(1<i>R</i>,3<i>R</i>,4<i>S</i>)-8-Phenylmenthyl (8<i>S</i>,9<i>S</i>)-8-ferrocenyl-6-methyl-1,4-dithia-6-azaspiro[4,4]nonane-9-carboxylate
García-Granda, Santiago; Fernández-Rodríguez, Manuel A.; Aguilar, Enrique; Fernández-Marí, Félix; Acta Crystallographica Section E 58 (2002) m502–m503; doi:10.1107/S1600536802015246

data_2201661
_publ_section_title
;(1<i>R</i>,3<i>R</i>,4<i>S</i>)-8-Phenylmenthyl
 (8<i>S</i>,9<i>S</i>)-8-ferrocenyl-6-methyl-1,4-dithia-6-azaspiro[4,4]nonane-9-carboxylate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m502
_journal_page_last               m503
_journal_paper_doi               10.1107/S1600536802015246
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Fe (C5 H5) (C29 H38 N O2 S2)]'
_chemical_formula_moiety         'C34 H43 Fe N O2 S2'
_chemical_formula_sum            'C34 H43 Fe N O2 S2'
_chemical_formula_weight         617.66
_chemical_name_systematic
;
(1R,3R,4S)-8-phenylmenthyl(8S,9S)-8-ferrocenyl-6-
methyl-1,4-dithia-6-azaspiro[4,4]nonan-9-carboxylate.
;
_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     Patterson
_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                   8.679(8)
_cell_length_b                   14.784(4)
_cell_length_c                   23.593(15)
_cell_measurement_reflns_used    1251
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      58.99
_cell_measurement_theta_min      3.53
_cell_volume                     3027(3)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12512
_diffrn_reflns_theta_full        58.99
_diffrn_reflns_theta_max         58.99
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    5.524
_exptl_absorpt_correction_T_max  0.437
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(XABS2; Parkin et al., 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.339
_refine_ls_abs_structure_details 'Flack (1983), 1005 Friedel pairs'
_refine_ls_abs_structure_Flack   0.039(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         3218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0696P)^2^+4.833P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                2699
_reflns_number_total             3218
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6114.cif
_cod_data_source_block           I
_cod_database_code               2201661
_cod_database_fobs_code          2201661