Absolute configuration and conformational disorder of a tricyclic thiosemicarbazone derivative
Ourhriss, N; Giorgi, M.; Mazoir, N.; Benharref, A.; Acta Crystallographica Section C 61 (2005) o699–o701; doi:10.1107/S0108270105033470

data_2015178
_publ_section_title
;
 Absolute configuration and conformational disorder of a tricyclic
 thiosemicarbazone derivative
;
_journal_coeditor_code           LN1186
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o699
_journal_page_last               o701
_journal_paper_doi               10.1107/S0108270105033470
_journal_volume                  61
_journal_year                    2005
_chemical_formula_moiety         'C17 H25 Cl2 N3 S'
_chemical_formula_sum            'C17 H25 Cl2 N3 S'
_chemical_formula_weight         374.38
_chemical_name_systematic
;
(1S,3R,8R)-2,2-dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.0^1.3^]dodecan-
11-one thiosemicarbazone
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6379(2)
_cell_length_b                   13.3638(3)
_cell_length_c                   16.3161(3)
_cell_measurement_reflns_used    22028
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      1.25
_cell_volume                     1883.45(7)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \f
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22028
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.180
_refine_ls_abs_structure_details
'Flack & Bernardinelli (1999, 2000), with 1566 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_coef       0.033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.029P)^2^+0.5086P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                3499
_reflns_number_total             3671
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln1186.cif
_cod_data_source_block           I
_cod_original_cell_volume        1883.49(7)
_cod_database_code               2015178
_cod_database_fobs_code          2015178