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_4333824
_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         'C25 H29 N3'
_chemical_formula_sum            'C25 H29 N3'
_chemical_formula_weight         371.51
_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                80.974(5)
_cell_angle_beta                 77.125(4)
_cell_angle_gamma                80.902(5)
_cell_formula_units_Z            2
_cell_length_a                   8.391(5)
_cell_length_b                   11.547(4)
_cell_length_c                   12.017(5)
_cell_measurement_reflns_used    2408
_cell_measurement_temperature    298(3)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.98
_cell_volume                     1111.8(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    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      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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9035
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9857
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'
_exptl_crystal_colour            WHITE
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.2410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                3641
_reflns_number_total             4548
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302058u_si_001_6.cif
_cod_data_source_block           LH22,5-xylyl
_cod_database_code               4333824