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_7717310
_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         'C13 H21 Cl2 Fe N3 O0.5'
_chemical_formula_sum            'C13 H20 Cl2 Fe N3.5 O0.12'
_chemical_formula_weight         354.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90.579(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8062(4)
_cell_length_b                   10.1238(3)
_cell_length_c                   21.3450(7)
_cell_measurement_reflns_used    5249
_cell_measurement_temperature    170.0(4)
_cell_measurement_theta_max      74.3140
_cell_measurement_theta_min      4.0940
_cell_volume                     3199.35(17)
_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(4)
_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 0.957
_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    0.47    --   46.69 -19.00-120.00   52
  2  \w     33.00 105.00   0.50    1.88    --  105.35 -77.00 -30.00  144
  3  \w     49.00  74.00   0.50    1.88    --  105.35 -61.00   0.00   50
  4  \w    -10.00  30.00   0.50    0.47    --   46.69 -19.00  60.00   80
  5  \w     95.00 137.00   0.50    1.88    --  105.35  45.00  30.00   84
  6  \w     93.00 157.00   0.50    1.88    --  105.35  97.00  77.00  128
  7  \w     91.00 161.00   0.50    1.88    --  105.35  45.00   0.00  140
  8  \w     46.00  71.00   0.50    1.88    --  105.35 -97.00 -29.00   50
  9  \w    -13.00  68.00   0.50    0.47    --   46.69 -97.00 -29.00  162
 10  \w    -14.00  26.00   0.50    0.47    --  -46.69  19.00-120.00   80
 11  \w    -65.00 -34.00   0.50    1.88    -- -104.50  61.00-180.00   62
 12  \w    -68.00 -43.00   0.50    1.88    -- -104.50  61.00-150.00   50
 13  \w    -58.00 -32.00   0.50    1.88    -- -104.50  61.00 -60.00   52
 14  \w    -10.00  18.00   0.50    0.47    --  -46.69  19.00  90.00   56
 15  \w    -73.00 -30.00   0.50    0.47    --  -46.69  97.00  77.00   86
 16  \w   -104.00 -65.00   0.50    1.88    -- -104.50 125.00 120.00   78
 17  \w   -105.00 -45.00   0.50    1.88    -- -104.50 125.00  90.00  120
 18  \w    -80.00 -33.00   0.50    1.88    -- -104.50  97.00  77.00   94
 19  \w   -107.00 -34.00   0.50    1.88    -- -104.50 125.00-180.00  146
 20  \w   -174.00-103.00   0.50    1.88    -- -104.50 -30.00-180.00  142
 21  \w   -154.00-129.00   0.50    1.88    -- -104.50 -97.00 -29.00   50
;
_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      0.0191178000
_diffrn_orient_matrix_UB_12      0.0718037000
_diffrn_orient_matrix_UB_13      0.0623552000
_diffrn_orient_matrix_UB_21      0.0389496000
_diffrn_orient_matrix_UB_22      -0.1286828000
_diffrn_orient_matrix_UB_23      0.0278816000
_diffrn_orient_matrix_UB_31      0.0944690000
_diffrn_orient_matrix_UB_32      0.0386847000
_diffrn_orient_matrix_UB_33      -0.0232732000
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9671
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.958
_diffrn_reflns_theta_min         4.143
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36501
_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    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0875P)^2^+4.5422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2886
_reflns_number_total             3203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02659d2.cif
_cod_data_source_block           tx16240_auto
_cod_depositor_comments
'Adding full bibliography for 7717310--7717311.cif.'
_cod_original_formula_sum        'C13 H20 Cl2 Fe N3.50 O0.12'
_cod_database_code               7717310
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNFeCl
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C10(H10A,H10B), C7(H7A,H7B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), C2(H2A)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              27853
_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 2.946
_oxdiff_exptl_absorpt_empirical_full_min 0.664