Folding-induced selective hydrogenation of helical 9,10-anthraquinone analogues.
Hu, Hai-Yu; Xiang, Jun-Feng; Cao, Jing; Chen, Chuan-Feng; Organic letters 10 (2008) 5035–5038; doi:10.1021/ol802241h

data_1504956
_publ_section_title
;
 Folding-induced selective hydrogenation of helical 9,10-anthraquinone
 analogues.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5035
_journal_page_last               5038
_journal_paper_doi               10.1021/ol802241h
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C138 H160 N16 O26'
_chemical_formula_weight         2458.82
_space_group_IT_number           2
_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                84.27(3)
_cell_angle_beta                 70.17(2)
_cell_angle_gamma                67.43(3)
_cell_formula_units_Z            2
_cell_length_a                   16.062(4)
_cell_length_b                   20.088(5)
_cell_length_c                   22.642(6)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8884
_cell_measurement_theta_min      1.4530
_cell_volume                     6342(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_sigmaI/netI    0.1453
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47418
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_correction_T_min  0.9875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1649
_refine_ls_number_reflns         21900
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.2082
_refine_ls_R_factor_gt           0.1533
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1813P)^2^+14.3359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3804
_refine_ls_wR_factor_ref         0.4190
_reflns_number_gt                13609
_reflns_number_total             21900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol802241h_si_002.cif
_cod_data_source_block           shelxs
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1504956