Diastereoselective Photocycloaddition of Axially Chiral Monothiosuccinimides to 1,1-Diphenylethylene
Masami Sakamoto; Tsutomu Fujita; Takashi Mino; Tomoko Ohtake; Ayako Saitoh; Masaki Shigekura; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b304435a

data_7103857
_publ_section_title
;
Diastereoselective Photocycloaddition of Axially
Chiral Monothiosuccinimides to 1,1-Diphenylethylene
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b304435a
_journal_year                    2003
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C29 H32 N O S '
_chemical_formula_sum            'C29 H32 N O S'
_chemical_formula_weight         442.645
_chemical_name_common
;5-(2,5-Dimethyl-phenyl)-3,3-diphenyl-1-thia-5-aza-
spiro(3.4)octan-6-one
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 107.60(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.851(3)
_cell_length_b                   9.336(2)
_cell_length_c                   27.569(9)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    298
_cell_volume                     2417.1(12)
_computing_cell_refinement       'MXC(MAC Science)'
_computing_data_collection       'MXC(MAC Science)'
_computing_data_reduction        'maXus (Mackay et al., 1999)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maXus(Mackay et al., 1999)'
_computing_structure_refinement  'maXus(Mackay et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device       'Mac Science MXC18'
_diffrn_measurement_method       '\q \w scans'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01666
_diffrn_orient_matrix_UB_12      0.03115
_diffrn_orient_matrix_UB_13      -0.08379
_diffrn_orient_matrix_UB_21      0.00251
_diffrn_orient_matrix_UB_22      0.09997
_diffrn_orient_matrix_UB_23      0.03623
_diffrn_orient_matrix_UB_31      0.03412
_diffrn_orient_matrix_UB_32      -0.02249
_diffrn_orient_matrix_UB_33      0.04478
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' CuK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4989
_diffrn_reflns_theta_full        70.05
_diffrn_reflns_theta_max         70.05
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.34
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.521
_refine_ls_goodness_of_fit_gt    1.166
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    8
_refine_ls_number_parameters     357
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.084
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.422
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details     ' w = 1 / ( s^2^(Fo^2^) + 0.10000 * Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.186
_refine_ls_wR_factor_gt          0.184
_refine_ls_wR_factor_ref         0.184
_reflns_d_resolution_high        0.64
_reflns_d_resolution_low         2.56
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              -33
_reflns_number_gt                3506
_reflns_number_total             4864
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            b304435a.txt
_cod_data_source_block           compound_2
_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:

'_atom_site_adp_type' tag value 'Uij' was replaced with 'Uani' value
32 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom, diff' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c        '
_cod_original_formula_sum        'C29 H32 N O S '
_cod_database_code               7103857