Evidence for the formation of the (Ph3P)2Pt complex of 3,7-dimethyltricyclo[3.3.0.03,7]oct-1(5)-ene, the most highly pyramidalized alkene in a homologous series. Isolation and X-ray structure of the product of the ethanol addition to the complex.
Theophanous, Fanitsa A.; Tasiopoulos, Anastasios J.; Nicolaides, Athanassios; Zhou, Xin; Johnson, William T. G.; Borden, Weston Thatcher; Organic letters 8 (2006) 3001–3004; doi:10.1021/ol060994j

data_1506055
_publ_section_title
;
 Evidence for the formation of the (Ph3P)2Pt complex of
 3,7-dimethyltricyclo[3.3.0.03,7]oct-1(5)-ene, the most highly
 pyramidalized alkene in a homologous series. Isolation and X-ray
 structure of the product of the ethanol addition to the complex.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3001
_journal_page_last               3004
_journal_paper_doi               10.1021/ol060994j
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C48 H50 O P2 Pt'
_chemical_formula_weight         899.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.931(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5273(7)
_cell_length_b                   10.3442(5)
_cell_length_c                   21.1903(10)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2738
_cell_measurement_theta_min      3.0111
_cell_volume                     3905.1(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction CCD'
_diffrn_measurement_method       '\w/\f 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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67777
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.712
_exptl_absorpt_correction_T_max  0.75351
_exptl_absorpt_correction_T_min  0.49132
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
Analytical numeric absorption correction using a multifaceted crystal
  model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.10187
_exptl_crystal_size_mid          0.07287
_exptl_crystal_size_min          0.02287
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                8446
_reflns_number_total             10327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol060994jsi20060425_072540.cif
_cod_data_source_block           ft01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1506055