Modulation of 2-imino-6,7-dihydroquinlin-8(5H)-imine-iron ethylene polymerization catalysts through (cyclo)alkyl, benzhydryl and halide substitution
Zhang, Randi; Ma, Yanping; Solan, Gregory A.; Wang, Yizhou; Gao, Jiahao; Liang, Tongling; Sun, Wen-Hua; RSC Advances 15 (2025) 35055–35067; doi:10.1039/D5RA06630A

data_7250906
_publ_section_title
;
 Modulation of 2-imino-6,7-dihydroquinlin-8(5H)-imine-iron ethylene
 polymerization catalysts through (cyclo)alkyl, benzhydryl and halide
 substitution
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              35055
_journal_page_last               35067
_journal_paper_doi               10.1039/D5RA06630A
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C61 H60 Cl2 Fe N3, C H2 Cl2'
_chemical_formula_sum            'C63 H64 Cl6 Fe N3'
_chemical_formula_weight         1131.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-12-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2025-09-01 deposited with the CCDC.	2025-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                96.212(3)
_cell_angle_beta                 90.550(3)
_cell_angle_gamma                100.482(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3002(4)
_cell_length_b                   13.7002(6)
_cell_length_c                   22.4970(7)
_cell_measurement_reflns_used    8332
_cell_measurement_temperature    169.99(14)
_cell_measurement_theta_max      71.7950
_cell_measurement_theta_min      3.2780
_cell_volume                     2800.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      169.99(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.951
_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    -39.00  25.00   0.50    7.00    --  -47.20  38.00   0.00  128
  2  \w     -8.00  25.00   0.50    7.00    --  -47.20  57.00  30.00   66
  3  \w     -7.00  26.00   0.50    7.00    --  -47.20  38.00  90.00   66
  4  \w    -22.00  16.00   0.50    7.00    --  -47.20  19.00 -30.00   76
  5  \w    -21.00  27.00   0.50    7.00    --  -47.20  19.00 -90.00   96
  6  \w     31.00  82.00   0.50    7.00    --   47.20-114.00 -34.00  102
  7  \w     46.00  71.00   0.50    8.00    --  103.25-114.00 -34.00   50
  8  \w     45.00 106.00   0.50    8.00    --  103.25 -94.00   0.00  122
  9  \w     38.00  75.00   0.50    8.00    --  103.25 -61.00-120.00   74
 10  \w     45.00  70.00   0.50    8.00    --  103.25 -61.00-180.00   50
 11  \w     58.00 111.00   0.50    8.00    --  103.25-125.00-150.00  106
 12  \w     85.00 111.00   0.50    8.00    --  103.25-125.00-120.00   52
 13  \w     41.00  89.00   0.50    8.00    --  103.25-125.00 -90.00   96
 14  \w     33.00  81.00   0.50    8.00    --  103.25-125.00-120.00   96
 15  \w     31.00  75.00   0.50    8.00    --  103.25 -61.00 -60.00   88
 16  \w    136.00 168.00   0.50    8.00    --  103.25  15.00-180.00   64
 17  \w    124.00 167.00   0.50    8.00    --  103.25  45.00-150.00   86
 18  \w    119.00 145.00   0.50    8.00    --  103.25  45.00 -60.00   52
 19  \w     88.00 155.00   0.50    8.00    --  103.25 114.00  56.00  134
 20  \w    105.00 164.00   0.50    8.00    --  103.25  45.00  60.00  118
 21  \w     80.00 165.00   0.50    8.00    --  103.25 125.00-120.00  170
 22  \w    100.00 133.00   0.50    8.00    --  103.25  15.00-180.00   66
 23  \w     33.00  85.00   0.50    8.00    --  103.25 -94.00 150.00  104
 24  \w    -61.00 -11.00   0.50    7.00    --  -47.20  57.00  30.00  100
 25  \w    -75.00  -5.00   0.50    7.00    --  -47.20 114.00  56.00  140
 26  \w    -67.00 -36.00   0.50    8.00    --  -99.00  61.00-150.00   62
 27  \w    -65.00 -28.00   0.50    8.00    --  -99.00  61.00-180.00   74
 28  \w   -110.00 -27.00   0.50    8.00    --  -99.00 125.00 -90.00  166
 29  \w   -108.00 -55.00   0.50    8.00    --  -99.00 114.00  56.00  106
 30  \w    -98.00 -26.00   0.50    8.00    --  -99.00  77.00  90.00  144
 31  \w   -112.00 -68.00   0.50    8.00    --  -99.00 125.00  90.00   88
 32  \w   -112.00 -51.00   0.50    8.00    --  -99.00 125.00 -60.00  122
 33  \w   -112.00 -79.00   0.50    8.00    --  -99.00 125.00-120.00   66
 34  \w   -162.00 -86.00   0.50    8.00    --  -99.00 -48.00-111.31  152
 35  \w   -118.00 -77.00   0.50    7.00    --  -47.20-125.00-180.00   82
 36  \w   -145.00-106.00   0.50    8.00    --  -99.00-114.00 -34.00   78
 37  \w   -113.00 -88.00   0.50    7.00    --  -47.20-125.00   0.00   50
 38  \w   -119.00 -74.00   0.50    7.00    --  -47.20-125.00  90.00   90
 39  \w   -168.00 -86.00   0.50    8.00    --  -99.00 -45.00   0.00  164
 40  \w   -168.00 -87.00   0.50    8.00    --  -99.00 -48.00  31.85  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0076568000
_diffrn_orient_matrix_UB_12      0.0166065000
_diffrn_orient_matrix_UB_13      -0.0666243000
_diffrn_orient_matrix_UB_21      -0.1466723000
_diffrn_orient_matrix_UB_22      -0.0728140000
_diffrn_orient_matrix_UB_23      -0.0127192000
_diffrn_orient_matrix_UB_31      -0.0826607000
_diffrn_orient_matrix_UB_32      0.0875526000
_diffrn_orient_matrix_UB_33      0.0121878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.746
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1986P)^2^+0.1772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.2973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7228
_reflns_number_total             11095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra06630a2.cif
_cod_data_source_block           Fe3
_cod_database_code               7250906
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Fe Cl'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C42(H42), C23(H23), C57(H57), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C58(H58A,H58B), C61(H61A,H61B), C60(H60A,H60B), C19(H19A,H19B),
 C62(H62A,H62B), C22(H22A,H22B), C59(H59A,H59B), C21(H21A,H21B), C20(H20A,H20B),
  C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C51(H51), C14(H14), C48(H48), C38(H38), C16(H16), C29(H29),
 C52(H52), C28(H28), C31(H31), C46(H46), C47(H47), C32(H32), C5(H5), C55(H55),
 C25(H25), C33(H33), C4(H4), C35(H35), C44(H44), C53(H53), C27(H27), C45(H45),
 C34(H34), C26(H26), C54(H54), C7(H7)
2.d Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C36(H36A,H36B,H36C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              5837
_shelx_fab_checksum              57782
_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 1.534
_oxdiff_exptl_absorpt_empirical_full_min 0.648