[1-(1-Adamantylamino)ethylidene]oxonium methanesulfonate
Vícha, Robert; Nečas, Marek; Kozubková, Zuzana; Potáček, Milan; Acta Crystallographica Section E 65 (2009) o1307–; doi:10.1107/S1600536809017632

data_2222117
_publ_section_title
;
 [1-(1-Adamantylamino)ethylidene]oxonium methanesulfonate
;
_journal_coeditor_code           PK2161
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1307
_journal_paper_doi               10.1107/S1600536809017632
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C12 H20 N O +, C H3 S O3 -'
_chemical_formula_moiety         'C12 H20 N O +, C H3 O3 S -'
_chemical_formula_sum            'C13 H23 N O4 S'
_chemical_formula_weight         289.38
_chemical_melting_point          445
_chemical_name_systematic
;
[1-(1-Adamantylamino)ethylidene]oxonium methanesulfonate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   12.9848(7)
_cell_length_b                   11.2625(6)
_cell_length_c                   19.0037(10)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.14
_cell_volume                     2779.1(3)
_computing_cell_refinement       'Xcalibur (Oxford Diffraction, 2006)'
_computing_data_collection       'Xcalibur (Oxford Diffraction, 2006)'
_computing_data_reduction        'Xcalibur (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       \w
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19453
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Xcalibur; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.470
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0337
_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^)+(0.054P)^2^+1.529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                2000
_reflns_number_total             2454
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2161.cif
_cod_data_source_block           I
_cod_database_code               2222117
_cod_database_fobs_code          2222117