2,4,5-Trichloroanilinium perchlorate 18-crown-6 clathrate
Xu, Jie; Acta Crystallographica Section E 68 (2012) o739–; doi:10.1107/S1600536812006162

data_2233843
_publ_section_title
;
 2,4,5-Trichloroanilinium perchlorate 18-crown-6 clathrate
;
_journal_coeditor_code           HB6625
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o739
_journal_paper_doi               10.1107/S1600536812006162
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H5 Cl3 N +, Cl O4 -, C12 H24 O6'
_chemical_formula_moiety         'C6 H5 Cl3 N +, Cl O4 -, C12 H24 O6'
_chemical_formula_sum            'C18 H29 Cl4 N O10'
_chemical_formula_weight         561.22
_chemical_name_systematic
;
2,4,5-Trichloroanilinium perchlorate
1,4,7,10,13,16-hexaoxacyclooctadecane
;
_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                97.86(3)
_cell_angle_beta                 90.39(3)
_cell_angle_gamma                105.26(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4961(19)
_cell_length_b                   11.783(2)
_cell_length_c                   11.852(2)
_cell_measurement_reflns_used    4713
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      3.11
_cell_volume                     1266.1(4)
_computing_cell_refinement       '<i>CrystalClear</i> (Rigaku, 2005)'
_computing_data_collection       '<i>CrystalClear</i> (Rigaku, 2005)'
_computing_data_reduction        '<i>CrystalClear</i> (Rigaku, 2005)'
_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      298(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'CCD profile fitting'
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11310
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            ColourLess
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.276
_refine_ls_extinction_coef       0.019(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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0700P)^2^+0.5750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                3562
_reflns_number_total             4713
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6625.cif
_cod_data_source_block           I
_cod_database_code               2233843