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_4127999
_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 O5 Zn, 5.06(C5 H11 N O), 0.44(O1)'
_chemical_formula_sum            'C117.3 H119.66 N5.06 O10.5 Zn'
_chemical_formula_weight         1833.64
_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                74.73(2)
_cell_angle_beta                 71.112(19)
_cell_angle_gamma                61.065(16)
_cell_formula_units_Z            2
_cell_length_a                   19.039(4)
_cell_length_b                   19.244(5)
_cell_length_c                   19.579(6)
_cell_measurement_reflns_used    10832
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.08
_cell_volume                     5890(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.983
_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  0.1432
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            72179
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.426
_diffrn_reflns_theta_min         3.078
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REUAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_description       prism
_exptl_crystal_F_000             1946
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1324
_refine_ls_number_reflns         26405
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.2057
_refine_ls_R_factor_gt           0.1489
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_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          0.3903
_refine_ls_wR_factor_ref         0.4361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13955
_reflns_number_total             26405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MOF-1_93K.cif
_cod_data_source_block           MOF1-93K
_cod_original_formula_sum        'C117.30 H119.66 N5.06 O10.50 Zn'
_cod_database_code               4127999
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H91A,H91B,H91C} of C91, {H83A,H83B,H83C} of C83, {H92A,
  H92B,H92C} of C92, {H90A,H90B,H90C} of C90, {H81A,H81B,H81C} of C81, {H97A,
  H97B,H97C} of C97, {H95A,H95B,H95C} of C95, {H82A,H82B,H82C} of C82, {H37A,
  H37B,H37C} of C37, {H45A,H45B,H45C} of C45, {H36A,H36B,H36C} of C36, {H46A,
  H46B,H46C} of C46, {H35A,H35B,H35C} of C35, {H44A,H44B,H44C} of C44, All C(H,
  H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  {H10C,H10D,H10E} of C100, {H12H,H12I,H12J} of C120, {H10F,H10G,H10H} of
  C107, {H11C,H11D,H11E} of C117, {H10I,H10J,H10K} of C105, {H12E,H12F,H12G} of
  C122, {H11J,H11K,H11L} of C115, {H11R,H11S,H11T} of C112, {H12K,H12L,H12M} of
  C123, {H1BA,H1BB,H1BC} of C1B, {H11M,H11N,H11O} of C110
2. Restrained distances
 O7-C98
 1.23 with sigma of 0.02
 O10-C113
 1.23 with sigma of 0.02
 O8-C103
 1.23 with sigma of 0.02
 N5-C114 = N5-C113 = N5-C116
 1.42 with sigma of 0.02
 N3-C106 = N3-C103 = N3-C104
 1.42 with sigma of 0.02
 N6-C1A
 1.42 with sigma of 0.02
 O11-C1A
 1.23 with sigma of 0.02
 O11-C118
 1.23 with sigma of 0.02
 N6-C119 = N6-C118 = N6-C121
 1.42 with sigma of 0.02
 C107-C106 = C105-C104
 1.54 with sigma of 0.02
 C112-C107
 -3.2 with sigma of 0.02
 O9-C108
 1.23 with sigma of 0.02
 N4-C108 = N4-C111 = N4-C109
 1.42 with sigma of 0.02
 C110-C109 = C112-C111
 1.54 with sigma of 0.02
 C122-C121 = C120-C119
 1.54 with sigma of 0.02
 N2-C99 = N2-C101 = N2-C98
 1.42 with sigma of 0.02
 C99-C100
 1.54 with sigma of 0.02
 C117-C116 = C115-C114
 1.54 with sigma of 0.02
 C103-C106
 2.49 with sigma of 0.01
 O9-N4
 2.2 with sigma of 0.04
 N5-O10
 2.2 with sigma of 0.04
 O8-N3
 2.2 with sigma of 0.04
 C104-C106
 2.49 with sigma of 0.01
 C110-N4
 2.54 with sigma of 0.01
 C107-N3
 2.54 with sigma of 0.04
 C112-N4
 2.49 with sigma of 0.01
 C111-C108
 2.49 with sigma of 0.01
 C108-C109
 2.49 with sigma of 0.01
 C109-C111
 2.49 with sigma of 0.01
 C121-C122 \\sim C121-C1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O8 \\sim C103 \\sim N3 \\sim C106 \\sim C104 \\sim C107 \\sim C105: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C110 \\sim C112 \\sim C111 \\sim N4 \\sim C108 \\sim C109 \\sim O9: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
O11 \\sim C118 \\sim N6 \\sim C119 \\sim C121 \\sim C120 \\sim C122 \\sim C1A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C113 \\sim N5 \\sim C116 \\sim C114 \\sim C117 \\sim C115 \\sim O10: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
O7 \\sim C98 \\sim N2 \\sim C99 \\sim C100 \\sim C101 \\sim C123: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C106, O8, C103, N3, C104, C107, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C110, C112, C111, N4, C108, C109, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C120, O11, C118, N6, C119, C121, C122, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C113, N5, C116, C114, C117, C115, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C98, N2, C99, C100, C101, C123
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Zn1B)=Sof(O1B)=1-FVAR(1)
 Sof(Zn1A)=Sof(O1A)=FVAR(1)
 Sof(O12)=1-FVAR(2)
 Sof(O8)=Sof(C103)=Sof(H103)=Sof(N3)=Sof(C107)=Sof(H10F)=Sof(H10G)=Sof(H10H)=
 Sof(C105)=Sof(H10I)=Sof(H10J)=Sof(H10K)=Sof(C106)=Sof(H10L)=Sof(H10M)=
 Sof(C104)=Sof(H10N)=Sof(H10O)=FVAR(2)
 Sof(H12C)=Sof(H12D)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(3)
 Sof(H12A)=Sof(H12B)=Sof(C122)=Sof(H12E)=Sof(H12F)=Sof(H12G)=FVAR(3)
 Fixed Sof: C118(0.5) H118(0.5) O9(0.5) C108(0.5) H108(0.5) C110(0.5)
 H11M(0.5) H11N(0.5) H11O(0.5) N4(0.5) C111(0.5) H11P(0.5) H11Q(0.5) C109(0.5)
 H10P(0.5) H10Q(0.5) C112(0.5) H11R(0.5) H11S(0.5) H11T(0.5) C1A(0.5) H1A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C96(H96A,H96B), C94(H94A,H94B), C99(H99A,H99B), C101(H10A,H10B), C119(H11A,
 H11B), C121(H12A,H12B), C121(H12C,H12D), C116(H11F,H11G), C114(H11H,H11I),
 C106(H10L,H10M), C104(H10N,H10O), C111(H11P,H11Q), C109(H10P,H10Q)
6.b Me refined with riding coordinates:
 C122(H12E,H12F,H12G), C120(H12H,H12I,H12J), C117(H11C,H11D,H11E), C115(H11J,
 H11K,H11L), C107(H10F,H10G,H10H), C105(H10I,H10J,H10K), C110(H11M,H11N,H11O),
 C112(H11R,H11S,H11T), C1B(H1BA,H1BB,H1BC), C123(H12K,H12L,H12M)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C13(H13), C14(H14), C16(H16),
 C20(H20), C24(H24), C31(H31), C33(H33), C40(H40), C42(H42), C49(H49), C50(H50),
  C52(H52), C53(H53), C55(H55), C59(H59), C60(H60), C62(H62), C67(H67),
 C69(H69), C77(H77), C79(H79), C86(H86), C88(H88), C93(H93), C98(H98),
 C118(H118), C113(H113), C103(H103), C108(H108), C1A(H1A)
6.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C),
 C92(H92A,H92B,H92C), C97(H97A,H97B,H97C), C95(H95A,H95B,H95C), C100(H10C,H10D,
 H10E)
;
_shelx_res_checksum              77979
_shelx_hkl_checksum              1417
_shelx_fab_checksum              63020
_olex2_submission_special_instructions 'No special instructions were received'