# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Emily091116_0m
_database_code_depnum_ccdc_archive 'CCDC 1523760'
_audit_update_record             
;
2016-12-20 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
_audit_creation_date             2016-12-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_chemical_formula_moiety         'C56 H36 Ce N4 O4, O, 0.5(C6)'
_chemical_formula_sum            'C59 H36 Ce N4 O5'
_chemical_formula_weight         1021.08
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
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'
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'
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'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'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'

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

_symmetry_Int_Tables_number      14
_cell_length_a                   13.0103(8)
_cell_length_b                   13.9521(8)
_cell_length_c                   26.1970(15)
_cell_angle_alpha                90
_cell_angle_beta                 99.6888(12)
_cell_angle_gamma                90
_cell_volume                     4687.5(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      28.217
_cell_measurement_theta_min      2.203
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0959 before and 0.0417 after correction. The Ratio of minimum to maximum transmission is 0.8156. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orangish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.4468
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064.4438
_exptl_crystal_preparation       
'slow diffusion of hexanes into a concentration solution in toluene'
_exptl_crystal_recrystallization_method 
'slow diffusion of hexanes into a concentration solution in toluene'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61172
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.58
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -12
_reflns_number_gt                8118
_reflns_number_total             9966
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.7761
_refine_diff_density_min         -0.6007
_refine_diff_density_rms         0.1251
_refine_ls_d_res_high            0.7900
_refine_ls_d_res_low             12.9117
_refine_ls_goodness_of_fit_ref   1.0683
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9966
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0292
_refine_ls_restrained_S_all      1.0683
_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)+(0.0370P)²+3.6257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0769
_olex2_refinement_description    
;
;
_atom_sites_solution_primary     direct
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 0.131850(10) 0.092477(10) 0.175727(5) 0.01696(5) Uani 1.000000 .
O1 O 0.21530(13) 0.16364(12) 0.24526(6) 0.0205(4) Uani 1.000000 .
O2 O 0.02188(13) 0.21579(13) 0.17769(7) 0.0226(4) Uani 1.000000 .
N4 N 0.04728(16) 0.01129(14) 0.24392(8) 0.0193(4) Uani 1.000000 .
C39 C 0.29885(19) -0.10635(17) 0.21304(10) 0.0194(5) Uani 1.000000 .
H39 H 0.32725(19) -0.15291(17) 0.23793(10) 0.0232(6) Uiso 1.000000 R
O4 O -0.02109(14) 0.02857(13) 0.13910(7) 0.0253(4) Uani 1.000000 .
N1 N 0.29699(16) 0.17615(15) 0.15624(8) 0.0197(5) Uani 1.000000 .
N2 N 0.11301(16) 0.18726(15) 0.09275(8) 0.0193(4) Uani 1.000000 .
O3 O 0.19493(14) -0.00805(12) 0.12348(7) 0.0229(4) Uani 1.000000 .
N3 N 0.23562(16) -0.04376(15) 0.22745(8) 0.0187(4) Uani 1.000000 .
C46 C -0.05200(19) 0.00037(18) 0.24342(10) 0.0210(5) Uani 1.000000 .
H46 H -0.07200(19) -0.02532(18) 0.27387(10) 0.0252(6) Uiso 1.000000 R
C9 C 0.4885(2) 0.24323(17) 0.27248(10) 0.0216(5) Uani 1.000000 .
C11 C 0.37384(19) 0.21430(18) 0.18787(10) 0.0214(5) Uani 1.000000 .
H11 H 0.42551(19) 0.24629(18) 0.17256(10) 0.0256(7) Uiso 1.000000 R
C19 C -0.0626(2) 0.24911(18) 0.09126(10) 0.0214(5) Uani 1.000000 .
C53 C -0.3244(2) 0.02607(19) 0.16880(12) 0.0294(6) Uani 1.000000 .
C29 C 0.2767(2) -0.06166(18) 0.12033(10) 0.0206(5) Uani 1.000000 .
C8 C 0.5785(2) 0.25900(18) 0.25009(11) 0.0260(6) Uani 1.000000 .
H8 H 0.5748(2) 0.25091(18) 0.21382(11) 0.0312(7) Uiso 1.000000 R
C20 C -0.1563(2) 0.28232(19) 0.05780(11) 0.0256(6) Uani 1.000000 .
C37 C 0.41491(19) -0.17529(17) 0.15557(10) 0.0200(5) Uani 1.000000 .
C12 C 0.2995(2) 0.18157(19) 0.10217(10) 0.0222(6) Uani 1.000000 .
C40 C 0.2174(2) -0.04835(18) 0.27946(10) 0.0203(5) Uani 1.000000 .
C10 C 0.38900(19) 0.21331(17) 0.24327(9) 0.0190(5) Uani 1.000000 .
C45 C 0.11838(19) -0.01874(18) 0.28812(10) 0.0206(5) Uani 1.000000 .
C56 C -0.1155(2) 0.03011(18) 0.15060(11) 0.0247(6) Uani 1.000000 .
C47 C -0.13484(19) 0.02317(18) 0.20151(10) 0.0217(5) Uani 1.000000 .
C17 C 0.2031(2) 0.18381(18) 0.06854(10) 0.0218(6) Uani 1.000000 .
C35 C 0.5527(2) -0.2890(2) 0.18743(11) 0.0277(6) Uani 1.000000 .
H35 H 0.5906(2) -0.3245(2) 0.21538(11) 0.0332(7) Uiso 1.000000 R
C42 C 0.2694(2) -0.0761(2) 0.37097(11) 0.0306(7) Uani 1.000000 .
H42 H 0.3205(2) -0.0964(2) 0.39916(11) 0.0367(8) Uiso 1.000000 R
C18 C 0.03001(19) 0.23054(18) 0.06962(10) 0.0217(5) Uani 1.000000 .
H18 H 0.03030(19) 0.25198(18) 0.03523(10) 0.0260(7) Uiso 1.000000 R
C38 C 0.33009(19) -0.11188(17) 0.16283(10) 0.0187(5) Uani 1.000000 .
C16 C 0.1999(2) 0.1792(2) 0.01519(10) 0.0285(6) Uani 1.000000 .
H16 H 0.1348(2) 0.1787(2) -0.00751(10) 0.0342(7) Uiso 1.000000 R
C32 C 0.4439(2) -0.18273(19) 0.10582(10) 0.0254(6) Uani 1.000000 .
C52 C -0.4287(2) 0.0219(2) 0.17809(14) 0.0365(7) Uani 1.000000 .
H52 H -0.4845(2) 0.0225(2) 0.14959(14) 0.0438(9) Uiso 1.000000 R
C43 C 0.1721(2) -0.0462(2) 0.37977(11) 0.0314(7) Uani 1.000000 .
H43 H 0.1568(2) -0.0459(2) 0.41397(11) 0.0377(8) Uiso 1.000000 R
C34 C 0.5788(2) -0.2974(2) 0.13792(11) 0.0293(6) Uani 1.000000 .
H34 H 0.6331(2) -0.3393(2) 0.13202(11) 0.0351(8) Uiso 1.000000 R
C4 C 0.4988(2) 0.25418(19) 0.32723(11) 0.0246(6) Uani 1.000000 .
C1 C 0.30725(19) 0.18894(17) 0.27000(10) 0.0193(5) Uani 1.000000 .
C31 C 0.3890(2) -0.1274(2) 0.06462(11) 0.0328(7) Uani 1.000000 .
H31 H 0.4089(2) -0.1314(2) 0.03141(11) 0.0393(8) Uiso 1.000000 R
C44 C 0.0976(2) -0.01692(19) 0.33876(10) 0.0265(6) Uani 1.000000 .
H44 H 0.0316(2) 0.00466(19) 0.34505(10) 0.0318(7) Uiso 1.000000 R
C36 C 0.4729(2) -0.22996(19) 0.19597(11) 0.0244(6) Uani 1.000000 .
H36 H 0.4561(2) -0.22572(19) 0.22982(11) 0.0293(7) Uiso 1.000000 R
C48 C -0.2409(2) 0.02311(18) 0.21129(11) 0.0250(6) Uani 1.000000 .
C21 C -0.1670(2) 0.2843(2) 0.00335(11) 0.0342(7) Uani 1.000000 .
H21 H -0.1123(2) 0.2604(2) -0.01294(11) 0.0411(8) Uiso 1.000000 R
C25 C -0.2421(2) 0.3140(2) 0.08064(12) 0.0321(7) Uani 1.000000 .
C6 C 0.6792(2) 0.3009(2) 0.33291(12) 0.0327(7) Uani 1.000000 .
H6 H 0.7429(2) 0.3222(2) 0.35283(12) 0.0392(8) Uiso 1.000000 R
C5 C 0.5945(2) 0.2847(2) 0.35597(11) 0.0311(6) Uani 1.000000 .
H5 H 0.6001(2) 0.2942(2) 0.39224(11) 0.0373(8) Uiso 1.000000 R
C30 C 0.3090(2) -0.0690(2) 0.07122(11) 0.0303(7) Uani 1.000000 .
H30 H 0.2742(2) -0.0328(2) 0.04281(11) 0.0364(8) Uiso 1.000000 R
C28 C -0.0597(2) 0.24602(18) 0.14520(10) 0.0219(6) Uani 1.000000 .
C33 C 0.5257(2) -0.2450(2) 0.09845(12) 0.0312(7) Uani 1.000000 .
H33 H 0.5441(2) -0.2504(2) 0.06497(12) 0.0374(8) Uiso 1.000000 R
C14 C 0.3874(2) 0.1757(2) 0.02828(12) 0.0396(8) Uani 1.000000 .
H14 H 0.4502(2) 0.1746(2) 0.01435(12) 0.0475(9) Uiso 1.000000 R
C27 C -0.1472(2) 0.2805(2) 0.16614(11) 0.0321(7) Uani 1.000000 .
H27 H -0.1443(2) 0.2814(2) 0.20262(11) 0.0386(8) Uiso 1.000000 R
C41 C 0.2920(2) -0.07647(19) 0.32119(11) 0.0264(6) Uani 1.000000 .
H41 H 0.3591(2) -0.09608(19) 0.31549(11) 0.0316(7) Uiso 1.000000 R
C54 C -0.3012(2) 0.0320(2) 0.11788(12) 0.0350(7) Uani 1.000000 .
H54 H -0.3570(2) 0.0344(2) 0.08940(12) 0.0421(8) Uiso 1.000000 R
C3 C 0.4123(2) 0.2301(2) 0.35169(11) 0.0288(6) Uani 1.000000 .
H3 H 0.4185(2) 0.2378(2) 0.38812(11) 0.0345(7) Uiso 1.000000 R
C51 C -0.4502(2) 0.0171(2) 0.22725(14) 0.0396(8) Uani 1.000000 .
H51 H -0.5204(2) 0.0135(2) 0.23279(14) 0.0475(9) Uiso 1.000000 R
C15 C 0.2917(2) 0.1754(2) -0.00469(11) 0.0366(7) Uani 1.000000 .
H15 H 0.2894(2) 0.1726(2) -0.04110(11) 0.0439(9) Uiso 1.000000 R
C7 C 0.6715(2) 0.2858(2) 0.27974(12) 0.0301(6) Uani 1.000000 .
H7 H 0.7313(2) 0.2942(2) 0.26381(12) 0.0361(8) Uiso 1.000000 R
C50 C -0.3690(2) 0.0174(2) 0.26916(13) 0.0356(7) Uani 1.000000 .
H50 H -0.3841(2) 0.0155(2) 0.30339(13) 0.0428(9) Uiso 1.000000 R
C23 C -0.3382(3) 0.3541(3) -0.00403(14) 0.0485(9) Uani 1.000000 .
H23 H -0.3983(3) 0.3800(3) -0.02510(14) 0.0582(11) Uiso 1.000000 R
C26 C -0.2341(2) 0.3119(2) 0.13492(12) 0.0371(7) Uani 1.000000 .
H26 H -0.2914(2) 0.3333(2) 0.15006(12) 0.0445(9) Uiso 1.000000 R
C55 C -0.2020(2) 0.0344(2) 0.10869(12) 0.0324(7) Uani 1.000000 .
H55 H -0.1894(2) 0.0390(2) 0.07409(12) 0.0389(8) Uiso 1.000000 R
C13 C 0.3911(2) 0.1774(2) 0.08146(11) 0.0309(7) Uani 1.000000 .
H13 H 0.4565(2) 0.1758(2) 0.10389(11) 0.0371(8) Uiso 1.000000 R
C49 C -0.2668(2) 0.0203(2) 0.26154(12) 0.0300(6) Uani 1.000000 .
H49 H -0.2125(2) 0.0204(2) 0.29074(12) 0.0360(8) Uiso 1.000000 R
C22 C -0.2555(3) 0.3205(3) -0.02645(13) 0.0456(8) Uani 1.000000 .
H22 H -0.2603(3) 0.3226(3) -0.06303(13) 0.0548(10) Uiso 1.000000 R
C24 C -0.3325(2) 0.3495(2) 0.04833(14) 0.0425(8) Uani 1.000000 .
H24 H -0.3901(2) 0.3705(2) 0.06343(14) 0.0510(10) Uiso 1.000000 R
C2 C 0.3217(2) 0.19681(19) 0.32464(10) 0.0246(6) Uani 1.000000 .
H2 H 0.2670(2) 0.17843(19) 0.34250(10) 0.0295(7) Uiso 1.000000 R
O5s O -0.0207(2) 0.0742(2) -0.04124(11) 0.0760(9) Uani 1.000000 .
C59s C 0.5082(7) 0.0060(5) 0.4725(3) 0.164(6) Uani 1.000000 .
C58s C 0.6109(7) 0.0503(6) 0.4711(4) 0.164(4) Uani 1.000000 .
C57s C 0.6480(10) 0.0598(6) 0.4228(3) 0.209(6) Uani 1.000000 .


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 O1 2.1948(17) . ?
Ce1 O2 2.2437(17) . ?
Ce1 N4 2.519(2) . ?
Ce1 O4 2.2433(17) . ?
Ce1 N1 2.571(2) . ?
Ce1 N2 2.521(2) . ?
Ce1 O3 2.2117(17) . ?
Ce1 N3 2.580(2) . ?
Ce1 C56 3.291(3) . ?
Ce1 C28 3.281(3) . ?
O1 C1 1.309(3) . ?
O2 C28 1.313(3) . ?
N4 C46 1.299(3) . ?
N4 C45 1.418(3) . ?
C39 N3 1.299(3) . ?
C39 C38 1.443(3) . ?
O4 C56 1.313(3) . ?
N1 C11 1.300(3) . ?
N1 C12 1.424(3) . ?
N2 C17 1.424(3) . ?
N2 C18 1.295(3) . ?
O3 C29 1.315(3) . ?
N3 C40 1.423(3) . ?
C46 C47 1.439(4) . ?
C9 C8 1.413(4) . ?
C9 C10 1.450(3) . ?
C9 C4 1.426(4) . ?
C11 C10 1.431(3) . ?
C19 C20 1.452(4) . ?
C19 C18 1.439(4) . ?
C19 C28 1.408(4) . ?
C53 C52 1.418(4) . ?
C53 C48 1.419(4) . ?
C53 C54 1.419(4) . ?
C29 C38 1.397(4) . ?
C29 C30 1.423(4) . ?
C8 C7 1.374(4) . ?
C20 C21 1.410(4) . ?
C20 C25 1.423(4) . ?
C37 C38 1.452(3) . ?
C37 C32 1.420(4) . ?
C37 C36 1.415(4) . ?
C12 C17 1.407(4) . ?
C12 C13 1.391(4) . ?
C40 C45 1.407(3) . ?
C40 C41 1.391(4) . ?
C10 C1 1.410(3) . ?
C45 C44 1.398(4) . ?
C56 C47 1.402(4) . ?
C56 C55 1.435(4) . ?
C47 C48 1.446(3) . ?
C17 C16 1.393(4) . ?
C35 C34 1.400(4) . ?
C35 C36 1.374(4) . ?
C42 C43 1.388(4) . ?
C42 C41 1.384(4) . ?
C16 C15 1.381(4) . ?
C32 C31 1.418(4) . ?
C32 C33 1.413(4) . ?
C52 C51 1.365(5) . ?
C43 C44 1.383(4) . ?
C34 C33 1.356(4) . ?
C4 C5 1.408(4) . ?
C4 C3 1.426(4) . ?
C1 C2 1.416(4) . ?
C31 C30 1.355(4) . ?
C48 C49 1.413(4) . ?
C21 C22 1.374(4) . ?
C25 C26 1.409(4) . ?
C25 C24 1.418(4) . ?
C6 C5 1.362(4) . ?
C6 C7 1.396(4) . ?
C28 C27 1.428(4) . ?
C14 C15 1.391(4) . ?
C14 C13 1.386(4) . ?
C27 C26 1.352(4) . ?
C54 C55 1.353(4) . ?
C3 C2 1.351(4) . ?
C51 C50 1.390(4) . ?
C50 C49 1.378(4) . ?
C23 C22 1.391(5) . ?
C23 C24 1.363(5) . ?
C59s C59s 1.503(19) 3_656 ?
C59s C58s 1.479(14) . ?
C58s C57s 1.435(13) . ?

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
O2 Ce1 O1 82.09(6) . . ?
N4 Ce1 O1 80.15(6) . . ?
N4 Ce1 O2 88.41(6) . . ?
O4 Ce1 O1 144.50(6) . . ?
O4 Ce1 O2 77.96(7) . . ?
O4 Ce1 N4 70.29(6) . . ?
N1 Ce1 O1 69.28(6) . . ?
N1 Ce1 O2 102.34(6) . . ?
N1 Ce1 N4 145.52(7) . . ?
N1 Ce1 O4 143.74(6) . . ?
N2 Ce1 O1 116.18(6) . . ?
N2 Ce1 O2 69.37(6) . . ?
N2 Ce1 N4 148.94(7) . . ?
N2 Ce1 O4 83.64(6) . . ?
N2 Ce1 N1 63.50(6) . . ?
O3 Ce1 O1 128.11(6) . . ?
O3 Ce1 O2 143.59(6) . . ?
O3 Ce1 N4 113.92(7) . . ?
O3 Ce1 O4 83.00(7) . . ?
O3 Ce1 N1 75.85(7) . . ?
O3 Ce1 N2 77.96(7) . . ?
N3 Ce1 O1 75.83(6) . . ?
N3 Ce1 O2 146.33(6) . . ?
N3 Ce1 N4 63.17(6) . . ?
N3 Ce1 O4 106.25(6) . . ?
N3 Ce1 N1 93.32(6) . . ?
N3 Ce1 N2 143.68(6) . . ?
N3 Ce1 O3 69.02(6) . . ?
C56 Ce1 O1 128.03(6) . . ?
C56 Ce1 O2 66.52(6) . . ?
C56 Ce1 N4 59.60(7) . . ?
C56 Ce1 O4 16.74(7) . . ?
C56 Ce1 N1 154.42(7) . . ?
C56 Ce1 N2 90.93(7) . . ?
C56 Ce1 O3 99.25(7) . . ?
C56 Ce1 N3 108.54(6) . . ?
C28 Ce1 O1 98.99(6) . . ?
C28 Ce1 O2 17.06(6) . . ?
C28 Ce1 N4 93.55(6) . . ?
C28 Ce1 O4 64.70(6) . . ?
C28 Ce1 N1 106.32(6) . . ?
C28 Ce1 N2 59.18(6) . . ?
C28 Ce1 O3 127.50(6) . . ?
C28 Ce1 N3 156.60(6) . . ?
C28 Ce1 C56 56.43(6) . . ?
C1 O1 Ce1 144.66(16) . . ?
C28 O2 Ce1 132.87(15) . . ?
C46 N4 Ce1 126.73(17) . . ?
C45 N4 Ce1 114.15(15) . . ?
C45 N4 C46 119.0(2) . . ?
C38 C39 N3 126.2(2) . . ?
C56 O4 Ce1 133.78(17) . . ?
C11 N1 Ce1 129.64(16) . . ?
C12 N1 Ce1 112.42(15) . . ?
C12 N1 C11 117.9(2) . . ?
C17 N2 Ce1 113.49(15) . . ?
C18 N2 Ce1 126.90(16) . . ?
C18 N2 C17 119.4(2) . . ?
C29 O3 Ce1 142.02(16) . . ?
C39 N3 Ce1 130.07(17) . . ?
C40 N3 Ce1 112.28(15) . . ?
C40 N3 C39 117.6(2) . . ?
C47 C46 N4 126.7(2) . . ?
C10 C9 C8 123.7(2) . . ?
C4 C9 C8 117.2(2) . . ?
C4 C9 C10 119.1(2) . . ?
C10 C11 N1 127.0(2) . . ?
C18 C19 C20 119.5(2) . . ?
C28 C19 C20 119.6(2) . . ?
C28 C19 C18 120.5(2) . . ?
C48 C53 C52 119.5(3) . . ?
C54 C53 C52 121.7(3) . . ?
C54 C53 C48 118.9(3) . . ?
C38 C29 O3 122.3(2) . . ?
C30 C29 O3 117.6(2) . . ?
C30 C29 C38 120.1(2) . . ?
C7 C8 C9 121.3(3) . . ?
C21 C20 C19 123.2(3) . . ?
C25 C20 C19 118.9(2) . . ?
C25 C20 C21 117.9(3) . . ?
C32 C37 C38 119.3(2) . . ?
C36 C37 C38 123.5(2) . . ?
C36 C37 C32 117.2(2) . . ?
C17 C12 N1 117.2(2) . . ?
C13 C12 N1 123.4(2) . . ?
C13 C12 C17 119.3(2) . . ?
C45 C40 N3 116.5(2) . . ?
C41 C40 N3 123.9(2) . . ?
C41 C40 C45 119.5(2) . . ?
C11 C10 C9 119.4(2) . . ?
C1 C10 C9 119.2(2) . . ?
C1 C10 C11 121.3(2) . . ?
C40 C45 N4 116.3(2) . . ?
C44 C45 N4 124.4(2) . . ?
C44 C45 C40 119.2(2) . . ?
O4 C56 Ce1 29.48(11) . . ?
C47 C56 Ce1 98.86(16) . . ?
C47 C56 O4 122.8(2) . . ?
C55 C56 Ce1 139.15(19) . . ?
C55 C56 O4 117.9(2) . . ?
C55 C56 C47 119.2(2) . . ?
C56 C47 C46 120.7(2) . . ?
C48 C47 C46 118.7(2) . . ?
C48 C47 C56 119.9(2) . . ?
C12 C17 N2 115.8(2) . . ?
C16 C17 N2 124.2(2) . . ?
C16 C17 C12 120.0(2) . . ?
C36 C35 C34 120.6(3) . . ?
C41 C42 C43 120.1(3) . . ?
C19 C18 N2 125.9(2) . . ?
C29 C38 C39 121.4(2) . . ?
C37 C38 C39 119.3(2) . . ?
C37 C38 C29 119.2(2) . . ?
C15 C16 C17 119.9(3) . . ?
C31 C32 C37 118.8(2) . . ?
C33 C32 C37 119.5(2) . . ?
C33 C32 C31 121.7(2) . . ?
C51 C52 C53 121.2(3) . . ?
C44 C43 C42 120.0(3) . . ?
C33 C34 C35 119.3(3) . . ?
C5 C4 C9 119.7(2) . . ?
C3 C4 C9 118.6(2) . . ?
C3 C4 C5 121.7(3) . . ?
C10 C1 O1 121.5(2) . . ?
C2 C1 O1 118.4(2) . . ?
C2 C1 C10 120.0(2) . . ?
C30 C31 C32 121.9(3) . . ?
C43 C44 C45 120.6(2) . . ?
C35 C36 C37 121.6(3) . . ?
C47 C48 C53 119.3(3) . . ?
C49 C48 C53 117.4(2) . . ?
C49 C48 C47 123.3(2) . . ?
C22 C21 C20 120.9(3) . . ?
C26 C25 C20 119.2(3) . . ?
C24 C25 C20 119.2(3) . . ?
C24 C25 C26 121.5(3) . . ?
C7 C6 C5 119.3(3) . . ?
C6 C5 C4 121.5(3) . . ?
C31 C30 C29 120.6(3) . . ?
O2 C28 Ce1 30.07(11) . . ?
C19 C28 Ce1 98.96(16) . . ?
C19 C28 O2 122.9(2) . . ?
C27 C28 Ce1 138.44(18) . . ?
C27 C28 O2 118.0(2) . . ?
C27 C28 C19 119.1(2) . . ?
C34 C33 C32 121.8(3) . . ?
C13 C14 C15 120.0(3) . . ?
C26 C27 C28 121.1(3) . . ?
C42 C41 C40 120.5(3) . . ?
C55 C54 C53 122.0(3) . . ?
C2 C3 C4 122.0(2) . . ?
C50 C51 C52 119.7(3) . . ?
C14 C15 C16 120.4(3) . . ?
C6 C7 C8 120.9(3) . . ?
C49 C50 C51 120.6(3) . . ?
C24 C23 C22 119.6(3) . . ?
C27 C26 C25 122.0(3) . . ?
C54 C55 C56 120.8(3) . . ?
C14 C13 C12 120.4(3) . . ?
C50 C49 C48 121.5(3) . . ?
C23 C22 C21 121.2(3) . . ?
C23 C24 C25 121.1(3) . . ?
C3 C2 C1 120.8(2) . . ?
C57s C58s C59s 120.0(9) . . ?

_olex2_exptl_crystal_mounting_method 
'mounted on a glass fibre using n-paratone oil '
_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_Emily100316_ThL2
_database_code_depnum_ccdc_archive 'CCDC 1548265'
_audit_update_record             
;
2017-05-05 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_Emily100316_ThL2    
;
PROBLEM: Check Calcd Positive Residual Density on     Th1       3.47 eA-3
RESPONSE: The atom type is correct and there is no evidence of twinning. The large residual density near Th atom may be due to an anomalous dispersion effect and has no chemical significance.
;
# Added during the CSD deposition process: Friday 05 May 2017 11:56 PM
# end Validation Reply Form

_audit_creation_date             2017-05-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_formula_moiety         'C56 H36 N4 O4 Th, C7 H8, C3.5 H3.5'
_chemical_formula_sum            'C66.5 H47.5 N4 O4 Th'
_chemical_formula_weight         1198.68
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
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'
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'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'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'
Th -6.65024 8.81044 35.56450 23.42190 12.74730 4.80703 0.56336 3.46204 17.83090
99.17220 13.4314002991
'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'

_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                   11.4987(3)
_cell_length_b                   14.3617(4)
_cell_length_c                   16.2769(5)
_cell_angle_alpha                106.2207(11)
_cell_angle_beta                 90.8257(11)
_cell_angle_gamma                94.1515(11)
_cell_volume                     2572.52(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      21.022
_cell_measurement_theta_min      2.166
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.7609.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5474
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1180.2268
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'layered diffusion of hexanes into a saturated toluene solution'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59819
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.30
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9953
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8478
_reflns_number_total             10098
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.5980
_refine_diff_density_min         -1.7340
_refine_diff_density_rms         0.1940
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             15.6187
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    94
_refine_ls_number_parameters     686
_refine_ls_number_reflns         10098
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.0413
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0582
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C67S(0.5) H67a(0.5) H67b(0.5) H67c(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C43(H43), C42(H42), C41(H41), C2(H2), C3(H3), C55(H55), C54(H54),
 C31(H31), C30(H30), C27(H27), C26(H26), C16(H16), C15(H15), C14(H14), C13(H13),
  C8(H8), C7(H7), C6(H6), C5(H5), C52(H52), C51(H51), C50(H50), C49(H49),
 C36(H36), C35(H35), C34(H34), C33(H33), C21(H21), C22(H22), C23(H23), C24(H24),
  C61S(H61S), C60S(H60S), C59S(H59S), C58S(H58S), C57S(H57S), C11(H11),
 C18(H18), C39(H39), C46(H46), C66S(H66S), C65S(H65S)
3.b Idealised Me refined as rotating group:
 C63S(H63a,H63b,H63c), C67S(H67a,H67b,H67c)
;
_atom_sites_solution_primary     direct
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
Th1 Th 0.510588(10) 0.504805(9) 0.255887(7) 0.01807(5) Uani 1.000000 .
O3 O 0.52075(18) 0.58089(16) 0.39926(13) 0.0224(5) Uani 1.000000 .
O1 O 0.43786(17) 0.53812(16) 0.13873(13) 0.0209(5) Uani 1.000000 .
N3 N 0.5399(2) 0.69507(19) 0.29050(16) 0.0179(6) Uani 1.000000 .
N2 N 0.3517(2) 0.40847(19) 0.31930(16) 0.0180(6) Uani 1.000000 .
N4 N 0.6929(2) 0.58136(19) 0.19507(16) 0.0183(6) Uani 1.000000 .
O4 O 0.68032(18) 0.44306(17) 0.28323(14) 0.0275(6) Uani 1.000000 .
N1 N 0.3016(2) 0.57098(19) 0.28091(16) 0.0177(6) Uani 1.000000 .
O2 O 0.47548(19) 0.34392(17) 0.17370(14) 0.0286(6) Uani 1.000000 .
C45 C 0.6693(3) 0.6680(2) 0.1726(2) 0.0202(8) Uani 1.000000 .
C40 C 0.5889(3) 0.7270(2) 0.2228(2) 0.0186(8) Uani 1.000000 .
C19 C 0.3774(3) 0.2380(2) 0.2444(2) 0.0217(8) Uani 1.000000 .
C11 C 0.2412(3) 0.6116(2) 0.2344(2) 0.0194(8) Uani 1.000000 .
C53 C 1.0055(3) 0.3642(2) 0.1944(2) 0.0238(8) Uani 1.000000 .
C28 C 0.4414(3) 0.2559(3) 0.1768(2) 0.0249(8) Uani 1.000000 .
C12 C 0.2495(2) 0.5542(2) 0.35488(19) 0.0168(7) Uani 1.000000 .
C18 C 0.3287(3) 0.3158(2) 0.3054(2) 0.0199(8) Uani 1.000000 .
C9 C 0.1992(3) 0.6884(2) 0.1185(2) 0.0203(8) Uani 1.000000 .
C16 C 0.2409(3) 0.4538(2) 0.4525(2) 0.0238(8) Uani 1.000000 .
C10 C 0.2755(3) 0.6344(2) 0.15619(19) 0.0194(8) Uani 1.000000 .
C17 C 0.2793(3) 0.4717(2) 0.37703(19) 0.0187(8) Uani 1.000000 .
C1 C 0.3714(3) 0.5941(2) 0.11104(19) 0.0179(7) Uani 1.000000 .
C4 C 0.2242(3) 0.7003(2) 0.0368(2) 0.0242(8) Uani 1.000000 .
C48 C 0.9540(3) 0.4378(2) 0.16752(19) 0.0180(7) Uani 1.000000 .
C29 C 0.4823(3) 0.6563(3) 0.4548(2) 0.0213(8) Uani 1.000000 .
C20 C 0.3467(3) 0.1391(2) 0.2472(2) 0.0236(8) Uani 1.000000 .
C39 C 0.5099(3) 0.7608(3) 0.3584(2) 0.0219(8) Uani 1.000000 .
C37 C 0.4189(3) 0.8230(3) 0.4996(2) 0.0246(8) Uani 1.000000 .
C46 C 0.7965(3) 0.5520(2) 0.18172(19) 0.0186(7) Uani 1.000000 .
C41 C 0.5600(3) 0.8106(2) 0.2019(2) 0.0257(8) Uani 1.000000 .
C56 C 0.7838(3) 0.4205(3) 0.2532(2) 0.0231(8) Uani 1.000000 .
C31 C 0.4194(3) 0.7238(3) 0.5995(2) 0.0316(9) Uani 1.000000 .
C49 C 1.0137(3) 0.4750(2) 0.1062(2) 0.0230(8) Uani 1.000000 .
C2 C 0.3944(3) 0.6097(2) 0.0302(2) 0.0247(8) Uani 1.000000 .
C47 C 0.8410(3) 0.4684(2) 0.20006(19) 0.0193(8) Uani 1.000000 .
C30 C 0.4577(3) 0.6480(3) 0.5384(2) 0.0270(9) Uani 1.000000 .
C50 C 1.1195(3) 0.4432(2) 0.0772(2) 0.0252(8) Uani 1.000000 .
C51 C 1.1724(3) 0.3734(3) 0.1068(2) 0.0295(9) Uani 1.000000 .
C32 C 0.3985(3) 0.8129(3) 0.5826(2) 0.0266(9) Uani 1.000000 .
C3 C 0.3240(3) 0.6609(2) -0.0048(2) 0.0280(9) Uani 1.000000 .
C38 C 0.4664(3) 0.7440(2) 0.43609(19) 0.0198(8) Uani 1.000000 .
C13 C 0.1760(3) 0.6166(3) 0.4075(2) 0.0261(8) Uani 1.000000 .
C54 C 0.9444(3) 0.3210(3) 0.2517(2) 0.0307(9) Uani 1.000000 .
C44 C 0.7167(3) 0.6942(2) 0.1042(2) 0.0253(8) Uani 1.000000 .
C8 C 0.0976(3) 0.7291(2) 0.1572(2) 0.0288(9) Uani 1.000000 .
C7 C 0.0269(3) 0.7771(3) 0.1169(3) 0.0354(10) Uani 1.000000 .
C25 C 0.3714(3) 0.0610(3) 0.1763(2) 0.0301(9) Uani 1.000000 .
C27 C 0.4653(3) 0.1748(3) 0.1072(2) 0.0344(9) Uani 1.000000 .
C21 C 0.2952(3) 0.1164(3) 0.3173(2) 0.0340(9) Uani 1.000000 .
C52 C 1.1149(3) 0.3335(3) 0.1631(2) 0.0286(9) Uani 1.000000 .
C35 C 0.3434(3) 0.9827(3) 0.5458(3) 0.0408(10) Uani 1.000000 .
C55 C 0.8382(3) 0.3467(3) 0.2797(2) 0.0276(9) Uani 1.000000 .
C42 C 0.6105(3) 0.8369(3) 0.1343(2) 0.0303(9) Uani 1.000000 .
C26 C 0.4299(3) 0.0826(3) 0.1071(2) 0.0394(10) Uani 1.000000 .
C14 C 0.1342(3) 0.5958(3) 0.4802(2) 0.0330(9) Uani 1.000000 .
C15 C 0.1673(3) 0.5161(3) 0.5028(2) 0.0338(9) Uani 1.000000 .
C43 C 0.6900(3) 0.7786(3) 0.0854(2) 0.0322(9) Uani 1.000000 .
C5 C 0.1492(3) 0.7510(3) -0.0022(2) 0.0332(9) Uani 1.000000 .
C36 C 0.3877(3) 0.9088(3) 0.4832(2) 0.0336(9) Uani 1.000000 .
C24 C 0.3375(3) -0.0351(3) 0.1772(3) 0.0405(11) Uani 1.000000 .
C23 C 0.2846(3) -0.0541(3) 0.2459(3) 0.0438(11) Uani 1.000000 .
C33 C 0.3552(3) 0.8893(3) 0.6459(2) 0.0398(11) Uani 1.000000 .
C6 C 0.0528(3) 0.7867(3) 0.0364(2) 0.0369(10) Uani 1.000000 .
C34 C 0.3285(3) 0.9724(3) 0.6280(3) 0.0449(11) Uani 1.000000 .
C22 C 0.2658(3) 0.0217(3) 0.3162(3) 0.0432(11) Uani 1.000000 .
C62S C 0.9786(4) 0.8331(3) 0.5027(3) 0.0506(12) Uani 1.000000 .
C57S C 0.8832(4) 0.7671(3) 0.4740(3) 0.0650(14) Uani 1.000000 .
C60S C 0.9762(5) 0.8613(4) 0.3642(3) 0.0728(15) Uani 1.000000 .
C61S C 1.0254(4) 0.8778(3) 0.4452(3) 0.0639(14) Uani 1.000000 .
C59S C 0.8807(5) 0.7979(4) 0.3389(3) 0.0761(16) Uani 1.000000 .
C63S C 1.0300(4) 0.8528(4) 0.5916(3) 0.0813(17) Uani 1.000000 .
C58S C 0.8348(4) 0.7486(4) 0.3946(4) 0.0833(18) Uani 1.000000 .
C66S C -0.1170(5) 0.9856(5) 0.9983(7) 0.104(3) Uani 1.000000 .
C64S C 0.0612(8) 0.9770(5) 0.9229(6) 0.103(2) Uani 1.000000 .
C65S C -0.0552(9) 0.9615(4) 0.9202(6) 0.109(3) Uani 1.000000 .
C67S C 0.1188(14) 0.9570(9) 0.8471(8) 0.138(7) Uani 0.500000 .
H44 H 0.7689(3) 0.6534(2) 0.0691(2) 0.0303(10) Uiso 1.000000 R
H43 H 0.7258(3) 0.7965(3) 0.0392(2) 0.0387(11) Uiso 1.000000 R
H42 H 0.5911(3) 0.8946(3) 0.1214(2) 0.0363(10) Uiso 1.000000 R
H41 H 0.5047(3) 0.8500(2) 0.2347(2) 0.0308(10) Uiso 1.000000 R
H2 H 0.4603(3) 0.5836(2) 0.0002(2) 0.0296(10) Uiso 1.000000 R
H3 H 0.3421(3) 0.6707(2) -0.0587(2) 0.0336(10) Uiso 1.000000 R
H55 H 0.7995(3) 0.3156(3) 0.3173(2) 0.0331(10) Uiso 1.000000 R
H54 H 0.9795(3) 0.2726(3) 0.2709(2) 0.0368(11) Uiso 1.000000 R
H31 H 0.4064(3) 0.7169(3) 0.6550(2) 0.0379(11) Uiso 1.000000 R
H30 H 0.4682(3) 0.5886(3) 0.5514(2) 0.0324(10) Uiso 1.000000 R
H27 H 0.5066(3) 0.1855(3) 0.0601(2) 0.0413(11) Uiso 1.000000 R
H26 H 0.4449(3) 0.0305(3) 0.0588(2) 0.0473(12) Uiso 1.000000 R
H16 H 0.2650(3) 0.3996(2) 0.4690(2) 0.0285(10) Uiso 1.000000 R
H15 H 0.1392(3) 0.5036(3) 0.5536(2) 0.0406(11) Uiso 1.000000 R
H14 H 0.0820(3) 0.6371(3) 0.5148(2) 0.0397(11) Uiso 1.000000 R
H13 H 0.1548(3) 0.6731(3) 0.3933(2) 0.0314(10) Uiso 1.000000 R
H8 H 0.0781(3) 0.7230(2) 0.2120(2) 0.0346(10) Uiso 1.000000 R
H7 H -0.0402(3) 0.8041(3) 0.1443(3) 0.0425(12) Uiso 1.000000 R
H6 H 0.0021(3) 0.8185(3) 0.0084(2) 0.0443(12) Uiso 1.000000 R
H5 H 0.1674(3) 0.7600(3) -0.0563(2) 0.0399(11) Uiso 1.000000 R
H52 H 1.1489(3) 0.2842(3) 0.1818(2) 0.0343(11) Uiso 1.000000 R
H51 H 1.2471(3) 0.3540(3) 0.0880(2) 0.0354(11) Uiso 1.000000 R
H50 H 1.1576(3) 0.4693(2) 0.0362(2) 0.0302(10) Uiso 1.000000 R
H49 H 0.9800(3) 0.5225(2) 0.0849(2) 0.0276(10) Uiso 1.000000 R
H36 H 0.3973(3) 0.9164(3) 0.4275(2) 0.0403(11) Uiso 1.000000 R
H35 H 0.3231(3) 1.0402(3) 0.5330(3) 0.0490(12) Uiso 1.000000 R
H34 H 0.2996(3) 1.0236(3) 0.6715(3) 0.0539(14) Uiso 1.000000 R
H33 H 0.3446(3) 0.8828(3) 0.7018(2) 0.0478(13) Uiso 1.000000 R
H21 H 0.2804(3) 0.1674(3) 0.3666(2) 0.0408(11) Uiso 1.000000 R
H22 H 0.2317(3) 0.0083(3) 0.3649(3) 0.0519(13) Uiso 1.000000 R
H23 H 0.2610(3) -0.1192(3) 0.2451(3) 0.0526(13) Uiso 1.000000 R
H24 H 0.3517(3) -0.0876(3) 0.1290(3) 0.0486(13) Uiso 1.000000 R
H61S H 1.0935(4) 0.9212(3) 0.4615(3) 0.0766(16) Uiso 1.000000 R
H60S H 1.0093(5) 0.8944(4) 0.3260(3) 0.0874(18) Uiso 1.000000 R
H59S H 0.8456(5) 0.7873(4) 0.2835(3) 0.0913(19) Uiso 1.000000 R
H58S H 0.7697(4) 0.7021(4) 0.3770(4) 0.100(2) Uiso 1.000000 R
H57S H 0.8503(4) 0.7334(3) 0.5118(3) 0.0780(17) Uiso 1.000000 R
H11 H 0.1658(3) 0.6284(2) 0.2537(2) 0.0233(9) Uiso 1.000000 R
H18 H 0.2717(3) 0.2970(2) 0.3406(2) 0.0239(9) Uiso 1.000000 R
H39 H 0.5175(3) 0.8264(3) 0.3563(2) 0.0263(10) Uiso 1.000000 R
H46 H 0.8491(3) 0.5898(2) 0.15709(19) 0.0223(9) Uiso 1.000000 R
H63a H 0.9753(14) 0.826(2) 0.6265(7) 0.122(3) Uiso 1.000000 GR
H63b H 1.1035(16) 0.822(2) 0.5894(4) 0.122(3) Uiso 1.000000 GR
H63c H 1.045(3) 0.9232(4) 0.6170(9) 0.122(3) Uiso 1.000000 GR
H66S H -0.1997(5) 0.9753(5) 0.9954(7) 0.125(3) Uiso 1.000000 R
H65S H -0.0966(9) 0.9346(4) 0.8670(6) 0.131(3) Uiso 1.000000 R
H67a H 0.183(6) 0.916(7) 0.850(3) 0.207(10) Uiso 0.500000 GR
H67b H 0.064(2) 0.923(7) 0.7998(12) 0.207(10) Uiso 0.500000 GR
H67c H 0.151(8) 1.0180(10) 0.837(4) 0.207(10) Uiso 0.500000 GR


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
Th1 O3 2.281(2) . ?
Th1 O1 2.255(2) . ?
Th1 N3 2.627(3) . ?
Th1 N2 2.608(3) . ?
Th1 N4 2.630(2) . ?
Th1 O4 2.289(2) . ?
Th1 N1 2.643(2) . ?
Th1 O2 2.327(2) . ?
O3 C29 1.311(4) . ?
O1 C1 1.309(4) . ?
N3 C40 1.416(4) . ?
N3 C39 1.306(4) . ?
N2 C18 1.293(4) . ?
N2 C17 1.434(4) . ?
N4 C45 1.434(4) . ?
N4 C46 1.293(4) . ?
O4 C56 1.320(4) . ?
N1 C11 1.299(4) . ?
N1 C12 1.424(4) . ?
O2 C28 1.311(4) . ?
C45 C40 1.409(4) . ?
C45 C44 1.380(4) . ?
C40 C41 1.396(4) . ?
C19 C28 1.404(4) . ?
C19 C18 1.427(4) . ?
C19 C20 1.452(4) . ?
C11 C10 1.452(4) . ?
C53 C48 1.414(4) . ?
C53 C54 1.424(4) . ?
C53 C52 1.418(4) . ?
C28 C27 1.426(5) . ?
C12 C17 1.394(4) . ?
C12 C13 1.397(4) . ?
C9 C10 1.448(4) . ?
C9 C4 1.418(4) . ?
C9 C8 1.420(4) . ?
C16 C17 1.395(4) . ?
C16 C15 1.381(4) . ?
C10 C1 1.404(4) . ?
C1 C2 1.420(4) . ?
C4 C3 1.414(5) . ?
C4 C5 1.418(4) . ?
C48 C49 1.421(4) . ?
C48 C47 1.461(4) . ?
C29 C30 1.429(4) . ?
C29 C38 1.400(4) . ?
C20 C25 1.415(5) . ?
C20 C21 1.400(5) . ?
C39 C38 1.442(4) . ?
C37 C32 1.421(4) . ?
C37 C38 1.451(4) . ?
C37 C36 1.400(5) . ?
C46 C47 1.442(4) . ?
C41 C42 1.382(4) . ?
C56 C47 1.393(4) . ?
C56 C55 1.430(4) . ?
C31 C30 1.357(5) . ?
C31 C32 1.418(5) . ?
C49 C50 1.373(4) . ?
C2 C3 1.351(4) . ?
C50 C51 1.400(5) . ?
C51 C52 1.364(5) . ?
C32 C33 1.405(5) . ?
C13 C14 1.384(4) . ?
C54 C55 1.350(4) . ?
C44 C43 1.383(4) . ?
C8 C7 1.372(4) . ?
C7 C6 1.389(5) . ?
C25 C26 1.415(5) . ?
C25 C24 1.411(5) . ?
C27 C26 1.357(5) . ?
C21 C22 1.372(5) . ?
C35 C36 1.384(5) . ?
C35 C34 1.398(5) . ?
C42 C43 1.389(5) . ?
C14 C15 1.373(5) . ?
C5 C6 1.345(5) . ?
C24 C23 1.364(5) . ?
C23 C22 1.374(5) . ?
C33 C34 1.360(5) . ?
C62S C57S 1.381(6) . ?
C62S C61S 1.370(6) . ?
C62S C63S 1.498(6) . ?
C57S C58S 1.347(6) . ?
C60S C61S 1.378(6) . ?
C60S C59S 1.356(6) . ?
C59S C58S 1.386(7) . ?
C66S C64S 1.374(9) 2_577 ?
C66S C65S 1.433(9) . ?
C64S C65S 1.339(9) . ?
C64S C67S 1.377(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Th1 O3 135.38(8) . . ?
N3 Th1 O3 67.17(8) . . ?
N3 Th1 O1 75.32(8) . . ?
N2 Th1 O3 75.53(8) . . ?
N2 Th1 O1 110.25(7) . . ?
N2 Th1 N3 125.53(8) . . ?
N4 Th1 O3 104.70(7) . . ?
N4 Th1 O1 76.17(7) . . ?
N4 Th1 N3 61.63(8) . . ?
N4 Th1 N2 170.91(8) . . ?
O4 Th1 O3 84.21(8) . . ?
O4 Th1 O1 132.68(7) . . ?
O4 Th1 N3 110.41(8) . . ?
O4 Th1 N2 103.46(8) . . ?
O4 Th1 N4 67.67(8) . . ?
N1 Th1 O3 78.26(7) . . ?
N1 Th1 O1 68.14(7) . . ?
N1 Th1 N3 73.04(8) . . ?
N1 Th1 N2 61.31(8) . . ?
N1 Th1 N4 127.77(8) . . ?
N1 Th1 O4 159.13(8) . . ?
O2 Th1 O3 134.38(8) . . ?
O2 Th1 O1 83.68(8) . . ?
O2 Th1 N3 158.16(8) . . ?
O2 Th1 N2 67.45(8) . . ?
O2 Th1 N4 107.82(8) . . ?
O2 Th1 O4 79.59(8) . . ?
O2 Th1 N1 104.80(8) . . ?
C29 O3 Th1 140.24(19) . . ?
C1 O1 Th1 145.04(19) . . ?
C40 N3 Th1 113.27(19) . . ?
C39 N3 Th1 128.5(2) . . ?
C39 N3 C40 118.1(3) . . ?
C18 N2 Th1 130.3(2) . . ?
C17 N2 Th1 112.12(19) . . ?
C17 N2 C18 117.5(3) . . ?
C45 N4 Th1 112.71(18) . . ?
C46 N4 Th1 130.1(2) . . ?
C46 N4 C45 117.2(3) . . ?
C56 O4 Th1 143.8(2) . . ?
C11 N1 Th1 129.4(2) . . ?
C12 N1 Th1 112.68(18) . . ?
C12 N1 C11 117.9(3) . . ?
C28 O2 Th1 143.8(2) . . ?
C40 C45 N4 116.7(3) . . ?
C44 C45 N4 124.1(3) . . ?
C44 C45 C40 119.1(3) . . ?
C45 C40 N3 116.8(3) . . ?
C41 C40 N3 124.2(3) . . ?
C41 C40 C45 119.0(3) . . ?
C18 C19 C28 120.4(3) . . ?
C20 C19 C28 120.6(3) . . ?
C20 C19 C18 118.5(3) . . ?
C10 C11 N1 127.5(3) . . ?
C54 C53 C48 118.7(3) . . ?
C52 C53 C48 120.0(3) . . ?
C52 C53 C54 121.2(3) . . ?
C19 C28 O2 122.6(3) . . ?
C27 C28 O2 119.1(3) . . ?
C27 C28 C19 118.2(3) . . ?
C17 C12 N1 116.6(3) . . ?
C13 C12 N1 124.3(3) . . ?
C13 C12 C17 119.0(3) . . ?
C19 C18 N2 128.8(3) . . ?
C4 C9 C10 118.9(3) . . ?
C8 C9 C10 124.3(3) . . ?
C8 C9 C4 116.8(3) . . ?
C15 C16 C17 119.0(3) . . ?
C9 C10 C11 118.6(3) . . ?
C1 C10 C11 121.3(3) . . ?
C1 C10 C9 119.6(3) . . ?
C12 C17 N2 116.7(3) . . ?
C16 C17 N2 122.6(3) . . ?
C16 C17 C12 120.7(3) . . ?
C10 C1 O1 122.3(3) . . ?
C2 C1 O1 118.2(3) . . ?
C2 C1 C10 119.4(3) . . ?
C3 C4 C9 119.2(3) . . ?
C5 C4 C9 119.9(3) . . ?
C5 C4 C3 120.9(3) . . ?
C49 C48 C53 117.3(3) . . ?
C47 C48 C53 119.4(3) . . ?
C47 C48 C49 123.2(3) . . ?
C30 C29 O3 117.9(3) . . ?
C38 C29 O3 122.9(3) . . ?
C38 C29 C30 119.2(3) . . ?
C25 C20 C19 118.8(3) . . ?
C21 C20 C19 123.4(3) . . ?
C21 C20 C25 117.7(3) . . ?
C38 C39 N3 126.7(3) . . ?
C38 C37 C32 119.1(3) . . ?
C36 C37 C32 117.1(3) . . ?
C36 C37 C38 123.8(3) . . ?
C47 C46 N4 127.3(3) . . ?
C42 C41 C40 121.1(3) . . ?
C47 C56 O4 122.0(3) . . ?
C55 C56 O4 117.6(3) . . ?
C55 C56 C47 120.4(3) . . ?
C32 C31 C30 121.8(3) . . ?
C50 C49 C48 120.9(3) . . ?
C3 C2 C1 121.1(3) . . ?
C46 C47 C48 119.0(3) . . ?
C56 C47 C48 118.9(3) . . ?
C56 C47 C46 121.9(3) . . ?
C31 C30 C29 121.0(3) . . ?
C51 C50 C49 121.5(3) . . ?
C52 C51 C50 118.8(3) . . ?
C31 C32 C37 118.8(3) . . ?
C33 C32 C37 120.2(4) . . ?
C33 C32 C31 121.0(3) . . ?
C2 C3 C4 121.7(3) . . ?
C39 C38 C29 120.3(3) . . ?
C37 C38 C29 119.9(3) . . ?
C37 C38 C39 119.3(3) . . ?
C14 C13 C12 119.8(3) . . ?
C55 C54 C53 122.2(3) . . ?
C43 C44 C45 121.4(3) . . ?
C7 C8 C9 121.4(3) . . ?
C6 C7 C8 120.6(4) . . ?
C26 C25 C20 118.4(3) . . ?
C24 C25 C20 119.1(4) . . ?
C24 C25 C26 122.5(4) . . ?
C26 C27 C28 121.0(4) . . ?
C22 C21 C20 121.2(4) . . ?
C51 C52 C53 121.3(3) . . ?
C34 C35 C36 119.7(4) . . ?
C54 C55 C56 120.3(3) . . ?
C43 C42 C41 119.6(3) . . ?
C27 C26 C25 122.5(3) . . ?
C15 C14 C13 120.6(3) . . ?
C14 C15 C16 120.8(3) . . ?
C42 C43 C44 119.8(3) . . ?
C6 C5 C4 121.0(3) . . ?
C35 C36 C37 121.9(4) . . ?
C23 C24 C25 121.4(4) . . ?
C22 C23 C24 119.3(4) . . ?
C34 C33 C32 120.8(4) . . ?
C5 C6 C7 120.3(3) . . ?
C33 C34 C35 120.2(4) . . ?
C23 C22 C21 121.3(4) . . ?
C61S C62S C57S 116.6(4) . . ?
C63S C62S C57S 121.5(4) . . ?
C63S C62S C61S 121.8(4) . . ?
C58S C57S C62S 122.7(5) . . ?
C59S C60S C61S 120.1(5) . . ?
C60S C61S C62S 121.6(4) . . ?
C58S C59S C60S 119.3(5) . . ?
C59S C58S C57S 119.5(5) . . ?
C65S C66S C64S 122.5(7) . 2_577 ?
C65S C64S C66S 117.8(8) . 2_577 ?
C67S C64S C66S 123.2(11) . 2_577 ?
C67S C64S C65S 118.9(12) . . ?
C64S C65S C66S 119.6(7) . . ?

_olex2_exptl_crystal_mounting_method 
'suitable crystal was mounted on a glass fibre using paratone-n oil'
_olex2_submission_special_instructions 'No special instructions were received'
