5,6-Disubstituted 1,2,3-Trisilaindanes as Silicon Analogues of Phantolide-Type Musk Odorants: Synthesis, Structure, Reactivity, and Olfactory Properties§
Gluyas, Josef B. G.; Burschka, Christian; Kraft, Philip; Tacke, Reinhold; Organometallics 29 (2010) 5897–; doi:10.1021/om100720k

data_4066929
_publ_section_title
;
 5,6-Disubstituted 1,2,3-Trisilaindanes as Silicon Analogues of
 Phantolide-Type Musk Odorants: Synthesis, Structure, Reactivity, and
 Olfactory Properties&#x00A7;
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5897
_journal_paper_doi               10.1021/om100720k
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C16 H28 O Si3'
_chemical_formula_sum            'C16 H28 O Si3'
_chemical_formula_weight         320.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 89.999(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.8718(13)
_cell_length_b                   35.093(4)
_cell_length_c                   10.3208(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      7.6
_cell_volume                     3937.6(8)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  image_plate_Stoe-IPDS
_diffrn_measurement_method       'omega scan'
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47192
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.9539
_exptl_absorpt_correction_T_min  0.8537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0672P)^2^+0.9943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                8495
_reflns_number_total             9388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100720k_si_002.cif
_cod_data_source_block           glu04g
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066929