Group VI metal complexes of tris(diphenylphosphinomethyl)phenylborate: modulation of ligand donation via coordination of M(CO)3 units at the borate phenyl substituent.
Fischer, Paul J.; Weberg, Alexander B.; Bohrmann, Trent D.; Xu, Hanyue; Young, Victor G.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3737–3744; doi:10.1039/c4dt03857f

data_7033628
_publ_section_title
;
 Group VI metal complexes of tris(diphenylphosphinomethyl)phenylborate:
 modulation of ligand donation via coordination of M(CO)3 units at the
 borate phenyl substituent.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3737
_journal_page_last               3744
_journal_paper_doi               10.1039/c4dt03857f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C51 H41 B Cr O6 P3 W, C8 H20 N'
_chemical_formula_sum            'C59 H61 B Cr N O6 P3 W'
_chemical_formula_weight         1219.65
_chemical_melting_point          553
_chemical_name_common            14169d
_chemical_name_systematic        '[Et4N][W(CO)3{6-(PhBP3)W(CO)3}]'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.660(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1281(19)
_cell_length_b                   23.778(3)
_cell_length_c                   17.324(2)
_cell_measurement_reflns_used    2967
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.50
_cell_volume                     5819.4(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            67782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.413
_diffrn_reflns_theta_min         1.454
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Et2O'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_transmission_factor_max   0.3334
_exptl_transmission_factor_min   0.2777
_platon_squeeze_details
;
 The refined structure exhibited two putative THF molecules that had 
 excessively large Uij terms or refined partial occupancies. Both appeared
 overlayed with difference Fourier peaks from other unknown solvents. The
 crystallization included both THF and DEE. No DEE could be identified. 
 Analysis of both void space and refined electrons suggest the possibility
 of additional solvent that is invisible. The empirical formula includes only
 the anions and cations.
 =============================================================================
  
 N: No S.U.'s (esd) on observed/calculated parameters.
 -----------------------------------------------------------------------------
 N: Number of Isotropic Non-H Atoms ....................................    2
 N: Number of moved primary input atoms: ...............................  104
 N: Number of modified (= # ) ATOM labels ..............................   51
 W: Number of unusual anisotropic displacement parameters ..............    1
 N: Total Potential Solvent Accessible Void Vol ...............   580.9 Ang^3
 N: Electron Count / Cell = 196 - To be included in D(calc), F000 & Mol.Wght.
 
 =============================================================================

;
_refine_diff_density_max         1.830
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 10829 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1305
_refine_ls_number_reflns         26263
_refine_ls_number_restraints     1359
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                24123
_reflns_number_total             26263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03857f2.cif
_cod_data_source_block           14169d
_cod_depositor_comments
'Adding full bibliography for 7033620--7033630.cif.'
_cod_original_cell_volume        5819.4(14)
_cod_database_code               7033628
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.598
_shelxl_version_number           2014-3