Synthesis and Reactivity toward Isonitriles of (2-Aminoaryl)palladium(II) Complexes
José Vicente; José-Antonio Abad; Andrew D. Frankland; Joaquín López-Serrano; M. Carmen Ramírez de Arellano; Peter G. Jones; Organometallics 21 (2002) 272–282; doi:10.1021/om0104971

data_4060842
_publ_section_title
;
 Synthesis and Reactivity toward Isonitriles of
 (2-Aminoaryl)palladium(II) Complexes
;
_journal_name_full               Organometallics
_journal_page_first              272
_journal_page_last               282
_journal_paper_doi               10.1021/om0104971
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C46.5 H43 Cl3 F6 N6 O6 Pd S2'
_chemical_formula_weight         1172.74
_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   'Fourier NH, others geom'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.938(14)
_cell_angle_beta                 103.146(12)
_cell_angle_gamma                111.112(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6708(18)
_cell_length_b                   14.029(2)
_cell_length_c                   18.294(3)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.34
_cell_measurement_theta_min      6.15
_cell_volume                     2596.4(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'SHELXTL v5.1 (Bruker, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  Siemens-P4
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9284
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.8053
_exptl_absorpt_correction_T_min  0.6988
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    'NH free, Me rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         8881
_refine_ls_number_restraints     605
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0608P)^2^+7.4858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                7391
_reflns_number_total             8881
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46.50 H43 Cl3 F6 N6 O6 Pd S2'
_cod_database_code               4060842