Formation of Diphosphates. A NMR Study on the Mechanism and Stereochemistry of Diphosphate Formation from Chiral Dioxaphosphorinanes
Ron Hulst; Johanna M. Visser; Robert W. J. Zijlstra; Huub Kooijman; Wilberth Smeets; Anthony L. Spek; Ben L. Feringa; Journal of the American Chemical Society 122 (2000) 3135–3150; doi:10.1021/ja992770k

data_4115962
_publ_contact_author_address
;
    Bijvoet Center for Biomolecular Research
    Department of Crystal and Structural Chemistry
    Utrecht University
    Padualaan 8
    3584 CH Utrecht
    The Netherlands
;
_publ_contact_author_email       spea@chem.uu.nl
_publ_contact_author_fax         '+31 30 2533940'
_publ_contact_author_name        '   Dr. A.L. Spek'
_publ_contact_author_phone       '+31 30 2532538'
_publ_section_title
;
 Formation of Diphosphates. A NMR Study on the Mechanism and
 Stereochemistry of Diphosphate Formation from Chiral Dioxaphosphorinanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3135
_journal_page_last               3150
_journal_paper_doi               10.1021/ja992770k
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C20 H25 O4 P'
_chemical_formula_sum            'C20 H25 O4 P'
_chemical_formula_weight         360.37
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4799(10)
_cell_length_b                   17.165(2)
_cell_length_c                   17.189(2)
_cell_measurement_temperature    295
_cell_volume                     1911.9(4)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'Locally modified CAD4-Version 5 Software'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2271
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            1966
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.16
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          1.1
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.7(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    'H-atom refinement: see text '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         1958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[S
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                1061
_reflns_number_total             1958
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ja992770k_2.cif
_cod_data_source_block           s691a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[S' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[S'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115962