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_7247117
_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         'C72 H72 Fe4 O60, 0.5(H8 N2), 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H80 Cl4 Fe4 N O60'
_chemical_formula_weight         2308.59
_chemical_name_systematic        C74H76Cl4Fe4NO60
_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             2023-07-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 133.512(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.2657(8)
_cell_length_b                   17.98779(19)
_cell_length_c                   15.0294(4)
_cell_measurement_reflns_used    38132
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      30.6240
_cell_measurement_theta_min      1.7890
_cell_volume                     5345.8(5)
_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 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      223.15
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43615
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.490
_diffrn_reflns_theta_min         3.873
_exptl_absorpt_coefficient_mu    6.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.47a(Rigaku Oxford Diffraction, 2022)'
_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    1.434
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2366
_exptl_crystal_preparation       'rocal laboratory'
_exptl_crystal_recrystallization_method 'vapor diffusion with poor solbent'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.437(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10810
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0823P)^2^+20.8647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                10626
_reflns_number_total             10810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00429e2.cif
_cod_data_source_block           1-ch2cl2
_cod_depositor_comments
'Adding full bibliography for 7247116--7247119.cif.'
_cod_original_cell_volume        5345.8(4)
_cod_database_code               7247117
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.636
_shelx_estimated_absorpt_t_min   0.513
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.563(5)
 0.437(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,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
 C99-Cl1
 1.78 with sigma of 0.02
 C99-Cl2
 1.78 with sigma of 0.02
 C99A-Cl1A
 1.78 with sigma of 0.02
 C99A-Cl2A
 1.78 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
 Cl1-Cl2
 3.2 with sigma of 0.04
 C99-Cl1 \\sim C99A-Cl1A
 with sigma of 0.02
 C99-Cl2 \\sim C99A-Cl2A
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl2A
 with sigma of 0.04
 O8-C9 \\sim O8-C9A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C99 \\sim C99: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Uanis(O8) = Uanis(C9) = Uanis(C9A)
Uanis(C99) = Uanis(Cl1) = Uanis(Cl2)
Uanis(C99A) = Uanis(Cl1A) = Uanis(Cl2A)
5. Rigid body (RIGU) restrains
 Cl1, Cl2, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl2A)=Sof(Cl1A)=Sof(C99A)=Sof(H99C)=Sof(H99D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C99)=Sof(H99A)=Sof(H99B)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C99(H99A,H99B), C99A(H99C,H99D)
7.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C20(H20A,H20B,
 H20C), C2(H2A,H2B,H2C), C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C27(H27A,H27B,
 H27C), C32(H32A,H32B,H32C), C3(H3A,H3B,H3C), C15(H15A,H15B,H15C), C9(H9A,H9B,
 H9C), C9A(H9AA,H9AB,H9AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12059
_shelx_fab_checksum              84645
_olex2_submission_special_instructions 'No special instructions were received'