#------------------------------------------------------------------------------
#$Date: 2008-03-16 06:59:57 +0000 (Sun, 16 Mar 2008) $
#$Revision: 274 $
#$URL: svn://www.crystallography.net/cod/cif/2/2002986.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_2002986
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     1999
_journal_volume     B55
_journal_page_first     432
_journal_page_last     440
_chemical_name_systematic
;
1:1 complex of
 (R)-2,3:4,5-bis[1,2-(3-phenylnaphtho)]-1,6,9,12,15,18-hexaoxacycloeicosa-2,4-
 diene with phenylglycinium methyl ester perchlorate
;
_chemical_name_common     'D20P'
_chemical_formula_moiety
; C42 H40 O6, C9 H12 N O2, Cl O4, H2 O
;
_chemical_formula_sum     'C51 H52 Cl1 N1 O13'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_weight     924.44
_chemical_melting_point     420(2)
_symmetry_cell_setting     'orthorhombic'
_symmetry_space_group_name_H-M     'P 21 21 21'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    'x+1/2, -y+1/2, -z'
    '-x, y+1/2, -z+1/2'
    '-x+1/2, -y, z+1/2'
_cell_length_a     23.048(7)
_cell_length_b     34.383(6)
_cell_length_c     11.992(6)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     9503(6)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     25
_cell_measurement_theta_min     7.95
_cell_measurement_theta_max     10.0
_cell_measurement_temperature     175
_exptl_crystal_description     'cut needle'
_exptl_crystal_colour     'colorless'
_exptl_crystal_size_max     0.39
_exptl_crystal_size_mid     0.20
_exptl_crystal_size_min     0.18
_exptl_crystal_density_diffrn     1.292
_exptl_crystal_density_meas
; 1.261 Mg m^-3^ at 295 K.  The unit-cell volume at this temperature is
  9753; correcting  for the difference in volume at 175 K leads to a
  calculated density at 175 K of 1.294
;
_exptl_crystal_density_method     'flotation (carbon tetrachloride/benzene)'
_exptl_crystal_F_000     3904
_exptl_absorpt_coefficient_mu     1.261
_exptl_absorpt_correction_type     'none'
_exptl_absorpt_correction_T_min     ?
_exptl_absorpt_correction_T_max     ?
_diffrn_ambient_temperature     175(2)
_diffrn_radiation_type     CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_source     'fine-focus sealed  tube'
_diffrn_radiation_monochromator     'graphite'
_diffrn_measurement_device     'Rigaku AFC5R'
_diffrn_measurement_method     \q/2\q
_diffrn_reflns_number     7823
_diffrn_reflns_av_R_equivalents     '0.14'
_diffrn_reflns_av_sigmaI/netI     0.0648
_diffrn_reflns_theta_min     2.57
_diffrn_reflns_theta_max     60.09
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     25
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     38
_diffrn_reflns_limit_l_min     0
_diffrn_reflns_limit_l_max     13
_diffrn_standards_number     3
_diffrn_standards_interval_count     147
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     4
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
    4 -2 1
    0 -6 1
    0 -3 -2
_reflns_number_total     7821
_reflns_number_observed     6928
_reflns_observed_criterion     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     fullcycle
_refine_ls_R_factor_all     0.0896
_refine_ls_R_factor_obs     0.0793
_refine_ls_wR_factor_all     0.2247
_refine_ls_wR_factor_obs     0.2112
_refine_ls_goodness_of_fit_all     1.003
_refine_ls_goodness_of_fit_obs     1.010
_refine_ls_restrained_S_all     1.001
_refine_ls_restrained_S_obs     1.007
_refine_ls_number_reflns     7784
_refine_ls_number_parameters     1208
_refine_ls_number_restraints     29
_refine_ls_hydrogen_treatment
;
 H atoms riding; fixed C-H distances,<u^2^>~H~ = 1.2 times U~eq~ of
 attached C, except for CH~3~ and NH~3~^+^ groups, for which factor
 was 1.5; CH~3~ groups rotating about O-C bond; NH~3~^+^ groups rotating
 about C-N bond
;
_refine_ls_weighting_scheme
        'calc w=1/[\s^2^(Fo^2^)+(0.1470P)^2^+18.9318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_shift/esd_max     '0.051,0.342,0.287'
_refine_ls_shift/esd_mean     '0.005,0.039,0.044'
_refine_diff_density_max     1.032
_refine_diff_density_min     -0.590
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef     0.00111(12)
_refine_ls_abs_structure_details     'Flack (1983)'
_refine_ls_abs_structure_Flack     -0.14(4)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'O' 'O' 0.0492 0.0322
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0311 0.0180
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'C' 'C' 0.0181 0.0091
                         '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'
    'Cl' 'Cl' 0.3639 0.7018
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_publication_material
;CRUNCH (preproduction version; de Graaff, 1998)
;
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_thermal_displace_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_group
    _atom_site_type_symbol
    C1 0.7311(3) 0.2966(2) 0.4886(7) 0.039(2) Uani d . 1 . C
    H1 0.7506 0.3168 0.5242 0.047 Uiso calc R 1 . H
    C2 0.7375(4) 0.2920(2) 0.3761(7) 0.047(2) Uani d . 1 . C
    H2 0.7603 0.3094 0.3358 0.056 Uiso calc R 1 . H
    C3 0.7098(4) 0.2612(2) 0.3214(7) 0.047(2) Uani d . 1 . C
    H3 0.7148 0.2575 0.2452 0.056 Uiso calc R 1 . H
    C4 0.6750(4) 0.2365(2) 0.3824(6) 0.040(2) Uani d . 1 . C
    H4 0.6556 0.2163 0.3466 0.048 Uiso calc R 1 . H
    C5 0.6687(3) 0.2413(2) 0.4955(6) 0.034(2) Uani d . 1 . C
    H5 0.6457 0.2239 0.5354 0.040 Uiso calc R 1 . H
    C6 0.6961(3) 0.2717(2) 0.5517(7) 0.034(2) Uani d . 1 . C
    C7 0.6888(3) 0.2789(2) 0.6732(6) 0.0286(14) Uani d . 1 . C
    C8 0.6822(3) 0.3165(2) 0.7095(6) 0.0289(15) Uani d . 1 . C
    H8 0.6820 0.3366 0.6577 0.035 Uiso calc R 1 . H
    C9 0.6756(3) 0.3254(2) 0.8241(6) 0.0297(15) Uani d . 1 . C
    C10 0.6714(3) 0.3643(2) 0.8611(7) 0.036(2) Uani d . 1 . C
    H10 0.6730 0.3844 0.8093 0.044 Uiso calc R 1 . H
    C11 0.6650(4) 0.3730(2) 0.9717(6) 0.040(2) Uani d . 1 . C
    H11 0.6625 0.3988 0.9947 0.049 Uiso calc R 1 . H
    C12 0.6621(3) 0.3428(2) 1.0505(7) 0.041(2) Uani d . 1 . C
    H12 0.6573 0.3486 1.1256 0.049 Uiso calc R 1 . H
    C13 0.6662(3) 0.3046(2) 1.0173(6) 0.033(2) Uani d . 1 . C
    H13 0.6641 0.2849 1.0702 0.040 Uiso calc R 1 . H
    C14 0.6735(3) 0.2951(2) 0.9037(5) 0.0252(14) Uani d . 1 . C
    C15 0.6816(3) 0.2560(2) 0.8658(6) 0.0261(14) Uani d . 1 . C
    C16 0.6884(3) 0.2486(2) 0.7567(6) 0.0244(14) Uani d . 1 . C
    O17 0.6970(2) 0.21010(12) 0.7224(4) 0.0277(10) Uani d . 1 . O
    C18 0.7562(3) 0.2017(2) 0.6933(7) 0.030(2) Uani d . 1 . C
    H18A 0.7825 0.2124 0.7484 0.036 Uiso calc R 1 . H
    H18B 0.7656 0.2126 0.6210 0.036 Uiso calc R 1 . H
    C19 0.7606(3) 0.1579(2) 0.6906(7) 0.035(2) Uani d . 1 . C
    H19A 0.7989 0.1506 0.6644 0.042 Uiso calc R 1 . H
    H19B 0.7562 0.1479 0.7658 0.042 Uiso calc R 1 . H
    O20 0.7181(2) 0.14019(13) 0.6206(4) 0.0319(10) Uani d . 1 . O
    C21 0.7290(3) 0.1451(2) 0.5038(6) 0.037(2) Uani d . 1 . C
    H21A 0.7645 0.1319 0.4827 0.045 Uiso calc R 1 . H
    H21B 0.7330 0.1725 0.4860 0.045 Uiso calc R 1 . H
    C22 0.6787(3) 0.1282(2) 0.4427(6) 0.039(2) Uani d . 1 . C
    H22A 0.6861 0.1288 0.3631 0.046 Uiso calc R 1 . H
    H22B 0.6732 0.1013 0.4650 0.046 Uiso calc R 1 . H
    O23 0.6276(2) 0.15005(14) 0.4673(4) 0.0345(11) Uani d . 1 . O
    C24 0.5774(3) 0.1364(2) 0.4099(6) 0.037(2) Uani d . 1 . C
    H24A 0.5668 0.1108 0.4372 0.045 Uiso calc R 1 . H
    H24B 0.5855 0.1344 0.3307 0.045 Uiso calc R 1 . H
    C25 0.5292(3) 0.1642(2) 0.4290(7) 0.042(2) Uani d . 1 . C
    H25A 0.5399 0.1897 0.4013 0.050 Uiso calc R 1 . H
    H25B 0.4949 0.1556 0.3892 0.050 Uiso calc R 1 . H
    O26 0.5171(2) 0.16630(14) 0.5462(4) 0.0357(11) Uani d . 1 . O
    C27 0.4698(3) 0.1926(2) 0.5691(7) 0.037(2) Uani d . 1 . C
    H27A 0.4352 0.1842 0.5299 0.044 Uiso calc R 1 . H
    H27B 0.4797 0.2186 0.5439 0.044 Uiso calc R 1 . H
    C28 0.4588(3) 0.1929(2) 0.6927(7) 0.038(2) Uani d . 1 . C
    H28A 0.4255 0.2091 0.7093 0.046 Uiso calc R 1 . H
    H28B 0.4506 0.1667 0.7182 0.046 Uiso calc R 1 . H
    O29 0.5096(2) 0.20781(14) 0.7497(5) 0.0346(11) Uani d . 1 . O
    C30 0.4997(3) 0.2131(2) 0.8643(6) 0.033(2) Uani d . 1 . C
    H30A 0.4863 0.1889 0.8974 0.039 Uiso calc R 1 . H
    H30B 0.4701 0.2327 0.8757 0.039 Uiso calc R 1 . H
    C31 0.5557(3) 0.2256(2) 0.9180(6) 0.0301(15) Uani d . 1 . C
    H31A 0.5709 0.2484 0.8801 0.036 Uiso calc R 1 . H
    H31B 0.5489 0.2324 0.9955 0.036 Uiso calc R 1 . H
    O32 0.5964(2) 0.19441(12) 0.9111(4) 0.0276(10) Uani d . 1 . O
    C33 0.6470(3) 0.1972(2) 0.9747(5) 0.0254(14) Uani d . 1 . C
    C34 0.6887(3) 0.2246(2) 0.9516(6) 0.0270(14) Uani d . 1 . C
    C35 0.7424(3) 0.2234(2) 1.0115(6) 0.0291(15) Uani d . 1 . C
    C36 0.7874(3) 0.2511(2) 0.9957(7) 0.033(2) Uani d . 1 . C
    H36 0.7829 0.2708 0.9432 0.040 Uiso calc R 1 . H
    C37 0.8375(3) 0.2491(2) 1.0573(7) 0.040(2) Uani d . 1 . C
    H37 0.8662 0.2677 1.0470 0.048 Uiso calc R 1 . H
    C38 0.8461(3) 0.2195(2) 1.1353(6) 0.038(2) Uani d . 1 . C
    H38 0.8803 0.2185 1.1765 0.046 Uiso calc R 1 . H
    C39 0.8040(3) 0.1919(2) 1.1508(6) 0.035(2) Uani d . 1 . C
    H39 0.8105 0.1717 1.2009 0.042 Uiso calc R 1 . H
    C40 0.7511(3) 0.1935(2) 1.0925(6) 0.031(2) Uani d . 1 . C
    C41 0.7066(3) 0.1666(2) 1.1132(6) 0.0313(15) Uani d . 1 . C
    H41 0.7127 0.1472 1.1658 0.038 Uiso calc R 1 . H
    C42 0.6544(3) 0.1680(2) 1.0585(6) 0.0276(14) Uani d . 1 . C
    C43 0.6090(3) 0.1388(2) 1.0876(6) 0.031(2) Uani d . 1 . C
    C44 0.5507(3) 0.1493(2) 1.1095(6) 0.035(2) Uani d . 1 . C
    H44 0.5394 0.1752 1.1022 0.042 Uiso calc R 1 . H
    C45 0.5106(3) 0.1221(2) 1.1413(6) 0.040(2) Uani d . 1 . C
    H45 0.4722 0.1293 1.1531 0.048 Uiso calc R 1 . H
    C46 0.5274(3) 0.0834(2) 1.1560(6) 0.042(2) Uani d . 1 . C
    H46 0.5006 0.0650 1.1801 0.051 Uiso calc R 1 . H
    C47 0.5836(4) 0.0726(2) 1.1349(7) 0.043(2) Uani d . 1 . C
    H47 0.5943 0.0467 1.1414 0.052 Uiso calc R 1 . H
    C48 0.6246(3) 0.1003(2) 1.1037(6) 0.035(2) Uani d . 1 . C
    H48 0.6630 0.0928 1.0935 0.042 Uiso calc R 1 . H
    C1C 0.5014(3) 0.0779(2) 0.6655(7) 0.037(2) Uani d . 1 . C
    H1C 0.5155 0.0711 0.5956 0.044 Uiso calc R 1 . H
    C2C 0.4435(3) 0.0700(2) 0.6948(8) 0.044(2) Uani d . 1 . C
    H2C 0.4191 0.0581 0.6434 0.052 Uiso calc R 1 . H
    C3C 0.4222(3) 0.0798(2) 0.7986(8) 0.041(2) Uani d . 1 . C
    H3C 0.3838 0.0743 0.8170 0.050 Uiso calc R 1 . H
    C4C 0.4585(3) 0.0980(2) 0.8763(7) 0.039(2) Uani d . 1 . C
    H4C 0.4447 0.1046 0.9467 0.047 Uiso calc R 1 . H
    C5C 0.5160(3) 0.1060(2) 0.8459(7) 0.035(2) Uani d . 1 . C
    H5C 0.5402 0.1184 0.8967 0.042 Uiso calc R 1 . H
    C6C 0.5372(3) 0.0961(2) 0.7430(6) 0.0293(15) Uani d . 1 . C
    C7C 0.5989(3) 0.1063(2) 0.7106(6) 0.0299(15) Uani d . 1 . C
    H7C 0.6071 0.0951 0.6371 0.036 Uiso calc R 1 . H
    N8C 0.6066(2) 0.1496(2) 0.7042(5) 0.0306(13) Uani d . 1 . N
    H8C1 0.6412(9) 0.1550(2) 0.675(4)   0.046 Uiso calc R 1 . H
    H8C2 0.604(2)   0.1597(2) 0.7724(7) 0.046 Uiso calc R 1 . H
    H8C3 0.5790(13) 0.1598(2) 0.661(3)   0.046 Uiso calc R 1 . H
    C9C 0.6429(3) 0.0907(2) 0.7937(7) 0.031(2) Uani d . 1 . C
    O10C 0.6726(2) 0.11054(14) 0.8516(4) 0.0380(12) Uani d . 1 . O
    O11C 0.6442(2) 0.05208(15) 0.7893(6) 0.051(2) Uani d . 1 . O
    C12C 0.6847(4) 0.0328(2) 0.8657(9) 0.055(2) Uani d . 1 . C
    H12C 0.680(2)   0.0052(2) 0.861(4)   0.082 Uiso calc R 1 . H
    H12D 0.6770(19) 0.0412(15) 0.9406(10) 0.082 Uiso calc R 1 . H
    H12E 0.7237(4) 0.0395(15) 0.846(3)   0.082 Uiso calc R 1 . H
    C51 1.1974(3) 0.0186(2) 0.2335(7) 0.039(2) Uani d . 1 . C
    H51 1.2302 0.0110 0.2729 0.047 Uiso calc R 1 . H
    C52 1.1913(3) 0.0075(2) 0.1237(7) 0.043(2) Uani d . 1 . C
    H52 1.2202 -0.0070 0.0894 0.051 Uiso calc R 1 . H
    C53 1.1424(3) 0.0180(2) 0.0647(7) 0.040(2) Uani d . 1 . C
    H53 1.1382 0.0104 -0.0093 0.048 Uiso calc R 1 . H
    C54 1.0997(3) 0.0396(2) 0.1160(6) 0.036(2) Uani d . 1 . C
    H54 1.0667 0.0466 0.0762 0.043 Uiso calc R 1 . H
    C55 1.1055(3) 0.0509(2) 0.2259(6) 0.031(2) Uani d . 1 . C
    H55 1.0759 0.0651 0.2595 0.037 Uiso calc R 1 . H
    C56 1.1549(3) 0.0415(2) 0.2876(7) 0.035(2) Uani d . 1 . C
    C57 1.1656(3) 0.0544(2) 0.4030(6) 0.0315(15) Uani d . 1 . C
    C58 1.2181(3) 0.0705(2) 0.4299(7) 0.036(2) Uani d . 1 . C
    H58 1.2450 0.0743 0.3733 0.044 Uiso calc R 1 . H
    C59 1.2333(3) 0.0814(2) 0.5384(7) 0.033(2) Uani d . 1 . C
    C60 1.2874(3) 0.1007(2) 0.5618(7) 0.040(2) Uani d . 1 . C
    H60 1.3130 0.1065 0.5042 0.049 Uiso calc R 1 . H
    C61 1.3009(3) 0.1103(2) 0.6691(7) 0.042(2) Uani d . 1 . C
    H61 1.3359 0.1228 0.6840 0.051 Uiso calc R 1 . H
    C62 1.2633(3) 0.1019(2) 0.7568(8) 0.048(2) Uani d . 1 . C
    H62 1.2738 0.1085 0.8292 0.058 Uiso calc R 1 . H
    C63 1.2106(3) 0.0837(2) 0.7379(7) 0.043(2) Uani d . 1 . C
    H63 1.1865 0.0774 0.7974 0.051 Uiso calc R 1 . H
    C64 1.1934(3) 0.0746(2) 0.6257(7) 0.035(2) Uani d . 1 . C
    C65 1.1374(3) 0.0594(2) 0.5984(6) 0.031(2) Uani d . 1 . C
    C66 1.1242(3) 0.0513(2) 0.4908(6) 0.032(2) Uani d . 1 . C
    O67 1.0665(2) 0.04193(12) 0.4669(4) 0.0318(11) Uani d . 1 . O
    C68 1.0535(3) 0.0017(2) 0.4456(8) 0.037(2) Uani d . 1 . C
    H68A 1.0723 -0.0148 0.5002 0.045 Uiso calc R 1 . H
    H68B 1.0667 -0.0057 0.3719 0.045 Uiso calc R 1 . H
    C69 0.9885(3) -0.0020(2) 0.4540(9) 0.047(2) Uani d . 1 . C
    H69A 0.9773 -0.0283 0.4348 0.056 Uiso calc R 1 . H
    H69B 0.9767 0.0028 0.5304 0.056 Uiso calc R 1 . H
    O70 0.9586(2) 0.02497(13) 0.3811(5) 0.0364(11) Uani d . 1 . O
    C71 0.9595(3) 0.0149(2) 0.2651(7) 0.041(2) Uani d . 1 . C
    H71A 0.9382 -0.0091 0.2530 0.049 Uiso calc R 1 . H
    H71B 0.9991 0.0111 0.2402 0.049 Uiso calc R 1 . H
    C72 0.9317(3) 0.0476(2) 0.2011(7) 0.043(2) Uani d . 1 . C
    H72A 0.9282 0.0407 0.1230 0.051 Uiso calc R 1 . H
    H72B 0.8932 0.0528 0.2301 0.051 Uiso calc R 1 . H
    O73 0.9668(2) 0.08071(14) 0.2125(4) 0.0351(11) Uani d . 1 . O
    C74 0.9457(3) 0.1133(2) 0.1526(6) 0.042(2) Uani d . 1 . C
    H74A 0.9081 0.1209 0.1816 0.050 Uiso calc R 1 . H
    H74B 0.9411 0.1065 0.0745 0.050 Uiso calc R 1 . H
    C75 0.9870(4) 0.1461(2) 0.1632(6) 0.039(2) Uani d . 1 . C
    H75A 1.0251 0.1382 0.1373 0.047 Uiso calc R 1 . H
    H75B 0.9740 0.1678 0.1178 0.047 Uiso calc R 1 . H
    O76 0.9901(2) 0.15769(14) 0.2778(4) 0.0346(11) Uani d . 1 . O
    C77 1.0264(3) 0.1909(2) 0.2914(7) 0.040(2) Uani d . 1 . C
    H77A 1.0102 0.2128 0.2510 0.048 Uiso calc R 1 . H
    H77B 1.0646 0.1855 0.2613 0.048 Uiso calc R 1 . H
    C78 1.0313(3) 0.2008(2) 0.4126(7) 0.035(2) Uani d . 1 . C
    H78A 1.0554 0.2237 0.4221 0.042 Uiso calc R 1 . H
    H78B 0.9932 0.2064 0.4429 0.042 Uiso calc R 1 . H
    O79 1.0564(2) 0.16852(13) 0.4696(4) 0.0337(11) Uani d . 1 . O
    C80 1.0689(3) 0.1780(2) 0.5848(6) 0.034(2) Uani d . 1 . C
    H80A 1.0338 0.1866 0.6220 0.041 Uiso calc R 1 . H
    H80B 1.0972 0.1988 0.5883 0.041 Uiso calc R 1 . H
    C81 1.0922(3) 0.1427(2) 0.6411(7) 0.037(2) Uani d . 1 . C
    H81A 1.1238 0.1317 0.5979 0.045 Uiso calc R 1 . H
    H81B 1.1067 0.1493 0.7146 0.045 Uiso calc R 1 . H
    O82 1.0456(2) 0.11497(13) 0.6502(4) 0.0314(10) Uani d . 1 . O
    C83 1.0529(3) 0.0812(2) 0.7134(6) 0.032(2) Uani d . 1 . C
    C84 1.0937(3) 0.0535(2) 0.6904(5) 0.0304(15) Uani d . 1 . C
    C85 1.0922(3) 0.0169(2) 0.7468(6) 0.035(2) Uani d . 1 . C
    C86 1.1309(3) -0.0141(2) 0.7230(7) 0.042(2) Uani d . 1 . C
    H86 1.1602 -0.0106 0.6707 0.051 Uiso calc R 1 . H
    C87 1.1257(4) -0.0490(2) 0.7762(7) 0.046(2) Uani d . 1 . C
    H87 1.1514 -0.0690 0.7589 0.055 Uiso calc R 1 . H
    C88 1.0827(4) -0.0554(2) 0.8556(8) 0.048(2) Uani d . 1 . C
    H88 1.0804 -0.0793 0.8917 0.057 Uiso calc R 1 . H
    C89 1.0444(3) -0.0268(2) 0.8804(7) 0.041(2) Uani d . 1 . C
    H89 1.0152 -0.0316 0.9323 0.049 Uiso calc R 1 . H
    C90 1.0478(3) 0.0105(2) 0.8285(6) 0.035(2) Uani d . 1 . C
    C91 1.0095(3) 0.0405(2) 0.8533(6) 0.040(2) Uani d . 1 . C
    H91 0.9812 0.0362 0.9073 0.048 Uiso calc R 1 . H
    C92 1.0112(3) 0.0762(2) 0.8022(6) 0.035(2) Uani d . 1 . C
    C93 0.9692(4) 0.1067(3) 0.8332(7) 0.046(2) Uani d . 1 . C
    C94 0.9877(5) 0.1448(3) 0.8550(7) 0.059(3) Uani d . 1 . C
    H94 1.0267 0.1513 0.8495 0.071 Uiso calc R 1 . H
    C95 0.9461(5) 0.1734(3) 0.8856(7) 0.068(3) Uani d . 1 . C
    H95 0.9565 0.1994 0.8954 0.082 Uiso calc R 1 . H
    C96 0.8873(5) 0.1606(4) 0.9006(8) 0.070(3) Uani d . 1 . C
    H96 0.8597 0.1786 0.9237 0.084 Uiso calc R 1 . H
    C97 0.8699(4) 0.1233(3) 0.8828(8) 0.064(3) Uani d . 1 . C
    H97 0.8313 0.1160 0.8915 0.077 Uiso calc R 1 . H
    C98 0.9111(4) 0.0973(3) 0.8519(7) 0.052(2) Uani d . 1 . C
    H98 0.8999 0.0715 0.8425 0.063 Uiso calc R 1 . H
    C55C 0.9155(3) 0.1664(2) 0.5960(6) 0.0305(15) Uani d . 1 . C
    H55C 0.9337 0.1507 0.6486 0.037 Uiso calc R 1 . H
    C54C 0.9043(3) 0.2056(2) 0.6199(6) 0.034(2) Uani d . 1 . C
    H54C 0.9159 0.2162 0.6878 0.040 Uiso calc R 1 . H
    C53C 0.8759(3) 0.2287(2) 0.5420(6) 0.035(2) Uani d . 1 . C
    H53C 0.8687 0.2548 0.5575 0.042 Uiso calc R 1 . H
    C52C 0.8588(3) 0.2131(2) 0.4426(7) 0.037(2) Uani d . 1 . C
    H52C 0.8390 0.2285 0.3915 0.044 Uiso calc R 1 . H
    C51C 0.8705(3) 0.1743(2) 0.4168(6) 0.035(2) Uani d . 1 . C
    H51C 0.8592 0.1640 0.3485 0.042 Uiso calc R 1 . H
    C56C 0.8994(3) 0.1513(2) 0.4944(6) 0.0275(14) Uani d . 1 . C
    C57C 0.9118(3) 0.1094(2) 0.4668(6) 0.0304(15) Uani d . 1 . C
    H57C 0.8920 0.1034 0.3966 0.036 Uiso calc R 1 . H
    N58C 0.9752(2) 0.1025(2) 0.4493(5) 0.0304(12) Uani d . 1 . N
    H58C 0.9806(3) 0.0789(6) 0.421(4)   0.046 Uiso calc R 1 . H
    H58D 0.9937(4) 0.1043(14) 0.5143(8) 0.046 Uiso calc R 1 . H
    H58E 0.9892(5) 0.1203(9) 0.402(3)   0.046 Uiso calc R 1 . H
    C59C 0.8908(3) 0.0807(2) 0.5530(7) 0.038(2) Uani d . 1 . C
    O60C 0.9218(2) 0.06103(15) 0.6092(5) 0.0425(13) Uani d . 1 . O
    O61C 0.8327(2) 0.0810(2) 0.5589(5) 0.0479(14) Uani d . 1 . O
    C62C 0.8062(4) 0.0559(3) 0.6419(8) 0.056(2) Uani d . 1 . C
    H62C 0.7649(5) 0.0593(15) 0.641(4)   0.085 Uiso calc R 1 . H
    H62D 0.821(2)   0.0626(13) 0.7145(11) 0.085 Uiso calc R 1 . H
    H62E 0.816(2)   0.0293(3) 0.626(3)   0.085 Uiso calc R 1 . H
    Cl1A 0.66440(9) 0.01254(5) 0.4372(2) 0.0546(5) Uani d . 1 1 Cl
    O2A 0.7178(9) 0.0287(6) 0.4802(18) 0.090(6) Uiso d P 0.50 1 O
    O2A' 0.7168(6) 0.0354(4) 0.4325(13) 0.055(3) Uiso d P 0.50 1 O
    O3A 0.6168(4) 0.0333(2) 0.4805(10) 0.101(3) Uani d . 1 1 O
    O4A 0.6683(5) -0.0254(2) 0.4733(11) 0.131(4) Uani d . 1 1 O
    O5A 0.6608(6) 0.0099(4) 0.3164(9) 0.139(4) Uani d . 1 1 O
    O1W 0.7958(3) 0.0915(2) 0.2974(7) 0.081(2) Uani d . 1 . O
    O2W 0.7432(4) 0.0455(2) 0.1498(8) 0.078(2) Uani d P 0.85 . O
    O3W 1.3175(14) 0.1045(9) 1.034(3)   0.036(7) Uiso d P 0.15 . O
    Cl11 0.8483(2) 0.33241(10) 0.7379(3) 0.0620(10) Uiso d PD 0.55 4 Cl
    O12A 0.8241(2) 0.29351(12) 0.7383(6) 0.066(2) Uiso d PD 0.80 4 O
    O13A 0.8040(3) 0.3601(2) 0.7057(8) 0.066(3) Uiso d PD 0.55 4 O
    O14A 0.8960(3) 0.3342(2) 0.6593(8) 0.156(10) Uiso d PD 0.55 4 O
    O15A 0.8694(5) 0.3419(2) 0.8487(5) 0.119(7) Uiso d PD 0.55 4 O
    Cl16 0.9087(4) 0.2968(2) 0.8110(7) 0.052(2) Uiso d PD 0.20 5 Cl
    O17A 0.9591(5) 0.2726(4) 0.8314(15) 0.039(6) Uiso d PD 0.20 5 O
    O18A 0.8586(5) 0.2723(5) 0.7904(17) 0.054(7) Uiso d PD 0.20 5 O
    O19A 0.8979(9) 0.3211(5) 0.9077(13) 0.064(9) Uiso d PD 0.20 5 O
    O20A 0.9192(8) 0.3212(5) 0.7145(13) 0.068(9) Uiso d PD 0.20 5 O
    Cl21 0.8784(2) 0.3129(2) 0.7637(5) 0.040(2) Uiso d PD 0.25 6 Cl
    O22A 0.9261(3) 0.2859(4) 0.7486(18) 0.103(11) Uiso d PD 0.25 6 O
    O23A 0.8774(6) 0.3263(6) 0.8783(8) 0.069(8) Uiso d PD 0.25 6 O
    O24A 0.8859(6) 0.3458(4) 0.6896(15) 0.077(8) Uiso d PD 0.25 6 O
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    C1 0.043(4) 0.028(4) 0.048(5) -0.002(3) -0.002(4) 0.002(3)
    C2 0.055(5) 0.038(4) 0.047(5) 0.001(4) 0.016(4) 0.009(4)
    C3 0.054(5) 0.040(4) 0.046(5) 0.009(4) 0.009(4) 0.001(4)
    C4 0.048(4) 0.034(4) 0.037(4) 0.003(4) -0.006(4) 0.001(3)
    C5 0.033(4) 0.029(4) 0.039(4) 0.002(3) 0.000(3) 0.004(3)
    C6 0.033(4) 0.026(3) 0.042(4) 0.004(3) 0.007(3) 0.000(3)
    C7 0.025(3) 0.031(3) 0.029(3) -0.002(3) 0.001(3) 0.003(3)
    C8 0.029(3) 0.028(3) 0.030(3) -0.001(3) -0.001(3) 0.002(3)
    C9 0.027(3) 0.030(3) 0.032(4) -0.002(3) -0.003(3) 0.001(3)
    C10 0.041(4) 0.022(3) 0.046(4) 0.004(3) 0.002(4) -0.001(3)
    C11 0.052(5) 0.028(4) 0.042(4) 0.000(3) 0.001(4) -0.003(3)
    C12 0.048(4) 0.033(4) 0.041(4) 0.000(3) 0.000(4) -0.008(3)
    C13 0.034(4) 0.031(4) 0.035(4) -0.002(3) 0.003(3) 0.004(3)
    C14 0.024(3) 0.028(3) 0.024(3) -0.001(3) 0.000(3) -0.001(3)
    C15 0.019(3) 0.024(3) 0.036(4) 0.000(3) 0.000(3) 0.001(3)
    C16 0.020(3) 0.020(3) 0.034(4) 0.000(3) 0.000(3) 0.002(3)
    O17 0.022(2) 0.023(2) 0.038(3) 0.002(2) 0.003(2) -0.006(2)
    C18 0.017(3) 0.027(3) 0.048(4) 0.003(3) 0.003(3) -0.007(3)
    C19 0.023(3) 0.031(4) 0.050(4) 0.001(3) -0.004(3) -0.004(3)
    O20 0.028(2) 0.030(2) 0.038(3) 0.000(2) 0.003(2) -0.005(2)
    C21 0.035(4) 0.041(4) 0.036(4) 0.001(3) 0.004(3) -0.002(3)
    C22 0.042(4) 0.042(4) 0.032(4) 0.004(3) -0.001(3) -0.009(3)
    O23 0.032(2) 0.035(3) 0.037(3) 0.002(2) -0.004(2) -0.006(2)
    C24 0.037(4) 0.042(4) 0.032(4) -0.008(3) -0.005(3) -0.001(3)
    C25 0.038(4) 0.047(4) 0.041(4) -0.006(4) -0.011(4) 0.006(4)
    O26 0.034(3) 0.034(2) 0.038(3) 0.003(2) -0.010(2) 0.003(2)
    C27 0.031(4) 0.029(4) 0.050(4) 0.002(3) -0.012(4) 0.001(3)
    C28 0.021(3) 0.035(4) 0.058(5) 0.001(3) -0.010(3) -0.004(4)
    O29 0.026(2) 0.033(2) 0.045(3) -0.002(2) -0.006(2) -0.001(2)
    C30 0.020(3) 0.032(4) 0.047(4) 0.003(3) 0.000(3) 0.001(3)
    C31 0.030(3) 0.023(3) 0.037(4) 0.007(3) -0.003(3) -0.001(3)
    O32 0.022(2) 0.023(2) 0.037(3) 0.000(2) -0.006(2) 0.000(2)
    C33 0.023(3) 0.025(3) 0.028(3) 0.001(3) -0.001(3) -0.001(3)
    C34 0.025(3) 0.026(3) 0.030(3) 0.005(3) -0.003(3) -0.002(3)
    C35 0.022(3) 0.026(3) 0.039(4) 0.005(3) 0.005(3) -0.003(3)
    C36 0.027(3) 0.026(3) 0.047(4) 0.002(3) 0.000(3) -0.001(3)
    C37 0.024(3) 0.044(4) 0.052(5) -0.002(3) -0.003(3) -0.010(4)
    C38 0.031(4) 0.046(4) 0.037(4) 0.002(3) -0.006(3) -0.004(3)
    C39 0.033(4) 0.038(4) 0.035(4) 0.002(3) -0.006(3) 0.001(3)
    C40 0.025(3) 0.028(3) 0.040(4) 0.003(3) -0.003(3) -0.002(3)
    C41 0.028(3) 0.033(4) 0.032(4) 0.006(3) 0.001(3) 0.002(3)
    C42 0.024(3) 0.032(3) 0.026(3) 0.004(3) -0.001(3) 0.003(3)
    C43 0.030(4) 0.029(4) 0.035(4) 0.000(3) 0.001(3) -0.002(3)
    C44 0.031(4) 0.037(4) 0.037(4) 0.002(3) 0.001(3) 0.000(3)
    C45 0.032(4) 0.051(5) 0.036(4) -0.003(3) 0.002(3) -0.002(4)
    C46 0.040(4) 0.052(5) 0.035(4) -0.014(4) 0.003(3) 0.000(4)
    C47 0.059(5) 0.031(4) 0.040(4) -0.008(4) 0.002(4) 0.004(3)
    C48 0.034(4) 0.037(4) 0.034(4) -0.003(3) -0.003(3) -0.001(3)
    C1C 0.031(4) 0.028(4) 0.051(4) -0.003(3) -0.005(3) 0.002(3)
    C2C 0.031(4) 0.032(4) 0.068(6) -0.004(3) -0.016(4) 0.017(4)
    C3C 0.021(3) 0.035(4) 0.069(6) -0.009(3) -0.010(4) 0.017(4)
    C4C 0.026(4) 0.040(4) 0.051(5) -0.001(3) 0.007(3) 0.017(4)
    C5C 0.026(4) 0.027(3) 0.053(5) -0.005(3) -0.004(3) 0.008(3)
    C6C 0.030(4) 0.020(3) 0.038(4) 0.000(3) -0.002(3) 0.006(3)
    C7C 0.027(3) 0.024(3) 0.039(4) -0.002(3) -0.007(3) 0.003(3)
    N8C 0.022(3) 0.023(3) 0.046(3) -0.003(2) -0.003(3) 0.002(3)
    C9C 0.021(3) 0.024(3) 0.048(4) 0.001(3) -0.001(3) -0.005(3)
    O10C 0.035(3) 0.036(3) 0.043(3) -0.002(2) -0.004(2) 0.002(2)
    O11C 0.045(3) 0.028(3) 0.080(4) 0.007(2) -0.024(3) 0.000(3)
    C12C 0.044(5) 0.035(4) 0.086(7) 0.013(4) -0.019(5) 0.011(4)
    C51 0.034(4) 0.039(4) 0.045(4) 0.006(3) -0.001(4) 0.001(3)
    C52 0.038(4) 0.038(4) 0.053(5) 0.009(3) 0.005(4) -0.005(4)
    C53 0.044(4) 0.037(4) 0.040(4) -0.008(3) 0.001(4) -0.005(3)
    C54 0.033(4) 0.033(4) 0.043(4) -0.001(3) -0.002(3) 0.005(3)
    C55 0.027(3) 0.026(3) 0.040(4) -0.005(3) 0.000(3) 0.001(3)
    C56 0.029(4) 0.025(3) 0.052(4) 0.001(3) 0.001(3) 0.000(3)
    C57 0.028(3) 0.027(3) 0.040(4) 0.006(3) -0.001(3) -0.001(3)
    C58 0.031(4) 0.030(3) 0.048(4) 0.000(3) 0.000(3) -0.001(3)
    C59 0.026(3) 0.024(3) 0.050(4) 0.009(3) -0.005(3) -0.009(3)
    C60 0.030(4) 0.038(4) 0.054(5) 0.005(3) -0.005(4) -0.006(4)
    C61 0.024(4) 0.040(4) 0.063(5) 0.011(3) -0.013(4) -0.007(4)
    C62 0.037(4) 0.047(4) 0.061(5) 0.015(4) -0.018(4) -0.015(4)
    C63 0.036(4) 0.041(4) 0.051(5) 0.011(3) -0.008(4) -0.011(4)
    C64 0.031(4) 0.029(3) 0.045(4) 0.011(3) -0.008(3) -0.005(3)
    C65 0.026(3) 0.028(3) 0.040(4) 0.008(3) -0.001(3) -0.003(3)
    C66 0.025(3) 0.023(3) 0.047(4) 0.002(3) -0.001(3) -0.002(3)
    O67 0.027(2) 0.021(2) 0.048(3) -0.001(2) -0.003(2) -0.004(2)
    C68 0.029(4) 0.018(3) 0.065(5) -0.004(3) -0.001(4) 0.001(3)
    C69 0.034(4) 0.021(3) 0.085(6) -0.006(3) 0.013(4) 0.004(4)
    O70 0.029(2) 0.025(2) 0.055(3) 0.000(2) 0.000(2) -0.005(2)
    C71 0.031(4) 0.038(4) 0.054(5) -0.006(3) 0.001(4) -0.018(4)
    C72 0.030(4) 0.051(5) 0.047(5) -0.003(3) -0.004(3) -0.017(4)
    O73 0.030(2) 0.036(3) 0.039(3) 0.004(2) -0.006(2) -0.003(2)
    C74 0.038(4) 0.059(5) 0.028(4) 0.013(4) -0.003(3) 0.000(3)
    C75 0.051(4) 0.046(4) 0.019(3) 0.011(4) -0.002(3) 0.009(3)
    O76 0.033(2) 0.038(3) 0.033(3) 0.002(2) 0.000(2) 0.008(2)
    C77 0.038(4) 0.037(4) 0.045(4) -0.003(3) 0.001(4) 0.017(3)
    C78 0.027(3) 0.022(3) 0.056(5) -0.001(3) 0.005(3) 0.000(3)
    O79 0.028(2) 0.026(2) 0.047(3) 0.002(2) -0.004(2) 0.005(2)
    C80 0.034(4) 0.025(3) 0.043(4) 0.001(3) -0.005(3) -0.004(3)
    C81 0.038(4) 0.035(4) 0.039(4) 0.004(3) -0.009(3) -0.002(3)
    O82 0.032(2) 0.027(2) 0.035(3) 0.007(2) -0.005(2) 0.002(2)
    C83 0.036(4) 0.029(3) 0.031(4) 0.007(3) -0.006(3) 0.001(3)
    C84 0.035(4) 0.033(4) 0.023(3) 0.009(3) -0.004(3) -0.002(3)
    C85 0.036(4) 0.034(4) 0.034(4) 0.004(3) -0.006(3) 0.003(3)
    C86 0.040(4) 0.036(4) 0.051(5) 0.002(3) -0.007(4) 0.005(4)
    C87 0.048(5) 0.034(4) 0.056(5) 0.010(4) -0.018(4) 0.002(4)
    C88 0.051(5) 0.035(4) 0.058(5) -0.004(4) -0.020(4) 0.008(4)
    C89 0.044(4) 0.040(4) 0.038(4) -0.009(3) -0.010(4) 0.009(3)
    C90 0.037(4) 0.041(4) 0.026(3) 0.004(3) -0.008(3) 0.000(3)
    C91 0.042(4) 0.047(4) 0.031(4) 0.005(4) -0.002(3) 0.008(3)
    C92 0.036(4) 0.042(4) 0.027(3) 0.008(3) 0.000(3) 0.001(3)
    C93 0.056(5) 0.049(5) 0.032(4) 0.018(4) -0.006(4) 0.004(4)
    C94 0.075(6) 0.068(6) 0.034(4) 0.039(5) -0.003(4) 0.003(4)
    C95 0.116(9) 0.063(6) 0.027(4) 0.047(6) -0.018(5) -0.008(4)
    C96 0.062(6) 0.114(10) 0.033(5) 0.047(7) -0.006(4) 0.008(5)
    C97 0.056(6) 0.093(8) 0.044(5) 0.038(6) -0.006(4) -0.004(5)
    C98 0.045(5) 0.073(6) 0.038(4) 0.026(4) 0.002(4) 0.002(4)
    C55C 0.030(3) 0.030(3) 0.031(4) 0.007(3) -0.002(3) 0.004(3)
    C54C 0.032(3) 0.029(3) 0.040(4) 0.002(3) 0.003(3) -0.004(3)
    C53C 0.032(4) 0.028(3) 0.044(4) 0.002(3) 0.005(3) 0.002(3)
    C52C 0.031(4) 0.036(4) 0.044(4) 0.010(3) 0.005(3) 0.013(3)
    C51C 0.036(4) 0.041(4) 0.027(3) 0.007(3) -0.001(3) 0.004(3)
    C56C 0.022(3) 0.029(3) 0.031(4) 0.003(3) 0.009(3) 0.002(3)
    C57C 0.025(3) 0.030(3) 0.036(4) 0.002(3) -0.002(3) 0.000(3)
    N58C 0.025(3) 0.027(3) 0.039(3) 0.006(2) 0.001(3) -0.005(3)
    C59C 0.033(4) 0.031(4) 0.049(5) -0.001(3) 0.005(4) -0.007(4)
    O60C 0.041(3) 0.036(3) 0.050(3) 0.006(2) 0.007(3) 0.010(3)
    O61C 0.031(3) 0.042(3) 0.070(4) -0.004(2) 0.010(3) 0.011(3)
    C62C 0.054(5) 0.051(5) 0.064(6) -0.019(4) 0.014(5) 0.011(4)
    Cl1A 0.0495(11) 0.0353(9) 0.0789(15) 0.0012(9) -0.0056(11) -0.0122(10)
    O3A 0.075(5) 0.076(5) 0.153(9) 0.017(4) 0.025(6) -0.027(6)
    O4A 0.151(9) 0.057(5) 0.185(11) 0.026(6) 0.064(9) 0.031(6)
    O5A 0.158(10) 0.178(11) 0.081(6) -0.007(9) -0.022(7) -0.013(7)
    O1W 0.062(4) 0.086(5) 0.096(6) 0.011(4) 0.018(4) -0.016(5)
    O2W 0.073(5) 0.064(5) 0.096(6) 0.008(4) -0.019(5) -0.016(5)