Rhodomollacetals A-C, PTP1B Inhibitory Diterpenoids with a 2,3:5,6-Di-seco-grayanane Skeleton from the Leaves of Rhododendron molle.
Zhou, Junfei; Sun, Na; Zhang, Hanqi; Zheng, Guijuan; Liu, Junjun; Yao, Guangmin; Organic letters 19 (2017) 5352–5355; doi:10.1021/acs.orglett.7b02633

data_1547393
_publ_section_title
;
 Rhodomollacetals A-C, PTP1B Inhibitory Diterpenoids with a
 2,3:5,6-Di-seco-grayanane Skeleton from the Leaves of Rhododendron molle.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              5352
_journal_page_last               5355
_journal_paper_doi               10.1021/acs.orglett.7b02633
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C22 H34 O7'
_chemical_formula_weight         410.49
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.0500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1637(3)
_cell_length_b                   6.9628(2)
_cell_length_c                   13.0151(4)
_cell_measurement_reflns_used    9191
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      3.50
_cell_volume                     1069.32(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12135
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.9130
_exptl_absorpt_correction_T_min  0.8609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881;
Flack  parameter = 0.1(1), 1721 Friedel pairs.
Hooft <i>et al.</i> (2010) and Spek (2009);
Hooft parameter = 0.05(6), 1731 Bijvoet pairs.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3833
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.1140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                3647
_reflns_number_total             3833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b02633_si_003.cif
_cod_data_source_block           p
_cod_depositor_comments
'Adding full bibliography for 1547392--1547393.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1547393
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.754