Synthesis and Characterization of a Series of (Hydroperoxo)-, (Alkylperoxo)-, and (μ-Peroxo)palladium Complexes Containing the Hydrotris(3,5-diisopropylpyrazolyl)borato Ligand (TpiPr2): (TpiPr2)(py)Pd-OO-X [X = H, t-Bu, Pd(TpiPr2)(py)] and (TpiPr2)(py)Pd-(μ-κ1:κ2-OO)-PdTpiPr2
Taichi Miyaji; Masato Kujime; Shiro Hikichi; Yoshihiko Moro-oka; Munetaka Akita; Inorganic Chemistry 41 (2002) 5286–5295; doi:10.1021/ic020355e

data_4318595
_publ_section_title
;
 Synthesis and Characterization of a Series of (Hydroperoxo)-,
 (Alkylperoxo)-, and (\m-Peroxo)palladium Complexes Containing the
 Hydrotris(3,5-diisopropylpyrazolyl)borato Ligand (TpiPr2):
 (TpiPr2)(py)Pd-OO-X [X = H, t-Bu, Pd(TpiPr2)(py)] and
 (TpiPr2)(py)Pd-(\m-\k1:\k2-OO)-PdTpiPr2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5286
_journal_page_last               5295
_journal_paper_doi               10.1021/ic020355e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C36 H60 B N7 O2 Pd'
_chemical_formula_weight         740.12
_chemical_name_common            'compound 3'
_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                109.69(6)
_cell_angle_beta                 92.41(7)
_cell_angle_gamma                88.66(5)
_cell_formula_units_Z            2
_cell_length_a                   13.002(7)
_cell_length_b                   14.579(7)
_cell_length_c                   11.293(14)
_cell_measurement_temperature    213(2)
_cell_volume                     2014(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7854
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.499
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_refine_diff_density_max         2.054
_refine_diff_density_min         -2.452
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.752
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.752
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2158
_refine_ls_wR_factor_ref         0.2212
_reflns_number_gt                7578
_reflns_number_total             7854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020355e_2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2020-11-04
Z value changed to be consistent with given formula
                 miguel
;
_cod_original_formula_units_Z    1
_cod_database_code               4318595