Allenyl azide cycloaddition chemistry: application to the total synthesis of (±)-meloscine.
Feldman, Ken S.; Antoline, Joshua F.; Organic letters 14 (2012) 934–937; doi:10.1021/ol203463n

data_1503613
_publ_section_title
;
 Allenyl azide cycloaddition chemistry: application to the total synthesis
 of (+-)-meloscine.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              934
_journal_page_last               937
_journal_paper_doi               10.1021/ol203463n
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C29 H42 Br N O4 Si'
_chemical_formula_sum            'C29 H42 Br N O4 Si'
_chemical_formula_weight         576.64
_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                72.580(7)
_cell_angle_beta                 77.245(6)
_cell_angle_gamma                78.328(6)
_cell_formula_units_Z            2
_cell_length_a                   8.533(4)
_cell_length_b                   12.505(5)
_cell_length_c                   14.664(6)
_cell_measurement_reflns_used    2022
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.214
_cell_measurement_theta_min      2.474
_cell_volume                     1440.4(11)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21654
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.075
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    ride
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         7066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1496P)^2^+1.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2617
_reflns_number_gt                4654
_reflns_number_total             7066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol203463n_si_002.cif
_cod_data_source_block           jfa-6-96
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1440.3(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1503613