#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012558.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_2012558 loop_ _publ_author_name 'Taylor, Stephen P.' 'Krawiec, Mariusz' 'Hwu, Shiou-Jyh' _publ_section_title ; High-temperature synthesis of Rb~2~MnP~2~S~6~ in molten salt medium ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i27 _journal_page_last i28 _journal_volume 58 _journal_year 2002 _chemical_formula_structural 'Rb2 Mn P2 S6' _chemical_formula_sum 'Mn P2 Rb2 S6' _chemical_formula_weight 480.18 _chemical_name_systematic ; rubidium manganese hexathiodiphosphate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 97.74(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.1570(12) _cell_length_b 12.308(3) _cell_length_c 7.5610(15) _cell_measurement_reflns_used 6144 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.08 _cell_measurement_theta_min 1.65 _cell_volume 567.8(2) _computing_cell_refinement 'CrystalClear (Rigaku Corporation, 1999)' _computing_data_collection 'CrystalClear (Rigaku Corporation, 1999)' _computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)' _computing_publication_material 'Molecular Structure Corporation, 1997-1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full .988 _diffrn_measured_fraction_theta_max .988 _diffrn_measurement_device_type 'Rigaku APC8' _diffrn_measurement_method '\w scans' _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 .0549 _diffrn_reflns_av_sigmaI/netI .0294 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 5210 _diffrn_reflns_theta_full 26.08 _diffrn_reflns_theta_max 26.08 _diffrn_reflns_theta_min 3.18 _exptl_absorpt_coefficient_mu 11.002 _exptl_absorpt_correction_T_max .577 _exptl_absorpt_correction_T_min .258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; REQABA Empirical Absorption Correction using REQABA (Jacobson, 1999) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 450 _exptl_crystal_size_max .15 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .05 _refine_diff_density_max 1.060 _refine_diff_density_min -.728 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_matrix_type full _refine_ls_number_parameters 52 _refine_ls_number_reflns 1110 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.318 _refine_ls_R_factor_all .0600 _refine_ls_R_factor_gt .0549 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+12.3434P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .1349 _refine_ls_wR_factor_ref .1369 _reflns_number_gt 1034 _reflns_number_total 1110 _reflns_threshold_expression I>2sigma(I) _[local]_cod_data_source_file br1335.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012558 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Rb1 .22904(19) .17337(9) .02473(16) .0383(4) Uani d . 1 Rb Mn1 .0000 .0000 .5000 .0233(5) Uani d S 1 Mn P1 .4702(4) .04003(19) .6252(3) .0166(5) Uani d . 1 P S1 .2286(4) -.0774(2) .2535(3) .0251(6) Uani d . 1 S S2 .3017(4) -.0697(2) .7518(3) .0235(5) Uani d . 1 S S3 .2731(4) .1673(2) .5466(4) .0263(6) Uani d . 1 S 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 Rb1 .0377(6) .0316(6) .0425(7) .0101(5) -.0056(5) -.0046(5) Mn1 .0109(9) .0270(11) .0320(12) -.0009(8) .0030(8) .0000(9) P1 .0119(10) .0161(11) .0220(12) -.0011(8) .0032(9) -.0010(9) S1 .0159(11) .0325(13) .0262(13) -.0047(10) -.0003(9) -.0068(10) S2 .0166(11) .0275(13) .0273(13) -.0005(9) .0061(9) .0093(10) S3 .0194(11) .0159(11) .0445(16) .0038(9) .0071(11) .0005(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P .1023 .0942 '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' Mn Mn .3368 .7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -.9393 2.9676 '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 S2 Rb1 S3 3_656 4_565 146.56(8) ? S2 Rb1 S1 3_656 3 137.51(7) ? S3 Rb1 S1 4_565 3 67.94(7) ? S2 Rb1 S1 3_656 2 95.04(7) ? S3 Rb1 S1 4_565 2 59.03(6) ? S1 Rb1 S1 3 2 126.14(7) ? S2 Rb1 S1 3_656 . 59.02(6) ? S3 Rb1 S1 4_565 . 114.75(7) ? S1 Rb1 S1 3 . 86.88(7) ? S1 Rb1 S1 2 . 122.48(4) ? S2 Rb1 S3 3_656 1_554 108.21(7) ? S3 Rb1 S3 4_565 1_554 103.17(7) ? S1 Rb1 S3 3 1_554 63.83(6) ? S1 Rb1 S3 2 1_554 118.79(7) ? S1 Rb1 S3 . 1_554 118.02(6) ? S2 Rb1 S2 3_656 1_554 79.31(7) ? S3 Rb1 S2 4_565 1_554 130.39(7) ? S1 Rb1 S2 3 1_554 62.47(6) ? S1 Rb1 S2 2 1_554 166.73(7) ? S1 Rb1 S2 . 1_554 64.84(6) ? S3 Rb1 S2 1_554 1_554 53.25(6) ? S2 Rb1 S2 3_656 2 124.45(7) ? S3 Rb1 S2 4_565 2 64.55(6) ? S1 Rb1 S2 3 2 88.49(6) ? S1 Rb1 S2 2 2 61.67(6) ? S1 Rb1 S2 . 2 175.16(6) ? S3 Rb1 S2 1_554 2 58.40(6) ? S2 Rb1 S2 1_554 2 111.66(4) ? S2 Rb1 S3 3_656 4_665 59.65(6) ? S3 Rb1 S3 4_565 4_665 114.59(7) ? S1 Rb1 S3 3 4_665 145.35(7) ? S1 Rb1 S3 2 4_665 61.66(6) ? S1 Rb1 S3 . 4_665 118.64(6) ? S3 Rb1 S3 1_554 4_665 82.73(7) ? S2 Rb1 S3 1_554 4_665 105.37(6) ? S2 Rb1 S3 2 4_665 65.04(6) ? S2 Rb1 P1 3_656 1_554 80.80(6) ? S3 Rb1 P1 4_565 1_554 132.34(7) ? S1 Rb1 P1 3 1_554 75.61(6) ? S1 Rb1 P1 2 1_554 136.90(7) ? S1 Rb1 P1 . 1_554 92.12(6) ? S3 Rb1 P1 1_554 1_554 30.79(5) ? S2 Rb1 P1 1_554 1_554 30.69(5) ? S2 Rb1 P1 2 1_554 85.39(6) ? S3 Rb1 P1 4_665 1_554 80.12(6) ? S2 Rb1 S3 3_656 . 63.43(6) ? S3 Rb1 S3 4_565 . 84.78(7) ? S1 Rb1 S3 3 . 122.79(7) ? S1 Rb1 S3 2 . 62.75(6) ? S1 Rb1 S3 . . 59.72(6) ? S3 Rb1 S3 1_554 . 171.55(8) ? S2 Rb1 S3 1_554 . 123.34(6) ? S2 Rb1 S3 2 . 124.33(6) ? S3 Rb1 S3 4_665 . 91.41(7) ? P1 Rb1 S3 1_554 . 142.13(6) ? S2 Rb1 P1 3_656 4_565 124.99(6) ? S3 Rb1 P1 4_565 4_565 30.48(5) ? S1 Rb1 P1 3 4_565 95.94(6) ? S1 Rb1 P1 2 4_565 30.25(5) ? S1 Rb1 P1 . 4_565 130.71(7) ? S3 Rb1 P1 1_554 4_565 106.90(6) ? S2 Rb1 P1 1_554 4_565 154.75(6) ? S2 Rb1 P1 2 4_565 51.22(5) ? S3 Rb1 P1 4_665 4_565 84.80(6) ? P1 Rb1 P1 1_554 4_565 136.32(6) ? S3 Rb1 P1 . 4_565 78.48(6) ? S2 Mn1 S2 . 3_556 180.0 ? S2 Mn1 S3 . 3_556 102.54(8) y S2 Mn1 S3 3_556 3_556 77.46(8) ? S2 Mn1 S3 . . 77.46(8) y S2 Mn1 S3 3_556 . 102.54(8) ? S3 Mn1 S3 3_556 . 180.00(10) ? S2 Mn1 S1 . 3_556 89.90(8) y S2 Mn1 S1 3_556 3_556 90.10(8) ? S3 Mn1 S1 3_556 3_556 89.15(8) ? S3 Mn1 S1 . 3_556 90.85(8) y S2 Mn1 S1 . . 90.10(8) y S2 Mn1 S1 3_556 . 89.90(8) ? S3 Mn1 S1 3_556 . 90.85(8) ? S3 Mn1 S1 . . 89.15(8) y S1 Mn1 S1 3_556 . 180.00(7) ? S2 Mn1 P1 . . 41.88(7) ? S2 Mn1 P1 3_556 . 138.12(7) ? S3 Mn1 P1 3_556 . 138.26(7) ? S3 Mn1 P1 . . 41.74(7) ? S1 Mn1 P1 3_556 . 107.65(7) ? S1 Mn1 P1 . . 72.35(7) ? S2 Mn1 P1 . 3_556 138.12(7) ? S2 Mn1 P1 3_556 3_556 41.88(7) ? S3 Mn1 P1 3_556 3_556 41.74(7) ? S3 Mn1 P1 . 3_556 138.26(7) ? S1 Mn1 P1 3_556 3_556 72.35(7) ? S1 Mn1 P1 . 3_556 107.65(7) ? P1 Mn1 P1 . 3_556 180.0 ? S1 P1 S2 3_656 . 115.95(15) y S1 P1 S3 3_656 . 115.97(16) y S2 P1 S3 . . 109.32(14) y S1 P1 P1 3_656 3_656 104.14(16) y S2 P1 P1 . 3_656 105.25(17) y S3 P1 P1 . 3_656 104.85(18) y S1 P1 Mn1 3_656 . 170.44(13) ? S2 P1 Mn1 . . 59.90(9) ? S3 P1 Mn1 . . 60.85(9) ? P1 P1 Mn1 3_656 . 85.41(12) ? S1 P1 Rb1 3_656 1_556 88.52(11) ? S2 P1 Rb1 . 1_556 68.96(10) ? S3 P1 Rb1 . 1_556 68.02(10) ? P1 P1 Rb1 3_656 1_556 167.32(15) ? Mn1 P1 Rb1 . 1_556 81.95(6) ? S1 P1 Rb1 3_656 4_666 61.07(10) ? S2 P1 Rb1 . 4_666 157.75(12) ? S3 P1 Rb1 . 4_666 59.85(9) ? P1 P1 Rb1 3_656 4_666 96.60(13) ? Mn1 P1 Rb1 . 4_666 119.00(7) ? Rb1 P1 Rb1 1_556 4_666 88.79(5) ? S1 P1 Rb1 3_656 3_656 62.06(10) ? S2 P1 Rb1 . 3_656 57.95(9) ? S3 P1 Rb1 . 3_656 155.38(13) ? P1 P1 Rb1 3_656 3_656 99.13(13) ? Mn1 P1 Rb1 . 3_656 116.56(7) ? Rb1 P1 Rb1 1_556 3_656 87.38(6) ? Rb1 P1 Rb1 4_666 3_656 123.07(6) ? P1 S1 Mn1 3_656 . 98.10(12) ? P1 S1 Rb1 3_656 3 167.00(13) ? Mn1 S1 Rb1 . 3 94.77(7) ? P1 S1 Rb1 3_656 2_545 88.68(11) ? Mn1 S1 Rb1 . 2_545 89.44(8) ? Rb1 S1 Rb1 3 2_545 89.66(6) ? P1 S1 Rb1 3_656 . 87.84(11) ? Mn1 S1 Rb1 . . 93.76(8) ? Rb1 S1 Rb1 3 . 93.12(7) ? Rb1 S1 Rb1 2_545 . 175.57(8) ? P1 S2 Mn1 . . 78.22(10) ? P1 S2 Rb1 . 3_656 91.74(10) ? Mn1 S2 Rb1 . 3_656 163.36(10) ? P1 S2 Rb1 . 1_556 80.34(11) ? Mn1 S2 Rb1 . 1_556 90.77(7) ? Rb1 S2 Rb1 3_656 1_556 100.69(7) ? P1 S2 Rb1 . 2_545 106.70(11) ? Mn1 S2 Rb1 . 2_545 83.92(7) ? Rb1 S2 Rb1 3_656 2_545 86.37(6) ? Rb1 S2 Rb1 1_556 2_545 170.01(7) ? P1 S3 Mn1 . . 77.41(10) ? P1 S3 Rb1 . 4_666 89.67(10) ? Mn1 S3 Rb1 . 4_666 160.30(10) ? P1 S3 Rb1 . 1_556 81.19(11) ? Mn1 S3 Rb1 . 1_556 90.97(8) ? Rb1 S3 Rb1 4_666 1_556 101.82(8) ? P1 S3 Rb1 . 4_566 152.64(12) ? Mn1 S3 Rb1 . 4_566 81.83(6) ? Rb1 S3 Rb1 4_666 4_566 114.59(7) ? Rb1 S3 Rb1 1_556 4_566 81.54(6) ? P1 S3 Rb1 . . 105.55(12) ? Mn1 S3 Rb1 . . 85.67(7) ? Rb1 S3 Rb1 4_666 . 83.53(7) ? Rb1 S3 Rb1 1_556 . 171.55(8) ? Rb1 S3 Rb1 4_566 . 90.30(6) ? 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 Rb1 S2 3_656 3.393(3) ? Rb1 S3 4_565 3.446(3) ? Rb1 S1 3 3.488(3) ? Rb1 S1 2 3.489(3) ? Rb1 S1 . 3.538(3) ? Rb1 S3 1_554 3.663(3) ? Rb1 S2 1_554 3.695(3) ? Rb1 S2 2 3.782(3) ? Rb1 S3 4_665 3.866(3) ? Rb1 P1 1_554 3.903(3) ? Rb1 S3 . 3.919(3) ? Rb1 P1 4_565 3.986(3) ? Mn1 S2 . 2.619(3) y Mn1 S2 3_556 2.619(3) ? Mn1 S3 3_556 2.652(3) ? Mn1 S3 . 2.652(3) y Mn1 S1 3_556 2.659(3) ? Mn1 S1 . 2.659(3) y Mn1 P1 . 2.964(2) y Mn1 P1 3_556 2.964(2) ? P1 S1 3_656 2.008(3) y P1 S2 . 2.021(3) y P1 S3 . 2.022(3) y P1 P1 3_656 2.208(5) y P1 Rb1 1_556 3.903(3) ? P1 Rb1 4_666 3.986(3) ? P1 Rb1 3_656 4.002(3) ? S1 P1 3_656 2.008(3) ? S1 Rb1 3 3.488(3) ? S1 Rb1 2_545 3.489(3) ? S2 Rb1 3_656 3.393(3) ? S2 Rb1 1_556 3.695(3) ? S2 Rb1 2_545 3.782(3) ? S3 Rb1 4_666 3.446(3) ? S3 Rb1 1_556 3.663(3) ? S3 Rb1 4_566 3.866(3) ?