#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:29:52 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180013 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/07/7030785.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_7030785
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_moiety         'C20 H32 Cl4 Nb P4, C2 H3 N, Cl'
_chemical_formula_sum            'C22 H35 Cl5 N Nb P4'
_chemical_formula_weight         707.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.431(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.764(6)
_cell_length_b                   10.178(2)
_cell_length_c                   14.770(4)
_cell_measurement_reflns_used    5934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.6
_cell_measurement_theta_min      2.2
_cell_volume                     3085.4(13)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 (Rigaku, 2013)
;
_computing_publication_material  'WINGX (Farrugia, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-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 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9182
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.911
_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            orange
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3191
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0213P)²+4.0161P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2992
_reflns_number_total             3191
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt01029a2.cif
_cod_data_source_block           1010b
_cod_depositor_comments
'Adding full bibliography for 7030785--7030792.cif.'
_cod_original_cell_volume        3085.6(13)
_cod_database_code               7030785
#BEGIN Tags that were not found in dictionaries:
_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   0.885
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
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'
'-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 0.58546(2) 0.0000 0.28880(2) 0.01233(6) Uani 1 2 d S T P . .
Cl1 Cl 0.53644(3) 0.0000 0.41460(5) 0.01829(16) Uani 1 2 d S T P . .
Cl2 Cl 0.56508(3) 0.0000 0.11590(5) 0.01672(15) Uani 1 2 d S T P . .
Cl3 Cl 0.62027(2) -0.22844(5) 0.31212(3) 0.01690(11) Uani 1 1 d . . . . .
Cl4 Cl 0.14320(3) 0.0000 -0.13259(5) 0.01762(16) Uani 1 2 d S T P . .
P1 P 0.67920(4) 0.0000 0.46148(5) 0.01454(16) Uani 1 2 d S T P . .
P2 P 0.70000(4) 0.0000 0.25685(5) 0.01332(16) Uani 1 2 d S T P . .
P3 P 0.48078(2) 0.15555(5) 0.21859(4) 0.01477(12) Uani 1 1 d . . . . .
C1 C 0.67883(10) -0.1401(2) 0.53814(14) 0.0206(5) Uani 1 1 d . . . . .
H1A H 0.6871 -0.2208 0.5079 0.031 Uiso 1 1 calc R U . . .
H1B H 0.6363 -0.1462 0.5471 0.031 Uiso 1 1 calc R U . . .
H1C H 0.7129 -0.1286 0.6006 0.031 Uiso 1 1 calc R U . . .
C2 C 0.76148(13) 0.0000 0.4555(2) 0.0138(6) Uani 1 2 d S T P . .
C3 C 0.81537(14) 0.0000 0.5397(2) 0.0178(7) Uani 1 2 d S T P . .
H3 H 0.8093 0.0000 0.6004 0.021 Uiso 1 2 calc R U P . .
C4 C 0.87792(15) 0.0000 0.5343(2) 0.0193(7) Uani 1 2 d S T P . .
H4 H 0.9146 0.0000 0.5915 0.023 Uiso 1 2 calc R U P . .
C5 C 0.88688(15) 0.0000 0.4460(2) 0.0221(7) Uani 1 2 d S T P . .
H5 H 0.9298 0.0000 0.4429 0.027 Uiso 1 2 calc R U P . .
C6 C 0.83370(14) 0.0000 0.3617(2) 0.0206(7) Uani 1 2 d S T P . .
H6 H 0.8402 0.0000 0.3012 0.025 Uiso 1 2 calc R U P . .
C7 C 0.77048(14) 0.0000 0.3665(2) 0.0149(6) Uani 1 2 d S T P . .
C8 C 0.71468(10) -0.1395(2) 0.19013(15) 0.0184(5) Uani 1 1 d . . . . .
H8A H 0.7549 -0.1250 0.1755 0.028 Uiso 1 1 calc R U . . .
H8B H 0.6781 -0.1493 0.1301 0.028 Uiso 1 1 calc R U . . .
H8C H 0.7190 -0.2195 0.2287 0.028 Uiso 1 1 calc R U . . .
C9 C 0.46234(10) 0.2602(2) 0.30632(15) 0.0218(5) Uani 1 1 d . . . . .
H9A H 0.5020 0.3058 0.3452 0.033 Uiso 1 1 calc R U . . .
H9B H 0.4458 0.2062 0.3481 0.033 Uiso 1 1 calc R U . . .
H9C H 0.4293 0.3250 0.2729 0.033 Uiso 1 1 calc R U . . .
C10 C 0.48487(10) 0.2705(2) 0.12668(15) 0.0232(5) Uani 1 1 d . . . . .
H10A H 0.4801 0.2227 0.0672 0.035 Uiso 1 1 calc R U . . .
H10B H 0.5270 0.3158 0.1482 0.035 Uiso 1 1 calc R U . . .
H10C H 0.4497 0.3351 0.1151 0.035 Uiso 1 1 calc R U . . .
C11 C 0.40508(9) 0.06875(19) 0.16032(13) 0.0158(5) Uani 1 1 d . . . . .
C12 C 0.34746(10) 0.1379(2) 0.11360(15) 0.0216(5) Uani 1 1 d . . . . .
H12 H 0.3470 0.2312 0.1145 0.026 Uiso 1 1 calc R U . . .
C13 C 0.29114(10) 0.0680(2) 0.06601(15) 0.0232(5) Uani 1 1 d . . . . .
H13 H 0.2521 0.1141 0.0331 0.028 Uiso 1 1 calc R U . . .
N1A N 0.7767(3) 0.006(3) 0.7515(5) 0.0261(6) Uiso 0.220(5) 1 d D . P A -1
C14A C 0.8204(4) 0.009(2) 0.8182(6) 0.0261(6) Uiso 0.220(5) 1 d D . P A -1
C15A C 0.8782(4) 0.0230(11) 0.9083(6) 0.0261(6) Uiso 0.220(5) 1 d D . P A -1
H15A H 0.8926 0.1148 0.9161 0.039 Uiso 0.220(5) 1 calc R U P A -1
H15B H 0.9137 -0.0330 0.9038 0.039 Uiso 0.220(5) 1 calc R U P A -1
H15C H 0.8659 -0.0039 0.9636 0.039 Uiso 0.220(5) 1 calc R U P A -1
N1B N 0.7933(3) 0.0150(10) 0.7561(4) 0.0261(6) Uiso 0.280(5) 1 d D . P A -2
C14B C 0.8326(3) 0.002(5) 0.8268(4) 0.0261(6) Uiso 0.280(5) 1 d D . P A -2
C15B C 0.8816(4) -0.0495(8) 0.9167(6) 0.0261(6) Uiso 0.280(5) 1 d D . P A -2
H15D H 0.8889 -0.1432 0.9091 0.039 Uiso 0.280(5) 1 calc R U P A -2
H15E H 0.8654 -0.0372 0.9706 0.039 Uiso 0.280(5) 1 calc R U P A -2
H15F H 0.9227 -0.0016 0.9294 0.039 Uiso 0.280(5) 1 calc R U P A -2
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'
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
Cl1 Nb1 Cl3 94.989(16) . .
Cl1 Nb1 Cl3 94.989(16) . 6
Cl3 Nb1 Cl3 145.57(3) . 6
Cl1 Nb1 Cl2 145.69(3) . .
Cl3 Nb1 Cl2 95.029(14) . .
Cl3 Nb1 Cl2 95.028(14) 6 .
Cl1 Nb1 P3 76.31(2) . 6
Cl3 Nb1 P3 71.06(2) . 6
Cl3 Nb1 P3 143.373(18) 6 6
Cl2 Nb1 P3 76.14(2) . 6
Cl1 Nb1 P3 76.31(2) . .
Cl3 Nb1 P3 143.376(18) . .
Cl3 Nb1 P3 71.06(2) 6 .
Cl2 Nb1 P3 76.14(2) . .
P3 Nb1 P3 72.32(3) 6 .
Cl1 Nb1 P1 70.24(3) . .
Cl3 Nb1 P1 76.299(14) . .
Cl3 Nb1 P1 76.300(14) 6 .
Cl2 Nb1 P1 144.08(3) . .
P3 Nb1 P1 130.272(19) 6 .
P3 Nb1 P1 130.272(19) . .
Cl1 Nb1 P2 143.41(3) . .
Cl3 Nb1 P2 76.203(15) . .
Cl3 Nb1 P2 76.205(15) 6 .
Cl2 Nb1 P2 70.90(3) . .
P3 Nb1 P2 130.55(2) 6 .
P3 Nb1 P2 130.55(2) . .
P1 Nb1 P2 73.18(3) . .
C1 P1 C1 102.96(14) 6 .
C1 P1 C2 103.76(9) 6 .
C1 P1 C2 103.76(9) . .
C1 P1 Nb1 115.55(7) 6 .
C1 P1 Nb1 115.55(7) . .
C2 P1 Nb1 113.72(9) . .
C8 P2 C8 102.84(14) . 6
C8 P2 C7 103.53(9) . .
C8 P2 C7 103.53(9) 6 .
C8 P2 Nb1 115.87(7) . .
C8 P2 Nb1 115.86(7) 6 .
C7 P2 Nb1 113.58(10) . .
C11 P3 C10 102.80(9) . .
C11 P3 C9 104.00(10) . .
C10 P3 C9 103.41(10) . .
C11 P3 Nb1 114.60(7) . .
C10 P3 Nb1 114.99(7) . .
C9 P3 Nb1 115.44(7) . .
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 . .
C7 C2 C3 120.0(3) . .
C7 C2 P1 119.7(2) . .
C3 C2 P1 120.3(2) . .
C4 C3 C2 119.9(3) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C5 C4 C3 120.1(3) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.6(3) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C5 C6 C7 119.6(3) . .
C5 C6 H6 120.2 . .
C7 C6 H6 120.2 . .
C2 C7 C6 119.8(3) . .
C2 C7 P2 119.8(2) . .
C6 C7 P2 120.4(2) . .
P2 C8 H8A 109.5 . .
P2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
P2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
P3 C9 H9A 109.5 . .
P3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
P3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
P3 C10 H10A 109.5 . .
P3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
P3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C11 C11 C12 120.10(12) 6 .
C11 C11 P3 119.13(6) 6 .
C12 C11 P3 120.75(16) . .
C13 C12 C11 119.1(2) . .
C13 C12 H12 120.5 . .
C11 C12 H12 120.5 . .
C13 C13 C12 120.80(13) 6 .
C13 C13 H13 119.6 6 .
C12 C13 H13 119.6 . .
N1A C14A C15A 176(2) . .
C14A C15A H15A 109.5 . .
C14A C15A H15B 109.5 . .
H15A C15A H15B 109.5 . .
C14A C15A H15C 109.5 . .
H15A C15A H15C 109.5 . .
H15B C15A H15C 109.5 . .
N1B C14B C15B 166(4) . .
C14B C15B H15D 109.5 . .
C14B C15B H15E 109.5 . .
H15D C15B H15E 109.5 . .
C14B C15B H15F 109.5 . .
H15D C15B H15F 109.5 . .
H15E C15B H15F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 Cl1 2.4309(9) .
Nb1 Cl3 2.4341(6) .
Nb1 Cl3 2.4341(6) 6
Nb1 Cl2 2.4424(10) .
Nb1 P3 2.6833(7) 6
Nb1 P3 2.6833(7) .
Nb1 P1 2.6843(10) .
Nb1 P2 2.6869(10) .
P1 C1 1.822(2) 6
P1 C1 1.822(2) .
P1 C2 1.822(3) .
P2 C8 1.816(2) .
P2 C8 1.816(2) 6
P2 C7 1.823(3) .
P3 C11 1.815(2) .
P3 C10 1.817(2) .
P3 C9 1.822(2) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C7 1.392(4) .
C2 C3 1.397(4) .
C3 C4 1.389(4) .
C3 H3 0.9500 .
C4 C5 1.382(4) .
C4 H4 0.9500 .
C5 C6 1.390(4) .
C5 H5 0.9500 .
C6 C7 1.401(4) .
C6 H6 0.9500 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C11 1.400(4) 6
C11 C12 1.403(3) .
C12 C13 1.389(3) .
C12 H12 0.9500 .
C13 C13 1.384(4) 6
C13 H13 0.9500 .
N1A C14A 1.120(8) .
C14A C15A 1.502(10) .
C15A H15A 0.9800 .
C15A H15B 0.9800 .
C15A H15C 0.9800 .
N1B C14B 1.116(8) .
C14B C15B 1.493(16) .
C15B H15D 0.9800 .
C15B H15E 0.9800 .
C15B H15F 0.9800 .
