PtII-Promoted [2 + 3] Cycloaddition of Azide to Cyanopyridines: Convenient Tool toward Heterometallic Structures
Suman Mukhopadhyay; Bhaswati Ghosh Mukhopadhyay; M. Fátima C. Guedes da Silva; Jamal Lasri; M. Adília Januário Charmier; Armando J. L. Pombeiro; Inorganic Chemistry 47 (2008) 11334–11341; doi:10.1021/ic8014223

data_4306595
_publ_section_title
;
PtII-Promoted [2 + 3] Cycloaddition of Azide to Cyanopyridines: Convenient
Tool toward Heterometallic Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11334
_journal_page_last               11341
_journal_paper_doi               10.1021/ic8014223
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C48 H38 N10 P2 Pt'
_chemical_formula_sum            'C48 H38 N10 P2 Pt'
_chemical_formula_weight         1011.91
_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                88.584(15)
_cell_angle_beta                 74.856(13)
_cell_angle_gamma                72.836(14)
_cell_formula_units_Z            2
_cell_length_a                   12.153(8)
_cell_length_b                   12.336(8)
_cell_length_c                   16.907(11)
_cell_measurement_reflns_used    2684
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.1640
_cell_measurement_theta_min      2.4662
_cell_volume                     2334(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.1400
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15642
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    3.118
_exptl_absorpt_correction_T_max  0.6520
_exptl_absorpt_correction_T_min  0.5094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         2.516
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         8331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                5148
_reflns_number_total             8331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8014223_si_001_2.cif
_cod_data_source_block           comp3c
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4306595