Novel Cyclopalladated Imino-thiophenes: Synthesis and Reactivity Toward Alkynes and Carbon Monoxide
Luciano Cuesta; Dune Prat; Tatiana Soler; Rafael Navarro; Esteban P. Urriolabeitia; Inorganic Chemistry 50 (2011) 8598–8607; doi:10.1021/ic201158v

data_4326172
_publ_contact_author_address
;
ICMA, CSIC-Universidad de Zaragoza, Plaza S. Francisco, 
50009 Zaragoza (Spain)
;
_publ_contact_author_email       esteban@unizar.es
_publ_contact_author_fax         (+34)976761187
_publ_contact_author_name        'Esteban P. Urriolabeitia'
_publ_contact_author_phone       (+34)976762302
_publ_section_title
;
 Novel Cyclopalladated Imino-thiophenes: Synthesis and Reactivity Toward
 Alkynes and Carbon Monoxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8598
_journal_page_last               8607
_journal_paper_doi               10.1021/ic201158v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C22 H16 N2 Pd S2'
_chemical_formula_sum            'C22 H16 N2 Pd S2'
_chemical_formula_weight         478.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.676(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.5125(13)
_cell_length_b                   10.2662(8)
_cell_length_c                   22.1841(17)
_cell_measurement_reflns_used    6531
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.34
_cell_volume                     3742.2(5)
_computing_cell_refinement       'Bruker SMART V5.625'
_computing_data_collection       'Bruker SMART V5.625'
_computing_data_reduction        'Bruker SAINT V6.28A'
_computing_molecular_graphics    'SHELXTL  Rel. 6.12/V (Siemens, 1996)'
_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(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22231
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.7733
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker/Siemens SADABS V2.03'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+1.2157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                4713
_reflns_number_total             5464
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201158v_si_002_3.cif
_cod_data_source_block           '__6a'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4326172