A Single-Crystal Open-Capsule Metal-Organic Framework.
Wei, Yong-Sheng; Zhang, Mei; Kitta, Mitsunori; Liu, Zheng; Horike, Satoshi; Xu, Qiang; Journal of the American Chemical Society 141 (2019) 7906–7916; doi:10.1021/jacs.9b02417

data_4128231
_publ_section_title
;
 A Single-Crystal Open-Capsule Metal-Organic Framework.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7906
_journal_page_last               7916
_journal_paper_doi               10.1021/jacs.9b02417
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(C88 H40 Fe6 N14 O26)'
_chemical_formula_sum            'C44 H20 Fe3 N7 O13'
_chemical_formula_weight         1022.22
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.8853(4)
_cell_length_b                   16.8853(4)
_cell_length_c                   14.8612(5)
_cell_measurement_reflns_used    5842
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.9790
_cell_measurement_theta_min      2.3850
_cell_volume                     3669.46(17)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13573
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         1.954
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_description       plate
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1387
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0930P)^2^+1.3982P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1232
_reflns_number_total             1387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02417_si_003.cif
_cod_data_source_block           Fe-MIL-88B-tpy
_cod_original_cell_volume        3669.5(2)
_cod_database_code               4128231
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Shared sites
{N3, C8}
3. Restrained distances
 N1-C3
 1.5 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N3) = Uanis(C8)
5. Others
 Fixed Sof: N1(0.25) H1A(0.16667) H1B(0.16667) H1C(0.16667) C8(0.16667)
 H8(0.16667) N3(0.08333)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_platon_squeeze_void_probe_radius 1.20