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_7700200
_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 P4, C32 H12 B F24'
_chemical_formula_sum            'C94 H62 B Co F24 P4'
_chemical_formula_weight         1841.05
_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
_atom_sites_solution_primary     dual
_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                94.1390(10)
_cell_angle_beta                 94.6490(10)
_cell_angle_gamma                95.3480(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9047(4)
_cell_length_b                   16.5989(6)
_cell_length_c                   19.3561(7)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.47
_cell_volume                     4101.2(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.997
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62714
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.615
_diffrn_reflns_theta_min         2.466
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1320 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.8533. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.853
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         22911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0710P)^2^+8.1886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15655
_reflns_number_total             22911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02313e2.cif
_cod_data_source_block           mo_ry_ss_4_4ab_0m
_cod_depositor_comments
'Adding full bibliography for 7700199--7700202.cif.'
_cod_database_code               7700200
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: F1B(0.5) F2A(0.5) F2B(0.5) F1A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C64(H64), C68(H68), C88(H88), C92(H92), C4(H4), C66(H66), C84(H84), C7(H7),
 C25(H25), C21(H21), C80(H80), C22(H22), C90(H90), C56(H56), C72(H72), C6(H6),
 C76(H76), C82(H82), C74(H74), C58(H58), C45(H45), C52(H52), C39(H39), C59(H59),
  C55(H55), C23(H23), C24(H24), C61(H61), C60(H60), C15(H15), C62(H62),
 C53(H53), C5(H5), C31(H31), C46(H46), C19(H19), C9(H9), C40(H40), C28(H28),
 C29(H29), C30(H30), C27(H27), C18(H18), C43(H43), C54(H54), C49(H49), C37(H37),
  C17(H17), C10(H10), C33(H33), C47(H47), C35(H35), C41(H41), C16(H16),
 C34(H34), C42(H42), C12(H12), C36(H36), C48(H48), C11(H11)
;
_shelx_res_checksum              8717
_olex2_submission_special_instructions 'No special instructions were received'