#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:08:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179441 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/38/4333853.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_4333853
loop_
_publ_author_name
'Hamid Khaledi'
'Marilyn M. Olmstead'
'Hapipah Mohd Ali'
'Noel F. Thomas'
_publ_section_title
;
 Indolenine meso-Substituted Dibenzotetraaza[14]annulene and Its
 Coordination Chemistry toward the Transition Metal Ions MnIII, FeIII,
 CoII, NiII, CuII, and PdII
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1926
_journal_page_last               1941
_journal_paper_doi               10.1021/ic302150j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C38 H34 N6'
_chemical_formula_sum            'C38 H34 N6'
_chemical_formula_weight         574.71
_chemical_name_systematic
; 
 ? 
;
_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                82.332(3)
_cell_angle_beta                 85.697(4)
_cell_angle_gamma                87.857(4)
_cell_formula_units_Z            2
_cell_length_a                   6.8570(5)
_cell_length_b                   14.2898(8)
_cell_length_c                   14.9747(9)
_cell_measurement_reflns_used    2822
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      2.75
_cell_volume                     1449.52(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7648
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.9858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       lath
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         4927
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0778
_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/[σ²(Fo²)+(0.0507P)²+6.7967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2138
_refine_ls_wR_factor_ref         0.2217
_reflns_number_gt                3932
_reflns_number_total             4927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302150j_si_002_01.cif
_cod_data_source_block           LH2
_cod_database_code               4333853
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
N1 N 0.4267(5) 0.7572(2) 0.7433(2) 0.0196(8) Uani 1 1 d .
N2 N 0.4863(5) 0.4564(2) 0.6327(2) 0.0192(8) Uani 1 1 d D
H2N H 0.488(7) 0.482(3) 0.5760(16) 0.023 Uiso 1 1 d D
N3 N 0.4802(5) 0.6252(2) 0.5203(2) 0.0185(8) Uani 1 1 d .
C1 C 0.4117(6) 0.7920(3) 0.8274(3) 0.0195(9) Uani 1 1 d .
C2 C 0.4014(6) 0.8860(3) 0.8418(3) 0.0236(10) Uani 1 1 d .
H2 H 0.4031 0.9355 0.7926 0.028 Uiso 1 1 calc R
C3 C 0.3886(7) 0.9055(3) 0.9301(3) 0.0288(11) Uani 1 1 d .
H3 H 0.3811 0.9693 0.9417 0.035 Uiso 1 1 calc R
C4 C 0.3865(7) 0.8329(3) 1.0025(3) 0.0294(11) Uani 1 1 d .
H4 H 0.3778 0.8479 1.0626 0.035 Uiso 1 1 calc R
C5 C 0.3970(6) 0.7392(3) 0.9875(3) 0.0255(10) Uani 1 1 d .
H5 H 0.3965 0.6897 1.0366 0.031 Uiso 1 1 calc R
C6 C 0.4082(6) 0.7192(3) 0.8991(3) 0.0205(9) Uani 1 1 d .
C7 C 0.4220(6) 0.6268(3) 0.8610(3) 0.0189(9) Uani 1 1 d .
C8 C 0.6070(6) 0.5709(3) 0.8905(3) 0.0211(9) Uani 1 1 d .
H8A H 0.7230 0.6045 0.8628 0.032 Uiso 1 1 calc R
H8B H 0.6076 0.5081 0.8711 0.032 Uiso 1 1 calc R
H8C H 0.6085 0.5645 0.9564 0.032 Uiso 1 1 calc R
C9 C 0.2353(6) 0.5705(3) 0.8912(3) 0.0230(9) Uani 1 1 d .
H9A H 0.2166 0.5621 0.9572 0.034 Uiso 1 1 calc R
H9B H 0.2488 0.5085 0.8698 0.034 Uiso 1 1 calc R
H9C H 0.1219 0.6051 0.8656 0.034 Uiso 1 1 calc R
C10 C 0.4332(6) 0.6652(3) 0.7593(3) 0.0164(8) Uani 1 1 d .
C11 C 0.4537(6) 0.6085(3) 0.6842(3) 0.0196(9) Uani 1 1 d .
C12 C 0.4648(6) 0.5121(3) 0.6984(3) 0.0204(9) Uani 1 1 d .
H12 H 0.4567 0.4822 0.7591 0.025 Uiso 1 1 calc R
C13 C 0.4970(6) 0.3582(3) 0.6429(3) 0.0177(9) Uani 1 1 d .
C14 C 0.4931(6) 0.3024(3) 0.7264(3) 0.0220(9) Uani 1 1 d .
H14 H 0.4850 0.3320 0.7798 0.026 Uiso 1 1 calc R
C15 C 0.5008(7) 0.2057(3) 0.7335(3) 0.0261(10) Uani 1 1 d .
H15 H 0.4959 0.1690 0.7913 0.031 Uiso 1 1 calc R
C16 C 0.5157(7) 0.1617(3) 0.6561(3) 0.0263(10) Uani 1 1 d .
H16 H 0.5207 0.0948 0.6607 0.032 Uiso 1 1 calc R
C17 C 0.5231(6) 0.2156(3) 0.5725(3) 0.0233(10) Uani 1 1 d .
H17 H 0.5344 0.1848 0.5199 0.028 Uiso 1 1 calc R
C18 C 0.5145(6) 0.3138(3) 0.5631(3) 0.0180(9) Uani 1 1 d .
C19 C 0.4618(6) 0.6612(3) 0.5951(3) 0.0184(9) Uani 1 1 d .
H19 H 0.4528 0.7281 0.5911 0.022 Uiso 1 1 calc R
N4 N 0.0711(5) 0.2700(2) 0.2347(2) 0.0190(8) Uani 1 1 d .
N5 N 0.0167(5) 0.3595(2) 0.5321(2) 0.0184(8) Uani 1 1 d D
H5N H 0.010(7) 0.4180(17) 0.504(3) 0.022 Uiso 1 1 d D
N6 N 0.0247(5) 0.4879(2) 0.3790(2) 0.0186(8) Uani 1 1 d .
C20 C 0.0855(6) 0.1872(3) 0.1923(3) 0.0183(9) Uani 1 1 d .
C21 C 0.1009(6) 0.1827(3) 0.1008(3) 0.0205(9) Uani 1 1 d .
H21 H 0.1034 0.2386 0.0585 0.025 Uiso 1 1 calc R
C22 C 0.1127(7) 0.0941(3) 0.0720(3) 0.0250(10) Uani 1 1 d .
H22 H 0.1216 0.0892 0.0091 0.030 Uiso 1 1 calc R
C23 C 0.1118(7) 0.0125(3) 0.1340(3) 0.0265(10) Uani 1 1 d .
H23 H 0.1202 -0.0475 0.1131 0.032 Uiso 1 1 calc R
C24 C 0.0985(6) 0.0178(3) 0.2268(3) 0.0229(9) Uani 1 1 d .
H24 H 0.0995 -0.0379 0.2692 0.028 Uiso 1 1 calc R
C25 C 0.0839(6) 0.1054(3) 0.2554(3) 0.0187(9) Uani 1 1 d .
C26 C 0.0664(6) 0.1360(3) 0.3489(3) 0.0187(9) Uani 1 1 d .
C27 C -0.1238(6) 0.0992(3) 0.4004(3) 0.0230(9) Uani 1 1 d .
H27A H -0.2362 0.1272 0.3687 0.034 Uiso 1 1 calc R
H27B H -0.1316 0.1167 0.4616 0.034 Uiso 1 1 calc R
H27C H -0.1249 0.0303 0.4035 0.034 Uiso 1 1 calc R
C28 C 0.2464(6) 0.1002(3) 0.4003(3) 0.0231(9) Uani 1 1 d .
H28A H 0.2580 0.0312 0.4039 0.035 Uiso 1 1 calc R
H28B H 0.2315 0.1181 0.4614 0.035 Uiso 1 1 calc R
H28C H 0.3643 0.1283 0.3682 0.035 Uiso 1 1 calc R
C29 C 0.0601(6) 0.2445(3) 0.3217(3) 0.0169(9) Uani 1 1 d .
C30 C 0.0424(6) 0.3171(3) 0.3825(3) 0.0187(9) Uani 1 1 d .
C31 C 0.0321(6) 0.2949(3) 0.4745(3) 0.0187(9) Uani 1 1 d .
H31 H 0.0362 0.2300 0.4989 0.022 Uiso 1 1 calc R
C32 C 0.0044(6) 0.3427(3) 0.6265(3) 0.0183(9) Uani 1 1 d .
C33 C 0.0164(6) 0.2523(3) 0.6735(3) 0.0222(9) Uani 1 1 d .
H33 H 0.0325 0.1994 0.6412 0.027 Uiso 1 1 calc R
C34 C 0.0052(7) 0.2387(3) 0.7669(3) 0.0230(10) Uani 1 1 d .
H34 H 0.0146 0.1766 0.7984 0.028 Uiso 1 1 calc R
C35 C -0.0196(6) 0.3154(3) 0.8146(3) 0.0234(10) Uani 1 1 d .
H35 H -0.0282 0.3062 0.8788 0.028 Uiso 1 1 calc R
C36 C -0.0319(6) 0.4059(3) 0.7680(3) 0.0216(9) Uani 1 1 d .
H36 H -0.0501 0.4582 0.8010 0.026 Uiso 1 1 calc R
C37 C -0.0182(6) 0.4217(3) 0.6740(3) 0.0177(9) Uani 1 1 d .
C38 C 0.0373(6) 0.4132(3) 0.3383(3) 0.0182(9) Uani 1 1 d .
H38 H 0.0438 0.4224 0.2742 0.022 Uiso 1 1 calc R
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 N1 C1 107.4(3) . ?
C12 N2 C13 127.3(4) . y
C12 N2 H2N 120(3) . ?
C13 N2 H2N 113(3) . ?
C19 N3 C18 119.3(3) 2_666 y
C2 C1 C6 121.3(4) . ?
C2 C1 N1 126.8(4) . ?
C6 C1 N1 111.8(4) . ?
C3 C2 C1 117.9(4) . ?
C3 C2 H2 121.0 . ?
C1 C2 H2 121.0 . ?
C2 C3 C4 121.1(4) . ?
C2 C3 H3 119.5 . ?
C4 C3 H3 119.5 . ?
C5 C4 C3 120.7(4) . ?
C5 C4 H4 119.7 . ?
C3 C4 H4 119.7 . ?
C4 C5 C6 118.5(4) . ?
C4 C5 H5 120.8 . ?
C6 C5 H5 120.8 . ?
C5 C6 C1 120.5(4) . ?
C5 C6 C7 131.3(4) . ?
C1 C6 C7 108.2(4) . ?
C6 C7 C8 110.0(3) . ?
C6 C7 C9 109.7(3) . ?
C8 C7 C9 111.7(3) . ?
C6 C7 C10 99.0(3) . ?
C8 C7 C10 113.3(3) . ?
C9 C7 C10 112.4(3) . ?
C7 C8 H8A 109.5 . ?
C7 C8 H8B 109.5 . ?
H8A C8 H8B 109.5 . ?
C7 C8 H8C 109.5 . ?
H8A C8 H8C 109.5 . ?
H8B C8 H8C 109.5 . ?
C7 C9 H9A 109.5 . ?
C7 C9 H9B 109.5 . ?
H9A C9 H9B 109.5 . ?
C7 C9 H9C 109.5 . ?
H9A C9 H9C 109.5 . ?
H9B C9 H9C 109.5 . ?
N1 C10 C11 120.2(4) . ?
N1 C10 C7 113.6(3) . ?
C11 C10 C7 126.2(3) . ?
C12 C11 C19 122.5(4) . y
C12 C11 C10 121.9(4) . ?
C19 C11 C10 115.6(4) . ?
N2 C12 C11 124.7(4) . y
N2 C12 H12 117.6 . ?
C11 C12 H12 117.6 . ?
C14 C13 N2 123.3(4) . ?
C14 C13 C18 119.1(4) . ?
N2 C13 C18 117.5(4) . y
C15 C14 C13 121.5(4) . ?
C15 C14 H14 119.3 . ?
C13 C14 H14 119.3 . ?
C14 C15 C16 119.8(4) . ?
C14 C15 H15 120.1 . ?
C16 C15 H15 120.1 . ?
C17 C16 C15 119.7(4) . ?
C17 C16 H16 120.2 . ?
C15 C16 H16 120.2 . ?
C16 C17 C18 121.9(4) . ?
C16 C17 H17 119.1 . ?
C18 C17 H17 119.1 . ?
C17 C18 C13 118.0(4) . ?
C17 C18 N3 125.6(4) 2_666 ?
C13 C18 N3 116.4(3) 2_666 y
N3 C19 C11 125.5(4) . y
N3 C19 H19 117.3 . ?
C11 C19 H19 117.3 . ?
C29 N4 C20 107.9(3) . ?
C31 N5 C32 127.3(3) . ?
C31 N5 H5N 113(3) . ?
C32 N5 H5N 120(3) . ?
C38 N6 C37 118.8(3) 2_566 ?
C21 C20 C25 121.6(4) . ?
C21 C20 N4 126.6(4) . ?
C25 C20 N4 111.8(4) . ?
C20 C21 C22 118.1(4) . ?
C20 C21 H21 121.0 . ?
C22 C21 H21 121.0 . ?
C21 C22 C23 120.8(4) . ?
C21 C22 H22 119.6 . ?
C23 C22 H22 119.6 . ?
C22 C23 C24 120.7(4) . ?
C22 C23 H23 119.6 . ?
C24 C23 H23 119.6 . ?
C25 C24 C23 118.5(4) . ?
C25 C24 H24 120.7 . ?
C23 C24 H24 120.7 . ?
C24 C25 C20 120.3(4) . ?
C24 C25 C26 132.0(4) . ?
C20 C25 C26 107.7(3) . ?
C25 C26 C27 109.8(3) . ?
C25 C26 C28 110.0(3) . ?
C27 C26 C28 111.3(4) . ?
C25 C26 C29 99.0(3) . ?
C27 C26 C29 112.7(3) . ?
C28 C26 C29 113.3(3) . ?
C26 C27 H27A 109.5 . ?
C26 C27 H27B 109.5 . ?
H27A C27 H27B 109.5 . ?
C26 C27 H27C 109.5 . ?
H27A C27 H27C 109.5 . ?
H27B C27 H27C 109.5 . ?
C26 C28 H28A 109.5 . ?
C26 C28 H28B 109.5 . ?
H28A C28 H28B 109.5 . ?
C26 C28 H28C 109.5 . ?
H28A C28 H28C 109.5 . ?
H28B C28 H28C 109.5 . ?
N4 C29 C30 119.3(4) . ?
N4 C29 C26 113.6(3) . ?
C30 C29 C26 127.1(4) . ?
C31 C30 C38 122.8(4) . ?
C31 C30 C29 122.1(4) . ?
C38 C30 C29 115.2(4) . ?
N5 C31 C30 123.7(4) . ?
N5 C31 H31 118.1 . ?
C30 C31 H31 118.1 . ?
C33 C32 N5 122.4(4) . ?
C33 C32 C37 120.0(4) . ?
N5 C32 C37 117.7(4) . ?
C34 C33 C32 120.6(4) . ?
C34 C33 H33 119.7 . ?
C32 C33 H33 119.7 . ?
C33 C34 C35 120.1(4) . ?
C33 C34 H34 119.9 . ?
C35 C34 H34 119.9 . ?
C34 C35 C36 119.5(4) . ?
C34 C35 H35 120.2 . ?
C36 C35 H35 120.2 . ?
C35 C36 C37 121.6(4) . ?
C35 C36 H36 119.2 . ?
C37 C36 H36 119.2 . ?
C36 C37 C32 118.2(4) . ?
C36 C37 N6 125.2(4) 2_566 ?
C32 C37 N6 116.6(4) 2_566 ?
N6 C38 C30 125.3(4) . ?
N6 C38 H38 117.4 . ?
C30 C38 H38 117.4 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C10 1.305(5) . y
N1 C1 1.410(5) . ?
N2 C12 1.341(5) . y
N2 C13 1.392(5) . y
N2 H2N 0.876(19) . ?
N3 C19 1.290(5) . y
N3 C18 1.423(5) 2_666 y
C1 C2 1.388(6) . ?
C1 C6 1.391(6) . ?
C2 C3 1.382(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.504(6) . ?
C7 C8 1.535(6) . ?
C7 C9 1.545(6) . ?
C7 C10 1.545(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.467(6) . y
C11 C12 1.366(6) . y
C11 C19 1.441(6) . y
C12 H12 0.9500 . ?
C13 C14 1.389(6) . ?
C13 C18 1.421(6) . ?
C14 C15 1.371(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(6) . ?
C17 H17 0.9500 . ?
C18 N3 1.423(5) 2_666 ?
C19 H19 0.9500 . ?
N4 C29 1.303(5) . ?
N4 C20 1.411(5) . ?
N5 C31 1.342(5) . ?
N5 C32 1.398(5) . ?
N5 H5N 0.884(19) . ?
N6 C38 1.295(5) . ?
N6 C37 1.424(5) 2_566 ?
C20 C21 1.376(6) . ?
C20 C25 1.401(6) . ?
C21 C22 1.389(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.374(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.517(6) . ?
C26 C27 1.537(6) . ?
C26 C28 1.538(6) . ?
C26 C29 1.549(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.465(6) . ?
C30 C31 1.369(6) . ?
C30 C38 1.442(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.388(6) . ?
C32 C37 1.411(6) . ?
C33 C34 1.384(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.388(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(6) . ?
C36 H36 0.9500 . ?
C37 N6 1.425(5) 2_566 ?
C38 H38 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N N3 0.876(19) 2.11(4) 2.751(5) 130(4) .
N2 H2N N3 0.876(19) 2.23(4) 2.697(5) 113(4) 2_666
N5 H5N N6 0.884(19) 2.00(3) 2.737(5) 140(4) .
N5 H5N N6 0.884(19) 2.34(4) 2.698(5) 105(3) 2_566
C8 H8A N4 0.98 2.55 3.489(6) 159.4 2_666
C9 H9C N4 0.98 2.57 3.500(5) 158.7 2_566
C27 H27A N1 0.98 2.58 3.510(6) 157.9 2_566
C28 H28C N1 0.98 2.57 3.499(6) 158.4 2_666
#BEGIN Loops that were not found in dictionaries:
loop_
_shelx_res_file
;
TITL LH2 in P-1
CELL 0.71073   6.8570  14.2898  14.9747  82.332  85.697  87.857
ZERR    2.00   0.0005   0.0008   0.0009   0.003   0.004   0.004
LATT 1
SFAC C  H  n
UNIT 76  68  12
OMIT 2 1 0
OMIT -2 50.1
L.S. 12
ACTA
BOND $H
SIZE 0.18 0.08 0.03
DFIX 0.88 N2 H2N N5 H5N
TEMP -173
WGHT    0.050700    6.796700
FVAR       0.13111
N1    3    0.426706    0.757244    0.743251    11.00000    0.01937    0.02143 =
         0.01913   -0.00551   -0.00270   -0.00167
N2    3    0.486252    0.456449    0.632686    11.00000    0.02596    0.01794 =
         0.01372   -0.00269   -0.00020   -0.00034
H2N   2    0.488392    0.481879    0.576049    11.00000   -1.20000
N3    3    0.480228    0.625190    0.520273    11.00000    0.02019    0.01922 =
         0.01619   -0.00393    0.00053   -0.00048
C1    1    0.411678    0.791972    0.827367    11.00000    0.01200    0.02319 =
         0.02390   -0.00501   -0.00167    0.00093
C2    1    0.401397    0.886030    0.841837    11.00000    0.02286    0.02082 =
         0.02808   -0.00608   -0.00285    0.00052
AFIX  43
H2    2    0.403097    0.935462    0.792630    11.00000   -1.20000
AFIX   0
C3    1    0.388607    0.905514    0.930096    11.00000    0.02523    0.02864 =
         0.03656   -0.01948   -0.00149    0.00009
AFIX  43
H3    2    0.381116    0.969350    0.941712    11.00000   -1.20000
AFIX   0
C4    1    0.386518    0.832896    1.002451    11.00000    0.02795    0.04411 =
         0.01962   -0.01691   -0.00359    0.00303
AFIX  43
H4    2    0.377817    0.847904    1.062569    11.00000   -1.20000
AFIX   0
C5    1    0.397000    0.739209    0.987471    11.00000    0.02189    0.03372 =
         0.02093   -0.00542    0.00004    0.00131
AFIX  43
H5    2    0.396494    0.689747    1.036634    11.00000   -1.20000
AFIX   0
C6    1    0.408247    0.719249    0.899115    11.00000    0.01393    0.02676 =
         0.02163   -0.00720    0.00043    0.00052
C7    1    0.422016    0.626833    0.860976    11.00000    0.01730    0.02317 =
         0.01616   -0.00321   -0.00064    0.00158
C8    1    0.607014    0.570920    0.890491    11.00000    0.02191    0.02416 =
         0.01618    0.00031   -0.00144    0.00388
AFIX 137
H8A   2    0.723040    0.604462    0.862824    11.00000   -1.50000
H8B   2    0.607553    0.508071    0.871076    11.00000   -1.50000
H8C   2    0.608540    0.564537    0.956414    11.00000   -1.50000
AFIX   0
C9    1    0.235259    0.570460    0.891168    11.00000    0.02224    0.02587 =
         0.01934    0.00044    0.00152   -0.00006
AFIX 137
H9A   2    0.216569    0.562074    0.957248    11.00000   -1.50000
H9B   2    0.248787    0.508473    0.869820    11.00000   -1.50000
H9C   2    0.121943    0.605071    0.865592    11.00000   -1.50000
AFIX   0
C10   1    0.433210    0.665200    0.759318    11.00000    0.01323    0.02134 =
         0.01443   -0.00136   -0.00083   -0.00104
C11   1    0.453695    0.608492    0.684240    11.00000    0.01452    0.02515 =
         0.01904   -0.00218   -0.00151   -0.00124
C12   1    0.464788    0.512064    0.698359    11.00000    0.01853    0.02593 =
         0.01722   -0.00581    0.00126    0.00009
AFIX  43
H12   2    0.456714    0.482244    0.759090    11.00000   -1.20000
AFIX   0
C13   1    0.496954    0.358164    0.642864    11.00000    0.01637    0.01735 =
         0.01888    0.00002   -0.00256   -0.00084
C14   1    0.493117    0.302437    0.726365    11.00000    0.02525    0.02503 =
         0.01570   -0.00188   -0.00323   -0.00070
AFIX  43
H14   2    0.484985    0.331997    0.779759    11.00000   -1.20000
AFIX   0
C15   1    0.500799    0.205750    0.733472    11.00000    0.03258    0.02585 =
         0.01842    0.00327   -0.00319   -0.00113
AFIX  43
H15   2    0.495932    0.169004    0.791307    11.00000   -1.20000
AFIX   0
C16   1    0.515679    0.161742    0.656117    11.00000    0.02674    0.01959 =
         0.03123    0.00113   -0.00243   -0.00020
AFIX  43
H16   2    0.520732    0.094757    0.660687    11.00000   -1.20000
AFIX   0
C17   1    0.523107    0.215610    0.572549    11.00000    0.02526    0.02599 =
         0.01956   -0.00800    0.00039    0.00012
AFIX  43
H17   2    0.534450    0.184813    0.519885    11.00000   -1.20000
AFIX   0
C18   1    0.514472    0.313835    0.563072    11.00000    0.01191    0.02509 =
         0.01735   -0.00451    0.00056   -0.00040
C19   1    0.461791    0.661206    0.595070    11.00000    0.01738    0.01760 =
         0.01993   -0.00211   -0.00127    0.00114
AFIX  43
H19   2    0.452788    0.728119    0.591054    11.00000   -1.20000
AFIX   0
N4    3    0.071116    0.269955    0.234665    11.00000    0.01717    0.01842 =
         0.02208   -0.00633    0.00036    0.00102
N5    3    0.016677    0.359455    0.532129    11.00000    0.02533    0.01247 =
         0.01735   -0.00188   -0.00094    0.00047
H5N   2    0.010180    0.417952    0.504385    11.00000   -1.20000
N6    3    0.024690    0.487881    0.379026    11.00000    0.01881    0.01788 =
         0.01921   -0.00319   -0.00016   -0.00043
C20   1    0.085465    0.187238    0.192286    11.00000    0.01481    0.01963 =
         0.02067   -0.00354   -0.00176   -0.00008
C21   1    0.100891    0.182724    0.100770    11.00000    0.01919    0.02420 =
         0.01772   -0.00143   -0.00123   -0.00036
AFIX  43
H21   2    0.103361    0.238602    0.058535    11.00000   -1.20000
AFIX   0
C22   1    0.112737    0.094109    0.071969    11.00000    0.02684    0.03298 =
         0.01692   -0.01081    0.00050   -0.00059
AFIX  43
H22   2    0.121597    0.089185    0.009144    11.00000   -1.20000
AFIX   0
C23   1    0.111782    0.012509    0.134019    11.00000    0.02687    0.02270 =
         0.03216   -0.01457    0.00144    0.00086
AFIX  43
H23   2    0.120244   -0.047523    0.113112    11.00000   -1.20000
AFIX   0
C24   1    0.098505    0.017839    0.226835    11.00000    0.02541    0.01746 =
         0.02595   -0.00496    0.00227   -0.00102
AFIX  43
H24   2    0.099534   -0.037894    0.269219    11.00000   -1.20000
AFIX   0
C25   1    0.083938    0.105449    0.255400    11.00000    0.01631    0.01950 =
         0.02056   -0.00426   -0.00063   -0.00081
C26   1    0.066429    0.135988    0.348942    11.00000    0.01938    0.01830 =
         0.01981   -0.00739   -0.00244    0.00279
C27   1   -0.123820    0.099239    0.400360    11.00000    0.02655    0.01792 =
         0.02382   -0.00243    0.00299   -0.00245
AFIX 137
H27A  2   -0.236238    0.127235    0.368685    11.00000   -1.50000
H27B  2   -0.131598    0.116739    0.461641    11.00000   -1.50000
H27C  2   -0.124911    0.030314    0.403533    11.00000   -1.50000
AFIX   0
C28   1    0.246364    0.100157    0.400254    11.00000    0.02542    0.02277 =
         0.02112   -0.00356   -0.00415    0.00467
AFIX 137
H28A  2    0.258018    0.031216    0.403853    11.00000   -1.50000
H28B  2    0.231463    0.118089    0.461374    11.00000   -1.50000
H28C  2    0.364278    0.128332    0.368233    11.00000   -1.50000
AFIX   0
C29   1    0.060109    0.244472    0.321730    11.00000    0.01449    0.01819 =
         0.01868   -0.00447   -0.00121    0.00009
C30   1    0.042381    0.317142    0.382475    11.00000    0.01664    0.01886 =
         0.02060   -0.00221   -0.00151   -0.00175
C31   1    0.032130    0.294862    0.474477    11.00000    0.02126    0.01525 =
         0.01982   -0.00282   -0.00266   -0.00048
AFIX  43
H31   2    0.036189    0.230002    0.498872    11.00000   -1.20000
AFIX   0
C32   1    0.004445    0.342694    0.626470    11.00000    0.01568    0.01786 =
         0.02090   -0.00231    0.00052   -0.00022
C33   1    0.016439    0.252345    0.673474    11.00000    0.02817    0.01836 =
         0.02125   -0.00641   -0.00191   -0.00132
AFIX  43
H33   2    0.032488    0.199377    0.641171    11.00000   -1.20000
AFIX   0
C34   1    0.005236    0.238712    0.766941    11.00000    0.03082    0.01577 =
         0.02112    0.00414   -0.00230   -0.00475
AFIX  43
H34   2    0.014623    0.176619    0.798437    11.00000   -1.20000
AFIX   0
C35   1   -0.019621    0.315382    0.814609    11.00000    0.02461    0.02980 =
         0.01502   -0.00144    0.00198   -0.00239
AFIX  43
H35   2   -0.028191    0.306152    0.878779    11.00000   -1.20000
AFIX   0
C36   1   -0.031933    0.405858    0.767957    11.00000    0.02137    0.02304 =
         0.02181   -0.00883   -0.00057   -0.00103
AFIX  43
H36   2   -0.050143    0.458233    0.800963    11.00000   -1.20000
AFIX   0
C37   1   -0.018246    0.421698    0.674005    11.00000    0.01411    0.01892 =
         0.02051   -0.00434    0.00039   -0.00138
C38   1    0.037333    0.413209    0.338318    11.00000    0.01722    0.01950 =
         0.01708   -0.00080    0.00011    0.00126
AFIX  43
H38   2    0.043811    0.422440    0.274165    11.00000   -1.20000
HKLF 4
 
REM  HamidRR_0m in P-1
REM R1 =  0.0778 for   3932 Fo > 4sig(Fo)  and  0.0937 for all   4927 data
REM    407 parameters refined using      2 restraints
 
END  
     
WGHT      0.0512      6.7710 
REM Highest difference peak  0.382,  deepest hole -0.331,  1-sigma level  0.079
Q1    1   0.1686  0.3578  0.5240  11.00000  0.05    0.38
Q2    1   0.2870  0.0412  0.2371  11.00000  0.05    0.36
Q3    1   0.6422  0.6001  0.6444  11.00000  0.05    0.33
Q4    1  -0.2571  0.0774  0.5347  11.00000  0.05    0.33
;
#END Loops that were not found in dictionaries
