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#$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1144 $
#$URL: svn://crystallography.net/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 ω-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/[σ²(Fo²)+(0.0153P)²] where P=(Fo²+2Fc²)/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 > 2σ(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
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_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 . ?
