#------------------------------------------------------------------------------
#$Date: 2019-11-28 21:15:00 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244640 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/92/7239298.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_7239298
loop_
_publ_author_name
'Pan, Mingguang'
'Xue, Min'
_publ_section_title
;
 Pillar[5]arene derivatives with three different kinds of repeating units:
 first examples, crystal structures and selective preparation
;
_journal_issue                   1
_journal_name_full               'RSC Adv.'
_journal_page_first              260
_journal_paper_doi               10.1039/C3RA44581J
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety
'2(C51 H54 O18), 3.25(C H2 Cl2), C2 H3 N, 0.74(C Cl), 0.75(Cl),'
_chemical_formula_sum            'C108 H119 Cl8 N O36'
_chemical_formula_weight         2290.17
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                91.89(3)
_cell_angle_beta                 95.89(3)
_cell_angle_gamma                101.88(3)
_cell_formula_units_Z            1
_cell_length_a                   12.101(2)
_cell_length_b                   15.262(3)
_cell_length_c                   15.448(3)
_cell_measurement_reflns_used    21810
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.00
_cell_volume                     2772.9(10)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21810
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.236
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.752
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         9730
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.761
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.1214
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3832
_refine_ls_wR_factor_ref         0.4225
_reflns_number_gt                7110
_reflns_number_total             9730
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3ra44581j.txt
_cod_data_source_block           1
_cod_database_code               7239298
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
C53A C 0.3560(13) 0.5553(9) 0.2825(8) 0.074(3) Uani 0.625(6) 1 d PDU A 1
H53A H 0.2758 0.5569 0.2776 0.089 Uiso 0.625(6) 1 calc PR A 1
H53B H 0.3854 0.5640 0.3437 0.089 Uiso 0.625(6) 1 calc PR A 1
Cl1A Cl 0.4284(3) 0.6414(2) 0.22435(19) 0.0696(9) Uani 0.625(6) 1 d PD A 1
Cl2A Cl 0.3731(5) 0.4476(3) 0.2404(3) 0.0787(13) Uani 0.625(6) 1 d P A 1
C53B C 0.4358(17) 0.5613(15) 0.2812(12) 0.074(3) Uani 0.37 1 d PDU A 2
H53C H 0.5100 0.5979 0.2753 0.089 Uiso 0.375(6) 1 calc PR A 2
H53D H 0.4261 0.5616 0.3428 0.089 Uiso 0.375(6) 1 calc PR A 2
Cl1B Cl 0.3309(5) 0.6114(4) 0.2262(3) 0.0696(9) Uani 0.37 1 d PD A 2
Cl2B Cl 0.4336(8) 0.4543(6) 0.2453(6) 0.083(2) Uani 0.375(6) 1 d P A 2
Cl3 Cl 0.9234(2) 0.19715(13) 0.19838(14) 0.0754(7) Uani 1 1 d . . .
Cl4 Cl 0.9361(2) 0.12734(16) 0.37090(14) 0.0894(8) Uani 1 1 d . . .
O1 O 0.2429(5) -0.0647(3) 0.1011(5) 0.100(3) Uani 1 1 d . . .
O2 O 0.3523(5) 0.0995(4) 0.1515(4) 0.0808(17) Uani 1 1 d . . .
O3 O 0.2177(5) 0.1251(4) 0.2395(5) 0.097(2) Uani 1 1 d . . .
O4 O 0.0914(4) -0.4321(2) 0.0817(2) 0.0385(9) Uani 1 1 d . . .
O5 O 0.0360(4) -0.6058(3) 0.1120(2) 0.0434(10) Uani 1 1 d . . .
O6 O 0.1612(4) -0.6381(2) 0.0246(3) 0.0424(10) Uani 1 1 d . . .
O7 O 0.6499(3) -0.0838(2) 0.5136(2) 0.0358(9) Uani 1 1 d . . .
O8 O 0.5874(5) 0.0262(3) 0.6270(3) 0.0614(14) Uani 1 1 d . . .
O9 O 0.6922(3) 0.1452(2) 0.5736(2) 0.0391(10) Uani 1 1 d . . .
O10 O 0.7343(3) -0.3358(2) 0.2768(2) 0.0297(8) Uani 1 1 d . . .
O11 O 0.7150(4) -0.4710(2) 0.1518(2) 0.0406(9) Uani 1 1 d . . .
O12 O 0.7522(4) -0.5632(2) 0.2581(2) 0.0401(10) Uani 1 1 d . . .
O13 O 0.6758(3) -0.0069(2) 0.2043(2) 0.0338(8) Uani 1 1 d . . .
O14 O 0.4641(4) -0.3084(2) -0.0046(2) 0.0398(9) Uani 1 1 d . . .
O15 O 0.3161(3) -0.5073(2) 0.4879(2) 0.0390(9) Uani 1 1 d . . .
H15A H 0.2529 -0.5149 0.4604 0.058 Uiso 1 1 calc R . .
O16 O 0.4633(3) -0.1565(2) 0.6179(2) 0.0380(9) Uani 1 1 d . . .
H16A H 0.5157 -0.1298 0.5928 0.057 Uiso 1 1 calc R . .
O17 O 0.1073(3) -0.5370(2) 0.3955(2) 0.0414(10) Uani 1 1 d . . .
O18 O 0.0014(3) -0.2097(3) 0.3213(2) 0.0430(10) Uani 1 1 d . . .
C1 C 0.2020(5) -0.1576(4) 0.0961(5) 0.0567(18) Uani 1 1 d . . .
C2 C 0.1130(5) -0.1996(4) 0.1386(5) 0.0585(19) Uani 1 1 d . . .
H2A H 0.0784 -0.1648 0.1733 0.070 Uiso 1 1 calc R . .
C3 C 0.0742(4) -0.2887(4) 0.1321(4) 0.0369(12) Uani 1 1 d . . .
C4 C 0.1310(4) -0.3410(3) 0.0834(3) 0.0312(11) Uani 1 1 d . . .
C5 C 0.2180(5) -0.3004(3) 0.0362(3) 0.0331(12) Uani 1 1 d . . .
H5A H 0.2518 -0.3358 0.0014 0.040 Uiso 1 1 calc R . .
C6 C 0.2552(5) -0.2075(4) 0.0406(3) 0.0354(12) Uani 1 1 d . . .
C7 C 0.3537(5) -0.1645(4) -0.0063(3) 0.0364(12) Uani 1 1 d . . .
H7A H 0.3466 -0.1041 -0.0196 0.044 Uiso 1 1 calc R . .
H7B H 0.3518 -0.1983 -0.0609 0.044 Uiso 1 1 calc R . .
C8 C 0.4668(4) -0.1610(3) 0.0481(3) 0.0314(11) Uani 1 1 d . . .
C9 C 0.5172(5) -0.2360(3) 0.0505(3) 0.0312(11) Uani 1 1 d . . .
C10 C 0.6172(4) -0.2336(3) 0.1067(3) 0.0284(11) Uani 1 1 d . . .
H10A H 0.6506 -0.2833 0.1084 0.034 Uiso 1 1 calc R . .
C11 C 0.6660(4) -0.1573(3) 0.1595(3) 0.0271(11) Uani 1 1 d . . .
C12 C 0.6173(4) -0.0829(3) 0.1545(3) 0.0272(11) Uani 1 1 d . . .
C13 C 0.5186(4) -0.0843(3) 0.0995(3) 0.0278(11) Uani 1 1 d . . .
H13A H 0.4871 -0.0337 0.0970 0.033 Uiso 1 1 calc R . .
C14 C 0.7675(4) -0.1585(3) 0.2254(3) 0.0257(10) Uani 1 1 d . . .
H14A H 0.8175 -0.0996 0.2311 0.031 Uiso 1 1 calc R . .
H14B H 0.8097 -0.2011 0.2047 0.031 Uiso 1 1 calc R . .
C15 C 0.7306(4) -0.1843(3) 0.3142(3) 0.0256(10) Uani 1 1 d . . .
C16 C 0.7194(4) -0.2730(3) 0.3396(3) 0.0263(10) Uani 1 1 d . . .
C17 C 0.6936(4) -0.2944(3) 0.4222(3) 0.0290(11) Uani 1 1 d . . .
H17A H 0.6912 -0.3527 0.4390 0.035 Uiso 1 1 calc R . .
C18 C 0.6709(4) -0.2307(3) 0.4814(3) 0.0276(11) Uani 1 1 d . . .
C19 C 0.6788(4) -0.1442(3) 0.4540(3) 0.0286(11) Uani 1 1 d . . .
C20 C 0.7106(4) -0.1211(3) 0.3735(3) 0.0266(10) Uani 1 1 d . . .
H20A H 0.7189 -0.0617 0.3587 0.032 Uiso 1 1 calc R . .
C21 C 0.6358(4) -0.2583(3) 0.5694(3) 0.0285(11) Uani 1 1 d . . .
H21A H 0.6569 -0.2069 0.6108 0.034 Uiso 1 1 calc R . .
H21B H 0.6758 -0.3038 0.5903 0.034 Uiso 1 1 calc R . .
C22 C 0.5081(5) -0.2950(3) 0.5638(3) 0.0302(11) Uani 1 1 d . . .
C23 C 0.4645(5) -0.3830(3) 0.5322(3) 0.0315(11) Uani 1 1 d . . .
H23A H 0.5143 -0.4187 0.5179 0.038 Uiso 1 1 calc R . .
C24 C 0.3491(5) -0.4187(3) 0.5216(3) 0.0319(11) Uani 1 1 d . . .
C25 C 0.2719(5) -0.3687(3) 0.5458(3) 0.0321(12) Uani 1 1 d . . .
C26 C 0.3161(5) -0.2810(3) 0.5771(3) 0.0317(11) Uani 1 1 d . . .
H26A H 0.2663 -0.2461 0.5935 0.038 Uiso 1 1 calc R . .
C27 C 0.4319(5) -0.2428(3) 0.5852(3) 0.0310(11) Uani 1 1 d . . .
C28 C 0.1460(5) -0.4055(4) 0.5346(3) 0.0382(13) Uani 1 1 d . . .
H28A H 0.1108 -0.3759 0.5774 0.046 Uiso 1 1 calc R . .
H28B H 0.1312 -0.4691 0.5445 0.046 Uiso 1 1 calc R . .
C29 C 0.0933(4) -0.3913(4) 0.4426(4) 0.0349(12) Uani 1 1 d . . .
C30 C 0.0638(5) -0.3106(4) 0.4255(4) 0.0391(13) Uani 1 1 d . . .
H30A H 0.0695 -0.2683 0.4713 0.047 Uiso 1 1 calc R . .
C31 C 0.0257(5) -0.2904(4) 0.3418(4) 0.0403(14) Uani 1 1 d . . .
C32 C 0.0146(4) -0.3554(4) 0.2731(3) 0.0351(12) Uani 1 1 d . . .
C33 C 0.0406(5) -0.4369(4) 0.2911(4) 0.0383(13) Uani 1 1 d . . .
H33A H 0.0323 -0.4805 0.2461 0.046 Uiso 1 1 calc R . .
C34 C 0.0790(5) -0.4558(4) 0.3747(3) 0.0357(12) Uani 1 1 d . . .
C35 C -0.0226(5) -0.3349(4) 0.1806(4) 0.0403(13) Uani 1 1 d . . .
H35A H -0.0777 -0.2970 0.1822 0.048 Uiso 1 1 calc R . .
H35B H -0.0601 -0.3906 0.1486 0.048 Uiso 1 1 calc R . .
C36 C 0.2075(8) -0.0223(6) 0.1852(6) 0.078(2) Uani 1 1 d . . .
H36A H 0.2265 -0.0552 0.2353 0.093 Uiso 1 1 calc R . .
H36B H 0.1261 -0.0260 0.1787 0.093 Uiso 1 1 calc R . .
C37 C 0.2716(10) 0.0787(6) 0.1998(7) 0.100(4) Uani 1 1 d . . .
C38 C 0.3955(8) 0.1901(4) 0.1608(4) 0.066(2) Uani 1 1 d . . .
H38A H 0.4594 0.2050 0.1281 0.100 Uiso 1 1 calc R . .
H38B H 0.4192 0.2073 0.2213 0.100 Uiso 1 1 calc R . .
H38C H 0.3380 0.2215 0.1396 0.100 Uiso 1 1 calc R . .
C39 C 0.1539(5) -0.4878(4) 0.0401(4) 0.0378(13) Uani 1 1 d . . .
H39A H 0.2342 -0.4699 0.0605 0.045 Uiso 1 1 calc R . .
H39B H 0.1441 -0.4832 -0.0226 0.045 Uiso 1 1 calc R . .
C40 C 0.1074(5) -0.5828(4) 0.0636(3) 0.0357(12) Uani 1 1 d . . .
C41 C 0.1286(7) -0.7327(4) 0.0431(5) 0.0578(18) Uani 1 1 d . . .
H41A H 0.1755 -0.7662 0.0154 0.087 Uiso 1 1 calc R . .
H41B H 0.0504 -0.7554 0.0212 0.087 Uiso 1 1 calc R . .
H41C H 0.1384 -0.7387 0.1049 0.087 Uiso 1 1 calc R . .
C42 C 0.6767(5) 0.0078(3) 0.4974(3) 0.0307(11) Uani 1 1 d . . .
H42A H 0.6336 0.0192 0.4440 0.037 Uiso 1 1 calc R . .
H42B H 0.7570 0.0265 0.4913 0.037 Uiso 1 1 calc R . .
C43 C 0.6465(5) 0.0585(3) 0.5740(3) 0.0311(11) Uani 1 1 d . . .
C44 C 0.6593(6) 0.2033(4) 0.6392(4) 0.0451(15) Uani 1 1 d . . .
H44A H 0.6958 0.2644 0.6328 0.068 Uiso 1 1 calc R . .
H44B H 0.6821 0.1859 0.6964 0.068 Uiso 1 1 calc R . .
H44C H 0.5783 0.1976 0.6316 0.068 Uiso 1 1 calc R . .
C45 C 0.7305(5) -0.4237(3) 0.3050(3) 0.0346(12) Uani 1 1 d . . .
H45A H 0.6620 -0.4441 0.3326 0.042 Uiso 1 1 calc R . .
H45B H 0.7956 -0.4242 0.3471 0.042 Uiso 1 1 calc R . .
C46 C 0.7319(5) -0.4847(3) 0.2266(3) 0.0330(12) Uani 1 1 d . . .
C47 C 0.7471(6) -0.6342(4) 0.1931(3) 0.0431(14) Uani 1 1 d . . .
H47A H 0.7638 -0.6861 0.2209 0.065 Uiso 1 1 calc R . .
H47B H 0.8019 -0.6148 0.1532 0.065 Uiso 1 1 calc R . .
H47C H 0.6724 -0.6491 0.1618 0.065 Uiso 1 1 calc R . .
C48 C 0.0050(6) -0.1451(5) 0.3907(4) 0.0549(17) Uani 1 1 d . . .
H48A H -0.0134 -0.0917 0.3675 0.082 Uiso 1 1 calc R . .
H48B H 0.0799 -0.1310 0.4218 0.082 Uiso 1 1 calc R . .
H48C H -0.0490 -0.1691 0.4297 0.082 Uiso 1 1 calc R . .
C49 C 0.0864(7) -0.6080(4) 0.3285(4) 0.0535(17) Uani 1 1 d . . .
H49A H 0.1095 -0.6598 0.3519 0.080 Uiso 1 1 calc R . .
H49B H 0.1291 -0.5888 0.2810 0.080 Uiso 1 1 calc R . .
H49C H 0.0069 -0.6229 0.3081 0.080 Uiso 1 1 calc R . .
C50 C 0.6114(5) 0.0569(3) 0.2277(4) 0.0381(13) Uani 1 1 d . . .
H50A H 0.6602 0.1057 0.2625 0.057 Uiso 1 1 calc R . .
H50B H 0.5518 0.0287 0.2604 0.057 Uiso 1 1 calc R . .
H50C H 0.5788 0.0792 0.1758 0.057 Uiso 1 1 calc R . .
C51 C 0.5140(7) -0.3865(4) -0.0013(4) 0.0570(19) Uani 1 1 d . . .
H51A H 0.4696 -0.4328 -0.0416 0.086 Uiso 1 1 calc R . .
H51B H 0.5153 -0.4076 0.0566 0.086 Uiso 1 1 calc R . .
H51C H 0.5902 -0.3711 -0.0167 0.086 Uiso 1 1 calc R . .
C52 C 0.9370(8) 0.1059(5) 0.2594(5) 0.068(2) Uani 1 1 d . . .
H52A H 1.0076 0.0884 0.2497 0.082 Uiso 1 1 calc R . .
H52B H 0.8752 0.0559 0.2393 0.082 Uiso 1 1 calc R . .
C55 C 0.0936(8) 0.0159(7) -0.0343(6) 0.028(2) Uiso 0.50 1 d PD . 1
H55A H 0.1651 -0.0061 -0.0240 0.042 Uiso 0.50 1 d P B 1
H55B H 0.0438 -0.0247 -0.0820 0.042 Uiso 0.50 1 d P C 1
H55C H 0.1041 0.0746 -0.0361 0.042 Uiso 0.50 1 d P D 1
C54 C 0.0207(8) -0.0211(6) 0.0495(6) 0.0264(19) Uiso 0.50 1 d PD . 1
N1A N -0.0349(13) -0.0179(10) 0.0829(10) 0.077(4) Uiso 0.50 1 d P . 1
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'
Cl Cl 0.1484 0.1585 '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
Cl1A C53A Cl2A 110.3(6) . .
Cl1A C53A H53A 109.6 . .
Cl2A C53A H53A 109.6 . .
Cl1A C53A H53B 109.6 . .
Cl2A C53A H53B 109.6 . .
H53A C53A H53B 108.1 . .
Cl2B C53B Cl1B 115.0(13) . .
Cl2B C53B H53C 108.5 . .
Cl1B C53B H53C 108.5 . .
Cl2B C53B H53D 108.5 . .
Cl1B C53B H53D 108.5 . .
H53C C53B H53D 107.5 . .
C1 O1 C36 109.7(6) . .
C37 O2 C38 109.5(7) . .
C4 O4 C39 117.7(4) . .
C40 O6 C41 115.9(5) . .
C19 O7 C42 117.5(4) . .
C43 O9 C44 116.0(4) . .
C16 O10 C45 115.7(3) . .
C46 O12 C47 115.3(4) . .
C12 O13 C50 116.9(4) . .
C9 O14 C51 116.6(4) . .
C24 O15 H15A 109.5 . .
C27 O16 H16A 109.5 . .
C34 O17 C49 118.4(5) . .
C31 O18 C48 118.0(5) . .
C2 C1 O1 123.6(5) . .
C2 C1 C6 120.7(5) . .
O1 C1 C6 115.7(5) . .
C3 C2 C1 122.7(5) . .
C3 C2 H2A 118.6 . .
C1 C2 H2A 118.6 . .
C2 C3 C4 118.1(5) . .
C2 C3 C35 122.5(5) . .
C4 C3 C35 119.3(5) . .
O4 C4 C5 123.3(4) . .
O4 C4 C3 116.1(5) . .
C5 C4 C3 120.5(5) . .
C4 C5 C6 120.9(5) . .
C4 C5 H5A 119.6 . .
C6 C5 H5A 119.6 . .
C5 C6 C1 116.8(5) . .
C5 C6 C7 120.6(5) . .
C1 C6 C7 122.5(5) . .
C6 C7 C8 111.6(4) . .
C6 C7 H7A 109.3 . .
C8 C7 H7A 109.3 . .
C6 C7 H7B 109.3 . .
C8 C7 H7B 109.3 . .
H7A C7 H7B 108.0 . .
C13 C8 C9 119.2(5) . .
C13 C8 C7 120.0(4) . .
C9 C8 C7 120.8(5) . .
O14 C9 C8 116.2(4) . .
O14 C9 C10 124.0(4) . .
C8 C9 C10 119.8(5) . .
C11 C10 C9 120.2(4) . .
C11 C10 H10A 119.9 . .
C9 C10 H10A 119.9 . .
C12 C11 C10 119.3(5) . .
C12 C11 C14 121.0(4) . .
C10 C11 C14 119.6(4) . .
C11 C12 O13 116.0(4) . .
C11 C12 C13 121.1(4) . .
O13 C12 C13 122.8(4) . .
C8 C13 C12 120.3(4) . .
C8 C13 H13A 119.8 . .
C12 C13 H13A 119.8 . .
C11 C14 C15 111.3(4) . .
C11 C14 H14A 109.4 . .
C15 C14 H14A 109.4 . .
C11 C14 H14B 109.4 . .
C15 C14 H14B 109.4 . .
H14A C14 H14B 108.0 . .
C20 C15 C16 117.7(4) . .
C20 C15 C14 121.4(4) . .
C16 C15 C14 120.9(4) . .
C17 C16 O10 123.3(4) . .
C17 C16 C15 120.4(4) . .
O10 C16 C15 116.2(4) . .
C16 C17 C18 121.7(4) . .
C16 C17 H17A 119.2 . .
C18 C17 H17A 119.2 . .
C19 C18 C17 116.9(4) . .
C19 C18 C21 123.0(4) . .
C17 C18 C21 120.0(4) . .
C20 C19 C18 121.8(4) . .
C20 C19 O7 123.3(4) . .
C18 C19 O7 114.9(4) . .
C19 C20 C15 121.4(4) . .
C19 C20 H20A 119.3 . .
C15 C20 H20A 119.3 . .
C18 C21 C22 111.0(4) . .
C18 C21 H21A 109.4 . .
C22 C21 H21A 109.4 . .
C18 C21 H21B 109.4 . .
C22 C21 H21B 109.4 . .
H21A C21 H21B 108.0 . .
C23 C22 C27 118.2(5) . .
C23 C22 C21 119.0(4) . .
C27 C22 C21 122.8(4) . .
C24 C23 C22 121.7(5) . .
C24 C23 H23A 119.1 . .
C22 C23 H23A 119.1 . .
C23 C24 C25 121.0(5) . .
C23 C24 O15 116.2(4) . .
C25 C24 O15 122.8(5) . .
C26 C25 C24 116.9(5) . .
C26 C25 C28 120.8(4) . .
C24 C25 C28 122.2(5) . .
C25 C26 C27 122.9(4) . .
C25 C26 H26A 118.6 . .
C27 C26 H26A 118.6 . .
O16 C27 C26 116.6(4) . .
O16 C27 C22 124.1(5) . .
C26 C27 C22 119.3(5) . .
C25 C28 C29 111.1(4) . .
C25 C28 H28A 109.4 . .
C29 C28 H28A 109.4 . .
C25 C28 H28B 109.4 . .
C29 C28 H28B 109.4 . .
H28A C28 H28B 108.0 . .
C30 C29 C34 118.5(5) . .
C30 C29 C28 119.3(5) . .
C34 C29 C28 122.1(5) . .
C29 C30 C31 122.1(5) . .
C29 C30 H30A 118.9 . .
C31 C30 H30A 118.9 . .
O18 C31 C30 123.9(5) . .
O18 C31 C32 117.2(5) . .
C30 C31 C32 118.8(5) . .
C33 C32 C31 118.8(5) . .
C33 C32 C35 120.7(5) . .
C31 C32 C35 120.5(5) . .
C32 C33 C34 121.7(5) . .
C32 C33 H33A 119.2 . .
C34 C33 H33A 119.2 . .
C33 C34 C29 120.1(5) . .
C33 C34 O17 123.5(5) . .
C29 C34 O17 116.4(5) . .
C32 C35 C3 113.9(5) . .
C32 C35 H35A 108.8 . .
C3 C35 H35A 108.8 . .
C32 C35 H35B 108.8 . .
C3 C35 H35B 108.8 . .
H35A C35 H35B 107.7 . .
O1 C36 C37 109.6(7) . .
O1 C36 H36A 109.8 . .
C37 C36 H36A 109.8 . .
O1 C36 H36B 109.8 . .
C37 C36 H36B 109.8 . .
H36A C36 H36B 108.2 . .
O3 C37 O2 132.0(9) . .
O3 C37 C36 112.5(8) . .
O2 C37 C36 113.0(7) . .
O2 C38 H38A 109.5 . .
O2 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
O2 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
O4 C39 C40 106.6(4) . .
O4 C39 H39A 110.4 . .
C40 C39 H39A 110.4 . .
O4 C39 H39B 110.4 . .
C40 C39 H39B 110.4 . .
H39A C39 H39B 108.6 . .
O5 C40 O6 124.5(5) . .
O5 C40 C39 126.4(5) . .
O6 C40 C39 109.1(4) . .
O6 C41 H41A 109.5 . .
O6 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
O6 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
O7 C42 C43 107.1(4) . .
O7 C42 H42A 110.3 . .
C43 C42 H42A 110.3 . .
O7 C42 H42B 110.3 . .
C43 C42 H42B 110.3 . .
H42A C42 H42B 108.6 . .
O8 C43 O9 124.0(4) . .
O8 C43 C42 125.3(5) . .
O9 C43 C42 110.7(4) . .
O9 C44 H44A 109.5 . .
O9 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
O9 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
O10 C45 C46 108.3(4) . .
O10 C45 H45A 110.0 . .
C46 C45 H45A 110.0 . .
O10 C45 H45B 110.0 . .
C46 C45 H45B 110.0 . .
H45A C45 H45B 108.4 . .
O11 C46 O12 125.2(4) . .
O11 C46 C45 128.4(5) . .
O12 C46 C45 106.3(4) . .
O12 C47 H47A 109.5 . .
O12 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
O12 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
O18 C48 H48A 109.5 . .
O18 C48 H48B 109.5 . .
H48A C48 H48B 109.5 . .
O18 C48 H48C 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
O17 C49 H49A 109.5 . .
O17 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
O17 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
O13 C50 H50A 109.5 . .
O13 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
O13 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
O14 C51 H51A 109.5 . .
O14 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
O14 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
Cl3 C52 Cl4 113.2(4) . .
Cl3 C52 H52A 108.9 . .
Cl4 C52 H52A 108.9 . .
Cl3 C52 H52B 108.9 . .
Cl4 C52 H52B 108.9 . .
H52A C52 H52B 107.7 . .
N1A C55 C54 39.7(10) 2 2
N1A C55 C54 105.0(12) 2 .
C54 C55 C54 68.1(7) 2 .
N1A C55 H55A 138.3 2 .
C54 C55 H55A 163.8 2 .
C54 C55 H55A 104.2 . .
N1A C55 H55B 40.0 2 .
C54 C55 H55B 61.6 2 .
C54 C55 H55B 97.7 . .
H55A C55 H55B 106.9 . .
N1A C55 H55C 82.1 2 .
C54 C55 H55C 82.5 2 .
C54 C55 H55C 111.2 . .
H55A C55 H55C 113.7 . .
H55B C55 H55C 120.8 . .
N1A C54 C55 44.5(11) . 2
N1A C54 C55 149.8(14) . .
C55 C54 C55 111.9(7) 2 .
N1A C54 C54 105.4(14) . 2
C55 C54 C54 63.9(6) 2 2
C55 C54 C54 48.0(6) . 2
C54 N1A C55 95.8(16) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C53A Cl1A 1.752(11) .
C53A Cl2A 1.806(14) .
C53A H53A 0.9700 .
C53A H53B 0.9700 .
C53B Cl2B 1.70(2) .
C53B Cl1B 1.772(17) .
C53B H53C 0.9700 .
C53B H53D 0.9700 .
Cl3 C52 1.734(8) .
Cl4 C52 1.744(8) .
O1 C1 1.399(7) .
O1 C36 1.570(10) .
O2 C37 1.283(10) .
O2 C38 1.371(9) .
O3 C37 1.244(10) .
O4 C4 1.373(6) .
O4 C39 1.426(6) .
O5 C40 1.206(7) .
O6 C40 1.332(6) .
O6 C41 1.462(7) .
O7 C19 1.400(6) .
O7 C42 1.406(6) .
O8 C43 1.195(6) .
O9 C43 1.326(6) .
O9 C44 1.463(6) .
O10 C16 1.393(5) .
O10 C45 1.418(6) .
O11 C46 1.186(6) .
O12 C46 1.366(6) .
O12 C47 1.441(6) .
O13 C12 1.389(6) .
O13 C50 1.426(6) .
O14 C9 1.375(6) .
O14 C51 1.444(7) .
O15 C24 1.396(6) .
O15 H15A 0.8200 .
O16 C27 1.358(6) .
O16 H16A 0.8200 .
O17 C34 1.391(7) .
O17 C49 1.439(7) .
O18 C31 1.364(7) .
O18 C48 1.423(7) .
C1 C2 1.375(9) .
C1 C6 1.415(8) .
C2 C3 1.341(9) .
C2 H2A 0.9300 .
C3 C4 1.403(7) .
C3 C35 1.518(8) .
C4 C5 1.393(7) .
C5 C6 1.394(7) .
C5 H5A 0.9300 .
C6 C7 1.503(8) .
C7 C8 1.520(7) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C13 1.388(7) .
C8 C9 1.405(7) .
C9 C10 1.408(7) .
C10 C11 1.388(7) .
C10 H10A 0.9300 .
C11 C12 1.383(7) .
C11 C14 1.516(7) .
C12 C13 1.389(7) .
C13 H13A 0.9300 .
C14 C15 1.525(6) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C20 1.383(6) .
C15 C16 1.405(7) .
C16 C17 1.378(7) .
C17 C18 1.400(7) .
C17 H17A 0.9300 .
C18 C19 1.388(7) .
C18 C21 1.512(7) .
C19 C20 1.375(7) .
C20 H20A 0.9300 .
C21 C22 1.525(7) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C23 1.390(7) .
C22 C27 1.393(7) .
C23 C24 1.380(8) .
C23 H23A 0.9300 .
C24 C25 1.393(7) .
C25 C26 1.387(7) .
C25 C28 1.502(8) .
C26 C27 1.393(8) .
C26 H26A 0.9300 .
C28 C29 1.537(8) .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C29 C30 1.376(8) .
C29 C34 1.387(7) .
C30 C31 1.394(9) .
C30 H30A 0.9300 .
C31 C32 1.404(7) .
C32 C33 1.376(8) .
C32 C35 1.515(8) .
C33 C34 1.386(8) .
C33 H33A 0.9300 .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
C36 C37 1.574(13) .
C36 H36A 0.9700 .
C36 H36B 0.9700 .
C38 H38A 0.9600 .
C38 H38B 0.9600 .
C38 H38C 0.9600 .
C39 C40 1.514(8) .
C39 H39A 0.9700 .
C39 H39B 0.9700 .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
C42 C43 1.510(6) .
C42 H42A 0.9700 .
C42 H42B 0.9700 .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
C45 C46 1.506(7) .
C45 H45A 0.9700 .
C45 H45B 0.9700 .
C47 H47A 0.9600 .
C47 H47B 0.9600 .
C47 H47C 0.9600 .
C48 H48A 0.9600 .
C48 H48B 0.9600 .
C48 H48C 0.9600 .
C49 H49A 0.9600 .
C49 H49B 0.9600 .
C49 H49C 0.9600 .
C50 H50A 0.9600 .
C50 H50B 0.9600 .
C50 H50C 0.9600 .
C51 H51A 0.9600 .
C51 H51B 0.9600 .
C51 H51C 0.9600 .
C52 H52A 0.9700 .
C52 H52B 0.9700 .
C55 N1A 0.985(16) 2
C55 C54 1.397(14) 2
C55 C54 1.688(11) .
C55 H55A 0.9914 .
C55 H55B 1.0078 .
C55 H55C 0.8793 .
C54 N1A 0.896(15) .
C54 C55 1.397(14) 2
C54 C54 1.745(17) 2
N1A C55 0.985(16) 2
