# 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_c:\doktor~1.201\lnee07~1\2je_16~1\scxrd\sad
_database_code_depnum_ccdc_archive 'CCDC 1023837'
_audit_update_record             
;
2014-09-11 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'polycatena-[tri-chlorido-(μ-4-[(E)-2-(4-pyridinyl)ethanyl]pyridine) -1\kN1:1\kN2-bis(pyridine)-gadolinium(III)]0.5([(E)-2-(4-pyridinyl)ethanyl]pyridine) 0.5(pyridine)'
_chemical_name_common            
;
1[GdCl3(dpa)(py)2]0.5(dpa)0.5(py)
;
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C22 H22 Cl3 Gd N4, 0.5(C12 H12 N2), 0.5(C6 H6)
;
_chemical_formula_sum            'C31 H31 Cl3 Gd N5'
_chemical_formula_weight         737.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3394(10)
_cell_length_b                   12.9250(14)
_cell_length_c                   14.0640(16)
_cell_angle_alpha                103.440(2)
_cell_angle_beta                 102.030(3)
_cell_angle_gamma                101.850(2)
_cell_volume                     1556.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    168(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      1.43
_cell_measurement_theta_max      27.09

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             734
_exptl_absorpt_coefficient_mu    2.417
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_T_max  0.7941
_exptl_absorpt_process_details   'Bruker SADABS (2011)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      168(2)
_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 SMART Apex diffractometer'
_diffrn_measurement_method       'omega und phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19153
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.09
_reflns_number_total             6810
_reflns_number_gt                6339
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART Apex Software (2001)'
_computing_cell_refinement       'Bruker SMART Apex Software (2001)'
_computing_data_reduction        'Bruker SMART Apex Software (2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'POVRAY (2001)'
_computing_publication_material  'X-SEED (2008)'

_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. 
;
_vrf_PLAT331_c__doktor~1.201_lnee07~1_2je_16~1_scxrd_sad 
;
PROBLEM: Small Average Phenyl   C-C Dist. C29    -C31_d         1.35 Ang. 
RESPONSE: Pyridine is disordered
;
_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)+(0.0246P)²+1.4067P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         6810
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.208
_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
Gd1 Gd 1.01227(2) 0.292892(15) 0.232671(13) 0.01930(6) Uani 1 1 d . . .
Cl1 Cl 0.92197(12) 0.47225(8) 0.28834(8) 0.0334(2) Uani 1 1 d . . .
Cl2 Cl 1.06694(11) 0.09725(8) 0.18145(7) 0.0286(2) Uani 1 1 d . . .
Cl3 Cl 1.24879(11) 0.40720(8) 0.18579(8) 0.0312(2) Uani 1 1 d . . .
N1 N 0.9316(4) 0.2272(3) 0.3791(2) 0.0271(7) Uani 1 1 d . . .
N2 N 0.9098(4) 0.2741(3) 1.0455(2) 0.0250(7) Uani 1 1 d . . .
C1 C 0.8562(4) 0.2866(3) 0.4315(3) 0.0291(9) Uani 1 1 d . . .
H1 H 0.8020 0.3294 0.3994 0.035 Uiso 1 1 calc R . .
C2 C 0.8533(4) 0.2887(3) 0.5295(3) 0.0275(8) Uani 1 1 d . . .
H2 H 0.7997 0.3332 0.5636 0.033 Uiso 1 1 calc R . .
C3 C 0.9285(4) 0.2259(3) 0.5782(3) 0.0260(8) Uani 1 1 d . . .
C4 C 1.0007(5) 0.1597(3) 0.5226(3) 0.0320(9) Uani 1 1 d . . .
H4 H 1.0506 0.1129 0.5518 0.038 Uiso 1 1 calc R . .
C5 C 0.9992(5) 0.1624(3) 0.4245(3) 0.0323(9) Uani 1 1 d . . .
H5 H 1.0483 0.1162 0.3876 0.039 Uiso 1 1 calc R . .
C6 C 0.9392(5) 0.2313(4) 0.6876(3) 0.0321(9) Uani 1 1 d . . .
H6B H 1.0351 0.2861 0.7299 0.039 Uiso 1 1 calc R . .
H6A H 0.9461 0.1586 0.6966 0.039 Uiso 1 1 calc R . .
C7 C 0.8100(5) 0.2610(4) 0.7281(3) 0.0309(9) Uani 1 1 d . . .
H7B H 0.8019 0.3340 0.7207 0.037 Uiso 1 1 calc R . .
H7A H 0.7132 0.2058 0.6880 0.037 Uiso 1 1 calc R . .
C8 C 0.8360(4) 0.2642(3) 0.8386(3) 0.0265(8) Uani 1 1 d . . .
C9 C 0.8520(5) 0.3597(3) 0.9131(3) 0.0310(9) Uani 1 1 d . . .
H9 H 0.8379 0.4240 0.8950 0.037 Uiso 1 1 calc R . .
C10 C 0.8887(5) 0.3617(3) 1.0145(3) 0.0306(9) Uani 1 1 d . . .
H10 H 0.8994 0.4285 1.0645 0.037 Uiso 1 1 calc R . .
C11 C 0.8909(5) 0.1805(3) 0.9730(3) 0.0278(8) Uani 1 1 d . . .
H11 H 0.9040 0.1170 0.9930 0.033 Uiso 1 1 calc R . .
C12 C 0.8529(5) 0.1721(3) 0.8702(3) 0.0294(9) Uani 1 1 d . . .
H12 H 0.8386 0.1035 0.8215 0.035 Uiso 1 1 calc R . .
N3 N 1.2323(4) 0.3522(3) 0.3950(2) 0.0285(7) Uani 1 1 d . . .
C13 C 1.2349(5) 0.4185(3) 0.4846(3) 0.0322(9) Uani 1 1 d . . .
H13 H 1.1538 0.4518 0.4882 0.039 Uiso 1 1 calc R . .
C14 C 1.3506(5) 0.4406(4) 0.5719(3) 0.0382(10) Uani 1 1 d . . .
H14 H 1.3481 0.4879 0.6340 0.046 Uiso 1 1 calc R . .
C15 C 1.4696(5) 0.3931(4) 0.5677(3) 0.0396(11) Uani 1 1 d . . .
H15 H 1.5513 0.4078 0.6262 0.047 Uiso 1 1 calc R . .
C16 C 1.4663(5) 0.3240(4) 0.4762(3) 0.0389(10) Uani 1 1 d . . .
H16 H 1.5449 0.2882 0.4711 0.047 Uiso 1 1 calc R . .
C17 C 1.3484(5) 0.3068(4) 0.3919(3) 0.0324(9) Uani 1 1 d . . .
H17 H 1.3496 0.2607 0.3288 0.039 Uiso 1 1 calc R . .
N4 N 0.7258(4) 0.1934(3) 0.1761(2) 0.0264(7) Uani 1 1 d . . .
C18 C 0.6182(5) 0.2454(4) 0.1547(3) 0.0375(10) Uani 1 1 d . . .
H18 H 0.6495 0.3213 0.1582 0.045 Uiso 1 1 calc R . .
C19 C 0.4650(5) 0.1951(4) 0.1280(4) 0.0414(11) Uani 1 1 d . . .
H19 H 0.3930 0.2357 0.1145 0.050 Uiso 1 1 calc R . .
C20 C 0.4181(5) 0.0854(4) 0.1212(4) 0.0440(12) Uani 1 1 d . . .
H20 H 0.3130 0.0484 0.1025 0.053 Uiso 1 1 calc R . .
C21 C 0.5264(5) 0.0298(4) 0.1420(4) 0.0459(12) Uani 1 1 d . . .
H21 H 0.4973 -0.0466 0.1369 0.055 Uiso 1 1 calc R . .
C22 C 0.6775(5) 0.0867(3) 0.1702(3) 0.0339(10) Uani 1 1 d . . .
H22 H 0.7512 0.0482 0.1863 0.041 Uiso 1 1 calc R . .
N5 N 0.7136(4) 0.8476(3) 0.2323(3) 0.0395(9) Uani 1 1 d . . .
C23 C 0.7618(5) 0.8194(4) 0.1493(4) 0.0382(10) Uani 1 1 d . . .
H23 H 0.8266 0.8759 0.1333 0.046 Uiso 1 1 calc R . .
C24 C 0.7233(5) 0.7133(4) 0.0854(3) 0.0363(10) Uani 1 1 d . . .
H24 H 0.7621 0.6984 0.0278 0.044 Uiso 1 1 calc R . .
C25 C 0.6283(5) 0.6288(3) 0.1054(3) 0.0321(9) Uani 1 1 d . . .
C26 C 0.5778(6) 0.6569(4) 0.1914(4) 0.0433(11) Uani 1 1 d . . .
H26 H 0.5124 0.6022 0.2091 0.052 Uiso 1 1 calc R . .
C27 C 0.6234(6) 0.7654(4) 0.2512(4) 0.0458(12) Uani 1 1 d . . .
H27 H 0.5879 0.7824 0.3100 0.055 Uiso 1 1 calc R . .
C28 C 0.5783(5) 0.5128(4) 0.0365(4) 0.0401(11) Uani 1 1 d . . .
H28A H 0.5762 0.4606 0.0781 0.048 Uiso 1 1 calc R . .
H28B H 0.6529 0.5018 -0.0030 0.048 Uiso 1 1 calc R . .
C29 C 0.3640(11) 0.0296(6) 0.4834(8) 0.096(3) Uani 1 1 d . . .
H29 H 0.2706 0.0492 0.4709 0.115 Uiso 1 1 calc R . .
C30 C 0.4148(13) 0.0001(6) 0.5656(8) 0.110(4) Uani 1 1 d . . .
H30 H 0.3577 0.0001 0.6142 0.132 Uiso 1 1 calc R . .
C31 C 0.5481(14) -0.0305(5) 0.5819(6) 0.105(3) Uani 1 1 d . . .
H31 H 0.5796 -0.0530 0.6408 0.126 Uiso 1 1 calc R . .


_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
Gd1 N2 2.542(3) 1_554 ?
Gd1 N3 2.570(3) . ?
Gd1 N4 2.582(3) . ?
Gd1 N1 2.594(3) . ?
Gd1 Cl1 2.6330(10) . ?
Gd1 Cl2 2.6477(10) . ?
Gd1 Cl3 2.6864(10) . ?
N1 C1 1.343(5) . ?
N1 C5 1.345(5) . ?
N2 C11 1.340(5) . ?
N2 C10 1.340(5) . ?
N2 Gd1 2.542(3) 1_556 ?
C1 C2 1.378(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.383(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(6) . ?
C3 C6 1.505(5) . ?
C4 C5 1.385(5) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.518(6) . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C7 C8 1.511(5) . ?
C7 H7B 0.9900 . ?
C7 H7A 0.9900 . ?
C8 C9 1.378(6) . ?
C8 C12 1.391(5) . ?
C9 C10 1.389(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.387(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C17 1.339(5) . ?
N3 C13 1.341(5) . ?
C13 C14 1.383(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(6) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N4 C22 1.337(5) . ?
N4 C18 1.341(5) . ?
C18 C19 1.375(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.369(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.376(6) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
N5 C27 1.329(6) . ?
N5 C23 1.337(6) . ?
C23 C24 1.381(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(6) . ?
C25 C28 1.502(6) . ?
C26 C27 1.383(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C28 1.523(9) 2_665 ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.326(13) . ?
C29 C31 1.354(11) 2_656 ?
C29 H29 0.9500 . ?
C30 C31 1.373(13) . ?
C30 H30 0.9500 . ?
C31 C29 1.354(11) 2_656 ?
C31 H31 0.9500 . ?

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
N2 Gd1 N3 151.27(10) 1_554 . ?
N2 Gd1 N4 71.13(10) 1_554 . ?
N3 Gd1 N4 137.55(10) . . ?
N2 Gd1 N1 140.73(10) 1_554 . ?
N3 Gd1 N1 67.59(10) . . ?
N4 Gd1 N1 70.05(10) . . ?
N2 Gd1 Cl1 92.13(8) 1_554 . ?
N3 Gd1 Cl1 92.70(8) . . ?
N4 Gd1 Cl1 84.41(8) . . ?
N1 Gd1 Cl1 89.82(8) . . ?
N2 Gd1 Cl2 89.14(8) 1_554 . ?
N3 Gd1 Cl2 90.09(8) . . ?
N4 Gd1 Cl2 88.29(8) . . ?
N1 Gd1 Cl2 84.05(8) . . ?
Cl1 Gd1 Cl2 171.74(3) . . ?
N2 Gd1 Cl3 76.36(7) 1_554 . ?
N3 Gd1 Cl3 75.25(8) . . ?
N4 Gd1 Cl3 146.95(7) . . ?
N1 Gd1 Cl3 142.83(8) . . ?
Cl1 Gd1 Cl3 91.13(3) . . ?
Cl2 Gd1 Cl3 97.10(3) . . ?
C1 N1 C5 116.7(3) . . ?
C1 N1 Gd1 117.1(3) . . ?
C5 N1 Gd1 122.8(3) . . ?
C11 N2 C10 116.8(3) . . ?
C11 N2 Gd1 122.0(3) . 1_556 ?
C10 N2 Gd1 120.8(3) . 1_556 ?
N1 C1 C2 123.4(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 117.0(4) . . ?
C2 C3 C6 122.4(4) . . ?
C4 C3 C6 120.6(4) . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
N1 C5 C4 123.1(4) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C3 C6 C7 116.6(3) . . ?
C3 C6 H6B 108.2 . . ?
C7 C6 H6B 108.2 . . ?
C3 C6 H6A 108.2 . . ?
C7 C6 H6A 108.2 . . ?
H6B C6 H6A 107.3 . . ?
C8 C7 C6 110.9(3) . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
H7B C7 H7A 108.0 . . ?
C9 C8 C12 117.0(4) . . ?
C9 C8 C7 121.7(4) . . ?
C12 C8 C7 121.2(4) . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 123.2(4) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C12 123.1(4) . . ?
N2 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C8 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C8 C12 H12 120.1 . . ?
C17 N3 C13 117.3(3) . . ?
C17 N3 Gd1 117.3(3) . . ?
C13 N3 Gd1 125.2(3) . . ?
N3 C13 C14 123.0(4) . . ?
N3 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C15 C14 C13 119.1(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 118.1(4) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 119.6(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
N3 C17 C16 122.8(4) . . ?
N3 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
C22 N4 C18 116.5(4) . . ?
C22 N4 Gd1 120.8(3) . . ?
C18 N4 Gd1 122.6(3) . . ?
N4 C18 C19 123.6(4) . . ?
N4 C18 H18 118.2 . . ?
C19 C18 H18 118.2 . . ?
C20 C19 C18 118.9(4) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 118.6(4) . . ?
C19 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
C22 C21 C20 118.9(4) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
N4 C22 C21 123.4(4) . . ?
N4 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
C27 N5 C23 115.4(4) . . ?
N5 C23 C24 124.2(4) . . ?
N5 C23 H23 117.9 . . ?
C24 C23 H23 117.9 . . ?
C25 C24 C23 119.8(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 116.6(4) . . ?
C24 C25 C28 122.1(4) . . ?
C26 C25 C28 121.3(4) . . ?
C27 C26 C25 119.3(4) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
N5 C27 C26 124.6(4) . . ?
N5 C27 H27 117.7 . . ?
C26 C27 H27 117.7 . . ?
C25 C28 C28 112.3(5) . 2_665 ?
C25 C28 H28A 109.2 . . ?
C28 C28 H28A 109.2 2_665 . ?
C25 C28 H28B 109.2 . . ?
C28 C28 H28B 109.2 2_665 . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C31 116.6(10) . 2_656 ?
C30 C29 H29 121.7 . . ?
C31 C29 H29 121.7 2_656 . ?
C29 C30 C31 121.4(9) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
C29 C31 C30 122.0(9) 2_656 . ?
C29 C31 H31 119.0 2_656 . ?
C30 C31 H31 119.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Gd1 N1 C1 -85.8(3) 1_554 . . . ?
N3 Gd1 N1 C1 100.3(3) . . . . ?
N4 Gd1 N1 C1 -76.8(3) . . . . ?
Cl1 Gd1 N1 C1 7.3(3) . . . . ?
Cl2 Gd1 N1 C1 -167.1(3) . . . . ?
Cl3 Gd1 N1 C1 99.0(3) . . . . ?
N2 Gd1 N1 C5 115.6(3) 1_554 . . . ?
N3 Gd1 N1 C5 -58.3(3) . . . . ?
N4 Gd1 N1 C5 124.6(3) . . . . ?
Cl1 Gd1 N1 C5 -151.3(3) . . . . ?
Cl2 Gd1 N1 C5 34.3(3) . . . . ?
Cl3 Gd1 N1 C5 -59.6(4) . . . . ?
C5 N1 C1 C2 4.0(6) . . . . ?
Gd1 N1 C1 C2 -155.9(3) . . . . ?
N1 C1 C2 C3 -1.2(6) . . . . ?
C1 C2 C3 C4 -2.1(6) . . . . ?
C1 C2 C3 C6 175.3(4) . . . . ?
C2 C3 C4 C5 2.4(6) . . . . ?
C6 C3 C4 C5 -175.1(4) . . . . ?
C1 N1 C5 C4 -3.6(6) . . . . ?
Gd1 N1 C5 C4 155.1(3) . . . . ?
C3 C4 C5 N1 0.5(7) . . . . ?
C2 C3 C6 C7 28.7(6) . . . . ?
C4 C3 C6 C7 -154.1(4) . . . . ?
C3 C6 C7 C8 -179.6(3) . . . . ?
C6 C7 C8 C9 118.0(4) . . . . ?
C6 C7 C8 C12 -58.5(5) . . . . ?
C12 C8 C9 C10 2.2(6) . . . . ?
C7 C8 C9 C10 -174.5(4) . . . . ?
C11 N2 C10 C9 -1.3(6) . . . . ?
Gd1 N2 C10 C9 171.4(3) 1_556 . . . ?
C8 C9 C10 N2 -0.2(6) . . . . ?
C10 N2 C11 C12 0.7(6) . . . . ?
Gd1 N2 C11 C12 -171.9(3) 1_556 . . . ?
N2 C11 C12 C8 1.3(6) . . . . ?
C9 C8 C12 C11 -2.8(6) . . . . ?
C7 C8 C12 C11 173.9(4) . . . . ?
N2 Gd1 N3 C17 -58.8(4) 1_554 . . . ?
N4 Gd1 N3 C17 117.1(3) . . . . ?
N1 Gd1 N3 C17 113.1(3) . . . . ?
Cl1 Gd1 N3 C17 -158.2(3) . . . . ?
Cl2 Gd1 N3 C17 29.6(3) . . . . ?
Cl3 Gd1 N3 C17 -67.7(3) . . . . ?
N2 Gd1 N3 C13 126.4(3) 1_554 . . . ?
N4 Gd1 N3 C13 -57.7(4) . . . . ?
N1 Gd1 N3 C13 -61.7(3) . . . . ?
Cl1 Gd1 N3 C13 27.0(3) . . . . ?
Cl2 Gd1 N3 C13 -145.2(3) . . . . ?
Cl3 Gd1 N3 C13 117.4(3) . . . . ?
C17 N3 C13 C14 -0.4(6) . . . . ?
Gd1 N3 C13 C14 174.5(3) . . . . ?
N3 C13 C14 C15 0.3(7) . . . . ?
C13 C14 C15 C16 -1.0(7) . . . . ?
C14 C15 C16 C17 1.9(7) . . . . ?
C13 N3 C17 C16 1.3(6) . . . . ?
Gd1 N3 C17 C16 -174.0(3) . . . . ?
C15 C16 C17 N3 -2.1(7) . . . . ?
N2 Gd1 N4 C22 110.9(3) 1_554 . . . ?
N3 Gd1 N4 C22 -67.1(4) . . . . ?
N1 Gd1 N4 C22 -63.1(3) . . . . ?
Cl1 Gd1 N4 C22 -154.9(3) . . . . ?
Cl2 Gd1 N4 C22 21.2(3) . . . . ?
Cl3 Gd1 N4 C22 121.6(3) . . . . ?
N2 Gd1 N4 C18 -71.6(3) 1_554 . . . ?
N3 Gd1 N4 C18 110.5(3) . . . . ?
N1 Gd1 N4 C18 114.5(3) . . . . ?
Cl1 Gd1 N4 C18 22.6(3) . . . . ?
Cl2 Gd1 N4 C18 -161.2(3) . . . . ?
Cl3 Gd1 N4 C18 -60.8(4) . . . . ?
C22 N4 C18 C19 0.1(7) . . . . ?
Gd1 N4 C18 C19 -177.6(4) . . . . ?
N4 C18 C19 C20 -0.9(7) . . . . ?
C18 C19 C20 C21 0.4(8) . . . . ?
C19 C20 C21 C22 0.9(8) . . . . ?
C18 N4 C22 C21 1.3(7) . . . . ?
Gd1 N4 C22 C21 179.0(4) . . . . ?
C20 C21 C22 N4 -1.8(8) . . . . ?
C27 N5 C23 C24 0.1(7) . . . . ?
N5 C23 C24 C25 0.6(7) . . . . ?
C23 C24 C25 C26 -0.7(6) . . . . ?
C23 C24 C25 C28 177.7(4) . . . . ?
C24 C25 C26 C27 0.2(7) . . . . ?
C28 C25 C26 C27 -178.2(4) . . . . ?
C23 N5 C27 C26 -0.6(7) . . . . ?
C25 C26 C27 N5 0.5(8) . . . . ?
C24 C25 C28 C28 -97.5(6) . . . 2_665 ?
C26 C25 C28 C28 80.8(7) . . . 2_665 ?
C31 C29 C30 C31 -1.5(12) 2_656 . . . ?
C29 C30 C31 C29 1.6(13) . . . 2_656 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.313
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.108
####################################################################### 
# 
# 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_e:\doktor~1.201\lncl3_~4\3je_17~1\scxrd\rechnung\sad
_database_code_depnum_ccdc_archive 'CCDC 1023838'
_audit_update_record             
;
2014-09-11 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 polycatena-[tri-chlorido-(μ-4-[1,2-bis(4-pyridyl)
 ethane]pyridine) -1\kN1:1\kN2-bis(pyridine)-
 erbium(III)]0.5([1,2-bis(4-pyridyl)ethane)
 0.5(pyridine)    
;
_chemical_name_common            
;
1[ErCl3(dpa)(py)2]0.5(dpa)0.5(py)
;
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C22 H22 Cl3 Er N4, 0.5(C12 H12 N2), 0.5(C6 H6)
;
_chemical_formula_sum            'C31 H31 Cl3 Er N5'
_chemical_formula_weight         747.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3175(10)
_cell_length_b                   12.8780(14)
_cell_length_c                   13.9710(16)
_cell_angle_alpha                103.280(2)
_cell_angle_beta                 102.030(3)
_cell_angle_gamma                101.880(2)
_cell_volume                     1538.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    168(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      1.69
_cell_measurement_theta_max      27.07

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             742
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_process_details   'Bruker SADABS (2011)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      168(2)
_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 SMART Apex diffractometer'
_diffrn_measurement_method       'omega und phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18949
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         27.07
_reflns_number_total             6716
_reflns_number_gt                6128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART Apex Software (2001)'
_computing_cell_refinement       'Bruker SMART Apex Software (2001)'
_computing_data_reduction        'Bruker SMART Apex Software (2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'POVRAY (2001)'
_computing_publication_material  'X-SEED (2008)'

_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)+(0.0246P)²+1.4067P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         6716
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_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
Er1 Er 1.012673(14) 0.292480(10) 0.233332(9) 0.01884(4) Uani 1 1 d . . .
Cl1 Cl 0.92814(9) 0.47054(6) 0.28939(6) 0.03041(16) Uani 1 1 d . . .
Cl2 Cl 1.06891(8) 0.10085(6) 0.18264(5) 0.02638(15) Uani 1 1 d . . .
Cl3 Cl 1.24539(8) 0.40493(6) 0.18550(6) 0.02910(16) Uani 1 1 d . . .
N1 N 0.9332(3) 0.2277(2) 0.37814(18) 0.0257(5) Uani 1 1 d . . .
N2 N 0.9116(3) 0.2742(2) 1.04873(18) 0.0245(5) Uani 1 1 d . . .
C1 C 0.8563(3) 0.2865(3) 0.4309(2) 0.0283(7) Uani 1 1 d . . .
H1 H 0.8018 0.3292 0.3983 0.034 Uiso 1 1 calc R . .
C2 C 0.8519(3) 0.2884(3) 0.5293(2) 0.0279(6) Uani 1 1 d . . .
H2 H 0.7967 0.3322 0.5630 0.033 Uiso 1 1 calc R . .
C3 C 0.9284(3) 0.2260(3) 0.5787(2) 0.0269(6) Uani 1 1 d . . .
C4 C 1.0020(4) 0.1601(3) 0.5227(2) 0.0317(7) Uani 1 1 d . . .
H4 H 1.0521 0.1133 0.5524 0.038 Uiso 1 1 calc R . .
C5 C 1.0018(4) 0.1630(3) 0.4245(2) 0.0289(7) Uani 1 1 d . . .
H5 H 1.0522 0.1174 0.3880 0.035 Uiso 1 1 calc R . .
C6 C 0.9386(4) 0.2308(3) 0.6884(2) 0.0332(7) Uani 1 1 d . . .
H6B H 1.0347 0.2858 0.7311 0.040 Uiso 1 1 calc R . .
H6A H 0.9456 0.1578 0.6974 0.040 Uiso 1 1 calc R . .
C7 C 0.8078(4) 0.2606(3) 0.7293(2) 0.0322(7) Uani 1 1 d . . .
H7B H 0.7995 0.3338 0.7217 0.039 Uiso 1 1 calc R . .
H7A H 0.7109 0.2051 0.6890 0.039 Uiso 1 1 calc R . .
C8 C 0.8340(3) 0.2636(3) 0.8403(2) 0.0259(6) Uani 1 1 d . . .
C9 C 0.8522(4) 0.3600(3) 0.9155(2) 0.0293(7) Uani 1 1 d . . .
H9 H 0.8388 0.4248 0.8974 0.035 Uiso 1 1 calc R . .
C10 C 0.8899(4) 0.3618(3) 1.0171(2) 0.0291(7) Uani 1 1 d . . .
H10 H 0.9011 0.4289 1.0673 0.035 Uiso 1 1 calc R . .
C11 C 0.8890(3) 0.1797(2) 0.9753(2) 0.0267(6) Uani 1 1 d . . .
H11 H 0.9005 0.1155 0.9953 0.032 Uiso 1 1 calc R . .
C12 C 0.8503(4) 0.1712(3) 0.8725(2) 0.0298(7) Uani 1 1 d . . .
H12 H 0.8347 0.1022 0.8237 0.036 Uiso 1 1 calc R . .
N3 N 1.2301(3) 0.3520(2) 0.39277(18) 0.0254(5) Uani 1 1 d . . .
C13 C 1.2317(4) 0.4188(3) 0.4823(2) 0.0301(7) Uani 1 1 d . . .
H13 H 1.1499 0.4517 0.4854 0.036 Uiso 1 1 calc R . .
C14 C 1.3479(4) 0.4420(3) 0.5710(2) 0.0360(8) Uani 1 1 d . . .
H14 H 1.3456 0.4900 0.6331 0.043 Uiso 1 1 calc R . .
C15 C 1.4662(4) 0.3939(3) 0.5668(3) 0.0379(8) Uani 1 1 d . . .
H15 H 1.5474 0.4085 0.6260 0.046 Uiso 1 1 calc R . .
C16 C 1.4650(4) 0.3244(3) 0.4754(3) 0.0371(8) Uani 1 1 d . . .
H16 H 1.5447 0.2894 0.4710 0.045 Uiso 1 1 calc R . .
C17 C 1.3468(3) 0.3062(3) 0.3905(2) 0.0317(7) Uani 1 1 d . . .
H17 H 1.3479 0.2591 0.3276 0.038 Uiso 1 1 calc R . .
N4 N 0.7308(3) 0.1953(2) 0.17799(18) 0.0241(5) Uani 1 1 d . . .
C18 C 0.6235(4) 0.2475(3) 0.1560(3) 0.0340(7) Uani 1 1 d . . .
H18 H 0.6553 0.3235 0.1593 0.041 Uiso 1 1 calc R . .
C19 C 0.4698(4) 0.1976(3) 0.1290(3) 0.0389(8) Uani 1 1 d . . .
H19 H 0.3981 0.2388 0.1159 0.047 Uiso 1 1 calc R . .
C20 C 0.4222(4) 0.0876(3) 0.1214(3) 0.0420(8) Uani 1 1 d . . .
H20 H 0.3167 0.0508 0.1014 0.050 Uiso 1 1 calc R . .
C21 C 0.5297(4) 0.0306(3) 0.1431(3) 0.0408(8) Uani 1 1 d . . .
H21 H 0.4997 -0.0459 0.1383 0.049 Uiso 1 1 calc R . .
C22 C 0.6823(3) 0.0879(3) 0.1720(3) 0.0314(7) Uani 1 1 d . . .
H22 H 0.7561 0.0491 0.1883 0.038 Uiso 1 1 calc R . .
N5 N 0.7153(3) 0.8480(2) 0.2329(2) 0.0384(7) Uani 1 1 d . . .
C23 C 0.7638(4) 0.8195(3) 0.1492(3) 0.0380(8) Uani 1 1 d . . .
H23 H 0.8288 0.8764 0.1332 0.046 Uiso 1 1 calc R . .
C24 C 0.7262(4) 0.7140(3) 0.0848(3) 0.0353(7) Uani 1 1 d . . .
H24 H 0.7653 0.6992 0.0270 0.042 Uiso 1 1 calc R . .
C25 C 0.6300(4) 0.6292(3) 0.1058(2) 0.0319(7) Uani 1 1 d . . .
C26 C 0.5785(4) 0.6574(3) 0.1919(3) 0.0412(8) Uani 1 1 d . . .
H26 H 0.5118 0.6026 0.2092 0.049 Uiso 1 1 calc R . .
C27 C 0.6249(4) 0.7655(3) 0.2523(3) 0.0434(9) Uani 1 1 d . . .
H27 H 0.5900 0.7823 0.3118 0.052 Uiso 1 1 calc R . .
C28 C 0.5784(4) 0.5123(3) 0.0363(3) 0.0388(8) Uani 1 1 d . . .
H28A H 0.5761 0.4599 0.0783 0.047 Uiso 1 1 calc R . .
H28B H 0.6527 0.5008 -0.0037 0.047 Uiso 1 1 calc R . .
C29 C 0.3637(7) 0.0297(4) 0.4827(5) 0.0840(17) Uani 1 1 d . . .
H29 H 0.2704 0.0497 0.4698 0.101 Uiso 1 1 calc R . .
C30 C 0.4128(9) -0.0009(4) 0.5652(6) 0.099(2) Uani 1 1 d . . .
H30 H 0.3540 -0.0020 0.6131 0.119 Uiso 1 1 calc R . .
C31 C 0.5467(9) -0.0310(4) 0.5829(4) 0.094(2) Uani 1 1 d . . .
H31 H 0.5777 -0.0534 0.6424 0.113 Uiso 1 1 calc R . .


_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
Er1 N2 2.492(2) 1_554 ?
Er1 N3 2.520(2) . ?
Er1 N4 2.533(2) . ?
Er1 N1 2.546(2) . ?
Er1 Cl1 2.5822(7) . ?
Er1 Cl2 2.5981(7) . ?
Er1 Cl3 2.6460(7) . ?
N1 C5 1.347(4) . ?
N1 C1 1.348(4) . ?
N2 C10 1.339(4) . ?
N2 C11 1.346(4) . ?
N2 Er1 2.492(2) 1_556 ?
C1 C2 1.379(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.384(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.399(4) . ?
C3 C6 1.502(4) . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.530(4) . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C7 C8 1.509(4) . ?
C7 H7B 0.9900 . ?
C7 H7A 0.9900 . ?
C8 C9 1.383(4) . ?
C8 C12 1.391(4) . ?
C9 C10 1.383(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.379(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N3 C13 1.341(4) . ?
N3 C17 1.342(4) . ?
C13 C14 1.390(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
N4 C22 1.341(4) . ?
N4 C18 1.338(4) . ?
C18 C19 1.374(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.366(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.386(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
N5 C27 1.331(4) . ?
N5 C23 1.340(4) . ?
C23 C24 1.375(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.392(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(5) . ?
C25 C28 1.508(4) . ?
C26 C27 1.377(5) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C28 1.520(7) 2_665 ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.325(9) . ?
C29 C31 1.363(8) 2_656 ?
C29 H29 0.9500 . ?
C30 C31 1.373(9) . ?
C30 H30 0.9500 . ?
C31 C29 1.363(8) 2_656 ?
C31 H31 0.9500 . ?

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
N2 Er1 N3 150.88(8) 1_554 . ?
N2 Er1 N4 71.09(7) 1_554 . ?
N3 Er1 N4 138.01(7) . . ?
N2 Er1 N1 140.66(8) 1_554 . ?
N3 Er1 N1 68.10(8) . . ?
N4 Er1 N1 70.03(8) . . ?
N2 Er1 Cl1 92.49(6) 1_554 . ?
N3 Er1 Cl1 91.79(6) . . ?
N4 Er1 Cl1 85.04(6) . . ?
N1 Er1 Cl1 89.95(6) . . ?
N2 Er1 Cl2 89.10(6) 1_554 . ?
N3 Er1 Cl2 90.14(6) . . ?
N4 Er1 Cl2 89.01(6) . . ?
N1 Er1 Cl2 84.51(6) . . ?
Cl1 Er1 Cl2 172.98(2) . . ?
N2 Er1 Cl3 76.12(6) 1_554 . ?
N3 Er1 Cl3 75.05(6) . . ?
N4 Er1 Cl3 146.66(5) . . ?
N1 Er1 Cl3 143.14(6) . . ?
Cl1 Er1 Cl3 90.60(3) . . ?
Cl2 Er1 Cl3 96.42(2) . . ?
C5 N1 C1 116.4(2) . . ?
C5 N1 Er1 122.77(19) . . ?
C1 N1 Er1 117.55(19) . . ?
C10 N2 C11 116.4(2) . . ?
C10 N2 Er1 121.07(19) . 1_556 ?
C11 N2 Er1 122.31(19) . 1_556 ?
N1 C1 C2 124.0(3) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C1 C2 C3 119.5(3) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 117.0(3) . . ?
C2 C3 C6 122.4(3) . . ?
C4 C3 C6 120.7(3) . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 123.0(3) . . ?
N1 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C3 C6 C7 116.6(3) . . ?
C3 C6 H6B 108.2 . . ?
C7 C6 H6B 108.2 . . ?
C3 C6 H6A 108.2 . . ?
C7 C6 H6A 108.2 . . ?
H6B C6 H6A 107.3 . . ?
C8 C7 C6 110.8(2) . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
H7B C7 H7A 108.1 . . ?
C9 C8 C12 116.8(3) . . ?
C9 C8 C7 121.7(3) . . ?
C12 C8 C7 121.4(3) . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 123.6(3) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C12 123.3(3) . . ?
N2 C11 H11 118.3 . . ?
C12 C11 H11 118.3 . . ?
C11 C12 C8 120.0(3) . . ?
C11 C12 H12 120.0 . . ?
C8 C12 H12 120.0 . . ?
C13 N3 C17 117.4(3) . . ?
C13 N3 Er1 124.6(2) . . ?
C17 N3 Er1 117.71(19) . . ?
N3 C13 C14 122.9(3) . . ?
N3 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C15 C14 C13 118.6(3) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C16 C15 C14 119.0(3) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 119.2(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
N3 C17 C16 122.9(3) . . ?
N3 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
C22 N4 C18 116.6(3) . . ?
C22 N4 Er1 120.62(19) . . ?
C18 N4 Er1 122.7(2) . . ?
N4 C18 C19 123.9(3) . . ?
N4 C18 H18 118.1 . . ?
C19 C18 H18 118.1 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 119.1(3) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C22 C21 C20 118.4(3) . . ?
C22 C21 H21 120.8 . . ?
C20 C21 H21 120.8 . . ?
N4 C22 C21 123.2(3) . . ?
N4 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
C27 N5 C23 115.5(3) . . ?
N5 C23 C24 124.8(3) . . ?
N5 C23 H23 117.6 . . ?
C24 C23 H23 117.6 . . ?
C25 C24 C23 118.9(3) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 117.0(3) . . ?
C24 C25 C28 121.9(3) . . ?
C26 C25 C28 121.0(3) . . ?
C27 C26 C25 119.5(3) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
N5 C27 C26 124.4(3) . . ?
N5 C27 H27 117.8 . . ?
C26 C27 H27 117.8 . . ?
C25 C28 C28 112.1(3) . 2_665 ?
C25 C28 H28A 109.2 . . ?
C28 C28 H28A 109.2 2_665 . ?
C25 C28 H28B 109.2 . . ?
C28 C28 H28B 109.2 2_665 . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C31 116.9(6) . 2_656 ?
C30 C29 H29 121.6 . . ?
C31 C29 H29 121.6 2_656 . ?
C29 C30 C31 121.4(6) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
C29 C31 C30 121.7(6) 2_656 . ?
C29 C31 H31 119.1 2_656 . ?
C30 C31 H31 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Er1 N1 C5 116.2(2) 1_554 . . . ?
N3 Er1 N1 C5 -58.0(2) . . . . ?
N4 Er1 N1 C5 125.3(2) . . . . ?
Cl1 Er1 N1 C5 -150.0(2) . . . . ?
Cl2 Er1 N1 C5 34.3(2) . . . . ?
Cl3 Er1 N1 C5 -59.1(3) . . . . ?
N2 Er1 N1 C1 -85.2(2) 1_554 . . . ?
N3 Er1 N1 C1 100.6(2) . . . . ?
N4 Er1 N1 C1 -76.1(2) . . . . ?
Cl1 Er1 N1 C1 8.7(2) . . . . ?
Cl2 Er1 N1 C1 -167.0(2) . . . . ?
Cl3 Er1 N1 C1 99.6(2) . . . . ?
C5 N1 C1 C2 3.8(4) . . . . ?
Er1 N1 C1 C2 -156.3(2) . . . . ?
N1 C1 C2 C3 -0.8(5) . . . . ?
C1 C2 C3 C4 -2.5(4) . . . . ?
C1 C2 C3 C6 175.2(3) . . . . ?
C2 C3 C4 C5 2.8(5) . . . . ?
C6 C3 C4 C5 -174.9(3) . . . . ?
C1 N1 C5 C4 -3.4(5) . . . . ?
Er1 N1 C5 C4 155.5(2) . . . . ?
C3 C4 C5 N1 0.2(5) . . . . ?
C2 C3 C6 C7 28.0(5) . . . . ?
C4 C3 C6 C7 -154.4(3) . . . . ?
C3 C6 C7 C8 -179.4(3) . . . . ?
C6 C7 C8 C9 117.0(3) . . . . ?
C6 C7 C8 C12 -59.0(4) . . . . ?
C12 C8 C9 C10 2.2(5) . . . . ?
C7 C8 C9 C10 -174.0(3) . . . . ?
C11 N2 C10 C9 -2.4(4) . . . . ?
Er1 N2 C10 C9 171.8(2) 1_556 . . . ?
C8 C9 C10 N2 0.4(5) . . . . ?
C10 N2 C11 C12 1.9(4) . . . . ?
Er1 N2 C11 C12 -172.2(2) 1_556 . . . ?
N2 C11 C12 C8 0.6(5) . . . . ?
C9 C8 C12 C11 -2.6(5) . . . . ?
C7 C8 C12 C11 173.5(3) . . . . ?
N2 Er1 N3 C13 126.0(2) 1_554 . . . ?
N4 Er1 N3 C13 -57.0(3) . . . . ?
N1 Er1 N3 C13 -61.6(2) . . . . ?
Cl1 Er1 N3 C13 27.6(2) . . . . ?
Cl2 Er1 N3 C13 -145.6(2) . . . . ?
Cl3 Er1 N3 C13 117.7(2) . . . . ?
N2 Er1 N3 C17 -60.1(3) 1_554 . . . ?
N4 Er1 N3 C17 117.0(2) . . . . ?
N1 Er1 N3 C17 112.3(2) . . . . ?
Cl1 Er1 N3 C17 -158.4(2) . . . . ?
Cl2 Er1 N3 C17 28.3(2) . . . . ?
Cl3 Er1 N3 C17 -68.3(2) . . . . ?
C17 N3 C13 C14 0.2(5) . . . . ?
Er1 N3 C13 C14 174.2(2) . . . . ?
N3 C13 C14 C15 -0.3(5) . . . . ?
C13 C14 C15 C16 -0.3(5) . . . . ?
C14 C15 C16 C17 1.0(5) . . . . ?
C13 N3 C17 C16 0.5(5) . . . . ?
Er1 N3 C17 C16 -173.9(3) . . . . ?
C15 C16 C17 N3 -1.1(5) . . . . ?
N2 Er1 N4 C22 110.6(2) 1_554 . . . ?
N3 Er1 N4 C22 -67.9(3) . . . . ?
N1 Er1 N4 C22 -63.3(2) . . . . ?
Cl1 Er1 N4 C22 -155.1(2) . . . . ?
Cl2 Er1 N4 C22 21.2(2) . . . . ?
Cl3 Er1 N4 C22 121.4(2) . . . . ?
N2 Er1 N4 C18 -71.2(2) 1_554 . . . ?
N3 Er1 N4 C18 110.3(2) . . . . ?
N1 Er1 N4 C18 114.9(2) . . . . ?
Cl1 Er1 N4 C18 23.2(2) . . . . ?
Cl2 Er1 N4 C18 -160.5(2) . . . . ?
Cl3 Er1 N4 C18 -60.3(3) . . . . ?
C22 N4 C18 C19 0.5(5) . . . . ?
Er1 N4 C18 C19 -177.8(3) . . . . ?
N4 C18 C19 C20 -1.7(5) . . . . ?
C18 C19 C20 C21 1.4(6) . . . . ?
C19 C20 C21 C22 0.0(6) . . . . ?
C18 N4 C22 C21 1.0(5) . . . . ?
Er1 N4 C22 C21 179.4(3) . . . . ?
C20 C21 C22 N4 -1.3(5) . . . . ?
C27 N5 C23 C24 0.2(5) . . . . ?
N5 C23 C24 C25 0.6(5) . . . . ?
C23 C24 C25 C26 -0.3(5) . . . . ?
C23 C24 C25 C28 177.4(3) . . . . ?
C24 C25 C26 C27 -0.6(5) . . . . ?
C28 C25 C26 C27 -178.4(3) . . . . ?
C23 N5 C27 C26 -1.3(5) . . . . ?
C25 C26 C27 N5 1.5(6) . . . . ?
C24 C25 C28 C28 -97.5(5) . . . 2_665 ?
C26 C25 C28 C28 80.1(5) . . . 2_665 ?
C31 C29 C30 C31 -0.8(9) 2_656 . . . ?
C29 C30 C31 C29 0.8(9) . . . 2_656 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_TEST
_database_code_depnum_ccdc_archive 'CCDC 1414453'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_audit_creation_date             2016-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_formula_moiety         'C15 H15 Cl3 La N4 S3'
_chemical_formula_sum            'C15 H15 Cl3 La N4 S3'
_chemical_formula_weight         593.18
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
La -0.10497 2.62773 20.57800 19.59900 11.37270 3.28719 2.94817 0.24448 18.77260
133.12399 2.14678001404
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   9.1981(18)
_cell_length_b                   9.7269(19)
_cell_length_c                   12.425(3)
_cell_angle_alpha                77.92(3)
_cell_angle_beta                 79.77(3)
_cell_angle_gamma                79.08(3)
_cell_volume                     1056.3(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.491
_cell_measurement_theta_min      2.180
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1283 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.7015.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.8649
_exptl_crystal_description       block
_exptl_crystal_F_000             579.9122
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.137
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15684
_diffrn_reflns_theta_full        28.3846
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.69
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9822
_diffrn_measured_fraction_theta_max 0.9822
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4882
_reflns_number_total             5201
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.53A (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_refine_diff_density_max         1.0365
_refine_diff_density_min         -0.5175
_refine_diff_density_rms         0.1169
_refine_ls_d_res_high            0.7475
_refine_ls_d_res_low             12.0241
_refine_ls_goodness_of_fit_ref   1.0278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.0278
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0326P)²+0.1905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0573
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C5, S2A}
{S2, C5A}
{S3, C8A}
{C8, S3A}
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(S2A)
Uanis(S2) = Uanis(C5A)
Uanis(S3) = Uanis(C8A)
Uanis(C8) = Uanis(S3A)
4. Others
 Sof(S2A)=Sof(H6a)=1-FVAR(1)
 Sof(C5)=Sof(H6)=Sof(H2)=FVAR(1)
 Sof(C5A)=Sof(H5A)=Sof(H4)=1-FVAR(2)
 Sof(S2)=Sof(H5)=FVAR(2)
 Sof(C8A)=Sof(H8A)=Sof(H7)=1-FVAR(3)
 Sof(S3)=Sof(H32)=FVAR(3)
 Sof(S3A)=Sof(H9)=1-FVAR(4)
 Sof(C8)=Sof(H36)=Sof(H24)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15b,H15a)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2a), C1(H1), C14(H14), C13(H13), C11(H11), C10(H10), C5A(H5A),
 C8A(H8A), C7(H32), C7(H7), C9(H36), C9(H9), C6(H6), C6(H6a), C4(H5), C4(H4),
 C8(H24), C5(H2)
;
# start Validation Reply Form
_vrf_PLAT073_TEST                
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr       
RESPONSE: this is caused by the hydrogen treatment in the refinement using olex.refine and presents an artefact of chifcheck
;
# end Validation Reply Form
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_refinement_flags_posn
_atom_site_disorder_group
La1 La 0.406540(12) 0.877553(11) 0.171078(8) 0.01103(5) Uani 1.000000 . .
Cl1 Cl 0.59461(5) 0.64936(6) 0.08452(4) 0.01612(10) Uani 1.000000 . .
Cl2 Cl 0.33767(5) 0.98918(5) -0.04990(4) 0.01533(10) Uani 1.000000 . .
Cl3 Cl 0.26449(6) 0.78261(6) 0.38756(4) 0.01843(11) Uani 1.000000 . .
S1 S 0.11029(6) 0.50563(7) 0.09894(5) 0.02418(13) Uani 1.000000 . .
S3 S 0.49421(8) 1.33629(7) 0.28336(5) 0.0238(2) Uani 0.930(4) . 1
N1 N 0.2155(2) 0.7128(2) 0.13803(14) 0.0161(4) Uani 1.000000 . .
N4 N 0.62547(19) 0.77718(19) 0.30449(14) 0.0141(3) Uani 1.000000 . .
N3 N 0.4264(2) 1.1014(2) 0.26290(14) 0.0156(4) Uani 1.000000 . .
C2 C -0.0142(3) 0.6422(3) 0.14752(19) 0.0227(5) Uani 1.000000 . .
C10 C 0.7302(2) 0.8429(2) 0.32718(16) 0.0146(4) Uani 1.000000 . .
C11 C 0.8336(2) 0.7756(2) 0.39883(17) 0.0165(4) Uani 1.000000 . .
C8 C 0.4799(2) 1.2126(2) 0.39897(16) 0.0299(8) Uani 0.913(5) . 1
C14 C 0.6258(2) 0.6399(2) 0.35361(17) 0.0155(4) Uani 1.000000 . .
C1 C 0.2548(2) 0.5916(2) 0.10223(18) 0.0192(4) Uani 1.000000 . .
C3 C 0.0614(3) 0.7414(3) 0.16297(18) 0.0212(5) Uani 1.000000 . .
C7 C 0.4529(3) 1.2263(2) 0.20652(18) 0.0203(5) Uani 1.000000 . .
C13 C 0.7249(2) 0.5656(2) 0.42510(17) 0.0172(4) Uani 1.000000 . .
C12 C 0.8320(2) 0.6343(2) 0.44977(16) 0.0166(4) Uani 1.000000 . .
C9 C 0.4391(2) 1.0916(2) 0.37334(17) 0.0170(4) Uani 1.000000 . .
N2 N 0.1325(2) 1.0624(2) 0.19668(15) 0.0186(4) Uani 1.000000 . .
C15 C 0.9420(2) 0.5552(3) 0.52714(18) 0.0201(5) Uani 1.000000 . .
C4 C 0.0465(3) 1.1229(3) 0.11973(19) 0.0226(5) Uani 1.000000 . .
C6 C 0.0632(3) 1.0954(3) 0.29775(19) 0.0236(5) Uani 1.000000 . .
S2 S -0.11787(8) 1.21985(8) 0.16537(6) 0.0266(3) Uani 0.834(4) . 1
C5 C -0.0848(2) 1.1884(2) 0.29510(15) 0.0355(7) Uani 0.829(5) . 1
H3 H 0.0118(3) 0.8255(3) 0.18933(18) 0.0254(6) Uiso 1.000000 R .
H2a H -0.1199(3) 0.6472(3) 0.16138(19) 0.0272(6) Uiso 1.000000 R .
H1 H 0.3563(2) 0.5543(2) 0.07973(18) 0.0230(5) Uiso 1.000000 R .
H14 H 0.5536(2) 0.5912(2) 0.33825(17) 0.0186(5) Uiso 1.000000 R .
H13 H 0.7203(2) 0.4687(2) 0.45721(17) 0.0206(5) Uiso 1.000000 R .
H11 H 0.9049(2) 0.8263(2) 0.41276(17) 0.0199(5) Uiso 1.000000 R .
H10 H 0.7337(2) 0.9394(2) 0.29280(16) 0.0175(5) Uiso 1.000000 R .
H15b H 0.9940(2) 0.6241(3) 0.54773(18) 0.0242(5) Uiso 1.000000 R .
H15a H 0.8871(2) 0.5065(3) 0.59607(18) 0.0242(5) Uiso 1.000000 R .
S2A S -0.0848(2) 1.1884(2) 0.29510(15) 0.0355(7) Uani 0.171(5) . 2
C5A C -0.11787(8) 1.21985(8) 0.16537(6) 0.0266(3) Uani 0.166(4) . 2
C8A C 0.49421(8) 1.33629(7) 0.28336(5) 0.0238(2) Uani 0.070(4) . 2
S3A S 0.4799(2) 1.2126(2) 0.39897(16) 0.0299(8) Uani 0.087(5) . 2
H5A H -0.19924(8) 1.27286(8) 0.12936(6) 0.0319(3) Uiso 0.166(4) R 2
H8A H 0.51651(8) 1.43055(7) 0.26695(5) 0.0286(3) Uiso 0.070(4) R 2
H32 H 0.4493(3) 1.2533(2) 0.12889(18) 0.0243(5) Uiso 0.930(4) R 1
H7 H 0.4493(3) 1.2533(2) 0.12889(18) 0.0243(5) Uiso 0.070(4) R 2
H36 H 0.4217(2) 1.0098(2) 0.42791(17) 0.0204(5) Uiso 0.913(5) R 1
H9 H 0.4217(2) 1.0098(2) 0.42791(17) 0.0204(5) Uiso 0.087(5) R 2
H6 H 0.1067(3) 1.0614(3) 0.36415(19) 0.0283(6) Uiso 0.829(5) R 1
H6a H 0.1067(3) 1.0614(3) 0.36415(19) 0.0283(6) Uiso 0.171(5) R 2
H5 H 0.0748(3) 1.1128(3) 0.04410(19) 0.0271(6) Uiso 0.834(4) R 1
H4 H 0.0748(3) 1.1128(3) 0.04410(19) 0.0271(6) Uiso 0.166(4) R 2
H24 H 0.4966(2) 1.2222(2) 0.47017(16) 0.0359(10) Uiso 0.913(5) R 1
H2 H -0.1479(2) 1.2230(2) 0.35618(15) 0.0426(9) Uiso 0.829(5) R 1


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
La1 Cl1 2.8212(11) . ?
La1 Cl2 2.8685(9) . ?
La1 Cl2 2.9263(11) 2_675 ?
La1 Cl3 2.8221(10) . ?
La1 N1 2.7245(18) . ?
La1 N4 2.7422(19) . ?
La1 N3 2.7098(19) . ?
La1 N2 2.816(2) . ?
S1 C2 1.719(3) . ?
S1 C1 1.710(2) . ?
S3 C8 1.673(2) . ?
S3 C7 1.707(2) . ?
N1 C1 1.311(3) . ?
N1 C3 1.383(3) . ?
N4 C10 1.350(3) . ?
N4 C14 1.347(3) . ?
N3 C7 1.311(3) . ?
N3 C9 1.380(3) . ?
C2 C3 1.354(3) . ?
C10 C11 1.395(3) . ?
C11 C12 1.389(3) . ?
C8 C9 1.412(3) . ?
C14 C13 1.383(3) . ?
C7 C8A 1.707(2) . ?
C13 C12 1.398(3) . ?
C12 C15 1.510(3) . ?
C9 S3A 1.412(3) . ?
N2 C4 1.320(3) . ?
N2 C6 1.376(3) . ?
C15 C15 1.537(5) 2_766 ?
C4 S2 1.696(3) . ?
C4 C5A 1.696(3) . ?
C6 C5 1.486(3) . ?
C6 S2A 1.486(3) . ?
S2 C5 1.648(2) . ?
S2A C5A 1.648(2) . ?
C8A S3A 1.673(2) . ?

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
Cl2 La1 Cl1 87.321(15) . . ?
Cl2 La1 Cl1 77.811(14) 2_675 . ?
Cl3 La1 Cl1 110.762(16) . . ?
Cl3 La1 Cl2 140.450(15) . . ?
Cl3 La1 Cl2 142.588(14) . 2_675 ?
N1 La1 Cl1 75.43(4) . . ?
N1 La1 Cl2 74.70(4) . . ?
N1 La1 Cl2 139.33(4) . 2_675 ?
N1 La1 Cl3 76.40(4) . . ?
N4 La1 Cl1 72.90(4) . . ?
N4 La1 Cl2 75.95(4) . 2_675 ?
N4 La1 Cl2 146.86(4) . . ?
N4 La1 Cl3 72.51(4) . . ?
N4 La1 N1 123.08(5) . . ?
N3 La1 Cl1 139.49(4) . . ?
N3 La1 Cl2 70.84(4) . 2_675 ?
N3 La1 Cl2 107.35(4) . . ?
N3 La1 Cl3 81.91(4) . . ?
N3 La1 N1 144.35(5) . . ?
N3 La1 N4 75.06(5) . . ?
N2 La1 Cl1 152.08(4) . . ?
N2 La1 Cl2 115.68(4) . 2_675 ?
N2 La1 Cl2 74.39(4) . . ?
N2 La1 Cl3 74.24(4) . . ?
N2 La1 N1 79.42(5) . . ?
N2 La1 N4 132.56(5) . . ?
N2 La1 N3 67.55(5) . . ?
C1 S1 C2 89.67(11) . . ?
C1 N1 La1 125.64(14) . . ?
C3 N1 La1 124.50(14) . . ?
C3 N1 C1 109.77(18) . . ?
C10 N4 La1 130.38(14) . . ?
C14 N4 La1 112.97(13) . . ?
C14 N4 C10 116.65(18) . . ?
C7 N3 La1 124.82(13) . . ?
C9 N3 La1 124.08(14) . . ?
C9 N3 C7 110.01(18) . . ?
C3 C2 S1 109.51(17) . . ?
C11 C10 N4 123.0(2) . . ?
C12 C11 C10 119.88(19) . . ?
C13 C14 N4 123.81(19) . . ?
N1 C1 S1 115.16(17) . . ?
C2 C3 N1 115.9(2) . . ?
C12 C13 C14 119.5(2) . . ?
C13 C12 C11 117.16(19) . . ?
C15 C12 C11 122.4(2) . . ?
C15 C12 C13 120.5(2) . . ?
C4 N2 La1 127.42(15) . . ?
C6 N2 La1 122.96(14) . . ?
C6 N2 C4 109.49(19) . . ?
C15 C15 C12 111.5(2) 2_766 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Ce_dpa
_database_code_depnum_ccdc_archive 'CCDC 1414454'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_audit_creation_date             2014-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
__publ_contact_author_name       'Klaus M\"uller-Buschbaum,Nicole Dannenbauer'
__publ_contact_author_phone      +499313188724
_chemical_name_common            CeCl3(dpa)2
_chemical_formula_moiety         'C24 H24 Ce Cl3 N4, C3 H3 N S'
_chemical_formula_sum            'C27 H27 Ce Cl3 N5 S'
_chemical_formula_weight         700.09
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ce -0.09320 2.74072 21.16710 19.76950 11.85130 3.33049 2.81219 0.22684 17.60830
127.11300 1.86264002323
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   36.032(7)
_cell_length_b                   9.2604(19)
_cell_length_c                   18.688(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.34(3)
_cell_angle_gamma                90
_cell_volume                     5919(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100
_exptl_absorpt_coefficient_mu    1.905
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0927 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.8813.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5711
_exptl_crystal_description       block
_exptl_crystal_F_000             2796.4204
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.096
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43306
_diffrn_reflns_theta_full        28.3507
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.19
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9937
_diffrn_measured_fraction_theta_max 0.9937
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              45
_reflns_limit_h_min              -48
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6188
_reflns_number_total             7360
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_refine_diff_density_max         0.7948
_refine_diff_density_min         -0.5398
_refine_diff_density_rms         0.1194
_refine_ls_d_res_high            0.7483
_refine_ls_d_res_low             17.1009
_refine_ls_goodness_of_fit_ref   1.0291
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.0291
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0216P)²+7.1723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0518
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24a,H24b), C6(H6a,H6b), C12(H12a,H12b), C18(H18a,H18b)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C8(H8), C7(H7), C13(H13), C14(H14), C16(H16), C17(H17),
 C23(H23), C19(H19), C20(H20), C22(H22), C2(H2), C1(H1), C5(H5), C4(H4),
 C27(H27), C26(H26), C25(H25)
;
# start Validation Reply Form
_vrf_PLAT073_Ce_dpa              
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr       
RESPONSE: this is caused by the hydrogen treatment in the refinment using olex.refine and respents an artefact of checkcif
;
# end Validation Reply Form
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_refinement_flags_posn
Ce1 Ce 0.134912(3) 0.435418(12) 0.384184(6) 0.01397(4) Uani 1.000000 .
Cl1 Cl 0.075369(14) 0.31295(6) 0.42557(3) 0.01922(10) Uani 1.000000 .
Cl2 Cl 0.150487(14) 0.18111(6) 0.32415(3) 0.02178(11) Uani 1.000000 .
Cl3 Cl 0.185050(15) 0.59340(6) 0.33150(3) 0.02368(11) Uani 1.000000 .
N4 N 0.08813(5) 0.44847(19) 0.24273(9) 0.0180(4) Uani 1.000000 .
N2 N 0.16123(5) 0.6179(2) 0.50150(9) 0.0186(4) Uani 1.000000 .
N3 N 0.08798(5) 0.66731(19) 0.36160(9) 0.0174(4) Uani 1.000000 .
C21 C 0.03992(6) 0.4430(2) 0.09160(10) 0.0164(4) Uani 1.000000 .
C20 C 0.06744(6) 0.5525(2) 0.11842(11) 0.0186(4) Uani 1.000000 .
C19 C 0.09065(6) 0.5509(2) 0.19364(11) 0.0197(4) Uani 1.000000 .
C13 C 0.10062(6) 0.8010(2) 0.35275(11) 0.0192(4) Uani 1.000000 .
N1 N 0.18113(6) 0.3053(2) 0.50759(10) 0.0289(5) Uani 1.000000 .
C11 C 0.15097(6) 0.5869(2) 0.56300(11) 0.0200(4) Uani 1.000000 .
C22 C 0.03695(6) 0.3384(2) 0.14254(11) 0.0227(5) Uani 1.000000 .
C16 C 0.02345(6) 0.7681(2) 0.33579(11) 0.0179(4) Uani 1.000000 .
C17 C 0.04953(6) 0.6535(2) 0.35333(10) 0.0179(4) Uani 1.000000 .
C23 C 0.06139(6) 0.3447(3) 0.21666(11) 0.0241(5) Uani 1.000000 .
C24 C 0.01483(6) 0.4388(2) 0.01004(11) 0.0195(4) Uani 1.000000 .
C14 C 0.07612(6) 0.9208(2) 0.33343(11) 0.0184(4) Uani 1.000000 .
C8 C 0.20999(6) 0.7784(2) 0.57881(11) 0.0220(5) Uani 1.000000 .
C15 C 0.03627(6) 0.9042(2) 0.32279(10) 0.0165(4) Uani 1.000000 .
C9 C 0.20028(6) 0.7422(2) 0.64278(11) 0.0167(4) Uani 1.000000 .
C10 C 0.16948(6) 0.6446(2) 0.63385(11) 0.0197(4) Uani 1.000000 .
C3 C 0.22840(6) 0.2258(2) 0.65317(11) 0.0220(5) Uani 1.000000 .
C18 C 0.00836(6) 1.0282(2) 0.29387(11) 0.0177(4) Uani 1.000000 .
C2 C 0.24281(7) 0.3115(3) 0.60689(12) 0.0281(5) Uani 1.000000 .
C7 C 0.19017(6) 0.7147(2) 0.51007(11) 0.0223(5) Uani 1.000000 .
C1 C 0.21841(7) 0.3482(3) 0.53545(12) 0.0295(5) Uani 1.000000 .
C4 C 0.18980(7) 0.1798(3) 0.62396(14) 0.0362(6) Uani 1.000000 .
C5 C 0.16762(8) 0.2202(3) 0.55132(15) 0.0430(7) Uani 1.000000 .
C12 C 0.22315(6) 0.8005(2) 0.71941(11) 0.0181(4) Uani 1.000000 .
C6 C 0.25306(6) 0.1792(2) 0.73125(11) 0.0227(5) Uani 1.000000 .
S1 S 0.09002(2) 0.88866(7) 0.53642(3) 0.03251(14) Uani 1.000000 .
N5 N 0.04857(6) 1.0756(2) 0.57819(11) 0.0339(5) Uani 1.000000 .
C27 C 0.10517(7) 0.9423(3) 0.62894(13) 0.0298(5) Uani 1.000000 .
C26 C 0.08008(7) 1.0407(3) 0.63993(13) 0.0292(5) Uani 1.000000 .
C25 C 0.05087(7) 1.0029(3) 0.52023(13) 0.0306(5) Uani 1.000000 .
H10 H 0.16135(6) 0.6183(2) 0.67573(11) 0.0237(5) Uiso 1.000000 R
H11 H 0.12988(6) 0.5219(2) 0.55770(11) 0.0240(5) Uiso 1.000000 R
H8 H 0.23016(6) 0.8465(2) 0.58202(11) 0.0263(5) Uiso 1.000000 R
H7 H 0.19738(6) 0.7408(2) 0.46708(11) 0.0267(5) Uiso 1.000000 R
H13 H 0.12771(6) 0.8143(2) 0.36008(11) 0.0230(5) Uiso 1.000000 R
H14 H 0.08644(6) 1.0129(2) 0.32757(11) 0.0221(5) Uiso 1.000000 R
H16 H -0.00311(6) 0.7537(2) 0.33266(11) 0.0215(5) Uiso 1.000000 R
H17 H 0.03987(6) 0.5607(2) 0.35987(10) 0.0215(5) Uiso 1.000000 R
H23 H 0.05902(6) 0.2716(3) 0.25061(11) 0.0289(6) Uiso 1.000000 R
H19 H 0.10922(6) 0.6261(2) 0.21115(11) 0.0236(5) Uiso 1.000000 R
H20 H 0.07028(6) 0.6272(2) 0.08569(11) 0.0223(5) Uiso 1.000000 R
H22 H 0.01831(6) 0.2628(2) 0.12687(11) 0.0273(6) Uiso 1.000000 R
H2 H 0.26909(7) 0.3448(3) 0.62390(12) 0.0338(6) Uiso 1.000000 R
H1 H 0.22875(7) 0.4071(3) 0.50465(12) 0.0354(7) Uiso 1.000000 R
H5 H 0.14156(8) 0.1855(3) 0.53199(15) 0.0516(9) Uiso 1.000000 R
H4 H 0.17863(7) 0.1209(3) 0.65345(14) 0.0435(8) Uiso 1.000000 R
H27 H 0.12781(7) 0.9077(3) 0.66664(13) 0.0358(6) Uiso 1.000000 R
H26 H 0.08387(7) 1.0840(3) 0.68779(13) 0.0351(6) Uiso 1.000000 R
H25 H 0.03198(7) 1.0126(3) 0.47182(13) 0.0367(6) Uiso 1.000000 R
H24a H 0.03185(6) 0.4450(2) -0.02239(11) 0.0235(5) Uiso 1.000000 R
H24b H 0.00082(6) 0.3453(2) -0.00036(11) 0.0235(5) Uiso 1.000000 R
H6a H 0.23567(6) 0.1363(2) 0.75732(11) 0.0273(6) Uiso 1.000000 R
H6b H 0.27130(6) 0.1027(2) 0.72623(11) 0.0273(6) Uiso 1.000000 R
H12a H 0.24097(6) 0.8779(2) 0.71374(11) 0.0217(5) Uiso 1.000000 R
H12b H 0.20494(6) 0.8425(2) 0.74391(11) 0.0217(5) Uiso 1.000000 R
H18a H -0.01349(6) 1.0211(2) 0.31518(11) 0.0212(5) Uiso 1.000000 R
H18b H 0.02216(6) 1.1205(2) 0.31109(11) 0.0212(5) Uiso 1.000000 R


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
Ce1 Cl1 2.7444(7) . ?
Ce1 Cl2 2.7415(7) . ?
Ce1 Cl3 2.7373(7) . ?
Ce1 N4 2.6534(18) . ?
Ce1 N2 2.6929(17) . ?
Ce1 N3 2.6834(18) . ?
Ce1 N1 2.6700(19) . ?
N4 C19 1.342(3) . ?
N4 C23 1.339(3) . ?
N2 C11 1.344(3) . ?
N2 C7 1.346(3) . ?
N3 C13 1.347(3) . ?
N3 C17 1.351(3) . ?
C21 C20 1.396(3) . ?
C21 C22 1.385(3) . ?
C21 C24 1.508(3) . ?
C20 C19 1.391(3) . ?
C13 C14 1.393(3) . ?
N1 C1 1.339(3) . ?
N1 C5 1.332(3) . ?
C11 C10 1.389(3) . ?
C22 C23 1.389(3) . ?
C16 C17 1.387(3) . ?
C16 C15 1.390(3) . ?
C24 C24 1.522(4) 3_565 ?
C14 C15 1.395(3) . ?
C8 C9 1.388(3) . ?
C8 C7 1.390(3) . ?
C15 C18 1.510(3) . ?
C9 C10 1.400(3) . ?
C9 C12 1.510(3) . ?
C3 C2 1.389(3) . ?
C3 C4 1.392(3) . ?
C3 C6 1.513(3) . ?
C18 C18 1.559(4) 2 ?
C2 C1 1.390(3) . ?
C4 C5 1.393(3) . ?
C12 C6 1.533(3) 6_556 ?
S1 C27 1.715(2) . ?
S1 C25 1.712(3) . ?
N5 C26 1.379(3) . ?
N5 C25 1.300(3) . ?
C27 C26 1.344(3) . ?

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
Cl2 Ce1 Cl1 92.246(16) . . ?
Cl3 Ce1 Cl1 170.128(16) . . ?
Cl3 Ce1 Cl2 93.937(17) . . ?
N4 Ce1 Cl1 89.52(4) . . ?
N4 Ce1 Cl2 77.24(4) . . ?
N4 Ce1 Cl3 84.35(4) . . ?
N2 Ce1 Cl1 97.82(4) . . ?
N2 Ce1 Cl2 143.82(4) . . ?
N2 Ce1 Cl3 81.63(4) . . ?
N2 Ce1 N4 137.15(5) . . ?
N3 Ce1 Cl1 82.25(4) . . ?
N3 Ce1 Cl2 145.40(4) . . ?
N3 Ce1 Cl3 88.30(4) . . ?
N3 Ce1 N4 68.62(5) . . ?
N3 Ce1 N2 70.67(5) . . ?
N1 Ce1 Cl1 84.29(5) . . ?
N1 Ce1 Cl2 79.24(4) . . ?
N1 Ce1 Cl3 104.42(5) . . ?
N1 Ce1 N4 155.40(6) . . ?
N1 Ce1 N2 67.41(5) . . ?
N1 Ce1 N3 133.48(5) . . ?
C19 N4 Ce1 123.69(13) . . ?
C23 N4 Ce1 119.24(13) . . ?
C23 N4 C19 117.00(17) . . ?
C11 N2 Ce1 116.18(13) . . ?
C7 N2 Ce1 125.17(13) . . ?
C7 N2 C11 116.83(17) . . ?
C13 N3 Ce1 122.28(13) . . ?
C17 N3 Ce1 121.02(14) . . ?
C17 N3 C13 116.54(18) . . ?
C22 C21 C20 117.43(17) . . ?
C24 C21 C20 120.90(18) . . ?
C24 C21 C22 121.67(19) . . ?
C19 C20 C21 119.21(19) . . ?
C20 C19 N4 123.34(19) . . ?
C14 C13 N3 123.55(19) . . ?
C1 N1 Ce1 118.58(16) . . ?
C5 N1 Ce1 123.20(15) . . ?
C5 N1 C1 116.91(19) . . ?
C10 C11 N2 123.7(2) . . ?
C23 C22 C21 119.6(2) . . ?
C15 C16 C17 119.85(19) . . ?
C16 C17 N3 123.31(19) . . ?
C22 C23 N4 123.4(2) . . ?
C24 C24 C21 112.4(2) 3_565 . ?
C15 C14 C13 119.29(19) . . ?
C7 C8 C9 119.9(2) . . ?
C14 C15 C16 117.31(19) . . ?
C18 C15 C16 122.12(18) . . ?
C18 C15 C14 120.47(19) . . ?
C10 C9 C8 117.28(18) . . ?
C12 C9 C8 121.37(19) . . ?
C12 C9 C10 121.29(18) . . ?
C9 C10 C11 119.15(19) . . ?
C4 C3 C2 117.0(2) . . ?
C6 C3 C2 122.9(2) . . ?
C6 C3 C4 120.1(2) . . ?
C18 C18 C15 111.71(15) 2 . ?
C1 C2 C3 119.4(2) . . ?
C8 C7 N2 123.12(19) . . ?
C2 C1 N1 123.7(2) . . ?
C5 C4 C3 119.8(2) . . ?
C4 C5 N1 123.3(2) . . ?
C6 C12 C9 110.10(17) 6_556 . ?
C12 C6 C3 114.73(18) 6_546 . ?
C25 S1 C27 89.00(12) . . ?
C25 N5 C26 108.9(2) . . ?
C26 C27 S1 109.53(18) . . ?
C27 C26 N5 116.6(2) . . ?
N5 C25 S1 115.95(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Pr_dpa
_database_code_depnum_ccdc_archive 'CCDC 1414455'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_audit_creation_date             2014-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
__publ_contact_author_name       'Klaus M\"uller-Buschbaum,Nicole Dannenbauer'
__publ_contact_author_phone      +499313188724
_chemical_name_common            PrCl3(dpa)2
_chemical_formula_moiety         'C24 H24 Cl3 N4 Pr, C3 H3 N S'
_chemical_formula_sum            'C27 H27 Cl3 N5 Pr S'
_chemical_formula_weight         700.88
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Pr -0.09076 2.91177 22.04400 19.66970 12.38560 2.82428 2.77393 0.22209 16.76690
143.64400 2.05830001831
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   35.8284(17)
_cell_length_b                   9.2397(4)
_cell_length_c                   18.6155(9)
_cell_angle_alpha                90
_cell_angle_beta                 108.312(1)
_cell_angle_gamma                90
_cell_volume                     5850.5(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.145
_cell_measurement_theta_min      2.239
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0541 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.8876.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5913
_exptl_crystal_description       block
_exptl_crystal_F_000             2804.4599
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.149
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38871
_diffrn_reflns_theta_full        28.3196
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.24
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              45
_reflns_limit_h_min              -47
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5737
_reflns_number_total             7282
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.53A (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_refine_diff_density_max         0.8270
_refine_diff_density_min         -1.1515
_refine_diff_density_rms         0.1799
_refine_ls_d_res_high            0.7491
_refine_ls_d_res_low             9.0973
_refine_ls_goodness_of_fit_ref   1.0518
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.0518
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+10.8795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0664
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24a,H24b), C18(H18a,H18b), C12(H12a,H12b), C6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C13(H13), C11(H11), C22(H22), C16(H16), C17(H17),
 C23(H23), C14(H14), C8(H8), C10(H10), C2(H2), C7(H7), C1(H1), C4(H4), C5(H5),
 C27(H27), C26(H26), C25(H25)
;
# start Validation Reply Form
_vrf_PLAT073_Pr_dpa              
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr       
RESPONSE: this is caused the the hydrogen treatment in the refinement using olex.refine and presents an artefact of checkcif
;
# end Validation Reply Form
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_refinement_flags_posn
Pr1 Pr 0.134748(4) 0.436429(17) 0.384428(8) 0.01181(5) Uani 1.000000 .
Cl1 Cl 0.07541(2) 0.31454(8) 0.42564(4) 0.01709(14) Uani 1.000000 .
Cl2 Cl 0.15025(2) 0.18411(8) 0.32472(4) 0.01936(15) Uani 1.000000 .
Cl3 Cl 0.18510(2) 0.59186(8) 0.33231(4) 0.02093(16) Uani 1.000000 .
N4 N 0.08811(7) 0.4488(3) 0.24371(12) 0.0157(5) Uani 1.000000 .
N2 N 0.16114(7) 0.6174(3) 0.50125(12) 0.0154(5) Uani 1.000000 .
N3 N 0.08793(7) 0.6669(3) 0.36213(12) 0.0152(5) Uani 1.000000 .
C21 C 0.03988(8) 0.4437(3) 0.09235(14) 0.0144(5) Uani 1.000000 .
C20 C 0.06733(8) 0.5531(3) 0.11920(15) 0.0169(6) Uani 1.000000 .
H20 H 0.07013(8) 0.6281(3) 0.08641(15) 0.0203(7) Uiso 1.000000 R
C19 C 0.09061(8) 0.5514(3) 0.19442(15) 0.0180(6) Uani 1.000000 .
H19 H 0.10930(8) 0.6267(3) 0.21196(15) 0.0215(7) Uiso 1.000000 R
C13 C 0.10087(8) 0.7998(3) 0.35367(15) 0.0170(6) Uani 1.000000 .
H13 H 0.12815(8) 0.8128(3) 0.36131(15) 0.0203(7) Uiso 1.000000 R
N1 N 0.18098(8) 0.3070(3) 0.50671(13) 0.0263(6) Uani 1.000000 .
C11 C 0.15066(8) 0.5862(3) 0.56274(15) 0.0162(6) Uani 1.000000 .
H11 H 0.12943(8) 0.5211(3) 0.55735(15) 0.0195(7) Uiso 1.000000 R
C22 C 0.03674(9) 0.3390(3) 0.14332(15) 0.0213(7) Uani 1.000000 .
H22 H 0.01798(9) 0.2634(3) 0.12748(15) 0.0256(8) Uiso 1.000000 R
C16 C 0.02329(8) 0.7679(3) 0.33614(15) 0.0157(6) Uani 1.000000 .
H16 H -0.00344(8) 0.7536(3) 0.33299(15) 0.0188(7) Uiso 1.000000 R
C17 C 0.04935(8) 0.6533(3) 0.35374(14) 0.0154(6) Uani 1.000000 .
H17 H 0.03958(8) 0.5603(3) 0.36024(14) 0.0184(7) Uiso 1.000000 R
C23 C 0.06113(9) 0.3453(3) 0.21761(16) 0.0216(7) Uani 1.000000 .
H23 H 0.05857(9) 0.2723(3) 0.25173(16) 0.0259(8) Uiso 1.000000 R
C24 C 0.01481(8) 0.4380(3) 0.01030(14) 0.0171(6) Uani 1.000000 .
H24a H 0.03200(8) 0.4429(3) -0.02216(14) 0.0205(7) Uiso 1.000000 R
H24b H 0.00054(8) 0.3447(3) 0.00026(14) 0.0205(7) Uiso 1.000000 R
C14 C 0.07621(8) 0.9201(3) 0.33420(15) 0.0169(6) Uani 1.000000 .
H14 H 0.08663(8) 1.0124(3) 0.32855(15) 0.0203(7) Uiso 1.000000 R
C8 C 0.20989(9) 0.7782(3) 0.57863(15) 0.0184(6) Uani 1.000000 .
H8 H 0.23011(9) 0.8468(3) 0.58181(15) 0.0221(7) Uiso 1.000000 R
C15 C 0.03619(8) 0.9035(3) 0.32312(15) 0.0149(6) Uani 1.000000 .
C9 C 0.20006(8) 0.7419(3) 0.64275(14) 0.0131(5) Uani 1.000000 .
C10 C 0.16930(8) 0.6443(3) 0.63376(15) 0.0173(6) Uani 1.000000 .
H10 H 0.16115(8) 0.6177(3) 0.67583(15) 0.0208(7) Uiso 1.000000 R
C3 C 0.22835(9) 0.2266(3) 0.65246(16) 0.0199(6) Uani 1.000000 .
C18 C 0.00834(9) 1.0279(3) 0.29383(15) 0.0160(6) Uani 1.000000 .
H18a H -0.01368(9) 1.0215(3) 0.31515(15) 0.0191(7) Uiso 1.000000 R
H18b H 0.02233(9) 1.1202(3) 0.31107(15) 0.0191(7) Uiso 1.000000 R
C2 C 0.24271(9) 0.3125(4) 0.60646(16) 0.0257(7) Uani 1.000000 .
H2 H 0.26912(9) 0.3458(4) 0.62379(16) 0.0309(9) Uiso 1.000000 R
C7 C 0.18999(9) 0.7139(3) 0.50967(15) 0.0196(6) Uani 1.000000 .
H7 H 0.19725(9) 0.7398(3) 0.46649(15) 0.0235(8) Uiso 1.000000 R
C1 C 0.21850(10) 0.3499(4) 0.53491(16) 0.0268(8) Uani 1.000000 .
H1 H 0.22905(10) 0.4091(4) 0.50427(16) 0.0322(9) Uiso 1.000000 R
C4 C 0.18978(10) 0.1796(4) 0.62268(19) 0.0337(9) Uani 1.000000 .
H4 H 0.17860(10) 0.1193(4) 0.65184(19) 0.0405(11) Uiso 1.000000 R
C5 C 0.16759(11) 0.2209(4) 0.5503(2) 0.0385(10) Uani 1.000000 .
H5 H 0.14142(11) 0.1858(4) 0.5308(2) 0.0462(12) Uiso 1.000000 R
C12 C 0.22297(8) 0.8004(3) 0.71951(14) 0.0155(6) Uani 1.000000 .
H12a H 0.24094(8) 0.8778(3) 0.71377(14) 0.0186(7) Uiso 1.000000 R
H12b H 0.20465(8) 0.8428(3) 0.74398(14) 0.0186(7) Uiso 1.000000 R
C6 C 0.25320(9) 0.1792(3) 0.73077(15) 0.0194(6) Uani 1.000000 .
H6a H 0.23574(9) 0.1357(3) 0.75687(15) 0.0233(8) Uiso 1.000000 R
H6b H 0.27158(9) 0.1029(3) 0.72552(15) 0.0233(8) Uiso 1.000000 R
S1 S 0.09003(3) 0.88850(10) 0.53693(5) 0.0304(2) Uani 1.000000 .
N5 N 0.04892(9) 1.0775(3) 0.57811(15) 0.0316(7) Uani 1.000000 .
C27 C 0.10515(10) 0.9418(4) 0.62947(17) 0.0276(7) Uani 1.000000 .
H27 H 0.12776(10) 0.9064(4) 0.66740(17) 0.0331(9) Uiso 1.000000 R
C26 C 0.08025(10) 1.0413(4) 0.64039(17) 0.0275(7) Uani 1.000000 .
H26 H 0.08399(10) 1.0845(4) 0.68846(17) 0.0330(9) Uiso 1.000000 R
C25 C 0.05117(10) 1.0039(4) 0.52031(18) 0.0283(7) Uani 1.000000 .
H25 H 0.03228(10) 1.0138(4) 0.47162(18) 0.0340(9) Uiso 1.000000 R


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
Pr1 Cl1 2.7206(7) . ?
Pr1 Cl2 2.7142(7) . ?
Pr1 Cl3 2.7127(7) . ?
Pr1 N4 2.630(2) . ?
Pr1 N2 2.670(2) . ?
Pr1 N3 2.661(2) . ?
Pr1 N1 2.643(2) . ?
N4 C19 1.341(4) . ?
N4 C23 1.338(4) . ?
N2 C11 1.343(4) . ?
N2 C7 1.336(4) . ?
N3 C13 1.339(4) . ?
N3 C17 1.347(4) . ?
C21 C20 1.389(4) . ?
C21 C22 1.384(4) . ?
C21 C24 1.510(3) . ?
C20 C19 1.387(4) . ?
C13 C14 1.395(4) . ?
N1 C1 1.340(4) . ?
N1 C5 1.329(5) . ?
C11 C10 1.388(4) . ?
C22 C23 1.386(4) . ?
C16 C17 1.381(4) . ?
C16 C15 1.383(4) . ?
C24 C24 1.526(6) 3_565 ?
C14 C15 1.392(4) . ?
C8 C9 1.388(4) . ?
C8 C7 1.391(4) . ?
C15 C18 1.507(4) . ?
C9 C10 1.393(4) . ?
C9 C12 1.507(3) . ?
C3 C2 1.380(5) . ?
C3 C4 1.387(4) . ?
C3 C6 1.514(4) . ?
C18 C18 1.552(5) 2 ?
C2 C1 1.386(4) . ?
C4 C5 1.385(4) . ?
C12 C6 1.531(4) 6_556 ?
S1 C27 1.708(3) . ?
S1 C25 1.703(4) . ?
N5 C26 1.378(4) . ?
N5 C25 1.296(4) . ?
C27 C26 1.340(5) . ?

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
Cl2 Pr1 Cl1 92.20(2) . . ?
Cl3 Pr1 Cl1 170.57(2) . . ?
Cl3 Pr1 Cl2 93.65(2) . . ?
N4 Pr1 Cl1 89.47(5) . . ?
N4 Pr1 Cl2 77.12(5) . . ?
N4 Pr1 Cl3 84.64(5) . . ?
N2 Pr1 Cl1 97.91(6) . . ?
N2 Pr1 Cl2 143.70(5) . . ?
N2 Pr1 Cl3 81.64(6) . . ?
N2 Pr1 N4 137.36(7) . . ?
N3 Pr1 Cl1 82.25(5) . . ?
N3 Pr1 Cl2 145.43(5) . . ?
N3 Pr1 Cl3 88.74(5) . . ?
N3 Pr1 N4 68.77(7) . . ?
N3 Pr1 N2 70.76(7) . . ?
N1 Pr1 Cl1 84.47(7) . . ?
N1 Pr1 Cl2 79.08(6) . . ?
N1 Pr1 Cl3 103.90(7) . . ?
N1 Pr1 N4 155.18(8) . . ?
N1 Pr1 N2 67.43(7) . . ?
N1 Pr1 N3 133.63(7) . . ?
C19 N4 Pr1 123.64(18) . . ?
C23 N4 Pr1 119.40(18) . . ?
C23 N4 C19 116.9(2) . . ?
C11 N2 Pr1 115.93(18) . . ?
C7 N2 Pr1 125.19(18) . . ?
C7 N2 C11 117.1(2) . . ?
C13 N3 Pr1 121.85(19) . . ?
C17 N3 Pr1 121.14(18) . . ?
C17 N3 C13 116.9(2) . . ?
C22 C21 C20 117.6(2) . . ?
C24 C21 C20 121.2(3) . . ?
C24 C21 C22 121.2(3) . . ?
C19 C20 C21 119.2(3) . . ?
C20 C19 N4 123.4(3) . . ?
C14 C13 N3 123.2(3) . . ?
C1 N1 Pr1 118.9(2) . . ?
C5 N1 Pr1 123.2(2) . . ?
C5 N1 C1 116.6(3) . . ?
C10 C11 N2 123.3(3) . . ?
C23 C22 C21 119.6(3) . . ?
C15 C16 C17 119.9(3) . . ?
C16 C17 N3 123.3(3) . . ?
C22 C23 N4 123.3(3) . . ?
C24 C24 C21 111.9(3) 3_565 . ?
C15 C14 C13 119.3(3) . . ?
C7 C8 C9 119.7(3) . . ?
C14 C15 C16 117.4(3) . . ?
C18 C15 C16 122.3(3) . . ?
C18 C15 C14 120.2(3) . . ?
C10 C9 C8 117.3(2) . . ?
C12 C9 C8 121.3(3) . . ?
C12 C9 C10 121.4(2) . . ?
C9 C10 C11 119.4(3) . . ?
C4 C3 C2 116.8(3) . . ?
C6 C3 C2 122.8(3) . . ?
C6 C3 C4 120.3(3) . . ?
C18 C18 C15 111.9(2) 2 . ?
C1 C2 C3 119.8(3) . . ?
C8 C7 N2 123.1(3) . . ?
C2 C1 N1 123.4(3) . . ?
C5 C4 C3 119.8(3) . . ?
C4 C5 N1 123.5(3) . . ?
C6 C12 C9 110.2(2) 6_556 . ?
C12 C6 C3 114.7(2) 6_546 . ?
C25 S1 C27 89.13(16) . . ?
C25 N5 C26 108.9(3) . . ?
C26 C27 S1 109.6(2) . . ?
C27 C26 N5 116.4(3) . . ?
N5 C25 S1 116.0(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_TEST
_database_code_depnum_ccdc_archive 'CCDC 1414456'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_audit_creation_date             2016-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_formula_moiety         'C48 H45 Cl6 Dy2 N8, 2(C4 H3 S)'
_chemical_formula_sum            'C56 H51 Cl6 Dy2 N8 S2'
_chemical_formula_weight         1437.93
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Dy -0.09334 4.42894 26.50700 17.63830 14.55960 2.96577 2.18020 0.20217 12.18990
111.87400 4.29727983475
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   35.642(2)
_cell_length_b                   9.2416(6)
_cell_length_c                   18.5076(11)
_cell_angle_alpha                90
_cell_angle_beta                 109.058(1)
_cell_angle_gamma                90
_cell_volume                     5762.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8409
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.090
_cell_measurement_theta_min      2.246
_exptl_absorpt_coefficient_mu    2.969
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0583 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.8911.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.6574
_exptl_crystal_description       block
_exptl_crystal_F_000             2840.4868
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.157
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42289
_diffrn_reflns_theta_full        28.3378
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.25
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_diffrn_measurement_device_type  ApexII
_diffrn_radiation_type           'Mo K\a'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              44
_reflns_limit_h_min              -47
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5213
_reflns_number_total             7194
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.53A (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_refine_diff_density_max         1.1335
_refine_diff_density_min         -2.3016
_refine_diff_density_rms         0.2241
_refine_ls_d_res_high            0.7487
_refine_ls_d_res_low             9.0672
_refine_ls_goodness_of_fit_ref   1.0303
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    71
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7194
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0332
_refine_ls_restrained_S_all      1.0303
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0226P)²+30.0424P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0750
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H16(0.5) S1(0.5) S1A(0.5) C30(0.5) H30(0.5) C29(0.5) H29(0.5)
 C31(0.5) H31(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5) C25(0.5) H25(0.5)
 C19(0.5) H19(0.5) C23(0.5) H23(0.5) C21(0.5) C22(0.5) H22(0.5) C22A(0.5)
 H22A(0.5) C21A(0.5) C23A(0.5) H23A(0.5) C20A(0.5) H20A(0.5) C19A(0.5)
 H19A(0.5) C24(0.5) C24A(0.5) H24a(0.5) H24b(0.5) C20(0.5) H20(0.5) C13(0.5)
 H13(0.5) C15(0.5) C14(0.5) H14(0.5) C14A(0.5) H14A(0.5) C13A(0.5) H13A(0.5)
 C18(0.5) H18a(0.5) H18b(0.5) C18A(0.5) H18c(0.5) H18d(0.5) C15A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C12(H12a,H12b), C24A(H24a,H24b), C18(H18a,H18b), C18A(H18c,H18d)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C17(H17), C10(H10), C11(H11), C7(H7), C4(H4), C5(H5), C1(H1),
 C16(H16), C30(H30), C29(H29), C31(H31), C27(H27), C28(H28), C25(H25), C19(H19),
  C23(H23), C22(H22), C22A(H22A), C23A(H23A), C20A(H20A), C19A(H19A), C20(H20),
 C13(H13), C14(H14), C14A(H14A), C13A(H13A)
;
# start Validation Reply Form
_vrf_PLAT073_TEST                
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr Check 
RESPONSE: this is caused by the hydrogen treatment in the refinement using olex.refine and presents an artefact of checkcif
;
# end Validation Reply Form
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_refinement_flags_posn
_atom_site_disorder_group
Dy1 Dy -0.135255(5) 0.49323(2) -0.384650(9) 0.01781(6) Uani 1.000000 . .
Cl1 Cl -0.07933(3) 0.37129(10) -0.42806(5) 0.01652(18) Uani 1.000000 . .
Cl3 Cl -0.18726(3) 0.63816(15) -0.34288(6) 0.0339(3) Uani 1.000000 . .
Cl2 Cl -0.14496(3) 0.24853(13) -0.32028(6) 0.0299(3) Uani 1.000000 . .
N2 N -0.15786(9) 0.6400(3) -0.50822(17) 0.0164(7) Uani 1.000000 . .
N1 N -0.18729(10) 0.3620(4) -0.49018(19) 0.0291(9) Uani 1.000000 . .
N3 N -0.09126(10) 0.7200(4) -0.36469(17) 0.0225(8) Uani 1.000000 . .
N4 N -0.08968(10) 0.5163(5) -0.24834(18) 0.0368(10) Uani 1.000000 . .
C6 C -0.26070(12) 0.1924(4) -0.7084(2) 0.0222(9) Uani 1.000000 . .
H6a H -0.24393(12) 0.1292(4) -0.7284(2) 0.0267(11) Uiso 1.000000 R .
H6b H -0.28227(12) 0.1321(4) -0.7016(2) 0.0267(11) Uiso 1.000000 R .
C9 C -0.19856(11) 0.7509(4) -0.6547(2) 0.0143(7) Uani 1.000000 . .
C8 C -0.20599(12) 0.8005(4) -0.5903(2) 0.0224(9) Uani 1.000000 . .
H8 H -0.22535(12) 0.8736(4) -0.5948(2) 0.0268(11) Uiso 1.000000 R .
C2 C -0.24945(13) 0.3558(6) -0.5930(2) 0.0347(12) Uani 1.000000 . .
H2 H -0.27573(13) 0.3922(6) -0.6136(2) 0.0416(14) Uiso 1.000000 R .
C17 C -0.05275(12) 0.7078(4) -0.3576(2) 0.0214(9) Uani 1.000000 . .
H17 H -0.04353(12) 0.6156(4) -0.3670(2) 0.0257(10) Uiso 1.000000 R .
C10 C -0.16934(12) 0.6447(5) -0.6431(2) 0.0230(9) Uani 1.000000 . .
H10 H -0.16280(12) 0.6075(5) -0.6854(2) 0.0276(11) Uiso 1.000000 R .
C3 C -0.23587(12) 0.2507(5) -0.6316(2) 0.0234(9) Uani 1.000000 . .
C11 C -0.14991(12) 0.5935(4) -0.5703(2) 0.0207(9) Uani 1.000000 . .
H11 H -0.12995(12) 0.5219(4) -0.5640(2) 0.0248(10) Uiso 1.000000 R .
C7 C -0.18535(13) 0.7440(5) -0.5193(2) 0.0273(10) Uani 1.000000 . .
H7 H -0.19096(13) 0.7808(5) -0.4760(2) 0.0328(12) Uiso 1.000000 R .
C4 C -0.19783(14) 0.1995(5) -0.5954(3) 0.0429(14) Uani 1.000000 . .
H4 H -0.18723(14) 0.1251(5) -0.6185(3) 0.0515(17) Uiso 1.000000 R .
C5 C -0.17535(15) 0.2564(5) -0.5260(3) 0.0434(14) Uani 1.000000 . .
H5 H -0.14960(15) 0.2174(5) -0.5022(3) 0.0521(17) Uiso 1.000000 R .
C12 C -0.22102(12) 0.8101(4) -0.7328(2) 0.0181(8) Uani 1.000000 . .
H12a H -0.20274(12) 0.8691(4) -0.7511(2) 0.0218(10) Uiso 1.000000 R .
H12b H -0.24240(12) 0.8746(4) -0.7287(2) 0.0218(10) Uiso 1.000000 R .
C1 C -0.22430(13) 0.4076(6) -0.5237(2) 0.0362(12) Uani 1.000000 . .
H1 H -0.23419(13) 0.4805(6) -0.4985(2) 0.0435(15) Uiso 1.000000 R .
C16 C -0.02527(14) 0.8198(5) -0.3375(2) 0.0282(10) Uani 1.000000 . .
H16 H 0.00167(14) 0.7944(5) -0.3289(2) 0.0339(12) Uiso 0.500000 R 1
S1 S -0.05827(9) 0.8674(3) -0.54124(15) 0.0451(7) Uani 0.500000 . 1
S1A S -0.09935(9) 0.9768(4) -0.53406(16) 0.0517(8) Uani 0.500000 . 2
C30 C -0.0435(2) 0.9688(10) -0.5881(5) 0.026(2) Uani 0.500000 . 2
H30 H -0.0178(2) 0.9668(10) -0.5930(5) 0.031(2) Uiso 0.500000 R 2
C29 C -0.0506(3) 0.9899(11) -0.5252(5) 0.0277(18) Uani 0.500000 . 2
H29 H -0.0305(3) 1.0107(11) -0.4781(5) 0.033(2) Uiso 0.500000 R 2
C31 C -0.0779(3) 0.9501(11) -0.6465(5) 0.034(2) Uani 0.500000 . 2
H31 H -0.0763(3) 0.9244(11) -0.6950(5) 0.040(3) Uiso 0.500000 R 2
C27 C -0.1035(2) 1.0765(9) -0.5984(5) 0.0223(18) Uani 0.500000 . 1
H27 H -0.1150(2) 1.1700(9) -0.6096(5) 0.027(2) Uiso 0.500000 R 1
C28 C -0.0754(3) 1.0359(9) -0.5363(5) 0.029(2) Uani 0.500000 . 1
H28 H -0.0657(3) 1.0958(9) -0.4924(5) 0.034(2) Uiso 0.500000 R 1
C25 C -0.0878(3) 0.8453(11) -0.6302(5) 0.031(2) Uani 0.500000 . 1
H25 H -0.0880(3) 0.7698(11) -0.6652(5) 0.037(3) Uiso 0.500000 R 1
C26 C -0.11206(16) 0.9643(6) -0.6406(4) 0.0549(17) Uani 1.000000 . .
C19 C -0.0982(3) 0.6313(10) -0.1972(6) 0.013(2) Uiso 0.500000 . 1
H19 H -0.1219(3) 0.6870(10) -0.2148(6) 0.016(3) Uiso 0.500000 R 1
C23 C -0.0570(5) 0.4661(11) -0.2249(9) 0.017(3) Uani 0.500000 . 1
H23 H -0.0494(5) 0.4056(11) -0.2593(9) 0.020(3) Uiso 0.500000 R 1
C21 C -0.0360(3) 0.5818(11) -0.1013(7) 0.016(2) Uani 0.500000 . 1
C22 C -0.0286(3) 0.4861(11) -0.1526(6) 0.0156(19) Uani 0.500000 . 1
H22 H -0.0043(3) 0.4341(11) -0.1388(6) 0.019(2) Uiso 0.500000 R 1
C22A C -0.0277(3) 0.4160(12) -0.1549(6) 0.018(2) Uani 0.500000 . 2
H22A H -0.0049(3) 0.3553(12) -0.1416(6) 0.021(3) Uiso 0.500000 R 2
C21A C -0.0327(3) 0.5146(12) -0.1020(7) 0.015(2) Uani 0.500000 . 2
C23A C -0.0558(5) 0.4065(12) -0.2268(9) 0.017(3) Uani 0.500000 . 2
H23A H -0.0540(5) 0.3337(12) -0.2618(9) 0.021(3) Uiso 0.500000 R 2
C20A C -0.0673(3) 0.5969(10) -0.1247(5) 0.013(2) Uiso 0.500000 . 2
H20A H -0.0730(3) 0.6622(10) -0.0900(5) 0.016(3) Uiso 0.500000 R 2
C19A C -0.0933(3) 0.5822(11) -0.1985(5) 0.017(2) Uani 0.500000 . 2
H19A H -0.1176(3) 0.6340(11) -0.2094(5) 0.021(2) Uiso 0.500000 R 2
C24 C -0.0051(3) 0.6097(10) -0.0219(5) 0.021(2) Uani 0.500000 . 1
C24A C -0.0025(2) 0.5346(10) -0.0229(5) 0.0138(19) Uani 0.500000 . 2
H24a H 0.0234(2) 0.5459(10) -0.0310(5) 0.017(2) Uiso 0.500000 R 2
H24b H -0.0086(2) 0.6296(10) -0.0047(5) 0.017(2) Uiso 0.500000 R 2
C20 C -0.0712(3) 0.6548(11) -0.1242(5) 0.0173(18) Uani 0.500000 . 1
H20 H -0.0773(3) 0.7216(11) -0.0906(5) 0.021(2) Uiso 0.500000 R 1
C13 C -0.0989(5) 0.8642(18) -0.3601(8) 0.015(3) Uani 0.500000 . 1
H13 H -0.1260(5) 0.8896(18) -0.3707(8) 0.018(3) Uiso 0.500000 R 1
C15 C -0.0322(4) 0.9511(15) -0.3295(8) 0.017(3) Uani 0.500000 . 1
C14 C -0.0717(3) 0.9793(11) -0.3415(6) 0.0114(19) Uani 0.500000 . 1
H14 H -0.0804(3) 1.0751(11) -0.3372(6) 0.014(2) Uiso 0.500000 R 1
C14A C -0.0839(3) 0.9630(10) -0.3247(5) 0.0134(19) Uani 0.500000 . 2
H14A H -0.0952(3) 1.0509(10) -0.3149(5) 0.016(2) Uiso 0.500000 R 2
C13A C -0.1076(4) 0.8430(19) -0.3461(8) 0.016(3) Uani 0.500000 . 2
H13A H -0.1345(4) 0.8450(19) -0.3479(8) 0.020(3) Uiso 0.500000 R 2
C18 C -0.0014(3) 1.0734(9) -0.3034(5) 0.0143(16) Uani 0.500000 . 1
H18a H 0.0243(3) 1.0481(9) -0.3099(5) 0.017(2) Uiso 0.500000 R 1
H18b H -0.0112(3) 1.1665(9) -0.3292(5) 0.017(2) Uiso 0.500000 R 1
C18A C -0.0170(3) 1.0818(10) -0.2854(5) 0.0192(18) Uani 0.500000 . 2
H18c H -0.0343(3) 1.1621(10) -0.2801(5) 0.023(2) Uiso 0.500000 R 2
H18d H -0.0062(3) 1.1112(10) -0.3262(5) 0.023(2) Uiso 0.500000 R 2
C15A C -0.0437(4) 0.9592(13) -0.3168(8) 0.012(2) Uani 0.500000 . 2


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
Dy1 Cl1 2.6332(9) . ?
Dy1 Cl3 2.6005(11) . ?
Dy1 Cl2 2.6309(11) . ?
Dy1 N2 2.553(3) . ?
Dy1 N1 2.522(3) . ?
Dy1 N3 2.571(4) . ?
Dy1 N4 2.524(3) . ?
N2 C11 1.342(5) . ?
N2 C7 1.340(5) . ?
N1 C5 1.326(6) . ?
N1 C1 1.330(6) . ?
N3 C17 1.340(5) . ?
N3 C13 1.369(17) . ?
N3 C13A 1.371(17) . ?
N4 C19 1.518(10) . ?
N4 C23 1.195(16) . ?
N4 C23A 1.528(14) . ?
N4 C19A 1.148(11) . ?
C6 H6a 0.9900 . ?
C6 H6b 0.9900 . ?
C6 C3 1.507(5) . ?
C6 C12 1.526(5) 6_443 ?
C9 C8 1.382(5) . ?
C9 C10 1.396(5) . ?
C9 C12 1.508(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.382(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(6) . ?
C2 C1 1.388(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.389(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(5) . ?
C3 C4 1.385(6) . ?
C11 H11 0.9500 . ?
C7 H7 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.377(6) . ?
C5 H5 0.9500 . ?
C12 H12a 0.9900 . ?
C12 H12b 0.9900 . ?
C1 H1 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.257(14) . ?
C16 C15A 1.551(12) . ?
S1 C28 1.687(10) . ?
S1 C25 1.652(8) . ?
S1A C29 1.694(10) . ?
S1A C26 1.877(7) . ?
C30 H30 0.9500 . ?
C30 C29 1.287(11) . ?
C30 C31 1.356(12) . ?
C29 H29 0.9500 . ?
C31 H31 0.9500 . ?
C31 C26 1.262(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.308(12) . ?
C27 C26 1.275(10) . ?
C28 H28 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.373(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.397(13) . ?
C23 H23 0.9500 . ?
C23 C22 1.403(19) . ?
C21 C22 1.384(15) . ?
C21 C24 1.544(15) . ?
C21 C20 1.364(14) . ?
C22 H22 0.9500 . ?
C22A H22A 0.9500 . ?
C22A C21A 1.391(14) . ?
C22A C23A 1.382(19) . ?
C21A C20A 1.391(13) . ?
C21A C24A 1.520(14) . ?
C23A H23A 0.9500 . ?
C20A H20A 0.9500 . ?
C20A C19A 1.384(13) . ?
C19A H19A 0.9500 . ?
C24A C24A 1.029(17) 3_565 ?
C24A H24a 0.9900 . ?
C24A H24b 0.9900 . ?
C20 H20 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.405(18) . ?
C15 C14 1.376(13) . ?
C15 C18 1.541(18) . ?
C14 H14 0.9500 . ?
C14A H14A 0.9500 . ?
C14A C13A 1.372(19) . ?
C14A C15A 1.390(13) . ?
C13A H13A 0.9500 . ?
C18 C18 1.946(17) 2_554 ?
C18 H18a 0.9900 . ?
C18 H18b 0.9900 . ?
C18A C18A 1.463(18) 2_554 ?
C18A H18c 0.9900 . ?
C18A H18d 0.9900 . ?
C18A C15A 1.473(16) . ?

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
Cl3 Dy1 Cl1 174.32(4) . . ?
Cl2 Dy1 Cl1 89.70(3) . . ?
Cl2 Dy1 Cl3 95.53(4) . . ?
N2 Dy1 Cl1 90.17(7) . . ?
N2 Dy1 Cl3 86.88(8) . . ?
N2 Dy1 Cl2 144.36(7) . . ?
N1 Dy1 Cl1 89.80(10) . . ?
N1 Dy1 Cl3 93.59(10) . . ?
N1 Dy1 Cl2 76.42(8) . . ?
N1 Dy1 N2 67.94(10) . . ?
N3 Dy1 Cl1 84.59(8) . . ?
N3 Dy1 Cl3 89.88(8) . . ?
N3 Dy1 Cl2 143.11(7) . . ?
N3 Dy1 N2 72.24(10) . . ?
N3 Dy1 N1 139.74(10) . . ?
N4 Dy1 Cl1 92.12(10) . . ?
N4 Dy1 Cl3 87.01(10) . . ?
N4 Dy1 Cl2 75.94(10) . . ?
N4 Dy1 N2 139.67(12) . . ?
N4 Dy1 N1 152.28(12) . . ?
N4 Dy1 N3 67.92(12) . . ?
C11 N2 Dy1 120.3(2) . . ?
C7 N2 Dy1 121.3(3) . . ?
C7 N2 C11 116.6(3) . . ?
C5 N1 Dy1 117.8(3) . . ?
C1 N1 Dy1 125.1(3) . . ?
C1 N1 C5 115.6(4) . . ?
C17 N3 Dy1 120.2(3) . . ?
C23 N4 C19 114.6(8) . . ?
C19A N4 C23A 115.5(8) . . ?
H6b C6 H6a 107.7 . . ?
C3 C6 H6a 108.9(2) . . ?
C3 C6 H6b 108.9(2) . . ?
C12 C6 H6a 108.9(2) 6_443 . ?
C12 C6 H6b 108.9(2) 6_443 . ?
C12 C6 C3 113.5(3) 6_443 . ?
C10 C9 C8 116.3(3) . . ?
C12 C9 C8 121.1(3) . . ?
C12 C9 C10 122.6(3) . . ?
H8 C8 C9 119.9(2) . . ?
C7 C8 C9 120.2(4) . . ?
C7 C8 H8 119.9(2) . . ?
C3 C2 H2 120.3(2) . . ?
C1 C2 H2 120.3(3) . . ?
C1 C2 C3 119.4(4) . . ?
H17 C17 N3 117.5(2) . . ?
C16 C17 N3 125.0(4) . . ?
C16 C17 H17 117.5(3) . . ?
H10 C10 C9 119.9(2) . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10 119.9(2) . . ?
C2 C3 C6 122.8(4) . . ?
C4 C3 C6 121.0(4) . . ?
C4 C3 C2 116.2(4) . . ?
C10 C11 N2 123.2(4) . . ?
H11 C11 N2 118.4(2) . . ?
H11 C11 C10 118.4(2) . . ?
C8 C7 N2 123.5(4) . . ?
H7 C7 N2 118.2(2) . . ?
H7 C7 C8 118.2(2) . . ?
H4 C4 C3 120.0(3) . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 H4 120.0(3) . . ?
C4 C5 N1 124.3(4) . . ?
H5 C5 N1 117.8(2) . . ?
H5 C5 C4 117.8(3) . . ?
C9 C12 C6 113.2(3) . 6_453 ?
H12a C12 C6 108.9(2) . 6_453 ?
H12a C12 C9 108.9(2) . . ?
H12b C12 C6 108.9(2) . 6_453 ?
H12b C12 C9 108.9(2) . . ?
H12b C12 H12a 107.8 . . ?
C2 C1 N1 124.4(5) . . ?
H1 C1 N1 117.8(3) . . ?
H1 C1 C2 117.8(3) . . ?
C15 C16 H16 116.5(7) . . ?
C25 S1 C28 92.5(5) . . ?
C29 C30 H30 124.9(5) . . ?
C31 C30 H30 124.9(5) . . ?
C31 C30 C29 110.1(8) . . ?
C30 C29 S1A 113.7(7) . . ?
H29 C29 S1A 123.2(3) . . ?
H29 C29 C30 123.2(5) . . ?
H31 C31 C30 117.8(5) . . ?
C28 C27 H27 127.3(5) . . ?
C27 C28 S1 113.8(7) . . ?
H28 C28 S1 123.1(4) . . ?
H28 C28 C27 123.1(5) . . ?
H25 C25 S1 129.0(4) . . ?
C31 C26 S1A 100.8(5) . . ?
C25 C26 C27 123.5(6) . . ?
C20 C19 H19 120.1(6) . . ?
C22 C23 H23 116.2(7) . . ?
C24 C21 C22 121.4(10) . . ?
C20 C21 C22 117.7(10) . . ?
C20 C21 C24 120.8(10) . . ?
C21 C22 C23 119.9(11) . . ?
H22 C22 C23 120.1(7) . . ?
H22 C22 C21 120.1(6) . . ?
C21A C22A H22A 120.0(6) . . ?
C23A C22A H22A 120.0(7) . . ?
C23A C22A C21A 120.0(10) . . ?
C20A C21A C22A 116.9(10) . . ?
C24A C21A C22A 122.9(9) . . ?
C24A C21A C20A 120.2(9) . . ?
H23A C23A C22A 120.9(7) . . ?
H20A C20A C21A 120.5(6) . . ?
C19A C20A C21A 119.0(9) . . ?
C19A C20A H20A 120.5(6) . . ?
H19A C19A C20A 115.5(6) . . ?
C24A C24A C21A 126.6(13) 3_565 . ?
H24a C24A C21A 105.7(5) . . ?
H24b C24A C21A 105.7(5) . . ?
H24b C24A H24a 106.133296912(15) . . ?
C21 C20 C19 119.8(9) . . ?
H20 C20 C19 120.1(6) . . ?
H20 C20 C21 120.1(6) . . ?
C14 C13 H13 116.0(8) . . ?
C18 C15 C14 119.9(11) . . ?
C15 C14 C13 119.0(12) . . ?
H14 C14 C13 120.5(8) . . ?
H14 C14 C15 120.5(8) . . ?
C13A C14A H14A 119.2(8) . . ?
C15A C14A H14A 119.2(7) . . ?
C15A C14A C13A 121.7(11) . . ?
H13A C13A C14A 120.9(8) . . ?
C18 C18 C15 96.5(7) 2_554 . ?
H18a C18 C15 112.5(6) . . ?
H18b C18 C15 112.5(6) . . ?
H18b C18 H18a 110.0 . . ?
H18d C18A H18c 106.2 . . ?
C15A C18A H18c 105.7(6) . . ?
C15A C18A H18d 105.7(6) . . ?
C18A C15A C14A 122.3(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_TEST-Kopie
_database_code_depnum_ccdc_archive 'CCDC 1414457'
_audit_update_record             
;
2016-02-22 deposited with the CCDC.
2016-02-25 downloaded from the CCDC.
;
_audit_creation_date             2016-02-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H48 Cl6 Yb2 N8, C8 H7 S2'
_chemical_formula_sum            'C56 H55 Cl6 N8 S2 Yb2'
_chemical_formula_weight         1463.04
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Yb -0.21013 5.79943 28.66410 15.43450 15.30870 2.98963 1.98890 0.25712 10.66470
100.41700 7.56672000885
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   35.641(8)
_cell_length_b                   9.257(2)
_cell_length_c                   18.512(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.781(7)
_cell_angle_gamma                90
_cell_volume                     5747(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9048
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.986
_cell_measurement_theta_min      2.240
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0700 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.8931.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.6908
_exptl_crystal_description       block
_exptl_crystal_F_000             2887.6881
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.152
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41295
_diffrn_reflns_theta_full        28.2902
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.21
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_device_type  ApexII
_diffrn_radiation_type           'Mo K\a'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              44
_reflns_limit_h_min              -47
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5227
_reflns_number_total             7146
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.53A (Bruker, 2008)'
_computing_data_reduction        'SAINT v7.53A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_refine_diff_density_max         1.9613
_refine_diff_density_min         -2.1524
_refine_diff_density_rms         0.2146
_refine_ls_d_res_high            0.7498
_refine_ls_d_res_low             16.7688
_refine_ls_goodness_of_fit_ref   1.0462
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    59
_refine_ls_number_parameters     357
_refine_ls_number_reflns         7146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.0462
_refine_ls_shift/su_max          0.0012
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0239P)²+37.1708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0813
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C23) = Uanis(C22) = Uanis(C21)
3. Others
 Fixed Sof: S1(0.5) C28(0.5) H28(0.5) C26(0.5) H26(0.5) C25(0.5) H25(0.5)
 S1A(0.5) C25A(0.5) H25A(0.5) C28A(0.5) C26A(0.5) H26A(0.5) H27(0.5) H27a(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C18(H18a,H18b), C6(H6a,H6b), C24(H24a,H24b), C12(H12a,H12b)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C13(H13), C23(H23), C7(H7), C11(H11), C2(H2), C14(H14),
 C1(H1), C16(H16), C20(H20), C22(H22), C8(H8), C10(H10), C4(H4), C5(H5),
 C28(H28), C26(H26), C25(H25), C25A(H25A), C26A(H26A), C27(H27), C27(H27a)
;
# start Validation Reply Form
_vrf_PLAT073_TEST-Kopie          
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr Check 
RESPONSE: this is caused by the hydrogen treatment in the refinement using olex.refine and presents an artefact of checkcif
;
_vrf_PLAT411_TEST-Kopie          
;
PROBLEM: Short Inter H...H Contact  H18A   ..  H26A    ..       1.67 Ang.  
RESPONSE: due to the possible disorder of the intercalated thiazole molecule
;
# end Validation Reply Form


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_refinement_flags_posn
_atom_site_disorder_group
Yb1 Yb 0.134879(5) 0.49310(2) 0.385826(9) 0.02318(6) Uani 1.000000 . .
Cl1 Cl 0.08003(3) 0.37415(12) 0.42886(6) 0.0257(2) Uani 1.000000 . .
Cl3 Cl 0.18626(3) 0.63253(15) 0.34440(6) 0.0350(3) Uani 1.000000 . .
Cl2 Cl 0.14434(3) 0.25057(14) 0.32323(6) 0.0334(3) Uani 1.000000 . .
N1 N 0.18654(12) 0.3649(5) 0.4903(2) 0.0351(10) Uani 1.000000 . .
N3 N 0.09186(12) 0.7167(4) 0.36486(19) 0.0288(9) Uani 1.000000 . .
C17 C 0.05296(14) 0.7062(5) 0.3580(2) 0.0309(11) Uani 1.000000 . .
H17 H 0.04334(14) 0.6148(5) 0.3673(2) 0.0371(13) Uiso 1.000000 R .
C19 C 0.09535(16) 0.5999(7) 0.1991(3) 0.0457(15) Uani 1.000000 . .
H19 H 0.11891(16) 0.6568(7) 0.2142(3) 0.0548(18) Uiso 1.000000 R .
N4 N 0.08918(11) 0.5099(5) 0.2516(2) 0.0379(11) Uani 1.000000 . .
C13 C 0.10405(16) 0.8500(6) 0.3537(3) 0.0423(13) Uani 1.000000 . .
H13 H 0.13104(16) 0.8642(6) 0.3575(3) 0.0507(16) Uiso 1.000000 R .
C23 C 0.05606(15) 0.4323(9) 0.2288(3) 0.0662(13) Uani 1.000000 . .
H23 H 0.05123(15) 0.3666(9) 0.2641(3) 0.0794(16) Uiso 1.000000 R .
N2 N 0.15755(10) 0.6388(4) 0.50727(19) 0.0239(8) Uani 1.000000 . .
C7 C 0.18540(14) 0.7413(5) 0.5191(2) 0.0318(11) Uani 1.000000 . .
H7 H 0.19168(14) 0.7758(5) 0.4762(2) 0.0382(13) Uiso 1.000000 R .
C11 C 0.14889(14) 0.5962(6) 0.5686(3) 0.0311(11) Uani 1.000000 . .
H11 H 0.12852(14) 0.5260(6) 0.5616(3) 0.0374(13) Uiso 1.000000 R .
C2 C 0.24960(14) 0.3565(6) 0.5918(3) 0.0401(13) Uani 1.000000 . .
H2 H 0.27615(14) 0.3918(6) 0.6120(3) 0.0481(16) Uiso 1.000000 R .
C3 C 0.23654(13) 0.2527(5) 0.6311(2) 0.0286(10) Uani 1.000000 . .
C14 C 0.07727(16) 0.9711(6) 0.3363(3) 0.0498(16) Uani 1.000000 . .
H14 H 0.08674(16) 1.0659(6) 0.3328(3) 0.060(2) Uiso 1.000000 R .
C1 C 0.22386(14) 0.4094(6) 0.5227(3) 0.0382(13) Uani 1.000000 . .
H1 H 0.23353(14) 0.4818(6) 0.4971(3) 0.0459(15) Uiso 1.000000 R .
C15 C 0.03876(17) 0.9472(6) 0.3250(3) 0.0486(16) Uani 1.000000 . .
C16 C 0.02654(17) 0.8189(6) 0.3387(3) 0.0437(14) Uani 1.000000 . .
H16 H -0.00043(17) 0.8047(6) 0.3351(3) 0.0524(16) Uiso 1.000000 R .
C21 C 0.03458(15) 0.5377(9) 0.1021(3) 0.0662(13) Uani 1.000000 . .
C20 C 0.06923(15) 0.6132(9) 0.1251(3) 0.060(2) Uani 1.000000 . .
H20 H 0.07551(15) 0.6755(9) 0.0900(3) 0.071(2) Uiso 1.000000 R .
C18 C 0.0095(2) 1.0746(6) 0.2948(4) 0.073(3) Uani 1.000000 . .
H18a H -0.0120(2) 1.0686(6) 0.3174(4) 0.088(3) Uiso 1.000000 R .
H18b H 0.0239(2) 1.1667(6) 0.3117(4) 0.088(3) Uiso 1.000000 R .
C22 C 0.02818(16) 0.4427(9) 0.1558(3) 0.0662(13) Uani 1.000000 . .
H22 H 0.00469(16) 0.3854(9) 0.1420(3) 0.0794(16) Uiso 1.000000 R .
C9 C 0.19732(13) 0.7530(5) 0.6542(2) 0.0241(9) Uani 1.000000 . .
C8 C 0.20554(14) 0.7995(5) 0.5904(2) 0.0286(10) Uani 1.000000 . .
H8 H 0.22514(14) 0.8720(5) 0.5955(2) 0.0344(12) Uiso 1.000000 R .
C6 C 0.26226(14) 0.1948(5) 0.7083(2) 0.0311(11) Uani 1.000000 . .
H6a H 0.24592(14) 0.1304(5) 0.7285(2) 0.0373(13) Uiso 1.000000 R .
H6b H 0.28403(14) 0.1361(5) 0.7014(2) 0.0373(13) Uiso 1.000000 R .
C10 C 0.16798(14) 0.6488(6) 0.6425(3) 0.0328(11) Uani 1.000000 . .
H10 H 0.16095(14) 0.6135(6) 0.6844(3) 0.0394(13) Uiso 1.000000 R .
C24 C 0.00356(18) 0.5656(10) 0.0215(3) 0.077(3) Uani 1.000000 . .
H24a H -0.02164(18) 0.6012(10) 0.0265(3) 0.092(3) Uiso 1.000000 R .
H24b H 0.01371(18) 0.6402(10) -0.0055(3) 0.092(3) Uiso 1.000000 R .
C12 C 0.21961(14) 0.8130(5) 0.7329(2) 0.0285(10) Uani 1.000000 . .
H12a H 0.24113(14) 0.8775(5) 0.7296(2) 0.0342(12) Uiso 1.000000 R .
H12b H 0.20111(14) 0.8716(5) 0.7505(2) 0.0342(12) Uiso 1.000000 R .
C4 C 0.19849(16) 0.2011(6) 0.5959(3) 0.0475(15) Uani 1.000000 . .
H4 H 0.18828(16) 0.1270(6) 0.6196(3) 0.0570(19) Uiso 1.000000 R .
C5 C 0.17506(17) 0.2579(6) 0.5257(3) 0.0512(17) Uani 1.000000 . .
H5 H 0.14931(17) 0.2177(6) 0.5016(3) 0.061(2) Uiso 1.000000 R .
S1 S 0.06245(16) 0.8751(5) 0.5455(2) 0.0853(14) Uani 0.500000 . 1
C28 C 0.0864(5) 0.8501(15) 0.6349(9) 0.043(4) Uani 0.500000 . 1
H28 H 0.0848(5) 0.7749(15) 0.6686(9) 0.052(4) Uiso 0.500000 R 1
C26 C 0.1070(4) 1.0811(15) 0.6011(6) 0.057(4) Uani 0.500000 . 1
H26 H 0.1224(4) 1.1671(15) 0.6095(6) 0.069(4) Uiso 0.500000 R 1
C25 C 0.0771(6) 1.0479(15) 0.5378(11) 0.066(5) Uani 0.500000 . 1
H25 H 0.0657(6) 1.1102(15) 0.4952(11) 0.079(6) Uiso 0.500000 R 1
S1A S 0.09819(17) 0.9689(8) 0.5438(3) 0.117(2) Uani 0.500000 . 2
C25A C 0.0498(6) 1.0045(19) 0.5274(9) 0.075(5) Uani 0.500000 . 2
H25A H 0.0308(6) 1.0384(19) 0.4810(9) 0.091(6) Uiso 0.500000 R 2
C28A C 0.0800(9) 0.935(3) 0.6448(10) 0.118(11) Uani 0.500000 . 2
C26A C 0.0439(6) 0.975(3) 0.5926(11) 0.128(10) Uani 0.500000 . 2
H26A H 0.0192(6) 0.981(3) 0.6017(11) 0.154(11) Uiso 0.500000 R 2
C27 C 0.1114(3) 0.9786(11) 0.6483(6) 0.100(3) Uani 1.000000 . .
H27 H 0.1326(3) 0.9858(11) 0.6960(6) 0.120(4) Uiso 0.500000 R 1
H27a H 0.1346(3) 1.0075(11) 0.6892(6) 0.120(4) Uiso 0.500000 R 2


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
Yb1 Cl1 2.5928(12) . ?
Yb1 Cl3 2.5609(13) . ?
Yb1 Cl2 2.6002(13) . ?
Yb1 N1 2.475(4) . ?
Yb1 N3 2.526(4) . ?
Yb1 N4 2.473(3) . ?
Yb1 N2 2.509(3) . ?
N1 C1 1.326(6) . ?
N1 C5 1.327(7) . ?
N3 C17 1.352(6) . ?
N3 C13 1.347(6) . ?
C17 C16 1.369(7) . ?
C19 N4 1.352(7) . ?
C19 C20 1.378(6) . ?
N4 C23 1.323(7) . ?
C13 C14 1.436(8) . ?
C23 C22 1.384(7) . ?
N2 C7 1.336(6) . ?
N2 C11 1.334(6) . ?
C7 C8 1.380(6) . ?
C11 C10 1.393(6) . ?
C2 C3 1.377(7) . ?
C2 C1 1.387(6) . ?
C3 C6 1.511(6) . ?
C3 C4 1.376(7) . ?
C14 C15 1.335(8) . ?
C15 C16 1.318(8) . ?
C15 C18 1.548(8) . ?
C21 C20 1.356(9) . ?
C21 C22 1.403(10) . ?
C21 C24 1.549(8) . ?
C18 C18 1.565(12) 2 ?
C9 C8 1.379(6) . ?
C9 C10 1.385(6) . ?
C9 C12 1.509(5) . ?
C6 C12 1.524(6) 6_546 ?
C24 C24 1.427(16) 3_565 ?
C4 C5 1.389(7) . ?
S1 C28 1.600(16) . ?
S1 C25 1.704(15) . ?
C28 C27 1.46(2) . ?
C26 C25 1.33(2) . ?
C26 C27 1.263(15) . ?
S1A C25A 1.68(2) . ?
S1A C28A 2.20(2) . ?
S1A C27 1.832(11) . ?
C25A C26A 1.32(2) . ?
C28A C26A 1.38(3) . ?
C28A C27 1.17(3) . ?

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
Cl3 Yb1 Cl1 174.85(4) . . ?
Cl2 Yb1 Cl1 89.73(4) . . ?
Cl2 Yb1 Cl3 95.05(4) . . ?
N1 Yb1 Cl1 89.73(11) . . ?
N1 Yb1 Cl3 93.28(11) . . ?
N1 Yb1 Cl2 76.09(9) . . ?
N3 Yb1 Cl1 85.04(10) . . ?
N3 Yb1 Cl3 89.97(10) . . ?
N3 Yb1 Cl2 143.36(8) . . ?
N3 Yb1 N1 139.93(12) . . ?
N4 Yb1 Cl1 91.54(11) . . ?
N4 Yb1 Cl3 87.82(11) . . ?
N4 Yb1 Cl2 75.35(10) . . ?
N4 Yb1 N1 151.40(13) . . ?
N4 Yb1 N3 68.59(12) . . ?
N2 Yb1 Cl1 90.03(9) . . ?
N2 Yb1 Cl3 87.21(9) . . ?
N2 Yb1 Cl2 144.33(8) . . ?
N2 Yb1 N1 68.24(12) . . ?
N2 Yb1 N3 72.06(11) . . ?
N2 Yb1 N4 140.31(13) . . ?
C1 N1 Yb1 124.9(4) . . ?
C5 N1 Yb1 118.1(3) . . ?
C5 N1 C1 116.0(4) . . ?
C17 N3 Yb1 120.4(3) . . ?
C13 N3 Yb1 124.3(3) . . ?
C13 N3 C17 115.1(4) . . ?
C16 C17 N3 124.2(5) . . ?
C20 C19 N4 123.4(6) . . ?
C19 N4 Yb1 123.3(3) . . ?
C23 N4 Yb1 120.0(4) . . ?
C23 N4 C19 116.7(4) . . ?
C14 C13 N3 121.7(5) . . ?
C22 C23 N4 122.8(6) . . ?
C7 N2 Yb1 121.6(3) . . ?
C11 N2 Yb1 120.5(3) . . ?
C11 N2 C7 116.3(4) . . ?
C8 C7 N2 123.4(4) . . ?
C10 C11 N2 123.8(4) . . ?
C1 C2 C3 119.8(5) . . ?
C6 C3 C2 122.8(4) . . ?
C4 C3 C2 116.6(4) . . ?
C4 C3 C6 120.6(5) . . ?
C15 C14 C13 118.4(5) . . ?
C2 C1 N1 123.8(5) . . ?
C16 C15 C14 120.6(6) . . ?
C18 C15 C14 117.5(6) . . ?
C18 C15 C16 122.0(6) . . ?
C15 C16 C17 119.6(6) . . ?
C22 C21 C20 116.8(5) . . ?
C24 C21 C20 119.6(6) . . ?
C24 C21 C22 123.6(6) . . ?
C21 C20 C19 120.2(6) . . ?
C18 C18 C15 112.3(6) 2 . ?
C21 C22 C23 120.0(6) . . ?
C10 C9 C8 116.8(4) . . ?
C12 C9 C8 121.1(4) . . ?
C12 C9 C10 122.0(4) . . ?
C9 C8 C7 120.3(4) . . ?
C12 C6 C3 113.3(4) 6_546 . ?
C9 C10 C11 119.3(4) . . ?
C24 C24 C21 109.2(9) 3_565 . ?
C6 C12 C9 112.5(4) 6_556 . ?
C5 C4 C3 119.7(5) . . ?
C4 C5 N1 123.8(5) . . ?
C25 S1 C28 98.7(9) . . ?
C26 C25 S1 108.7(12) . . ?
C28A S1A C25A 66.5(10) . . ?
C26A C25A S1A 105.5(14) . . ?
C26A C28A S1A 80.7(11) . . ?
C28A C26A C25A 107.2(17) . . ?
C26 C27 C28 124.7(10) . . ?
C28A C27 S1A 91.4(11) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
