4-Bromo-3-methylanilinium perchlorate 18-crown-6 clathrate
Xu, Qian; Zhao, Min Min; Acta Crystallographica Section E 67 (2011) o579–; doi:10.1107/S1600536811003540

data_2229421
_publ_section_title
;
 4-Bromo-3-methylanilinium perchlorate 18-crown-6 clathrate
;
_journal_coeditor_code           JH2260
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o579
_journal_paper_doi               10.1107/S1600536811003540
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C7 H9 Br N +, Cl O4 -, C12 H24 O6'
_chemical_formula_moiety         'C7 H9 Br N +, Cl O4 -, C12 H24 O6'
_chemical_formula_sum            'C19 H33 Br Cl N O10'
_chemical_formula_weight         550.81
_chemical_name_systematic
;
4-Bromo-3-methylanilinium perchlorate--18-crown-6 (1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.967(2)
_cell_length_b                   13.446(3)
_cell_length_c                   15.677(3)
_cell_measurement_reflns_used    20001
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      3.01
_cell_volume                     2516.3(9)
_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      296(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku SCXmini'
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25007
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>CrystalClear</i>; Rigaku, 2005)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.4000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.979
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0769P)^2^+0.8528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                4005
_reflns_number_total             5665
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jh2260.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229421
_cod_database_fobs_code          2229421