(2<i>S</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>)-Diethyl 2-(10,10-dimethyl-3,3-dioxo-3λ^6^-thia-4-azatricyclo[5.2.1.0^1,5^]decan-4-ylcarbonyl)-5-phenylpyrrolidine-3,4-dicarboxylate: a novel isomorphous-by-addition compound
Gainsford, Graeme J.; Mee, Simon P. H.; Luxenburger, Andreas; Acta Crystallographica Section C 65 (2009) o15–o18; doi:10.1107/S0108270108040584

data_2016938
_publ_section_title
;(2<i>S</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>)-Diethyl
 2-(10,10-dimethyl-3,3-dioxo-3\l^6^-thia-4-azatricyclo[5.2.1.0^1,5^]decan-4-ylcarbonyl)-5-phenylpyrrolidine-3,4-dicarboxylate:
 a novel isomorphous-by-addition compound
;
_journal_coeditor_code           SK3280
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o15
_journal_page_last               o18
_journal_paper_doi               10.1107/S0108270108040584
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C27 H36 N2 O7 S'
_chemical_formula_moiety         'C27 H36 N2 O7 S'
_chemical_formula_sum            'C27 H36 N2 O7 S'
_chemical_formula_weight         532.64
_chemical_name_systematic
;
(2<i>S</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>)-Diethyl
2-(10,10-dimethyl-3,3-dioxo-3\l^6^-thia-4-azatricyclo[5.2.1.0^1,5^]decan-4-
ylcarbonyl)-5-phenylpyrrolidine-3,4-dicarboxylate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.148(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7194(9)
_cell_length_b                   6.9464(4)
_cell_length_c                   14.9703(9)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      31.14
_cell_measurement_theta_min      2.35
_cell_volume                     1363.26(15)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'SMART (Bruker, 2006)'
_computing_data_reduction
;
SAINT (Bruker, 2006) and SADABS (Bruker, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2003) and Mercury
(Macrae <i>et al.</i>,  2006)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker Nonius APEX2 CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28357
_diffrn_reflns_theta_full        31.99
_diffrn_reflns_theta_max         32.60
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.231
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         8865
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0797P)^2^+0.1530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                6778
_reflns_number_total             9045
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3280.cif
_cod_data_source_block           I
_cod_original_cell_volume        1363.25(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2016938
_cod_database_fobs_code          2016938