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_7701465
_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         'C50 H45 B Cr O3 P3, 0.5(C4 H8 O)'
_chemical_formula_sum            'C52 H49 B Cr O3.5 P3'
_chemical_formula_weight         885.63
_chemical_name_common            17199z
_chemical_name_systematic        Cr(CO)3(((3,5-Me)C6H3)BPPh3)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-09-02 deposited with the CCDC.    2019-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.316(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4916(17)
_cell_length_b                   12.0782(9)
_cell_length_c                   40.404(3)
_cell_measurement_reflns_used    2979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.63
_cell_measurement_theta_min      2.33
_cell_volume                     8929.2(13)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            37511
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.189
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             3704
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and pentane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6965
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         11040
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0373P)^2^+12.2975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9353
_reflns_number_total             11040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03562a2.cif
_cod_data_source_block           17199z
_cod_original_formula_sum        'C52 H49 B Cr O3.50 P3'
_cod_database_code               7701465
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2014/6
_shelx_res_checksum              40067