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_7033623
_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_absolute_configuration ad
_chemical_formula_moiety         'C51 H41 B O6 P3 W2, C8 H20 N'
_chemical_formula_sum            'C59 H61 B N O6 P3 W2'
_chemical_formula_weight         1351.50
_chemical_melting_point          553
_chemical_name_common            14145a
_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                 108.1280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0742(11)
_cell_length_b                   13.3231(12)
_cell_length_c                   17.7935(16)
_cell_measurement_reflns_used    2900
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.34
_cell_volume                     2720.3(4)
_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 0.987
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31902
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.801
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.365
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/E2O'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 4973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         12578
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0306P)^2^+0.8723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                11336
_reflns_number_total             12578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03857f2.cif
_cod_data_source_block           14145b
_cod_depositor_comments
'Adding full bibliography for 7033620--7033630.cif.'
_cod_database_code               7033623
_shelx_estimated_absorpt_t_min   0.476
_shelx_estimated_absorpt_t_max   0.845
_shelxl_version_number           2014-3