Crystal structure of bis(3,5-dimethyl-1H-pyrazol-4-ammonium) tetrafluoroterephthate, 2[C5H10N3][C8F4O4]
Fujisawa, Kiyoshi; Harakuni, Seigo; Ageishi, Keigo; Tiekink, Edward R. T.; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1017–1020; doi:10.1515/ncrs-2023-0333

data_8107627
_publ_section_title
;
 Crystal structure of bis(3,5-dimethyl-1H-pyrazol-4-ammonium)
 tetrafluoroterephthate, 2[C5H10N3][C8F4O4]
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1017
_journal_page_last               1020
_journal_paper_doi               10.1515/ncrs-2023-0333
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C8 F4 O4, 2(C5 H10 N3)'
_chemical_formula_sum            'C18 H20 F4 N6 O4'
_chemical_formula_weight         460.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 94.386(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1490(2)
_cell_length_b                   11.0063(3)
_cell_length_c                   14.0214(3)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     946.16(5)
_computing_cell_refinement       'CrysAlis^PRO^ [1]'
_computing_data_collection       'CrysAlis^PRO^ [1]'
_computing_data_reduction        'CrysAlis^PRO^ [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2018/3 [3]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SIR2008 [2]'
_diffrn_ambient_temperature      178(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.589
_diffrn_reflns_theta_min         2.355
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2414
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0694P)^2^+0.3151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2259
_reflns_number_total             2414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0333_suppl_001.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8107627
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              89466
_shelx_hkl_checksum              83587