Enhancing isoprene polymerization with high activity and adjustable monomer enchainment using cyclooctyl-fused iminopyridine iron precatalysts.
Yousuf, Nighat; Ma, Yanping; Mahmood, Qaiser; Zhang, Wenjuan; Wang, Yizhou; Saeed, Hassan; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 53 (2024) 753–764; doi:10.1039/d3dt03674j

data_7714594
_publ_section_title
;
 Enhancing isoprene polymerization with high activity and adjustable
 monomer enchainment using cyclooctyl-fused iminopyridine iron
 precatalysts.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              753
_journal_page_last               764
_journal_paper_doi               10.1039/d3dt03674j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C51 H54 Fe N6), 3(Cl4 Fe), Cl, 1[], 1[]'
_chemical_formula_sum            'C102 H108 Cl13 Fe5 N12'
_chemical_formula_weight         2242.10
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-27 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   12.4440(5)
_cell_length_b                   12.4440(5)
_cell_length_c                   20.0425(11)
_cell_measurement_reflns_used    4234
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.3310
_cell_measurement_theta_min      2.2040
_cell_volume                     2687.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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(10)
_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 0.945
_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    -52.00  27.00   0.50    1.00    --  -46.17  49.00  34.00  158
  2  \w   -161.00-135.00   0.50    4.00    -- -104.50 -99.00 -27.00   52
  3  \w   -170.00 -85.00   0.50    4.00    -- -104.50 -65.00-167.00  170
  4  \w     42.00  69.00   0.50    4.00    --  108.85 -65.00-167.00   54
  5  \w    -14.00  27.00   0.50    1.00    --  -46.17  19.00 -90.00   82
  6  \w    -23.00  23.00   0.50    1.00    --  -46.17  19.00-180.00   92
  7  \w   -152.00 -90.00   0.50    4.00    -- -104.50 -45.00-120.00  124
  8  \w    -66.00 -31.00   0.50    4.00    -- -104.50  61.00  90.00   70
  9  \w   -173.00 -94.00   0.50    4.00    -- -104.50 -45.00 -60.00  158
 10  \w     47.00  72.00   0.50    4.00    --  108.85 -61.00-150.00   50
 11  \w     37.00  74.00   0.50    4.00    --  108.85 -61.00   0.00   74
 12  \w    104.00 177.00   0.50    4.00    --  108.85  45.00  90.00  146
;
_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      0.0673570000
_diffrn_orient_matrix_UB_12      -0.0559267000
_diffrn_orient_matrix_UB_13      -0.0390265000
_diffrn_orient_matrix_UB_21      -0.0534397000
_diffrn_orient_matrix_UB_22      -0.1111186000
_diffrn_orient_matrix_UB_23      0.0481348000
_diffrn_orient_matrix_UB_31      -0.1144203000
_diffrn_orient_matrix_UB_32      -0.0699796000
_diffrn_orient_matrix_UB_33      -0.0453652000
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10315
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.354
_diffrn_reflns_theta_min         2.204
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1155
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.23(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5957
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+1.5094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1450
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.684
_reflns_Friedel_fraction_max     0.608
_reflns_number_gt                4568
_reflns_number_total             5957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03674j2.cif
_cod_data_source_block           tx13927_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7714594--7714596.cif.'
_cod_original_cell_volume        2687.9(3)
_cod_database_code               7714594
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Fe Cl'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C18 \\sim N3 \\sim C19 \\sim C20 \\sim C21 \\sim C28: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl5A)=1-FVAR(1)
 Sof(Fe5A)=Sof(Cl6A)=0.33333*(1-FVAR(2))
 Sof(Fe5)=Sof(Cl6)=0.33333*FVAR(2)
 Sof(Cl5)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              96992
_shelx_fab_checksum              62257
_platon_squeeze_void_probe_radius 1.20
_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 2.206
_oxdiff_exptl_absorpt_empirical_full_min 0.647