#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/97/7109744.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_7109744
loop_
_publ_author_name
'Jun Liang'
'Xin-Long Wang'
'Yan-Qing Jiao'
'Chao Qin'
'Kui-Zhan Shao'
'Zhong-Min Su'
'Qing-Yin Wu'
_publ_section_title
;
 Metal ion directed metal-organic rotaxane frameworks with intrinsic
 features of self-penetration and interpenetration
;
_journal_name_full               Chem.Commun.
_journal_page_first              8555
_journal_paper_doi               10.1039/c3cc43990a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C58 H81 N26 O23.5'
_chemical_formula_weight         1518.49
_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                94.549(5)
_cell_angle_beta                 93.303(5)
_cell_angle_gamma                111.017(5)
_cell_formula_units_Z            2
_cell_length_a                   12.485(5)
_cell_length_b                   17.202(5)
_cell_length_c                   17.659(5)
_cell_measurement_reflns_used    18336
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.82
_cell_volume                     3514(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18336
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.9711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1598
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.565
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       0.018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         12219
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.2023
_refine_ls_R_factor_gt           0.1483
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.4000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4220
_refine_ls_wR_factor_ref         0.5006
_reflns_number_gt                6966
_reflns_number_total             12219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43990a.txt
_cod_data_source_block           ww
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C58 H81 N26 O23.50'
_cod_database_code               7109744
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C4 C 0.1618(7) 0.9998(5) 0.3500(4) 0.074(2) Uiso 1 1 d G A 1
C2 C 0.1484(8) 0.9191(5) 0.3556(5) 0.087(4) Uiso 0.80 1 d PG A 1
H2A H 0.1531 0.8854 0.3129 0.104 Uiso 0.80 1 calc PR A 1
C3 C 0.1283(10) 0.8872(6) 0.4231(6) 0.110(5) Uiso 0.80 1 d PG A 1
H3A H 0.1191 0.8316 0.4269 0.131 Uiso 0.80 1 calc PR A 1
C1 C 0.1216(11) 0.9361(7) 0.4850(7) 0.064(4) Uiso 0.50 1 d PGD A 1
C5 C 0.1349(12) 1.0168(7) 0.4793(6) 0.097(6) Uiso 0.50 1 d PG A 1
H5A H 0.1303 1.0505 0.5220 0.116 Uiso 0.50 1 calc PR A 1
C6 C 0.1550(10) 1.0487(6) 0.4118(6) 0.106(5) Uiso 0.70 1 d PG A 1
H6A H 0.1642 1.1043 0.4080 0.127 Uiso 0.70 1 calc PR A 1
C2A C 0.245(3) 0.970(2) 0.374(2) 0.054(9) Uiso 0.20 1 d P A 2
C3A C 0.232(4) 0.927(3) 0.424(3) 0.069(11) Uiso 0.20 1 d P A 2
C1A C 0.1344(19) 0.8888(14) 0.4682(14) 0.084(5) Uiso 0.50 1 d P A 2
C5A C 0.054(2) 0.9222(17) 0.4521(16) 0.109(8) Uiso 0.50 1 d P A 2
C6A C 0.065(3) 0.9749(19) 0.3969(17) 0.069(7) Uiso 0.30 1 d P A 2
C30 C 0.5516(11) 0.9930(8) 0.3527(7) 0.107(4) Uiso 1 1 d GD B 1
C31 C 0.4744(11) 0.9135(7) 0.3339(7) 0.098(7) Uiso 0.50 1 d PG B 1
H31A H 0.4289 0.8996 0.2877 0.118 Uiso 0.50 1 calc PR B 1
C32 C 0.4639(10) 0.8544(7) 0.3828(6) 0.079(5) Uiso 0.50 1 d PG B 1
H32A H 0.4112 0.8002 0.3700 0.095 Uiso 0.50 1 calc PR B 1
C33 C 0.5305(9) 0.8748(6) 0.4505(6) 0.088(3) Uiso 1 1 d G B 1
C34 C 0.6077(13) 0.9543(8) 0.4693(8) 0.206(18) Uiso 0.50 1 d PG B 1
H34A H 0.6532 0.9682 0.5155 0.247 Uiso 0.50 1 calc PR B 1
C35 C 0.6182(14) 1.0134(8) 0.4204(8) 0.22(3) Uiso 0.40 1 d PG B 1
H35A H 0.6709 1.0677 0.4332 0.267 Uiso 0.40 1 calc PR B 1
C31A C 0.6443(15) 0.9773(11) 0.3753(10) 0.066(4) Uiso 0.50 1 d P C 2
C32A C 0.6377(14) 0.9207(10) 0.4236(10) 0.060(4) Uiso 0.50 1 d P C 2
C34A C 0.430(3) 0.885(2) 0.425(2) 0.149(11) Uiso 0.50 1 d P D 2
C35A C 0.462(4) 0.951(3) 0.377(2) 0.189(14) Uiso 0.60 1 d P D 2
C7 C 0.1863(11) 1.0439(7) 0.2842(6) 0.112(5) Uani 1 1 d . . .
H7A H 0.2621 1.0472 0.2712 0.134 Uiso 1 1 calc R A 1
H7B H 0.1908 1.1007 0.2982 0.134 Uiso 1 1 calc R A 1
C8 C 0.1392(8) 1.0611(7) 0.1509(5) 0.076(3) Uani 1 1 d . . .
H8A H 0.2135 1.0616 0.1371 0.092 Uiso 1 1 calc R A .
H8B H 0.1478 1.1184 0.1675 0.092 Uiso 1 1 calc R . .
C9 C 0.0559(13) 1.0307(10) 0.0832(9) 0.116(4) Uiso 1 1 d . A .
C10 C 0.0819(15) 1.0598(11) 0.0144(10) 0.066(4) Uiso 0.50 1 d P . .
C10A C 0.011(2) 0.9695(15) 0.0570(13) 0.092(6) Uiso 0.50 1 d P . .
C11 C 1.3767(6) 1.0378(5) 0.0081(4) 0.0518(18) Uani 1 1 d . . .
C12 C 1.3137(6) 0.8840(5) 0.0159(5) 0.057(2) Uani 1 1 d . . .
H12A H 1.3522 0.8491 -0.0066 0.069 Uiso 1 1 calc R . .
H12B H 1.3468 0.9023 0.0682 0.069 Uiso 1 1 calc R . .
C13 C 1.1391(6) 0.8294(5) 0.0819(4) 0.0471(17) Uani 1 1 d . . .
C14 C 0.9657(6) 0.7324(5) 0.1300(4) 0.0522(18) Uani 1 1 d . . .
H14A H 1.0127 0.7566 0.1777 0.063 Uiso 1 1 calc R . .
H14B H 0.9449 0.6722 0.1269 0.063 Uiso 1 1 calc R . .
C15 C 0.8518(6) 0.8123(4) 0.1785(4) 0.0453(16) Uani 1 1 d . . .
C16 C 0.7063(7) 0.8739(5) 0.2098(4) 0.0531(18) Uani 1 1 d . . .
H16A H 0.6270 0.8456 0.2201 0.064 Uiso 1 1 calc R . .
H16B H 0.7527 0.8928 0.2583 0.064 Uiso 1 1 calc R . .
C17 C 0.8026(6) 1.0222(5) 0.1889(4) 0.0503(18) Uani 1 1 d . . .
C18 C 0.8399(7) 1.1694(5) 0.1668(4) 0.0539(18) Uani 1 1 d . . .
H18A H 0.7841 1.1960 0.1740 0.065 Uiso 1 1 calc R . .
H18B H 0.8877 1.1796 0.2146 0.065 Uiso 1 1 calc R . .
C19 C 0.6647(6) 1.0464(4) 0.1065(4) 0.0468(16) Uani 1 1 d . . .
H19A H 0.6144 1.0746 0.1256 0.056 Uiso 1 1 calc R . .
C20 C 0.6213(6) 0.9531(4) 0.1232(4) 0.0496(17) Uani 1 1 d . . .
H20A H 0.5500 0.9380 0.1486 0.060 Uiso 1 1 calc R . .
C21 C 0.6726(6) 0.7522(5) 0.1063(4) 0.0486(17) Uani 1 1 d . . .
H21A H 0.6033 0.7132 0.1251 0.058 Uiso 1 1 calc R . .
C22 C 0.7557(6) 0.7075(4) 0.0809(4) 0.0465(16) Uani 1 1 d . . .
H22A H 0.7243 0.6477 0.0877 0.056 Uiso 1 1 calc R . .
C23 C 1.0231(6) 0.7172(4) -0.0042(4) 0.0483(17) Uani 1 1 d . . .
H23A H 1.0192 0.6602 0.0021 0.058 Uiso 1 1 calc R . .
C24 C 1.1339(6) 0.7670(5) -0.0416(4) 0.0511(17) Uani 1 1 d . . .
H24A H 1.1794 0.7326 -0.0546 0.061 Uiso 1 1 calc R . .
C25 C 0.9708(6) 0.7581(4) -0.1205(4) 0.0482(17) Uani 1 1 d . . .
C26 C 0.8101(6) 0.6746(4) -0.0517(4) 0.0492(17) Uani 1 1 d . . .
H26A H 0.7679 0.6657 -0.1015 0.059 Uiso 1 1 calc R . .
H26B H 0.7979 0.6201 -0.0346 0.059 Uiso 1 1 calc R . .
C27 C 0.6922(6) 0.7587(4) -0.0235(4) 0.0444(16) Uani 1 1 d . . .
C28 C 0.5589(6) 0.8193(5) 0.0296(5) 0.0541(18) Uani 1 1 d . . .
H28A H 0.4996 0.7947 0.0630 0.065 Uiso 1 1 calc R . .
H28B H 0.5233 0.8051 -0.0224 0.065 Uiso 1 1 calc R . .
C29 C 0.5572(10) 1.0588(9) 0.3015(11) 0.140(6) Uani 1 1 d D . .
C36 C 0.5163(13) 0.8131(6) 0.5109(7) 0.103(4) Uani 1 1 d . . .
H36A H 0.5821 0.8352 0.5489 0.123 Uiso 1 1 calc R B 1
H36B H 0.4480 0.8088 0.5365 0.123 Uiso 1 1 calc R B 1
C37 C 0.4851(8) 0.6713(5) 0.5378(5) 0.067(2) Uani 1 1 d . . .
C38 C 0.501(3) 0.5861(16) 0.4971(16) 0.087(7) Uiso 0.50 1 d P B 1
C39 C 0.4721(14) 0.5230(11) 0.5525(10) 0.063(4) Uiso 0.50 1 d P B 1
C38A C 0.449(3) 0.5789(16) 0.5135(16) 0.097(8) Uiso 0.50 1 d P B 2
C39A C 0.545(3) 0.5704(18) 0.4743(17) 0.109(8) Uiso 0.50 1 d P B 2
C40 C 0.8197(6) 0.7135(4) 0.5061(4) 0.0431(15) Uani 1 1 d . . .
C41 C 0.8422(6) 0.7182(4) 0.3677(4) 0.0531(18) Uani 1 1 d . . .
H41A H 0.8343 0.7722 0.3768 0.064 Uiso 1 1 calc R . .
H41B H 0.9117 0.7268 0.3422 0.064 Uiso 1 1 calc R . .
C42 C 0.6413(6) 0.6749(4) 0.3109(4) 0.0445(16) Uani 1 1 d . . .
C43 C 0.4507(6) 0.6066(4) 0.2383(4) 0.0481(16) Uani 1 1 d . . .
H43A H 0.4436 0.6599 0.2532 0.058 Uiso 1 1 calc R . .
H43B H 0.4332 0.5945 0.1834 0.058 Uiso 1 1 calc R . .
C44 C 0.3042(6) 0.5608(4) 0.3272(4) 0.0431(15) Uani 1 1 d . . .
C45 C 0.1163(7) 0.4901(5) 0.3795(4) 0.0529(18) Uani 1 1 d . . .
H45A H 0.0435 0.4590 0.3497 0.063 Uiso 1 1 calc R . .
H45B H 0.1209 0.5474 0.3902 0.063 Uiso 1 1 calc R . .
C46 C 0.0713(6) 0.3667(4) 0.4591(4) 0.0452(16) Uani 1 1 d . . .
H46A H -0.0071 0.3405 0.4341 0.054 Uiso 1 1 calc R . .
C48 C 0.2039(6) 0.4193(4) 0.2820(4) 0.0441(15) Uani 1 1 d . . .
H48A H 0.1308 0.3962 0.2497 0.053 Uiso 1 1 calc R . .
C49 C 0.3076(5) 0.4564(4) 0.2346(4) 0.0402(15) Uani 1 1 d . . .
H49A H 0.2819 0.4587 0.1816 0.048 Uiso 1 1 calc R . .
C50 C 0.6213(6) 0.5576(4) 0.2258(4) 0.0422(15) Uani 1 1 d . . .
H50A H 0.6240 0.5595 0.1706 0.051 Uiso 1 1 calc R . .
C51 C 0.7435(6) 0.5930(4) 0.2679(4) 0.0442(16) Uani 1 1 d . . .
H51A H 0.8025 0.6096 0.2320 0.053 Uiso 1 1 calc R . .
C52 C 0.9270(5) 0.6383(4) 0.4546(4) 0.0463(16) Uani 1 1 d . . .
H52A H 1.0048 0.6650 0.4390 0.056 Uiso 1 1 calc R . .
C53 C 0.8554(6) 0.4987(5) 0.4795(5) 0.0523(18) Uani 1 1 d . . .
C54 C 0.8554(6) 0.5212(5) 0.3440(4) 0.0510(17) Uani 1 1 d . . .
H54A H 0.8529 0.4641 0.3377 0.061 Uiso 1 1 calc R . .
H54B H 0.9199 0.5552 0.3185 0.061 Uiso 1 1 calc R . .
C55 C 0.6537(6) 0.4525(4) 0.2863(4) 0.0446(16) Uani 1 1 d . . .
C56 C 0.4716(6) 0.4089(4) 0.2030(4) 0.0473(16) Uani 1 1 d . . .
H56A H 0.4630 0.4238 0.1518 0.057 Uiso 1 1 calc R . .
H56B H 0.4815 0.3554 0.1988 0.057 Uiso 1 1 calc R . .
C57 C 0.3195(5) 0.3396(4) 0.2866(4) 0.0394(14) Uani 1 1 d . . .
C58 C 0.1461(6) 0.2932(4) 0.3557(4) 0.0452(16) Uani 1 1 d . . .
H58A H 0.0704 0.2805 0.3295 0.054 Uiso 1 1 calc R . .
H58B H 0.1621 0.2419 0.3528 0.054 Uiso 1 1 calc R . .
C59 C 0.080(3) 0.9000(12) 0.5534(12) 0.264(14) Uiso 1 1 d D . .
N1 N 0.1061(6) 1.0104(5) 0.2152(4) 0.0673(18) Uani 1 1 d . A .
H1A H 0.0353 1.0074 0.2263 0.081 Uiso 1 1 calc R . .
H1B H 0.1022 0.9580 0.2008 0.081 Uiso 1 1 calc R . .
N2 N 0.5062(6) 0.7288(4) 0.4791(4) 0.0617(17) Uani 1 1 d . B .
H2B H 0.4479 0.7091 0.4418 0.074 Uiso 1 1 calc R . .
H2C H 0.5716 0.7317 0.4584 0.074 Uiso 1 1 calc R . .
N3 N 0.7796(5) 1.0806(4) 0.1492(3) 0.0468(14) Uani 1 1 d . . .
N4 N 0.7139(5) 0.9457(4) 0.1706(3) 0.0517(15) Uani 1 1 d . . .
N5 N 0.7448(5) 0.8145(4) 0.1667(3) 0.0518(15) Uani 1 1 d . . .
N6 N 0.8616(5) 0.7513(4) 0.1304(3) 0.0520(15) Uani 1 1 d . . .
N7 N 1.0334(5) 0.7638(4) 0.0673(3) 0.0486(14) Uani 1 1 d . . .
N8 N 1.1939(5) 0.8344(4) 0.0162(3) 0.0508(14) Uani 1 1 d . . .
N9 N 1.3370(5) 0.9575(4) -0.0256(4) 0.0547(16) Uani 1 1 d . . .
N10 N 1.0885(5) 0.7923(4) -0.1088(3) 0.0532(15) Uani 1 1 d . . .
N11 N 0.9309(5) 0.7165(4) -0.0590(3) 0.0463(14) Uani 1 1 d . . .
N12 N 0.7640(5) 0.7204(4) 0.0009(3) 0.0467(14) Uani 1 1 d . . .
N13 N 0.6459(5) 0.7833(4) 0.0379(3) 0.0518(15) Uani 1 1 d . . .
N14 N 0.6024(5) 0.9088(4) 0.0468(4) 0.0550(16) Uani 1 1 d . . .
N15 N 0.1173(5) 0.4541(4) 0.4517(3) 0.0500(15) Uani 1 1 d . . .
N16 N 0.2089(5) 0.4895(3) 0.3345(3) 0.0461(14) Uani 1 1 d . . .
N17 N 0.3668(5) 0.5415(3) 0.2750(3) 0.0434(13) Uani 1 1 d . . .
N18 N 0.5696(5) 0.6137(4) 0.2578(3) 0.0496(14) Uani 1 1 d . . .
N19 N 0.7459(5) 0.6639(4) 0.3179(3) 0.0486(14) Uani 1 1 d . . .
N20 N 0.8558(5) 0.6879(3) 0.4408(3) 0.0462(14) Uani 1 1 d . . .
N21 N 0.8750(5) 0.5501(4) 0.4230(3) 0.0499(15) Uani 1 1 d . . .
N22 N 0.7502(5) 0.5236(3) 0.3072(3) 0.0462(14) Uani 1 1 d . . .
N23 N 0.5759(5) 0.4727(3) 0.2445(3) 0.0441(13) Uani 1 1 d . . .
N24 N 0.3674(4) 0.3999(3) 0.2392(3) 0.0421(13) Uani 1 1 d . . .
N25 N 0.2312(5) 0.3547(3) 0.3171(3) 0.0456(14) Uani 1 1 d . . .
N26 N 0.1444(5) 0.3208(3) 0.4346(3) 0.0462(14) Uani 1 1 d . . .
O1 O 1.3937(5) 1.0582(4) 0.0779(3) 0.0653(15) Uani 1 1 d . . .
O2 O 1.1746(4) 0.8758(3) 0.1416(3) 0.0583(13) Uani 1 1 d . . .
O3 O 0.9268(5) 0.8574(3) 0.2272(3) 0.0596(14) Uani 1 1 d . . .
O4 O 0.8865(5) 1.0363(4) 0.2326(3) 0.0600(14) Uani 1 1 d . . .
O5 O 0.9122(5) 0.7616(3) -0.1764(3) 0.0571(13) Uani 1 1 d . . .
O6 O 0.6709(4) 0.7691(3) -0.0895(3) 0.0558(13) Uani 1 1 d . . .
O7 O 0.7657(4) 0.7604(3) 0.5118(3) 0.0551(13) Uani 1 1 d . . .
O8 O 0.6196(5) 0.7311(3) 0.3452(3) 0.0567(13) Uani 1 1 d . . .
O9 O 0.3241(5) 0.6293(3) 0.3622(3) 0.0566(13) Uani 1 1 d . . .
O10 O 0.3514(4) 0.2813(3) 0.2978(3) 0.0495(12) Uani 1 1 d . . .
O11 O 0.6407(4) 0.3815(3) 0.3041(3) 0.0566(13) Uani 1 1 d . . .
O12 O 0.8204(5) 0.4212(3) 0.4688(3) 0.0641(15) Uani 1 1 d . . .
O13 O 0.4607(6) 1.0656(4) 0.2745(4) 0.254(8) Uani 1 1 d DU B .
H1 H 0.4778 1.1114 0.2409 0.381 Uiso 1 1 d R . .
O14 O 0.6424(6) 1.1034(4) 0.2786(4) 0.127(3) Uani 1 1 d RD B .
O15 O 0.0996(6) 0.9538(4) 0.6103(4) 0.408(15) Uani 1 1 d RDU A .
O16 O 0.0823(6) 0.8343(4) 0.5754(4) 0.167(5) Uani 1 1 d RD A .
H2 H 0.0590 0.8318 0.6283 0.251 Uiso 1 1 d R . .
O1W O 0.4564(5) 0.1912(4) 0.2106(4) 0.0754(17) Uiso 1 1 d . . .
O2W O 0.8939(12) 0.3081(9) 0.6939(8) 0.177(5) Uiso 1 1 d . . .
O3W O 0.3447(9) 0.7269(6) 0.8687(6) 0.135(3) Uiso 1 1 d . . .
O4W O 0.7733(12) 0.2761(8) 0.3421(8) 0.177(5) Uiso 1 1 d . . .
O5W O 0.7673(11) 0.2680(8) 0.5157(8) 0.169(4) Uiso 1 1 d . . .
O6W O 0.3943(14) 0.7939(10) 0.1811(10) 0.207(6) Uiso 1 1 d . . .
O7W O 0.9174(15) 0.3662(11) 0.2331(10) 0.223(7) Uiso 1 1 d . . .
O8W O 0.5000 0.5000 0.0000 0.50(3) Uiso 1 2 d S . .
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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C6 C4 C2 120.0 . .
C6 C4 C7 112.6(8) . .
C2 C4 C7 127.4(8) . .
C3 C2 C4 120.0 . .
C3 C2 H2A 120.0 . .
C4 C2 H2A 120.0 . .
C2 C3 C1 120.0 . .
C2 C3 H3A 120.0 . .
C1 C3 H3A 120.0 . .
C3 C1 C5 120.0 . .
C3 C1 C59 120.6(10) . .
C5 C1 C59 118.5(10) . .
C6 C5 C1 120.0 . .
C6 C5 H5A 120.0 . .
C1 C5 H5A 120.0 . .
C4 C6 C5 120.0 . .
C4 C6 H6A 120.0 . .
C5 C6 H6A 120.0 . .
C2A C3A C1A 133(4) . .
C5A C1A C3A 108(3) . .
C5A C1A C59 75.5(18) . .
C3A C1A C59 143(3) . .
C1A C5A C6A 122(3) . .
C1A C5A C59 60.9(17) . .
C6A C5A C59 153(2) . .
C31 C30 C35 120.0 . .
C31 C30 C29 119.8(11) . .
C35 C30 C29 120.0(11) . .
C32 C31 C30 120.0 . .
C32 C31 H31A 120.0 . .
C30 C31 H31A 120.0 . .
C31 C32 C33 120.0 . .
C31 C32 H32A 120.0 . .
C33 C32 H32A 120.0 . .
C34 C33 C32 120.0 . .
C34 C33 C36 117.3(8) . .
C32 C33 C36 122.5(9) . .
C33 C34 C35 120.0 . .
C33 C34 H34A 120.0 . .
C35 C34 H34A 120.0 . .
C34 C35 C30 120.0 . .
C34 C35 H35A 120.0 . .
C30 C35 H35A 120.0 . .
C4 C7 N1 118.0(8) . .
C4 C7 H7A 107.8 . .
N1 C7 H7A 107.8 . .
C4 C7 H7B 107.8 . .
N1 C7 H7B 107.8 . .
H7A C7 H7B 107.1 . .
N1 C8 C9 113.7(10) . .
N1 C8 H8A 108.8 . .
C9 C8 H8A 108.8 . .
N1 C8 H8B 108.8 . .
C9 C8 H8B 108.8 . .
H8A C8 H8B 107.7 . .
C10A C9 C10 91.5(19) . .
C10A C9 C8 131(2) . .
C10 C9 C8 121.6(14) . .
C9 C10 C10A 121.1(16) . 2_575
C9 C10 C10A 37.1(10) . .
C10A C10 C10A 91.8(15) 2_575 .
C9 C10A C10 128(2) . 2_575
C9 C10A C10 51.4(15) . .
C10 C10A C10 88.2(15) 2_575 .
O1 C11 N9 124.8(7) . .
O1 C11 N14 126.0(8) . 2_775
N9 C11 N14 109.2(7) . 2_775
N8 C12 N9 114.4(6) . .
N8 C12 H12A 108.6 . .
N9 C12 H12A 108.6 . .
N8 C12 H12B 108.6 . .
N9 C12 H12B 108.7 . .
H12A C12 H12B 107.6 . .
O2 C13 N8 126.8(7) . .
O2 C13 N7 126.1(6) . .
N8 C13 N7 107.1(6) . .
N7 C14 N6 113.4(6) . .
N7 C14 H14A 108.9 . .
N6 C14 H14A 108.9 . .
N7 C14 H14B 108.9 . .
N6 C14 H14B 108.9 . .
H14A C14 H14B 107.7 . .
O3 C15 N6 125.3(7) . .
O3 C15 N5 125.2(7) . .
N6 C15 N5 109.5(6) . .
N4 C16 N5 113.2(6) . .
N4 C16 H16A 108.9 . .
N5 C16 H16A 108.9 . .
N4 C16 H16B 108.9 . .
N5 C16 H16B 108.9 . .
H16A C16 H16B 107.7 . .
O4 C17 N4 126.2(8) . .
O4 C17 N3 125.0(7) . .
N4 C17 N3 108.9(6) . .
N10 C18 N3 113.6(6) 2_775 .
N10 C18 H18A 108.8 2_775 .
N3 C18 H18A 108.8 . .
N10 C18 H18B 108.8 2_775 .
N3 C18 H18B 108.8 . .
H18A C18 H18B 107.7 . .
N9 C19 N3 115.9(5) 2_775 .
N9 C19 C20 104.4(6) 2_775 .
N3 C19 C20 102.1(5) . .
N9 C19 H19A 111.3 2_775 .
N3 C19 H19A 111.3 . .
C20 C19 H19A 111.3 . .
N4 C20 N14 114.2(6) . .
N4 C20 C19 105.1(6) . .
N14 C20 C19 102.2(6) . .
N4 C20 H20A 111.6 . .
N14 C20 H20A 111.6 . .
C19 C20 H20A 111.6 . .
N13 C21 N5 116.3(6) . .
N13 C21 C22 102.9(5) . .
N5 C21 C22 101.6(5) . .
N13 C21 H21A 111.7 . .
N5 C21 H21A 111.7 . .
C22 C21 H21A 111.7 . .
N12 C22 N6 114.9(5) . .
N12 C22 C21 103.3(5) . .
N6 C22 C21 103.9(5) . .
N12 C22 H22A 111.4 . .
N6 C22 H22A 111.4 . .
C21 C22 H22A 111.4 . .
N7 C23 N11 115.7(6) . .
N7 C23 C24 104.3(6) . .
N11 C23 C24 102.9(5) . .
N7 C23 H23A 111.1 . .
N11 C23 H23A 111.1 . .
C24 C23 H23A 111.1 . .
N8 C24 N10 114.3(6) . .
N8 C24 C23 102.6(5) . .
N10 C24 C23 103.0(6) . .
N8 C24 H24A 112.0 . .
N10 C24 H24A 112.0 . .
C23 C24 H24A 112.0 . .
O5 C25 N11 125.9(7) . .
O5 C25 N10 126.3(7) . .
N11 C25 N10 107.7(6) . .
N12 C26 N11 113.5(5) . .
N12 C26 H26A 108.9 . .
N11 C26 H26A 108.9 . .
N12 C26 H26B 108.9 . .
N11 C26 H26B 108.9 . .
H26A C26 H26B 107.7 . .
O6 C27 N12 126.1(6) . .
O6 C27 N13 125.0(7) . .
N12 C27 N13 108.9(6) . .
N13 C28 N14 113.5(6) . .
N13 C28 H28A 108.9 . .
N14 C28 H28A 108.9 . .
N13 C28 H28B 108.9 . .
N14 C28 H28B 108.9 . .
H28A C28 H28B 107.7 . .
O14 C29 O13 115.7(10) . .
O14 C29 C30 125.0(10) . .
O13 C29 C30 119.1(9) . .
N2 C36 C33 113.4(9) . .
N2 C36 H36A 108.9 . .
C33 C36 H36A 108.9 . .
N2 C36 H36B 108.9 . .
C33 C36 H36B 108.9 . .
H36A C36 H36B 107.7 . .
N2 C37 C38A 118.6(13) . .
N2 C37 C38 104.9(11) . .
C38A C37 C38 25.1(11) . .
C39 C38 C37 107(2) . .
C37 C38A C39A 105(2) . .
O7 C40 N20 126.2(7) . .
O7 C40 N26 125.2(6) . 2_666
N20 C40 N26 108.6(6) . 2_666
N19 C41 N20 114.6(5) . .
N19 C41 H41A 108.6 . .
N20 C41 H41A 108.6 . .
N19 C41 H41B 108.6 . .
N20 C41 H41B 108.6 . .
H41A C41 H41B 107.6 . .
O8 C42 N18 126.8(7) . .
O8 C42 N19 125.4(7) . .
N18 C42 N19 107.9(6) . .
N17 C43 N18 113.2(5) . .
N17 C43 H43A 108.9 . .
N18 C43 H43A 108.9 . .
N17 C43 H43B 108.9 . .
N18 C43 H43B 108.9 . .
H43A C43 H43B 107.8 . .
O9 C44 N17 126.8(7) . .
O9 C44 N16 124.4(6) . .
N17 C44 N16 108.7(5) . .
N16 C45 N15 114.0(6) . .
N16 C45 H45A 108.8 . .
N15 C45 H45A 108.8 . .
N16 C45 H45B 108.8 . .
N15 C45 H45B 108.8 . .
H45A C45 H45B 107.6 . .
N15 C46 N26 114.6(5) . .
N15 C46 C52 104.4(6) . 2_666
N26 C46 C52 103.6(6) . 2_666
N15 C46 H46A 111.2 . .
N26 C46 H46A 111.2 . .
C52 C46 H46A 111.2 2_666 .
N16 C48 N25 114.5(6) . .
N16 C48 C49 103.8(5) . .
N25 C48 C49 102.5(5) . .
N16 C48 H48A 111.8 . .
N25 C48 H48A 111.8 . .
C49 C48 H48A 111.8 . .
N24 C49 N17 116.2(5) . .
N24 C49 C48 103.6(5) . .
N17 C49 C48 102.3(5) . .
N24 C49 H49A 111.4 . .
N17 C49 H49A 111.4 . .
C48 C49 H49A 111.4 . .
N23 C50 N18 116.6(5) . .
N23 C50 C51 103.5(5) . .
N18 C50 C51 102.2(5) . .
N23 C50 H50A 111.3 . .
N18 C50 H50A 111.3 . .
C51 C50 H50A 111.3 . .
N19 C51 N22 114.2(6) . .
N19 C51 C50 105.1(5) . .
N22 C51 C50 103.5(5) . .
N19 C51 H51A 111.2 . .
N22 C51 H51A 111.2 . .
C50 C51 H51A 111.2 . .
N20 C52 N21 114.7(6) . .
N20 C52 C46 103.5(5) . 2_666
N21 C52 C46 103.0(5) . 2_666
N20 C52 H52A 111.7 . .
N21 C52 H52A 111.7 . .
C46 C52 H52A 111.7 2_666 .
O12 C53 N21 124.6(7) . .
O12 C53 N15 126.2(7) . 2_666
N21 C53 N15 109.2(6) . 2_666
N21 C54 N22 114.2(6) . .
N21 C54 H54A 108.7 . .
N22 C54 H54A 108.7 . .
N21 C54 H54B 108.7 . .
N22 C54 H54B 108.7 . .
H54A C54 H54B 107.6 . .
O11 C55 N23 125.7(6) . .
O11 C55 N22 125.2(7) . .
N23 C55 N22 109.1(6) . .
N24 C56 N23 113.5(5) . .
N24 C56 H56A 108.9 . .
N23 C56 H56A 108.9 . .
N24 C56 H56B 108.9 . .
N23 C56 H56B 108.9 . .
H56A C56 H56B 107.7 . .
O10 C57 N25 126.5(6) . .
O10 C57 N24 125.1(6) . .
N25 C57 N24 108.3(5) . .
N26 C58 N25 113.1(5) . .
N26 C58 H58A 109.0 . .
N25 C58 H58A 109.0 . .
N26 C58 H58B 109.0 . .
N25 C58 H58B 109.0 . .
H58A C58 H58B 107.8 . .
O16 C59 O15 109.0(15) . .
O16 C59 C1 128.0(19) . .
O15 C59 C1 113.2(16) . .
O16 C59 C1A 95.9(15) . .
O15 C59 C1A 139(2) . .
C1 C59 C1A 32.4(10) . .
O16 C59 C5A 127.9(15) . .
O15 C59 C5A 123.1(14) . .
C1 C59 C5A 28.7(10) . .
C1A C59 C5A 43.6(11) . .
C7 N1 C8 113.4(7) . .
C7 N1 H1A 108.9 . .
C8 N1 H1A 108.9 . .
C7 N1 H1B 108.9 . .
C8 N1 H1B 108.9 . .
H1A N1 H1B 107.7 . .
C37 N2 C36 111.2(7) . .
C37 N2 H2B 109.4 . .
C36 N2 H2B 109.4 . .
C37 N2 H2C 109.4 . .
C36 N2 H2C 109.4 . .
H2B N2 H2C 108.0 . .
C17 N3 C18 123.3(6) . .
C17 N3 C19 112.1(6) . .
C18 N3 C19 121.4(6) . .
C17 N4 C20 111.5(6) . .
C17 N4 C16 122.1(6) . .
C20 N4 C16 124.9(6) . .
C15 N5 C16 123.3(6) . .
C15 N5 C21 113.2(6) . .
C16 N5 C21 123.4(6) . .
C15 N6 C14 122.7(6) . .
C15 N6 C22 111.8(6) . .
C14 N6 C22 125.5(6) . .
C13 N7 C23 112.2(6) . .
C13 N7 C14 119.8(6) . .
C23 N7 C14 124.4(6) . .
C13 N8 C12 121.4(6) . .
C13 N8 C24 113.1(6) . .
C12 N8 C24 122.4(6) . .
C11 N9 C19 112.1(6) . 2_775
C11 N9 C12 124.2(7) . .
C19 N9 C12 123.2(7) 2_775 .
C25 N10 C18 122.7(6) . 2_775
C25 N10 C24 113.0(6) . .
C18 N10 C24 122.4(6) 2_775 .
C25 N11 C26 122.5(6) . .
C25 N11 C23 112.9(6) . .
C26 N11 C23 124.5(6) . .
C27 N12 C26 121.8(6) . .
C27 N12 C22 111.5(5) . .
C26 N12 C22 123.6(6) . .
C27 N13 C21 112.7(6) . .
C27 N13 C28 122.0(6) . .
C21 N13 C28 123.8(6) . .
C11 N14 C28 122.8(7) 2_775 .
C11 N14 C20 111.9(6) 2_775 .
C28 N14 C20 125.1(6) . .
C53 N15 C46 112.2(6) 2_666 .
C53 N15 C45 122.8(6) 2_666 .
C46 N15 C45 124.2(6) . .
C44 N16 C48 111.9(5) . .
C44 N16 C45 123.4(6) . .
C48 N16 C45 123.9(6) . .
C44 N17 C43 121.1(6) . .
C44 N17 C49 112.4(5) . .
C43 N17 C49 120.6(5) . .
C42 N18 C50 113.8(6) . .
C42 N18 C43 121.6(6) . .
C50 N18 C43 124.6(6) . .
C42 N19 C41 123.0(6) . .
C42 N19 C51 111.1(6) . .
C41 N19 C51 125.9(6) . .
C40 N20 C41 123.6(6) . .
C40 N20 C52 112.5(6) . .
C41 N20 C52 123.1(6) . .
C53 N21 C54 123.9(6) . .
C53 N21 C52 111.0(6) . .
C54 N21 C52 124.9(6) . .
C55 N22 C54 122.8(6) . .
C55 N22 C51 110.6(6) . .
C54 N22 C51 124.2(6) . .
C55 N23 C50 112.5(6) . .
C55 N23 C56 122.4(6) . .
C50 N23 C56 122.5(6) . .
C57 N24 C49 112.1(5) . .
C57 N24 C56 123.8(6) . .
C49 N24 C56 123.9(5) . .
C57 N25 C58 122.4(6) . .
C57 N25 C48 112.2(5) . .
C58 N25 C48 121.0(6) . .
C40 N26 C58 123.2(6) 2_666 .
C40 N26 C46 111.6(5) 2_666 .
C58 N26 C46 122.4(6) . .
C29 O13 H1 110.1 . .
C59 O16 H2 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C4 C6 1.350(7) .
C4 C2 1.350(7) .
C4 C7 1.425(12) .
C2 C3 1.350(7) .
C2 H2A 0.9300 .
C3 C1 1.350(7) .
C3 H3A 0.9300 .
C1 C5 1.350(7) .
C1 C59 1.44(2) .
C5 C6 1.350(7) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C2A C3A 1.18(5) .
C3A C1A 1.46(5) .
C1A C5A 1.35(3) .
C1A C59 1.71(3) .
C5A C6A 1.36(4) .
C5A C59 1.89(3) .
C30 C31 1.361(8) .
C30 C35 1.361(8) .
C30 C29 1.488(16) .
C31 C32 1.361(8) .
C31 H31A 0.9300 .
C32 C33 1.361(8) .
C32 H32A 0.9300 .
C33 C34 1.361(8) .
C33 C36 1.537(14) .
C34 C35 1.361(8) .
C34 H34A 0.9300 .
C35 H35A 0.9300 .
C31A C32A 1.33(2) .
C34A C35A 1.43(5) .
C7 N1 1.467(11) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 N1 1.474(11) .
C8 C9 1.468(17) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10A 1.05(2) .
C9 C10 1.36(2) .
C10 C10A 1.58(3) 2_575
C10 C10A 1.74(3) .
C10A C10 1.58(3) 2_575
C11 O1 1.240(9) .
C11 N9 1.361(10) .
C11 N14 1.361(10) 2_775
C12 N8 1.433(9) .
C12 N9 1.458(10) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 O2 1.227(9) .
C13 N8 1.373(9) .
C13 N7 1.389(9) .
C14 N7 1.452(8) .
C14 N6 1.448(9) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 O3 1.224(8) .
C15 N6 1.342(9) .
C15 N5 1.355(9) .
C16 N4 1.439(9) .
C16 N5 1.457(9) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 O4 1.204(9) .
C17 N4 1.382(10) .
C17 N3 1.370(10) .
C18 N10 1.439(9) 2_775
C18 N3 1.438(9) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 N9 1.424(9) 2_775
C19 N3 1.474(9) .
C19 C20 1.556(10) .
C19 H19A 0.9800 .
C20 N4 1.437(10) .
C20 N14 1.458(9) .
C20 H20A 0.9800 .
C21 N13 1.428(9) .
C21 N5 1.455(9) .
C21 C22 1.562(10) .
C21 H21A 0.9800 .
C22 N12 1.451(9) .
C22 N6 1.458(9) .
C22 H22A 0.9800 .
C23 N7 1.413(9) .
C23 N11 1.457(9) .
C23 C24 1.558(10) .
C23 H23A 0.9800 .
C24 N8 1.431(10) .
C24 N10 1.449(10) .
C24 H24A 0.9800 .
C25 O5 1.213(9) .
C25 N11 1.369(9) .
C25 N10 1.369(9) .
C26 N12 1.444(9) .
C26 N11 1.438(9) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C27 O6 1.223(8) .
C27 N12 1.358(9) .
C27 N13 1.364(9) .
C28 N13 1.437(9) .
C28 N14 1.436(10) .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C29 O14 1.182(11) .
C29 O13 1.318(12) .
C36 N2 1.472(11) .
C36 H36A 0.9700 .
C36 H36B 0.9700 .
C37 N2 1.459(10) .
C37 C38A 1.51(3) .
C37 C38 1.66(3) .
C38 C39 1.48(3) .
C38A C39A 1.46(4) .
C40 O7 1.225(8) .
C40 N20 1.359(9) .
C40 N26 1.372(9) 2_666
C41 N19 1.426(9) .
C41 N20 1.455(9) .
C41 H41A 0.9700 .
C41 H41B 0.9700 .
C42 O8 1.220(8) .
C42 N18 1.363(9) .
C42 N19 1.385(9) .
C43 N17 1.457(8) .
C43 N18 1.463(9) .
C43 H43A 0.9700 .
C43 H43B 0.9700 .
C44 O9 1.220(8) .
C44 N17 1.337(8) .
C44 N16 1.390(9) .
C45 N16 1.442(8) .
C45 N15 1.462(9) .
C45 H45A 0.9700 .
C45 H45B 0.9700 .
C46 N15 1.424(9) .
C46 N26 1.467(8) .
C46 C52 1.532(10) 2_666
C46 H46A 0.9800 .
C48 N16 1.444(8) .
C48 N25 1.446(9) .
C48 C49 1.549(9) .
C48 H48A 0.9800 .
C49 N24 1.427(8) .
C49 N17 1.483(8) .
C49 H49A 0.9800 .
C50 N23 1.437(8) .
C50 N18 1.439(9) .
C50 C51 1.544(10) .
C50 H50A 0.9800 .
C51 N19 1.438(9) .
C51 N22 1.453(9) .
C51 H51A 0.9800 .
C52 N20 1.459(9) .
C52 N21 1.467(9) .
C52 C46 1.532(10) 2_666
C52 H52A 0.9800 .
C53 O12 1.239(9) .
C53 N21 1.359(10) .
C53 N15 1.361(10) 2_666
C54 N21 1.420(9) .
C54 N22 1.446(9) .
C54 H54A 0.9700 .
C54 H54B 0.9700 .
C55 O11 1.242(8) .
C55 N23 1.346(9) .
C55 N22 1.380(9) .
C56 N24 1.446(8) .
C56 N23 1.475(9) .
C56 H56A 0.9700 .
C56 H56B 0.9700 .
C57 O10 1.228(8) .
C57 N25 1.351(8) .
C57 N24 1.373(8) .
C58 N26 1.438(9) .
C58 N25 1.451(8) .
C58 H58A 0.9700 .
C58 H58B 0.9700 .
C59 O16 1.233(17) .
C59 O15 1.261(18) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
N2 H2B 0.9000 .
N2 H2C 0.9000 .
N9 C19 1.424(9) 2_775
N10 C18 1.439(9) 2_775
N14 C11 1.361(10) 2_775
N15 C53 1.361(10) 2_666
N26 C40 1.372(9) 2_666
O13 H1 0.9930 .
O16 H2 0.9930 .
