Tandem pinacol coupling-rearrangement of aromatic aldehydes with hydrogen catalyzed by a combination of a platinum complex and a polyoxometalate.
Branytska, Olena; Shimon, Linda J W; Neumann, Ronny; Chemical communications (Cambridge, England)  (2007) 3957–3959; doi:10.1039/b710100g

data_7102171
_publ_section_title
;
 Tandem pinacol coupling-rearrangement of aromatic aldehydes with
 hydrogen catalyzed by a combination of a platinum complex and a
 polyoxometalate.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3957
_journal_page_last               3959
_journal_paper_doi               10.1039/b710100g
_journal_year                    2007
_chemical_formula_sum            'C18.5 H23.5 Cl6.5 N3 Pt'
_chemical_formula_weight         713.42
_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                98.9290(17)
_cell_angle_beta                 94.3500(16)
_cell_angle_gamma                90.9850(11)
_cell_formula_units_Z            4
_cell_length_a                   11.1610(3)
_cell_length_b                   15.0510(4)
_cell_length_c                   15.2210(3)
_cell_measurement_reflns_used    11055
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2517.54(11)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11399
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    6.275
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.5726
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         11399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.9345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                9756
_reflns_number_total             11399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710100g.txt
_cod_data_source_block           n107a
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18.50 H23.50 Cl6.50 N3 Pt'
_cod_database_code               7102171