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_7033627
_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 H651 B Cr Mo O6 P3, C8 H20 N, C4 H8 O'
_chemical_formula_sum            'C63 H69 B Cr Mo N O7 P3'
_chemical_formula_weight         1203.85
_chemical_melting_point          562.5(5)
_chemical_name_common            14167aaa
_chemical_name_systematic        '[Et4N][Cr(CO)3{6-(PhBP3)Mo(CO)3}]'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.4969(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2709(17)
_cell_length_b                   33.329(5)
_cell_length_c                   14.548(2)
_cell_measurement_reflns_used    2977
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.30
_cell_volume                     5944.1(15)
_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 0.988
_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  0.0603
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            69510
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.737
_diffrn_reflns_theta_min         1.528
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_correction_T_min  0.4430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2504
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/Et2O'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_transmission_factor_max   0.4915
_exptl_transmission_factor_min   0.4430
_platon_squeeze_details
;

 PLATON/SQUEEZE applied to treat apparent THF/DEE compositional disorder
 PLATON/SQUEEZE RESULTS Summary and Remarks :N = NOTE, W = WARNING, E = ERROR
 ============================================================================

 N: No S.U.'s (esd) on observed/calculated parameters.
 ---------------------------------------------------------------------------
 N: Number of moved primary input atoms: ................................ 104
 N: Total Potential Solvent Accessible Void Vol ..............   811.5 Ang^3
 N: Electron Count / Cell = 186 - To be included in D(calc), F000 & Mol.Wght.

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

 empirical formula assumes 100% THF
 
;
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         13814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10110
_reflns_number_total             13814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03857f2.cif
_cod_data_source_block           14167aaa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '562-563' was changed to '562.5(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        5944.2(15)
_cod_database_code               7033627
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2014-3