Redetermination of (6<i>R</i>,7<i>S</i>,9<i>S</i>,11<i>S</i>)-(–)-sparteinium monoperchlorate
Lee, Yong-Min; Shim, Yoon-Bo; Lee, Seung Jae; Kang, Sung Kwon; Choi, Sung-Nak; Acta Crystallographica Section C 58 (2002) o733–o734; doi:10.1107/S0108270102020425

data_2013085
_publ_section_title
;
 Redetermination of
 (6<i>R</i>,7<i>S</i>,9<i>S</i>,11<i>S</i>)-(--)-sparteinium
 monoperchlorate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o733
_journal_page_last               o734
_journal_paper_doi               10.1107/S0108270102020425
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C15 H27 N2 1+, Cl O4 1-'
_chemical_formula_moiety         'C15 H27 N2 1+, Cl O4 1-'
_chemical_formula_sum            'C15 H27 Cl N2 O4'
_chemical_formula_weight         334.84
_chemical_name_common            '(-)-Sparteinium monoperchlorate'
_chemical_name_systematic
;
(6R,7S,9S,11S)-Sparteinium monoperchlorate
;
_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                   8.029(2)
_cell_length_b                   13.4196(16)
_cell_length_c                   15.3094(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.09
_cell_measurement_theta_min      11.34
_cell_volume                     1649.5(5)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w/2\q'
_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  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2438
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_correction_T_min  0.8872
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.242
_refine_ls_abs_structure_details 'Flack (1983), 232 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0533P)^2^+0.3075P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                1559
_reflns_number_total             2402
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob1088.cif
_cod_data_source_block           I
_cod_original_cell_volume        1649.6(5)
_cod_database_code               2013085
_cod_database_fobs_code          2013085