#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:21:35 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180074 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/20/7052062.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_7052062
loop_
_publ_author_name
'Antti Åhman'
'Minna Luostarinen'
'Kari Rissanen'
'Maija Nissinen'
_publ_section_title
;
 Complexation of C-methyl pyrogallarene with small quaternary and
 tertiary alkyl ammonium cations
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              169
_journal_paper_doi               10.1039/b609117b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety         'C32 H32 O12, C6 H16 N, C2 H6 O, C H4 O, Cl'
_chemical_formula_sum            'C41 H58 Cl N O14'
_chemical_formula_weight         824.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.883(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.2275(11)
_cell_length_b                   25.3429(13)
_cell_length_c                   17.9561(5)
_cell_measurement_temperature    173.0(1)
_cell_volume                     8112.1(7)
_computing_cell_refinement       Denzo-SMN
_computing_data_collection       Collect
_computing_data_reduction        Denzo-SMN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0877
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27871
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.9525
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
'Blessing, R. H. Acta Crystallogr., Sect A 1995, 51, 33-38'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7814
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.1021
_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)+(0.0693P)²+76.5581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2296
_refine_ls_wR_factor_ref         0.2541
_reflns_number_gt                5216
_reflns_number_total             7814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609117b.txt
_cod_data_source_block           PC1_TriEA
_cod_original_cell_volume        8112.1(6)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7052062
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
C1 C 0.2290(3) 0.0374(2) 0.2212(3) 0.0263(12) Uani 1 1 d . . .
C2 C 0.2556(3) 0.02489(19) 0.3088(3) 0.0261(12) Uani 1 1 d . . .
H2 H 0.3068 0.0152 0.3466 0.031 Uiso 1 1 calc R . .
C3 C 0.2111(3) 0.0259(2) 0.3441(3) 0.0267(12) Uani 1 1 d . . .
C4 C 0.1363(3) 0.0409(2) 0.2873(4) 0.0334(13) Uani 1 1 d . . .
C5 C 0.1086(3) 0.0554(2) 0.2016(3) 0.0321(13) Uani 1 1 d . . .
C6 C 0.1536(3) 0.0524(2) 0.1676(3) 0.0290(12) Uani 1 1 d . . .
C7 C 0.2426(3) 0.0119(2) 0.4408(3) 0.0250(11) Uani 1 1 d . . .
H7 H 0.1994 -0.0005 0.4440 0.030 Uiso 1 1 calc R . .
C8 C 0.2741(3) 0.0609(2) 0.4993(3) 0.0229(11) Uani 1 1 d . . .
C9 C 0.3476(3) 0.0773(2) 0.5348(3) 0.0241(11) Uani 1 1 d . . .
H9 H 0.3777 0.0577 0.5205 0.029 Uiso 1 1 calc R . .
C10 C 0.3793(3) 0.1208(2) 0.5900(3) 0.0230(11) Uani 1 1 d . . .
C11 C 0.3337(3) 0.1495(2) 0.6094(3) 0.0251(11) Uani 1 1 d . . .
C12 C 0.2596(3) 0.1353(2) 0.5722(3) 0.0253(11) Uani 1 1 d . . .
C13 C 0.2294(3) 0.0914(2) 0.5183(3) 0.0253(11) Uani 1 1 d . . .
C14 C 0.4593(3) 0.1388(2) 0.6240(3) 0.0259(11) Uani 1 1 d . . .
H14 H 0.4762 0.1601 0.6787 0.031 Uiso 1 1 calc R . .
C15 C 0.4609(3) 0.1762(2) 0.5580(3) 0.0238(11) Uani 1 1 d . . .
C16 C 0.4720(3) 0.1575(2) 0.4930(3) 0.0222(11) Uani 1 1 d . . .
H16 H 0.4769 0.1205 0.4890 0.027 Uiso 1 1 calc R . .
C17 C 0.4762(3) 0.1903(2) 0.4338(3) 0.0234(11) Uani 1 1 d . . .
C18 C 0.4667(3) 0.2445(2) 0.4394(3) 0.0262(11) Uani 1 1 d . . .
C19 C 0.4537(3) 0.2646(2) 0.5010(3) 0.0287(12) Uani 1 1 d . . .
C20 C 0.4517(3) 0.2303(2) 0.5612(3) 0.0278(12) Uani 1 1 d . . .
C21 C 0.4895(3) 0.1679(2) 0.3641(3) 0.0262(12) Uani 1 1 d . . .
H21 H 0.5113 0.1970 0.3473 0.031 Uiso 1 1 calc R . .
C22 C 0.4151(3) 0.1524(2) 0.2803(3) 0.0245(11) Uani 1 1 d . . .
C23 C 0.3817(3) 0.1038(2) 0.2693(3) 0.0239(11) Uani 1 1 d . . .
H23 H 0.4059 0.0792 0.3168 0.029 Uiso 1 1 calc R . .
C24 C 0.3144(3) 0.0886(2) 0.1923(3) 0.0259(12) Uani 1 1 d . . .
C25 C 0.2800(3) 0.1254(2) 0.1238(3) 0.0271(12) Uani 1 1 d . . .
C26 C 0.3113(3) 0.1748(2) 0.1327(3) 0.0281(12) Uani 1 1 d . . .
C27 C 0.3777(3) 0.1885(2) 0.2106(3) 0.0249(11) Uani 1 1 d . . .
C28 C 0.2783(3) 0.0350(2) 0.1838(3) 0.0276(12) Uani 1 1 d . . .
H28 H 0.2444 0.0277 0.1189 0.033 Uiso 1 1 calc R . .
C29 C 0.2991(3) -0.0338(2) 0.4740(4) 0.0335(13) Uani 1 1 d . . .
H29A H 0.3430 -0.0230 0.4731 0.050 Uiso 1 1 calc R . .
H29B H 0.2756 -0.0645 0.4353 0.050 Uiso 1 1 calc R . .
H29C H 0.3148 -0.0430 0.5347 0.050 Uiso 1 1 calc R . .
C30 C 0.5144(3) 0.0934(2) 0.6522(3) 0.0332(13) Uani 1 1 d . . .
H30A H 0.5005 0.0715 0.6005 0.050 Uiso 1 1 calc R . .
H30B H 0.5132 0.0721 0.6969 0.050 Uiso 1 1 calc R . .
H30C H 0.5651 0.1075 0.6774 0.050 Uiso 1 1 calc R . .
C31 C 0.5466(3) 0.1226(2) 0.4007(4) 0.0297(12) Uani 1 1 d . . .
H31A H 0.5270 0.0932 0.4178 0.045 Uiso 1 1 calc R . .
H31B H 0.5939 0.1349 0.4527 0.045 Uiso 1 1 calc R . .
H31C H 0.5552 0.1108 0.3550 0.045 Uiso 1 1 calc R . .
C32 C 0.3361(3) -0.0098(2) 0.2230(4) 0.0328(13) Uani 1 1 d . . .
H32A H 0.3631 -0.0111 0.1929 0.049 Uiso 1 1 calc R . .
H32B H 0.3103 -0.0435 0.2148 0.049 Uiso 1 1 calc R . .
H32C H 0.3718 -0.0035 0.2865 0.049 Uiso 1 1 calc R . .
O4 O 0.0882(3) 0.0410(2) 0.3178(3) 0.0534(13) Uani 1 1 d . . .
H4 H 0.0912 0.0119 0.3420 0.080 Uiso 1 1 calc R . .
O5 O 0.0343(2) 0.07045(18) 0.1432(3) 0.0427(11) Uani 1 1 d D . .
H5 H 0.0220 0.0924 0.1681 0.064 Uiso 1 1 calc R . .
O6 O 0.1241(2) 0.06362(18) 0.0793(2) 0.0418(11) Uani 1 1 d . . .
H6 H 0.0803 0.0753 0.0561 0.063 Uiso 1 1 calc RD . .
O11 O 0.3583(2) 0.19280(15) 0.6653(3) 0.0334(9) Uani 1 1 d . . .
H11 H 0.3879 0.2106 0.6579 0.050 Uiso 1 1 calc R . .
O12 O 0.2165(2) 0.16679(16) 0.5914(3) 0.0372(10) Uani 1 1 d . . .
H12 H 0.1719 0.1561 0.5625 0.056 Uiso 1 1 calc R . .
O13 O 0.1554(2) 0.08076(17) 0.4867(3) 0.0381(10) Uani 1 1 d . . .
H13 H 0.1336 0.0700 0.4341 0.057 Uiso 1 1 calc R . .
O18 O 0.4698(2) 0.28120(15) 0.3842(3) 0.0401(10) Uani 1 1 d . . .
H18 H 0.4495 0.2686 0.3329 0.060 Uiso 1 1 calc R . .
O19 O 0.4422(2) 0.31727(14) 0.5084(3) 0.0375(10) Uani 1 1 d . . .
H19 H 0.4530 0.3352 0.4774 0.056 Uiso 1 1 calc R . .
O20 O 0.4410(2) 0.24983(16) 0.6252(3) 0.0376(10) Uani 1 1 d . . .
H20 H 0.4538 0.2817 0.6346 0.056 Uiso 1 1 calc R . .
O25 O 0.2150(2) 0.11530(18) 0.0435(2) 0.0412(11) Uani 1 1 d . . .
H25 H 0.1838 0.1007 0.0519 0.062 Uiso 1 1 calc R . .
O26 O 0.2779(2) 0.21267(15) 0.0677(2) 0.0370(10) Uani 1 1 d . . .
H26 H 0.2374 0.2009 0.0245 0.056 Uiso 1 1 calc R . .
O27 O 0.4078(2) 0.23830(15) 0.2209(2) 0.0352(9) Uani 1 1 d . . .
H27 H 0.3776 0.2573 0.1776 0.053 Uiso 1 1 calc R . .
Cl1 Cl 0.5000 0.34603(8) 0.7500 0.0405(5) Uani 1 2 d S . .
N50 N 0.2151(2) 0.25282(17) 0.2638(3) 0.0240(9) Uani 1 1 d . . .
H50X H 0.2093 0.2757 0.3003 0.029 Uiso 1 1 calc R . .
C50 C 0.1381(3) 0.2326(2) 0.1959(4) 0.0324(13) Uani 1 1 d . . .
H50A H 0.1052 0.2629 0.1627 0.039 Uiso 1 1 calc R . .
H50B H 0.1170 0.2147 0.2267 0.039 Uiso 1 1 calc R . .
C51 C 0.1381(4) 0.1944(3) 0.1310(4) 0.0498(18) Uani 1 1 d . . .
H51A H 0.1541 0.2129 0.0960 0.075 Uiso 1 1 calc R . .
H51B H 0.0874 0.1803 0.0913 0.075 Uiso 1 1 calc R . .
H51C H 0.1728 0.1654 0.1637 0.075 Uiso 1 1 calc R . .
C52 C 0.2677(3) 0.2103(2) 0.3227(4) 0.0349(13) Uani 1 1 d . . .
H52A H 0.3165 0.2264 0.3673 0.042 Uiso 1 1 calc R . .
H52B H 0.2763 0.1855 0.2866 0.042 Uiso 1 1 calc R . .
C53 C 0.2383(4) 0.1799(3) 0.3702(5) 0.058(2) Uani 1 1 d . . .
H53A H 0.2201 0.2047 0.3964 0.088 Uiso 1 1 calc R . .
H53B H 0.2786 0.1583 0.4172 0.088 Uiso 1 1 calc R . .
H53C H 0.1969 0.1570 0.3279 0.088 Uiso 1 1 calc R . .
C54 C 0.2503(4) 0.2846(2) 0.2248(4) 0.0399(14) Uani 1 1 d . . .
H54A H 0.3015 0.2952 0.2729 0.048 Uiso 1 1 calc R . .
H54B H 0.2547 0.2622 0.1827 0.048 Uiso 1 1 calc R . .
C55 C 0.2059(5) 0.3333(3) 0.1772(6) 0.069(2) Uani 1 1 d . . .
H55A H 0.1599 0.3231 0.1214 0.104 Uiso 1 1 calc R . .
H55B H 0.2361 0.3563 0.1645 0.104 Uiso 1 1 calc R . .
H55C H 0.1929 0.3522 0.2146 0.104 Uiso 1 1 calc R . .
O50 O -0.0070(3) 0.10455(19) -0.0502(3) 0.0304(11) Uiso 0.75 1 d P A 1
H50 H 0.0109 0.1110 -0.0810 0.046 Uiso 0.75 1 calc PR A 1
O50B O -0.0493(11) 0.0942(8) -0.0329(12) 0.054(5) Uiso 0.25 1 d P A 2
H50C H -0.0291 0.0769 0.0146 0.082 Uiso 0.25 1 calc PRD A 2
C56 C -0.0627(4) 0.0656(3) -0.0922(5) 0.061(2) Uiso 1 1 d . . .
H56A H -0.0798 0.0549 -0.0529 0.074 Uiso 0.75 1 calc PR A 1
H56B H -0.0419 0.0341 -0.1041 0.074 Uiso 0.75 1 calc PR A 1
H56C H -0.0749 0.0300 -0.0810 0.074 Uiso 0.25 1 calc PR A 2
H56D H -0.0181 0.0627 -0.0962 0.074 Uiso 0.25 1 calc PR A 2
C57 C -0.1270(7) 0.0865(5) -0.1767(8) 0.112(4) Uiso 1 1 d . A .
H57A H -0.1475 0.1177 -0.1646 0.169 Uiso 1 1 calc R . .
H57B H -0.1660 0.0594 -0.2055 0.169 Uiso 1 1 calc R . .
H57C H -0.1101 0.0964 -0.2159 0.169 Uiso 1 1 calc R . .
O51 O 0.3790(3) 0.3011(2) 0.0861(4) 0.0540(15) Uani 0.50 1 d P B 1
H51 H 0.4235 0.3091 0.1043 0.081 Uiso 0.50 1 calc PR B 1
C58 C 0.3490(6) 0.3388(3) 0.1270(5) 0.113(3) Uani 0.50 1 d P B 1
H58A H 0.3400 0.3192 0.1673 0.170 Uiso 0.50 1 calc PR B 1
H58B H 0.3020 0.3548 0.0797 0.170 Uiso 0.50 1 calc PR B 1
H58C H 0.3861 0.3667 0.1601 0.170 Uiso 0.50 1 calc PR B 1
C58B C 0.3790(3) 0.3011(2) 0.0861(4) 0.0540(15) Uani 0.50 1 d P C 2
H58D H 0.3921 0.3213 0.0498 0.081 Uiso 0.50 1 calc PR C 2
H58E H 0.3402 0.2751 0.0489 0.081 Uiso 0.50 1 calc PR C 2
H58F H 0.4236 0.2829 0.1336 0.081 Uiso 0.50 1 calc PR C 2
O51B O 0.3490(6) 0.3388(3) 0.1270(5) 0.113(3) Uani 0.50 1 d P C 2
H51D H 0.3182 0.3599 0.0880 0.170 Uiso 0.50 1 calc PR C 2
Cl2 Cl 0.4304(2) 0.41572(18) 0.1544(2) 0.0712(12) Uani 0.50 1 d P . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C2 C1 C6 116.8(5) . . ?
C2 C1 C28 122.5(5) . . ?
C6 C1 C28 120.7(4) . . ?
C1 C2 C3 123.5(5) . . ?
C2 C3 C4 117.0(5) . . ?
C2 C3 C7 121.8(5) . . ?
C4 C3 C7 121.1(5) . . ?
C5 C4 C3 121.3(5) . . ?
C5 C4 O4 118.8(5) . . ?
C3 C4 O4 119.9(5) . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 O5 122.8(5) . . ?
C6 C5 O5 117.0(5) . . ?
O6 C6 C5 120.1(5) . . ?
O6 C6 C1 118.8(5) . . ?
C5 C6 C1 121.0(5) . . ?
C3 C7 C8 110.5(4) . . ?
C3 C7 C29 112.6(4) . . ?
C8 C7 C29 112.9(4) . . ?
C9 C8 C13 117.6(5) . . ?
C9 C8 C7 121.5(4) . . ?
C13 C8 C7 120.9(5) . . ?
C10 C9 C8 123.6(5) . . ?
C9 C10 C11 117.2(5) . . ?
C9 C10 C14 121.7(4) . . ?
C11 C10 C14 121.0(5) . . ?
C12 C11 O11 116.1(4) . . ?
C12 C11 C10 120.3(5) . . ?
O11 C11 C10 123.6(5) . . ?
C11 C12 C13 121.4(4) . . ?
C11 C12 O12 117.4(4) . . ?
C13 C12 O12 121.2(5) . . ?
O13 C13 C12 115.9(4) . . ?
O13 C13 C8 124.4(5) . . ?
C12 C13 C8 119.7(5) . . ?
C30 C14 C10 113.2(5) . . ?
C30 C14 C15 113.0(4) . . ?
C10 C14 C15 111.2(4) . . ?
C20 C15 C16 117.5(5) . . ?
C20 C15 C14 121.0(4) . . ?
C16 C15 C14 121.5(5) . . ?
C17 C16 C15 123.2(5) . . ?
C16 C17 C18 117.5(5) . . ?
C16 C17 C21 121.4(4) . . ?
C18 C17 C21 121.2(4) . . ?
C19 C18 O18 115.8(5) . . ?
C19 C18 C17 121.3(5) . . ?
O18 C18 C17 122.9(5) . . ?
C18 C19 O19 124.0(5) . . ?
C18 C19 C20 119.5(5) . . ?
O19 C19 C20 116.5(5) . . ?
O20 C20 C15 118.7(5) . . ?
O20 C20 C19 120.3(5) . . ?
C15 C20 C19 121.0(5) . . ?
C22 C21 C31 112.5(4) . . ?
C22 C21 C17 110.4(4) . . ?
C31 C21 C17 112.3(4) . . ?
C23 C22 C27 117.3(5) . . ?
C23 C22 C21 123.1(4) . . ?
C27 C22 C21 119.6(5) . . ?
C22 C23 C24 123.8(4) . . ?
C25 C24 C23 117.0(5) . . ?
C25 C24 C28 120.9(5) . . ?
C23 C24 C28 122.2(4) . . ?
O25 C25 C26 115.7(5) . . ?
O25 C25 C24 123.3(5) . . ?
C26 C25 C24 121.0(5) . . ?
O26 C26 C25 122.7(5) . . ?
O26 C26 C27 117.1(5) . . ?
C25 C26 C27 120.2(4) . . ?
O27 C27 C26 120.4(4) . . ?
O27 C27 C22 118.8(5) . . ?
C26 C27 C22 120.8(5) . . ?
C1 C28 C24 110.5(4) . . ?
C1 C28 C32 113.4(4) . . ?
C24 C28 C32 112.3(5) . . ?
C52 N50 C50 113.1(4) . . ?
C52 N50 C54 110.2(4) . . ?
C50 N50 C54 113.6(4) . . ?
N50 C50 C51 112.8(4) . . ?
N50 C52 C53 112.8(5) . . ?
C55 C54 N50 112.8(5) . . ?
O50B C56 O50 50.8(10) . . ?
O50B C56 C57 109.8(12) . . ?
O50 C56 C57 109.7(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.388(7) . ?
C1 C6 1.400(8) . ?
C1 C28 1.521(7) . ?
C2 C3 1.395(7) . ?
C3 C4 1.396(7) . ?
C3 C7 1.525(7) . ?
C4 C5 1.367(8) . ?
C4 O4 1.397(7) . ?
C5 C6 1.388(8) . ?
C5 O5 1.391(6) . ?
C6 O6 1.381(6) . ?
C7 C8 1.528(7) . ?
C7 C29 1.535(7) . ?
C8 C9 1.389(7) . ?
C8 C13 1.400(7) . ?
C9 C10 1.388(7) . ?
C10 C11 1.397(7) . ?
C10 C14 1.530(7) . ?
C11 C12 1.381(7) . ?
C11 O11 1.384(6) . ?
C12 C13 1.383(7) . ?
C12 O12 1.391(6) . ?
C13 O13 1.377(6) . ?
C14 C30 1.518(7) . ?
C14 C15 1.532(7) . ?
C15 C20 1.390(7) . ?
C15 C16 1.393(7) . ?
C16 C17 1.389(7) . ?
C17 C18 1.401(7) . ?
C17 C21 1.534(7) . ?
C18 C19 1.376(7) . ?
C18 O18 1.386(6) . ?
C19 O19 1.376(6) . ?
C19 C20 1.406(8) . ?
C20 O20 1.378(6) . ?
C21 C22 1.527(7) . ?
C21 C31 1.534(7) . ?
C22 C23 1.380(7) . ?
C22 C27 1.398(7) . ?
C23 C24 1.399(7) . ?
C24 C25 1.393(7) . ?
C24 C28 1.525(8) . ?
C25 O25 1.374(6) . ?
C25 C26 1.386(8) . ?
C26 O26 1.374(6) . ?
C26 C27 1.387(7) . ?
C27 O27 1.381(6) . ?
C28 C32 1.534(7) . ?
N50 C52 1.498(7) . ?
N50 C50 1.502(6) . ?
N50 C54 1.506(7) . ?
C50 C51 1.515(8) . ?
C52 C53 1.512(9) . ?
C54 C55 1.505(9) . ?
O50 C56 1.405(9) . ?
O50B C56 1.186(19) . ?
C56 C57 1.483(13) . ?
O51 C58 1.538(11) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 Cl2 0.84 2.49 3.272(7) 155.5 4_545
O5 H5 Cl1 0.84 2.36 3.195(4) 174.3 7_556
O6 H6 O50 0.84 1.95 2.683(6) 146.1 .
O6 H6 O5 0.84 2.25 2.711(6) 114.6 .
O6 H6 O50B 0.84 2.36 3.19(2) 167.6 .
O11 H11 O20 0.84 1.82 2.658(5) 171.7 .
O12 H12 O19 0.84 2.14 2.858(5) 142.8 7_556
O12 H12 O13 0.84 2.26 2.706(6) 113.6 .
O13 H13 O4 0.84 1.91 2.748(6) 175.8 .
O18 H18 O27 0.84 1.87 2.705(6) 177.5 .
O19 H19 O50B 0.84 1.80 2.401(19) 127.2 8_556
O19 H19 O50 0.84 1.94 2.726(6) 155.5 8_556
O19 H19 O18 0.84 2.33 2.751(6) 111.2 .
O20 H20 Cl1 0.84 2.39 3.080(4) 140.1 .
O25 H25 O6 0.84 1.85 2.684(6) 173.5 .
O26 H26 O51 0.84 2.17 2.975(7) 159.6 7
O26 H26 O25 0.84 2.29 2.726(6) 113.0 .
O26 H26 O51B 0.84 2.52 3.310(9) 156.7 7
O27 H27 O51 0.84 2.00 2.675(6) 137.3 .
O27 H27 O51B 0.84 2.21 2.934(8) 144.9 .
O27 H27 O26 0.84 2.26 2.713(5) 113.9 .
N50 H50X O11 0.93 2.01 2.846(5) 148.4 7_556
N50 H50X O12 0.93 2.25 2.986(6) 135.6 7_556
O50 H50 Cl2 0.84 2.35 3.115(7) 151.6 7
O50B H50C O5 0.84 1.95 2.724(19) 152.9 .
O51 H51 O18 0.84 2.27 2.999(7) 144.7 2_655
Cl2 H58C O51 1.60 2.08 3.111(8) 115.0 .
O51B H51D O25 0.84 2.16 2.838(8) 137.8 7
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.0(8) . . . . ?
C28 C1 C2 C3 -178.9(5) . . . . ?
C1 C2 C3 C4 -0.7(8) . . . . ?
C1 C2 C3 C7 180.0(5) . . . . ?
C2 C3 C4 C5 -1.9(8) . . . . ?
C7 C3 C4 C5 177.5(5) . . . . ?
C2 C3 C4 O4 177.9(5) . . . . ?
C7 C3 C4 O4 -2.7(8) . . . . ?
C3 C4 C5 C6 4.0(9) . . . . ?
O4 C4 C5 C6 -175.8(5) . . . . ?
C3 C4 C5 O5 179.9(5) . . . . ?
O4 C4 C5 O5 0.1(9) . . . . ?
C4 C5 C6 O6 175.6(5) . . . . ?
O5 C5 C6 O6 -0.5(8) . . . . ?
C4 C5 C6 C1 -3.6(8) . . . . ?
O5 C5 C6 C1 -179.7(5) . . . . ?
C2 C1 C6 O6 -178.1(5) . . . . ?
C28 C1 C6 O6 1.9(8) . . . . ?
C2 C1 C6 C5 1.1(8) . . . . ?
C28 C1 C6 C5 -179.0(5) . . . . ?
C2 C3 C7 C8 89.4(6) . . . . ?
C4 C3 C7 C8 -90.0(6) . . . . ?
C2 C3 C7 C29 -37.9(7) . . . . ?
C4 C3 C7 C29 142.8(5) . . . . ?
C3 C7 C8 C9 -87.0(5) . . . . ?
C29 C7 C8 C9 40.1(6) . . . . ?
C3 C7 C8 C13 92.3(5) . . . . ?
C29 C7 C8 C13 -140.6(5) . . . . ?
C13 C8 C9 C10 2.3(7) . . . . ?
C7 C8 C9 C10 -178.4(4) . . . . ?
C8 C9 C10 C11 -0.6(7) . . . . ?
C8 C9 C10 C14 -177.2(4) . . . . ?
C9 C10 C11 C12 -2.0(7) . . . . ?
C14 C10 C11 C12 174.6(4) . . . . ?
C9 C10 C11 O11 178.2(4) . . . . ?
C14 C10 C11 O11 -5.2(7) . . . . ?
O11 C11 C12 C13 -177.3(5) . . . . ?
C10 C11 C12 C13 2.8(8) . . . . ?
O11 C11 C12 O12 2.5(7) . . . . ?
C10 C11 C12 O12 -177.3(4) . . . . ?
C11 C12 C13 O13 178.7(5) . . . . ?
O12 C12 C13 O13 -1.1(7) . . . . ?
C11 C12 C13 C8 -1.1(7) . . . . ?
O12 C12 C13 C8 179.1(4) . . . . ?
C9 C8 C13 O13 178.8(4) . . . . ?
C7 C8 C13 O13 -0.5(7) . . . . ?
C9 C8 C13 C12 -1.4(7) . . . . ?
C7 C8 C13 C12 179.2(4) . . . . ?
C9 C10 C14 C30 -41.7(6) . . . . ?
C11 C10 C14 C30 141.9(5) . . . . ?
C9 C10 C14 C15 86.7(6) . . . . ?
C11 C10 C14 C15 -89.7(5) . . . . ?
C30 C14 C15 C20 -143.2(5) . . . . ?
C10 C14 C15 C20 88.2(5) . . . . ?
C30 C14 C15 C16 36.3(7) . . . . ?
C10 C14 C15 C16 -92.3(5) . . . . ?
C20 C15 C16 C17 1.7(7) . . . . ?
C14 C15 C16 C17 -177.8(4) . . . . ?
C15 C16 C17 C18 -1.7(7) . . . . ?
C15 C16 C17 C21 179.2(4) . . . . ?
C16 C17 C18 C19 0.0(7) . . . . ?
C21 C17 C18 C19 179.1(5) . . . . ?
C16 C17 C18 O18 179.9(4) . . . . ?
C21 C17 C18 O18 -1.0(7) . . . . ?
O18 C18 C19 O19 1.7(7) . . . . ?
C17 C18 C19 O19 -178.4(5) . . . . ?
O18 C18 C19 C20 -178.3(4) . . . . ?
C17 C18 C19 C20 1.6(7) . . . . ?
C16 C15 C20 O20 -179.7(4) . . . . ?
C14 C15 C20 O20 -0.1(7) . . . . ?
C16 C15 C20 C19 0.0(7) . . . . ?
C14 C15 C20 C19 179.5(4) . . . . ?
C18 C19 C20 O20 178.1(5) . . . . ?
O19 C19 C20 O20 -2.0(7) . . . . ?
C18 C19 C20 C15 -1.6(7) . . . . ?
O19 C19 C20 C15 178.4(4) . . . . ?
C16 C17 C21 C22 86.9(5) . . . . ?
C18 C17 C21 C22 -92.2(6) . . . . ?
C16 C17 C21 C31 -39.6(7) . . . . ?
C18 C17 C21 C31 141.3(5) . . . . ?
C31 C21 C22 C23 40.1(6) . . . . ?
C17 C21 C22 C23 -86.2(6) . . . . ?
C31 C21 C22 C27 -140.2(5) . . . . ?
C17 C21 C22 C27 93.5(5) . . . . ?
C27 C22 C23 C24 1.6(7) . . . . ?
C21 C22 C23 C24 -178.6(5) . . . . ?
C22 C23 C24 C25 -0.2(7) . . . . ?
C22 C23 C24 C28 -178.3(5) . . . . ?
C23 C24 C25 O25 178.0(5) . . . . ?
C28 C24 C25 O25 -3.9(7) . . . . ?
C23 C24 C25 C26 -0.6(7) . . . . ?
C28 C24 C25 C26 177.5(5) . . . . ?
O25 C25 C26 O26 3.3(7) . . . . ?
C24 C25 C26 O26 -178.0(5) . . . . ?
O25 C25 C26 C27 -178.8(4) . . . . ?
C24 C25 C26 C27 -0.1(7) . . . . ?
O26 C26 C27 O27 0.1(7) . . . . ?
C25 C26 C27 O27 -177.9(4) . . . . ?
O26 C26 C27 C22 179.7(4) . . . . ?
C25 C26 C27 C22 1.6(7) . . . . ?
C23 C22 C27 O27 177.2(4) . . . . ?
C21 C22 C27 O27 -2.5(7) . . . . ?
C23 C22 C27 C26 -2.3(7) . . . . ?
C21 C22 C27 C26 177.9(4) . . . . ?
C2 C1 C28 C24 -92.0(6) . . . . ?
C6 C1 C28 C24 88.1(6) . . . . ?
C2 C1 C28 C32 35.1(7) . . . . ?
C6 C1 C28 C32 -144.8(5) . . . . ?
C25 C24 C28 C1 -92.0(5) . . . . ?
C23 C24 C28 C1 86.0(6) . . . . ?
C25 C24 C28 C32 140.4(5) . . . . ?
C23 C24 C28 C32 -41.6(6) . . . . ?
C52 N50 C50 C51 -63.4(6) . . . . ?
C54 N50 C50 C51 63.3(6) . . . . ?
C50 N50 C52 C53 -56.5(6) . . . . ?
C54 N50 C52 C53 175.1(5) . . . . ?
C52 N50 C54 C55 -170.5(6) . . . . ?
C50 N50 C54 C55 61.3(7) . . . . ?
