Facile, efficient, and diastereoselective synthesis of heterohelicene-like molecules.
Lin, Wei; Dou, Guo-Lan; Hu, Ming-Hua; Cao, Cheng-Pao; Huang, Zhi-Bin; Shi, Da-Qing; Organic letters 15 (2013) 1238–1241; doi:10.1021/ol400154j

data_1511858
_publ_section_title
;
 Facile, efficient, and diastereoselective synthesis of
 heterohelicene-like molecules.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1238
_journal_page_last               1241
_journal_paper_doi               10.1021/ol400154j
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C26 H18.5 N2 O4.25'
_chemical_formula_weight         426.93
_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                67.939(4)
_cell_angle_beta                 71.678(3)
_cell_angle_gamma                65.260(4)
_cell_formula_units_Z            4
_cell_length_a                   11.735(3)
_cell_length_b                   13.252(4)
_cell_length_c                   15.517(5)
_cell_measurement_reflns_used    2125
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      2.575
_cell_volume                     1995.4(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10409
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.9546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         6900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0636P)^2^+0.6326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                3552
_reflns_number_total             6900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol400154j_si_002.cif
_cod_data_source_block           060711b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1995.5(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26 H18.50 N2 O4.25'
_cod_database_code               1511858