#------------------------------------------------------------------------------
#$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003082.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2003082
_journal_name_full               'Acta Crystallographica, Section B'
_journal_volume                  55
_journal_year     1999
_journal_page_first     410
_journal_page_last     423
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
loop_
_publ_author_name
;
Frederik C. Krebs
;
_chemical_name_systematic
;
 4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium
nitratehydrogennitrate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C19 H10 N2 O9,H N O3,N O3'
_chemical_formula_sum     'C19 H10 N2 O9'
_chemical_formula_weight     410.29
_symmetry_cell_setting     monoclinic
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x-1/2, -y-1/2, z-1/2'
_cell_length_a     6.4960(13)
_cell_length_b     7.6530(15)
_cell_length_c     33.039(7)
_cell_angle_alpha     90.00
_cell_angle_beta     91.95(3)
_cell_angle_gamma     90.00
_cell_volume     1641.5(6)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min     ?
_cell_measurement_theta_max     ?
_cell_measurement_temperature     120(2)
_exptl_crystal_description     plate
_exptl_crystal_colour     orange
_exptl_crystal_size_max     0.43
_exptl_crystal_size_mid     0.18
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     1.660
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     840
_exptl_absorpt_coefficient_mu     0.136
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_correction_T_min     0.776
_exptl_absorpt_correction_T_max     0.980
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens SMART CCD'
_diffrn_measurement_method     'omega scan, frame data integration'
_diffrn_detector_area_resol_mean     8.192
_diffrn_reflns_number     17025
_diffrn_reflns_av_R_equivalents     0.0622
_diffrn_reflns_av_sigmaI/netI     0.0479
_diffrn_reflns_theta_min     1.23
_diffrn_reflns_theta_max     26.33
_diffrn_reflns_theta_full     26.33
_diffrn_measured_fraction_theta_max     0.926
_diffrn_measured_fraction_theta_full     0.926
_diffrn_reflns_limit_h_min     -8
_diffrn_reflns_limit_h_max     8
_diffrn_reflns_limit_k_min     -9
_diffrn_reflns_limit_k_max     9
_diffrn_reflns_limit_l_min     -41
_diffrn_reflns_limit_l_max     41
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_reflns_number_total     3345
_reflns_number_gt     2173
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0852
_refine_ls_R_factor_gt     0.0425
_refine_ls_wR_factor_ref     0.1134
_refine_ls_goodness_of_fit_ref     1.002
_refine_ls_restrained_S_all     1.002
_refine_ls_number_reflns     3345
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme
         'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.5233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_shift/su_max     0.002
_refine_diff_density_max     0.219
_refine_diff_density_min     -0.268
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    O1 0.7353(2) 0.89044(19) 0.16804(4) 0.0197(4) Uani d . 1 . . O
    O2 0.2733(2) 1.00261(19) 0.05309(4) 0.0209(4) Uani d . 1 . . O
    O3 0.1106(2) 1.22049(19) 0.18556(4) 0.0216(4) Uani d . 1 . . O
    C1 0.3724(3) 1.0371(3) 0.13560(6) 0.0163(5) Uani d . 1 . . C
    C2 0.5040(3) 0.9468(3) 0.11042(6) 0.0164(5) Uani d . 1 . . C
    C3 0.6851(3) 0.8702(3) 0.12728(6) 0.0175(5) Uani d . 1 . . C
    C4 0.8125(3) 0.7748(3) 0.10320(7) 0.0213(5) Uani d . 1 . . C
    H4 0.9314 0.7223 0.1139 0.026 Uiso calc . 1 . . H
    C5 0.7569(4) 0.7596(3) 0.06216(7) 0.0237(5) Uani d . 1 . . C
    H5 0.8422 0.6953 0.0457 0.028 Uiso calc . 1 . . H
    C6 0.5798(4) 0.8359(3) 0.04435(7) 0.0224(5) Uani d . 1 . . C
    H6 0.5492 0.8244 0.0168 0.027 Uiso calc . 1 . . H
    C7 0.4524(3) 0.9288(3) 0.06910(6) 0.0179(5) Uani d . 1 . . C
    C8 0.1912(3) 1.1098(3) 0.11928(6) 0.0182(5) Uani d . 1 . . C
    C9 0.1438(3) 1.0947(3) 0.07770(6) 0.0192(5) Uani d . 1 . . C
    C10 -0.0301(3) 1.1744(3) 0.06117(7) 0.0235(5) Uani d . 1 . . C
    H10 -0.0631 1.1666 0.0336 0.028 Uiso calc . 1 . . H
    C11 -0.1544(4) 1.2668(3) 0.08711(7) 0.0251(5) Uani d . 1 . . C
    H11 -0.2718 1.3205 0.0761 0.030 Uiso calc . 1 . . H
    C12 -0.1141(3) 1.2843(3) 0.12880(7) 0.0242(5) Uani d . 1 . . C
    H12 -0.2017 1.3470 0.1451 0.029 Uiso calc . 1 . . H
    C13 0.0611(3) 1.2045(3) 0.14470(6) 0.0192(5) Uani d . 1 . . C
    C14 0.4229(3) 1.0553(3) 0.17675(6) 0.0171(5) Uani d . 1 . . C
    C15 0.2893(3) 1.1470(3) 0.20178(6) 0.0193(5) Uani d . 1 . . C
    C16 0.3357(4) 1.1634(3) 0.24261(7) 0.0246(5) Uani d . 1 . . C
    H16 0.2479 1.2217 0.2597 0.029 Uiso calc . 1 . . H
    C17 0.5194(4) 1.0892(3) 0.25738(7) 0.0247(5) Uani d . 1 . . C
    H17 0.5523 1.1006 0.2849 0.030 Uiso calc . 1 . . H
    C18 0.6572(4) 0.9988(3) 0.23348(7) 0.0231(5) Uani d . 1 . . C
    H18 0.7785 0.9521 0.2446 0.028 Uiso calc . 1 . . H
    C19 0.6070(3) 0.9813(3) 0.19297(7) 0.0188(5) Uani d . 1 . . C
    N1 0.2727(3) 0.5112(2) 0.03952(6) 0.0213(4) Uani d . 1 . . N
    O4 0.2160(2) 0.58203(19) 0.07456(4) 0.0230(4) Uani d . 1 . . O
    H4A 0.2701 0.5281 0.0935 0.035 Uiso calc PR 0.50 . . H
    O5 0.3911(2) 0.3865(2) 0.04094(5) 0.0268(4) Uani d . 1 . . O
    O6 0.1997(3) 0.5790(2) 0.00891(5) 0.0307(4) Uani d . 1 . . O
    N2 0.4074(3) 0.5514(2) 0.16270(6) 0.0216(4) Uani d . 1 . . N
    O7 0.2678(3) 0.6628(2) 0.16200(5) 0.0276(4) Uani d . 1 . . O
    O8 0.5267(3) 0.5279(2) 0.19189(5) 0.0353(5) Uani d . 1 . . O
    O9 0.4293(2) 0.45440(19) 0.13082(5) 0.0250(4) Uani d . 1 . . O
    H9 0.3957 0.3537 0.1359 0.038 Uiso calc PR 0.50 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    O1 0.0199(8) 0.0211(8) 0.0180(8) 0.0043(6) 0.0003(6) -0.0006(6)
    O2 0.0225(9) 0.0213(8) 0.0187(8) -0.0001(7) -0.0024(7) -0.0001(6)
    O3 0.0200(9) 0.0250(8) 0.0199(8) 0.0040(7) 0.0025(7) -0.0004(6)
    C1 0.0178(12) 0.0124(10) 0.0189(12) -0.0039(8) 0.0020(9) 0.0021(8)
    C2 0.0167(11) 0.0145(11) 0.0179(11) -0.0025(8) 0.0002(9) -0.0003(8)
    C3 0.0196(12) 0.0169(11) 0.0162(11) -0.0025(9) 0.0014(9) 0.0015(9)
    C4 0.0214(13) 0.0174(11) 0.0251(13) 0.0012(9) 0.0019(10) -0.0009(9)
    C5 0.0234(13) 0.0187(11) 0.0295(14) -0.0008(9) 0.0086(10) -0.0040(10)
    C6 0.0275(13) 0.0211(12) 0.0188(12) -0.0046(10) 0.0034(10) -0.0018(9)
    C7 0.0166(12) 0.0161(11) 0.0208(12) -0.0039(9) -0.0011(9) 0.0014(9)
    C8 0.0168(11) 0.0174(11) 0.0204(12) -0.0030(9) 0.0000(9) 0.0030(9)
    C9 0.0185(12) 0.0169(11) 0.0223(12) -0.0045(9) 0.0005(9) 0.0012(9)
    C10 0.0239(13) 0.0227(12) 0.0234(12) -0.0055(10) -0.0054(10) 0.0041(10)
    C11 0.0179(12) 0.0236(13) 0.0335(14) -0.0015(9) -0.0045(11) 0.0062(10)
    C12 0.0176(12) 0.0203(12) 0.0350(14) 0.0004(9) 0.0047(10) 0.0031(10)
    C13 0.0182(12) 0.0166(11) 0.0230(12) -0.0031(9) 0.0008(10) 0.0019(9)
    C14 0.0183(12) 0.0168(11) 0.0164(11) -0.0032(9) 0.0016(9) 0.0014(9)
    C15 0.0203(12) 0.0175(11) 0.0202(12) -0.0009(9) 0.0013(9) 0.0011(9)
    C16 0.0318(14) 0.0214(12) 0.0209(12) -0.0021(10) 0.0073(10) -0.0018(9)
    C17 0.0335(14) 0.0248(12) 0.0155(11) -0.0041(11) -0.0008(10) 0.0004(9)
    C18 0.0267(13) 0.0216(11) 0.0208(12) 0.0014(10) -0.0038(10) 0.0010(9)
    C19 0.0201(12) 0.0161(11) 0.0201(12) -0.0006(9) 0.0018(9) 0.0009(9)
    N1 0.0176(10) 0.0249(10) 0.0216(11) -0.0039(8) 0.0021(8) -0.0031(8)
    O4 0.0242(9) 0.0267(8) 0.0182(8) 0.0056(7) 0.0016(7) -0.0032(7)
    O5 0.0262(9) 0.0242(9) 0.0301(10) 0.0060(7) 0.0033(7) -0.0055(7)
    O6 0.0326(10) 0.0381(10) 0.0212(9) 0.0016(8) -0.0048(8) 0.0039(7)
    N2 0.0245(11) 0.0205(10) 0.0199(10) -0.0056(8) 0.0022(9) 0.0019(8)
    O7 0.0365(10) 0.0242(9) 0.0223(9) 0.0066(8) 0.0045(7) 0.0002(7)
    O8 0.0343(11) 0.0475(11) 0.0234(10) -0.0017(8) -0.0106(8) 0.0009(8)
    O9 0.0270(9) 0.0231(8) 0.0248(9) 0.0017(7) -0.0013(7) -0.0040(7)
_cod_database_code 2003082