(2<i>S</i>,3a'<i>R</i>,4'<i>R</i>,5'<i>S</i>,6'<i>R</i>)-4',5'-Isoprolidenedioxy-6'-(trityloxymethyl)-2'-oxotetrahydro-1<i>H</i>-spiro[pyrrolidine-2,3'-pyrrolo[1,2-<i>b</i>]isoxazole]-1-carbaldehyde
Chu-Yi Yu; Ying Fu; Acta Crystallographica Section E 62 (2006) o3172–o3173; doi:10.1107/S1600536806024500

data_2209844
_publ_section_title
(2<i>S</i>,3a'<i>R</i>,4'<i>R</i>,5'<i>S</i>,6'<i>R</i>)-4',5'-Isoprolidenedioxy-6'-(trityloxymethyl)-2'-oxotetrahydro-1<i>H</i>-spiro[pyrrolidine-2,3'-pyrrolo[1,2-<i>b</i>]isoxazole]-1-carbaldehyde
_journal_coeditor_code           HB2085
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3172
_journal_page_last               o3173
_journal_paper_doi               10.1107/S1600536806024500
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C33 H34 N2 O6'
_chemical_formula_moiety         'C33 H34 N2 O6'
_chemical_formula_sum            'C33 H34 N2 O6'
_chemical_formula_weight         554.62
_chemical_melting_point          464
_chemical_name_common
;
(2S,3a'R,4'R,5'S,6'R)-4',5'-isoprolidenedioxy-6'-(trityloxymethyl)
-2'-oxotetrahydro-1H-spiro[pyrrolidine-2,3'-pyrrolo[1,2-b]isoxazole]
-1-carbaldehyde
;
_chemical_name_systematic
;
(2S,3a'R,4'R,5'S,6'R)-4',5'-Isoprolidenedioxy-6'-(trityloxymethyl)-2'-
oxotetrahydro-1<i>H</i>-spiro[pyrrolidine-2,3'-
pyrrolo[1,2-<i>b</i>]isoxazole]-1-carbaldehyde
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.942(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0296(14)
_cell_length_b                   12.7262(17)
_cell_length_c                   11.4028(16)
_cell_measurement_reflns_used    3060
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.41
_cell_volume                     1437.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8933
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.172
_refine_ls_abs_structure_details 'none, Friedel pairs merged'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3556
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.0766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                2445
_reflns_number_total             3556
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2085.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21'
_cod_database_code               2209844
_cod_database_fobs_code          2209844