4,4,7,7-Tetramethyl-2-tosyl-2,3,3a,4,6,7,8,9-octahydro-1<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[6,5-<i>b</i>]cyclohexan-9-one
K. Chinnakali; D. Sudha; M. Jayagopi; R. Raghunathan; Hoong-Kun Fun; Acta Crystallographica Section E 63 (2007) o4436–o4437; doi:10.1107/S1600536807052221

data_2216163
_publ_section_title
4,4,7,7-Tetramethyl-2-tosyl-2,3,3a,4,6,7,8,9-octahydro-1<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[6,5-<i>b</i>]cyclohexan-9-one
_journal_coeditor_code           WN2210
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4436
_journal_page_last               o4437
_journal_paper_doi               10.1107/S1600536807052221
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H29 N O4 S'
_chemical_formula_moiety         'C22 H29 N O4 S'
_chemical_formula_sum            'C22 H29 N O4 S'
_chemical_formula_weight         403.53
_chemical_name_systematic
;
4,4,7,7-Tetramethyl-2-tosyl-2,3,3a,4,6,7,8,9-octahydro-1H-
pyrrolo[3,4-c]pyrano[6,5-b]cyclohexan-9-one
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.059(2)
_cell_angle_beta                 69.821(2)
_cell_angle_gamma                71.636(3)
_cell_formula_units_Z            6
_cell_length_a                   14.5021(7)
_cell_length_b                   15.0787(7)
_cell_length_c                   16.9696(8)
_cell_measurement_reflns_used    6958
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.47
_cell_measurement_theta_min      2.63
_cell_volume                     3072.3(3)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1998)'
_computing_publication_material
;
SHELXTL (Sheldrick, 1998) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
Bruker SMART APEX2 CCD area-detector
;
_diffrn_measurement_method       \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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64276
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         1.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.8940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.510
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         20257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0615P)^2^+0.432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                15293
_reflns_number_total             20257
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2210.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2216163
_cod_database_fobs_code          2216163