Crystal structure of bis(1-benzyl-1<i>H</i>-1,2,4-triazole) perchloric acid monosolvate
Qin, Yong-Qi; Xue, Jin-hui; Qiao, Yuan-Biao; Zhang, Zi-Feng; Acta Crystallographica Section E 70 (2014) o1290–o1291; doi:10.1107/S1600536814024829

data_2240254
_publ_section_title
;
 Crystal structure of bis(1-benzyl-1<i>H</i>-1,2,4-triazole) perchloric
 acid monosolvate
;
_journal_coeditor_code           RK2425
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1290
_journal_page_last               o1291
_journal_paper_doi               10.1107/S1600536814024829
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '2C9 H9 N3, H Cl O4'
_chemical_formula_moiety         '2(C9 H9 N3), H Cl O4 '
_chemical_formula_sum            'C18 H19 Cl N6 O4'
_chemical_formula_weight         418.84
_chemical_name_systematic
;
Bis(1-benzyl-1<i>H</i>-1,2,4-triazole) perchloric acid monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 95.136(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.7173(10)
_cell_length_b                   7.7671(12)
_cell_length_c                   21.955(4)
_cell_measurement_reflns_used    637
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.64
_cell_measurement_theta_min      3.22
_cell_volume                     971.0(3)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 1997)
;
_computing_data_collection
;
<i>SMART</i> (Bruker, 1997)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 1997)
;
_computing_molecular_graphics
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SHELXS97</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9373
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.387
_refine_ls_abs_structure_details
;
Flack (1983) parameter determined using 873 quotients
;
_refine_ls_abs_structure_Flack   0.27(9)
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0604P)^2^+0.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                2680
_reflns_number_total             3981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2425sup1.cif
_cod_data_source_block           I
_cod_database_code               2240254
_cod_database_fobs_code          2240254