Enantioselective Synthesis of Ring-Fused Spiroannulated 1,2,3-Thiadiazole Derivatives.
Zeng, Xue-Mei; Xie, Jian-Wu; The Journal of organic chemistry 81 (2016) 3553–3559; doi:10.1021/acs.joc.6b00127

data_4036636
_publ_section_title
;
 Enantioselective Synthesis of Ring-Fused Spiroannulated 1,2,3-Thiadiazole
 Derivatives.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3553
_journal_page_last               3559
_journal_paper_doi               10.1021/acs.joc.6b00127
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C25 H27 N3 O5 S'
_chemical_formula_weight         481.56
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                76.6160(10)
_cell_angle_beta                 70.0600(10)
_cell_angle_gamma                65.5420(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4968(3)
_cell_length_b                   11.6056(3)
_cell_length_c                   12.3250(3)
_cell_measurement_reflns_used    10144
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.868
_cell_measurement_theta_min      2.347
_cell_volume                     1277.61(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43556
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  .986
_exptl_absorpt_correction_T_min  .968
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0488
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1842
_reflns_number_gt                4296
_reflns_number_total             5911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b00127_si_002.cif
_cod_data_source_block           150604
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4036636