(3a<i>S</i>,4<i>S</i>,4a<i>S</i>,7<i>R</i>,9<i>S</i>,9a<i>S</i>)-Methyl 4-benzyloxy-9-methylsulfonyloxy-2,2-dimethyl-8-oxooctahydro-1,3-dioxa-5-thia-7a-azacyclopenta[<i>f</i>]azulene-7-carboxylate toluene solvate
Hörger, Rolf; Marsch, Michael; Geyer, Armin; Harms, Klaus; Acta Crystallographica Section E 61 (2005) o3447–o3448; doi:10.1107/S160053680503031X

data_2206992
_publ_section_title
;(3a<i>S</i>,4<i>S</i>,4a<i>S</i>,7<i>R</i>,9<i>S</i>,9a<i>S</i>)-Methyl
 4-benzyloxy-9-methylsulfonyloxy-2,2-dimethyl-8-oxooctahydro-1,3-dioxa-5-thia-7a-azacyclopenta[<i>f</i>]azulene-7-carboxylate
 toluene solvate
;
_journal_coeditor_code           IS6126
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3447
_journal_page_last               o3448
_journal_paper_doi               10.1107/S160053680503031X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C21 H27 N O9 S2 , C7 H8'
_chemical_formula_moiety         'C21 H27 N O9 S2 , C7 H8'
_chemical_formula_sum            'C28 H35 N O9 S2'
_chemical_formula_weight         593.69
_chemical_name_systematic
;
(3aS,4S,4aS,7R,9S,9aS)-Methyl
4-benzyloxy-9-methanesulfonyloxy-2,2-dimethyl-8-oxo-
octahydro-1,3-dioxa-5-thia-7a-aza-cyclopenta[f]azulene-7-carboxylate
toluene solvate
;
_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'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1251(6)
_cell_length_b                   11.4082(5)
_cell_length_c                   25.4972(15)
_cell_measurement_reflns_used    21120
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      1.6
_cell_volume                     2945.2(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2004)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29561
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.18
_refine_ls_abs_structure_details 'Flack (1983), with 2479 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.89
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.89
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0245P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                4668
_reflns_number_total             5724
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is6126.cif
_cod_data_source_block           I
_cod_database_code               2206992
_cod_database_fobs_code          2206992