Formation of Trinuclear Palladium Orthometalated Complexes with Unprecedented Asymmetrical (μ3-S)(μ3-X) Bridges (X = OH, SR, O2CR) from μ2-Hydroxo Dimeric Complexes and CS2
Pablo Espinet; Celia Hernández; José M. Martín-Alvarez; Jesús A. Miguel; Inorganic Chemistry 43 (2004) 843–845; doi:10.1021/ic0351085

data_4310566
_publ_contact_author
;
 Jose M. Martin-Alvarez
 Departamento de Quimica Inorganica
 Facultad de Ciencias
 Universidad de Valladolid
 E47005
 Valladolid
 Spain
;
_publ_contact_author_email       jmmartin@qi.uva.es
_publ_contact_author_fax         '+34 983 423013'
_publ_contact_author_phone       '+34 983 423232'
_publ_section_title
;
 Formation of Trinuclear Palladium Orthometalated Complexes with
 Unprecedented Asymmetrical (\m3-S)(\m3-X) Bridges (X = OH, SR, O2CR) from
 \m2-Hydroxo Dimeric Complexes and CS2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              843
_journal_page_last               845
_journal_paper_doi               10.1021/ic0351085
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C57 H67 Cl4 N3 O6 Pd3 S2'
_chemical_formula_weight         1415.26
_chemical_name_systematic
; 
 ? 
;
_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                80.885(15)
_cell_angle_beta                 82.382(15)
_cell_angle_gamma                78.950(14)
_cell_formula_units_Z            2
_cell_length_a                   13.630(10)
_cell_length_b                   14.167(11)
_cell_length_c                   16.393(12)
_cell_measurement_temperature    298(2)
_cell_volume                     3050(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14026
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.640120
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.860
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         8713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          2.952
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                5872
_reflns_number_total             8713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351085si20030919_020201.cif
_cod_data_source_block           ch135
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310566