3,4,5-Trihydroxybenzohydrazidium perchlorate–3,4,5-trihydroxybenzohydrazide–water (1/1/1)
A. Alhadi, Abeer; Khaledi, Hamid; Mohd Ali, Hapipah; Acta Crystallographica Section E 67 (2011) o2229–o2230; doi:10.1107/S1600536811030595

data_2231619
_publ_section_title
;
 3,4,5-Trihydroxybenzohydrazidium
 perchlorate--3,4,5-trihydroxybenzohydrazide--water (1/1/1)
;
_journal_coeditor_code           LX2194
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2229
_journal_page_last               o2230
_journal_paper_doi               10.1107/S1600536811030595
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C7 H9 N2 O4 +, Cl O4 -, C7 H8 N2 O4, H2 O'
_chemical_formula_moiety         'C7 H9 N2 O4 +, Cl O4 -, C7 H8 N2 O4, H2 O'
_chemical_formula_sum            'C14 H19 Cl N4 O13'
_chemical_formula_weight         486.78
_chemical_name_common
;
3,4,5-Trihydroxybenzohydrazidium perchlorate--3,4,5-trihydroxybenzohydrazide--
water (1/1/1)
;
_chemical_name_systematic
;
(3,4,5-Trihydroxybenzamido)ammonium
perchlorate--3,4,5-trihydroxybenzohydrazide--water (1/1/1)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1213(7)
_cell_length_b                   12.9178(4)
_cell_length_c                   7.0122(2)
_cell_measurement_reflns_used    1227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      3.15
_cell_volume                     1822.63(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14383
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.532
_refine_ls_abs_structure_details 'Flack (1983), 1545 Friedel pairs'
_refine_ls_abs_structure_Flack   0.28(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                2653
_reflns_number_total             3393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lx2194.cif
_cod_data_source_block           I
_cod_database_code               2231619
_cod_database_fobs_code          2231619