Synthesis and Characterization of Dicyclopalladated Complexes of Azobenzene Derivatives by Experimental and Computational Methods
Darko Babić; Manda Ćurić; Krešimir Molčanov; Gregor Ilc; Janez Plavec; Inorganic Chemistry 47 (2008) 10446–10454; doi:10.1021/ic8010234

data_4306100
_publ_contact_author_address
;
Institute Rudjer Boskovic
Bijenicka 54
HR-10002 Zagreb
Croatia
;
_publ_contact_author_email       dbabic@irb.hr
_publ_contact_author_fax         385(1)4680245
_publ_contact_author_name        'Darko Babic'
_publ_contact_author_phone       385(1)4651013
_publ_section_title
;
Synthesis and Characterization of Dicyclopalladated Complexes of Azobenzene
Derivatives by Experimental and Computational Methods
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10446
_journal_page_last               10454
_journal_paper_doi               10.1021/ic8010234
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C18 H24 Cl2 N2 O2 Pd2 S2'
_chemical_formula_sum            'C18 H24 Cl2 N2 O2 Pd2 S2'
_chemical_formula_weight         648.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2004-04-20T15:35:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.916(4)
_cell_angle_beta                 81.087(4)
_cell_angle_gamma                67.428(4)
_cell_formula_units_Z            1
_cell_length_a                   6.5629(4)
_cell_length_b                   7.2720(3)
_cell_length_c                   12.5433(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.21
_cell_measurement_theta_min      6.59
_cell_measurement_wavelength     1.54184
_cell_volume                     545.93(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54179
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2486
_diffrn_reflns_theta_full        76.37
_diffrn_reflns_theta_max         76.37
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.476
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.2742
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   4
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.63
_refine_diff_density_min         -1.03
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.7952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                1913
_reflns_number_total             2298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8010234_si_002_4.cif
_cod_data_source_block           2b
_cod_database_code               4306100
_exptl_absorpt_factor_mur        0.523
_exptl_absorpt_correction_t_ave  0.4616
_exptl_absorpt_rmerge_before     0.0156
_exptl_absorpt_rmerge_after      0.0156
_exptl_absorpt_theta_corr_max    0.9996
_exptl_absorpt_theta_corr_min    0.9191