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_4077125
_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_sum            'C31 H43 F3 O2 P2 Pt'
_chemical_formula_weight         761.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                103.727(5)
_cell_angle_beta                 90.644(6)
_cell_angle_gamma                94.374(5)
_cell_formula_units_Z            2
_cell_length_a                   8.4097(6)
_cell_length_b                   10.9877(6)
_cell_length_c                   17.809(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.0
_cell_volume                     1593.22(17)
_diffrn_ambient_temperature      296
_diffrn_measurement_device_type  'Nonius CAD-4 serial diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.03078
_diffrn_orient_matrix_UB_12      0.08609
_diffrn_orient_matrix_UB_13      0.02491
_diffrn_orient_matrix_UB_21      0.00469
_diffrn_orient_matrix_UB_22      0.02277
_diffrn_orient_matrix_UB_23      -0.05110
_diffrn_orient_matrix_UB_31      -0.11520
_diffrn_orient_matrix_UB_32      -0.02995
_diffrn_orient_matrix_UB_33      -0.01047
_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  0.015
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6707
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.530
_exptl_absorpt_correction_T_max  0.351
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews, 1968'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             760.00
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.58
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       '2.78(6) \\times 10^-6^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.38
_refine_ls_goodness_of_fit_ref   1.41
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_gt           0.022
_refine_ls_shift/su_max          0.038
_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         0.055
_refine_ls_wR_factor_ref         0.028
_reflns_number_gt                5904
_reflns_number_total             6257
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            om0206507.cif
_cod_data_source_block           VJ0502
_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        1593.2(2)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C31 H43 F3 O2 P2 Pt '
_cod_database_code               4077125
_publ_section_exptl
;The crystal for data collection was glued to a glass fibre. The 
intensity data were corrected for absorption (azimuthal scans) and 
for linear decay. Structure solution: SIR92 E-map (Altomare et al., 
1994).  All hydrogen atoms were located near expected positions, and 
were included in the refined model 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.
;