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_7033629
_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 Mn O6 P3 W'
_chemical_formula_sum            'C51 H41 B Mn O6 P3 W'
_chemical_formula_weight         1092.35
_chemical_name_common            14175b
_chemical_name_systematic        W(CO)3{6-(PhBP3)Mn(CO)3}
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.161(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9471(11)
_cell_length_b                   25.023(2)
_cell_length_c                   17.8217(15)
_cell_measurement_reflns_used    2982
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.35
_cell_volume                     5420.0(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62668
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.464
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_correction_T_min  0.4006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Et2O/pentane'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.4915
_exptl_transmission_factor_min   0.4006
_platon_squeeze_details
;

Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
 =============================================================================

 N: DISORDERED structure ATOMS with Pop. .LT. 1.0 are not moved or as a group.
 -----------------------------------------------------------------------------
 N: Number of moved primary input atoms: ...............................  115
 W: Number of unusual anisotropic displacement parameters ................   1
 N: Total Potential Solvent Accessible Void Vol ................  1270.3 Ang^3
 N: Electron Count / Cell =  358 - To be included in D(calc), F000 & Mol.Wght.

 =============================================================================

 The specimens were grown in DEE/THF/pentane. There are
 channels of disordered solvent of unknown composition.
 The 1270.3 Ang^3 volume could contain 12-14 total molecules of
 these 5-non-hydrogen atom solvents. The refined electron count
 corresponds to about 9 of these solvent molecules.
;
_refine_diff_density_max         1.937
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         12411
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0105P)^2^+17.8669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10953
_reflns_number_total             12411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03857f2.cif
_cod_data_source_block           14175b
_cod_depositor_comments
'Adding full bibliography for 7033620--7033630.cif.'
_cod_original_cell_volume        5419.9(8)
_cod_database_code               7033629
_shelx_estimated_absorpt_t_min   0.401
_shelx_estimated_absorpt_t_max   0.663
_shelxl_version_number           2014-3