Unimodal polyethylenes of high linearity and narrow dispersity by using ortho-4,4′-dichlorobenzhydryl-modified bis(imino)pyridyl-iron catalysts
Liu, Tian; Ma, Yanping; Solan, Gregory A.; Sun, Yang; Sun, Wen-Hua; New Journal of Chemistry 47 (2023) 5786–5795; doi:10.1039/D2NJ06212G

data_7062321
_publ_section_title
;
 Unimodal polyethylenes of high linearity and narrow dispersity by using
 ortho-4,4&#x2032;-dichlorobenzhydryl-modified bis(imino)pyridyl-iron
 catalysts
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5786
_journal_page_last               5795
_journal_paper_doi               10.1039/D2NJ06212G
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C52 H46 Cl6 Fe N3'
_chemical_formula_sum            'C52 H46 Cl6 Fe N3'
_chemical_formula_weight         981.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-20
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6131)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.610(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5593(3)
_cell_length_b                   35.4325(9)
_cell_length_c                   14.4482(4)
_cell_measurement_reflns_used    9005
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      75.0670
_cell_measurement_theta_min      2.5010
_cell_volume                     4689.5(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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_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    -24.00   4.00   0.50    0.40    --  -47.45  29.00-101.00   56
  2  \w    -22.00  28.00   0.50    0.40    --  -47.45  19.00  30.00  100
  3  \w     35.00 121.00   0.50    0.40    --   47.45  29.00-101.00  172
  4  \w    113.00 155.00   0.50    4.00    --  103.25  29.00-101.00   84
  5  \w     54.00 100.00   0.50    4.00    --  103.25 -94.00   0.00   92
  6  \w     45.00  73.00   0.50    4.00    --  103.25 -61.00  90.00   56
  7  \w     42.00  71.00   0.50    4.00    --  103.25 -61.00 150.00   58
  8  \w     33.00  74.00   0.50    4.00    --  103.25 -61.00 120.00   82
  9  \w     90.00 159.00   0.50    4.00    --  103.25  15.00 120.00  138
 10  \w    135.00 162.00   0.50    4.00    --  103.25 125.00 150.00   54
 11  \w     85.00 124.00   0.50    4.00    --  103.25 125.00 150.00   78
 12  \w    -18.00   7.00   0.50    0.40    --   47.45 -29.00  97.00   50
 13  \w     20.00  92.00   0.50    0.40    --   47.45-125.00 -60.00  144
 14  \w     31.00  73.00   0.50    4.00    --  103.25 -61.00-150.00   84
 15  \w     34.00  59.00   0.50    4.00    --  103.25 -61.00-180.00   50
 16  \w    -96.00 -47.00   0.50    0.40    --  -47.45 -29.00  97.00   98
 17  \w    -61.00 -36.00   0.50    4.00    --  -99.00  77.00  60.00   50
 18  \w    -66.00 -27.00   0.50    4.00    --  -99.00  61.00  90.00   78
 19  \w    -62.00 -36.00   0.50    4.00    --  -99.00  61.00 150.00   52
 20  \w    -68.00 -42.00   0.50    4.00    --  -99.00  61.00 120.00   52
 21  \w    -62.00 -33.00   0.50    4.00    --  -99.00  61.00  60.00   58
 22  \w    -68.00 -37.00   0.50    4.00    --  -99.00  61.00   0.00   62
 23  \w    -67.00 -35.00   0.50    4.00    --  -99.00  61.00 -30.00   64
 24  \w    -67.00 -41.00   0.50    4.00    --  -99.00  61.00-150.00   52
 25  \w   -102.00 -32.00   0.50    4.00    --  -99.00  77.00   0.00  140
 26  \w   -101.00 -74.00   0.50    4.00    --  -99.00  77.00  60.00   54
 27  \w   -167.00-126.00   0.50    4.00    --  -99.00 -29.00  97.00   82
 28  \w   -163.00-106.00   0.50    4.00    --  -99.00 -30.00   0.00  114
;
_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      0.0106916000
_diffrn_orient_matrix_UB_12      0.0166559000
_diffrn_orient_matrix_UB_13      0.1002669000
_diffrn_orient_matrix_UB_21      0.1678200000
_diffrn_orient_matrix_UB_22      -0.0005801000
_diffrn_orient_matrix_UB_23      0.0250233000
_diffrn_orient_matrix_UB_31      -0.0019000000
_diffrn_orient_matrix_UB_32      0.0401702000
_diffrn_orient_matrix_UB_33      -0.0411849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35059
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.402
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18334
_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    1.390
_exptl_crystal_description       plate
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+9.5617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1959
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6935
_reflns_number_total             9295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06212g2.cif
_cod_data_source_block           Fe2
_cod_depositor_comments
'Adding full bibliography for 7062321--7062322.cif.'
_cod_database_code               7062321
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'C H N  Fe Cl'
_reflns_odcompleteness_completeness 99.71
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C30(H30), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C49(H49A,H49B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C14(H14), C42(H42), C38(H38), C41(H41), C4(H4), C12(H12),
 C28(H28), C36(H36), C6(H6), C39(H39), C22(H22), C27(H27), C21(H21), C32(H32),
 C35(H35), C24(H24), C47(H47), C33(H33), C46(H46), C18(H18), C25(H25), C45(H45),
  C19(H19)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C29(H29A,H29B,H29C), C9(H9A,H9B,H9C), C52(H52A,H52B,H52C),
 C50(H50A,H50B,H50C)
;
_shelx_res_checksum              13444
_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 3.945
_oxdiff_exptl_absorpt_empirical_full_min 0.448