Imido-Bridged Homo- and Heterobimetallic Complexes
Christian Lorber; Laure Vendier; Inorganic Chemistry 50 (2011) 9927–9929; doi:10.1021/ic201466f

data_4326553
_publ_contact_author
;
Christian Lorber
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       lorber@lcc-toulouse.fr
_publ_section_title
;
 Imido-Bridged Homo- and Heterobimetallic Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9927
_journal_page_last               9929
_journal_paper_doi               10.1021/ic201466f
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H63 N7 Ti1 Zr1'
_chemical_formula_sum            'C32 H63 N7 Ti Zr'
_chemical_formula_weight         685.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                99.137(4)
_cell_angle_beta                 96.922(4)
_cell_angle_gamma                96.429(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1482(6)
_cell_length_b                   11.2282(6)
_cell_length_c                   16.9595(9)
_cell_measurement_reflns_used    4226
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.2214
_cell_measurement_theta_min      2.7462
_cell_measurement_wavelength     0.71073
_cell_volume                     2062.0(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0545253907
_diffrn_orient_matrix_UB_12      0.0269311149
_diffrn_orient_matrix_UB_13      0.0003783241
_diffrn_orient_matrix_UB_21      0.0344899157
_diffrn_orient_matrix_UB_22      0.0574976623
_diffrn_orient_matrix_UB_23      0.0157968084
_diffrn_orient_matrix_UB_31      0.0034476168
_diffrn_orient_matrix_UB_32      0.0109668485
_diffrn_orient_matrix_UB_33      -0.0397432875
_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  0.0724
_diffrn_reflns_av_unetI/netI     0.1218
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15051
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.84161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.27 (release 29-05-2008 CrysAlis171 .NET)
        (compiled May 29 2008,13:12:44)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.115
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                4517
_reflns_number_total             7536
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201466f_si_001_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        2061.98(19)
_cod_database_code               4326553