#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:01:19 +0100 (vie 25 de mar de 2016) $
#$Revision: 179947 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/42/7024275.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_7024275
loop_
_publ_author_name
'Kennedy, Stuart'
'Teat, Simon J.'
'Dalgarno, Scott J.'
_publ_section_title
;
 Versatile assembly of p-carboxylatocalix[4]arene-O-alkyl ethers.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              384
_journal_page_last               387
_journal_paper_doi               10.1039/b914133b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'C48 H56 O12, 0.5(C12 H12), 4(C5 H5 N), 0.5(C6 H6)'
_chemical_formula_sum            'C77 H85 N4 O12'
_chemical_formula_weight         1258.49
_chemical_name_common            9Py
_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                92.18(3)
_cell_angle_beta                 100.82(3)
_cell_angle_gamma                99.60(3)
_cell_formula_units_Z            2
_cell_length_a                   12.236(2)
_cell_length_b                   13.141(3)
_cell_length_c                   22.319(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3466.7(13)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Nonius X8 Apex 2'
_diffrn_measurement_method       'omega and phi 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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34541
_diffrn_reflns_theta_full        21.46
_diffrn_reflns_theta_max         21.46
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         7628
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0594
_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)+(0.0809P)²+5.4870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                5602
_reflns_number_total             7628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914133b.txt
_cod_data_source_block           9Py
_cod_original_cell_volume        3466.7(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024275
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
O12 O 0.6443(2) 0.11418(18) 0.37261(11) 0.0270(6) Uani 1 1 d . . .
C1 C 0.8216(3) 0.0751(3) 0.30425(16) 0.0227(9) Uani 1 1 d . . .
O3 O 0.9258(2) 0.17088(18) 0.39706(11) 0.0256(6) Uani 1 1 d . . .
C2 C 0.7864(3) 0.0725(3) 0.24152(17) 0.0255(9) Uani 1 1 d . . .
H2 H 0.7431 0.0106 0.2201 0.031 Uiso 1 1 calc R . .
O6 O 0.7620(2) 0.35249(18) 0.37980(11) 0.0292(7) Uani 1 1 d . . .
C3 C 0.8129(3) 0.1580(3) 0.20904(16) 0.0268(9) Uani 1 1 d . . .
O10 O 0.3159(3) -0.2827(2) 0.24212(13) 0.0440(8) Uani 1 1 d . . .
H10O H 0.2881 -0.3435 0.2279 0.053 Uiso 1 1 calc R . .
C4 C 0.8722(3) 0.2499(3) 0.24090(17) 0.0281(10) Uani 1 1 d . . .
H4 H 0.8870 0.3097 0.2191 0.034 Uiso 1 1 calc R . .
O11 O 0.4788(2) -0.3428(2) 0.25137(12) 0.0390(7) Uani 1 1 d . . .
C5 C 0.9101(3) 0.2561(3) 0.30366(16) 0.0229(9) Uani 1 1 d . . .
O9 O 0.4887(2) 0.29209(18) 0.38672(10) 0.0253(6) Uani 1 1 d . . .
C6 C 0.8867(3) 0.1668(3) 0.33425(16) 0.0218(9) Uani 1 1 d . . .
O4 O 0.9976(3) 0.7025(2) 0.23827(14) 0.0506(9) Uani 1 1 d . . .
H4O H 1.0158 0.7597 0.2240 0.061 Uiso 1 1 calc R . .
C7 C 0.7821(4) 0.1558(4) 0.14151(19) 0.0429(12) Uani 1 1 d . . .
O5 O 0.8467(2) 0.7696(2) 0.25058(13) 0.0396(7) Uani 1 1 d . . .
C8 C 1.0299(3) 0.1319(3) 0.41363(17) 0.0313(10) Uani 1 1 d . . .
H8A H 1.0901 0.1731 0.3961 0.038 Uiso 1 1 calc R . .
H8B H 1.0196 0.0589 0.3976 0.038 Uiso 1 1 calc R . .
C9 C 1.0624(3) 0.1400(3) 0.48236(17) 0.0316(10) Uani 1 1 d . . .
H9A H 1.1291 0.1065 0.4947 0.038 Uiso 1 1 calc R . .
H9B H 0.9994 0.1018 0.4991 0.038 Uiso 1 1 calc R . .
C10 C 1.0896(4) 0.2500(3) 0.50978(17) 0.0376(11) Uani 1 1 d . . .
H10A H 1.1568 0.2865 0.4958 0.045 Uiso 1 1 calc R . .
H10B H 1.0255 0.2853 0.4944 0.045 Uiso 1 1 calc R . .
C11 C 1.1124(4) 0.2589(4) 0.5786(2) 0.0556(13) Uani 1 1 d . . .
H11A H 1.0452 0.2257 0.5930 0.083 Uiso 1 1 calc R . .
H11B H 1.1309 0.3321 0.5934 0.083 Uiso 1 1 calc R . .
H11C H 1.1762 0.2246 0.5943 0.083 Uiso 1 1 calc R . .
O7 O 0.5076(3) 0.3406(2) 0.10806(12) 0.0510(9) Uani 1 1 d . . .
H7O H 0.4925 0.3308 0.0698 0.061 Uiso 1 1 calc R . .
C12 C 0.9714(3) 0.3585(3) 0.33673(18) 0.0289(10) Uani 1 1 d . . .
H12A H 1.0424 0.3802 0.3219 0.035 Uiso 1 1 calc R . .
H12B H 0.9913 0.3496 0.3811 0.035 Uiso 1 1 calc R . .
C13 C 0.8990(3) 0.4424(3) 0.32656(16) 0.0259(9) Uani 1 1 d . . .
C14 C 0.9304(3) 0.5282(3) 0.29513(17) 0.0279(10) Uani 1 1 d . . .
H14 H 1.0020 0.5383 0.2834 0.033 Uiso 1 1 calc R . .
O1 O 0.7196(3) 0.0707(2) 0.11527(13) 0.0513(8) Uani 1 1 d . . .
H1O H 0.7059 0.0750 0.0772 0.062 Uiso 1 1 calc R . .
C15 C 0.8589(3) 0.5999(3) 0.28042(16) 0.0271(10) Uani 1 1 d . . .
C16 C 0.7502(3) 0.5801(3) 0.29293(16) 0.0257(9) Uani 1 1 d . . .
H16 H 0.6991 0.6256 0.2798 0.031 Uiso 1 1 calc R . .
O8 O 0.4016(3) 0.1842(3) 0.10187(13) 0.0681(11) Uani 1 1 d . . .
C17 C 0.7152(3) 0.4953(3) 0.32407(16) 0.0225(9) Uani 1 1 d . . .
C18 C 0.7937(3) 0.4318(3) 0.34432(16) 0.0244(9) Uani 1 1 d . . .
C19 C 0.8985(4) 0.6984(3) 0.25458(18) 0.0326(10) Uani 1 1 d . . .
C20 C 0.8242(4) 0.3619(3) 0.44119(17) 0.0340(10) Uani 1 1 d . . .
H20A H 0.9004 0.4028 0.4425 0.041 Uiso 1 1 calc R . .
H20B H 0.8338 0.2921 0.4540 0.041 Uiso 1 1 calc R . .
C21 C 0.7684(4) 0.4129(3) 0.48610(19) 0.0409(11) Uani 1 1 d . . .
H21A H 0.6890 0.3775 0.4815 0.049 Uiso 1 1 calc R . .
H21B H 0.7680 0.4860 0.4769 0.049 Uiso 1 1 calc R . .
C22 C 0.8304(4) 0.4089(4) 0.55247(19) 0.0478(12) Uani 1 1 d . . .
H22A H 0.8417 0.3369 0.5590 0.057 Uiso 1 1 calc R . .
H22B H 0.9061 0.4529 0.5581 0.057 Uiso 1 1 calc R . .
C23 C 0.7716(5) 0.4429(5) 0.5995(2) 0.0734(17) Uani 1 1 d . . .
H23A H 0.7700 0.5170 0.5976 0.110 Uiso 1 1 calc R . .
H23B H 0.8117 0.4300 0.6401 0.110 Uiso 1 1 calc R . .
H23C H 0.6940 0.4042 0.5922 0.110 Uiso 1 1 calc R . .
O2 O 0.8164(3) 0.2293(2) 0.11305(13) 0.0570(9) Uani 1 1 d . . .
C24 C 0.5955(3) 0.4686(3) 0.33406(16) 0.0264(9) Uani 1 1 d . . .
H24A H 0.5542 0.5255 0.3215 0.032 Uiso 1 1 calc R . .
H24B H 0.5962 0.4605 0.3780 0.032 Uiso 1 1 calc R . .
C25 C 0.5355(3) 0.3685(3) 0.29700(16) 0.0222(9) Uani 1 1 d . . .
N2 N 1.0695(3) 0.8818(3) 0.19992(17) 0.0453(10) Uani 1 1 d . . .
C26 C 0.5305(3) 0.3589(3) 0.23459(16) 0.0266(9) Uani 1 1 d . . .
H26 H 0.5619 0.4164 0.2149 0.032 Uiso 1 1 calc R . .
C27 C 0.4803(3) 0.2669(3) 0.19993(17) 0.0298(10) Uani 1 1 d . . .
C28 C 0.4419(3) 0.1817(3) 0.23003(17) 0.0292(10) Uani 1 1 d . . .
H28 H 0.4120 0.1175 0.2071 0.035 Uiso 1 1 calc R . .
C29 C 0.4456(3) 0.1873(3) 0.29233(16) 0.0235(9) Uani 1 1 d . . .
C30 C 0.4893(3) 0.2830(3) 0.32469(16) 0.0220(9) Uani 1 1 d . . .
C31 C 0.4604(4) 0.2589(3) 0.13231(19) 0.0422(12) Uani 1 1 d . . .
C32 C 0.3950(4) 0.3355(3) 0.40000(17) 0.0341(10) Uani 1 1 d . . .
H32A H 0.3232 0.2874 0.3839 0.041 Uiso 1 1 calc R . .
H32B H 0.3920 0.4017 0.3805 0.041 Uiso 1 1 calc R . .
C33 C 0.4112(4) 0.3534(3) 0.46827(18) 0.0342(10) Uani 1 1 d . . .
H33A H 0.3510 0.3895 0.4778 0.041 Uiso 1 1 calc R . .
H33B H 0.4846 0.3996 0.4836 0.041 Uiso 1 1 calc R . .
C34 C 0.4087(4) 0.2556(3) 0.50195(18) 0.0385(11) Uani 1 1 d . . .
H34A H 0.3346 0.2100 0.4876 0.046 Uiso 1 1 calc R . .
H34B H 0.4678 0.2186 0.4919 0.046 Uiso 1 1 calc R . .
C35 C 0.4278(5) 0.2760(5) 0.5706(2) 0.0691(16) Uani 1 1 d . . .
H35A H 0.5019 0.3198 0.5853 0.104 Uiso 1 1 calc R . .
H35B H 0.4254 0.2101 0.5899 0.104 Uiso 1 1 calc R . .
H35C H 0.3686 0.3112 0.5810 0.104 Uiso 1 1 calc R . .
C36 C 0.4043(3) 0.0917(3) 0.32390(17) 0.0264(9) Uani 1 1 d . . .
H36A H 0.4082 0.1118 0.3676 0.032 Uiso 1 1 calc R . .
H36B H 0.3241 0.0649 0.3052 0.032 Uiso 1 1 calc R . .
C37 C 0.4723(3) 0.0065(3) 0.31949(16) 0.0251(9) Uani 1 1 d . . .
C38 C 0.4204(3) -0.0900(3) 0.29144(17) 0.0274(9) Uani 1 1 d . . .
H38 H 0.3406 -0.1042 0.2781 0.033 Uiso 1 1 calc R . .
C39 C 0.4837(3) -0.1669(3) 0.28246(16) 0.0262(10) Uani 1 1 d . . .
C40 C 0.6013(3) -0.1427(3) 0.29695(16) 0.0258(9) Uani 1 1 d . . .
H40 H 0.6446 -0.1923 0.2871 0.031 Uiso 1 1 calc R . .
N4 N 0.2114(9) -0.4673(8) 0.2036(3) 0.0413(17) Uani 0.70 1 d PDU A 1
C41 C 0.6562(3) -0.0473(3) 0.32553(16) 0.0225(9) Uani 1 1 d . . .
C42 C 0.5896(3) 0.0228(3) 0.33999(16) 0.0240(9) Uani 1 1 d . . .
C43 C 0.4275(4) -0.2727(3) 0.25712(17) 0.0305(10) Uani 1 1 d . . .
C44 C 0.6253(3) 0.1226(3) 0.43409(16) 0.0266(9) Uani 1 1 d . . .
H44A H 0.5476 0.0871 0.4348 0.032 Uiso 1 1 calc R . .
H44B H 0.6308 0.1965 0.4468 0.032 Uiso 1 1 calc R . .
C45 C 0.7081(3) 0.0767(3) 0.47980(17) 0.0303(10) Uani 1 1 d . . .
H45A H 0.7863 0.1073 0.4768 0.036 Uiso 1 1 calc R . .
H45B H 0.6975 0.0011 0.4700 0.036 Uiso 1 1 calc R . .
C46 C 0.6912(4) 0.0971(3) 0.54463(17) 0.0355(10) Uani 1 1 d . . .
H46A H 0.6163 0.0590 0.5487 0.043 Uiso 1 1 calc R . .
H46B H 0.6913 0.1718 0.5521 0.043 Uiso 1 1 calc R . .
C47 C 0.7819(4) 0.0649(4) 0.59317(19) 0.0449(12) Uani 1 1 d . . .
H47A H 0.7773 -0.0103 0.5887 0.067 Uiso 1 1 calc R . .
H47B H 0.7700 0.0848 0.6339 0.067 Uiso 1 1 calc R . .
H47C H 0.8567 0.0994 0.5881 0.067 Uiso 1 1 calc R . .
C48 C 0.7840(3) -0.0177(3) 0.33865(17) 0.0245(9) Uani 1 1 d . . .
H48A H 0.8172 -0.0770 0.3263 0.029 Uiso 1 1 calc R . .
H48B H 0.8118 -0.0011 0.3831 0.029 Uiso 1 1 calc R . .
C49 C 0.5939(5) 0.0277(5) -0.0410(3) 0.0801(18) Uani 1 1 d . . .
H49 H 0.5755 -0.0391 -0.0270 0.096 Uiso 1 1 calc R . .
C50 C 0.5508(5) 0.0448(5) -0.0972(3) 0.0678(16) Uani 1 1 d . . .
H50 H 0.4984 -0.0088 -0.1221 0.081 Uiso 1 1 calc R . .
C51 C 0.5791(5) 0.1374(4) -0.1209(2) 0.0603(14) Uani 1 1 d . . .
H51 H 0.5474 0.1473 -0.1620 0.072 Uiso 1 1 calc R . .
C52 C 0.6533(6) 0.2161(5) -0.0853(3) 0.0786(18) Uani 1 1 d . . .
H52 H 0.6772 0.2812 -0.1002 0.094 Uiso 1 1 calc R . .
N3 N 0.4462(4) 0.3198(3) -0.01455(16) 0.0518(11) Uani 1 1 d . . .
C53 C 0.6949(4) 0.1898(5) -0.0186(3) 0.0646(16) Uani 1 1 d . . .
H53 H 0.7444 0.2390 0.0107 0.078 Uiso 1 1 calc R . .
C54 C 0.3703(5) 0.2358(4) -0.0388(2) 0.0562(14) Uani 1 1 d . . .
H54 H 0.3417 0.1878 -0.0122 0.067 Uiso 1 1 calc R . .
C55 C 0.3318(5) 0.2167(4) -0.1021(2) 0.0564(14) Uani 1 1 d . . .
H55 H 0.2786 0.1565 -0.1187 0.068 Uiso 1 1 calc R . .
C56 C 0.3734(5) 0.2880(4) -0.1394(2) 0.0540(13) Uani 1 1 d . . .
H56 H 0.3488 0.2782 -0.1825 0.065 Uiso 1 1 calc R . .
C57 C 0.4504(5) 0.3727(4) -0.1139(2) 0.0569(14) Uani 1 1 d . . .
H57 H 0.4804 0.4223 -0.1392 0.068 Uiso 1 1 calc R . .
N1 N 0.6586(4) 0.0972(4) -0.0054(2) 0.0631(12) Uani 1 1 d . . .
C58 C 0.4843(5) 0.3863(4) -0.0519(2) 0.0545(13) Uani 1 1 d . . .
H58 H 0.5377 0.4462 -0.0349 0.065 Uiso 1 1 calc R . .
C59 C 1.1455(4) 0.8937(4) 0.1641(2) 0.0503(13) Uani 1 1 d . . .
H59 H 1.1727 0.8342 0.1517 0.060 Uiso 1 1 calc R . .
C60 C 1.1862(4) 0.9855(4) 0.1443(2) 0.0590(14) Uani 1 1 d . . .
H60 H 1.2385 0.9899 0.1176 0.071 Uiso 1 1 calc R . .
C61 C 1.1515(5) 1.0694(4) 0.1630(3) 0.0771(19) Uani 1 1 d . . .
H61 H 1.1783 1.1349 0.1494 0.092 Uiso 1 1 calc R . .
C62 C 1.0748(5) 1.0613(4) 0.2032(3) 0.084(2) Uani 1 1 d . . .
H62 H 1.0515 1.1209 0.2185 0.101 Uiso 1 1 calc R . .
C63 C 1.0349(4) 0.9646(4) 0.2194(3) 0.0609(15) Uani 1 1 d . . .
H63 H 0.9811 0.9570 0.2452 0.073 Uiso 1 1 calc R . .
C64 C 0.1053(10) -0.4851(12) 0.1723(4) 0.0335(17) Uani 0.70 1 d PDU A 1
H64 H 0.0679 -0.4279 0.1640 0.040 Uiso 0.70 1 calc PR A 1
C65 C 0.0481(14) -0.5820(11) 0.1516(5) 0.0409(17) Uani 0.70 1 d PDU A 1
H65 H -0.0276 -0.5919 0.1295 0.049 Uiso 0.70 1 calc PR A 1
C66 C 0.1015(6) -0.6644(5) 0.1634(3) 0.0516(17) Uani 0.70 1 d PDU A 1
H66 H 0.0638 -0.7326 0.1493 0.062 Uiso 0.70 1 calc PR A 1
C67 C 0.2117(6) -0.6470(5) 0.1962(3) 0.0678(19) Uani 0.70 1 d PDU A 1
H67 H 0.2505 -0.7030 0.2056 0.081 Uiso 0.70 1 calc PR A 1
C68 C 0.2638(6) -0.5469(5) 0.2150(3) 0.0589(18) Uani 0.70 1 d PDU A 1
H68 H 0.3398 -0.5344 0.2369 0.071 Uiso 0.70 1 calc PR A 1
C71 C 0.1063(13) -0.6569(13) 0.1261(7) 0.049(3) Uani 0.30 1 d PDU B 2
H71 H 0.0665 -0.7202 0.1049 0.058 Uiso 0.30 1 calc PR B 2
C72 C 0.2216(12) -0.6349(10) 0.1355(7) 0.055(3) Uani 0.30 1 d PDU B 2
H72 H 0.2626 -0.6828 0.1210 0.066 Uiso 0.30 1 calc PR B 2
C73 C 0.2778(13) -0.5420(10) 0.1663(6) 0.051(3) Uani 0.30 1 d PDU B 2
H73 H 0.3580 -0.5269 0.1724 0.061 Uiso 0.30 1 calc PR B 2
C74 C 0.0900(6) 0.0159(6) -0.0270(3) 0.0842(19) Uani 1 1 d . . .
H74 H 0.1535 0.0244 -0.0463 0.101 Uiso 1 1 calc R . .
C75 C 0.0551(6) 0.0989(5) -0.0068(3) 0.0721(16) Uani 1 1 d . . .
H75 H 0.0919 0.1670 -0.0112 0.087 Uiso 1 1 calc R . .
C76 C -0.0358(6) 0.0816(5) 0.0204(3) 0.0792(18) Uani 1 1 d . . .
H76 H -0.0628 0.1392 0.0355 0.095 Uiso 1 1 calc R . .
C97 C 0.8300(11) 0.4541(12) 0.0174(6) 0.091(3) Uani 0.50 1 d PDU C 1
H97 H 0.8112 0.3917 -0.0081 0.110 Uiso 0.50 1 calc PR C 1
C98 C 0.9116(11) 0.5229(10) 0.0058(6) 0.101(3) Uani 0.50 1 d PDU C 1
H98 H 0.9473 0.5062 -0.0267 0.122 Uiso 0.50 1 calc PR C 1
C99 C 0.9495(12) 0.6181(11) 0.0374(6) 0.104(3) Uani 0.50 1 d PDU C 1
H99 H 1.0086 0.6678 0.0281 0.125 Uiso 0.50 1 calc PR C 1
C94 C 0.8057(14) 0.5552(15) 0.0939(10) 0.090(3) Uani 0.50 1 d PDU C 1
H94 H 0.7678 0.5676 0.1262 0.108 Uiso 0.50 1 calc PR C 1
C101 C 0.8315(13) 0.5621(15) 0.0979(11) 0.091(3) Uani 0.50 1 d PDU D 2
H101 H 0.8404 0.5670 0.1412 0.110 Uiso 0.50 1 calc PR D 2
C96 C 0.7700(16) 0.4607(18) 0.0606(8) 0.088(3) Uani 0.50 1 d PDU C 1
H96 H 0.7112 0.4083 0.0676 0.106 Uiso 0.50 1 calc PR C 1
C90 C 0.7595(9) 0.4546(10) 0.0016(5) 0.074(3) Uani 0.50 1 d PDU D 2
H90 H 0.7218 0.3896 -0.0183 0.089 Uiso 0.50 1 calc PR D 2
C91 C 0.8000(10) 0.5383(9) -0.0284(6) 0.096(3) Uani 0.50 1 d PDU D 2
H91 H 0.7895 0.5312 -0.0717 0.116 Uiso 0.50 1 calc PR D 2
C92 C 0.8549(11) 0.6316(10) 0.0013(6) 0.103(3) Uani 0.50 1 d PDU D 2
H92 H 0.8818 0.6874 -0.0209 0.123 Uiso 0.50 1 calc PR D 2
C100 C 0.8699(13) 0.6422(15) 0.0647(7) 0.097(3) Uani 0.50 1 d PDU D 2
H100 H 0.9077 0.7064 0.0857 0.117 Uiso 0.50 1 calc PR D 2
N5 N 0.223(2) -0.4714(19) 0.1881(9) 0.044(3) Uani 0.30 1 d PDU B 2
C69 C 0.106(2) -0.495(3) 0.1782(12) 0.038(3) Uani 0.30 1 d PDU B 2
H69 H 0.0656 -0.4476 0.1929 0.045 Uiso 0.30 1 calc PR B 2
C70 C 0.048(3) -0.587(2) 0.1475(11) 0.042(3) Uani 0.30 1 d PDU B 2
H70 H -0.0321 -0.6024 0.1412 0.050 Uiso 0.30 1 calc PR B 2
C93 C 0.8916(12) 0.6346(15) 0.0852(6) 0.091(3) Uani 0.50 1 d PDU C 1
H93 H 0.9104 0.6973 0.1105 0.110 Uiso 0.50 1 calc PR C 1
C95 C 0.7798(14) 0.4761(19) 0.0619(8) 0.089(3) Uani 0.50 1 d PDU D 2
H95 H 0.7525 0.4200 0.0839 0.106 Uiso 0.50 1 calc PR D 2
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'
O O 0.0106 0.0060 '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
C42 O12 C44 113.9(3) .
C2 C1 C6 117.8(3) .
C2 C1 C48 119.9(3) .
C6 C1 C48 122.1(3) .
C6 O3 C8 113.1(3) .
C1 C2 C3 121.6(3) .
C18 O6 C20 115.2(3) .
C2 C3 C4 118.9(3) .
C2 C3 C7 122.9(4) .
C4 C3 C7 118.2(4) .
C5 C4 C3 121.5(3) .
C4 C5 C6 117.7(3) .
C4 C5 C12 119.8(3) .
C6 C5 C12 122.5(3) .
C30 O9 C32 113.0(3) .
O3 C6 C5 118.6(3) .
O3 C6 C1 119.1(3) .
C5 C6 C1 122.2(3) .
O2 C7 O1 123.3(4) .
O2 C7 C3 121.8(4) .
O1 C7 C3 114.8(4) .
O3 C8 C9 107.8(3) .
C8 C9 C10 113.2(3) .
C11 C10 C9 113.7(3) .
C5 C12 C13 111.5(3) .
C14 C13 C18 117.4(3) .
C14 C13 C12 121.2(3) .
C18 C13 C12 121.1(3) .
C13 C14 C15 121.3(4) .
C16 C15 C14 119.2(3) .
C16 C15 C19 119.6(4) .
C14 C15 C19 121.1(4) .
C17 C16 C15 121.2(3) .
C16 C17 C18 117.8(3) .
C16 C17 C24 121.9(3) .
C18 C17 C24 120.3(3) .
O6 C18 C17 117.8(3) .
O6 C18 C13 119.8(3) .
C17 C18 C13 122.2(3) .
O5 C19 O4 123.3(4) .
O5 C19 C15 123.2(4) .
O4 C19 C15 113.5(4) .
O6 C20 C21 113.5(3) .
C20 C21 C22 111.5(4) .
C23 C22 C21 114.7(4) .
C17 C24 C25 110.1(3) .
C26 C25 C30 118.0(3) .
C26 C25 C24 120.2(3) .
C30 C25 C24 121.7(3) .
C63 N2 C59 118.6(4) .
C25 C26 C27 121.5(3) .
C28 C27 C26 118.4(3) .
C28 C27 C31 119.1(3) .
C26 C27 C31 122.4(3) .
C29 C28 C27 122.1(3) .
C28 C29 C30 117.5(3) .
C28 C29 C36 120.6(3) .
C30 C29 C36 121.9(3) .
O9 C30 C25 119.1(3) .
O9 C30 C29 118.7(3) .
C25 C30 C29 122.2(3) .
O8 C31 O7 123.0(4) .
O8 C31 C27 122.2(4) .
O7 C31 C27 114.7(4) .
O9 C32 C33 108.0(3) .
C32 C33 C34 114.1(3) .
C35 C34 C33 113.1(4) .
C37 C36 C29 113.0(3) .
C38 C37 C42 117.3(3) .
C38 C37 C36 120.5(3) .
C42 C37 C36 122.0(3) .
C37 C38 C39 121.2(4) .
C40 C39 C38 119.1(3) .
C40 C39 C43 119.8(4) .
C38 C39 C43 121.1(4) .
C41 C40 C39 121.1(3) .
C68 N4 C64 118.7(10) .
C40 C41 C42 117.7(3) .
C40 C41 C48 121.7(3) .
C42 C41 C48 120.5(3) .
O12 C42 C41 117.5(3) .
O12 C42 C37 119.8(3) .
C41 C42 C37 122.6(3) .
O11 C43 O10 123.8(4) .
O11 C43 C39 123.2(4) .
O10 C43 C39 113.0(4) .
O12 C44 C45 113.5(3) .
C44 C45 C46 111.0(3) .
C45 C46 C47 113.2(3) .
C41 C48 C1 110.8(3) .
N1 C49 C50 121.6(7) .
C49 C50 C51 121.8(6) .
C50 C51 C52 119.9(5) .
C51 C52 C53 114.2(5) .
C58 N3 C54 118.4(4) .
N1 C53 C52 116.1(5) .
N3 C54 C55 121.9(4) .
C56 C55 C54 117.9(5) .
C57 C56 C55 119.3(4) .
C56 C57 C58 119.8(5) .
C49 N1 C53 126.1(5) .
N3 C58 C57 122.8(5) .
N2 C59 C60 123.7(5) .
C61 C60 C59 118.5(5) .
C60 C61 C62 119.8(5) .
C63 C62 C61 117.8(5) .
N2 C63 C62 121.6(5) .
N4 C64 C65 122.7(12) .
C66 C65 C64 118.9(14) .
C65 C66 C67 119.0(9) .
C68 C67 C66 118.6(6) .
N4 C68 C67 122.1(8) .
C72 C71 C70 120(2) .
C71 C72 C73 119.1(15) .
N5 C73 C72 122.5(18) .
C75 C74 C76 120.9(6) 2
C74 C75 C76 116.7(6) .
C75 C76 C74 122.4(6) 2
C98 C97 C96 127.8(18) .
C97 C98 C99 124.3(15) .
C98 C99 C93 113.3(15) .
C96 C94 C93 127(2) .
C95 C101 C100 112(2) .
C97 C96 C94 110(2) .
C95 C90 C91 111.7(15) .
C92 C91 C90 123.2(12) .
C91 C92 C100 118.4(15) .
C101 C100 C92 122(2) .
C73 N5 C69 117(3) .
N5 C69 C70 121(3) .
C71 C70 C69 120(3) .
C94 C93 C99 117.6(19) .
C90 C95 C101 132(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O12 C42 1.379(4) .
O12 C44 1.437(4) .
C1 C2 1.383(5) .
C1 C6 1.398(5) .
C1 C48 1.519(5) .
O3 C6 1.389(4) .
O3 C8 1.441(4) .
C2 C3 1.386(5) .
O6 C18 1.381(4) .
O6 C20 1.427(4) .
C3 C4 1.393(5) .
C3 C7 1.481(6) .
O10 C43 1.327(5) .
C4 C5 1.385(5) .
O11 C43 1.212(5) .
C5 C6 1.396(5) .
C5 C12 1.515(5) .
O9 C30 1.387(4) .
O9 C32 1.435(4) .
O4 C19 1.324(5) .
C7 O2 1.234(5) .
C7 O1 1.295(5) .
O5 C19 1.211(5) .
C8 C9 1.506(5) .
C9 C10 1.507(5) .
C10 C11 1.505(6) .
O7 C31 1.317(5) .
C12 C13 1.524(5) .
C13 C14 1.388(5) .
C13 C18 1.405(5) .
C14 C15 1.397(5) .
C15 C16 1.395(5) .
C15 C19 1.483(5) .
C16 C17 1.385(5) .
O8 C31 1.214(5) .
C17 C18 1.398(5) .
C17 C24 1.508(5) .
C20 C21 1.510(6) .
C21 C22 1.539(6) .
C22 C23 1.475(7) .
C24 C25 1.524(5) .
C25 C26 1.383(5) .
C25 C30 1.392(5) .
N2 C63 1.318(6) .
N2 C59 1.330(6) .
C26 C27 1.393(5) .
C27 C28 1.388(5) .
C27 C31 1.480(6) .
C28 C29 1.381(5) .
C29 C30 1.397(5) .
C29 C36 1.522(5) .
C32 C33 1.503(5) .
C33 C34 1.512(5) .
C34 C35 1.512(6) .
C36 C37 1.513(5) .
C37 C38 1.388(5) .
C37 C42 1.400(5) .
C38 C39 1.402(5) .
C39 C40 1.393(5) .
C39 C43 1.483(5) .
C40 C41 1.388(5) .
N4 C68 1.323(10) .
N4 C64 1.332(10) .
C41 C42 1.394(5) .
C41 C48 1.516(5) .
C44 C45 1.514(5) .
C45 C46 1.520(5) .
C46 C47 1.524(6) .
C49 N1 1.249(7) .
C49 C50 1.309(8) .
C50 C51 1.362(7) .
C51 C52 1.371(8) .
C52 C53 1.552(8) .
N3 C58 1.321(6) .
N3 C54 1.341(6) .
C53 N1 1.289(7) .
C54 C55 1.402(6) .
C55 C56 1.375(7) .
C56 C57 1.361(7) .
C57 C58 1.362(6) .
C59 C60 1.349(6) .
C60 C61 1.327(8) .
C61 C62 1.409(8) .
C62 C63 1.370(7) .
C64 C65 1.364(10) .
C65 C66 1.364(11) .
C66 C67 1.386(9) .
C67 C68 1.374(8) .
C71 C72 1.366(16) .
C71 C70 1.373(19) .
C72 C73 1.384(15) .
C73 N5 1.360(18) .
C74 C75 1.329(9) .
C74 C76 1.367(8) 2
C75 C76 1.355(8) .
C76 C74 1.367(8) 2
C97 C98 1.303(14) .
C97 C96 1.324(17) .
C98 C99 1.378(14) .
C99 C93 1.416(15) .
C94 C96 1.383(16) .
C94 C93 1.399(17) .
C101 C95 1.351(16) .
C101 C100 1.379(16) .
C90 C95 1.333(16) .
C90 C91 1.380(13) .
C91 C92 1.374(13) .
C92 C100 1.391(15) .
N5 C69 1.377(19) .
C69 C70 1.38(2) .
