Selective Derivatization and Characterization of Bifunctional “Janus-Type” Cyclotetrasiloxanes
Panisch, Robin; Bassindale, Alan R.; Korlyukov, Alexander A.; Pitak, Mateusz B.; Coles, Simon J.; Taylor, Peter G.; Organometallics 32 (2013) 1732–; doi:10.1021/om301158w

data_4080387
_publ_section_title
;
 Selective Derivatization and Characterization of Bifunctional
 &#x201C;Janus-Type&#x201D; Cyclotetrasiloxanes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1732
_journal_paper_doi               10.1021/om301158w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C94 H90 O8 Si8'
_chemical_formula_sum            'C94 H90 O8 Si8'
_chemical_formula_weight         1572.38
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-08
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   68.514(6)
_cell_length_b                   68.514(6)
_cell_length_c                   10.8220(10)
_cell_measurement_reflns_used    9463
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.03
_cell_measurement_theta_min      2.25
_cell_volume                     43994(7)
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_limit_h_max       84
_diffrn_reflns_limit_h_min       -84
_diffrn_reflns_limit_k_max       84
_diffrn_reflns_limit_k_min       -84
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            140449
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         0.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.7996.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14940
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         19230
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.1019
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+204.6780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2507
_reflns_number_gt                7874
_reflns_number_total             19230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301158w_si_001.cif
_cod_data_source_block           cts21
_cod_database_code               4080387