Reactions of d0 Group 4 Amides with Dioxygen. Preparation of Unusual Oxo Aminoxy Complexes and Theoretical Studies of Their Formation
Ruitao Wang; Xin-Hao Zhang; Shu-Jian Chen; Xianghua Yu; Chang-Sheng Wang; David B. Beach; Yun-Dong Wu; Zi-Ling Xue; Journal of the American Chemical Society 127 (2005) 5204–5211; doi:10.1021/ja042307u

data_4111604
_publ_section_title
;
 Reactions of d0 Group 4 Amides with Dioxygen. Preparation of Unusual Oxo
 Aminoxy Complexes and Theoretical Studies of Their Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5204
_journal_page_last               5211
_journal_paper_doi               10.1021/ja042307u
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C20 H60 N10 O2 Zr3'
_chemical_formula_weight         746.44
_chemical_name_common            zirconium
_chemical_name_systematic
; 
 Zirconium amide O2 adduct
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.767(10)
_cell_length_b                   28.493(17)
_cell_length_c                   19.631(7)
_cell_measurement_temperature    173(2)
_cell_volume                     14413(11)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       multi-scan
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33464
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  0.6925
_exptl_absorpt_correction_T_min  0.5981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       fragment
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.99(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         8579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+25.1580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                8267
_reflns_number_total             8579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042307urom20041222_011219.cif
_cod_data_source_block           zro
_cod_original_cell_volume        14413(12)
_cod_database_code               4111604