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_4519036
_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         'C51.631 H35.905 Fe3 N6 O16'
_chemical_formula_sum            'C51 H30 Fe3 N6 O16'
_chemical_formula_weight         1150.36
_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
_audit_creation_date             2021-07-08
_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                   29.8619(7)
_cell_length_b                   29.8619(7)
_cell_length_c                   29.8619(7)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      50.37
_cell_measurement_theta_min      5.54
_cell_volume                     26628.8(11)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      243.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17499
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        50.367
_diffrn_reflns_theta_max         50.367
_diffrn_reflns_theta_min         4.187
_exptl_absorpt_coefficient_mu    2.839
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5291
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0960 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.7055.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.574
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 894 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.252(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0718
_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^)+(0.0990P)^2^+212.4569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2026
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.863
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                2269
_reflns_number_total             2407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c13757_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        26628.8(19)
_cod_database_code               4519036
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.601
_shelx_estimated_absorpt_t_min   0.601
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C7-C7_$1
 2.336 with sigma of 0.01
 C6-C6_$1
 2.34 with sigma of 0.01
 N1-C7 = C7-C6
 1.43 with sigma of 0.02
 C7-C6 = C6-C5
 1.43 with sigma of 0.02
 O3-C4
 1.43 with sigma of 0.02
 N2-C4
 1.43 with sigma of 0.02
 C4-C13
 1.43 with sigma of 0.02
 C7-C5
 2.477 with sigma of 0.04
 N1-C6
 2.477 with sigma of 0.04
 C4-C12 \\sim C4-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C7 \\sim C6 \\sim Fe1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C10 \\sim C11 \\sim C14 \\sim C13 \\sim C12 \\sim C9: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, C2, O2, Fe1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C9, C10, C11, C14, C13, C4, O3, N2, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C5, N2, C7, N1, Fe1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C14)=Sof(C9)=0.5*FVAR(2)
 Sof(H14)=Sof(C11)=Sof(H11)=Sof(C10)=Sof(H9)=Sof(C12)=Sof(H12)=Sof(C13)=FVAR(1)
 Fixed Sof: O3(0.5) N2(0.5) H2(0.5) C4(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C6(H6), C7(H7), C14(H14), C11(H11), C9(H9), C12(H12)
6.b Fitted hexagon refined as free rotating group:
 C14(C11,C10,C9,C12,C13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45345
_shelx_hkl_checksum              35156
_shelx_fab_checksum              28157
_olex2_submission_special_instructions 'No special instructions were received'