Synthesis of differentially protected/functionalised acetylenic building blocks from p-benzoquinone and their use in the synthesis of new enediynesElectronic supplementary information (ESI) available: 400 MHz 1H NMR and 13C NMR spectra. See http://www.rsc.org/suppdata/ob/b3/b302323k/
Sankararaman, Sethuraman; Srinivasan, Manivannan; Organic & Biomolecular Chemistry 1 (2003) 2388–; doi:10.1039/b302323k

data_7151416
_publ_section_title
;
 Synthesis of differentially protected/functionalised acetylenic
 building blocks from p-benzoquinone and their use in the synthesis of
 new enediynesElectronic supplementary information (ESI) available: 400
 MHz 1H NMR and 13C NMR spectra. See
 http://www.rsc.org/suppdata/ob/b3/b302323k/
;
_journal_issue                   13
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2388
_journal_paper_doi               10.1039/b302323k
_journal_volume                  1
_journal_year                    2003
_chemical_formula_sum            'C16 H24 O2 Si2'
_chemical_formula_weight         304.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.818(7)
_cell_length_b                   10.012(5)
_cell_length_c                   29.263(14)
_cell_measurement_reflns_used    313
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_volume                     3755(3)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.1206
_diffrn_reflns_av_sigmaI/netI    0.1555
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18239
_diffrn_reflns_theta_full        24.12
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.0757
_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^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                2540
_reflns_number_total             5904
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b302323k.txt
_cod_data_source_block           diol
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_cell_volume        3756(3)
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7151416