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_7246353
_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         'C25 H30 Fe K N2 O8'
_chemical_formula_sum            'C25 H30 Fe K N2 O8'
_chemical_formula_weight         581.46
_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   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                66.668(6)
_cell_angle_beta                 83.456(5)
_cell_angle_gamma                83.448(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8770(6)
_cell_length_b                   12.1262(9)
_cell_length_c                   12.1406(8)
_cell_measurement_reflns_used    5448
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.0090
_cell_measurement_theta_min      3.9390
_cell_volume                     1322.68(17)
_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_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -20.00  15.00   1.00    7.50    --  -41.27  37.00 -90.00   35
  2  \w     -2.00  24.00   1.00    7.50    --  -41.27  19.00-180.00   26
  3  \w    -11.00  15.00   1.00    7.50    --  -41.27  37.00-120.00   26
  4  \w    -43.00  24.00   1.00    7.50    --  -41.27  57.00 120.00   67
  5  \w    -18.00  26.00   1.00    7.50    --  -41.27  37.00-150.00   44
  6  \w     48.00  95.00   1.00    7.50    --   41.27-125.00   0.00   47
  7  \w    106.00 168.00   1.00   30.00    --  111.00  77.00  90.00   62
  8  \w    109.00 178.00   1.00   30.00    --  111.00  77.00-150.00   69
  9  \w    116.00 169.00   1.00   30.00    --  111.00  77.00 120.00   53
 10  \w     33.00  84.00   1.00   30.00    --  111.00 -94.00  30.00   51
 11  \w     51.00 107.00   1.00   30.00    --  111.00 -94.00  60.00   56
 12  \w     60.00  90.00   1.00   30.00    --  111.00 -61.00 150.00   30
 13  \w     44.00  70.00   1.00   30.00    --  111.00 -45.00-180.00   26
 14  \w    134.00 164.00   1.00   30.00    --  111.00 125.00   0.00   30
 15  \w     73.00 101.00   1.00   30.00    --  111.00 -94.00-150.00   28
 16  \w     51.00  91.00   1.00   30.00    --  111.00 -61.00 120.00   40
 17  \w     60.00 104.00   1.00   30.00    --  111.00 -94.00  90.00   44
 18  \w     99.00 125.00   1.00   30.00    --  111.00 125.00   0.00   26
 19  \w    103.00 163.00   1.00   30.00    --  111.00  77.00-180.00   60
 20  \w     96.00 123.00   1.00   30.00    --  111.00-138.00-136.16   27
 21  \w     45.00  72.00   1.00   30.00    --  111.00-138.00-136.16   27
 22  \w     -5.00  24.00   1.00    7.50    --  -41.27  19.00 -60.00   29
 23  \w    -21.00   4.00   1.00    7.50    --  -41.27  37.00  30.00   25
 24  \w      2.00  28.00   1.00    7.50    --  -41.27  19.00-180.00   26
 25  \w    -17.00  20.00   1.00    7.50    --  -41.27  37.00  60.00   37
 26  \w    -15.00  26.00   1.00    7.50    --  -41.27  37.00 -30.00   41
 27  \w     49.00  88.00   1.00    7.50    --   41.27-125.00 150.00   39
 28  \w     48.00  74.00   1.00    7.50    --   41.27-125.00 -60.00   26
 29  \w     65.00 105.00   1.00   30.00    --  111.00 -94.00 -30.00   40
 30  \w     59.00  89.00   1.00   30.00    --  111.00 -61.00  60.00   30
 31  \w     72.00  98.00   1.00   30.00    --  111.00  15.00 -30.00   26
 32  \w    145.00 172.00   1.00   30.00    --  111.00  45.00-180.00   27
 33  \w     83.00 124.00   1.00   30.00    --  111.00  61.00  90.00   41
 34  \w     31.00  71.00   1.00   30.00    --  111.00 -94.00   0.00   40
 35  \w     55.00 112.00   1.00   30.00    --  111.00-125.00 -60.00   57
 36  \w    110.00 158.00   1.00   30.00    --  111.00  77.00 -30.00   48
 37  \w     78.00 106.00   1.00   30.00    --  111.00 -94.00 -90.00   28
 38  \w     41.00  68.00   1.00   30.00    --  111.00 -45.00 -90.00   27
 39  \w     97.00 165.00   1.00   30.00    --  111.00 125.00  30.00   68
 40  \w     42.00  68.00   1.00   30.00    --  111.00 -61.00 -90.00   26
 41  \w     79.00 107.00   1.00   30.00    --  111.00 -94.00   0.00   28
 42  \w     39.00  85.00   1.00   30.00    --  111.00-125.00-180.00   46
 43  \w     40.00  65.00   1.00   30.00    --  111.00 -45.00   0.00   25
 44  \w     99.00 145.00   1.00   30.00    --  111.00  15.00 -30.00   46
 45  \w     75.00 107.00   1.00   30.00    --  111.00 -94.00 -60.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0387555000
_diffrn_orient_matrix_UB_12      -0.0843776000
_diffrn_orient_matrix_UB_13      0.1272482000
_diffrn_orient_matrix_UB_21      0.0540493000
_diffrn_orient_matrix_UB_22      0.1062835000
_diffrn_orient_matrix_UB_23      0.0165663000
_diffrn_orient_matrix_UB_31      -0.1427104000
_diffrn_orient_matrix_UB_32      0.0289129000
_diffrn_orient_matrix_UB_33      0.0523523000
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14130
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.469
_diffrn_reflns_theta_min         3.977
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0522P)^2^+0.2281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4834
_reflns_number_total             5480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2gc04580j2.cif
_cod_data_source_block           008rwfk22
_cod_depositor_comments
'Adding full bibliography for 7246353--7246354.cif.'
_cod_original_cell_volume        1322.68(16)
_cod_database_code               7246353
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H33Fe1K1N2O8
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.436
_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:
 C9(H9A,H9B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C16(H16), C18(H18), C5(H5), C3(H3), C17(H17), C4(H4)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C1(H1A,H1B,
 H1C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C)
;
_ins_header
;
TITL 008RWFK22 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.877000  12.126201  12.140591  66.6684  83.4557  83.4475
ZERR    4.00   0.000615   0.000856   0.000759   0.0064   0.0051   0.0055
LATT  1
SFAC C H N O K Fe
UNIT 100.00 132.00 8.00 32.00 4.00 4.00
TREF
HKLF 4
END
;
_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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.841