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_4089245
_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            'C22 H40 Cl Hf N O3 Si4'
_chemical_formula_weight         692.85
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 98.649(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.397(3)
_cell_length_b                   11.523(3)
_cell_length_c                   21.702(5)
_cell_measurement_reflns_used    12344
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.526
_cell_measurement_theta_min      4.820
_cell_volume                     2817.7(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21898
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    3.991
_exptl_absorpt_correction_T_max  0.7153
_exptl_absorpt_correction_T_min  0.4476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.815
_refine_diff_density_min         -1.715
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0376P)^2^+12.3658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                5372
_reflns_number_total             5719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00084_si_002.cif
_cod_data_source_block           5_1183j
_cod_original_cell_volume        2817.6(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4089245