#------------------------------------------------------------------------------ #$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $ #$Revision: 1144 $ #$URL: svn://localhost/testcod/cif/7/70/00/7700020.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_7700020 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 Cl4 Nb P4' _chemical_formula_sum 'C12 H32 Cl4 Nb P4' _chemical_formula_weight 534.96 _chemical_name_common '[NbCl4(DMPE)2]' _space_group_crystal_system orthorhombic _space_group_IT_number 18 _space_group_name_Hall 'P 2 2ab' _space_group_name_H-M_alt 'P 21 21 2' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _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 10.7216(9) _cell_length_b 11.2891(10) _cell_length_c 9.4711(9) _cell_measurement_reflns_used 10275 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.4 _cell_volume 1146.36(18) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 (Left)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_collimation 'Confocal mirrors, HF Varimax ' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_Laue_measured_fraction_full 0.996 _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 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9661 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.982 _diffrn_reflns_theta_min 3.390 _diffrn_source 'Rotating Anode' _diffrn_source_current 55.0 _diffrn_source_power 2.475 _diffrn_source_voltage 45.0 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.773 _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 1.550 _exptl_crystal_description Chip _exptl_crystal_F_000 546 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.263 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.057 _refine_ls_abs_structure_details ; Flack x determined using 894 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 2248 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0209 _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^)+(0.0152P)^2^+0.4233P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.0457 _reflns_Friedel_coverage 0.715 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.001 _reflns_number_gt 2167 _reflns_number_total 2248 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6dt01099g2.cif _cod_data_source_block 140515ypc1 _cod_database_code 7700020 _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. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL 140515ypc1 in P2(1)2(1)2 CELL 0.71073 10.7216 11.2891 9.4711 90.000 90.000 90.000 ZERR 2.00 0.0009 0.0010 0.0009 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 0.5-X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H P Cl Nb UNIT 24 64 8 8 2 OMIT -4.00 52.00 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 TEMP -173 WGHT 0.015200 0.423300 FVAR 0.23328 MOLE 1 NB1 5 0.000000 1.000000 0.258112 10.50000 0.01094 0.01109 = 0.00862 0.00000 0.00000 -0.00023 CL1 4 0.151584 1.103734 0.096259 11.00000 0.01585 0.01837 = 0.01711 0.00562 0.00270 -0.00181 CL2 4 0.030758 1.174501 0.420250 11.00000 0.01922 0.01703 = 0.01804 -0.00619 -0.00338 -0.00017 P1 3 0.121428 0.831779 0.118467 11.00000 0.01596 0.01472 = 0.01218 -0.00086 0.00028 0.00217 P2 3 0.216068 0.971054 0.391327 11.00000 0.01561 0.01756 = 0.01201 0.00040 -0.00246 0.00013 C1 1 0.335426 1.085025 0.366935 11.00000 0.01978 0.02628 = 0.02235 -0.00097 -0.00389 -0.00006 AFIX 137 H1A 2 0.402740 1.072897 0.435424 11.00000 -1.50000 H1B 2 0.298284 1.163420 0.381329 11.00000 -1.50000 H1C 2 0.369194 1.079814 0.270983 11.00000 -1.50000 AFIX 0 C2 1 0.210439 0.957402 0.582425 11.00000 0.02778 0.02960 = 0.01469 0.00165 -0.00639 0.00297 AFIX 137 H2A 2 0.149277 0.896741 0.608594 11.00000 -1.50000 H2B 2 0.186116 1.033516 0.623867 11.00000 -1.50000 H2C 2 0.292890 0.934586 0.617856 11.00000 -1.50000 AFIX 0 C3 1 0.295115 0.836182 0.332028 11.00000 0.01692 0.02080 = 0.01969 0.00198 -0.00387 0.00270 AFIX 23 H3A 2 0.383818 0.838552 0.360927 11.00000 -1.20000 H3B 2 0.255871 0.766103 0.376470 11.00000 -1.20000 AFIX 0 C4 1 0.286175 0.826167 0.171399 11.00000 0.01564 0.02120 = 0.02009 0.00020 -0.00052 0.00407 AFIX 23 H4A 2 0.323836 0.750622 0.139772 11.00000 -1.20000 H4B 2 0.332475 0.892090 0.126624 11.00000 -1.20000 AFIX 0 C5 1 0.070963 0.678706 0.141606 11.00000 0.02558 0.01967 = 0.02612 -0.00358 0.00211 0.00221 AFIX 137 H5A 2 -0.018873 0.672980 0.123778 11.00000 -1.50000 H5B 2 0.088774 0.653167 0.238423 11.00000 -1.50000 H5C 2 0.115872 0.627726 0.075051 11.00000 -1.50000 AFIX 0 C6 1 0.126101 0.846952 -0.072718 11.00000 0.02679 0.02555 = 0.01304 -0.00388 0.00070 0.00397 AFIX 137 H6A 2 0.178708 0.784422 -0.112779 11.00000 -1.50000 H6B 2 0.160685 0.924562 -0.097542 11.00000 -1.50000 H6C 2 0.041426 0.840045 -0.110807 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P2(1)2(1)2 REM R1 = 0.0209 for 2167 Fo > 4sig(Fo) and 0.0223 for all 2248 data REM 100 parameters refined using 0 restraints END WGHT 0.0151 0.4230 REM Highest difference peak 0.263, deepest hole -0.320, 1-sigma level 0.057 Q1 1 0.0446 0.9960 0.3651 11.00000 0.05 0.26 Q2 1 -0.0042 0.9415 0.3778 11.00000 0.05 0.25 Q3 1 0.1079 1.0380 0.2554 11.00000 0.05 0.25 Q4 1 0.2111 0.8237 0.1356 11.00000 0.05 0.23 Q5 1 0.2726 1.0298 0.3819 11.00000 0.05 0.23 ; _shelx_res_checksum 57221 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -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 0.0000 1.0000 0.25811(4) 0.01021(10) Uani 1 2 d S T P . . Cl1 Cl 0.15158(7) 1.10373(7) 0.09626(9) 0.01711(18) Uani 1 1 d . . . . . Cl2 Cl 0.03076(7) 1.17450(7) 0.42025(8) 0.01809(19) Uani 1 1 d . . . . . P1 P 0.12143(8) 0.83178(7) 0.11847(9) 0.01428(18) Uani 1 1 d . . . . . P2 P 0.21607(7) 0.97105(7) 0.39133(9) 0.01506(19) Uani 1 1 d . . . . . C1 C 0.3354(3) 1.0850(3) 0.3669(4) 0.0228(8) Uani 1 1 d . . . . . H1A H 0.4027 1.0729 0.4354 0.034 Uiso 1 1 calc R U . . . H1B H 0.2983 1.1634 0.3813 0.034 Uiso 1 1 calc R U . . . H1C H 0.3692 1.0798 0.2710 0.034 Uiso 1 1 calc R U . . . C2 C 0.2104(3) 0.9574(3) 0.5824(3) 0.0240(8) Uani 1 1 d . . . . . H2A H 0.1493 0.8967 0.6086 0.036 Uiso 1 1 calc R U . . . H2B H 0.1861 1.0335 0.6239 0.036 Uiso 1 1 calc R U . . . H2C H 0.2929 0.9346 0.6179 0.036 Uiso 1 1 calc R U . . . C3 C 0.2951(3) 0.8362(3) 0.3320(3) 0.0191(8) Uani 1 1 d . . . . . H3A H 0.3838 0.8386 0.3609 0.023 Uiso 1 1 calc R U . . . H3B H 0.2559 0.7661 0.3765 0.023 Uiso 1 1 calc R U . . . C4 C 0.2862(3) 0.8262(3) 0.1714(3) 0.0190(7) Uani 1 1 d . . . . . H4A H 0.3238 0.7506 0.1398 0.023 Uiso 1 1 calc R U . . . H4B H 0.3325 0.8921 0.1266 0.023 Uiso 1 1 calc R U . . . C5 C 0.0710(3) 0.6787(3) 0.1416(4) 0.0238(8) Uani 1 1 d . . . . . H5A H -0.0189 0.6730 0.1238 0.036 Uiso 1 1 calc R U . . . H5B H 0.0888 0.6532 0.2384 0.036 Uiso 1 1 calc R U . . . H5C H 0.1159 0.6277 0.0751 0.036 Uiso 1 1 calc R U . . . C6 C 0.1261(3) 0.8470(3) -0.0727(3) 0.0218(8) Uani 1 1 d . . . . . H6A H 0.1787 0.7844 -0.1128 0.033 Uiso 1 1 calc R U . . . H6B H 0.1607 0.9246 -0.0975 0.033 Uiso 1 1 calc R U . . . H6C H 0.0414 0.8400 -0.1108 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 0.01094(18) 0.01109(18) 0.00862(17) 0.000 0.000 -0.00023(16) Cl1 0.0158(4) 0.0184(4) 0.0171(4) 0.0056(3) 0.0027(3) -0.0018(3) Cl2 0.0192(4) 0.0170(4) 0.0180(4) -0.0062(3) -0.0034(3) -0.0002(3) P1 0.0160(4) 0.0147(4) 0.0122(4) -0.0009(4) 0.0003(3) 0.0022(4) P2 0.0156(4) 0.0176(5) 0.0120(4) 0.0004(3) -0.0025(3) 0.0001(3) C1 0.0198(17) 0.026(2) 0.0223(18) -0.0010(16) -0.0039(15) -0.0001(16) C2 0.0278(19) 0.030(2) 0.0147(16) 0.0016(15) -0.0064(15) 0.0030(16) C3 0.0169(17) 0.0208(19) 0.0197(18) 0.0020(15) -0.0039(14) 0.0027(16) C4 0.0156(17) 0.0212(19) 0.0201(17) 0.0002(15) -0.0005(14) 0.0041(16) C5 0.0256(19) 0.0197(19) 0.0261(19) -0.0036(15) 0.0021(15) 0.0022(16) C6 0.0268(19) 0.0255(19) 0.0130(16) -0.0039(15) 0.0007(15) 0.0040(16) 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 Cl2 104.89(4) 2_575 . ? Cl2 Nb1 Cl1 85.59(3) 2_575 2_575 ? Cl2 Nb1 Cl1 144.86(2) . 2_575 ? Cl2 Nb1 Cl1 144.86(2) 2_575 . ? Cl2 Nb1 Cl1 85.59(3) . . ? Cl1 Nb1 Cl1 105.15(4) 2_575 . ? Cl2 Nb1 P1 143.00(2) 2_575 2_575 ? Cl2 Nb1 P1 78.96(3) . 2_575 ? Cl1 Nb1 P1 73.35(3) 2_575 2_575 ? Cl1 Nb1 P1 71.41(3) . 2_575 ? Cl2 Nb1 P1 78.96(3) 2_575 . ? Cl2 Nb1 P1 143.00(2) . . ? Cl1 Nb1 P1 71.41(3) 2_575 . ? Cl1 Nb1 P1 73.35(3) . . ? P1 Nb1 P1 120.25(4) 2_575 . ? Cl2 Nb1 P2 72.10(2) 2_575 2_575 ? Cl2 Nb1 P2 74.25(2) . 2_575 ? Cl1 Nb1 P2 77.53(3) 2_575 2_575 ? Cl1 Nb1 P2 142.46(2) . 2_575 ? P1 Nb1 P2 73.81(3) 2_575 2_575 ? P1 Nb1 P2 138.74(3) . 2_575 ? Cl2 Nb1 P2 74.26(2) 2_575 . ? Cl2 Nb1 P2 72.11(2) . . ? Cl1 Nb1 P2 142.46(2) 2_575 . ? Cl1 Nb1 P2 77.53(3) . . ? P1 Nb1 P2 138.74(3) 2_575 . ? P1 Nb1 P2 73.81(3) . . ? P2 Nb1 P2 123.32(4) 2_575 . ? C6 P1 C5 102.53(16) . . ? C6 P1 C4 104.38(16) . . ? C5 P1 C4 102.69(17) . . ? C6 P1 Nb1 116.22(12) . . ? C5 P1 Nb1 118.18(11) . . ? C4 P1 Nb1 111.11(12) . . ? C2 P2 C1 102.04(16) . . ? C2 P2 C3 104.50(16) . . ? C1 P2 C3 102.85(17) . . ? C2 P2 Nb1 117.01(12) . . ? C1 P2 Nb1 117.60(12) . . ? C3 P2 Nb1 111.10(11) . . ? P2 C1 H1A 109.5 . . ? P2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P2 C2 H2A 109.5 . . ? P2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P2 109.7(3) . . ? C4 C3 H3A 109.7 . . ? P2 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? P2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 P1 109.2(2) . . ? C3 C4 H4A 109.8 . . ? P1 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? P1 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 2.5194(8) 2_575 ? Nb1 Cl2 2.5195(8) . ? Nb1 Cl1 2.5224(8) 2_575 ? Nb1 Cl1 2.5224(8) . ? Nb1 P1 2.6553(8) 2_575 ? Nb1 P1 2.6553(8) . ? Nb1 P2 2.6580(8) 2_575 ? Nb1 P2 2.6581(8) . ? P1 C6 1.820(3) . ? P1 C5 1.824(4) . ? P1 C4 1.837(3) . ? P2 C2 1.817(3) . ? P2 C1 1.829(3) . ? P2 C3 1.831(4) . ? 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 1.529(4) . ? 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 . ?