Quasi single-crystalline transformation of porous frameworks accompanied by interlayer rearrangements of hydrogen bonds.
Kubo, Haruka; Oketani, Ryusei; Hisaki, Ichiro; Chemical communications (Cambridge, England) 57 (2021) 8568–8571; doi:10.1039/d1cc03287a

data_7128715
_publ_section_title
;
 Quasi single-crystalline transformation of porous frameworks accompanied
 by interlayer rearrangements of hydrogen bonds.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8568
_journal_page_last               8571
_journal_paper_doi               10.1039/d1cc03287a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C38 H20.28 Br1.72 N4 O8'
_chemical_formula_sum            'C38 H20.28 Br1.72 N4 O8'
_chemical_formula_weight         798.32
_chemical_name_common            BrPQ-3a
_chemical_name_systematic
'4,4',4'',4'''-(5,10-dibromopyrazino[2,3-g]quinoxaline-2,3,7,8-tetrayl)tetrabenzoic acid'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-07-28 deposited with the CCDC.	2021-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                103.84(2)
_cell_angle_beta                 93.62(3)
_cell_angle_gamma                91.13(3)
_cell_formula_units_Z            1
_cell_length_a                   5.584(2)
_cell_length_b                   12.305(3)
_cell_length_c                   15.827(5)
_cell_measurement_reflns_used    628
_cell_measurement_temperature    113
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      3.43
_cell_volume                     1053.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type  PILATUS200K
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2401
_diffrn_reflns_av_unetI/netI     0.2642
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17280
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.468
_diffrn_reflns_theta_min         3.413
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             400.48
_exptl_crystal_recrystallization_method
'heat-induced structural change from BrPQ-2a'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.38
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     235
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2465
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.3275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2063
_reflns_number_total             6035
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1cc03287a2.cif
_cod_data_source_block           BrPQ-3a
_cod_depositor_comments
'Adding full bibliography for 7128714--7128717.cif.'
_cod_database_code               7128715
_shelx_res_checksum              40486
_shelx_fab_checksum              13285