Doubly fused N,N,N-iron ethylene polymerization catalysts appended with fluoride substituents; probing catalytic performance via a combined experimental and MLR study
Zhang, Qiuyue; Yang, Wenhong; Wang, Zheng; Solan, Gregory A.; Liang, Tongling; Sun, Wen-Hua; Catalysis Science & Technology 11 (2021) 4605–4618; doi:10.1039/D1CY00821H

data_1563132
_publ_section_title
;
 Doubly fused N,N,N-iron ethylene polymerization catalysts appended with
 fluoride substituents; probing catalytic performance via a combined
 experimental and MLR study
;
_journal_issue                   13
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4605
_journal_page_last               4618
_journal_paper_doi               10.1039/D1CY00821H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C57 H51 Cl2 F4 Fe N3'
_chemical_formula_sum            'C57 H51 Cl2 F4 Fe N3'
_chemical_formula_weight         980.75
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-07 deposited with the CCDC.	2021-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.6606(3)
_cell_length_b                   14.6606(3)
_cell_length_c                   22.0189(5)
_cell_measurement_reflns_used    10963
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.3320
_cell_measurement_theta_min      3.4660
_cell_volume                     4098.55(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_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     -5.00  28.00   0.50    1.00    --  -47.20  25.00   3.00   66
  2  \w    -38.00 -12.00   0.50    1.00    --  -47.20  38.00 150.00   52
  3  \w   -104.00 -50.00   0.50    3.00    --  -99.00  99.00 150.00  108
  4  \w   -112.00 -86.00   0.50    3.00    --  -99.00 -45.00 120.00   52
  5  \w   -103.00 -76.00   0.50    3.00    --  -99.00 -77.00  90.00   54
  6  \w   -103.00 -77.00   0.50    3.00    --  -99.00 -74.00 104.28   52
  7  \w   -102.00 -76.00   0.50    3.00    --  -99.00 -77.00 150.00   52
  8  \w   -101.00 -75.00   0.50    3.00    --  -99.00 -79.00 132.59   52
  9  \w   -103.00 -77.00   0.50    3.00    --  -99.00 -75.00 139.62   52
 10  \w   -108.00 -81.00   0.50    3.00    --  -99.00 -66.00  98.69   54
 11  \w   -110.00 -78.00   0.50    3.00    --  -99.00 -72.00 130.18   64
 12  \w   -101.00 -75.00   0.50    3.00    --  -99.00 -80.00 106.99   52
 13  \w   -102.00 -77.00   0.50    3.00    --  -99.00 -76.00 164.68   50
 14  \w   -107.00 -81.00   0.50    3.00    --  -99.00 -65.00 142.20   52
 15  \w   -108.00 -81.00   0.50    3.00    --  -99.00 -64.00  98.78   54
 16  \w   -112.00 -76.00   0.50    3.00    --  -99.00 -77.00 120.00   72
 17  \w   -118.00 -76.00   0.50    3.00    --  -99.00 -77.00  85.95   84
 18  \w   -108.00 -82.00   0.50    3.00    --  -99.00 -61.00 150.00   52
 19  \w   -123.00 -80.00   0.50    3.00    --  -99.00 -68.00  87.09   86
 20  \w   -115.00 -77.00   0.50    1.00    --  -47.20-140.00 168.00   76
 21  \w     71.00 116.00   0.50    1.00    --   47.20 140.00-132.00   90
 22  \w     97.00 163.00   0.50    3.00    --  103.25 130.00  54.00  132
 23  \w    130.00 163.00   0.50    3.00    --  103.25 101.00 129.00   66
 24  \w     92.00 169.00   0.50    3.00    --  103.25  99.00 150.00  154
 25  \w     36.00 119.00   0.50    1.00    --   47.20  38.00  60.00  166
 26  \w     47.00  72.00   0.50    1.00    --   47.20  38.00 120.00   50
 27  \w     33.00  66.00   0.50    1.00    --   47.20  57.00 120.00   66
 28  \w     28.00 114.00   0.50    1.00    --   47.20  77.00 120.00  172
 29  \w     36.00  73.00   0.50    3.00    --  103.25 -61.00  90.00   74
 30  \w     78.00 104.00   0.50    3.00    --  103.25-101.00  25.00   52
 31  \w     67.00 106.00   0.50    3.00    --  103.25 -94.00 -30.00   78
 32  \w     36.00  62.00   0.50    3.00    --  103.25 -94.00 -30.00   52
 33  \w    -14.00  12.00   0.50    1.00    --   47.20 -25.00-159.00   52
 34  \w   -102.00 -77.00   0.50    1.00    --  -47.20 -25.00-159.00   50
 35  \w   -151.00-126.00   0.50    3.00    --  -99.00 -25.00-159.00   50
 36  \w   -168.00 -95.00   0.50    3.00    --  -99.00-100.00  67.00  146
 37  \w   -149.00-122.00   0.50    3.00    --  -99.00 -77.00  85.95   54
 38  \w   -163.00 -97.00   0.50    3.00    --  -99.00-105.00  89.00  132
 39  \w   -150.00-124.00   0.50    3.00    --  -99.00 -76.00 164.68   52
 40  \w   -167.00 -77.00   0.50    3.00    --  -99.00 -76.00 124.99  180
 41  \w   -163.00 -80.00   0.50    3.00    --  -99.00-140.00 168.00  166
;
_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      -0.0247461000
_diffrn_orient_matrix_UB_12      -0.1150450000
_diffrn_orient_matrix_UB_13      0.0041255000
_diffrn_orient_matrix_UB_21      -0.1138285000
_diffrn_orient_matrix_UB_22      -0.0381164000
_diffrn_orient_matrix_UB_23      -0.0206306000
_diffrn_orient_matrix_UB_31      0.0336495000
_diffrn_orient_matrix_UB_32      0.0046770000
_diffrn_orient_matrix_UB_33      -0.0667796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45877
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.673
_diffrn_reflns_theta_min         3.481
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60931
_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    1.192
_exptl_crystal_description       needle
_exptl_crystal_F_000             1530
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 3197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10662
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+1.4837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                8421
_reflns_number_total             10662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00821h2.cif
_cod_data_source_block           Fe6
_cod_depositor_comments
'Adding full bibliography for 1563131--1563133.cif.'
_cod_original_cell_volume        4098.54(19)
_cod_database_code               1563132
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N Fe Cl'
_reflns_odcompleteness_completeness 99.94
_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:
 C25(H25), C45(H45)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C10(H10A,H10B), C3(H3A,H3B), C11(H11A,H11B),
 C6(H6A,H6B), C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C19(H19), C37(H37), C41(H41), C21(H21), C57(H57), C8(H8), C30(H30),
 C33(H33), C31(H31), C51(H51), C47(H47), C53(H53), C36(H36), C28(H28), C54(H54),
  C48(H48), C34(H34), C56(H56), C27(H27), C50(H50)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              40339
_shelx_fab_checksum              95671
_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 1.678
_oxdiff_exptl_absorpt_empirical_full_min 0.656