Racemic 3,6-Dimethyl-3,6-bis(<i>tert</i>-butyldimethylsilyloxy)-1,7-cyclododecadiyne
Boss, C.; Keese, R.; Förtsch, M.; Acta Crystallographica Section C 52 (1996) 2370–2372; doi:10.1107/S0108270196004891

data_2005408
_publ_section_title
;
 Racemic
 3,6-Dimethyl-3,6-bis(<i>tert</i>-butyldimethylsilyloxy)-1,7-cyclododecadiyne
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2370
_journal_page_last               2372
_journal_paper_doi               10.1107/S0108270196004891
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C26 H48 O2 Si2'
_chemical_formula_sum            'C26 H48 O2 Si2'
_chemical_formula_weight         448.82
_chemical_melting_point          353.15
_chemical_name_systematic
;
rac.-1,10-Dimethyl-1,10-bis-(tert.-butyldimethylsilyloxy)-cyclododeca-
2,8-diyne
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   17.242(4)
_cell_length_b                   15.244(3)
_cell_length_c                   11.406(5)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      10.7
_cell_volume                     2997.9(16)
_computing_cell_refinement       'CAD4 Software'
_computing_data_collection       'CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'SDP (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick 1991)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3876
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.994
_exptl_crystal_density_meas      0.95(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.142
_refine_ls_extinction_coef       0.0044(7)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.091
_refine_ls_goodness_of_fit_obs   1.206
_refine_ls_hydrogen_treatment
;
 H atoms refined with group U~iso~
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2418
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.118
_refine_ls_restrained_S_obs      1.218
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.9495P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.1454
_refine_ls_wR_factor_obs         0.1180
_reflns_number_observed          1721
_reflns_number_total             2956
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1231.cif
_cod_data_source_block           diin1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '80\%C' was changed to '353.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2005408