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_7049346
_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         'C29 H36 Co N2'
_chemical_formula_sum            'C29 H36 Co N2'
_chemical_formula_weight         471.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2019-02-13 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7929(17)
_cell_length_b                   10.5688(8)
_cell_length_c                   22.0184(18)
_cell_measurement_reflns_used    5021
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      2.35
_cell_volume                     4838.7(7)
_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      296.15
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.978
_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_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32796
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.850
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0516 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.9108.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.713
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00043(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4651
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0964
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+24.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3810
_reflns_number_total             4651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00731h2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7049344--7049347.cif.'
_cod_database_code               7049346
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C21-C24 = C22-C26 = C23-C28 = C25-C26 = C26-C27 = C27-C28 = C28-C29 = C29-C24
 1.53 with sigma of 0.01
 C21'-C24' = C22'-C26' = C23'-C28' = C25'-C26' = C26'-C27'
 1.53 with sigma of 0.01
 C27'-C28' = C28'-C29' = C29'-C24'
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim C21' \\sim C20' \\sim C22 \\sim C20 \\sim C22' \\sim C23 \\sim C27
\\sim C26 \\sim C25 \\sim C28' \\sim C24' \\sim C24 \\sim C29' \\sim C29 \\sim
C28 \\sim C27' \\sim C25': within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C20') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C20(0.5) C23(0.5) H23A(0.5) H23B(0.5) C21(0.5) H21(0.5) C24(0.5)
 H24(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5) H28(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) C20'(0.5) C21'(0.5) H21'(0.5) C22'(0.5) H22C(0.5) H22D(0.5)
 C23'(0.5) H23C(0.5) H23D(0.5) C24'(0.5) H24'(0.5) C25'(0.5) H25C(0.5)
 H25D(0.5) C26'(0.5) H26'(0.5) C27'(0.5) H27C(0.5) H27D(0.5) C28'(0.5)
 H28'(0.5) C29'(0.5) H29C(0.5) H29D(0.5)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C26(H26), C28(H28), C21'(H21'), C24'(H24'), C26'(H26'),
 C28'(H28')
5.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C25(H25A,H25B), C22(H22A,H22B), C27(H27A,H27B), C29(H29A,
 H29B), C22'(H22C,H22D), C23'(H23C,H23D), C25'(H25C,H25D), C27'(H27C,H27D),
 C29'(H29C,H29D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C13(H13), C15(H15)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              12547
_olex2_submission_special_instructions 'No special instructions were received'