A π-π interaction strategy for targeting highly thermostable bis(arylimino)pyridyliron precatalysts in ethylene polymerization.
Zada, Muhammad; Zhang, Qiuyue; Mahmood, Qaiser; Ma, Yanping; Sun, Yang; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 54 (2025) 7676–7689; doi:10.1039/d5dt00571j

data_7718484
_publ_section_title
;
 A &#x3c0;-&#x3c0; interaction strategy for targeting highly thermostable
 bis(arylimino)pyridyliron precatalysts in ethylene polymerization.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7676
_journal_page_last               7689
_journal_paper_doi               10.1039/d5dt00571j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C57 H54 Cl2 F Fe N3'
_chemical_formula_sum            'C57 H54 Cl2 F Fe N3'
_chemical_formula_weight         926.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-03-07 deposited with the CCDC.	2025-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2129(4)
_cell_length_b                   15.7448(6)
_cell_length_c                   29.0570(9)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      23.9330
_cell_measurement_theta_min      3.4700
_cell_volume                     5587.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -40.00 -14.00   0.50   20.00    --    5.00  45.00  90.00   52
  2  \w     27.00  53.00   0.50   20.00    --    5.00  45.00  90.00   52
  3  \w    -70.00 -44.00   0.50   20.00    --  -14.80  45.00  60.00   52
  4  \w   -103.00  59.00   0.50   20.00    --  -14.80  45.00 120.00  324
  5  \w    -14.00  16.00   0.50   20.00    --  -14.80  45.00  60.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0495545000
_diffrn_orient_matrix_UB_12      -0.0054537000
_diffrn_orient_matrix_UB_13      0.0123878000
_diffrn_orient_matrix_UB_21      -0.0287912000
_diffrn_orient_matrix_UB_22      -0.0223187000
_diffrn_orient_matrix_UB_23      0.0174670000
_diffrn_orient_matrix_UB_31      0.0096321000
_diffrn_orient_matrix_UB_32      -0.0387354000
_diffrn_orient_matrix_UB_33      -0.0117011000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            38282
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.718
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 3341 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         14595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0568P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.774
_reflns_number_gt                10000
_reflns_number_total             14595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00571j2.cif
_cod_data_source_block           Fe3
_cod_depositor_comments
'Adding full bibliography for 7718483--7718484.cif.'
_cod_database_code               7718484
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N Fe Cl'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_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:
 C31(H31), C16(H16), C52(H52), C55(H55)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C39(H39A,H39B), C38(H38A,H38B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C48(H48), C50(H50), C18(H18), C5(H5), C29(H29), C49(H49),
 C6(H6), C19(H19), C4(H4), C44(H44), C33(H33), C41(H41), C20(H20), C28(H28),
 C21(H21), C27(H27), C43(H43), C26(H26), C42(H42), C35(H35), C34(H34), C36(H36)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C),
 C54(H54A,H54B,H54C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              51096
_shelx_hkl_checksum              61294
_shelx_fab_checksum              85292
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_oxdiff_exptl_absorpt_empirical_full_min 0.590