One-Step Synthesis of an Adaptive Nanographene MOF: Adsorbed Gas-Dependent Geometrical Diversity.
Suginome, Shun; Sato, Hiroshi; Hori, Akihiro; Mishima, Akio; Harada, Yuki; Kusaka, Shinpei; Matsuda, Ryotaro; Pirillo, Jenny; Hijikata, Yuh; Aida, Takuzo; Journal of the American Chemical Society 141 (2019) 15649–15655; doi:10.1021/jacs.9b07732

data_4128001
_publ_section_title
;
 One-Step Synthesis of an Adaptive Nanographene MOF: Adsorbed
 Gas-Dependent Geometrical Diversity.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15649
_journal_page_last               15655
_journal_paper_doi               10.1021/jacs.9b07732
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C92 H64 O4.76 Zn'
_chemical_formula_sum            'C92 H64 O4.76 Zn'
_chemical_formula_weight         1310.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                79.032(17)
_cell_angle_beta                 63.984(13)
_cell_angle_gamma                71.306(15)
_cell_formula_units_Z            2
_cell_length_a                   19.145(2)
_cell_length_b                   19.421(3)
_cell_length_c                   20.420(3)
_cell_measurement_reflns_used    5809
_cell_measurement_temperature    298
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      2.43
_cell_volume                     6452.2(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2010
_diffrn_reflns_av_unetI/netI     0.1602
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            118130
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        23.818
_diffrn_reflns_theta_max         23.818
_diffrn_reflns_theta_min         2.422
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.675
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         19649
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1956
_refine_ls_R_factor_gt           0.1167
_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^)+(0.1896P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3285
_refine_ls_wR_factor_ref         0.3778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7008
_reflns_number_total             19649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MOF-1_298K.cif
_cod_data_source_block           MOF1-298K
_cod_database_code               4128001
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H84A,H84B,H84C} of C84, {H93A,H93B,H93C} of C93, {H91A,
  H91B,H91C} of C91, {H81A,H81B,H81C} of C81, {H89A,H89B,H89C} of C89, {H88A,
  H88B,H88C} of C88, {H79A,H79B,H79C} of C79, {H80A,H80B,H80C} of C80, {H76A,
  H76B,H76C} of C76, {H65A,H65B,H65C} of C65, {H66A,H66B,H66C} of C66
 At 1.5 times of:
  {H90A,H90B,H90C} of C90
2. Restrained distances
 C58-C90
 1.55 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C55, C56, C57, C58, C59, C60, C89, C91, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C82, C73, C75, C78, C77, C79, C80, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Zn2)=1-FVAR(1)
 Sof(Zn1)=Sof(O5)=FVAR(1)
5.a Me refined with riding coordinates:
 C90(H90A,H90B,H90C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C13(H13), C14(H14), C16(H16),
 C22(H22), C24(H24), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C39(H39),
  C40(H40), C42(H42), C47(H47), C49(H49), C57(H57), C59(H59), C63(H63),
 C69(H69), C71(H71), C73(H73), C78(H78), C86(H86)
5.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C76(H76A,H76B,H76C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C84(H84A,H84B,H84C), C88(H88A,
 H88B,H88C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C93(H93A,H93B,H93C)
;
_shelx_res_checksum              92104
_shelx_hkl_checksum              96642
_shelx_fab_checksum              57257
_olex2_submission_special_instructions 'No special instructions were received'