[Fe<sub>15</sub>]: a frustrated, centred tetrakis hexahedron.
Cutler, Daniel J.; Singh, Mukesh K.; Nichol, Gary S.; Evangelisti, Marco; Schnack, Jürgen; Cronin, Leroy; Brechin, Euan K.; Chemical communications (Cambridge, England) 57 (2021) 8925–8928; doi:10.1039/d1cc03919a

data_7128759
_publ_section_title
;
 [Fe<sub>15</sub>]: a frustrated, centred tetrakis hexahedron.
;
_journal_issue                   71
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8925
_journal_page_last               8928
_journal_paper_doi               10.1039/d1cc03919a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C48 H96 Cl6 Fe15 N8 O30, 2(Cl1 O4), 1(H O)'
_chemical_formula_sum            'C48 H97 Cl8 Fe15 N8 O39'
_chemical_formula_weight         2531.68
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.1578(5)
_cell_length_b                   15.1578(5)
_cell_length_c                   31.4738(12)
_cell_measurement_reflns_used    11929
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      28.6120
_cell_measurement_theta_min      3.8860
_cell_volume                     6262.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.885
_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    -52.00  86.00   1.00  137.03    --   17.54  -6.00 103.00  138
  2  \w     10.00  78.00   1.00  137.03    --   17.54-139.00  96.00   68
  3  \w     -9.00  39.00   1.00  137.03    --   17.54  77.00-180.00   48
  4  \w     -2.00  73.00   1.00  137.03    --   17.54  37.00 -90.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0534846000
_diffrn_orient_matrix_UB_12      0.0322609000
_diffrn_orient_matrix_UB_13      -0.0017530000
_diffrn_orient_matrix_UB_21      0.0063308000
_diffrn_orient_matrix_UB_22      -0.0433387000
_diffrn_orient_matrix_UB_23      -0.0003558000
_diffrn_orient_matrix_UB_31      -0.0042814000
_diffrn_orient_matrix_UB_32      -0.0018651000
_diffrn_orient_matrix_UB_33      -0.0224502000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            15300
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.352
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    2.014
_exptl_crystal_description       block
_exptl_crystal_F_000             3837
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.682
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0295P)^2^+117.2156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2914
_reflns_number_total             3385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03919a2.cif
_cod_data_source_block           fe15
_cod_depositor_comments          'Adding full bibliography for 7128759.cif.'
_cod_original_cell_volume        6262.6(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7128759
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     '@120 Fe15(tea)8Cl6'
_shelx_estimated_absorpt_t_max   0.480
_shelx_estimated_absorpt_t_min   0.208
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
2. Restrained distances
 O999-H999
 0.84 with sigma of 0.02
 N1-C5 \\sim N1-C6A \\sim N1-C2 \\sim N1-C2A \\sim N1-C3 \\sim N1-C3A
 with sigma of 0.02
 Cl2-O7A \\sim Cl2-O6 \\sim Cl2-O6A \\sim Cl2-O7
 with sigma of 0.02
 C8A-C7A \\sim C8-C7 \\sim C2-C1 \\sim C2A-C1A \\sim C4-C3 \\sim C3A-C4A \\sim
C6-C5 \\sim C6A-C5A
 with sigma of 0.02
 O4-C7 \\sim O4A-C7A \\sim O3A-C5A \\sim O3-C6 \\sim O2A-C4A \\sim O2-C4 \\sim
O1-C1 \\sim O1A-C1A
 with sigma of 0.02
3. Rigid bond restraints
 O1, O2, O3, O4, C1, C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1A, O2A, O3A, O4A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1A \\sim O2A \\sim O3A \\sim O4A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim
C5A \\sim C6A \\sim C7A \\sim C8A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C3) = Uanis(C3A)
5. Rigid body (RIGU) restrains
 O1, O2, O3, O4, C1, C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, O2A, O3A, O4A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6A, O7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O6A)=1-FVAR(1)
 Sof(O7A)=0.33333*(1-FVAR(2))
 Sof(O7)=0.33333*FVAR(2)
 Sof(O6)=FVAR(1)
 Fixed Sof: O1(0.5) O1A(0.5) O2(0.5) O2A(0.5) O3(0.5) O3A(0.5) O4(0.5)
 O4A(0.5) C1(0.5) H1a(0.5) H1b(0.5) C1A(0.5) H1Aa(0.5) H1Ab(0.5) C2(0.5)
 H2a(0.5) H2b(0.5) C2A(0.5) H2Aa(0.5) H2Ab(0.5) C3(0.5) H3a(0.5) H3b(0.5)
 C3A(0.5) H3Aa(0.5) H3Ab(0.5) C4(0.5) H4a(0.5) H4b(0.5) C4A(0.5) H4Aa(0.5)
 H4Ab(0.5) C5(0.5) H5a(0.5) H5b(0.5) C5A(0.5) H5Aa(0.5) H5Ab(0.5) C6(0.5)
 H6a(0.5) H6b(0.5) C6A(0.5) H6Aa(0.5) H6Ab(0.5) C7(0.5) H7a(0.5) H7b(0.5)
 C7A(0.5) H7Aa(0.5) H7Ab(0.5) C8(0.5) H8a(0.5) H8b(0.5) C8A(0.5) H8Aa(0.5)
 H8Ab(0.5) O999(0.16667) H999(0.16667)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C1A(H1Aa,H1Ab), C2(H2a,H2b), C2A(H2Aa,H2Ab), C3(H3a,H3b),
 C3A(H3Aa,H3Ab), C4(H4a,H4b), C4A(H4Aa,H4Ab), C5(H5a,H5b), C5A(H5Aa,H5Ab),
 C6(H6a,H6b), C6A(H6Aa,H6Ab), C7(H7a,H7b), C7A(H7Aa,H7Ab), C8(H8a,H8b),
 C8A(H8Aa,H8Ab)
;
_shelx_res_checksum              77875
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_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 1.614
_oxdiff_exptl_absorpt_empirical_full_min 0.787