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_1572387
_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_absolute_configuration ad
_chemical_formula_moiety         'C16 H17 Cl2 Fe N3'
_chemical_formula_sum            'C16 H17 Cl2 Fe N3'
_chemical_formula_weight         378.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.8158(2)
_cell_length_b                   10.8158(2)
_cell_length_c                   27.7228(9)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      74.60
_cell_measurement_theta_min      4.39
_cell_volume                     3243.06(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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_temperature      150.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32532
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.690
_diffrn_reflns_theta_min         4.388
_diffrn_source_current           0.95
_diffrn_source_power             0.0475
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.471
_exptl_absorpt_correction_T_max  0.0872
_exptl_absorpt_correction_T_min  0.0068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1576 before and 0.0969 after correction.
The Ratio of minimum to maximum transmission is 0.0780.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1102 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.040(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0823P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                2994
_reflns_number_total             3321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00576g1.cif
_cod_data_source_block           cu_1122_8_0m
_cod_depositor_comments
'Adding full bibliography for 1572385--1572387.cif.'
_cod_original_cell_volume        3243.06(16)
_cod_database_code               1572387
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.421
_shelx_estimated_absorpt_t_min   0.229
_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.a Secondary CH2 refined with riding coordinates:
 C00A(H00A,H00B), C00C(H00D,H00E)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00C), C00D(H00F), C00E(H00G), C00G(H00H), C00I(H00I), C00J(H00J),
 C00M(H00Q)
2.c Idealised Me refined as rotating group:
 C00K(H00K,H00L,H00M), C00L(H00N,H00O,H00P)
;
_shelx_res_checksum              14751
_shelx_hkl_checksum              98095
_olex2_submission_special_instructions 'No special instructions were received'