Trimesitylmethylphosphonium Cation. Supramolecular Stereocontrol and Simple Enantiomerization Mechanism Determination
Benoît Laleu; Gérald Bernardinelli; Remi Chauvin; Jérôme Lacour; Journal of Organic Chemistry 71 (2006) 7412–7416; doi:10.1021/jo061097w

data_4021954
_publ_contact_author
;
     Dr Gerald Bernardinelli
     Laboratory of X-ray Crystallography
     University of Geneva
     24, quai E. Ansermet
     CH - 1211 Geneva 4
     Switzerland
;
_publ_contact_author_email       gerald.bernardinelli@cryst.unige.ch
_publ_contact_author_fax         '41 22 379 61 08'
_publ_contact_author_phone       '41 22 379 62 02'
_publ_section_title
;
 Trimesitylmethylphosphonium Cation. Supramolecular Stereocontrol
 and Simple Enantiomerization Mechanism Determination
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7412
_journal_page_last               7416
_journal_paper_doi               10.1021/jo061097w
_journal_volume                  71
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_moiety 
'C28 H36 P, C18 Cl12 O6 P, 0.5(C6 H14) , 0.75(C4 H8 O2)'
_chemical_formula_sum            'C52 H49 Cl12 O7.5 P2'
_chemical_formula_weight         1281.3
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1
_audit_creation_date             2004-10-25
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2006-02-09
_cell_angle_alpha                90.00000
_cell_angle_beta                 101.707(5)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   12.3799(5)
_cell_length_b                   24.2382(12)
_cell_length_c                   21.2644(10)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.1
_cell_volume                     6248.0(5)
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 6
_diffrn_measured_fraction_theta_full .99
_diffrn_measured_fraction_theta_max .99
_diffrn_measurement_device_type  'Stoe Ipds'
_diffrn_measurement_method       \f
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .077
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49644
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.0
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .63
_exptl_absorpt_correction_T_max  .9618
_exptl_absorpt_correction_T_min  .8668
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED; Stoe & Cie, 1999'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .06
_refine_diff_density_max         .921
_refine_diff_density_min         -.579
_refine_ls_abs_structure_details Flack_xabs_refined
_refine_ls_abs_structure_Flack   .06(10)
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.28(1)
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         10548
_refine_ls_R_factor_gt           .044
_refine_ls_shift/su_max          .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     \w=1/[\s^2^(Fo)+0.0002(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .042
_reflns_Friedel_coverage         .97
_reflns_number_gt                9272
_reflns_number_total             24214
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_cod_data_source_file            jo061097wsi20060529_123819.cif
_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 

2025-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C104 H98 Cl24 O15 P4'
_cod_original_formula_weight         2562.7
_cod_original_formula_moiety
' (C28 H36 P)2 , (C18 Cl12 O6 P)4 , C6 H14 , (C4 H8 O2)1.5 '
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4021954