Total syntheses of +/- -musellarins A-C
Zhilong Li; Tsz-Fai Leung; Rongbiao Tong; Chem.Commun. 50 (2014) 10990–; doi:10.1039/C4cc05248J

data_7115630
_publ_section_title
;
 Total syntheses of +/- -musellarins A-C
;
_journal_name_full               Chem.Commun.
_journal_page_first              10990
_journal_paper_doi               10.1039/C4cc05248J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C23 H36 O4 Si'
_chemical_formula_sum            'C23 H36 O4 Si'
_chemical_formula_weight         404.61
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-31
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                82.362(2)
_cell_angle_beta                 86.419(2)
_cell_angle_gamma                85.558(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4432(3)
_cell_length_b                   10.8187(3)
_cell_length_c                   12.5225(3)
_cell_measurement_reflns_used    10546
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      75.2600
_cell_measurement_theta_min      5.0810
_cell_volume                     1128.73(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9806
_diffrn_measurement_details
;
  1 omega  125.00  167.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  -30.0000 42

  2 omega    3.00   28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   88.0000  138.0414 25

  3 omega  -48.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -77.0000  120.0000 41

  4 omega -115.00  -60.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -77.0000  120.0000 55

  5 omega -114.00  -49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000  -30.0000 65

  6 omega  -63.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   57.0000    0.0000 94

  7 omega  -45.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000  -30.0000 34

  8 omega -116.00  -17.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -37.0000 -150.0000 99

  9 omega   23.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8203 -125.0000 -150.0000 74

 10 omega   24.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8203 -125.0000  120.0000 58

 11 omega    7.00   32.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   88.0000    1.2798 25

 12 omega   12.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   84.0000   19.7750 26

 13 omega   17.00   42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000 -156.8586 25

 14 omega   18.00   43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000   94.8138 25

 15 omega   18.00   45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   80.0000  -84.9812 27

 16 omega   28.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000  -65.4432 26

 17 omega   27.00   64.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000  116.0645 37

 18 omega   84.00  129.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000  -65.4432 45

 19 omega   31.00   57.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   76.0000  -29.0843 26

 20 omega  114.00  139.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   71.0000 -139.8777 25

 21 omega   35.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000 -101.7372 32

 22 omega   32.00   60.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   71.0000 -139.8777 28

 23 omega   37.00   79.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000   -1.0981 42

 24 omega   34.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  149.9014 47

 25 omega   87.00  146.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   76.0000   -1.0981 59

 26 omega  112.00  143.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   44.8032 31

 27 omega   34.00   69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   44.8032 35

 28 omega   52.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   70.0000   75.2857 26

 29 omega   32.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  150.0000 69

 30 omega   77.00  104.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000   60.0000 27

 31 omega   47.00   97.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  -60.0000 50

 32 omega   78.00  105.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  -30.0000 27

 33 omega   77.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000 -150.0000 100

 34 omega  125.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000    0.0000 53

 35 omega   81.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000   90.0000 25

 36 omega   79.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000    0.0000 27

 37 omega   80.00  147.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000  120.0000 67

 38 omega  124.00  154.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  150.0000 30

 39 omega   77.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  150.0000 26

 40 omega   36.00   95.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  -90.0000 59

 41 omega   80.00  144.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000    0.0000 64

 42 omega   83.00  119.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000  -60.0000 36

 43 omega   78.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000   90.0000 25

 44 omega   81.00  118.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000 -180.0000 37

 45 omega   77.00  153.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000 -180.0000 76

 46 omega   78.00  148.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  120.0000 70

 47 omega  123.00  149.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000 -120.0000 26

 48 omega   80.00  115.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000  -90.0000 35

 49 omega   81.00  142.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  -90.0000 61

 50 omega   82.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000 -150.0000 26

 51 omega   77.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000 -120.0000 26

 52 omega   77.00  146.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000  -60.0000 69

 53 omega   81.00  159.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000   30.0000 78

 54 omega   26.00  104.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000 -180.0000 78

 55 omega   32.00  115.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000    0.0000 83

 56 omega   39.00   95.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000   90.0000 56

 57 omega   80.00  107.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   61.0000  -30.0000 27

 58 omega  111.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000   60.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1170047000
_diffrn_orient_matrix_UB_12      -0.0542294000
_diffrn_orient_matrix_UB_13      -0.0680164000
_diffrn_orient_matrix_UB_21      -0.0034434000
_diffrn_orient_matrix_UB_22      0.1215107000
_diffrn_orient_matrix_UB_23      -0.0796680000
_diffrn_orient_matrix_UB_31      0.1410136000
_diffrn_orient_matrix_UB_32      -0.0551138000
_diffrn_orient_matrix_UB_33      -0.0669097000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16557
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         5.10
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3970
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0580P)^2^+0.6903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                3600
_reflns_number_total             3970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05248j2.cif
_cod_data_source_block           lzl1cult
_cod_original_cell_volume        1128.73(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115630
_chemical_oxdiff_formula         'Si O4 Ph2 Bu3 Me'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13