1,3-Dipolar Cycloaddition Reactions of Vinylidenecyclopropane-Diesters with Aromatic Diazomethanes Generated in Situ
Lei Wu; Min Shi; Journal of Organic Chemistry 75 (2010) 2296–2301; doi:10.1021/jo100105k

data_4025327
_publ_section_title
;
 1,3-Dipolar Cycloaddition Reactions of Vinylidenecyclopropane-Diesters
 with Aromatic Diazomethanes Generated in Situ
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2296
_journal_page_last               2301
_journal_paper_doi               10.1021/jo100105k
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C31 H30 N2 O6 S'
_chemical_formula_weight         558.63
_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                74.723(2)
_cell_angle_beta                 83.403(2)
_cell_angle_gamma                88.871(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2000(13)
_cell_length_b                   10.9423(15)
_cell_length_c                   14.273(2)
_cell_measurement_reflns_used    2159
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.632
_cell_measurement_theta_min      5.460
_cell_volume                     1376.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7238
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4532
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                3330
_reflns_number_total             5048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo100105k_si_002.cif
_cod_data_source_block           cd29522
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4025327