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_7701642
_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         'C38 H49 Cl2 Co N3'
_chemical_formula_sum            'C38 H49 Cl2 Co N3'
_chemical_formula_weight         677.67
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-04-08 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.30(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.061(2)
_cell_length_b                   24.985(5)
_cell_length_c                   14.220(3)
_cell_measurement_reflns_used    11252
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4783
_cell_measurement_theta_min      1.4382
_cell_volume                     3559.3(13)
_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      173.0
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38806
_diffrn_reflns_theta_full        27.4777
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            'metallic dark yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2646
_exptl_crystal_description       needle
_exptl_crystal_F_000             1438.9960
_exptl_crystal_size_max          0.891
_exptl_crystal_size_mid          0.431
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.4614
_refine_diff_density_min         -0.3776
_refine_diff_density_rms         0.0648
_refine_ls_d_res_high            0.7702
_refine_ls_d_res_low             12.3186
_refine_ls_goodness_of_fit_ref   1.0396
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8134
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.0272
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+3.5869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -9
_reflns_number_gt                7783
_reflns_number_total             8134
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt04892d2.cif
_cod_data_source_block           mx6164
_cod_original_cell_volume        3559.3(12)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7701642
_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
 C9-C8 = C8-C5A = C9-C10 = C5A-C4A = C11-C10 = C4A-C3A = C12-C11 = C3A-C13 =
 C13-C12 = C6-C5 = C9A-C6 = C9A-C10A = C5-C4 = C11A-C10A = C12A-C11A = C4-C3 =
 C3-C2 = C2-C12A
 1.53 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C3 \\sim C5 \\sim C4 \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C12 \\sim
C10 \\sim C11 \\sim C5A \\sim C4A \\sim C3A \\sim C9: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
Cl1 \\sim Cl1A \\sim Cl2 \\sim Cl2A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C9A) \\sim
Ueq, Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl2A) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl1A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=Sof(C10A)=Sof(H10c)=Sof(H10d)=Sof(C11A)=
 Sof(H11c)=Sof(H11d)=Sof(C12A)=Sof(H12c)=Sof(H12d)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=
 Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(Cl1A)=Sof(Cl2A)=
 1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C3)=Sof(H3a)=Sof(H3b)=Sof(C5)=Sof(H5a)=Sof(H5b)=
 Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C10)=Sof(H10a)=
 Sof(H10b)=Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(C9)=Sof(H9a)=Sof(H9b)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C37(H37), C33(H33), C24(H24)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C5(H5a,H5b), C12(H12a,H12b), C4(H4a,H4b), C10(H10a,H10b),
 C11(H11a,H11b), C9(H9a,H9b), C9A(H9Aa,H9Ab), C10A(H10c,H10d), C11A(H11c,H11d),
 C12A(H12c,H12d), C5A(H5Aa,H5Ab), C4A(H4Aa,H4Ab), C3A(H3Aa,H3Ab)
5.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C30(H30), C18(H18), C19(H19), C29(H29), C17(H17), C7(H7)
5.d Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C22(H22a,H22b,H22c), C38(H38a,H38b,H38c), C39(H39a,H39b,
 H39c), C25(H25a,H25b,H25c), C23(H23a,H23b,H23c), C36(H36a,H36b,H36c), C34(H34a,
 H34b,H34c)
;
_olex2_submission_special_instructions 'No special instructions were received'