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_1563133
_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, C H2 Cl2'
_chemical_formula_sum            'C58 H53 Cl4 F4 Fe N3'
_chemical_formula_weight         1065.68
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-14
_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                 117.144(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1017(5)
_cell_length_b                   15.0497(3)
_cell_length_c                   18.8974(5)
_cell_measurement_reflns_used    11630
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      73.5050
_cell_measurement_theta_min      2.5010
_cell_volume                     5087.3(3)
_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    'ShelXT (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -36.00 -11.00   0.50    0.05    --  -46.95  63.00 176.00   50
  2  \w     -8.00  25.00   0.50    0.05    --  -46.95  63.00 176.00   66
  3  \w    -25.00  61.00   0.50    0.05    --   46.95 -63.00  40.00  172
  4  \w     40.00 115.00   0.50    0.05    --   46.95  63.00 176.00  150
  5  \w    -65.00 -32.00   0.50    0.40    --  -99.00  63.00 176.00   66
  6  \w   -149.00-124.00   0.50    0.40    --  -99.00 -63.00  40.00   50
  7  \w     99.00 155.00   0.50    0.40    --  103.25  63.00 176.00  112
  8  \w     33.00  71.00   0.50    0.40    --  103.25 -63.00  40.00   76
  9  \w    -22.00  23.00   0.50    0.05    --  -46.95  19.00-180.00   90
 10  \w    -99.00 -74.00   0.50    0.05    --  -46.95 -63.00  40.00   50
 11  \w   -118.00 -77.00   0.50    0.05    --  -46.95-125.00-180.00   82
 12  \w   -108.00 -78.00   0.50    0.40    --  -99.00 -77.00 120.00   60
 13  \w    -61.00 -34.00   0.50    0.40    --  -99.00  61.00   0.00   54
 14  \w   -155.00-130.00   0.50    0.40    --  -99.00 -77.00 120.00   50
 15  \w    -93.00 -28.00   0.50    0.40    --  -99.00  77.00-180.00  130
 16  \w    -52.00 -27.00   0.50    0.40    --  -99.00  61.00  30.00   50
 17  \w    -60.00 -34.00   0.50    0.40    --  -99.00  61.00 -60.00   52
 18  \w     46.00 108.00   0.50    0.40    --  103.25 -77.00 -60.00  124
 19  \w     31.00 101.00   0.50    0.40    --  103.25 -77.00  30.00  140
 20  \w     87.00 169.00   0.50    0.40    --  103.25  61.00 -60.00  164
 21  \w    110.00 168.00   0.50    0.40    --  103.25  45.00 120.00  116
 22  \w     31.00  75.00   0.50    0.40    --  103.25 -61.00 -30.00   88
 23  \w     96.00 164.00   0.50    0.40    --  103.25  61.00  90.00  136
 24  \w    114.00 167.00   0.50    0.40    --  103.25  77.00  60.00  106
 25  \w    129.00 158.00   0.50    0.40    --  103.25  30.00-120.00   58
 26  \w     92.00 122.00   0.50    0.40    --  103.25  30.00-120.00   60
;
_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      -0.0837324000
_diffrn_orient_matrix_UB_12      -0.0240539000
_diffrn_orient_matrix_UB_13      -0.0433934000
_diffrn_orient_matrix_UB_21      -0.0122926000
_diffrn_orient_matrix_UB_22      0.0713387000
_diffrn_orient_matrix_UB_23      -0.0632927000
_diffrn_orient_matrix_UB_31      0.0160660000
_diffrn_orient_matrix_UB_32      -0.0692221000
_diffrn_orient_matrix_UB_33      -0.0501778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40098
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.447
_diffrn_reflns_theta_min         2.470
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56251
_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    1.391
_exptl_crystal_description       needle
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.550
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10213
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0799
_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^)+(0.1107P)^2^+13.1141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8588
_reflns_number_total             10213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00821h2.cif
_cod_data_source_block           Fe5
_cod_depositor_comments
'Adding full bibliography for 1563131--1563133.cif.'
_cod_original_cell_volume        5087.3(2)
_cod_database_code               1563133
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N Fe Cl F'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Rigid bond restraints
 C39, C40
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
3.a Ternary CH refined with riding coordinates:
 C25(H25), C45(H45)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C13(H13A,H13B), C6(H6A,H6B), C5(H5A,H5B), C4(H4A,H4B), C12(H12A,
 H12B), C10(H10A,H10B), C11(H11A,H11B), C58(H58A,H58B)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C21(H21), C33(H33), C28(H28), C27(H27), C37(H37), C34(H34),
 C31(H31), C8(H8), C30(H30), C36(H36), C53(H53), C57(H57), C50(H50), C54(H54),
 C56(H56), C47(H47), C39(H39), C41(H41), C51(H51), C48(H48)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C43(H43A,H43B,
 H43C)
;
_shelx_res_checksum              51939
_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 1.753
_oxdiff_exptl_absorpt_empirical_full_min 0.610