Insertion Reactions of Six-Membered CyclopalladatedN,N′,N″-Triarylguanidine, [Pd{κ2(C,N)-C6H3Me-3(NHC(NHAr)(═NAr))-2}(μ-Br)]2(Ar = 2-MeC6H4) with PhC≡C—C(O)OR (R = Me and Et): A Gateway to Second Orthopalladation through Novel Rearrangements
Saxena, Priya; Thirupathi, Natesan; Nethaji, Munirathinam; Organometallics 32 (2013) 7580–; doi:10.1021/om4010719

data_4082226
_publ_contact_author             'Thirupathi N.'
_publ_section_title
;
 Insertion Reactions of Six-Membered
 CyclopalladatedN,N&#x2032;,N&#x2033;-Triarylguanidine,
 [Pd{\k2(C,N)-C6H3Me-3(NHC(NHAr)(&#x2550;NAr))-2}(\m-Br)]2(Ar = 2-MeC6H4)
 with PhC\\tb C---C(O)OR (R = Me and Et): A Gateway to Second
 Orthopalladation through Novel Rearrangements
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7580
_journal_paper_doi               10.1021/om4010719
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C53 H46 F3 N3 O10 Pd S, C H2 Cl2, H2 O'
_chemical_formula_sum            'C54 H50 Cl2 F3 N3 O10 Pd S'
_chemical_formula_weight         1167.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.806(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5054(5)
_cell_length_b                   14.2285(5)
_cell_length_c                   28.8166(14)
_cell_measurement_reflns_used    19101
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.95
_cell_volume                     5530.8(4)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'OLEX 2-1.2'
_computing_publication_material  'WINGX V1.80.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.3703
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Sapphire-3 CCD detector'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            58980
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.8136
_exptl_absorpt_correction_T_min  0.7899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       CUBOIDAL
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.121
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     645
_refine_ls_number_reflns         11282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+28.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2002
_refine_ls_wR_factor_ref         0.2045
_reflns_number_gt                10283
_reflns_number_total             11282
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4010719_si_002.cif
_cod_data_source_block           7a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4082226