Allenyl Azide Cycloaddition Chemistry. 2,3-Cyclopentennelated Indole Synthesis through Indolidene Intermediates
Feldman, Ken S.; Hester, D. Keith; Iyer, Malliga R.; Munson, Paul J.; Silva López, Carlos; Faza, Olalla Nieto; Journal of Organic Chemistry 74 (2009) 4958–4974; doi:10.1021/jo900659w

data_4028954
_publ_section_title
;
 Allenyl Azide Cycloaddition Chemistry. 2,3-Cyclopentennelated Indole
 Synthesis through Indolidene Intermediates
;
_journal_coden_ASTM              JOCEAH
_journal_issue                   14
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4958
_journal_page_last               4974
_journal_paper_doi               10.1021/jo900659w
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C24 H34 N O Si'
_chemical_formula_sum            'C24 H34 N O Si'
_chemical_formula_weight         380.61
_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                102.001(7)
_cell_angle_beta                 98.593(7)
_cell_angle_gamma                100.478(7)
_cell_formula_units_Z            4
_cell_length_a                   9.466(4)
_cell_length_b                   13.596(5)
_cell_length_c                   19.082(7)
_cell_measurement_temperature    93(2)
_cell_volume                     2316.9(16)
_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      93(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
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_refine_diff_density_max         0.365
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_refine_ls_R_factor_all          0.2006
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                5002
_reflns_number_total             11513
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4024645
_cod_data_source_file            jo900659wsup6.cif
_cod_data_source_block           dkh5s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2317.0(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4028954