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_7703860
_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         'C32 H39 Cl3 Co2 N2, C16 H32 Li O4'
_chemical_formula_sum            'C48 H71 Cl3 Co2 Li N2 O4'
_chemical_formula_weight         971.21
_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
_atom_sites_solution_primary     heavy
_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                101.3510(10)
_cell_angle_beta                 105.3260(10)
_cell_angle_gamma                109.0460(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2848(7)
_cell_length_b                   13.9972(9)
_cell_length_c                   18.1516(12)
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.48
_cell_volume                     2484.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0189
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12989
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.619
_exptl_absorpt_coefficient_mu    0.871
_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    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0564P)^2^+0.4419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6582
_reflns_number_total             8651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00747a2.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 7703856--7703861.cif.'
_cod_database_code               7703860
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.859
_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.a Ternary CH refined with riding coordinates:
 C30(H30), C15(H15), C27(H27), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C45(H45A,H45B), C40(H40A,H40B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C41(H41A,H41B), C39(H39A,H39B), C33(H33A,H33B),
 C35(H35A,H35B), C48(H48A,H48B), C37(H37A,H37B), C38(H38A,H38B), C34(H34A,H34B),
  C47(H47A,H47B), C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C8(H8), C7(H7), C3(H3), C23(H23), C25(H25), C11(H11), C13(H13),
 C12(H12), C5(H5), C4(H4)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C19(H19A,
 H19B,H19C)
;
_shelx_res_checksum              19764
_olex2_submission_special_instructions 'No special instructions were received'