`Segmented' crystals solved using synchrotron radiation: (2<i>S</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>)-4-(10,10-dimethyl-3,3-dioxo-3λ^6^-thia-4-azatricyclo[5.2.1.0^1,5^]decan-4-ylcarbonyl)-2,6-diphenylperhydropyrrolo[3,4-<i>c</i>]pyrrole-1,3-dione
Gainsford, Graeme J.; Mee, Simon P. H.; Luxenburger, Andreas; Acta Crystallographica Section C 65 (2009) o331–o334; doi:10.1107/S0108270109020435

data_2017207
_publ_section_title
;`Segmented' crystals solved using synchrotron radiation:
 (2<i>S</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>)-4-(10,10-dimethyl-3,3-dioxo-3\l^6^-thia-4-azatricyclo[5.2.1.0^1,5^]decan-4-ylcarbonyl)-2,6-diphenylperhydropyrrolo[3,4-<i>c</i>]pyrrole-1,3-dione
;
_journal_coeditor_code           SQ3199
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o331
_journal_page_last               o334
_journal_paper_doi               10.1107/S0108270109020435
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C29 H31 N3 O5 S'
_chemical_formula_moiety         'C29 H31 N3 O5 S'
_chemical_formula_sum            'C29 H31 N3 O5 S'
_chemical_formula_weight         533.63
_chemical_name_systematic
;
(2<i>S</i>,3<i>R</i>,4<i>S</i>,5<i>R</i>)-
4-(10,10-dimethyl-3,3-dioxo-3\l^6^-thia-4-azatricyclo[5.2.1.0^1,5^]decan-
4-ylcarbonyl)-2,6-diphenylperhydropyrrolo[3,4-<i>c</i>]pyrrole-1,3-dione
;
_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                 91.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3990(15)
_cell_length_b                   26.328(5)
_cell_length_c                   13.214(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2573.6(9)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'ADSC Quantum 210r software (ADSC, 2009)'
_computing_data_reduction
;
XDS (Kabsch, 1993; locally modified) and XPREP (Bruker, 2001)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ADSC Quantum 210r CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77300
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29004
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.387
_refine_ls_abs_structure_details 'Flack (1983), with 3898 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       0.042(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         8071
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0698P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                7637
_reflns_number_total             8071
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3199.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2017207
_cod_database_fobs_code          2017207