Group VI Metal Carbonyl Complexes of Bis((diphenylphosphino)methyl)diphenylborate and an Assessment of Their Utility for Template Ligand Syntheses
Fischer, Paul J.; Avena, Laura; Bohrmann, Trent D.; Neary, Michelle C.; Putka, Grace K.; Sullivan, Kevin P.; Organometallics 33 (2014) 1300–; doi:10.1021/om5001056

data_4082668
_publ_section_title
;
 Group VI Metal Carbonyl Complexes of
 Bis((diphenylphosphino)methyl)diphenylborate and an Assessment of Their
 Utility for Template Ligand Syntheses
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1300
_journal_paper_doi               10.1021/om5001056
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C48 H38 B Mo N2 O5 P2, C8 H16 N'
_chemical_formula_sum            'C56 H54 B Mo N3 O5 P2'
_chemical_formula_weight         1017.71
_chemical_name_common            13181a
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.124(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6111(3)
_cell_length_b                   16.9866(6)
_cell_length_c                   23.0540(7)
_cell_measurement_reflns_used    2863
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.14
_cell_measurement_theta_min      3.86
_cell_volume                     4910.4(3)
_computing_cell_refinement       'Bruker-AXS APEX-II'
_computing_data_collection       'Bruker-AXS APEX-II'
_computing_data_reduction        'Bruker-AXS APEX-II'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CMOS Bruker Photon-100'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'parabolic mirrors'
_diffrn_radiation_source         'ImuS microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30603
_diffrn_reflns_theta_full        68.47
_diffrn_reflns_theta_max         68.47
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012/1)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.837
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         8933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+16.4194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                6249
_reflns_number_total             8933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5001056_si_003.cif
_cod_data_source_block           13181a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4082668