Catalytic polymerization of isoprene using an ultrahigh active iron(ii) complex with an ortho-modified 1,10-phenanthroline ligand, access to a thermal plastic rubber
Ge, Jiajia; Chen, Binghui; Gong, Dirong; Polymer Chemistry 15 (2024) 3751–3762; doi:10.1039/D4PY00576G

data_1572385
_publ_section_title
;
 Catalytic polymerization of isoprene using an ultrahigh active iron(ii)
 complex with an ortho-modified 1,10-phenanthroline ligand, access to a
 thermal plastic rubber
;
_journal_issue                   37
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3751
_journal_page_last               3762
_journal_paper_doi               10.1039/D4PY00576G
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C28 H24 Cl2 Fe N4 O2, H2 O, C4 H7 N O'
_chemical_formula_sum            'C32 H33 Cl2 Fe N5 O4'
_chemical_formula_weight         678.38
_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             2023-12-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-25 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                89.362(3)
_cell_angle_beta                 75.855(3)
_cell_angle_gamma                75.243(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9973(4)
_cell_length_b                   10.5261(4)
_cell_length_c                   15.9410(6)
_cell_measurement_reflns_used    9183
_cell_measurement_temperature    100.03(10)
_cell_measurement_theta_max      75.5810
_cell_measurement_theta_min      2.8580
_cell_volume                     1570.66(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (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      100.03(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 0.964
_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    -26.00   0.00   0.50    0.18    --  -52.00  78.00 -48.00   52
  2  \w    -59.00 -31.00   0.50    0.18    --  -52.00  78.00 -48.00   56
  3  \w    -74.00 -47.00   0.50    0.18    --  -38.95  78.00 -48.00   54
  4  \w    -43.00 -18.00   0.50    0.18    --  -38.95  78.00 -48.00   50
  5  \w    -32.00  31.00   0.50    0.18    --  -52.00  30.00 120.00  126
  6  \w     40.00 120.00   0.50    0.18    --   38.95-179.00 -60.00  160
  7  \w     75.00 101.00   0.50    0.71    --  111.82-111.00 -90.00   52
  8  \w     36.00  72.00   0.50    0.71    --  111.82-111.00 -90.00   72
  9  \w     35.00  60.00   0.50    0.71    --  111.82-111.00 -30.00   50
 10  \w     37.00  64.00   0.50    0.71    --  111.82-111.00 -60.00   54
 11  \w     43.00 107.00   0.50    0.71    --  111.82-111.00-120.00  128
 12  \w     81.00 107.00   0.50    0.71    --  111.82-111.00 -30.00   52
 13  \w     83.00 108.00   0.50    0.71    --  111.82-111.00 -60.00   50
 14  \w     35.00 106.00   0.50    0.71    --  111.82-111.00-150.00  142
 15  \w     81.00 106.00   0.50    0.71    --  111.82-111.00  30.00   50
 16  \w     35.00 107.00   0.50    0.71    --  111.82-111.00 120.00  144
 17  \w     36.00  68.00   0.50    0.71    --  111.82 -94.00  60.00   64
 18  \w     36.00  68.00   0.50    0.71    --  111.82-111.00  30.00   64
 19  \w     34.00 103.00   0.50    0.71    --  111.82 -94.00  30.00  138
 20  \w    -17.00  51.00   0.50    0.18    --   38.95 -78.00-173.00  136
 21  \w     47.00  73.00   0.50    0.71    --  111.82 -78.00-173.00   52
 22  \w     38.00 103.00   0.50    0.71    --  111.82 -77.00 -90.00  130
 23  \w     40.00  66.00   0.50    0.71    --  111.82 -61.00 -90.00   52
 24  \w     38.00  65.00   0.50    0.71    --  111.82 -61.00 -30.00   54
 25  \w    -31.00  -6.00   0.50    0.18    --   38.95 -19.00-180.00   50
 26  \w     40.00  65.00   0.50    0.71    --  111.82 -61.00  60.00   50
 27  \w     45.00  99.00   0.50    0.71    --  111.82 -77.00  90.00  108
 28  \w     38.00  63.00   0.50    0.71    --  111.82 -61.00 120.00   50
 29  \w     68.00  94.00   0.50    0.71    --  111.82   0.00  60.00   52
 30  \w     85.00 172.00   0.50    0.71    --  111.82  78.00 -48.00  174
 31  \w    132.00 171.00   0.50    0.71    --  111.82  61.00-150.00   78
 32  \w     85.00 144.00   0.50    0.71    --  111.82  61.00-120.00  118
 33  \w     84.00 109.00   0.50    0.71    --  111.82  61.00-150.00   50
 34  \w     83.00 145.00   0.50    0.71    --  111.82  61.00 -90.00  124
 35  \w    146.00 171.00   0.50    0.71    --  111.82  61.00-120.00   50
 36  \w    134.00 175.00   0.50    0.71    --  111.82  45.00-120.00   82
 37  \w     89.00 121.00   0.50    0.71    --  111.82  45.00-120.00   64
 38  \w      4.00 112.00   0.50    0.18    --   38.95  78.00 -48.00  216
 39  \w    145.00 170.00   0.50    0.71    --  111.82   0.00  60.00   50
 40  \w    126.00 175.00   0.50    0.71    --  111.82  30.00   0.00   98
 41  \w     78.00 121.00   0.50    0.71    --  111.82  30.00   0.00   86
 42  \w     88.00 149.00   0.50    0.71    --  111.82 111.00 -90.00  122
 43  \w     44.00 121.00   0.50    0.18    --   38.95 179.00-180.00  154
 44  \w     57.00  87.00   0.50    0.71    --  111.82 179.00 -90.00   60
 45  \w     52.00  98.00   0.50    0.71    --  111.82 179.00-150.00   92
 46  \w    111.00 146.00   0.50    0.71    --  111.82 179.00 -90.00   70
 47  \w    119.00 144.00   0.50    0.71    --  111.82 179.00-150.00   50
 48  \w     43.00 118.00   0.50    0.18    --   38.95 179.00  90.00  150
 49  \w     45.00  99.00   0.50    0.71    --  111.82 179.00 120.00  108
 50  \w    106.00 142.00   0.50    0.71    --  111.82 179.00 120.00   72
 51  \w    -59.00 -20.00   0.50    0.18    --  -38.95 -78.00-173.00   78
 52  \w   -101.00 -71.00   0.50    0.18    --  -52.00 -78.00-173.00   60
 53  \w   -124.00 -92.00   0.50    0.18    --  -52.00 -94.00-180.00   64
 54  \w   -130.00 -87.00   0.50    0.18    --  -52.00 -94.00 -90.00   86
 55  \w   -131.00 -99.00   0.50    0.18    --  -52.00 -94.00 120.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1411714000
_diffrn_orient_matrix_UB_12      0.0403913000
_diffrn_orient_matrix_UB_13      -0.0301710000
_diffrn_orient_matrix_UB_21      0.0456173000
_diffrn_orient_matrix_UB_22      -0.0981370000
_diffrn_orient_matrix_UB_23      -0.0791106000
_diffrn_orient_matrix_UB_31      -0.0712280000
_diffrn_orient_matrix_UB_32      0.1082242000
_diffrn_orient_matrix_UB_33      -0.0528554000
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17459
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.000
_diffrn_reflns_theta_min         2.863
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0729P)^2^+0.5024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5894
_reflns_number_total             6324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00576g1.cif
_cod_data_source_block           8304-hwh-oet-100k_autored
_cod_depositor_comments
'Adding full bibliography for 1572385--1572387.cif.'
_cod_database_code               1572385
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.595
_shelx_estimated_absorpt_t_min   0.391
_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, All O(H,H) groups
2. Others
 Sof(H01L)=Sof(H01M)=Sof(H01N)=Sof(N1)=Sof(C25)=Sof(H25)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=Sof(H2C)=1-FVAR(1)
 Sof(H01I)=Sof(H01J)=Sof(H01K)=Sof(N016)=Sof(C017)=Sof(H017)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(H1C)=FVAR(1)
3.a Free rotating group:
 O006(H00C,H00D)
3.b Secondary CH2 refined with riding coordinates:
 C00Y(H00A,H00B), C011(H01A,H01B)
3.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P), C00R(H00R), C00S(H00S), C00U(H00U), C00V(H00V), C00X(H00X),
 C00Z(H00Z), C010(H010), C017(H017), C25(H25)
3.d Idealised Me refined as rotating group:
 C012(H01C,H01D,H01E), C013(H01F,H01G,H01H), C014(H01I,H01J,H01K), C015(H01L,
 H01M,H01N), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              14592
_shelx_hkl_checksum              19101
_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 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.607