The synthesis, characterisation and application of iron(iii)-acetate complexes for cyclic carbonate formation and the polymerisation of lactide.
Driscoll, Oliver J.; Hafford-Tear, Claudia H; McKeown, Paul; Stewart, Jack A.; Kociok-Köhn, Gabriele; Mahon, Mary F.; Jones, Matthew D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15049–15058; doi:10.1039/c9dt03327k

data_7701057
_publ_section_title
;
 The synthesis, characterisation and application of iron(iii)-acetate
 complexes for cyclic carbonate formation and the polymerisation of
 lactide.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15049
_journal_page_last               15058
_journal_paper_doi               10.1039/c9dt03327k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H41.4 Fe N2 O5.3'
_chemical_formula_sum            'C30 H42.4 Fe N2 O5.3'
_chemical_formula_weight         571.71
_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'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-15 deposited with the CCDC.    2019-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.24770(10)
_cell_length_b                   10.24770(10)
_cell_length_c                   28.1421(5)
_cell_measurement_reflns_used    19222
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8200
_cell_measurement_theta_min      4.5800
_cell_volume                     2955.35(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            79340
_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         73.308
_diffrn_reflns_theta_min         4.592
_exptl_absorpt_coefficient_mu    4.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       plank
_exptl_crystal_F_000             1219
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 992 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0670P)^2^+0.2461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2767
_reflns_number_total             2968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03327k2.cif
_cod_data_source_block           Fe(6RR)(OAc)
_cod_depositor_comments
'Adding full bibliography for 7701052--7701059.cif.'
_cod_original_cell_volume        2955.35(8)
_cod_original_formula_sum        'C30 H42.40 Fe N2 O5.30'
_cod_database_code               7701057
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 O2-C14 \\sim O2-C14A
 with sigma of 0.005
 O3-C14 \\sim O15A-C14A
 with sigma of 0.005
 C15A-C14A \\sim C15-C14
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C14B \\sim C15B \\sim O3 \\sim C14 \\sim C15 \\sim O15A \\sim C14A \\sim C15A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C14B(0.35) H14A(0.35) H14B(0.35) C15B(0.35) H15A(0.35) H15B(0.35)
 H15C(0.35) O3(0.35) C14(0.35) C15(0.35) H15D(0.35) H15E(0.35) H15F(0.35)
 O15A(0.3) C14A(0.3) C15A(0.3) H15G(0.3) H15H(0.3) H15I(0.3)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C14B(H14A,H14B)
5.c Me refined with riding coordinates:
 C12(H12A,H12B,H12C)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11)
5.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15B(H15A,H15B,H15C), C15(H15D,H15E,H15F), C15A(H15G,
 H15H,H15I)
;
_olex2_submission_special_instructions 'No special instructions were received'