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_1549893
_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
'C45 H49 Co N P4, C32 H12 B F24, C0.75 H0.5 F0.13'
_chemical_formula_sum            'C77.75 H61.5 B Co F24.12 N P4'
_chemical_formula_weight         1661.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-06-10 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.121(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5988(9)
_cell_length_b                   21.2082(17)
_cell_length_c                   18.9102(12)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.39
_cell_volume                     7459.1(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1570
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            88599
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.555
_diffrn_reflns_theta_min         2.211
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1083 before and 0.0812 after correction.
The Ratio of minimum to maximum transmission is 0.8622.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         15441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+35.4389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2245
_refine_ls_wR_factor_ref         0.2786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8354
_reflns_number_total             15441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02782j3.cif
_cod_data_source_block           Compound_10
_cod_depositor_comments
'Adding full bibliography for 1549887--1549897.cif.'
_cod_original_formula_sum        'C77.75 H61.50 B Co F24.12 N P4'
_cod_database_code               1549893
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F13B(0.25) F15A(0.75) F6B(0.5) F14A(0.75) F4B(0.5) F18A(0.5)
 F9B(0.5) C71A(0.75) H71A(0.75) C70A(0.75) C73A(0.75) H73A(0.75) C75A(0.75)
 H75A(0.75) F12B(0.5) C74A(0.75) F5BB(0.25) C72A(0.75) F11B(0.5) F15B(0.25)
 C76A(0.75) F13A(0.75) F14B(0.25) F17A(0.5) C76B(0.25) C0AA(0.25) H0AA(0.25)
 C1AA(0.25) H1AA(0.25) C2AA(0.25) F25(0.125) C73B(0.25) H73B(0.25) C72B(0.25)
 C70B(0.25) C71B(0.25) H71B(0.25) C75B(0.25) H75B(0.25) C74B(0.25) F11A(0.5)
 F12A(0.5) F17B(0.5) F16A(0.25) F18C(0.25) F5AB(0.25) F5AA(0.25) F16C(0.25)
 F5BA(0.25) F6A(0.5) F4A(0.5) F16D(0.25) F18B(0.25) F9A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C47(H47), C51(H51), C55(H55), C49(H49), C65(H65), C67(H67), C59(H59),
 C71A(H71A), C63(H63), C33(H33), C73A(H73A), C75A(H75A), C35(H35), C23(H23),
 C57(H57), C31(H31), C17(H17), C25(H25), C29(H29), C32(H32), C24(H24), C27(H27),
  C26(H26), C30(H30), C21(H21), C6(H6), C9(H9), C14(H14), C36(H36), C11(H11),
 C18(H18), C20(H20), C19(H19), C39(H39), C37(H37), C38(H38), C7(H7), C8(H8),
 C12(H12), C13(H13), C0AA(H0AA), C1AA(H1AA), C73B(H73B), C71B(H71B), C75B(H75B)
3.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C3(H3A,H3B,
 H3C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              27505
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'