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_4519037
_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 N9 O16'
_chemical_formula_sum            'C60 H39 Fe3 N9 O16'
_chemical_formula_weight         1309.55
_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     iterative
_audit_creation_date             2021-06-03
_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                   33.5266(5)
_cell_length_b                   33.5266(5)
_cell_length_c                   33.5266(5)
_cell_measurement_reflns_used    8089
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      39.28
_cell_measurement_theta_min      3.23
_cell_volume                     37685.0(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      243.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            16844
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        39.522
_diffrn_reflns_theta_max         39.522
_diffrn_reflns_theta_min         1.863
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1012 before and 0.0861 after correction.
The Ratio of minimum to maximum transmission is 0.8480.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.462
_exptl_crystal_description       Polyhedron
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 798 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.430(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2035
_refine_ls_number_restraints     848
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+314.0114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2361
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                1891
_reflns_number_total             2035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c13757_si_004.cif
_cod_data_source_block           a
_cod_original_cell_volume        37685.0(17)
_cod_database_code               4519037
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.750
_olex2_refinement_description
;
1. Restrained distances
 C00J-N00F
 1.5 with sigma of 0.05
 C13-C00J = C00J-N00F
 1.43 with sigma of 0.02
 C00I-C15 = C15-C5
 1.43 with sigma of 0.02
 N00F-N00F_$1
 1.43 with sigma of 0.01
 C15-C5 = C5-C13
 1.43 with sigma of 0.02
 C5-C13 = C13-C00J
 1.43 with sigma of 0.02
 C8-C7
 1.43 with sigma of 0.02
 C39-C96 = C96-C00B
 1.43 with sigma of 0.02
 N3-C39 = C39-C96
 1.43 with sigma of 0.02
 O5-C8
 1.43 with sigma of 0.02
 N00A-C8
 1.43 with sigma of 0.02
 N00A-C00B
 1.43 with sigma of 0.02
 N3-C39
 1.43 with sigma of 0.001
 N00F-N1
 1.25 with sigma of 0.001
 O05-C00I
 1.239 with sigma of 0.01
 C11-C00I_$3
 1.482 with sigma of 0.001
 C13-N00F
 2.477 with sigma of 0.04
 C00I-C5
 2.477 with sigma of 0.04
 C5-C00J
 2.477 with sigma of 0.04
 C15-C13
 2.477 with sigma of 0.04
 C39-C00B
 2.477 with sigma of 0.04
 N3-C96
 2.477 with sigma of 0.04
 C8-C1 \\sim C8-C21
 with sigma of 0.02
 C6-C00I \\sim C5-C00I
 with sigma of 0.02
 N1-C4 \\sim N1-C14
 with sigma of 0.02
 N00F-C9 \\sim N00F-C13
 with sigma of 0.02
2. Restrained planarity
 N00F, C00J, C13, C5, C15
 with sigma of 0.1
 N1, C12, C4, C3, C11, C10, C14
 with sigma of 0.1
 N00F, C15, C6, C9, C00J, C13, C5
 with sigma of 0.1
 C00I, C15, C6, C9, C00J, C13, C5, N00F
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C39 \\sim C96 \\sim C00B \\sim N3 \\sim N00A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C00I \\sim C15 \\sim C6 \\sim C9 \\sim C00J \\sim C13 \\sim C5 \\sim C009 \\sim
C00B \\sim C39 \\sim C96 \\sim C8 \\sim C7 \\sim C21 \\sim C23 \\sim C00P \\sim
C2 \\sim C1 \\sim C12 \\sim C4 \\sim C3 \\sim C11 \\sim C10 \\sim C14 \\sim N3
\\sim N00A \\sim N00F \\sim N1: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
Uanis(C23) \\sim Ueq, Uanis(C009) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C00P)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C00J) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C96) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O03) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00I) \\sim Ueq, Uanis(O03) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C00J, C00I, N00F, C13, C5, C15, O05
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00P, C23, C21, C7, C2, C1, C8, O5, N00A, C00B, C96
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C009, O02, Fe00
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C00P, C2, C1, C7, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, N00F, C15, C00J, C13, C3, C4, C6, C9, C10, N1, C11, C12, C14, C00I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N00A(0.5) H00A(0.5) N00F(0.25) C15(0.25) C6(0.25) H6(0.25)
 C9(0.25) H9(0.25) C00J(0.25) C13(0.25) H13(0.25) C5(0.25) H5(0.25) O5(0.5)
 C8(0.5) C7(0.5) C21(0.5) H21(0.5) C23(0.5) H23(0.5) C00P(0.5) C2(0.5) H2(0.5)
 C1(0.5) H1(0.5) N1(0.25) C12(0.25) C4(0.25) H4(0.25) C3(0.25) H3(0.25)
 C11(0.25) C10(0.25) H10(0.25) C14(0.25) H14(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 N00A(H00A), C6(H6), C9(H9), C13(H13), C5(H5), C39(H39), C96(H96), C21(H21),
 C23(H23), C2(H2), C1(H1), C4(H4), C3(H3), C10(H10), C14(H14)
6.b Fitted hexagon refined as free rotating group:
 C15(C6,C9,C00J,C13,C5), C7(C21,C23,C00P,C2,C1), C12(C4,C3,C11,C10,C14)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83507
_shelx_hkl_checksum              69718
_shelx_fab_checksum              97669
_olex2_submission_special_instructions 'No special instructions were received'