Contraction and Expansion of the Silicon Scaffold of Stable Si6R6 Isomers
Kai Abersfelder; Adam Russell; Henry S. Rzepa; Andrew J. P. White; Peter R. Haycock; David Scheschkewitz; Journal of the American Chemical Society 134 (2012) 16008–16016; doi:10.1021/ja307344f

data_4118688
_publ_section_title
;
 Contraction and Expansion of the Silicon Scaffold of Stable Si6R6 Isomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16008
_journal_page_last               16016
_journal_paper_doi               10.1021/ja307344f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C60 H92 I6 Si5, 1.5(C6 H14)'
_chemical_formula_sum            'C69 H113 I6 Si5'
_chemical_formula_weight         1844.44
_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                90.6585(18)
_cell_angle_beta                 103.886(2)
_cell_angle_gamma                99.861(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1361(4)
_cell_length_b                   15.2175(3)
_cell_length_c                   17.7339(4)
_cell_measurement_reflns_used    17862
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.3151
_cell_measurement_theta_min      2.5683
_cell_volume                     3900.84(16)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32112
_diffrn_reflns_theta_full        71.50
_diffrn_reflns_theta_max         72.46
_diffrn_reflns_theta_min         2.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.756
_exptl_absorpt_correction_T_max  0.306
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) 
(compiled Oct 25 2010,18:11:34) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       'blocky needles'
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.000058(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         15075
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                12651
_reflns_number_total             15075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307344f_si_002_5.cif
_cod_data_source_block           11
_cod_database_code               4118688