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_1549890
_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         'C47 H42 Co O P3, C32 H12 B F24'
_chemical_formula_sum            'C79 H54 B Co F24 O P3'
_chemical_formula_weight         1637.87
_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             2018-05-22
_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                 104.992(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3130(10)
_cell_length_b                   28.967(2)
_cell_length_c                   18.3198(12)
_cell_measurement_reflns_used    2851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.93
_cell_measurement_theta_min      3.05
_cell_volume                     7336.9(9)
_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      100.01
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2343
_diffrn_reflns_av_unetI/netI     0.2021
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50478
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.592
_diffrn_reflns_theta_max         66.592
_diffrn_reflns_theta_min         2.926
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.406
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1385 before and 0.0822 after correction.
The Ratio of minimum to maximum transmission is 0.6510.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             3316
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         12715
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1972
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.2557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5471
_reflns_number_total             12715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02782j3.cif
_cod_data_source_block           Compound_7
_cod_depositor_comments
'Adding full bibliography for 1549887--1549897.cif.'
_cod_original_cell_volume        7336.8(9)
_cod_database_code               1549890
_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. Uiso/Uaniso restraints and constraints
Uanis(F23A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22A) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: F22B(0.6) F22A(0.4) F23B(0.6) F23A(0.4) F21A(0.4) F21B(0.6)
4.a Aromatic/amide H refined with riding coordinates:
 C77(H77), C65(H65), C11(H11), C13(H13), C69(H69), C53(H53), C44(H44),
 C49(H49), C61(H61), C28(H28), C34(H34), C10(H10), C67(H67), C24(H24), C73(H73),
  C26(H26), C17(H17), C7(H7), C25(H25), C35(H35), C36(H36), C4(H4), C51(H51),
 C57(H57), C6(H6), C75(H75), C20(H20), C5(H5), C23(H23), C22(H22), C32(H32),
 C30(H30), C40(H40), C59(H59), C12(H12), C29(H29), C37(H37), C38(H38), C31(H31),
  C16(H16), C42(H42), C18(H18), C43(H43), C41(H41), C19(H19)
4.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              49672
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'