Cyclopalladated compounds derived from a [C,N,S] terdentate ligand: synthesis, characterization and reactivity. Crystal and molecular structures of [Pd{2-ClC6H3C(H)NCH2CH2SMe}(Cl)] and [{Pd[2-ClC6H3C(H)NCH2CH2SMe]}2{µ-Ph2P(CH2)4PPh2}][CF3SO3]2
Fernández, Alberto; Vázquez-García, Digna; Fernández, Jesús J.; López-Torres, Margarita; Suárez, Antonio; Castro-Juiz, Samuel; Ortigueira, Juan M.; Vila, José M.; New Journal of Chemistry 26 (2002) 105–; doi:10.1039/b106511d

data_7050698
_publ_section_title
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 Cyclopalladated compounds derived from a [C,N,S] terdentate ligand:
 synthesis, characterization and reactivity. Crystal and molecular
 structures of [Pd{2-ClC6H3C(H)&#xE006;NCH2CH2SMe}(Cl)] and
 [{Pd[2-ClC6H3C(H)&#xE006;NCH2CH2SMe]}2{&#x00B5;-Ph2P(CH2)4PPh2}][CF3SO3]2
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              105
_journal_paper_doi               10.1039/b106511d
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C50 H50 Cl2 F6 N2 O6 P2 Pd2 S4'
_chemical_formula_weight         1362.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   '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                74.691(3)
_cell_angle_beta                 82.642(3)
_cell_angle_gamma                82.434(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3501(15)
_cell_length_b                   11.1288(16)
_cell_length_c                   12.7800(19)
_cell_measurement_reflns_used    190
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      1.66
_cell_volume                     1400.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9629
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        <1%
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1513
_reflns_number_gt                4357
_reflns_number_total             6726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106511d.txt
_cod_data_source_block           11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050698