Interaction of hydroperoxopalladium complexes, (TpR)(py)Pd-OOH, with hydroxo-nickel and -cobalt complexes, [(μ-OH)(MTpR')]2 (M = Ni, Co), leading to oxidative dehydrogenation of the saturated hydrocarbyl moiety in the ancillary ligand (TpiPr2)
Kujime, Masato; Hikichi, Shiro; Akita, Munetaka; Dalton Transactions 2003 (2003) 3506–; doi:10.1039/b307262m

data_7013379
_publ_section_title
;
 Interaction of hydroperoxopalladium complexes, (TpR)(py)Pd-OOH, with
 hydroxo-nickel and -cobalt complexes, [(\m-OH)(MTpR')]2 (M = Ni,
 Co), leading to oxidative dehydrogenation of the saturated hydrocarbyl
 moiety in the ancillary ligand (TpiPr2)
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3506
_journal_paper_doi               10.1039/b307262m
_journal_volume                  2003
_journal_year                    2003
_chemical_formula_moiety         'C46 H74 B2 N14 O2 Ni Pd '
_chemical_formula_sum            'C46 H74 B2 N14 Ni O2 Pd'
_chemical_formula_weight         1041.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Thu Jul 17 21:27:12 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 94.160(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.458(3)
_cell_length_b                   9.007(1)
_cell_length_c                   26.689(4)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    213.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      0.8
_cell_volume                     5384.4(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11219
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.50
_refine_diff_density_min         -1.20
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     612
_refine_ls_number_reflns         3583
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.0330
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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_ref         0.2352
_reflns_number_gt                3583
_reflns_number_total             7556
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b307262m.txt
_cod_data_source_block           compound_5c(Ni)
_cod_original_cell_volume        5384(1)
_cod_original_formula_sum        'C46 H74 B2 N14 O2 Ni Pd '
_cod_database_code               7013379