(<i>R</i>,<i>R</i>)-Disynephrine ether bis(hydrogen sulfate)
Arbuckle, William; Kennedy, Alan R.; Morrison, Catriona A.; Acta Crystallographica Section E 65 (2009) o1768–o1769; doi:10.1107/S1600536809025288

data_2222914
_publ_section_title
;
 (<i>R</i>,<i>R</i>)-Disynephrine ether bis(hydrogen sulfate)
;
_journal_coeditor_code           WM2243
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1768
_journal_page_last               o1769
_journal_paper_doi               10.1107/S1600536809025288
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C18 H26 N2 O3 2+, 2H S O4 -'
_chemical_formula_moiety         'C18 H26 N2 O3 2+, 2(H O4 S -)'
_chemical_formula_sum            'C18 H28 N2 O11 S2'
_chemical_formula_weight         512.54
_chemical_name_common
'(R,R)-di-synephrine ether di-hydrogen sulfate'
_chemical_name_systematic
;
(<i>R</i>,<i>R</i>)-2,4-bis(4-hydroxyphenyl)-<i>N</i>,<i>N</i>'-dimethyl-
3-oxapentane-1,5-diammonium bis(hydrogen sulfate)
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 116.413(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7204(9)
_cell_length_b                   11.5853(5)
_cell_length_c                   7.6579(5)
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.40
_cell_volume                     1090.19(13)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_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      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S 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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5888
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.433
_refine_ls_abs_structure_details 'Flack (1983), 1032 Friedel pairs'
_refine_ls_abs_structure_Flack   0.08(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.071P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                2034
_reflns_number_total             2401
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2243.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2222914
_cod_database_fobs_code          2222914