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_4318594
_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            'C47 H66 B Cl4 N6 O2 P Pd'
_chemical_formula_weight         1037.04
_chemical_name_common            'compound 2b'
_chemical_name_systematic
;
    ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   21.1718(11)
_cell_length_b                   16.9093(7)
_cell_length_c                   14.7058(6)
_cell_measurement_temperature    213(2)
_cell_volume                     5264.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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    0.1133
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5905
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.627
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2160
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         5905
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.893
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.244
_refine_ls_shift/su_mean         0.010
_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          0.2199
_refine_ls_wR_factor_ref         0.2218
_reflns_number_gt                5640
_reflns_number_total             5905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020355e_1.cif
_cod_data_source_block           shelxl
_cod_database_code               4318594