Catalyst-free Synthesis of Novel Dimeric β-Carboline Derivatives via An Unexpected [2 + 2 + 2] Annulation
Cui, Hai-Lei; Wang, Jiang-Fang; Zhou, Hai-Lin; You, Xiao-Lin; Jiang, Xiao-Jie; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB00689F

data_7155578
_publ_section_title
;
 Catalyst-free Synthesis of Novel Dimeric \b-Carboline Derivatives via An
 Unexpected [2 + 2 + 2] Annulation
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB00689F
_journal_year                    2017
_chemical_formula_moiety         'C2.24 H2.15 N0.24 O0.21'
_chemical_formula_sum            'C2.24 H2.15 N0.24 O0.21'
_chemical_formula_weight         35.74
_chemical_name_systematic
; 
 ? 
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                87.669(10)
_cell_angle_beta                 72.107(9)
_cell_angle_gamma                70.902(9)
_cell_formula_units_Z            67
_cell_length_a                   13.255(2)
_cell_length_b                   15.682(3)
_cell_length_c                   17.830(3)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.53
_cell_volume                     3325.5(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      296(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.1154
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            108746
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1268
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0082(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         14891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2105
_refine_ls_R_factor_gt           0.1099
_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^)+(0.1798P)^2^+3.2582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2901
_refine_ls_wR_factor_ref         0.3683
_reflns_number_gt                6840
_reflns_number_total             14891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ob00689f3.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3325.3(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7155578