Bis(imino)pyridines fused with 6- and 7-membered carbocylic rings as N,N,N-scaffolds for cobalt ethylene polymerization catalysts.
Wang, Zheng; Ma, Yanping; Guo, Jingjing; Liu, Qingbin; Solan, Gregory A.; Liang, Tongling; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2582–2591; doi:10.1039/c8dt04892d

data_7701641
_publ_section_title
;
 Bis(imino)pyridines fused with 6- and 7-membered carbocylic rings as
 N,N,N-scaffolds for cobalt ethylene polymerization catalysts.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2582
_journal_page_last               2591
_journal_paper_doi               10.1039/c8dt04892d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H37 Cl2 Co N3'
_chemical_formula_sum            'C32 H37 Cl2 Co N3'
_chemical_formula_weight         593.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-08 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.99(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.045(5)
_cell_length_b                   8.9623(18)
_cell_length_c                   13.812(3)
_cell_measurement_reflns_used    4517
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.4812
_cell_measurement_theta_min      1.4752
_cell_volume                     2974.7(11)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16643
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.197
_diffrn_reflns_theta_max         25.197
_diffrn_reflns_theta_min         1.695
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.51554
_exptl_absorpt_correction_type   multi-scan
_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    1.325
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2666
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0838
_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^)+(0.0960P)^2^+10.5622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2098
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2500
_reflns_number_total             2666
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04892d2.cif
_cod_data_source_block           mx6928_pl
_cod_database_code               7701641
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.884
_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
 C8-C9 = C5-C4 = C9-C10 = C11-C10 = C3-C4 = C3-C2 = C11-C2
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim C10 \\sim C9 \\sim C8 \\sim C5 \\sim C3 \\sim C4: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C11(0.5) H11A(0.5) H11B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C5(H5A,H5B), C3(H3A,
 H3B), C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C7(H7)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              16218
_olex2_submission_special_instructions 'No special instructions were received'