Enhancing thermostability of iron ethylene polymerization catalysts through N,N,N-chelation of doubly fused α,α′-bis(arylimino)-2,3:5,6-bis(hexamethylene)pyridines
Wang, Zheng; Zhang, Randi; Zhang, Wenjuan; Solan, Gregory; Liu, Qingbin; tongling, liang; Sun, Wen Hua; Catalysis Science & Technology  (2019) –; doi:10.1039/C9CY00293F

data_1550763
_publ_section_title
;
 Enhancing thermostability of iron ethylene polymerization catalysts
 through N,N,N-chelation of doubly fused
 \a,\a&#x2032;-bis(arylimino)-2,3:5,6-bis(hexamethylene)pyridines
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C9CY00293F
_journal_year                    2019
_chemical_formula_moiety         'C41 H55 Cl4 Fe2 N3 O'
_chemical_formula_sum            'C41 H55 Cl4 Fe2 N3 O'
_chemical_formula_weight         859.41
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-12-29 deposited with the CCDC.    2019-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.228(2)
_cell_length_b                   21.820(4)
_cell_length_c                   16.338(3)
_cell_measurement_reflns_used    12683
_cell_measurement_temperature    175.1500
_cell_measurement_theta_max      27.4764
_cell_measurement_theta_min      0.9332
_cell_volume                     4226.0(14)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      175.1500
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45762
_diffrn_reflns_theta_full        27.4767
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.85681
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.3507
_exptl_crystal_description       needle
_exptl_crystal_F_000             1805.6871
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.8079
_refine_diff_density_min         -0.8544
_refine_diff_density_rms         0.1542
_refine_ls_d_res_high            0.7702
_refine_ls_d_res_low             12.8179
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    85
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9671
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.0364
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+21.6623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8798
_reflns_number_total             9671
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cy00293f2.cif
_cod_data_source_block           Fe3A
_cod_original_cell_volume        4225.9(16)
_cod_database_code               1550763
_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
Cl3 \\sim Cl1a \\sim Cl5 \\sim Cl4 \\sim Cl2 \\sim Cl0a: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(Cl3) \\sim Ueq, Uanis(Cl1a) \\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl0a) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
3. Others
 Sof(Cl4)=Sof(Cl0a)=Sof(Cl1a)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl2)=Sof(Cl5)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C27(H27), C39(H39), C24(H24), C36(H36)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C14(H14a,H14b), C17(H17a,H17b), C11(H11a,H11b), C9(H9a,H9b),
 C8(H8a,H8b), C15(H15a,H15b), C13(H13a,H13b), C10(H10a,H10b), C16(H16a,H16b)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C21(H21), C20(H20), C22(H22), C34(H34), C33(H33), C32(H32)
4.d Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C25(H25a,H25b,H25c), C28(H28a,H28b,H28c), C26(H26a,H26b,
 H26c), C37(H37a,H37b,H37c), C41(H41a,H41b,H41c), C38(H38a,H38b,H38c), C40(H40a,
 H40b,H40c)
;
_olex2_submission_special_instructions 'No special instructions were received'