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_4029042
_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         'C14 H20 O7'
_chemical_formula_sum            'C14 H20 O7'
_chemical_formula_weight         300.30
_chemical_name_systematic
;
 ? 
;
_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             2013-11-14
_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            12
_cell_length_a                   11.4480(2)
_cell_length_b                   14.0412(2)
_cell_length_c                   29.0912(4)
_cell_measurement_reflns_used    13144
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      71.4820
_cell_measurement_theta_min      4.1300
_cell_volume                     4676.23(12)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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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
;
XH, 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 0.9930
_diffrn_measured_fraction_theta_max 0.8423
_diffrn_measurement_details
;
  1 omega   85.00  174.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   77.0000  -90.0000 89

  2 omega   38.00   68.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  -60.0000 30

  3 omega  -21.00   10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -30.0000 31

  4 omega   17.00   42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -30.0000 25

  5 omega   73.00  123.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  -90.0000 50

  6 omega   91.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   30.0000 26

  7 omega  -15.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -19.0000  -30.0000 108

  8 omega   49.00   77.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 28

  9 omega   40.00   83.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 43

 10 omega   38.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -150.0000 29

 11 omega   42.00   68.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -120.0000 26

 12 omega  -31.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   78.0000  140.0000 101

 13 omega -124.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000  150.0000 90

 14 omega -112.00  -18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000  150.0000 94

 15 omega -127.00  -29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -38.0000   30.0000 98

 16 omega   38.00   77.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000 -120.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0603826000
_diffrn_orient_matrix_UB_12      0.0960733000
_diffrn_orient_matrix_UB_13      -0.0095315000
_diffrn_orient_matrix_UB_21      -0.0748552000
_diffrn_orient_matrix_UB_22      0.0127046000
_diffrn_orient_matrix_UB_23      -0.0435826000
_diffrn_orient_matrix_UB_31      -0.0941325000
_diffrn_orient_matrix_UB_32      0.0514231000
_diffrn_orient_matrix_UB_33      0.0285374000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            16525
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.50
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30451
_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    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(17)
_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     571
_refine_ls_number_reflns         7317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+2.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                7058
_reflns_number_total             7317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo402602h_si_003.cif
_cod_data_source_block           song6b
_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               4029042
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97