Syntheses of the Eastern Halves of Ritterazines B, F, G, and H, Leading to Reassignment of the 5,5-Spiroketal Stereochemistry of Ritterazines B and F
Scott T. Phillips; Matthew D. Shair; Journal of the American Chemical Society 129 (2007) 6589–6598; doi:10.1021/ja0705487

data_4109429
_publ_section_title
;
 Syntheses of the Eastern Halves of Ritterazines B, F, G, and H, Leading
 to Reassignment of the 5,5-Spiroketal Stereochemistry of Ritterazines B
 and F
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6589
_journal_page_last               6598
_journal_paper_doi               10.1021/ja0705487
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C41 H50 N2 O10'
_chemical_formula_weight         730.83
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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                   6.6933(13)
_cell_length_b                   21.217(4)
_cell_length_c                   26.837(5)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15.66
_cell_measurement_theta_min      2.45
_cell_volume                     3811.2(13)
_computing_cell_refinement       'SMART (BRUKER, V5.625, 2001)'
_computing_data_collection       'ASTRO (BRUKER, V5.007, 1997)'
_computing_data_reduction        'SAINT (BRUKER, V6.22, 2001)'
_computing_molecular_graphics    'SHELXTL (BRUKER, 2000, V6.1)'
_computing_publication_material  'XCIF (Sheldrick and BRUKER, 1997, V5.1)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       '\w, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_sigmaI/netI    0.2897
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20675
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9964
_exptl_absorpt_correction_T_min  0.9910
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            cololress
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.646
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.646
_refine_ls_R_factor_all          0.1969
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0136P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                2185
_reflns_number_total             6698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0705487si20070129_043342.cif
_cod_data_source_block           ms46t
_cod_original_cell_volume        3811.1(13)
_cod_database_code               4109429