Preparation and Study of 1,8-Di(pyrid-2'-yl)carbazoles
Maria S. Mudadu; Ajay N. Singh; Randolph P. Thummel; Journal of Organic Chemistry 73 (2008) 6513–6520; doi:10.1021/jo801132w

data_4023652
_publ_section_title
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 Preparation and Study of 1,8-Di(pyrid-2'-yl)carbazoles
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6513
_journal_page_last               6520
_journal_paper_doi               10.1021/jo801132w
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C30 H31 N3'
_chemical_formula_weight         433.58
_chemical_name_systematic
; 
 ? 
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_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                64.843(2)
_cell_angle_beta                 86.835(4)
_cell_angle_gamma                82.569(2)
_cell_formula_units_Z            4
_cell_length_a                   11.888(1)
_cell_length_b                   14.020(2)
_cell_length_c                   16.414(3)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      1.62
_cell_volume                     2455.4(7)
_computing_cell_refinement       'Bruker SAINT software (Bruker, 1999)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11379
_diffrn_reflns_theta_full        23.51
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9429
_exptl_absorpt_correction_T_min  0.8806
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular column'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0064(7)
_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   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7231
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.227
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+2.0211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                4508
_reflns_number_total             7231
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            jo801132w_si_001.cif
_cod_data_source_block           5H
_cod_depositor_comments
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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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4023652