#------------------------------------------------------------------------------
#$Date: 2025-08-21 15:10:22 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301849 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/07/7030790.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_7030790
loop_
_publ_author_name
'Levason, William'
'Light, Mark E.'
'Reid, Gillian'
'Zhang, Wenjian'
_publ_section_title
;
 Soft diphosphine and diarsine complexes of niobium(v) and tantalum(v)
 fluorides: synthesis, properties, structures and comparisons with the
 corresponding chlorides.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9557
_journal_page_last               9566
_journal_paper_doi               10.1039/c4dt01029a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C20 H32 As4 F10 Nb2'
_chemical_formula_weight         947.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.989(4)
_cell_length_b                   21.329(6)
_cell_length_c                   22.051(6)
_cell_measurement_reflns_used    5669
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.7
_cell_measurement_theta_min      2.1
_cell_volume                     6109(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 '
_diffrn_measurement_method       'Profile data from ω-scans'
_diffrn_radiation_collimation    'Confocal mirrors, VHF VariMax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5513
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ Superbright'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.121
_exptl_absorpt_correction_T_max  0.8615
_exptl_absorpt_correction_T_min  0.7838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R.A. (1998). REQAB. Private communication to the 
 Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.427
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1510
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1708
_reflns_number_gt                1399
_reflns_number_total             1510
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4dt01029a2.cif
_cod_data_source_block           14rwz213
_cod_depositor_comments
'Adding full bibliography for 7030785--7030792.cif.'
_cod_database_code               7030790
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
As1 As 0.20310(5) 0.56692(3) 0.02351(3) 0.0384(3) Uani 1 1 d .
Nb1 Nb 0.1250 0.6250 0.1250 0.0357(4) Uani 1 4 d S
Nb2 Nb 0.6250 0.6250 0.1250 0.0308(4) Uani 1 4 d S
F1 F 0.0194(3) 0.56229(18) 0.10036(18) 0.0482(9) Uani 1 1 d .
C1 C 0.3521(6) 0.5626(3) 0.0177(4) 0.0499(18) Uani 1 1 d .
H1A H 0.3796 0.5407 0.0533 0.075 Uiso 1 1 calc R
H1B H 0.3804 0.6051 0.0160 0.075 Uiso 1 1 calc R
H1C H 0.3714 0.5397 -0.0191 0.075 Uiso 1 1 calc R
C2 C 0.1617(7) 0.4799(3) 0.0197(4) 0.0504(17) Uani 1 1 d .
H2A H 0.0864 0.4772 0.0206 0.076 Uiso 1 1 calc R
H2B H 0.1903 0.4573 0.0545 0.076 Uiso 1 1 calc R
H2C H 0.1874 0.4611 -0.0179 0.076 Uiso 1 1 calc R
C3 C 0.1596(6) 0.6003(3) -0.0550(3) 0.0438(14) Uani 1 1 d .
C4 C 0.1920(6) 0.5752(4) -0.1103(4) 0.0547(19) Uani 1 1 d .
H4 H 0.2373 0.5402 -0.1108 0.066 Uiso 1 1 calc R
C5 C 0.1594(7) 0.6003(4) -0.1632(3) 0.0536(18) Uani 1 1 d .
H5 H 0.1838 0.5838 -0.2005 0.064 Uiso 1 1 calc R
F2 F 0.4858(8) 0.6467(6) 0.1139(8) 0.131(5) Uani 0.70 1 d PU
F3 F 0.5961(16) 0.6794(11) 0.0699(9) 0.113(7) Uani 0.40 1 d PU
F4 F 0.6507(12) 0.6918(8) 0.0649(7) 0.074(4) Uani 0.40 1 d PU
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
C2 As1 C1 103.2(3) . .
C2 As1 C3 103.3(3) . .
C1 As1 C3 104.3(3) . .
C2 As1 Nb1 111.4(2) . .
C1 As1 Nb1 116.3(2) . .
C3 As1 Nb1 116.7(2) . .
F1 Nb1 F1 95.6(2) . 11_454
F1 Nb1 F1 148.3(2) . 14_455
F1 Nb1 F1 92.9(2) 11_454 14_455
F1 Nb1 F1 92.9(2) . 8_554
F1 Nb1 F1 148.3(2) 11_454 8_554
F1 Nb1 F1 95.6(2) 14_455 8_554
F1 Nb1 As1 141.10(12) . 8_554
F1 Nb1 As1 80.02(11) 11_454 8_554
F1 Nb1 As1 70.46(12) 14_455 8_554
F1 Nb1 As1 74.31(12) 8_554 8_554
F1 Nb1 As1 74.31(12) . .
F1 Nb1 As1 70.46(12) 11_454 .
F1 Nb1 As1 80.02(11) 14_455 .
F1 Nb1 As1 141.10(12) 8_554 .
As1 Nb1 As1 136.74(3) 8_554 .
F1 Nb1 As1 70.46(12) . 11_454
F1 Nb1 As1 74.31(12) 11_454 11_454
F1 Nb1 As1 141.10(12) 14_455 11_454
F1 Nb1 As1 80.02(11) 8_554 11_454
As1 Nb1 As1 71.17(3) 8_554 11_454
As1 Nb1 As1 126.49(3) . 11_454
F1 Nb1 As1 80.02(11) . 14_455
F1 Nb1 As1 141.10(12) 11_454 14_455
F1 Nb1 As1 74.31(12) 14_455 14_455
F1 Nb1 As1 70.46(12) 8_554 14_455
As1 Nb1 As1 126.49(3) 8_554 14_455
As1 Nb1 As1 71.17(3) . 14_455
As1 Nb1 As1 136.74(3) 11_454 14_455
F3 Nb2 F3 90.2(18) 11_554 8_554
F3 Nb2 F3 154.8(13) 11_554 14
F3 Nb2 F3 95.3(18) 8_554 14
F3 Nb2 F3 95.3(18) 11_554 .
F3 Nb2 F3 154.8(13) 8_554 .
F3 Nb2 F3 90.2(18) 14 .
F3 Nb2 F2 62.2(8) 11_554 11_554
F3 Nb2 F2 106.4(9) 8_554 11_554
F3 Nb2 F2 92.8(7) 14 11_554
F3 Nb2 F2 97.8(9) . 11_554
F3 Nb2 F2 92.8(7) 11_554 14
F3 Nb2 F2 97.8(9) 8_554 14
F3 Nb2 F2 62.2(8) 14 14
F3 Nb2 F2 106.4(9) . 14
F2 Nb2 F2 32.3(7) 11_554 14
F3 Nb2 F2 106.4(9) 11_554 8_554
F3 Nb2 F2 62.2(8) 8_554 8_554
F3 Nb2 F2 97.8(9) 14 8_554
F3 Nb2 F2 92.8(7) . 8_554
F2 Nb2 F2 165.0(10) 11_554 8_554
F2 Nb2 F2 151.6(9) 14 8_554
F3 Nb2 F2 97.8(9) 11_554 .
F3 Nb2 F2 92.8(7) 8_554 .
F3 Nb2 F2 106.4(9) 14 .
F3 Nb2 F2 62.2(8) . .
F2 Nb2 F2 151.6(9) 11_554 .
F2 Nb2 F2 165.0(10) 14 .
F2 Nb2 F2 32.3(7) 8_554 .
F3 Nb2 F4 88.6(9) 11_554 8_554
F3 Nb2 F4 22.6(7) 8_554 8_554
F3 Nb2 F4 87.2(9) 14 8_554
F3 Nb2 F4 175.6(11) . 8_554
F2 Nb2 F4 85.9(7) 11_554 8_554
F2 Nb2 F4 75.4(7) 14 8_554
F2 Nb2 F4 84.1(6) 8_554 8_554
F2 Nb2 F4 115.3(6) . 8_554
F3 Nb2 F4 175.6(11) 11_554 14
F3 Nb2 F4 87.2(9) 8_554 14
F3 Nb2 F4 22.6(7) 14 14
F3 Nb2 F4 88.6(9) . 14
F2 Nb2 F4 115.3(6) 11_554 14
F2 Nb2 F4 84.1(6) 14 14
F2 Nb2 F4 75.4(7) 8_554 14
F2 Nb2 F4 85.9(7) . 14
F4 Nb2 F4 87.5(11) 8_554 14
F3 Nb2 F4 22.6(7) 11_554 11_554
F3 Nb2 F4 88.6(9) 8_554 11_554
F3 Nb2 F4 175.6(11) 14 11_554
F3 Nb2 F4 87.2(9) . 11_554
F2 Nb2 F4 84.1(6) 11_554 11_554
F2 Nb2 F4 115.3(6) 14 11_554
F2 Nb2 F4 85.9(7) 8_554 11_554
F2 Nb2 F4 75.4(7) . 11_554
F4 Nb2 F4 95.7(12) 8_554 11_554
F4 Nb2 F4 160.6(9) 14 11_554
F3 Nb2 F4 87.2(9) 11_554 .
F3 Nb2 F4 175.6(11) 8_554 .
F3 Nb2 F4 88.6(9) 14 .
F3 Nb2 F4 22.6(7) . .
F2 Nb2 F4 75.4(7) 11_554 .
F2 Nb2 F4 85.9(7) 14 .
F2 Nb2 F4 115.3(6) 8_554 .
F2 Nb2 F4 84.1(6) . .
F4 Nb2 F4 160.6(9) 8_554 .
F4 Nb2 F4 95.7(12) 14 .
F4 Nb2 F4 87.5(11) 11_554 .
As1 C1 H1A 109.5 . .
As1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
As1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
As1 C2 H2A 109.5 . .
As1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
As1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C3 C3 C4 119.1(5) 14_455 .
C3 C3 As1 117.7(2) 14_455 .
C4 C3 As1 123.1(6) . .
C5 C4 C3 120.5(8) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C4 C5 C5 120.3(5) . 14_455
C4 C5 H5 119.8 . .
C5 C5 H5 119.8 14_455 .
F2 F2 Nb2 73.9(3) 8_554 .
F4 F3 Nb2 98(2) . .
F3 F4 Nb2 59.7(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 C2 1.935(7) .
As1 C1 1.941(7) .
As1 C3 1.954(7) .
As1 Nb1 2.7518(8) .
Nb1 F1 1.991(4) .
Nb1 F1 1.991(4) 11_454
Nb1 F1 1.991(4) 14_455
Nb1 F1 1.991(4) 8_554
Nb1 As1 2.7518(8) 8_554
Nb1 As1 2.7518(8) 11_454
Nb1 As1 2.7518(8) 14_455
Nb2 F3 1.721(15) 11_554
Nb2 F3 1.721(15) 8_554
Nb2 F3 1.721(15) 14
Nb2 F3 1.721(15) .
Nb2 F2 1.882(10) 11_554
Nb2 F2 1.882(10) 14
Nb2 F2 1.882(10) 8_554
Nb2 F2 1.882(10) .
Nb2 F4 1.975(11) 8_554
Nb2 F4 1.975(11) 14
Nb2 F4 1.975(11) 11_554
Nb2 F4 1.975(11) .
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 1.385(14) 14_455
C3 C4 1.398(10) .
C4 C5 1.350(11) .
C4 H4 0.9500 .
C5 C5 1.382(17) 14_455
C5 H5 0.9500 .
F2 F2 1.05(2) 8_554
F3 F4 0.764(18) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139164221
