Fluoro- & trifluoromethoxy-modified bis(imino)pyridyliron chloride enhancing the activity and stability of vinyl polyethylenes.
Hosseinzadeh, Zahra; Zhang, Qiuyue; Gao, Jiahao; Wang, Yizhou; Wang, Quanchao; Ren, Geng; Liang, Tongling; Ma, Yanping; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12590–12600; doi:10.1039/d5dt00837a

data_7719142
_publ_section_title
;
 Fluoro- &amp; trifluoromethoxy-modified bis(imino)pyridyliron chloride
 enhancing the activity and stability of vinyl polyethylenes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12590
_journal_page_last               12600
_journal_paper_doi               10.1039/d5dt00837a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C51 H40 Cl2 F7 Fe N3 O, C H2 Cl2'
_chemical_formula_sum            'C52 H42 Cl4 F7 Fe N3 O'
_chemical_formula_weight         1055.53
_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     iterative
_audit_creation_date             2025-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-06-07 deposited with the CCDC.	2025-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.251(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4460(6)
_cell_length_b                   15.9337(4)
_cell_length_c                   18.7644(8)
_cell_measurement_reflns_used    15542
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      76.418
_cell_measurement_theta_min      2.8570
_cell_volume                     5140.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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_temperature      170.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10513
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.196
_diffrn_reflns_theta_min         2.878
_exptl_absorpt_coefficient_mu    4.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.587
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         10513
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1538
_refine_ls_R_factor_gt           0.1414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1892P)^2^+41.1062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3968
_refine_ls_wR_factor_ref         0.4097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9132
_reflns_number_total             10513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00837a2.cif
_cod_data_source_block           Fe4
_cod_depositor_comments
'Adding full bibliography for 7719142--7719143.cif.'
_cod_database_code               7719142
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.688(6)
 0.312(6)
2. 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
3. Restrained distances
 Cl5-C53 = Cl6-C53
 1.76 with sigma of 0.01
 Cl3-C52 = Cl4-C52
 1.76 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Cl5 \\sim Cl6 \\sim C53: within 1.9A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Cl3 \\sim Cl4 \\sim C52: within 1.9A with sigma of 0.02 and sigma for terminal
atoms of 0.04
5. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C52(0.5) H52A(0.5) H52B(0.5) Cl5(0.5) Cl6(0.5)
 C53(0.5) H53A(0.5) H53B(0.5)
6.a Ternary CH refined with riding coordinates:
 C25(H25), C39(H39)
6.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C4(H4), C5(H5), C6(H6), C21(H21), C23(H23), C27(H27),
 C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C41(H41),
  C42(H42), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C1(H1A,H1B,
 H1C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              69380
_shelx_hkl_checksum              28787
_olex2_submission_special_instructions 'No special instructions were received'