Rearrangement of a σ-2-(Cycloprop-2-enyl)vinyl- to an η3-Cyclopentadienylplatinum(II) Complex. Selective Protonolysis of the Platinum−Methyl Bond
Jacob, Volker; Weakley, Timothy J. R.; Haley, Michael M.; Organometallics 21 (2002) 5394–; doi:10.1021/om0206507

data_4077124
_publ_section_title
;
 Rearrangement of a \s-2-(Cycloprop-2-enyl)vinyl- to an
 \h3-Cyclopentadienylplatinum(II) Complex. Selective Protonolysis of the
 Platinum&#x2212;Methyl Bond
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5394
_journal_paper_doi               10.1021/om0206507
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C30 H46 P2 Pt '
_chemical_formula_structural     'Pt (P (C2 H5)3 )2 (C H3) (C17 H13)'
_chemical_formula_sum            'C30 H46 P2 Pt'
_chemical_formula_weight         663.73
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 92.97(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.466(2)
_cell_length_b                   16.583(2)
_cell_length_c                   9.866(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      13.9
_cell_volume                     1546.6(5)
_diffrn_ambient_temperature      296
_diffrn_measurement_device_type  'Nonius CAD-4 serial diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.03828
_diffrn_orient_matrix_UB_12      -0.05580
_diffrn_orient_matrix_UB_13      -0.00941
_diffrn_orient_matrix_UB_21      0.00614
_diffrn_orient_matrix_UB_22      0.00855
_diffrn_orient_matrix_UB_23      -0.09985
_diffrn_orient_matrix_UB_31      0.09843
_diffrn_orient_matrix_UB_32      0.02119
_diffrn_orient_matrix_UB_33      0.01555
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3512
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        28.7
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.64
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North,Phillips & Matthews, 1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.77
_refine_diff_density_min         -1.73
_refine_ls_abs_structure_details 'see exptl section'
_refine_ls_extinction_coef       '2.6(5) \\times 10^-7^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.27
_refine_ls_goodness_of_fit_ref   1.28
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.0008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I) + (0.025I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.070
_refine_ls_wR_factor_ref         0.034
_reflns_number_gt                2712
_reflns_number_total             3319
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            om0206507.cif
_cod_data_source_block           VJ0302
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1546.6(6)
_cod_original_sg_symbol_H-M      'P 21       '
_cod_original_formula_sum        'C30 H46 P2 Pt '
_cod_database_code               4077124
_publ_section_exptl
;The crystal for data collection was coated with epoxy and mounted on 
a glass fiber.  Data were collected in shells (1.5-21.5\%, 21.5-27\% 
\q).  Collection was stopped in the second shell when the intensity of 
standard reflections has fallen by 29%.  The intensity data were 
corrected for absorption (azimuthal scans) and for linear decay. 
Structure solution: SIR92 E-map (Altomare et al., 1994).  Hydrogen 
atoms were included at calculated, updated positions [d(C-H) = 
0.95 \%A; B(H) = 1.2B~eq~(C)].  The value of a secondary extinction 
parameter was also refined.  The enantiomeric structure (x, -y, z) 
refined to R(F) 0.040 (obs. data), wR(F^2^) 0.075, S 1.45 (all data), 
and was rejected.
;