One-pot synthesis of cobalt complexes with 2,6-bis(arylimino)phenoxyl/phenthioxyl ligands and catalysis on isoprene polymerization.
Chen, Xue-Meng; Huang, Li-Cheng; Gao, Wei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5218–5225; doi:10.1039/d1dt00371b

data_7706829
_publ_section_title
;
 One-pot synthesis of cobalt complexes with
 2,6-bis(arylimino)phenoxyl/phenthioxyl ligands and catalysis on isoprene
 polymerization.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5218
_journal_page_last               5225
_journal_paper_doi               10.1039/d1dt00371b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H54 Cl4 Co2 Li N2 O3, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H70 Cl4 Co2 Li N2 O5'
_chemical_formula_weight         1021.66
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.843(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.092(5)
_cell_length_b                   17.586(5)
_cell_length_c                   19.569(6)
_cell_measurement_reflns_used    5703
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.20
_cell_volume                     5241(3)
_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)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      184.65
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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  0.0864
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32019
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.200
_diffrn_reflns_theta_min         1.597
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.8793
_exptl_absorpt_correction_T_min  0.245881
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1106 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.2459.
The \l/2 correction factor is 0.0015.
;
_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    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         10327
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1201P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2082
_refine_ls_wR_factor_ref         0.2338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6677
_reflns_number_total             10327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00371b2.cif
_cod_data_source_block           Complex_4b
_cod_depositor_comments
'Adding full bibliography for 7706827--7706830.cif.'
_cod_database_code               7706829
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.851
_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
 C46-C47 \\sim C58-C57
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C27(H27), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C57(H57A,H57B),
  C58(H58A,H58B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C38(H38)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              89135
_shelx_hkl_checksum              40381
_olex2_submission_special_instructions 'No special instructions were received'