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_4305579
_publ_contact_author             'Prof. Dr. Dietmar Stalke'
_publ_contact_author_email       dstalke@chemie.uni-goettingen.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            'C76 H107 Al2 N4 O3 Zr'
_chemical_formula_weight         1269.84
_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                111.6850(10)
_cell_angle_beta                 93.8700(10)
_cell_angle_gamma                109.3090(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2881(9)
_cell_length_b                   17.1318(13)
_cell_length_c                   19.858(2)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.022
_cell_measurement_theta_min      2.567
_cell_volume                     3579.3(5)
_computing_cell_refinement       'SAINT V7.23A'
_computing_data_collection       'APEX2 v2.0-2'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega 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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37690
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.815451
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12607
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+2.3106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                10735
_reflns_number_total             12607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800567g-file003_2.cif
_cod_data_source_block           nikifurovzr
_cod_database_code               4305579