Cooperative Diastereoselectivity of Palladium- and Platinum-Promoted Intramolecular [4+2] Diels-Alder Cycloaddition Reactions of 3,4-Dimethyl-1-phenylphosphole
Kent D. Redwine; William L. Wilson; Donald G. Moses; Vincent J. Catalano; John H. Nelson; Inorganic Chemistry 39 (2000) 3392–3402; doi:10.1021/ic990885j

data_4321164
_publ_section_title
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 Cooperative Diastereoselectivity of Palladium- and Platinum-Promoted
 Intramolecular [4+2] Diels-Alder Cycloaddition Reactions of
 3,4-Dimethyl-1-phenylphosphole
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3392
_journal_page_last               3402
_journal_paper_doi               10.1021/ic990885j
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C34 H44 B2 F8 N2 O2 P2 Pt'
_chemical_formula_weight         943.36
_chemical_name_common            2b
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.961(7)
_cell_length_b                   10.583(3)
_cell_length_c                   19.869(4)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.55
_cell_measurement_theta_min      4.55
_cell_volume                     3733(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
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_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        2.97
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.3743
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .51
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00229(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.070
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_refine_ls_number_reflns         2445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_obs          0.0339
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0796
_refine_ls_wR_factor_obs         0.0762
_reflns_number_observed          2166
_reflns_number_total             2445
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990885j_4.cif
_cod_data_source_block           122
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        3733.2(19)
_cod_database_code               4321164