Cyclic diynes with tetramethyldisilyl groups in the bridges. Syntheses and properties
Haberhauer, Gebhard; Gleiter, Rolf; Irngartinger, Hermann; Oeser, Thomas; Rominger, Frank; Journal of the Chemical Society, Perkin Transactions 2  (1999) 2093–; doi:10.1039/a904409d

data_7213113
_publ_section_title
;
 Cyclic diynes with tetramethyldisilyl groups in the bridges. Syntheses
 and properties
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2093
_journal_paper_doi               10.1039/a904409d
_journal_year                    1999
_chemical_formula_sum            'C12 H20 Si2'
_chemical_formula_weight         220.46
_chemical_name_systematic
; 
 1,1,2,2-Tetramethyl-1,2-disilacyclodeca-4,8-diyne (8) 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1723(8)
_cell_length_b                   10.5020(8)
_cell_length_c                   12.9640(10)
_cell_measurement_temperature    200(2)
_cell_volume                     1384.94(19)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w 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  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3206
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.956241
_exptl_absorpt_correction_T_min  0.858456
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       fragment
_exptl_crystal_F_000             480
_exptl_crystal_size_max          .31
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .27
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.126
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_obs          0.0228
_refine_ls_shift/esd_max         -0.010
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0614
_refine_ls_wR_factor_obs         0.0607
_reflns_number_observed          1148
_reflns_number_total             1181
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904409dsup1.cif
_cod_data_source_block           gh1
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0071P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0071P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1384.9(2)
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               7213113