Structural Revision of Cephalosporolide J and Bassianolone.
Song, Liyan; Lee, Ka-Ho; Lin, Zhenyang; Tong, Rongbiao; The Journal of organic chemistry 79 (2014) 1493–; doi:10.1021/jo402602h

data_4029043
_publ_section_title
;
 Structural Revision of Cephalosporolide J and Bassianolone.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1493
_journal_paper_doi               10.1021/jo402602h
_journal_volume                  79
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H16 O5'
_chemical_formula_sum            'C10 H16 O5'
_chemical_formula_weight         216.23
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-25
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.55970(10)
_cell_length_b                   8.6192(3)
_cell_length_c                   21.5904(6)
_cell_measurement_reflns_used    4390
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.5470
_cell_measurement_theta_min      4.0830
_cell_volume                     1034.62(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.9804
_diffrn_measurement_details
;
  1 omega   40.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000   30.0000 108

  2 omega   32.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 45

  3 omega  -25.00    2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -120.0000 27

  4 omega   16.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -120.0000 26

  5 omega -126.00  -29.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -38.0000  -90.0000 97

  6 omega   26.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   76.0000   14.0000 26

  7 omega -134.00  -43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -50.0000   30.0000 91

  8 omega  -82.00  -53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  120.0000 29

  9 omega  -87.00    2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   64.0000 -180.0000 89

 10 omega -141.00  -86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  120.0000 55

 11 omega   37.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 25

 12 omega   53.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 30

 13 omega   38.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 31

 14 omega   39.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   60.0000 30

 15 omega   40.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -180.0000 39

 16 omega   39.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 28

 17 omega  119.00  144.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -30.0000 25

 18 omega   74.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -30.0000 26

 19 omega   40.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 43

 20 omega   41.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   30.0000 28

 21 omega   38.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -12.0000  150.0000 137

 22 omega   92.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000 -180.0000 81

 23 omega   38.00  132.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -93.0000 -156.7432 94
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1636395000
_diffrn_orient_matrix_UB_12      -0.1056167000
_diffrn_orient_matrix_UB_13      0.0392099000
_diffrn_orient_matrix_UB_21      -0.0489560000
_diffrn_orient_matrix_UB_22      -0.1357636000
_diffrn_orient_matrix_UB_23      -0.0446820000
_diffrn_orient_matrix_UB_31      0.2180688000
_diffrn_orient_matrix_UB_32      0.0487472000
_diffrn_orient_matrix_UB_33      -0.0394772000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5285
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         66.92
_diffrn_reflns_theta_min         4.10
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0540P)^2^+0.1570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                1790
_reflns_number_total             1819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo402602h_si_002.cif
_cod_data_source_block           song5cult
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4029043
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13