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_4322395
_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            'C35 H47 N3 O2 Ru Si4 Ti'
_chemical_formula_weight         803.09
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.63(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.424(3)
_cell_length_b                   19.497(4)
_cell_length_c                   16.504(4)
_cell_measurement_reflns_used    45
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.60
_cell_measurement_theta_min      2.99
_cell_volume                     3989.8(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8518
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.3091
_exptl_absorpt_correction_T_min  0.2373
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.291
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_obs          0.0431
_refine_ls_shift/esd_max         0.078
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.8323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1418
_refine_ls_wR_factor_obs         0.1042
_reflns_number_observed          5034
_reflns_number_total             6986
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990562n_1.cif
_cod_data_source_block           si018
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.8323P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.8323P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3989.8(15)
_cod_database_code               4322395