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_7701464
_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, C36 H30 N P2, 0.5(C5 H12), 0.54(C4 H10 O), 0.46(C4 H8 O)'
;
_chemical_formula_sum            'C92.5 H90.08 B Cr N O4 P5'
_chemical_formula_weight         1497.39
_chemical_name_common            17164z
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1z7c1m
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-02-16 deposited with the CCDC.    2019-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                92.848(8)
_cell_angle_beta                 96.030(7)
_cell_angle_gamma                92.184(8)
_cell_formula_units_Z            2
_cell_length_a                   13.241(3)
_cell_length_b                   13.693(3)
_cell_length_c                   21.408(4)
_cell_measurement_reflns_used    2895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.29
_cell_volume                     3851.5(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AVENTURE PHOTON-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75317
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.295
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5579
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0069(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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         15712
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+6.0819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12257
_reflns_number_total             15712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03562a2.cif
_cod_data_source_block           17164z
_cod_original_cell_volume        3851.3(13)
_cod_original_formula_sum        'C92.50 H90.08 B Cr N O4 P5'
_cod_database_code               7701464
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014/6
_shelx_res_checksum              98835