Aziridine-based concise synthesis of (+/-)-alstonerine
Donald Craig; Frederick W. Goldberg; Richard W. Pett; Niels T. H. Tholen; Andrew J. P. White; Chem.Commun. 49 (2013) 9275–; doi:10.1039/c3cc45543b

data_7109790
_publ_section_title
;
 Aziridine-based concise synthesis of (+/-)-alstonerine
;
_journal_name_full               Chem.Commun.
_journal_page_first              9275
_journal_paper_doi               10.1039/c3cc45543b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C29 H30 N2 O6 S2'
_chemical_formula_sum            'C29 H30 N2 O6 S2'
_chemical_formula_weight         566.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.4896(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.95229(13)
_cell_length_b                   16.6978(3)
_cell_length_c                   20.2810(4)
_cell_measurement_reflns_used    7246
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.4962
_cell_measurement_theta_min      2.9965
_cell_volume                     2692.93(8)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22471
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'blocky needles'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0530
_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^)+(0.0428P)^2^+0.9602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                5366
_reflns_number_total             6598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45543b.txt
_cod_data_source_block           8a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7109790