Bis[(4-cyanobenzyl)ammonium] bis(perchlorate) monohydrate
Huang, Yao; Acta Crystallographica Section E 67 (2011) o3431–; doi:10.1107/S1600536811048884

data_2232891
_publ_section_title
;
 Bis[(4-cyanobenzyl)ammonium] bis(perchlorate) monohydrate
;
_journal_coeditor_code           PV2463
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3431
_journal_paper_doi               10.1107/S1600536811048884
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '2C8 H9 N2 +, 2Cl O4 -, H2 O'
_chemical_formula_moiety         '2(C8 H9 N2 +), 2(Cl O4 -), H2 O'
_chemical_formula_sum            'C16 H20 Cl2 N4 O9'
_chemical_formula_weight         483.26
_chemical_name_systematic
;
Bis[(4-cyanobenzyl)ammonium] bis(perchlorate) monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.79(3)
_cell_angle_beta                 86.17(3)
_cell_angle_gamma                88.97(3)
_cell_formula_units_Z            2
_cell_length_a                   5.0305(10)
_cell_length_b                   13.616(3)
_cell_length_c                   16.695(3)
_cell_measurement_reflns_used    3490
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.26
_cell_volume                     1048.6(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       '\w scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10950
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.8
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.697
_refine_ls_extinction_coef       0.047(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4796
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+1.7940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1786
_reflns_number_gt                3490
_reflns_number_total             4796
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2463.cif
_cod_data_source_block           I
_cod_database_code               2232891
_cod_database_fobs_code          2232891