Synthesis and Characterization of the Double Salts [Pt(bzq)(CNR)2][Pt(bzq)(CN)2] with Significant Pt···Pt and π···π Interactions. Mechanistic Insights into the Ligand Exchange Process from Joint Experimental and DFT Study
Forniés, Juan; Fuertes, Sara; Larraz, Carmen; Martín, Antonio; Sicilia, Violeta; Tsipis, Athanassios C.; Organometallics 31 (2012) 2729–; doi:10.1021/om201036z

data_4077912
_publ_section_title
;
 Synthesis and Characterization of the Double Salts
 [Pt(bzq)(CNR)2][Pt(bzq)(CN)2] with Significant
 Pt&#x00B7;&#x00B7;&#x00B7;Pt and \p&#x00B7;&#x00B7;&#x00B7;\p
 Interactions. Mechanistic Insights into the Ligand Exchange Process from
 Joint Experimental and DFT Study
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2729
_journal_paper_doi               10.1021/om201036z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C47.5 H40 N6 O1.5 Pt2'
_chemical_formula_weight         1109.04
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.86700(10)
_cell_length_b                   13.3363(3)
_cell_length_c                   34.4243(5)
_cell_measurement_reflns_used    13272
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7974
_cell_measurement_theta_min      3.7353
_cell_volume                     4070.78(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -53.00   52.70   0.7000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.8053   77.0000   39.0000    0.0000    0.0000 151

  2 omega  -11.00   43.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2271   77.0000  270.0000    0.0000    0.0000 78

  3 omega   40.00   94.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2271   77.0000  120.0000    0.0000    0.0000 78

  4 omega  -95.00   45.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.8053    0.0000  150.0000    0.0000    0.0000 200

;
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       w
_diffrn_orient_matrix_UB_11      0.0260305315
_diffrn_orient_matrix_UB_12      -0.0290474680
_diffrn_orient_matrix_UB_13      -0.0158988790
_diffrn_orient_matrix_UB_21      0.0421699798
_diffrn_orient_matrix_UB_22      0.0415999610
_diffrn_orient_matrix_UB_23      -0.0067819177
_diffrn_orient_matrix_UB_31      0.0627221451
_diffrn_orient_matrix_UB_32      -0.0158621398
_diffrn_orient_matrix_UB_33      0.0111833517
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            25152
_diffrn_reflns_theta_full        26.24
_diffrn_reflns_theta_max         26.24
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    6.911
_exptl_absorpt_correction_T_max  0.5449
_exptl_absorpt_correction_T_min  0.1551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.048(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8128
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                7101
_reflns_number_total             8128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201036z_si_002.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C47.50 H40 N6 O1.50 Pt2'
_cod_database_code               4077912