Cyclometallation reactions of a three-coordinate cobalt(i) complex bearing a nonsymmetric N-heterocyclic carbene ligand.
Gao, Yafei; Chen, Qi; Leng, Xuebing; Deng, Liang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9676–9683; doi:10.1039/c9dt00731h

data_7049345
_publ_section_title
;
 Cyclometallation reactions of a three-coordinate cobalt(i) complex
 bearing a nonsymmetric N-heterocyclic carbene ligand.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9676
_journal_page_last               9683
_journal_paper_doi               10.1039/c9dt00731h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C42 H46 Co N2 P, 1.5(C6 H14)'
_chemical_formula_sum            'C51 H67 Co N2 P'
_chemical_formula_weight         797.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-15 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.541(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.139(5)
_cell_length_b                   14.698(4)
_cell_length_c                   17.703(5)
_cell_measurement_reflns_used    2935
_cell_measurement_temperature    130
_cell_measurement_theta_max      23.750
_cell_measurement_theta_min      2.310
_cell_volume                     4327(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10007
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.662
_diffrn_reflns_theta_min         1.225
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.

Final HKLF 4 output contains 51866 reflections, Rint = 0.1050
 (16687 with I > 3sig(I), Rint = 0.0764)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.088
_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     505
_refine_ls_number_reflns         10007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0886P)^2^+4.9646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6836
_reflns_number_total             10007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00731h2.cif
_cod_data_source_block           dm15035
_cod_depositor_comments
'Adding full bibliography for 7049344--7049347.cif.'
_cod_database_code               7049345
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6744(16)
 0.3256(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C2(H2), C15(H15), C17(H17), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,
 H21B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C50(H50A,H50B), C51(H51A,H51B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C24(H24), C26(H26), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C)
;
_shelx_res_checksum              26264
_olex2_submission_special_instructions 'No special instructions were received'