Acid Responsive Hydrogen-Bonded Organic Frameworks.
Hisaki, Ichiro; Suzuki, Yuto; Gomez, Eduardo; Ji, Qin; Tohnai, Norimitsu; Nakamura, Takayoshi; Douhal, Abderrazzak; Journal of the American Chemical Society 141 (2019) 2111–2121; doi:10.1021/jacs.8b12124

data_4127927
_publ_section_title
;
 Acid Responsive Hydrogen-Bonded Organic Frameworks.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2111
_journal_page_last               2121
_journal_paper_doi               10.1021/jacs.8b12124
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C66 H36 N6 O12, 5(C4 H9 N O)'
_chemical_formula_sum            'C86 H81 N11 O17'
_chemical_formula_weight         1540.65
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                71.418(3)
_cell_angle_beta                 83.519(2)
_cell_angle_gamma                82.560(2)
_cell_formula_units_Z            2
_cell_length_a                   7.55733(14)
_cell_length_b                   20.5126(7)
_cell_length_c                   26.9565(9)
_cell_measurement_reflns_used    13342
_cell_measurement_temperature    213
_cell_measurement_theta_max      73.70
_cell_measurement_theta_min      3.49
_cell_volume                     3916.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD Version 2013/2 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35462
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         74.640
_diffrn_reflns_theta_min         3.267
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1620.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         15186
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.9559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12245
_reflns_number_total             15186
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8b12124_si_004.cif
_cod_data_source_block           CPHATN-NP_DMAc
_cod_database_code               4127927
_shelx_res_checksum              81283
_shelx_hkl_checksum              38928