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_1563131
_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         'C85 H71 Cl2 F8 Fe N3'
_chemical_formula_sum            'C85 H71 Cl2 F8 Fe N3'
_chemical_formula_weight         1413.19
_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     iterative
_audit_creation_date             2020-03-17
_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                 107.7390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.1891(3)
_cell_length_b                   13.76670(10)
_cell_length_c                   33.3782(3)
_cell_measurement_reflns_used    44450
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.1770
_cell_measurement_theta_min      2.5520
_cell_volume                     15838.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (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      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_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    -24.00  61.00   0.50    1.47    --   47.20 -54.00  68.00  170
  2  \w     35.00 118.00   0.50    5.88    --  103.25 -54.00  68.00  166
  3  \w    128.00 154.00   0.50    5.88    --  103.25  15.00 120.00   52
  4  \w     91.00 116.00   0.50    5.88    --  103.25  15.00 120.00   50
  5  \w     35.00 113.00   0.50    5.88    --  103.25 -61.00 -30.00  156
  6  \w     95.00 120.00   0.50    5.88    --  103.25  30.00-150.00   50
  7  \w     89.00 164.00   0.50    5.88    --  103.25  54.00-148.00  150
  8  \w     87.00 113.00   0.50    5.88    --  103.25 -30.00-150.00   52
  9  \w     75.00 101.00   0.50    1.47    --   47.20  54.00-148.00   52
 10  \w     37.00  63.00   0.50    5.88    --  103.25 -30.00-150.00   52
 11  \w    -37.00  24.00   0.50    1.47    --  -47.20  54.00-148.00  122
 12  \w    -69.00 -27.00   0.50    5.88    --  -99.00  45.00  60.00   84
 13  \w    -87.00 -24.00   0.50    5.88    --  -99.00  15.00  60.00  126
 14  \w    -96.00 -70.00   0.50    5.88    --  -99.00  45.00  60.00   52
 15  \w   -120.00 -42.00   0.50    1.47    --  -47.20 -54.00  68.00  156
 16  \w   -119.00 -72.00   0.50    1.47    --  -47.20-125.00  60.00   94
 17  \w   -162.00-126.00   0.50    5.88    --  -99.00 -54.00  68.00   72
 18  \w   -159.00 -85.00   0.50    5.88    --  -99.00 -15.00 150.00  148
 19  \w   -166.00 -94.00   0.50    5.88    --  -99.00 -94.00 150.00  144
 20  \w    -94.00 -69.00   0.50    5.88    --  -99.00  54.00-148.00   50
 21  \w   -120.00 -71.00   0.50    1.47    --  -47.20-125.00-150.00   98
 22  \w   -120.00 -95.00   0.50    1.47    --  -47.20-125.00-180.00   50
;
_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      0.0008770000
_diffrn_orient_matrix_UB_12      -0.0563115000
_diffrn_orient_matrix_UB_13      0.0401703000
_diffrn_orient_matrix_UB_21      -0.0387407000
_diffrn_orient_matrix_UB_22      0.0472020000
_diffrn_orient_matrix_UB_23      -0.0005376000
_diffrn_orient_matrix_UB_31      -0.0222496000
_diffrn_orient_matrix_UB_32      -0.0844084000
_diffrn_orient_matrix_UB_33      -0.0271070000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            119114
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.640
_diffrn_reflns_theta_min         2.564
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             5872
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1791
_refine_ls_number_reflns         31330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+8.8331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25022
_reflns_number_total             31330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy00821h2.cif
_cod_data_source_block           Fe3
_cod_depositor_comments
;
Adding full bibliography for 1563131--1563133.cif.

2022-05-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C170 H142 Cl4 F16 Fe2 N6'
_cod_original_formula_weight         2826.39
_cod_original_formula_moiety         '2(C85 H71 Cl2 F8 Fe N3)'
_cod_original_formula_units_Z            4
_cod_database_code               1563131
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H N F Fe'
_reflns_odcompleteness_completeness 99.70
_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:
 C107(H107), C57(H57), C70(H70), C142(H142), C155(H155), C22(H22), C48(H48),
 C83(H83), C120(H120), C35(H35), C168(H168), C133(H133)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C91(H91A,H91B), C5(H5A,H5B), C13(H13A,H13B), C88(H88A,H88B),
 C90(H90A,H90B), C3(H3A,H3B), C12(H12A,H12B), C10(H10A,H10B), C89(H89A,H89B),
 C98(H98A,H98B), C4(H4A,H4B), C95(H95A,H95B), C11(H11A,H11B), C97(H97A,H97B),
 C96(H96A,H96B)
2.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C8(H8), C53(H53), C150(H150), C65(H65), C140(H140), C93(H93),
 C138(H138), C18(H18), C76(H76), C63(H63), C78(H78), C66(H66), C144(H144),
 C151(H151), C113(H113), C20(H20), C79(H79), C75(H75), C82(H82), C148(H148),
 C59(H59), C72(H72), C69(H69), C62(H62), C103(H103), C105(H105), C68(H68),
 C163(H163), C167(H167), C153(H153), C154(H154), C115(H115), C161(H161),
 C147(H147), C157(H157), C145(H145), C112(H112), C41(H41), C60(H60), C119(H119),
  C34(H34), C109(H109), C73(H73), C24(H24), C81(H81), C132(H132), C160(H160),
 C158(H158), C164(H164), C28(H28), C128(H128), C116(H116), C30(H30), C40(H40),
 C33(H33), C131(H131), C166(H166), C110(H110), C129(H129), C122(H122), C37(H37),
  C43(H43), C118(H118), C31(H31), C126(H126), C44(H44), C38(H38), C123(H123),
 C25(H25), C47(H47), C27(H27), C125(H125), C46(H46)
2.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C134(H13C,H13D,H13E), C170(H17A,
 H17B,H17C), C85(H85A,H85B,H85C), C169(H16A,H16B,H16C), C135(H13F,H13G,H13H),
 C84(H84A,H84B,H84C)
;
_shelx_res_checksum              88117
_shelx_fab_checksum              96574
_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 2.135
_oxdiff_exptl_absorpt_empirical_full_min 0.654