ent-Rosane diterpenoids from Euphorbia milii showing an Epstein–Barr virus lytic replication assay
Liu, Shao-Nan; Hu, Jiayuan; Tan, Shen H.; Wang, Qian; Xu, Jun; Wang, Yan; Yuan, Yan; Gu, Qiong; RSC Adv. 7 (2017) 46938–; doi:10.1039/C7RA08877A

data_7229291
_publ_section_title
;
 ent-Rosane diterpenoids from Euphorbia milii showing an Epstein--Barr
 virus lytic replication assay
;
_journal_issue                   74
_journal_name_full               'RSC Adv.'
_journal_page_first              46938
_journal_paper_doi               10.1039/C7RA08877A
_journal_volume                  7
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C27 H33 Br O3'
_chemical_formula_sum            'C27 H33 Br O3'
_chemical_formula_weight         485.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-10 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4504(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.86059(7)
_cell_length_b                   12.67519(17)
_cell_length_c                   15.73654(19)
_cell_measurement_reflns_used    16985
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.2500
_cell_measurement_theta_min      3.4460
_cell_volume                     1165.45(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2417
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -114.00 -19.00   1.00    2.00    --  -44.40 -57.00 -90.00   95
  2  \w   -118.00 -73.00   1.00    2.00    --  -44.40-125.00  60.00   45
  3  \w   -118.00 -73.00   1.00    2.00    --  -44.40-125.00 -30.00   45
  4  \w   -126.00 -79.00   1.00    2.00    --  -44.40 -99.00-180.00   47
  5  \w   -126.00 -79.00   1.00    2.00    --  -44.40 -99.00-150.00   47
  6  \w    -25.00  70.00   1.00    2.00    --   44.40 -57.00 -30.00   95
  7  \w    -25.00  70.00   1.00    2.00    --   44.40 -57.00-150.00   95
  8  \w     26.00 121.00   1.00    5.00    --  100.00-125.00-180.00   95
  9  \w     61.00 178.00   1.00    5.00    --  100.00  15.00  90.00  117
 10  \w     26.00 121.00   1.00    5.00    --  100.00-125.00   0.00   95
 11  \w     68.00 174.00   1.00    5.00    --  100.00  77.00-120.00  106
 12  \w     26.00 121.00   1.00    5.00    --  100.00-125.00  30.00   95
 13  \w     30.00 127.00   1.00    5.00    --  100.00 -61.00  30.00   97
 14  \w     26.00 121.00   1.00    5.00    --  100.00-125.00 120.00   95
 15  \w     76.00 171.00   1.00    5.00    --  100.00  45.00  90.00   95
 16  \w     26.00 132.00   1.00    5.00    --  100.00 -77.00 150.00  106
 17  \w     25.00 117.00   1.00    5.00    --  100.00-117.00-107.00   92
 18  \w     26.00 121.00   1.00    5.00    --  100.00-125.00 -30.00   95
 19  \w     17.00 109.00   1.00    5.00    --  100.00 -94.00  30.00   92
 20  \w     29.00 124.00   1.00    5.00    --  100.00 -45.00 150.00   95
 21  \w     17.00 109.00   1.00    5.00    --  100.00 -94.00   0.00   92
 22  \w     17.00 109.00   1.00    5.00    --  100.00 -94.00 150.00   92
 23  \w     73.00 174.00   1.00    5.00    --  100.00 125.00-120.00  101
 24  \w     76.00 171.00   1.00    5.00    --  100.00  45.00-180.00   95
 25  \w     29.00 124.00   1.00    5.00    --  100.00 -45.00-120.00   95
 26  \w     17.00 109.00   1.00    5.00    --  100.00 -94.00-150.00   92
 27  \w     74.00 156.00   1.00    5.00    --  100.00  30.00-120.00   82
 28  \w    103.00 169.00   1.00    5.00    --  100.00  45.00 -30.00   66
 29  \w     88.00 138.00   1.00    5.00    --  100.00 -15.00 -90.00   50
 30  \w     56.00  85.00   1.00    5.00    --  100.00 -94.00 -60.00   29
 31  \w     30.00  98.00   1.00    5.00    --  100.00 -45.00 -60.00   68
 32  \w     94.00 121.00   1.00    5.00    --  100.00-125.00-150.00   27
 33  \w    114.00 156.00   1.00    5.00    --  100.00 125.00  30.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1469905000
_diffrn_orient_matrix_UB_12      0.0537925000
_diffrn_orient_matrix_UB_13      -0.0729759000
_diffrn_orient_matrix_UB_21      -0.0383424000
_diffrn_orient_matrix_UB_22      -0.1076169000
_diffrn_orient_matrix_UB_23      -0.0444594000
_diffrn_orient_matrix_UB_31      -0.2154155000
_diffrn_orient_matrix_UB_32      -0.0175946000
_diffrn_orient_matrix_UB_33      0.0483482000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21844
_diffrn_reflns_theta_full        72.1236
_diffrn_reflns_theta_max         72.12
_diffrn_reflns_theta_min         4.48
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3833
_exptl_crystal_description       block
_exptl_crystal_F_000             507.9511
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2453
_refine_diff_density_min         -0.4392
_refine_diff_density_rms         0.0499
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             9.8596
_refine_ls_goodness_of_fit_ref   1.0350
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    48
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4565
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0350
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.4722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.994
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                4538
_reflns_number_total             4565
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ra08877a2.cif
_cod_data_source_block           lsn_170707
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7229291
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C12(H12a,H12b), C22(H22a,H22b), C23(H23a,H23b), C25(H25a,H25b),
 C26(H26a,H26b), C29(H29a,H29b), C32(H32a,H32b)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C11(H11), C13(H13), C5(H5), C27(H27)
2.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C17(H17a,H17b,H17c), C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.372
_oxdiff_exptl_absorpt_empirical_full_min 0.535