Clerodane Diterpenoids from Croton crassifolius.
Wang, Guo-Cai; Li, Jia-Gui; Li, Guo-Qiang; Xu, Jiao-Jiao; Wu, Xia; Ye, Wen-Cai; Li, Yao-Lan; Journal of natural products 75 (2012) 2188–2192; doi:10.1021/np300636k

data_1508565
_publ_section_title
;
 Clerodane Diterpenoids from Croton crassifolius.
;
_journal_issue                   12
_journal_name_full               'Journal of natural products'
_journal_page_first              2188
_journal_page_last               2192
_journal_paper_doi               10.1021/np300636k
_journal_volume                  75
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C19 H20 O6'
_chemical_formula_sum            'C19 H20 O6'
_chemical_formula_weight         344.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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             2012-09-18
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7585(2)
_cell_length_b                   7.0786(3)
_cell_length_c                   35.5061(12)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.6066
_cell_measurement_theta_min      3.7316
_cell_volume                     1698.64(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega -107.00  -63.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184 -178.0000 -180.0000 44

  2 omega  -86.00  -57.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184 -178.0000  -60.0000 29

  3 omega   17.00   45.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   57.0000   30.0000 28

  4 omega    8.00   59.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000  -60.0000 51

  5 omega   64.00  100.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000  -60.0000 36

  6 omega   36.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000  120.0000 45

  7 omega   20.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000    0.0000 49

  8 omega   20.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000 -150.0000 47

  9 omega   46.00   79.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000 -150.0000 33

 10 omega   30.00   55.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -30.0000  -90.0000 25

 11 omega  109.00  160.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  150.0000 51

 12 omega   63.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  150.0000 38
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.2001936000
_diffrn_orient_matrix_UB_12      0.0744601000
_diffrn_orient_matrix_UB_13      0.0145090000
_diffrn_orient_matrix_UB_21      -0.0916197000
_diffrn_orient_matrix_UB_22      0.0326918000
_diffrn_orient_matrix_UB_23      0.0392222000
_diffrn_orient_matrix_UB_31      0.0586325000
_diffrn_orient_matrix_UB_32      -0.2018310000
_diffrn_orient_matrix_UB_33      0.0116563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0143
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            3532
_diffrn_reflns_theta_full        62.70
_diffrn_reflns_theta_max         62.70
_diffrn_reflns_theta_min         4.98
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             693
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.132
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0533P)^2^+0.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                2176
_reflns_number_total             2257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np300636k_si_005.cif
_cod_data_source_block           lijiagui_k5423
_cod_depositor_comments
;

2019-03-16
Z value and formula fixed, original values are absolutely absurd
                 miguel
;
_cod_original_cell_volume        1698.63(10)
_cod_original_formula_moiety     '0.14(C76 H80 O24)'
_cod_original_formula_sum        'C11 H10 N O2'
_cod_original_formula_units_Z    7
_cod_original_formula_weight     188.20
_cod_database_code               1508565
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08