Cinnamomols A and B, Immunostimulative Diterpenoids with a New Carbon Skeleton from the Leaves of Cinnamomum cassia.
Zhou, Lei; Tuo, Yali; Hao, Yi; Guo, Xiaoman; Tang, Wei; Xue, Yongbo; Zeng, Junfen; Zhou, Yu; Xiang, Ming; Zuo, Jianping; Yao, Guangmin; Zhang, Yonghui; Organic letters 19 (2017) 3029–3032; doi:10.1021/acs.orglett.7b01323

data_1546099
_publ_section_title
;
 Cinnamomols A and B, Immunostimulative Diterpenoids with a New Carbon
 Skeleton from the Leaves of Cinnamomum cassia.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              3029
_journal_page_last               3032
_journal_paper_doi               10.1021/acs.orglett.7b01323
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H30 O8, 3(H2 O)'
_chemical_formula_sum            'C20 H36 O11'
_chemical_formula_weight         452.49
_space_group_IT_number           154
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   17.1874(8)
_cell_length_b                   17.1874(8)
_cell_length_c                   42.085(2)
_cell_measurement_reflns_used    7811
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      71.24
_cell_measurement_theta_min      3.70
_cell_volume                     10766.6(9)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12148
_diffrn_reflns_theta_full        65.83
_diffrn_reflns_theta_max         65.83
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.8462
_exptl_absorpt_correction_T_min  0.8066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
?
;
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881;
Flack  parameter = 0.0(1), 5363 Friedel pairs.
Hooft <i>et al.</i> (2010) and Spek (2009);
Hooft parameter = 0.07(5), 5363 Bijvoet pairs.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         12148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0607
_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^)+(0.1227P)^2^+2.4043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                11443
_reflns_number_total             12148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b01323_si_002.cif
_cod_data_source_block           cu_150330e_0m
_cod_depositor_comments
'Adding full bibliography for 1546098--1546099.cif.'
_cod_database_code               1546099