Achieving isopropenyl-enriched polyisoprene: unraveling the role of bidentate <i>vs.</i> tridentate iron precatalysts through ligand framework design.
Sohail, Sunny; Ma, Yanping; Mahmood, Qaiser; Hu, Zexu; Wang, Yizhou; Liang, Tongling; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19325–19336; doi:10.1039/d4dt02659d

data_7717311
_publ_section_title
;
 Achieving isopropenyl-enriched polyisoprene: unraveling the role of
 bidentate <i>vs.</i> tridentate iron precatalysts through ligand
 framework design.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19325
_journal_page_last               19336
_journal_paper_doi               10.1039/d4dt02659d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C45 H45 Fe N9), Cl7 Fe2, 2(C H2 Cl2), 2(Cl)'
_chemical_formula_sum            'C92 H94 Cl13 Fe4 N18'
_chemical_formula_weight         2136.10
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-19 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                89.086(2)
_cell_angle_beta                 70.721(2)
_cell_angle_gamma                85.196(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3257(3)
_cell_length_b                   13.4312(3)
_cell_length_c                   15.1114(3)
_cell_measurement_reflns_used    15437
_cell_measurement_temperature    170.0(6)
_cell_measurement_theta_max      75.2150
_cell_measurement_theta_min      3.2710
_cell_volume                     2352.91(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      170.0(6)
_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 0.962
_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   -116.00 -44.00   0.50    0.82    --  -46.42 -48.00 -37.00  144
  2  \w    -43.00  -9.00   0.50    0.82    --  -46.42  48.00 109.00   68
  3  \w     33.00 118.00   0.50    0.82    --   46.42  48.00 109.00  170
  4  \w    -10.00  57.00   0.50    0.82    --   46.42 -48.00 -37.00  134
  5  \w   -171.00 -90.00   0.50    6.00    -- -104.50 -48.00 -37.00  162
  6  \w     91.00 173.00   0.50    6.00    --  105.35  48.00 109.00  164
  7  \w     -6.00  27.00   0.50    0.82    --  -46.42  48.00 109.00   66
  8  \w    -61.00 -34.00   0.50    0.82    --  -46.42 -41.00 179.78   54
  9  \w    -19.00  27.00   0.50    0.82    --  -46.42  19.00  60.00   92
 10  \w    -39.00  -4.00   0.50    0.82    --  -46.42  38.00-180.00   70
 11  \w      1.00  26.00   0.50    0.82    --  -46.42  38.00-180.00   50
 12  \w     52.00  80.00   0.50    0.82    --   46.42-125.00-180.00   56
 13  \w     20.00  88.00   0.50    0.82    --   46.42-125.00 -30.00  136
 14  \w    -12.00  30.00   0.50    0.82    --   46.42 -19.00-180.00   84
 15  \w    -63.00 -37.00   0.50    6.00    -- -104.50  61.00-150.00   52
 16  \w   -108.00 -83.00   0.50    6.00    -- -104.50 125.00   0.00   50
 17  \w   -110.00 -76.00   0.50    6.00    -- -104.50 125.00-120.00   68
 18  \w    -69.00 -43.00   0.50    6.00    -- -104.50 125.00-120.00   52
 19  \w   -174.00-102.00   0.50    6.00    -- -104.50 -64.00 -61.34  144
 20  \w    -67.00 -31.00   0.50    6.00    -- -104.50  61.00 -90.00   72
 21  \w   -109.00 -82.00   0.50    6.00    -- -104.50 125.00 -90.00   54
 22  \w    -67.00 -37.00   0.50    6.00    -- -104.50 140.00   8.66   60
 23  \w   -122.00 -95.00   0.50    6.00    -- -104.50 140.00   8.66   54
 24  \w   -123.00 -93.00   0.50    6.00    -- -104.50 140.00-157.52   60
 25  \w    -73.00 -38.00   0.50    6.00    -- -104.50 142.00  98.53   70
 26  \w    -92.00 -66.00   0.50    6.00    -- -104.50  77.00  30.00   52
 27  \w   -173.00-118.00   0.50    6.00    -- -104.50 -30.00-150.00  110
 28  \w    -65.00 -39.00   0.50    6.00    -- -104.50 125.00 -90.00   52
 29  \w   -122.00 -90.00   0.50    6.00    -- -104.50 142.00  98.53   64
 30  \w   -111.00 -37.00   0.50    6.00    -- -104.50 125.00 120.00  148
 31  \w    -62.00 -36.00   0.50    6.00    -- -104.50 125.00   0.00   52
 32  \w   -154.00-127.00   0.50    6.00    -- -104.50 -61.00  16.06   54
 33  \w    -65.00 -31.00   0.50    6.00    -- -104.50  61.00 150.00   68
 34  \w    137.00 162.00   0.50    6.00    --  105.35  30.00-120.00   50
 35  \w    103.00 134.00   0.50    6.00    --  105.35  30.00-120.00   62
 36  \w     33.00  99.00   0.50    6.00    --  105.35 -94.00 -30.00  132
 37  \w    115.00 177.00   0.50    6.00    --  105.35  30.00  30.00  124
 38  \w     41.00 102.00   0.50    6.00    --  105.35-125.00-120.00  122
 39  \w     35.00 103.00   0.50    6.00    --  105.35 -94.00  30.00  136
 40  \w     77.00 104.00   0.50    6.00    --  105.35 -77.00  60.00   54
 41  \w     34.00  71.00   0.50    6.00    --  105.35 -61.00-120.00   74
 42  \w     43.00  80.00   0.50    6.00    --  105.35 -77.00  90.00   74
 43  \w     33.00  68.00   0.50    6.00    --  105.35 -77.00  60.00   70
 44  \w     73.00 106.00   0.50    6.00    --  105.35 -77.00-120.00   66
 45  \w     35.00  66.00   0.50    6.00    --  105.35 -77.00-120.00   62
 46  \w     38.00  83.00   0.50    6.00    --  105.35 -77.00 -30.00   90
 47  \w     99.00 177.00   0.50    6.00    --  105.35  45.00   0.00  156
 48  \w     64.00 104.00   0.50    6.00    --  105.35 -94.00  60.00   80
 49  \w     34.00 109.00   0.50    6.00    --  105.35 -77.00 150.00  150
;
_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      0.0851371000
_diffrn_orient_matrix_UB_12      0.0139762000
_diffrn_orient_matrix_UB_13      0.0530776000
_diffrn_orient_matrix_UB_21      -0.0147253000
_diffrn_orient_matrix_UB_22      -0.1070314000
_diffrn_orient_matrix_UB_23      0.0376961000
_diffrn_orient_matrix_UB_31      0.1009474000
_diffrn_orient_matrix_UB_32      -0.0400010000
_diffrn_orient_matrix_UB_33      -0.0861876000
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            32567
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.529
_diffrn_reflns_theta_min         3.098
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.694
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.341
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         9496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1334P)^2^+1.5046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1864
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8162
_reflns_number_total             9496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02659d2.cif
_cod_data_source_block           tx16045c_auto
_cod_depositor_comments
'Adding full bibliography for 7717310--7717311.cif.'
_cod_original_cell_volume        2352.91(9)
_cod_database_code               7717311
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNClFe
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Riding coordinates:
 N3(H3), N6(H6), N9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C23(H23A,H23B), C6(H6A,H6B), C22(H22A,H22B),
 C21(H21A,H21B), C38(H38A,H38B), C36(H36A,H36B), C46(H46A,H46B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C31(H31), C26(H26), C16(H16), C41(H41), C2(H2), C30(H30), C3(H3A),
 C45(H45), C15(H15), C11(H11), C42(H42), C12(H12), C17(H17), C13(H13), C32(H32),
  C29(H29), C27(H27), C14(H14), C44(H44), C18(H18), C33(H33), C28(H28), C43(H43)
;
_shelx_res_checksum              27256
_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 2.019
_oxdiff_exptl_absorpt_empirical_full_min 0.675