Soft diphosphine and diarsine complexes of niobium(v) and tantalum(v) fluorides: synthesis, properties, structures and comparisons with the corresponding chlorides.
Levason, William; Light, Mark E.; Reid, Gillian; Zhang, Wenjian; Dalton transactions (Cambridge, England : 2003) 43 (2014) 9557–9566; doi:10.1039/c4dt01029a

data_7030787
_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 Cl4 N Nb O, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C22.5 H36 Cl9 N Nb2 O P4'
_chemical_formula_weight         965.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   15.733(2)
_cell_length_b                   14.914(2)
_cell_length_c                   32.080(5)
_cell_measurement_reflns_used    15304
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.7
_cell_measurement_theta_min      2.0
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_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)'
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_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 0.995
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-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  0.0871
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_Laue_measured_fraction_full 0.994
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            29471
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
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_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  1.000
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_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    1.704
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.070
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_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0745
_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/[\s^2^(Fo^2^)+(0.0180P)^2^+9.9885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5695
_reflns_number_total             7372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01029a2.cif
_cod_data_source_block           2013rwz711a
_cod_depositor_comments
'Adding full bibliography for 7030785--7030792.cif.'
_cod_original_cell_volume        7527.2(18)
_cod_original_formula_sum        'C22.50 H36 Cl9 N Nb2 O P4'
_cod_database_code               7030787
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-3
_shelx_res_checksum              66928