On the Quest for New Mixed-Metal μ-Oxo-bridged Complexes: Synthesis of Compounds Containing Transition Metal-Oxygen-Main Group Metal Motifs M-O-M1 (M = Ti, Zr; M1= Al, Ga) without Cyclopentadienyl Ligands
Grigory B. Nikiforov; Herbert W. Roesky; Thomas Schulz; Dietmar Stalke; M. Witt; Inorganic Chemistry 47 (2008) 6435–6443; doi:10.1021/ic800567g

data_4305580
_publ_contact_author             'Prof. Dr. H. W. Roesky'
_publ_contact_author_email       hroesky@gwdg.de
_publ_section_title
;
On the Quest for New Mixed-Metal \m-Oxo-bridged Complexes: Synthesis of
Compounds Containing Transition Metal-Oxygen-Main Group Metal Motifs
M-O-M1 (M = Ti, Zr; M1= Al, Ga) without Cyclopentadienyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6435
_journal_page_last               6443
_journal_paper_doi               10.1021/ic800567g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C62 H86 Ga6 N2 O7 Ti'
_chemical_formula_weight         1437.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                81.7410(10)
_cell_angle_beta                 81.7230(10)
_cell_angle_gamma                77.0610(10)
_cell_formula_units_Z            4
_cell_length_a                   12.9331(12)
_cell_length_b                   14.5324(14)
_cell_length_c                   35.544(3)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.8145
_cell_measurement_theta_min      2.246
_cell_volume                     6399.9(10)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.1.0'
_computing_data_reduction        'SAINT V7.23A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.12'
_computing_publication_material  'XP in SHELXTL ver. 6.12'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.12'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.12'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Bruker TXS-Mo rotating anode with APEX II detector'
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            107136
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.889277
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         23474
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0321P)^2^+9.3272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                16568
_reflns_number_total             23474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800567g-file003_3.cif
_cod_data_source_block           gatio
_cod_database_code               4305580