Hypercohin A, a new polycyclic polyprenylated acylphloroglucinol possessing an unusual bicyclo[5.3.1]hendecane core from Hypericum cohaerens
Xing-Wei Yang; Xu Deng; Xia Liu; Chun-Yan Wu; Xiao-Nian Li; Bin Wu; Huai-Rong Luo; Yan Li; Hong-Xi Xu; Qin-Shi Zhao; Gang Xu; Chem.Commun. 48 (2012) 5998–; doi:10.1039/c2cc32352d

data_7107840
_publ_section_title
;
 Hypercohin A, a new polycyclic polyprenylated acylphloroglucinol
 possessing an unusual bicyclo[5.3.1]hendecane core from Hypericum
 cohaerens
;
_journal_name_full               Chem.Commun.
_journal_page_first              5998
_journal_paper_doi               10.1039/c2cc32352d
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H51 Br O6'
_chemical_formula_sum            'C45 H51 Br O6'
_chemical_formula_weight         767.77
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.794(2)
_cell_angle_beta                 70.787(2)
_cell_angle_gamma                78.211(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0921(12)
_cell_length_b                   9.5542(12)
_cell_length_c                   12.8573(17)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.25
_cell_volume                     1000.4(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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13227
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.5556
_exptl_absorpt_correction_T_min  0.4448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.62
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9544
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                8716
_reflns_number_total             9544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32352d.txt
_cod_data_source_block           mo_fxy70_sad
_cod_database_code               7107840