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_7714596
_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         'C44 H56 Cl Fe N4, Cl4 Fe'
_chemical_formula_sum            'C44 H56 Cl5 Fe2 N4'
_chemical_formula_weight         929.87
_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             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                 99.2860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1364(2)
_cell_length_b                   17.4597(2)
_cell_length_c                   14.3755(2)
_cell_measurement_reflns_used    18280
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      76.7430
_cell_measurement_theta_min      2.4660
_cell_volume                     4492.44(10)
_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      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_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   -102.00 -77.00   0.50    1.00    -- -104.50  77.00  60.00   50
  2  \w    -56.00 -31.00   0.50    1.00    -- -104.50  77.00  60.00   50
  3  \w    -68.00 -43.00   0.50    1.00    -- -104.50  61.00 -60.00   50
  4  \w    -67.00 -33.00   0.50    1.00    -- -104.50  61.00 -90.00   68
  5  \w    -61.00 -31.00   0.50    1.00    -- -104.50  61.00-150.00   60
  6  \w    -60.00 -35.00   0.50    1.00    -- -104.50  61.00-180.00   50
  7  \w    -39.00  25.00   0.50    0.26    --  -46.67  38.00-180.00  128
  8  \w    -18.00  28.00   0.50    0.26    --  -46.67  19.00  60.00   92
  9  \w    -23.00  16.00   0.50    0.26    --  -46.67  19.00  30.00   78
 10  \w    -23.00   3.00   0.50    0.26    --  -46.67  19.00 -30.00   52
 11  \w    -23.00  26.00   0.50    0.26    --  -46.67  19.00 150.00   98
 12  \w    -44.00  13.00   0.50    0.26    --  -46.67 102.00  59.00  114
 13  \w   -103.00 -69.00   0.50    1.00    -- -104.50 102.00  59.00   68
 14  \w   -110.00 -36.00   0.50    1.00    -- -104.50 125.00  60.00  148
 15  \w   -173.00-148.00   0.50    1.00    -- -104.50 -30.00 150.00   50
 16  \w   -163.00 -95.00   0.50    1.00    -- -104.50 -45.00   0.00  136
 17  \w   -152.00-101.00   0.50    1.00    -- -104.50-102.00 -44.00  102
 18  \w     45.00  75.00   0.50    1.00    --  108.85 -61.00-180.00   60
 19  \w     37.00  74.00   0.50    1.00    --  108.85 -61.00 -60.00   74
 20  \w     45.00  74.00   0.50    1.00    --  108.85 -61.00 -30.00   58
 21  \w     36.00  74.00   0.50    1.00    --  108.85 -61.00   0.00   76
 22  \w     36.00  74.00   0.50    1.00    --  108.85 -61.00 150.00   76
 23  \w     45.00  71.00   0.50    1.00    --  108.85 -61.00 120.00   52
 24  \w     39.00  73.00   0.50    1.00    --  108.85 -61.00  90.00   68
 25  \w     11.00  82.00   0.50    0.26    --   46.67-102.00 -44.00  142
 26  \w     72.00 107.00   0.50    1.00    --  108.85-102.00 -44.00   70
 27  \w     52.00  78.00   0.50    1.00    --  108.85 -94.00 -30.00   52
 28  \w     50.00 100.00   0.50    1.00    --  108.85 -94.00  30.00  100
 29  \w    111.00 178.00   0.50    1.00    --  108.85 102.00  59.00  134
 30  \w    144.00 178.00   0.50    1.00    --  108.85 125.00   0.00   68
 31  \w     80.00 135.00   0.50    1.00    --  108.85 125.00   0.00  110
;
_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      -0.0103357000
_diffrn_orient_matrix_UB_12      0.0838234000
_diffrn_orient_matrix_UB_13      0.0289675000
_diffrn_orient_matrix_UB_21      -0.0603820000
_diffrn_orient_matrix_UB_22      0.0110590000
_diffrn_orient_matrix_UB_23      -0.0874422000
_diffrn_orient_matrix_UB_31      -0.0604646000
_diffrn_orient_matrix_UB_32      -0.0253249000
_diffrn_orient_matrix_UB_33      0.0574334000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36748
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.670
_diffrn_reflns_theta_min         2.469
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38049
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9243
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0545P)^2^+2.2959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8165
_reflns_number_total             9243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03674j2.cif
_cod_data_source_block           tx13928_auto
_cod_depositor_comments
'Adding full bibliography for 7714594--7714596.cif.'
_cod_database_code               7714596
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Fe Cl'
_shelx_estimated_absorpt_t_max   0.291
_shelx_estimated_absorpt_t_min   0.208
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H33B-H29A
 2.2 with sigma of 0.01
 C42-C41 = C42A-C41
 1.54 with sigma of 0.01
 C35A-C19A = C35-C19
 1.54 with sigma of 0.01
 C36-C35A = C36-C35
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C42 \\sim C42A \\sim C41: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
4. Others
 Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C35A)=Sof(H35C)=Sof(H35D)=1-FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C10(H10A,H10B), C30(H30A,H30B), C21(H21A,H21B), C4(H4A,H4B),
 C33(H33A,H33B), C31(H31A,H31B), C32(H32A,H32B), C16(H16A,H16B), C13(H13A,H13B),
  C14(H14A,H14B), C41(H41A,H41B), C41(H41C,H41D), C15(H15A,H15B), C35(H35A,
 H35B), C35A(H35C,H35D)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C27(H27), C17(H17), C3(H3), C12(H12), C25(H25), C26(H26), C8(H8),
 C38(H38), C37(H37)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C7(H7A,H7B,H7C), C40(H40A,H40B,H40C),
 C19(H19A,H19B,H19C), C42(H42A,H42B,H42C), C42A(H42D,H42E,H42F), C19A(H19D,H19E,
 H19F)
;
_shelx_res_checksum              1511
_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 2.278
_oxdiff_exptl_absorpt_empirical_full_min 0.708