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_7703857
_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         'C67 H87 Co N4 P'
_chemical_formula_sum            'C67 H87 Co N4 P'
_chemical_formula_weight         1038.30
_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                76.217(2)
_cell_angle_beta                 82.452(2)
_cell_angle_gamma                76.299(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4966(12)
_cell_length_b                   13.3441(13)
_cell_length_c                   22.168(2)
_cell_measurement_reflns_used    1332
_cell_measurement_temperature    184(2)
_cell_measurement_theta_max      20.89
_cell_measurement_theta_min      2.53
_cell_volume                     3198.8(5)
_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 0.978
_diffrn_measured_fraction_theta_max 0.968
_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  0.0602
_diffrn_reflns_av_unetI/netI     0.1744
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16589
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.030
_diffrn_reflns_theta_min         1.608
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         12220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_gt           0.0883
_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^)+(0.0945P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5894
_reflns_number_total             12220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00747a2.cif
_cod_data_source_block           4d
_cod_depositor_comments
'Adding full bibliography for 7703856--7703861.cif.'
_cod_original_cell_volume        3198.8(6)
_cod_database_code               7703857
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.946
_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.a Ternary CH refined with riding coordinates:
 C41(H41), C44(H44), C47(H47), C50(H50), C53(H53), C56(H56), C59(H59), C62(H62)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14),
 C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C27(H27), C30(H30),
  C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C)
;
_shelx_res_checksum              72435
_shelx_fab_checksum              53488
_olex2_submission_special_instructions 'No special instructions were received'