# 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. 
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data_Smtmoga_270K
_database_code_depnum_ccdc_archive 'CCDC 1434511'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H48 Cl3 N6 O21 Sm'
_chemical_formula_weight         1013.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0076 0.0040
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1697 0.1896
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Sm Sm -0.0663 4.0092
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.5604(7)
_cell_length_b                   14.3327(5)
_cell_length_c                   14.8420(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.143(2)
_cell_angle_gamma                90
_cell_volume                     4096.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    9334
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      34.07

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             2060
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.146
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_process_details   'SADABS 2014/5 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      270(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            27012
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.306
_diffrn_reflns_theta_max         34.234
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6559
_reflns_number_gt                5604
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 Once solved by SHELXT the model for the Eu version of the compound was
 used for the refinement, with Eu changed for Sm, to keep the numdering
 identical.
 All non-hydrogen atoms were refined anisotropically. Hydrogen atoms
 were placed geometrically on the carbon atoms, constrained and refined
 using a riding model. Geometrically and displacement parameter
 restraints were under to model the disordered perchlorate. Some of
 the perchlorate oxygen atoms still have displacement parameter ratios 
 that are larger than ideal. These were left as they were as it best
 reflects the nature of the perchlorates. Data was collected at 270K 
 as the compound undergo a phase transition at low temperature.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0521P)²+3.0530P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6559
_refine_ls_number_parameters     306
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.5000 0.69019(2) 0.2500 0.03832(6) Uani 1 2 d S T P . .
O1 O 0.50241(10) 0.55894(14) 0.15150(16) 0.0552(5) Uani 1 1 d . . . . .
C1 C 0.45412(13) 0.50366(19) 0.12298(19) 0.0457(5) Uani 1 1 d . . . . .
C2 C 0.38119(14) 0.5281(2) 0.1360(2) 0.0516(6) Uani 1 1 d . . . . .
H2A H 0.3521 0.5414 0.0775 0.062 Uiso 1 1 calc R U . . .
H2B H 0.3608 0.4767 0.1646 0.062 Uiso 1 1 calc R U . . .
O2 O 0.38675(8) 0.60774(13) 0.19284(14) 0.0495(4) Uani 1 1 d . . . . .
C3 C 0.32225(12) 0.6396(2) 0.2117(2) 0.0538(7) Uani 1 1 d . . . . .
H3A H 0.2959 0.5880 0.2304 0.065 Uiso 1 1 calc R U . . .
H3B H 0.2952 0.6682 0.1577 0.065 Uiso 1 1 calc R U . . .
C4 C 0.33847(13) 0.71023(19) 0.2880(2) 0.0460(5) Uani 1 1 d . . . . .
O3 O 0.39968(9) 0.73639(14) 0.31283(13) 0.0489(4) Uani 1 1 d . . . . .
N1 N 0.46444(13) 0.42441(16) 0.08339(17) 0.0528(5) Uani 1 1 d . . . . .
C5 C 0.53571(18) 0.3940(2) 0.0790(3) 0.0658(8) Uani 1 1 d . . . . .
H5A H 0.5654 0.4476 0.0813 0.099 Uiso 1 1 calc R U . . .
H5B H 0.5359 0.3607 0.0230 0.099 Uiso 1 1 calc R U . . .
H5C H 0.5523 0.3540 0.1300 0.099 Uiso 1 1 calc R U . . .
C6 C 0.4089(2) 0.3605(2) 0.0446(3) 0.0728(10) Uani 1 1 d . . . . .
H6A H 0.4144 0.3026 0.0776 0.109 Uiso 1 1 calc R U . . .
H6B H 0.4111 0.3493 -0.0186 0.109 Uiso 1 1 calc R U . . .
H6C H 0.3648 0.3877 0.0493 0.109 Uiso 1 1 calc R U . . .
N2 N 0.28680(12) 0.7430(2) 0.32526(19) 0.0582(6) Uani 1 1 d . . . . .
C7 C 0.3008(2) 0.8165(3) 0.3936(3) 0.0745(10) Uani 1 1 d . . . . .
H7A H 0.3497 0.8289 0.4066 0.112 Uiso 1 1 calc R U . . .
H7B H 0.2854 0.7969 0.4486 0.112 Uiso 1 1 calc R U . . .
H7C H 0.2763 0.8721 0.3707 0.112 Uiso 1 1 calc R U . . .
C8 C 0.21423(17) 0.7139(3) 0.2980(3) 0.0797(11) Uani 1 1 d . . . . .
H8A H 0.1889 0.7614 0.2604 0.120 Uiso 1 1 calc R U . . .
H8B H 0.1939 0.7046 0.3517 0.120 Uiso 1 1 calc R U . . .
H8C H 0.2124 0.6567 0.2641 0.120 Uiso 1 1 calc R U . . .
O4 O 0.55579(11) 0.76789(16) 0.38628(14) 0.0561(5) Uani 1 1 d . . . . .
C9 C 0.56145(15) 0.8533(2) 0.3998(2) 0.0549(7) Uani 1 1 d . . . . .
C10 C 0.52997(17) 0.9196(2) 0.3256(2) 0.0604(7) Uani 1 1 d . . . . .
H10A H 0.4948 0.9578 0.3462 0.072 Uiso 1 1 calc R U . . .
H10B H 0.5654 0.9603 0.3090 0.072 Uiso 1 1 calc R U . . .
O5 O 0.5000 0.86465(17) 0.2500 0.0491(6) Uani 1 2 d S T P . .
N3 N 0.59522(16) 0.8887(3) 0.47752(19) 0.0770(9) Uani 1 1 d . . . . .
C11 C 0.6341(3) 0.8262(4) 0.5464(3) 0.1031(18) Uani 1 1 d . . . . .
H11A H 0.6375 0.7656 0.5200 0.155 Uiso 1 1 calc R U . . .
H11B H 0.6103 0.8212 0.5975 0.155 Uiso 1 1 calc R U . . .
H11C H 0.6798 0.8509 0.5668 0.155 Uiso 1 1 calc R U . . .
C12 C 0.6032(3) 0.9882(4) 0.4937(4) 0.115(2) Uani 1 1 d . . . . .
H12A H 0.6454 1.0091 0.4756 0.172 Uiso 1 1 calc R U . . .
H12B H 0.6050 1.0008 0.5576 0.172 Uiso 1 1 calc R U . . .
H12C H 0.5645 1.0206 0.4587 0.172 Uiso 1 1 calc R U . . .
Cl1 Cl 0.24557(5) 0.93199(8) 0.13968(9) 0.0845(3) Uani 1 1 d . . . . .
O11 O 0.1961(2) 0.9270(4) 0.1967(4) 0.1530(19) Uani 1 1 d . . . . .
O12 O 0.3069(2) 0.9524(5) 0.1920(5) 0.212(3) Uani 1 1 d . . . . .
O13 O 0.2509(5) 0.8505(4) 0.1001(6) 0.287(6) Uani 1 1 d . . . . .
O14 O 0.2317(3) 1.0007(4) 0.0760(4) 0.182(2) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 0.17687(10) 0.2500 0.1046(7) Uani 1 2 d DS TU P . .
O21 O 0.5315(9) 0.2678(6) 0.2554(17) 0.097(6) Uani 0.25 1 d D U P A 1
O22 O 0.5557(5) 0.1161(8) 0.2327(10) 0.062(3) Uani 0.25 1 d D U P A 1
O23 O 0.4429(10) 0.1684(14) 0.1777(15) 0.199(14) Uani 0.25 1 d D U P A 1
O24 O 0.4837(15) 0.1526(16) 0.3367(11) 0.26(3) Uani 0.25 1 d D . P B 1
O21' O 0.5000 0.2753(5) 0.2500 0.140(8) Uani 0.5 2 d DS TU P A 2
O22' O 0.5675(5) 0.1381(10) 0.2694(14) 0.105(6) Uani 0.25 1 d D U P A 2
O23' O 0.4760(10) 0.1502(9) 0.1529(6) 0.098(5) Uani 0.25 1 d D U P C 2
O24' O 0.4536(9) 0.1328(10) 0.2996(12) 0.101(6) Uani 0.25 1 d D U P A 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
Sm1 O1 2.3880(19) 2_655 ?
Sm1 O1 2.3880(19) . ?
Sm1 O4 2.3968(19) . ?
Sm1 O4 2.3968(19) 2_655 ?
Sm1 O3 2.4089(18) 2_655 ?
Sm1 O3 2.4089(18) . ?
Sm1 O5 2.501(2) . ?
Sm1 O2 2.5222(16) 2_655 ?
Sm1 O2 2.5222(16) . ?
O1 C1 1.248(3) . ?
C1 N1 1.311(3) . ?
C1 C2 1.514(4) . ?
C2 O2 1.412(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O2 C3 1.415(3) . ?
C3 C4 1.511(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.247(3) . ?
C4 N2 1.321(3) . ?
N1 C6 1.459(4) . ?
N1 C5 1.473(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N2 C7 1.454(4) . ?
N2 C8 1.466(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O4 C9 1.242(4) . ?
C9 N3 1.325(4) . ?
C9 C10 1.502(5) . ?
C10 O5 1.412(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5 C10 1.412(3) 2_655 ?
N3 C12 1.450(6) . ?
N3 C11 1.467(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
Cl1 O13 1.320(5) . ?
Cl1 O12 1.342(5) . ?
Cl1 O14 1.359(5) . ?
Cl1 O11 1.396(4) . ?
Cl2 O23 1.411(8) . ?
Cl2 O23 1.411(8) 2_655 ?
Cl2 O21' 1.411(7) . ?
Cl2 O22' 1.414(7) . ?
Cl2 O22' 1.414(7) 2_655 ?
Cl2 O24' 1.415(7) 2_655 ?
Cl2 O24' 1.415(7) . ?
Cl2 O21 1.438(7) . ?
Cl2 O21 1.438(7) 2_655 ?
Cl2 O22 1.453(7) 2_655 ?
Cl2 O22 1.453(7) . ?
Cl2 O24 1.422(8) 2_655 ?
O21 O21 1.21(3) 2_655 ?
O21 O23 1.76(3) 2_655 ?
O22 O23 1.52(2) 2_655 ?
O22 O24 1.28(3) 2_655 ?
O23 O22 1.52(2) 2_655 ?
O23 O24 1.51(2) 2_655 ?
O23 O21 1.76(3) 2_655 ?
O24 O22 1.28(3) 2_655 ?
O24 O23 1.51(2) 2_655 ?
O22' O24' 1.04(2) 2_655 ?
O22' O23' 1.56(2) 2_655 ?
O23' O24' 1.45(2) 2_655 ?
O23' O22' 1.56(2) 2_655 ?
O24' O22' 1.04(2) 2_655 ?
O24' O23' 1.45(2) 2_655 ?

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
O1 Sm1 O1 76.05(11) 2_655 . ?
O1 Sm1 O4 84.52(8) 2_655 . ?
O1 Sm1 O4 145.85(8) . . ?
O1 Sm1 O4 145.85(8) 2_655 2_655 ?
O1 Sm1 O4 84.52(8) . 2_655 ?
O4 Sm1 O4 124.63(11) . 2_655 ?
O1 Sm1 O3 123.97(6) 2_655 2_655 ?
O1 Sm1 O3 82.78(7) . 2_655 ?
O4 Sm1 O3 85.30(7) . 2_655 ?
O4 Sm1 O3 80.01(7) 2_655 2_655 ?
O1 Sm1 O3 82.78(7) 2_655 . ?
O1 Sm1 O3 123.97(6) . . ?
O4 Sm1 O3 80.01(7) . . ?
O4 Sm1 O3 85.30(7) 2_655 . ?
O3 Sm1 O3 148.09(10) 2_655 . ?
O1 Sm1 O5 141.98(6) 2_655 . ?
O1 Sm1 O5 141.98(6) . . ?
O4 Sm1 O5 62.31(5) . . ?
O4 Sm1 O5 62.31(5) 2_655 . ?
O3 Sm1 O5 74.04(5) 2_655 . ?
O3 Sm1 O5 74.04(5) . . ?
O1 Sm1 O2 62.34(6) 2_655 2_655 ?
O1 Sm1 O2 74.10(7) . 2_655 ?
O4 Sm1 O2 72.03(7) . 2_655 ?
O4 Sm1 O2 138.07(7) 2_655 2_655 ?
O3 Sm1 O2 62.09(6) 2_655 2_655 ?
O3 Sm1 O2 136.52(6) . 2_655 ?
O5 Sm1 O2 117.94(4) . 2_655 ?
O1 Sm1 O2 74.10(7) 2_655 . ?
O1 Sm1 O2 62.34(6) . . ?
O4 Sm1 O2 138.07(7) . . ?
O4 Sm1 O2 72.03(7) 2_655 . ?
O3 Sm1 O2 136.52(6) 2_655 . ?
O3 Sm1 O2 62.09(6) . . ?
O5 Sm1 O2 117.94(4) . . ?
O2 Sm1 O2 124.12(9) 2_655 . ?
C1 O1 Sm1 127.75(17) . . ?
O1 C1 N1 122.3(2) . . ?
O1 C1 C2 118.9(2) . . ?
N1 C1 C2 118.7(2) . . ?
O2 C2 C1 106.8(2) . . ?
O2 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
O2 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C2 O2 C3 113.66(19) . . ?
C2 O2 Sm1 123.39(14) . . ?
C3 O2 Sm1 122.90(15) . . ?
O2 C3 C4 106.7(2) . . ?
O2 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
O2 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
O3 C4 N2 122.4(3) . . ?
O3 C4 C3 119.1(2) . . ?
N2 C4 C3 118.5(2) . . ?
C4 O3 Sm1 127.48(17) . . ?
C1 N1 C6 123.9(3) . . ?
C1 N1 C5 119.8(3) . . ?
C6 N1 C5 116.2(3) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 N2 C7 119.1(3) . . ?
C4 N2 C8 123.9(3) . . ?
C7 N2 C8 116.9(3) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 O4 Sm1 127.49(18) . . ?
O4 C9 N3 122.3(3) . . ?
O4 C9 C10 119.5(2) . . ?
N3 C9 C10 118.2(3) . . ?
O5 C10 C9 106.8(2) . . ?
O5 C10 H10A 110.4 . . ?
C9 C10 H10A 110.4 . . ?
O5 C10 H10B 110.4 . . ?
C9 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
C10 O5 C10 112.1(3) . 2_655 ?
C10 O5 Sm1 123.93(16) . . ?
C10 O5 Sm1 123.93(16) 2_655 . ?
C9 N3 C12 122.9(4) . . ?
C9 N3 C11 119.4(4) . . ?
C12 N3 C11 117.2(3) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 Cl1 O12 108.5(6) . . ?
O13 Cl1 O14 110.7(5) . . ?
O12 Cl1 O14 107.1(4) . . ?
O13 Cl1 O11 110.0(4) . . ?
O12 Cl1 O11 107.8(4) . . ?
O14 Cl1 O11 112.6(3) . . ?
O23 Cl2 O23 170.2(16) . 2_655 ?
O21' Cl2 O22' 113.2(6) . . ?
O21' Cl2 O22' 113.2(6) . 2_655 ?
O22' Cl2 O22' 133.7(13) . 2_655 ?
O21' Cl2 O24' 116.5(7) . 2_655 ?
O22' Cl2 O24' 43.0(8) . 2_655 ?
O22' Cl2 O24' 112.3(8) 2_655 2_655 ?
O21' Cl2 O24' 116.5(7) . . ?
O22' Cl2 O24' 112.3(8) . . ?
O22' Cl2 O24' 43.0(8) 2_655 . ?
O24' Cl2 O24' 127.0(13) 2_655 . ?
O23 Cl2 O21 113.2(9) . . ?
O23 Cl2 O21 76.2(14) 2_655 . ?
O23 Cl2 O21 76.2(14) . 2_655 ?
O23 Cl2 O21 113.2(9) 2_655 2_655 ?
O21 Cl2 O21 50.0(15) . 2_655 ?
O23 Cl2 O22 64.2(11) . 2_655 ?
O23 Cl2 O22 109.4(9) 2_655 2_655 ?
O21 Cl2 O22 149.4(10) . 2_655 ?
O21 Cl2 O22 103.1(7) 2_655 2_655 ?
O23 Cl2 O22 109.4(9) . . ?
O23 Cl2 O22 64.2(11) 2_655 . ?
O21 Cl2 O22 103.1(7) . . ?
O21 Cl2 O22 149.5(11) 2_655 . ?
O22 Cl2 O22 106.3(10) 2_655 . ?
O23 Cl2 O24 64.2(9) . 2_655 ?
O23 Cl2 O24 113.2(9) 2_655 2_655 ?
O21 Cl2 O24 96.3(15) . 2_655 ?
O21 Cl2 O24 109.5(9) 2_655 2_655 ?
O22 Cl2 O24 107.9(8) 2_655 2_655 ?
O22 Cl2 O24 53.0(11) . 2_655 ?
O21 O21 Cl2 65.0(7) 2_655 . ?
O21 O21 O23 104.8(14) 2_655 2_655 ?
Cl2 O21 O23 51.2(7) . 2_655 ?
O23 O22 O24 114.6(9) 2_655 2_655 ?
O23 O22 Cl2 56.6(6) 2_655 . ?
O24 O22 Cl2 62.3(6) 2_655 . ?
O22 O23 Cl2 59.2(7) 2_655 . ?
O22 O23 O24 100.3(13) 2_655 2_655 ?
Cl2 O23 O24 58.2(6) . 2_655 ?
O22 O23 O21 86.9(10) 2_655 2_655 ?
Cl2 O23 O21 52.6(8) . 2_655 ?
O24 O23 O21 91.1(11) 2_655 2_655 ?
O22 O24 Cl2 64.7(7) 2_655 . ?
O22 O24 O23 113.6(14) 2_655 2_655 ?
Cl2 O24 O23 57.6(6) . 2_655 ?
O24' O22' Cl2 68.5(6) 2_655 . ?
O24' O22' O23' 124.4(12) 2_655 2_655 ?
Cl2 O22' O23' 59.7(5) . 2_655 ?
Cl2 O23' O24' 57.5(5) . 2_655 ?
Cl2 O23' O22' 55.3(5) . 2_655 ?
O24' O23' O22' 102.5(9) 2_655 2_655 ?
O22' O24' Cl2 68.5(6) 2_655 . ?
O22' O24' O23' 130.1(10) 2_655 2_655 ?
Cl2 O24' O23' 62.3(6) . 2_655 ?

_refine_diff_density_max         0.613
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.078

####################################################################### 
# 
# 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_eutmoga_270k
_database_code_depnum_ccdc_archive 'CCDC 1434512'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H48 Cl3 Eu N6 O21'
_chemical_formula_weight         1014.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0076 0.0040
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1697 0.1896
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Eu Eu -0.0721 4.2696
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.490(3)
_cell_length_b                   14.339(2)
_cell_length_c                   14.811(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.191(2)
_cell_angle_gamma                90
_cell_volume                     4073.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    9097
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      34.10

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_F_000             2064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.271
_shelx_estimated_absorpt_T_min   0.659
_shelx_estimated_absorpt_T_max   0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      270(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            22853
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.933
_diffrn_reflns_theta_max         34.203
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6521
_reflns_number_gt                5518
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen atoms
 were placed geometrically on the carbon atoms, constrained and refined
 using a riding model. Geometrically and displacement parameter
 restraints were under to model the disordered perchlorate. Some of
 the perchlorate oxygen atoms still have displacement parameter ratios 
 that are larger than ideal. These were left as they were as it best
 reflects the nature of the perchlorates. Data was collected at 270K 
 as the compound undergo a phase transition at low temperature.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+2.0469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6521
_refine_ls_number_parameters     306
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.077
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.5000 0.69012(2) 0.2500 0.03582(6) Uani 1 2 d S T P . .
O1 O 0.50285(11) 0.55955(15) 0.15133(17) 0.0514(5) Uani 1 1 d . . . . .
C1 C 0.45439(15) 0.5043(2) 0.1233(2) 0.0441(6) Uani 1 1 d . . . . .
C2 C 0.38127(15) 0.5290(2) 0.1361(2) 0.0489(7) Uani 1 1 d . . . . .
H2A H 0.3522 0.5426 0.0774 0.059 Uiso 1 1 calc R U . . .
H2B H 0.3606 0.4776 0.1644 0.059 Uiso 1 1 calc R U . . .
O2 O 0.38702(9) 0.60814(14) 0.19323(15) 0.0462(5) Uani 1 1 d . . . . .
C3 C 0.32217(14) 0.6397(2) 0.2123(2) 0.0511(7) Uani 1 1 d . . . . .
H3A H 0.2959 0.5880 0.2313 0.061 Uiso 1 1 calc R U . . .
H3B H 0.2948 0.6681 0.1582 0.061 Uiso 1 1 calc R U . . .
C4 C 0.33890(14) 0.7105(2) 0.2889(2) 0.0434(6) Uani 1 1 d . . . . .
O3 O 0.40041(10) 0.73673(15) 0.31331(15) 0.0464(4) Uani 1 1 d . . . . .
N1 N 0.46484(14) 0.42484(17) 0.08333(19) 0.0494(6) Uani 1 1 d . . . . .
C5 C 0.53638(19) 0.3948(2) 0.0800(3) 0.0615(9) Uani 1 1 d . . . . .
H5A H 0.5665 0.4482 0.0855 0.092 Uiso 1 1 calc R U . . .
H5B H 0.5374 0.3640 0.0228 0.092 Uiso 1 1 calc R U . . .
H5C H 0.5520 0.3526 0.1297 0.092 Uiso 1 1 calc R U . . .
C6 C 0.4090(2) 0.3609(3) 0.0448(3) 0.0687(10) Uani 1 1 d . . . . .
H6A H 0.4172 0.3011 0.0737 0.103 Uiso 1 1 calc R U . . .
H6B H 0.4080 0.3545 -0.0200 0.103 Uiso 1 1 calc R U . . .
H6C H 0.3652 0.3851 0.0552 0.103 Uiso 1 1 calc R U . . .
N2 N 0.28714(13) 0.7432(2) 0.3268(2) 0.0533(6) Uani 1 1 d . . . . .
C7 C 0.3019(2) 0.8169(3) 0.3950(3) 0.0676(10) Uani 1 1 d . . . . .
H7A H 0.3507 0.8311 0.4053 0.101 Uiso 1 1 calc R U . . .
H7B H 0.2889 0.7965 0.4514 0.101 Uiso 1 1 calc R U . . .
H7C H 0.2757 0.8716 0.3733 0.101 Uiso 1 1 calc R U . . .
C8 C 0.21449(19) 0.7140(3) 0.2996(4) 0.0760(12) Uani 1 1 d . . . . .
H8A H 0.1893 0.7606 0.2607 0.114 Uiso 1 1 calc R U . . .
H8B H 0.1938 0.7062 0.3533 0.114 Uiso 1 1 calc R U . . .
H8C H 0.2127 0.6559 0.2670 0.114 Uiso 1 1 calc R U . . .
O4 O 0.55595(12) 0.76647(17) 0.38618(15) 0.0529(5) Uani 1 1 d . . . . .
C9 C 0.56134(16) 0.8523(3) 0.4001(2) 0.0519(7) Uani 1 1 d . . . . .
C10 C 0.5297(2) 0.9181(2) 0.3261(3) 0.0590(8) Uani 1 1 d . . . . .
H10A H 0.4941 0.9558 0.3467 0.071 Uiso 1 1 calc R U . . .
H10B H 0.5650 0.9592 0.3097 0.071 Uiso 1 1 calc R U . . .
O5 O 0.5000 0.86356(19) 0.2500 0.0460(6) Uani 1 2 d S T P . .
N3 N 0.59571(17) 0.8870(3) 0.4779(2) 0.0726(10) Uani 1 1 d . . . . .
C11 C 0.6346(3) 0.8246(4) 0.5468(3) 0.0953(18) Uani 1 1 d . . . . .
H11A H 0.6354 0.7630 0.5216 0.143 Uiso 1 1 calc R U . . .
H11B H 0.6125 0.8227 0.5997 0.143 Uiso 1 1 calc R U . . .
H11C H 0.6815 0.8470 0.5643 0.143 Uiso 1 1 calc R U . . .
C12 C 0.6032(3) 0.9872(4) 0.4940(4) 0.108(2) Uani 1 1 d . . . . .
H12A H 0.6436 1.0093 0.4718 0.162 Uiso 1 1 calc R U . . .
H12B H 0.6084 0.9995 0.5586 0.162 Uiso 1 1 calc R U . . .
H12C H 0.5625 1.0187 0.4623 0.162 Uiso 1 1 calc R U . . .
Cl1 Cl 0.24594(5) 0.93127(8) 0.14120(9) 0.0788(3) Uani 1 1 d . . . . .
O11 O 0.1960(2) 0.9251(4) 0.1982(4) 0.1391(18) Uani 1 1 d . . . . .
O12 O 0.3076(3) 0.9543(6) 0.1937(5) 0.201(3) Uani 1 1 d . . . . .
O13 O 0.2526(6) 0.8496(4) 0.1025(6) 0.273(6) Uani 1 1 d . . . . .
O14 O 0.2309(3) 0.9996(4) 0.0771(4) 0.170(2) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 0.17567(11) 0.2500 0.0991(7) Uani 1 2 d DS TU P . .
O21 O 0.5293(10) 0.2674(6) 0.2572(18) 0.094(7) Uani 0.25 1 d D U P A 1
O22 O 0.5550(6) 0.1172(8) 0.2286(11) 0.061(3) Uani 0.25 1 d D U P A 1
O23 O 0.4406(10) 0.1683(15) 0.1812(17) 0.203(15) Uani 0.25 1 d D U P A 1
O24 O 0.4873(15) 0.1454(16) 0.3369(12) 0.27(3) Uani 0.25 1 d D . P B 1
O21' O 0.5000 0.2740(5) 0.2500 0.139(9) Uani 0.5 2 d DS TU P A 2
O22' O 0.5674(4) 0.1370(10) 0.2641(13) 0.088(5) Uani 0.25 1 d D U P A 2
O23' O 0.4723(10) 0.1482(9) 0.1549(7) 0.101(5) Uani 0.25 1 d D U P C 2
O24' O 0.4564(11) 0.1354(13) 0.3053(14) 0.134(9) Uani 0.25 1 d D U P A 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
Eu1 O1 2.382(2) . ?
Eu1 O1 2.382(2) 2_655 ?
Eu1 O4 2.383(2) 2_655 ?
Eu1 O4 2.383(2) . ?
Eu1 O3 2.3952(19) 2_655 ?
Eu1 O3 2.3953(19) . ?
Eu1 O5 2.487(3) . ?
Eu1 O2 2.5064(18) . ?
Eu1 O2 2.5064(18) 2_655 ?
O1 C1 1.246(3) . ?
C1 N1 1.316(4) . ?
C1 C2 1.513(4) . ?
C2 O2 1.408(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O2 C3 1.417(3) . ?
C3 C4 1.515(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.247(3) . ?
C4 N2 1.324(4) . ?
N1 C6 1.460(4) . ?
N1 C5 1.468(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N2 C7 1.455(5) . ?
N2 C8 1.463(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O4 C9 1.249(4) . ?
C9 N3 1.324(4) . ?
C9 C10 1.495(5) . ?
C10 O5 1.408(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5 C10 1.408(3) 2_655 ?
N3 C12 1.459(6) . ?
N3 C11 1.464(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
Cl1 O13 1.320(6) . ?
Cl1 O12 1.351(5) . ?
Cl1 O14 1.360(5) . ?
Cl1 O11 1.400(4) . ?
Cl2 O23 1.404(8) . ?
Cl2 O23 1.404(8) 2_655 ?
Cl2 O24' 1.404(8) . ?
Cl2 O24' 1.404(8) 2_655 ?
Cl2 O21' 1.410(7) . ?
Cl2 O22' 1.407(7) . ?
Cl2 O22' 1.407(7) 2_655 ?
Cl2 O21 1.431(7) . ?
Cl2 O21 1.431(7) 2_655 ?
Cl2 O22 1.439(8) . ?
Cl2 O22 1.439(8) 2_655 ?
Cl2 O24 1.421(8) 2_655 ?
O21 O21 1.12(4) 2_655 ?
O21 O23 1.73(3) 2_655 ?
O22 O23 1.51(3) 2_655 ?
O22 O24 1.23(3) 2_655 ?
O23 O22 1.51(3) 2_655 ?
O23 O24 1.51(2) 2_655 ?
O23 O21 1.73(3) 2_655 ?
O24 O22 1.23(3) 2_655 ?
O24 O23 1.51(2) 2_655 ?
O22' O24' 1.05(2) 2_655 ?
O22' O23' 1.55(2) 2_655 ?
O23' O24' 1.42(2) 2_655 ?
O23' O22' 1.55(2) 2_655 ?
O24' O22' 1.05(2) 2_655 ?
O24' O23' 1.42(2) 2_655 ?

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
O1 Eu1 O1 76.36(12) . 2_655 ?
O1 Eu1 O4 84.18(8) . 2_655 ?
O1 Eu1 O4 145.46(8) 2_655 2_655 ?
O1 Eu1 O4 145.46(8) . . ?
O1 Eu1 O4 84.18(8) 2_655 . ?
O4 Eu1 O4 125.29(12) 2_655 . ?
O1 Eu1 O3 82.57(8) . 2_655 ?
O1 Eu1 O3 124.61(7) 2_655 2_655 ?
O4 Eu1 O3 79.72(8) 2_655 2_655 ?
O4 Eu1 O3 85.52(8) . 2_655 ?
O1 Eu1 O3 124.62(7) . . ?
O1 Eu1 O3 82.57(8) 2_655 . ?
O4 Eu1 O3 85.53(8) 2_655 . ?
O4 Eu1 O3 79.72(8) . . ?
O3 Eu1 O3 147.59(10) 2_655 . ?
O1 Eu1 O5 141.82(6) . . ?
O1 Eu1 O5 141.82(6) 2_655 . ?
O4 Eu1 O5 62.65(6) 2_655 . ?
O4 Eu1 O5 62.65(6) . . ?
O3 Eu1 O5 73.79(5) 2_655 . ?
O3 Eu1 O5 73.80(5) . . ?
O1 Eu1 O2 62.61(7) . . ?
O1 Eu1 O2 73.90(8) 2_655 . ?
O4 Eu1 O2 71.83(8) 2_655 . ?
O4 Eu1 O2 137.97(7) . . ?
O3 Eu1 O2 136.40(7) 2_655 . ?
O3 Eu1 O2 62.46(6) . . ?
O5 Eu1 O2 117.97(5) . . ?
O1 Eu1 O2 73.90(8) . 2_655 ?
O1 Eu1 O2 62.61(6) 2_655 2_655 ?
O4 Eu1 O2 137.97(7) 2_655 2_655 ?
O4 Eu1 O2 71.83(8) . 2_655 ?
O3 Eu1 O2 62.46(6) 2_655 2_655 ?
O3 Eu1 O2 136.40(7) . 2_655 ?
O5 Eu1 O2 117.97(5) . 2_655 ?
O2 Eu1 O2 124.06(10) . 2_655 ?
C1 O1 Eu1 127.25(18) . . ?
O1 C1 N1 122.1(3) . . ?
O1 C1 C2 119.0(3) . . ?
N1 C1 C2 118.9(3) . . ?
O2 C2 C1 106.7(2) . . ?
O2 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
O2 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C2 O2 C3 113.4(2) . . ?
C2 O2 Eu1 123.47(15) . . ?
C3 O2 Eu1 123.05(16) . . ?
O2 C3 C4 106.4(2) . . ?
O2 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
O2 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.6 . . ?
O3 C4 N2 122.4(3) . . ?
O3 C4 C3 119.2(2) . . ?
N2 C4 C3 118.4(3) . . ?
C4 O3 Eu1 127.32(18) . . ?
C1 N1 C6 123.7(3) . . ?
C1 N1 C5 119.5(3) . . ?
C6 N1 C5 116.7(3) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 N2 C7 118.7(3) . . ?
C4 N2 C8 123.7(3) . . ?
C7 N2 C8 117.5(3) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 O4 Eu1 127.2(2) . . ?
O4 C9 N3 121.9(4) . . ?
O4 C9 C10 119.3(3) . . ?
N3 C9 C10 118.8(3) . . ?
O5 C10 C9 107.1(3) . . ?
O5 C10 H10A 110.3 . . ?
C9 C10 H10A 110.3 . . ?
O5 C10 H10B 110.3 . . ?
C9 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
C10 O5 C10 112.6(4) 2_655 . ?
C10 O5 Eu1 123.71(18) 2_655 . ?
C10 O5 Eu1 123.71(18) . . ?
C9 N3 C12 122.2(4) . . ?
C9 N3 C11 119.8(4) . . ?
C12 N3 C11 117.6(4) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 Cl1 O12 108.7(6) . . ?
O13 Cl1 O14 111.2(5) . . ?
O12 Cl1 O14 106.6(4) . . ?
O13 Cl1 O11 109.8(4) . . ?
O12 Cl1 O11 108.1(4) . . ?
O14 Cl1 O11 112.3(4) . . ?
O23 Cl2 O23 171.4(18) . 2_655 ?
O24' Cl2 O24' 131.4(17) . 2_655 ?
O24' Cl2 O21' 114.3(8) . . ?
O24' Cl2 O21' 114.3(8) 2_655 . ?
O24' Cl2 O22' 113.4(9) . . ?
O24' Cl2 O22' 43.9(9) 2_655 . ?
O21' Cl2 O22' 113.2(6) . . ?
O24' Cl2 O22' 43.9(9) . 2_655 ?
O24' Cl2 O22' 113.4(9) 2_655 2_655 ?
O21' Cl2 O22' 113.2(6) . 2_655 ?
O22' Cl2 O22' 133.6(12) . 2_655 ?
O23 Cl2 O21 112.9(9) . . ?
O23 Cl2 O21 75.4(15) 2_655 . ?
O23 Cl2 O21 75.4(15) . 2_655 ?
O23 Cl2 O21 112.9(9) 2_655 2_655 ?
O21 Cl2 O21 46.3(15) . 2_655 ?
O23 Cl2 O22 110.3(9) . . ?
O23 Cl2 O22 64.3(12) 2_655 . ?
O21 Cl2 O22 104.4(7) . . ?
O21 Cl2 O22 145.3(11) 2_655 . ?
O23 Cl2 O22 64.3(12) . 2_655 ?
O23 Cl2 O22 110.3(9) 2_655 2_655 ?
O21 Cl2 O22 145.3(11) . 2_655 ?
O21 Cl2 O22 104.4(7) 2_655 2_655 ?
O22 Cl2 O22 108.8(11) . 2_655 ?
O23 Cl2 O24 64.7(10) . 2_655 ?
O23 Cl2 O24 112.4(9) 2_655 2_655 ?
O21 Cl2 O24 102.5(16) . 2_655 ?
O21 Cl2 O24 110.2(9) 2_655 2_655 ?
O22 Cl2 O24 50.7(12) . 2_655 ?
O22 Cl2 O24 106.1(8) 2_655 2_655 ?
O21 O21 Cl2 66.9(8) 2_655 . ?
O21 O21 O23 109.7(15) 2_655 2_655 ?
Cl2 O21 O23 51.6(7) . 2_655 ?
O23 O22 O24 117.7(9) 2_655 2_655 ?
O23 O22 Cl2 56.7(6) 2_655 . ?
O24 O22 Cl2 63.9(7) 2_655 . ?
O22 O23 Cl2 59.0(7) 2_655 . ?
O22 O23 O24 98.2(14) 2_655 2_655 ?
Cl2 O23 O24 58.2(6) . 2_655 ?
O22 O23 O21 88.4(10) 2_655 2_655 ?
Cl2 O23 O21 53.0(9) . 2_655 ?
O24 O23 O21 91.9(11) 2_655 2_655 ?
O22 O24 Cl2 65.4(8) 2_655 . ?
O22 O24 O23 116.5(14) 2_655 2_655 ?
Cl2 O24 O23 57.1(6) . 2_655 ?
O24' O22' Cl2 67.9(7) 2_655 . ?
O24' O22' O23' 124.4(12) 2_655 2_655 ?
Cl2 O22' O23' 59.4(5) . 2_655 ?
Cl2 O23' O24' 58.1(6) . 2_655 ?
Cl2 O23' O22' 55.5(5) . 2_655 ?
O24' O23' O22' 104.5(10) 2_655 2_655 ?
O22' O24' Cl2 68.2(7) 2_655 . ?
O22' O24' O23' 129.3(12) 2_655 2_655 ?
Cl2 O24' O23' 62.7(6) . 2_655 ?

_refine_diff_density_max         0.702
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_TbTmoga_270K
_database_code_depnum_ccdc_archive 'CCDC 1434513'
_audit_update_record             
;
2015-11-01 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H48 Cl3 N6 O21 Tb'
_chemical_formula_weight         1021.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0076 0.0040
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1697 0.1896
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Tb Tb -0.1250 4.8273
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.469(3)
_cell_length_b                   14.456(2)
_cell_length_c                   14.717(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.331(2)
_cell_angle_gamma                90
_cell_volume                     4074.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    9921
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      36.58

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             2072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.515
_shelx_estimated_absorpt_T_min   0.704
_shelx_estimated_absorpt_T_max   0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_process_details   'SADABS 2014/5 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      270(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            27393
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.924
_diffrn_reflns_theta_max         36.670
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7761
_reflns_number_gt                6609
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 Once solved by SHELXT the model for the Eu version of the compound was
 used for the refinement, with Eu changed for Tb, to keep the numdering
 identical.
 All non-hydrogen atoms were refined anisotropically. Hydrogen atoms
 were placed geometrically on the carbon atoms, constrained and refined
 using a riding model. Geometrically and displacement parameter
 restraints were under to model the disordered perchlorate. Some of
 the perchlorate oxygen atoms still have displacement parameter ratios 
 that are larger than ideal. These were left as they were as it best
 reflects the nature of the perchlorates. Data was collected at 270K 
 as the compound undergo a phase transition at low temperature.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+1.2597P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7761
_refine_ls_number_parameters     306
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0890
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.148
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.5000 0.69029(2) 0.2500 0.03468(5) Uani 1 2 d S T P . .
O1 O 0.50304(9) 0.56185(12) 0.15164(14) 0.0491(4) Uani 1 1 d . . . . .
C1 C 0.45444(12) 0.50667(17) 0.12403(17) 0.0420(4) Uani 1 1 d . . . . .
C2 C 0.38137(12) 0.53069(18) 0.13644(18) 0.0474(5) Uani 1 1 d . . . . .
H2A H 0.3523 0.5445 0.0773 0.057 Uiso 1 1 calc R U . . .
H2B H 0.3607 0.4795 0.1646 0.057 Uiso 1 1 calc R U . . .
O2 O 0.38740(8) 0.60926(12) 0.19455(12) 0.0455(4) Uani 1 1 d . . . . .
C3 C 0.32301(11) 0.6410(2) 0.2147(2) 0.0496(6) Uani 1 1 d . . . . .
H3A H 0.2969 0.5899 0.2345 0.060 Uiso 1 1 calc R U . . .
H3B H 0.2952 0.6691 0.1605 0.060 Uiso 1 1 calc R U . . .
C4 C 0.34060(12) 0.71138(17) 0.29128(17) 0.0420(4) Uani 1 1 d . . . . .
O3 O 0.40237(8) 0.73697(12) 0.31498(12) 0.0450(4) Uani 1 1 d . . . . .
N1 N 0.46543(12) 0.42678(14) 0.08508(15) 0.0479(4) Uani 1 1 d . . . . .
C5 C 0.53707(16) 0.3970(2) 0.0821(2) 0.0588(7) Uani 1 1 d . . . . .
H5A H 0.5672 0.4500 0.0874 0.088 Uiso 1 1 calc R U . . .
H5B H 0.5381 0.3661 0.0246 0.088 Uiso 1 1 calc R U . . .
H5C H 0.5527 0.3553 0.1323 0.088 Uiso 1 1 calc R U . . .
C6 C 0.4096(2) 0.3628(2) 0.0468(3) 0.0685(9) Uani 1 1 d . . . . .
H6A H 0.4160 0.3053 0.0799 0.103 Uiso 1 1 calc R U . . .
H6B H 0.4108 0.3521 -0.0172 0.103 Uiso 1 1 calc R U . . .
H6C H 0.3653 0.3890 0.0527 0.103 Uiso 1 1 calc R U . . .
N2 N 0.28956(11) 0.74368(17) 0.33038(17) 0.0524(5) Uani 1 1 d . . . . .
C7 C 0.3046(2) 0.8176(2) 0.3986(3) 0.0664(9) Uani 1 1 d . . . . .
H7A H 0.3518 0.8384 0.4015 0.100 Uiso 1 1 calc R U . . .
H7B H 0.2988 0.7949 0.4580 0.100 Uiso 1 1 calc R U . . .
H7C H 0.2732 0.8683 0.3810 0.100 Uiso 1 1 calc R U . . .
C8 C 0.21654(16) 0.7154(3) 0.3042(3) 0.0734(10) Uani 1 1 d . . . . .
H8A H 0.1909 0.7627 0.2668 0.110 Uiso 1 1 calc R U . . .
H8B H 0.1968 0.7064 0.3589 0.110 Uiso 1 1 calc R U . . .
H8C H 0.2140 0.6587 0.2699 0.110 Uiso 1 1 calc R U . . .
O4 O 0.55650(10) 0.76389(14) 0.38625(12) 0.0515(4) Uani 1 1 d . . . . .
C9 C 0.56188(14) 0.8485(2) 0.40106(18) 0.0520(6) Uani 1 1 d . . . . .
C10 C 0.52964(16) 0.91522(18) 0.3268(2) 0.0567(6) Uani 1 1 d . . . . .
H10A H 0.4940 0.9522 0.3479 0.068 Uiso 1 1 calc R U . . .
H10B H 0.5649 0.9564 0.3106 0.068 Uiso 1 1 calc R U . . .
O5 O 0.5000 0.86098(16) 0.2500 0.0465(5) Uani 1 2 d S T P . .
N3 N 0.59642(14) 0.8827(2) 0.47983(17) 0.0709(8) Uani 1 1 d . . . . .
C11 C 0.6355(2) 0.8207(3) 0.5482(3) 0.0910(15) Uani 1 1 d . . . . .
H11A H 0.6414 0.7620 0.5201 0.136 Uiso 1 1 calc R U . . .
H11B H 0.6105 0.8122 0.5981 0.136 Uiso 1 1 calc R U . . .
H11C H 0.6805 0.8471 0.5715 0.136 Uiso 1 1 calc R U . . .
C12 C 0.6038(3) 0.9825(3) 0.4967(3) 0.1068(18) Uani 1 1 d . . . . .
H12A H 0.6463 1.0038 0.4792 0.160 Uiso 1 1 calc R U . . .
H12B H 0.6052 0.9947 0.5611 0.160 Uiso 1 1 calc R U . . .
H12C H 0.5649 1.0143 0.4608 0.160 Uiso 1 1 calc R U . . .
Cl1 Cl 0.24718(4) 0.93152(6) 0.14423(8) 0.0764(2) Uani 1 1 d . . . . .
O11 O 0.19729(19) 0.9236(3) 0.2025(3) 0.1387(16) Uani 1 1 d . . . . .
O12 O 0.3079(2) 0.9585(5) 0.1985(4) 0.206(3) Uani 1 1 d . . . . .
O13 O 0.2578(5) 0.8501(4) 0.1073(6) 0.268(5) Uani 1 1 d . . . . .
O14 O 0.2305(3) 0.9985(4) 0.0789(3) 0.163(2) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 0.17258(10) 0.2500 0.0994(6) Uani 1 2 d DS TU P . .
O21 O 0.5324(8) 0.2628(6) 0.2536(16) 0.090(5) Uani 0.25 1 d D U P A 1
O22 O 0.5533(6) 0.1129(8) 0.2242(10) 0.066(3) Uani 0.25 1 d D U P A 1
O23 O 0.4354(7) 0.1669(14) 0.1911(16) 0.175(8) Uani 0.25 1 d D U P A 1
O24 O 0.4979(12) 0.1449(12) 0.3445(8) 0.125(6) Uani 0.25 1 d D U P A 1
O21' O 0.5000 0.2705(5) 0.2500 0.132(7) Uani 0.5 2 d DS TU P A 2
O22' O 0.5668(5) 0.1311(9) 0.2597(13) 0.084(4) Uani 0.25 1 d D U P A 2
O23' O 0.4678(9) 0.1477(9) 0.1529(7) 0.103(5) Uani 0.25 1 d D U P B 2
O24' O 0.4553(10) 0.1324(12) 0.3051(14) 0.135(8) Uani 0.25 1 d D U P A 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
Tb1 O4 2.3605(17) . ?
Tb1 O4 2.3605(17) 2_655 ?
Tb1 O1 2.3615(17) . ?
Tb1 O1 2.3615(17) 2_655 ?
Tb1 O3 2.3737(16) 2_655 ?
Tb1 O3 2.3737(16) . ?
Tb1 O5 2.468(2) . ?
Tb1 O2 2.4903(15) 2_655 ?
Tb1 O2 2.4904(15) . ?
O1 C1 1.249(3) . ?
C1 N1 1.324(3) . ?
C1 C2 1.507(3) . ?
C2 O2 1.414(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O2 C3 1.415(3) . ?
C3 C4 1.512(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 O3 1.247(3) . ?
C4 N2 1.320(3) . ?
N1 C6 1.460(4) . ?
N1 C5 1.468(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N2 C7 1.459(4) . ?
N2 C8 1.463(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O4 C9 1.244(4) . ?
C9 N3 1.327(3) . ?
C9 C10 1.507(4) . ?
C10 O5 1.411(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O5 C10 1.411(3) 2_655 ?
N3 C11 1.456(5) . ?
N3 C12 1.467(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
Cl1 O13 1.328(5) . ?
Cl1 O12 1.360(5) . ?
Cl1 O14 1.362(4) . ?
Cl1 O11 1.411(4) . ?
Cl2 O23 1.397(7) 2_655 ?
Cl2 O23 1.397(7) . ?
Cl2 O21' 1.415(7) . ?
Cl2 O22' 1.416(7) 2_655 ?
Cl2 O22' 1.416(7) . ?
Cl2 O24' 1.417(7) . ?
Cl2 O24' 1.417(7) 2_655 ?
Cl2 O21 1.445(7) . ?
Cl2 O21 1.445(7) 2_655 ?
Cl2 O22 1.452(7) . ?
Cl2 O22 1.452(7) 2_655 ?
Cl2 O24 1.455(7) . ?
O21 O21 1.25(3) 2_655 ?
O21 O23 1.67(3) 2_655 ?
O22 O24 1.37(2) 2_655 ?
O22 O23 1.45(2) 2_655 ?
O23 O22 1.45(2) 2_655 ?
O23 O24 1.519(19) 2_655 ?
O23 O21 1.67(3) 2_655 ?
O24 O22 1.37(2) 2_655 ?
O24 O23 1.519(19) 2_655 ?
O22' O24' 0.97(2) 2_655 ?
O22' O23' 1.573(18) 2_655 ?
O23' O24' 1.53(2) 2_655 ?
O23' O22' 1.573(18) 2_655 ?
O24' O22' 0.97(2) 2_655 ?
O24' O23' 1.53(2) 2_655 ?

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
O4 Tb1 O4 126.41(10) . 2_655 ?
O4 Tb1 O1 144.69(7) . . ?
O4 Tb1 O1 83.84(7) 2_655 . ?
O4 Tb1 O1 83.84(7) . 2_655 ?
O4 Tb1 O1 144.69(7) 2_655 2_655 ?
O1 Tb1 O1 76.33(10) . 2_655 ?
O4 Tb1 O3 85.95(6) . 2_655 ?
O4 Tb1 O3 79.30(6) 2_655 2_655 ?
O1 Tb1 O3 82.34(6) . 2_655 ?
O1 Tb1 O3 125.48(6) 2_655 2_655 ?
O4 Tb1 O3 79.30(6) . . ?
O4 Tb1 O3 85.95(6) 2_655 . ?
O1 Tb1 O3 125.48(6) . . ?
O1 Tb1 O3 82.34(6) 2_655 . ?
O3 Tb1 O3 146.97(9) 2_655 . ?
O4 Tb1 O5 63.21(5) . . ?
O4 Tb1 O5 63.21(5) 2_655 . ?
O1 Tb1 O5 141.83(5) . . ?
O1 Tb1 O5 141.83(5) 2_655 . ?
O3 Tb1 O5 73.48(4) 2_655 . ?
O3 Tb1 O5 73.48(4) . . ?
O4 Tb1 O2 71.63(7) . 2_655 ?
O4 Tb1 O2 137.66(6) 2_655 2_655 ?
O1 Tb1 O2 73.37(6) . 2_655 ?
O1 Tb1 O2 63.04(5) 2_655 2_655 ?
O3 Tb1 O2 62.90(5) 2_655 2_655 ?
O3 Tb1 O2 136.31(6) . 2_655 ?
O5 Tb1 O2 118.06(4) . 2_655 ?
O4 Tb1 O2 137.65(6) . . ?
O4 Tb1 O2 71.64(7) 2_655 . ?
O1 Tb1 O2 63.05(5) . . ?
O1 Tb1 O2 73.36(6) 2_655 . ?
O3 Tb1 O2 136.31(6) 2_655 . ?
O3 Tb1 O2 62.89(5) . . ?
O5 Tb1 O2 118.06(4) . . ?
O2 Tb1 O2 123.89(8) 2_655 . ?
C1 O1 Tb1 126.94(15) . . ?
O1 C1 N1 121.8(2) . . ?
O1 C1 C2 119.3(2) . . ?
N1 C1 C2 118.9(2) . . ?
O2 C2 C1 106.29(18) . . ?
O2 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
O2 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C2 O2 C3 113.96(17) . . ?
C2 O2 Tb1 123.28(12) . . ?
C3 O2 Tb1 122.68(13) . . ?
O2 C3 C4 106.47(18) . . ?
O2 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
O2 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
O3 C4 N2 122.5(2) . . ?
O3 C4 C3 119.1(2) . . ?
N2 C4 C3 118.4(2) . . ?
C4 O3 Tb1 127.22(15) . . ?
C1 N1 C6 123.5(2) . . ?
C1 N1 C5 119.8(2) . . ?
C6 N1 C5 116.6(2) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 N2 C7 119.0(2) . . ?
C4 N2 C8 124.0(2) . . ?
C7 N2 C8 116.8(2) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 O4 Tb1 127.15(17) . . ?
O4 C9 N3 122.2(3) . . ?
O4 C9 C10 119.4(2) . . ?
N3 C9 C10 118.4(3) . . ?
O5 C10 C9 106.4(2) . . ?
O5 C10 H10A 110.4 . . ?
C9 C10 H10A 110.4 . . ?
O5 C10 H10B 110.4 . . ?
C9 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
C10 O5 C10 112.5(3) . 2_655 ?
C10 O5 Tb1 123.75(14) . . ?
C10 O5 Tb1 123.75(14) 2_655 . ?
C9 N3 C11 119.7(3) . . ?
C9 N3 C12 122.2(4) . . ?
C11 N3 C12 117.7(3) . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 Cl1 O12 108.2(5) . . ?
O13 Cl1 O14 112.0(5) . . ?
O12 Cl1 O14 106.4(3) . . ?
O13 Cl1 O11 110.6(3) . . ?
O12 Cl1 O11 106.7(4) . . ?
O14 Cl1 O11 112.6(3) . . ?
O23 Cl2 O23 173.3(16) 2_655 . ?
O21' Cl2 O22' 115.1(6) . 2_655 ?
O21' Cl2 O22' 115.1(6) . . ?
O22' Cl2 O22' 129.9(12) 2_655 . ?
O21' Cl2 O24' 114.2(8) . . ?
O22' Cl2 O24' 40.2(8) 2_655 . ?
O22' Cl2 O24' 114.6(8) . . ?
O21' Cl2 O24' 114.2(8) . 2_655 ?
O22' Cl2 O24' 114.6(8) 2_655 2_655 ?
O22' Cl2 O24' 40.2(8) . 2_655 ?
O24' Cl2 O24' 131.6(15) . 2_655 ?
O23 Cl2 O21 72.0(13) 2_655 . ?
O23 Cl2 O21 114.5(8) . . ?
O23 Cl2 O21 114.5(8) 2_655 2_655 ?
O23 Cl2 O21 72.0(13) . 2_655 ?
O21 Cl2 O21 51.1(13) . 2_655 ?
O23 Cl2 O22 61.4(10) 2_655 . ?
O23 Cl2 O22 114.2(9) . . ?
O21 Cl2 O22 102.6(7) . . ?
O21 Cl2 O22 148.7(10) 2_655 . ?
O23 Cl2 O22 114.2(9) 2_655 2_655 ?
O23 Cl2 O22 61.4(10) . 2_655 ?
O21 Cl2 O22 148.7(10) . 2_655 ?
O21 Cl2 O22 102.6(7) 2_655 2_655 ?
O22 Cl2 O22 107.0(10) . 2_655 ?
O23 Cl2 O24 64.3(9) 2_655 . ?
O23 Cl2 O24 113.6(8) . . ?
O21 Cl2 O24 107.4(8) . . ?
O21 Cl2 O24 101.3(12) 2_655 . ?
O22 Cl2 O24 103.3(7) . . ?
O22 Cl2 O24 56.1(9) 2_655 . ?
O21 O21 Cl2 64.5(7) 2_655 . ?
O21 O21 O23 109.1(12) 2_655 2_655 ?
Cl2 O21 O23 52.7(6) . 2_655 ?
O24 O22 Cl2 62.0(5) 2_655 . ?
O24 O22 O23 115.5(8) 2_655 2_655 ?
Cl2 O22 O23 57.4(5) . 2_655 ?
Cl2 O23 O22 61.2(6) . 2_655 ?
Cl2 O23 O24 59.7(5) . 2_655 ?
O22 O23 O24 100.1(12) 2_655 2_655 ?
Cl2 O23 O21 55.3(8) . 2_655 ?
O22 O23 O21 92.4(11) 2_655 2_655 ?
O24 O23 O21 94.1(10) 2_655 2_655 ?
O22 O24 Cl2 61.8(6) 2_655 . ?
O22 O24 O23 111.8(11) 2_655 2_655 ?
Cl2 O24 O23 56.0(5) . 2_655 ?
O24' O22' Cl2 70.0(7) 2_655 . ?
O24' O22' O23' 128.3(11) 2_655 2_655 ?
Cl2 O22' O23' 59.9(5) . 2_655 ?
Cl2 O23' O24' 55.8(5) . 2_655 ?
Cl2 O23' O22' 54.8(4) . 2_655 ?
O24' O23' O22' 100.3(9) 2_655 2_655 ?
O22' O24' Cl2 69.8(7) 2_655 . ?
O22' O24' O23' 128.7(12) 2_655 2_655 ?
Cl2 O24' O23' 60.9(5) . 2_655 ?

_refine_diff_density_max         0.771
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.082

