Synthesis of the C19 methyl ether of aspercyclide A via germyl-Stille macrocyclisation and ELISA evaluation of both enantiomers following optical resolution.
Carr, James L.; Sejberg, Jimmy J. P.; Saab, Fabienne; Holdom, Mary D.; Davies, Anna M.; White, Andrew J. P.; Leatherbarrow, Robin J.; Beavil, Andrew J.; Sutton, Brian J.; Lindell, Stephen D.; Spivey, Alan C.; Organic & biomolecular chemistry 9 (2011) 6814–6824; doi:10.1039/c1ob05862b

data_7152001
_publ_section_title
;
 Synthesis of the C19 methyl ether of aspercyclide A via germyl-Stille
 macrocyclisation and ELISA evaluation of both enantiomers following
 optical resolution.
;
_journal_issue                   19
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6814
_journal_page_last               6824
_journal_paper_doi               10.1039/c1ob05862b
_journal_volume                  9
_journal_year                    2011
_chemical_formula_moiety         'C32 H23 F17 Ge'
_chemical_formula_sum            'C32 H23 F17 Ge'
_chemical_formula_weight         803.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.8926(19)
_cell_angle_beta                 87.4794(19)
_cell_angle_gamma                88.9974(18)
_cell_formula_units_Z            2
_cell_length_a                   6.09459(14)
_cell_length_b                   7.56496(17)
_cell_length_c                   33.7307(8)
_cell_measurement_reflns_used    11842
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.2012
_cell_measurement_theta_min      2.6306
_cell_volume                     1547.35(6)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173(2)
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            21958
_diffrn_reflns_theta_full        71.38
_diffrn_reflns_theta_max         71.38
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     1574
_refine_ls_restrained_S_all      1.643
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0823P)^2^+1.5358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                4961
_reflns_number_total             5920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ob05862b.txt
_cod_data_source_block           27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
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_sg_symbol_H-M      P-1
_cod_database_code               7152001