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_4127928
_publ_section_title
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 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, 1/3(C6 H3 Cl3), 4(C5 H9 N O)'
_chemical_formula_sum            'C88 H73 Cl N10 O16'
_chemical_formula_weight         1562.02
_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                108.6710(4)
_cell_angle_beta                 100.8300(5)
_cell_angle_gamma                108.2700(5)
_cell_formula_units_Z            6
_cell_length_a                   23.53390(13)
_cell_length_b                   25.94850(12)
_cell_length_c                   27.49620(15)
_cell_measurement_reflns_used    84641
_cell_measurement_temperature    223
_cell_measurement_theta_max      68.96
_cell_measurement_theta_min      2.10
_cell_volume                     14309.08(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  XtaLAB_P200
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            187607
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.264
_diffrn_reflns_theta_min         2.087
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             8900.00
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.43
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     3080
_refine_ls_number_reflns         52815
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1590P)^2^+6.1030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.2597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44018
_reflns_number_total             52815
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8b12124_si_005.cif
_cod_data_source_block           CPHATN_NP_NMP
_cod_depositor_comments
;

2020-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C264 H219 Cl3 N30 O48'
_cod_original_formula_weight         4686.05
_cod_original_formula_moiety    '3(C66 H36 N6 O12), C6 H3 Cl3, 12(C5 H9 N O)'
_cod_original_formula_units_Z            2
_cod_database_code               4127928
_shelx_res_checksum              61849
_shelx_hkl_checksum              95716
_shelx_fab_checksum              82429