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_7706830
_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         'C32 H39 Cl4 Co2 Li N2 O3'
_chemical_formula_sum            'C32 H39 Cl4 Co2 Li N2 O3'
_chemical_formula_weight         766.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5708(10)
_cell_length_b                   23.5866(12)
_cell_length_c                   20.4402(11)
_cell_measurement_reflns_used    3825
_cell_measurement_temperature    184.65
_cell_measurement_theta_max      18.52
_cell_measurement_theta_min      2.32
_cell_volume                     8480.5(8)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      184.65
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0776
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41654
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.049
_diffrn_reflns_theta_max         23.049
_diffrn_reflns_theta_min         1.553
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  0.892248
_exptl_absorpt_correction_T_min  0.724574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0528 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.7246.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         11826
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0686
_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^)+(0.1343P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7020
_reflns_number_total             11826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00371b2.cif
_cod_data_source_block           ya007m_sq
_cod_depositor_comments
;
Adding full bibliography for 7706827--7706830.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H78 Cl8 Co4 Li2 N4 O6'
_cod_original_formula_weight         1532.50
_cod_original_formula_moiety         '2(C32 H39 Cl4 Co2 Li N2 O3)'
_cod_original_formula_units_Z            4
_cod_database_code               7706830
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.832
_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. Uiso/Uaniso restraints and constraints
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Li2, C66, C68, C67, C65, O6, O5, C64, C63, C62, C61, Li1, C53, C55, C56, C54,
 O4, O3, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C56(H56A,H56B), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
  C68(H68A,H68B), C55(H55A,H55B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
  C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C)
;
_shelx_res_checksum              46823
_shelx_hkl_checksum              66362
_shelx_fab_checksum              3261
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'