Practical radical cyclisations leading to the construction of near-stereopure quaternary carbon stereogenic centres
McCague, Raymond; Pritchard, Robin G.; Stoodley, Richard J.; Williamson, Douglas S.; Chemical Communications  (1998) 2691–; doi:10.1039/a807930g

data_7110388
_publ_section_title
;
 Practical radical cyclisations leading to the construction of
 near-stereopure quaternary carbon stereogenic centres
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2691
_journal_paper_doi               10.1039/a807930g
_journal_year                    1998
_chemical_formula_sum            'C23 H34 O12'
_chemical_formula_weight         502.50
_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'
_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                 90.36(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.425(6)
_cell_length_b                   23.566(7)
_cell_length_c                   17.545(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2656(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1840
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4309
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.102
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(4)
_refine_ls_extinction_coef       0.110(10)
_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   1.340
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         4309
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.2519
_refine_ls_R_factor_gt           0.1276
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2893
_reflns_number_gt                2004
_reflns_number_total             4309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807930gsup1.cif
_cod_data_source_block           stud96
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7110388