Explorations into Neolignan Biosynthesis: Concise Total Syntheses of Helicterin B, Helisorin, and Helisterculin A from a Common Intermediate
Scott A. Snyder; Ferenc Kontes; Journal of the American Chemical Society 131 (2009) 1745–1752; doi:10.1021/ja806865u

data_4103868
_publ_section_title
;
 Explorations into Neolignan Biosynthesis: Concise Total Syntheses of
 Helicterin B, Helisorin, and Helisterculin A from a Common Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1745
_journal_page_last               1752
_journal_paper_doi               10.1021/ja806865u
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C46.5 H53 Cl5 O16'
_chemical_formula_weight         1045.14
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.477(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.622(4)
_cell_length_b                   12.7487(17)
_cell_length_c                   26.301(4)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.25
_cell_volume                     10025(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            68654
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.9964
_exptl_absorpt_correction_T_min  0.8557
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             4360
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains 20 dichloromethane molecules which have been treated 
as a diffuse cotribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON
;
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         12417
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1922
_reflns_number_gt                6159
_reflns_number_total             12417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806865u_si_004.cif
_cod_data_source_block           fkd2s10p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C46.50 H53 Cl5 O16'
_cod_database_code               4103868