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_7701640
_publ_section_title
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 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_absolute_configuration unk
_chemical_formula_moiety         'C30 H34 Cl2 Co N3'
_chemical_formula_sum            'C30 H34 Cl2 Co N3'
_chemical_formula_weight         566.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_Int_Tables_number      43
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.273(3)
_cell_length_b                   46.113(9)
_cell_length_c                   9.1517(18)
_cell_measurement_reflns_used    4269
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.4403
_cell_measurement_theta_min      2.7393
_cell_volume                     5601(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9963
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17831
_diffrn_reflns_theta_full        27.4131
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.3433
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2373.8308
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.4353
_refine_diff_density_min         -0.4583
_refine_diff_density_rms         0.0798
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_d_res_high            0.7719
_refine_ls_d_res_low             7.4358
_refine_ls_goodness_of_fit_ref   1.0495
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    39
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.0205
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+19.7523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.995
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              59
_reflns_limit_k_min              -59
_reflns_limit_l_max              11
_reflns_limit_l_min              -11
_reflns_number_gt                3033
_reflns_number_total             3189
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt04892d2.cif
_cod_data_source_block           mx6161a
_cod_original_cell_volume        5601.4(19)
_cod_original_sg_symbol_Hall     ' F 2 -2d'
_cod_database_code               7701640
_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
 C5-C6 = C4-C5 = C4-C3 = C3-C2 = C14-C2 = C6-C14
 1.53 with sigma of 0.01
 C8-C9 = C10-C9 = C10-C11 = C12-C11 = C12-C13 = C1-C13 = C8-C1
 1.53 with sigma of 0.01
 C7-C8 = C7-C6
 1.38 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C13 \\sim C12 \\sim C11 \\sim C10 \\sim C8 \\sim C1 \\sim C9 \\sim C2 \\sim C3
\\sim C4 \\sim C5 \\sim C6 \\sim C14: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Fixed Sof: C13(0.5) C12(0.5) H12a(0.5) H12b(0.5) C11(0.5) H11a(0.5) H11b(0.5)
 C10(0.5) H10a(0.5) H10b(0.5) C8(0.5) C1(0.5) C9(0.5) H9a(0.5) H9b(0.5) C2(0.5)
 C3(0.5) H3a(0.5) H3b(0.5) C4(0.5) H4a(0.5) H4b(0.5) C5(0.5) H5a(0.5) H5b(0.5)
 C6(0.5) C14(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C11(H11a,H11b), C10(H10a,H10b), C9(H9a,H9b), C3(H3a,H3b),
 C4(H4a,H4b), C5(H5a,H5b)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7b), C7(H7a), C19(H19), C18(H18), C17(H17)
5.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'