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_4321169
_publ_section_title
;
 Cooperative Diastereoselectivity of Palladium- and Platinum-Promoted
 Intramolecular [4+2] Diels-Alder Cycloaddition Reactions of
 3,4-Dimethyl-1-phenylphosphole
;
_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            'C44 H53 F12 N2 O2 P4 Pd'
_chemical_formula_weight         1100.16
_chemical_name_common            6a
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                74.937(6)
_cell_angle_beta                 83.354(9)
_cell_angle_gamma                84.189(9)
_cell_formula_units_Z            2
_cell_length_a                   10.384(2)
_cell_length_b                   11.9120(11)
_cell_length_c                   21.260(2)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      4.78
_cell_volume                     2515.4(6)
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10392
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         1.78
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_correction_T_min  0.8116
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .65
_exptl_crystal_size_min          .42
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.419
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_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_obs          0.0638
_refine_ls_shift/esd_max         -15.000
_refine_ls_shift/esd_mean        0.200
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+6.8484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2030
_refine_ls_wR_factor_obs         0.1852
_reflns_number_observed          6990
_reflns_number_total             8798
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990885j_9.cif
_cod_data_source_block           jhn190a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+6.8484P] 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^)+(0.1208P)^2^+6.8484P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2515.3(5)
_cod_database_code               4321169