A highly active, thermally robust iron(iii)/potassium(i) heterodinuclear catalyst for bio-derived epoxide/anhydride ring-opening copolymerizations
Diment, Wilfred T.; Rosetto, Gloria; Ezaz-Nikpay, Noura; Kerr, Ryan W. F.; Williams, Charlotte K.; Green Chemistry 25 (2023) 2262–2267; doi:10.1039/D2GC04580J

data_7246354
_publ_section_title
;
 A highly active, thermally robust iron(iii)/potassium(i) heterodinuclear
 catalyst for bio-derived epoxide/anhydride ring-opening copolymerizations
;
_journal_issue                   6
_journal_name_full               'Green Chemistry'
_journal_page_first              2262
_journal_page_last               2267
_journal_paper_doi               10.1039/D2GC04580J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C23 H27 Fe N2 O6'
_chemical_formula_sum            'C23 H27 Fe N2 O6'
_chemical_formula_weight         483.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.797(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0238(2)
_cell_length_b                   12.9234(2)
_cell_length_c                   19.4802(3)
_cell_measurement_reflns_used    22679
_cell_measurement_temperature    150.0(5)
_cell_measurement_theta_max      76.3170
_cell_measurement_theta_min      4.0710
_cell_volume                     2255.78(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 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
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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     -5.00  29.00   1.00    2.00    --  -41.15  19.00 -90.00   34
  2  \w     -1.00  26.00   1.00    2.00    --  -41.15  19.00-180.00   27
  3  \w     -5.00  28.00   1.00    2.00    --  -41.15  19.00-150.00   33
  4  \w    -43.00 -17.00   1.00    2.00    --  -41.15  57.00   0.00   26
  5  \w     -3.00  32.00   1.00    2.00    --  -41.15  19.00 150.00   35
  6  \w     -5.00  30.00   1.00    2.00    --  -41.15  19.00-120.00   35
  7  \w     -4.00  34.00   1.00    2.00    --  -41.15  19.00 -60.00   38
  8  \w     59.00  90.00   1.00    2.00    --   41.15-125.00-120.00   31
  9  \w     44.00  71.00   1.00    6.00    --  111.00 -45.00  30.00   27
 10  \w     45.00  88.00   1.00    6.00    --  111.00 -61.00 -60.00   43
 11  \w     99.00 137.00   1.00    6.00    --  111.00  30.00 -30.00   38
 12  \w     74.00 112.00   1.00    6.00    --  111.00-125.00 -60.00   38
 13  \w     41.00  67.00   1.00    6.00    --  111.00 -45.00  90.00   26
 14  \w     42.00  72.00   1.00    6.00    --  111.00 -45.00 -60.00   30
 15  \w     39.00  79.00   1.00    6.00    --  111.00 -77.00  30.00   40
 16  \w     45.00  71.00   1.00    6.00    --  111.00 -45.00-120.00   26
 17  \w     49.00 102.00   1.00    6.00    --  111.00-125.00 -90.00   53
 18  \w     52.00  77.00   1.00    6.00    --  111.00 -61.00 -90.00   25
 19  \w     88.00 158.00   1.00    6.00    --  111.00  30.00-180.00   70
 20  \w     40.00  72.00   1.00    6.00    --  111.00 -45.00  60.00   32
 21  \w     84.00 116.00   1.00    6.00    --  111.00 -77.00  30.00   32
 22  \w     60.00  87.00   1.00    6.00    --  111.00 -61.00-120.00   27
 23  \w     41.00  66.00   1.00    6.00    --  111.00 -61.00 150.00   25
 24  \w     44.00  72.00   1.00    6.00    --  111.00 -45.00-150.00   28
 25  \w    111.00 161.00   1.00    6.00    --  111.00  77.00-180.00   50
 26  \w     67.00  92.00   1.00    6.00    --  111.00 -61.00  60.00   25
 27  \w     43.00  83.00   1.00    6.00    --  111.00 -61.00  30.00   40
 28  \w    -43.00  23.00   1.00    2.00    --  -41.15  57.00  30.00   66
 29  \w    -20.00  18.00   1.00    2.00    --  -41.15  37.00-180.00   38
 30  \w    -20.00  13.00   1.00    2.00    --  -41.15  37.00 120.00   33
 31  \w     37.00  96.00   1.00    2.00    --   41.15-125.00 -90.00   59
 32  \w     41.00  85.00   1.00    2.00    --   41.15-125.00  90.00   44
 33  \w     42.00  86.00   1.00    6.00    --  111.00-125.00-150.00   44
 34  \w    105.00 159.00   1.00    6.00    --  111.00  77.00  30.00   54
 35  \w     44.00  71.00   1.00    6.00    --  111.00-133.00  25.25   27
 36  \w     39.00 111.00   1.00    6.00    --  111.00-125.00  60.00   72
 37  \w     57.00 106.00   1.00    6.00    --  111.00 -94.00 150.00   49
 38  \w    109.00 152.00   1.00    6.00    --  111.00 125.00 120.00   43
 39  \w     75.00 111.00   1.00    6.00    --  111.00-125.00-180.00   36
 40  \w     79.00 106.00   1.00    6.00    --  111.00 -94.00  60.00   27
 41  \w    110.00 153.00   1.00    6.00    --  111.00  77.00-150.00   43
 42  \w    111.00 138.00   1.00    6.00    --  111.00  77.00  90.00   27
 43  \w     82.00 107.00   1.00    6.00    --  111.00 -94.00 -90.00   25
 44  \w    151.00 178.00   1.00    6.00    --  111.00  30.00 -60.00   27
 45  \w     88.00 135.00   1.00    6.00    --  111.00  30.00 -60.00   47
 46  \w     41.00  68.00   1.00    6.00    --  111.00 -45.00 150.00   27
 47  \w     86.00 112.00   1.00    6.00    --  111.00-125.00  90.00   26
 48  \w     80.00 107.00   1.00    6.00    --  111.00 -94.00 -60.00   27
 49  \w     92.00 118.00   1.00    6.00    --  111.00-133.00  25.25   26
 50  \w     80.00 107.00   1.00    6.00    --  111.00-105.00-119.05   27
 51  \w     80.00 107.00   1.00    6.00    --  111.00 -94.00  90.00   27
 52  \w    104.00 156.00   1.00    6.00    --  111.00 125.00-150.00   52
 53  \w     72.00 112.00   1.00    6.00    --  111.00-125.00-120.00   40
 54  \w     77.00 106.00   1.00    6.00    --  111.00 -94.00   0.00   29
 55  \w     35.00  63.00   1.00    6.00    --  111.00-105.00-119.05   28
 56  \w    -75.00 -12.00   1.00    2.00    --  -41.15 -19.00  30.00   63
 57  \w     -3.00  36.00   1.00    2.00    --  -41.15  19.00   0.00   39
 58  \w     -4.00  26.00   1.00    2.00    --  -41.15  19.00  90.00   30
 59  \w     16.00  86.00   1.00    2.00    --   41.15  57.00 150.00   70
 60  \w      8.00  33.00   1.00    2.00    --   41.15  83.00 128.92   25
 61  \w     15.00  42.00   1.00    2.00    --   41.15  79.00  42.07   27
 62  \w     10.00  36.00   1.00    2.00    --   41.15  75.00 104.97   26
 63  \w     55.00  82.00   1.00    2.00    --   41.15  57.00  30.00   27
 64  \w      8.00  33.00   1.00    2.00    --   41.15  83.00 -40.48   25
 65  \w     10.00  38.00   1.00    2.00    --   41.15  76.00-147.14   28
 66  \w     17.00 105.00   1.00    2.00    --   41.15  57.00-150.00   88
 67  \w     23.00  88.00   1.00    2.00    --   41.15  57.00 -60.00   65
 68  \w     12.00  42.00   1.00    2.00    --   41.15  80.00-102.66   30
 69  \w     15.00  46.00   1.00    2.00    --   41.15  57.00  30.00   31
 70  \w     10.00  37.00   1.00    2.00    --   41.15  81.00  -7.03   27
 71  \w    153.00 178.00   1.00    6.00    --  111.00  63.00 -72.84   25
 72  \w     83.00 109.00   1.00    6.00    --  111.00  63.00 -72.84   26
 73  \w     85.00 112.00   1.00    6.00    --  111.00  55.00-156.84   27
 74  \w     83.00 110.00   1.00    6.00    --  111.00  64.00-107.22   27
 75  \w    147.00 174.00   1.00    6.00    --  111.00  65.00  39.44   27
 76  \w     83.00 109.00   1.00    6.00    --  111.00  61.00 -78.21   26
 77  \w    132.00 159.00   1.00    6.00    --  111.00  71.00 -36.07   27
 78  \w     82.00 109.00   1.00    6.00    --  111.00  66.00 130.96   27
 79  \w    117.00 144.00   1.00    6.00    --  111.00  66.00 130.96   27
 80  \w     82.00 109.00   1.00    6.00    --  111.00  67.00 154.32   27
 81  \w     84.00 110.00   1.00    6.00    --  111.00  63.00-175.39   26
 82  \w    153.00 178.00   1.00    6.00    --  111.00  63.00-175.39   25
 83  \w     83.00 110.00   1.00    6.00    --  111.00  65.00 119.79   27
 84  \w     81.00 107.00   1.00    6.00    --  111.00  71.00  90.93   26
 85  \w     83.00 109.00   1.00    6.00    --  111.00  65.00  39.44   26
 86  \w     81.00 107.00   1.00    6.00    --  111.00  70.00 -67.01   26
 87  \w     82.00 164.00   1.00    6.00    --  111.00  66.00 -19.22   82
 88  \w     86.00 129.00   1.00    6.00    --  111.00  50.00 -23.98   43
 89  \w    148.00 175.00   1.00    6.00    --  111.00  62.00-109.48   27
 90  \w     83.00 120.00   1.00    6.00    --  111.00  61.00   0.00   37
 91  \w     83.00 130.00   1.00    6.00    --  111.00  61.00-120.00   47
 92  \w     82.00 162.00   1.00    6.00    --  111.00  69.00  64.41   80
 93  \w     83.00 129.00   1.00    6.00    --  111.00  61.00  60.00   46
 94  \w    132.00 159.00   1.00    6.00    --  111.00  67.00 108.59   27
 95  \w     84.00 168.00   1.00    6.00    --  111.00  60.00  17.06   84
 96  \w     83.00 178.00   1.00    6.00    --  111.00  61.00  90.00   95
 97  \w     84.00 111.00   1.00    6.00    --  111.00  61.00 -30.00   27
 98  \w     83.00 110.00   1.00    6.00    --  111.00  61.00 150.00   27
 99  \w     84.00 111.00   1.00    6.00    --  111.00  64.00  47.84   27
100  \w     82.00 108.00   1.00    6.00    --  111.00  67.00 108.59   26
101  \w     83.00 110.00   1.00    6.00    --  111.00  61.00 -47.51   27
102  \w     83.00 110.00   1.00    6.00    --  111.00  61.00-180.00   27
103  \w     83.00 110.00   1.00    6.00    --  111.00  61.00-150.00   27
104  \w     83.00 109.00   1.00    6.00    --  111.00  61.00 -90.00   26
105  \w    140.00 171.00   1.00    6.00    --  111.00  61.00 -90.00   31
106  \w     83.00 110.00   1.00    6.00    --  111.00  61.00  30.00   27
107  \w     82.00 116.00   1.00    6.00    --  111.00  69.00-144.81   34
108  \w     84.00 109.00   1.00    6.00    --  111.00  64.00  18.05   25
109  \w    138.00 163.00   1.00    6.00    --  111.00  55.00-156.84   25
110  \w     83.00 109.00   1.00    6.00    --  111.00  62.00-109.48   26
111  \w     81.00 107.00   1.00    6.00    --  111.00  71.00 -36.07   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52275
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.286
_diffrn_reflns_theta_min         4.114
_exptl_absorpt_coefficient_mu    5.720
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0438P)^2^+0.7379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4128
_reflns_number_total             4720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2gc04580j2.cif
_cod_data_source_block           013rwfk22
_cod_depositor_comments
'Adding full bibliography for 7246353--7246354.cif.'
_cod_database_code               7246354
_shelx_shelxl_version_number     2018/3
_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:
 C13(H13A,H13B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C8(H8), C5(H5), C3(H3), C4(H4), C18(H18), C17(H17)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C1(H1A,H1B,H1C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C)
;
_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
;