One Pot Synthesis of Disilatricycloheptene Analogue and Jutzi's Disilene
Shabana Khan; Sakya S. Sen; Herbert W. Roesky; Daniel Kratzert; Reent Michel; Dietmar Stalke; Inorganic Chemistry 49 (2010) 9689–9693; doi:10.1021/ic101552r

data_4316869
_publ_section_title
;
 One Pot Synthesis of Disilatricycloheptene Analogue and Jutzi's Disilene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9689
_journal_page_last               9693
_journal_paper_doi               10.1021/ic101552r
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C32 H66 N2 Si6'
_chemical_formula_weight         647.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.668(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.655(3)
_cell_length_b                   10.1597(15)
_cell_length_c                   23.368(4)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.21
_cell_volume                     3921.7(11)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2009.11'
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_refinement  'SHELXS in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            102129
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         9365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0487P)^2^+2.2392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                7585
_reflns_number_total             9365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101552r_si_003.cif
_cod_data_source_block           p21n
_cod_original_cell_volume        3921.9(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4316869