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_1550762
_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 Cl2 Fe N3, C4 H8 O'
_chemical_formula_sum            'C45 H63 Cl2 Fe N3 O'
_chemical_formula_weight         788.71
_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     dual
_audit_creation_date             2018-10-10
_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                 102.600(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3638(3)
_cell_length_b                   34.6037(6)
_cell_length_c                   18.3685(4)
_cell_measurement_reflns_used    23669
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.1780
_cell_measurement_theta_min      1.7180
_cell_volume                     8289.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.636
_exptl_absorpt_coefficient_mu    0.530
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       rod
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.801
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         19015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.1006
_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^)+(0.0742P)^2^+46.4080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2461
_refine_ls_wR_factor_ref         0.2641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13319
_reflns_number_total             19015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy00293f2.cif
_cod_data_source_block           Fe3
_cod_depositor_comments
;

2019-05-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H122 Cl4 Fe2 N6 O2'
_cod_original_formula_weight         1573.43
_cod_original_formula_moiety         '2(C41 H55 Cl2 Fe N3), C4 H8 O, C4 H4 O'
_cod_original_formula_units_Z            4
_cod_database_code               1550762
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C68(H68), C77(H77), C39(H39), C36(H36), C27(H27), C80(H80), C65(H65), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C11(H11a,H11b), C58(H58a,H58b), C14(H14a,H14b), C13(H13a,
 H13b), C57(H57a,H57b), C15(H15a,H15b), C54(H54a,H54b), C52(H52a,H52b), C7(H7a,
 H7b), C48(H48a,H48b), C10(H10a,H10b), C51(H51a,H51b), C55(H55a,H55b), C16(H16a,
 H16b), C50(H50a,H50b), C9(H9a,H9b), C56(H56a,H56b), C8(H8a,H8b), C49(H49a,
 H49b), C87(H87a,H87b), C90(H90a,H90b), C89(H89a,H89b), C88(H88a,H88b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C44(H44), C75(H75), C33(H33), C74(H74), C34(H34), C61(H61), C62(H62),
 C25(H25), C73(H73), C32(H32), C63(H63), C23(H23), C24(H24), C85(H85), C83(H83),
  C86(H86), C84(H84)
2.d Idealised Me refined as rotating group:
 C69(H69a,H69b,H69c), C29(H29a,H29b,H29c), C70(H70a,H70b,H70c), C28(H28a,H28b,
 H28c), C38(H38a,H38b,H38c), C37(H37a,H37b,H37c), C82(H82a,H82b,H82c), C67(H67a,
 H67b,H67c), C81(H81a,H81b,H81c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c),
 C66(H66a,H66b,H66c), C41(H41a,H41b,H41c), C78(H78a,H78b,H78c), C79(H79a,H79b,
 H79c), C40(H40a,H40b,H40c)
;
_shelx_res_checksum              7370
_olex2_submission_special_instructions 'No special instructions were received'