Palladium(II)-Induced Activation of Carbon-Nitrogen Single Bond of Coordinated N4S Ligand. Characterization of Product with Modified Ligand Structure: Kinetics versus Thermodynamic Considerations
Sudeep Bhattacharyya; Timothy J. R. Weakley; Muktimoy Chaudhury; Inorganic Chemistry 38 (1999) 5453–5456; doi:10.1021/ic9813720

data_4322367
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Palladium(II)-Induced Activation of Carbon-Nitrogen Single Bond of
 Coordinated N4S Ligand. Characterization of Product with Modified Ligand
 Structure: Kinetics versus Thermodynamic Considerations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5453
_journal_page_last               5456
_journal_paper_doi               10.1021/ic9813720
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural
'((C10 H17 N2 Pd S2 )2 (C5 H7 N2 ) 1+) (Cl O4 1-)'
_chemical_formula_sum            'C25 H41 Cl N6 O4 Pd2 S4'
_chemical_formula_weight         866.13
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      45
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.056(3)
_cell_length_b                   11.248(1)
_cell_length_c                   16.188(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      26.0
_cell_volume                     3469.8(9)
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.01069
_diffrn_orient_matrix_UB_12      -0.03539
_diffrn_orient_matrix_UB_13      0.06381
_diffrn_orient_matrix_UB_21      -0.00820
_diffrn_orient_matrix_UB_22      -0.03705
_diffrn_orient_matrix_UB_23      -0.06184
_diffrn_orient_matrix_UB_31      0.06029
_diffrn_orient_matrix_UB_32      -0.01131
_diffrn_orient_matrix_UB_33      0.00288
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1722
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0.19
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  1.236
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.49
_refine_ls_abs_structure_details 'No change when z axis reversed'
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.99
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         1379
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0330
_refine_ls_shift/esd_max         0.063
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0377
_reflns_number_observed          1379
_reflns_number_total             1722
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic9813720_2.cif
_cod_data_source_block           compound_3b_C21H31ClN6O4PdS2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3469(1)
_cod_original_sg_symbol_H-M      'I b a 2 '
_cod_original_formula_sum        'C25 H41 Cl N6 O4 Pd2 S4 '
_cod_database_code               4322367