Direct oxide transfer from an η<sup>2</sup>-keto ligand to generate a cobalt PC<sub>carbene</sub>P(O) pincer complex.
Sung, Simon; Tinnermann, Hendrik; Krämer, Tobias; Young, Rowan D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9920–9924; doi:10.1039/c9dt02313e

data_7700202
_publ_section_title
;
 Direct oxide transfer from an \h<sup>2</sup>-keto ligand to generate a
 cobalt PC<sub>carbene</sub>P(O) pincer complex.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9920
_journal_page_last               9924
_journal_paper_doi               10.1039/c9dt02313e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C62 H50 Co O P4, C32 H12 B F23.8, 0.2(F)'
_chemical_formula_sum            'C94 H62 B Co F24 O P4'
_chemical_formula_weight         1857.05
_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             2019-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                103.307(2)
_cell_angle_beta                 102.563(2)
_cell_angle_gamma                111.047(2)
_cell_formula_units_Z            2
_cell_length_a                   16.0295(8)
_cell_length_b                   19.6246(9)
_cell_length_c                   20.1719(9)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.585
_cell_measurement_theta_min      2.434
_cell_volume                     5439.3(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0762
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            182253
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.755
_diffrn_reflns_theta_min         2.286
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1254 before and 0.0681 after correction. The Ratio of minimum to maximum transmission is 0.9153. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       plate
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1356
_refine_ls_number_reflns         28184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0800P)^2^+9.0731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19776
_reflns_number_total             28184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02313e2.cif
_cod_data_source_block           p-1_sq
_cod_depositor_comments
'Adding full bibliography for 7700199--7700202.cif.'
_cod_database_code               7700202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: F18A(0.66667) F2A(0.66667) F13A(0.66667) F10A(0.66667)
 F12A(0.66667) F3A(0.66667) F1A(0.66667) F17A(0.66667) F9A(0.66667)
 F16A(0.66667) F8A(0.66667) F15A(0.66667) F7A(0.66667) F5A(0.66667)
 F14A(0.66667) F4A(0.66667) C57A(0.6) F11A(0.66667) C71A(0.66667) C66A(0.66667)
 H66A(0.66667) C65A(0.66667) C72A(0.66667) H72A(0.66667) C62A(0.6) H62A(0.6)
 C58A(0.6) H58A(0.6) F24A(0.33333) C64A(0.66667) H64A(0.66667) C88A(0.66667)
 H88A(0.66667) C76A(0.66667) H76A(0.66667) C67A(0.66667) C87A(0.66667)
 C63A(0.66667) C69A(0.66667) C83A(0.66667) C73A(0.66667) C68A(0.66667)
 H68A(0.66667) C79A(0.66667) C82A(0.66667) H82A(0.66667) C84A(0.66667)
 H84A(0.66667) C80A(0.66667) H80A(0.66667) C92A(0.66667) H92A(0.66667)
 C75A(0.66667) C74A(0.66667) H74A(0.66667) C86A(0.66667) C89A(0.66667)
 C85A(0.66667) B1A(0.66667) C59A(0.6) H59A(0.6) C78A(0.66667) C77A(0.66667)
 C81A(0.66667) C70A(0.66667) F20A(0.33333) F6B(0.3) C61A(0.6) H61A(0.6)
 F23C(0.33333) F22B(0.33333) C91A(0.66667) C90A(0.66667) H90A(0.66667)
 C60A(0.6) H60A(0.6) F21C(0.33333) F20B(0.33333) F17B(0.33333) B1B(0.33333)
 F18B(0.33333) C86B(0.33333) F16B(0.33333) C83B(0.33333) C82B(0.33333)
 H82B(0.33333) C84B(0.33333) H84B(0.33333) C81B(0.33333) C79B(0.33333)
 C80B(0.33333) H80B(0.33333) C85B(0.33333) F13B(0.33333) F15B(0.33333)
 F14B(0.33333) C71B(0.33333) C63B(0.33333) C72B(0.33333) H72B(0.33333)
 C76B(0.33333) H76B(0.33333) C92B(0.33333) H92B(0.33333) C91B(0.33333)
 C90B(0.33333) H90B(0.33333) C89B(0.33333) C88B(0.33333) H88B(0.33333)
 C87B(0.33333) C64B(0.33333) H64B(0.33333) C68B(0.33333) H68B(0.33333)
 C73B(0.33333) C75B(0.33333) C65B(0.33333) C67B(0.33333) C74B(0.33333)
 H74B(0.33333) C77B(0.33333) C78B(0.33333) C66B(0.33333) H66B(0.33333)
 C69B(0.33333) C70B(0.33333) F9B(0.33333) F8B(0.33333) F7B(0.33333)
 F10B(0.33333) F12B(0.33333) F11B(0.33333) F21B(0.33333) F24B(0.33333)
 F23B(0.33333) F22A(0.33333) F2B(0.33333) F3B(0.33333) F1B(0.33333) F4B(0.3)
 F5C(0.2) F6A(0.66667) F19C(0.33333) F5B(0.2) C61B(0.4) H61B(0.4) C62B(0.4)
 H62B(0.4) C57B(0.4) C59B(0.4) H59B(0.4) C60B(0.4) H60B(0.4) C58B(0.4)
 H58B(0.4) F19A(0.33333) F21A(0.33333) F19B(0.33333) F20C(0.33333)
 F22C(0.33333) F23A(0.33333) F24C(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C52(H52), C39(H39), C37(H37), C33(H33), C41(H41), C35(H35),
 C22(H22), C40(H40), C42(H42), C45(H45), C6(H6), C27(H27), C31(H31), C13(H13),
 C12(H12), C19(H19), C43(H43), C28(H28), C36(H36), C56(H56), C3(H3), C10(H10),
 C34(H34), C49(H49), C30(H30), C53(H53), C66A(H66A), C54(H54), C11(H11),
 C72A(H72A), C15(H15), C62A(H62A), C23(H23), C5(H5), C58A(H58A), C29(H29),
 C4(H4), C64A(H64A), C46(H46), C88A(H88A), C76A(H76A), C18(H18), C55(H55),
 C68A(H68A), C25(H25), C16(H16), C82A(H82A), C48(H48), C24(H24), C84A(H84A),
 C17(H17), C47(H47), C80A(H80A), C92A(H92A), C74A(H74A), C59A(H59A), C61A(H61A),
  C90A(H90A), C60A(H60A), C82B(H82B), C84B(H84B), C80B(H80B), C72B(H72B),
 C76B(H76B), C92B(H92B), C90B(H90B), C88B(H88B), C64B(H64B), C68B(H68B),
 C74B(H74B), C66B(H66B), C61B(H61B), C62B(H62B), C59B(H59B), C60B(H60B),
 C58B(H58B)
3.c Fitted hexagon refined as free rotating group:
 C92B(C91B,C90B,C89B,C88B,C87B)
;
_shelx_res_checksum              34537
_shelx_fab_checksum              85272
_olex2_submission_special_instructions 'No special instructions were received'