Synthesis of α-hydroxy and α-oxospiranes through ruthenium(II)-catalyzed ring-closing metathesis
Aburel, Pompiliu S.; Rømming, Christian; Ma, Kuangbiao; Undheim, Kjell; Journal of the Chemical Society, Perkin Transactions 1  (2001) 1458–; doi:10.1039/b101462p

data_7216904
_publ_section_title
;
 Synthesis of \a-hydroxy and \a-oxospiranes through
 ruthenium(II)-catalyzed ring-closing metathesis
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1458
_journal_paper_doi               10.1039/b101462p
_journal_year                    2001
_chemical_formula_sum            'C20 H23 N O6'
_chemical_formula_weight         373.39
_chemical_name_systematic
; 
cis-7,7-ethylenedioxospiro[5,5]undecan-3-en-1-yl p-nitrobenzoate
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.055(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8560(7)
_cell_length_b                   12.8358(14)
_cell_length_c                   20.535(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1797.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38813
_diffrn_reflns_theta_full        35.84
_diffrn_reflns_theta_max         35.84
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.102
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         8006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                6221
_reflns_number_total             8006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101462p.txt
_cod_data_source_block           44
_cod_original_cell_volume        1797.1(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7216904