Genuine Examples of Tetrahedral Tetradentate Sulfide Ligand Bridging Four Pd Atoms: Controlled Formation of [(μ4-S){(μ2-X)Pd2(C^N)2}2] (X = OH or Cl; HC^N =p-C2H5OC6H4CHNC6H4-p-C2H5) Complexes
Rut Benavente; Pablo Espinet; José M. Martín-Álvarez; Jesús A. Miguel; Gabriel Aullón; Inorganic Chemistry 46 (2007) 2035–2040; doi:10.1021/ic061367t

data_4306975
_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
;
Genuine Examples of Tetrahedral Tetradentate Sulfide Ligand Bridging Four
Pd Atoms: Controlled Formation of [(\m4-S){(\m2-X)Pd2(C^N)2}2] (X = OH
or Cl; HC^N =p-C2H5OC6H4CHNC6H4-p-C2H5) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2035
_journal_page_last               2040
_journal_paper_doi               10.1021/ic061367t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C51 H55 N3 O4 Pd3 S'
_chemical_formula_weight         1125.24
_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                69.010(9)
_cell_angle_beta                 86.773(9)
_cell_angle_gamma                76.679(9)
_cell_formula_units_Z            2
_cell_length_a                   9.123(4)
_cell_length_b                   15.099(6)
_cell_length_c                   18.519(7)
_cell_measurement_temperature    298(2)
_cell_volume                     2316.6(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10936
_diffrn_reflns_theta_full        23.38
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.779657
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         6675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          4.846
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                5249
_reflns_number_total             6675
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061367tsi20061027_021425_1.cif
_cod_data_source_block           2
_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 

2020-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C102 H110 N6 O8 Pd6 S2'
_cod_original_formula_weight         2250.48
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2316.5(16)
_cod_database_code               4306975