Total Syntheses of the Assigned Structures of Lituarines B and C
Amos B. Smith; Matthew O. Duffey; Kallol Basu; Shawn P. Walsh; Hans W. Suennemann; Michael Frohn; Journal of the American Chemical Society 130 (2008) 422–423; doi:10.1021/ja078293k

data_4107305
_publ_section_title
;
 Total Syntheses of the Assigned Structures of Lituarines B and C
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              422
_journal_page_last               423
_journal_paper_doi               10.1021/ja078293k
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C34 H59 Cl2 I O8 Si'
_chemical_formula_weight         821.70
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.578(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.719(10)
_cell_length_b                   10.141(10)
_cell_length_c                   21.25(2)
_cell_measurement_temperature    143(1)
_cell_volume                     2071(4)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13698
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9913
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         13698
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+8.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1985
_refine_ls_wR_factor_ref         0.2242
_reflns_number_gt                10109
_reflns_number_total             13698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja078293k-file006.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2072(4)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               4107305