 4_554 . 60.59(10) n V Cu2 Rb 1_554 . 108.65(6) n V Cu2 Rb . . 70.50(6) n Rb Cu2 Rb 6_654 . 78.03(3) n S1 Cu2 Rb . 1_455 62.32(4) n S3 Cu2 Rb . 1_455 93.02(7) n S2 Cu2 Rb 1_554 1_455 60.59(10) n S2 Cu2 Rb 4_554 1_455 152.10(13) n V Cu2 Rb 1_554 1_455 108.65(6) n V Cu2 Rb . 1_455 70.50(6) n Rb Cu2 Rb 6_654 1_455 78.03(3) n Rb Cu2 Rb . 1_455 124.34(8) n V S1 Cu2 . . 75.16(14) n V S1 Rb . 6_655 91.5(3) n Cu2 S1 Rb . 6_655 166.7(3) n V S1 Rb . 6_654 163.3(3) n Cu2 S1 Rb . 6_654 88.1(3) n Rb S1 Rb 6_655 6_654 105.20(11) n V S1 Rb . 1_455 85.67(11) n Cu2 S1 Rb . 1_455 84.60(11) n Rb S1 Rb 6_655 1_455 94.55(15) n Rb S1 Rb 6_654 1_455 92.9(2) n V S1 Rb . . 85.67(11) n Cu2 S1 Rb . . 84.60(11) n Rb S1 Rb 6_655 . 94.5(2) n Rb S1 Rb 6_654 . 92.9(2) n Rb S1 Rb 1_455 . 167.60(11) n V S2 Cu1 . . 74.47(13) n V S2 Cu2 . 1_556 74.03(11) n Cu1 S2 Cu2 . 1_556 107.95(11) n V S2 Rb . 1_455 91.1(2) n Cu1 S2 Rb . 1_455 86.90(10) n Cu2 S2 Rb 1_556 1_455 154.63(13) n V S2 Rb . 1_456 150.59(14) n Cu1 S2 Rb . 1_456 133.39(10) n Cu2 S2 Rb 1_556 1_456 86.03(13) n Rb S2 Rb 1_455 1_456 98.74(7) n V S3 Cu2 . . 73.45(14) n V S3 Cu1 . 3 73.28(12) n Cu2 S3 Cu1 . 3 115.01(10) n V S3 Cu1 . . 73.28(12) n Cu2 S3 Cu1 . . 115.01(10) n Cu1 S3 Cu1 3 . 106.3(2) n V S3 Rb . 2_655 147.1(2) n Cu2 S3 Rb . 2_655 139.5(2) n Cu1 S3 Rb 3 2_655 87.44(9) n Cu1 S3 Rb . 2_655 87.44(9) n S1 Rb S3 6_654 2_655 129.5(2) n S1 Rb S1 6_654 6_655 105.20(11) n S3 Rb S1 2_655 6_655 125.3(2) n S1 Rb S2 6_654 1_655 145.35(5) n S3 Rb S2 2_655 1_655 66.44(8) n S1 Rb S2 6_655 1_655 68.29(14) n S1 Rb S2 6_654 4 145.35(5) n S3 Rb S2 2_655 4 66.44(8) n S1 Rb S2 6_655 4 68.29(13) n S2 Rb S2 1_655 4 66.12(11) n S1 Rb S2 6_654 4_554 67.51(15) n S3 Rb S2 2_655 4_554 69.80(9) n S1 Rb S2 6_655 4_554 146.73(5) n S2 Rb S2 1_655 4_554 136.16(9) n S2 Rb S2 4 4_554 98.74(7) n S1 Rb S2 6_654 1_654 67.51(15) n S3 Rb S2 2_655 1_654 69.80(9) n S1 Rb S2 6_655 1_654 146.73(5) n S2 Rb S2 1_655 1_654 98.74(7) n S2 Rb S2 4 1_654 136.16(9) n S2 Rb S2 4_554 1_654 62.91(9) n S1 Rb S1 6_654 1_655 87.01(13) n S3 Rb S1 2_655 1_655 96.09(5) n S1 Rb S1 6_655 1_655 85.55(14) n S2 Rb S1 1_655 1_655 59.03(14) n S2 Rb S1 4 1_655 124.8(2) n S2 Rb S1 4_554 1_655 124.8(2) n S2 Rb S1 1_654 1_655 62.19(14) n S1 Rb S1 6_654 . 87.01(14) n S3 Rb S1 2_655 . 96.09(5) n S1 Rb S1 6_655 . 85.55(14) n S2 Rb S1 1_655 . 124.8(2) n S2 Rb S1 4 . 59.03(14) n S2 Rb S1 4_554 . 62.19(14) n S2 Rb S1 1_654 . 124.8(2) n S1 Rb S1 1_655 . 167.60(11) n S1 Rb V 6_654 6_654 32.24(11) n S3 Rb V 2_655 6_654 161.7(2) n S1 Rb V 6_655 6_654 72.95(10) n S2 Rb V 1_655 6_654 127.63(7) n S2 Rb V 4 6_654 127.63(7) n S2 Rb V 4_554 6_654 94.78(9) n S2 Rb V 1_654 6_654 94.78(9) n S1 Rb V 1_655 6_654 84.57(8) n S1 Rb V . 6_654 84.57(8) n S1 Rb Cu1 6_654 3 141.80(13) n S3 Rb Cu1 2_655 3 34.53(6) n S1 Rb Cu1 6_655 3 101.50(15) n S2 Rb Cu1 1_655 3 70.62(7) n S2 Rb Cu1 4 3 34.21(5) n S2 Rb Cu1 4_554 3 75.14(6) n S2 Rb Cu1 1_654 3 102.54(6) n S1 Rb Cu1 1_655 3 122.14(11) n S1 Rb Cu1 . 3 68.25(8) n V Rb Cu1 6_654 3 152.72(2) n S1 Rb Cu1 6_654 1_655 141.80(13) n S3 Rb Cu1 2_655 1_655 34.53(6) n S1 Rb Cu1 6_655 1_655 101.50(15) n S2 Rb Cu1 1_655 1_655 34.21(5) n S2 Rb Cu1 4 1_655 70.62(7) n S2 Rb Cu1 4_554 1_655 102.54(6) n S2 Rb Cu1 1_654 1_655 75.14(6) n S1 Rb Cu1 1_655 1_655 68.25(8) n S1 Rb Cu1 . 1_655 122.14(11) n V Rb Cu1 6_654 1_655 152.72(2) n Cu1 Rb Cu1 3 1_655 53.99(4) n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V S1 . 2.153(7) y V S2 4 2.186(4) n V S2 . 2.186(4) y V S3 . 2.232(5) y V Cu2 1_556 2.703(4) y V Cu1 . 2.709(2) y V Cu1 3 2.709(2) n V Cu2 . 2.711(4) y V Rb 6_655 4.035(4) n V Rb 1_455 4.149(2) n V Rb . 4.149(2) n Cu1 S2 . 2.290(3) y Cu1 S2 2 2.290(3) n Cu1 S3 2 2.307(3) n Cu1 S3 . 2.307(3) y Cu1 V 2 2.709(2) n Cu1 Rb 2_655 4.066(2) n Cu1 Rb 1_455 4.066(2) n Cu2 S1 . 2.288(6) y Cu2 S3 . 2.300(4) y Cu2 S2 1_554 2.302(3) y Cu2 S2 4_554 2.302(3) n Cu2 V 1_554 2.703(4) n Cu2 Rb 6_654 4.083(4) n Cu2 Rb . 4.174(2) n Cu2 Rb 1_455 4.174(2) n S1 Rb 6_655 3.356(9) n S1 Rb 6_654 3.458(10) n S1 Rb 1_455 3.713(2) n S1 Rb . 3.713(2) n S2 Cu2 1_556 2.302(3) n S2 Rb 1_455 3.486(4) n S2 Rb 1_456 3.645(4) n S3 Cu1 3 2.307(3) n S3 Rb 2_655 3.453(4) n Rb S1 6_654 3.356(9) y Rb S3 2_655 3.453(4) y Rb S1 6_655 3.458(10) y Rb S2 1_655 3.486(4) y Rb S2 4 3.486(4) n Rb S2 4_554 3.645(4) y Rb S2 1_654 3.645(4) n Rb S1 1_655 3.713(2) y Rb V 6_654 4.035(4) n Rb Cu1 3 4.066(2) n Rb Cu1 1_655 4.066(2) n