#------------------------------------------------------------------------------
#$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1144 $
#$URL: svn://crystallography.net/testcod/cif/7/70/00/7700021.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_7700021
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         'C30 H72 Cl6 Nb2 O2 P6'
_chemical_formula_sum            'C30 H72 Cl6 Nb2 O2 P6'
_chemical_formula_weight         1049.21
_chemical_name_common            '[{NbOCl3(DEPE)2}(DEPE)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 95.496(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8162(3)
_cell_length_b                   11.6449(3)
_cell_length_c                   20.2185(14)
_cell_measurement_reflns_used    17854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2300.53(19)
_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 0.995
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.042
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.758
_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            Orange
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0288
_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/[σ²(Fo²)+(0.0245P)²+2.3917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4591
_reflns_number_total             5247
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01099g2.cif
_cod_data_source_block           2015_0606r3
_cod_original_cell_volume        2300.52(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7700021
_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   0.863
_shelx_estimated_absorpt_t_max   0.948
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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 0.21947(2) 0.20723(2) 0.11474(2) 0.01321(6) Uani 1 1 d . U . . .
Cl1 Cl 0.10248(6) 0.06239(5) 0.18058(3) 0.02252(13) Uani 1 1 d . . . . .
Cl2 Cl 0.43888(6) 0.18235(5) 0.19424(3) 0.02053(12) Uani 1 1 d . . . . .
Cl3 Cl 0.36831(6) 0.23311(5) 0.02394(3) 0.02226(13) Uani 1 1 d . . . . .
O1 O 0.07385(16) 0.25770(14) 0.06960(8) 0.0189(3) Uani 1 1 d . . . . .
P1 P 0.13046(6) 0.30369(5) 0.22420(3) 0.01533(12) Uani 1 1 d . . . . .
P2 P 0.31048(6) 0.42305(5) 0.12649(3) 0.01566(12) Uani 1 1 d . . . . .
P3 P 0.21288(6) -0.00222(5) 0.05033(3) 0.01488(11) Uani 1 1 d . U . . .
C1 C -0.0561(2) 0.3004(2) 0.22644(12) 0.0217(5) Uani 1 1 d . . . . .
H1A H -0.0870 0.2194 0.2236 0.026 Uiso 1 1 calc R U . . .
H1B H -0.0783 0.3309 0.2698 0.026 Uiso 1 1 calc R U . . .
C2 C -0.1365(3) 0.3686(2) 0.17123(13) 0.0275(5) Uani 1 1 d . . . . .
H2A H -0.1105 0.4498 0.1749 0.041 Uiso 1 1 calc R U . . .
H2B H -0.2348 0.3608 0.1754 0.041 Uiso 1 1 calc R U . . .
H2C H -0.1159 0.3390 0.1279 0.041 Uiso 1 1 calc R U . . .
C3 C 0.2036(2) 0.2369(2) 0.30211(11) 0.0200(5) Uani 1 1 d . . . . .
H3A H 0.2165 0.1540 0.2940 0.024 Uiso 1 1 calc R U . . .
H3B H 0.2952 0.2706 0.3143 0.024 Uiso 1 1 calc R U . . .
C4 C 0.1189(3) 0.2503(3) 0.36091(12) 0.0323(6) Uani 1 1 d . . . . .
H4A H 0.0926 0.3310 0.3651 0.049 Uiso 1 1 calc R U . . .
H4B H 0.1731 0.2257 0.4017 0.049 Uiso 1 1 calc R U . . .
H4C H 0.0364 0.2028 0.3538 0.049 Uiso 1 1 calc R U . . .
C5 C 0.4795(3) 0.4547(2) 0.10153(13) 0.0238(5) Uani 1 1 d . . . . .
H5A H 0.5460 0.4013 0.1251 0.029 Uiso 1 1 calc R U . . .
H5B H 0.4789 0.4392 0.0534 0.029 Uiso 1 1 calc R U . . .
C6 C 0.5293(3) 0.5770(2) 0.11484(14) 0.0351(7) Uani 1 1 d . . . . .
H6A H 0.4656 0.6309 0.0910 0.053 Uiso 1 1 calc R U . . .
H6B H 0.6204 0.5862 0.0995 0.053 Uiso 1 1 calc R U . . .
H6C H 0.5341 0.5927 0.1626 0.053 Uiso 1 1 calc R U . . .
C7 C 0.1918(3) 0.5249(2) 0.08191(12) 0.0233(5) Uani 1 1 d . . . . .
H7A H 0.0982 0.5090 0.0940 0.028 Uiso 1 1 calc R U . . .
H7B H 0.2166 0.6035 0.0973 0.028 Uiso 1 1 calc R U . . .
C8 C 0.1895(3) 0.5215(2) 0.00664(13) 0.0310(6) Uani 1 1 d . . . . .
H8A H 0.2801 0.5420 -0.0062 0.047 Uiso 1 1 calc R U . . .
H8B H 0.1215 0.5764 -0.0130 0.047 Uiso 1 1 calc R U . . .
H8C H 0.1654 0.4440 -0.0093 0.047 Uiso 1 1 calc R U . . .
C9 C 0.1777(3) 0.45493(19) 0.23808(12) 0.0209(5) Uani 1 1 d . . . . .
H9A H 0.1077 0.5053 0.2145 0.025 Uiso 1 1 calc R U . . .
H9B H 0.1828 0.4729 0.2861 0.025 Uiso 1 1 calc R U . . .
C10 C 0.3157(3) 0.4758(2) 0.21222(11) 0.0212(5) Uani 1 1 d . . . . .
H10A H 0.3881 0.4351 0.2405 0.025 Uiso 1 1 calc R U . . .
H10B H 0.3370 0.5589 0.2136 0.025 Uiso 1 1 calc R U . . .
C11 C 0.2942(2) -0.0192(2) -0.02704(12) 0.0210(5) Uani 1 1 d . . . . .
H11A H 0.2661 0.0462 -0.0565 0.025 Uiso 1 1 calc R U . . .
H11B H 0.3946 -0.0138 -0.0163 0.025 Uiso 1 1 calc R U . . .
C12 C 0.2633(3) -0.1303(2) -0.06596(13) 0.0288(6) Uani 1 1 d . . . . .
H12A H 0.2891 -0.1963 -0.0374 0.043 Uiso 1 1 calc R U . . .
H12B H 0.3157 -0.1317 -0.1048 0.043 Uiso 1 1 calc R U . . .
H12C H 0.1653 -0.1340 -0.0806 0.043 Uiso 1 1 calc R U . . .
C13 C 0.2756(2) -0.1262(2) 0.10039(12) 0.0217(5) Uani 1 1 d . . . . .
H13A H 0.2200 -0.1342 0.1384 0.026 Uiso 1 1 calc R U . . .
H13B H 0.2621 -0.1965 0.0730 0.026 Uiso 1 1 calc R U . . .
C14 C 0.4259(3) -0.1181(2) 0.12684(15) 0.0326(6) Uani 1 1 d . . . . .
H14A H 0.4831 -0.1247 0.0898 0.049 Uiso 1 1 calc R U . . .
H14B H 0.4484 -0.1804 0.1586 0.049 Uiso 1 1 calc R U . . .
H14C H 0.4430 -0.0440 0.1491 0.049 Uiso 1 1 calc R U . . .
C15 C 0.0342(2) -0.04037(19) 0.02672(11) 0.0165(4) Uani 1 1 d . . . . .
H15A H 0.0297 -0.1201 0.0097 0.020 Uiso 1 1 calc R U . . .
H15B H -0.0171 -0.0373 0.0665 0.020 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'
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'
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
O1 Nb1 Cl3 94.84(6) . . ?
O1 Nb1 Cl1 96.44(6) . . ?
Cl3 Nb1 Cl1 144.44(2) . . ?
O1 Nb1 Cl2 165.81(5) . . ?
Cl3 Nb1 Cl2 87.64(2) . . ?
Cl1 Nb1 Cl2 89.49(2) . . ?
O1 Nb1 P2 88.83(5) . . ?
Cl3 Nb1 P2 74.621(18) . . ?
Cl1 Nb1 P2 139.092(19) . . ?
Cl2 Nb1 P2 78.337(19) . . ?
O1 Nb1 P1 88.57(5) . . ?
Cl3 Nb1 P1 144.942(19) . . ?
Cl1 Nb1 P1 69.054(18) . . ?
Cl2 Nb1 P1 81.511(18) . . ?
P2 Nb1 P1 70.570(18) . . ?
O1 Nb1 P3 94.05(5) . . ?
Cl3 Nb1 P3 75.307(18) . . ?
Cl1 Nb1 P3 70.342(18) . . ?
Cl2 Nb1 P3 100.089(19) . . ?
P2 Nb1 P3 149.926(19) . . ?
P1 Nb1 P3 139.348(18) . . ?
C9 P1 C1 104.72(11) . . ?
C9 P1 C3 101.68(11) . . ?
C1 P1 C3 106.18(11) . . ?
C9 P1 Nb1 115.31(8) . . ?
C1 P1 Nb1 114.40(8) . . ?
C3 P1 Nb1 113.28(8) . . ?
C5 P2 C10 104.53(11) . . ?
C5 P2 C7 106.61(12) . . ?
C10 P2 C7 101.92(11) . . ?
C5 P2 Nb1 118.20(8) . . ?
C10 P2 Nb1 112.19(8) . . ?
C7 P2 Nb1 111.89(8) . . ?
C15 P3 C11 103.67(10) . . ?
C15 P3 C13 102.46(10) . . ?
C11 P3 C13 103.58(11) . . ?
C15 P3 Nb1 108.43(7) . . ?
C11 P3 Nb1 120.33(8) . . ?
C13 P3 Nb1 116.30(8) . . ?
C2 C1 P1 114.71(17) . . ?
C2 C1 H1A 108.6 . . ?
P1 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
P1 C1 H1B 108.6 . . ?
H1A C1 H1B 107.6 . . ?
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 115.30(17) . . ?
C4 C3 H3A 108.4 . . ?
P1 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
P1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
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 . . ?
C6 C5 P2 115.27(18) . . ?
C6 C5 H5A 108.5 . . ?
P2 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
P2 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
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 114.98(18) . . ?
C8 C7 H7A 108.5 . . ?
P2 C7 H7A 108.5 . . ?
C8 C7 H7B 108.5 . . ?
P2 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
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 108.75(16) . . ?
C10 C9 H9A 109.9 . . ?
P1 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
P1 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 P2 109.08(16) . . ?
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 116.68(17) . . ?
C12 C11 H11A 108.1 . . ?
P3 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
P3 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
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 114.03(17) . . ?
C14 C13 H13A 108.7 . . ?
P3 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
P3 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
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 . . ?
C15 C15 P3 112.2(2) 3 . ?
C15 C15 H15A 109.2 3 . ?
P3 C15 H15A 109.2 . . ?
C15 C15 H15B 109.2 3 . ?
P3 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
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 O1 1.7239(16) . ?
Nb1 Cl3 2.4717(6) . ?
Nb1 Cl1 2.4956(6) . ?
Nb1 Cl2 2.5774(6) . ?
Nb1 P2 2.6703(6) . ?
Nb1 P1 2.7007(6) . ?
Nb1 P3 2.7627(6) . ?
P1 C9 1.836(2) . ?
P1 C1 1.837(2) . ?
P1 C3 1.840(2) . ?
P2 C5 1.818(2) . ?
P2 C10 1.835(2) . ?
P2 C7 1.837(2) . ?
P3 C15 1.828(2) . ?
P3 C11 1.834(2) . ?
P3 C13 1.836(2) . ?
C1 C2 1.527(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.523(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.522(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.520(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.518(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.529(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.523(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C15 1.537(4) 3 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
