# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1415404'
_audit_update_record             
;
2015-07-27 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Ce(hfac)3(BrPyDTDA)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H9 Br2 Ce F18 N6 O6 S4'
_chemical_formula_sum            'C27 H9 Br2 Ce F18 N6 O6 S4'
_chemical_formula_weight         1283.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   16.7572(3)
_cell_length_b                   12.4340(2)
_cell_length_c                   19.4838(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.3502(15)
_cell_angle_gamma                90
_cell_volume                     4058.50(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14482
_cell_measurement_theta_min      9.1140
_cell_measurement_theta_max      75.8100

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_F_000             2460
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    14.137
_shelx_estimated_absorpt_T_min   0.242
_shelx_estimated_absorpt_T_max   0.282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3693
_diffrn_reflns_number            15668
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.439
_diffrn_reflns_theta_max         76.393
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15668
_reflns_number_gt                14216
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were generated using two matrices implying
 pseudomerohedral twinning around [100] direction.
 The ratio of twin components was 0.51:0.49.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component perfect twin using HKLF 5 instruction.
 Restrains were imposed on displacement parameters.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0686P)²+16.0126P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15668
_refine_ls_number_parameters     577
_refine_ls_number_restraints     954
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1486
_refine_ls_wR_factor_gt          0.1445
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.44569(2) 0.77214(3) 0.75172(2) 0.02705(11) Uani 1 1 d . U . . .
C5 C 0.2773(4) 0.6594(6) 0.8442(3) 0.0326(13) Uani 1 1 d . U . . .
C6 C 0.3390(4) 0.6651(6) 0.9000(3) 0.0328(14) Uani 1 1 d . U . . .
C7 C 0.3194(5) 0.6507(8) 0.9676(4) 0.0431(17) Uani 1 1 d . U . . .
H7 H 0.2652 0.6449 0.9802 0.052 Uiso 1 1 calc R U . . .
C8 C 0.3802(5) 0.6449(8) 1.0170(4) 0.0467(18) Uani 1 1 d . U . . .
H8 H 0.3689 0.6352 1.0641 0.056 Uiso 1 1 calc R U . . .
C9 C 0.4576(5) 0.6537(7) 0.9954(4) 0.0419(16) Uani 1 1 d . U . . .
C10 C 0.4726(5) 0.6708(7) 0.9268(4) 0.0403(16) Uani 1 1 d . U . . .
H10 H 0.5264 0.6777 0.9130 0.048 Uiso 1 1 calc R U . . .
C25 C 0.2763(4) 0.8954(6) 0.6584(3) 0.0283(12) Uani 1 1 d . U . . .
C26 C 0.3329(4) 0.8807(6) 0.6012(3) 0.0316(13) Uani 1 1 d . U . . .
C27 C 0.3073(5) 0.8955(8) 0.5339(4) 0.0450(17) Uani 1 1 d . U . . .
H27 H 0.2533 0.9124 0.5228 0.054 Uiso 1 1 calc R U . . .
C28 C 0.3639(6) 0.8845(8) 0.4826(4) 0.0485(19) Uani 1 1 d . U . . .
H28 H 0.3494 0.8923 0.4354 0.058 Uiso 1 1 calc R U . . .
C29 C 0.4408(6) 0.8622(8) 0.5026(4) 0.0503(19) Uani 1 1 d . U . . .
C30 C 0.4620(5) 0.8485(8) 0.5708(4) 0.0487(19) Uani 1 1 d . U . . .
H30 H 0.5160 0.8335 0.5832 0.058 Uiso 1 1 calc R U . . .
C42 C 0.4362(8) 0.9827(8) 0.8705(5) 0.071(3) Uani 1 1 d . U . . .
C43 C 0.4961(10) 1.0443(9) 0.8431(7) 0.086(3) Uani 1 1 d . U . . .
H43 H 0.5172 1.1025 0.8693 0.104 Uiso 1 1 calc R U . . .
C44 C 0.5256(9) 1.0249(10) 0.7808(7) 0.083(3) Uani 1 1 d . U . . .
C46 C 0.3999(10) 1.0173(11) 0.9371(6) 0.089(4) Uani 1 1 d . U . . .
C47 C 0.5932(13) 1.0985(15) 0.7536(10) 0.117(5) Uani 1 1 d . U . . .
C52 C 0.6412(5) 0.7865(11) 0.8141(5) 0.068(3) Uani 1 1 d . U . . .
C53 C 0.6791(5) 0.7743(11) 0.7527(5) 0.076(3) Uani 1 1 d . U . . .
H53 H 0.7358 0.7745 0.7529 0.091 Uiso 1 1 calc R U . . .
C54 C 0.6387(6) 0.7621(11) 0.6915(5) 0.069(3) Uani 1 1 d . U . . .
C56 C 0.6927(7) 0.7999(17) 0.8823(8) 0.097(4) Uani 1 1 d . U . . .
C57 C 0.6860(7) 0.7563(17) 0.6256(7) 0.094(4) Uani 1 1 d . U . . .
C62 C 0.5306(8) 0.5205(9) 0.7280(6) 0.075(3) Uani 1 1 d . U . . .
C63 C 0.4993(9) 0.4980(9) 0.6644(6) 0.078(3) Uani 1 1 d . U . . .
H63 H 0.5217 0.4414 0.6384 0.094 Uiso 1 1 calc R U . . .
C64 C 0.4355(8) 0.5557(9) 0.6368(5) 0.069(3) Uani 1 1 d . U . . .
C66 C 0.5966(11) 0.4467(13) 0.7566(10) 0.106(4) Uani 1 1 d . U . . .
C67 C 0.3953(10) 0.5224(12) 0.5677(6) 0.090(4) Uani 1 1 d . U . . .
N1 N 0.3027(3) 0.6672(5) 0.7790(3) 0.0293(11) Uani 1 1 d . U . . .
N4 N 0.2020(3) 0.6427(5) 0.8593(3) 0.0354(13) Uani 1 1 d . U . . .
N11 N 0.4142(3) 0.6782(5) 0.8790(3) 0.0332(12) Uani 1 1 d . U . . .
N21 N 0.3069(3) 0.8902(5) 0.7225(3) 0.0291(11) Uani 1 1 d . U . . .
N24 N 0.2007(4) 0.9139(6) 0.6441(3) 0.0367(13) Uani 1 1 d . U . . .
N31 N 0.4068(4) 0.8560(6) 0.6203(3) 0.0378(13) Uani 1 1 d . U . . .
O41 O 0.4053(4) 0.8972(5) 0.8442(3) 0.0510(15) Uani 1 1 d . U . . .
O45 O 0.5069(4) 0.9536(5) 0.7389(3) 0.0602(17) Uani 1 1 d . U . . .
O51 O 0.5679(3) 0.7905(6) 0.8247(3) 0.0493(15) Uani 1 1 d . U . . .
O55 O 0.5640(3) 0.7571(6) 0.6809(3) 0.0511(15) Uani 1 1 d . U . . .
O61 O 0.5111(4) 0.5938(5) 0.7680(3) 0.0540(15) Uani 1 1 d . U . . .
O65 O 0.4021(4) 0.6392(5) 0.6624(3) 0.0519(15) Uani 1 1 d . U . . .
F41 F 0.4460(7) 1.0807(7) 0.9747(4) 0.129(4) Uani 1 1 d . U . . .
F42 F 0.3794(8) 0.9348(8) 0.9754(3) 0.135(4) Uani 1 1 d . U . . .
F43 F 0.3325(7) 1.0723(9) 0.9238(4) 0.140(5) Uani 1 1 d . U . . .
F44 F 0.6264(11) 1.1516(14) 0.8019(8) 0.220(9) Uani 1 1 d . U . . .
F45 F 0.5644(13) 1.1710(16) 0.7158(9) 0.250(10) Uani 1 1 d . U . . .
F46 F 0.6438(13) 1.0510(18) 0.7211(15) 0.295(12) Uani 1 1 d . U . . .
F51 F 0.6885(10) 0.8969(17) 0.9037(7) 0.200(7) Uani 1 1 d . U . . .
F52 F 0.6702(5) 0.7375(13) 0.9284(5) 0.180(7) Uani 1 1 d . U . . .
F53 F 0.7692(4) 0.7805(12) 0.8713(5) 0.145(5) Uani 1 1 d . U . . .
F54 F 0.7624(5) 0.7654(12) 0.6344(5) 0.156(6) Uani 1 1 d . U . . .
F55 F 0.6721(10) 0.6754(17) 0.5944(8) 0.230(10) Uani 1 1 d . U . . .
F56 F 0.6673(7) 0.8356(15) 0.5843(6) 0.195(7) Uani 1 1 d . U . . .
F61 F 0.6553(11) 0.5037(15) 0.7818(15) 0.283(11) Uani 1 1 d . U . . .
F62 F 0.5777(10) 0.3938(15) 0.8059(6) 0.205(8) Uani 1 1 d . U . . .
F63 F 0.6282(8) 0.3865(10) 0.7118(6) 0.167(6) Uani 1 1 d . U . . .
F64 F 0.4414(9) 0.4453(9) 0.5378(5) 0.156(5) Uani 1 1 d . U . . .
F65 F 0.3287(7) 0.4724(13) 0.5794(5) 0.180(7) Uani 1 1 d . U . . .
F66 F 0.3877(9) 0.5964(10) 0.5258(5) 0.151(5) Uani 1 1 d . U . . .
S2 S 0.23217(10) 0.64850(14) 0.72053(8) 0.0328(3) Uani 1 1 d . U . . .
S3 S 0.14261(10) 0.62817(17) 0.79228(9) 0.0401(4) Uani 1 1 d . U . . .
S22 S 0.24198(10) 0.91453(14) 0.78213(8) 0.0324(3) Uani 1 1 d . U . . .
S23 S 0.14695(10) 0.93454(16) 0.71220(9) 0.0392(4) Uani 1 1 d . U . . .
Br9 Br 0.54604(6) 0.63890(9) 1.05614(4) 0.0557(3) Uani 1 1 d . U . . .
Br29 Br 0.52405(9) 0.84987(13) 0.43913(6) 0.0876(5) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O55 2.448(5) . ?
Ce1 O51 2.477(6) . ?
Ce1 O41 2.486(5) . ?
Ce1 O61 2.490(5) . ?
Ce1 O45 2.494(6) . ?
Ce1 O65 2.497(6) . ?
Ce1 N1 2.790(5) . ?
Ce1 N21 2.797(5) . ?
Ce1 N11 2.803(5) . ?
Ce1 N31 2.827(6) . ?
C5 N4 1.318(9) . ?
C5 N1 1.353(8) . ?
C5 C6 1.484(10) . ?
C6 N11 1.344(9) . ?
C6 C7 1.376(10) . ?
C7 C8 1.386(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(10) . ?
C9 Br9 1.883(8) . ?
C10 N11 1.337(10) . ?
C10 H10 0.9500 . ?
C25 N24 1.312(9) . ?
C25 N21 1.340(8) . ?
C25 C26 1.492(9) . ?
C26 N31 1.320(9) . ?
C26 C27 1.382(10) . ?
C27 C28 1.401(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.366(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.376(12) . ?
C29 Br29 1.892(8) . ?
C30 N31 1.356(9) . ?
C30 H30 0.9500 . ?
C42 O41 1.284(12) . ?
C42 C43 1.38(2) . ?
C42 C46 1.510(18) . ?
C43 C44 1.34(2) . ?
C43 H43 0.9500 . ?
C44 O45 1.240(14) . ?
C44 C47 1.56(2) . ?
C46 F41 1.315(16) . ?
C46 F42 1.318(18) . ?
C46 F43 1.341(16) . ?
C47 F46 1.22(3) . ?
C47 F45 1.25(2) . ?
C47 F44 1.27(2) . ?
C52 O51 1.251(11) . ?
C52 C53 1.375(15) . ?
C52 C56 1.577(16) . ?
C53 C54 1.366(16) . ?
C53 H53 0.9500 . ?
C54 O55 1.265(11) . ?
C54 C57 1.526(15) . ?
C56 F52 1.252(15) . ?
C56 F51 1.28(3) . ?
C56 F53 1.327(17) . ?
C57 F55 1.20(2) . ?
C57 F54 1.292(16) . ?
C57 F56 1.307(19) . ?
C62 O61 1.249(12) . ?
C62 C63 1.363(19) . ?
C62 C66 1.531(19) . ?
C63 C64 1.386(19) . ?
C63 H63 0.9500 . ?
C64 O65 1.286(12) . ?
C64 C67 1.547(18) . ?
C66 F62 1.214(18) . ?
C66 F63 1.275(17) . ?
C66 F61 1.30(3) . ?
C67 F66 1.236(18) . ?
C67 F65 1.302(15) . ?
C67 F64 1.369(17) . ?
N1 S2 1.639(6) . ?
N4 S3 1.633(6) . ?
N21 S22 1.639(5) . ?
N24 S23 1.641(6) . ?
S2 S3 2.090(2) . ?
S22 S23 2.086(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
O55 Ce1 O51 70.2(2) . . ?
O55 Ce1 O41 133.9(3) . . ?
O51 Ce1 O41 76.2(2) . . ?
O55 Ce1 O61 69.1(2) . . ?
O51 Ce1 O61 69.7(2) . . ?
O41 Ce1 O61 126.3(2) . . ?
O55 Ce1 O45 70.9(3) . . ?
O51 Ce1 O45 68.7(2) . . ?
O41 Ce1 O45 68.0(3) . . ?
O61 Ce1 O45 129.6(2) . . ?
O55 Ce1 O65 77.5(2) . . ?
O51 Ce1 O65 133.3(2) . . ?
O41 Ce1 O65 147.0(2) . . ?
O61 Ce1 O65 67.7(2) . . ?
O45 Ce1 O65 130.0(2) . . ?
O55 Ce1 N1 141.4(2) . . ?
O51 Ce1 N1 129.49(17) . . ?
O41 Ce1 N1 84.5(2) . . ?
O61 Ce1 N1 86.37(19) . . ?
O45 Ce1 N1 143.1(2) . . ?
O65 Ce1 N1 65.47(17) . . ?
O55 Ce1 N21 127.27(17) . . ?
O51 Ce1 N21 137.8(2) . . ?
O41 Ce1 N21 65.16(17) . . ?
O61 Ce1 N21 148.7(2) . . ?
O45 Ce1 N21 81.2(2) . . ?
O65 Ce1 N21 88.7(2) . . ?
N1 Ce1 N21 64.59(17) . . ?
O55 Ce1 N11 129.67(18) . . ?
O51 Ce1 N11 72.59(17) . . ?
O41 Ce1 N11 63.9(2) . . ?
O61 Ce1 N11 66.90(19) . . ?
O45 Ce1 N11 123.5(2) . . ?
O65 Ce1 N11 106.4(2) . . ?
N1 Ce1 N11 57.04(17) . . ?
N21 Ce1 N11 103.06(17) . . ?
O55 Ce1 N31 71.97(18) . . ?
O51 Ce1 N31 131.01(18) . . ?
O41 Ce1 N31 111.38(19) . . ?
O61 Ce1 N31 122.4(2) . . ?
O45 Ce1 N31 70.3(2) . . ?
O65 Ce1 N31 63.6(2) . . ?
N1 Ce1 N31 99.46(18) . . ?
N21 Ce1 N31 56.56(16) . . ?
N11 Ce1 N31 155.65(18) . . ?
N4 C5 N1 123.0(6) . . ?
N4 C5 C6 119.8(6) . . ?
N1 C5 C6 117.1(6) . . ?
N11 C6 C7 123.6(7) . . ?
N11 C6 C5 115.1(6) . . ?
C7 C6 C5 121.2(6) . . ?
C6 C7 C8 118.9(7) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 117.8(7) . . ?
C9 C8 H8 121.1 . . ?
C7 C8 H8 121.1 . . ?
C8 C9 C10 120.0(7) . . ?
C8 C9 Br9 122.3(6) . . ?
C10 C9 Br9 117.7(6) . . ?
N11 C10 C9 122.4(7) . . ?
N11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
N24 C25 N21 123.5(6) . . ?
N24 C25 C26 119.5(6) . . ?
N21 C25 C26 117.0(6) . . ?
N31 C26 C27 124.5(7) . . ?
N31 C26 C25 115.2(6) . . ?
C27 C26 C25 120.3(7) . . ?
C26 C27 C28 117.6(8) . . ?
C26 C27 H27 121.2 . . ?
C28 C27 H27 121.2 . . ?
C29 C28 C27 117.7(7) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 121.1 . . ?
C28 C29 C30 121.4(7) . . ?
C28 C29 Br29 122.3(6) . . ?
C30 C29 Br29 116.3(7) . . ?
N31 C30 C29 120.9(8) . . ?
N31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
O41 C42 C43 126.6(11) . . ?
O41 C42 C46 114.3(13) . . ?
C43 C42 C46 119.1(11) . . ?
C44 C43 C42 122.5(10) . . ?
C44 C43 H43 118.8 . . ?
C42 C43 H43 118.8 . . ?
O45 C44 C43 129.0(12) . . ?
O45 C44 C47 111.7(15) . . ?
C43 C44 C47 119.2(13) . . ?
F41 C46 F42 108.0(9) . . ?
F41 C46 F43 106.4(10) . . ?
F42 C46 F43 106.1(16) . . ?
F41 C46 C42 114.0(15) . . ?
F42 C46 C42 112.3(10) . . ?
F43 C46 C42 109.5(8) . . ?
F46 C47 F45 108(2) . . ?
F46 C47 F44 110(2) . . ?
F45 C47 F44 102.6(18) . . ?
F46 C47 C44 114.3(16) . . ?
F45 C47 C44 110.5(17) . . ?
F44 C47 C44 111.3(18) . . ?
O51 C52 C53 128.6(9) . . ?
O51 C52 C56 112.1(10) . . ?
C53 C52 C56 119.3(9) . . ?
C54 C53 C52 122.8(8) . . ?
C54 C53 H53 118.6 . . ?
C52 C53 H53 118.6 . . ?
O55 C54 C53 128.0(9) . . ?
O55 C54 C57 113.1(10) . . ?
C53 C54 C57 118.8(9) . . ?
F52 C56 F51 109(2) . . ?
F52 C56 F53 108.1(13) . . ?
F51 C56 F53 106.6(15) . . ?
F52 C56 C52 111.8(12) . . ?
F51 C56 C52 110.0(13) . . ?
F53 C56 C52 110.8(14) . . ?
F55 C57 F54 108.7(18) . . ?
F55 C57 F56 106.3(18) . . ?
F54 C57 F56 103.8(14) . . ?
F55 C57 C54 111.7(14) . . ?
F54 C57 C54 114.7(12) . . ?
F56 C57 C54 111.1(14) . . ?
O61 C62 C63 128.1(11) . . ?
O61 C62 C66 114.1(13) . . ?
C63 C62 C66 117.8(11) . . ?
C62 C63 C64 121.6(9) . . ?
C62 C63 H63 119.2 . . ?
C64 C63 H63 119.2 . . ?
O65 C64 C63 127.3(11) . . ?
O65 C64 C67 111.7(12) . . ?
C63 C64 C67 121.0(11) . . ?
F62 C66 F63 110.2(15) . . ?
F62 C66 F61 102(2) . . ?
F63 C66 F61 104.9(18) . . ?
F62 C66 C62 114.3(13) . . ?
F63 C66 C62 114.3(16) . . ?
F61 C66 C62 110.2(14) . . ?
F66 C67 F65 113.3(19) . . ?
F66 C67 F64 106.9(11) . . ?
F65 C67 F64 103.6(12) . . ?
F66 C67 C64 114.3(11) . . ?
F65 C67 C64 109.5(9) . . ?
F64 C67 C64 108.7(15) . . ?
C5 N1 S2 113.9(5) . . ?
C5 N1 Ce1 120.2(4) . . ?
S2 N1 Ce1 122.8(3) . . ?
C5 N4 S3 114.1(5) . . ?
C10 N11 C6 117.2(6) . . ?
C10 N11 Ce1 119.6(4) . . ?
C6 N11 Ce1 121.1(5) . . ?
C25 N21 S22 114.0(5) . . ?
C25 N21 Ce1 120.9(4) . . ?
S22 N21 Ce1 121.0(3) . . ?
C25 N24 S23 113.7(5) . . ?
C26 N31 C30 117.7(6) . . ?
C26 N31 Ce1 122.4(4) . . ?
C30 N31 Ce1 118.2(5) . . ?
C42 O41 Ce1 133.9(8) . . ?
C44 O45 Ce1 132.8(7) . . ?
C52 O51 Ce1 134.7(7) . . ?
C54 O55 Ce1 135.7(6) . . ?
C62 O61 Ce1 133.8(7) . . ?
C64 O65 Ce1 133.0(8) . . ?
N1 S2 S3 94.0(2) . . ?
N4 S3 S2 95.0(2) . . ?
N21 S22 S23 93.9(2) . . ?
N24 S23 S22 94.9(2) . . ?

_refine_diff_density_max         1.549
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.135

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method Sublimation
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1415405'
_audit_update_record             
;
2015-07-27 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Ce(hfac)3(BrPyDTDA)2]*0.5{SbPh3Cl2}'
_chemical_melting_point          ?
_chemical_formula_moiety         
'C27 H9 Br2 Ce F18 N6 O6 S4, 0.5(C18 H15 Cl2 Sb)'
_chemical_formula_sum            'C36 H16.50 Br2 Ce Cl F18 N6 O6 S4 Sb0.50'
_chemical_formula_weight         1495.56

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   36.8971(5)
_cell_length_b                   30.3093(4)
_cell_length_c                   17.87564(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19990.8(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    30666
_cell_measurement_theta_min      2.8370
_cell_measurement_theta_max      30.4490

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_F_000             11504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.112
_shelx_estimated_absorpt_T_min   0.575
_shelx_estimated_absorpt_T_max   0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3693
_diffrn_reflns_number            99135
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.847
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             15221
_reflns_number_gt                13354
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Some restrains were imposed on displacement parameters
 of one of SbPh3Cl2 molecule phenyls
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0675P)²+180.7032P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5929 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.013(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15221
_refine_ls_number_parameters     687
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1275
_refine_ls_wR_factor_gt          0.1189
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.50706(2) 0.73620(2) 0.58314(2) 0.02237(9) Uani 1 1 d . . . . .
C5 C 0.4645(2) 0.7418(3) 0.7654(4) 0.0269(14) Uani 1 1 d . . . . .
C6 C 0.4666(2) 0.7897(3) 0.7486(4) 0.0286(15) Uani 1 1 d . . . . .
C7 C 0.4490(3) 0.8204(3) 0.7932(6) 0.043(2) Uani 1 1 d . . . . .
H7A H 0.4355 0.8116 0.8360 0.052 Uiso 1 1 calc R U . . .
C8 C 0.4518(3) 0.8642(3) 0.7732(6) 0.049(2) Uani 1 1 d . . . . .
H8A H 0.4401 0.8862 0.8024 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4712(3) 0.8757(3) 0.7120(6) 0.047(2) Uani 1 1 d . . . . .
C10 C 0.4885(3) 0.8434(3) 0.6693(5) 0.0382(18) Uani 1 1 d . . . . .
H10A H 0.5023 0.8520 0.6270 0.046 Uiso 1 1 calc R U . . .
C25 C 0.4726(2) 0.7563(2) 0.3966(4) 0.0247(13) Uani 1 1 d . . . . .
C26 C 0.4735(2) 0.7069(2) 0.3961(4) 0.0236(13) Uani 1 1 d . . . . .
C27 C 0.4569(2) 0.6836(3) 0.3383(5) 0.0321(15) Uani 1 1 d . . . . .
H27A H 0.4441 0.6984 0.2997 0.039 Uiso 1 1 calc R U . . .
C28 C 0.4599(3) 0.6385(3) 0.3391(5) 0.0365(17) Uani 1 1 d . . . . .
H28A H 0.4490 0.6212 0.3010 0.044 Uiso 1 1 calc R U . . .
C29 C 0.4790(3) 0.6188(3) 0.3965(5) 0.040(2) Uani 1 1 d . . . . .
C30 C 0.4945(2) 0.6444(3) 0.4513(4) 0.0323(16) Uani 1 1 d . . . . .
H30A H 0.5078 0.6303 0.4901 0.039 Uiso 1 1 calc R U . . .
C42 C 0.5637(2) 0.6532(3) 0.6439(5) 0.0331(16) Uani 1 1 d . . . . .
C43 C 0.5906(3) 0.6785(3) 0.6757(5) 0.0378(18) Uani 1 1 d . . . . .
H43A H 0.6129 0.6650 0.6897 0.045 Uiso 1 1 calc R U . . .
C44 C 0.5858(2) 0.7238(3) 0.6879(4) 0.0306(15) Uani 1 1 d . . . . .
C46 C 0.5710(3) 0.6031(3) 0.6388(6) 0.046(2) Uani 1 1 d . . . . .
C47 C 0.6190(2) 0.7474(3) 0.7223(5) 0.0397(19) Uani 1 1 d . . . . .
C52 C 0.5749(3) 0.8131(3) 0.5444(6) 0.041(2) Uani 1 1 d . . . . .
C53 C 0.6017(3) 0.7840(4) 0.5206(6) 0.045(2) Uani 1 1 d . . . . .
H53A H 0.6259 0.7942 0.5150 0.054 Uiso 1 1 calc R U . . .
C54 C 0.5935(2) 0.7392(3) 0.5046(5) 0.0379(19) Uani 1 1 d . . . . .
C57 C 0.6245(3) 0.7102(5) 0.4761(6) 0.053(3) Uani 1 1 d . . . . .
C62 C 0.4222(2) 0.6816(3) 0.5756(5) 0.0349(16) Uani 1 1 d . . . . .
C63 C 0.3996(3) 0.7166(4) 0.5621(7) 0.050(2) Uani 1 1 d . . . . .
H63A H 0.3745 0.7117 0.5531 0.060 Uiso 1 1 calc R U . . .
C64 C 0.4135(2) 0.7594(3) 0.5615(5) 0.040(2) Uani 1 1 d . . . . .
C66 C 0.4050(3) 0.6349(3) 0.5782(6) 0.044(2) Uani 1 1 d . . . . .
C67 C 0.3879(3) 0.7983(4) 0.5506(10) 0.068(4) Uani 1 1 d . . . . .
N1 N 0.48235(19) 0.7142(2) 0.7213(3) 0.0272(12) Uani 1 1 d . . . . .
N4 N 0.44454(19) 0.7284(2) 0.8234(4) 0.0329(14) Uani 1 1 d . . . . .
N11 N 0.48605(19) 0.8000(2) 0.6869(4) 0.0298(13) Uani 1 1 d . . . . .
N21 N 0.49262(18) 0.7766(2) 0.4492(3) 0.0259(12) Uani 1 1 d . . . . .
N24 N 0.45402(17) 0.7775(2) 0.3445(3) 0.0267(12) Uani 1 1 d . . . . .
N31 N 0.49172(18) 0.6886(2) 0.4523(3) 0.0259(12) Uani 1 1 d . . . . .
O41 O 0.53371(16) 0.66465(18) 0.6200(3) 0.0305(11) Uani 1 1 d . . . . .
O45 O 0.55979(16) 0.74766(19) 0.6713(3) 0.0302(11) Uani 1 1 d . . . . .
O51 O 0.54255(17) 0.80498(19) 0.5579(3) 0.0325(12) Uani 1 1 d . . . . .
O55 O 0.56373(16) 0.7203(2) 0.5111(3) 0.0320(12) Uani 1 1 d . . . . .
O61 O 0.45533(16) 0.68096(19) 0.5855(3) 0.0324(11) Uani 1 1 d . . . . .
O65 O 0.44590(15) 0.77058(19) 0.5689(3) 0.0308(11) Uani 1 1 d . . . . .
F41 F 0.6057(2) 0.5926(2) 0.6431(6) 0.075(2) Uani 1 1 d . . . . .
F42 F 0.5544(3) 0.5825(2) 0.6946(5) 0.079(2) Uani 1 1 d . . . . .
F43 F 0.5586(3) 0.5871(2) 0.5745(5) 0.080(3) Uani 1 1 d . . . . .
F44 F 0.6277(2) 0.7310(3) 0.7889(4) 0.072(2) Uani 1 1 d . . . . .
F45 F 0.64817(18) 0.7435(3) 0.6808(5) 0.070(2) Uani 1 1 d . . . . .
F46 F 0.61311(18) 0.7905(2) 0.7321(5) 0.065(2) Uani 1 1 d . . . . .
F54 F 0.6559(2) 0.7275(5) 0.4818(8) 0.128(5) Uani 1 1 d . . . . .
F55 F 0.6266(4) 0.6737(5) 0.5128(8) 0.161(8) Uani 1 1 d . . . . .
F56 F 0.6199(2) 0.7000(3) 0.4066(4) 0.083(3) Uani 1 1 d . . . . .
F61 F 0.36956(17) 0.6346(2) 0.5691(4) 0.0607(18) Uani 1 1 d . . . . .
F62 F 0.4193(2) 0.6094(2) 0.5236(4) 0.0604(18) Uani 1 1 d . . . . .
F63 F 0.4121(2) 0.6147(2) 0.6431(4) 0.067(2) Uani 1 1 d . . . . .
F64 F 0.3540(2) 0.7873(4) 0.5486(12) 0.170(9) Uani 1 1 d . . . . .
F65 F 0.3916(4) 0.8275(5) 0.6042(10) 0.153(6) Uani 1 1 d . . . . .
F66 F 0.3959(3) 0.8204(4) 0.4906(9) 0.137(5) Uani 1 1 d . . . . .
S2 S 0.47979(6) 0.66201(6) 0.74659(10) 0.0296(4) Uani 1 1 d . . . . .
S3 S 0.44468(6) 0.67476(7) 0.83492(12) 0.0337(4) Uani 1 1 d . . . . .
S22 S 0.49286(6) 0.83038(6) 0.44178(10) 0.0284(4) Uani 1 1 d . . . . .
S23 S 0.45811(6) 0.83116(6) 0.35039(10) 0.0301(4) Uani 1 1 d . . . . .
Br9 Br 0.47611(6) 0.93485(4) 0.68043(10) 0.0860(5) Uani 1 1 d . . . . .
Br29 Br 0.48491(5) 0.55727(3) 0.39791(7) 0.0748(5) Uani 1 1 d . . . . .
C56A C 0.5852(8) 0.8626(10) 0.560(2) 0.061(9) Uani 0.78(2) 1 d . . P A -1
F51A F 0.6196(4) 0.8694(5) 0.5549(13) 0.124(8) Uani 0.78(2) 1 d . . P A -1
F52A F 0.5678(7) 0.8873(4) 0.5169(15) 0.174(13) Uani 0.78(2) 1 d . . P A -1
F53A F 0.5766(5) 0.8741(5) 0.6268(11) 0.122(8) Uani 0.78(2) 1 d . . P A -1
C56B C 0.590(4) 0.859(4) 0.548(6) 0.039(5) Uiso 0.22(2) 1 d . U P A -2
F51B F 0.6042(11) 0.8748(13) 0.489(2) 0.066(9) Uiso 0.22(2) 1 d . U P A -2
F52B F 0.5626(12) 0.8851(15) 0.568(3) 0.066(9) Uiso 0.22(2) 1 d . U P A -2
F53B F 0.6132(12) 0.8627(14) 0.599(2) 0.066(9) Uiso 0.22(2) 1 d . U P A -2
Sb1 Sb 0.5000 0.5000 0.85729(4) 0.02588(14) Uani 1 2 d S T P . .
Cl1 Cl 0.51717(6) 0.42054(6) 0.85666(11) 0.0328(4) Uani 1 1 d . . . . .
C71 C 0.4554(3) 0.4848(3) 0.9258(5) 0.0387(18) Uani 1 1 d . U . . .
C72 C 0.4359(3) 0.4476(4) 0.9195(6) 0.047(2) Uani 1 1 d . U . . .
H72A H 0.4404 0.4279 0.8793 0.057 Uiso 1 1 calc R U . . .
C73 C 0.4088(4) 0.4379(5) 0.9727(8) 0.065(3) Uani 1 1 d . U . . .
H73A H 0.3954 0.4112 0.9687 0.077 Uiso 1 1 calc R U . . .
C74 C 0.4020(5) 0.4654(6) 1.0279(10) 0.089(4) Uani 1 1 d . U . . .
H74A H 0.3823 0.4600 1.0606 0.107 Uiso 1 1 calc R U . . .
C75 C 0.4238(5) 0.5027(6) 1.0384(11) 0.098(5) Uani 1 1 d . U . . .
H75A H 0.4201 0.5212 1.0806 0.117 Uiso 1 1 calc R U . . .
C76 C 0.4507(5) 0.5125(5) 0.9876(9) 0.078(4) Uani 1 1 d . U . . .
H76A H 0.4659 0.5375 0.9945 0.094 Uiso 1 1 calc R U . . .
C81 C 0.5000 0.5000 0.7389(6) 0.028(2) Uani 1 2 d S T P . .
C82 C 0.5258(3) 0.4758(3) 0.7007(6) 0.044(2) Uani 1 1 d . . . . .
H82A H 0.5432 0.4587 0.7271 0.053 Uiso 1 1 calc R U . . .
C83 C 0.5258(5) 0.4768(4) 0.6230(6) 0.070(4) Uani 1 1 d . . . . .
H83A H 0.5439 0.4612 0.5959 0.084 Uiso 1 1 calc R U . . .
C84 C 0.5000 0.5000 0.5860(10) 0.071(6) Uani 1 2 d S T P . .
H84A H 0.5000 0.5000 0.5329 0.086 Uiso 1 2 calc R U P . .


_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
Ce1 O41 2.470(5) . ?
Ce1 O65 2.499(5) . ?
Ce1 O55 2.502(6) . ?
Ce1 O51 2.503(6) . ?
Ce1 O45 2.528(6) . ?
Ce1 O61 2.539(6) . ?
Ce1 N1 2.716(6) . ?
Ce1 N21 2.741(6) . ?
Ce1 N11 2.791(7) . ?
Ce1 N31 2.805(6) . ?
C5 N1 1.326(10) . ?
C5 N4 1.335(10) . ?
C5 C6 1.482(11) . ?
C6 N11 1.352(10) . ?
C6 C7 1.388(12) . ?
C7 C8 1.378(15) . ?
C7 H7A 0.9500 . ?
C8 C9 1.354(16) . ?
C8 H8A 0.9500 . ?
C9 C10 1.397(13) . ?
C9 Br9 1.887(10) . ?
C10 N11 1.353(11) . ?
C10 H10A 0.9500 . ?
C25 N24 1.324(9) . ?
C25 N21 1.343(9) . ?
C25 C26 1.499(9) . ?
C26 N31 1.330(9) . ?
C26 C27 1.393(10) . ?
C27 C28 1.370(12) . ?
C27 H27A 0.9500 . ?
C28 C29 1.381(13) . ?
C28 H28A 0.9500 . ?
C29 C30 1.375(12) . ?
C29 Br29 1.878(9) . ?
C30 N31 1.344(10) . ?
C30 H30A 0.9500 . ?
C42 O41 1.235(10) . ?
C42 C43 1.379(13) . ?
C42 C46 1.545(12) . ?
C43 C44 1.402(12) . ?
C43 H43A 0.9500 . ?
C44 O45 1.236(10) . ?
C44 C47 1.546(12) . ?
C46 F41 1.322(12) . ?
C46 F42 1.325(14) . ?
C46 F43 1.329(13) . ?
C47 F45 1.315(12) . ?
C47 F44 1.329(12) . ?
C47 F46 1.334(12) . ?
C52 O51 1.241(11) . ?
C52 C53 1.393(15) . ?
C52 C56B 1.49(14) . ?
C52 C56A 1.57(3) . ?
C53 C54 1.420(15) . ?
C53 H53A 0.9500 . ?
C54 O55 1.245(11) . ?
C54 C57 1.528(14) . ?
C57 F54 1.275(15) . ?
C57 F55 1.289(16) . ?
C57 F56 1.290(13) . ?
C62 O61 1.237(10) . ?
C62 C63 1.370(14) . ?
C62 C66 1.552(12) . ?
C63 C64 1.397(15) . ?
C63 H63A 0.9500 . ?
C64 O65 1.249(10) . ?
C64 C67 1.522(15) . ?
C66 F61 1.317(11) . ?
C66 F63 1.337(13) . ?
C66 F62 1.352(12) . ?
C67 F64 1.293(16) . ?
C67 F66 1.298(19) . ?
C67 F65 1.31(2) . ?
N1 S2 1.648(7) . ?
N4 S3 1.640(7) . ?
N21 S22 1.637(6) . ?
N24 S23 1.637(7) . ?
S2 S3 2.079(3) . ?
S22 S23 2.077(3) . ?
C56A F52A 1.25(4) . ?
C56A F53A 1.28(3) . ?
C56A F51A 1.29(4) . ?
C56B F53B 1.26(14) . ?
C56B F51B 1.28(12) . ?
C56B F52B 1.34(12) . ?
Sb1 C71 2.104(9) . ?
Sb1 C71 2.104(9) 2_665 ?
Sb1 C81 2.116(11) . ?
Sb1 Cl1 2.4904(17) . ?
Sb1 Cl1 2.4904(17) 2_665 ?
C71 C72 1.341(14) . ?
C71 C76 1.397(16) . ?
C72 C73 1.411(16) . ?
C72 H72A 0.9500 . ?
C73 C74 1.32(2) . ?
C73 H73A 0.9500 . ?
C74 C75 1.40(2) . ?
C74 H74A 0.9500 . ?
C75 C76 1.378(19) . ?
C75 H75A 0.9500 . ?
C76 H76A 0.9500 . ?
C81 C82 1.383(11) . ?
C81 C82 1.383(11) 2_665 ?
C82 C83 1.389(15) . ?
C82 H82A 0.9500 . ?
C83 C84 1.357(17) . ?
C83 H83A 0.9500 . ?
C84 C83 1.357(17) 2_665 ?
C84 H84A 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
O41 Ce1 O65 138.82(19) . . ?
O41 Ce1 O55 68.63(19) . . ?
O65 Ce1 O55 141.51(18) . . ?
O41 Ce1 O51 124.82(19) . . ?
O65 Ce1 O51 96.13(19) . . ?
O55 Ce1 O51 68.3(2) . . ?
O41 Ce1 O45 69.40(18) . . ?
O65 Ce1 O45 134.53(18) . . ?
O55 Ce1 O45 72.79(19) . . ?
O51 Ce1 O45 66.13(18) . . ?
O41 Ce1 O61 73.50(19) . . ?
O65 Ce1 O61 66.28(19) . . ?
O55 Ce1 O61 120.7(2) . . ?
O51 Ce1 O61 160.99(19) . . ?
O45 Ce1 O61 131.19(19) . . ?
O41 Ce1 N1 71.08(19) . . ?
O65 Ce1 N1 83.78(19) . . ?
O55 Ce1 N1 134.5(2) . . ?
O51 Ce1 N1 122.96(19) . . ?
O45 Ce1 N1 74.0(2) . . ?
O61 Ce1 N1 64.56(19) . . ?
O41 Ce1 N21 134.59(19) . . ?
O65 Ce1 N21 63.22(19) . . ?
O55 Ce1 N21 78.41(19) . . ?
O51 Ce1 N21 64.69(18) . . ?
O45 Ce1 N21 129.27(19) . . ?
O61 Ce1 N21 99.37(19) . . ?
N1 Ce1 N21 147.0(2) . . ?
O41 Ce1 N11 122.82(19) . . ?
O65 Ce1 N11 61.80(19) . . ?
O55 Ce1 N11 135.0(2) . . ?
O51 Ce1 N11 71.8(2) . . ?
O45 Ce1 N11 72.78(19) . . ?
O61 Ce1 N11 103.7(2) . . ?
N1 Ce1 N11 58.15(19) . . ?
N21 Ce1 N11 102.55(19) . . ?
O41 Ce1 N31 81.45(18) . . ?
O65 Ce1 N31 86.97(19) . . ?
O55 Ce1 N31 68.95(19) . . ?
O51 Ce1 N31 112.55(19) . . ?
O45 Ce1 N31 138.23(18) . . ?
O61 Ce1 N31 61.54(19) . . ?
N1 Ce1 N31 124.35(19) . . ?
N21 Ce1 N31 57.44(18) . . ?
N11 Ce1 N31 148.71(19) . . ?
N1 C5 N4 122.9(7) . . ?
N1 C5 C6 118.1(7) . . ?
N4 C5 C6 118.9(7) . . ?
N11 C6 C7 124.1(8) . . ?
N11 C6 C5 114.9(7) . . ?
C7 C6 C5 121.1(8) . . ?
C8 C7 C6 117.6(9) . . ?
C8 C7 H7A 121.2 . . ?
C6 C7 H7A 121.2 . . ?
C9 C8 C7 119.8(9) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 120.1(9) . . ?
C8 C9 Br9 122.5(7) . . ?
C10 C9 Br9 117.4(8) . . ?
N11 C10 C9 121.6(9) . . ?
N11 C10 H10A 119.2 . . ?
C9 C10 H10A 119.2 . . ?
N24 C25 N21 123.8(6) . . ?
N24 C25 C26 119.4(6) . . ?
N21 C25 C26 116.7(6) . . ?
N31 C26 C27 124.8(7) . . ?
N31 C26 C25 115.0(6) . . ?
C27 C26 C25 120.2(6) . . ?
C28 C27 C26 117.6(7) . . ?
C28 C27 H27A 121.2 . . ?
C26 C27 H27A 121.2 . . ?
C27 C28 C29 118.7(7) . . ?
C27 C28 H28A 120.7 . . ?
C29 C28 H28A 120.7 . . ?
C30 C29 C28 119.8(8) . . ?
C30 C29 Br29 120.2(7) . . ?
C28 C29 Br29 119.9(7) . . ?
N31 C30 C29 122.7(8) . . ?
N31 C30 H30A 118.7 . . ?
C29 C30 H30A 118.7 . . ?
O41 C42 C43 129.2(8) . . ?
O41 C42 C46 114.3(8) . . ?
C43 C42 C46 116.5(8) . . ?
C42 C43 C44 121.1(8) . . ?
C42 C43 H43A 119.4 . . ?
C44 C43 H43A 119.4 . . ?
O45 C44 C43 129.3(8) . . ?
O45 C44 C47 116.1(8) . . ?
C43 C44 C47 114.4(7) . . ?
F41 C46 F42 107.0(9) . . ?
F41 C46 F43 107.2(10) . . ?
F42 C46 F43 108.6(10) . . ?
F41 C46 C42 113.7(9) . . ?
F42 C46 C42 109.8(9) . . ?
F43 C46 C42 110.5(8) . . ?
F45 C47 F44 105.8(8) . . ?
F45 C47 F46 107.1(9) . . ?
F44 C47 F46 106.8(9) . . ?
F45 C47 C44 112.5(8) . . ?
F44 C47 C44 112.0(8) . . ?
F46 C47 C44 112.1(7) . . ?
O51 C52 C53 128.1(9) . . ?
O51 C52 C56B 122(5) . . ?
C53 C52 C56B 109(5) . . ?
O51 C52 C56A 112.8(13) . . ?
C53 C52 C56A 119.1(13) . . ?
C52 C53 C54 121.1(8) . . ?
C52 C53 H53A 119.4 . . ?
C54 C53 H53A 119.4 . . ?
O55 C54 C53 127.4(9) . . ?
O55 C54 C57 115.4(9) . . ?
C53 C54 C57 117.3(9) . . ?
F54 C57 F55 104.9(13) . . ?
F54 C57 F56 107.2(11) . . ?
F55 C57 F56 107.0(14) . . ?
F54 C57 C54 114.6(11) . . ?
F55 C57 C54 111.6(9) . . ?
F56 C57 C54 111.1(9) . . ?
O61 C62 C63 129.7(8) . . ?
O61 C62 C66 112.7(8) . . ?
C63 C62 C66 117.6(8) . . ?
C62 C63 C64 119.8(8) . . ?
C62 C63 H63A 120.1 . . ?
C64 C63 H63A 120.1 . . ?
O65 C64 C63 127.1(9) . . ?
O65 C64 C67 113.5(9) . . ?
C63 C64 C67 119.5(9) . . ?
F61 C66 F63 107.3(8) . . ?
F61 C66 F62 107.2(8) . . ?
F63 C66 F62 106.9(9) . . ?
F61 C66 C62 114.0(9) . . ?
F63 C66 C62 111.2(8) . . ?
F62 C66 C62 109.9(7) . . ?
F64 C67 F66 109.4(15) . . ?
F64 C67 F65 107.0(15) . . ?
F66 C67 F65 103.4(15) . . ?
F64 C67 C64 113.8(11) . . ?
F66 C67 C64 111.3(12) . . ?
F65 C67 C64 111.3(12) . . ?
C5 N1 S2 114.5(6) . . ?
C5 N1 Ce1 123.5(5) . . ?
S2 N1 Ce1 120.3(3) . . ?
C5 N4 S3 113.4(6) . . ?
C6 N11 C10 116.8(7) . . ?
C6 N11 Ce1 121.9(5) . . ?
C10 N11 Ce1 120.0(5) . . ?
C25 N21 S22 113.7(5) . . ?
C25 N21 Ce1 121.0(4) . . ?
S22 N21 Ce1 121.0(3) . . ?
C25 N24 S23 112.9(5) . . ?
C26 N31 C30 116.4(6) . . ?
C26 N31 Ce1 121.2(5) . . ?
C30 N31 Ce1 120.5(5) . . ?
C42 O41 Ce1 134.0(5) . . ?
C44 O45 Ce1 131.8(5) . . ?
C52 O51 Ce1 134.6(6) . . ?
C54 O55 Ce1 134.3(6) . . ?
C62 O61 Ce1 137.0(6) . . ?
C64 O65 Ce1 139.7(6) . . ?
N1 S2 S3 93.8(3) . . ?
N4 S3 S2 95.2(3) . . ?
N21 S22 S23 94.1(2) . . ?
N24 S23 S22 95.5(2) . . ?
F52A C56A F53A 106(3) . . ?
F52A C56A F51A 112(3) . . ?
F53A C56A F51A 105(3) . . ?
F52A C56A C52 110(2) . . ?
F53A C56A C52 111(2) . . ?
F51A C56A C52 112(2) . . ?
F53B C56B F51B 107(10) . . ?
F53B C56B F52B 105(9) . . ?
F51B C56B F52B 107(9) . . ?
F53B C56B C52 112(9) . . ?
F51B C56B C52 118(9) . . ?
F52B C56B C52 106(9) . . ?
C71 Sb1 C71 108.8(6) . 2_665 ?
C71 Sb1 C81 125.6(3) . . ?
C71 Sb1 C81 125.6(3) 2_665 . ?
C71 Sb1 Cl1 89.5(2) . . ?
C71 Sb1 Cl1 90.8(2) 2_665 . ?
C81 Sb1 Cl1 89.74(5) . . ?
C71 Sb1 Cl1 90.8(2) . 2_665 ?
C71 Sb1 Cl1 89.5(2) 2_665 2_665 ?
C81 Sb1 Cl1 89.74(5) . 2_665 ?
Cl1 Sb1 Cl1 179.49(10) . 2_665 ?
C72 C71 C76 120.3(10) . . ?
C72 C71 Sb1 123.6(8) . . ?
C76 C71 Sb1 115.2(8) . . ?
C71 C72 C73 119.9(11) . . ?
C71 C72 H72A 120.0 . . ?
C73 C72 H72A 120.0 . . ?
C74 C73 C72 120.4(13) . . ?
C74 C73 H73A 119.8 . . ?
C72 C73 H73A 119.8 . . ?
C73 C74 C75 120.3(13) . . ?
C73 C74 H74A 119.9 . . ?
C75 C74 H74A 119.9 . . ?
C76 C75 C74 119.9(15) . . ?
C76 C75 H75A 120.1 . . ?
C74 C75 H75A 120.1 . . ?
C75 C76 C71 118.7(14) . . ?
C75 C76 H76A 120.6 . . ?
C71 C76 H76A 120.6 . . ?
C82 C81 C82 120.8(12) . 2_665 ?
C82 C81 Sb1 119.6(6) . . ?
C82 C81 Sb1 119.6(6) 2_665 . ?
C81 C82 C83 118.8(10) . . ?
C81 C82 H82A 120.6 . . ?
C83 C82 H82A 120.6 . . ?
C84 C83 C82 119.9(12) . . ?
C84 C83 H83A 120.0 . . ?
C82 C83 H83A 120.0 . . ?
C83 C84 C83 121.6(16) 2_665 . ?
C83 C84 H84A 119.2 2_665 . ?
C83 C84 H84A 119.2 . . ?

_refine_diff_density_max         5.159
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.144

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method Sublimation
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
