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_4082227
_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 O9 Pd S'
_chemical_formula_sum            'C53 H46 F3 N3 O9 Pd S'
_chemical_formula_weight         1064.39
_chemical_name_systematic
;
 ?
;
_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                108.216(4)
_cell_angle_beta                 90.186(3)
_cell_angle_gamma                93.039(3)
_cell_formula_units_Z            4
_cell_length_a                   15.5705(5)
_cell_length_b                   16.5957(5)
_cell_length_c                   21.0323(6)
_cell_measurement_reflns_used    6417
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.98
_cell_volume                     5154.1(3)
_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      298(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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            84241
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.9040
_exptl_absorpt_correction_T_min  0.8959
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.154
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         21053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+4.2404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1434
_reflns_number_gt                17587
_reflns_number_total             21053
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4010719_si_002.cif
_cod_data_source_block           9a
_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 2.4.2 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 

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C106 H92 F6 N6 O18 Pd2 S2'
_cod_original_formula_weight         2128.78
_cod_original_formula_moiety         'C106 H92 F6 N6 O18 Pd2 S2'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082227