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_7033621
_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         'C48 H41 B Mo O3 P3, C8 H20 N'
_chemical_formula_sum            'C56 H61 B Mo N O3 P3'
_chemical_formula_weight         995.71
_chemical_melting_point          546.5(5)
_chemical_name_common            14132a
_chemical_name_systematic        '[Et4N][Mo(CO)3(PhBP3)]'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.795(2)
_cell_length_b                   20.281(2)
_cell_length_c                   22.166(2)
_cell_measurement_reflns_used    2930
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.29
_cell_volume                     9797.9(16)
_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-2014/3 (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 0.999
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            109647
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.451
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_correction_T_min  0.7618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       Needle
_exptl_crystal_F_000             4160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN/Et2O'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0279P)^2^+9.9603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8879
_reflns_number_total             11192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03857f2.cif
_cod_data_source_block           14132a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '546-547' was changed to '546.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7033620--7033630.cif.
;
_cod_original_cell_volume        9798.3(18)
_cod_database_code               7033621
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.984