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_4082229
_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         'C54 H45 D3 N4 O6 Pd, 2(H2 O)'
_chemical_formula_sum            'C54 H49 D3 N4 O8 Pd'
_chemical_formula_weight         994.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.289(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.8293(17)
_cell_length_b                   12.9042(5)
_cell_length_c                   26.2493(16)
_cell_measurement_reflns_used    13509
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.90
_cell_volume                     10413.4(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71677
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.9186
_exptl_absorpt_correction_T_min  0.9150
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            'LIGHT YELLOW'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       IRREGULAR
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         10637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+19.6258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.1952
_reflns_number_gt                9496
_reflns_number_total             10637
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4010719_si_002.cif
_cod_data_source_block           11a
_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_cell_volume        10413.4(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4082229