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_4320065
_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 O2 P2 Pd S '
_chemical_formula_sum            'C16 H30 O2 P2 Pd S'
_chemical_formula_weight         454.82
_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 Oct 16 12:48:44 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 94.59(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.244(4)
_cell_length_b                   17.519(3)
_cell_length_c                   13.854(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290.2
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      13.7
_cell_volume                     1994.5(12)
_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      -0.00132
_diffrn_orient_matrix_UB_12      -0.03478
_diffrn_orient_matrix_UB_13      0.05717
_diffrn_orient_matrix_UB_21      -0.00583
_diffrn_orient_matrix_UB_22      0.04522
_diffrn_orient_matrix_UB_23      0.04363
_diffrn_orient_matrix_UB_31      -0.12154
_diffrn_orient_matrix_UB_32      -0.00179
_diffrn_orient_matrix_UB_33      -0.00851
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  8.06
_diffrn_reflns_number            3932
_diffrn_reflns_theta_max         25.05
_diffrn_standards_decay_%        -2.20
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            colourlessprism
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       prism
_exptl_crystal_F_000             936.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         -0.61
_refine_diff_density_min         1.39
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2234
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0391
_refine_ls_shift/esd_max         0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0452
_reflns_number_observed          2234
_reflns_number_total             3932
_reflns_observed_criterion       3.00
_cod_data_source_file            ic010114r_3.cif
_cod_data_source_block           '[PD(ME3P)2(SO2CH2C(ME2)PH]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 52 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1994(1)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C16 H30 O2 P2 Pd S '
_cod_database_code               4320065