Diaza[3.3]benzenopyridino[2]phane
Boomgaarden, Wolfgang; Nieger, Martin; Acta Crystallographica Section E 60 (2004) o523–o524; doi:10.1107/S1600536804004751

data_2203443
_publ_section_title
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 Diaza[3.3]benzenopyridino[2]phane
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o523
_journal_page_last               o524
_journal_paper_doi               10.1107/S1600536804004751
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C35 H37 N3 O8 S2'
_chemical_formula_moiety         'C35 H37 N3 O8 S2'
_chemical_formula_sum            'C35 H37 N3 O8 S2'
_chemical_formula_weight         691.80
_chemical_name_systematic
;
14,16-Bis(ethoxycarbonyl)2,11-bis(4-tolylsulfonyl)-2,11-diaza[3.3](1,3)-
benzeno(2,6)pyridino[2]phane
;
_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           SHELXL97
_cell_angle_alpha                104.690(10)
_cell_angle_beta                 97.850(10)
_cell_angle_gamma                106.770(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5040(10)
_cell_length_b                   11.3590(10)
_cell_length_c                   17.5480(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44
_cell_measurement_theta_min      30
_cell_volume                     1709.0(3)
_computing_cell_refinement       CAD-4-PC
_computing_data_collection       'CAD-4-PC (Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2001)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius MACH3'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8256
_diffrn_reflns_theta_full        67.90
_diffrn_reflns_theta_max         67.90
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_count '200 (orientation)'
_diffrn_standards_interval_time  '60 min (intensity)'
_diffrn_standards_number         '3 (orientation), 2 (intensity)'
_exptl_absorpt_coefficient_mu    1.880
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(SHELXTL-NT; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0651P)^2^+0.6802P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                5009
_reflns_number_total             6149
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6022.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               2203443
_cod_database_fobs_code          2203443