Grayanane Diterpenoid Glucosides from the Leaves of Rhododendron micranthum and Their Bioactivities Evaluation.
Sun, Na; Zhu, Yan; Zhou, Haofeng; Zhou, Junfei; Zhang, Hanqi; Zhang, Mengke; Zeng, Hong; Yao, Guangmin; Journal of natural products 81 (2018) 2673–2681; doi:10.1021/acs.jnatprod.8b00490

data_1553394
_publ_section_title
;
 Grayanane Diterpenoid Glucosides from the Leaves of Rhododendron
 micranthum and Their Bioactivities Evaluation.
;
_journal_issue                   12
_journal_name_full               'Journal of natural products'
_journal_page_first              2673
_journal_page_last               2681
_journal_paper_doi               10.1021/acs.jnatprod.8b00490
_journal_volume                  81
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H42 O8, 0.5(C H4 O), 3(H2 O) '
_chemical_formula_sum            'C26.5 H50 O11.5'
_chemical_formula_weight         552.66
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.621(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.3352(3)
_cell_length_b                   39.6779(16)
_cell_length_c                   11.4316(5)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      3.87
_cell_volume                     2873.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40859
_diffrn_reflns_theta_full        67.51
_diffrn_reflns_theta_max         67.51
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.9077
_exptl_absorpt_correction_T_min  0.8796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881;
Flack  parameter = 0.0(2), 4740 Friedel pairs.
Hooft <i>et al.</i> (2010) and Spek (2009);
Hooft parameter = 0.04(9), 4747 Bijvoet pairs.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         10000
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0956P)^2^+0.5164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                8300
_reflns_number_total             10000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np8b00490_si_004.cif
_cod_data_source_block           t
_cod_depositor_comments
;

2022-11-30
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(C26 H42 O8), C H4 O, 6(H2 O) '"
_cod_original_formula_sum        'C53 H100 O23'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1105.33
_cod_database_code               1553394