Jatrophane Diterpenoids from Euphorbia glomerulans.
Hasan, Aobulikasimu; Liu, Ge-Yu; Hu, Rui; Aisa, H. A.; Journal of natural products 82 (2019) 724–734; doi:10.1021/acs.jnatprod.8b00507

data_1552631
_publ_section_title
;
 Jatrophane Diterpenoids from Euphorbia glomerulans.
;
_journal_issue                   4
_journal_name_full               'Journal of natural products'
_journal_page_first              724
_journal_page_last               734
_journal_paper_doi               10.1021/acs.jnatprod.8b00507
_journal_volume                  82
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C42 H48 O13'
_chemical_formula_sum            'C42 H48 O13'
_chemical_formula_weight         760.80
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9837(6)
_cell_length_b                   14.7826(9)
_cell_length_c                   27.9856(17)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.996
_cell_measurement_theta_min      3.159
_cell_volume                     4130.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            49724
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.699
_diffrn_reflns_theta_min         3.158
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1645 before and 0.0755 after correction. The Ratio of minimum to maximum transmission is 0.8517. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 2553 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         7627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.6273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                6495
_reflns_number_total             7627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np8b00507_si_004.cif
_cod_data_source_block           cu_20181199-egm-4_0m
_cod_database_code               1552631
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.817
_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:
 C13(H13), C3(H3), C15(H15), C4(H4), C12(H12), C7(H7), C2(H2), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C9(H9), C36(H36), C8(H8), C37(H37), C39(H39), C38(H38), C22(H22),
 C18(H18), C19(H19), C21(H21), C20(H20)
2.d X=CH2 refined with riding coordinates:
 C40(H40A,H40B)
2.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C26(H26A,H26B,H26C), C42(H42A,H42B,H42C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C28(H28A,
 H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'