Tuning the Si-N Interaction in Metalated Oligosilanylsilatranes.
Aghazadeh Meshgi, Mohammad; Zitz, Rainer; Walewska, Małgorzata; Baumgartner, Judith; Marschner, Christoph; Organometallics 36 (2017) 1365–1371; doi:10.1021/acs.organomet.7b00084

data_4089247
_publ_section_title
;
 Tuning the Si-N Interaction in Metalated Oligosilanylsilatranes.
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1365
_journal_page_last               1371
_journal_paper_doi               10.1021/acs.organomet.7b00084
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C32 H76 N2 O8 Si8 Yb'
_chemical_formula_weight         1014.71
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                81.587(3)
_cell_angle_beta                 87.487(2)
_cell_angle_gamma                86.698(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9691(12)
_cell_length_b                   15.4589(19)
_cell_length_c                   16.395(2)
_cell_measurement_reflns_used    2112
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      48.800
_cell_measurement_theta_min      4.722
_cell_volume                     2493.7(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       '\w scans'
_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  0.0849
_diffrn_reflns_av_sigmaI/netI    0.1488
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20142
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  0.8839
_exptl_absorpt_correction_T_min  0.7859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         2.273
_refine_diff_density_min         -2.667
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         10041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                7449
_reflns_number_total             10041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00084_si_002.cif
_cod_data_source_block           7_1159j
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089247