Synthesis and Reactivity of (η1-Alkynyl)diorganoplatinum(IV) Species, Including Structural Studies of PtIMe(p-Tol)(CCSiMe3)(dmpe) [dmpe = 1,2-bis(dimethylphosphino)ethane] and the Platinum(II) Reagent PtPh2(dmpe)
Canty, Allan J.; Watson, Russell P.; Karpiniec, Samuel S.; Rodemann, Thomas; Gardiner, Michael G.; Jones, Roderick C.; Organometallics 27 (2008) 3203–; doi:10.1021/om800122k

data_4071355
_publ_section_title
;
 Synthesis and Reactivity of (\h1-Alkynyl)diorganoplatinum(IV) Species,
 Including Structural Studies of PtIMe(p-Tol)(C&#xE5FC;CSiMe3)(dmpe) [dmpe
 = 1,2-bis(dimethylphosphino)ethane] and the Platinum(II) Reagent
 PtPh2(dmpe)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3203
_journal_paper_doi               10.1021/om800122k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C19 H35 I P2 Pt Si'
_chemical_formula_sum            'C19 H35 I P2 Pt Si'
_chemical_formula_weight         675.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 113.21(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.982(10)
_cell_length_b                   10.492(5)
_cell_length_c                   15.289(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      13.806
_cell_measurement_theta_min      9.905
_cell_volume                     2504(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
'X-SEED (Barbour, 2001) and ORTEPIII (Farrugia, 1997)'
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.1409
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4024
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.30
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        11
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.013
_exptl_absorpt_correction_T_max  0.8237
_exptl_absorpt_correction_T_min  0.7996
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.313
_refine_diff_density_min         -2.641
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1116P)^2^+29.2395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                2288
_reflns_number_total             3870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800122k-file003.cif
_cod_data_source_block           c:257rw1\analytical_correction
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4071355
_exptl_absorpt_correction_t_ave  0.8176
_diffrn_standards_decay_corr_max 1.193
_diffrn_standards_decay_corr_min 0.999