Structure, Bonding, and Reactivity of Ti and Zr Amidate Complexes: DFT and X-Ray Crystallographic Studies
Robert K. Thomson; Federico E. Zahariev; Zhe Zhang; Brian O. Patrick; Yan Alexander Wang; Laurel L. Schafer; Inorganic Chemistry 44 (2005) 8680–8689; doi:10.1021/ic0502980

data_4310035
_publ_section_title
;
Structure, Bonding, and Reactivity of Ti and Zr Amidate Complexes: DFT
and X-Ray Crystallographic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8680
_journal_page_last               8689
_journal_paper_doi               10.1021/ic0502980
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C34 H56 N4 O3 Ti'
_chemical_formula_weight         616.73
_chemical_melting_point          'C34 H56 N4 O3 Ti'
_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                102.30(1)
_cell_angle_beta                 90.63(1)
_cell_angle_gamma                110.60(1)
_cell_formula_units_Z            2
_cell_length_a                   9.561(2)
_cell_length_b                   10.519(2)
_cell_length_c                   19.121(3)
_cell_measurement_reflns_used    3050
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.7
_cell_measurement_theta_min      2.15
_cell_volume                     1751.0(6)
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1349
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5454
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9990
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5454
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1198P)^2^+2.5885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2556
_refine_ls_wR_factor_ref         0.2753
_reflns_number_gt                3202
_reflns_number_total             5454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0502980si20050226_101828.cif
_cod_data_source_block           hklf4_1
_cod_database_code               4310035