Anti-inflammatory Grayanane Diterpenoids from the Leaves of Rhododendron molle
Zhou, Junfei; Liu, Tingting; Zhang, Hanqi; Zheng, Guijuan; Qiu, Yue; Deng, Mengyi; Zhang, Chun; Yao, Guangmin; Journal of Natural Products  (2017) –; doi:10.1021/acs.jnatprod.7b00799

data_1548539
_publ_section_title
;
 Anti-inflammatory Grayanane Diterpenoids from the Leaves of Rhododendron
 molle
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.7b00799
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H30 O5, 0.5(H2 O)'
_chemical_formula_sum            'C20 H31 O5.5'
_chemical_formula_weight         359.4
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2016-03-29T18:17:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.0960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2989(2)
_cell_length_b                   27.0429(6)
_cell_length_c                   11.3517(3)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      4.02
_cell_volume                     1875.43(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19443
_diffrn_reflns_theta_full        66.69
_diffrn_reflns_theta_max         66.69
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.03
_refine_ls_abs_structure_details
;
        Flack H D (1983), Acta Cryst. A39, 876-881;
        Flack  parameter = 0.1(1), 3398 Friedel pairs.
        Hooft <i>et al.</i> (2010) and Spek (2009);
        Hooft parameter = 0.09(4), 3133 Bijvoet pairs.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6531
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.2512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                6276
_reflns_number_total             6531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np7b00799_si_004.cif
_cod_data_source_block           p
_cod_depositor_comments
;

2019-03-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_moiety     '2(C20 H30 O5), H2 O'
_cod_original_formula_sum        'C40 H62 O11'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     718.9
_cod_database_code               1548539