gem-Dimethyl-substituted bis(imino)dihydroquinolines as thermally stable supports for highly active cobalt catalysts that produce linear PE waxes.
Zhang, Randi; Huang, Yongfeng; Solan, Gregory A.; Zhang, Wenjuan; Hu, Xinquan; Hao, Xiang; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8175–8185; doi:10.1039/c9dt01345h

data_7049998
_publ_section_title
;
 gem-Dimethyl-substituted bis(imino)dihydroquinolines as thermally stable
 supports for highly active cobalt catalysts that produce linear PE waxes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8175
_journal_page_last               8185
_journal_paper_doi               10.1039/c9dt01345h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C33 H41 Cl2 Co N3'
_chemical_formula_sum            'C33 H41 Cl2 Co N3'
_chemical_formula_weight         609.52
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-05 deposited with the CCDC.    2019-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.73(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.285(4)
_cell_length_b                   9.0803(18)
_cell_length_c                   18.993(4)
_cell_measurement_reflns_used    9490
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.4793
_cell_measurement_theta_min      1.0877
_cell_volume                     3108.1(12)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20874
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.582
_diffrn_reflns_theta_min         2.176
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74490
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.551
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7063
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0530P)^2^+3.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6361
_reflns_number_total             7063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01345h2.cif
_cod_data_source_block           Co2
_cod_depositor_comments
'Adding full bibliography for 7049998--7049999.cif.'
_cod_original_cell_volume        3108.2(11)
_cod_database_code               7049998
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-C22 = C23-C22 = C22-C19
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim C23 \\sim C22: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(H22C)=Sof(H22D)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C31(H31A,H31B), C8(H8A,H8B), C33(H33A,H33B), C20(H20A,H20B),
 C22(H22A,H22B), C22(H22C,H22D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C28(H28), C5(H5), C30(H30), C29(H29), C16(H16), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C32(H32A,H32B,
 H32C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              41658
_olex2_submission_special_instructions 'No special instructions were received'