The first synthetic studies on pestalotiopsin A. A stereocontrolled approach to the functionalised bicyclic coreElectronic supplementary information (ESI) available: crystal structure analysis of 18a. See http://www.rsc.org/suppdata/ob/b2/b209066j/
Johnston, Derek; Couché, Emmanuel; Edmonds, David J.; Muir, Kenneth W.; Procter, David J.; Organic & Biomolecular Chemistry 1 (2003) 328–; doi:10.1039/b209066j

data_7150452
_publ_section_title
;
 The first synthetic studies on pestalotiopsin A. A stereocontrolled
 approach to the functionalised bicyclic coreElectronic supplementary
 information (ESI) available: crystal structure analysis of 18a. See
 http://www.rsc.org/suppdata/ob/b2/b209066j/
;
_journal_issue                   2
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              328
_journal_paper_doi               10.1039/b209066j
_journal_volume                  1
_journal_year                    2003
_chemical_formula_moiety         'C18 H34 O5 Si1'
_chemical_formula_sum            'C18 H34 O5 Si'
_chemical_formula_weight         358.54
_chemical_name_common            'Compound X'
_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                102.1470(10)
_cell_angle_beta                 95.2180(10)
_cell_angle_gamma                91.1660(10)
_cell_formula_units_Z            4
_cell_length_a                   12.6770(2)
_cell_length_b                   12.7397(2)
_cell_length_c                   13.0974(2)
_cell_measurement_reflns_used    8464
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2057.62(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'WINGX (Farrugia, 1999)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31303
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical correction based on variations in
observed intensities.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.24
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.9369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                7639
_reflns_number_total             9393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b209066j.txt
_cod_data_source_block           km1102
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7150452