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#$Date: 2025-07-01 13:54:44 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1144 $
#$URL: svn://crystallography.net/testcod/cif/7/70/00/7700020.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 κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-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/[σ²(Fo²)+(0.0152P)²+0.4233P]
 where P=(Fo²+2Fc²)/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 > 2σ(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
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_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 . ?
