Stille/Diels-Alder reaction sequences: diversity-oriented access to novel steroids.
Sünnemann, Hans Wolf; Hofmeister, Anja; Magull, Jörg; Banwell, Martin G.; de Meijere, Armin; Organic letters 9 (2007) 517–520; doi:10.1021/ol062878m

data_1505282
_publ_section_title
;
 Stille/Diels-Alder reaction sequences: diversity-oriented access to novel
 steroids.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              517
_journal_page_last               520
_journal_paper_doi               10.1021/ol062878m
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C26 H36 O6'
_chemical_formula_weight         444.55
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9811(2)
_cell_length_b                   11.3120(3)
_cell_length_c                   33.5143(10)
_cell_measurement_temperature    133(2)
_cell_volume                     2267.52(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            39241
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.091
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.4611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                3662
_reflns_number_total             3851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol062878msi20061127_063937.cif
_cod_data_source_block           ha600neu
_cod_database_code               1505282