Bis(imino)aryl NCN pincer cobalt complexes: synthesis and disproportionation.
Huang, Li-Cheng; Zhang, Jing-Shun; Jia, Teng; Mu, Ying; Gao, Wei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5219–5227; doi:10.1039/d0dt00747a

data_7703861
_publ_section_title
;
 Bis(imino)aryl NCN pincer cobalt complexes: synthesis and
 disproportionation.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5219
_journal_page_last               5227
_journal_paper_doi               10.1039/d0dt00747a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C64 H78 Br0.6 Cl3.4 Co3 N4'
_chemical_formula_sum            'C64 H78 Br0.6 Cl3.41 Co3 N4'
_chemical_formula_weight         1248.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                70.3670(10)
_cell_angle_beta                 80.8620(10)
_cell_angle_gamma                69.8850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4692(8)
_cell_length_b                   15.6632(11)
_cell_length_c                   21.5144(15)
_cell_measurement_reflns_used    5804
_cell_measurement_temperature    184(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.42
_cell_volume                     3414.1(4)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      184.65
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21693
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.048
_diffrn_reflns_theta_min         1.453
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1299
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         13146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9732
_reflns_number_total             13146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00747a2.cif
_cod_data_source_block           1d-CoCl2
_cod_depositor_comments
'Adding full bibliography for 7703856--7703861.cif.'
_cod_original_formula_sum        'C64 H78 Br0.60 Cl3.41 Co3 N4'
_cod_database_code               7703861
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.790
_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
 Sof(Cl3)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
 Sof(Cl4)=1-FVAR(2)
 Sof(Br3)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C59(H59), C50(H50), C47(H47), C27(H27), C62(H62), C18(H18), C15(H15), C30(H30)
3.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C8(H8), C43(H43), C36(H36), C55(H55), C45(H45), C40(H40), C44(H44),
 C37(H37), C35(H35), C56(H56), C57(H57), C4(H4), C24(H24), C7(H7), C13(H13),
 C5(H5), C11(H11), C3(H3), C25(H25), C23(H23), C12(H12)
3.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C61(H61A,H61B,H61C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C60(H60A,H60B,H60C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C17(H17A,
 H17B,H17C), C48(H48A,H48B,H48C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              8813
_shelx_fab_checksum              20808
_olex2_submission_special_instructions 'No special instructions were received'