Syntheses and crystal structures of 4-(4-nitrophenyl)piperazin-1-ium benzoate monohydrate and 4-(4-nitrophenyl)piperazin-1-ium 2-carboxy-4,6-dinitrophenolate
Shankara Prasad, Holehundi J.; Devaraju; Vinaya; Yathirajan, Hemmige S.; Parkin, Sean R.; Glidewell, Christopher; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022007472

data_2244132
_publ_section_title
;
 Syntheses and crystal structures of 4-(4-nitrophenyl)piperazin-1-ium
 benzoate monohydrate and 4-(4-nitrophenyl)piperazin-1-ium
 2-carboxy-4,6-dinitrophenolate
;
_journal_coeditor_code           HB8030
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022007472
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C10 H14 N3 O2 +, C7 H3 N2 O7 -'
_chemical_formula_moiety         'C10 H14 N3 O2 +, C7 H3 N2 O7 -'
_chemical_formula_sum            'C17 H17 N5 O9'
_chemical_formula_weight         435.35
_chemical_name_systematic
;
4-(4-Nitrophenyl)piperazin-1-ium 2-carboxy-4,6-dinitrophenolate
;
_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     dual
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.426(2)
_cell_angle_beta                 105.2730(10)
_cell_angle_gamma                98.538(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9599(4)
_cell_length_b                   8.5391(4)
_cell_length_c                   14.2227(5)
_cell_measurement_reflns_used    4212
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.510
_cell_measurement_theta_min      2.415
_cell_volume                     921.15(7)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38287
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         2.415
_diffrn_source                   microsource
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.3527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3662
_reflns_number_total             4212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8030sup1.cif
_cod_data_source_block           II
_cod_database_code               2244132
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              56528
_shelx_res_checksum              34436
_shelxl_version_number           2.014
_cod_database_fobs_code 2244132