4,4-Dimethyl-2-tosyl-1,2,3,3a,4,11b-hexahydro-11<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[5,6-<i>c</i>]chromen-11-one 0.125-hydrate
Chinnakali, K.; Sudha, D.; Jayagobi, M.; Raghunathan, R.; Fun, Hoong-Kun; Acta Crystallographica Section E 65 (2009) o2943–o2944; doi:10.1107/S1600536809044730

data_2223656
_publ_section_title
;4,4-Dimethyl-2-tosyl-1,2,3,3a,4,11b-hexahydro-11<i>H</i>-pyrrolo[3,4-<i>c</i>]pyrano[5,6-<i>c</i>]chromen-11-one
 0.125-hydrate
;
_journal_coeditor_code           BT5116
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2943
_journal_page_last               o2944
_journal_paper_doi               10.1107/S1600536809044730
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C23 H23 N O5 S, 0.125H2 O'
_chemical_formula_moiety         'C23 H23 N O5 S, 0.125(H2 O)'
_chemical_formula_sum            'C23 H23.25 N O5.125 S'
_chemical_formula_weight         427.74
_chemical_name_systematic
;
4,4-Dimethyl-2-tosyl-1,2,3,3a,4,11b-hexahydro-11<i>H</i>-
pyrrolo[3,4-<i>c</i>]pyrano[5,6-<i>c</i>]chromen-11-one 0.125-hydrate
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.1932(2)
_cell_length_b                   15.1932(2)
_cell_length_c                   17.7180(3)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      2.22
_cell_volume                     4089.90(10)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEXII 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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97892
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1802
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6004
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0592P)^2^+1.3394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                5114
_reflns_number_total             6004
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5116.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 'Tetragonal' changed to 'tetragonal'
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_original_cell_volume        4089.91(10)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               2223656
_cod_database_fobs_code          2223656