Carbon−Nitrogen Bond-Forming Reactions of Palladacycles with Hypervalent Iodine Reagents
Dick, Allison R.; Remy, Matthew S.; Kampf, Jeff W.; Sanford, Melanie S.; Organometallics 26 (2007) 1365–; doi:10.1021/om061052l

data_4072804
_publ_section_title
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 Carbon&#x2212;Nitrogen Bond-Forming Reactions of Palladacycles with
 Hypervalent Iodine Reagents
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1365
_journal_paper_doi               10.1021/om061052l
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C26 H22 N4 O4 Pd S2'
_chemical_formula_sum            'C26 H22 N4 O4 Pd S2'
_chemical_formula_weight         625.00
_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                93.819(6)
_cell_angle_beta                 97.112(6)
_cell_angle_gamma                99.438(6)
_cell_formula_units_Z            4
_cell_length_a                   9.011(2)
_cell_length_b                   13.302(3)
_cell_length_c                   21.558(5)
_cell_measurement_reflns_used    5918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.57
_cell_volume                     2519.5(10)
_computing_cell_refinement       'Bruker APEX2 v1.0-27'
_computing_data_collection       'Bruker APEX2 v1.0-27'
_computing_data_reduction        'Bruker SAINT v7.06a'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.77580
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22855
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_correction_T_min  0.8337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of 
  Gottingen, Germany 2003.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.00051(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         8604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+32.3143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                5865
_reflns_number_total             8604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061052lsi20061115_093615.cif
_cod_data_source_block           ad96a
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2519.5(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072804