Reactions of zirconium amide amidinates with dioxygen. Observation of an unusual peroxo intermediate in the formation of oxo compounds
Adam C. Lamb; Zheng Lu; Zi-Ling Xue; Chem.Commun. 50 (2014) 10517–; doi:10.1039/C4cc04032E

data_7115557
_publ_section_title
;
 Reactions of zirconium amide amidinates with dioxygen. Observation of an
 unusual peroxo intermediate in the formation of oxo compounds
;
_journal_name_full               Chem.Commun.
_journal_page_first              10517
_journal_paper_doi               10.1039/C4cc04032E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C48 H102 N12 O6 Zr3'
_chemical_formula_weight         1217.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.2850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4504(4)
_cell_length_b                   13.3481(2)
_cell_length_c                   20.7646(3)
_cell_measurement_temperature    100(2)
_cell_volume                     6325.76(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            87696
_diffrn_reflns_theta_full        29.59
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.9485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         17768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.9273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                14696
_reflns_number_total             17768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04032e2.cif
_cod_data_source_block           Zr-peroxo
_cod_original_sg_symbol_H-M      'p 21/c'
_cod_database_code               7115557