Synthesis and Insertion Reactions of the Cyclometalated Palladium-Alkyl Complexes Pd(CH2CMe2-o-C6H4)L2. Observation of a Pentacoordinated Intermediate in the Insertion of SO2
J. Cámpora; J. A. López; P. Palma; D. del Rio; E. Carmona; P. Valerga; C. Graiff; A. Tiripicchio; Inorganic Chemistry 40 (2001) 4116–4126; doi:10.1021/ic010114r

data_4320063
_publ_section_title
;
 Synthesis and Insertion Reactions of the Cyclometalated Palladium-Alkyl
 Complexes Pd(CH2CMe2-o-C6H4)L2. Observation of a Pentacoordinated
 Intermediate in the Insertion of SO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4116
_journal_page_last               4126
_journal_paper_doi               10.1021/ic010114r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C16 H30 P2 Pd '
_chemical_formula_sum            'C16 H30 P2 Pd'
_chemical_formula_weight         390.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Mon Sep 11 11:13:10 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 93.90(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.331(3)
_cell_length_b                   16.349(1)
_cell_length_c                   12.628(3)
_cell_measurement_reflns_used    11
_cell_measurement_temperature    290.2
_cell_measurement_theta_max      41.4
_cell_measurement_theta_min      39.2
_cell_volume                     1922.0(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      290.2
_diffrn_measurement_device       AFC6S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.00834
_diffrn_orient_matrix_UB_12      -0.05632
_diffrn_orient_matrix_UB_13      0.02986
_diffrn_orient_matrix_UB_21      -0.06308
_diffrn_orient_matrix_UB_22      0.02150
_diffrn_orient_matrix_UB_23      0.05454
_diffrn_orient_matrix_UB_31      -0.08655
_diffrn_orient_matrix_UB_32      -0.01032
_diffrn_orient_matrix_UB_33      -0.04933
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuKalpha
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  16.51
_diffrn_reflns_number            6109
_diffrn_reflns_theta_max         60.07
_diffrn_standards_decay_%        -10.00
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.476
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       irregular
_exptl_crystal_F_000             808.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.240
_refine_diff_density_max         -0.91
_refine_diff_density_min         0.73
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.704
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1663
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0716
_refine_ls_shift/esd_max         0.2521
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0864
_reflns_number_observed          1663
_reflns_number_total             6109
_reflns_observed_criterion       3.00
_cod_data_source_file            ic010114r_1.cif
_cod_data_source_block           '[Pd(PMe3)2(CH2CMe2Ph)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 49 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1922(1)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C16 H30 P2 Pd '
_cod_database_code               4320063