#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1144 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700017.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_7700017 loop_ _publ_author_name 'Benjamin, Sophie L.' 'Chang, Yao-Pang' 'Hector, Andrew L.' 'Jura, Marek' 'Levason, William' 'Reid, Gillian' 'Stenning, Gavin' _publ_section_title ; Niobium tetrahalide complexes with neutral diphosphine ligands ; _journal_issue 19 _journal_name_full 'Dalton Transactions' _journal_page_first 8192 _journal_page_last 8200 _journal_paper_doi 10.1039/C6DT01099G _journal_volume 45 _journal_year 2016 _chemical_formula_moiety 'C12 H32 Br4 Nb P4' _chemical_formula_sum 'C12 H32 Br4 Nb P4' _chemical_formula_weight 712.80 _chemical_name_common '[NbBr4(DMPE)2]]' _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-02-15 deposited with the CCDC. 2016-04-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.3974(9) _cell_length_b 12.4285(9) _cell_length_c 14.1808(10) _cell_measurement_reflns_used 20103 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.7 _cell_volume 2361.2(3) _computing_cell_refinement 'Bruker XSCANS' _computing_data_collection 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku AFC12 (Right)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_unetI/netI 0.0378 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 18564 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 2.657 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 7.543 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour Green _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Chip _exptl_crystal_F_000 1380 _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.432 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.081 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.023(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 4641 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0221 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0435 _reflns_Friedel_coverage 0.915 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 4406 _reflns_number_total 4641 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6dt01099g2.cif _cod_data_source_block 1009r2 _cod_database_code 7700017 _shelx_shelxl_version_number 2014/7 _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_min 0.660 _shelx_estimated_absorpt_t_max 0.805 _shelx_res_file ; 1009r2.res created by SHELXL-2014/7 TITL 1009r2 in Pca2(1) CELL 0.71073 13.3974 12.4285 14.1808 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0009 0.0010 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, -Y, Z SYMM 0.5-X, Y, 0.5+Z SFAC C H P Br Nb UNIT 48 128 16 16 4 OMIT 2 2 6 OMIT -4.00 52.00 L.S. 4 ACTA BOND BOND $H FMAP 2 PLAN 5 TWIN SIZE 0.06 0.04 0.03 TEMP -173 WGHT 0.015300 BASF 0.02306 FVAR 0.08760 MOLE 1 NB1 5 0.011922 0.261006 0.906597 11.00000 0.01174 0.01170 = 0.01252 -0.00043 0.00053 0.00006 BR1 4 -0.164633 0.263718 0.815186 11.00000 0.01530 0.02835 = 0.01851 -0.00038 -0.00332 0.00214 BR2 4 -0.048586 0.067815 0.974619 11.00000 0.01786 0.01378 = 0.01898 -0.00013 0.00262 -0.00199 BR3 4 0.122698 0.341602 1.048002 11.00000 0.01638 0.02039 = 0.01986 -0.00673 -0.00139 -0.00087 BR4 4 0.138482 0.366346 0.791680 11.00000 0.01824 0.01823 = 0.02339 0.00435 0.00578 -0.00035 P1 3 -0.116265 0.294854 1.051072 11.00000 0.01619 0.01658 = 0.01519 -0.00129 0.00285 0.00166 P2 3 -0.043522 0.468948 0.899017 11.00000 0.01823 0.01502 = 0.02578 0.00322 0.00402 0.00179 P3 3 0.028115 0.139888 0.749533 11.00000 0.01747 0.02262 = 0.01331 -0.00258 0.00097 -0.00162 P4 3 0.176550 0.138371 0.924469 11.00000 0.01386 0.01421 = 0.01639 -0.00124 0.00013 0.00124 C1 1 -0.082573 0.244093 1.168599 11.00000 0.02606 0.02886 = 0.01260 -0.00068 0.00632 0.00212 AFIX 137 H1A 2 -0.130744 0.270600 1.215128 11.00000 -1.50000 H1B 2 -0.015562 0.269368 1.185246 11.00000 -1.50000 H1C 2 -0.083451 0.165250 1.168075 11.00000 -1.50000 AFIX 0 C2 1 -0.243886 0.245191 1.040287 11.00000 0.01529 0.03215 = 0.02059 -0.00027 0.00633 0.00046 AFIX 137 H2A 2 -0.278053 0.252350 1.101070 11.00000 -1.50000 H2B 2 -0.242713 0.169304 1.021551 11.00000 -1.50000 H2C 2 -0.279453 0.287239 0.992447 11.00000 -1.50000 AFIX 0 C3 1 -0.136425 0.439448 1.070803 11.00000 0.02839 0.01723 = 0.02184 -0.00309 0.00780 0.00517 AFIX 23 H3A 2 -0.195862 0.450303 1.111178 11.00000 -1.20000 H3B 2 -0.077899 0.470799 1.103385 11.00000 -1.20000 AFIX 0 C4 1 -0.151831 0.495358 0.975612 11.00000 0.02444 0.01785 = 0.03100 0.00279 0.00499 0.00864 AFIX 23 H4A 2 -0.159464 0.573816 0.985283 11.00000 -1.20000 H4B 2 -0.213353 0.467951 0.945306 11.00000 -1.20000 AFIX 0 C5 1 -0.082448 0.523134 0.784841 11.00000 0.02908 0.02419 = 0.03417 0.01287 0.00268 0.00700 AFIX 137 H5A 2 -0.139250 0.481594 0.760954 11.00000 -1.50000 H5B 2 -0.026878 0.518215 0.740109 11.00000 -1.50000 H5C 2 -0.102068 0.598617 0.792299 11.00000 -1.50000 AFIX 0 C6 1 0.045103 0.572256 0.938233 11.00000 0.02574 0.01511 = 0.04949 -0.00162 0.00595 -0.00093 AFIX 137 H6A 2 0.106567 0.566925 0.901057 11.00000 -1.50000 H6B 2 0.060581 0.561350 1.005096 11.00000 -1.50000 H6C 2 0.015490 0.643663 0.929489 11.00000 -1.50000 AFIX 0 C7 1 0.016569 0.205787 0.634477 11.00000 0.03135 0.04221 = 0.01612 -0.00310 0.00012 -0.00026 AFIX 137 H7A 2 0.014987 0.151117 0.584699 11.00000 -1.50000 H7B 2 0.073782 0.253584 0.624513 11.00000 -1.50000 H7C 2 -0.045239 0.247908 0.632676 11.00000 -1.50000 AFIX 0 C8 1 -0.055996 0.024951 0.735494 11.00000 0.02656 0.03485 = 0.02083 -0.00816 0.00277 -0.00794 AFIX 137 H8A 2 -0.124598 0.050843 0.727732 11.00000 -1.50000 H8B 2 -0.052028 -0.021010 0.791522 11.00000 -1.50000 H8C 2 -0.036397 -0.016522 0.679710 11.00000 -1.50000 AFIX 0 C9 1 0.150407 0.073416 0.742113 11.00000 0.01777 0.02425 = 0.01911 -0.00932 0.00371 -0.00061 AFIX 23 H9A 2 0.147889 0.014568 0.695123 11.00000 -1.20000 H9B 2 0.201745 0.125821 0.721818 11.00000 -1.20000 AFIX 0 C10 1 0.177312 0.028043 0.838914 11.00000 0.01603 0.01288 = 0.02764 -0.00113 0.00459 -0.00063 AFIX 23 H10A 2 0.244259 -0.005587 0.836745 11.00000 -1.20000 H10B 2 0.128254 -0.027578 0.857606 11.00000 -1.20000 AFIX 0 C11 1 0.196795 0.070703 1.036890 11.00000 0.02469 0.02555 = 0.02165 0.00292 -0.00140 0.00920 AFIX 137 H11A 2 0.146653 0.014061 1.045099 11.00000 -1.50000 H11B 2 0.190981 0.122980 1.088333 11.00000 -1.50000 H11C 2 0.263636 0.038684 1.037680 11.00000 -1.50000 AFIX 0 C12 1 0.299059 0.198846 0.904324 11.00000 0.01213 0.02023 = 0.03297 -0.00254 0.00008 0.00316 AFIX 137 H12A 2 0.308731 0.258972 0.948090 11.00000 -1.50000 H12B 2 0.303018 0.225245 0.839312 11.00000 -1.50000 H12C 2 0.351116 0.144749 0.914767 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1009r2 in Pca2(1) REM R1 = 0.0221 for 4406 Fo > 4sig(Fo) and 0.0250 for all 4641 data REM 199 parameters refined using 1 restraints END WGHT 0.0153 0.0000 REM Highest difference peak 0.432, deepest hole -0.317, 1-sigma level 0.081 Q1 1 0.1798 0.3448 1.0929 11.00000 0.05 0.43 Q2 1 -0.0058 0.0763 0.9221 11.00000 0.05 0.42 Q3 1 -0.1195 0.2735 0.7568 11.00000 0.05 0.36 Q4 1 -0.2120 0.2670 0.8790 11.00000 0.05 0.36 Q5 1 0.1921 0.3737 0.8471 11.00000 0.05 0.33 ; _shelx_res_checksum 66437 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' 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 Nb1 Nb 0.01192(3) 0.26101(4) 0.90660(3) 0.01199(10) Uani 1 1 d . . . . . Br1 Br -0.16463(4) 0.26372(5) 0.81519(4) 0.02072(13) Uani 1 1 d . . . . . Br2 Br -0.04859(4) 0.06782(4) 0.97462(4) 0.01687(12) Uani 1 1 d . . . . . Br3 Br 0.12270(4) 0.34160(4) 1.04800(4) 0.01888(12) Uani 1 1 d . . . . . Br4 Br 0.13848(4) 0.36635(5) 0.79168(4) 0.01995(13) Uani 1 1 d . . . . . P1 P -0.11626(11) 0.29485(11) 1.05107(9) 0.0160(3) Uani 1 1 d . . . . . P2 P -0.04352(11) 0.46895(12) 0.89902(10) 0.0197(3) Uani 1 1 d . . . . . P3 P 0.02811(11) 0.13989(12) 0.74953(9) 0.0178(3) Uani 1 1 d . . . . . P4 P 0.17655(10) 0.13837(12) 0.92447(10) 0.0148(3) Uani 1 1 d . . . . . C1 C -0.0826(5) 0.2441(5) 1.1686(3) 0.0225(14) Uani 1 1 d . . . . . H1A H -0.1307 0.2706 1.2151 0.034 Uiso 1 1 calc R U . . . H1B H -0.0156 0.2694 1.1852 0.034 Uiso 1 1 calc R U . . . H1C H -0.0835 0.1652 1.1681 0.034 Uiso 1 1 calc R U . . . C2 C -0.2439(4) 0.2452(5) 1.0403(4) 0.0227(13) Uani 1 1 d . . . . . H2A H -0.2781 0.2523 1.1011 0.034 Uiso 1 1 calc R U . . . H2B H -0.2427 0.1693 1.0216 0.034 Uiso 1 1 calc R U . . . H2C H -0.2795 0.2872 0.9924 0.034 Uiso 1 1 calc R U . . . C3 C -0.1364(5) 0.4394(5) 1.0708(4) 0.0225(13) Uani 1 1 d . . . . . H3A H -0.1959 0.4503 1.1112 0.027 Uiso 1 1 calc R U . . . H3B H -0.0779 0.4708 1.1034 0.027 Uiso 1 1 calc R U . . . C4 C -0.1518(4) 0.4954(5) 0.9756(4) 0.0244(13) Uani 1 1 d . . . . . H4A H -0.1595 0.5738 0.9853 0.029 Uiso 1 1 calc R U . . . H4B H -0.2134 0.4680 0.9453 0.029 Uiso 1 1 calc R U . . . C5 C -0.0824(5) 0.5231(5) 0.7848(4) 0.0291(15) Uani 1 1 d . . . . . H5A H -0.1392 0.4816 0.7610 0.044 Uiso 1 1 calc R U . . . H5B H -0.0269 0.5182 0.7401 0.044 Uiso 1 1 calc R U . . . H5C H -0.1021 0.5986 0.7923 0.044 Uiso 1 1 calc R U . . . C6 C 0.0451(5) 0.5723(5) 0.9382(4) 0.0301(16) Uani 1 1 d . . . . . H6A H 0.1066 0.5669 0.9011 0.045 Uiso 1 1 calc R U . . . H6B H 0.0606 0.5613 1.0051 0.045 Uiso 1 1 calc R U . . . H6C H 0.0155 0.6437 0.9295 0.045 Uiso 1 1 calc R U . . . C7 C 0.0166(5) 0.2058(5) 0.6345(4) 0.0299(15) Uani 1 1 d . . . . . H7A H 0.0150 0.1511 0.5847 0.045 Uiso 1 1 calc R U . . . H7B H 0.0738 0.2536 0.6245 0.045 Uiso 1 1 calc R U . . . H7C H -0.0452 0.2479 0.6327 0.045 Uiso 1 1 calc R U . . . C8 C -0.0560(5) 0.0250(5) 0.7355(4) 0.0274(14) Uani 1 1 d . . . . . H8A H -0.1246 0.0508 0.7277 0.041 Uiso 1 1 calc R U . . . H8B H -0.0520 -0.0210 0.7915 0.041 Uiso 1 1 calc R U . . . H8C H -0.0364 -0.0165 0.6797 0.041 Uiso 1 1 calc R U . . . C9 C 0.1504(4) 0.0734(5) 0.7421(4) 0.0204(13) Uani 1 1 d . . . . . H9A H 0.1479 0.0146 0.6951 0.024 Uiso 1 1 calc R U . . . H9B H 0.2017 0.1258 0.7218 0.024 Uiso 1 1 calc R U . . . C10 C 0.1773(4) 0.0280(4) 0.8389(3) 0.0189(12) Uani 1 1 d . . . . . H10A H 0.2443 -0.0056 0.8367 0.023 Uiso 1 1 calc R U . . . H10B H 0.1283 -0.0276 0.8576 0.023 Uiso 1 1 calc R U . . . C11 C 0.1968(4) 0.0707(5) 1.0369(4) 0.0240(13) Uani 1 1 d . . . . . H11A H 0.1467 0.0141 1.0451 0.036 Uiso 1 1 calc R U . . . H11B H 0.1910 0.1230 1.0883 0.036 Uiso 1 1 calc R U . . . H11C H 0.2636 0.0387 1.0377 0.036 Uiso 1 1 calc R U . . . C12 C 0.2991(4) 0.1988(4) 0.9043(4) 0.0218(12) Uani 1 1 d . . . . . H12A H 0.3087 0.2590 0.9481 0.033 Uiso 1 1 calc R U . . . H12B H 0.3030 0.2252 0.8393 0.033 Uiso 1 1 calc R U . . . H12C H 0.3511 0.1447 0.9148 0.033 Uiso 1 1 calc R U . . . 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 0.0117(2) 0.0117(2) 0.01252(19) -0.0004(2) 0.0005(2) 0.00006(19) Br1 0.0153(3) 0.0283(4) 0.0185(2) -0.0004(2) -0.0033(2) 0.0021(2) Br2 0.0179(3) 0.0138(3) 0.0190(2) -0.0001(2) 0.0026(2) -0.0020(2) Br3 0.0164(3) 0.0204(3) 0.0199(2) -0.0067(2) -0.0014(2) -0.0009(2) Br4 0.0182(3) 0.0182(3) 0.0234(3) 0.0044(2) 0.0058(2) -0.0004(2) P1 0.0162(7) 0.0166(7) 0.0152(6) -0.0013(6) 0.0028(6) 0.0017(6) P2 0.0182(8) 0.0150(8) 0.0258(7) 0.0032(6) 0.0040(6) 0.0018(6) P3 0.0175(8) 0.0226(8) 0.0133(6) -0.0026(6) 0.0010(6) -0.0016(6) P4 0.0139(7) 0.0142(7) 0.0164(6) -0.0012(5) 0.0001(6) 0.0012(6) C1 0.026(4) 0.029(4) 0.013(2) -0.001(2) 0.006(2) 0.002(3) C2 0.015(3) 0.032(4) 0.021(3) 0.000(3) 0.006(2) 0.000(3) C3 0.028(4) 0.017(3) 0.022(3) -0.003(2) 0.008(2) 0.005(3) C4 0.024(3) 0.018(3) 0.031(3) 0.003(3) 0.005(3) 0.009(3) C5 0.029(4) 0.024(3) 0.034(3) 0.013(3) 0.003(3) 0.007(3) C6 0.026(4) 0.015(3) 0.049(4) -0.002(3) 0.006(3) -0.001(3) C7 0.031(4) 0.042(4) 0.016(3) -0.003(3) 0.000(3) 0.000(3) C8 0.027(4) 0.035(4) 0.021(3) -0.008(3) 0.003(2) -0.008(3) C9 0.018(3) 0.024(3) 0.019(3) -0.009(2) 0.004(2) -0.001(3) C10 0.016(3) 0.013(3) 0.028(3) -0.001(2) 0.005(2) -0.001(2) C11 0.025(3) 0.026(3) 0.022(3) 0.003(2) -0.001(2) 0.009(3) C12 0.012(3) 0.020(3) 0.033(3) -0.003(3) 0.000(3) 0.003(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 Br3 Nb1 P2 79.88(4) . . ? Br3 Nb1 Br4 85.56(2) . . ? P2 Nb1 Br4 71.49(3) . . ? Br3 Nb1 P4 71.85(3) . . ? P2 Nb1 P4 140.66(5) . . ? Br4 Nb1 P4 79.42(4) . . ? Br3 Nb1 P3 141.22(4) . . ? P2 Nb1 P3 121.68(5) . . ? Br4 Nb1 P3 73.79(4) . . ? P4 Nb1 P3 72.30(4) . . ? Br3 Nb1 Br1 146.92(2) . . ? P2 Nb1 Br1 74.14(4) . . ? Br4 Nb1 Br1 104.80(2) . . ? P4 Nb1 Br1 140.40(4) . . ? P3 Nb1 Br1 71.38(4) . . ? Br3 Nb1 P1 74.20(3) . . ? P2 Nb1 P1 72.89(4) . . ? Br4 Nb1 P1 141.49(4) . . ? P4 Nb1 P1 122.44(5) . . ? P3 Nb1 P1 139.73(5) . . ? Br1 Nb1 P1 78.78(4) . . ? Br3 Nb1 Br2 103.28(2) . . ? P2 Nb1 Br2 141.45(4) . . ? Br4 Nb1 Br2 146.55(2) . . ? P4 Nb1 Br2 73.15(3) . . ? P3 Nb1 Br2 79.84(4) . . ? Br1 Nb1 Br2 85.40(2) . . ? P1 Nb1 Br2 71.25(3) . . ? C2 P1 C1 101.0(3) . . ? C2 P1 C3 101.9(3) . . ? C1 P1 C3 103.5(3) . . ? C2 P1 Nb1 118.60(18) . . ? C1 P1 Nb1 118.5(2) . . ? C3 P1 Nb1 111.12(18) . . ? C5 P2 C6 101.2(3) . . ? C5 P2 C4 103.4(3) . . ? C6 P2 C4 101.9(3) . . ? C5 P2 Nb1 117.9(2) . . ? C6 P2 Nb1 118.8(2) . . ? C4 P2 Nb1 111.41(19) . . ? C8 P3 C7 101.5(3) . . ? C8 P3 C9 101.1(3) . . ? C7 P3 C9 103.0(3) . . ? C8 P3 Nb1 118.42(19) . . ? C7 P3 Nb1 118.6(2) . . ? C9 P3 Nb1 111.71(18) . . ? C11 P4 C12 101.1(3) . . ? C11 P4 C10 103.5(3) . . ? C12 P4 C10 101.5(3) . . ? C11 P4 Nb1 117.73(19) . . ? C12 P4 Nb1 119.21(18) . . ? C10 P4 Nb1 111.47(19) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 109.2(4) . . ? C4 C3 H3A 109.8 . . ? P1 C3 H3A 109.8 . . ? C4 C3 H3B 109.8 . . ? P1 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 C4 P2 109.4(4) . . ? C3 C4 H4A 109.8 . . ? P2 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? P2 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P3 109.0(4) . . ? C10 C9 H9A 109.9 . . ? P3 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? P3 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C9 C10 P4 108.5(4) . . ? C9 C10 H10A 110.0 . . ? P4 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? P4 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 Nb1 Br3 2.6883(7) . ? Nb1 P2 2.6912(16) . ? Nb1 Br4 2.6916(7) . ? Nb1 P4 2.6929(15) . ? Nb1 P3 2.6970(15) . ? Nb1 Br1 2.6975(7) . ? Nb1 P1 2.7062(15) . ? Nb1 Br2 2.7116(7) . ? P1 C2 1.824(6) . ? P1 C1 1.838(5) . ? P1 C3 1.839(6) . ? P2 C5 1.829(5) . ? P2 C6 1.835(6) . ? P2 C4 1.842(6) . ? P3 C8 1.830(6) . ? P3 C7 1.832(6) . ? P3 C9 1.838(6) . ? P4 C11 1.823(5) . ? P4 C12 1.828(5) . ? P4 C10 1.831(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.532(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.527(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ?