#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1144 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700019.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_7700019 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 H32 Cl4 Nb P4' _chemical_formula_sum 'C20 H32 Cl4 Nb P4' _chemical_formula_weight 631.04 _chemical_name_common '[NbCl4(o-DMPB)2]' _space_group_crystal_system tetragonal _space_group_IT_number 121 _space_group_name_Hall 'I -4 2' _space_group_name_H-M_alt 'I -4 2 m' _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 2 _cell_length_a 8.9876(7) _cell_length_b 8.9876(7) _cell_length_c 16.1482(11) _cell_measurement_reflns_used 2286 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 4.1 _cell_volume 1304.40(17) _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 0.992 _diffrn_measured_fraction_theta_max 0.993 _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 0.0346 _diffrn_reflns_av_unetI/netI 0.0430 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 2204 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.941 _diffrn_reflns_theta_min 4.081 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.703 _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 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 642 _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.380 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.118 _refine_ls_abs_structure_details ; Flack x determined using 263 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.03(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 43 _refine_ls_number_reflns 754 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.114 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0477 _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^)+(0.0158P)^2^+13.9926P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1111 _refine_ls_wR_factor_ref 0.1149 _reflns_Friedel_coverage 0.672 _reflns_Friedel_fraction_full 0.955 _reflns_Friedel_fraction_max 0.929 _reflns_number_gt 703 _reflns_number_total 754 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6dt01099g2.cif _cod_data_source_block shelx _cod_original_cell_volume 1304.4(2) _cod_database_code 7700019 _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 0.915 _shelx_estimated_absorpt_t_max 0.978 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelx in I-42m CELL 0.71073 8.9876 8.9876 16.1482 90.000 90.000 90.000 ZERR 2.00 0.0007 0.0007 0.0011 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SYMM -X, Y, -Z SYMM X, -Y, -Z SYMM -Y, -X, Z SYMM Y, X, Z SFAC C H P Cl Nb UNIT 40 64 8 8 2 OMIT -4.00 54.00 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 SIZE 0.08 0.04 0.02 TEMP -173 WGHT 0.015800 13.992596 FVAR 0.59736 MOLE 1 NB1 5 0.000000 1.000000 1.000000 10.12500 0.03974 0.03974 = 0.01878 0.00000 0.00000 0.00000 CL1 4 -0.183638 0.816362 0.955766 10.50000 0.03888 0.03888 = 0.03567 -0.00313 -0.00313 -0.00137 P1 3 0.124833 0.875167 0.864494 10.50000 0.01573 0.01573 = 0.01694 -0.00119 0.00119 0.00207 C1 1 0.100690 0.674987 0.854516 11.00000 0.04802 0.02038 = 0.02397 -0.00140 0.00450 0.00513 AFIX 137 H1A 2 -0.005321 0.652012 0.848335 11.00000 -1.50000 H1B 2 0.139445 0.625575 0.904129 11.00000 -1.50000 H1C 2 0.154942 0.639542 0.805709 11.00000 -1.50000 AFIX 0 C2 1 0.054603 0.945397 0.765520 10.50000 0.01818 0.01818 = 0.01289 -0.00331 0.00331 -0.00791 C3 1 0.109821 0.890179 0.689536 10.50000 0.02243 0.02243 = 0.01785 -0.00525 0.00525 -0.00388 AFIX 43 H3 2 0.184558 0.815442 0.688895 10.50000 -1.20000 AFIX 0 C4 1 0.053562 0.946438 0.615887 10.50000 0.03131 0.03131 = 0.01058 -0.00435 0.00435 -0.01783 AFIX 43 H4 2 0.090356 0.909644 0.564679 10.50000 -1.20000 AFIX 0 HKLF 4 REM shelx in I-42m REM R1 = 0.0477 for 703 Fo > 4sig(Fo) and 0.0523 for all 754 data REM 43 parameters refined using 0 restraints END WGHT 0.0180 14.0397 REM Highest difference peak 1.380, deepest hole -0.876, 1-sigma level 0.118 Q1 1 -0.0443 1.0443 1.0226 10.50000 0.05 1.38 Q2 1 -0.1222 0.8778 0.9758 10.50000 0.05 0.90 Q3 1 0.1252 1.0580 1.0305 11.00000 0.05 0.47 Q4 1 0.0000 1.0000 0.8505 10.25000 0.05 0.46 Q5 1 0.1728 0.8272 0.8449 10.50000 0.05 0.42 ; _shelx_res_checksum 38427 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x, y, -z' 'x, -y, -z' '-y, -x, z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+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 0.0000 1.0000 1.0000 0.0327(6) Uani 1 8 d S T P . . Cl1 Cl -0.1836(2) 0.8164(2) 0.95577(16) 0.0378(7) Uani 1 2 d S T P . . P1 P 0.12483(19) 0.87517(19) 0.86449(13) 0.0161(5) Uani 1 2 d S T P . . C1 C 0.1007(9) 0.6750(8) 0.8545(4) 0.0308(17) Uani 1 1 d . . . . . H1A H -0.0053 0.6520 0.8483 0.046 Uiso 1 1 calc R U . . . H1B H 0.1394 0.6256 0.9041 0.046 Uiso 1 1 calc R U . . . H1C H 0.1549 0.6395 0.8057 0.046 Uiso 1 1 calc R U . . . C2 C 0.0546(7) 0.9454(7) 0.7655(5) 0.0164(17) Uani 1 2 d S T P . . C3 C 0.1098(8) 0.8902(8) 0.6895(5) 0.0209(19) Uani 1 2 d S T P . . H3 H 0.1846 0.8154 0.6889 0.025 Uiso 1 2 calc R U P . . C4 C 0.0536(9) 0.9464(9) 0.6159(5) 0.024(2) Uani 1 2 d S T P . . H4 H 0.0904 0.9096 0.5647 0.029 Uiso 1 2 calc R U 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 Nb1 0.0397(8) 0.0397(8) 0.0188(9) 0.000 0.000 0.000 Cl1 0.0389(10) 0.0389(10) 0.0357(14) -0.0031(9) -0.0031(9) -0.0014(14) P1 0.0157(7) 0.0157(7) 0.0169(11) -0.0012(6) 0.0012(6) 0.0021(10) C1 0.048(5) 0.020(3) 0.024(3) -0.001(3) 0.005(3) 0.005(3) C2 0.018(3) 0.018(3) 0.013(4) -0.003(3) 0.003(3) -0.008(4) C3 0.022(3) 0.022(3) 0.018(4) -0.005(3) 0.005(3) -0.004(4) C4 0.031(3) 0.031(3) 0.011(4) -0.004(3) 0.004(3) -0.018(4) 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 Cl1 Nb1 Cl1 145.97(13) . 2_575 ? Cl1 Nb1 Cl1 94.91(4) . 4_667 ? Cl1 Nb1 Cl1 94.91(4) 2_575 4_667 ? Cl1 Nb1 Cl1 94.91(4) . 3_467 ? Cl1 Nb1 Cl1 94.91(4) 2_575 3_467 ? Cl1 Nb1 Cl1 145.97(13) 4_667 3_467 ? Cl1 Nb1 P1 142.96(8) . 4_667 ? Cl1 Nb1 P1 71.07(8) 2_575 4_667 ? Cl1 Nb1 P1 76.30(5) 4_667 4_667 ? Cl1 Nb1 P1 76.30(5) 3_467 4_667 ? Cl1 Nb1 P1 76.30(5) . 2_575 ? Cl1 Nb1 P1 76.30(5) 2_575 2_575 ? Cl1 Nb1 P1 142.96(8) 4_667 2_575 ? Cl1 Nb1 P1 71.07(8) 3_467 2_575 ? P1 Nb1 P1 130.95(6) 4_667 2_575 ? Cl1 Nb1 P1 71.07(8) . 3_467 ? Cl1 Nb1 P1 142.96(8) 2_575 3_467 ? Cl1 Nb1 P1 76.30(5) 4_667 3_467 ? Cl1 Nb1 P1 76.30(5) 3_467 3_467 ? P1 Nb1 P1 71.89(10) 4_667 3_467 ? P1 Nb1 P1 130.95(6) 2_575 3_467 ? Cl1 Nb1 P1 76.30(5) . . ? Cl1 Nb1 P1 76.30(5) 2_575 . ? Cl1 Nb1 P1 71.07(8) 4_667 . ? Cl1 Nb1 P1 142.96(8) 3_467 . ? P1 Nb1 P1 130.95(6) 4_667 . ? P1 Nb1 P1 71.89(10) 2_575 . ? P1 Nb1 P1 130.95(6) 3_467 . ? C1 P1 C1 103.2(5) 7_665 . ? C1 P1 C2 102.9(3) 7_665 . ? C1 P1 C2 102.9(3) . . ? C1 P1 Nb1 115.6(2) 7_665 . ? C1 P1 Nb1 115.6(2) . . ? C2 P1 Nb1 114.9(3) . . ? 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 . . ? C2 C2 C3 119.8(6) 2_575 . ? C2 C2 P1 119.2(3) 2_575 . ? C3 C2 P1 121.0(7) . . ? C4 C3 C2 119.2(9) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C4 C4 C3 121.0(6) 2_575 . ? C4 C4 H4 119.5 2_575 . ? C3 C4 H4 119.5 . . ? 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 Cl1 2.441(3) . ? Nb1 Cl1 2.441(3) 2_575 ? Nb1 Cl1 2.441(3) 4_667 ? Nb1 Cl1 2.441(3) 3_467 ? Nb1 P1 2.703(2) 4_667 ? Nb1 P1 2.703(2) 2_575 ? Nb1 P1 2.703(2) 3_467 ? Nb1 P1 2.703(2) . ? P1 C1 1.819(8) 7_665 ? P1 C1 1.819(8) . ? P1 C2 1.831(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C2 1.388(19) 2_575 ? C2 C3 1.414(12) . ? C3 C4 1.388(13) . ? C3 H3 0.9500 . ? C4 C4 1.36(2) 2_575 ? C4 H4 0.9500 . ?