N/O- and C-Bound (Enolato)palladium Complexes with Hydrotris(pyrazolyl)borato Ligands (TpR: R = iPr2, Me2) Obtained via Dehydrative Condensation between the Hydroxo Complexes TpRPd(Py)OH and Active Methylene Compounds: Factors Determining the Isomer Distribution and Dimerization of Cyano Compounds
Kujime, Masato; Hikichi, Shiro; Akita, Munetaka; Organometallics 20 (2001) 4049–; doi:10.1021/om010448o

data_4089311
_publ_section_title
;
 N/O- and C-Bound (Enolato)palladium Complexes with
 Hydrotris(pyrazolyl)borato Ligands (TpR:&#x00A0; R = iPr2, Me2) Obtained
 via Dehydrative Condensation between the Hydroxo Complexes TpRPd(Py)OH
 and Active Methylene Compounds:&#x00A0; Factors Determining the Isomer
 Distribution and Dimerization of Cyano Compounds
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4049
_journal_paper_doi               10.1021/om010448o
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C40.5 H62 B Cl N9 O4 Pd'
_chemical_formula_weight         891.65
_chemical_name_common            'compound 6iPr2b'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                98.428(19)
_cell_angle_beta                 97.843(4)
_cell_angle_gamma                80.516(18)
_cell_formula_units_Z            2
_cell_length_a                   10.378(3)
_cell_length_b                   22.092(4)
_cell_length_c                   10.381(3)
_cell_measurement_temperature    213(2)
_cell_volume                     2306.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.768
_diffrn_measured_fraction_theta_max 0.768
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1110
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8142
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.508
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_refine_diff_density_max         0.829
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_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          0.2069
_refine_ls_wR_factor_ref         0.2209
_reflns_number_gt                5121
_reflns_number_total             8142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010448o.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
 Corrected the values of the '_diffrn_radiation_type' and
 '_refine_ls_weighting_details' data items by replacing a
 sequence of malformed symbols with the backslash symbol ('\')
 after consulting the original publication.

 Antanas Vaitkus,
 2019-12-11
;
_cod_original_cell_volume        2306.6(10)
_cod_original_formula_sum        'C40.50 H62 B Cl N9 O4 Pd'
_cod_database_code               4089311