Synthesis and reactivity of a PC<sub>carbene</sub>P cobalt(i) complex: the missing link in the cobalt PXP pincer series (X = B, C, N).
Sung, Simon; Wang, Qingyang; Krämer, Tobias; Young, Rowan D.; Chemical science 9 (2018) 8234–8241; doi:10.1039/c8sc02782j

data_1549887
_publ_section_title
;
 Synthesis and reactivity of a PC<sub>carbene</sub>P cobalt(i) complex:
 the missing link in the cobalt PXP pincer series (X = B, C, N).
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              8234
_journal_page_last               8241
_journal_paper_doi               10.1039/c8sc02782j
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C75 H58 B1 Br1 Co1 F24 P4'
_chemical_formula_sum            'C75 H58 B Br Co F24 P4'
_chemical_formula_weight         1688.78
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-09
_audit_creation_method           CRYSTALS_ver_14.61_build_6720
_audit_update_record
;
2018-06-10 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.632(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2806(16)
_cell_length_b                   27.575(3)
_cell_length_c                   20.326(2)
_cell_measurement_reflns_used    16572
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.352
_cell_measurement_theta_min      2.145
_cell_volume                     7338.7(14)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.134
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            83209
_diffrn_reflns_theta_full        27.352
_diffrn_reflns_theta_max         27.352
_diffrn_reflns_theta_min         2.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3404
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.75
_refine_diff_density_min         -1.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0304
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         16503
_refine_ls_number_restraints     522
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.0014180
_refine_ls_shift/su_mean         0.0000384
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +12.17P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1324
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1313
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                10116
_reflns_number_total             16572
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.37
_oxford_diffrn_Wilson_scale      333.35
_oxford_refine_ls_r_factor_ref   0.1106
_oxford_refine_ls_scale          0.057758(7)
_oxford_reflns_number_all        16524
_oxford_structure_analysis_title Compound_5
_cod_data_source_file            c8sc02782j3.cif
_cod_data_source_block           global
_cod_depositor_comments
'Adding full bibliography for 1549887--1549897.cif.'
_cod_original_cell_volume        7338.9(15)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C75 H58 B1 Br1 Co1 F24 P4'
_cod_database_code               1549887
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)