Dimethylammonium perchlorate 18-crown-6 monohydrate clathrate
Ge, Jia-Zhen; Zhao, Min-Min; Shi, Ping-Ping; Acta Crystallographica Section E 66 (2010) o1740–; doi:10.1107/S1600536810023421

data_2226356
_publ_section_title
;
 Dimethylammonium perchlorate 18-crown-6 monohydrate clathrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1740
_journal_paper_doi               10.1107/S1600536810023421
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C2 H8 N +, Cl O4 -, C12 H24 O6, H2 O'
_chemical_formula_moiety         'C2 H8 N +, Cl O4 -, C12 H24 O6, H2 O'
_chemical_formula_sum            'C14 H34 Cl N O11'
_chemical_formula_weight         427.87
_chemical_melting_point          353
_chemical_name_systematic
;
Dimethylammonium perchlorate 18-crown-6 monohydrate clathrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.684(2)
_cell_length_b                   13.954(3)
_cell_length_c                   14.583(3)
_cell_measurement_reflns_used    2814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.15
_cell_volume                     2174.1(8)
_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>PRPKAPPA</i> (Ferguson, 1999)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(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 SCXmini diffractometer'
_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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22574
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>CrystalClear</i> (Rigaku, 2005)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.146
_refine_ls_abs_structure_details 'Flack (1983), 2168 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+0.2447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1713
_reflns_number_gt                2814
_reflns_number_total             4973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2290.cif
_cod_data_source_block           I
_cod_database_code               2226356
_cod_database_fobs_code          2226356