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_1549892
_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         'C80.50 H65 B1 Co1 F24 N1 P3'
_chemical_formula_sum            'C80.5 H65 B Co F24 N P3'
_chemical_formula_weight         1665.02
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-16
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2018-06-10 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                115.7837(19)
_cell_angle_beta                 99.469(2)
_cell_angle_gamma                97.331(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6883(9)
_cell_length_b                   18.4229(13)
_cell_length_c                   18.5758(12)
_cell_measurement_reflns_used    17374
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.619
_cell_measurement_theta_min      2.225
_cell_volume                     3758.4(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.111
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17374
_diffrn_reflns_theta_full        27.066
_diffrn_reflns_theta_max         27.619
_diffrn_reflns_theta_min         2.225
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.67
_refine_diff_density_min         -1.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9321
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         17320
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.0007786
_refine_ls_shift/su_mean         0.0000205
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 7.36P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1299
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1298
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              -23
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10395
_reflns_number_total             17374
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.04
_oxford_diffrn_Wilson_scale      174.89
_oxford_refine_ls_r_factor_ref   0.1218
_oxford_refine_ls_scale          0.082733(14)
_oxford_reflns_number_all        17322
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title Compound_3
_cod_data_source_file            c8sc02782j3.cif
_cod_data_source_block           'global_CCDC2'
_cod_depositor_comments
'Adding full bibliography for 1549887--1549897.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C80.50 H65 B1 Co1 F24 N1 P3'
_cod_database_code               1549892
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(16) TO C(30) 
U(IJ)'S  0.0, 0.010000 = C(16) TO C(31) 
END                                                                             
;