An [FeIII8] molecular oxyhydroxide
Brechin, Euan K.; Cutler, Daniel J.; Coletta, Marco; Singh, Mukesh; Tsanai, Angelos B.; McCormick McPherson, Laura J.; Coles, Simon; Schnack, Jürgen; Dalton Transactions  (2022) –; doi:10.1039/D2DT01477G

data_7710287
_publ_section_title
;
 An [FeIII8] molecular oxyhydroxide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01477G
_journal_year                    2022
_chemical_formula_moiety
'4(Br), C72 H90 Br2 Fe8 N12 O24, 2(H2 O), 2(C6 H7 N O), 0.5(O)'
_chemical_formula_sum            'C84 H109 Br6 Fe8 N14 O28.5'
_chemical_formula_weight         2697.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.242(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5496(9)
_cell_length_b                   27.2170(10)
_cell_length_c                   16.4374(7)
_cell_measurement_reflns_used    8666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1740
_cell_measurement_theta_min      1.7430
_cell_volume                     10430.9(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -60.50  23.00   0.50   43.00    --   -9.10 -60.00 -60.00  167
  2  \w    -98.00  22.00   0.50   43.00    --   -9.10 -57.00-150.00  240
  3  \w    -60.50  23.00   0.50   43.00    --   -9.10 -60.00  30.00  167
  4  \w    -83.50  23.00   0.50   43.00    --   -9.10 -60.00 150.00  213
  5  \w    -62.50  52.00   0.50   43.00    --   -9.10 -19.00  30.00  229
  6  \w     36.50  80.00   0.50   43.00    --   -9.10  60.00 150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0036720000
_diffrn_orient_matrix_UB_12      0.0249840000
_diffrn_orient_matrix_UB_13      0.0128792000
_diffrn_orient_matrix_UB_21      0.0295153000
_diffrn_orient_matrix_UB_22      -0.0044040000
_diffrn_orient_matrix_UB_23      0.0213427000
_diffrn_orient_matrix_UB_31      0.0064266000
_diffrn_orient_matrix_UB_32      0.0059597000
_diffrn_orient_matrix_UB_33      -0.0379800000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            80637
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.496
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             5428
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         11498
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0606P)^2^+5.6824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8514
_reflns_number_total             11498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01477g2.cif
_cod_data_source_block           2021ncs0282_ljm3a
_cod_original_formula_sum        'C84 H109 Br6 Fe8 N14 O28.50'
_cod_database_code               7710287
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe8 C84 O28.5 Br6 H96 N14'
_chemical_oxdiff_usercomment     DC-1198A
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.682
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 H1WA-O1W = H1WB-O1W = O1H-H1H = O2H-H2H = O3H-H3H
 0.84 with sigma of 0.01
 H1WA-H1WB
 1.32 with sigma of 0.01
 Fe2-N4A \\sim Fe2-N4B
 with sigma of 0.02
 O4A-C24A \\sim O4B-C24B
 with sigma of 0.02
 N4A-C19A \\sim N4B-C23B
 with sigma of 0.02
 C21A-C24A \\sim C21B-C24B
 with sigma of 0.04
 N4A-C23A \\sim N4B-C19B
 with sigma of 0.02
 C19A-C20A \\sim C23B-C22B
 with sigma of 0.02
 O4A-C22A \\sim O4B-C20B
 with sigma of 0.04
 C23A-C22A \\sim C19B-C20B
 with sigma of 0.02
 C23A-C21A \\sim C19B-C21B
 with sigma of 0.04
 O4A-C21A \\sim O4B-C21B
 with sigma of 0.02
 C22A-C20A \\sim C20B-C22B
 with sigma of 0.04
 C22A-C21A \\sim C20B-C21B
 with sigma of 0.02
 C20A-C21A \\sim C22B-C21B
 with sigma of 0.02
 O4A-C20A \\sim O4B-C22B
 with sigma of 0.04
 Fe2-C19A \\sim Fe2-C23B
 with sigma of 0.04
 Fe2-C23A \\sim Fe2-C19B
 with sigma of 0.04
 N4A-C22A \\sim N4B-C20B
 with sigma of 0.04
 N4A-C20A \\sim N4B-C22B
 with sigma of 0.04
 C19A-C23A \\sim C23B-C19B
 with sigma of 0.04
 C19A-C21A \\sim C23B-C21B
 with sigma of 0.04
3. Others
 Sof(O4B)=Sof(N4B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(C22B)=
 Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(O4A)=Sof(N4A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Fixed Sof: O2W(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C19A(H19A), C19B(H19B), C20A(H20A), C20B(H20B),
 C22A(H22A), C22B(H22B), C23A(H23A), C23B(H23B), C25(H25), C26(H26), C28(H28),
 C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C1G(H1G), C2G(H2G), C4G(H4G),
  C5G(H5G)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C24A(H24A,H24B,
 H24C), C24B(H24D,H24E,H24F), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C),
 C6G(H6GA,H6GB,H6GC)
;
_shelx_res_checksum              92906
_shelx_hkl_checksum              84264
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id DC-1198A
_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 3.307
_oxdiff_exptl_absorpt_empirical_full_min 0.340