#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1144 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700021.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_7700021 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 'C30 H72 Cl6 Nb2 O2 P6' _chemical_formula_sum 'C30 H72 Cl6 Nb2 O2 P6' _chemical_formula_weight 1049.21 _chemical_name_common '[{NbOCl3(DEPE)2}(DEPE)]' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _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 95.496(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.8162(3) _cell_length_b 11.6449(3) _cell_length_c 20.2185(14) _cell_measurement_reflns_used 17854 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.0 _cell_volume 2300.53(19) _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 0.998 _diffrn_measured_fraction_theta_max 0.995 _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 0.0349 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 20644 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.481 _diffrn_reflns_theta_min 3.042 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.758 _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 Orange _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Column _exptl_crystal_F_000 1084 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.502 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 214 _refine_ls_number_reflns 5247 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0288 _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^)+(0.0245P)^2^+2.3917P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.0665 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4591 _reflns_number_total 5247 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6dt01099g2.cif _cod_data_source_block 2015_0606r3 _cod_original_cell_volume 2300.52(19) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7700021 _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 0.863 _shelx_estimated_absorpt_t_max 0.948 _shelx_res_file ; 2015_0606r3.res created by SHELXL-2014/7 TITL 2015_0606r3 in P2(1)/c CELL 0.71073 9.8162 11.6449 20.2185 90.000 95.496 90.000 ZERR 2.00 0.0003 0.0003 0.0014 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O P Cl Nb UNIT 60 144 4 12 12 4 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 DELU 0.0001 Nb1 P3 SIZE 0.14 0.06 0.05 DELU P3 TEMP -173 WGHT 0.024500 2.391700 FVAR 0.19654 MOLE 1 NB1 6 0.219472 0.207226 0.114743 11.00000 0.01408 0.01273 = 0.01269 -0.00046 0.00057 -0.00134 CL1 5 0.102484 0.062386 0.180580 11.00000 0.03134 0.01816 = 0.01924 -0.00114 0.00846 -0.00772 CL2 5 0.438884 0.182350 0.194235 11.00000 0.01728 0.02327 = 0.02051 0.00178 -0.00094 0.00537 CL3 5 0.368312 0.233108 0.023944 11.00000 0.02788 0.02099 = 0.01915 -0.00360 0.00872 -0.00759 O1 3 0.073852 0.257697 0.069603 11.00000 0.01612 0.01994 = 0.02023 -0.00289 -0.00080 -0.00186 P1 4 0.130455 0.303695 0.224205 11.00000 0.01480 0.01583 = 0.01515 -0.00167 0.00032 0.00059 P2 4 0.310475 0.423051 0.126492 11.00000 0.01491 0.01395 = 0.01767 -0.00011 -0.00072 -0.00094 P3 4 0.212880 -0.002217 0.050330 11.00000 0.01429 0.01351 = 0.01669 -0.00183 0.00080 -0.00129 C1 1 -0.056118 0.300381 0.226439 11.00000 0.01607 0.02605 = 0.02296 -0.00230 0.00252 0.00146 AFIX 23 H1A 2 -0.086970 0.219440 0.223581 11.00000 -1.20000 H1B 2 -0.078304 0.330918 0.269829 11.00000 -1.20000 AFIX 0 C2 1 -0.136536 0.368588 0.171233 11.00000 0.02110 0.03259 = 0.02793 -0.00503 -0.00278 0.00600 AFIX 137 H2A 2 -0.110548 0.449755 0.174934 11.00000 -1.50000 H2B 2 -0.234758 0.360835 0.175396 11.00000 -1.50000 H2C 2 -0.115920 0.338952 0.127933 11.00000 -1.50000 AFIX 0 C3 1 0.203649 0.236923 0.302109 11.00000 0.02051 0.02272 = 0.01618 0.00049 -0.00138 0.00327 AFIX 23 H3A 2 0.216493 0.153953 0.294018 11.00000 -1.20000 H3B 2 0.295239 0.270577 0.314284 11.00000 -1.20000 AFIX 0 C4 1 0.118891 0.250287 0.360913 11.00000 0.03523 0.04479 = 0.01683 0.00311 0.00149 0.01045 AFIX 137 H4A 2 0.092629 0.330962 0.365103 11.00000 -1.50000 H4B 2 0.173120 0.225720 0.401676 11.00000 -1.50000 H4C 2 0.036384 0.202777 0.353800 11.00000 -1.50000 AFIX 0 C5 1 0.479511 0.454683 0.101526 11.00000 0.01729 0.02376 = 0.03029 -0.00110 0.00256 -0.00603 AFIX 23 H5A 2 0.546026 0.401316 0.125101 11.00000 -1.20000 H5B 2 0.478910 0.439153 0.053357 11.00000 -1.20000 AFIX 0 C6 1 0.529314 0.577008 0.114839 11.00000 0.03583 0.03396 = 0.03725 -0.01071 0.01221 -0.02001 AFIX 137 H6A 2 0.465558 0.630910 0.090988 11.00000 -1.50000 H6B 2 0.620397 0.586175 0.099481 11.00000 -1.50000 H6C 2 0.534061 0.592722 0.162623 11.00000 -1.50000 AFIX 0 C7 1 0.191778 0.524892 0.081909 11.00000 0.02429 0.01940 = 0.02571 0.00197 -0.00072 0.00221 AFIX 23 H7A 2 0.098248 0.509012 0.094017 11.00000 -1.20000 H7B 2 0.216579 0.603534 0.097288 11.00000 -1.20000 AFIX 0 C8 1 0.189509 0.521544 0.006644 11.00000 0.03252 0.03398 = 0.02585 0.00944 -0.00104 0.00106 AFIX 137 H8A 2 0.280115 0.542048 -0.006249 11.00000 -1.50000 H8B 2 0.121536 0.576400 -0.013012 11.00000 -1.50000 H8C 2 0.165414 0.444027 -0.009325 11.00000 -1.50000 AFIX 0 C9 1 0.177675 0.454926 0.238076 11.00000 0.02530 0.01681 = 0.02059 -0.00305 0.00190 0.00103 AFIX 23 H9A 2 0.107666 0.505264 0.214516 11.00000 -1.20000 H9B 2 0.182794 0.472898 0.286109 11.00000 -1.20000 AFIX 0 C10 1 0.315693 0.475763 0.212218 11.00000 0.02232 0.01787 = 0.02276 -0.00498 -0.00116 -0.00451 AFIX 23 H10A 2 0.388148 0.435086 0.240539 11.00000 -1.20000 H10B 2 0.336980 0.558879 0.213567 11.00000 -1.20000 AFIX 0 C11 1 0.294230 -0.019226 -0.027042 11.00000 0.01436 0.02519 = 0.02363 -0.00340 0.00257 -0.00266 AFIX 23 H11A 2 0.266115 0.046207 -0.056504 11.00000 -1.20000 H11B 2 0.394558 -0.013840 -0.016286 11.00000 -1.20000 AFIX 0 C12 1 0.263280 -0.130279 -0.065965 11.00000 0.02521 0.02832 = 0.03433 -0.01102 0.01049 -0.00268 AFIX 137 H12A 2 0.289060 -0.196323 -0.037429 11.00000 -1.50000 H12B 2 0.315684 -0.131689 -0.104848 11.00000 -1.50000 H12C 2 0.165259 -0.134000 -0.080562 11.00000 -1.50000 AFIX 0 C13 1 0.275648 -0.126236 0.100394 11.00000 0.01978 0.01951 = 0.02538 0.00248 0.00040 0.00249 AFIX 23 H13A 2 0.219958 -0.134235 0.138449 11.00000 -1.20000 H13B 2 0.262134 -0.196486 0.072973 11.00000 -1.20000 AFIX 0 C14 1 0.425928 -0.118087 0.126837 11.00000 0.02799 0.02270 = 0.04458 0.00336 -0.01027 0.00539 AFIX 137 H14A 2 0.483090 -0.124672 0.089849 11.00000 -1.50000 H14B 2 0.448363 -0.180373 0.158620 11.00000 -1.50000 H14C 2 0.443022 -0.043974 0.149058 11.00000 -1.50000 AFIX 0 C15 1 0.034164 -0.040366 0.026719 11.00000 0.01523 0.01665 = 0.01753 -0.00180 0.00049 -0.00283 AFIX 23 H15A 2 0.029684 -0.120146 0.009732 11.00000 -1.20000 H15B 2 -0.017059 -0.037293 0.066547 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2015_0606r3 in P2(1)/c REM R1 = 0.0288 for 4591 Fo > 4sig(Fo) and 0.0358 for all 5247 data REM 214 parameters refined using 1 restraints END WGHT 0.0245 2.3917 REM Highest difference peak 0.502, deepest hole -0.544, 1-sigma level 0.080 Q1 1 0.2263 0.0455 0.0682 11.00000 0.05 0.50 Q2 1 0.3824 0.4337 0.1095 11.00000 0.05 0.47 Q3 1 0.2426 -0.0536 0.0304 11.00000 0.05 0.45 Q4 1 0.2456 -0.0750 0.0752 11.00000 0.05 0.42 Q5 1 0.1492 0.3779 0.2401 11.00000 0.05 0.40 ; _shelx_res_checksum 7401 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, 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 0.21947(2) 0.20723(2) 0.11474(2) 0.01321(6) Uani 1 1 d . U . . . Cl1 Cl 0.10248(6) 0.06239(5) 0.18058(3) 0.02252(13) Uani 1 1 d . . . . . Cl2 Cl 0.43888(6) 0.18235(5) 0.19424(3) 0.02053(12) Uani 1 1 d . . . . . Cl3 Cl 0.36831(6) 0.23311(5) 0.02394(3) 0.02226(13) Uani 1 1 d . . . . . O1 O 0.07385(16) 0.25770(14) 0.06960(8) 0.0189(3) Uani 1 1 d . . . . . P1 P 0.13046(6) 0.30369(5) 0.22420(3) 0.01533(12) Uani 1 1 d . . . . . P2 P 0.31048(6) 0.42305(5) 0.12649(3) 0.01566(12) Uani 1 1 d . . . . . P3 P 0.21288(6) -0.00222(5) 0.05033(3) 0.01488(11) Uani 1 1 d . U . . . C1 C -0.0561(2) 0.3004(2) 0.22644(12) 0.0217(5) Uani 1 1 d . . . . . H1A H -0.0870 0.2194 0.2236 0.026 Uiso 1 1 calc R U . . . H1B H -0.0783 0.3309 0.2698 0.026 Uiso 1 1 calc R U . . . C2 C -0.1365(3) 0.3686(2) 0.17123(13) 0.0275(5) Uani 1 1 d . . . . . H2A H -0.1105 0.4498 0.1749 0.041 Uiso 1 1 calc R U . . . H2B H -0.2348 0.3608 0.1754 0.041 Uiso 1 1 calc R U . . . H2C H -0.1159 0.3390 0.1279 0.041 Uiso 1 1 calc R U . . . C3 C 0.2036(2) 0.2369(2) 0.30211(11) 0.0200(5) Uani 1 1 d . . . . . H3A H 0.2165 0.1540 0.2940 0.024 Uiso 1 1 calc R U . . . H3B H 0.2952 0.2706 0.3143 0.024 Uiso 1 1 calc R U . . . C4 C 0.1189(3) 0.2503(3) 0.36091(12) 0.0323(6) Uani 1 1 d . . . . . H4A H 0.0926 0.3310 0.3651 0.049 Uiso 1 1 calc R U . . . H4B H 0.1731 0.2257 0.4017 0.049 Uiso 1 1 calc R U . . . H4C H 0.0364 0.2028 0.3538 0.049 Uiso 1 1 calc R U . . . C5 C 0.4795(3) 0.4547(2) 0.10153(13) 0.0238(5) Uani 1 1 d . . . . . H5A H 0.5460 0.4013 0.1251 0.029 Uiso 1 1 calc R U . . . H5B H 0.4789 0.4392 0.0534 0.029 Uiso 1 1 calc R U . . . C6 C 0.5293(3) 0.5770(2) 0.11484(14) 0.0351(7) Uani 1 1 d . . . . . H6A H 0.4656 0.6309 0.0910 0.053 Uiso 1 1 calc R U . . . H6B H 0.6204 0.5862 0.0995 0.053 Uiso 1 1 calc R U . . . H6C H 0.5341 0.5927 0.1626 0.053 Uiso 1 1 calc R U . . . C7 C 0.1918(3) 0.5249(2) 0.08191(12) 0.0233(5) Uani 1 1 d . . . . . H7A H 0.0982 0.5090 0.0940 0.028 Uiso 1 1 calc R U . . . H7B H 0.2166 0.6035 0.0973 0.028 Uiso 1 1 calc R U . . . C8 C 0.1895(3) 0.5215(2) 0.00664(13) 0.0310(6) Uani 1 1 d . . . . . H8A H 0.2801 0.5420 -0.0062 0.047 Uiso 1 1 calc R U . . . H8B H 0.1215 0.5764 -0.0130 0.047 Uiso 1 1 calc R U . . . H8C H 0.1654 0.4440 -0.0093 0.047 Uiso 1 1 calc R U . . . C9 C 0.1777(3) 0.45493(19) 0.23808(12) 0.0209(5) Uani 1 1 d . . . . . H9A H 0.1077 0.5053 0.2145 0.025 Uiso 1 1 calc R U . . . H9B H 0.1828 0.4729 0.2861 0.025 Uiso 1 1 calc R U . . . C10 C 0.3157(3) 0.4758(2) 0.21222(11) 0.0212(5) Uani 1 1 d . . . . . H10A H 0.3881 0.4351 0.2405 0.025 Uiso 1 1 calc R U . . . H10B H 0.3370 0.5589 0.2136 0.025 Uiso 1 1 calc R U . . . C11 C 0.2942(2) -0.0192(2) -0.02704(12) 0.0210(5) Uani 1 1 d . . . . . H11A H 0.2661 0.0462 -0.0565 0.025 Uiso 1 1 calc R U . . . H11B H 0.3946 -0.0138 -0.0163 0.025 Uiso 1 1 calc R U . . . C12 C 0.2633(3) -0.1303(2) -0.06596(13) 0.0288(6) Uani 1 1 d . . . . . H12A H 0.2891 -0.1963 -0.0374 0.043 Uiso 1 1 calc R U . . . H12B H 0.3157 -0.1317 -0.1048 0.043 Uiso 1 1 calc R U . . . H12C H 0.1653 -0.1340 -0.0806 0.043 Uiso 1 1 calc R U . . . C13 C 0.2756(2) -0.1262(2) 0.10039(12) 0.0217(5) Uani 1 1 d . . . . . H13A H 0.2200 -0.1342 0.1384 0.026 Uiso 1 1 calc R U . . . H13B H 0.2621 -0.1965 0.0730 0.026 Uiso 1 1 calc R U . . . C14 C 0.4259(3) -0.1181(2) 0.12684(15) 0.0326(6) Uani 1 1 d . . . . . H14A H 0.4831 -0.1247 0.0898 0.049 Uiso 1 1 calc R U . . . H14B H 0.4484 -0.1804 0.1586 0.049 Uiso 1 1 calc R U . . . H14C H 0.4430 -0.0440 0.1491 0.049 Uiso 1 1 calc R U . . . C15 C 0.0342(2) -0.04037(19) 0.02672(11) 0.0165(4) Uani 1 1 d . . . . . H15A H 0.0297 -0.1201 0.0097 0.020 Uiso 1 1 calc R U . . . H15B H -0.0171 -0.0373 0.0665 0.020 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 0.01408(10) 0.01273(9) 0.01269(9) -0.00046(7) 0.00057(7) -0.00134(8) Cl1 0.0313(3) 0.0182(3) 0.0192(3) -0.0011(2) 0.0085(2) -0.0077(2) Cl2 0.0173(3) 0.0233(3) 0.0205(3) 0.0018(2) -0.0009(2) 0.0054(2) Cl3 0.0279(3) 0.0210(3) 0.0191(3) -0.0036(2) 0.0087(2) -0.0076(2) O1 0.0161(8) 0.0199(8) 0.0202(8) -0.0029(6) -0.0008(6) -0.0019(6) P1 0.0148(3) 0.0158(3) 0.0152(3) -0.0017(2) 0.0003(2) 0.0006(2) P2 0.0149(3) 0.0140(3) 0.0177(3) -0.0001(2) -0.0007(2) -0.0009(2) P3 0.0143(3) 0.0135(2) 0.0167(3) -0.00183(17) 0.0008(2) -0.0013(2) C1 0.0161(11) 0.0261(12) 0.0230(11) -0.0023(10) 0.0025(9) 0.0015(10) C2 0.0211(13) 0.0326(14) 0.0279(12) -0.0050(11) -0.0028(10) 0.0060(11) C3 0.0205(12) 0.0227(12) 0.0162(10) 0.0005(9) -0.0014(9) 0.0033(9) C4 0.0352(16) 0.0448(16) 0.0168(11) 0.0031(11) 0.0015(11) 0.0104(13) C5 0.0173(12) 0.0238(12) 0.0303(13) -0.0011(10) 0.0026(10) -0.0060(10) C6 0.0358(16) 0.0340(15) 0.0372(15) -0.0107(12) 0.0122(13) -0.0200(13) C7 0.0243(13) 0.0194(11) 0.0257(12) 0.0020(10) -0.0007(10) 0.0022(10) C8 0.0325(15) 0.0340(14) 0.0258(13) 0.0094(11) -0.0010(11) 0.0011(12) C9 0.0253(13) 0.0168(11) 0.0206(11) -0.0031(9) 0.0019(10) 0.0010(9) C10 0.0223(13) 0.0179(11) 0.0228(11) -0.0050(9) -0.0012(9) -0.0045(9) C11 0.0144(11) 0.0252(12) 0.0236(11) -0.0034(10) 0.0026(9) -0.0027(9) C12 0.0252(14) 0.0283(13) 0.0343(14) -0.0110(11) 0.0105(11) -0.0027(11) C13 0.0198(12) 0.0195(11) 0.0254(12) 0.0025(9) 0.0004(10) 0.0025(9) C14 0.0280(15) 0.0227(13) 0.0446(16) 0.0034(11) -0.0103(12) 0.0054(11) C15 0.0152(11) 0.0167(11) 0.0175(10) -0.0018(9) 0.0005(9) -0.0028(9) 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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 O1 Nb1 Cl3 94.84(6) . . ? O1 Nb1 Cl1 96.44(6) . . ? Cl3 Nb1 Cl1 144.44(2) . . ? O1 Nb1 Cl2 165.81(5) . . ? Cl3 Nb1 Cl2 87.64(2) . . ? Cl1 Nb1 Cl2 89.49(2) . . ? O1 Nb1 P2 88.83(5) . . ? Cl3 Nb1 P2 74.621(18) . . ? Cl1 Nb1 P2 139.092(19) . . ? Cl2 Nb1 P2 78.337(19) . . ? O1 Nb1 P1 88.57(5) . . ? Cl3 Nb1 P1 144.942(19) . . ? Cl1 Nb1 P1 69.054(18) . . ? Cl2 Nb1 P1 81.511(18) . . ? P2 Nb1 P1 70.570(18) . . ? O1 Nb1 P3 94.05(5) . . ? Cl3 Nb1 P3 75.307(18) . . ? Cl1 Nb1 P3 70.342(18) . . ? Cl2 Nb1 P3 100.089(19) . . ? P2 Nb1 P3 149.926(19) . . ? P1 Nb1 P3 139.348(18) . . ? C9 P1 C1 104.72(11) . . ? C9 P1 C3 101.68(11) . . ? C1 P1 C3 106.18(11) . . ? C9 P1 Nb1 115.31(8) . . ? C1 P1 Nb1 114.40(8) . . ? C3 P1 Nb1 113.28(8) . . ? C5 P2 C10 104.53(11) . . ? C5 P2 C7 106.61(12) . . ? C10 P2 C7 101.92(11) . . ? C5 P2 Nb1 118.20(8) . . ? C10 P2 Nb1 112.19(8) . . ? C7 P2 Nb1 111.89(8) . . ? C15 P3 C11 103.67(10) . . ? C15 P3 C13 102.46(10) . . ? C11 P3 C13 103.58(11) . . ? C15 P3 Nb1 108.43(7) . . ? C11 P3 Nb1 120.33(8) . . ? C13 P3 Nb1 116.30(8) . . ? C2 C1 P1 114.71(17) . . ? C2 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 115.30(17) . . ? C4 C3 H3A 108.4 . . ? P1 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? P1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P2 115.27(18) . . ? C6 C5 H5A 108.5 . . ? P2 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? P2 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 P2 114.98(18) . . ? C8 C7 H7A 108.5 . . ? P2 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? P2 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 108.75(16) . . ? C10 C9 H9A 109.9 . . ? P1 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? P1 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? C9 C10 P2 109.08(16) . . ? C9 C10 H10A 109.9 . . ? P2 C10 H10A 109.9 . . ? C9 C10 H10B 109.9 . . ? P2 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C12 C11 P3 116.68(17) . . ? C12 C11 H11A 108.1 . . ? P3 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? P3 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P3 114.03(17) . . ? C14 C13 H13A 108.7 . . ? P3 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? P3 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 C15 P3 112.2(2) 3 . ? C15 C15 H15A 109.2 3 . ? P3 C15 H15A 109.2 . . ? C15 C15 H15B 109.2 3 . ? P3 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? 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 O1 1.7239(16) . ? Nb1 Cl3 2.4717(6) . ? Nb1 Cl1 2.4956(6) . ? Nb1 Cl2 2.5774(6) . ? Nb1 P2 2.6703(6) . ? Nb1 P1 2.7007(6) . ? Nb1 P3 2.7627(6) . ? P1 C9 1.836(2) . ? P1 C1 1.837(2) . ? P1 C3 1.840(2) . ? P2 C5 1.818(2) . ? P2 C10 1.835(2) . ? P2 C7 1.837(2) . ? P3 C15 1.828(2) . ? P3 C11 1.834(2) . ? P3 C13 1.836(2) . ? C1 C2 1.527(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.523(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.522(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.520(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.518(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.529(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.523(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C15 1.537(4) 3 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ?