Crystallographic and dielectric studies of tetrahedral {NH4@Fe4} crystallized with halomethane molecules
Matsumoto, Daiki; Tanaka, Chiaki; Fujibayashi, Masaru; Nishihara, Sadafumi; Takahashi, Kiyonori; Nakamura, Takayoshi; Akutagawa, Tomoyuki; Masuya-Suzuki, Atsuko; Tsunashima, Ryo; CrystEngComm 25 (2023) 4793–4797; doi:10.1039/D3CE00429E

data_7247119
_publ_section_title
;
 Crystallographic and dielectric studies of tetrahedral {NH4@Fe4}
 crystallized with halomethane molecules
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              4793
_journal_page_last               4797
_journal_paper_doi               10.1039/D3CE00429E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         '2(C H Br3), C72 H72 Fe4 O60, 0.5(H8 N2)'
_chemical_formula_sum            'C74 H78 Br6 Fe4 N O60'
_chemical_formula_weight         2644.23
_chemical_name_systematic        C72H72O60Fe4(CHBr3)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-13 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.527(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.5848(4)
_cell_length_b                   17.97775(10)
_cell_length_c                   15.1052(2)
_cell_measurement_reflns_used    20804
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.4000
_cell_measurement_theta_min      3.8980
_cell_volume                     5431.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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      223.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -68.00 -14.00   0.50    1.16    --  -43.03  95.00  95.00  108
  2  \w    -11.00  25.00   0.50    1.16    --  -43.03  95.00  95.00   72
  3  \w      9.00  67.00   0.50    1.16    --   43.03 -95.00 -14.00  116
  4  \w    -25.00   3.00   0.50    1.16    --   43.03 -95.00 -14.00   56
  5  \w    -67.00 -40.00   0.50    4.64    -- -103.00  95.00  95.00   54
  6  \w     92.00 178.00   0.50    4.64    --  113.50  95.00  95.00  172
  7  \w     21.00 115.00   0.50    1.16    --   43.03  57.00  30.00  188
  8  \w     26.00  64.00   0.50    1.16    --   43.03 -38.00 -30.00   76
  9  \w    -32.00  22.00   0.50    1.16    --   43.03 -38.00 -30.00  108
 10  \w     22.00 116.00   0.50    1.16    --   43.03  57.00  90.00  188
 11  \w     23.00 116.00   0.50    1.16    --   43.03  57.00 -90.00  186
 12  \w   -153.00-128.00   0.50    4.64    -- -103.00 -95.00 -14.00   50
 13  \w     39.00 105.00   0.50    4.64    --  113.50 -95.00  90.00  132
 14  \w     98.00 135.00   0.50    4.64    --  113.50 -45.00-180.00   74
 15  \w     85.00 178.00   0.50    4.64    --  113.50  77.00-120.00  186
 16  \w     38.00  90.00   0.50    4.64    --  113.50 -45.00-180.00  104
 17  \w     90.00 172.00   0.50    4.64    --  113.50  61.00  60.00  164
 18  \w     38.00  82.00   0.50    4.64    --  113.50 -45.00 -60.00   88
 19  \w     89.00 134.00   0.50    4.64    --  113.50 -45.00 -60.00   90
 20  \w     90.00 174.00   0.50    4.64    --  113.50  61.00 -60.00  168
 21  \w     39.00 105.00   0.50    4.64    --  113.50 -95.00 120.00  132
 22  \w     85.00 173.00   0.50    4.64    --  113.50  77.00  30.00  176
 23  \w     90.00 178.00   0.50    4.64    --  113.50  61.00-150.00  176
 24  \w     91.00 177.00   0.50    4.64    --  113.50  45.00-180.00  172
 25  \w     41.00 105.00   0.50    4.64    --  113.50 -95.00 -90.00  128
 26  \w     39.00 103.00   0.50    4.64    --  113.50 -95.00  30.00  128
 27  \w     43.00 103.00   0.50    4.64    --  113.50 -95.00 -60.00  120
 28  \w     57.00 105.00   0.50    4.64    --  113.50 -95.00 -14.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.744
_diffrn_reflns_theta_min         3.305
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    7.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             2646
_exptl_crystal_preparation       'local laboratory'
_exptl_crystal_recrystallization_method 'vaper diffusion with hexane'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.441(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10523
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1438P)^2^+24.0166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                10136
_reflns_number_total             10523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00429e2.cif
_cod_data_source_block           1-chbr3
_cod_depositor_comments
'Adding full bibliography for 7247116--7247119.cif.'
_cod_original_cell_volume        5431.3(2)
_cod_database_code               7247119
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.443
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.559(7)
 0.441(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1A
 1.07 with sigma of 0.02
 N1-H1B
 1.07 with sigma of 0.02
 N1-H1C
 1.07 with sigma of 0.02
 N1-H1D
 1.07 with sigma of 0.02
 H1A-H1B
 1.75 with sigma of 0.04
 H1A-H1C
 1.75 with sigma of 0.04
 H1A-H1D
 1.75 with sigma of 0.04
 H1B-H1C
 1.75 with sigma of 0.04
 H1B-H1D
 1.75 with sigma of 0.04
 H1C-H1D
 1.75 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(O8)
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
6.a Ternary CH refined with riding coordinates:
 C99(H99)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56858
_shelx_fab_checksum              92819
_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
;