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_1549889
_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         'C44 H46 Co P4 S, C32 H12 B F24, C3 H2 F0.5'
_chemical_formula_sum            'C79 H60 B Co F24.5 P4 S'
_chemical_formula_weight         1700.45
_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   geom
_audit_creation_date             2018-04-10
_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                107.508(7)
_cell_angle_beta                 101.067(8)
_cell_angle_gamma                114.080(5)
_cell_formula_units_Z            2
_cell_length_a                   15.234(3)
_cell_length_b                   17.698(3)
_cell_length_c                   18.812(3)
_cell_measurement_reflns_used    5870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.31
_cell_volume                     4117.5(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.94
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.1359
_diffrn_reflns_av_unetI/netI     0.1336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60160
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.421
_diffrn_reflns_theta_min         2.290
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1115 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.7301.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             1725
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         16810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+5.8269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.2370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7801
_reflns_number_total             16810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02782j3.cif
_cod_data_source_block           Compound_8a
_cod_depositor_comments
'Adding full bibliography for 1549887--1549897.cif.'
_cod_original_cell_volume        4117.5(12)
_cod_original_formula_sum        'C79 H60 B Co F24.50 P4 S'
_cod_database_code               1549889
_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: F13A(0.33333) F23A(0.5) F22B(0.5) C20B(0.5) F14A(0.33333)
 C25A(0.5) H25A(0.5) C22A(0.5) H22A(0.5) C21B(0.5) H21B(0.5) F15B(0.33333)
 C24A(0.5) H24A(0.5) C23A(0.5) H23A(0.5) F21A(0.5) F3A(0.5) C52A(0.5) F2B(0.5)
 F3B(0.5) F036(0.5) F1B(0.5) F2A(0.5) F1A(0.5) F13C(0.33333) F14C(0.33333)
 F22A(0.5) F23B(0.5) F21B(0.5) C52B(0.5) C25B(0.5) H25B(0.5) C20A(0.5)
 C21A(0.5) H21A(0.5) C22B(0.5) H22B(0.5) C23B(0.5) H23B(0.5) C24B(0.5)
 H24B(0.5) F14B(0.33333) F15C(0.33333) F13B(0.33333) F15A(0.33333)
3.a Aromatic/amide H refined with riding coordinates:
 C58(H58), C70(H70), C66(H66), C27(H27), C54(H54), C28(H28), C6AA(H6AA),
 C46(H46), C4AA(H4AA), C74(H74), C5AA(H5AA), C64(H64), C56(H56), C62(H62),
 C6(H6), C33(H33), C31(H31), C8AA(H8AA), C15(H15), C29(H29), C30(H30), C34(H34),
  C50(H50), C25A(H25A), C22A(H22A), C16(H16), C19(H19), C11(H11), C21B(H21B),
 C37(H37), C35(H35), C72(H72), C1AA(H1AA), C12(H12), C48(H48), C17(H17),
 C24A(H24A), C23A(H23A), C36(H36), C18(H18), C77(H77), C79(H79), C25B(H25B),
 C21A(H21A), C22B(H22B), C23B(H23B), C24B(H24B)
3.b Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C43(H43A,H43B,
 H43C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              67268
_shelx_fab_checksum              44593
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'