Practical Method for the Absolute Configuration Assignment of tert/tert 1,2-Diols Using Their Complexes with Mo~2~(OAc)~4~
Marcin Górecki; Ewa Jabłońska; Anna Kruszewska; Suszczyńska; Zofia Urbańczyk-Lipkowska; Michael Gerards; Jacek W. Morzycki; Wojciech J. Szczepek; Jadwiga Frelek; Journal of Organic Chemistry 72 (2007) 2906–2916; doi:10.1021/jo062445x

data_4022794
_publ_section_title
;
 Practical Method for the Absolute Configuration Assignment
 of tert/tert 1,2-Diols Using Their Complexes with Mo~2~(OAc)~4~
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2906
_journal_page_last               2916
_journal_paper_doi               10.1021/jo062445x
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C19 H31 O3.50'
_chemical_formula_sum            'C19 H31 O3.5'
_chemical_formula_weight         313.42
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 119.475(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.186(2)
_cell_length_b                   7.5405(10)
_cell_length_c                   12.8359(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      43.23
_cell_measurement_theta_min      20.87
_cell_volume                     1785.2(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2046
_diffrn_reflns_theta_full        74.17
_diffrn_reflns_theta_max         74.17
_diffrn_reflns_theta_min         3.96
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.9969
_exptl_absorpt_correction_T_min  0.8863
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'psi scan for 6 reflections'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_coef       0.0018(5)
_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_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         1957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+0.0169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                1178
_reflns_number_total             1957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo062445xrom20070205_095610.cif
_cod_data_source_block           triol_1/2H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C19 H31 O3.50'
_cod_database_code               4022794