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_7700201
_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         'C43 H47 Co O P4, C32 H12 B F24'
_chemical_formula_sum            'C75 H59 B Co F24 O P4'
_chemical_formula_weight         1625.84
_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     direct
_audit_creation_date             2018-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                85.307(6)
_cell_angle_beta                 82.481(6)
_cell_angle_gamma                81.765(6)
_cell_formula_units_Z            2
_cell_length_a                   13.892(2)
_cell_length_b                   14.673(2)
_cell_length_c                   19.142(3)
_cell_measurement_reflns_used    3393
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.81
_cell_volume                     3820.5(10)
_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      99.96
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1745
_diffrn_reflns_av_unetI/netI     0.1336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.811
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1219 before and 0.0761 after correction.
The Ratio of minimum to maximum transmission is 0.8681.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       plate
_exptl_crystal_F_000             1650
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.376
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1337P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7347
_reflns_number_total             13490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02313e2.cif
_cod_data_source_block           mo_ry_ss_3_149a_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7700199--7700202.cif.'
_cod_original_cell_volume        3820.7(10)
_cod_database_code               7700201
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.928
_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: F19B(0.5) F24B(0.5) F17B(0.5) F18B(0.5) F18A(0.5) F17A(0.5)
 F24A(0.5) F19A(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C73(H73), C69(H69), C57(H57), C53(H53), C49(H49), C45(H45), C71(H71),
 C61(H61), C55(H55), C9(H9), C65(H65), C12(H12), C11(H11), C21(H21), C33(H33),
 C63(H63), C10(H10), C7(H7), C17(H17), C25(H25), C47(H47), C36(H36), C37(H37),
 C18(H18), C4(H4), C15(H15), C31(H31), C19(H19), C6(H6), C35(H35), C34(H34),
 C30(H30), C24(H24), C27(H27), C23(H23), C16(H16), C5(H5), C28(H28), C22(H22),
 C29(H29)
3.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,
 H40C), C43(H43A,H43B,H43C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              27629
_shelx_fab_checksum              9640
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'