A novel mesoporous hydrogen-bonded organic framework with high porosity and stability.
Wang, Bin; Lv, Xiu-Liang; Lv, Jie; Ma, Li; Lin, Rui-Biao; Cui, Hui; Zhang, Jian; Zhang, Zhangjing; Xiang, Shengchang; Chen, Banglin; Chemical communications (Cambridge, England) 56 (2019) 66–69; doi:10.1039/c9cc07802a

data_7125643
_publ_section_title
;
 A novel mesoporous hydrogen-bonded organic framework with high porosity
 and stability.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              66
_journal_page_last               69
_journal_paper_doi               10.1039/c9cc07802a
_journal_volume                  56
_journal_year                    2019
_chemical_formula_moiety         'C60 H34 O8'
_chemical_formula_sum            'C60 H34 O8'
_chemical_formula_weight         882.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2019-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.815(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.192(2)
_cell_length_b                   32.9021(18)
_cell_length_c                   3.7820(2)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.38
_cell_volume                     4373.9(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            25210
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.708
_diffrn_reflns_theta_max         25.708
_diffrn_reflns_theta_min         1.739
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.047
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    0.670
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3945
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.1581
_refine_ls_R_factor_gt           0.1458
_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^)+(0.3000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3867
_refine_ls_wR_factor_ref         0.4128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2965
_reflns_number_total             3945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07802a2.cif
_cod_data_source_block           zhang_2019_9_18_pttna_0m
_cod_depositor_comments          'Adding full bibliography for 7125643.cif.'
_cod_original_cell_volume        4373.8(4)
_cod_database_code               7125643
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C002-C007 \\sim C0-C007
 with sigma of 0.02
 C002-C008 \\sim C0-C1
 with sigma of 0.02
 C007-C009 \\sim C007-C2
 with sigma of 0.02
 C009-C00C \\sim C2-C00D
 with sigma of 0.02
 C00C-C00B \\sim C00D-C0AA
 with sigma of 0.02
 C00B-C008 \\sim C0AA-C1
 with sigma of 0.02
 C00B-C00E \\sim C0AA-C00F
 with sigma of 0.02
 C008-C00G \\sim C1-C1AA
 with sigma of 0.02
 C00G-C00I \\sim C1AA-C00J
 with sigma of 0.02
 C00I-C00H \\sim C00J-C2AA
 with sigma of 0.02
 C00H-C00E \\sim C2AA-C00F
 with sigma of 0.02
 C00H-C11 \\sim C2AA-C11A
 with sigma of 0.02
 O00D-C11 \\sim O00E-C11A
 with sigma of 0.02
 O00F-C11 \\sim O00G-C11A
 with sigma of 0.02
 C002-C00B \\sim C0-C0AA
 with sigma of 0.04
 C002-C00G \\sim C0-C1AA
 with sigma of 0.04
 C007-C00C \\sim C007-C00D
 with sigma of 0.04
 C007-C008 \\sim C007-C1
 with sigma of 0.04
 C009-C00B \\sim C2-C0AA
 with sigma of 0.04
 C00C-C008 \\sim C00D-C1
 with sigma of 0.04
 C00C-C00E \\sim C00D-C00F
 with sigma of 0.04
 C00B-C00G \\sim C0AA-C1AA
 with sigma of 0.04
 C00B-C00H \\sim C0AA-C2AA
 with sigma of 0.04
 C008-C00I \\sim C1-C00J
 with sigma of 0.04
 C008-C00E \\sim C1-C00F
 with sigma of 0.04
 C00G-C00H \\sim C1AA-C2AA
 with sigma of 0.04
 C00I-C00E \\sim C00J-C00F
 with sigma of 0.04
 C00I-C11 \\sim C00J-C11A
 with sigma of 0.04
 C00H-O00D \\sim C2AA-O00E
 with sigma of 0.04
 C00H-O00F \\sim C2AA-O00G
 with sigma of 0.04
 C00E-C11 \\sim C00F-C11A
 with sigma of 0.04
 O00D-O00F \\sim O00E-O00G
 with sigma of 0.04
3. Restrained planarity
 H00F, O00F, C11, O00D
 with sigma of 0.1
 O00E, C11A, O00G, H00B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O00E) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00F) \\sim Ueq, Uanis(O00E) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C001) \\sim Ueq, Uanis(C002) \\sim Ueq, Uanis(C007) \\sim Ueq,
Uanis(C009) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(C00B) \\sim Ueq,
Uanis(C008) \\sim Ueq, Uanis(C00G) \\sim Ueq, Uanis(C00I) \\sim Ueq,
Uanis(C00H) \\sim Ueq, Uanis(C00E) \\sim Ueq, Uanis(C003) \\sim Ueq,
Uanis(C004) \\sim Ueq, Uanis(C005) \\sim Ueq, Uanis(C006) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C0AA) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C00D) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C00J)
\\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C00F) \\sim Ueq, Uanis(C11A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00D) \\sim Ueq, Uanis(O00F) \\sim Ueq, Uanis(O00E) \\sim Ueq,
Uanis(O00G) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00E) = Uanis(O00F)
5. Others
 Sof(C0)=Sof(H0)=Sof(C1)=Sof(C0AA)=Sof(C2)=Sof(H2)=Sof(C00D)=Sof(H00D)=
 Sof(C1AA)=Sof(H1AA)=Sof(C00J)=Sof(H00J)=Sof(C2AA)=Sof(C00F)=Sof(H00A)=
 Sof(C11A)=Sof(O00E)=Sof(O00G)=Sof(H00B)=1-FVAR(1)
 Sof(C002)=Sof(H002)=Sof(C009)=Sof(H009)=Sof(C00C)=Sof(H00C)=Sof(C00B)=
 Sof(C008)=Sof(C00G)=Sof(H00G)=Sof(C00I)=Sof(H00I)=Sof(C00H)=Sof(C00E)=
 Sof(H00E)=Sof(O00D)=Sof(O00F)=Sof(H00F)=Sof(C11)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C002(H002), C009(H009), C00C(H00C), C00G(H00G), C00I(H00I), C00E(H00E),
 C005(H005), C006(H006), C0(H0), C2(H2), C00D(H00D), C1AA(H1AA), C00J(H00J),
 C00F(H00A)
6.b Naphthalene refined as free rotating group:
 C002(C007,C009,C00C,C00B,C008,C00G,C00I,C00H,C00E)
6.c Idealised tetrahedral OH refined as rotating group:
 O00F(H00F), O00G(H00B)
;
_shelx_res_checksum              5810
_shelx_fab_checksum              98739
_olex2_submission_special_instructions 'No special instructions were received'