First asymmetric synthesis of a differentially silyl-protected tris(alkynyl)methyl methyl ether.
Convertino, Vito; Manini, Peter; Schweizer, W. Bernd; Diederich, François; Organic & biomolecular chemistry 4 (2006) 1206–1208; doi:10.1039/b601380e

data_7150444
_publ_section_title
;
 First asymmetric synthesis of a differentially silyl-protected
 tris(alkynyl)methyl methyl ether.
;
_journal_issue                   7
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1206
_journal_page_last               1208
_journal_paper_doi               10.1039/b601380e
_journal_volume                  4
_journal_year                    2006
_chemical_compound_source        'Diederich Group'
_chemical_formula_moiety         'C24 H38 N2 O3 S Si2 '
_chemical_formula_sum            'C24 H38 N2 O3 S Si2'
_chemical_formula_weight         490.815
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.0511(6)
_cell_angle_beta                 88.3274(5)
_cell_angle_gamma                82.8675(9)
_cell_formula_units_Z            6
_cell_length_a                   11.2537(2)
_cell_length_b                   13.9426(2)
_cell_length_c                   28.9064(5)
_cell_measurement_reflns_used    11736
_cell_measurement_temperature    172
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     4466.96(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.07346
_diffrn_orient_matrix_UB_12      -0.00119
_diffrn_orient_matrix_UB_13      -0.05122
_diffrn_orient_matrix_UB_21      -0.03245
_diffrn_orient_matrix_UB_22      -0.01861
_diffrn_orient_matrix_UB_23      0.06244
_diffrn_orient_matrix_UB_31      -0.00276
_diffrn_orient_matrix_UB_32      0.03451
_diffrn_orient_matrix_UB_33      0.00404
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24791
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.571
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.625
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1727
_refine_ls_number_reflns         24791
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.625
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.348
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2102
_reflns_number_gt                22370
_reflns_number_total             24791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b601380e.txt
_cod_data_source_block           compound_1
_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_original_sg_symbol_H-M      'P 1 '
_cod_original_formula_sum        'C24 H38 N2 O3 S Si2 '
_cod_database_code               7150444