Synthesis and Reactivity of Early-Late Heterodinuclear Complexes Stabilized by a Trisilylsilane-Based Tripodal Amido Ligand
Lutz H. Gade; Martin Schubart; Bernd Findeis; Sylvie Fabre; Izoldi Bezougli; Matthias Lutz; Ian J. Scowen; Mary McPartlin; Inorganic Chemistry 38 (1999) 5282–5294; doi:10.1021/ic990562n

data_4322413
_publ_section_title
;
 Synthesis and Reactivity of Early-Late Heterodinuclear Complexes
 Stabilized by a Trisilylsilane-Based Tripodal Amido Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5282
_journal_page_last               5294
_journal_paper_doi               10.1021/ic990562n
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C32 H38 F3 Fe N3 O2 Si4 Ti'
_chemical_formula_weight         769.76
_chemical_name_systematic
; 
 ? 
;
_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                 112.939(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.903(2)
_cell_length_b                   10.572(4)
_cell_length_c                   19.111(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3703.2(16)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       theta/2theta
_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  0.1386
_diffrn_reflns_av_sigmaI/netI    0.3008
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3338
_diffrn_reflns_theta_full        18.00
_diffrn_reflns_theta_max         18.00
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.9063
_exptl_absorpt_correction_T_min  0.6746
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   DIFABS
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          o.32
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         2548
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.2591
_refine_ls_R_factor_gt           0.0974
_refine_ls_shift/su_max          1.500
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1574
_reflns_number_gt                996
_reflns_number_total             2548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990562n_3.cif
_cod_data_source_block           sh157
_cod_original_cell_volume        3703.5(14)
_cod_database_code               4322413