Syntheses and crystal structures of four 4-(4-nitro-phen-yl)piperazinium salts with hydrogen succinate, 4-amino-benzoate, 2-(4-chloro-phen-yl)acetate and 2,3,4,5,6-penta-fluoro-benzoate anions.
Vinaya, ?; Basavaraju, Yeriyur B.; Yathirajan, Hemmige S.; Parkin, Sean; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 151–156; doi:10.1107/S2056989023001093

data_2312069
_publ_section_title
;
 Syntheses and crystal structures of four 4-(4-nitro-phen-yl)piperazinium
 salts with hydrogen succinate, 4-amino-benzoate,
 2-(4-chloro-phen-yl)acetate and 2,3,4,5,6-penta-fluoro-benzoate anions.
;
_journal_coeditor_code           HB8053
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              151
_journal_page_last               156
_journal_paper_doi               10.1107/S2056989023001093
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C10 H14 N3 O2 +, C7 F5 O2 -'
_chemical_formula_moiety         'C10 H14 N3 O2 +, C7 F5 O2 -'
_chemical_formula_sum            'C17 H14 F5 N3 O4'
_chemical_formula_weight         419.31
_chemical_name_systematic
;
4-(4-Nitrophenyl)piperazinium 2,3,4,5,6-pentafluorobenzoate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                75.754(2)
_cell_angle_beta                 81.670(2)
_cell_angle_gamma                87.717(2)
_cell_formula_units_Z            2
_cell_length_a                   5.9779(3)
_cell_length_b                   11.3934(8)
_cell_length_c                   12.9312(9)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.75
_cell_volume                     844.63(9)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38650
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         2.150
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       tablet
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.221
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0359P)^2^+0.4190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                3456
_reflns_number_total             3882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8053sup1.cif
_cod_data_source_block           IV
_cod_database_code               2312069
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              82801
_shelx_res_checksum              14868
_cod_database_fobs_code 2312069