Dual Role of Acetate as a Nucleophile and as an Internal Base in Cycloplatination Reaction of sym-N,N',N"-Triarylguanidines
Palani Elumalai; Natesan Thirupathi; Munirathinam Nethaji; Inorganic Chemistry 52 (2013) 1883–1894; doi:10.1021/ic302058u

data_4333820
_publ_contact_author_email       tnat@chemistry.du.ac.in
_publ_contact_author_name        'Natesan Thirupathi.'
_publ_section_title
;
 Dual Role of Acetate as a Nucleophile and as an Internal Base in
 Cycloplatination Reaction of sym-N,N',N"-Triarylguanidines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1883
_journal_page_last               1894
_journal_paper_doi               10.1021/ic302058u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C24 H29 Cl2 N3 O4 Pt S), 3(C H Cl3)'
_chemical_formula_sum            'C25.5 H30.5 Cl6.5 N3 O4 Pt S'
_chemical_formula_weight         900.60
_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                79.543(5)
_cell_angle_beta                 75.782(5)
_cell_angle_gamma                76.201(4)
_cell_formula_units_Z            4
_cell_length_a                   12.658(5)
_cell_length_b                   16.391(5)
_cell_length_c                   16.940(4)
_cell_measurement_reflns_used    22559
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.96
_cell_volume                     3280.3(18)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    OLEX2
_computing_publication_material  'WINGX VI.80.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'CrysAlisPro, Oxford Diffraction Ltd.'
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48345
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    4.907
_exptl_absorpt_correction_T_max  0.4892
_exptl_absorpt_correction_T_min  0.3734
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       CUBOIDAL
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.873
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     749
_refine_ls_number_reflns         13401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+12.2119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                11912
_reflns_number_total             13401
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302058u_si_001_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        3280.4(19)
_cod_database_code               4333820