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_4128000
_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 O6 Zn, C5 H9 N O'
_chemical_formula_sum            'C97 H73 N O7 Zn'
_chemical_formula_weight         1429.93
_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                73.98(4)
_cell_angle_beta                 74.49(4)
_cell_angle_gamma                80.60(5)
_cell_formula_units_Z            2
_cell_length_a                   14.057(8)
_cell_length_b                   16.947(9)
_cell_length_c                   20.427(11)
_cell_measurement_reflns_used    34847
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      2.044
_cell_volume                     4486(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_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  0.1667
_diffrn_reflns_av_unetI/netI     0.1567
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34847
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        23.499
_diffrn_reflns_theta_max         23.499
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.630
_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    1.059
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         12510
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.2365
_refine_ls_R_factor_gt           0.1741
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4121
_refine_ls_wR_factor_ref         0.4674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5633
_reflns_number_total             12510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MOF-2_93K.cif
_cod_data_source_block           MOF2-93K
_cod_database_code               4128000
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H66A,H66B,H66C} of C66, {H41A,H41B,H41C} of C41, {H35A,
  H35B,H35C} of C35, {H39A,H39B,H39C} of C39, {H47A,H47B,H47C} of C47, {H53A,
  H53B,H53C} of C53, {H48A,H48B,H48C} of C48, {H56A,H56B,H56C} of C56, {H2A,H2B,
  H2C} of C2, {H6A,H6B,H6C} of C6, {H8A,H8B,H8C} of C8, {H69A,H69B,H69C} of C69,
   All C(H,H) groups
 At 1.5 times of:
  {H10A,H10B,H10C} of C103, {H10F,H10G,H10H} of C107
2. Restrained distances
 N1-C102 = N1-C108
 1.47 with sigma of 0.01
 N1-C101
 1.47 with sigma of 0.01
 C108-C103 = C107-C102
 1.54 with sigma of 0.01
 N1-C107
 2.49 with sigma of 0.01
 C101-C108
 2.38 with sigma of 0.04
 C101-C102
 2.38 with sigma of 0.04
 C103-N1
 2.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C47 \\sim C45 \\sim C68 \\sim C33 \\sim C31 \\sim C32 \\sim C64 \\sim C48 \\sim
C66: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C102 \\sim O7 \\sim C101 \\sim N1 \\sim C108 \\sim C107 \\sim C103: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C47, C45, C68, C33, C31, C32, C64, C48, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C103, O7, C101, N1, C102, C108, C107
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C102(H10D,H10E)
5.b Me refined with riding coordinates:
 C103(H10A,H10B,H10C), C107(H10F,H10G,H10H)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C11(H11), C12(H12), C19(H19), C27(H27), C29(H29),
 C36(H36), C38(H38), C51(H51), C54(H54), C60(H60), C62(H62), C63(H63), C64(H64),
  C68(H68), C74(H74), C75(H75), C84(H84), C85(H85), C88(H88), C93(H93),
 C94(H94), C95(H95), C96(H96), C98(H98), C100(H100), C101(H101)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C35(H35A,H35B,H35C),
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C66(H66A,H66B,H66C), C69(H69A,
 H69B,H69C)
;
_shelx_res_checksum              12530
_shelx_hkl_checksum              51813
_shelx_fab_checksum              7017
_olex2_submission_special_instructions 'No special instructions were received'