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#$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1144 $
#$URL: svn://crystallography.net/testcod/cif/7/70/00/7700022.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_7700022
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, C2 H3 Br4 N Nb O'
_chemical_formula_sum            'C14 H35 Br8 N Nb2 O P4'
_chemical_formula_weight         1182.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_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                   12.011(3)
_cell_length_b                   12.011(3)
_cell_length_c                   11.065(4)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     1596.3(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10587
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         3.392
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    10.942
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.688
_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            Red
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0188
_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)+(0.0188P)²+2.7440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1758
_reflns_number_total             1835
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01099g2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1596.3(10)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7700022
_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. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-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 0.7500 0.2500 0.5000 0.00529(9) Uani 1 4 d S T P . .
Br1 Br 0.94288(2) 0.17314(2) 0.43301(2) 0.01028(7) Uani 1 1 d . . . . .
P1 P 0.87604(5) 0.21023(5) 0.69826(5) 0.00785(12) Uani 1 1 d . . . . .
C1 C 1.0150(2) 0.2712(2) 0.7029(2) 0.0147(5) Uani 1 1 d . . . . .
H1A H 1.0380 0.2810 0.7872 0.022 Uiso 1 1 calc R U . . .
H1B H 1.0140 0.3437 0.6623 0.022 Uiso 1 1 calc R U . . .
H1C H 1.0676 0.2217 0.6618 0.022 Uiso 1 1 calc R U . . .
C2 C 0.9017(2) 0.0648(2) 0.7348(2) 0.0142(5) Uani 1 1 d . . . . .
H2A H 0.9285 0.0258 0.6627 0.021 Uiso 1 1 calc R U . . .
H2B H 0.8324 0.0303 0.7628 0.021 Uiso 1 1 calc R U . . .
H2C H 0.9580 0.0601 0.7987 0.021 Uiso 1 1 calc R U . . .
C3 C 0.81181(19) 0.2645(2) 0.8359(2) 0.0124(5) Uani 1 1 d . . . . .
H3A H 0.8482 0.2314 0.9077 0.015 Uiso 1 1 calc R U . . .
H3B H 0.8214 0.3463 0.8396 0.015 Uiso 1 1 calc R U . . .
Nb2 Nb 0.2500 0.2500 0.00311(3) 0.00795(9) Uani 1 4 d S T P . .
Br2 Br 0.06204(2) 0.15483(2) 0.03408(2) 0.01639(8) Uani 1 1 d . . . . .
N1 N 0.2500 0.2500 0.2237(4) 0.0161(8) Uani 1 4 d S T P . .
O1 O 0.2500 0.2500 -0.1504(3) 0.0116(6) Uani 1 4 d S T P . .
C4 C 0.2500 0.2500 0.3270(4) 0.0134(9) Uani 1 4 d S T P . .
C5 C 0.2500 0.2500 0.4585(4) 0.0202(11) Uani 1 4 d S T P . .
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'
N N 0.0061 0.0033 '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'
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
Br1 Nb1 Br1 94.656(4) . 8_656 ?
Br1 Nb1 Br1 94.656(5) . 7_666 ?
Br1 Nb1 Br1 146.895(17) 8_656 7_666 ?
Br1 Nb1 Br1 146.894(17) . 2_655 ?
Br1 Nb1 Br1 94.655(4) 8_656 2_655 ?
Br1 Nb1 Br1 94.655(4) 7_666 2_655 ?
Br1 Nb1 P1 70.76(2) . . ?
Br1 Nb1 P1 74.210(15) 8_656 . ?
Br1 Nb1 P1 79.076(16) 7_666 . ?
Br1 Nb1 P1 142.300(14) 2_655 . ?
Br1 Nb1 P1 74.209(15) . 7_666 ?
Br1 Nb1 P1 142.301(14) 8_656 7_666 ?
Br1 Nb1 P1 70.75(2) 7_666 7_666 ?
Br1 Nb1 P1 79.077(15) 2_655 7_666 ?
P1 Nb1 P1 131.02(2) . 7_666 ?
Br1 Nb1 P1 142.302(14) . 2_655 ?
Br1 Nb1 P1 79.077(16) 8_656 2_655 ?
Br1 Nb1 P1 74.210(15) 7_666 2_655 ?
Br1 Nb1 P1 70.75(2) 2_655 2_655 ?
P1 Nb1 P1 71.78(3) . 2_655 ?
P1 Nb1 P1 131.02(2) 7_666 2_655 ?
Br1 Nb1 P1 79.077(16) . 8_656 ?
Br1 Nb1 P1 70.75(2) 8_656 8_656 ?
Br1 Nb1 P1 142.301(14) 7_666 8_656 ?
Br1 Nb1 P1 74.210(14) 2_655 8_656 ?
P1 Nb1 P1 131.02(2) . 8_656 ?
P1 Nb1 P1 71.78(3) 7_666 8_656 ?
P1 Nb1 P1 131.02(2) 2_655 8_656 ?
C2 P1 C1 102.98(12) . . ?
C2 P1 C3 103.20(11) . . ?
C1 P1 C3 102.68(11) . . ?
C2 P1 Nb1 116.37(8) . . ?
C1 P1 Nb1 117.64(8) . . ?
C3 P1 Nb1 112.10(8) . . ?
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 . . ?
C3 C3 P1 109.26(12) 2_655 . ?
C3 C3 H3A 109.8 2_655 . ?
P1 C3 H3A 109.8 . . ?
C3 C3 H3B 109.8 2_655 . ?
P1 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
O1 Nb2 N1 180.0 . . ?
O1 Nb2 Br2 97.711(11) . . ?
N1 Nb2 Br2 82.289(11) . . ?
O1 Nb2 Br2 97.712(11) . 2 ?
N1 Nb2 Br2 82.288(11) . 2 ?
Br2 Nb2 Br2 164.58(2) . 2 ?
O1 Nb2 Br2 97.712(11) . 4 ?
N1 Nb2 Br2 82.288(11) . 4 ?
Br2 Nb2 Br2 88.968(3) . 4 ?
Br2 Nb2 Br2 88.968(3) 2 4 ?
O1 Nb2 Br2 97.712(11) . 3 ?
N1 Nb2 Br2 82.288(11) . 3 ?
Br2 Nb2 Br2 88.969(3) . 3 ?
Br2 Nb2 Br2 88.968(3) 2 3 ?
Br2 Nb2 Br2 164.58(2) 4 3 ?
C4 N1 Nb2 180.0 . . ?
N1 C4 C5 180.0 . . ?
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 Br1 2.6017(6) . ?
Nb1 Br1 2.6017(6) 8_656 ?
Nb1 Br1 2.6017(6) 7_666 ?
Nb1 Br1 2.6017(6) 2_655 ?
Nb1 P1 2.7079(9) . ?
Nb1 P1 2.7079(9) 7_666 ?
Nb1 P1 2.7079(9) 2_655 ?
Nb1 P1 2.7079(9) 8_656 ?
P1 C2 1.819(2) . ?
P1 C1 1.823(3) . ?
P1 C3 1.827(2) . ?
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 C3 1.525(5) 2_655 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
Nb2 O1 1.699(3) . ?
Nb2 N1 2.441(4) . ?
Nb2 Br2 2.5535(7) . ?
Nb2 Br2 2.5536(7) 2 ?
Nb2 Br2 2.5536(7) 4 ?
Nb2 Br2 2.5536(7) 3 ?
N1 C4 1.142(6) . ?
C4 C5 1.455(6) . ?
