Synthesis and characterization of new carbazolocarbazoles: toward pi-extended N-fused heteroacenes
Curiel, David; Más-Montoya, Miriam; Uruvakili, Anasuyama; Orenes, Raúl A; Pallamreddy, Haranath; Molina, Pedro; Organic letters 12 (2010) 3164–3167; doi:10.1021/ol101076m

data_1503040
_publ_section_title
;
 Synthesis and characterization of new carbazolocarbazoles: toward
 pi-extended N-fused heteroacenes
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3164
_journal_page_last               3167
_journal_paper_doi               10.1021/ol101076m
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C39 H50 N2 O3'
_chemical_formula_weight         594.81
_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                97.279(2)
_cell_angle_beta                 92.240(2)
_cell_angle_gamma                117.315(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6711(9)
_cell_length_b                   8.7650(9)
_cell_length_c                   24.820(3)
_cell_measurement_reflns_used    4445
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.50
_cell_volume                     1652.4(3)
_computing_cell_refinement       'Bruker SAINT'
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20710
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_correction_T_min  0.8603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    'Me rigid, others riding, NH free'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7800
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0702
_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^)+(0.1202P)^2^+0.4908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2128
_reflns_number_gt                5453
_reflns_number_total             7800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol101076m_si_002.cif
_cod_data_source_block           mm48cls
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-01-01

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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               1503040