Synthesis and conformational properties of 2,6-bis-anilino-3-nitropyridines.
Schmid, Sylvia; Röttgen, Martin; Thewalt, Ulf; Austel, Volkhard; Organic & biomolecular chemistry 3 (2005) 3408–3421; doi:10.1039/b508819b

data_7150266
_publ_section_title
;
 Synthesis and conformational properties of
 2,6-bis-anilino-3-nitropyridines.
;
_journal_issue                   18
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3408
_journal_page_last               3421
_journal_paper_doi               10.1039/b508819b
_journal_volume                  3
_journal_year                    2005
_chemical_formula_sum            'C22 H22 N4 O4'
_chemical_formula_weight         406.44
_chemical_name_systematic
;
2-Anilino-6-(N-tert-bytyloxycarbonylanilino)-3-nitropyridine
;
_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
_cell_angle_alpha                72.57(2)
_cell_angle_beta                 83.91(2)
_cell_angle_gamma                75.36(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5952(16)
_cell_length_b                   9.790(2)
_cell_length_c                   13.308(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1033.2(4)
_computing_cell_refinement       'IPDS software (STOE, 1997)'
_computing_data_collection       'IPDS software (STOE, 1997)'
_computing_data_reduction        'IPDS software (STOE, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Johnson & Burnett, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'STOE IPDS system'
_diffrn_measurement_method       'Imaging plate'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11455
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9729
_exptl_absorpt_correction_T_min  0.9641
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                2720
_reflns_number_total             3763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508819b.txt
_cod_data_source_block           7i
_cod_original_cell_volume        1033.1(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7150266