Dynamics of Water Molecules in a 3-Fold Interpenetrated Hydrogen-Bonded Organic Framework Based on Tetrakis(4-pyridyl)methane
Inokuchi, Daisuke; Hirao, Yasukazu; Takahashi, Kazuyuki; Matsumoto, Kouzou; Mori, Hatsumi; Kubo, Takashi; The Journal of Physical Chemistry C 123 (2019) 6599–; doi:10.1021/acs.jpcc.8b12421

data_1554131
_publ_section_title
;
 Dynamics of Water Molecules in a 3-Fold Interpenetrated Hydrogen-Bonded
 Organic Framework Based on Tetrakis(4-pyridyl)methane
;
_journal_issue                   11
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              6599
_journal_paper_doi               10.1021/acs.jpcc.8b12421
_journal_volume                  123
_journal_year                    2019
_chemical_formula_moiety         'C21 H18 N4 2+, (B1 F4 1-)2, 2.5(H2 O1)'
_chemical_formula_sum            'C21 H23 B2 F8 N4 O2.5'
_chemical_formula_weight         545.05
_chemical_name_systematic
'bis(4-Pyridyl)bis(pyridinium-4-yl)methane bis(tetrafluoroborate) acetonitrile solvate'
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-12-22 deposited with the CCDC.
2018-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.3447(3)
_cell_length_b                   18.3447(3)
_cell_length_c                   37.850(3)
_cell_measurement_reflns_used    134010
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      3.02
_cell_volume                     11031.1(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics
;
Yadokari-XG 2009 (K. Wakita, T. Nemoto, et al., 2009)
;
_computing_publication_material
;
Yadokari-XG 2009 (K. Wakita, T. Nemoto, et al., 2009)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Rigaku VariMax RAPID FR-E
;
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            139251
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.219
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical Absorption Correction   March 2001 T. Higashi
    Rigaku Corporation, Tokyo, Japan
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5022
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 2288 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1346P)^2^+10.1138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2354
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6273
_reflns_number_total             6748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp8b12421_si_003.cif
_cod_data_source_block           1_Water-100K
_cod_original_cell_volume        11031.2(9)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_original_formula_sum        'C21 H23 B2 F8 N4 O2.50'
_cod_database_code               1554131
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.713
_shelx_res_checksum              76147
_shelx_hkl_checksum              55883