Stereocontrolled construction of rigid tricyclic bis(Î±-amino acid) derivatives by Ru(Ii)-catalyzed cascade and Dielsâ€“Alder reactions
Efskind, Jon; RÃ¶mming, Christian; Undheim, Kjell; Journal of the Chemical Society, Perkin Transactions 1  (2001) 2697–; doi:10.1039/b103254m

data_7213484
_publ_section_title
;
 Stereocontrolled construction of rigid tricyclic bis(\^I+--amino acid)
 derivatives by Ru(Ii)-catalyzed cascade and Diels\^a&#x20AC;&#x201C;Alder
 reactions
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2697
_journal_paper_doi               10.1039/b103254m
_journal_year                    2001
_chemical_formula_sum            'C27 H40 N4 O4'
_chemical_formula_weight         484.63
_chemical_name_systematic
; 
(2R,5S)-2,5-dihydro-2-isopropyl-3,6-dimethoxy-4'-[2R,5R)-2,5-dihydro-2-
isopropyl-3,6-dimethoxypyrazine-5-spiro(cyclo-2'-penten-2'-yl]pyrazine-5-
spiro(cyclo-3'-hexene)
;
_space_group_IT_number           4
_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                 96.189(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0943(10)
_cell_length_b                   10.1836(7)
_cell_length_c                   17.8280(11)
_cell_measurement_temperature    150(2)
_cell_volume                     2724.4(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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51259
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         5.92
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         16207
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                12435
_reflns_number_total             16207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103254msup1.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7213484