#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1144 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700018.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_7700018 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 'C20 H48 Cl4 Nb P4' _chemical_formula_sum 'C20 H48 Cl4 Nb P4' _chemical_formula_weight 647.17 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 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 95.008(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.5571(5) _cell_length_b 11.6652(5) _cell_length_c 11.9053(8) _cell_measurement_reflns_used 13285 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.0 _cell_volume 1460.55(14) _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 0.998 _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 0.0190 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12265 _diffrn_reflns_point_group_measured_fraction_full 0.851 _diffrn_reflns_point_group_measured_fraction_max 0.838 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 3.028 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.883 _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 Blue _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Chip _exptl_crystal_F_000 674 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.324 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.047 _refine_ls_abs_structure_details ; Flack x determined using 1758 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.039(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 4819 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0170 _refine_ls_R_factor_gt 0.0166 _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^)+(0.0170P)^2^+0.5735P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0404 _reflns_Friedel_coverage 0.597 _reflns_Friedel_fraction_full 0.688 _reflns_Friedel_fraction_max 0.661 _reflns_number_gt 4748 _reflns_number_total 4819 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6dt01099g2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7700018 _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 0.933 _shelx_estimated_absorpt_t_max 0.980 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelx in P2(1) CELL 0.71073 10.5571 11.6652 11.9053 90 95.008 90 ZERR 2 0.0005 0.0005 0.0008 0 0.007 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H P Cl Nb UNIT 40 96 8 8 2 OMIT -4 52 OMIT 4 -4 0 OMIT 7 7 2 OMIt -4 -3 10 OMIT 0 1 12 OMIT -5 -4 9 L.S. 4 PLAN 5 TEMP -173 BOND fmap 2 BOND $H SIZE 0.07 0.05 0.02 acta MORE -1 BOND $H WGHT 0.017000 0.573500 FVAR 0.32007 NB1 5 0.246676 0.884194 0.269260 11.00000 0.00903 0.00736 = 0.00707 0.00029 0.00008 0.00027 CL1 4 0.053099 0.953789 0.359336 11.00000 0.01530 0.01271 = 0.01460 0.00037 0.00457 0.00379 CL2 4 0.379891 0.957549 0.440474 11.00000 0.01523 0.01302 = 0.01108 -0.00127 -0.00261 -0.00156 CL3 4 0.391918 0.926841 0.116622 11.00000 0.01642 0.01722 = 0.01439 0.00446 0.00615 0.00051 CL4 4 0.164348 0.709964 0.160353 11.00000 0.01466 0.00924 = 0.01106 -0.00078 -0.00114 -0.00067 P1 3 0.079329 0.949558 0.098864 11.00000 0.01267 0.01017 = 0.00953 0.00051 -0.00115 0.00079 P2 3 0.270516 1.111803 0.250159 11.00000 0.01499 0.00982 = 0.01183 0.00100 -0.00167 -0.00181 P3 3 0.196804 0.735559 0.435342 11.00000 0.01152 0.01062 = 0.00870 0.00126 0.00115 -0.00022 P4 3 0.438080 0.728539 0.286806 11.00000 0.01075 0.01253 = 0.01023 0.00002 0.00104 0.00199 C1 1 -0.082763 0.894206 0.102532 11.00000 0.01656 0.02181 = 0.02116 0.00541 -0.00607 -0.00672 AFIX 23 H1A 2 -0.085361 0.816288 0.069453 11.00000 -1.20000 H1B 2 -0.100107 0.886245 0.182549 11.00000 -1.20000 AFIX 0 C2 1 -0.190186 0.963239 0.042810 11.00000 0.01264 0.02681 = 0.05190 0.01653 0.00385 0.00342 AFIX 137 H2A 2 -0.196151 1.037703 0.080095 11.00000 -1.50000 H2B 2 -0.270437 0.921579 0.045765 11.00000 -1.50000 H2C 2 -0.173394 0.975051 -0.036028 11.00000 -1.50000 AFIX 0 C3 1 0.123039 0.912327 -0.042534 11.00000 0.03416 0.02669 = 0.01085 0.00037 -0.00021 0.01254 PART 1 AFIX 23 H3AA 2 0.216957 0.907548 -0.038434 10.50000 -1.20000 H3AB 2 0.090021 0.834339 -0.060090 10.50000 -1.20000 AFIX 23 PART 0 PART 2 H3BC 2 0.207423 0.946549 -0.051302 10.50000 -1.20000 H3BD 2 0.133538 0.828062 -0.045175 10.50000 -1.20000 AFIX 0 PART 0 C5 1 0.197714 1.199343 0.355188 11.00000 0.02721 0.01381 = 0.01510 -0.00082 -0.00163 0.00002 AFIX 23 H5A 2 0.104659 1.186810 0.345354 11.00000 -1.20000 H5B 2 0.228056 1.170178 0.430885 11.00000 -1.20000 AFIX 0 C6 1 0.221680 1.328669 0.353851 11.00000 0.04871 0.01401 = 0.02886 -0.00166 0.00278 -0.00005 AFIX 137 H6A 2 0.313286 1.343386 0.365373 11.00000 -1.50000 H6B 2 0.178918 1.365151 0.414347 11.00000 -1.50000 H6C 2 0.188186 1.360307 0.280976 11.00000 -1.50000 AFIX 0 C7 1 0.434629 1.166741 0.256080 11.00000 0.01774 0.01726 = 0.02335 0.00472 -0.00361 -0.00680 AFIX 23 H7A 2 0.453483 1.205851 0.329436 11.00000 -1.20000 H7B 2 0.492839 1.100306 0.254809 11.00000 -1.20000 AFIX 0 C8 1 0.465534 1.248716 0.163750 11.00000 0.02829 0.05728 = 0.04170 0.02693 -0.00911 -0.02112 AFIX 137 H8A 2 0.455091 1.209401 0.090782 11.00000 -1.50000 H8B 2 0.553577 1.275141 0.178101 11.00000 -1.50000 H8C 2 0.407941 1.314674 0.162595 11.00000 -1.50000 AFIX 0 C9 1 0.060867 1.106281 0.096814 11.00000 0.01696 0.01214 = 0.01373 0.00071 -0.00171 0.00179 AFIX 23 H9A 2 0.018485 1.130752 0.023260 11.00000 -1.20000 H9B 2 0.007055 1.130212 0.156723 11.00000 -1.20000 AFIX 0 C10 1 0.191122 1.163046 0.115764 11.00000 0.01993 0.01194 = 0.01279 0.00355 -0.00166 -0.00106 AFIX 23 H10A 2 0.181318 1.247398 0.117980 11.00000 -1.20000 H10B 2 0.243060 1.143577 0.053106 11.00000 -1.20000 AFIX 0 C11 1 0.070915 0.627936 0.407827 11.00000 0.01593 0.01177 = 0.01291 0.00176 0.00119 -0.00156 AFIX 23 H11A 2 0.096449 0.575336 0.348567 11.00000 -1.20000 H11B 2 0.065652 0.582078 0.477236 11.00000 -1.20000 AFIX 0 C12 1 -0.061732 0.673991 0.370960 11.00000 0.01365 0.01916 = 0.02207 0.00019 0.00289 -0.00256 AFIX 137 H12A 2 -0.085505 0.731691 0.425143 11.00000 -1.50000 H12B 2 -0.123178 0.610857 0.367968 11.00000 -1.50000 H12C 2 -0.061585 0.708960 0.296125 11.00000 -1.50000 AFIX 0 C13 1 0.162787 0.796463 0.572276 11.00000 0.02231 0.01773 = 0.01012 0.00018 0.00441 -0.00106 AFIX 23 H13A 2 0.217639 0.864477 0.587743 11.00000 -1.20000 H13B 2 0.073378 0.822990 0.566519 11.00000 -1.20000 AFIX 0 C14 1 0.183105 0.714126 0.672520 11.00000 0.02269 0.02384 = 0.01073 0.00212 0.00235 -0.00203 AFIX 137 H14A 2 0.130079 0.645860 0.658037 11.00000 -1.50000 H14B 2 0.159467 0.752388 0.740935 11.00000 -1.50000 H14C 2 0.272762 0.691471 0.682696 11.00000 -1.50000 AFIX 0 C15 1 0.589353 0.767820 0.365261 11.00000 0.01226 0.01999 = 0.01575 -0.00092 -0.00238 0.00313 AFIX 23 H15A 2 0.571972 0.792585 0.441957 11.00000 -1.20000 H15B 2 0.643930 0.698780 0.373265 11.00000 -1.20000 AFIX 0 C16 1 0.662904 0.863113 0.311006 11.00000 0.01447 0.02784 = 0.02673 0.00108 0.00161 -0.00335 AFIX 137 H16A 2 0.682904 0.838811 0.235763 11.00000 -1.50000 H16B 2 0.741998 0.878751 0.357865 11.00000 -1.50000 H16C 2 0.610896 0.932781 0.304655 11.00000 -1.50000 AFIX 0 C17 1 0.486074 0.665282 0.155996 11.00000 0.01937 0.02231 = 0.01468 -0.00265 0.00443 0.00478 AFIX 23 H17A 2 0.409245 0.634704 0.112484 11.00000 -1.20000 H17B 2 0.520617 0.727006 0.110441 11.00000 -1.20000 AFIX 0 C18 1 0.584043 0.570034 0.170489 11.00000 0.04903 0.04144 = 0.02727 -0.00827 0.00688 0.02693 AFIX 137 H18A 2 0.664819 0.601374 0.203970 11.00000 -1.50000 H18B 2 0.596465 0.536529 0.096766 11.00000 -1.50000 H18C 2 0.554113 0.510687 0.220090 11.00000 -1.50000 AFIX 0 C19 1 0.333751 0.641896 0.472550 11.00000 0.01406 0.01486 = 0.01361 0.00573 -0.00001 0.00089 AFIX 23 H19A 2 0.398294 0.683807 0.522018 11.00000 -1.20000 H19B 2 0.306231 0.574235 0.514338 11.00000 -1.20000 AFIX 0 C20 1 0.391919 0.602757 0.365855 11.00000 0.01273 0.01142 = 0.01851 0.00248 -0.00064 0.00301 AFIX 23 H20A 2 0.329301 0.556506 0.318564 11.00000 -1.20000 H20B 2 0.467453 0.554374 0.386373 11.00000 -1.20000 AFIX 0 PART 1 C4 1 0.081501 0.986645 -0.139487 10.50000 0.03564 0.02932 = 0.01385 0.00820 0.00976 0.00990 AFIX 137 H4A 2 -0.010257 1.000118 -0.140972 10.50000 -1.50000 H4B 2 0.100625 0.949008 -0.209635 10.50000 -1.50000 H4C 2 0.126612 1.060046 -0.132091 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C4A 1 0.036720 0.946358 -0.142538 10.50000 0.01800 0.02484 = 0.01490 0.00280 0.00213 0.00444 AFIX 137 H4AA 2 -0.043990 0.904980 -0.141782 10.50000 -1.50000 H4AB 2 0.076495 0.927443 -0.211556 10.50000 -1.50000 H4AC 2 0.020828 1.029053 -0.140111 10.50000 -1.50000 AFIX 0 HKLF 4 REM shelx in P2(1) REM R1 = 0.0166 for 4748 Fo > 4sig(Fo) and 0.0170 for all 4819 data REM 280 parameters refined using 1 restraints END WGHT 0.0170 0.5674 REM Highest difference peak 0.324, deepest hole -0.208, 1-sigma level 0.047 Q1 1 0.2489 1.1469 0.3219 11.00000 0.05 0.32 Q2 1 0.4124 0.6650 0.3264 11.00000 0.05 0.27 Q3 1 0.2686 0.6771 0.4437 11.00000 0.05 0.27 Q4 1 -0.0014 0.9268 0.1011 11.00000 0.05 0.25 Q5 1 0.4724 0.6999 0.2209 11.00000 0.05 0.25 ; _shelx_res_checksum 76132 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Nb1 Nb 0.24668(2) 0.88419(2) 0.26926(2) 0.00786(6) Uani 1 1 d . . . . . Cl1 Cl 0.05310(6) 0.95379(6) 0.35934(5) 0.01401(14) Uani 1 1 d . . . . . Cl2 Cl 0.37989(6) 0.95755(6) 0.44047(5) 0.01333(14) Uani 1 1 d . . . . . Cl3 Cl 0.39192(6) 0.92684(6) 0.11662(5) 0.01573(15) Uani 1 1 d . . . . . Cl4 Cl 0.16435(6) 0.70996(6) 0.16035(5) 0.01178(13) Uani 1 1 d . . . . . P1 P 0.07933(7) 0.94956(6) 0.09886(6) 0.01091(15) Uani 1 1 d . . . . . P2 P 0.27052(7) 1.11180(7) 0.25016(6) 0.01238(15) Uani 1 1 d . . . . . P3 P 0.19680(7) 0.73556(6) 0.43534(5) 0.01026(14) Uani 1 1 d . . . . . P4 P 0.43808(7) 0.72854(6) 0.28681(6) 0.01116(15) Uani 1 1 d . . . . . C1 C -0.0828(3) 0.8942(3) 0.1025(2) 0.0203(6) Uani 1 1 d . . . . . H1A H -0.0854 0.8163 0.0695 0.024 Uiso 1 1 calc R U . . . H1B H -0.1001 0.8862 0.1825 0.024 Uiso 1 1 calc R U . . . C2 C -0.1902(3) 0.9632(3) 0.0428(3) 0.0304(8) Uani 1 1 d . . . . . H2A H -0.1962 1.0377 0.0801 0.046 Uiso 1 1 calc R U . . . H2B H -0.2704 0.9216 0.0458 0.046 Uiso 1 1 calc R U . . . H2C H -0.1734 0.9751 -0.0360 0.046 Uiso 1 1 calc R U . . . C3 C 0.1230(3) 0.9123(3) -0.0425(2) 0.0240(8) Uani 1 1 d . . . . . H3AA H 0.2170 0.9075 -0.0384 0.029 Uiso 0.5 1 calc R U P A 1 H3AB H 0.0900 0.8343 -0.0601 0.029 Uiso 0.5 1 calc R U P A 1 H3BC H 0.2074 0.9465 -0.0513 0.029 Uiso 0.5 1 calc R U P B 2 H3BD H 0.1335 0.8281 -0.0452 0.029 Uiso 0.5 1 calc R U P B 2 C5 C 0.1977(3) 1.1993(3) 0.3552(2) 0.0189(6) Uani 1 1 d . . . . . H5A H 0.1047 1.1868 0.3454 0.023 Uiso 1 1 calc R U . . . H5B H 0.2281 1.1702 0.4309 0.023 Uiso 1 1 calc R U . . . C6 C 0.2217(4) 1.3287(3) 0.3539(3) 0.0306(8) Uani 1 1 d . . . . . H6A H 0.3133 1.3434 0.3654 0.046 Uiso 1 1 calc R U . . . H6B H 0.1789 1.3652 0.4143 0.046 Uiso 1 1 calc R U . . . H6C H 0.1882 1.3603 0.2810 0.046 Uiso 1 1 calc R U . . . C7 C 0.4346(3) 1.1667(3) 0.2561(3) 0.0198(6) Uani 1 1 d . . . . . H7A H 0.4535 1.2059 0.3294 0.024 Uiso 1 1 calc R U . . . H7B H 0.4928 1.1003 0.2548 0.024 Uiso 1 1 calc R U . . . C8 C 0.4655(4) 1.2487(4) 0.1637(3) 0.0431(11) Uani 1 1 d . . . . . H8A H 0.4551 1.2094 0.0908 0.065 Uiso 1 1 calc R U . . . H8B H 0.5536 1.2751 0.1781 0.065 Uiso 1 1 calc R U . . . H8C H 0.4079 1.3147 0.1626 0.065 Uiso 1 1 calc R U . . . C9 C 0.0609(3) 1.1063(2) 0.0968(2) 0.0145(6) Uani 1 1 d . . . . . H9A H 0.0185 1.1308 0.0233 0.017 Uiso 1 1 calc R U . . . H9B H 0.0071 1.1302 0.1567 0.017 Uiso 1 1 calc R U . . . C10 C 0.1911(3) 1.1630(3) 0.1158(2) 0.0151(6) Uani 1 1 d . . . . . H10A H 0.1813 1.2474 0.1180 0.018 Uiso 1 1 calc R U . . . H10B H 0.2431 1.1436 0.0531 0.018 Uiso 1 1 calc R U . . . C11 C 0.0709(3) 0.6279(2) 0.4078(2) 0.0135(6) Uani 1 1 d . . . . . H11A H 0.0964 0.5753 0.3486 0.016 Uiso 1 1 calc R U . . . H11B H 0.0657 0.5821 0.4772 0.016 Uiso 1 1 calc R U . . . C12 C -0.0617(3) 0.6740(3) 0.3710(2) 0.0182(6) Uani 1 1 d . . . . . H12A H -0.0855 0.7317 0.4251 0.027 Uiso 1 1 calc R U . . . H12B H -0.1232 0.6109 0.3680 0.027 Uiso 1 1 calc R U . . . H12C H -0.0616 0.7090 0.2961 0.027 Uiso 1 1 calc R U . . . C13 C 0.1628(3) 0.7965(3) 0.5723(2) 0.0165(6) Uani 1 1 d . . . . . H13A H 0.2176 0.8645 0.5877 0.020 Uiso 1 1 calc R U . . . H13B H 0.0734 0.8230 0.5665 0.020 Uiso 1 1 calc R U . . . C14 C 0.1831(3) 0.7141(3) 0.6725(2) 0.0190(6) Uani 1 1 d . . . . . H14A H 0.1301 0.6459 0.6580 0.029 Uiso 1 1 calc R U . . . H14B H 0.1595 0.7524 0.7409 0.029 Uiso 1 1 calc R U . . . H14C H 0.2728 0.6915 0.6827 0.029 Uiso 1 1 calc R U . . . C15 C 0.5894(3) 0.7678(3) 0.3653(2) 0.0162(6) Uani 1 1 d . . . . . H15A H 0.5720 0.7926 0.4420 0.019 Uiso 1 1 calc R U . . . H15B H 0.6439 0.6988 0.3733 0.019 Uiso 1 1 calc R U . . . C16 C 0.6629(3) 0.8631(3) 0.3110(3) 0.0230(7) Uani 1 1 d . . . . . H16A H 0.6829 0.8388 0.2358 0.035 Uiso 1 1 calc R U . . . H16B H 0.7420 0.8788 0.3579 0.035 Uiso 1 1 calc R U . . . H16C H 0.6109 0.9328 0.3047 0.035 Uiso 1 1 calc R U . . . C17 C 0.4861(3) 0.6653(3) 0.1560(2) 0.0186(6) Uani 1 1 d . . . . . H17A H 0.4092 0.6347 0.1125 0.022 Uiso 1 1 calc R U . . . H17B H 0.5206 0.7270 0.1104 0.022 Uiso 1 1 calc R U . . . C18 C 0.5840(4) 0.5700(4) 0.1705(3) 0.0390(10) Uani 1 1 d . . . . . H18A H 0.6648 0.6014 0.2040 0.059 Uiso 1 1 calc R U . . . H18B H 0.5965 0.5365 0.0968 0.059 Uiso 1 1 calc R U . . . H18C H 0.5541 0.5107 0.2201 0.059 Uiso 1 1 calc R U . . . C19 C 0.3338(3) 0.6419(3) 0.4726(2) 0.0142(6) Uani 1 1 d . . . . . H19A H 0.3983 0.6838 0.5220 0.017 Uiso 1 1 calc R U . . . H19B H 0.3062 0.5742 0.5143 0.017 Uiso 1 1 calc R U . . . C20 C 0.3919(3) 0.6028(3) 0.3659(2) 0.0143(6) Uani 1 1 d . . . . . H20A H 0.3293 0.5565 0.3186 0.017 Uiso 1 1 calc R U . . . H20B H 0.4675 0.5544 0.3864 0.017 Uiso 1 1 calc R U . . . C4 C 0.0815(9) 0.9866(8) -0.1395(8) 0.026(2) Uani 0.5 1 d . . P C 1 H4A H -0.0103 1.0001 -0.1410 0.039 Uiso 0.5 1 calc R U P C 1 H4B H 0.1006 0.9490 -0.2096 0.039 Uiso 0.5 1 calc R U P C 1 H4C H 0.1266 1.0600 -0.1321 0.039 Uiso 0.5 1 calc R U P C 1 C4A C 0.0367(8) 0.9464(8) -0.1425(8) 0.0192(18) Uani 0.5 1 d . . P C 2 H4AA H -0.0440 0.9050 -0.1418 0.029 Uiso 0.5 1 calc R U P C 2 H4AB H 0.0765 0.9274 -0.2116 0.029 Uiso 0.5 1 calc R U P C 2 H4AC H 0.0208 1.0291 -0.1401 0.029 Uiso 0.5 1 calc R U P C 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.00903(10) 0.00736(11) 0.00707(10) 0.00029(10) 0.00008(7) 0.00027(11) Cl1 0.0153(3) 0.0127(3) 0.0146(3) 0.0004(3) 0.0046(2) 0.0038(3) Cl2 0.0152(3) 0.0130(3) 0.0111(3) -0.0013(2) -0.0026(2) -0.0016(3) Cl3 0.0164(3) 0.0172(3) 0.0144(3) 0.0045(3) 0.0061(2) 0.0005(3) Cl4 0.0147(3) 0.0092(3) 0.0111(3) -0.0008(2) -0.0011(2) -0.0007(3) P1 0.0127(3) 0.0102(4) 0.0095(3) 0.0005(3) -0.0012(3) 0.0008(3) P2 0.0150(4) 0.0098(4) 0.0118(3) 0.0010(3) -0.0017(3) -0.0018(3) P3 0.0115(3) 0.0106(4) 0.0087(3) 0.0013(3) 0.0012(2) -0.0002(3) P4 0.0107(3) 0.0125(4) 0.0102(3) 0.0000(3) 0.0010(2) 0.0020(3) C1 0.0166(13) 0.0218(17) 0.0212(14) 0.0054(14) -0.0061(11) -0.0067(15) C2 0.0126(15) 0.0268(19) 0.052(2) 0.0165(17) 0.0039(14) 0.0034(15) C3 0.0342(18) 0.027(2) 0.0109(13) 0.0004(12) -0.0002(12) 0.0125(15) C5 0.0272(16) 0.0138(16) 0.0151(14) -0.0008(12) -0.0016(12) 0.0000(13) C6 0.049(2) 0.0140(17) 0.0289(18) -0.0017(14) 0.0028(15) -0.0001(16) C7 0.0177(15) 0.0173(16) 0.0233(15) 0.0047(13) -0.0036(12) -0.0068(14) C8 0.028(2) 0.057(3) 0.042(2) 0.027(2) -0.0091(16) -0.021(2) C9 0.0170(14) 0.0121(15) 0.0137(13) 0.0007(11) -0.0017(11) 0.0018(13) C10 0.0199(15) 0.0119(14) 0.0128(13) 0.0035(11) -0.0017(11) -0.0011(13) C11 0.0159(14) 0.0118(14) 0.0129(13) 0.0018(11) 0.0012(11) -0.0016(12) C12 0.0137(14) 0.0192(16) 0.0221(14) 0.0002(13) 0.0029(11) -0.0026(13) C13 0.0223(15) 0.0177(15) 0.0101(13) 0.0002(11) 0.0044(11) -0.0011(14) C14 0.0227(16) 0.0238(17) 0.0107(12) 0.0021(12) 0.0024(11) -0.0020(14) C15 0.0123(14) 0.0200(16) 0.0158(14) -0.0009(12) -0.0024(11) 0.0031(12) C16 0.0145(13) 0.028(2) 0.0267(16) 0.0011(14) 0.0016(11) -0.0033(14) C17 0.0194(15) 0.0223(17) 0.0147(14) -0.0026(13) 0.0044(11) 0.0048(14) C18 0.049(2) 0.041(2) 0.0273(18) -0.0083(17) 0.0069(16) 0.027(2) C19 0.0141(14) 0.0149(15) 0.0136(13) 0.0057(11) 0.0000(11) 0.0009(12) C20 0.0127(14) 0.0114(15) 0.0185(14) 0.0025(12) -0.0006(11) 0.0030(12) C4 0.036(6) 0.029(6) 0.014(3) 0.008(4) 0.010(4) 0.010(4) C4A 0.018(4) 0.025(5) 0.015(3) 0.003(4) 0.002(3) 0.004(3) 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' 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 Cl2 Nb1 Cl1 87.85(2) . . ? Cl2 Nb1 Cl4 146.19(2) . . ? Cl1 Nb1 Cl4 102.83(2) . . ? Cl2 Nb1 Cl3 100.59(2) . . ? Cl1 Nb1 Cl3 143.79(2) . . ? Cl4 Nb1 Cl3 89.57(2) . . ? Cl2 Nb1 P2 71.49(2) . . ? Cl1 Nb1 P2 78.62(2) . . ? Cl4 Nb1 P2 141.75(2) . . ? Cl3 Nb1 P2 71.12(2) . . ? Cl2 Nb1 P1 143.01(2) . . ? Cl1 Nb1 P1 74.07(2) . . ? Cl4 Nb1 P1 70.48(2) . . ? Cl3 Nb1 P1 78.53(2) . . ? P2 Nb1 P1 73.41(2) . . ? Cl2 Nb1 P4 78.80(2) . . ? Cl1 Nb1 P4 143.95(2) . . ? Cl4 Nb1 P4 73.81(2) . . ? Cl3 Nb1 P4 72.08(2) . . ? P2 Nb1 P4 126.55(2) . . ? P1 Nb1 P4 133.32(2) . . ? Cl2 Nb1 P3 76.00(2) . . ? Cl1 Nb1 P3 71.36(2) . . ? Cl4 Nb1 P3 77.29(2) . . ? Cl3 Nb1 P3 144.84(2) . . ? P2 Nb1 P3 136.08(2) . . ? P1 Nb1 P3 125.13(2) . . ? P4 Nb1 P3 72.95(2) . . ? C1 P1 C3 104.38(15) . . ? C1 P1 C9 104.62(15) . . ? C3 P1 C9 104.95(14) . . ? C1 P1 Nb1 115.88(9) . . ? C3 P1 Nb1 115.13(10) . . ? C9 P1 Nb1 110.78(9) . . ? C5 P2 C10 103.05(14) . . ? C5 P2 C7 103.23(15) . . ? C10 P2 C7 106.00(13) . . ? C5 P2 Nb1 116.48(10) . . ? C10 P2 Nb1 110.90(10) . . ? C7 P2 Nb1 115.88(11) . . ? C19 P3 C11 100.29(13) . . ? C19 P3 C13 103.08(13) . . ? C11 P3 C13 103.15(13) . . ? C19 P3 Nb1 110.92(9) . . ? C11 P3 Nb1 119.33(9) . . ? C13 P3 Nb1 117.60(10) . . ? C20 P4 C17 102.68(14) . . ? C20 P4 C15 101.37(13) . . ? C17 P4 C15 103.88(14) . . ? C20 P4 Nb1 110.25(9) . . ? C17 P4 Nb1 117.60(10) . . ? C15 P4 Nb1 118.77(10) . . ? C2 C1 P1 117.6(2) . . ? C2 C1 H1A 107.9 . . ? P1 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? P1 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? 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 119.7(4) . . ? C4A C3 P1 119.0(4) . . ? C4 C3 H3AA 107.4 . . ? P1 C3 H3AA 107.4 . . ? C4 C3 H3AB 107.4 . . ? P1 C3 H3AB 107.4 . . ? H3AA C3 H3AB 106.9 . . ? C4A C3 H3BC 107.6 . . ? P1 C3 H3BC 107.6 . . ? C4A C3 H3BD 107.6 . . ? P1 C3 H3BD 107.6 . . ? H3BC C3 H3BD 107.0 . . ? C6 C5 P2 117.5(2) . . ? C6 C5 H5A 107.9 . . ? P2 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? P2 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? 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 117.0(2) . . ? C8 C7 H7A 108.1 . . ? P2 C7 H7A 108.1 . . ? C8 C7 H7B 108.1 . . ? P2 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? 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 109.67(19) . . ? C10 C9 H9A 109.7 . . ? P1 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? P1 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 P2 108.90(19) . . ? 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 116.2(2) . . ? C12 C11 H11A 108.2 . . ? P3 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? P3 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? 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 115.0(2) . . ? C14 C13 H13A 108.5 . . ? P3 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? P3 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? 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 . . ? C16 C15 P4 114.7(2) . . ? C16 C15 H15A 108.6 . . ? P4 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? P4 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P4 115.7(2) . . ? C18 C17 H17A 108.3 . . ? P4 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? P4 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 P3 110.03(19) . . ? C20 C19 H19A 109.7 . . ? P3 C19 H19A 109.7 . . ? C20 C19 H19B 109.7 . . ? P3 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C19 C20 P4 109.4(2) . . ? C19 C20 H20A 109.8 . . ? P4 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? P4 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? 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 . . ? C3 C4A H4AA 109.5 . . ? C3 C4A H4AB 109.5 . . ? H4AA C4A H4AB 109.5 . . ? C3 C4A H4AC 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 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 Cl2 2.5228(7) . ? Nb1 Cl1 2.5235(7) . ? Nb1 Cl4 2.5240(7) . ? Nb1 Cl3 2.5273(7) . ? Nb1 P2 2.6785(8) . ? Nb1 P1 2.6818(7) . ? Nb1 P4 2.7111(7) . ? Nb1 P3 2.7157(7) . ? P1 C1 1.833(3) . ? P1 C3 1.836(3) . ? P1 C9 1.839(3) . ? P2 C5 1.834(3) . ? P2 C10 1.840(3) . ? P2 C7 1.843(3) . ? P3 C19 1.835(3) . ? P3 C11 1.837(3) . ? P3 C13 1.842(3) . ? P4 C20 1.832(3) . ? P4 C17 1.834(3) . ? P4 C15 1.836(3) . ? C1 C2 1.516(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.479(9) . ? C3 C4A 1.489(9) . ? C3 H3AA 0.9900 . ? C3 H3AB 0.9900 . ? C3 H3BC 0.9900 . ? C3 H3BD 0.9900 . ? C5 C6 1.530(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.514(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.525(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.528(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.532(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.531(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.518(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.528(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ?