#------------------------------------------------------------------------------ #$Date: 2024-04-04 04:07:16 +0300 (Thu, 04 Apr 2024) $ #$Revision: 290776 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248380.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_7248380 loop_ _publ_author_name 'Grahlow, Fabian' 'Strauß, Fabian' 'Scheele, Marcus' 'Ströbele, Markus' 'Carta, Alberto' 'Weber, Sophie F.' 'Kroeker, Scott' 'Romao, Carl P.' 'Meyer, H-Jürgen' _publ_section_title ; Electronic structure and transport in the potential Luttinger liquids CsNb3Br7S and RbNb3Br7S. ; _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_paper_doi 10.1039/d4cp00293h _journal_year 2024 _chemical_formula_moiety 'Br7 Nb3 Rb S' _chemical_formula_sum 'Br7 Nb3 Rb S' _chemical_formula_weight 955.63 _space_group_crystal_system orthorhombic _space_group_IT_number 26 _space_group_name_Hall 'P 2c -2' _space_group_name_H-M_alt 'P m c 21' _atom_sites_solution_primary dual _audit_creation_date 2020-12-06 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032) ; _audit_update_record ; 2020-12-07 deposited with the CCDC. 2024-03-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.0218(7) _cell_length_b 9.8353(15) _cell_length_c 18.445(3) _cell_measurement_reflns_used 2080 _cell_measurement_temperature 100.00(14) _cell_measurement_theta_max 25.9850 _cell_measurement_theta_min 4.4230 _cell_volume 1273.8(3) _computing_cell_refinement 'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(14) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -60.00 4.05 0.15 61.00 -- -7.20 -57.00-120.00 427 2 \w -60.00 4.05 0.15 61.00 -- -7.20 -57.00 30.00 427 3 \w -21.00 30.00 0.15 61.00 -- 9.31 -77.00 -30.00 340 4 \w 0.00 85.05 0.15 61.00 -- 9.31 37.00-150.00 567 5 \w -4.00 41.00 0.15 61.00 -- 9.31 -99.00 150.00 300 6 \w -16.00 69.05 0.15 61.00 -- -7.20 37.00-180.00 567 7 \w -4.00 41.00 0.15 61.00 -- 9.31 -99.00-150.00 300 8 \w -68.00 4.00 0.15 61.00 -- 9.31 -19.00 0.00 480 9 \w -66.00 1.05 0.15 61.00 -- 9.31 -37.00 -90.00 447 10 \w -21.00 30.00 0.15 61.00 -- 9.31 -77.00 60.00 340 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0055377000 _diffrn_orient_matrix_UB_12 -0.0190515000 _diffrn_orient_matrix_UB_13 0.0626069000 _diffrn_orient_matrix_UB_21 -0.0194899000 _diffrn_orient_matrix_UB_22 -0.0325781000 _diffrn_orient_matrix_UB_23 -0.0355309000 _diffrn_orient_matrix_UB_31 0.0989691000 _diffrn_orient_matrix_UB_32 -0.0074545000 _diffrn_orient_matrix_UB_33 -0.0036954000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_unetI/netI 0.0485 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 19173 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.053 _diffrn_reflns_theta_min 3.565 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 28.519 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.122 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 4.983 _exptl_crystal_description needle _exptl_crystal_F_000 1684 _exptl_crystal_size_max 0.921 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.011 _refine_diff_density_max 2.591 _refine_diff_density_min -2.215 _refine_diff_density_rms 0.468 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.50(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2718 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0540 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+42.3816P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1228 _refine_ls_wR_factor_ref 0.1260 _reflns_Friedel_coverage 0.930 _reflns_Friedel_fraction_full 0.989 _reflns_Friedel_fraction_max 0.989 _reflns_number_gt 2517 _reflns_number_total 2718 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cp00293h2.cif _cod_data_source_block rb16 _cod_original_cell_volume 1273.9(3) _cod_database_code 7248380 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Rb1 Nb3 Br7 S1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.744 _shelx_estimated_absorpt_t_min 0.015 _reflns_odcompleteness_completeness 97.01 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.50(3) 0.50(3) 2. Uiso/Uaniso restraints and constraints Uanis(S1) \\sim Ueq, Uanis(S2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 ; _shelx_res_file ; TITL rb16_a.res in Pmc2(1) rb16.res created by SHELXL-2018/3 at 22:58:54 on 06-Dec-2020 REM Old TITL Rb16 in Pmmm REM SHELXT solution in Pmc2(1): R1 0.255, Rweak 0.027, Alpha 0.035 CELL 0.71073 7.0218 9.8353 18.4452 90 90 90 ZERR 4 0.0007 0.0015 0.0026 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM +X,-Y,0.5+Z SYMM -X,+Y,+Z SFAC Br Nb Rb S UNIT 28 12 4 4 ISOR 0.001 0.002 $S L.S. 15 0 0 PLAN 8 SIZE 0.011 0.015 0.921 TEMP -173.15(14) CONF list 4 MORE -1 fmap 2 53 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 4 0 0 REM REM REM WGHT 0.075200 42.381599 BASF 0.50363 FVAR 0.06617 RB1 3 1.500000 1.073735 0.667234 10.50000 0.01576 0.01491 = 0.02165 0.00249 0.00000 0.00000 RB2 3 1.000000 1.111296 0.352837 10.50000 0.01460 0.02053 = 0.00517 0.00619 0.00000 0.00000 NB1 2 1.200232 0.555915 0.577751 11.00000 0.00419 0.00610 = 0.00787 0.00025 -0.00016 -0.00078 NB2 2 1.000000 0.812327 0.587603 10.50000 0.00720 0.00959 = 0.00484 0.00287 0.00000 0.00000 NB3 2 0.294471 0.571156 0.413631 11.00000 0.00170 0.00707 = 0.00702 -0.00020 -0.00067 0.00004 NB4 2 0.500000 0.827233 0.417601 10.50000 0.00229 0.00413 = 0.00325 -0.00150 0.00000 0.00000 BR1 1 1.251352 0.730933 0.680662 11.00000 0.00819 0.00757 = 0.00876 -0.00016 -0.00371 0.00287 BR2 1 1.000000 0.406920 0.663047 10.50000 0.00456 0.01863 = 0.02362 0.00209 0.00000 0.00000 BR3 1 1.500000 0.429850 0.649835 10.50000 0.03135 0.01717 = 0.01750 0.00381 0.00000 0.00000 BR4 1 0.248171 0.344921 0.491485 11.00000 0.01118 0.01193 = 0.00993 -0.00105 -0.00498 0.00129 BR5 1 0.749929 0.954999 0.509316 11.00000 0.01568 0.01292 = 0.01163 -0.00225 0.00195 0.00316 BR6 1 1.000000 1.038005 0.671997 10.50000 0.00531 0.00708 = 0.00643 0.00043 0.00000 0.00000 BR7 1 0.246420 0.758716 0.323794 11.00000 0.00698 0.01563 = 0.01317 -0.00004 -0.00066 0.00322 BR8 1 0.500000 0.430628 0.325124 10.50000 0.01901 0.02551 = 0.03352 -0.00819 0.00000 0.00000 BR9 1 0.000000 0.453169 0.340123 10.50000 0.01297 0.01846 = 0.02278 -0.00325 0.00000 0.00000 BR10 1 0.500000 1.067546 0.351367 10.50000 0.02247 0.02997 = 0.05612 0.01428 0.00000 0.00000 S1 4 1.000000 0.662406 0.489837 10.50000 0.00761 0.00773 = 0.00638 -0.00014 0.00000 0.00000 S2 4 0.500000 0.649353 0.515046 10.50000 0.01234 0.01352 = 0.01294 -0.00107 0.00000 0.00000 HKLF 4 REM rb16_a.res in Pmc2(1) REM wR2 = 0.1260, GooF = S = 1.006, Restrained GooF = 1.005 for all data REM R1 = 0.0540 for 2517 Fo > 4sig(Fo) and 0.0587 for all 2718 data REM 128 parameters refined using 13 restraints END WGHT 0.0721 38.8483 REM Highest difference peak 2.591, deepest hole -2.215, 1-sigma level 0.468 Q1 1 1.0000 0.2999 0.5751 10.50000 0.05 2.59 Q2 1 0.5000 0.1874 0.4985 10.50000 0.05 2.38 Q3 1 0.0000 0.5000 0.4190 10.50000 0.05 1.97 Q4 1 1.0000 1.0171 0.5755 10.50000 0.05 1.88 Q5 1 1.5000 0.4964 0.5786 10.50000 0.05 1.78 Q6 1 0.2448 0.3964 0.3975 11.00000 0.05 1.74 Q7 1 0.5000 0.5556 0.4118 10.50000 0.05 1.71 Q8 1 0.0000 0.2378 0.5097 10.50000 0.05 1.62 ; _shelx_res_checksum 36560 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.810 _oxdiff_exptl_absorpt_empirical_full_min 0.425 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rb1 Rb 1.500000 1.0737(3) 0.66723(19) 0.0174(7) Uani 1 2 d S T P . . Rb2 Rb 1.000000 1.1113(4) 0.35284(16) 0.0134(7) Uani 1 2 d S T P . . Nb1 Nb 1.2002(3) 0.55592(18) 0.57775(10) 0.0061(4) Uani 1 1 d . . . . . Nb2 Nb 1.000000 0.8123(3) 0.58760(15) 0.0072(6) Uani 1 2 d S T P . . Nb3 Nb 0.2945(3) 0.57116(19) 0.41363(10) 0.0053(4) Uani 1 1 d . . . . . Nb4 Nb 0.500000 0.8272(3) 0.41760(14) 0.0032(5) Uani 1 2 d S T P . . Br1 Br 1.2514(3) 0.7309(2) 0.68066(12) 0.0082(5) Uani 1 1 d . . . . . Br2 Br 1.000000 0.4069(4) 0.6630(2) 0.0156(7) Uani 1 2 d S T P . . Br3 Br 1.500000 0.4298(4) 0.6498(2) 0.0220(9) Uani 1 2 d S T P . . Br4 Br 0.2482(4) 0.3449(2) 0.49149(12) 0.0110(4) Uani 1 1 d . . . . . Br5 Br 0.7499(4) 0.9550(2) 0.50932(12) 0.0134(5) Uani 1 1 d . . . . . Br6 Br 1.000000 1.0380(3) 0.67200(16) 0.0063(6) Uani 1 2 d S T P . . Br7 Br 0.2464(3) 0.7587(2) 0.32379(13) 0.0119(5) Uani 1 1 d . . . . . Br8 Br 0.500000 0.4306(4) 0.3251(2) 0.0260(9) Uani 1 2 d S T P . . Br9 Br 0.000000 0.4532(4) 0.3401(2) 0.0181(8) Uani 1 2 d S T P . . Br10 Br 0.500000 1.0675(5) 0.3514(3) 0.0362(11) Uani 1 2 d S T P . . S1 S 1.000000 0.6624(8) 0.4898(4) 0.0072(15) Uani 1 2 d S TU P . . S2 S 0.500000 0.6494(9) 0.5150(5) 0.0129(16) Uani 1 2 d S TU 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 Rb1 0.0158(18) 0.0149(15) 0.0217(18) 0.0025(13) 0.000 0.000 Rb2 0.0146(17) 0.0205(16) 0.0052(14) 0.0062(12) 0.000 0.000 Nb1 0.0042(10) 0.0061(8) 0.0079(9) 0.0002(7) -0.0002(7) -0.0008(7) Nb2 0.0072(15) 0.0096(13) 0.0048(12) 0.0029(10) 0.000 0.000 Nb3 0.0017(9) 0.0071(8) 0.0070(8) -0.0002(7) -0.0007(7) 0.0000(7) Nb4 0.0023(13) 0.0041(12) 0.0033(11) -0.0015(10) 0.000 0.000 Br1 0.0082(12) 0.0076(9) 0.0088(9) -0.0002(8) -0.0037(8) 0.0029(8) Br2 0.0046(17) 0.0186(16) 0.0236(19) 0.0021(13) 0.000 0.000 Br3 0.031(2) 0.0172(17) 0.0175(18) 0.0038(14) 0.000 0.000 Br4 0.0112(9) 0.0119(9) 0.0099(10) -0.0011(9) -0.0050(8) 0.0013(10) Br5 0.0157(10) 0.0129(9) 0.0116(11) -0.0022(8) 0.0019(11) 0.0032(10) Br6 0.0053(14) 0.0071(13) 0.0064(13) 0.0004(11) 0.000 0.000 Br7 0.0070(12) 0.0156(11) 0.0132(10) 0.0000(8) -0.0007(9) 0.0032(9) Br8 0.019(2) 0.026(2) 0.034(2) -0.0082(17) 0.000 0.000 Br9 0.013(2) 0.0185(16) 0.0228(18) -0.0033(14) 0.000 0.000 Br10 0.022(2) 0.030(2) 0.056(3) 0.014(2) 0.000 0.000 S1 0.0076(19) 0.0077(18) 0.0064(18) -0.0001(13) 0.000 0.000 S2 0.012(2) 0.014(2) 0.013(2) -0.0011(13) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -12 -12 0.0066 0 11 12 0.0085 -10 3 -1 0.4245 0 25 -3 0.0067 0 10 -13 0.0103 0 14 12 0.0048 0 17 -10 0.0094 0 -17 10 0.0010 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Rb2 Rb1 Rb2 84.33(8) 2_875 2_775 ? Br1 Rb1 Rb2 87.54(8) . 2_875 ? Br1 Rb1 Rb2 48.78(6) 4_855 2_875 ? Br1 Rb1 Rb2 48.78(6) . 2_775 ? Br1 Rb1 Rb2 87.54(8) 4_855 2_775 ? Br1 Rb1 Br1 54.63(8) . 4_855 ? Br3 Rb1 Rb2 113.97(8) 1_565 2_875 ? Br3 Rb1 Rb2 113.97(8) 1_565 2_775 ? Br3 Rb1 Br1 152.67(4) 1_565 . ? Br3 Rb1 Br1 152.67(4) 1_565 4_855 ? Br3 Rb1 Br5 104.45(11) 1_565 1_655 ? Br3 Rb1 Br5 104.45(11) 1_565 4_755 ? Br3 Rb1 Br6 95.82(7) 1_565 1_655 ? Br3 Rb1 Br6 95.82(7) 1_565 . ? Br3 Rb1 Br7 68.58(9) 1_565 3_675 ? Br3 Rb1 Br7 68.58(9) 1_565 2_775 ? Br3 Rb1 Br10 117.49(13) 1_565 2_775 ? Br5 Rb1 Rb2 138.15(9) 4_755 2_875 ? Br5 Rb1 Rb2 138.15(9) 1_655 2_775 ? Br5 Rb1 Rb2 95.14(6) 4_755 2_775 ? Br5 Rb1 Rb2 95.14(6) 1_655 2_875 ? Br5 Rb1 Br1 62.68(7) 1_655 4_855 ? Br5 Rb1 Br1 89.37(9) 4_755 4_855 ? Br5 Rb1 Br1 89.36(9) 1_655 . ? Br5 Rb1 Br1 62.68(7) 4_755 . ? Br5 Rb1 Br5 58.43(11) 4_755 1_655 ? Br5 Rb1 Br7 173.02(12) 1_655 3_675 ? Br5 Rb1 Br7 173.02(12) 4_755 2_775 ? Br5 Rb1 Br7 122.12(6) 4_755 3_675 ? Br5 Rb1 Br7 122.12(6) 1_655 2_775 ? Br5 Rb1 Br10 128.81(10) 1_655 2_775 ? Br5 Rb1 Br10 128.81(10) 4_755 2_775 ? Br6 Rb1 Rb2 128.08(10) . 2_875 ? Br6 Rb1 Rb2 128.08(10) 1_655 2_775 ? Br6 Rb1 Rb2 44.06(6) 1_655 2_875 ? Br6 Rb1 Rb2 44.06(6) . 2_775 ? Br6 Rb1 Br1 56.89(6) 1_655 4_855 ? Br6 Rb1 Br1 56.89(6) . . ? Br6 Rb1 Br1 111.51(10) . 4_855 ? Br6 Rb1 Br1 111.51(10) 1_655 . ? Br6 Rb1 Br5 118.25(11) 1_655 4_755 ? Br6 Rb1 Br5 60.15(7) 1_655 1_655 ? Br6 Rb1 Br5 60.15(7) . 4_755 ? Br6 Rb1 Br5 118.25(11) . 1_655 ? Br6 Rb1 Br6 168.22(14) 1_655 . ? Br6 Rb1 Br7 119.61(10) 1_655 3_675 ? Br6 Rb1 Br7 63.57(7) 1_655 2_775 ? Br6 Rb1 Br7 119.61(10) . 2_775 ? Br6 Rb1 Br7 63.57(7) . 3_675 ? Br6 Rb1 Br10 86.52(7) 1_655 2_775 ? Br6 Rb1 Br10 86.52(7) . 2_775 ? Br7 Rb1 Rb2 88.15(8) 3_675 2_875 ? Br7 Rb1 Rb2 48.24(6) 3_675 2_775 ? Br7 Rb1 Rb2 48.24(6) 2_775 2_875 ? Br7 Rb1 Rb2 88.15(8) 2_775 2_775 ? Br7 Rb1 Br1 123.64(10) 2_775 . ? Br7 Rb1 Br1 96.93(8) 2_775 4_855 ? Br7 Rb1 Br1 123.64(10) 3_675 4_855 ? Br7 Rb1 Br1 96.93(8) 3_675 . ? Br7 Rb1 Br7 56.34(8) 2_775 3_675 ? Br10 Rb1 Rb2 42.48(4) 2_775 2_775 ? Br10 Rb1 Rb2 42.48(4) 2_775 2_875 ? Br10 Rb1 Br1 66.68(9) 2_775 4_855 ? Br10 Rb1 Br1 66.69(9) 2_775 . ? Br10 Rb1 Br7 57.10(8) 2_775 2_775 ? Br10 Rb1 Br7 57.10(8) 2_775 3_675 ? Br1 Rb2 Br1 53.07(8) 2_774 3_574 ? Br4 Rb2 Br1 120.08(10) 4_665 3_574 ? Br4 Rb2 Br1 95.58(8) 1_665 3_574 ? Br4 Rb2 Br1 120.08(10) 1_665 2_774 ? Br4 Rb2 Br1 95.58(8) 4_665 2_774 ? Br4 Rb2 Br4 53.76(10) 1_665 4_665 ? Br4 Rb2 Br7 145.00(10) 1_665 4_655 ? Br4 Rb2 Br7 114.79(7) 1_665 1_655 ? Br4 Rb2 Br7 114.79(7) 4_665 4_655 ? Br4 Rb2 Br7 145.00(10) 4_665 1_655 ? Br5 Rb2 Br1 125.20(6) . 2_774 ? Br5 Rb2 Br1 125.20(6) 4_755 3_574 ? Br5 Rb2 Br1 177.54(10) . 3_574 ? Br5 Rb2 Br1 177.54(10) 4_755 2_774 ? Br5 Rb2 Br4 86.84(8) . 1_665 ? Br5 Rb2 Br4 61.12(6) . 4_665 ? Br5 Rb2 Br4 61.12(6) 4_755 1_665 ? Br5 Rb2 Br4 86.84(8) 4_755 4_665 ? Br5 Rb2 Br5 56.47(10) . 4_755 ? Br5 Rb2 Br7 87.05(8) . 1_655 ? Br5 Rb2 Br7 61.98(6) . 4_655 ? Br5 Rb2 Br7 87.05(8) 4_755 4_655 ? Br5 Rb2 Br7 61.98(6) 4_755 1_655 ? Br6 Rb2 Br1 54.73(6) 2_774 3_574 ? Br6 Rb2 Br1 54.73(6) 2_774 2_774 ? Br6 Rb2 Br4 147.94(7) 2_774 1_665 ? Br6 Rb2 Br4 147.94(7) 2_774 4_665 ? Br6 Rb2 Br5 123.01(10) 2_774 4_755 ? Br6 Rb2 Br5 123.01(10) 2_774 . ? Br6 Rb2 Br7 61.16(8) 2_774 4_655 ? Br6 Rb2 Br7 61.16(8) 2_774 1_655 ? Br7 Rb2 Br1 115.83(10) 1_655 2_774 ? Br7 Rb2 Br1 92.32(7) 4_655 2_774 ? Br7 Rb2 Br1 115.83(10) 4_655 3_574 ? Br7 Rb2 Br1 92.32(7) 1_655 3_574 ? Br7 Rb2 Br7 52.50(9) 4_655 1_655 ? Br9 Rb2 Br1 63.40(8) 1_665 3_574 ? Br9 Rb2 Br1 63.40(8) 1_665 2_774 ? Br9 Rb2 Br4 56.73(8) 1_665 4_665 ? Br9 Rb2 Br4 56.73(8) 1_665 1_665 ? Br9 Rb2 Br5 117.86(10) 1_665 . ? Br9 Rb2 Br5 117.86(10) 1_665 4_755 ? Br9 Rb2 Br6 109.77(11) 1_665 2_774 ? Br9 Rb2 Br7 151.01(6) 1_665 1_655 ? Br9 Rb2 Br7 151.01(6) 1_665 4_655 ? Br9 Rb2 Br10 96.94(9) 1_665 1_655 ? Br9 Rb2 Br10 96.94(9) 1_665 . ? Br10 Rb2 Br1 66.31(9) . 2_774 ? Br10 Rb2 Br1 66.31(9) 1_655 3_574 ? Br10 Rb2 Br1 119.01(11) 1_655 2_774 ? Br10 Rb2 Br1 119.01(11) . 3_574 ? Br10 Rb2 Br4 121.76(13) 1_655 4_665 ? Br10 Rb2 Br4 121.76(13) . 1_665 ? Br10 Rb2 Br4 68.21(10) 1_655 1_665 ? Br10 Rb2 Br4 68.21(10) . 4_665 ? Br10 Rb2 Br5 115.16(12) . 4_755 ? Br10 Rb2 Br5 115.16(12) 1_655 . ? Br10 Rb2 Br5 59.07(10) . . ? Br10 Rb2 Br5 59.07(10) 1_655 4_755 ? Br10 Rb2 Br6 86.79(11) 1_655 2_774 ? Br10 Rb2 Br6 86.79(11) . 2_774 ? Br10 Rb2 Br7 56.78(9) 1_655 1_655 ? Br10 Rb2 Br7 109.28(11) 1_655 4_655 ? Br10 Rb2 Br7 56.78(9) . 4_655 ? Br10 Rb2 Br7 109.28(12) . 1_655 ? Br10 Rb2 Br10 166.00(18) 1_655 . ? Nb1 Nb1 Nb2 60.92(5) 4_755 . ? Nb1 Nb1 Nb3 102.32(4) 4_755 1_655 ? Nb2 Nb1 Nb3 97.06(9) . 1_655 ? Br1 Nb1 Nb1 97.97(7) . 4_755 ? Br1 Nb1 Nb2 56.04(8) . . ? Br1 Nb1 Nb3 130.85(9) . 1_655 ? Br1 Nb1 Br3 80.84(11) . . ? Br1 Nb1 Br4 161.56(12) . 1_655 ? Br2 Nb1 Nb1 56.82(7) . 4_755 ? Br2 Nb1 Nb2 101.12(10) . . ? Br2 Nb1 Nb3 137.89(11) . 1_655 ? Br2 Nb1 Br1 90.35(12) . . ? Br2 Nb1 Br3 82.36(9) . . ? Br2 Nb1 Br4 89.45(11) . 1_655 ? Br2 Nb1 S2 158.02(19) . 1_655 ? Br3 Nb1 Nb1 139.18(7) . 4_755 ? Br3 Nb1 Nb2 136.58(12) . . ? Br3 Nb1 Nb3 109.06(10) . 1_655 ? Br4 Nb1 Nb1 97.34(8) 1_655 4_755 ? Br4 Nb1 Nb2 141.82(11) 1_655 . ? Br4 Nb1 Nb3 54.68(7) 1_655 1_655 ? Br4 Nb1 Br3 80.85(11) 1_655 . ? S1 Nb1 Nb1 53.93(12) . 4_755 ? S1 Nb1 Nb2 51.26(19) . . ? S1 Nb1 Nb3 56.07(15) . 1_655 ? S1 Nb1 Br1 106.7(2) . . ? S1 Nb1 Br2 110.11(15) . . ? S1 Nb1 Br3 164.94(17) . . ? S1 Nb1 Br4 90.6(2) . 1_655 ? S1 Nb1 S2 91.1(2) . 1_655 ? S2 Nb1 Nb1 144.94(17) 1_655 4_755 ? S2 Nb1 Nb2 96.58(19) 1_655 . ? S2 Nb1 Nb3 50.90(18) 1_655 1_655 ? S2 Nb1 Br1 88.8(2) 1_655 . ? S2 Nb1 Br3 75.81(18) 1_655 . ? S2 Nb1 Br4 84.6(2) 1_655 1_655 ? Nb1 Nb2 Nb1 58.16(10) 4_755 . ? Br1 Nb2 Nb1 95.93(11) 4_755 . ? Br1 Nb2 Nb1 56.00(8) 4_755 4_755 ? Br1 Nb2 Nb1 56.00(8) . . ? Br1 Nb2 Nb1 95.94(11) . 4_755 ? Br1 Nb2 Br1 85.96(13) . 4_755 ? Br1 Nb2 Br5 165.66(15) 4_755 4_755 ? Br1 Nb2 Br5 94.17(8) . 4_755 ? Br1 Nb2 Br5 165.66(15) . . ? Br1 Nb2 Br5 94.17(8) 4_755 . ? Br1 Nb2 Br6 82.67(10) 4_755 . ? Br1 Nb2 Br6 82.67(10) . . ? Br5 Nb2 Nb1 138.02(12) 4_755 4_755 ? Br5 Nb2 Nb1 96.00(8) 4_755 . ? Br5 Nb2 Nb1 138.02(12) . . ? Br5 Nb2 Nb1 96.00(8) . 4_755 ? Br5 Nb2 Br5 82.18(14) 4_755 . ? Br5 Nb2 Br6 83.13(10) 4_755 . ? Br5 Nb2 Br6 83.13(10) . . ? Br6 Nb2 Nb1 138.57(10) . . ? Br6 Nb2 Nb1 138.57(10) . 4_755 ? S1 Nb2 Nb1 53.10(16) . . ? S1 Nb2 Nb1 53.10(17) . 4_755 ? S1 Nb2 Br1 108.51(17) . . ? S1 Nb2 Br1 108.51(17) . 4_755 ? S1 Nb2 Br5 85.07(16) . . ? S1 Nb2 Br5 85.07(16) . 4_755 ? S1 Nb2 Br6 164.3(2) . . ? Nb3 Nb3 Nb1 102.32(4) 4_655 1_455 ? Nb3 Nb3 Nb4 60.20(5) 4_655 . ? Nb4 Nb3 Nb1 97.08(8) . 1_455 ? Br4 Nb3 Nb1 53.74(7) . 1_455 ? Br4 Nb3 Nb3 97.00(8) . 4_655 ? Br4 Nb3 Nb4 140.38(10) . . ? Br4 Nb3 Br9 79.67(11) . . ? Br7 Nb3 Nb1 130.77(10) . 1_455 ? Br7 Nb3 Nb3 97.75(7) . 4_655 ? Br7 Nb3 Nb4 56.24(8) . . ? Br7 Nb3 Br4 162.69(12) . . ? Br7 Nb3 Br8 92.94(13) . . ? Br7 Nb3 Br9 83.25(12) . . ? Br7 Nb3 S1 89.79(19) . 1_455 ? Br8 Nb3 Nb1 135.30(13) . 1_455 ? Br8 Nb3 Nb3 55.99(7) . 4_655 ? Br8 Nb3 Nb4 101.69(10) . . ? Br8 Nb3 Br4 87.82(13) . . ? Br8 Nb3 Br9 83.21(10) . . ? Br8 Nb3 S1 162.00(17) . 1_455 ? Br9 Nb3 Nb1 107.60(10) . 1_455 ? Br9 Nb3 Nb3 139.20(7) . 4_655 ? Br9 Nb3 Nb4 139.22(12) . . ? S1 Nb3 Nb1 48.24(16) 1_455 1_455 ? S1 Nb3 Nb3 141.11(14) 1_455 4_655 ? S1 Nb3 Nb4 94.62(16) 1_455 . ? S1 Nb3 Br4 84.38(19) 1_455 . ? S1 Nb3 Br9 79.45(15) 1_455 . ? S2 Nb3 Nb1 53.43(16) . 1_455 ? S2 Nb3 Nb3 54.49(13) . 4_655 ? S2 Nb3 Nb4 54.8(2) . . ? S2 Nb3 Br4 85.6(2) . . ? S2 Nb3 Br7 110.4(2) . . ? S2 Nb3 Br8 108.50(15) . . ? S2 Nb3 Br9 160.9(2) . . ? S2 Nb3 S1 87.1(2) . 1_455 ? Nb3 Nb4 Nb3 59.61(9) . 4_655 ? Br5 Nb4 Nb3 136.98(12) 4_655 4_655 ? Br5 Nb4 Nb3 136.98(12) . . ? Br5 Nb4 Nb3 95.45(8) 4_655 . ? Br5 Nb4 Nb3 95.45(8) . 4_655 ? Br5 Nb4 Br5 79.57(13) . 4_655 ? Br7 Nb4 Nb3 95.73(10) 4_655 . ? Br7 Nb4 Nb3 53.97(7) 4_655 4_655 ? Br7 Nb4 Nb3 53.97(7) . . ? Br7 Nb4 Nb3 95.73(10) . 4_655 ? Br7 Nb4 Br5 167.91(13) . . ? Br7 Nb4 Br5 95.28(8) 4_655 . ? Br7 Nb4 Br5 95.28(8) . 4_655 ? Br7 Nb4 Br5 167.91(13) 4_655 4_655 ? Br7 Nb4 Br7 87.60(14) 4_655 . ? Br7 Nb4 Br10 85.63(13) . . ? Br7 Nb4 Br10 85.63(13) 4_655 . ? Br10 Nb4 Nb3 139.37(11) . . ? Br10 Nb4 Nb3 139.37(11) . 4_655 ? Br10 Nb4 Br5 82.89(12) . 4_655 ? Br10 Nb4 Br5 82.89(12) . . ? S2 Nb4 Nb3 54.06(17) . . ? S2 Nb4 Nb3 54.06(17) . 4_655 ? S2 Nb4 Br5 82.97(17) . 4_655 ? S2 Nb4 Br5 82.97(17) . . ? S2 Nb4 Br7 107.41(16) . . ? S2 Nb4 Br7 107.41(16) . 4_655 ? S2 Nb4 Br10 161.6(2) . . ? Rb1 Br1 Rb2 84.79(8) . 2_775 ? Nb1 Br1 Rb1 127.26(10) . . ? Nb1 Br1 Rb2 142.09(10) . 2_775 ? Nb1 Br1 Nb2 67.96(10) . . ? Nb2 Br1 Rb1 89.75(9) . . ? Nb2 Br1 Rb2 96.14(9) . 2_775 ? Nb1 Br2 Nb1 66.36(13) . 4_755 ? Nb1 Br3 Rb1 119.18(10) . 1_545 ? Nb1 Br3 Rb1 119.18(10) 4_855 1_545 ? Nb1 Br3 Nb1 98.37(14) 4_855 . ? Nb1 Br4 Rb2 144.28(12) 1_455 1_445 ? Nb1 Br4 Nb3 71.58(7) 1_455 . ? Nb3 Br4 Rb2 101.25(9) . 1_445 ? Rb1 Br5 Rb2 136.58(10) 1_455 . ? Nb2 Br5 Rb1 93.07(10) . 1_455 ? Nb2 Br5 Rb2 109.08(10) . . ? Nb2 Br5 Nb4 120.89(10) . . ? Nb4 Br5 Rb1 109.65(10) . 1_455 ? Nb4 Br5 Rb2 90.73(9) . . ? Rb1 Br6 Rb1 168.22(14) 1_455 . ? Rb1 Br6 Rb2 93.61(7) . 2_775 ? Rb1 Br6 Rb2 93.61(8) 1_455 2_775 ? Nb2 Br6 Rb1 93.85(7) . 1_455 ? Nb2 Br6 Rb1 93.85(7) . . ? Nb2 Br6 Rb2 101.28(12) . 2_775 ? Rb1 Br7 Rb2 85.78(8) 2_774 1_455 ? Nb3 Br7 Rb1 139.94(10) . 2_774 ? Nb3 Br7 Rb2 128.49(10) . 1_455 ? Nb3 Br7 Nb4 69.78(10) . . ? Nb4 Br7 Rb1 94.23(9) . 2_774 ? Nb4 Br7 Rb2 88.96(9) . 1_455 ? Nb3 Br8 Nb3 68.01(14) 4_655 . ? Nb3 Br9 Rb2 112.91(11) 4 1_445 ? Nb3 Br9 Rb2 112.91(11) . 1_445 ? Nb3 Br9 Nb3 98.41(15) 4 . ? Rb2 Br10 Rb1 93.05(11) . 2_774 ? Rb2 Br10 Rb1 93.05(11) 1_455 2_774 ? Rb2 Br10 Rb2 166.00(18) 1_455 . ? Nb4 Br10 Rb1 95.08(16) . 2_774 ? Nb4 Br10 Rb2 96.00(9) . . ? Nb4 Br10 Rb2 96.00(9) . 1_455 ? Nb1 S1 Nb1 72.1(2) . 4_755 ? Nb1 S1 Nb3 132.0(3) 4_755 1_655 ? Nb1 S1 Nb3 75.69(12) . 1_655 ? Nb1 S1 Nb3 132.0(3) . 4_655 ? Nb1 S1 Nb3 75.69(12) 4_755 4_655 ? Nb2 S1 Nb1 75.6(2) . 4_755 ? Nb2 S1 Nb1 75.6(2) . . ? Nb2 S1 Nb3 128.57(14) . 1_655 ? Nb2 S1 Nb3 128.57(14) . 4_655 ? Nb3 S1 Nb3 102.2(3) 4_655 1_655 ? Nb1 S2 Nb1 109.9(3) 4_755 1_455 ? Nb3 S2 Nb1 134.7(3) 4_655 1_455 ? Nb3 S2 Nb1 134.7(3) . 4_755 ? Nb3 S2 Nb1 75.67(12) . 1_455 ? Nb3 S2 Nb1 75.68(12) 4_655 4_755 ? Nb3 S2 Nb3 71.0(2) . 4_655 ? Nb3 S2 Nb4 71.1(2) 4_655 . ? Nb3 S2 Nb4 71.1(2) . . ? Nb4 S2 Nb1 124.86(17) . 1_455 ? Nb4 S2 Nb1 124.86(17) . 4_755 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb1 Rb2 5.230(4) 2_775 ? Rb1 Rb2 5.230(4) 2_875 ? Rb1 Br1 3.805(4) 4_855 ? Rb1 Br1 3.805(4) . ? Rb1 Br3 3.517(5) 1_565 ? Rb1 Br5 3.596(4) 1_655 ? Rb1 Br5 3.596(4) 4_755 ? Rb1 Br6 3.5295(6) . ? Rb1 Br6 3.5295(6) 1_655 ? Rb1 Br7 3.772(4) 2_775 ? Rb1 Br7 3.772(4) 3_675 ? Rb1 Br10 3.670(7) 2_775 ? Rb2 Br1 3.951(4) 2_774 ? Rb2 Br1 3.951(4) 3_574 ? Rb2 Br4 3.854(4) 1_665 ? Rb2 Br4 3.854(4) 4_665 ? Rb2 Br5 3.712(4) . ? Rb2 Br5 3.712(4) 4_755 ? Rb2 Br6 3.645(4) 2_774 ? Rb2 Br7 3.912(4) 4_655 ? Rb2 Br7 3.912(4) 1_655 ? Rb2 Br9 3.371(5) 1_665 ? Rb2 Br10 3.5373(8) . ? Rb2 Br10 3.5373(8) 1_655 ? Nb1 Nb1 2.812(4) 4_755 ? Nb1 Nb2 2.893(3) . ? Nb1 Nb3 3.102(2) 1_655 ? Nb1 Br1 2.587(3) . ? Nb1 Br2 2.569(4) . ? Nb1 Br3 2.781(3) . ? Nb1 Br4 2.637(3) 1_655 ? Nb1 S1 2.388(7) . ? Nb1 S2 2.572(6) 1_655 ? Nb2 Br1 2.589(3) . ? Nb2 Br1 2.589(3) 4_755 ? Nb2 Br5 2.672(3) 4_755 ? Nb2 Br5 2.672(3) . ? Nb2 Br6 2.711(4) . ? Nb2 S1 2.329(8) . ? Nb3 Nb3 2.886(4) 4_655 ? Nb3 Nb4 2.904(3) . ? Nb3 Br4 2.668(3) . ? Nb3 Br7 2.503(3) . ? Nb3 Br8 2.580(4) . ? Nb3 Br9 2.731(3) . ? Nb3 S1 2.656(5) 1_455 ? Nb3 S2 2.485(7) . ? Nb4 Br5 2.742(3) 4_655 ? Nb4 Br5 2.742(3) . ? Nb4 Br7 2.573(3) 4_655 ? Nb4 Br7 2.573(3) . ? Nb4 Br10 2.661(5) . ? Nb4 S2 2.508(9) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.50(3) 2 0.50(3) loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.1835 -11.5525 -12.4417 -0.5599 0.8148 0.1503 0.1222 11.4436 12.4727 0.5622 -0.8184 -0.1193 -9.7783 3.0495 -1.4628 -0.0955 0.1432 -0.9851 0.0395 25.3108 -3.1240 -0.6780 -0.7143 -0.1732 0.1732 9.8570 -12.8196 -0.9913 0.1310 -0.0090 -0.4019 13.9950 11.6969 0.4679 -0.8637 -0.1873 -0.2004 17.0595 -10.4398 -0.9775 -0.1809 -0.1084 0.0396 -17.0030 10.4689 0.9791 0.1812 0.0920