Crystal structure and Hirshfeld surface analysis of the hydrated 2:1 adduct of piperazine-1,4-diium 3,5-dinitro-2-oxidobenzoate and piperazine
Subha, Veerappan; Seethalakshmi, Thangaraj; Balakrishnan, Thangavelu; Judith Percino, M.; Venkatesan, Perumal; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022000226

data_2244005
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of the hydrated 2:1
 adduct of piperazine-1,4-diium 3,5-dinitro-2-oxidobenzoate and piperazine
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022000226
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
;
C4 H12 N2 2+, C7 H2 N2 O7 2-, 0.5C4 H10 N2, H2 O
;
_chemical_formula_moiety
;
C7 H2 N2 O7, C4 H12 N2, 0.5(C4 H10 N2), H2 O
;
_chemical_formula_sum            'C13 H21 N5 O8'
_chemical_formula_weight         375.35
_chemical_name_systematic
;
Bis(piperazine-1,4-diium)-3,5-dinitro-2-oxidobenzoate--piperazine (1/1)
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                116.320(5)
_cell_angle_beta                 98.878(5)
_cell_angle_gamma                98.390(5)
_cell_formula_units_Z            2
_cell_length_a                   6.6211(16)
_cell_length_b                   11.891(3)
_cell_length_c                   12.389(3)
_cell_measurement_reflns_used    2314
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.90
_cell_measurement_theta_min      3.21
_cell_volume                     838.1(4)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
PLATON  (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEXII'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15411
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.924
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.8335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.209
_refine_ls_extinction_coef       0.022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2018/3</i> (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3265
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0514P)^2^+0.1429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                1835
_reflns_number_total             3265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2181sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        838.1(3)
_cod_database_code               2244005
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.982
_shelx_hkl_checksum              46585
_shelx_res_checksum              14393
_cod_database_fobs_code 2244005