Seventeen-electron chromium(i)tricarbonyltris(phosphine) complexes supported by tris(phosphinomethyl)phenylborates
Fischer, Paul J.; Senthil, Shuruthi; Stephan, Jeremy T.; Swift, McKinley L.; Young, Victor G.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03562A

data_7701469
_publ_section_title
;
 Seventeen-electron chromium(i)tricarbonyltris(phosphine) complexes
 supported by tris(phosphinomethyl)phenylborates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03562A
_journal_year                    2019
_chemical_formula_moiety         'C51 H41 B Cr2 O6 P3'
_chemical_formula_sum            'C51 H41 B Cr2 O6 P3'
_chemical_formula_weight         957.56
_chemical_name_common            18126zzz
_chemical_name_systematic        Cr(CO)3{h6-(PhBPPh3)Cr(CO)3}
_chemical_properties_physical    Air-sensitive,Moisture-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-2018/3
_audit_update_record
;
2019-09-02 deposited with the CCDC.    2019-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.3610(13)
_cell_length_b                   20.185(2)
_cell_length_c                   45.506(6)
_cell_measurement_reflns_used    2835
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.90
_cell_measurement_theta_min      2.59
_cell_volume                     9517(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            89292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.384
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and pentane'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.4311
_exptl_transmission_factor_min   0.3642
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9037
_refine_ls_number_restraints     668
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+34.2701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8198
_reflns_number_total             9037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03562a2.cif
_cod_data_source_block           18126zzz
_cod_database_code               7701469
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              12984
_shelx_fab_checksum              4335