Engineering of Pore Geometry for Ultrahigh Capacity Methane Storage in Mesoporous Metal-Organic Frameworks.
Liang, Cong-Cong; Shi, Zhao-Lin; He, Chun-Ting; Tan, Jing; Zhou, Hu-Die; Zhou, Hao-Long; Lee, Yongjin; Zhang, Yue-Biao; Journal of the American Chemical Society 139 (2017) 13300–13303; doi:10.1021/jacs.7b08347

data_4131667
_publ_section_title
;
 Engineering of Pore Geometry for Ultrahigh Capacity Methane Storage in
 Mesoporous Metal-Organic Frameworks.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13300
_journal_page_last               13303
_journal_paper_doi               10.1021/jacs.7b08347
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         '0.06(C3648 H2208 N576 O1040 Zn320)'
_chemical_formula_sum            'C228 H138 N36 O65 Zn20'
_chemical_formula_weight         5729.14
_space_group_crystal_system      cubic
_space_group_IT_number           209
_space_group_name_Hall           'F 4 2 3'
_space_group_name_H-M_alt        'F 4 3 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.12 svn.r3442 for OlexSys, GUI svn.r5363)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   77.569(9)
_cell_length_b                   77.569(9)
_cell_length_c                   77.569(9)
_cell_measurement_reflns_used    15653
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.077
_cell_measurement_theta_min      1.331
_cell_volume                     466729(9)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  SSRF
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_wavelength     0.8265
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       82
_diffrn_reflns_limit_h_min       3
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25164
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.077
_diffrn_reflns_theta_max         26.077
_diffrn_reflns_theta_min         1.331
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.326
_exptl_crystal_description       cube
_exptl_crystal_F_000             46048
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.053
_refine_diff_density_min         -0.063
_refine_diff_density_rms         0.008
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.494(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         24546
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+42.5788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                15653
_reflns_number_total             24546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08347_si_005.cif
_cod_data_source_block           ST-4_sq
_cod_original_cell_volume        466729(162)
_cod_database_code               4131667
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.506(5)
 0.494(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 O12_$1-C37 \\sim O12-C37 \\sim O13-C46 \\sim O13_$1-C46
 with sigma of 0.02
 O12-C38 \\sim C38-O12_$1 \\sim C45-O13 \\sim C45-O13_$1
 with sigma of 0.02
 O13_$1-C45 \\sim O13-C45 \\sim C39-C39_$1 \\sim C39_$1-C41 \\sim C41-C39 \\sim
C38-C40_$1 ~
 C40_$1-C40 \\sim C40-C38 \\sim C42-C44 \\sim C42-C44_$1 \\sim C44_$1-C44 \\sim
C43-C43_$1 \\sim C43_$1-
 C45 \\sim C45-C43
 with sigma of 0.02
 C39_$1-C38 \\sim C39-C38 \\sim C39-C40 \\sim C40-C41 \\sim C40_$1-C41 \\sim
C39_$1-C40_$1 ~
 C43_$1-C42 \\sim C43-C42 \\sim C43-C44 \\sim C44-C45 \\sim C44_$1-C45 \\sim
C43_$1-C44_$1
 with sigma of 0.02
 C41-C42 \\sim C37-C38 \\sim C45-C46
 with sigma of 0.02
4. Restrained planarity
 O12_$1, C40_$1, C39_$1, C38, C37, C41, C40, C39, O12
 with sigma of 0.1
 C44_$1, C43_$1, O13_$1, C45, C42, C44, C43, C46, O13
 with sigma of 0.1
 C45, C42, C44_$1, C44, C43_$1, C43, C46, O13_$1, O13
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C43) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O12)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Rigid body (RIGU) restrains
 O12, O12, C38, C37, C41, C40, C40, C39, C39, C45, C42, C44, C44, C43, C43,
 C46, O13, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: O12(0.5) C38(0.25) C37(0.25) C41(0.25) C40(0.5) H40(0.5) C39(0.5)
 H39(0.5) C45(0.25) C42(0.25) C44(0.5) H44(0.5) C43(0.5) H43(0.5) C46(0.25)
 O13(0.5)
8.a Riding coordinates:
 N4(H4A), N5(H5), N6(H6A)
8.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3), C34(H34), C11(H11), C10(H10), C14(H14),
 C13(H13), C27(H27), C35(H35), C28(H28), C18(H18), C17(H17), C21(H21), C20(H20),
  C31(H31), C30(H30), C40(H40), C39(H39), C44(H44), C43(H43)
8.c Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3), C12(C11,C10,C9,C14,C13), C19(C18,C17,C16,C21,C20), C22(N1,
 C24,N3,C23,N2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_fab_checksum              71879