Tuning Open Metal Site-Free <b>ncb</b> Type of Metal-Organic Frameworks for Simultaneously High Gravimetric and Volumetric Methane Storage Working Capacities.
Zhang, Zong-Hui; Fang, Han; Xue, Dong-Xu; Bai, Junfeng; ACS applied materials & interfaces 13 (2021) 44956–44963; doi:10.1021/acsami.1c13757

data_4519035
_publ_section_title
;
 Tuning Open Metal Site-Free <b>ncb</b> Type of Metal-Organic Frameworks
 for Simultaneously High Gravimetric and Volumetric Methane Storage
 Working Capacities.
;
_journal_issue                   37
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              44956
_journal_page_last               44963
_journal_paper_doi               10.1021/acsami.1c13757
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C60 H39 Fe3 N6 O16'
_chemical_formula_sum            'C60 H39 Fe3 N6 O16'
_chemical_formula_weight         1267.52
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.5991(9)
_cell_length_b                   32.5991(9)
_cell_length_c                   32.5991(9)
_cell_measurement_reflns_used    5805
_cell_measurement_temperature    243.0
_cell_measurement_theta_max      39.97
_cell_measurement_theta_min      3.32
_cell_volume                     34643.1(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      243.0
_diffrn_measured_fraction_theta_full 0.998
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16106
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        39.972
_diffrn_reflns_theta_max         39.972
_diffrn_reflns_theta_min         1.916
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.201
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.4198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0904 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.5743.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.486
_exptl_crystal_description       Polyhedron
_exptl_crystal_F_000             5176
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 724 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.217(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1945
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1042P)^2^+249.1832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                1764
_reflns_number_total             1945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c13757_si_003.cif
_cod_data_source_block           a
_cod_original_cell_volume        34643(3)
_cod_database_code               4519035
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Restrained distances
 C16-C2 = C2-C10
 1.43 with sigma of 0.02
 N1-C16 = C16-C2
 1.43 with sigma of 0.02
 C9-C5
 1.43 with sigma of 0.001
 N2-C9
 1.43 with sigma of 0.001
 O3-C9
 1.43 with sigma of 0.001
 N2-C10
 1.43 with sigma of 0.001
 C1-C12 = C12-C14
 1.43 with sigma of 0.02
 C6-C14 = C14-C12
 1.43 with sigma of 0.02
 C16-C10
 2.477 with sigma of 0.04
 N1-C2
 2.477 with sigma of 0.04
 C6-C12
 2.477 with sigma of 0.04
 C1-C14
 2.477 with sigma of 0.04
 C9-C11 \\sim C15-C9
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O2, Fe1, O1, O4, N1, C4, C8, C16, C1, C2, C12, C10, C14, N2, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, N2, C9, O3, C5, C15, C7, C13, C3, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N2(0.5) H2(0.5) O3(0.5) C9(0.5) C5(0.5) C11(0.5) H11(0.5) C3(0.5)
 H3(0.5) C13(0.5) C7(0.5) H7(0.5) C15(0.5) H15(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C12(H12), C14(H14), C16(H16), C2(H2A), C11(H11), C3(H3), C7(H7),
 C15(H15)
5.b Fitted hexagon refined as free rotating group:
 C5(C11,C3,C13,C7,C15)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37003
_shelx_hkl_checksum              17083
_shelx_fab_checksum              53067
_olex2_submission_special_instructions 'No special instructions were received'