#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302722.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_4302722
loop_
_publ_author_name
'Dirk Burdinski'
'Jeroen A. Pikkemaat'
'Johan Lub'
'Peter de Peinder'
'Lidia Nieto Garrido'
'Thomas Weyhermüller'
_publ_section_title
;
Lanthanide Complexes of Triethylenetetramine Tetra-, Penta-, and
Hexaacetamide Ligands as Paramagnetic Chemical Exchange-Dependent
Saturation Transfer Contrast Agents for Magnetic Resonance Imaging: Nona-
versus Decadentate Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6692
_journal_page_last               6712
_journal_paper_doi               10.1021/ic900652y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '[C23 H39 N9 O5 Tm]3+, 3 (Cl O4)-, 4 (H2 O)'
_chemical_formula_sum            'C23 H47 Cl3 N9 O21 Tm'
_chemical_formula_weight         1060.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.456(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8565(5)
_cell_length_b                   18.8304(6)
_cell_length_c                   13.0221(4)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      2.51
_cell_volume                     3845.9(2)
_computing_cell_refinement       'Bruker SAINT 7.34A'
_computing_data_collection       'Bruker SAINT 7.34A'
_computing_data_reduction        'Bruker SAINT 7.34A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'rotating anode, 50 kV, 40 mA, Multi-Layer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            441190
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_T_max  0.9028
_exptl_absorpt_correction_T_min  0.8384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         16916
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0200P)²+6.2606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                15348
_reflns_number_total             16916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900652y_si_002_1.cif
_cod_data_source_block           '[(1bttpam)Tm](ClO4)3*4H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302722
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Tm1 Tm 0.736062(3) 0.975691(3) 1.168867(4) 0.00915(1) Uani 1 1 d . . .
N1 N 0.64216(6) 0.94705(6) 1.30940(8) 0.01104(18) Uani 1 1 d . . .
C2 C 0.65831(8) 1.00498(7) 1.38762(10) 0.0133(2) Uani 1 1 d . . .
H2A H 0.7185 1.0033 1.4212 0.016 Uiso 1 1 calc R . .
H2B H 0.6214 0.9984 1.4420 0.016 Uiso 1 1 calc R . .
C3 C 0.63982(8) 1.07644(7) 1.33531(10) 0.0141(2) Uani 1 1 d . . .
H3A H 0.5800 1.0773 1.3005 0.017 Uiso 1 1 calc R . .
H3B H 0.6466 1.1143 1.3887 0.017 Uiso 1 1 calc R . .
N4 N 0.69784(7) 1.09128(6) 1.25719(8) 0.01183(18) Uani 1 1 d . . .
C5 C 0.77560(8) 1.12729(7) 1.31169(10) 0.0139(2) Uani 1 1 d . . .
H5A H 0.7954 1.1020 1.3775 0.017 Uiso 1 1 calc R . .
H5B H 0.7608 1.1765 1.3291 0.017 Uiso 1 1 calc R . .
C6 C 0.84735(8) 1.12927(6) 1.24660(10) 0.0133(2) Uani 1 1 d . . .
H6A H 0.8277 1.1531 1.1796 0.016 Uiso 1 1 calc R . .
H6B H 0.8961 1.1565 1.2834 0.016 Uiso 1 1 calc R . .
N7 N 0.87474(7) 1.05549(6) 1.22748(8) 0.01130(18) Uani 1 1 d . . .
C8 C 0.92701(8) 1.05320(7) 1.14203(10) 0.0124(2) Uani 1 1 d . . .
H8A H 0.9812 1.0791 1.1629 0.015 Uiso 1 1 calc R . .
H8B H 0.8960 1.0766 1.0796 0.015 Uiso 1 1 calc R . .
C9 C 0.94568(7) 0.97634(7) 1.11719(9) 0.0120(2) Uani 1 1 d . . .
H9A H 0.9851 0.9750 1.0649 0.014 Uiso 1 1 calc R . .
H9B H 0.9741 0.9525 1.1808 0.014 Uiso 1 1 calc R . .
N10 N 0.86633(6) 0.93760(6) 1.07675(8) 0.01069(17) Uani 1 1 d . . .
C11 C 0.67029(8) 0.87744(7) 1.35434(9) 0.0123(2) Uani 1 1 d . . .
H11A H 0.6249 0.8562 1.3893 0.015 Uiso 1 1 calc R . .
H11B H 0.7220 0.8833 1.4063 0.015 Uiso 1 1 calc R . .
C12 C 0.68934(7) 0.82951(7) 1.26725(10) 0.0122(2) Uani 1 1 d . . .
O13 O 0.70204(6) 0.85629(5) 1.18222(7) 0.01348(17) Uani 1 1 d . . .
N14 N 0.69346(9) 0.76080(6) 1.28521(10) 0.0191(2) Uani 1 1 d . . .
H14A H 0.7055 0.7315 1.2368 0.023 Uiso 1 1 calc R . .
H14B H 0.6842 0.7441 1.3457 0.023 Uiso 1 1 calc R . .
C21 C 0.55052(8) 0.94135(7) 1.26647(10) 0.0135(2) Uani 1 1 d . . .
H21A H 0.5163 0.9650 1.3143 0.016 Uiso 1 1 calc R . .
H21B H 0.5341 0.8906 1.2621 0.016 Uiso 1 1 calc R . .
C22 C 0.53018(7) 0.97442(7) 1.16055(10) 0.0119(2) Uani 1 1 d . . .
O23 O 0.58902(6) 0.99298(5) 1.11142(7) 0.01347(17) Uani 1 1 d . . .
N24 N 0.44885(7) 0.98062(7) 1.12172(10) 0.0180(2) Uani 1 1 d . . .
H24A H 0.4341 0.9983 1.0591 0.022 Uiso 1 1 calc R . .
H24B H 0.4093 0.9670 1.1584 0.022 Uiso 1 1 calc R . .
C31 C 0.65495(8) 1.13894(7) 1.17495(10) 0.0144(2) Uani 1 1 d . . .
H31A H 0.6664 1.1889 1.1959 0.017 Uiso 1 1 calc R . .
H31B H 0.5926 1.1312 1.1672 0.017 Uiso 1 1 calc R . .
C32 C 0.68539(8) 1.12587(7) 1.07139(10) 0.0146(2) Uani 1 1 d . . .
O33 O 0.72805(6) 1.07146(5) 1.05735(7) 0.01362(17) Uani 1 1 d . . .
N34 N 0.66264(10) 1.17309(7) 0.99801(11) 0.0263(3) Uani 1 1 d . . .
H34A H 0.6773 1.1672 0.9360 0.032 Uiso 1 1 calc R . .
H34B H 0.6327 1.2105 1.0110 0.032 Uiso 1 1 calc R . .
C41 C 0.92647(8) 1.02769(7) 1.32284(10) 0.0127(2) Uani 1 1 d . . .
H41A H 0.9177 1.0578 1.3827 0.015 Uiso 1 1 calc R . .
H41B H 0.9876 1.0297 1.3153 0.015 Uiso 1 1 calc R . .
C42 C 0.90227(8) 0.95246(7) 1.34312(9) 0.0118(2) Uani 1 1 d . . .
O43 O 0.82922(6) 0.93051(5) 1.30669(7) 0.01382(17) Uani 1 1 d . . .
N44 N 0.95886(7) 0.91298(6) 1.40148(9) 0.0158(2) Uani 1 1 d . . .
H44A H 0.9462 0.8691 1.4165 0.019 Uiso 1 1 calc R . .
H44B H 1.0094 0.9305 1.4254 0.019 Uiso 1 1 calc R . .
C51 C 0.84077(8) 0.95554(7) 0.96625(9) 0.0114(2) Uani 1 1 d . . .
H51A H 0.8786 0.9312 0.9235 0.014 Uiso 1 1 calc R . .
H51B H 0.8458 1.0074 0.9561 0.014 Uiso 1 1 calc R . .
C52 C 0.74994(8) 0.93239(6) 0.93349(9) 0.0116(2) Uani 1 1 d . . .
O53 O 0.69987(6) 0.92990(5) 0.99987(7) 0.01294(16) Uani 1 1 d . . .
N54 N 0.72608(8) 0.91610(7) 0.83522(9) 0.0172(2) Uani 1 1 d . . .
H54A H 0.6732 0.9028 0.8137 0.021 Uiso 1 1 calc R . .
H54B H 0.7630 0.9185 0.7910 0.021 Uiso 1 1 calc R . .
C61 C 0.87881(8) 0.85864(6) 1.08976(10) 0.0124(2) Uani 1 1 d . . .
H61A H 0.8239 0.8350 1.0646 0.015 Uiso 1 1 calc R . .
H61B H 0.8928 0.8483 1.1649 0.015 Uiso 1 1 calc R . .
C62 C 0.94707(8) 0.82542(7) 1.03488(11) 0.0149(2) Uani 1 1 d . . .
C63 C 1.03131(9) 0.82007(8) 1.08329(13) 0.0205(3) Uani 1 1 d . . .
H63 H 1.0472 0.8399 1.1505 0.025 Uiso 1 1 calc R . .
C64 C 1.09256(10) 0.78589(9) 1.03401(16) 0.0287(3) Uani 1 1 d . . .
H64 H 1.1497 0.7823 1.0680 0.034 Uiso 1 1 calc R . .
C65 C 1.07034(11) 0.75722(9) 0.93556(16) 0.0319(4) Uani 1 1 d . . .
H65 H 1.1120 0.7337 0.9024 0.038 Uiso 1 1 calc R . .
C66 C 0.98727(12) 0.76300(8) 0.88595(14) 0.0277(3) Uani 1 1 d . . .
H66 H 0.9721 0.7442 0.8180 0.033 Uiso 1 1 calc R . .
C67 C 0.92572(10) 0.79636(7) 0.93558(12) 0.0196(3) Uani 1 1 d . . .
H67 H 0.8686 0.7994 0.9015 0.023 Uiso 1 1 calc R . .
Cl70 Cl 0.871084(19) 0.849815(17) 0.63642(2) 0.01459(5) Uani 1 1 d . . .
O711 O 0.95969(6) 0.83524(6) 0.63517(10) 0.0218(2) Uani 1 1 d . . .
O712 O 0.82969(9) 0.79087(7) 0.67593(14) 0.0388(3) Uani 1 1 d . . .
O713 O 0.86373(9) 0.90999(7) 0.70314(15) 0.0464(4) Uani 1 1 d . . .
O714 O 0.83247(10) 0.86683(16) 0.53451(12) 0.0779(8) Uani 1 1 d . . .
Cl80 Cl 0.75591(5) 1.12053(4) 0.73808(6) 0.02127(13) Uani 0.5402(1) 1 d PD A 1
O811 O 0.82709(18) 1.07455(16) 0.7730(2) 0.0374(6) Uani 0.5402(1) 1 d PD A 1
O812 O 0.7315(2) 1.10898(16) 0.62645(19) 0.0364(6) Uani 0.5402(1) 1 d PD A 1
O813 O 0.7781(2) 1.19413(12) 0.7559(2) 0.0373(6) Uani 0.5402(1) 1 d PD A 1
O814 O 0.6861(2) 1.1031(2) 0.7918(3) 0.0468(5) Uani 0.5402(1) 1 d PD A 1
Cl90 Cl 0.41626(5) 1.39410(5) 0.88050(6) 0.02039(11) Uani 0.5183(11) 1 d PD B 1
O911 O 0.44352(16) 1.36773(15) 0.78565(18) 0.0208(4) Uani 0.5183(11) 1 d PD B 1
O912 O 0.34228(15) 1.35590(18) 0.8996(2) 0.0360(6) Uani 0.5183(11) 1 d PD B 1
O913 O 0.48373(14) 1.39313(14) 0.96609(18) 0.0250(4) Uani 0.5183(11) 1 d PD B 1
O914 O 0.3922(2) 1.46915(13) 0.8620(2) 0.0355(5) Uani 0.5183(11) 1 d PD B 1
O200 O 0.6455(2) 0.77661(16) 0.9868(2) 0.0418(6) Uani 0.5183(11) 1 d P B 1
O400 O 0.58615(17) 1.29784(14) 1.0822(2) 0.0294(4) Uani 0.5183(11) 1 d P B 1
Cl81 Cl 0.73107(12) 1.12003(10) 0.7281(2) 0.0213(2) Uani 0.2827(2) 1 d PD C 2
O821 O 0.8029(3) 1.0801(3) 0.7783(5) 0.0374(6) Uani 0.2827(2) 1 d PD C 2
O822 O 0.7434(4) 1.1361(3) 0.6236(3) 0.0364(6) Uani 0.2827(2) 1 d PD C 2
O823 O 0.7235(4) 1.1856(2) 0.7840(4) 0.0373(6) Uani 0.2827(2) 1 d PD C 2
O824 O 0.6544(3) 1.0796(3) 0.7268(4) 0.0468(5) Uani 0.2827(2) 1 d PD C 2
Cl91 Cl 0.42299(6) 1.38149(7) 0.88450(8) 0.02039(11) Uani 0.4817(11) 1 d PD B 2
O921 O 0.43900(19) 1.38475(18) 0.7771(2) 0.0208(4) Uani 0.4817(11) 1 d PD B 2
O922 O 0.33452(16) 1.3951(2) 0.8870(2) 0.0360(6) Uani 0.4817(11) 1 d PD B 2
O923 O 0.47628(16) 1.43048(15) 0.94689(19) 0.0250(4) Uani 0.4817(11) 1 d PD B 2
O924 O 0.4448(2) 1.30949(14) 0.9222(2) 0.0355(5) Uani 0.4817(11) 1 d PD B 2
O205 O 0.6202(3) 0.79723(18) 0.9572(3) 0.0418(6) Uani 0.4817(11) 1 d P B 2
O405 O 0.53271(18) 1.26265(15) 1.0776(2) 0.0294(4) Uani 0.4817(11) 1 d P B 2
Cl82 Cl 0.72739(18) 1.12667(14) 0.7135(2) 0.02127(13) Uani 0.1771(2) 1 d PD D 3
O831 O 0.8109(4) 1.0920(4) 0.7209(7) 0.0374(6) Uani 0.1771(2) 1 d PD D 3
O832 O 0.6775(5) 1.1109(4) 0.6177(4) 0.0364(6) Uani 0.1771(2) 1 d PD D 3
O833 O 0.7441(6) 1.2013(3) 0.7288(7) 0.0373(6) Uani 0.1771(2) 1 d PD D 3
O834 O 0.6886(6) 1.1008(6) 0.7994(6) 0.0468(5) Uani 0.1771(2) 1 d PD D 3
O100 O 0.86787(7) 1.03560(6) 0.54998(9) 0.0205(2) Uani 1 1 d D . .
H101 H 0.8590(14) 0.9961(5) 0.5704(16) 0.027 Uiso 1 1 d D . .
H102 H 0.8393(9) 1.0608(9) 0.5816(14) 0.027 Uiso 1 1 d D . .
O300 O 0.53630(12) 1.22045(9) 0.79699(14) 0.0464(4) Uani 1 1 d D . .
H301 H 0.532(2) 1.2210(18) 0.7336(7) 0.060 Uiso 1 1 d D . .
H302 H 0.5099(13) 1.2564(8) 0.807(2) 0.060 Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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
O33 Tm1 O43 138.24(3) . . ?
O33 Tm1 O13 144.21(3) . . ?
O43 Tm1 O13 73.43(3) . . ?
O33 Tm1 O53 73.42(3) . . ?
O43 Tm1 O53 129.10(3) . . ?
O13 Tm1 O53 71.84(3) . . ?
O33 Tm1 O23 74.50(3) . . ?
O43 Tm1 O23 141.62(3) . . ?
O13 Tm1 O23 85.87(3) . . ?
O53 Tm1 O23 70.20(3) . . ?
O33 Tm1 N4 68.02(3) . . ?
O43 Tm1 N4 97.46(3) . . ?
O13 Tm1 N4 135.36(3) . . ?
O53 Tm1 N4 133.30(3) . . ?
O23 Tm1 N4 74.87(3) . . ?
O33 Tm1 N1 128.73(3) . . ?
O43 Tm1 N1 75.05(3) . . ?
O13 Tm1 N1 65.19(3) . . ?
O53 Tm1 N1 119.97(3) . . ?
O23 Tm1 N1 66.93(3) . . ?
N4 Tm1 N1 70.23(3) . . ?
O33 Tm1 N10 84.29(3) . . ?
O43 Tm1 N10 78.42(3) . . ?
O13 Tm1 N10 88.67(3) . . ?
O53 Tm1 N10 64.83(3) . . ?
O23 Tm1 N10 134.09(3) . . ?
N4 Tm1 N10 133.22(3) . . ?
N1 Tm1 N10 146.97(3) . . ?
O33 Tm1 N7 73.02(3) . . ?
O43 Tm1 N7 65.26(3) . . ?
O13 Tm1 N7 135.29(3) . . ?
O53 Tm1 N7 123.26(3) . . ?
O23 Tm1 N7 137.96(3) . . ?
N4 Tm1 N7 68.66(3) . . ?
N1 Tm1 N7 116.75(3) . . ?
N10 Tm1 N7 67.49(3) . . ?
C11 N1 C21 107.89(10) . . ?
C11 N1 C2 111.56(10) . . ?
C21 N1 C2 111.81(10) . . ?
C11 N1 Tm1 107.12(7) . . ?
C21 N1 Tm1 112.56(7) . . ?
C2 N1 Tm1 105.84(7) . . ?
N1 C2 C3 109.89(10) . . ?
N4 C3 C2 111.95(10) . . ?
C31 N4 C5 109.12(10) . . ?
C31 N4 C3 109.99(10) . . ?
C5 N4 C3 108.03(10) . . ?
C31 N4 Tm1 107.57(7) . . ?
C5 N4 Tm1 111.36(7) . . ?
C3 N4 Tm1 110.77(7) . . ?
N4 C5 C6 112.38(10) . . ?
N7 C6 C5 109.41(10) . . ?
C41 N7 C8 108.51(10) . . ?
C41 N7 C6 109.23(10) . . ?
C8 N7 C6 111.23(10) . . ?
C41 N7 Tm1 111.78(7) . . ?
C8 N7 Tm1 107.20(7) . . ?
C6 N7 Tm1 108.89(7) . . ?
N7 C8 C9 109.57(10) . . ?
N10 C9 C8 111.23(10) . . ?
C51 N10 C9 109.32(9) . . ?
C51 N10 C61 110.39(10) . . ?
C9 N10 C61 110.80(9) . . ?
C51 N10 Tm1 105.08(7) . . ?
C9 N10 Tm1 112.67(7) . . ?
C61 N10 Tm1 108.43(7) . . ?
N1 C11 C12 108.30(10) . . ?
O13 C12 N14 122.70(12) . . ?
O13 C12 C11 119.68(11) . . ?
N14 C12 C11 117.61(11) . . ?
C12 O13 Tm1 121.45(8) . . ?
N1 C21 C22 112.45(10) . . ?
O23 C22 N24 122.53(12) . . ?
O23 C22 C21 120.46(11) . . ?
N24 C22 C21 116.97(11) . . ?
C22 O23 Tm1 124.93(8) . . ?
N4 C31 C32 111.81(10) . . ?
O33 C32 N34 122.78(13) . . ?
O33 C32 C31 120.67(11) . . ?
N34 C32 C31 116.52(12) . . ?
C32 O33 Tm1 121.81(9) . . ?
N7 C41 C42 110.92(10) . . ?
O43 C42 N44 122.99(12) . . ?
O43 C42 C41 119.33(11) . . ?
N44 C42 C41 117.66(11) . . ?
C42 O43 Tm1 128.37(8) . . ?
N10 C51 C52 108.92(10) . . ?
O53 C52 N54 122.64(11) . . ?
O53 C52 C51 119.37(11) . . ?
N54 C52 C51 117.99(11) . . ?
C52 O53 Tm1 122.48(8) . . ?
N10 C61 C62 116.43(10) . . ?
C63 C62 C67 118.37(13) . . ?
C63 C62 C61 121.28(13) . . ?
C67 C62 C61 120.28(12) . . ?
C62 C63 C64 120.66(16) . . ?
C65 C64 C63 120.27(15) . . ?
C66 C65 C64 119.71(15) . . ?
C65 C66 C67 120.10(16) . . ?
C66 C67 C62 120.86(15) . . ?
O714 Cl70 O712 110.91(13) . . ?
O714 Cl70 O711 108.81(8) . . ?
O712 Cl70 O711 111.06(8) . . ?
O714 Cl70 O713 108.96(14) . . ?
O712 Cl70 O713 108.19(9) . . ?
O711 Cl70 O713 108.86(8) . . ?
O814 Cl80 O813 109.2(2) . . ?
O814 Cl80 O811 109.5(2) . . ?
O813 Cl80 O811 111.46(18) . . ?
O814 Cl80 O812 109.88(19) . . ?
O813 Cl80 O812 109.01(18) . . ?
O811 Cl80 O812 107.73(18) . . ?
O913 Cl90 O912 113.45(16) . . ?
O913 Cl90 O911 112.12(15) . . ?
O912 Cl90 O911 109.27(17) . . ?
O913 Cl90 O914 106.64(17) . . ?
O912 Cl90 O914 108.15(19) . . ?
O911 Cl90 O914 106.89(17) . . ?
O824 Cl81 O822 109.6(3) . . ?
O824 Cl81 O821 110.0(4) . . ?
O822 Cl81 O821 109.4(4) . . ?
O824 Cl81 O823 109.0(3) . . ?
O822 Cl81 O823 109.3(3) . . ?
O821 Cl81 O823 109.6(4) . . ?
O923 Cl91 O922 111.86(19) . . ?
O923 Cl91 O921 110.35(18) . . ?
O922 Cl91 O921 108.88(18) . . ?
O923 Cl91 O924 108.53(17) . . ?
O922 Cl91 O924 110.0(2) . . ?
O921 Cl91 O924 107.1(2) . . ?
O832 Cl82 O834 111.7(5) . . ?
O832 Cl82 O833 113.4(5) . . ?
O834 Cl82 O833 108.3(6) . . ?
O832 Cl82 O831 110.4(5) . . ?
O834 Cl82 O831 106.4(5) . . ?
O833 Cl82 O831 106.3(5) . . ?
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
Tm1 O33 2.3072(10) . ?
Tm1 O43 2.3124(9) . ?
Tm1 O13 2.3247(10) . ?
Tm1 O53 2.3547(9) . ?
Tm1 O23 2.3640(9) . ?
Tm1 N4 2.5755(11) . ?
Tm1 N1 2.5803(11) . ?
Tm1 N10 2.6360(11) . ?
Tm1 N7 2.6800(10) . ?
N1 C11 1.4775(16) . ?
N1 C21 1.4820(16) . ?
N1 C2 1.4887(17) . ?
C2 C3 1.5172(18) . ?
C3 N4 1.4949(17) . ?
N4 C31 1.4834(16) . ?
N4 C5 1.4921(17) . ?
C5 C6 1.5158(19) . ?
C6 N7 1.4875(16) . ?
N7 C41 1.4797(16) . ?
N7 C8 1.4826(17) . ?
C8 C9 1.5214(18) . ?
C9 N10 1.4825(16) . ?
N10 C51 1.4756(16) . ?
N10 C61 1.5064(16) . ?
C11 C12 1.5142(18) . ?
C12 O13 1.2595(15) . ?
C12 N14 1.3146(17) . ?
C21 C22 1.5046(18) . ?
C22 O23 1.2559(15) . ?
C22 N24 1.3193(16) . ?
C31 C32 1.5177(19) . ?
C32 O33 1.2558(16) . ?
C32 N34 1.3162(18) . ?
C41 C42 1.5010(18) . ?
C42 O43 1.2555(15) . ?
C42 N44 1.3172(16) . ?
C51 C52 1.5052(17) . ?
C52 O53 1.2575(15) . ?
C52 N54 1.3162(16) . ?
C61 C62 1.5168(18) . ?
C62 C63 1.3944(19) . ?
C62 C67 1.399(2) . ?
C63 C64 1.397(2) . ?
C64 C65 1.388(3) . ?
C65 C66 1.383(3) . ?
C66 C67 1.397(2) . ?
Cl70 O714 1.4141(15) . ?
Cl70 O712 1.4237(13) . ?
Cl70 O711 1.4340(11) . ?
Cl70 O713 1.4429(14) . ?
Cl80 O814 1.432(3) . ?
Cl80 O813 1.440(2) . ?
Cl80 O811 1.442(3) . ?
Cl80 O812 1.465(3) . ?
Cl90 O913 1.427(2) . ?
Cl90 O912 1.429(3) . ?
Cl90 O911 1.455(3) . ?
Cl90 O914 1.474(3) . ?
Cl81 O824 1.432(5) . ?
Cl81 O822 1.436(5) . ?
Cl81 O821 1.440(5) . ?
Cl81 O823 1.447(4) . ?
Cl91 O923 1.422(3) . ?
Cl91 O922 1.431(3) . ?
Cl91 O921 1.459(3) . ?
Cl91 O924 1.466(3) . ?
Cl82 O832 1.408(6) . ?
Cl82 O834 1.439(6) . ?
Cl82 O833 1.439(5) . ?
Cl82 O831 1.467(6) . ?
