An Exceptionally Stable Metal-Organic Framework Constructed from Chelate-based Metal-Organic Polyhedra.
Chiong, Jerika A.; Zhu, Jie; Bailey, Jake B.; Kalaj, Mark; Subramanian, Rohit; Xu, Wenqian; Cohen, Seth M.; Tezcan, F. Akif; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01626

data_4134603
_publ_section_title
;
 An Exceptionally Stable Metal-Organic Framework Constructed from
 Chelate-based Metal-Organic Polyhedra.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01626
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C48 H36 Fe4 N12 O24), 7.95(C3 H7 N O), 6(H2 O)'
_chemical_formula_sum            'C119.85 H139.65 Fe8 N31.95 O61.95'
_chemical_formula_weight         3465.78
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.604(4)
_cell_length_b                   27.604(4)
_cell_length_c                   27.604(4)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.21
_cell_volume                     21034(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            94216
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_min         1.278
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.4908
_exptl_absorpt_correction_T_min  0.4109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0808 before and 0.0459 after correction. The Ratio of minimum to maximum transmission is 0.8372. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       cube
_exptl_crystal_F_000             7144
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 4642 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         14345
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0753P)^2^+17.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                11914
_reflns_number_total             14345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01626_si_002.cif
_cod_data_source_block           mbdhfe_a
_cod_original_cell_volume        21034(10)
_cod_database_code               4134603
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N3B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O3S(0.65) N3S(0.65) C7S(0.65) H7S(0.65) C8S(0.65) H8SA(0.65)
 H8SB(0.65) H8SC(0.65) C9S(0.65) H9SA(0.65) H9SB(0.65) H9SC(0.65)
4.a Free rotating group:
 O4S(H4SA,H4SB), O5S(H5SD,H5SE)
4.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N2A(H2A), N3A(H3A), N4A(H4A), C3A(H3AA), C4A(H4AA), C5A(H5A),
 C8A(H8A), C11A(H11A), C12A(H12A), C13A(H13A), C15A(H15A), N1B(H1B), N2B(H2B),
 N3B(H3B), N4B(H4B), C3B(H3BA), C4B(H4BA), C5B(H5B), C7B(H7B), C11B(H11B),
 C12B(H12B), C13B(H13B), C16B(H16B), C1S(H1S), C4S(H4S), C7S(H7S)
4.c Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC), C8S(H8SA,H8SB,H8SC), C9S(H9SA,H9SB,H9SC)
;
_shelx_res_checksum              89398
_shelx_hkl_checksum              90235
_shelx_fab_checksum              55459
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'