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_1549896
_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         'C81 H64 B1 Co1 F25 O1 P4'
_chemical_formula_sum            'C81 H64 B Co F25 O P4'
_chemical_formula_weight         1721.99
_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_update_record
;
2018-06-10 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                71.3492(13)
_cell_angle_beta                 83.8715(14)
_cell_angle_gamma                80.5636(15)
_cell_formula_units_Z            2
_cell_length_a                   14.7060(6)
_cell_length_b                   15.1357(5)
_cell_length_c                   19.0310(7)
_cell_measurement_reflns_used    18075
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.482
_cell_measurement_theta_min      2.248
_cell_volume                     3952.6(3)
_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  0.034
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64554
_diffrn_reflns_theta_full        27.482
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.248
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1750
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.089
_refine_diff_density_max         2.91
_refine_diff_density_min         -0.92
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0241
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         18029
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.0027810
_refine_ls_shift/su_mean         0.0000986
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 7.05P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1426
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1426
_reflns_limit_h_max              19
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                14611
_reflns_number_total             18075
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.64
_oxford_diffrn_Wilson_scale      101.79
_oxford_refine_ls_r_factor_ref   0.0621
_oxford_refine_ls_scale          0.10479(3)
_oxford_reflns_number_all        18029
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c8sc02782j3.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1549887--1549897.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C81 H64 B1 Co1 F25 O1 P4'
_cod_database_code               1549896
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S  U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
SAME PART(1001) AND PART (1002) 
DIST 0, 0.01 = MEAN C(108) TO C(109), C(109) TO C(110), C(110) TO C(111), 
CONT C(111) TO C(112), C(112) TO C(113), C(113) TO C(108) 
DIST 0, 0.01 = MEAN C(108) TO C(111), C(109) TO C(112), C(110) TO C(113) 
PLANAR 0.010000  F(107) C(108) C(109) C(110) C(111) C(112) C(113) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.000200 = C(103) TO F(1061) 
VIBR .0, 0.000200 = C(103) TO F(1051) 
VIBR .0, 0.000200 = C(103) TO F(1040) 
VIBR .0, 0.000500 = F(1061) TO C(56) 
VIBR .0, 0.000500 = F(1051) TO C(56) 
VIBR .0, 0.000500 = F(1051) TO F(1061) 
VIBR .0, 0.000500 = F(1040) TO C(56) 
VIBR .0, 0.000500 = F(1040) TO F(1061) 
VIBR .0, 0.000500 = F(1040) TO F(1051) 
VIBR .0, 0.000200 = C(103) TO F(1060) 
VIBR .0, 0.000200 = C(103) TO F(1050) 
VIBR .0, 0.000200 = C(103) TO F(1041) 
VIBR .0, 0.000500 = F(1060) TO C(56) 
VIBR .0, 0.000500 = F(1050) TO C(56) 
VIBR .0, 0.000500 = F(1050) TO F(1060) 
VIBR .0, 0.000500 = F(1041) TO C(56) 
VIBR .0, 0.000500 = F(1041) TO F(1060) 
VIBR .0, 0.000500 = F(1041) TO F(1050) 
VIBR .0, 0.000200 = F(107) TO C(108) 
VIBR .0, 0.000200 = C(108) TO C(109) 
VIBR .0, 0.000200 = C(108) TO C(113) 
VIBR .0, 0.000500 = C(109) TO F(107) 
VIBR .0, 0.000500 = C(113) TO F(107) 
VIBR .0, 0.000500 = C(113) TO C(109) 
VIBR .0, 0.000200 = C(109) TO C(110) 
VIBR .0, 0.000500 = C(110) TO C(108) 
VIBR .0, 0.000200 = C(110) TO C(111) 
VIBR .0, 0.000500 = C(111) TO C(109) 
VIBR .0, 0.000200 = C(111) TO C(112) 
VIBR .0, 0.000500 = C(112) TO C(110) 
VIBR .0, 0.000200 = C(112) TO C(113) 
VIBR .0, 0.000500 = C(113) TO C(111) 
VIBR .0, 0.000500 = C(112) TO C(108) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.008000 = C(103) TO F(1061) 
U(IJ) .0, 0.008000 = C(103) TO F(1051) 
U(IJ) .0, 0.008000 = C(103) TO F(1040) 
U(IJ) .0, 0.008000 = C(103) TO F(1060) 
U(IJ) .0, 0.008000 = C(103) TO F(1050) 
U(IJ) .0, 0.008000 = C(103) TO F(1041) 
U(IJ) .0, 0.008000 = F(107) TO C(108) 
U(IJ) .0, 0.004000 = C(108) TO C(109) 
U(IJ) .0, 0.004000 = C(108) TO C(113) 
U(IJ) .0, 0.004000 = C(109) TO C(110) 
U(IJ) .0, 0.004000 = C(110) TO C(111) 
U(IJ) .0, 0.004000 = C(111) TO C(112) 
U(IJ) .0, 0.004000 = C(112) TO C(113) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;