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_7714595
_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         'C38 H44 Cl Fe N4, Cl4 Fe'
_chemical_formula_sum            'C38 H44 Cl5 Fe2 N4'
_chemical_formula_weight         845.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                86.305(2)
_cell_angle_beta                 79.243(2)
_cell_angle_gamma                89.108(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9529(3)
_cell_length_b                   13.3706(4)
_cell_length_c                   15.0002(3)
_cell_measurement_reflns_used    15763
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      74.8200
_cell_measurement_theta_min      3.0000
_cell_volume                     1957.00(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.961
_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    -13.00  13.00   0.50    0.20    --  -48.81  19.00 150.00   52
  2  \w    -22.00  22.00   0.50    0.20    --  -48.81  19.00  90.00   88
  3  \w    -23.00  23.00   0.50    0.20    --  -48.81  19.00 -30.00   92
  4  \w    -22.00   4.00   0.50    0.20    --  -48.81  19.00 -60.00   52
  5  \w    -17.00  25.00   0.50    0.20    --  -48.81  19.00-180.00   84
  6  \w    -62.00 -34.00   0.50    0.10    -- -103.25  57.00-180.00   56
  7  \w    -60.00 -31.00   0.50    0.10    -- -103.25  57.00 -60.00   58
  8  \w    -64.00 -35.00   0.50    0.10    -- -103.25 147.00 -71.12   58
  9  \w    -79.00 -53.00   0.50    0.10    -- -103.25 125.00-120.00   52
 10  \w    -84.00 -58.00   0.50    0.10    -- -103.25 125.00 -60.00   52
 11  \w   -111.00 -85.00   0.50    0.10    -- -103.25 125.00 -60.00   52
 12  \w   -112.00 -82.00   0.50    0.10    -- -103.25 125.00-120.00   60
 13  \w   -127.00 -83.00   0.50    0.10    -- -103.25 147.00 -71.12   88
 14  \w    -62.00 -37.00   0.50    0.10    -- -103.25  57.00  90.00   50
 15  \w    -77.00  23.00   0.50    0.20    --  -48.81  94.00 176.00  200
 16  \w   -112.00 -60.00   0.50    0.10    -- -103.25 125.00  90.00  104
 17  \w   -112.00 -36.00   0.50    0.10    -- -103.25 125.00 120.00  152
 18  \w    -74.00 -48.00   0.50    0.10    -- -103.25  94.00 176.00   52
 19  \w    120.00 173.00   0.50    0.10    --  101.25  38.00  60.00  106
 20  \w     89.00 172.00   0.50    0.10    --  101.25  57.00  90.00  166
 21  \w     90.00 169.00   0.50    0.10    --  101.25  57.00 120.00  158
 22  \w     95.00 168.00   0.50    0.10    --  101.25  94.00 176.00  146
 23  \w     16.00  41.00   0.50    0.20    --   48.81 -38.00 120.00   50
 24  \w     29.00  69.00   0.50    0.10    --  101.25 -57.00 150.00   80
 25  \w     44.00  94.00   0.50    0.10    --  101.25 -77.00  60.00  100
 26  \w     34.00  68.00   0.50    0.10    --  101.25 -57.00 -90.00   68
 27  \w     36.00  67.00   0.50    0.10    --  101.25 -77.00-120.00   62
 28  \w     71.00 107.00   0.50    0.10    --  101.25 -77.00-120.00   72
 29  \w     33.00  97.00   0.50    0.10    --  101.25-125.00 -90.00  128
 30  \w     43.00 108.00   0.50    0.10    --  101.25-125.00-120.00  130
 31  \w     56.00 105.00   0.50    0.10    --  101.25 -99.00-120.00   98
 32  \w     37.00  70.00   0.50    0.10    --  101.25 -99.00   0.00   66
 33  \w     36.00 104.00   0.50    0.10    --  101.25 -99.00  30.00  136
 34  \w     56.00  82.00   0.50    0.10    --  101.25 -94.00  65.00   52
 35  \w    -19.00  43.00   0.50    0.20    --   48.81 -94.00  65.00  124
 36  \w   -119.00 -47.00   0.50    0.20    --  -48.81 -38.00  30.00  144
 37  \w   -131.00-105.00   0.50    0.10    -- -103.25 -19.00 -90.00   52
 38  \w   -174.00-145.00   0.50    0.10    -- -103.25 -19.00-150.00   58
 39  \w   -171.00-145.00   0.50    0.10    -- -103.25 -19.00 -90.00   52
 40  \w   -174.00-119.00   0.50    0.10    -- -103.25 -38.00   0.00  110
 41  \w   -137.00 -85.00   0.50    0.10    -- -103.25 -94.00  65.00  104
;
_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      -0.0790407000
_diffrn_orient_matrix_UB_12      -0.0913661000
_diffrn_orient_matrix_UB_13      0.0505068000
_diffrn_orient_matrix_UB_21      0.0479300000
_diffrn_orient_matrix_UB_22      -0.0619538000
_diffrn_orient_matrix_UB_23      -0.0832915000
_diffrn_orient_matrix_UB_31      0.1275883000
_diffrn_orient_matrix_UB_32      -0.0338421000
_diffrn_orient_matrix_UB_33      0.0385124000
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26005
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.034
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (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    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00093(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0547P)^2^+1.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7204
_reflns_number_total             7859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03674j2.cif
_cod_data_source_block           tx13230_auto
_cod_depositor_comments
'Adding full bibliography for 7714594--7714596.cif.'
_cod_database_code               7714595
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H29B-H25A
 2.2 with sigma of 0.01
 H10B-H6A
 2.2 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21),
 C22(H22), C33(H33), C34(H34), C35(H35)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              50485
_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 1.497
_oxdiff_exptl_absorpt_empirical_full_min 0.696