First Total Synthesis and Assignment of the Stereochemistry of Crispatenine
Julien Bourdron; Laurent Commeiras; Gérard Audran; Nicolas Vanthuyne; J. C. Hubaud; Jean-Luc Parrain; Journal of Organic Chemistry 72 (2007) 3770–3775; doi:10.1021/jo070045j

data_4022885
_publ_section_title
;
 First Total Synthesis and Assignment of the Stereochemistry
 of Crispatenine
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3770
_journal_page_last               3775
_journal_paper_doi               10.1021/jo070045j
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C42 H80 O6 Si2'
_chemical_formula_weight         737.24
_chemical_name_systematic
; 
 ? 
;
_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                84.6300(10)
_cell_angle_beta                 80.4560(10)
_cell_angle_gamma                83.949(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3184(4)
_cell_length_b                   13.7588(4)
_cell_length_c                   15.7957(6)
_cell_measurement_reflns_used    28023
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      1.49
_cell_volume                     2404.99(14)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Bruker-Nonius, 1998)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'Phi scan'
_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  0.102
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28023
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            .5
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .05
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         11157
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      4.843
_refine_ls_R_factor_all          0.2714
_refine_ls_R_factor_gt           0.1726
_refine_ls_shift/su_max          0.373
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3760
_refine_ls_wR_factor_ref         0.4404
_reflns_number_gt                4997
_reflns_number_total             11157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070045jsi20070314_111247.cif
_cod_data_source_block           shelxl
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4022885