Titanium alkoxyimido (Ti=N-OR) complexes: reductive N-O bond cleavage at the boundary between hydrazide and peroxide ligands
Andrew D. Schwarz; Ainara Nova; Eric Clot; Philip Mountford; Chem.Commun. 47 (2011) 4926–; doi:10.1039/c1cc10862j

data_7106309
_publ_section_title
;
 Titanium alkoxyimido (Ti=N-OR) complexes: reductive N-O bond cleavage at
 the boundary between hydrazide and peroxide ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              4926
_journal_paper_doi               10.1039/c1cc10862j
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H43 N5 O1 Si2 Ti1'
_chemical_formula_sum            'C20 H43 N5 O Si2 Ti'
_chemical_formula_weight         473.67
_chemical_name_systematic        Ti(N2NMe)(NOtBu)(py)
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0550(2)
_cell_length_b                   15.5409(3)
_cell_length_c                   17.4207(4)
_cell_measurement_reflns_used    3372
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2722.22(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22523
_diffrn_reflns_theta_full        26.631
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         5.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.28
_refine_ls_abs_structure_details 'Flack (1983), 1762 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.0006135
_refine_ls_shift/su_mean         0.0012877
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.743 0.245 0.577 0.352E-01 0.189
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0790
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0457
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4759
_reflns_number_total             6101
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      10.90
_oxford_refine_ls_r_factor_ref   0.0390
_oxford_refine_ls_scale          0.3053(4)
_oxford_reflns_number_all        6101
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c1cc10862j.txt
_cod_data_source_block           COMPOUND_4a
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C20 H43 N5 O1 Si2 Ti1'
_cod_database_code               7106309