Concise Synthesis of Bridged Azatricyclic Framework via Domino Semipinacol-Schmidt Reaction
Manohar Puppala; Annamalai Murali; Sundarababu Baskaran; Chem.Commun. 48 (2012) 5778–5780; doi:10.1039/c2cc31906c

data_7107785
_publ_section_title
;
 Concise Synthesis of Bridged Azatricyclic Framework via Domino
 Semipinacol-Schmidt Reaction
;
_journal_issue                   46
_journal_name_full               Chem.Commun.
_journal_page_first              5778
_journal_page_last               5780
_journal_paper_doi               10.1039/c2cc31906c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C10 H15 N S '
_chemical_formula_sum            'C10 H15 N S'
_chemical_formula_weight         181.29
_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                106.662(2)
_cell_angle_beta                 102.457(2)
_cell_angle_gamma                113.512(2)
_cell_formula_units_Z            4
_cell_length_a                   9.3690(3)
_cell_length_b                   10.7722(3)
_cell_length_c                   11.8003(5)
_cell_measurement_reflns_used    3269
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.37
_cell_measurement_theta_min      2.44
_cell_volume                     969.54(7)
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_collection       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13277
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,2004)
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_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          0.1482
_refine_ls_wR_factor_ref         0.1801
_reflns_number_gt                2703
_reflns_number_total             4601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31906c.txt
_cod_data_source_block           new
_cod_original_cell_volume        969.54(6)
_cod_database_code               7107785