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_4066928
_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         'C19 H35 B O2 Si3'
_chemical_formula_sum            'C19 H35 B O2 Si3'
_chemical_formula_weight         390.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.14(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9177(17)
_cell_length_b                   11.9574(12)
_cell_length_c                   10.3355(16)
_cell_measurement_reflns_used    3286
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      7.15
_cell_volume                     1213.3(3)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16219
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.8563
_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    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thick_plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6149
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0824P)^2^+0.2881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5711
_reflns_number_total             6149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100720k_si_002.cif
_cod_data_source_block           glu03f
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4066928