Total synthesis of the proposed structure of trichodermatide a.
Myers, Eddie; Herrero-Gómez, Elena; Albrecht, Irina; Lachs, Jennifer; Mayer, Peter; Hanni, Matti; Ochsenfeld, Christian; Trauner, Dirk; The Journal of organic chemistry 79 (2014) 9812–9817; doi:10.1021/jo501206k

data_4029965
_publ_section_title
;
 Total synthesis of the proposed structure of trichodermatide a.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9812
_journal_page_last               9817
_journal_paper_doi               10.1021/jo501206k
_journal_volume                  79
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H66 Br2 O9 Si2'
_chemical_formula_sum            'C48 H66 Br2 O9 Si2'
_chemical_formula_weight         1003.011
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C48H66Br2O9Si2_po057_trauner
_audit_creation_date
;
'Tue Apr 05 07:24:37 2011'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             14-Apr-11
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.0291(6)
_cell_length_b                   25.3002(5)
_cell_length_c                   13.8427(4)
_cell_measurement_reflns_used    13318
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2495
_cell_measurement_theta_min      4.2018
_cell_volume                     9816.4(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -53.00   51.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931    0.0000  120.0000 104

  2 omega  -87.00    9.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -38.0000  -90.0000 96

  3 omega   59.00  101.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  179.0000    0.0000 42

  4 omega   -8.00   17.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  104.0000  -61.0000 25

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185635577
_diffrn_orient_matrix_UB_12      0.0155773200
_diffrn_orient_matrix_UB_13      0.0190155540
_diffrn_orient_matrix_UB_21      -0.0457133846
_diffrn_orient_matrix_UB_22      0.0123793073
_diffrn_orient_matrix_UB_23      0.0025604742
_diffrn_orient_matrix_UB_31      -0.0140038430
_diffrn_orient_matrix_UB_32      -0.0197696863
_diffrn_orient_matrix_UB_33      0.0165312244
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.1198
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            45391
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         4.22
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50_kV
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.35737(6)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         19645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0298P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                11272
_reflns_number_total             19645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo501206k_si_002.cif
_cod_data_source_block           po057
_cod_depositor_comments
'Adding full bibliography for 4029965--4029966.cif.'
_cod_database_code               4029965