# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_D1PyO_karasawa
_database_code_depnum_ccdc_archive 'CCDC 1037883'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C12 H9 N3 O'
_chemical_formula_moiety         'C12 H9 N3 O'
_chemical_formula_weight         211.22
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   9.582(4)
_cell_length_b                   11.591(5)
_cell_length_c                   9.149(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.212(5)
_cell_angle_gamma                90.0000
_cell_volume                     1000.1(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    90
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440.00
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      90
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            5322
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.160
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_reflns_number_total             2158
_reflns_number_gt                1795
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1266
_refine_ls_wR_factor_gt          0.1198
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_reflns         2158
_refine_ls_number_parameters     181
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0668P)²+0.2750P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.93825(12) 0.11316(10) 0.19075(13) 0.0187(3) Uani 1 4 d . . .
O1 O 0.99744(11) 0.15970(9) 0.08525(12) 0.0245(3) Uani 1 4 d . . .
N3 N 0.77599(14) -0.24597(10) 0.56600(14) 0.0248(3) Uani 1 4 d . . .
N2 N 0.76960(12) -0.14855(10) 0.55581(13) 0.0191(3) Uani 1 4 d . . .
C6 C 0.75971(15) -0.03544(12) 0.54140(16) 0.0183(3) Uani 1 4 d . . .
C3 C 0.81876(14) 0.01541(12) 0.41971(15) 0.0171(3) Uani 1 4 d . . .
C4 C 0.83651(15) 0.13486(12) 0.40879(16) 0.0195(3) Uani 1 4 d . . .
C2 C 0.86422(15) -0.05259(12) 0.30993(16) 0.0191(3) Uani 1 4 d . . .
C5 C 0.89497(15) 0.18121(12) 0.29552(16) 0.0200(3) Uani 1 4 d . . .
C12 C 0.70953(15) -0.01160(13) 0.79860(17) 0.0216(3) Uani 1 4 d . . .
C10 C 0.54354(16) 0.13149(13) 0.85339(18) 0.0243(3) Uani 1 4 d . . .
C7 C 0.68752(15) 0.02433(12) 0.65029(16) 0.0185(3) Uani 1 4 d . . .
C11 C 0.63679(16) 0.04143(14) 0.89887(18) 0.0245(3) Uani 1 4 d . . .
C1 C 0.92230(15) -0.00345(12) 0.19808(16) 0.0197(3) Uani 1 4 d . . .
C8 C 0.59325(15) 0.11490(13) 0.60496(17) 0.0219(3) Uani 1 4 d . . .
C9 C 0.52299(16) 0.16863(13) 0.70717(18) 0.0245(3) Uani 1 4 d . . .
H1 H 0.8572(17) -0.1359(14) 0.3134(19) 0.020(4) Uiso 1 4 d . . .
H4 H 0.9105(16) 0.2632(15) 0.2856(19) 0.018(4) Uiso 1 4 d . . .
H6 H 0.7761(18) -0.0717(14) 0.831(2) 0.025(4) Uiso 1 4 d . . .
H7 H 0.653(2) 0.0193(16) 1.001(2) 0.036(5) Uiso 1 4 d . . .
H3 H 0.8118(19) 0.1896(15) 0.481(2) 0.030(5) Uiso 1 4 d . . .
H9 H 0.4598(19) 0.2323(16) 0.678(2) 0.033(5) Uiso 1 4 d . . .
H5 H 0.5744(19) 0.1369(15) 0.499(2) 0.032(5) Uiso 1 4 d . . .
H8 H 0.4922(19) 0.1677(15) 0.921(2) 0.031(5) Uiso 1 4 d . . .
H2 H 0.9555(18) -0.0461(14) 0.127(2) 0.024(4) Uiso 1 4 d . . .



#==============================================================================
_computing_data_collection       Unknown
_computing_cell_refinement       Unknown
_computing_data_reduction        Unknown
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

#==============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
N1 O1 1.3185(17) yes . .
N1 C5 1.362(2) yes . .
N1 C1 1.3633(19) yes . .
N3 N2 1.1338(17) yes . .
N2 C6 1.3194(19) yes . .
C6 C3 1.460(2) yes . .
C6 C7 1.482(2) yes . .
C3 C4 1.401(2) yes . .
C3 C2 1.405(2) yes . .
C4 C5 1.372(2) yes . .
C2 C1 1.372(2) yes . .
C12 C7 1.399(2) yes . .
C12 C11 1.390(2) yes . .
C10 C11 1.389(2) yes . .
C10 C9 1.386(2) yes . .
C7 C8 1.399(2) yes . .
C8 C9 1.392(2) yes . .
C4 H3 0.977(19) no . .
C2 H1 0.969(17) no . .
C5 H4 0.969(17) no . .
C12 H6 0.954(17) no . .
C10 H8 0.95(2) no . .
C11 H7 0.96(2) no . .
C1 H2 0.919(19) no . .
C8 H5 0.99(2) no . .
C9 H9 0.963(18) no . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O1 N1 C5 120.17(12) yes . . .
O1 N1 C1 120.54(12) yes . . .
C5 N1 C1 119.27(13) yes . . .
N3 N2 C6 178.69(13) yes . . .
N2 C6 C3 116.54(13) yes . . .
N2 C6 C7 115.55(13) yes . . .
C3 C6 C7 127.91(13) yes . . .
C6 C3 C4 121.46(13) yes . . .
C6 C3 C2 122.00(13) yes . . .
C4 C3 C2 116.52(13) yes . . .
C3 C4 C5 120.80(14) yes . . .
C3 C2 C1 121.21(13) yes . . .
N1 C5 C4 121.40(13) yes . . .
C7 C12 C11 120.09(14) yes . . .
C11 C10 C9 119.76(15) yes . . .
C6 C7 C12 120.32(13) yes . . .
C6 C7 C8 120.36(13) yes . . .
C12 C7 C8 119.29(14) yes . . .
C12 C11 C10 120.39(15) yes . . .
N1 C1 C2 120.80(14) yes . . .
C7 C8 C9 120.01(14) yes . . .
C10 C9 C8 120.43(14) yes . . .
C3 C4 H3 123.2(11) no . . .
C5 C4 H3 116.0(11) no . . .
C3 C2 H1 120.3(11) no . . .
C1 C2 H1 118.5(11) no . . .
N1 C5 H4 115.5(11) no . . .
C4 C5 H4 123.0(11) no . . .
C7 C12 H6 119.5(12) no . . .
C11 C12 H6 120.4(12) no . . .
C11 C10 H8 121.0(11) no . . .
C9 C10 H8 119.2(11) no . . .
C12 C11 H7 120.9(12) no . . .
C10 C11 H7 118.7(12) no . . .
N1 C1 H2 116.3(11) no . . .
C2 C1 H2 122.9(11) no . . .
C7 C8 H5 118.8(11) no . . .
C9 C8 H5 121.2(11) no . . .
C10 C9 H9 119.0(12) no . . .
C8 C9 H9 120.6(12) no . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 N1 C5 C4 -178.25(10) no . . . .
O1 N1 C1 C2 178.25(10) no . . . .
C5 N1 C1 C2 -0.42(18) no . . . .
C1 N1 C5 C4 0.42(18) no . . . .
N2 C6 C3 C4 -168.84(10) no . . . .
N2 C6 C3 C2 9.41(18) no . . . .
N2 C6 C7 C12 38.89(17) no . . . .
N2 C6 C7 C8 -139.10(12) no . . . .
C3 C6 C7 C12 -142.12(13) no . . . .
C3 C6 C7 C8 39.9(2) no . . . .
C7 C6 C3 C4 12.2(2) no . . . .
C7 C6 C3 C2 -169.57(11) no . . . .
C6 C3 C4 C5 178.60(11) no . . . .
C6 C3 C2 C1 -178.58(11) no . . . .
C4 C3 C2 C1 -0.25(18) no . . . .
C2 C3 C4 C5 0.25(18) no . . . .
C3 C4 C5 N1 -0.3(2) no . . . .
C3 C2 C1 N1 0.34(19) no . . . .
C7 C12 C11 C10 -1.0(2) no . . . .
C11 C12 C7 C6 -177.17(12) no . . . .
C11 C12 C7 C8 0.8(2) no . . . .
C11 C10 C9 C8 1.2(2) no . . . .
C9 C10 C11 C12 -0.0(2) no . . . .
C6 C7 C8 C9 178.31(11) no . . . .
C12 C7 C8 C9 0.3(2) no . . . .
C7 C8 C9 C10 -1.3(2) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N1 C3 2.799(2) no . .
O1 C4 3.584(2) no . .
O1 C2 3.583(2) no . .
N3 C3 3.366(2) no . .
N3 C2 3.454(2) no . .
N3 C12 3.577(2) no . .
N3 C7 3.371(2) no . .
N2 C2 2.801(2) no . .
N2 C12 2.870(2) no . .
N2 C8 3.557(2) no . .
C3 C8 3.189(2) no . .
C4 C7 3.111(2) no . .
C4 C1 2.743(2) no . .
C4 C8 3.192(2) no . .
C2 C5 2.732(2) no . .
C12 C9 2.780(2) no . .
C10 C7 2.794(2) no . .
C11 C8 2.781(3) no . .
N1 N3 3.5581(19) no . 3_756
N1 N2 3.3287(18) no . 3_756
N1 C6 3.561(2) no . 3_756
N1 C12 3.560(2) no . 3_756
O1 N3 2.982(2) no . 2_755
O1 N2 3.5511(19) no . 2_755
O1 C4 3.1261(19) no . 4_554
O1 C5 3.235(2) no . 4_554
O1 C12 3.302(2) no . 3_756
O1 C1 3.361(2) no . 3_755
N3 N1 3.5581(19) no . 3_756
N3 O1 2.982(2) no . 2_745
N3 C2 3.237(2) no . 4_545
N3 C5 3.270(2) no . 3_756
N3 C10 3.569(2) no . 2_646
N3 C1 3.356(2) no . 4_545
N3 C9 3.566(2) no . 3_656
N2 N1 3.3287(18) no . 3_756
N2 O1 3.5511(19) no . 2_745
N2 C5 3.282(2) no . 3_756
N2 C8 3.548(2) no . 3_656
N2 C9 3.363(2) no . 3_656
C6 N1 3.561(2) no . 3_756
C6 C1 3.549(2) no . 3_756
C6 C8 3.532(2) no . 3_656
C6 C9 3.565(2) no . 3_656
C3 C3 3.541(2) no . 3_756
C3 C2 3.587(2) no . 3_756
C4 O1 3.1261(19) no . 4_555
C2 N3 3.237(2) no . 4_544
C2 C3 3.587(2) no . 3_756
C5 O1 3.235(2) no . 4_555
C5 N3 3.270(2) no . 3_756
C5 N2 3.282(2) no . 3_756
C12 N1 3.560(2) no . 3_756
C12 O1 3.302(2) no . 3_756
C12 C1 3.527(3) no . 3_756
C10 N3 3.569(2) no . 2_656
C11 C11 3.597(3) no . 3_657
C11 C1 3.549(2) no . 1_556
C1 O1 3.361(2) no . 3_755
C1 N3 3.356(2) no . 4_544
C1 C6 3.549(2) no . 3_756
C1 C12 3.527(3) no . 3_756
C1 C11 3.549(2) no . 1_554
C8 N2 3.548(2) no . 3_656
C8 C6 3.532(2) no . 3_656
C8 C8 3.572(2) no . 3_656
C9 N3 3.566(2) no . 3_656
C9 N2 3.363(2) no . 3_656
C9 C6 3.565(2) no . 3_656
N1 H1 3.241(17) no . .
N1 H3 3.23(2) no . .
O1 H4 2.456(18) no . .
O1 H2 2.460(17) no . .
N3 H1 2.866(18) no . .
N3 H6 3.153(18) no . .
N2 H1 2.511(18) no . .
N2 H6 2.657(19) no . .
C6 H1 2.697(18) no . .
C6 H6 2.656(19) no . .
C6 H3 2.731(18) no . .
C6 H5 2.655(18) no . .
C3 H4 3.303(17) no . .
C3 H5 2.932(19) no . .
C3 H2 3.26(2) no . .
C4 H1 3.273(17) no . .
C4 H5 2.78(2) no . .
C2 H3 3.297(19) no . .
C5 H2 3.159(18) no . .
C12 H5 3.300(19) no . .
C12 H8 3.276(19) no . .
C10 H6 3.274(17) no . .
C10 H5 3.31(2) no . .
C7 H7 3.29(2) no . .
C7 H3 2.852(19) no . .
C7 H9 3.291(19) no . .
C11 H9 3.264(18) no . .
C1 H4 3.200(17) no . .
C8 H6 3.275(17) no . .
C8 H3 2.69(2) no . .
C8 H8 3.26(2) no . .
C9 H7 3.255(19) no . .
H1 H2 2.34(3) no . .
H4 H3 2.33(3) no . .
H6 H7 2.36(3) no . .
H7 H8 2.34(3) no . .
H3 H5 2.39(3) no . .
H9 H5 2.39(3) no . .
H9 H8 2.32(3) no . .
N1 H1 3.511(17) no . 2_755
N1 H6 2.820(18) no . 3_756
N1 H7 3.159(18) no . 1_554
N1 H3 3.089(18) no . 4_554
N1 H2 3.34(2) no . 3_755
O1 H1 2.820(16) no . 2_755
O1 H4 2.863(16) no . 4_554
O1 H6 2.398(17) no . 3_756
O1 H3 2.553(17) no . 4_554
O1 H2 2.452(19) no . 3_755
N3 H1 2.642(17) no . 4_545
N3 H4 3.076(15) no . 3_756
N3 H6 3.018(18) no . 4_544
N3 H7 3.395(19) no . 4_544
N3 H9 3.54(2) no . 2_646
N3 H9 2.883(17) no . 3_656
N3 H5 3.538(18) no . 3_656
N3 H8 2.780(18) no . 2_646
N3 H2 2.956(17) no . 4_545
N2 H1 3.435(17) no . 4_545
N2 H4 3.419(15) no . 3_756
N2 H9 2.945(17) no . 3_656
N2 H5 3.248(18) no . 3_656
N2 H8 3.326(18) no . 2_646
C6 H9 3.486(18) no . 3_656
C6 H5 3.369(18) no . 3_656
C4 H1 3.526(15) no . 3_756
C4 H4 3.594(17) no . 4_555
C2 H4 3.264(17) no . 2_745
C2 H7 3.277(19) no . 1_554
C5 H1 3.459(17) no . 2_755
C5 H3 3.214(19) no . 4_554
C5 H2 3.491(17) no . 2_755
C12 H4 3.478(17) no . 4_555
C12 H9 3.408(19) no . 2_646
C12 H2 3.496(17) no . 1_556
C12 H2 3.231(17) no . 3_756
C10 H7 3.04(2) no . 3_657
C10 H3 3.348(17) no . 4_555
C10 H9 3.57(2) no . 4_555
C10 H5 2.988(18) no . 4_555
C7 H4 3.351(16) no . 4_555
C7 H5 3.232(17) no . 3_656
C11 H7 3.15(2) no . 3_657
C11 H3 3.557(18) no . 4_555
C11 H8 3.294(19) no . 3_657
C11 H2 3.528(16) no . 1_556
C1 H4 3.134(17) no . 2_745
C1 H6 3.497(18) no . 1_554
C1 H6 3.074(18) no . 3_756
C1 H7 2.885(18) no . 1_554
C1 H2 3.43(2) no . 3_755
C8 H4 3.491(15) no . 4_555
C8 H5 3.386(17) no . 3_656
C8 H8 3.089(17) no . 4_554
C9 H5 3.463(19) no . 4_555
C9 H8 3.205(19) no . 4_554
H1 N1 3.511(17) no . 2_745
H1 O1 2.820(16) no . 2_745
H1 N3 2.642(17) no . 4_544
H1 N2 3.435(17) no . 4_544
H1 C4 3.526(15) no . 3_756
H1 C5 3.459(17) no . 2_745
H1 H4 2.80(2) no . 2_745
H1 H6 3.49(2) no . 4_544
H1 H3 3.44(2) no . 3_756
H1 H9 3.25(3) no . 3_656
H4 O1 2.863(16) no . 4_555
H4 N3 3.076(15) no . 3_756
H4 N2 3.419(15) no . 3_756
H4 C4 3.594(17) no . 4_554
H4 C2 3.264(17) no . 2_755
H4 C12 3.478(17) no . 4_554
H4 C7 3.351(16) no . 4_554
H4 C1 3.134(17) no . 2_755
H4 C8 3.491(15) no . 4_554
H4 H1 2.80(2) no . 2_755
H4 H3 2.83(2) no . 4_554
H4 H2 2.61(2) no . 2_755
H6 N1 2.820(18) no . 3_756
H6 O1 2.398(17) no . 3_756
H6 N3 3.018(18) no . 4_545
H6 C1 3.497(18) no . 1_556
H6 C1 3.074(18) no . 3_756
H6 H1 3.49(2) no . 4_545
H6 H9 3.20(3) no . 2_646
H6 H2 2.96(2) no . 1_556
H6 H2 2.88(2) no . 3_756
H7 N1 3.159(18) no . 1_556
H7 N3 3.395(19) no . 4_545
H7 C2 3.277(19) no . 1_556
H7 C10 3.04(2) no . 3_657
H7 C11 3.15(2) no . 3_657
H7 C1 2.885(18) no . 1_556
H7 H7 2.96(3) no . 3_657
H7 H8 2.74(3) no . 3_657
H7 H2 3.02(2) no . 1_556
H3 N1 3.089(18) no . 4_555
H3 O1 2.553(17) no . 4_555
H3 C5 3.214(19) no . 4_555
H3 C10 3.348(17) no . 4_554
H3 C11 3.557(18) no . 4_554
H3 H1 3.44(2) no . 3_756
H3 H4 2.83(2) no . 4_555
H3 H8 3.44(2) no . 4_554
H9 N3 3.54(2) no . 2_656
H9 N3 2.883(17) no . 3_656
H9 N2 2.945(17) no . 3_656
H9 C6 3.486(18) no . 3_656
H9 C12 3.408(19) no . 2_656
H9 C10 3.57(2) no . 4_554
H9 H1 3.25(3) no . 3_656
H9 H6 3.20(3) no . 2_656
H9 H5 3.32(3) no . 4_555
H9 H8 2.69(3) no . 4_554
H5 N3 3.538(18) no . 3_656
H5 N2 3.248(18) no . 3_656
H5 C6 3.369(18) no . 3_656
H5 C10 2.988(18) no . 4_554
H5 C7 3.232(17) no . 3_656
H5 C8 3.386(17) no . 3_656
H5 C9 3.463(19) no . 4_554
H5 H9 3.32(3) no . 4_554
H5 H5 3.48(2) no . 3_656
H5 H8 2.46(2) no . 4_554
H8 N3 2.780(18) no . 2_656
H8 N2 3.326(18) no . 2_656
H8 C11 3.294(19) no . 3_657
H8 C8 3.089(17) no . 4_555
H8 C9 3.205(19) no . 4_555
H8 H7 2.74(3) no . 3_657
H8 H3 3.44(2) no . 4_555
H8 H9 2.69(3) no . 4_555
H8 H5 2.46(2) no . 4_555
H2 N1 3.34(2) no . 3_755
H2 O1 2.452(19) no . 3_755
H2 N3 2.956(17) no . 4_544
H2 C5 3.491(17) no . 2_745
H2 C12 3.496(17) no . 1_554
H2 C12 3.231(17) no . 3_756
H2 C11 3.528(16) no . 1_554
H2 C1 3.43(2) no . 3_755
H2 H4 2.61(2) no . 2_745
H2 H6 2.96(2) no . 1_554
H2 H6 2.88(2) no . 3_756
H2 H7 3.02(2) no . 1_554
H2 H2 2.82(3) no . 3_755

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1d_Gd
_database_code_depnum_ccdc_archive 'CCDC 1037884'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H44 Cl6 F18 Gd2 N6 O14 S6'
_chemical_formula_weight         2302.74

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.9824(14)
_cell_length_b                   16.7219(15)
_cell_length_c                   17.1700(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1760(11)
_cell_angle_gamma                90.00
_cell_volume                     4276.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.51

_exptl_crystal_description       brick
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2260
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            21045
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.51
_reflns_number_total             7935
_reflns_number_gt                7108
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0783P)²+16.4729P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7935
_refine_ls_number_parameters     636
_refine_ls_number_restraints     992
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1350
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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 0.5104(3) 0.2801(3) 0.6520(3) 0.0372(11) Uani 1 1 d U . .
H1A H 0.4883 0.2496 0.6910 0.045 Uiso 1 1 calc R . .
C010 C 0.6344(4) 0.5824(3) 0.6574(3) 0.0405(12) Uani 1 1 d U A .
H01A H 0.6513 0.6129 0.6162 0.049 Uiso 1 1 calc R . .
C011 C 0.9526(4) 0.5727(4) 0.5579(4) 0.0497(14) Uani 1 1 d U . .
H01B H 0.9649 0.5927 0.5097 0.060 Uiso 1 1 calc R . .
C012 C 0.8356(4) 0.2607(3) 0.4344(3) 0.0397(12) Uani 1 1 d U . .
C013 C 0.5785(4) 0.4952(3) 0.7775(3) 0.0393(11) Uani 1 1 d U . .
H01D H 0.5580 0.4657 0.8179 0.047 Uiso 1 1 calc R . .
C014 C 0.6343(4) 0.2433(3) 0.8007(3) 0.0396(12) Uani 1 1 d U . .
H01E H 0.5796 0.2179 0.8037 0.048 Uiso 1 1 calc R . .
C015 C 0.7279(5) 0.5117(4) 0.3816(4) 0.0528(14) Uani 1 1 d U . .
C016 C 0.7999(4) 0.5229(4) 0.4370(4) 0.0482(13) Uani 1 1 d U . .
H01F H 0.8543 0.5394 0.4210 0.058 Uiso 1 1 calc R . .
C017 C 0.6035(4) 0.2979(4) 0.3312(3) 0.0427(12) Uani 1 1 d U . .
C019 C 0.6926(4) 0.2757(4) 0.3462(3) 0.0440(13) Uani 1 1 d U . .
H01G H 0.7201 0.2507 0.3067 0.053 Uiso 1 1 calc R . .
C020 C 0.5523(5) 0.2746(4) 0.2527(4) 0.0533(15) Uani 1 1 d U . .
C021 C 0.7084(4) 0.2399(4) 0.8603(4) 0.0485(14) Uani 1 1 d U . .
H02A H 0.7071 0.2124 0.9073 0.058 Uiso 1 1 calc R . .
C022 C 0.5992(3) 0.3108(3) 0.6650(3) 0.0316(10) Uani 1 1 d U . .
C1A C 0.6863(5) 0.5139(3) 0.9423(3) 0.0481(19) Uani 0.611(6) 1 d PGU A -1
C2A C 0.6720(6) 0.5527(3) 1.0115(4) 0.061(2) Uani 0.611(6) 1 d PGU A -1
H2AA H 0.6702 0.6082 1.0131 0.073 Uiso 0.611(6) 1 calc PR A -1
C3A C 0.6602(6) 0.5084(4) 1.0781(3) 0.068(2) Uani 0.611(6) 1 d PGU A -1
H3AA H 0.6506 0.5344 1.1244 0.082 Uiso 0.611(6) 1 calc PR A -1
C4A C 0.6628(6) 0.4254(4) 1.0756(3) 0.058(2) Uani 0.611(6) 1 d PGU A -1
H4AA H 0.6549 0.3958 1.1202 0.070 Uiso 0.611(6) 1 calc PR A -1
C5A C 0.6772(5) 0.3866(3) 1.0065(4) 0.0446(19) Uani 0.611(6) 1 d PGU A -1
H5AA H 0.6789 0.3310 1.0048 0.054 Uiso 0.611(6) 1 calc PR A -1
C6A C 0.6889(5) 0.4308(3) 0.9398(3) 0.0404(18) Uani 0.611(6) 1 d PGU A -1
H6AA H 0.6985 0.4049 0.8935 0.048 Uiso 0.611(6) 1 calc PR A -1
C1B C 0.6582(7) 0.5161(7) 0.9453(5) 0.043(2) Uani 0.389(6) 1 d PGU A -2
C2B C 0.5712(6) 0.5291(7) 0.9634(6) 0.053(3) Uani 0.389(6) 1 d PGU A -2
H2BA H 0.5318 0.5602 0.9304 0.063 Uiso 0.389(6) 1 calc PR A -2
C3B C 0.5429(6) 0.4958(7) 1.0307(6) 0.058(3) Uani 0.389(6) 1 d PGU A -2
H3BA H 0.4847 0.5045 1.0428 0.070 Uiso 0.389(6) 1 calc PR A -2
C4B C 0.6017(8) 0.4494(7) 1.0800(5) 0.059(3) Uani 0.389(6) 1 d PGU A -2
H4BA H 0.5828 0.4271 1.1250 0.071 Uiso 0.389(6) 1 calc PR A -2
C5B C 0.6888(7) 0.4364(7) 1.0619(6) 0.057(3) Uani 0.389(6) 1 d PGU A -2
H5BA H 0.7281 0.4054 1.0948 0.068 Uiso 0.389(6) 1 calc PR A -2
C6B C 0.7170(6) 0.4698(7) 0.9945(6) 0.052(2) Uani 0.389(6) 1 d PGU A -2
H6BA H 0.7753 0.4611 0.9824 0.063 Uiso 0.389(6) 1 calc PR A -2
C01C C 0.6925(5) 0.5586(4) 0.8729(3) 0.0479(13) Uani 1 1 d U . .
C01D C 0.9822(4) 0.2306(4) 0.5021(4) 0.0564(15) Uani 1 1 d U . .
H01H H 1.0339 0.2250 0.5369 0.068 Uiso 1 1 calc R . .
C01E C 0.9749(4) 0.2027(4) 0.4288(4) 0.0578(15) Uani 1 1 d U . .
H01J H 1.0218 0.1749 0.4098 0.069 Uiso 1 1 calc R . .
C01G C 0.7803(5) 0.2808(4) 0.8413(4) 0.0581(17) Uani 1 1 d U . .
H01C H 0.8341 0.2841 0.8736 0.070 Uiso 1 1 calc R . .
C01H C 1.0099(5) 0.5778(4) 0.6283(5) 0.0604(16) Uani 1 1 d U . .
H01M H 1.0660 0.6022 0.6312 0.072 Uiso 1 1 calc R . .
C01I C 0.3623(4) 0.2553(4) 0.5759(4) 0.0531(15) Uani 1 1 d U . .
C01J C 0.9779(4) 0.5449(4) 0.6911(5) 0.0589(16) Uani 1 1 d U . .
H01N H 1.0091 0.5444 0.7410 0.071 Uiso 1 1 calc R . .
C01K C 0.7395(6) 0.5320(5) 0.2962(4) 0.0675(18) Uani 1 1 d U . .
C00R C 0.6761(4) 0.5935(3) 0.7310(3) 0.0420(12) Uani 1 1 d U . .
H00A H 0.7222 0.6306 0.7397 0.050 Uiso 1 1 calc R A .
C00S C 0.7939(4) 0.5102(3) 0.5176(3) 0.0397(11) Uani 1 1 d U . .
C1S C 0.4762(5) 0.9500(6) 0.5803(11) 0.125(4) Uani 0.728(7) 1 d PDU B 1
H1SA H 0.4894 0.9714 0.5296 0.149 Uiso 0.728(7) 1 calc PR B 1
C1T C 0.4917(9) 0.9137(12) 0.6153(15) 0.118(5) Uani 0.272(7) 1 d PDU B 2
H1TA H 0.4997 0.8802 0.6624 0.142 Uiso 0.272(7) 1 calc PR B 2
C00U C 0.8720(4) 0.5312(3) 0.5728(4) 0.0427(12) Uani 1 1 d U . .
C00V C 0.7431(4) 0.2894(3) 0.4188(3) 0.0393(11) Uani 1 1 d U . .
C00W C 0.6494(4) 0.5488(3) 0.7940(3) 0.0411(12) Uani 1 1 d U A .
C00X C 0.4562(4) 0.2942(3) 0.5837(3) 0.0392(11) Uani 1 1 d U . .
C00Y C 0.5385(4) 0.4856(3) 0.7020(3) 0.0370(11) Uani 1 1 d U A .
H00B H 0.4908 0.4502 0.6915 0.044 Uiso 1 1 calc R . .
C00Z C 0.6547(3) 0.2898(3) 0.7372(3) 0.0341(10) Uani 1 1 d U . .
Cl1S Cl 0.5809(2) 0.9576(3) 0.6271(3) 0.0713(11) Uani 0.728(7) 1 d PDU B 1
Cl2S Cl 0.4382(3) 0.8605(2) 0.5481(3) 0.1054(14) Uani 0.728(7) 1 d PDU B 1
Cl3S Cl 0.3990(3) 1.0189(2) 0.5991(2) 0.1000(15) Uani 0.728(7) 1 d PDU B 1
Cl1T Cl 0.5867(9) 0.9700(13) 0.6286(16) 0.144(7) Uani 0.272(7) 1 d PDU B 2
Cl2T Cl 0.4886(9) 0.8429(7) 0.5448(8) 0.108(4) Uani 0.272(7) 1 d PDU B 2
Cl3T Cl 0.3948(8) 0.9595(9) 0.6283(8) 0.124(4) Uani 0.272(7) 1 d PDU B 2
F1 F 0.3400(3) 0.2221(3) 0.6405(3) 0.0829(14) Uani 1 1 d U . .
F2 F 0.3002(2) 0.3061(3) 0.5467(3) 0.0747(12) Uani 1 1 d U . .
F3 F 0.3579(3) 0.1949(3) 0.5237(3) 0.0772(13) Uani 1 1 d U . .
F00G F 0.5155(3) 0.3361(3) 0.2153(2) 0.0783(14) Uani 1 1 d U . .
F00H F 0.6027(3) 0.2391(3) 0.2038(2) 0.0845(15) Uani 1 1 d U . .
F00K F 0.4867(4) 0.2240(3) 0.2632(3) 0.0896(15) Uani 1 1 d U . .
F00N F 0.6744(4) 0.5804(4) 0.2661(3) 0.1000(19) Uani 1 1 d U . .
F00O F 0.8162(4) 0.5698(4) 0.2862(3) 0.0949(16) Uani 1 1 d U . .
F00Q F 0.7387(4) 0.4672(3) 0.2529(3) 0.0884(15) Uani 1 1 d U . .
Gd01 Gd 0.594792(16) 0.411784(15) 0.491166(13) 0.03202(12) Uani 1 1 d U . .
N1 N 0.7533(5) 0.6150(4) 0.8841(3) 0.0667(16) Uani 1 1 d U A .
N00L N 0.5689(3) 0.5277(3) 0.6436(2) 0.0351(9) Uani 1 1 d U . .
N01L N 0.8053(6) 0.6651(6) 0.8950(4) 0.100(3) Uani 1 1 d U . .
C31 C 0.8910(3) 0.2170(3) 0.3795(3) 0.0350(11) Uani 1 1 d U . .
H31A H 0.8756 0.2029 0.3274 0.042 Uiso 1 1 calc R . .
O1 O 0.6332(2) 0.3563(2) 0.6179(2) 0.0323(7) Uani 1 1 d U . .
O2 O 0.5327(2) 0.5144(2) 0.56895(19) 0.0351(8) Uani 1 1 d U . .
O3 O 0.7255(2) 0.4835(2) 0.5453(2) 0.0355(8) Uani 1 1 d U . .
O00B O 0.7130(2) 0.3261(2) 0.4749(2) 0.0396(9) Uani 1 1 d U . .
O00C O 0.5556(3) 0.3354(2) 0.3759(2) 0.0421(9) Uani 1 1 d U . .
O00D O 0.4722(2) 0.3325(2) 0.5241(2) 0.0407(9) Uani 1 1 d U . .
O00E O 0.6498(3) 0.4857(3) 0.3901(2) 0.0485(10) Uani 1 1 d U . .
S002 S 0.76270(10) 0.32608(9) 0.75164(9) 0.0479(4) Uani 1 1 d U . .
S003 S 0.87440(10) 0.50447(11) 0.66946(11) 0.0559(4) Uani 1 1 d U . .
S004 S 0.88943(11) 0.27689(11) 0.52575(11) 0.0544(4) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 C00X 1.374(8) . ?
C1 C022 1.420(7) . ?
C1 H1A 0.9300 . ?
C010 N00L 1.343(8) . ?
C010 C00R 1.362(8) . ?
C010 H01A 0.9300 . ?
C011 C01H 1.409(11) . ?
C011 C00U 1.440(8) . ?
C011 H01B 0.9300 . ?
C012 C00V 1.465(7) . ?
C012 C31 1.509(7) . ?
C012 S004 1.707(6) . ?
C013 C00Y 1.378(7) . ?
C013 C00W 1.395(9) . ?
C013 H01D 0.9300 . ?
C014 C00Z 1.399(8) . ?
C014 C021 1.428(8) . ?
C014 H01E 0.9300 . ?
C015 O00E 1.271(8) . ?
C015 C016 1.372(10) . ?
C015 C01K 1.533(9) . ?
C016 C00S 1.412(8) . ?
C016 H01F 0.9300 . ?
C017 O00C 1.270(7) . ?
C017 C019 1.382(8) . ?
C017 C020 1.528(8) . ?
C019 C00V 1.406(8) . ?
C019 H01G 0.9300 . ?
C020 F00G 1.304(7) . ?
C020 F00K 1.323(9) . ?
C020 F00H 1.328(7) . ?
C021 C01G 1.345(9) . ?
C021 H02A 0.9300 . ?
C022 O1 1.258(6) . ?
C022 C00Z 1.461(7) . ?
C1A C2A 1.3900 . ?
C1A C6A 1.3900 . ?
C1A C01C 1.418(8) . ?
C2A C3A 1.3900 . ?
C2A H2AA 0.9300 . ?
C3A C4A 1.3900 . ?
C3A H3AA 0.9300 . ?
C4A C5A 1.3900 . ?
C4A H4AA 0.9300 . ?
C5A C6A 1.3900 . ?
C5A H5AA 0.9300 . ?
C6A H6AA 0.9300 . ?
C1B C2B 1.3900 . ?
C1B C6B 1.3900 . ?
C1B C01C 1.565(10) . ?
C2B C3B 1.3900 . ?
C2B H2BA 0.9300 . ?
C3B C4B 1.3900 . ?
C3B H3BA 0.9300 . ?
C4B C5B 1.3900 . ?
C4B H4BA 0.9300 . ?
C5B C6B 1.3900 . ?
C5B H5BA 0.9300 . ?
C6B H6BA 0.9300 . ?
C01C N1 1.312(10) . ?
C01C C00W 1.446(7) . ?
C01D C01E 1.337(10) . ?
C01D S004 1.677(6) . ?
C01D H01H 0.9300 . ?
C01E C31 1.458(8) . ?
C01E H01J 0.9300 . ?
C01G S002 1.710(6) . ?
C01G H01C 0.9300 . ?
C01H C01J 1.344(11) . ?
C01H H01M 0.9300 . ?
C01I F1 1.315(8) . ?
C01I F2 1.318(8) . ?
C01I F3 1.348(8) . ?
C01I C00X 1.543(8) . ?
C01J S003 1.697(7) . ?
C01J H01N 0.9300 . ?
C01K F00Q 1.314(10) . ?
C01K F00N 1.329(9) . ?
C01K F00O 1.339(10) . ?
C00R C00W 1.407(9) . ?
C00R H00A 0.9300 . ?
C00S O3 1.258(7) . ?
C00S C00U 1.467(9) . ?
C1S Cl2S 1.674(7) . ?
C1S Cl3S 1.689(7) . ?
C1S Cl1S 1.689(6) . ?
C1S H1SA 0.9800 . ?
C1T Cl3T 1.678(8) . ?
C1T Cl2T 1.691(8) . ?
C1T Cl1T 1.701(7) . ?
C1T H1TA 0.9800 . ?
C00U S003 1.716(6) . ?
C00V O00B 1.266(6) . ?
C00X O00D 1.252(7) . ?
C00Y N00L 1.344(7) . ?
C00Y H00B 0.9300 . ?
C00Z S002 1.721(5) . ?
Gd01 O00B 2.317(3) . ?
Gd01 O00E 2.352(4) . ?
Gd01 O00C 2.376(4) . ?
Gd01 O1 2.378(3) . ?
Gd01 O00D 2.382(4) . ?
Gd01 O3 2.397(4) . ?
Gd01 O2 2.411(3) 3_666 ?
Gd01 O2 2.421(3) . ?
N1 N01L 1.145(10) . ?
N00L O2 1.356(5) . ?
C31 H31A 0.9300 . ?
O2 Gd01 2.411(3) 3_666 ?

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
C00X C1 C022 122.0(5) . . ?
C00X C1 H1A 119.0 . . ?
C022 C1 H1A 119.0 . . ?
N00L C010 C00R 120.6(6) . . ?
N00L C010 H01A 119.7 . . ?
C00R C010 H01A 119.7 . . ?
C01H C011 C00U 108.8(6) . . ?
C01H C011 H01B 125.6 . . ?
C00U C011 H01B 125.6 . . ?
C00V C012 C31 128.2(5) . . ?
C00V C012 S004 117.4(4) . . ?
C31 C012 S004 114.5(4) . . ?
C00Y C013 C00W 120.7(5) . . ?
C00Y C013 H01D 119.7 . . ?
C00W C013 H01D 119.7 . . ?
C00Z C014 C021 111.2(5) . . ?
C00Z C014 H01E 124.4 . . ?
C021 C014 H01E 124.4 . . ?
O00E C015 C016 129.2(6) . . ?
O00E C015 C01K 112.7(6) . . ?
C016 C015 C01K 118.1(6) . . ?
C015 C016 C00S 122.1(6) . . ?
C015 C016 H01F 119.0 . . ?
C00S C016 H01F 119.0 . . ?
O00C C017 C019 128.1(5) . . ?
O00C C017 C020 113.3(5) . . ?
C019 C017 C020 118.6(5) . . ?
C017 C019 C00V 122.5(5) . . ?
C017 C019 H01G 118.7 . . ?
C00V C019 H01G 118.7 . . ?
F00G C020 F00K 106.9(6) . . ?
F00G C020 F00H 106.3(6) . . ?
F00K C020 F00H 106.4(6) . . ?
F00G C020 C017 112.3(5) . . ?
F00K C020 C017 110.6(6) . . ?
F00H C020 C017 114.0(5) . . ?
C01G C021 C014 112.8(5) . . ?
C01G C021 H02A 123.6 . . ?
C014 C021 H02A 123.6 . . ?
O1 C022 C1 123.7(5) . . ?
O1 C022 C00Z 117.3(4) . . ?
C1 C022 C00Z 119.0(5) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C01C 120.1(5) . . ?
C6A C1A C01C 119.8(5) . . ?
C1A C2A C3A 120.0 . . ?
C1A C2A H2AA 120.0 . . ?
C3A C2A H2AA 120.0 . . ?
C2A C3A C4A 120.0 . . ?
C2A C3A H3AA 120.0 . . ?
C4A C3A H3AA 120.0 . . ?
C5A C4A C3A 120.0 . . ?
C5A C4A H4AA 120.0 . . ?
C3A C4A H4AA 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A H5AA 120.0 . . ?
C6A C5A H5AA 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C5A C6A H6AA 120.0 . . ?
C1A C6A H6AA 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C01C 120.1(7) . . ?
C6B C1B C01C 119.7(7) . . ?
C3B C2B C1B 120.0 . . ?
C3B C2B H2BA 120.0 . . ?
C1B C2B H2BA 120.0 . . ?
C2B C3B C4B 120.0 . . ?
C2B C3B H3BA 120.0 . . ?
C4B C3B H3BA 120.0 . . ?
C5B C4B C3B 120.0 . . ?
C5B C4B H4BA 120.0 . . ?
C3B C4B H4BA 120.0 . . ?
C4B C5B C6B 120.0 . . ?
C4B C5B H5BA 120.0 . . ?
C6B C5B H5BA 120.0 . . ?
C5B C6B C1B 120.0 . . ?
C5B C6B H6BA 120.0 . . ?
C1B C6B H6BA 120.0 . . ?
N1 C01C C1A 111.3(6) . . ?
N1 C01C C00W 116.8(6) . . ?
C1A C01C C00W 131.7(6) . . ?
N1 C01C C1B 119.5(6) . . ?
C1A C01C C1B 15.6(5) . . ?
C00W C01C C1B 122.8(7) . . ?
C01E C01D S004 113.8(5) . . ?
C01E C01D H01H 123.1 . . ?
S004 C01D H01H 123.1 . . ?
C01D C01E C31 117.9(6) . . ?
C01D C01E H01J 121.1 . . ?
C31 C01E H01J 121.1 . . ?
C021 C01G S002 113.2(5) . . ?
C021 C01G H01C 123.4 . . ?
S002 C01G H01C 123.4 . . ?
C01J C01H C011 115.3(6) . . ?
C01J C01H H01M 122.4 . . ?
C011 C01H H01M 122.4 . . ?
F1 C01I F2 111.2(6) . . ?
F1 C01I F3 104.2(6) . . ?
F2 C01I F3 104.3(5) . . ?
F1 C01I C00X 114.6(5) . . ?
F2 C01I C00X 111.2(6) . . ?
F3 C01I C00X 110.6(5) . . ?
C01H C01J S003 112.6(6) . . ?
C01H C01J H01N 123.7 . . ?
S003 C01J H01N 123.7 . . ?
F00Q C01K F00N 108.7(8) . . ?
F00Q C01K F00O 105.8(6) . . ?
F00N C01K F00O 105.5(6) . . ?
F00Q C01K C015 111.3(6) . . ?
F00N C01K C015 110.7(6) . . ?
F00O C01K C015 114.4(7) . . ?
C010 C00R C00W 120.1(6) . . ?
C010 C00R H00A 120.0 . . ?
C00W C00R H00A 120.0 . . ?
O3 C00S C016 124.3(6) . . ?
O3 C00S C00U 117.8(5) . . ?
C016 C00S C00U 117.8(5) . . ?
Cl2S C1S Cl3S 117.3(5) . . ?
Cl2S C1S Cl1S 119.4(5) . . ?
Cl3S C1S Cl1S 118.5(5) . . ?
Cl2S C1S H1SA 97.4 . . ?
Cl3S C1S H1SA 97.4 . . ?
Cl1S C1S H1SA 97.4 . . ?
Cl3T C1T Cl2T 117.2(8) . . ?
Cl3T C1T Cl1T 117.0(8) . . ?
Cl2T C1T Cl1T 116.2(8) . . ?
Cl3T C1T H1TA 100.4 . . ?
Cl2T C1T H1TA 100.4 . . ?
Cl1T C1T H1TA 100.4 . . ?
C011 C00U C00S 128.8(6) . . ?
C011 C00U S003 111.5(5) . . ?
C00S C00U S003 119.7(4) . . ?
O00B C00V C019 123.5(5) . . ?
O00B C00V C012 115.4(5) . . ?
C019 C00V C012 121.1(5) . . ?
C013 C00W C00R 117.3(5) . . ?
C013 C00W C01C 121.1(6) . . ?
C00R C00W C01C 121.6(6) . . ?
O00D C00X C1 129.6(5) . . ?
O00D C00X C01I 113.5(5) . . ?
C1 C00X C01I 116.9(5) . . ?
N00L C00Y C013 119.5(5) . . ?
N00L C00Y H00B 120.2 . . ?
C013 C00Y H00B 120.2 . . ?
C014 C00Z C022 130.0(5) . . ?
C014 C00Z S002 111.4(4) . . ?
C022 C00Z S002 118.6(4) . . ?
O00B Gd01 O00E 84.42(14) . . ?
O00B Gd01 O00C 71.99(13) . . ?
O00E Gd01 O00C 75.10(16) . . ?
O00B Gd01 O1 75.90(12) . . ?
O00E Gd01 O1 144.17(13) . . ?
O00C Gd01 O1 124.48(13) . . ?
O00B Gd01 O00D 107.67(15) . . ?
O00E Gd01 O00D 143.94(14) . . ?
O00C Gd01 O00D 76.75(14) . . ?
O1 Gd01 O00D 71.51(12) . . ?
O00B Gd01 O3 75.70(13) . . ?
O00E Gd01 O3 71.72(14) . . ?
O00C Gd01 O3 135.27(13) . . ?
O1 Gd01 O3 74.52(12) . . ?
O00D Gd01 O3 143.62(12) . . ?
O00B Gd01 O2 147.70(12) . 3_666 ?
O00E Gd01 O2 74.90(13) . 3_666 ?
O00C Gd01 O2 78.78(12) . 3_666 ?
O1 Gd01 O2 133.94(12) . 3_666 ?
O00D Gd01 O2 77.92(13) . 3_666 ?
O3 Gd01 O2 119.09(13) . 3_666 ?
O00B Gd01 O2 148.04(12) . . ?
O00E Gd01 O2 102.75(14) . . ?
O00C Gd01 O2 139.96(11) . . ?
O1 Gd01 O2 80.86(11) . . ?
O00D Gd01 O2 84.91(13) . . ?
O3 Gd01 O2 77.17(12) . . ?
O2 Gd01 O2 62.58(13) 3_666 . ?
N01L N1 C01C 178.5(9) . . ?
C010 N00L C00Y 121.7(5) . . ?
C010 N00L O2 119.2(5) . . ?
C00Y N00L O2 119.1(5) . . ?
C01E C31 C012 102.4(5) . . ?
C01E C31 H31A 128.8 . . ?
C012 C31 H31A 128.8 . . ?
C022 O1 Gd01 138.5(3) . . ?
N00L O2 Gd01 122.6(3) . 3_666 ?
N00L O2 Gd01 119.9(3) . . ?
Gd01 O2 Gd01 117.42(13) 3_666 . ?
C00S O3 Gd01 134.1(4) . . ?
C00V O00B Gd01 137.0(3) . . ?
C017 O00C Gd01 131.5(4) . . ?
C00X O00D Gd01 134.4(3) . . ?
C015 O00E Gd01 131.6(4) . . ?
C01G S002 C00Z 91.4(3) . . ?
C01J S003 C00U 91.8(3) . . ?
C01D S004 C012 91.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.51
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.366
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.132
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2d_Tb
_database_code_depnum_ccdc_archive 'CCDC 1037885'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H44 Cl6 F18 N6 O14 S6 Tb2'
_chemical_formula_weight         2306.09

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.9961(9)
_cell_length_b                   16.7164(10)
_cell_length_c                   17.1809(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.1740(7)
_cell_angle_gamma                90.00
_cell_volume                     4281.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      25.52

_exptl_crystal_description       brick
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    2.076
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            20974
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.54
_reflns_number_total             7976
_reflns_number_gt                7204
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0638P)²+16.0476P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7976
_refine_ls_number_parameters     747
_refine_ls_number_restraints     1374
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.1014
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.4906(3) 0.7194(3) 0.3496(3) 0.0379(9) Uani 1 1 d U . .
H1A H 0.5128 0.7501 0.3109 0.046 Uiso 1 1 calc R . .
C2 C 0.4617(3) 0.5146(3) 0.2984(2) 0.0370(9) Uani 1 1 d U A .
H2A H 0.5093 0.5499 0.3090 0.044 Uiso 1 1 calc R . .
C012 C 0.3241(4) 0.4072(3) 0.2694(3) 0.0448(11) Uani 1 1 d U . .
H01A H 0.2779 0.3700 0.2606 0.054 Uiso 1 1 calc R . .
C014 C 0.2009(4) 0.4784(3) 0.5638(3) 0.0496(12) Uani 1 1 d U . .
H01B H 0.1463 0.4630 0.5801 0.060 Uiso 1 1 calc R . .
C015 C 0.3654(3) 0.4183(3) 0.3435(3) 0.0421(10) Uani 1 1 d U A .
H01C H 0.3480 0.3881 0.3848 0.051 Uiso 1 1 calc R . .
C016 C 0.3506(3) 0.4513(3) 0.2066(2) 0.0427(10) Uani 1 1 d U A .
C017 C 0.3081(3) 0.7241(3) 0.6538(3) 0.0462(11) Uani 1 1 d U . .
H01D H 0.2807 0.7496 0.6931 0.055 Uiso 1 1 calc R . .
C019 C 0.3972(3) 0.7015(3) 0.6683(3) 0.0454(11) Uani 1 1 d U B .
C020 C 0.4486(4) 0.7255(4) 0.7470(3) 0.0554(13) Uani 1 1 d U . .
C021 C 0.6382(3) 0.7432(4) 0.4265(3) 0.0543(13) Uani 1 1 d U . .
C022 C 0.3073(4) 0.4413(3) 0.1276(3) 0.0512(12) Uani 1 1 d U . .
C023 C 0.2610(5) 0.4687(4) 0.7036(4) 0.0706(16) Uani 1 1 d U . .
C024 C 0.5447(3) 0.7045(3) 0.4185(3) 0.0405(10) Uani 1 1 d U B .
C1A C 0.3133(5) 0.4859(3) 0.0582(3) 0.0494(18) Uani 0.594(5) 1 d PGU A -1
C2A C 0.3117(4) 0.5690(3) 0.0608(2) 0.0396(16) Uani 0.594(5) 1 d PGU A -1
H2AA H 0.3030 0.5950 0.1072 0.048 Uiso 0.594(5) 1 calc PR A -1
C3A C 0.3232(4) 0.6131(3) -0.0060(3) 0.0468(17) Uani 0.594(5) 1 d PGU A -1
H3AA H 0.3222 0.6687 -0.0042 0.056 Uiso 0.594(5) 1 calc PR A -1
C4A C 0.3363(5) 0.5742(4) -0.0753(3) 0.061(2) Uani 0.594(5) 1 d PGU A -1
H4AA H 0.3440 0.6037 -0.1200 0.073 Uiso 0.594(5) 1 calc PR A -1
C5A C 0.3378(5) 0.4911(4) -0.0779(3) 0.071(2) Uani 0.594(5) 1 d PGU A -1
H5AA H 0.3465 0.4650 -0.1243 0.085 Uiso 0.594(5) 1 calc PR A -1
C6A C 0.3263(5) 0.4469(3) -0.0112(3) 0.066(2) Uani 0.594(5) 1 d PGU A -1
H6AA H 0.3273 0.3913 -0.0129 0.079 Uiso 0.594(5) 1 calc PR A -1
C1B C 0.3423(6) 0.4847(6) 0.0556(4) 0.044(2) Uani 0.406(5) 1 d PGU A -2
C2B C 0.2830(5) 0.5305(6) 0.0063(5) 0.056(2) Uani 0.406(5) 1 d PGU A -2
H2BA H 0.2248 0.5390 0.0185 0.067 Uiso 0.406(5) 1 calc PR A -2
C3B C 0.3106(6) 0.5635(6) -0.0614(5) 0.061(2) Uani 0.406(5) 1 d PGU A -2
H3BA H 0.2710 0.5942 -0.0944 0.073 Uiso 0.406(5) 1 calc PR A -2
C4B C 0.3975(6) 0.5508(6) -0.0797(4) 0.060(2) Uani 0.406(5) 1 d PGU A -2
H4BA H 0.4160 0.5729 -0.1250 0.072 Uiso 0.406(5) 1 calc PR A -2
C5B C 0.4568(5) 0.5050(6) -0.0305(5) 0.060(3) Uani 0.406(5) 1 d PGU A -2
H5BA H 0.5150 0.4965 -0.0427 0.072 Uiso 0.406(5) 1 calc PR A -2
C6B C 0.4292(5) 0.4719(6) 0.0372(5) 0.054(3) Uani 0.406(5) 1 d PGU A -2
H6BA H 0.4688 0.4413 0.0702 0.065 Uiso 0.406(5) 1 calc PR A -2
C11C C 0.2577(3) 0.7095(3) 0.5810(3) 0.0407(10) Uani 1 1 d U B .
C12C C 0.1655(3) 0.7392(3) 0.5648(2) 0.0420(10) Uani 1 1 d DU . .
C13C C 0.1111(7) 0.7804(9) 0.6108(5) 0.0529(19) Uani 0.825(6) 1 d PDU B 1
H13A H 0.1293 0.7960 0.6620 0.063 Uiso 0.825(6) 1 calc PR B 1
C14C C 0.0265(6) 0.7963(7) 0.5727(4) 0.0578(17) Uani 0.825(6) 1 d PDU B 1
H14A H -0.0190 0.8214 0.5964 0.069 Uiso 0.825(6) 1 calc PR B 1
C15C C 0.0175(5) 0.7712(5) 0.4968(4) 0.0544(17) Uani 0.825(6) 1 d PDU B 1
H15A H -0.0337 0.7793 0.4620 0.065 Uiso 0.825(6) 1 calc PR B 1
C13D C 0.1100(14) 0.716(2) 0.4994(13) 0.049(3) Uani 0.175(6) 1 d PDU B 2
H13B H 0.1261 0.6796 0.4623 0.058 Uiso 0.175(6) 1 calc PR B 2
C14D C 0.0267(18) 0.753(3) 0.4959(16) 0.053(3) Uani 0.175(6) 1 d PDU B 2
H14B H -0.0194 0.7455 0.4560 0.063 Uiso 0.175(6) 1 calc PR B 2
C15D C 0.021(3) 0.803(3) 0.5581(17) 0.055(3) Uani 0.175(6) 1 d PDU B 2
H15B H -0.0233 0.8413 0.5607 0.066 Uiso 0.175(6) 1 calc PR B 2
C11E C 0.2068(3) 0.4902(3) 0.4829(3) 0.0415(10) Uani 1 1 d U C .
C12E C 0.1284(3) 0.4696(3) 0.4273(3) 0.0440(10) Uani 1 1 d DU . .
C13E C 0.0493(5) 0.4313(6) 0.4394(5) 0.0555(17) Uani 0.893(6) 1 d PDU C 1
H13C H 0.0365 0.4139 0.4884 0.067 Uiso 0.893(6) 1 calc PR C 1
C14E C -0.0090(4) 0.4214(7) 0.3721(5) 0.061(2) Uani 0.893(6) 1 d PDU C 1
H14C H -0.0638 0.3950 0.3707 0.073 Uiso 0.893(6) 1 calc PR C 1
C15E C 0.0223(4) 0.4542(4) 0.3082(4) 0.0578(18) Uani 0.893(6) 1 d PDU C 1
H15E H -0.0086 0.4539 0.2583 0.069 Uiso 0.893(6) 1 calc PR C 1
C13F C 0.118(3) 0.479(4) 0.3472(9) 0.053(3) Uani 0.107(6) 1 d PDU C 2
H13D H 0.1638 0.4891 0.3162 0.063 Uiso 0.107(6) 1 calc PR C 2
C14F C 0.028(3) 0.471(5) 0.320(2) 0.056(3) Uani 0.107(6) 1 d PDU C 2
H14D H 0.0018 0.4905 0.2724 0.067 Uiso 0.107(6) 1 calc PR C 2
C15F C -0.019(3) 0.430(7) 0.371(3) 0.058(3) Uani 0.107(6) 1 d PDU C 2
H15F H -0.0779 0.4138 0.3603 0.070 Uiso 0.107(6) 1 calc PR C 2
C11G C 0.4021(3) 0.6887(3) 0.3367(2) 0.0321(8) Uani 1 1 d U C .
C12G C 0.3465(3) 0.7095(3) 0.2641(2) 0.0357(9) Uani 1 1 d DU . .
C13G C 0.3659(4) 0.7544(4) 0.2006(3) 0.0411(12) Uani 0.951(5) 1 d PDU D 1
H13E H 0.4211 0.7790 0.1977 0.049 Uiso 0.951(5) 1 calc PR D 1
C14G C 0.2947(4) 0.7593(4) 0.1413(3) 0.0490(17) Uani 0.951(5) 1 d PDU D 1
H14E H 0.2974 0.7872 0.0947 0.059 Uiso 0.951(5) 1 calc PR D 1
C15G C 0.2215(4) 0.7190(4) 0.1595(3) 0.0562(18) Uani 0.951(5) 1 d PDU D 1
H15I H 0.1680 0.7159 0.1268 0.067 Uiso 0.951(5) 1 calc PR D 1
C13H C 0.256(2) 0.697(7) 0.247(6) 0.046(3) Uani 0.049(5) 1 d PDU D 2
H13F H 0.2214 0.6666 0.2779 0.055 Uiso 0.049(5) 1 calc PR D 2
C14H C 0.221(3) 0.734(8) 0.178(5) 0.049(3) Uani 0.049(5) 1 d PDU D 2
H14F H 0.1608 0.7321 0.1579 0.058 Uiso 0.049(5) 1 calc PR D 2
C15H C 0.284(4) 0.775(10) 0.143(6) 0.048(3) Uani 0.049(5) 1 d PDU D 2
H15G H 0.2740 0.8002 0.0949 0.058 Uiso 0.049(5) 1 calc PR D 2
C1S C 0.4645(4) 0.9330(5) 0.6207(6) 0.095(3) Uani 0.687(7) 1 d PDU E 1
H1SA H 0.4504 0.9115 0.6710 0.114 Uiso 0.687(7) 1 calc PR E 1
C1T C 0.4854(8) 0.9480(8) 0.5668(8) 0.067(4) Uani 0.313(7) 1 d PDU E 2
H1TA H 0.4778 0.9798 0.5186 0.080 Uiso 0.313(7) 1 calc PR E 2
C00U C 0.4219(3) 0.5048(3) 0.2226(2) 0.0401(10) Uani 1 1 d U . .
H00A H 0.4426 0.5339 0.1821 0.048 Uiso 1 1 calc R A .
C00Z C 0.2726(4) 0.4888(3) 0.6184(3) 0.0539(12) Uani 1 1 d U B .
Cl1S Cl 0.4011(3) 1.0214(2) 0.59958(19) 0.1050(14) Uani 0.687(7) 1 d PDU E 1
Cl2S Cl 0.4362(3) 0.8617(2) 0.5478(3) 0.1054(13) Uani 0.687(7) 1 d PDU E 1
Cl3S Cl 0.58123(18) 0.9567(2) 0.62798(17) 0.0694(8) Uani 0.687(7) 1 d PDU E 1
Cl1T Cl 0.3945(7) 0.9641(9) 0.6242(7) 0.152(4) Uani 0.313(7) 1 d PDU E 2
Cl2T Cl 0.4877(9) 0.8438(6) 0.5454(7) 0.139(4) Uani 0.313(7) 1 d PDU E 2
Cl3T Cl 0.5865(8) 0.9735(11) 0.6247(12) 0.211(8) Uani 0.313(7) 1 d PDU E 2
F00G F 0.3984(3) 0.7622(3) 0.7950(2) 0.0890(14) Uani 1 1 d U . .
F00H F 0.4840(3) 0.6638(2) 0.78482(19) 0.0842(13) Uani 1 1 d U . .
F00J F 0.5150(3) 0.7748(3) 0.7359(2) 0.0958(14) Uani 1 1 d U . .
F00N F 0.2627(3) 0.5336(3) 0.7470(2) 0.0950(14) Uani 1 1 d U . .
F00P F 0.1845(3) 0.4318(3) 0.7144(3) 0.0998(15) Uani 1 1 d U . .
F00Q F 0.3258(3) 0.4206(3) 0.7341(3) 0.1050(17) Uani 1 1 d U . .
N1 N 0.2469(4) 0.3855(4) 0.1166(3) 0.0713(14) Uani 1 1 d U A .
N00K N 0.4309(2) 0.4727(2) 0.35654(19) 0.0360(8) Uani 1 1 d U . .
N01N N 0.1935(6) 0.3359(5) 0.1058(4) 0.108(2) Uani 1 1 d U . .
O1 O 0.2752(2) 0.51694(19) 0.45518(18) 0.0379(7) Uani 1 1 d U . .
O2 O 0.4672(2) 0.48642(19) 0.43124(15) 0.0365(7) Uani 1 1 d U . .
O3 O 0.36776(18) 0.64298(18) 0.38346(16) 0.0327(6) Uani 1 1 d U . .
O009 O 0.2878(2) 0.6724(2) 0.52533(17) 0.0408(7) Uani 1 1 d U . .
O00A O 0.3504(2) 0.5152(2) 0.60985(19) 0.0500(9) Uani 1 1 d U . .
O00D O 0.5279(2) 0.6658(2) 0.47771(18) 0.0412(7) Uani 1 1 d U . .
F3 F 0.7003(2) 0.6927(2) 0.4570(3) 0.0766(11) Uani 1 1 d U . .
O00F O 0.4449(2) 0.6638(2) 0.62412(18) 0.0444(8) Uani 1 1 d U . .
F2 F 0.6622(2) 0.7755(3) 0.3620(2) 0.0859(13) Uani 1 1 d U . .
F1 F 0.6421(3) 0.8043(2) 0.4783(2) 0.0792(11) Uani 1 1 d U . .
S16C S 0.11161(10) 0.72281(11) 0.47314(10) 0.0445(5) Uani 0.825(6) 1 d PDU B 1
S16D S 0.1067(9) 0.7859(11) 0.6309(7) 0.050(2) Uani 0.175(6) 1 d PDU B 2
S16E S 0.12593(11) 0.49660(11) 0.33077(10) 0.0517(5) Uani 0.893(6) 1 d PDU C 1
S16F S 0.0454(13) 0.4124(12) 0.4583(13) 0.062(4) Uani 0.107(6) 1 d PDU C 2
S16G S 0.23861(9) 0.67401(9) 0.24959(8) 0.0460(5) Uani 0.951(5) 1 d PDU D 1
S16H S 0.386(2) 0.774(2) 0.1994(18) 0.044(4) Uani 0.049(5) 1 d PDU D 2
Tb01 Tb 0.405660(13) 0.587747(13) 0.509195(10) 0.03324(9) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 C024 1.383(6) . ?
C1 C11G 1.418(6) . ?
C2 N00K 1.341(6) . ?
C2 C00U 1.383(6) . ?
C012 C015 1.368(7) . ?
C012 C016 1.399(7) . ?
C014 C00Z 1.359(8) . ?
C014 C11E 1.416(7) . ?
C015 N00K 1.340(6) . ?
C016 C00U 1.398(7) . ?
C016 C022 1.450(6) . ?
C017 C019 1.386(7) . ?
C017 C11C 1.411(7) . ?
C019 O00F 1.266(6) . ?
C019 C020 1.535(7) . ?
C020 F00H 1.301(7) . ?
C020 F00G 1.326(6) . ?
C020 F00J 1.322(8) . ?
C021 F2 1.317(7) . ?
C021 F3 1.324(7) . ?
C021 F1 1.351(7) . ?
C021 C024 1.537(7) . ?
C022 N1 1.301(8) . ?
C022 C1A 1.417(7) . ?
C022 C1B 1.572(8) . ?
C023 F00N 1.316(9) . ?
C023 F00P 1.332(9) . ?
C023 F00Q 1.325(7) . ?
C023 C00Z 1.531(7) . ?
C024 O00D 1.254(6) . ?
C1A C2A 1.3900 . ?
C1A C6A 1.3900 . ?
C2A C3A 1.3900 . ?
C3A C4A 1.3900 . ?
C4A C5A 1.3900 . ?
C5A C6A 1.3900 . ?
C1B C2B 1.3900 . ?
C1B C6B 1.3900 . ?
C2B C3B 1.3900 . ?
C3B C4B 1.3900 . ?
C4B C5B 1.3900 . ?
C5B C6B 1.3900 . ?
C11C O009 1.262(5) . ?
C11C C12C 1.468(6) . ?
C12C C13C 1.379(8) . ?
C12C C13D 1.381(10) . ?
C12C S16D 1.701(8) . ?
C12C S16C 1.713(4) . ?
C13C C14C 1.390(8) . ?
C14C C15C 1.363(7) . ?
C15C S16C 1.713(6) . ?
C13D C14D 1.392(11) . ?
C14D C15D 1.362(9) . ?
C15D S16D 1.717(9) . ?
C11E O1 1.258(6) . ?
C11E C12E 1.474(7) . ?
C12E C13F 1.378(10) . ?
C12E C13E 1.382(8) . ?
C12E S16F 1.701(8) . ?
C12E S16E 1.716(5) . ?
C13E C14E 1.384(8) . ?
C14E C15E 1.356(7) . ?
C15E S16E 1.714(6) . ?
C13F C14F 1.390(10) . ?
C14F C15F 1.357(9) . ?
C15F S16F 1.714(9) . ?
C11G O3 1.258(5) . ?
C11G C12G 1.466(5) . ?
C12G C13H 1.379(11) . ?
C12G C13G 1.379(7) . ?
C12G S16H 1.702(9) . ?
C12G S16G 1.717(4) . ?
C13G C14G 1.397(7) . ?
C14G C15G 1.354(6) . ?
C15G S16G 1.716(5) . ?
C13H C14H 1.391(11) . ?
C14H C15H 1.358(9) . ?
C15H S16H 1.715(9) . ?
C1S Cl2S 1.748(7) . ?
C1S Cl1S 1.774(7) . ?
C1S Cl3S 1.786(7) . ?
C1T Cl3T 1.773(8) . ?
C1T Cl2T 1.782(8) . ?
C1T Cl1T 1.787(8) . ?
C00Z O00A 1.271(7) . ?
N1 N01N 1.153(9) . ?
N00K O2 1.359(4) . ?
O1 Tb01 2.388(3) . ?
O2 Tb01 2.404(3) . ?
O2 Tb01 2.408(3) 3_666 ?
O3 Tb01 2.362(3) . ?
O009 Tb01 2.305(3) . ?
O00A Tb01 2.336(3) . ?
O00D Tb01 2.360(3) . ?
O00F Tb01 2.369(3) . ?
Tb01 O2 2.408(3) 3_666 ?

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
C024 C1 C11G 121.5(4) . . ?
N00K C2 C00U 119.4(5) . . ?
C015 C012 C016 120.5(5) . . ?
C00Z C014 C11E 122.0(5) . . ?
N00K C015 C012 119.9(5) . . ?
C00U C016 C012 117.4(4) . . ?
C00U C016 C022 120.9(5) . . ?
C012 C016 C022 121.7(5) . . ?
C019 C017 C11C 121.7(4) . . ?
O00F C019 C017 128.6(5) . . ?
O00F C019 C020 113.3(4) . . ?
C017 C019 C020 118.1(4) . . ?
F00H C020 F00G 106.4(5) . . ?
F00H C020 F00J 107.0(5) . . ?
F00G C020 F00J 106.7(5) . . ?
F00H C020 C019 111.9(5) . . ?
F00G C020 C019 113.8(5) . . ?
F00J C020 C019 110.6(5) . . ?
F2 C021 F3 110.4(5) . . ?
F2 C021 F1 104.4(5) . . ?
F3 C021 F1 104.1(4) . . ?
F2 C021 C024 115.2(4) . . ?
F3 C021 C024 111.3(5) . . ?
F1 C021 C024 110.6(5) . . ?
N1 C022 C1A 111.2(5) . . ?
N1 C022 C016 116.9(5) . . ?
C1A C022 C016 131.7(5) . . ?
N1 C022 C1B 120.2(5) . . ?
C1A C022 C1B 16.0(4) . . ?
C016 C022 C1B 122.1(6) . . ?
F00N C023 F00P 105.5(5) . . ?
F00N C023 F00Q 107.9(6) . . ?
F00P C023 F00Q 105.7(6) . . ?
F00N C023 C00Z 111.3(5) . . ?
F00P C023 C00Z 115.0(6) . . ?
F00Q C023 C00Z 110.9(5) . . ?
O00D C024 C1 129.5(4) . . ?
O00D C024 C021 113.9(4) . . ?
C1 C024 C021 116.5(4) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C022 119.7(4) . . ?
C6A C1A C022 120.2(4) . . ?
C1A C2A C3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C022 119.2(6) . . ?
C6B C1B C022 120.6(6) . . ?
C1B C2B C3B 120.0 . . ?
C2B C3B C4B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C6B C5B C4B 120.0 . . ?
C5B C6B C1B 120.0 . . ?
O009 C11C C017 123.8(4) . . ?
O009 C11C C12C 115.3(4) . . ?
C017 C11C C12C 120.8(4) . . ?
C13C C12C C13D 105.4(10) . . ?
C13C C12C C11C 131.6(5) . . ?
C13D C12C C11C 122.1(9) . . ?
C13C C12C S16D 6.9(8) . . ?
C13D C12C S16D 111.3(8) . . ?
C11C C12C S16D 125.0(5) . . ?
C13C C12C S16C 110.9(4) . . ?
C13D C12C S16C 12.4(18) . . ?
C11C C12C S16C 117.5(3) . . ?
S16D C12C S16C 117.4(5) . . ?
C12C C13C C14C 113.1(6) . . ?
C15C C14C C13C 112.5(6) . . ?
C14C C15C S16C 111.9(5) . . ?
C12C C13D C14D 111.5(9) . . ?
C15D C14D C13D 111.8(9) . . ?
C14D C15D S16D 111.5(8) . . ?
O1 C11E C014 124.1(5) . . ?
O1 C11E C12E 117.6(4) . . ?
C014 C11E C12E 118.3(4) . . ?
C13F C12E C13E 101.2(13) . . ?
C13F C12E C11E 128.2(12) . . ?
C13E C12E C11E 130.4(5) . . ?
C13F C12E S16F 111.6(9) . . ?
C13E C12E S16F 12.6(10) . . ?
C11E C12E S16F 119.2(9) . . ?
C13F C12E S16E 10.2(19) . . ?
C13E C12E S16E 109.7(4) . . ?
C11E C12E S16E 119.9(3) . . ?
S16F C12E S16E 120.7(9) . . ?
C12E C13E C14E 114.0(6) . . ?
C15E C14E C13E 112.6(5) . . ?
C14E C15E S16E 111.6(5) . . ?
C12E C13F C14F 109(2) . . ?
C15F C14F C13F 112.3(9) . . ?
C14F C15F S16F 112.0(8) . . ?
O3 C11G C1 124.0(4) . . ?
O3 C11G C12G 117.0(4) . . ?
C1 C11G C12G 118.9(4) . . ?
C13H C12G C13G 101.6(17) . . ?
C13H C12G C11G 127(2) . . ?
C13G C12G C11G 130.8(4) . . ?
C13H C12G S16H 111.3(9) . . ?
C13G C12G S16H 11.8(13) . . ?
C11G C12G S16H 120.0(12) . . ?
C13H C12G S16G 12(4) . . ?
C13G C12G S16G 110.5(3) . . ?
C11G C12G S16G 118.8(3) . . ?
S16H C12G S16G 121.0(12) . . ?
C12G C13G C14G 113.5(5) . . ?
C15G C14G C13G 112.2(4) . . ?
C14G C15G S16G 112.3(4) . . ?
C12G C13H C14H 112.7(11) . . ?
C15H C14H C13H 112.4(9) . . ?
C14H C15H S16H 112.0(8) . . ?
Cl2S C1S Cl1S 109.8(5) . . ?
Cl2S C1S Cl3S 111.3(5) . . ?
Cl1S C1S Cl3S 109.2(5) . . ?
Cl3T C1T Cl2T 108.4(7) . . ?
Cl3T C1T Cl1T 108.1(7) . . ?
Cl2T C1T Cl1T 107.1(6) . . ?
C2 C00U C016 120.3(4) . . ?
O00A C00Z C014 129.3(5) . . ?
O00A C00Z C023 112.8(5) . . ?
C014 C00Z C023 117.9(5) . . ?
N01N N1 C022 179.1(6) . . ?
C2 N00K O2 118.7(4) . . ?
C2 N00K C015 122.3(4) . . ?
O2 N00K C015 119.0(4) . . ?
C11E O1 Tb01 134.1(3) . . ?
N00K O2 Tb01 120.4(2) . . ?
N00K O2 Tb01 122.2(2) . 3_666 ?
Tb01 O2 Tb01 117.38(10) . 3_666 ?
C11G O3 Tb01 138.3(3) . . ?
C11C O009 Tb01 137.1(3) . . ?
C00Z O00A Tb01 132.0(3) . . ?
C024 O00D Tb01 134.4(3) . . ?
C019 O00F Tb01 131.4(3) . . ?
C15C S16C C12C 91.5(3) . . ?
C12C S16D C15D 89.4(8) . . ?
C15E S16E C12E 92.0(3) . . ?
C12E S16F C15F 89.4(11) . . ?
C15G S16G C12G 91.5(2) . . ?
C12G S16H C15H 91.1(9) . . ?
O009 Tb01 O00A 83.80(12) . . ?
O009 Tb01 O3 75.98(10) . . ?
O00A Tb01 O3 144.15(11) . . ?
O009 Tb01 O00D 108.23(13) . . ?
O00A Tb01 O00D 143.40(12) . . ?
O3 Tb01 O00D 71.98(10) . . ?
O009 Tb01 O00F 72.25(11) . . ?
O00A Tb01 O00F 74.80(13) . . ?
O3 Tb01 O00F 124.48(11) . . ?
O00D Tb01 O00F 76.38(12) . . ?
O009 Tb01 O1 75.16(11) . . ?
O00A Tb01 O1 71.90(12) . . ?
O3 Tb01 O1 74.44(10) . . ?
O00D Tb01 O1 144.04(10) . . ?
O00F Tb01 O1 135.22(11) . . ?
O009 Tb01 O2 147.69(10) . . ?
O00A Tb01 O2 103.57(12) . . ?
O3 Tb01 O2 80.50(10) . . ?
O00D Tb01 O2 84.70(11) . . ?
O00F Tb01 O2 140.04(10) . . ?
O1 Tb01 O2 77.41(10) . . ?
O009 Tb01 O2 147.95(10) . 3_666 ?
O00A Tb01 O2 75.26(11) . 3_666 ?
O3 Tb01 O2 133.76(10) . 3_666 ?
O00D Tb01 O2 77.47(11) . 3_666 ?
O00F Tb01 O2 78.92(10) . 3_666 ?
O1 Tb01 O2 119.23(11) . 3_666 ?
O2 Tb01 O2 62.62(10) . 3_666 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.54
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.101
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3d_Dy
_database_code_depnum_ccdc_archive 'CCDC 1037886'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H44 Cl6 Dy2 F18 N6 O14 S6'
_chemical_formula_weight         2312.24

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.9627(13)
_cell_length_b                   16.7262(15)
_cell_length_c                   17.1610(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0290(11)
_cell_angle_gamma                90.00
_cell_volume                     4271.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       brick
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    2.174
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            23726
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         27.19
_reflns_number_total             9382
_reflns_number_gt                8026
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0492P)²+11.0039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9382
_refine_ls_number_parameters     741
_refine_ls_number_restraints     1365
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C2 C 0.5090(3) 0.2809(3) 0.6494(2) 0.0386(9) Uani 1 1 d U . .
H2A H 0.4866 0.2500 0.6880 0.046 Uiso 1 1 calc R . .
C011 C 0.7270(4) 0.5113(3) 0.3818(3) 0.0561(13) Uani 1 1 d U B .
C012 C 0.6755(3) 0.5930(3) 0.7305(3) 0.0476(11) Uani 1 1 d U . .
H01A H 0.7216 0.6303 0.7393 0.057 Uiso 1 1 calc R . .
C013 C 0.6033(3) 0.2991(3) 0.3325(2) 0.0459(10) Uani 1 1 d U B .
C015 C 0.6340(3) 0.5823(3) 0.6561(2) 0.0440(10) Uani 1 1 d U A .
H01B H 0.6509 0.6130 0.6149 0.053 Uiso 1 1 calc R . .
C018 C 0.7983(3) 0.5216(3) 0.4362(3) 0.0541(12) Uani 1 1 d U . .
H01D H 0.8530 0.5371 0.4196 0.065 Uiso 1 1 calc R . .
C019 C 0.6921(3) 0.2764(3) 0.3470(3) 0.0483(11) Uani 1 1 d U . .
H01E H 0.7198 0.2511 0.3077 0.058 Uiso 1 1 calc R . .
C20 C 0.6495(3) 0.5491(3) 0.7929(2) 0.0438(10) Uani 1 1 d U A .
C21 C 0.6929(4) 0.5590(3) 0.8717(2) 0.0528(12) Uani 1 1 d U . .
C1A C 0.6880(5) 0.5145(3) 0.9416(3) 0.051(2) Uani 0.595(5) 1 d PGU A -1
C2A C 0.6889(3) 0.4315(3) 0.9388(2) 0.0388(15) Uani 0.595(5) 1 d PGU A -1
H2AA H 0.6971 0.4055 0.8922 0.047 Uiso 0.595(5) 1 calc PR A -1
C3A C 0.6776(4) 0.3873(3) 1.0057(3) 0.0483(18) Uani 0.595(5) 1 d PGU A -1
H3AA H 0.6782 0.3317 1.0038 0.058 Uiso 0.595(5) 1 calc PR A -1
C4A C 0.6653(5) 0.4262(4) 1.0754(2) 0.063(3) Uani 0.595(5) 1 d PGU A -1
H4AA H 0.6577 0.3966 1.1201 0.075 Uiso 0.595(5) 1 calc PR A -1
C5A C 0.6644(5) 0.5092(4) 1.0782(3) 0.083(3) Uani 0.595(5) 1 d PGU A -1
H5AA H 0.6562 0.5352 1.1248 0.100 Uiso 0.595(5) 1 calc PR A -1
C6A C 0.6757(6) 0.5534(3) 1.0113(3) 0.074(3) Uani 0.595(5) 1 d PGU A -1
H6AA H 0.6751 0.6090 1.0132 0.089 Uiso 0.595(5) 1 calc PR A -1
C1B C 0.6583(5) 0.5160(6) 0.9444(4) 0.039(3) Uani 0.405(5) 1 d PGU A -2
C2B C 0.7181(4) 0.4708(6) 0.9939(5) 0.061(3) Uani 0.405(5) 1 d PGU A -2
H2BA H 0.7765 0.4628 0.9817 0.073 Uiso 0.405(5) 1 calc PR A -2
C3B C 0.6905(6) 0.4375(6) 1.0616(5) 0.063(3) Uani 0.405(5) 1 d PGU A -2
H3BA H 0.7304 0.4073 1.0947 0.076 Uiso 0.405(5) 1 calc PR A -2
C4B C 0.6031(6) 0.4495(6) 1.0799(4) 0.058(3) Uani 0.405(5) 1 d PGU A -2
H4BA H 0.5847 0.4272 1.1252 0.070 Uiso 0.405(5) 1 calc PR A -2
C5B C 0.5434(4) 0.4946(6) 1.0304(5) 0.066(3) Uani 0.405(5) 1 d PGU A -2
H5BA H 0.4849 0.5026 1.0426 0.079 Uiso 0.405(5) 1 calc PR A -2
C6B C 0.5710(5) 0.5279(6) 0.9627(4) 0.056(3) Uani 0.405(5) 1 d PGU A -2
H6BA H 0.5310 0.5581 0.9295 0.067 Uiso 0.405(5) 1 calc PR A -2
C22 C 0.5524(4) 0.2747(4) 0.2539(3) 0.0577(13) Uani 1 1 d U . .
N1 N 0.7542(4) 0.6142(4) 0.8824(2) 0.0763(15) Uani 1 1 d U A .
C1C C 0.7421(3) 0.2907(3) 0.4203(2) 0.0420(9) Uani 1 1 d U B .
C2C C 0.8344(3) 0.2611(3) 0.4361(2) 0.0440(10) Uani 1 1 d DU . .
C3C C 0.8881(7) 0.2204(8) 0.3906(5) 0.053(2) Uani 0.802(6) 1 d PDU B 1
H3CA H 0.8706 0.2071 0.3386 0.064 Uiso 0.802(6) 1 calc PR B 1
C4C C 0.9723(5) 0.2004(8) 0.4293(5) 0.061(2) Uani 0.802(6) 1 d PDU B 1
H4CA H 1.0163 0.1721 0.4065 0.073 Uiso 0.802(6) 1 calc PR B 1
C5C C 0.9815(5) 0.2276(5) 0.5045(4) 0.056(2) Uani 0.802(6) 1 d PDU B 1
H5CA H 1.0329 0.2200 0.5392 0.067 Uiso 0.802(6) 1 calc PR B 1
C3D C 0.8861(16) 0.2781(17) 0.5042(10) 0.049(5) Uani 0.198(6) 1 d PDU B 2
H3DA H 0.8654 0.3061 0.5455 0.059 Uiso 0.198(6) 1 calc PR B 2
C4D C 0.9737(18) 0.249(2) 0.5050(14) 0.055(5) Uani 0.198(6) 1 d PDU B 2
H4DA H 1.0183 0.2557 0.5465 0.066 Uiso 0.198(6) 1 calc PR B 2
C5D C 0.9856(18) 0.209(3) 0.4379(18) 0.056(5) Uani 0.198(6) 1 d PDU B 2
H5DA H 1.0384 0.1823 0.4297 0.067 Uiso 0.198(6) 1 calc PR B 2
C1E C 0.7929(3) 0.5097(3) 0.5172(3) 0.0433(10) Uani 1 1 d U C .
C2E C 0.8708(3) 0.5307(3) 0.5727(3) 0.0470(10) Uani 1 1 d DU . .
C3E C 0.9485(6) 0.5681(6) 0.5603(6) 0.060(2) Uani 0.846(6) 1 d PDU C 1
H3EA H 0.9601 0.5862 0.5111 0.072 Uiso 0.846(6) 1 calc PR C 1
C4E C 1.0097(5) 0.5773(7) 0.6267(5) 0.064(2) Uani 0.846(6) 1 d PDU C 1
H4EA H 1.0650 0.6028 0.6271 0.077 Uiso 0.846(6) 1 calc PR C 1
C5E C 0.9784(4) 0.5443(7) 0.6910(4) 0.0618(19) Uani 0.846(6) 1 d PDU C 1
H5EA H 1.0102 0.5438 0.7406 0.074 Uiso 0.846(6) 1 calc PR C 1
C3F C 0.880(2) 0.512(2) 0.6500(9) 0.056(6) Uani 0.154(6) 1 d PDU C 2
H3FA H 0.8380 0.4821 0.6746 0.068 Uiso 0.154(6) 1 calc PR C 2
C4F C 0.959(3) 0.543(4) 0.6877(13) 0.062(5) Uani 0.154(6) 1 d PDU C 2
H4FA H 0.9776 0.5363 0.7408 0.075 Uiso 0.154(6) 1 calc PR C 2
C5F C 1.007(3) 0.584(4) 0.6381(17) 0.063(6) Uani 0.154(6) 1 d PDU C 2
H5FA H 1.0620 0.6081 0.6537 0.075 Uiso 0.154(6) 1 calc PR C 2
C1G C 0.5975(2) 0.3119(2) 0.6623(2) 0.0336(8) Uani 1 1 d U D .
C2G C 0.6528(2) 0.2907(2) 0.7351(2) 0.0360(8) Uani 1 1 d DU . .
C3G C 0.6333(4) 0.2465(5) 0.7977(4) 0.0412(13) Uani 0.943(5) 1 d PDU D 1
H3GA H 0.5781 0.2217 0.8002 0.049 Uiso 0.943(5) 1 calc PR D 1
C4G C 0.7042(4) 0.2415(4) 0.8583(3) 0.0515(16) Uani 0.943(5) 1 d PDU D 1
H4GA H 0.7011 0.2140 0.9050 0.062 Uiso 0.943(5) 1 calc PR D 1
C5G C 0.7777(4) 0.2820(4) 0.8396(3) 0.0591(19) Uani 0.943(5) 1 d PDU D 1
H5GA H 0.8312 0.2852 0.8722 0.071 Uiso 0.943(5) 1 calc PR D 1
C3H C 0.7416(14) 0.308(4) 0.750(3) 0.047(6) Uani 0.057(5) 1 d PDU D 2
H3HA H 0.7737 0.3395 0.7185 0.056 Uiso 0.057(5) 1 calc PR D 2
C4H C 0.778(3) 0.272(7) 0.820(4) 0.049(6) Uani 0.057(5) 1 d PDU D 2
H4HA H 0.8385 0.2771 0.8400 0.059 Uiso 0.057(5) 1 calc PR D 2
C5H C 0.717(3) 0.230(7) 0.856(4) 0.049(6) Uani 0.057(5) 1 d PDU D 2
H5HA H 0.7296 0.2041 0.9031 0.058 Uiso 0.057(5) 1 calc PR D 2
C01L C 0.3617(3) 0.2571(4) 0.5722(3) 0.0589(13) Uani 1 1 d U . .
C01N C 0.7382(5) 0.5307(5) 0.2964(3) 0.0754(18) Uani 1 1 d U . .
C00P C 0.5383(3) 0.4856(3) 0.7014(2) 0.0386(9) Uani 1 1 d U A .
H00A H 0.4906 0.4503 0.6910 0.046 Uiso 1 1 calc R . .
C00Q C 0.4555(3) 0.2958(3) 0.5803(2) 0.0414(9) Uani 1 1 d U B .
C00S C 0.5781(3) 0.4954(3) 0.7772(2) 0.0412(10) Uani 1 1 d U . .
H00D H 0.5574 0.4662 0.8178 0.049 Uiso 1 1 calc R A .
C1S C 0.4691(5) 0.9382(5) 0.6105(9) 0.146(4) Uani 0.767(4) 1 d PDU E 1
H1SA H 0.4551 0.9170 0.6611 0.175 Uiso 0.767(4) 1 calc PR E 1
C1T C 0.4673(14) 0.9382(10) 0.5590(15) 0.146(4) Uani 0.233(4) 1 d PDU . 2
H1TA H 0.4292 0.9506 0.5105 0.175 Uiso 0.233(4) 1 calc PR E 2
Cl1S Cl 0.4368(3) 0.8621(2) 0.5486(2) 0.1198(12) Uani 0.767(4) 1 d PDU E 1
Cl2S Cl 0.58236(13) 0.95717(14) 0.62813(12) 0.0749(7) Uani 0.767(4) 1 d PDU E 1
Cl3S Cl 0.4022(2) 1.0220(2) 0.60014(18) 0.1262(14) Uani 0.767(4) 1 d PDU E 1
Cl1T Cl 0.4947(9) 0.8409(9) 0.5438(9) 0.163(6) Uani 0.233(4) 1 d PDU E 2
Cl2T Cl 0.5510(16) 1.0067(11) 0.5566(18) 0.352(15) Uani 0.233(4) 1 d PDU . 2
Cl3T Cl 0.3946(8) 0.9534(10) 0.6280(8) 0.152(5) Uani 0.233(4) 1 d PDU E 2
Dy01 Dy 0.594239(12) 0.412824(12) 0.490725(9) 0.03553(8) Uani 1 1 d U . .
F1 F 0.3369(2) 0.2254(3) 0.6365(2) 0.0887(12) Uani 1 1 d U . .
F2 F 0.29975(19) 0.3076(2) 0.5412(2) 0.0800(10) Uani 1 1 d U . .
F3 F 0.3585(2) 0.1962(2) 0.5203(2) 0.0824(11) Uani 1 1 d U . .
F00I F 0.6024(3) 0.2379(3) 0.20597(19) 0.0951(14) Uani 1 1 d U . .
F00K F 0.5170(3) 0.3366(2) 0.21571(17) 0.0910(13) Uani 1 1 d U . .
F00M F 0.4853(3) 0.2265(3) 0.2648(2) 0.0966(13) Uani 1 1 d U . .
F00N F 0.8158(3) 0.5672(3) 0.2853(2) 0.1049(15) Uani 1 1 d U . .
F00V F 0.6741(3) 0.5794(3) 0.2664(2) 0.1144(18) Uani 1 1 d U . .
F00W F 0.7360(3) 0.4662(3) 0.2533(2) 0.1050(15) Uani 1 1 d U . .
N00J N 0.5690(2) 0.5274(2) 0.64294(17) 0.0379(8) Uani 1 1 d U . .
N01M N 0.8072(5) 0.6636(5) 0.8933(3) 0.115(3) Uani 1 1 d U . .
O1 O 0.63204(17) 0.35743(17) 0.61565(15) 0.0342(6) Uani 1 1 d U . .
O2 O 0.72429(18) 0.48323(18) 0.54498(16) 0.0397(6) Uani 1 1 d U . .
O3 O 0.53279(18) 0.51380(19) 0.56847(14) 0.0392(7) Uani 1 1 d U . .
O009 O 0.71178(19) 0.32817(19) 0.47559(16) 0.0421(7) Uani 1 1 d U . .
O00C O 0.6490(2) 0.4850(2) 0.39090(17) 0.0534(8) Uani 1 1 d U . .
O00E O 0.5554(2) 0.3369(2) 0.37654(16) 0.0470(8) Uani 1 1 d U . .
O00F O 0.47321(19) 0.3345(2) 0.52156(16) 0.0428(7) Uani 1 1 d U . .
S1C S 0.88833(12) 0.27724(13) 0.52817(11) 0.0460(5) Uani 0.802(6) 1 d PDU B 1
S1D S 0.8934(8) 0.2129(10) 0.3702(7) 0.055(3) Uani 0.198(6) 1 d PDU B 2
S1E S 0.87336(12) 0.50386(13) 0.66963(11) 0.0519(5) Uani 0.846(6) 1 d PDU C 1
S1F S 0.9565(11) 0.5871(10) 0.5443(12) 0.075(4) Uani 0.154(6) 1 d PDU C 2
S1G S 0.76116(8) 0.32645(8) 0.74964(7) 0.0476(4) Uani 0.943(5) 1 d PDU D 1
S1H S 0.613(2) 0.231(2) 0.8039(18) 0.046(6) Uani 0.057(5) 1 d PDU D 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
C2 C00Q 1.380(5) . ?
C2 C1G 1.417(5) . ?
C011 O00C 1.271(6) . ?
C011 C018 1.353(8) . ?
C011 C01N 1.529(7) . ?
C012 C015 1.372(6) . ?
C012 C20 1.388(7) . ?
C013 O00E 1.263(5) . ?
C013 C019 1.379(6) . ?
C013 C22 1.534(6) . ?
C015 N00J 1.339(6) . ?
C018 C1E 1.416(6) . ?
C019 C1C 1.415(6) . ?
C20 C00S 1.399(7) . ?
C20 C21 1.448(5) . ?
C21 N1 1.301(8) . ?
C21 C1A 1.420(6) . ?
C21 C1B 1.574(8) . ?
C1A C2A 1.3900 . ?
C1A C6A 1.3900 . ?
C2A C3A 1.3900 . ?
C3A C4A 1.3900 . ?
C4A C5A 1.3900 . ?
C5A C6A 1.3900 . ?
C1B C2B 1.3900 . ?
C1B C6B 1.3900 . ?
C2B C3B 1.3900 . ?
C3B C4B 1.3900 . ?
C4B C5B 1.3900 . ?
C5B C6B 1.3900 . ?
C22 F00K 1.306(6) . ?
C22 F00M 1.316(7) . ?
C22 F00I 1.321(6) . ?
N1 N01M 1.147(8) . ?
C1C O009 1.260(5) . ?
C1C C2C 1.466(6) . ?
C2C C3D 1.361(10) . ?
C2C C3C 1.362(8) . ?
C2C S1D 1.709(7) . ?
C2C S1C 1.717(4) . ?
C3C C4C 1.402(9) . ?
C4C C5C 1.363(7) . ?
C5C S1C 1.708(6) . ?
C3D C4D 1.399(10) . ?
C4D C5D 1.358(9) . ?
C5D S1D 1.709(9) . ?
C1E O2 1.257(5) . ?
C1E C2E 1.469(6) . ?
C2E C3F 1.357(10) . ?
C2E C3E 1.357(8) . ?
C2E S1F 1.705(8) . ?
C2E S1E 1.719(4) . ?
C3E C4E 1.394(8) . ?
C4E C5E 1.359(7) . ?
C5E S1E 1.716(6) . ?
C3F C4F 1.397(10) . ?
C4F C5F 1.353(9) . ?
C5F S1F 1.706(9) . ?
C1G O1 1.255(5) . ?
C1G C2G 1.467(5) . ?
C2G C3H 1.358(10) . ?
C2G C3G 1.361(7) . ?
C2G S1H 1.707(8) . ?
C2G S1G 1.722(4) . ?
C3G C4G 1.407(6) . ?
C4G C5G 1.359(6) . ?
C5G S1G 1.707(5) . ?
C3H C4H 1.397(10) . ?
C4H C5H 1.355(9) . ?
C5H S1H 1.708(9) . ?
C01L F1 1.312(7) . ?
C01L F2 1.324(6) . ?
C01L F3 1.350(6) . ?
C01L C00Q 1.539(6) . ?
C01N F00W 1.306(8) . ?
C01N F00V 1.322(7) . ?
C01N F00N 1.343(8) . ?
C00P N00J 1.342(6) . ?
C00P C00S 1.382(5) . ?
C00Q O00F 1.251(5) . ?
C1S Cl1S 1.695(6) . ?
C1S Cl2S 1.719(7) . ?
C1S Cl3S 1.721(7) . ?
C1T Cl2T 1.701(8) . ?
C1T Cl1T 1.704(8) . ?
C1T Cl3T 1.708(8) . ?
C1T Cl2T 2.18(4) 3_676 ?
Cl2T C1T 2.18(4) 3_676 ?
Cl2T Cl2T 2.35(7) 3_676 ?
Dy01 O009 2.294(3) . ?
Dy01 O00C 2.315(3) . ?
Dy01 O00F 2.340(3) . ?
Dy01 O1 2.349(2) . ?
Dy01 O00E 2.356(3) . ?
Dy01 O2 2.379(3) . ?
Dy01 O3 2.395(3) . ?
Dy01 O3 2.397(2) 3_666 ?
N00J O3 1.354(4) . ?
O3 Dy01 2.397(2) 3_666 ?

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
C00Q C2 C1G 121.1(4) . . ?
O00C C011 C018 128.9(4) . . ?
O00C C011 C01N 112.7(5) . . ?
C018 C011 C01N 118.4(5) . . ?
C015 C012 C20 120.8(5) . . ?
O00E C013 C019 128.7(4) . . ?
O00E C013 C22 113.5(4) . . ?
C019 C013 C22 117.7(4) . . ?
N00J C015 C012 119.8(4) . . ?
C011 C018 C1E 122.4(5) . . ?
C013 C019 C1C 121.5(4) . . ?
C012 C20 C00S 117.5(4) . . ?
C012 C20 C21 121.7(5) . . ?
C00S C20 C21 120.8(4) . . ?
N1 C21 C1A 110.5(4) . . ?
N1 C21 C20 117.0(5) . . ?
C1A C21 C20 132.2(5) . . ?
N1 C21 C1B 119.9(5) . . ?
C1A C21 C1B 16.3(4) . . ?
C20 C21 C1B 122.4(5) . . ?
C2A C1A C6A 120.0 . . ?
C2A C1A C21 119.5(4) . . ?
C6A C1A C21 120.3(4) . . ?
C1A C2A C3A 120.0 . . ?
C2A C3A C4A 120.0 . . ?
C5A C4A C3A 120.0 . . ?
C6A C5A C4A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C2B C1B C6B 120.0 . . ?
C2B C1B C21 119.3(5) . . ?
C6B C1B C21 120.6(5) . . ?
C1B C2B C3B 120.0 . . ?
C4B C3B C2B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C4B C5B C6B 120.0 . . ?
C5B C6B C1B 120.0 . . ?
F00K C22 F00M 106.4(5) . . ?
F00K C22 F00I 106.5(4) . . ?
F00M C22 F00I 107.0(5) . . ?
F00K C22 C013 111.6(5) . . ?
F00M C22 C013 110.7(4) . . ?
F00I C22 C013 114.2(4) . . ?
N01M N1 C21 178.3(8) . . ?
O009 C1C C019 123.7(4) . . ?
O009 C1C C2C 115.8(4) . . ?
C019 C1C C2C 120.5(4) . . ?
C3D C2C C3C 106.3(12) . . ?
C3D C2C C1C 121.8(11) . . ?
C3C C2C C1C 131.6(5) . . ?
C3D C2C S1D 112.3(12) . . ?
C3C C2C S1D 6.4(8) . . ?
C1C C2C S1D 125.4(5) . . ?
C3D C2C S1C 7.5(13) . . ?
C3C C2C S1C 111.0(5) . . ?
C1C C2C S1C 117.4(3) . . ?
S1D C2C S1C 117.2(5) . . ?
C2C C3C C4C 113.8(7) . . ?
C5C C4C C3C 111.4(6) . . ?
C4C C5C S1C 112.6(4) . . ?
C2C C3D C4D 112.6(12) . . ?
C5D C4D C3D 111.7(8) . . ?
C4D C5D S1D 112.9(8) . . ?
O2 C1E C018 123.8(4) . . ?
O2 C1E C2E 117.5(4) . . ?
C018 C1E C2E 118.7(4) . . ?
C3F C2E C3E 105.4(15) . . ?
C3F C2E C1E 124.5(14) . . ?
C3E C2E C1E 130.0(5) . . ?
C3F C2E S1F 114.3(15) . . ?
C3E C2E S1F 10.5(11) . . ?
C1E C2E S1F 121.1(8) . . ?
C3F C2E S1E 4.5(14) . . ?
C3E C2E S1E 109.9(5) . . ?
C1E C2E S1E 120.1(3) . . ?
S1F C2E S1E 118.8(8) . . ?
C2E C3E C4E 115.0(6) . . ?
C5E C4E C3E 111.5(6) . . ?
C4E C5E S1E 111.9(5) . . ?
C2E C3F C4F 110.8(15) . . ?
C5F C4F C3F 112.3(9) . . ?
C4F C5F S1F 113.5(9) . . ?
O1 C1G C2 124.2(3) . . ?
O1 C1G C2G 117.1(3) . . ?
C2 C1G C2G 118.6(4) . . ?
C3H C2G C3G 104(2) . . ?
C3H C2G C1G 124(2) . . ?
C3G C2G C1G 130.9(4) . . ?
C3H C2G S1H 113.5(18) . . ?
C3G C2G S1H 9.5(13) . . ?
C1G C2G S1H 121.6(12) . . ?
C3H C2G S1G 8(3) . . ?
C3G C2G S1G 110.5(3) . . ?
C1G C2G S1G 118.6(3) . . ?
S1H C2G S1G 119.9(12) . . ?
C2G C3G C4G 114.1(5) . . ?
C5G C4G C3G 111.2(4) . . ?
C4G C5G S1G 112.8(3) . . ?
C2G C3H C4H 111.5(18) . . ?
C5H C4H C3H 112.2(10) . . ?
C4H C5H S1H 113.2(9) . . ?
F1 C01L F2 110.3(5) . . ?
F1 C01L F3 104.8(5) . . ?
F2 C01L F3 103.9(4) . . ?
F1 C01L C00Q 115.5(4) . . ?
F2 C01L C00Q 111.2(5) . . ?
F3 C01L C00Q 110.2(4) . . ?
F00W C01N F00V 108.4(6) . . ?
F00W C01N F00N 105.5(5) . . ?
F00V C01N F00N 105.5(5) . . ?
F00W C01N C011 111.6(5) . . ?
F00V C01N C011 110.8(5) . . ?
F00N C01N C011 114.6(6) . . ?
N00J C00P C00S 119.7(4) . . ?
O00F C00Q C2 129.3(4) . . ?
O00F C00Q C01L 114.4(4) . . ?
C2 C00Q C01L 116.3(4) . . ?
C00P C00S C20 120.1(4) . . ?
Cl1S C1S Cl2S 117.4(5) . . ?
Cl1S C1S Cl3S 114.9(5) . . ?
Cl2S C1S Cl3S 114.8(5) . . ?
Cl2T C1T Cl1T 116.8(8) . . ?
Cl2T C1T Cl3T 116.1(8) . . ?
Cl1T C1T Cl3T 115.4(8) . . ?
Cl2T C1T Cl2T 73.4(19) . 3_676 ?
Cl1T C1T Cl2T 105.9(14) . 3_676 ?
Cl3T C1T Cl2T 122.6(16) . 3_676 ?
C1T Cl2T C1T 106.6(19) . 3_676 ?
C1T Cl2T Cl2T 62.7(12) . 3_676 ?
C1T Cl2T Cl2T 43.9(11) 3_676 3_676 ?
O009 Dy01 O00C 84.42(11) . . ?
O009 Dy01 O00F 107.51(12) . . ?
O00C Dy01 O00F 143.29(11) . . ?
O009 Dy01 O1 75.28(9) . . ?
O00C Dy01 O1 144.19(10) . . ?
O00F Dy01 O1 71.99(9) . . ?
O009 Dy01 O00E 72.43(10) . . ?
O00C Dy01 O00E 75.00(13) . . ?
O00F Dy01 O00E 75.95(11) . . ?
O1 Dy01 O00E 124.12(11) . . ?
O009 Dy01 O2 75.20(11) . . ?
O00C Dy01 O2 72.12(11) . . ?
O00F Dy01 O2 144.01(9) . . ?
O1 Dy01 O2 74.30(9) . . ?
O00E Dy01 O2 135.43(10) . . ?
O009 Dy01 O3 147.37(9) . . ?
O00C Dy01 O3 103.36(11) . . ?
O00F Dy01 O3 85.25(11) . . ?
O1 Dy01 O3 80.77(9) . . ?
O00E Dy01 O3 140.17(9) . . ?
O2 Dy01 O3 77.23(9) . . ?
O009 Dy01 O3 148.36(9) . 3_666 ?
O00C Dy01 O3 75.29(10) . 3_666 ?
O00F Dy01 O3 77.55(10) . 3_666 ?
O1 Dy01 O3 133.86(9) . 3_666 ?
O00E Dy01 O3 78.95(9) . 3_666 ?
O2 Dy01 O3 119.47(11) . 3_666 ?
O3 Dy01 O3 62.69(10) . 3_666 ?
C015 N00J C00P 122.0(3) . . ?
C015 N00J O3 119.1(4) . . ?
C00P N00J O3 118.9(4) . . ?
C1G O1 Dy01 138.2(2) . . ?
C1E O2 Dy01 133.9(3) . . ?
N00J O3 Dy01 120.4(2) . . ?
N00J O3 Dy01 122.3(2) . 3_666 ?
Dy01 O3 Dy01 117.31(10) . 3_666 ?
C1C O009 Dy01 137.1(3) . . ?
C011 O00C Dy01 132.2(3) . . ?
C013 O00E Dy01 131.4(3) . . ?
C00Q O00F Dy01 135.0(2) . . ?
C5C S1C C2C 91.2(3) . . ?
C2C S1D C5D 90.3(9) . . ?
C5E S1E C2E 91.7(3) . . ?
C2E S1F C5F 89.1(11) . . ?
C5G S1G C2G 91.4(2) . . ?
C2G S1H C5H 89.6(13) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.19
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.106
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2dp_Tb
_database_code_depnum_ccdc_archive 'CCDC 1421170'
_audit_update_record             
;
2015-10-29 deposited with the CCDC.
2016-03-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C76 H44 Cl12 F18 N6 O14 S6 Tb2'
_chemical_formula_moiety         'C76 H44 Cl12 F18 N6 O14 S6 Tb2'
_chemical_formula_weight         2542.83
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_space_group_IT_number           2
loop_
_symmetry_equiv_pos_site_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
#------------------------------------------------------------------------------
_cell_length_a                   12.697(3)
_cell_length_b                   13.700(3)
_cell_length_c                   13.882(3)
_cell_angle_alpha                100.957(3)
_cell_angle_beta                 101.137(3)
_cell_angle_gamma                93.548(3)
_cell_volume                     2313.8(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    90
#------------------------------------------------------------------------------
_exptl_crystal_description       brick
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1246.00
_exptl_absorpt_coefficient_mu    2.093
_exptl_absorpt_correction_type   none

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      90
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12543
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.528
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_reflns_number_total             9588
_reflns_number_gt                7783
_reflns_threshold_expression     F²>2.0σ(F²)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.2125
_refine_ls_wR_factor_gt          0.1944
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9588
_refine_ls_number_parameters     604
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1425P)²+5.0592P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         5.20
_refine_diff_density_min         -2.52
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Tb Tb -0.1723 4.1537
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb38 Tb 0.64407(3) -0.03250(2) 0.57914(2) 0.02400(15) Uani 1 2 d . . .
Cl1 Cl 0.5259(5) 0.4864(3) 0.7351(5) 0.127(2) Uani 1 2 d . . .
Cl2 Cl 0.4452(5) 0.4187(4) 0.8920(3) 0.1154(16) Uani 1 2 d . . .
Cl7 Cl 0.3016(4) 0.4869(4) 0.7430(4) 0.1056(13) Uani 1 2 d . . .
Cl8 Cl 0.0503(4) 0.3291(4) 0.9112(4) 0.1255(18) Uani 1 2 d . . .
Cl10 Cl 0.1872(8) 0.4926(5) 1.0431(6) 0.193(4) Uani 1 2 d . . .
Cl11 Cl 0.2270(5) 0.2955(4) 1.0499(5) 0.1323(19) Uani 1 2 d . . .
S1 S 0.9564(2) 0.2263(2) 0.63041(19) 0.0545(7) Uani 1 2 d . . .
S2 S 0.5224(2) -0.24184(18) 0.80251(17) 0.0479(6) Uani 1 2 d . . .
S3 S 0.99546(19) 0.02118(19) 0.82911(17) 0.0467(6) Uani 1 2 d . . .
F1 F 0.7044(5) -0.4198(4) 0.6586(6) 0.0661(18) Uani 1 2 d . . .
F2 F 0.5562(5) -0.3858(4) 0.5724(5) 0.0570(15) Uani 1 2 d . . .
F3 F 0.6940(7) -0.4075(4) 0.5061(6) 0.077(2) Uani 1 2 d . . .
F4 F 0.6860(7) -0.2220(5) 0.2518(5) 0.072(2) Uani 1 2 d . . .
F5 F 0.7814(6) -0.1181(5) 0.2052(4) 0.071(2) Uani 1 2 d . . .
F6 F 0.6184(6) -0.0950(5) 0.2092(4) 0.0699(18) Uani 1 2 d . . .
F7 F 0.7228(6) 0.2410(4) 0.9539(4) 0.0611(17) Uani 1 2 d . . .
F8 F 0.6394(7) 0.2878(5) 0.8272(6) 0.085(2) Uani 1 2 d . . .
F9 F 0.8004(7) 0.2567(6) 0.8350(6) 0.100(3) Uani 1 2 d . . .
O1 O 0.5775(4) -0.0807(4) 0.7126(4) 0.0276(11) Uani 1 2 d . . .
O2 O 0.6559(4) 0.1091(4) 0.7058(4) 0.0307(11) Uani 1 2 d . . .
O3 O 0.6659(4) -0.0885(4) 0.4151(4) 0.0309(11) Uani 1 2 d . . .
O4 O 0.7829(4) 0.0711(4) 0.5514(4) 0.0278(11) Uani 1 2 d . . .
O5 O 0.8015(4) -0.0558(4) 0.6853(4) 0.0292(11) Uani 1 2 d . . .
O6 O 0.6491(5) -0.2066(4) 0.5608(4) 0.0340(12) Uani 1 2 d . . .
O7 O 0.5422(4) 0.0842(3) 0.4935(4) 0.0264(10) Uani 1 2 d . . .
N1 N 0.5948(5) 0.1711(4) 0.4850(4) 0.0264(13) Uani 1 2 d . . .
N2 N 0.7260(6) 0.1751(5) 0.2357(5) 0.0388(16) Uani 1 2 d . . .
N3 N 0.6992(8) 0.1120(7) 0.1678(7) 0.060(2) Uani 1 2 d . . .
C1 C 0.6425(6) 0.1690(5) 0.4058(5) 0.0270(15) Uani 1 2 d . . .
C2 C 0.7050(6) 0.2526(6) 0.3979(6) 0.0310(16) Uani 1 2 d . . .
C3 C 0.7133(7) 0.3373(6) 0.4726(6) 0.0349(17) Uani 1 2 d . . .
C4 C 0.6032(7) 0.2521(6) 0.5582(6) 0.0348(17) Uani 1 2 d . . .
C5 C 0.6623(7) 0.3372(6) 0.5500(6) 0.0382(19) Uani 1 2 d . . .
C6 C 0.7587(7) 0.2489(7) 0.3131(7) 0.0389(19) Uani 1 2 d . . .
C7 C 0.8470(7) 0.3208(6) 0.3044(7) 0.0412(19) Uani 1 2 d . . .
C8 C 0.9296(7) 0.3613(7) 0.3868(8) 0.046(2) Uani 1 2 d . . .
C9 C 0.8525(8) 0.3468(8) 0.2126(8) 0.050(2) Uani 1 2 d . . .
C10 C 1.0175(9) 0.4507(8) 0.2882(11) 0.064(3) Uani 1 2 d . . .
C11 C 0.9365(11) 0.4095(9) 0.2034(10) 0.069(3) Uani 1 2 d . . .
C12 C 0.9418(6) 0.1400(6) 0.5209(5) 0.0291(15) Uani 1 2 d . . .
C13 C 1.0773(8) 0.2752(8) 0.6204(8) 0.051(2) Uani 1 2 d . . .
C14 C 1.1088(7) 0.2308(7) 0.5366(7) 0.043(2) Uani 1 2 d . . .
C15 C 1.0341(5) 0.1508(4) 0.4676(5) 0.0198(13) Uani 1 2 d . . .
C16 C 0.8449(6) 0.0681(5) 0.4903(5) 0.0285(15) Uani 1 2 d . . .
C17 C 0.8242(6) 0.0028(6) 0.3959(5) 0.0309(16) Uani 1 2 d . . .
C18 C 0.7353(7) -0.0668(6) 0.3656(5) 0.0322(17) Uani 1 2 d . . .
C19 C 0.7065(8) -0.1259(7) 0.2568(6) 0.043(2) Uani 1 2 d . . .
C20 C 0.9352(7) -0.0993(7) 0.8076(6) 0.0386(18) Uani 1 2 d . . .
C21 C 0.9890(8) -0.1565(8) 0.8682(7) 0.046(2) Uani 1 2 d . . .
C22 C 1.0812(8) -0.0988(9) 0.9325(8) 0.056(3) Uani 1 2 d . . .
C23 C 1.0947(8) -0.0029(9) 0.9192(7) 0.054(3) Uani 1 2 d . . .
C24 C 0.8355(6) -0.1252(6) 0.7277(6) 0.0312(16) Uani 1 2 d . . .
C25 C 0.7855(7) -0.2238(6) 0.7017(6) 0.0378(18) Uani 1 2 d . . .
C26 C 0.7001(7) -0.2556(6) 0.6209(6) 0.0367(18) Uani 1 2 d . . .
C27 C 0.6634(9) -0.3675(7) 0.5897(8) 0.049(2) Uani 1 2 d . . .
C28 C 0.5703(7) -0.1207(6) 0.8657(6) 0.0335(17) Uani 1 2 d . . .
C29 C 0.5709(7) -0.1065(6) 0.9698(6) 0.0355(17) Uani 1 2 d . . .
C30 C 0.5284(9) -0.1985(7) 0.9902(7) 0.050(2) Uani 1 2 d . . .
C31 C 0.5010(10) -0.2741(8) 0.9084(7) 0.054(3) Uani 1 2 d . . .
C32 C 0.5996(6) -0.0496(6) 0.8071(5) 0.0302(16) Uani 1 2 d . . .
C33 C 0.6468(6) 0.0487(6) 0.8539(6) 0.0308(16) Uani 1 2 d . . .
C34 C 0.7093(7) 0.2263(6) 0.8562(6) 0.0396(19) Uani 1 2 d . . .
C35 C 0.6679(6) 0.1189(6) 0.8001(6) 0.0314(16) Uani 1 2 d . . .
C36 C 0.4177(12) 0.4242(11) 0.7640(12) 0.087(4) Uani 1 2 d . . .
C37 C 1.0143(9) 0.4276(8) 0.3787(10) 0.059(3) Uani 1 2 d . . .
C39 C 0.1818(13) 0.3723(14) 0.9759(12) 0.100(6) Uani 1 2 d . . .
H1 H 0.63332 0.11112 0.35626 0.0324 Uiso 1 2 calc R . .
H3 H 0.75422 0.39492 0.46969 0.0419 Uiso 1 2 calc R . .
H4 H 0.57044 0.25116 0.61247 0.0418 Uiso 1 2 calc R . .
H5 H 0.66729 0.39539 0.59834 0.0458 Uiso 1 2 calc R . .
H8 H 0.92843 0.34402 0.44826 0.0554 Uiso 1 2 calc R . .
H9 H 0.79794 0.32086 0.15669 0.0605 Uiso 1 2 calc R . .
H10A H 1.07393 0.49434 0.28237 0.0771 Uiso 1 2 calc R . .
H11 H 0.93983 0.42466 0.14144 0.0832 Uiso 1 2 calc R . .
H13 H 1.11859 0.32764 0.66783 0.0610 Uiso 1 2 calc R . .
H14 H 1.17513 0.25027 0.52338 0.0521 Uiso 1 2 calc R . .
H15 H 1.04144 0.11502 0.40563 0.0238 Uiso 1 2 calc R . .
H17 H 0.87167 0.00672 0.35315 0.0370 Uiso 1 2 calc R . .
H21 H 0.96802 -0.22302 0.86729 0.0556 Uiso 1 2 calc R . .
H22 H 1.12842 -0.12394 0.97952 0.0673 Uiso 1 2 calc R . .
H23 H 1.15174 0.04363 0.95549 0.0647 Uiso 1 2 calc R . .
H29 H 0.5947 -0.04754 1.01702 0.0426 Uiso 1 2 calc R . .
H30 H 0.52056 -0.20554 1.05384 0.0601 Uiso 1 2 calc R . .
H31 H 0.47288 -0.33768 0.91076 0.0649 Uiso 1 2 calc R . .
H33 H 0.66401 0.06603 0.92362 0.0370 Uiso 1 2 calc R . .
H36 H 0.40353 0.35626 0.72301 0.1038 Uiso 1 2 calc R . .
H37 H 1.06797 0.45555 0.43469 0.0704 Uiso 1 2 calc R . .
H39 H 0.22769 0.37266 0.92671 0.1199 Uiso 1 2 calc R . .



#==============================================================================
_computing_data_collection       Unknown
_computing_cell_refinement       Unknown
_computing_data_reduction        Unknown
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_molecular_graphics    'CrystalStructure 4.1'

#==============================================================================
# MOLECULAR GEOMETRY

_geom_special_details            
;
    ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Tb38 O1 2.363(6) yes . .
Tb38 O2 2.334(5) yes . .
Tb38 O3 2.336(5) yes . .
Tb38 O4 2.330(5) yes . .
Tb38 O5 2.321(5) yes . .
Tb38 O6 2.357(5) yes . .
Tb38 O7 2.455(5) yes . .
Tb38 O7 2.390(5) yes . 2_656
Cl1 C36 1.724(18) yes . .
Cl2 C36 1.761(17) yes . .
Cl7 C36 1.755(17) yes . .
Cl8 C39 1.744(16) yes . .
Cl10 C39 1.723(18) yes . .
Cl11 C39 1.66(2) yes . .
S1 C12 1.710(7) yes . .
S1 C13 1.679(11) yes . .
S2 C28 1.735(7) yes . .
S2 C31 1.678(12) yes . .
S3 C20 1.722(9) yes . .
S3 C23 1.692(10) yes . .
F1 C27 1.347(13) yes . .
F2 C27 1.335(12) yes . .
F3 C27 1.326(14) yes . .
F4 C19 1.312(11) yes . .
F5 C19 1.308(13) yes . .
F6 C19 1.321(11) yes . .
F7 C34 1.307(10) yes . .
F8 C34 1.321(12) yes . .
F9 C34 1.310(13) yes . .
O1 C32 1.270(8) yes . .
O2 C35 1.267(9) yes . .
O3 C18 1.271(11) yes . .
O4 C16 1.261(10) yes . .
O5 C24 1.267(10) yes . .
O6 C26 1.274(10) yes . .
O7 N1 1.365(8) yes . .
N1 C1 1.351(10) yes . .
N1 C4 1.337(9) yes . .
N2 N3 1.131(10) yes . .
N2 C6 1.309(10) yes . .
C1 C2 1.387(11) yes . .
C2 C3 1.385(10) yes . .
C2 C6 1.464(13) yes . .
C3 C5 1.357(14) yes . .
C4 C5 1.383(12) yes . .
C6 C7 1.485(13) yes . .
C7 C8 1.393(12) yes . .
C7 C9 1.399(16) yes . .
C8 C37 1.400(15) yes . .
C9 C11 1.368(17) yes . .
C10 C11 1.404(17) yes . .
C10 C37 1.36(2) yes . .
C12 C15 1.516(11) yes . .
C12 C16 1.467(10) yes . .
C13 C14 1.349(15) yes . .
C14 C15 1.464(10) yes . .
C16 C17 1.407(9) yes . .
C17 C18 1.376(11) yes . .
C18 C19 1.534(10) yes . .
C20 C21 1.373(14) yes . .
C20 C24 1.487(10) yes . .
C21 C22 1.417(12) yes . .
C22 C23 1.365(18) yes . .
C24 C25 1.407(11) yes . .
C25 C26 1.381(11) yes . .
C26 C27 1.529(12) yes . .
C28 C29 1.420(12) yes . .
C28 C32 1.457(12) yes . .
C29 C30 1.438(14) yes . .
C30 C31 1.356(12) yes . .
C32 C33 1.418(10) yes . .
C33 C35 1.369(12) yes . .
C34 C35 1.536(10) yes . .
C1 H1 0.930 no . .
C3 H3 0.930 no . .
C4 H4 0.930 no . .
C5 H5 0.930 no . .
C8 H8 0.930 no . .
C9 H9 0.930 no . .
C10 H10A 0.930 no . .
C11 H11 0.930 no . .
C13 H13 0.930 no . .
C14 H14 0.930 no . .
C15 H15 0.930 no . .
C17 H17 0.930 no . .
C21 H21 0.930 no . .
C22 H22 0.930 no . .
C23 H23 0.930 no . .
C29 H29 0.930 no . .
C30 H30 0.930 no . .
C31 H31 0.930 no . .
C33 H33 0.930 no . .
C36 H36 0.980 no . .
C37 H37 0.930 no . .
C39 H39 0.980 no . .

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
O1 Tb38 O2 71.74(18) yes . . .
O1 Tb38 O3 143.93(17) yes . . .
O1 Tb38 O4 140.30(15) yes . . .
O1 Tb38 O5 78.04(19) yes . . .
O1 Tb38 O6 72.52(19) yes . . .
O1 Tb38 O7 116.37(18) yes . . .
O1 Tb38 O7 76.99(17) yes . . 2_656
O2 Tb38 O3 144.0(2) yes . . .
O2 Tb38 O4 77.27(18) yes . . .
O2 Tb38 O5 80.66(18) yes . . .
O2 Tb38 O6 139.39(19) yes . . .
O2 Tb38 O7 76.53(17) yes . . .
O2 Tb38 O7 108.52(17) yes . . 2_656
O3 Tb38 O4 71.92(17) yes . . .
O3 Tb38 O5 106.94(19) yes . . .
O3 Tb38 O6 74.82(19) yes . . .
O3 Tb38 O7 79.48(18) yes . . .
O3 Tb38 O7 83.38(18) yes . . 2_656
O4 Tb38 O5 72.92(19) yes . . .
O4 Tb38 O6 122.3(2) yes . . .
O4 Tb38 O7 78.57(17) yes . . .
O4 Tb38 O7 137.61(18) yes . . 2_656
O5 Tb38 O6 73.63(18) yes . . .
O5 Tb38 O7 146.70(16) yes . . .
O5 Tb38 O7 148.83(19) yes . . 2_656
O6 Tb38 O7 138.03(16) yes . . .
O6 Tb38 O7 81.27(18) yes . . 2_656
O7 Tb38 O7 63.11(16) yes . . 2_656
C12 S1 C13 92.7(5) yes . . .
C28 S2 C31 91.6(4) yes . . .
C20 S3 C23 91.0(5) yes . . .
Tb38 O1 C32 133.7(5) yes . . .
Tb38 O2 C35 131.1(5) yes . . .
Tb38 O3 C18 134.2(4) yes . . .
Tb38 O4 C16 137.4(4) yes . . .
Tb38 O5 C24 135.9(5) yes . . .
Tb38 O6 C26 129.1(4) yes . . .
Tb38 O7 Tb38 116.9(2) yes . . 2_656
Tb38 O7 N1 119.2(4) yes . . .
Tb38 O7 N1 123.8(4) yes 2_656 . .
O7 N1 C1 117.8(5) yes . . .
O7 N1 C4 119.0(7) yes . . .
C1 N1 C4 123.1(7) yes . . .
N3 N2 C6 178.7(10) yes . . .
N1 C1 C2 120.3(6) yes . . .
C1 C2 C3 117.2(8) yes . . .
C1 C2 C6 120.0(7) yes . . .
C3 C2 C6 122.8(8) yes . . .
C2 C3 C5 120.8(8) yes . . .
N1 C4 C5 117.4(8) yes . . .
C3 C5 C4 121.2(7) yes . . .
N2 C6 C2 117.6(8) yes . . .
N2 C6 C7 115.4(8) yes . . .
C2 C6 C7 127.0(7) yes . . .
C6 C7 C8 120.7(9) yes . . .
C6 C7 C9 121.3(8) yes . . .
C8 C7 C9 118.0(9) yes . . .
C7 C8 C37 121.1(10) yes . . .
C7 C9 C11 121.4(9) yes . . .
C11 C10 C37 120.7(11) yes . . .
C9 C11 C10 119.4(13) yes . . .
S1 C12 C15 113.1(5) yes . . .
S1 C12 C16 118.0(6) yes . . .
C15 C12 C16 128.9(6) yes . . .
S1 C13 C14 113.3(7) yes . . .
C13 C14 C15 117.2(8) yes . . .
C12 C15 C14 103.6(6) yes . . .
O4 C16 C12 116.4(6) yes . . .
O4 C16 C17 123.8(7) yes . . .
C12 C16 C17 119.8(7) yes . . .
C16 C17 C18 121.4(8) yes . . .
O3 C18 C17 128.8(7) yes . . .
O3 C18 C19 111.5(7) yes . . .
C17 C18 C19 119.6(8) yes . . .
F4 C19 F5 105.5(8) yes . . .
F4 C19 F6 107.2(7) yes . . .
F4 C19 C18 112.0(8) yes . . .
F5 C19 F6 107.7(8) yes . . .
F5 C19 C18 115.0(7) yes . . .
F6 C19 C18 109.1(7) yes . . .
S3 C20 C21 113.3(6) yes . . .
S3 C20 C24 116.3(7) yes . . .
C21 C20 C24 130.4(8) yes . . .
C20 C21 C22 109.6(9) yes . . .
C21 C22 C23 114.1(10) yes . . .
S3 C23 C22 112.1(7) yes . . .
O5 C24 C20 116.9(7) yes . . .
O5 C24 C25 123.6(7) yes . . .
C20 C24 C25 119.5(8) yes . . .
C24 C25 C26 122.4(8) yes . . .
O6 C26 C25 130.1(7) yes . . .
O6 C26 C27 111.8(7) yes . . .
C25 C26 C27 117.9(8) yes . . .
F1 C27 F2 106.9(9) yes . . .
F1 C27 F3 106.1(8) yes . . .
F1 C27 C26 113.5(7) yes . . .
F2 C27 F3 107.1(8) yes . . .
F2 C27 C26 111.8(8) yes . . .
F3 C27 C26 111.0(9) yes . . .
S2 C28 C29 112.1(6) yes . . .
S2 C28 C32 117.9(5) yes . . .
C29 C28 C32 130.0(7) yes . . .
C28 C29 C30 108.6(7) yes . . .
C29 C30 C31 114.0(9) yes . . .
S2 C31 C30 113.6(8) yes . . .
O1 C32 C28 115.7(6) yes . . .
O1 C32 C33 123.0(7) yes . . .
C28 C32 C33 121.3(6) yes . . .
C32 C33 C35 122.3(7) yes . . .
F7 C34 F8 106.3(8) yes . . .
F7 C34 F9 107.8(7) yes . . .
F7 C34 C35 115.0(8) yes . . .
F8 C34 F9 105.9(8) yes . . .
F8 C34 C35 109.4(6) yes . . .
F9 C34 C35 111.8(8) yes . . .
O2 C35 C33 128.8(6) yes . . .
O2 C35 C34 112.2(7) yes . . .
C33 C35 C34 119.0(7) yes . . .
Cl1 C36 Cl2 110.2(8) yes . . .
Cl1 C36 Cl7 111.2(9) yes . . .
Cl2 C36 Cl7 106.7(9) yes . . .
C8 C37 C10 119.4(10) yes . . .
Cl8 C39 Cl10 110.6(10) yes . . .
Cl8 C39 Cl11 109.8(11) yes . . .
Cl10 C39 Cl11 111.4(9) yes . . .
N1 C1 H1 119.840 no . . .
C2 C1 H1 119.837 no . . .
C2 C3 H3 119.613 no . . .
C5 C3 H3 119.608 no . . .
N1 C4 H4 121.281 no . . .
C5 C4 H4 121.285 no . . .
C3 C5 H5 119.407 no . . .
C4 C5 H5 119.404 no . . .
C7 C8 H8 119.470 no . . .
C37 C8 H8 119.468 no . . .
C7 C9 H9 119.320 no . . .
C11 C9 H9 119.320 no . . .
C11 C10 H10A 119.627 no . . .
C37 C10 H10A 119.634 no . . .
C9 C11 H11 120.283 no . . .
C10 C11 H11 120.280 no . . .
S1 C13 H13 123.334 no . . .
C14 C13 H13 123.337 no . . .
C13 C14 H14 121.428 no . . .
C15 C14 H14 121.421 no . . .
C12 C15 H15 128.192 no . . .
C14 C15 H15 128.200 no . . .
C16 C17 H17 119.326 no . . .
C18 C17 H17 119.320 no . . .
C20 C21 H21 125.217 no . . .
C22 C21 H21 125.211 no . . .
C21 C22 H22 122.955 no . . .
C23 C22 H22 122.962 no . . .
S3 C23 H23 123.966 no . . .
C22 C23 H23 123.968 no . . .
C28 C29 H29 125.690 no . . .
C30 C29 H29 125.689 no . . .
C29 C30 H30 122.984 no . . .
C31 C30 H30 122.975 no . . .
S2 C31 H31 123.200 no . . .
C30 C31 H31 123.193 no . . .
C32 C33 H33 118.865 no . . .
C35 C33 H33 118.868 no . . .
Cl1 C36 H36 109.541 no . . .
Cl2 C36 H36 109.543 no . . .
Cl7 C36 H36 109.537 no . . .
C8 C37 H37 120.306 no . . .
C10 C37 H37 120.294 no . . .
Cl8 C39 H39 108.319 no . . .
Cl10 C39 H39 108.325 no . . .
Cl11 C39 H39 108.330 no . . .

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_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 Tb38 O2 C35 28.7(4) no . . . .
O2 Tb38 O1 C32 -31.3(4) no . . . .
O1 Tb38 O3 C18 -149.1(4) no . . . .
O3 Tb38 O1 C32 155.1(4) no . . . .
O1 Tb38 O4 C16 141.2(4) no . . . .
O4 Tb38 O1 C32 9.2(6) no . . . .
O1 Tb38 O5 C24 52.9(5) no . . . .
O5 Tb38 O1 C32 52.7(4) no . . . .
O1 Tb38 O6 C26 -60.2(5) no . . . .
O6 Tb38 O1 C32 129.1(5) no . . . .
O1 Tb38 O7 Tb38 -57.8(2) no . . . 2_656
O1 Tb38 O7 N1 125.7(3) no . . . .
O7 Tb38 O1 C32 -95.4(5) no . . . .
O1 Tb38 O7 Tb38 128.9(2) no . . 2_656 2_656
O1 Tb38 O7 N1 -47.4(3) no . . 2_656 2_656
O7 Tb38 O1 C32 -146.1(5) no 2_656 . . .
O2 Tb38 O3 C18 41.3(7) no . . . .
O3 Tb38 O2 C35 -157.7(4) no . . . .
O2 Tb38 O4 C16 -179.6(5) no . . . .
O4 Tb38 O2 C35 -126.2(5) no . . . .
O2 Tb38 O5 C24 126.1(5) no . . . .
O5 Tb38 O2 C35 -51.7(5) no . . . .
O2 Tb38 O6 C26 -30.9(7) no . . . .
O6 Tb38 O2 C35 -0.8(6) no . . . .
O2 Tb38 O7 Tb38 -119.2(3) no . . . 2_656
O2 Tb38 O7 N1 64.3(3) no . . . .
O7 Tb38 O2 C35 152.7(5) no . . . .
O2 Tb38 O7 Tb38 63.6(3) no . . 2_656 2_656
O2 Tb38 O7 N1 -112.8(3) no . . 2_656 2_656
O7 Tb38 O2 C35 97.5(5) no 2_656 . . .
O3 Tb38 O4 C16 -18.5(5) no . . . .
O4 Tb38 O3 C18 8.8(5) no . . . .
O3 Tb38 O5 C24 -90.1(5) no . . . .
O5 Tb38 O3 C18 -56.2(5) no . . . .
O3 Tb38 O6 C26 135.3(5) no . . . .
O6 Tb38 O3 C18 -123.4(5) no . . . .
O3 Tb38 O7 Tb38 87.9(2) no . . . 2_656
O3 Tb38 O7 N1 -88.6(3) no . . . .
O7 Tb38 O3 C18 90.1(5) no . . . .
O3 Tb38 O7 Tb38 -81.5(2) no . . 2_656 2_656
O3 Tb38 O7 N1 102.1(4) no . . 2_656 2_656
O7 Tb38 O3 C18 153.9(5) no 2_656 . . .
O4 Tb38 O5 C24 -154.5(5) no . . . .
O5 Tb38 O4 C16 96.4(5) no . . . .
O4 Tb38 O6 C26 78.8(5) no . . . .
O6 Tb38 O4 C16 39.3(5) no . . . .
O4 Tb38 O7 Tb38 161.3(2) no . . . 2_656
O4 Tb38 O7 N1 -15.2(3) no . . . .
O7 Tb38 O4 C16 -101.1(5) no . . . .
O4 Tb38 O7 Tb38 -27.7(4) no . . 2_656 2_656
O4 Tb38 O7 N1 155.9(3) no . . 2_656 2_656
O7 Tb38 O4 C16 -76.0(6) no 2_656 . . .
O5 Tb38 O6 C26 22.1(5) no . . . .
O6 Tb38 O5 C24 -22.1(5) no . . . .
O5 Tb38 O7 Tb38 -167.2(3) no . . . 2_656
O5 Tb38 O7 N1 16.2(5) no . . . .
O7 Tb38 O5 C24 173.2(4) no . . . .
O5 Tb38 O7 Tb38 166.5(3) no . . 2_656 2_656
O5 Tb38 O7 N1 -9.9(6) no . . 2_656 2_656
O7 Tb38 O5 C24 15.6(7) no 2_656 . . .
O6 Tb38 O7 Tb38 35.1(4) no . . . 2_656
O6 Tb38 O7 N1 -141.4(3) no . . . .
O7 Tb38 O6 C26 -170.5(4) no . . . .
O6 Tb38 O7 Tb38 -157.1(3) no . . 2_656 2_656
O6 Tb38 O7 N1 26.5(3) no . . 2_656 2_656
O7 Tb38 O6 C26 -139.2(5) no 2_656 . . .
O7 Tb38 O7 Tb38 0.00(19) no . . 2_656 2_656
O7 Tb38 O7 N1 -176.3(4) no . . 2_656 2_656
O7 Tb38 O7 Tb38 0.00(19) no 2_656 . . 2_656
O7 Tb38 O7 N1 -176.5(4) no 2_656 . . .
C12 S1 C13 C14 0.9(8) no . . . .
C13 S1 C12 C15 -3.0(6) no . . . .
C13 S1 C12 C16 177.8(6) no . . . .
C28 S2 C31 C30 -0.4(8) no . . . .
C31 S2 C28 C29 1.0(7) no . . . .
C31 S2 C28 C32 -177.1(7) no . . . .
C20 S3 C23 C22 -0.6(7) no . . . .
C23 S3 C20 C21 0.5(7) no . . . .
C23 S3 C20 C24 -179.3(6) no . . . .
Tb38 O1 C32 C28 -158.0(4) no . . . .
Tb38 O1 C32 C33 23.9(11) no . . . .
Tb38 O2 C35 C33 -21.0(12) no . . . .
Tb38 O2 C35 C34 160.6(4) no . . . .
Tb38 O3 C18 C17 -1.3(13) no . . . .
Tb38 O3 C18 C19 -177.9(4) no . . . .
Tb38 O4 C16 C12 -162.2(4) no . . . .
Tb38 O4 C16 C17 19.7(11) no . . . .
Tb38 O5 C24 C20 -167.6(4) no . . . .
Tb38 O5 C24 C25 13.9(12) no . . . .
Tb38 O6 C26 C25 -17.0(14) no . . . .
Tb38 O6 C26 C27 168.5(4) no . . . .
Tb38 O7 N1 C1 86.7(5) no . . . .
Tb38 O7 N1 C4 -88.9(6) no . . . .
Tb38 O7 N1 C1 -89.5(6) no 2_656 . . .
Tb38 O7 N1 C4 94.9(5) no 2_656 . . .
O7 N1 C1 C2 -174.4(5) no . . . .
O7 N1 C4 C5 176.4(5) no . . . .
C1 N1 C4 C5 1.0(11) no . . . .
C4 N1 C1 C2 1.1(10) no . . . .
N1 C1 C2 C3 -1.7(10) no . . . .
N1 C1 C2 C6 178.5(6) no . . . .
C1 C2 C3 C5 0.3(11) no . . . .
C1 C2 C6 N2 15.6(11) no . . . .
C1 C2 C6 C7 -164.7(7) no . . . .
C3 C2 C6 N2 -164.3(7) no . . . .
C3 C2 C6 C7 15.4(13) no . . . .
C6 C2 C3 C5 -179.9(7) no . . . .
C2 C3 C5 C4 1.8(12) no . . . .
N1 C4 C5 C3 -2.4(12) no . . . .
N2 C6 C7 C8 -141.2(8) no . . . .
N2 C6 C7 C9 36.1(12) no . . . .
C2 C6 C7 C8 39.1(13) no . . . .
C2 C6 C7 C9 -143.6(8) no . . . .
C6 C7 C8 C37 178.7(7) no . . . .
C6 C7 C9 C11 -177.0(8) no . . . .
C8 C7 C9 C11 0.4(14) no . . . .
C9 C7 C8 C37 1.3(13) no . . . .
C7 C8 C37 C10 -1.8(15) no . . . .
C7 C9 C11 C10 -1.6(17) no . . . .
C11 C10 C37 C8 0.5(16) no . . . .
C37 C10 C11 C9 1.2(17) no . . . .
S1 C12 C15 C14 3.9(7) no . . . .
S1 C12 C16 O4 -4.8(9) no . . . .
S1 C12 C16 C17 173.4(5) no . . . .
C15 C12 C16 O4 176.0(7) no . . . .
C15 C12 C16 C17 -5.8(12) no . . . .
C16 C12 C15 C14 -176.9(7) no . . . .
S1 C13 C14 C15 1.5(12) no . . . .
C13 C14 C15 C12 -3.4(10) no . . . .
O4 C16 C17 C18 -3.2(12) no . . . .
C12 C16 C17 C18 178.8(6) no . . . .
C16 C17 C18 O3 -5.4(13) no . . . .
C16 C17 C18 C19 171.0(6) no . . . .
O3 C18 C19 F4 -50.6(10) no . . . .
O3 C18 C19 F5 -171.0(7) no . . . .
O3 C18 C19 F6 68.0(9) no . . . .
C17 C18 C19 F4 132.5(8) no . . . .
C17 C18 C19 F5 12.1(12) no . . . .
C17 C18 C19 F6 -109.0(9) no . . . .
S3 C20 C21 C22 -0.3(10) no . . . .
S3 C20 C24 O5 -2.5(10) no . . . .
S3 C20 C24 C25 176.1(5) no . . . .
C21 C20 C24 O5 177.8(9) no . . . .
C21 C20 C24 C25 -3.6(14) no . . . .
C24 C20 C21 C22 179.4(8) no . . . .
C20 C21 C22 C23 -0.1(13) no . . . .
C21 C22 C23 S3 0.5(13) no . . . .
O5 C24 C25 C26 6.0(14) no . . . .
C20 C24 C25 C26 -172.6(7) no . . . .
C24 C25 C26 O6 -3.4(16) no . . . .
C24 C25 C26 C27 170.8(8) no . . . .
O6 C26 C27 F1 -171.2(8) no . . . .
O6 C26 C27 F2 -50.2(11) no . . . .
O6 C26 C27 F3 69.4(10) no . . . .
C25 C26 C27 F1 13.5(14) no . . . .
C25 C26 C27 F2 134.6(9) no . . . .
C25 C26 C27 F3 -105.9(10) no . . . .
S2 C28 C29 C30 -1.3(8) no . . . .
S2 C28 C32 O1 6.5(10) no . . . .
S2 C28 C32 C33 -175.3(5) no . . . .
C29 C28 C32 O1 -171.1(8) no . . . .
C29 C28 C32 C33 7.1(13) no . . . .
C32 C28 C29 C30 176.5(8) no . . . .
C28 C29 C30 C31 1.0(11) no . . . .
C29 C30 C31 S2 -0.3(13) no . . . .
O1 C32 C33 C35 2.8(12) no . . . .
C28 C32 C33 C35 -175.2(7) no . . . .
C32 C33 C35 O2 -4.0(13) no . . . .
C32 C33 C35 C34 174.4(6) no . . . .
F7 C34 C35 O2 179.8(7) no . . . .
F7 C34 C35 C33 1.2(11) no . . . .
F8 C34 C35 O2 60.2(10) no . . . .
F8 C34 C35 C33 -118.4(8) no . . . .
F9 C34 C35 O2 -56.8(9) no . . . .
F9 C34 C35 C33 124.6(8) no . . . .

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
S1 O4 2.859(5) no . .
S2 F2 3.538(7) no . .
S2 O1 2.848(6) no . .
S2 N2 3.312(8) no . 2_656
S2 N3 3.470(11) no . 2_656
S2 C1 3.572(8) no . 2_656
S2 C2 3.577(8) no . 2_656
S3 O5 2.854(5) no . .
F1 O6 3.502(9) no . .
F1 C25 2.727(10) no . .
F2 O6 2.703(8) no . .
F2 C3 3.486(10) no . 2_656
F2 C4 3.323(10) no . 2_656
F2 C5 3.141(11) no . 2_656
F2 C25 3.506(9) no . .
F3 O6 2.836(8) no . .
F3 C25 3.298(9) no . .
F4 O3 2.694(8) no . .
F4 C17 3.493(9) no . .
F5 O3 3.477(9) no . .
F5 N3 3.481(12) no . .
F5 C17 2.778(9) no . .
F6 O3 2.787(8) no . .
F6 N3 3.149(12) no . .
F6 C17 3.312(9) no . .
F6 C32 3.499(11) no . 2_656
F6 C33 3.442(10) no . 2_656
F7 O2 3.487(7) no . .
F7 C33 2.753(9) no . .
F8 O2 2.739(8) no . .
F8 C33 3.371(10) no . .
F9 O2 2.749(8) no . .
F9 C33 3.433(11) no . .
O1 N1 3.147(7) no . 2_656
O1 C1 3.003(8) no . 2_656
O1 C24 3.344(10) no . .
O1 C25 3.396(11) no . .
O1 C26 3.138(10) no . .
O1 C35 2.842(8) no . .
O2 N1 3.297(8) no . .
O2 C4 3.105(10) no . .
O2 C32 2.928(10) no . .
O3 C1 3.582(9) no . .
O3 C16 2.913(8) no . .
O4 N1 2.908(8) no . .
O4 C1 2.999(9) no . .
O4 C4 3.472(10) no . .
O4 C18 2.827(8) no . .
O5 C16 3.565(10) no . .
O5 C26 2.853(9) no . .
O5 C32 3.329(10) no . .
O5 C33 3.498(10) no . .
O5 C35 3.352(9) no . .
O6 N1 3.127(9) no . 2_656
O6 C4 3.270(10) no . 2_656
O6 C24 2.964(8) no . .
O7 C5 3.578(9) no . .
N1 C3 2.702(10) no . .
N1 C16 3.547(10) no . .
N2 C1 2.782(11) no . .
N2 C8 3.556(10) no . .
N2 C9 2.869(13) no . .
N3 C1 3.472(12) no . .
N3 C2 3.387(12) no . .
N3 C7 3.346(11) no . .
N3 C9 3.537(14) no . .
N3 C28 3.376(13) no . 2_656
N3 C29 3.577(12) no . 2_656
C1 C5 2.713(10) no . .
C1 C16 3.128(11) no . .
C1 C17 3.344(11) no . .
C1 C18 3.489(11) no . .
C2 C4 2.782(13) no . .
C2 C8 3.179(13) no . .
C2 C16 3.478(11) no . .
C3 C7 3.125(14) no . .
C3 C8 3.220(14) no . .
C7 C10 2.787(15) no . .
C8 C11 2.765(18) no . .
C8 C14 3.576(14) no . .
C8 C15 3.530(12) no . .
C9 C37 2.772(14) no . .
C15 C17 3.121(9) no . .
C21 C25 3.075(12) no . .
C24 C32 3.533(12) no . .
C29 C33 3.112(13) no . .
Cl1 F1 3.000(10) no . 1_565
Cl1 F2 3.173(9) no . 1_565
Cl1 F8 3.494(9) no . .
Cl2 Cl2 3.370(6) no . 2_667
Cl2 F4 3.183(7) no . 2_656
Cl2 F8 3.301(11) no . .
Cl7 F3 3.434(9) no . 2_656
Cl7 C7 3.425(11) no . 2_666
Cl7 C9 3.144(12) no . 2_666
Cl7 C11 3.565(15) no . 2_666
Cl8 F9 3.176(9) no . 1_455
Cl10 F8 3.568(9) no . 2_667
Cl10 F9 3.507(10) no . 2_667
Cl11 C30 3.552(13) no . 2_657
Cl11 C31 3.431(14) no . 2_657
S3 F5 3.211(8) no . 2_756
F1 Cl1 3.000(10) no . 1_545
F1 C5 3.347(9) no . 1_545
F1 C10 3.535(13) no . 2_756
F2 Cl1 3.173(9) no . 1_545
F2 F2 3.437(7) no . 2_646
F3 Cl7 3.434(9) no . 2_656
F3 C3 3.469(10) no . 1_545
F3 C14 3.584(13) no . 2_756
F4 Cl2 3.183(7) no . 2_656
F4 C13 3.378(12) no . 2_756
F4 C14 3.556(11) no . 2_756
F4 C36 2.943(17) no . 2_656
F5 S3 3.211(8) no . 2_756
F5 C23 3.165(14) no . 2_756
F6 C29 3.232(10) no . 1_554
F6 C30 3.063(10) no . 1_554
F7 C22 3.568(13) no . 2_757
F7 C30 3.467(14) no . 2_657
F8 Cl1 3.494(9) no . .
F8 Cl2 3.301(11) no . .
F8 Cl10 3.568(9) no . 2_667
F8 C36 3.537(18) no . .
F9 Cl8 3.176(9) no . 1_655
F9 Cl10 3.507(10) no . 2_667
O3 C14 3.589(11) no . 2_756
O5 C15 3.399(9) no . 2_756
O6 C14 3.599(12) no . 2_756
N3 C22 3.348(16) no . 2_756
N3 C23 3.400(15) no . 2_756
C3 F3 3.469(10) no . 1_565
C5 F1 3.347(9) no . 1_565
C7 Cl7 3.425(11) no . 2_666
C9 Cl7 3.144(12) no . 2_666
C9 C21 3.538(15) no . 2_756
C10 F1 3.535(13) no . 2_756
C11 Cl7 3.565(15) no . 2_666
C13 F4 3.378(12) no . 2_756
C14 F3 3.584(13) no . 2_756
C14 F4 3.556(11) no . 2_756
C14 O3 3.589(11) no . 2_756
C14 O6 3.599(12) no . 2_756
C14 C18 3.388(13) no . 2_756
C15 O5 3.399(9) no . 2_756
C15 C16 3.547(10) no . 2_756
C15 C17 3.452(10) no . 2_756
C15 C24 3.415(11) no . 2_756
C16 C15 3.547(10) no . 2_756
C17 C15 3.452(10) no . 2_756
C18 C14 3.388(13) no . 2_756
C21 C9 3.538(15) no . 2_756
C22 F7 3.568(13) no . 2_757
C22 N3 3.348(16) no . 2_756
C22 C23 3.498(15) no . 2_757
C23 F5 3.165(14) no . 2_756
C23 N3 3.400(15) no . 2_756
C23 C22 3.498(15) no . 2_757
C23 C23 3.585(15) no . 2_757
C24 C15 3.415(11) no . 2_756
C29 F6 3.232(10) no . 1_556
C29 C29 3.572(12) no . 2_657
C30 Cl11 3.552(13) no . 2_657
C30 F6 3.063(10) no . 1_556
C30 F7 3.467(14) no . 2_657
C31 Cl11 3.431(14) no . 2_657
C36 F4 2.943(17) no . 2_656
C36 F8 3.537(18) no . .
S1 H8 3.2240 no . .
S1 H14 3.4203 no . .
S1 H15 3.5952 no . .
S2 H1 3.4972 no . 2_656
S2 H29 3.5247 no . .
S2 H30 3.4342 no . .
S3 H21 3.4923 no . .
S3 H22 3.4342 no . .
F2 H5 3.3050 no . 2_656
F5 H17 2.4434 no . .
F6 H1 3.1252 no . .
F6 H17 3.4896 no . .
F7 H33 2.3992 no . .
F8 H4 2.8755 no . .
F8 H33 3.5529 no . .
F9 H33 3.5804 no . .
O1 H1 2.6405 no . 2_656
O1 H33 3.1742 no . .
O2 H4 2.7057 no . .
O2 H33 3.1724 no . .
O3 H1 3.0289 no . .
O3 H4 3.5389 no . 2_656
O3 H17 3.1844 no . .
O4 H1 3.1543 no . .
O4 H17 3.1660 no . .
O6 H4 3.2510 no . 2_656
O7 H1 2.4837 no . .
O7 H4 2.5143 no . .
N1 H5 3.1647 no . .
N2 H1 2.4794 no . .
N2 H9 2.6490 no . .
N2 H17 3.4916 no . .
N3 H1 2.8984 no . .
N3 H9 3.0949 no . .
C1 H3 3.2108 no . .
C1 H4 3.2013 no . .
C2 H5 3.2182 no . .
C2 H8 2.9267 no . .
C3 H1 3.2116 no . .
C3 H4 3.2276 no . .
C3 H8 2.8149 no . .
C4 H1 3.1906 no . .
C4 H3 3.2214 no . .
C6 H1 2.6235 no . .
C6 H3 2.6713 no . .
C6 H8 2.6504 no . .
C6 H9 2.6656 no . .
C7 H3 2.8270 no . .
C7 H11 3.2516 no . .
C7 H37 3.2681 no . .
C8 H3 2.7220 no . .
C8 H9 3.2337 no . .
C8 H10A 3.2250 no . .
C9 H8 3.2353 no . .
C9 H10A 3.2297 no . .
C10 H8 3.2181 no . .
C10 H9 3.2330 no . .
C11 H37 3.2444 no . .
C12 H8 3.1501 no . .
C12 H13 3.3663 no . .
C12 H14 3.2321 no . .
C12 H17 2.6324 no . .
C13 H8 3.0830 no . .
C13 H15 3.2824 no . .
C14 H8 3.0386 no . .
C15 H8 3.0741 no . .
C15 H13 3.2735 no . .
C15 H17 2.7766 no . .
C16 H1 3.1164 no . .
C16 H15 3.0406 no . .
C17 H1 2.9366 no . .
C17 H15 3.0400 no . .
C18 H1 2.8430 no . .
C19 H1 3.5319 no . .
C19 H17 2.6470 no . .
C20 H22 3.1586 no . .
C20 H23 3.3516 no . .
C21 H23 3.2135 no . .
C23 H21 3.2129 no . .
C24 H21 2.8961 no . .
C25 H21 2.9296 no . .
C28 H30 3.2049 no . .
C28 H31 3.3628 no . .
C28 H33 2.6606 no . .
C29 H31 3.2222 no . .
C29 H33 2.8144 no . .
C31 H29 3.2234 no . .
C32 H1 3.3125 no . 2_656
C32 H29 2.9216 no . .
C33 H29 2.9843 no . .
C34 H4 3.5895 no . .
C34 H33 2.6184 no . .
C35 H4 3.5249 no . .
C37 H11 3.2382 no . .
H1 H17 3.4307 no . .
H3 H5 2.2728 no . .
H3 H8 2.4154 no . .
H4 H5 2.3227 no . .
H8 H13 3.5573 no . .
H8 H14 3.5063 no . .
H8 H15 3.5258 no . .
H8 H37 2.3265 no . .
H9 H11 2.2929 no . .
H9 H31 3.4192 no . 2_656
H10A H11 2.3323 no . .
H10A H37 2.2897 no . .
H13 H14 2.3456 no . .
H14 H15 2.5247 no . .
H14 H37 3.5240 no . .
H15 H17 2.4424 no . .
H21 H22 2.4588 no . .
H22 H23 2.3905 no . .
H29 H30 2.4874 no . .
H29 H33 2.4320 no . .
H30 H31 2.3710 no . .
Cl1 H4 3.4804 no . .
Cl1 H5 3.0123 no . .
Cl1 H31 3.2881 no . 1_565
Cl2 H30 3.1851 no . 2_657
Cl2 H31 3.2899 no . 1_565
Cl2 H31 3.1634 no . 2_657
Cl2 H39 2.9444 no . .
Cl7 H9 3.1892 no . 2_666
Cl7 H13 2.9700 no . 1_455
Cl7 H31 3.3458 no . 1_565
Cl7 H39 3.4771 no . .
Cl8 H11 3.5846 no . 2_666
Cl10 H11 3.1906 no . 2_666
Cl11 H21 3.1097 no . 2_657
Cl11 H23 3.4540 no . 1_455
S3 H15 3.3630 no . 2_756
S3 H17 3.2794 no . 2_756
S3 H22 3.4612 no . 2_757
F1 H3 3.4687 no . 1_545
F1 H5 2.4954 no . 1_545
F1 H10A 3.0689 no . 2_756
F1 H37 3.4137 no . 2_756
F2 H5 3.4416 no . 1_545
F3 H3 2.8379 no . 1_545
F3 H5 3.2280 no . 1_545
F3 H14 2.7784 no . 2_756
F3 H36 3.4017 no . 2_656
F3 H37 3.1202 no . 2_756
F4 H13 3.0795 no . 2_756
F4 H14 3.3792 no . 2_756
F4 H30 3.1746 no . 1_554
F4 H36 2.2224 no . 2_656
F4 H39 3.3139 no . 2_656
F5 H23 2.8675 no . 2_756
F5 H29 3.4964 no . 1_554
F5 H30 3.5611 no . 1_554
F6 H29 2.8294 no . 1_554
F6 H30 2.4457 no . 1_554
F7 H9 2.7738 no . 1_556
F7 H22 2.6941 no . 2_757
F7 H30 3.0766 no . 2_657
F7 H31 3.5672 no . 2_657
F8 H30 3.1378 no . 2_657
F8 H36 3.3364 no . .
F9 H22 3.4410 no . 2_757
O3 H14 3.2131 no . 2_756
O4 H15 3.5504 no . 2_756
O5 H15 2.6482 no . 2_756
O6 H14 2.7594 no . 2_756
N3 H22 3.2879 no . 2_756
N3 H23 3.3797 no . 2_756
N3 H29 2.7839 no . 1_554
N3 H33 3.2641 no . 1_554
C8 H37 3.1674 no . 2_766
C9 H21 3.1682 no . 2_756
C10 H13 3.5958 no . 2_766
C10 H21 3.4766 no . 2_756
C11 H21 2.9748 no . 2_756
C16 H15 3.3883 no . 2_756
C18 H14 3.3366 no . 2_756
C19 H30 3.2631 no . 1_554
C19 H36 3.4547 no . 2_656
C20 H15 2.9996 no . 2_756
C21 H23 3.4876 no . 2_757
C22 H33 3.4118 no . 2_757
C24 H14 3.5532 no . 2_756
C24 H15 2.6604 no . 2_756
C25 H14 3.2150 no . 2_756
C25 H15 3.3123 no . 2_756
C26 H14 2.7919 no . 2_756
C27 H5 3.2758 no . 1_545
C27 H14 3.3232 no . 2_756
C28 H29 3.5833 no . 2_657
C29 H23 3.4781 no . 2_757
C29 H29 3.0751 no . 2_657
C30 H33 3.3983 no . 2_657
C33 H22 3.2766 no . 2_757
C33 H30 3.3680 no . 2_657
C34 H22 3.3417 no . 2_757
C34 H30 3.4051 no . 2_657
C35 H22 3.5911 no . 2_757
C35 H30 3.5439 no . 2_657
C36 H31 3.4532 no . 1_565
C37 H8 3.5036 no . 2_766
C37 H37 3.1687 no . 2_766
H3 F1 3.4687 no . 1_565
H3 F3 2.8379 no . 1_565
H3 H37 2.8796 no . 2_766
H4 Cl1 3.4804 no . .
H4 H36 3.1166 no . .
H5 Cl1 3.0123 no . .
H5 F1 2.4954 no . 1_565
H5 F2 3.4416 no . 1_565
H5 F3 3.2280 no . 1_565
H5 C27 3.2758 no . 1_565
H5 H10A 3.4862 no . 2_766
H8 C37 3.5036 no . 2_766
H8 H37 2.9055 no . 2_766
H9 Cl7 3.1892 no . 2_666
H9 F7 2.7738 no . 1_554
H9 H21 3.3829 no . 2_756
H9 H22 3.2838 no . 2_756
H10A F1 3.0689 no . 2_756
H10A H5 3.4862 no . 2_766
H11 Cl8 3.5846 no . 2_666
H11 Cl10 3.1906 no . 2_666
H11 H21 3.0565 no . 2_756
H13 Cl7 2.9700 no . 1_655
H13 F4 3.0795 no . 2_756
H13 C10 3.5958 no . 2_766
H13 H36 3.5313 no . 1_655
H13 H39 3.5132 no . 1_655
H14 F3 2.7784 no . 2_756
H14 F4 3.3792 no . 2_756
H14 O3 3.2131 no . 2_756
H14 O6 2.7594 no . 2_756
H14 C18 3.3366 no . 2_756
H14 C24 3.5532 no . 2_756
H14 C25 3.2150 no . 2_756
H14 C26 2.7919 no . 2_756
H14 C27 3.3232 no . 2_756
H15 S3 3.3630 no . 2_756
H15 O4 3.5504 no . 2_756
H15 O5 2.6482 no . 2_756
H15 C16 3.3883 no . 2_756
H15 C20 2.9996 no . 2_756
H15 C24 2.6604 no . 2_756
H15 C25 3.3123 no . 2_756
H17 S3 3.2794 no . 2_756
H21 Cl11 3.1097 no . 2_657
H21 C9 3.1682 no . 2_756
H21 C10 3.4766 no . 2_756
H21 C11 2.9748 no . 2_756
H21 H9 3.3829 no . 2_756
H21 H11 3.0565 no . 2_756
H22 S3 3.4612 no . 2_757
H22 F7 2.6941 no . 2_757
H22 F9 3.4410 no . 2_757
H22 N3 3.2879 no . 2_756
H22 C33 3.2766 no . 2_757
H22 C34 3.3417 no . 2_757
H22 C35 3.5911 no . 2_757
H22 H9 3.2838 no . 2_756
H22 H33 2.7112 no . 2_757
H23 Cl11 3.4540 no . 1_655
H23 F5 2.8675 no . 2_756
H23 N3 3.3797 no . 2_756
H23 C21 3.4876 no . 2_757
H23 C29 3.4781 no . 2_757
H23 H29 3.1639 no . 2_757
H23 H33 3.2285 no . 2_757
H29 F5 3.4964 no . 1_556
H29 F6 2.8294 no . 1_556
H29 N3 2.7839 no . 1_556
H29 C28 3.5833 no . 2_657
H29 C29 3.0751 no . 2_657
H29 H23 3.1639 no . 2_757
H29 H29 2.8082 no . 2_657
H29 H33 3.5435 no . 2_657
H30 Cl2 3.1851 no . 2_657
H30 F4 3.1746 no . 1_556
H30 F5 3.5611 no . 1_556
H30 F6 2.4457 no . 1_556
H30 F7 3.0766 no . 2_657
H30 F8 3.1378 no . 2_657
H30 C19 3.2631 no . 1_556
H30 C33 3.3680 no . 2_657
H30 C34 3.4051 no . 2_657
H30 C35 3.5439 no . 2_657
H30 H33 3.1390 no . 2_657
H31 Cl1 3.2881 no . 1_545
H31 Cl2 3.2899 no . 1_545
H31 Cl2 3.1634 no . 2_657
H31 Cl7 3.3458 no . 1_545
H31 F7 3.5672 no . 2_657
H31 C36 3.4532 no . 1_545
H33 N3 3.2641 no . 1_556
H33 C22 3.4118 no . 2_757
H33 C30 3.3983 no . 2_657
H33 H22 2.7112 no . 2_757
H33 H23 3.2285 no . 2_757
H33 H29 3.5435 no . 2_657
H33 H30 3.1390 no . 2_657
H36 F3 3.4017 no . 2_656
H36 F4 2.2224 no . 2_656
H36 F8 3.3364 no . .
H36 C19 3.4547 no . 2_656
H36 H4 3.1166 no . .
H36 H13 3.5313 no . 1_455
H37 F1 3.4137 no . 2_756
H37 F3 3.1202 no . 2_756
H37 C8 3.1674 no . 2_766
H37 C37 3.1687 no . 2_766
H37 H3 2.8796 no . 2_766
H37 H8 2.9055 no . 2_766
H37 H37 2.8948 no . 2_766
H39 Cl2 2.9444 no . .
H39 Cl7 3.4771 no . .
H39 F4 3.3139 no . 2_656
H39 H13 3.5132 no . 1_455

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.

#==============================================================================
#     End of CIF
#==============================================================================
