# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_Ia
_database_code_depnum_ccdc_archive 'CCDC 1403231'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H60 As2 Ce2 N12 S8'
_chemical_formula_sum            'C18 H60 As2 Ce2 N12 S8'
_chemical_formula_weight         1131.34

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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   38.8180(8)
_cell_length_b                   12.0130(3)
_cell_length_c                   20.7022(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.797(2)
_cell_angle_gamma                90.00
_cell_volume                     8205.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8509
_cell_measurement_theta_min      3.5190
_cell_measurement_theta_max      28.9720

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4496
_exptl_absorpt_coefficient_mu    4.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_T_max  0.7562
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18714
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         27.10
_reflns_number_total             8831
_reflns_number_gt                7398
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The command TWIN -10-2 0-10 001 is refined the pseudo-merohedral 
twinning, which makes R1/wR2 significantly lower.
The DELU restraint prevents the thermal ellipsoids of all 
adjacent C atoms from adopting different orientations. 
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)+(0.0490P)²+4.0000P] 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         8831
_refine_ls_number_parameters     452
_refine_ls_number_restraints     187
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.300013(8) 0.23278(2) 0.723139(15) 0.02919(8) Uani 1 1 d . A .
Ce2 Ce 0.069722(8) 0.27153(2) 0.494142(14) 0.02758(8) Uani 1 1 d . . .
As1 As 0.434221(14) 0.23551(4) 0.86872(3) 0.02748(11) Uani 1 1 d . . .
As2 As 0.183820(15) 0.24064(5) 0.61212(3) 0.03705(13) Uani 1 1 d . . .
S1 S 0.48555(3) 0.13198(11) 0.94261(7) 0.0357(3) Uani 1 1 d . . .
S2 S 0.43238(4) 0.37988(12) 0.92823(8) 0.0456(3) Uani 1 1 d . . .
S3 S 0.43585(5) 0.28154(14) 0.76935(8) 0.0491(4) Uani 1 1 d . . .
S4 S 0.38101(3) 0.13461(11) 0.83416(7) 0.0385(3) Uani 1 1 d . . .
S5 S 0.14994(4) 0.37246(15) 0.53385(10) 0.0622(5) Uani 1 1 d . . .
S6 S 0.21972(4) 0.15243(15) 0.57690(9) 0.0548(4) Uani 1 1 d . . .
S7 S 0.14074(4) 0.13162(14) 0.61544(9) 0.0525(4) Uani 1 1 d . . .
S8 S 0.22606(4) 0.31124(17) 0.72155(9) 0.0628(5) Uani 1 1 d . . .
N1 N 0.29397(16) 0.1153(4) 0.8282(3) 0.0535(13) Uani 1 1 d . . .
H1D H 0.2676 0.1072 0.8122 0.064 Uiso 1 1 calc R . .
H1E H 0.3043 0.0469 0.8320 0.064 Uiso 1 1 calc R . .
N2 N 0.32386(13) 0.3389(4) 0.8534(2) 0.0461(11) Uani 1 1 d . . .
H2B H 0.3511 0.3441 0.8795 0.055 Uiso 1 1 calc R . .
H2C H 0.3139 0.4086 0.8422 0.055 Uiso 1 1 calc R . .
N7 N 0.02526(14) 0.0973(4) 0.4130(3) 0.0532(13) Uani 1 1 d . . .
H7D H 0.0253 0.0467 0.4450 0.064 Uiso 1 1 calc R . .
H7E H -0.0005 0.1201 0.3819 0.064 Uiso 1 1 calc R . .
N8 N 0.09934(16) 0.1448(6) 0.4258(3) 0.0682(17) Uani 1 1 d . B .
H8B H 0.0955 0.1813 0.3845 0.082 Uiso 1 1 calc R . .
H8C H 0.1262 0.1371 0.4580 0.082 Uiso 1 1 calc R . .
N9 N 0.03866(13) 0.3501(4) 0.3538(2) 0.0394(10) Uani 1 1 d . . .
H9C H 0.0483 0.3100 0.3301 0.047 Uiso 1 1 calc R . .
H9D H 0.0116 0.3416 0.3278 0.047 Uiso 1 1 calc R . .
N10 N 0.06589(12) 0.4923(3) 0.4811(2) 0.0348(9) Uani 1 1 d . . .
H10D H 0.0498 0.5175 0.4970 0.042 Uiso 1 1 calc R . .
H10E H 0.0909 0.5198 0.5128 0.042 Uiso 1 1 calc R . .
N11 N 0.08506(17) 0.3595(4) 0.6239(3) 0.0571(14) Uani 1 1 d . . .
H11C H 0.1111 0.3458 0.6598 0.069 Uiso 1 1 calc R . .
H11D H 0.0820 0.4338 0.6182 0.069 Uiso 1 1 calc R . .
N12 N 0.04200(13) 0.1583(4) 0.5681(2) 0.0430(11) Uani 1 1 d . . .
H12B H 0.0148 0.1569 0.5391 0.052 Uiso 1 1 calc R . .
H12C H 0.0507 0.0875 0.5735 0.052 Uiso 1 1 calc R . .
C1 C 0.3315(3) 0.3369(8) 0.9807(4) 0.090(3) Uani 1 1 d . . .
H1A H 0.3251 0.4148 0.9769 0.134 Uiso 1 1 calc R . .
H1B H 0.3604 0.3279 1.0058 0.134 Uiso 1 1 calc R . .
H1C H 0.3220 0.2999 1.0094 0.134 Uiso 1 1 calc R . .
C2 C 0.3118(2) 0.2882(6) 0.9038(4) 0.070(2) Uani 1 1 d . . .
H2A H 0.2828 0.3042 0.8801 0.084 Uiso 1 1 calc R . .
C3 C 0.3150(3) 0.1672(6) 0.9041(4) 0.081(2) Uani 1 1 d . . .
H3A H 0.3040 0.1365 0.9330 0.098 Uiso 1 1 calc R . .
H3B H 0.3435 0.1473 0.9303 0.098 Uiso 1 1 calc R . .
C13 C 0.0594(2) 0.6585(6) 0.4032(4) 0.0688(19) Uani 1 1 d . . .
H13A H 0.0516 0.6997 0.4332 0.103 Uiso 1 1 calc R . .
H13B H 0.0442 0.6844 0.3516 0.103 Uiso 1 1 calc R . .
H13C H 0.0879 0.6689 0.4234 0.103 Uiso 1 1 calc R . .
C14 C 0.0510(3) 0.5380(6) 0.4053(4) 0.083(3) Uani 1 1 d . . .
H14A H 0.0222 0.5434 0.3878 0.099 Uiso 1 1 calc R . .
C15 C 0.0481(3) 0.4661(6) 0.3528(4) 0.103(3) Uani 1 1 d . . .
H15A H 0.0737 0.4687 0.3550 0.123 Uiso 1 1 calc R . .
H15B H 0.0277 0.4954 0.3035 0.123 Uiso 1 1 calc R . .
C16 C 0.0688(2) 0.3605(8) 0.7258(4) 0.088(3) Uani 1 1 d . . .
H16A H 0.0679 0.4403 0.7253 0.132 Uiso 1 1 calc R . .
H16B H 0.0953 0.3359 0.7649 0.132 Uiso 1 1 calc R . .
H16C H 0.0489 0.3316 0.7355 0.132 Uiso 1 1 calc R . .
C17 C 0.0600(3) 0.3192(7) 0.6502(4) 0.073(2) Uani 1 1 d . . .
H17A H 0.0332 0.3501 0.6140 0.088 Uiso 1 1 calc R . .
C18 C 0.0537(3) 0.2011(6) 0.6431(4) 0.071(2) Uani 1 1 d . . .
H18A H 0.0327 0.1824 0.6533 0.085 Uiso 1 1 calc R . .
H18B H 0.0785 0.1644 0.6811 0.085 Uiso 1 1 calc R . .
C7 C 0.2753(3) 0.5803(8) 0.5761(6) 0.080(4) Uani 0.647(9) 1 d PU A 1
H7A H 0.2475 0.5984 0.5576 0.120 Uiso 0.647(9) 1 calc PR A 1
H7B H 0.2775 0.5531 0.5349 0.120 Uiso 0.647(9) 1 calc PR A 1
H7C H 0.2917 0.6457 0.5972 0.120 Uiso 0.647(9) 1 calc PR A 1
C8 C 0.2889(4) 0.4958(12) 0.6338(8) 0.067(3) Uani 0.647(9) 1 d PU A 1
H8A H 0.2838 0.5277 0.6717 0.081 Uiso 0.647(9) 1 calc PR A 1
C9 C 0.3318(3) 0.4813(11) 0.6737(8) 0.059(3) Uani 0.647(9) 1 d PU A 1
H9A H 0.3447 0.5534 0.6912 0.071 Uiso 0.647(9) 1 calc PR A 1
H9B H 0.3391 0.4521 0.6388 0.071 Uiso 0.647(9) 1 calc PR A 1
C7B C 0.3548(6) 0.5854(17) 0.6849(11) 0.075(6) Uani 0.353(9) 1 d PU A 2
H7L H 0.3675 0.6413 0.7237 0.113 Uiso 0.353(9) 1 calc PR A 2
H7M H 0.3378 0.6206 0.6364 0.113 Uiso 0.353(9) 1 calc PR A 2
H7N H 0.3752 0.5420 0.6838 0.113 Uiso 0.353(9) 1 calc PR A 2
C8B C 0.3012(7) 0.473(2) 0.6167(12) 0.051(4) Uani 0.353(9) 1 d PU A 2
H8L H 0.3175 0.4361 0.6003 0.061 Uiso 0.353(9) 1 calc PR A 2
H8M H 0.2885 0.5384 0.5854 0.061 Uiso 0.353(9) 1 calc PR A 2
C9B C 0.3270(6) 0.5039(18) 0.7034(10) 0.044(4) Uani 0.353(9) 1 d PU A 2
H9L H 0.3123 0.5406 0.7241 0.053 Uiso 0.353(9) 1 calc PR A 2
N5 N 0.26858(15) 0.3913(5) 0.6150(3) 0.0739(18) Uani 1 1 d . . .
H5F H 0.2679 0.3645 0.5738 0.089 Uiso 0.647(9) 1 calc PR A 1
H5G H 0.2428 0.4031 0.6017 0.089 Uiso 0.647(9) 1 calc PR A 1
H5B H 0.2549 0.3581 0.5692 0.089 Uiso 0.353(9) 1 calc PR A 2
H5C H 0.2507 0.4317 0.6204 0.089 Uiso 0.353(9) 1 calc PR A 2
N6 N 0.34769(13) 0.4047(4) 0.7404(3) 0.0474(11) Uani 1 1 d . . .
H6C H 0.3521 0.4447 0.7808 0.057 Uiso 0.647(9) 1 calc PR A 1
H6D H 0.3718 0.3780 0.7510 0.057 Uiso 0.647(9) 1 calc PR A 1
H6F H 0.3635 0.4204 0.7905 0.057 Uiso 0.353(9) 1 d PR A 2
H6G H 0.3642 0.3821 0.7244 0.057 Uiso 0.353(9) 1 d PR A 2
C10 C 0.0236(6) -0.0614(13) 0.3356(10) 0.072(6) Uani 0.392(12) 1 d PU B 1
H10A H -0.0053 -0.0564 0.3023 0.107 Uiso 0.392(12) 1 calc PR B 1
H10B H 0.0300 -0.1134 0.3756 0.107 Uiso 0.392(12) 1 calc PR B 1
H10C H 0.0354 -0.0863 0.3074 0.107 Uiso 0.392(12) 1 calc PR B 1
C10B C 0.0882(5) -0.0424(10) 0.3508(8) 0.090(5) Uani 0.608(12) 1 d PU B 2
H10F H 0.1167 -0.0560 0.3733 0.135 Uiso 0.608(12) 1 calc PR B 2
H10G H 0.0775 -0.0082 0.3019 0.135 Uiso 0.608(12) 1 calc PR B 2
H10H H 0.0745 -0.1116 0.3449 0.135 Uiso 0.608(12) 1 calc PR B 2
C11 C 0.0817(3) 0.0362(8) 0.4029(5) 0.090(3) Uani 1 1 d . . .
H11A H 0.0887 0.0042 0.3683 0.108 Uiso 0.392(12) 1 calc PR B 1
H11B H 0.0925 -0.0118 0.4471 0.108 Uiso 0.392(12) 1 calc PR B 1
H11F H 0.0911 -0.0054 0.4500 0.108 Uiso 0.608(12) 1 calc PR B 2
C12 C 0.0390(2) 0.0422(7) 0.3665(4) 0.092(3) Uani 1 1 d . B .
H12A H 0.0302 0.0914 0.3228 0.110 Uiso 0.392(12) 1 calc PR B 1
H12F H 0.0280 -0.0327 0.3544 0.110 Uiso 0.608(12) 1 calc PR B 2
H12G H 0.0282 0.0825 0.3191 0.110 Uiso 0.608(12) 1 calc PR B 2
N3 N 0.33131(16) 0.1824(4) 0.6372(3) 0.0523(12) Uani 1 1 d . . .
H3C H 0.3225 0.2320 0.5990 0.063 Uiso 0.647(9) 1 calc PR A 1
H3D H 0.3585 0.1868 0.6657 0.063 Uiso 0.647(9) 1 calc PR A 1
H3G H 0.3133 0.2067 0.5897 0.063 Uiso 0.353(9) 1 d PR A 2
H3H H 0.3543 0.2220 0.6542 0.063 Uiso 0.353(9) 1 d PR A 2
N4 N 0.30201(14) 0.0185(4) 0.6954(3) 0.0467(11) Uani 1 1 d . . .
H4G H 0.3119 -0.0185 0.7395 0.056 Uiso 0.647(9) 1 calc PR A 1
H4H H 0.2763 -0.0045 0.6642 0.056 Uiso 0.647(9) 1 calc PR A 1
H4D H 0.3102 -0.0203 0.7385 0.056 Uiso 0.353(9) 1 d PR A 2
H4E H 0.2761 -0.0010 0.6617 0.056 Uiso 0.353(9) 1 d PR A 2
C4 C 0.3104(7) -0.1319(12) 0.6168(9) 0.084(5) Uani 0.647(9) 1 d PDU A 1
H4A H 0.3080 -0.1876 0.6475 0.126 Uiso 0.647(9) 1 calc PR A 1
H4B H 0.3303 -0.1549 0.6054 0.126 Uiso 0.647(9) 1 calc PR A 1
H4C H 0.2847 -0.1226 0.5704 0.126 Uiso 0.647(9) 1 calc PR A 1
C5 C 0.3244(4) -0.0135(10) 0.6632(7) 0.058(3) Uani 0.647(9) 1 d PDU A 1
H5A H 0.3532 -0.0171 0.7030 0.070 Uiso 0.647(9) 1 calc PR A 1
C6 C 0.3188(4) 0.0650(12) 0.6042(7) 0.065(3) Uani 0.647(9) 1 d PU A 1
H6A H 0.2906 0.0652 0.5632 0.078 Uiso 0.647(9) 1 calc PR A 1
H6B H 0.3350 0.0416 0.5836 0.078 Uiso 0.647(9) 1 calc PR A 1
C4B C 0.3198(10) -0.1320(19) 0.6437(14) 0.059(6) Uani 0.353(9) 1 d PDU A 2
H4L H 0.3203 -0.1552 0.6885 0.088 Uiso 0.353(9) 1 calc PR A 2
H4M H 0.3465 -0.1386 0.6519 0.088 Uiso 0.353(9) 1 calc PR A 2
H4I H 0.3014 -0.1784 0.6017 0.088 Uiso 0.353(9) 1 calc PR A 2
C5B C 0.3048(7) -0.0018(16) 0.6245(11) 0.050(4) Uani 0.353(9) 1 d PDU A 2
H5L H 0.2796 0.0102 0.5756 0.060 Uiso 0.353(9) 1 calc PR A 2
C6B C 0.3408(6) 0.0658(19) 0.6367(12) 0.052(4) Uani 0.353(9) 1 d PU A 2
H6L H 0.3650 0.0457 0.6846 0.062 Uiso 0.353(9) 1 calc PR A 2
H6M H 0.3457 0.0514 0.5961 0.062 Uiso 0.353(9) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 N4 2.647(5) . ?
Ce1 N2 2.669(4) . ?
Ce1 N6 2.669(4) . ?
Ce1 N5 2.692(5) . ?
Ce1 N3 2.700(4) . ?
Ce1 N1 2.705(4) . ?
Ce1 S4 2.9907(12) . ?
Ce1 S8 3.0051(15) . ?
Ce1 S6 3.1413(14) . ?
Ce2 N11 2.646(4) . ?
Ce2 N10 2.662(4) . ?
Ce2 N12 2.663(4) . ?
Ce2 N9 2.663(4) . ?
Ce2 N7 2.670(5) . ?
Ce2 N8 2.712(5) . ?
Ce2 S5 3.0241(14) . ?
Ce2 S7 3.0716(14) . ?
Ce2 S1 3.0798(12) 8_455 ?
As1 S2 2.1502(14) . ?
As1 S1 2.1551(13) . ?
As1 S3 2.1633(13) . ?
As1 S4 2.1655(13) . ?
As2 S5 2.1488(16) . ?
As2 S8 2.1506(16) . ?
As2 S7 2.1535(15) . ?
As2 S6 2.1604(15) . ?
S1 Ce2 3.0798(12) 8_556 ?
N1 C3 1.474(8) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N2 C2 1.482(7) . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N7 C12 1.478(8) . ?
N7 H7D 0.9000 . ?
N7 H7E 0.9000 . ?
N8 C11 1.433(10) . ?
N8 H8B 0.9000 . ?
N8 H8C 0.9000 . ?
N9 C15 1.444(8) . ?
N9 H9C 0.9000 . ?
N9 H9D 0.9000 . ?
N10 C14 1.463(7) . ?
N10 H10D 0.9000 . ?
N10 H10E 0.9000 . ?
N11 C17 1.426(8) . ?
N11 H11C 0.9000 . ?
N11 H11D 0.9000 . ?
N12 C18 1.461(7) . ?
N12 H12B 0.9000 . ?
N12 H12C 0.9000 . ?
C1 C2 1.476(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.458(10) . ?
C2 H2A 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 C14 1.489(9) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.346(9) . ?
C14 H14A 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.498(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.435(9) . ?
C17 H17A 0.9800 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C7 C8 1.439(15) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N5 1.423(14) . ?
C8 C9 1.428(17) . ?
C8 H8A 0.9800 . ?
C9 N6 1.495(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C7B C9B 1.64(3) . ?
C7B H7L 0.9600 . ?
C7B H7M 0.9600 . ?
C7B H7N 0.9600 . ?
C8B C9B 1.57(3) . ?
C8B N5 1.59(2) . ?
C8B H8L 0.9700 . ?
C8B H8M 0.9700 . ?
C9B N6 1.42(2) . ?
C9B H9L 0.9800 . ?
N5 H5F 0.9000 . ?
N5 H5G 0.9000 . ?
N5 H5B 0.9000 . ?
N5 H5C 0.9000 . ?
N6 H6C 0.9000 . ?
N6 H6D 0.9000 . ?
N6 H6F 0.9044 . ?
N6 H6G 0.9025 . ?
C10 C12 1.383(16) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10B C11 1.551(12) . ?
C10B H10F 0.9600 . ?
C10B H10G 0.9600 . ?
C10B H10H 0.9600 . ?
C11 C12 1.417(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12F 0.9700 . ?
C12 H12G 0.9700 . ?
N3 C6B 1.45(2) . ?
N3 C6 1.531(14) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N3 H3G 0.9038 . ?
N3 H3H 0.9017 . ?
N4 C5 1.398(12) . ?
N4 C5B 1.547(19) . ?
N4 H4G 0.9000 . ?
N4 H4H 0.9000 . ?
N4 H4D 0.9041 . ?
N4 H4E 0.9022 . ?
C4 C5 1.641(12) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.465(19) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4B C5B 1.643(13) . ?
C4B H4L 0.9600 . ?
C4B H4M 0.9600 . ?
C4B H4I 0.9600 . ?
C5B C6B 1.52(3) . ?
C5B H5L 0.9800 . ?
C6B H6L 0.9700 . ?
C6B H6M 0.9700 . ?

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
N4 Ce1 N2 130.51(14) . . ?
N4 Ce1 N6 133.15(14) . . ?
N2 Ce1 N6 69.42(14) . . ?
N4 Ce1 N5 124.01(17) . . ?
N2 Ce1 N5 105.44(18) . . ?
N6 Ce1 N5 62.76(14) . . ?
N4 Ce1 N3 64.16(14) . . ?
N2 Ce1 N3 137.41(14) . . ?
N6 Ce1 N3 74.95(15) . . ?
N5 Ce1 N3 76.97(18) . . ?
N4 Ce1 N1 72.08(14) . . ?
N2 Ce1 N1 64.38(15) . . ?
N6 Ce1 N1 130.11(15) . . ?
N5 Ce1 N1 147.61(17) . . ?
N3 Ce1 N1 132.31(15) . . ?
N4 Ce1 S4 69.16(11) . . ?
N2 Ce1 S4 75.37(10) . . ?
N6 Ce1 S4 80.12(10) . . ?
N5 Ce1 S4 138.62(12) . . ?
N3 Ce1 S4 76.24(11) . . ?
N1 Ce1 S4 71.20(11) . . ?
N4 Ce1 S8 116.08(11) . . ?
N2 Ce1 S8 71.46(10) . . ?
N6 Ce1 S8 110.48(11) . . ?
N5 Ce1 S8 75.95(14) . . ?
N3 Ce1 S8 145.30(11) . . ?
N1 Ce1 S8 71.66(11) . . ?
S4 Ce1 S8 138.04(4) . . ?
N4 Ce1 S6 67.64(11) . . ?
N2 Ce1 S6 139.49(10) . . ?
N6 Ce1 S6 129.24(10) . . ?
N5 Ce1 S6 68.35(12) . . ?
N3 Ce1 S6 81.86(11) . . ?
N1 Ce1 S6 98.76(12) . . ?
S4 Ce1 S6 136.63(4) . . ?
S8 Ce1 S6 68.21(4) . . ?
N11 Ce2 N10 71.10(13) . . ?
N11 Ce2 N12 64.10(14) . . ?
N10 Ce2 N12 123.35(12) . . ?
N11 Ce2 N9 134.13(15) . . ?
N10 Ce2 N9 64.35(12) . . ?
N12 Ce2 N9 136.09(13) . . ?
N11 Ce2 N7 132.62(15) . . ?
N10 Ce2 N7 137.23(14) . . ?
N12 Ce2 N7 68.80(14) . . ?
N9 Ce2 N7 79.64(15) . . ?
N11 Ce2 N8 145.41(17) . . ?
N10 Ce2 N8 121.51(16) . . ?
N12 Ce2 N8 115.08(18) . . ?
N9 Ce2 N8 72.71(15) . . ?
N7 Ce2 N8 62.77(17) . . ?
N11 Ce2 S5 85.14(12) . . ?
N10 Ce2 S5 67.83(9) . . ?
N12 Ce2 S5 135.96(10) . . ?
N9 Ce2 S5 87.93(10) . . ?
N7 Ce2 S5 135.80(11) . . ?
N8 Ce2 S5 73.03(14) . . ?
N11 Ce2 S7 76.33(12) . . ?
N10 Ce2 S7 127.32(9) . . ?
N12 Ce2 S7 73.19(10) . . ?
N9 Ce2 S7 141.36(10) . . ?
N7 Ce2 S7 95.14(11) . . ?
N8 Ce2 S7 71.01(12) . . ?
S5 Ce2 S7 69.22(4) . . ?
N11 Ce2 S1 80.30(12) . 8_455 ?
N10 Ce2 S1 66.27(9) . 8_455 ?
N12 Ce2 S1 73.44(10) . 8_455 ?
N9 Ce2 S1 72.60(9) . 8_455 ?
N7 Ce2 S1 82.02(11) . 8_455 ?
N8 Ce2 S1 134.00(12) . 8_455 ?
S5 Ce2 S1 134.09(4) . 8_455 ?
S7 Ce2 S1 145.13(4) . 8_455 ?
S2 As1 S1 110.86(6) . . ?
S2 As1 S3 111.42(6) . . ?
S1 As1 S3 110.07(6) . . ?
S2 As1 S4 109.08(6) . . ?
S1 As1 S4 106.00(5) . . ?
S3 As1 S4 109.24(6) . . ?
S5 As2 S8 109.13(8) . . ?
S5 As2 S7 107.17(6) . . ?
S8 As2 S7 112.34(7) . . ?
S5 As2 S6 110.75(7) . . ?
S8 As2 S6 106.23(6) . . ?
S7 As2 S6 111.24(7) . . ?
As1 S1 Ce2 116.36(5) . 8_556 ?
As1 S4 Ce1 117.82(5) . . ?
As2 S5 Ce2 92.46(5) . . ?
As2 S6 Ce1 90.74(5) . . ?
As2 S7 Ce2 91.07(5) . . ?
As2 S8 Ce1 94.68(5) . . ?
C3 N1 Ce1 113.7(4) . . ?
C3 N1 H1D 108.8 . . ?
Ce1 N1 H1D 108.8 . . ?
C3 N1 H1E 108.8 . . ?
Ce1 N1 H1E 108.8 . . ?
H1D N1 H1E 107.7 . . ?
C2 N2 Ce1 116.5(4) . . ?
C2 N2 H2B 108.2 . . ?
Ce1 N2 H2B 108.2 . . ?
C2 N2 H2C 108.2 . . ?
Ce1 N2 H2C 108.2 . . ?
H2B N2 H2C 107.3 . . ?
C12 N7 Ce2 115.2(4) . . ?
C12 N7 H7D 108.5 . . ?
Ce2 N7 H7D 108.5 . . ?
C12 N7 H7E 108.5 . . ?
Ce2 N7 H7E 108.5 . . ?
H7D N7 H7E 107.5 . . ?
C11 N8 Ce2 115.1(4) . . ?
C11 N8 H8B 108.5 . . ?
Ce2 N8 H8B 108.5 . . ?
C11 N8 H8C 108.5 . . ?
Ce2 N8 H8C 108.5 . . ?
H8B N8 H8C 107.5 . . ?
C15 N9 Ce2 112.7(3) . . ?
C15 N9 H9C 109.1 . . ?
Ce2 N9 H9C 109.1 . . ?
C15 N9 H9D 109.1 . . ?
Ce2 N9 H9D 109.1 . . ?
H9C N9 H9D 107.8 . . ?
C14 N10 Ce2 116.9(3) . . ?
C14 N10 H10D 108.1 . . ?
Ce2 N10 H10D 108.1 . . ?
C14 N10 H10E 108.1 . . ?
Ce2 N10 H10E 108.1 . . ?
H10D N10 H10E 107.3 . . ?
C17 N11 Ce2 114.8(4) . . ?
C17 N11 H11C 108.6 . . ?
Ce2 N11 H11C 108.6 . . ?
C17 N11 H11D 108.6 . . ?
Ce2 N11 H11D 108.6 . . ?
H11C N11 H11D 107.6 . . ?
C18 N12 Ce2 115.9(3) . . ?
C18 N12 H12B 108.3 . . ?
Ce2 N12 H12B 108.3 . . ?
C18 N12 H12C 108.3 . . ?
Ce2 N12 H12C 108.3 . . ?
H12B N12 H12C 107.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 113.4(6) . . ?
C3 C2 N2 110.8(6) . . ?
C1 C2 N2 114.8(6) . . ?
C3 C2 H2A 105.7 . . ?
C1 C2 H2A 105.7 . . ?
N2 C2 H2A 105.7 . . ?
C2 C3 N1 114.8(6) . . ?
C2 C3 H3A 108.6 . . ?
N1 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
N1 C3 H3B 108.6 . . ?
H3A C3 H3B 107.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N10 116.3(6) . . ?
C15 C14 C13 121.8(6) . . ?
N10 C14 C13 115.3(6) . . ?
C15 C14 H14A 98.6 . . ?
N10 C14 H14A 98.6 . . ?
C13 C14 H14A 98.6 . . ?
C14 C15 N9 121.4(6) . . ?
C14 C15 H15A 107.0 . . ?
N9 C15 H15A 107.0 . . ?
C14 C15 H15B 107.0 . . ?
N9 C15 H15B 107.0 . . ?
H15A C15 H15B 106.7 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N11 C17 C18 114.2(5) . . ?
N11 C17 C16 117.4(6) . . ?
C18 C17 C16 111.6(6) . . ?
N11 C17 H17A 103.9 . . ?
C18 C17 H17A 103.9 . . ?
C16 C17 H17A 103.9 . . ?
C17 C18 N12 113.5(5) . . ?
C17 C18 H18A 108.9 . . ?
N12 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
N12 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
N5 C8 C9 111.0(12) . . ?
N5 C8 C7 119.1(11) . . ?
C9 C8 C7 111.8(11) . . ?
N5 C8 H8A 104.4 . . ?
C9 C8 H8A 104.4 . . ?
C7 C8 H8A 104.4 . . ?
C8 C9 N6 113.4(10) . . ?
C8 C9 H9A 108.9 . . ?
N6 C9 H9A 108.9 . . ?
C8 C9 H9B 108.9 . . ?
N6 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9B C7B H7L 109.5 . . ?
C9B C7B H7M 109.5 . . ?
H7L C7B H7M 109.5 . . ?
C9B C7B H7N 109.5 . . ?
H7L C7B H7N 109.5 . . ?
H7M C7B H7N 109.5 . . ?
C9B C8B N5 101.1(14) . . ?
C9B C8B H8L 111.6 . . ?
N5 C8B H8L 111.6 . . ?
C9B C8B H8M 111.6 . . ?
N5 C8B H8M 111.6 . . ?
H8L C8B H8M 109.4 . . ?
N6 C9B C8B 105.0(17) . . ?
N6 C9B C7B 111.8(15) . . ?
C8B C9B C7B 88.6(14) . . ?
N6 C9B H9L 116.0 . . ?
C8B C9B H9L 116.0 . . ?
C7B C9B H9L 116.0 . . ?
C8 N5 Ce1 117.0(6) . . ?
C8B N5 Ce1 114.4(9) . . ?
C8 N5 H5F 108.1 . . ?
C8B N5 H5F 82.3 . . ?
Ce1 N5 H5F 108.1 . . ?
C8 N5 H5G 108.1 . . ?
C8B N5 H5G 130.9 . . ?
Ce1 N5 H5G 108.1 . . ?
H5F N5 H5G 107.3 . . ?
C8 N5 H5B 127.9 . . ?
C8B N5 H5B 108.7 . . ?
Ce1 N5 H5B 108.7 . . ?
H5G N5 H5B 78.6 . . ?
C8 N5 H5C 80.9 . . ?
C8B N5 H5C 108.7 . . ?
Ce1 N5 H5C 108.7 . . ?
H5F N5 H5C 132.2 . . ?
H5B N5 H5C 107.6 . . ?
C9B N6 Ce1 115.0(9) . . ?
C9 N6 Ce1 115.7(5) . . ?
C9B N6 H6C 80.2 . . ?
C9 N6 H6C 108.4 . . ?
Ce1 N6 H6C 108.4 . . ?
C9B N6 H6D 130.8 . . ?
C9 N6 H6D 108.4 . . ?
Ce1 N6 H6D 108.4 . . ?
H6C N6 H6D 107.4 . . ?
C9B N6 H6F 107.1 . . ?
C9 N6 H6F 129.2 . . ?
Ce1 N6 H6F 108.5 . . ?
H6D N6 H6F 78.8 . . ?
C9B N6 H6G 111.5 . . ?
C9 N6 H6G 82.8 . . ?
Ce1 N6 H6G 107.1 . . ?
H6C N6 H6G 132.6 . . ?
H6F N6 H6G 107.4 . . ?
C12 C10 H10A 109.5 . . ?
C12 C10 H10B 109.5 . . ?
C12 C10 H10C 109.5 . . ?
C11 C10B H10F 109.5 . . ?
C11 C10B H10G 109.5 . . ?
H10F C10B H10G 109.5 . . ?
C11 C10B H10H 109.5 . . ?
H10F C10B H10H 109.5 . . ?
H10G C10B H10H 109.5 . . ?
C12 C11 N8 110.6(7) . . ?
C12 C11 C10B 103.6(9) . . ?
N8 C11 C10B 124.1(8) . . ?
C12 C11 H11A 109.5 . . ?
N8 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
N8 C11 H11B 109.5 . . ?
C10B C11 H11B 98.4 . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11F 105.8 . . ?
N8 C11 H11F 105.8 . . ?
C10B C11 H11F 105.8 . . ?
H11A C11 H11F 115.6 . . ?
C10 C12 C11 107.5(10) . . ?
C10 C12 N7 119.2(11) . . ?
C11 C12 N7 113.5(6) . . ?
C10 C12 H12A 105.1 . . ?
C11 C12 H12A 105.1 . . ?
N7 C12 H12A 105.1 . . ?
C11 C12 H12F 108.9 . . ?
N7 C12 H12F 108.9 . . ?
H12A C12 H12F 115.4 . . ?
C10 C12 H12G 97.4 . . ?
C11 C12 H12G 108.9 . . ?
N7 C12 H12G 108.9 . . ?
H12F C12 H12G 107.7 . . ?
C6B N3 Ce1 115.2(9) . . ?
C6 N3 Ce1 110.6(5) . . ?
C6B N3 H3C 127.8 . . ?
C6 N3 H3C 109.5 . . ?
Ce1 N3 H3C 109.5 . . ?
C6B N3 H3D 81.1 . . ?
C6 N3 H3D 109.5 . . ?
Ce1 N3 H3D 109.5 . . ?
H3C N3 H3D 108.1 . . ?
C6B N3 H3G 111.0 . . ?
C6 N3 H3G 86.0 . . ?
Ce1 N3 H3G 106.6 . . ?
H3D N3 H3G 131.6 . . ?
C6B N3 H3H 107.9 . . ?
C6 N3 H3H 132.6 . . ?
Ce1 N3 H3H 108.6 . . ?
H3C N3 H3H 80.6 . . ?
H3G N3 H3H 107.2 . . ?
C5 N4 Ce1 117.9(5) . . ?
C5B N4 Ce1 112.6(8) . . ?
C5 N4 H4G 107.8 . . ?
C5B N4 H4G 132.7 . . ?
Ce1 N4 H4G 107.8 . . ?
C5 N4 H4H 107.8 . . ?
C5B N4 H4H 82.9 . . ?
Ce1 N4 H4H 107.8 . . ?
H4G N4 H4H 107.2 . . ?
C5 N4 H4D 110.1 . . ?
C5B N4 H4D 133.7 . . ?
Ce1 N4 H4D 108.8 . . ?
H4H N4 H4D 103.4 . . ?
C5 N4 H4E 106.4 . . ?
C5B N4 H4E 80.5 . . ?
Ce1 N4 H4E 105.8 . . ?
H4G N4 H4E 111.1 . . ?
H4D N4 H4E 107.3 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 C6 111.3(11) . . ?
N4 C5 C4 114.9(13) . . ?
C6 C5 C4 102.2(13) . . ?
N4 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
C5 C6 N3 110.4(9) . . ?
C5 C6 H6A 109.6 . . ?
N3 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
N3 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C5B C4B H4L 109.5 . . ?
C5B C4B H4M 109.5 . . ?
H4L C4B H4M 109.5 . . ?
C5B C4B H4I 109.5 . . ?
H4L C4B H4I 109.5 . . ?
H4M C4B H4I 109.5 . . ?
C6B C5B N4 106.1(14) . . ?
C6B C5B C4B 107(2) . . ?
N4 C5B C4B 96.6(17) . . ?
C6B C5B H5L 115.1 . . ?
N4 C5B H5L 115.1 . . ?
C4B C5B H5L 115.1 . . ?
N3 C6B C5B 107.6(16) . . ?
N3 C6B H6L 110.2 . . ?
C5B C6B H6L 110.2 . . ?
N3 C6B H6M 110.2 . . ?
C5B C6B H6M 110.2 . . ?
H6L C6B H6M 108.5 . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.724
_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_Ib
_database_code_depnum_ccdc_archive 'CCDC 1403232'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H60 As2 N12 Pr2 S8'
_chemical_formula_sum            'C18 H60 As2 N12 Pr2 S8'
_chemical_formula_weight         1132.92

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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   38.7385(4)
_cell_length_b                   11.99890(10)
_cell_length_c                   20.6700(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.7490(10)
_cell_angle_gamma                90.00
_cell_volume                     8170.11(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    26782
_cell_measurement_theta_min      3.5090
_cell_measurement_theta_max      28.8040

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4512
_exptl_absorpt_coefficient_mu    4.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5983
_exptl_absorpt_correction_T_max  0.7480
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59197
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         27.10
_reflns_number_total             8980
_reflns_number_gt                7716
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The command TWIN -10-2 0-10 001 is refined the pseudo-merohedral 
twinning, which makes R1/wR2 significantly lower.
The DELU restraint prevents the thermal ellipsoids of all 
adjacent C atoms from adopting different orientations.  
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)+(0.0750P)²+4.0000P] 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         8980
_refine_ls_number_parameters     451
_refine_ls_number_restraints     187
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.1039
_refine_ls_wR_factor_gt          0.0976
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.300013(6) 0.233537(16) 0.723472(12) 0.02935(8) Uani 1 1 d . A .
Pr2 Pr 0.069685(6) 0.272423(16) 0.494025(11) 0.02777(8) Uani 1 1 d . . .
As1 As 0.434167(10) 0.23598(3) 0.86870(2) 0.02738(10) Uani 1 1 d . . .
As2 As 0.183625(11) 0.24106(3) 0.61224(2) 0.03665(11) Uani 1 1 d . . .
S1 S 0.48550(2) 0.13184(8) 0.94237(5) 0.0347(2) Uani 1 1 d . . .
S2 S 0.43242(3) 0.38030(8) 0.92846(6) 0.0451(2) Uani 1 1 d . . .
S3 S 0.43581(3) 0.28211(10) 0.76902(6) 0.0484(3) Uani 1 1 d . . .
S4 S 0.38076(3) 0.13532(7) 0.83398(6) 0.0376(2) Uani 1 1 d . . .
S5 S 0.14976(3) 0.37372(10) 0.53478(8) 0.0614(4) Uani 1 1 d . . .
S6 S 0.21959(3) 0.15413(10) 0.57669(7) 0.0543(3) Uani 1 1 d . . .
S7 S 0.14037(3) 0.13186(9) 0.61516(7) 0.0507(3) Uani 1 1 d . . .
S8 S 0.22621(3) 0.31076(12) 0.72208(7) 0.0613(3) Uani 1 1 d . . .
N1 N 0.29391(12) 0.1176(3) 0.8275(2) 0.0530(9) Uani 1 1 d . . .
H1D H 0.2674 0.1097 0.8112 0.064 Uiso 1 1 calc R . .
H1E H 0.3041 0.0490 0.8310 0.064 Uiso 1 1 calc R . .
N2 N 0.32371(10) 0.3388(3) 0.85307(19) 0.0459(8) Uani 1 1 d . . .
H2B H 0.3510 0.3434 0.8793 0.055 Uiso 1 1 calc R . .
H2C H 0.3140 0.4088 0.8419 0.055 Uiso 1 1 calc R . .
N7 N 0.02557(11) 0.0994(3) 0.4131(2) 0.0543(9) Uani 1 1 d . . .
H7D H 0.0253 0.0488 0.4450 0.065 Uiso 1 1 calc R . .
H7E H -0.0002 0.1224 0.3816 0.065 Uiso 1 1 calc R . .
N8 N 0.09993(12) 0.1474(4) 0.4266(2) 0.0652(11) Uani 1 1 d . B .
H8B H 0.0962 0.1841 0.3854 0.078 Uiso 1 1 calc R . .
H8C H 0.1269 0.1397 0.4591 0.078 Uiso 1 1 calc R . .
N9 N 0.03842(10) 0.3491(3) 0.35390(17) 0.0403(7) Uani 1 1 d . . .
H9C H 0.0476 0.3076 0.3297 0.048 Uiso 1 1 calc R . .
H9D H 0.0112 0.3422 0.3285 0.048 Uiso 1 1 calc R . .
N10 N 0.06540(8) 0.4924(3) 0.48056(16) 0.0348(7) Uani 1 1 d . . .
H10D H 0.0491 0.5175 0.4963 0.042 Uiso 1 1 calc R . .
H10E H 0.0903 0.5205 0.5123 0.042 Uiso 1 1 calc R . .
N11 N 0.08509(12) 0.3605(3) 0.6231(2) 0.0536(9) Uani 1 1 d . . .
H11C H 0.1112 0.3470 0.6588 0.064 Uiso 1 1 calc R . .
H11D H 0.0820 0.4348 0.6171 0.064 Uiso 1 1 calc R . .
N12 N 0.04230(10) 0.1587(3) 0.56809(19) 0.0423(8) Uani 1 1 d . . .
H12B H 0.0150 0.1566 0.5389 0.051 Uiso 1 1 calc R . .
H12C H 0.0513 0.0881 0.5737 0.051 Uiso 1 1 calc R . .
C1 C 0.3315(2) 0.3376(5) 0.9806(3) 0.0858(18) Uani 1 1 d . . .
H1A H 0.3241 0.4147 0.9770 0.129 Uiso 1 1 calc R . .
H1B H 0.3604 0.3315 1.0042 0.129 Uiso 1 1 calc R . .
H1C H 0.3232 0.2985 1.0107 0.129 Uiso 1 1 calc R . .
C2 C 0.31139(18) 0.2887(5) 0.9041(3) 0.0694(15) Uani 1 1 d . . .
H2A H 0.2824 0.3051 0.8805 0.083 Uiso 1 1 calc R . .
C3 C 0.3147(2) 0.1675(4) 0.9039(3) 0.0762(17) Uani 1 1 d . . .
H3A H 0.3034 0.1358 0.9321 0.091 Uiso 1 1 calc R . .
H3B H 0.3432 0.1474 0.9303 0.091 Uiso 1 1 calc R . .
C13 C 0.05983(18) 0.6573(4) 0.4035(3) 0.0703(14) Uani 1 1 d . . .
H13A H 0.0577 0.6967 0.4417 0.105 Uiso 1 1 calc R . .
H13B H 0.0408 0.6877 0.3543 0.105 Uiso 1 1 calc R . .
H13C H 0.0869 0.6650 0.4133 0.105 Uiso 1 1 calc R . .
C14 C 0.0507(2) 0.5365(4) 0.4053(3) 0.0838(19) Uani 1 1 d . . .
H14A H 0.0217 0.5420 0.3870 0.101 Uiso 1 1 calc R . .
C15 C 0.0486(2) 0.4637(5) 0.3527(3) 0.097(2) Uani 1 1 d . . .
H15A H 0.0748 0.4649 0.3570 0.116 Uiso 1 1 calc R . .
H15B H 0.0290 0.4931 0.3028 0.116 Uiso 1 1 calc R . .
C16 C 0.0693(2) 0.3625(6) 0.7255(3) 0.0845(18) Uani 1 1 d . . .
H16A H 0.0788 0.4381 0.7327 0.127 Uiso 1 1 calc R . .
H16B H 0.0899 0.3166 0.7652 0.127 Uiso 1 1 calc R . .
H16C H 0.0450 0.3592 0.7270 0.127 Uiso 1 1 calc R . .
C17 C 0.06060(19) 0.3214(5) 0.6501(3) 0.0709(16) Uani 1 1 d . . .
H17A H 0.0338 0.3529 0.6141 0.085 Uiso 1 1 calc R . .
C18 C 0.05349(19) 0.2005(5) 0.6418(3) 0.0696(15) Uani 1 1 d . . .
H18A H 0.0780 0.1628 0.6801 0.083 Uiso 1 1 calc R . .
H18B H 0.0321 0.1826 0.6512 0.083 Uiso 1 1 calc R . .
C7 C 0.2751(3) 0.5808(6) 0.5761(5) 0.073(3) Uani 0.625(7) 1 d PU A 1
H7A H 0.2463 0.5919 0.5510 0.110 Uiso 0.625(7) 1 calc PR A 1
H7B H 0.2817 0.5554 0.5399 0.110 Uiso 0.625(7) 1 calc PR A 1
H7C H 0.2888 0.6499 0.5980 0.110 Uiso 0.625(7) 1 calc PR A 1
C8 C 0.2879(3) 0.4977(8) 0.6360(7) 0.068(3) Uani 0.625(7) 1 d PU A 1
H8A H 0.2837 0.5306 0.6747 0.082 Uiso 0.625(7) 1 calc PR A 1
C9 C 0.3324(3) 0.4791(7) 0.6729(6) 0.057(2) Uani 0.625(7) 1 d PU A 1
H9A H 0.3464 0.5501 0.6886 0.068 Uiso 0.625(7) 1 calc PR A 1
H9B H 0.3379 0.4454 0.6366 0.068 Uiso 0.625(7) 1 calc PR A 1
C7B C 0.3549(4) 0.5864(11) 0.6858(9) 0.075(4) Uani 0.375(7) 1 d PU A 2
H7L H 0.3675 0.6419 0.7250 0.113 Uiso 0.375(7) 1 calc PR A 2
H7M H 0.3375 0.6221 0.6376 0.113 Uiso 0.375(7) 1 calc PR A 2
H7N H 0.3755 0.5447 0.6838 0.113 Uiso 0.375(7) 1 calc PR A 2
C8B C 0.2997(5) 0.4745(11) 0.6194(8) 0.044(3) Uani 0.375(7) 1 d PU A 2
H8L H 0.2862 0.5407 0.5899 0.053 Uiso 0.375(7) 1 calc PR A 2
H8M H 0.3144 0.4399 0.5986 0.053 Uiso 0.375(7) 1 calc PR A 2
C9B C 0.3290(4) 0.5050(11) 0.7038(8) 0.045(3) Uani 0.375(7) 1 d PU A 2
H9L H 0.3155 0.5430 0.7265 0.054 Uiso 0.375(7) 1 calc PR A 2
N5 N 0.26859(12) 0.3927(3) 0.6175(3) 0.0748(13) Uani 1 1 d . . .
H5F H 0.2682 0.3670 0.5762 0.090 Uiso 0.625(7) 1 calc PR A 1
H5G H 0.2426 0.4032 0.6040 0.090 Uiso 0.625(7) 1 calc PR A 1
H5B H 0.2550 0.3601 0.5714 0.090 Uiso 0.375(7) 1 calc PR A 2
H5C H 0.2505 0.4317 0.6230 0.090 Uiso 0.375(7) 1 calc PR A 2
N6 N 0.34776(10) 0.4045(3) 0.7409(2) 0.0484(8) Uani 1 1 d . . .
H6C H 0.3515 0.4459 0.7804 0.058 Uiso 0.625(7) 1 calc PR A 1
H6D H 0.3722 0.3777 0.7530 0.058 Uiso 0.625(7) 1 calc PR A 1
H6F H 0.3636 0.4201 0.7910 0.058 Uiso 0.375(7) 1 d PR A 2
H6G H 0.3643 0.3819 0.7250 0.058 Uiso 0.375(7) 1 d PR A 2
C10 C 0.0228(4) -0.0586(10) 0.3355(7) 0.074(4) Uani 0.441(9) 1 d PU B 1
H10A H -0.0063 -0.0523 0.3073 0.111 Uiso 0.441(9) 1 calc PR B 1
H10B H 0.0312 -0.1127 0.3753 0.111 Uiso 0.441(9) 1 calc PR B 1
H10C H 0.0316 -0.0818 0.3020 0.111 Uiso 0.441(9) 1 calc PR B 1
C10B C 0.0889(3) -0.0425(7) 0.3528(6) 0.074(3) Uani 0.559(9) 1 d PU B 2
H10F H 0.1174 -0.0578 0.3767 0.111 Uiso 0.559(9) 1 calc PR B 2
H10G H 0.0791 -0.0086 0.3041 0.111 Uiso 0.559(9) 1 calc PR B 2
H10H H 0.0745 -0.1109 0.3462 0.111 Uiso 0.559(9) 1 calc PR B 2
C11 C 0.0819(2) 0.0374(6) 0.4033(4) 0.0892(19) Uani 1 1 d . . .
H11A H 0.0892 0.0050 0.3690 0.107 Uiso 0.441(9) 1 calc PR B 1
H11B H 0.0925 -0.0105 0.4475 0.107 Uiso 0.441(9) 1 calc PR B 1
H11F H 0.0910 -0.0034 0.4506 0.107 Uiso 0.559(9) 1 calc PR B 2
C12 C 0.03989(17) 0.0438(5) 0.3670(3) 0.0790(17) Uani 1 1 d . B .
H12A H 0.0314 0.0933 0.3235 0.095 Uiso 0.441(9) 1 calc PR B 1
H12F H 0.0288 -0.0310 0.3546 0.095 Uiso 0.559(9) 1 calc PR B 2
H12G H 0.0294 0.0843 0.3196 0.095 Uiso 0.559(9) 1 calc PR B 2
N3 N 0.33037(12) 0.1851(3) 0.6369(2) 0.0525(9) Uani 1 1 d . . .
H3C H 0.3215 0.2355 0.5992 0.063 Uiso 0.625(7) 1 calc PR A 1
H3D H 0.3576 0.1894 0.6652 0.063 Uiso 0.625(7) 1 calc PR A 1
H3G H 0.3123 0.2094 0.5894 0.063 Uiso 0.375(7) 1 d PR A 2
H3H H 0.3533 0.2246 0.6540 0.063 Uiso 0.375(7) 1 d PR A 2
N4 N 0.30135(10) 0.0205(3) 0.6946(2) 0.0458(8) Uani 1 1 d . . .
H4G H 0.3107 -0.0172 0.7384 0.055 Uiso 0.625(7) 1 calc PR A 1
H4H H 0.2756 -0.0016 0.6627 0.055 Uiso 0.625(7) 1 calc PR A 1
H4D H 0.3096 -0.0183 0.7378 0.055 Uiso 0.375(7) 1 d PR A 2
H4E H 0.2754 0.0010 0.6610 0.055 Uiso 0.375(7) 1 d PR A 2
C4 C 0.3085(6) -0.1286(10) 0.6162(10) 0.080(5) Uani 0.625(7) 1 d PDU A 1
H4A H 0.3061 -0.1840 0.6472 0.120 Uiso 0.625(7) 1 calc PR A 1
H4B H 0.3275 -0.1532 0.6030 0.120 Uiso 0.625(7) 1 calc PR A 1
H4C H 0.2824 -0.1171 0.5707 0.120 Uiso 0.625(7) 1 calc PR A 1
C5 C 0.3242(3) -0.0124(8) 0.6633(6) 0.061(2) Uani 0.625(7) 1 d PDU A 1
H5A H 0.3530 -0.0176 0.7030 0.073 Uiso 0.625(7) 1 calc PR A 1
C6 C 0.3180(3) 0.0693(8) 0.6029(6) 0.061(2) Uani 0.625(7) 1 d PU A 1
H6A H 0.2896 0.0695 0.5622 0.073 Uiso 0.625(7) 1 calc PR A 1
H6B H 0.3341 0.0472 0.5817 0.073 Uiso 0.625(7) 1 calc PR A 1
C4B C 0.3196(8) -0.1294(15) 0.6405(15) 0.066(6) Uani 0.375(7) 1 d PDU A 2
H4L H 0.3205 -0.1551 0.6853 0.099 Uiso 0.375(7) 1 calc PR A 2
H4M H 0.3460 -0.1369 0.6474 0.099 Uiso 0.375(7) 1 calc PR A 2
H4I H 0.3004 -0.1731 0.5975 0.099 Uiso 0.375(7) 1 calc PR A 2
C5B C 0.3060(5) 0.0009(12) 0.6256(9) 0.048(3) Uani 0.375(7) 1 d PDU A 2
H5L H 0.2807 0.0135 0.5767 0.057 Uiso 0.375(7) 1 calc PR A 2
C6B C 0.3411(5) 0.0698(12) 0.6355(10) 0.053(3) Uani 0.375(7) 1 d PU A 2
H6L H 0.3659 0.0505 0.6827 0.064 Uiso 0.375(7) 1 calc PR A 2
H6M H 0.3451 0.0571 0.5936 0.064 Uiso 0.375(7) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 N4 2.632(3) . ?
Pr1 N2 2.650(3) . ?
Pr1 N6 2.657(3) . ?
Pr1 N5 2.669(4) . ?
Pr1 N3 2.672(3) . ?
Pr1 N1 2.674(3) . ?
Pr1 S4 2.9784(9) . ?
Pr1 S8 2.9912(11) . ?
Pr1 S6 3.1418(11) . ?
Pr2 N11 2.629(3) . ?
Pr2 N9 2.648(3) . ?
Pr2 N7 2.650(4) . ?
Pr2 N10 2.650(3) . ?
Pr2 N12 2.654(3) . ?
Pr2 N8 2.699(4) . ?
Pr2 S5 3.0097(10) . ?
Pr2 S7 3.0653(10) . ?
Pr2 S1 3.0711(8) 8_455 ?
As1 S2 2.1488(10) . ?
As1 S1 2.1558(9) . ?
As1 S4 2.1660(9) . ?
As1 S3 2.1665(11) . ?
As2 S5 2.1466(11) . ?
As2 S8 2.1525(12) . ?
As2 S7 2.1527(11) . ?
As2 S6 2.1558(11) . ?
S1 Pr2 3.0711(8) 8_556 ?
N1 C3 1.470(6) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N2 C2 1.493(6) . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N7 C12 1.488(6) . ?
N7 H7D 0.9000 . ?
N7 H7E 0.9000 . ?
N8 C11 1.451(8) . ?
N8 H8B 0.9000 . ?
N8 H8C 0.9000 . ?
N9 C15 1.434(6) . ?
N9 H9C 0.9000 . ?
N9 H9D 0.9000 . ?
N10 C14 1.446(5) . ?
N10 H10D 0.9000 . ?
N10 H10E 0.9000 . ?
N11 C17 1.412(6) . ?
N11 H11C 0.9000 . ?
N11 H11D 0.9000 . ?
N12 C18 1.438(6) . ?
N12 H12B 0.9000 . ?
N12 H12C 0.9000 . ?
C1 C2 1.468(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.461(8) . ?
C2 H2A 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 C14 1.498(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.364(7) . ?
C14 H14A 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.492(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.469(8) . ?
C17 H17A 0.9800 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C7 C8 1.458(12) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N5 1.411(10) . ?
C8 C9 1.489(13) . ?
C8 H8A 0.9800 . ?
C9 N6 1.500(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C7B C9B 1.580(19) . ?
C7B H7L 0.9600 . ?
C7B H7M 0.9600 . ?
C7B H7N 0.9600 . ?
C8B N5 1.538(15) . ?
C8B C9B 1.54(2) . ?
C8B H8L 0.9700 . ?
C8B H8M 0.9700 . ?
C9B N6 1.409(14) . ?
C9B H9L 0.9800 . ?
N5 H5F 0.9000 . ?
N5 H5G 0.9000 . ?
N5 H5B 0.9000 . ?
N5 H5C 0.9000 . ?
N6 H6C 0.9000 . ?
N6 H6D 0.9000 . ?
N6 H6F 0.9035 . ?
N6 H6G 0.9007 . ?
C10 C12 1.386(11) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10B C11 1.541(9) . ?
C10B H10F 0.9600 . ?
C10B H10G 0.9600 . ?
C10B H10H 0.9600 . ?
C11 C12 1.391(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12F 0.9700 . ?
C12 H12G 0.9700 . ?
N3 C6B 1.449(14) . ?
N3 C6 1.517(10) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N3 H3G 0.9029 . ?
N3 H3H 0.9003 . ?
N4 C5 1.401(11) . ?
N4 C5B 1.546(14) . ?
N4 H4G 0.9000 . ?
N4 H4H 0.9000 . ?
N4 H4D 0.9030 . ?
N4 H4E 0.9010 . ?
C4 C5 1.623(10) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.503(15) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4B C5B 1.627(12) . ?
C4B H4L 0.9600 . ?
C4B H4M 0.9600 . ?
C4B H4I 0.9600 . ?
C5B C6B 1.51(2) . ?
C5B H5L 0.9800 . ?
C6B H6L 0.9700 . ?
C6B H6M 0.9700 . ?

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
N4 Pr1 N2 130.85(11) . . ?
N4 Pr1 N6 133.27(11) . . ?
N2 Pr1 N6 69.46(11) . . ?
N4 Pr1 N5 124.33(14) . . ?
N2 Pr1 N5 104.75(14) . . ?
N6 Pr1 N5 62.80(11) . . ?
N4 Pr1 N3 64.46(11) . . ?
N2 Pr1 N3 137.74(11) . . ?
N6 Pr1 N3 74.82(11) . . ?
N5 Pr1 N3 77.12(14) . . ?
N4 Pr1 N1 72.40(11) . . ?
N2 Pr1 N1 64.22(11) . . ?
N6 Pr1 N1 129.99(12) . . ?
N5 Pr1 N1 146.85(13) . . ?
N3 Pr1 N1 133.00(12) . . ?
N4 Pr1 S4 69.60(8) . . ?
N2 Pr1 S4 75.40(8) . . ?
N6 Pr1 S4 80.00(8) . . ?
N5 Pr1 S4 138.94(9) . . ?
N3 Pr1 S4 76.87(9) . . ?
N1 Pr1 S4 71.28(8) . . ?
N4 Pr1 S8 115.56(8) . . ?
N2 Pr1 S8 71.53(8) . . ?
N6 Pr1 S8 110.85(8) . . ?
N5 Pr1 S8 75.50(11) . . ?
N3 Pr1 S8 144.71(9) . . ?
N1 Pr1 S8 71.36(9) . . ?
S4 Pr1 S8 137.97(3) . . ?
N4 Pr1 S6 67.32(8) . . ?
N2 Pr1 S6 139.52(7) . . ?
N6 Pr1 S6 129.11(8) . . ?
N5 Pr1 S6 68.41(9) . . ?
N3 Pr1 S6 81.34(9) . . ?
N1 Pr1 S6 99.01(9) . . ?
S4 Pr1 S6 136.73(3) . . ?
S8 Pr1 S6 68.14(3) . . ?
N11 Pr2 N9 134.35(11) . . ?
N11 Pr2 N7 133.02(11) . . ?
N9 Pr2 N7 79.03(11) . . ?
N11 Pr2 N10 71.00(10) . . ?
N9 Pr2 N10 64.63(9) . . ?
N7 Pr2 N10 136.89(11) . . ?
N11 Pr2 N12 64.38(10) . . ?
N9 Pr2 N12 135.91(10) . . ?
N7 Pr2 N12 68.93(11) . . ?
N10 Pr2 N12 123.43(9) . . ?
N11 Pr2 N8 144.97(13) . . ?
N9 Pr2 N8 72.62(11) . . ?
N7 Pr2 N8 63.22(12) . . ?
N10 Pr2 N8 121.30(11) . . ?
N12 Pr2 N8 115.22(13) . . ?
N11 Pr2 S5 84.46(9) . . ?
N9 Pr2 S5 88.66(7) . . ?
N7 Pr2 S5 136.09(8) . . ?
N10 Pr2 S5 68.01(6) . . ?
N12 Pr2 S5 135.42(8) . . ?
N8 Pr2 S5 72.87(10) . . ?
N11 Pr2 S7 76.36(9) . . ?
N9 Pr2 S7 141.50(7) . . ?
N7 Pr2 S7 94.98(9) . . ?
N10 Pr2 S7 127.84(7) . . ?
N12 Pr2 S7 72.68(7) . . ?
N8 Pr2 S7 70.86(9) . . ?
S5 Pr2 S7 69.36(3) . . ?
N11 Pr2 S1 80.50(9) . 8_455 ?
N9 Pr2 S1 72.48(7) . 8_455 ?
N7 Pr2 S1 81.92(8) . 8_455 ?
N10 Pr2 S1 66.08(6) . 8_455 ?
N12 Pr2 S1 73.69(7) . 8_455 ?
N8 Pr2 S1 134.31(9) . 8_455 ?
S5 Pr2 S1 134.09(3) . 8_455 ?
S7 Pr2 S1 144.94(3) . 8_455 ?
S2 As1 S1 110.94(4) . . ?
S2 As1 S4 109.04(4) . . ?
S1 As1 S4 106.02(4) . . ?
S2 As1 S3 111.49(5) . . ?
S1 As1 S3 110.01(4) . . ?
S4 As1 S3 109.16(4) . . ?
S5 As2 S8 109.09(6) . . ?
S5 As2 S7 107.04(4) . . ?
S8 As2 S7 112.50(5) . . ?
S5 As2 S6 110.82(6) . . ?
S8 As2 S6 105.87(4) . . ?
S7 As2 S6 111.55(5) . . ?
As1 S1 Pr2 116.41(4) . 8_556 ?
As1 S4 Pr1 117.91(4) . . ?
As2 S5 Pr2 92.56(4) . . ?
As2 S6 Pr1 90.82(4) . . ?
As2 S7 Pr2 90.93(3) . . ?
As2 S8 Pr1 95.05(4) . . ?
C3 N1 Pr1 115.0(3) . . ?
C3 N1 H1D 108.5 . . ?
Pr1 N1 H1D 108.5 . . ?
C3 N1 H1E 108.5 . . ?
Pr1 N1 H1E 108.5 . . ?
H1D N1 H1E 107.5 . . ?
C2 N2 Pr1 116.9(3) . . ?
C2 N2 H2B 108.1 . . ?
Pr1 N2 H2B 108.1 . . ?
C2 N2 H2C 108.1 . . ?
Pr1 N2 H2C 108.1 . . ?
H2B N2 H2C 107.3 . . ?
C12 N7 Pr2 114.9(3) . . ?
C12 N7 H7D 108.5 . . ?
Pr2 N7 H7D 108.5 . . ?
C12 N7 H7E 108.5 . . ?
Pr2 N7 H7E 108.5 . . ?
H7D N7 H7E 107.5 . . ?
C11 N8 Pr2 114.4(3) . . ?
C11 N8 H8B 108.7 . . ?
Pr2 N8 H8B 108.7 . . ?
C11 N8 H8C 108.7 . . ?
Pr2 N8 H8C 108.7 . . ?
H8B N8 H8C 107.6 . . ?
C15 N9 Pr2 112.4(3) . . ?
C15 N9 H9C 109.1 . . ?
Pr2 N9 H9C 109.1 . . ?
C15 N9 H9D 109.1 . . ?
Pr2 N9 H9D 109.1 . . ?
H9C N9 H9D 107.9 . . ?
C14 N10 Pr2 116.4(3) . . ?
C14 N10 H10D 108.2 . . ?
Pr2 N10 H10D 108.2 . . ?
C14 N10 H10E 108.2 . . ?
Pr2 N10 H10E 108.2 . . ?
H10D N10 H10E 107.3 . . ?
C17 N11 Pr2 115.3(3) . . ?
C17 N11 H11C 108.4 . . ?
Pr2 N11 H11C 108.4 . . ?
C17 N11 H11D 108.4 . . ?
Pr2 N11 H11D 108.4 . . ?
H11C N11 H11D 107.5 . . ?
C18 N12 Pr2 116.3(3) . . ?
C18 N12 H12B 108.2 . . ?
Pr2 N12 H12B 108.2 . . ?
C18 N12 H12C 108.2 . . ?
Pr2 N12 H12C 108.2 . . ?
H12B N12 H12C 107.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 113.8(5) . . ?
C3 C2 N2 109.7(4) . . ?
C1 C2 N2 114.4(4) . . ?
C3 C2 H2A 106.1 . . ?
C1 C2 H2A 106.1 . . ?
N2 C2 H2A 106.1 . . ?
C2 C3 N1 114.1(4) . . ?
C2 C3 H3A 108.7 . . ?
N1 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
N1 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N10 116.6(4) . . ?
C15 C14 C13 121.0(5) . . ?
N10 C14 C13 114.6(4) . . ?
C15 C14 H14A 99.3 . . ?
N10 C14 H14A 99.3 . . ?
C13 C14 H14A 99.3 . . ?
C14 C15 N9 120.0(5) . . ?
C14 C15 H15A 107.3 . . ?
N9 C15 H15A 107.3 . . ?
C14 C15 H15B 107.3 . . ?
N9 C15 H15B 107.3 . . ?
H15A C15 H15B 106.9 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N11 C17 C18 113.9(4) . . ?
N11 C17 C16 118.2(5) . . ?
C18 C17 C16 112.0(5) . . ?
N11 C17 H17A 103.5 . . ?
C18 C17 H17A 103.5 . . ?
C16 C17 H17A 103.5 . . ?
N12 C18 C17 113.8(4) . . ?
N12 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
N12 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
N5 C8 C7 119.0(9) . . ?
N5 C8 C9 108.1(8) . . ?
C7 C8 C9 108.8(9) . . ?
N5 C8 H8A 106.8 . . ?
C7 C8 H8A 106.8 . . ?
C9 C8 H8A 106.8 . . ?
C8 C9 N6 110.6(7) . . ?
C8 C9 H9A 109.5 . . ?
N6 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
N6 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9B C7B H7L 109.5 . . ?
C9B C7B H7M 109.5 . . ?
H7L C7B H7M 109.5 . . ?
C9B C7B H7N 109.5 . . ?
H7L C7B H7N 109.5 . . ?
H7M C7B H7N 109.5 . . ?
N5 C8B C9B 106.3(10) . . ?
N5 C8B H8L 110.5 . . ?
C9B C8B H8L 110.5 . . ?
N5 C8B H8M 110.5 . . ?
C9B C8B H8M 110.5 . . ?
H8L C8B H8M 108.7 . . ?
N6 C9B C8B 105.9(10) . . ?
N6 C9B C7B 116.5(11) . . ?
C8B C9B C7B 93.5(11) . . ?
N6 C9B H9L 113.0 . . ?
C8B C9B H9L 113.0 . . ?
C7B C9B H9L 113.0 . . ?
C8 N5 Pr1 117.9(5) . . ?
C8B N5 Pr1 115.0(6) . . ?
C8 N5 H5F 107.8 . . ?
C8B N5 H5F 82.3 . . ?
Pr1 N5 H5F 107.8 . . ?
C8 N5 H5G 107.8 . . ?
C8B N5 H5G 130.7 . . ?
Pr1 N5 H5G 107.8 . . ?
H5F N5 H5G 107.2 . . ?
C8 N5 H5B 127.3 . . ?
C8B N5 H5B 108.5 . . ?
Pr1 N5 H5B 108.5 . . ?
H5G N5 H5B 78.4 . . ?
C8 N5 H5C 80.7 . . ?
C8B N5 H5C 108.5 . . ?
Pr1 N5 H5C 108.5 . . ?
H5F N5 H5C 132.3 . . ?
H5B N5 H5C 107.5 . . ?
C9B N6 Pr1 117.6(6) . . ?
C9 N6 Pr1 115.4(4) . . ?
C9B N6 H6C 79.2 . . ?
C9 N6 H6C 108.4 . . ?
Pr1 N6 H6C 108.4 . . ?
C9B N6 H6D 128.6 . . ?
C9 N6 H6D 108.4 . . ?
Pr1 N6 H6D 108.4 . . ?
H6C N6 H6D 107.5 . . ?
C9B N6 H6F 106.9 . . ?
C9 N6 H6F 130.3 . . ?
Pr1 N6 H6F 108.6 . . ?
H6D N6 H6F 77.1 . . ?
C9B N6 H6G 108.8 . . ?
C9 N6 H6G 81.1 . . ?
Pr1 N6 H6G 107.2 . . ?
H6C N6 H6G 133.8 . . ?
H6F N6 H6G 107.4 . . ?
C12 C10 H10A 109.5 . . ?
C12 C10 H10B 109.5 . . ?
C12 C10 H10C 109.5 . . ?
C11 C10B H10F 109.5 . . ?
C11 C10B H10G 109.5 . . ?
H10F C10B H10G 109.5 . . ?
C11 C10B H10H 109.5 . . ?
H10F C10B H10H 109.5 . . ?
H10G C10B H10H 109.5 . . ?
C12 C11 N8 110.5(5) . . ?
C12 C11 C10B 104.0(6) . . ?
N8 C11 C10B 124.5(6) . . ?
C12 C11 H11A 109.5 . . ?
N8 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
N8 C11 H11B 109.5 . . ?
C10B C11 H11B 97.6 . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11F 105.5 . . ?
N8 C11 H11F 105.5 . . ?
C10B C11 H11F 105.5 . . ?
H11A C11 H11F 116.1 . . ?
C10 C12 C11 109.8(7) . . ?
C10 C12 N7 116.9(7) . . ?
C11 C12 N7 113.9(5) . . ?
C10 C12 H12A 105.0 . . ?
C11 C12 H12A 105.0 . . ?
N7 C12 H12A 105.0 . . ?
C11 C12 H12F 108.8 . . ?
N7 C12 H12F 108.8 . . ?
H12A C12 H12F 115.5 . . ?
C10 C12 H12G 97.2 . . ?
C11 C12 H12G 108.8 . . ?
N7 C12 H12G 108.8 . . ?
H12F C12 H12G 107.7 . . ?
C6B N3 Pr1 116.9(6) . . ?
C6 N3 Pr1 111.4(4) . . ?
C6B N3 H3C 127.4 . . ?
C6 N3 H3C 109.3 . . ?
Pr1 N3 H3C 109.3 . . ?
C6B N3 H3D 79.5 . . ?
C6 N3 H3D 109.3 . . ?
Pr1 N3 H3D 109.3 . . ?
H3C N3 H3D 108.0 . . ?
C6B N3 H3G 110.6 . . ?
C6 N3 H3G 85.2 . . ?
Pr1 N3 H3G 107.3 . . ?
H3D N3 H3G 131.3 . . ?
C6B N3 H3H 106.0 . . ?
C6 N3 H3H 132.2 . . ?
Pr1 N3 H3H 108.4 . . ?
H3C N3 H3H 80.5 . . ?
H3G N3 H3H 107.2 . . ?
C5 N4 Pr1 118.1(4) . . ?
C5B N4 Pr1 112.5(6) . . ?
C5 N4 H4G 107.8 . . ?
C5B N4 H4G 132.1 . . ?
Pr1 N4 H4G 107.8 . . ?
C5 N4 H4H 107.8 . . ?
C5B N4 H4H 84.3 . . ?
Pr1 N4 H4H 107.8 . . ?
H4G N4 H4H 107.1 . . ?
C5 N4 H4D 109.3 . . ?
C5B N4 H4D 132.9 . . ?
Pr1 N4 H4D 108.4 . . ?
H4H N4 H4D 104.6 . . ?
C5 N4 H4E 106.8 . . ?
C5B N4 H4E 82.6 . . ?
Pr1 N4 H4E 106.3 . . ?
H4G N4 H4E 109.9 . . ?
H4D N4 H4E 107.4 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 C6 109.6(8) . . ?
N4 C5 C4 113.0(12) . . ?
C6 C5 C4 102.5(12) . . ?
N4 C5 H5A 110.5 . . ?
C6 C5 H5A 110.5 . . ?
C4 C5 H5A 110.5 . . ?
C5 C6 N3 109.9(7) . . ?
C5 C6 H6A 109.7 . . ?
N3 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
N3 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C5B C4B H4L 109.5 . . ?
C5B C4B H4M 109.5 . . ?
H4L C4B H4M 109.5 . . ?
C5B C4B H4I 109.5 . . ?
H4L C4B H4I 109.5 . . ?
H4M C4B H4I 109.5 . . ?
C6B C5B N4 109.0(11) . . ?
C6B C5B C4B 108.6(17) . . ?
N4 C5B C4B 99.0(15) . . ?
C6B C5B H5L 113.1 . . ?
N4 C5B H5L 113.1 . . ?
C4B C5B H5L 113.1 . . ?
N3 C6B C5B 106.1(11) . . ?
N3 C6B H6L 110.5 . . ?
C5B C6B H6L 110.5 . . ?
N3 C6B H6M 110.5 . . ?
C5B C6B H6M 110.5 . . ?
H6L C6B H6M 108.7 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_Ic
_database_code_depnum_ccdc_archive 'CCDC 1403233'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H60 As2 N12 Nd2 S8'
_chemical_formula_sum            'C18 H60 As2 N12 Nd2 S8'
_chemical_formula_weight         1139.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   38.7276(8)
_cell_length_b                   11.9905(3)
_cell_length_c                   20.6659(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.798(2)
_cell_angle_gamma                90.00
_cell_volume                     8156.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      3.5830
_cell_measurement_theta_max      28.7390

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4528
_exptl_absorpt_coefficient_mu    4.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_T_max  0.7404
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18874
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8310
_reflns_number_gt                7288
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The command TWIN -10-2 0-10 001 is refined the pseudo-merohedral 
twinning, which makes R1/wR2 significantly lower.
The DELU restraint prevents the thermal ellipsoids of all 
adjacent C atoms from adopting different orientations.  
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)+(0.0650P)²+84.0000P] 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         8310
_refine_ls_number_parameters     452
_refine_ls_number_restraints     187
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1445
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.046
_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
Nd1 Nd 0.300093(13) 0.23496(4) 0.72392(3) 0.03144(13) Uani 1 1 d . A .
Nd2 Nd 0.069650(12) 0.27261(4) 0.49399(2) 0.03033(13) Uani 1 1 d . . .
As1 As 0.43418(2) 0.23692(7) 0.86865(5) 0.02874(18) Uani 1 1 d . . .
As2 As 0.18338(3) 0.24214(8) 0.61212(6) 0.0371(2) Uani 1 1 d . . .
S1 S 0.48554(6) 0.13190(19) 0.94240(12) 0.0376(5) Uani 1 1 d . . .
S2 S 0.43260(7) 0.3810(2) 0.92863(15) 0.0487(6) Uani 1 1 d . . .
S3 S 0.43566(8) 0.2815(3) 0.76864(14) 0.0527(6) Uani 1 1 d . . .
S4 S 0.38059(6) 0.13598(19) 0.83378(14) 0.0415(5) Uani 1 1 d . . .
S5 S 0.14958(7) 0.3753(3) 0.53558(19) 0.0652(9) Uani 1 1 d . . .
S6 S 0.21943(7) 0.1553(3) 0.57630(16) 0.0586(7) Uani 1 1 d . . .
S7 S 0.14007(7) 0.1325(2) 0.61471(16) 0.0542(7) Uani 1 1 d . . .
S8 S 0.22641(8) 0.3102(3) 0.72246(16) 0.0643(8) Uani 1 1 d . . .
N1 N 0.2938(3) 0.1172(7) 0.8268(5) 0.058(2) Uani 1 1 d . . .
H1D H 0.2673 0.1069 0.8097 0.069 Uiso 1 1 calc R . .
H1E H 0.3051 0.0497 0.8317 0.069 Uiso 1 1 calc R . .
N2 N 0.3235(2) 0.3394(8) 0.8524(5) 0.051(2) Uani 1 1 d . . .
H2B H 0.3509 0.3429 0.8788 0.062 Uiso 1 1 calc R . .
H2C H 0.3143 0.4099 0.8410 0.062 Uiso 1 1 calc R . .
N7 N 0.0259(3) 0.1011(8) 0.4129(5) 0.058(2) Uani 1 1 d . . .
H7D H 0.0256 0.0502 0.4446 0.070 Uiso 1 1 calc R . .
H7E H 0.0001 0.1241 0.3815 0.070 Uiso 1 1 calc R . .
N8 N 0.1005(3) 0.1492(10) 0.4280(5) 0.067(3) Uani 1 1 d . B .
H8B H 0.0977 0.1872 0.3880 0.081 Uiso 1 1 calc R . .
H8C H 0.1272 0.1395 0.4615 0.081 Uiso 1 1 calc R . .
N9 N 0.0382(2) 0.3490(7) 0.3543(4) 0.0432(18) Uani 1 1 d . . .
H9C H 0.0471 0.3069 0.3300 0.052 Uiso 1 1 calc R . .
H9D H 0.0110 0.3424 0.3292 0.052 Uiso 1 1 calc R . .
N10 N 0.0654(2) 0.4918(6) 0.4801(4) 0.0386(16) Uani 1 1 d . . .
H10D H 0.0493 0.5170 0.4962 0.046 Uiso 1 1 calc R . .
H10E H 0.0904 0.5198 0.5117 0.046 Uiso 1 1 calc R . .
N11 N 0.0855(3) 0.3601(8) 0.6229(5) 0.058(2) Uani 1 1 d . . .
H11C H 0.1116 0.3455 0.6587 0.070 Uiso 1 1 calc R . .
H11D H 0.0828 0.4346 0.6173 0.070 Uiso 1 1 calc R . .
N12 N 0.0423(2) 0.1610(7) 0.5672(4) 0.0449(18) Uani 1 1 d . . .
H12B H 0.0150 0.1594 0.5377 0.054 Uiso 1 1 calc R . .
H12C H 0.0511 0.0902 0.5723 0.054 Uiso 1 1 calc R . .
C1 C 0.3316(5) 0.3360(15) 0.9810(8) 0.098(5) Uani 1 1 d . . .
H1A H 0.3559 0.2936 1.0126 0.147 Uiso 1 1 calc R . .
H1B H 0.3138 0.3292 0.9999 0.147 Uiso 1 1 calc R . .
H1C H 0.3385 0.4130 0.9815 0.147 Uiso 1 1 calc R . .
C2 C 0.3112(4) 0.2935(11) 0.9030(6) 0.066(3) Uani 1 1 d . . .
H2A H 0.2823 0.3114 0.8795 0.079 Uiso 1 1 calc R . .
C3 C 0.3139(5) 0.1722(12) 0.9037(7) 0.081(4) Uani 1 1 d . . .
H3A H 0.3019 0.1427 0.9311 0.097 Uiso 1 1 calc R . .
H3B H 0.3424 0.1515 0.9319 0.097 Uiso 1 1 calc R . .
C13 C 0.0594(5) 0.6575(10) 0.4038(8) 0.080(4) Uani 1 1 d . . .
H13A H 0.0532 0.6983 0.4364 0.120 Uiso 1 1 calc R . .
H13B H 0.0430 0.6852 0.3527 0.120 Uiso 1 1 calc R . .
H13C H 0.0876 0.6668 0.4213 0.120 Uiso 1 1 calc R . .
C14 C 0.0505(5) 0.5362(10) 0.4054(7) 0.083(4) Uani 1 1 d . . .
H14A H 0.0215 0.5411 0.3872 0.100 Uiso 1 1 calc R . .
C15 C 0.0487(6) 0.4650(10) 0.3524(7) 0.093(5) Uani 1 1 d . . .
H15A H 0.0749 0.4662 0.3570 0.111 Uiso 1 1 calc R . .
H15B H 0.0290 0.4946 0.3025 0.111 Uiso 1 1 calc R . .
C16 C 0.0701(5) 0.3635(15) 0.7266(7) 0.097(5) Uani 1 1 d . . .
H16A H 0.0475 0.3491 0.7324 0.145 Uiso 1 1 calc R . .
H16B H 0.0752 0.4423 0.7301 0.145 Uiso 1 1 calc R . .
H16C H 0.0938 0.3259 0.7662 0.145 Uiso 1 1 calc R . .
C17 C 0.0604(5) 0.3213(11) 0.6494(7) 0.071(3) Uani 1 1 d . . .
H17A H 0.0338 0.3536 0.6135 0.085 Uiso 1 1 calc R . .
C18 C 0.0532(5) 0.2010(10) 0.6415(7) 0.074(4) Uani 1 1 d . . .
H18A H 0.0775 0.1628 0.6800 0.088 Uiso 1 1 calc R . .
H18B H 0.0315 0.1834 0.6502 0.088 Uiso 1 1 calc R . .
C7 C 0.2760(6) 0.5820(16) 0.5778(13) 0.077(6) Uani 0.594(14) 1 d PU A 1
H7A H 0.2547 0.6269 0.5749 0.116 Uiso 0.594(14) 1 calc PR A 1
H7B H 0.2661 0.5445 0.5302 0.116 Uiso 0.594(14) 1 calc PR A 1
H7C H 0.2986 0.6287 0.5886 0.116 Uiso 0.594(14) 1 calc PR A 1
C8 C 0.2890(6) 0.5004(19) 0.6377(15) 0.064(5) Uani 0.594(14) 1 d PU A 1
H8A H 0.2852 0.5338 0.6768 0.077 Uiso 0.594(14) 1 calc PR A 1
C9 C 0.3320(5) 0.4796(18) 0.6727(14) 0.054(4) Uani 0.594(14) 1 d PU A 1
H9A H 0.3466 0.5499 0.6887 0.065 Uiso 0.594(14) 1 calc PR A 1
H9B H 0.3370 0.4458 0.6357 0.065 Uiso 0.594(14) 1 calc PR A 1
C7B C 0.3512(10) 0.584(2) 0.687(2) 0.091(10) Uani 0.406(14) 1 d PU A 2
H7L H 0.3583 0.6482 0.7191 0.137 Uiso 0.406(14) 1 calc PR A 2
H7M H 0.3355 0.6067 0.6344 0.137 Uiso 0.406(14) 1 calc PR A 2
H7N H 0.3755 0.5474 0.6963 0.137 Uiso 0.406(14) 1 calc PR A 2
C8B C 0.3016(10) 0.475(2) 0.6225(18) 0.052(5) Uani 0.406(14) 1 d PU A 2
H8L H 0.3177 0.4388 0.6053 0.062 Uiso 0.406(14) 1 calc PR A 2
H8M H 0.2889 0.5408 0.5917 0.062 Uiso 0.406(14) 1 calc PR A 2
C9B C 0.3267(8) 0.504(2) 0.7034(17) 0.046(5) Uani 0.406(14) 1 d PU A 2
H9L H 0.3118 0.5392 0.7245 0.055 Uiso 0.406(14) 1 calc PR A 2
N5 N 0.2685(3) 0.3923(9) 0.6182(6) 0.080(3) Uani 1 1 d . . .
H5B H 0.2677 0.3663 0.5766 0.095 Uiso 0.594(14) 1 calc PR A 1
H5C H 0.2426 0.4034 0.6052 0.095 Uiso 0.594(14) 1 calc PR A 1
H5F H 0.2547 0.3592 0.5721 0.095 Uiso 0.406(14) 1 d PR A 2
H5G H 0.2504 0.4306 0.6243 0.095 Uiso 0.406(14) 1 d PR A 2
N6 N 0.3476(2) 0.4033(7) 0.7409(5) 0.052(2) Uani 1 1 d . . .
H6C H 0.3518 0.4442 0.7809 0.062 Uiso 0.594(14) 1 calc PR A 1
H6D H 0.3719 0.3759 0.7523 0.062 Uiso 0.594(14) 1 calc PR A 1
H6F H 0.3634 0.4189 0.7910 0.062 Uiso 0.406(14) 1 d PR A 2
H6G H 0.3641 0.3807 0.7250 0.062 Uiso 0.406(14) 1 d PR A 2
C10 C 0.0233(9) -0.057(2) 0.3373(17) 0.093(9) Uani 0.50(2) 1 d PU B 1
H10A H -0.0055 -0.0503 0.3027 0.140 Uiso 0.50(2) 1 calc PR B 1
H10B H 0.0286 -0.1071 0.3779 0.140 Uiso 0.50(2) 1 calc PR B 1
H10C H 0.0355 -0.0860 0.3106 0.140 Uiso 0.50(2) 1 calc PR B 1
C10B C 0.0902(10) -0.043(2) 0.3528(16) 0.082(8) Uani 0.50(2) 1 d PU B 2
H10F H 0.1189 -0.0472 0.3738 0.122 Uiso 0.50(2) 1 calc PR B 2
H10G H 0.0770 -0.0164 0.3013 0.122 Uiso 0.50(2) 1 calc PR B 2
H10H H 0.0799 -0.1155 0.3535 0.122 Uiso 0.50(2) 1 calc PR B 2
C11 C 0.0815(5) 0.0400(12) 0.4017(10) 0.094(5) Uani 1 1 d . . .
H11A H 0.0879 0.0103 0.3657 0.113 Uiso 0.50(2) 1 calc PR B 1
H11B H 0.0923 -0.0107 0.4446 0.113 Uiso 0.50(2) 1 calc PR B 1
H11F H 0.0903 -0.0013 0.4489 0.113 Uiso 0.50(2) 1 calc PR B 2
C12 C 0.0395(4) 0.0465(12) 0.3672(8) 0.078(4) Uani 1 1 d . B .
H12A H 0.0304 0.0951 0.3229 0.094 Uiso 0.50(2) 1 calc PR B 1
H12F H 0.0285 -0.0284 0.3551 0.094 Uiso 0.50(2) 1 calc PR B 2
H12G H 0.0285 0.0868 0.3195 0.094 Uiso 0.50(2) 1 calc PR B 2
N3 N 0.3295(3) 0.1881(8) 0.6363(5) 0.055(2) Uani 1 1 d . . .
H3C H 0.3197 0.2372 0.5976 0.066 Uiso 0.594(14) 1 calc PR A 1
H3D H 0.3568 0.1945 0.6637 0.066 Uiso 0.594(14) 1 calc PR A 1
H3G H 0.3115 0.2124 0.5888 0.066 Uiso 0.406(14) 1 d PR A 2
H3H H 0.3525 0.2277 0.6534 0.066 Uiso 0.406(14) 1 d PR A 2
N4 N 0.3017(2) 0.0226(7) 0.6953(5) 0.0480(19) Uani 1 1 d . . .
H4G H 0.3111 -0.0150 0.7392 0.058 Uiso 0.594(14) 1 calc PR A 1
H4H H 0.2759 0.0004 0.6633 0.058 Uiso 0.594(14) 1 calc PR A 1
H4D H 0.3099 -0.0162 0.7385 0.058 Uiso 0.406(14) 1 d PR A 2
H4E H 0.2758 0.0031 0.6617 0.058 Uiso 0.406(14) 1 d PR A 2
C4 C 0.3082(11) -0.125(2) 0.6134(16) 0.083(8) Uani 0.594(14) 1 d PDU A 1
H4A H 0.3052 -0.1824 0.6426 0.124 Uiso 0.594(14) 1 calc PR A 1
H4B H 0.3273 -0.1491 0.6000 0.124 Uiso 0.594(14) 1 calc PR A 1
H4C H 0.2824 -0.1110 0.5679 0.124 Uiso 0.594(14) 1 calc PR A 1
C5 C 0.3248(7) -0.0108(17) 0.6641(14) 0.058(5) Uani 0.594(14) 1 d PDU A 1
H5A H 0.3537 -0.0162 0.7033 0.070 Uiso 0.594(14) 1 calc PR A 1
C6 C 0.3176(7) 0.0692(18) 0.6046(13) 0.057(4) Uani 0.594(14) 1 d PU A 1
H6A H 0.2891 0.0678 0.5645 0.068 Uiso 0.594(14) 1 calc PR A 1
H6B H 0.3334 0.0473 0.5825 0.068 Uiso 0.594(14) 1 calc PR A 1
C4B C 0.3196(11) -0.130(2) 0.641(2) 0.056(7) Uani 0.406(14) 1 d PDU A 2
H4L H 0.3201 -0.1570 0.6848 0.084 Uiso 0.406(14) 1 calc PR A 2
H4M H 0.3461 -0.1368 0.6482 0.084 Uiso 0.406(14) 1 calc PR A 2
H4I H 0.3004 -0.1718 0.5968 0.084 Uiso 0.406(14) 1 calc PR A 2
C5B C 0.3062(10) 0.002(2) 0.6277(19) 0.049(5) Uani 0.406(14) 1 d PDU A 2
H5L H 0.2807 0.0143 0.5792 0.059 Uiso 0.406(14) 1 calc PR A 2
C6B C 0.3391(10) 0.069(3) 0.6339(19) 0.056(6) Uani 0.406(14) 1 d PU A 2
H6L H 0.3418 0.0552 0.5905 0.067 Uiso 0.406(14) 1 calc PR A 2
H6M H 0.3645 0.0492 0.6798 0.067 Uiso 0.406(14) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 N4 2.622(8) . ?
Nd1 N2 2.627(8) . ?
Nd1 N6 2.628(8) . ?
Nd1 N5 2.648(9) . ?
Nd1 N3 2.659(8) . ?
Nd1 N1 2.668(8) . ?
Nd1 S4 2.970(2) . ?
Nd1 S8 2.978(3) . ?
Nd1 S6 3.152(3) . ?
Nd2 N11 2.617(8) . ?
Nd2 N12 2.624(7) . ?
Nd2 N7 2.631(9) . ?
Nd2 N9 2.636(7) . ?
Nd2 N10 2.640(7) . ?
Nd2 N8 2.681(9) . ?
Nd2 S5 3.005(2) . ?
Nd2 S7 3.052(2) . ?
Nd2 S1 3.066(2) 8_455 ?
As1 S2 2.146(2) . ?
As1 S1 2.161(2) . ?
As1 S3 2.165(2) . ?
As1 S4 2.171(2) . ?
As2 S5 2.140(3) . ?
As2 S7 2.154(3) . ?
As2 S8 2.154(3) . ?
As2 S6 2.161(3) . ?
S1 Nd2 3.066(2) 8_556 ?
N1 C3 1.504(15) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N2 C2 1.466(14) . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N7 C12 1.458(14) . ?
N7 H7D 0.9000 . ?
N7 H7E 0.9000 . ?
N8 C11 1.460(18) . ?
N8 H8B 0.9000 . ?
N8 H8C 0.9000 . ?
N9 C15 1.455(14) . ?
N9 H9C 0.9000 . ?
N9 H9D 0.9000 . ?
N10 C14 1.436(13) . ?
N10 H10D 0.9000 . ?
N10 H10E 0.9000 . ?
N11 C17 1.421(14) . ?
N11 H11C 0.9000 . ?
N11 H11D 0.9000 . ?
N12 C18 1.444(13) . ?
N12 H12B 0.9000 . ?
N12 H12C 0.9000 . ?
C1 C2 1.463(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.458(19) . ?
C2 H2A 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 C14 1.499(16) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.360(17) . ?
C14 H14A 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.521(15) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.462(17) . ?
C17 H17A 0.9800 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C7 C8 1.44(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.44(3) . ?
C8 N5 1.46(2) . ?
C8 H8A 0.9800 . ?
C9 N6 1.51(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C7B C9B 1.51(4) . ?
C7B H7L 0.9600 . ?
C7B H7M 0.9600 . ?
C7B H7N 0.9600 . ?
C8B C9B 1.47(5) . ?
C8B N5 1.59(3) . ?
C8B H8L 0.9700 . ?
C8B H8M 0.9700 . ?
C9B N6 1.44(3) . ?
C9B H9L 0.9800 . ?
N5 H5B 0.9000 . ?
N5 H5C 0.9000 . ?
N5 H5F 0.9023 . ?
N5 H5G 0.9001 . ?
N6 H6C 0.9000 . ?
N6 H6D 0.9000 . ?
N6 H6F 0.9027 . ?
N6 H6G 0.9005 . ?
C10 C12 1.38(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10B C11 1.58(2) . ?
C10B H10F 0.9600 . ?
C10B H10G 0.9600 . ?
C10B H10H 0.9600 . ?
C11 C12 1.389(18) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12F 0.9700 . ?
C12 H12G 0.9700 . ?
N3 C6B 1.49(3) . ?
N3 C6 1.54(2) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N3 H3G 0.9021 . ?
N3 H3H 0.8997 . ?
N4 C5 1.41(2) . ?
N4 C5B 1.52(3) . ?
N4 H4G 0.9000 . ?
N4 H4H 0.9000 . ?
N4 H4D 0.9025 . ?
N4 H4E 0.9002 . ?
C4 C5 1.64(2) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.47(4) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4B C5B 1.64(2) . ?
C4B H4L 0.9600 . ?
C4B H4M 0.9600 . ?
C4B H4I 0.9600 . ?
C5B C6B 1.45(5) . ?
C5B H5L 0.9800 . ?
C6B H6L 0.9700 . ?
C6B H6M 0.9700 . ?

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
N4 Nd1 N2 130.9(3) . . ?
N4 Nd1 N6 132.6(3) . . ?
N2 Nd1 N6 69.8(3) . . ?
N4 Nd1 N5 124.1(3) . . ?
N2 Nd1 N5 104.9(3) . . ?
N6 Nd1 N5 63.3(3) . . ?
N4 Nd1 N3 64.6(3) . . ?
N2 Nd1 N3 138.2(3) . . ?
N6 Nd1 N3 74.4(3) . . ?
N5 Nd1 N3 76.5(3) . . ?
N4 Nd1 N1 71.9(3) . . ?
N2 Nd1 N1 64.9(3) . . ?
N6 Nd1 N1 130.7(3) . . ?
N5 Nd1 N1 146.9(3) . . ?
N3 Nd1 N1 133.1(3) . . ?
N4 Nd1 S4 69.15(18) . . ?
N2 Nd1 S4 75.72(19) . . ?
N6 Nd1 S4 79.95(18) . . ?
N5 Nd1 S4 139.3(2) . . ?
N3 Nd1 S4 77.4(2) . . ?
N1 Nd1 S4 71.3(2) . . ?
N4 Nd1 S8 115.38(19) . . ?
N2 Nd1 S8 71.64(18) . . ?
N6 Nd1 S8 111.7(2) . . ?
N5 Nd1 S8 75.6(3) . . ?
N3 Nd1 S8 144.0(2) . . ?
N1 Nd1 S8 71.3(2) . . ?
S4 Nd1 S8 137.99(8) . . ?
N4 Nd1 S6 67.48(19) . . ?
N2 Nd1 S6 139.57(18) . . ?
N6 Nd1 S6 128.99(19) . . ?
N5 Nd1 S6 68.0(2) . . ?
N3 Nd1 S6 80.7(2) . . ?
N1 Nd1 S6 98.7(2) . . ?
S4 Nd1 S6 136.43(7) . . ?
S8 Nd1 S6 68.06(7) . . ?
N11 Nd2 N12 64.4(3) . . ?
N11 Nd2 N7 133.5(3) . . ?
N12 Nd2 N7 69.4(3) . . ?
N11 Nd2 N9 134.5(3) . . ?
N12 Nd2 N9 135.6(2) . . ?
N7 Nd2 N9 78.6(3) . . ?
N11 Nd2 N10 71.3(2) . . ?
N12 Nd2 N10 123.3(2) . . ?
N7 Nd2 N10 136.6(3) . . ?
N9 Nd2 N10 64.5(2) . . ?
N11 Nd2 N8 144.1(3) . . ?
N12 Nd2 N8 115.8(3) . . ?
N7 Nd2 N8 63.5(3) . . ?
N9 Nd2 N8 73.0(3) . . ?
N10 Nd2 N8 120.9(3) . . ?
N11 Nd2 S5 83.7(2) . . ?
N12 Nd2 S5 135.36(18) . . ?
N7 Nd2 S5 136.3(2) . . ?
N9 Nd2 S5 89.02(18) . . ?
N10 Nd2 S5 67.64(16) . . ?
N8 Nd2 S5 72.8(2) . . ?
N11 Nd2 S7 76.1(2) . . ?
N12 Nd2 S7 72.91(17) . . ?
N7 Nd2 S7 95.1(2) . . ?
N9 Nd2 S7 141.69(18) . . ?
N10 Nd2 S7 127.95(16) . . ?
N8 Nd2 S7 70.5(2) . . ?
S5 Nd2 S7 69.49(7) . . ?
N11 Nd2 S1 80.8(2) . 8_455 ?
N12 Nd2 S1 73.35(17) . 8_455 ?
N7 Nd2 S1 81.97(19) . 8_455 ?
N9 Nd2 S1 72.31(17) . 8_455 ?
N10 Nd2 S1 66.17(15) . 8_455 ?
N8 Nd2 S1 134.8(2) . 8_455 ?
S5 Nd2 S1 133.79(7) . 8_455 ?
S7 Nd2 S1 144.88(7) . 8_455 ?
S2 As1 S1 110.95(10) . . ?
S2 As1 S3 112.08(12) . . ?
S1 As1 S3 109.85(10) . . ?
S2 As1 S4 109.11(10) . . ?
S1 As1 S4 105.83(9) . . ?
S3 As1 S4 108.81(11) . . ?
S5 As2 S7 107.02(10) . . ?
S5 As2 S8 109.29(14) . . ?
S7 As2 S8 112.54(13) . . ?
S5 As2 S6 111.10(13) . . ?
S7 As2 S6 111.51(12) . . ?
S8 As2 S6 105.43(10) . . ?
As1 S1 Nd2 116.24(9) . 8_556 ?
As1 S4 Nd1 117.74(9) . . ?
As2 S5 Nd2 92.44(9) . . ?
As2 S6 Nd1 90.71(9) . . ?
As2 S7 Nd2 90.90(9) . . ?
As2 S8 Nd1 95.66(9) . . ?
C3 N1 Nd1 113.3(7) . . ?
C3 N1 H1D 108.9 . . ?
Nd1 N1 H1D 108.9 . . ?
C3 N1 H1E 108.9 . . ?
Nd1 N1 H1E 108.9 . . ?
H1D N1 H1E 107.7 . . ?
C2 N2 Nd1 118.2(7) . . ?
C2 N2 H2B 107.8 . . ?
Nd1 N2 H2B 107.8 . . ?
C2 N2 H2C 107.8 . . ?
Nd1 N2 H2C 107.8 . . ?
H2B N2 H2C 107.1 . . ?
C12 N7 Nd2 115.5(7) . . ?
C12 N7 H7D 108.4 . . ?
Nd2 N7 H7D 108.4 . . ?
C12 N7 H7E 108.4 . . ?
Nd2 N7 H7E 108.4 . . ?
H7D N7 H7E 107.5 . . ?
C11 N8 Nd2 114.3(7) . . ?
C11 N8 H8B 108.7 . . ?
Nd2 N8 H8B 108.7 . . ?
C11 N8 H8C 108.7 . . ?
Nd2 N8 H8C 108.7 . . ?
H8B N8 H8C 107.6 . . ?
C15 N9 Nd2 112.8(6) . . ?
C15 N9 H9C 109.0 . . ?
Nd2 N9 H9C 109.0 . . ?
C15 N9 H9D 109.0 . . ?
Nd2 N9 H9D 109.0 . . ?
H9C N9 H9D 107.8 . . ?
C14 N10 Nd2 116.9(6) . . ?
C14 N10 H10D 108.1 . . ?
Nd2 N10 H10D 108.1 . . ?
C14 N10 H10E 108.1 . . ?
Nd2 N10 H10E 108.1 . . ?
H10D N10 H10E 107.3 . . ?
C17 N11 Nd2 114.8(7) . . ?
C17 N11 H11C 108.6 . . ?
Nd2 N11 H11C 108.6 . . ?
C17 N11 H11D 108.6 . . ?
Nd2 N11 H11D 108.6 . . ?
H11C N11 H11D 107.5 . . ?
C18 N12 Nd2 117.6(6) . . ?
C18 N12 H12B 107.9 . . ?
Nd2 N12 H12B 107.9 . . ?
C18 N12 H12C 107.9 . . ?
Nd2 N12 H12C 107.9 . . ?
H12B N12 H12C 107.2 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 110.0(12) . . ?
C3 C2 N2 109.4(10) . . ?
C1 C2 N2 117.7(11) . . ?
C3 C2 H2A 106.3 . . ?
C1 C2 H2A 106.3 . . ?
N2 C2 H2A 106.3 . . ?
C2 C3 N1 115.6(10) . . ?
C2 C3 H3A 108.4 . . ?
N1 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
N1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.4 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N10 117.0(11) . . ?
C15 C14 C13 120.5(11) . . ?
N10 C14 C13 114.6(11) . . ?
C15 C14 H14A 99.4 . . ?
N10 C14 H14A 99.4 . . ?
C13 C14 H14A 99.4 . . ?
C14 C15 N9 118.4(11) . . ?
C14 C15 H15A 107.7 . . ?
N9 C15 H15A 107.7 . . ?
C14 C15 H15B 107.7 . . ?
N9 C15 H15B 107.7 . . ?
H15A C15 H15B 107.1 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N11 C17 C18 114.2(10) . . ?
N11 C17 C16 117.1(11) . . ?
C18 C17 C16 111.9(11) . . ?
N11 C17 H17A 104.0 . . ?
C18 C17 H17A 104.0 . . ?
C16 C17 H17A 104.0 . . ?
N12 C18 C17 112.2(9) . . ?
N12 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
N12 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C9 C8 C7 110(2) . . ?
C9 C8 N5 107.5(19) . . ?
C7 C8 N5 118.1(19) . . ?
C9 C8 H8A 107.1 . . ?
C7 C8 H8A 107.1 . . ?
N5 C8 H8A 107.1 . . ?
C8 C9 N6 111.2(16) . . ?
C8 C9 H9A 109.4 . . ?
N6 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
N6 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C9B C7B H7L 109.5 . . ?
C9B C7B H7M 109.5 . . ?
H7L C7B H7M 109.5 . . ?
C9B C7B H7N 109.5 . . ?
H7L C7B H7N 109.5 . . ?
H7M C7B H7N 109.5 . . ?
C9B C8B N5 104(2) . . ?
C9B C8B H8L 110.9 . . ?
N5 C8B H8L 110.9 . . ?
C9B C8B H8M 110.9 . . ?
N5 C8B H8M 110.9 . . ?
H8L C8B H8M 108.9 . . ?
N6 C9B C8B 105(2) . . ?
N6 C9B C7B 114(2) . . ?
C8B C9B C7B 91(3) . . ?
N6 C9B H9L 114.7 . . ?
C8B C9B H9L 114.7 . . ?
C7B C9B H9L 114.7 . . ?
C8 N5 Nd1 117.1(10) . . ?
C8B N5 Nd1 113.0(12) . . ?
C8 N5 H5B 108.0 . . ?
C8B N5 H5B 83.6 . . ?
Nd1 N5 H5B 108.0 . . ?
C8 N5 H5C 108.0 . . ?
C8B N5 H5C 131.6 . . ?
Nd1 N5 H5C 108.0 . . ?
H5B N5 H5C 107.3 . . ?
C8 N5 H5F 127.9 . . ?
C8B N5 H5F 110.2 . . ?
Nd1 N5 H5F 108.5 . . ?
H5C N5 H5F 78.7 . . ?
C8 N5 H5G 81.9 . . ?
C8B N5 H5G 109.7 . . ?
Nd1 N5 H5G 107.6 . . ?
H5B N5 H5G 132.5 . . ?
H5F N5 H5G 107.6 . . ?
C9B N6 Nd1 114.7(12) . . ?
C9 N6 Nd1 115.6(8) . . ?
C9B N6 H6C 79.2 . . ?
C9 N6 H6C 108.4 . . ?
Nd1 N6 H6C 108.4 . . ?
C9B N6 H6D 131.6 . . ?
C9 N6 H6D 108.4 . . ?
Nd1 N6 H6D 108.4 . . ?
H6C N6 H6D 107.5 . . ?
C9B N6 H6F 107.0 . . ?
C9 N6 H6F 129.8 . . ?
Nd1 N6 H6F 108.4 . . ?
H6D N6 H6F 78.0 . . ?
C9B N6 H6G 111.4 . . ?
C9 N6 H6G 81.7 . . ?
Nd1 N6 H6G 107.6 . . ?
H6C N6 H6G 132.9 . . ?
H6F N6 H6G 107.5 . . ?
C12 C10 H10A 109.5 . . ?
C12 C10 H10B 109.5 . . ?
C12 C10 H10C 109.5 . . ?
C11 C10B H10F 109.5 . . ?
C11 C10B H10G 109.5 . . ?
H10F C10B H10G 109.5 . . ?
C11 C10B H10H 109.5 . . ?
H10F C10B H10H 109.5 . . ?
H10G C10B H10H 109.5 . . ?
C12 C11 N8 111.3(11) . . ?
C12 C11 C10B 107.1(17) . . ?
N8 C11 C10B 124.6(15) . . ?
C12 C11 H11A 109.4 . . ?
N8 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
N8 C11 H11B 109.4 . . ?
C10B C11 H11B 93.2 . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11F 103.9 . . ?
N8 C11 H11F 103.9 . . ?
C10B C11 H11F 103.9 . . ?
H11A C11 H11F 118.8 . . ?
C10 C12 C11 108.2(18) . . ?
C10 C12 N7 117.1(18) . . ?
C11 C12 N7 114.7(11) . . ?
C10 C12 H12A 105.2 . . ?
C11 C12 H12A 105.2 . . ?
N7 C12 H12A 105.2 . . ?
C11 C12 H12F 108.6 . . ?
N7 C12 H12F 108.6 . . ?
H12A C12 H12F 114.7 . . ?
C10 C12 H12G 98.1 . . ?
C11 C12 H12G 108.6 . . ?
N7 C12 H12G 108.6 . . ?
H12F C12 H12G 107.6 . . ?
C6B N3 Nd1 115.5(13) . . ?
C6 N3 Nd1 110.3(9) . . ?
C6B N3 H3C 126.5 . . ?
C6 N3 H3C 109.6 . . ?
Nd1 N3 H3C 109.6 . . ?
C6B N3 H3D 82.6 . . ?
C6 N3 H3D 109.6 . . ?
Nd1 N3 H3D 109.6 . . ?
H3C N3 H3D 108.1 . . ?
C6B N3 H3G 109.8 . . ?
C6 N3 H3G 87.1 . . ?
Nd1 N3 H3G 108.0 . . ?
H3D N3 H3G 129.5 . . ?
C6B N3 H3H 107.9 . . ?
C6 N3 H3H 131.9 . . ?
Nd1 N3 H3H 108.2 . . ?
H3C N3 H3H 82.7 . . ?
H3G N3 H3H 107.2 . . ?
C5 N4 Nd1 118.4(10) . . ?
C5B N4 Nd1 113.1(11) . . ?
C5 N4 H4G 107.7 . . ?
C5B N4 H4G 131.8 . . ?
Nd1 N4 H4G 107.7 . . ?
C5 N4 H4H 107.7 . . ?
C5B N4 H4H 84.0 . . ?
Nd1 N4 H4H 107.7 . . ?
H4G N4 H4H 107.1 . . ?
C5 N4 H4D 109.1 . . ?
C5B N4 H4D 132.4 . . ?
Nd1 N4 H4D 108.4 . . ?
H4H N4 H4D 104.6 . . ?
C5 N4 H4E 106.9 . . ?
C5B N4 H4E 82.5 . . ?
Nd1 N4 H4E 106.1 . . ?
H4G N4 H4E 109.9 . . ?
H4D N4 H4E 107.3 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 C6 108.3(18) . . ?
N4 C5 C4 114(2) . . ?
C6 C5 C4 100(2) . . ?
N4 C5 H5A 111.4 . . ?
C6 C5 H5A 111.4 . . ?
C4 C5 H5A 111.4 . . ?
C5 C6 N3 111.5(16) . . ?
C5 C6 H6A 109.3 . . ?
N3 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
N3 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C5B C4B H4L 109.5 . . ?
C5B C4B H4M 109.5 . . ?
H4L C4B H4M 109.5 . . ?
C5B C4B H4I 109.5 . . ?
H4L C4B H4I 109.5 . . ?
H4M C4B H4I 109.5 . . ?
C6B C5B N4 111(2) . . ?
C6B C5B C4B 109(3) . . ?
N4 C5B C4B 101(2) . . ?
C6B C5B H5L 112.0 . . ?
N4 C5B H5L 112.0 . . ?
C4B C5B H5L 112.0 . . ?
C5B C6B N3 108(2) . . ?
C5B C6B H6L 110.1 . . ?
N3 C6B H6L 110.1 . . ?
C5B C6B H6M 110.1 . . ?
N3 C6B H6M 110.1 . . ?
H6L C6B H6M 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.751
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.150
####################################################################### 
# 
# 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_Id
_database_code_depnum_ccdc_archive 'CCDC 1403234'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H60 As2 N12 S8 Sm2'
_chemical_formula_sum            'C18 H60 As2 N12 S8 Sm2'
_chemical_formula_weight         1151.82

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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc '


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

_cell_length_a                   38.7381(9)
_cell_length_b                   11.9872(3)
_cell_length_c                   20.5952(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.791(2)
_cell_angle_gamma                90.00
_cell_volume                     8128.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7750
_cell_measurement_theta_min      3.5090
_cell_measurement_theta_max      28.4650

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4560
_exptl_absorpt_coefficient_mu    4.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_T_max  0.7246
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17620
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8283
_reflns_number_gt                7187
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The command TWIN -10-2 0-10 001 is refined the pseudo-merohedral 
twinning, which makes R1/wR2 significantly lower.
The DELU restraint prevents the thermal ellipsoids of all 
adjacent C atoms from adopting different orientations.  
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)+(0.0460P)²+4.0000P] 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         8283
_refine_ls_number_parameters     452
_refine_ls_number_restraints     187
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0845
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.011
_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
Sm1 Sm 0.300835(9) 0.23630(2) 0.72543(2) 0.03218(9) Uani 1 1 d . A .
Sm2 Sm 0.069631(9) 0.27476(2) 0.493770(16) 0.02793(8) Uani 1 1 d . . .
As1 As 0.434242(18) 0.23689(4) 0.86892(3) 0.02729(13) Uani 1 1 d . . .
As2 As 0.183422(19) 0.24309(5) 0.61209(4) 0.03667(15) Uani 1 1 d . . .
S1 S 0.48565(4) 0.13182(13) 0.94254(9) 0.0350(4) Uani 1 1 d . . .
S2 S 0.43313(6) 0.38168(13) 0.92962(10) 0.0455(4) Uani 1 1 d . . .
S3 S 0.43571(6) 0.28277(16) 0.76869(10) 0.0488(4) Uani 1 1 d . . .
S4 S 0.38047(4) 0.13744(12) 0.83427(10) 0.0385(4) Uani 1 1 d . . .
S5 S 0.14903(5) 0.37760(17) 0.53635(13) 0.0618(6) Uani 1 1 d . . .
S6 S 0.21877(6) 0.15832(17) 0.57426(13) 0.0613(6) Uani 1 1 d . . .
S7 S 0.13980(5) 0.13383(15) 0.61441(11) 0.0513(5) Uani 1 1 d . . .
S8 S 0.22681(6) 0.3102(2) 0.72279(12) 0.0679(6) Uani 1 1 d . . .
N1 N 0.29444(19) 0.1207(5) 0.8273(4) 0.0586(17) Uani 1 1 d . . .
H1D H 0.2679 0.1110 0.8101 0.070 Uiso 1 1 calc R . .
H1E H 0.3054 0.0527 0.8318 0.070 Uiso 1 1 calc R . .
N2 N 0.32389(16) 0.3413(5) 0.8528(3) 0.0463(14) Uani 1 1 d . . .
H2B H 0.3512 0.3465 0.8790 0.056 Uiso 1 1 calc R . .
H2C H 0.3140 0.4112 0.8411 0.056 Uiso 1 1 calc R . .
N7 N 0.02633(17) 0.1051(4) 0.4135(3) 0.0498(15) Uani 1 1 d . . .
H7D H 0.0259 0.0547 0.4455 0.060 Uiso 1 1 calc R . .
H7E H 0.0006 0.1285 0.3818 0.060 Uiso 1 1 calc R . .
N8 N 0.10070(18) 0.1540(6) 0.4282(4) 0.0656(19) Uani 1 1 d . B .
H8B H 0.0967 0.1906 0.3866 0.079 Uiso 1 1 calc R . .
H8C H 0.1277 0.1478 0.4609 0.079 Uiso 1 1 calc R . .
N9 N 0.03832(16) 0.3480(4) 0.3552(3) 0.0392(12) Uani 1 1 d . . .
H9C H 0.0471 0.3053 0.3308 0.047 Uiso 1 1 calc R . .
H9D H 0.0111 0.3417 0.3303 0.047 Uiso 1 1 calc R . .
N10 N 0.06504(13) 0.4915(4) 0.4804(2) 0.0327(10) Uani 1 1 d . . .
H10D H 0.0482 0.5159 0.4951 0.039 Uiso 1 1 calc R . .
H10E H 0.0898 0.5198 0.5133 0.039 Uiso 1 1 calc R . .
N11 N 0.08605(18) 0.3619(5) 0.6213(3) 0.0527(16) Uani 1 1 d . . .
H11C H 0.1124 0.3490 0.6565 0.063 Uiso 1 1 calc R . .
H11D H 0.0827 0.4362 0.6151 0.063 Uiso 1 1 calc R . .
N12 N 0.04266(16) 0.1621(4) 0.5659(3) 0.0417(13) Uani 1 1 d . . .
H12B H 0.0154 0.1596 0.5363 0.050 Uiso 1 1 calc R . .
H12C H 0.0518 0.0916 0.5715 0.050 Uiso 1 1 calc R . .
C1 C 0.3311(3) 0.3398(9) 0.9808(5) 0.092(3) Uani 1 1 d . . .
H1A H 0.3251 0.4180 0.9775 0.138 Uiso 1 1 calc R . .
H1B H 0.3600 0.3293 1.0069 0.138 Uiso 1 1 calc R . .
H1C H 0.3208 0.3028 1.0085 0.138 Uiso 1 1 calc R . .
C2 C 0.3119(3) 0.2926(8) 0.9037(5) 0.076(3) Uani 1 1 d . . .
H2A H 0.2829 0.3092 0.8795 0.091 Uiso 1 1 calc R . .
C3 C 0.3145(3) 0.1733(8) 0.9045(5) 0.084(3) Uani 1 1 d . . .
H3A H 0.3023 0.1437 0.9316 0.101 Uiso 1 1 calc R . .
H3B H 0.3430 0.1522 0.9328 0.101 Uiso 1 1 calc R . .
C13 C 0.0597(3) 0.6581(6) 0.4025(5) 0.073(3) Uani 1 1 d . . .
H13A H 0.0530 0.6996 0.4342 0.110 Uiso 1 1 calc R . .
H13B H 0.0436 0.6844 0.3509 0.110 Uiso 1 1 calc R . .
H13C H 0.0880 0.6678 0.4208 0.110 Uiso 1 1 calc R . .
C14 C 0.0512(3) 0.5373(6) 0.4052(5) 0.081(3) Uani 1 1 d . . .
H14A H 0.0221 0.5430 0.3865 0.097 Uiso 1 1 calc R . .
C15 C 0.0488(4) 0.4635(7) 0.3524(5) 0.095(4) Uani 1 1 d . . .
H15A H 0.0749 0.4638 0.3564 0.114 Uiso 1 1 calc R . .
H15B H 0.0290 0.4923 0.3023 0.114 Uiso 1 1 calc R . .
C16 C 0.0717(3) 0.3655(8) 0.7261(5) 0.088(3) Uani 1 1 d . . .
H16A H 0.0794 0.4425 0.7306 0.131 Uiso 1 1 calc R . .
H16B H 0.0936 0.3233 0.7662 0.131 Uiso 1 1 calc R . .
H16C H 0.0482 0.3589 0.7300 0.131 Uiso 1 1 calc R . .
C17 C 0.0620(3) 0.3217(7) 0.6504(5) 0.078(3) Uani 1 1 d . . .
H17A H 0.0353 0.3543 0.6150 0.094 Uiso 1 1 calc R . .
C18 C 0.0537(3) 0.2042(6) 0.6419(5) 0.066(2) Uani 1 1 d . . .
H18A H 0.0316 0.1889 0.6500 0.079 Uiso 1 1 calc R . .
H18B H 0.0775 0.1645 0.6809 0.079 Uiso 1 1 calc R . .
C7 C 0.2754(4) 0.5814(10) 0.5795(8) 0.077(5) Uani 0.602(10) 1 d PU A 1
H7A H 0.2475 0.5988 0.5611 0.116 Uiso 0.602(10) 1 calc PR A 1
H7B H 0.2777 0.5553 0.5378 0.116 Uiso 0.602(10) 1 calc PR A 1
H7C H 0.2917 0.6471 0.6011 0.116 Uiso 0.602(10) 1 calc PR A 1
C8 C 0.2889(5) 0.4981(16) 0.6355(12) 0.063(5) Uani 0.602(10) 1 d PU A 1
H8A H 0.2858 0.5315 0.6756 0.076 Uiso 0.602(10) 1 calc PR A 1
C9 C 0.3330(4) 0.4776(13) 0.6734(9) 0.050(4) Uani 0.602(10) 1 d PU A 1
H9A H 0.3473 0.5482 0.6893 0.060 Uiso 0.602(10) 1 calc PR A 1
H9B H 0.3386 0.4434 0.6372 0.060 Uiso 0.602(10) 1 calc PR A 1
C7B C 0.3542(6) 0.5839(16) 0.6855(12) 0.068(6) Uani 0.398(10) 1 d PU A 2
H7L H 0.3569 0.6548 0.7095 0.103 Uiso 0.398(10) 1 calc PR A 2
H7M H 0.3406 0.5940 0.6312 0.103 Uiso 0.398(10) 1 calc PR A 2
H7N H 0.3806 0.5527 0.7044 0.103 Uiso 0.398(10) 1 calc PR A 2
C8B C 0.2998(8) 0.473(2) 0.6214(17) 0.060(6) Uani 0.398(10) 1 d PU A 2
H8L H 0.2864 0.5388 0.5916 0.072 Uiso 0.398(10) 1 calc PR A 2
H8M H 0.3142 0.4368 0.6004 0.072 Uiso 0.398(10) 1 calc PR A 2
C9B C 0.3287(7) 0.5027(19) 0.7042(13) 0.047(4) Uani 0.398(10) 1 d PU A 2
H9L H 0.3154 0.5403 0.7275 0.056 Uiso 0.398(10) 1 calc PR A 2
N5 N 0.26836(19) 0.3917(5) 0.6204(4) 0.079(2) Uani 1 1 d . . .
H5B H 0.2658 0.3637 0.5775 0.094 Uiso 0.602(10) 1 calc PR A 1
H5C H 0.2431 0.4047 0.6104 0.094 Uiso 0.602(10) 1 calc PR A 1
H5F H 0.2546 0.3586 0.5743 0.094 Uiso 0.398(10) 1 d PR A 2
H5G H 0.2503 0.4300 0.6266 0.094 Uiso 0.398(10) 1 d PR A 2
N6 N 0.34805(16) 0.4036(4) 0.7411(3) 0.0487(15) Uani 1 1 d . . .
H6C H 0.3521 0.4454 0.7808 0.058 Uiso 0.602(10) 1 calc PR A 1
H6D H 0.3723 0.3760 0.7531 0.058 Uiso 0.602(10) 1 calc PR A 1
H6F H 0.3638 0.4192 0.7912 0.058 Uiso 0.398(10) 1 d PR A 2
H6G H 0.3645 0.3810 0.7252 0.058 Uiso 0.398(10) 1 d PR A 2
C10 C 0.0231(5) -0.0551(13) 0.3376(10) 0.073(6) Uani 0.494(14) 1 d PU B 1
H10A H -0.0059 -0.0482 0.3068 0.110 Uiso 0.494(14) 1 calc PR B 1
H10B H 0.0303 -0.1064 0.3787 0.110 Uiso 0.494(14) 1 calc PR B 1
H10C H 0.0332 -0.0822 0.3068 0.110 Uiso 0.494(14) 1 calc PR B 1
C10B C 0.0922(6) -0.0383(13) 0.3567(10) 0.079(6) Uani 0.506(14) 1 d PU B 2
H10F H 0.1194 -0.0662 0.3872 0.119 Uiso 0.506(14) 1 calc PR B 2
H10G H 0.0891 0.0008 0.3133 0.119 Uiso 0.506(14) 1 calc PR B 2
H10H H 0.0734 -0.0995 0.3397 0.119 Uiso 0.506(14) 1 calc PR B 2
C11 C 0.0834(3) 0.0429(7) 0.4055(6) 0.081(3) Uani 1 1 d . . .
H11A H 0.0910 0.0104 0.3716 0.098 Uiso 0.494(14) 1 calc PR B 1
H11B H 0.0941 -0.0044 0.4503 0.098 Uiso 0.494(14) 1 calc PR B 1
H11F H 0.0923 0.0031 0.4534 0.098 Uiso 0.506(14) 1 calc PR B 2
C12 C 0.0401(3) 0.0486(7) 0.3675(5) 0.080(3) Uani 1 1 d . B .
H12A H 0.0314 0.0969 0.3231 0.096 Uiso 0.494(14) 1 calc PR B 1
H12F H 0.0291 -0.0264 0.3557 0.096 Uiso 0.506(14) 1 calc PR B 2
H12G H 0.0295 0.0883 0.3196 0.096 Uiso 0.506(14) 1 calc PR B 2
N3 N 0.32949(18) 0.1894(5) 0.6387(3) 0.0509(15) Uani 1 1 d . . .
H3C H 0.3205 0.2403 0.6010 0.061 Uiso 0.602(10) 1 calc PR A 1
H3D H 0.3568 0.1930 0.6666 0.061 Uiso 0.602(10) 1 calc PR A 1
H3G H 0.3115 0.2137 0.5912 0.061 Uiso 0.398(10) 1 d PR A 2
H3H H 0.3525 0.2290 0.6557 0.061 Uiso 0.398(10) 1 d PR A 2
N4 N 0.29993(18) 0.0274(4) 0.6950(3) 0.0521(15) Uani 1 1 d . . .
H4G H 0.3083 -0.0113 0.7383 0.062 Uiso 0.602(10) 1 calc PR A 1
H4H H 0.2740 0.0077 0.6616 0.062 Uiso 0.602(10) 1 calc PR A 1
H4D H 0.3082 -0.0114 0.7382 0.062 Uiso 0.398(10) 1 d PR A 2
H4E H 0.2740 0.0079 0.6614 0.062 Uiso 0.398(10) 1 d PR A 2
C4 C 0.3046(8) -0.1228(15) 0.6156(15) 0.080(7) Uani 0.602(10) 1 d PDU A 1
H4A H 0.3023 -0.1781 0.6468 0.121 Uiso 0.602(10) 1 calc PR A 1
H4B H 0.3223 -0.1497 0.5996 0.121 Uiso 0.602(10) 1 calc PR A 1
H4C H 0.2782 -0.1081 0.5714 0.121 Uiso 0.602(10) 1 calc PR A 1
C5 C 0.3233(5) -0.0068(12) 0.6651(9) 0.055(4) Uani 0.602(10) 1 d PDU A 1
H5A H 0.3522 -0.0140 0.7048 0.066 Uiso 0.602(10) 1 calc PR A 1
C6 C 0.3164(5) 0.0742(13) 0.6043(9) 0.055(3) Uani 0.602(10) 1 d PU A 1
H6A H 0.2879 0.0751 0.5644 0.066 Uiso 0.602(10) 1 calc PR A 1
H6B H 0.3319 0.0518 0.5818 0.066 Uiso 0.602(10) 1 calc PR A 1
C4B C 0.3180(10) -0.1309(19) 0.637(2) 0.062(7) Uani 0.398(10) 1 d PDU A 2
H4L H 0.3193 -0.1604 0.6819 0.093 Uiso 0.398(10) 1 calc PR A 2
H4M H 0.3440 -0.1384 0.6426 0.093 Uiso 0.398(10) 1 calc PR A 2
H4I H 0.2980 -0.1711 0.5930 0.093 Uiso 0.398(10) 1 calc PR A 2
C5B C 0.3053(8) 0.0023(17) 0.6278(14) 0.051(5) Uani 0.398(10) 1 d PDU A 2
H5L H 0.2799 0.0154 0.5791 0.061 Uiso 0.398(10) 1 calc PR A 2
C6B C 0.3383(7) 0.072(2) 0.6336(15) 0.055(5) Uani 0.398(10) 1 d PU A 2
H6L H 0.3640 0.0508 0.6786 0.066 Uiso 0.398(10) 1 calc PR A 2
H6M H 0.3402 0.0602 0.5890 0.066 Uiso 0.398(10) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 N4 2.577(5) . ?
Sm1 N2 2.606(5) . ?
Sm1 N3 2.614(5) . ?
Sm1 N6 2.617(5) . ?
Sm1 N5 2.620(6) . ?
Sm1 N1 2.633(6) . ?
Sm1 S4 2.9427(15) . ?
Sm1 S8 2.9744(19) . ?
Sm1 S6 3.201(2) . ?
Sm2 N11 2.576(5) . ?
Sm2 N9 2.597(5) . ?
Sm2 N12 2.599(5) . ?
Sm2 N7 2.600(5) . ?
Sm2 N10 2.609(4) . ?
Sm2 N8 2.661(6) . ?
Sm2 S5 2.9844(18) . ?
Sm2 S7 3.0495(17) . ?
Sm2 S1 3.0551(15) 8_455 ?
As1 S2 2.1528(16) . ?
As1 S1 2.1610(16) . ?
As1 S3 2.1656(16) . ?
As1 S4 2.1687(15) . ?
As2 S5 2.1490(19) . ?
As2 S8 2.152(2) . ?
As2 S6 2.1537(19) . ?
As2 S7 2.1585(18) . ?
S1 Sm2 3.0551(15) 8_556 ?
N1 C3 1.492(11) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N2 C2 1.473(9) . ?
N2 H2B 0.9000 . ?
N2 H2C 0.9000 . ?
N7 C12 1.475(10) . ?
N7 H7D 0.9000 . ?
N7 H7E 0.9000 . ?
N8 C11 1.453(10) . ?
N8 H8B 0.9000 . ?
N8 H8C 0.9000 . ?
N9 C15 1.451(9) . ?
N9 H9C 0.9000 . ?
N9 H9D 0.9000 . ?
N10 C14 1.453(8) . ?
N10 H10D 0.9000 . ?
N10 H10E 0.9000 . ?
N11 C17 1.429(9) . ?
N11 H11C 0.9000 . ?
N11 H11D 0.9000 . ?
N12 C18 1.478(8) . ?
N12 H12B 0.9000 . ?
N12 H12C 0.9000 . ?
C1 C2 1.468(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.432(12) . ?
C2 H2A 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 C14 1.492(10) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.367(11) . ?
C14 H14A 0.9800 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.494(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.435(11) . ?
C17 H17A 0.9800 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C7 C8 1.40(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N5 1.45(2) . ?
C8 C9 1.48(2) . ?
C8 H8A 0.9800 . ?
C9 N6 1.489(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C7B C9B 1.57(3) . ?
C7B H7L 0.9600 . ?
C7B H7M 0.9600 . ?
C7B H7N 0.9600 . ?
C8B N5 1.55(3) . ?
C8B C9B 1.51(4) . ?
C8B H8L 0.9700 . ?
C8B H8M 0.9700 . ?
C9B N6 1.40(2) . ?
C9B H9L 0.9800 . ?
N5 H5B 0.9000 . ?
N5 H5C 0.9000 . ?
N5 H5F 0.8999 . ?
N5 H5G 0.8999 . ?
N6 H6C 0.9000 . ?
N6 H6D 0.9000 . ?
N6 H6F 0.9000 . ?
N6 H6G 0.8998 . ?
C10 C12 1.389(16) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10B C11 1.559(15) . ?
C10B H10F 0.9600 . ?
C10B H10G 0.9600 . ?
C10B H10H 0.9600 . ?
C11 C12 1.431(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12F 0.9700 . ?
C12 H12G 0.9700 . ?
N3 C6B 1.47(2) . ?
N3 C6 1.512(16) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N3 H3G 0.8999 . ?
N3 H3H 0.9000 . ?
N4 C5 1.399(16) . ?
N4 C5B 1.53(2) . ?
N4 H4G 0.9000 . ?
N4 H4H 0.9000 . ?
N4 H4D 0.9000 . ?
N4 H4E 0.9000 . ?
C4 C5 1.650(14) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.49(3) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C4B C5B 1.651(15) . ?
C4B H4L 0.9600 . ?
C4B H4M 0.9600 . ?
C4B H4I 0.9600 . ?
C5B C6B 1.48(4) . ?
C5B H5L 0.9800 . ?
C6B H6L 0.9700 . ?
C6B H6M 0.9700 . ?

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
N4 Sm1 N2 131.88(18) . . ?
N4 Sm1 N3 65.25(18) . . ?
N2 Sm1 N3 138.42(18) . . ?
N4 Sm1 N6 133.92(18) . . ?
N2 Sm1 N6 70.07(18) . . ?
N3 Sm1 N6 74.21(18) . . ?
N4 Sm1 N5 123.4(2) . . ?
N2 Sm1 N5 104.4(2) . . ?
N3 Sm1 N5 77.3(2) . . ?
N6 Sm1 N5 63.73(18) . . ?
N4 Sm1 N1 71.77(18) . . ?
N2 Sm1 N1 65.08(18) . . ?
N3 Sm1 N1 133.14(19) . . ?
N6 Sm1 N1 131.16(19) . . ?
N5 Sm1 N1 145.7(2) . . ?
N4 Sm1 S4 70.63(13) . . ?
N2 Sm1 S4 76.24(12) . . ?
N3 Sm1 S4 77.40(14) . . ?
N6 Sm1 S4 80.24(12) . . ?
N5 Sm1 S4 140.35(15) . . ?
N1 Sm1 S4 71.45(14) . . ?
N4 Sm1 S8 113.29(14) . . ?
N2 Sm1 S8 71.97(12) . . ?
N3 Sm1 S8 143.53(14) . . ?
N6 Sm1 S8 112.25(13) . . ?
N5 Sm1 S8 74.59(17) . . ?
N1 Sm1 S8 71.14(14) . . ?
S4 Sm1 S8 138.38(6) . . ?
N4 Sm1 S6 66.45(14) . . ?
N2 Sm1 S6 139.30(12) . . ?
N3 Sm1 S6 80.45(14) . . ?
N6 Sm1 S6 127.96(13) . . ?
N5 Sm1 S6 66.77(15) . . ?
N1 Sm1 S6 99.16(15) . . ?
S4 Sm1 S6 136.78(5) . . ?
S8 Sm1 S6 67.37(5) . . ?
N11 Sm2 N9 134.85(18) . . ?
N11 Sm2 N12 65.52(17) . . ?
N9 Sm2 N12 135.10(17) . . ?
N11 Sm2 N7 134.07(18) . . ?
N9 Sm2 N7 78.12(17) . . ?
N12 Sm2 N7 68.78(17) . . ?
N11 Sm2 N10 70.76(16) . . ?
N9 Sm2 N10 65.20(15) . . ?
N12 Sm2 N10 123.53(15) . . ?
N7 Sm2 N10 136.59(16) . . ?
N11 Sm2 N8 143.46(19) . . ?
N9 Sm2 N8 72.55(18) . . ?
N12 Sm2 N8 115.6(2) . . ?
N7 Sm2 N8 64.19(19) . . ?
N10 Sm2 N8 120.78(18) . . ?
N11 Sm2 S5 82.55(14) . . ?
N9 Sm2 S5 89.75(12) . . ?
N12 Sm2 S5 135.15(12) . . ?
N7 Sm2 S5 136.86(13) . . ?
N10 Sm2 S5 67.79(10) . . ?
N8 Sm2 S5 72.67(16) . . ?
N11 Sm2 S7 76.03(14) . . ?
N9 Sm2 S7 141.51(12) . . ?
N12 Sm2 S7 72.58(12) . . ?
N7 Sm2 S7 94.84(13) . . ?
N10 Sm2 S7 128.30(11) . . ?
N8 Sm2 S7 70.42(14) . . ?
S5 Sm2 S7 69.58(5) . . ?
N11 Sm2 S1 81.34(14) . 8_455 ?
N9 Sm2 S1 72.58(12) . 8_455 ?
N12 Sm2 S1 73.29(12) . 8_455 ?
N7 Sm2 S1 81.62(12) . 8_455 ?
N10 Sm2 S1 66.27(10) . 8_455 ?
N8 Sm2 S1 135.08(14) . 8_455 ?
S5 Sm2 S1 134.04(5) . 8_455 ?
S7 Sm2 S1 144.52(5) . 8_455 ?
S2 As1 S1 110.82(7) . . ?
S2 As1 S3 111.55(7) . . ?
S1 As1 S3 109.85(7) . . ?
S2 As1 S4 108.94(7) . . ?
S1 As1 S4 106.31(6) . . ?
S3 As1 S4 109.20(7) . . ?
S5 As2 S8 109.15(9) . . ?
S5 As2 S6 111.14(9) . . ?
S8 As2 S6 105.61(8) . . ?
S5 As2 S7 106.15(7) . . ?
S8 As2 S7 112.76(9) . . ?
S6 As2 S7 112.09(8) . . ?
As1 S1 Sm2 116.66(6) . 8_556 ?
As1 S4 Sm1 117.97(6) . . ?
As2 S5 Sm2 93.00(6) . . ?
As2 S6 Sm1 90.30(7) . . ?
As2 S7 Sm2 91.03(6) . . ?
As2 S8 Sm1 96.62(7) . . ?
C3 N1 Sm1 114.3(5) . . ?
C3 N1 H1D 108.7 . . ?
Sm1 N1 H1D 108.7 . . ?
C3 N1 H1E 108.7 . . ?
Sm1 N1 H1E 108.7 . . ?
H1D N1 H1E 107.6 . . ?
C2 N2 Sm1 117.1(4) . . ?
C2 N2 H2B 108.0 . . ?
Sm1 N2 H2B 108.0 . . ?
C2 N2 H2C 108.0 . . ?
Sm1 N2 H2C 108.0 . . ?
H2B N2 H2C 107.3 . . ?
C12 N7 Sm2 115.9(5) . . ?
C12 N7 H7D 108.3 . . ?
Sm2 N7 H7D 108.3 . . ?
C12 N7 H7E 108.3 . . ?
Sm2 N7 H7E 108.3 . . ?
H7D N7 H7E 107.4 . . ?
C11 N8 Sm2 114.0(5) . . ?
C11 N8 H8B 108.8 . . ?
Sm2 N8 H8B 108.8 . . ?
C11 N8 H8C 108.8 . . ?
Sm2 N8 H8C 108.8 . . ?
H8B N8 H8C 107.6 . . ?
C15 N9 Sm2 112.8(4) . . ?
C15 N9 H9C 109.0 . . ?
Sm2 N9 H9C 109.0 . . ?
C15 N9 H9D 109.0 . . ?
Sm2 N9 H9D 109.0 . . ?
H9C N9 H9D 107.8 . . ?
C14 N10 Sm2 117.1(4) . . ?
C14 N10 H10D 108.0 . . ?
Sm2 N10 H10D 108.0 . . ?
C14 N10 H10E 108.0 . . ?
Sm2 N10 H10E 108.0 . . ?
H10D N10 H10E 107.3 . . ?
C17 N11 Sm2 115.1(4) . . ?
C17 N11 H11C 108.5 . . ?
Sm2 N11 H11C 108.5 . . ?
C17 N11 H11D 108.5 . . ?
Sm2 N11 H11D 108.5 . . ?
H11C N11 H11D 107.5 . . ?
C18 N12 Sm2 116.7(4) . . ?
C18 N12 H12B 108.1 . . ?
Sm2 N12 H12B 108.1 . . ?
C18 N12 H12C 108.1 . . ?
Sm2 N12 H12C 108.1 . . ?
H12B N12 H12C 107.3 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 112.3(9) . . ?
C3 C2 N2 111.0(7) . . ?
C1 C2 N2 116.6(7) . . ?
C3 C2 H2A 105.3 . . ?
C1 C2 H2A 105.3 . . ?
N2 C2 H2A 105.3 . . ?
C2 C3 N1 114.5(7) . . ?
C2 C3 H3A 108.6 . . ?
N1 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
N1 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N10 115.8(6) . . ?
C15 C14 C13 121.5(7) . . ?
N10 C14 C13 116.2(7) . . ?
C15 C14 H14A 98.6 . . ?
N10 C14 H14A 98.6 . . ?
C13 C14 H14A 98.6 . . ?
C14 C15 N9 119.3(7) . . ?
C14 C15 H15A 107.5 . . ?
N9 C15 H15A 107.5 . . ?
C14 C15 H15B 107.5 . . ?
N9 C15 H15B 107.5 . . ?
H15A C15 H15B 107.0 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N11 C17 C18 115.7(7) . . ?
N11 C17 C16 117.3(7) . . ?
C18 C17 C16 112.8(7) . . ?
N11 C17 H17A 102.7 . . ?
C18 C17 H17A 102.7 . . ?
C16 C17 H17A 102.7 . . ?
C17 C18 N12 112.6(6) . . ?
C17 C18 H18A 109.1 . . ?
N12 C18 H18A 109.1 . . ?
C17 C18 H18B 109.1 . . ?
N12 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C7 C8 N5 121.7(15) . . ?
C7 C8 C9 112.3(15) . . ?
N5 C8 C9 108.6(14) . . ?
C7 C8 H8A 104.1 . . ?
N5 C8 H8A 104.1 . . ?
C9 C8 H8A 104.1 . . ?
C8 C9 N6 111.6(12) . . ?
C8 C9 H9A 109.3 . . ?
N6 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
N6 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C9B C7B H7L 109.5 . . ?
C9B C7B H7M 109.5 . . ?
H7L C7B H7M 109.5 . . ?
C9B C7B H7N 109.5 . . ?
H7L C7B H7N 109.5 . . ?
H7M C7B H7N 109.5 . . ?
N5 C8B C9B 106(2) . . ?
N5 C8B H8L 110.5 . . ?
C9B C8B H8L 110.5 . . ?
N5 C8B H8M 110.5 . . ?
C9B C8B H8M 110.5 . . ?
H8L C8B H8M 108.7 . . ?
N6 C9B C8B 106(2) . . ?
N6 C9B C7B 115.6(16) . . ?
C8B C9B C7B 93.4(19) . . ?
N6 C9B H9L 113.3 . . ?
C8B C9B H9L 113.3 . . ?
C7B C9B H9L 113.3 . . ?
C8 N5 Sm1 118.6(8) . . ?
C8B N5 Sm1 113.7(10) . . ?
C8 N5 H5B 107.7 . . ?
C8B N5 H5B 85.8 . . ?
Sm1 N5 H5B 107.7 . . ?
C8 N5 H5C 107.7 . . ?
C8B N5 H5C 130.2 . . ?
Sm1 N5 H5C 107.7 . . ?
H5B N5 H5C 107.1 . . ?
C8 N5 H5F 124.6 . . ?
C8B N5 H5F 108.4 . . ?
Sm1 N5 H5F 108.5 . . ?
H5C N5 H5F 82.3 . . ?
C8 N5 H5G 84.2 . . ?
C8B N5 H5G 110.0 . . ?
Sm1 N5 H5G 108.5 . . ?
H5B N5 H5G 129.4 . . ?
H5F N5 H5G 107.5 . . ?
C9B N6 Sm1 116.4(10) . . ?
C9 N6 Sm1 115.9(6) . . ?
C9B N6 H6C 78.9 . . ?
C9 N6 H6C 108.3 . . ?
Sm1 N6 H6C 108.3 . . ?
C9B N6 H6D 130.2 . . ?
C9 N6 H6D 108.3 . . ?
Sm1 N6 H6D 108.3 . . ?
H6C N6 H6D 107.4 . . ?
C9B N6 H6F 107.0 . . ?
C9 N6 H6F 130.2 . . ?
Sm1 N6 H6F 108.0 . . ?
H6D N6 H6F 77.4 . . ?
C9B N6 H6G 109.8 . . ?
C9 N6 H6G 80.9 . . ?
Sm1 N6 H6G 108.0 . . ?
H6C N6 H6G 133.0 . . ?
H6F N6 H6G 107.3 . . ?
C12 C10 H10A 109.5 . . ?
C12 C10 H10B 109.5 . . ?
C12 C10 H10C 109.5 . . ?
C11 C10B H10F 109.5 . . ?
C11 C10B H10G 109.5 . . ?
H10F C10B H10G 109.5 . . ?
C11 C10B H10H 109.5 . . ?
H10F C10B H10H 109.5 . . ?
H10G C10B H10H 109.5 . . ?
C12 C11 N8 109.9(7) . . ?
C12 C11 C10B 105.5(11) . . ?
N8 C11 C10B 124.1(10) . . ?
C12 C11 H11A 109.7 . . ?
N8 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
N8 C11 H11B 109.7 . . ?
C10B C11 H11B 96.9 . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11F 105.3 . . ?
N8 C11 H11F 105.3 . . ?
C10B C11 H11F 105.3 . . ?
H11A C11 H11F 116.7 . . ?
C10 C12 C11 110.2(10) . . ?
C10 C12 N7 116.6(11) . . ?
C11 C12 N7 112.8(7) . . ?
C10 C12 H12A 105.4 . . ?
C11 C12 H12A 105.4 . . ?
N7 C12 H12A 105.4 . . ?
C11 C12 H12F 109.0 . . ?
N7 C12 H12F 109.0 . . ?
H12A C12 H12F 115.2 . . ?
C10 C12 H12G 98.1 . . ?
C11 C12 H12G 109.0 . . ?
N7 C12 H12G 109.0 . . ?
H12F C12 H12G 107.8 . . ?
C6B N3 Sm1 116.9(10) . . ?
C6 N3 Sm1 111.0(7) . . ?
C6B N3 H3C 126.0 . . ?
C6 N3 H3C 109.4 . . ?
Sm1 N3 H3C 109.4 . . ?
C6B N3 H3D 81.5 . . ?
C6 N3 H3D 109.4 . . ?
Sm1 N3 H3D 109.4 . . ?
H3C N3 H3D 108.0 . . ?
C6B N3 H3G 108.0 . . ?
C6 N3 H3G 84.8 . . ?
Sm1 N3 H3G 107.9 . . ?
H3D N3 H3G 131.0 . . ?
C6B N3 H3H 108.4 . . ?
C6 N3 H3H 133.0 . . ?
Sm1 N3 H3H 108.0 . . ?
H3C N3 H3H 80.5 . . ?
H3G N3 H3H 107.2 . . ?
C5 N4 Sm1 117.5(7) . . ?
C5B N4 Sm1 114.8(9) . . ?
C5 N4 H4G 107.9 . . ?
C5B N4 H4G 130.1 . . ?
Sm1 N4 H4G 107.9 . . ?
C5 N4 H4H 107.9 . . ?
C5B N4 H4H 83.4 . . ?
Sm1 N4 H4H 107.9 . . ?
H4G N4 H4H 107.2 . . ?
C5 N4 H4D 108.0 . . ?
C5B N4 H4D 130.1 . . ?
Sm1 N4 H4D 108.1 . . ?
H4H N4 H4D 107.0 . . ?
C5 N4 H4E 107.7 . . ?
C5B N4 H4E 83.2 . . ?
Sm1 N4 H4E 107.8 . . ?
H4G N4 H4E 107.5 . . ?
H4D N4 H4E 107.2 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 C6 107.9(13) . . ?
N4 C5 C4 110.0(18) . . ?
C6 C5 C4 101.7(17) . . ?
N4 C5 H5A 112.2 . . ?
C6 C5 H5A 112.2 . . ?
C4 C5 H5A 112.2 . . ?
C5 C6 N3 109.5(11) . . ?
C5 C6 H6A 109.8 . . ?
N3 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
N3 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
C5B C4B H4L 109.5 . . ?
C5B C4B H4M 109.5 . . ?
H4L C4B H4M 109.5 . . ?
C5B C4B H4I 109.5 . . ?
H4L C4B H4I 109.5 . . ?
H4M C4B H4I 109.5 . . ?
C6B C5B N4 109.9(18) . . ?
C6B C5B C4B 110(3) . . ?
N4 C5B C4B 105(2) . . ?
C6B C5B H5L 110.6 . . ?
N4 C5B H5L 110.6 . . ?
C4B C5B H5L 110.6 . . ?
N3 C6B C5B 109.0(17) . . ?
N3 C6B H6L 109.9 . . ?
C5B C6B H6L 109.9 . . ?
N3 C6B H6M 109.9 . . ?
C5B C6B H6M 109.9 . . ?
H6L C6B H6M 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_IIa
_database_code_depnum_ccdc_archive 'CCDC 1403235'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H30 As N6 S4 Tb'
_chemical_formula_sum            'C9 H30 As N6 S4 Tb'
_chemical_formula_weight         584.48

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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'


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

_cell_length_a                   9.3565(5)
_cell_length_b                   19.5640(10)
_cell_length_c                   14.1839(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 129.238(2)
_cell_angle_gamma                90.00
_cell_volume                     2010.95(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3549
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5314
_exptl_absorpt_correction_T_max  0.6342
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14819
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3549
_reflns_number_gt                3312
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
the DELU restraint prevents the thermal ellipsoids of all adjacent 
C and N atoms from adopting different orientations, 
and the DFIX restraint makes all the CCC and CCN distances 
approximately equal. 
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)+(0.0639P)²+12.1722P] 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         3549
_refine_ls_number_parameters     209
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1094
_refine_ls_goodness_of_fit_ref   1.066
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.33616(4) 0.174694(15) 0.53370(3) 0.02700(14) Uani 1 1 d . A 1
As1 As 0.65572(8) 0.18247(3) 0.47425(5) 0.02386(17) Uani 1 1 d . A 1
S2 S 0.7181(17) 0.1518(16) 0.6429(14) 0.066(5) Uani 0.73(5) 1 d P A 1
S2' S 0.678(3) 0.1217(14) 0.613(2) 0.032(5) Uani 0.27(5) 1 d P A 1
S1 S 0.3640(2) 0.20985(8) 0.35488(13) 0.0284(3) Uani 1 1 d . A 1
S3 S 0.8167(3) 0.27203(11) 0.5167(3) 0.0813(10) Uani 1 1 d . A 1
S4 S 0.7036(2) 0.10563(10) 0.3901(2) 0.0497(5) Uani 1 1 d . A 1
N3 N 0.5227(10) 0.1253(4) 0.7461(7) 0.0599(15) Uani 1 1 d DU A 1
H3A H 0.5765 0.0869 0.7470 0.072 Uiso 1 1 calc R A 1
H3B H 0.6140 0.1551 0.7968 0.072 Uiso 1 1 calc R A 1
N4 N 0.1545(9) 0.1544(4) 0.6067(6) 0.0493(13) Uani 1 1 d DU A 1
H4A H 0.1432 0.1943 0.6328 0.059 Uiso 1 1 calc R A 1
H4B H 0.0403 0.1404 0.5431 0.059 Uiso 1 1 calc R A 1
N5 N 0.5070(10) 0.2843(4) 0.6300(7) 0.0685(19) Uani 1 1 d DU A 1
H5A H 0.5478 0.2857 0.7069 0.082 Uiso 1 1 calc R A 1
H5B H 0.6062 0.2850 0.6332 0.082 Uiso 1 1 calc R A 1
N6 N 0.1227(8) 0.2766(3) 0.4581(6) 0.0457(14) Uani 1 1 d DU A 1
H6A H 0.0810 0.2875 0.3829 0.055 Uiso 1 1 calc R A 1
H6B H 0.0246 0.2648 0.4525 0.055 Uiso 1 1 calc R A 1
C4 C 0.5200(16) 0.0480(5) 0.8840(10) 0.078(3) Uani 1 1 d DU A 1
H4C H 0.6512 0.0538 0.9434 0.117 Uiso 1 1 calc R A 1
H4D H 0.4934 0.0069 0.8384 0.117 Uiso 1 1 calc R A 1
H4E H 0.4679 0.0447 0.9244 0.117 Uiso 1 1 calc R A 1
C5 C 0.4371(10) 0.1086(5) 0.7985(8) 0.0640(19) Uani 1 1 d DU A 1
H5C H 0.4598 0.1480 0.8490 0.077 Uiso 1 1 calc R A 1
C6 C 0.2334(10) 0.1048(5) 0.7027(7) 0.0610(18) Uani 1 1 d DU A 1
H6C H 0.2013 0.0595 0.6670 0.073 Uiso 1 1 calc R A 1
H6D H 0.1775 0.1106 0.7410 0.073 Uiso 1 1 calc R A 1
C7 C 0.0905(13) 0.4010(4) 0.4780(9) 0.066(2) Uani 1 1 d DU A 1
H7A H -0.0241 0.3936 0.4626 0.099 Uiso 1 1 calc R A 1
H7B H 0.0665 0.4100 0.4026 0.099 Uiso 1 1 calc R A 1
H7C H 0.1531 0.4394 0.5315 0.099 Uiso 1 1 calc R A 1
C8 C 0.2108(9) 0.3377(3) 0.5371(7) 0.0496(17) Uani 1 1 d DU A 1
H8A H 0.2328 0.3288 0.6133 0.059 Uiso 1 1 calc R A 1
C9 C 0.3949(10) 0.3451(4) 0.5650(9) 0.0603(19) Uani 1 1 d DU A 1
H9A H 0.3762 0.3505 0.4899 0.072 Uiso 1 1 calc R A 1
H9B H 0.4581 0.3854 0.6146 0.072 Uiso 1 1 calc R A 1
N1 N 0.0199(8) 0.1437(3) 0.3368(6) 0.0403(12) Uani 1 1 d DU A 1
H1A H -0.0647 0.1493 0.3474 0.048 Uiso 1 1 calc R A 1
H1B H -0.0083 0.1727 0.2780 0.048 Uiso 1 1 calc R A 1
N2 N 0.3051(12) 0.0495(4) 0.4798(8) 0.082(2) Uani 1 1 d DU A 1
H2A H 0.3515 0.0424 0.4411 0.098 Uiso 1 1 calc R A 1
H2B H 0.3721 0.0246 0.5488 0.098 Uiso 1 1 calc R A 1
C2 C 0.0075(12) 0.0733(4) 0.2962(8) 0.065(2) Uani 1 1 d DU A 1
H2C H 0.0963 0.0765 0.2813 0.078 Uiso 1 1 calc R A 1
C1 C -0.1601(16) 0.0586(6) 0.1716(9) 0.094(4) Uani 1 1 d DU A 1
H1C H -0.1966 0.0988 0.1223 0.141 Uiso 1 1 calc R A 1
H1D H -0.2574 0.0452 0.1730 0.141 Uiso 1 1 calc R A 1
H1E H -0.1357 0.0223 0.1381 0.141 Uiso 1 1 calc R A 1
C3 C 0.1094(16) 0.0254(7) 0.4006(12) 0.070(3) Uani 0.60 1 d PDU A 1
H3C H 0.0999 -0.0210 0.3732 0.084 Uiso 0.60 1 calc PR A 1
H3D H 0.0612 0.0270 0.4442 0.084 Uiso 0.60 1 calc PR A 1
C3' C 0.203(3) 0.0430(11) 0.355(2) 0.059(4) Uani 0.40 1 d PU B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 N5 2.501(7) . ?
Tb1 N4 2.519(6) . ?
Tb1 N2 2.528(8) . ?
Tb1 N6 2.531(6) . ?
Tb1 N3 2.531(7) . ?
Tb1 N1 2.544(6) . ?
Tb1 S1 2.7948(15) . ?
Tb1 S2' 2.835(12) . ?
Tb1 S2 2.893(6) . ?
As1 S3 2.134(2) . ?
As1 S4 2.1363(18) . ?
As1 S2 2.158(5) . ?
As1 S1 2.1809(15) . ?
As1 S2' 2.193(12) . ?
S2 S2' 0.682(9) . ?
N3 C5 1.432(7) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C6 1.438(7) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C9 1.465(8) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.481(7) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C4 C5 1.513(8) . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C5 C6 1.486(8) . ?
C5 H5C 0.9800 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.520(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.511(8) . ?
C8 H8A 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N1 C2 1.469(7) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.495(9) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C2 C1 1.469(8) . ?
C2 C3 1.481(9) . ?
C2 H2C 0.9800 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?

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
N5 Tb1 N4 106.0(3) . . ?
N5 Tb1 N2 155.1(3) . . ?
N4 Tb1 N2 89.6(3) . . ?
N5 Tb1 N6 67.5(2) . . ?
N4 Tb1 N6 75.0(2) . . ?
N2 Tb1 N6 136.6(2) . . ?
N5 Tb1 N3 87.5(3) . . ?
N4 Tb1 N3 65.6(2) . . ?
N2 Tb1 N3 81.4(3) . . ?
N6 Tb1 N3 124.8(2) . . ?
N5 Tb1 N1 134.6(2) . . ?
N4 Tb1 N1 78.1(2) . . ?
N2 Tb1 N1 66.8(2) . . ?
N6 Tb1 N1 70.40(18) . . ?
N3 Tb1 N1 131.5(2) . . ?
N5 Tb1 S1 83.7(2) . . ?
N4 Tb1 S1 152.42(15) . . ?
N2 Tb1 S1 91.3(2) . . ?
N6 Tb1 S1 85.60(17) . . ?
N3 Tb1 S1 141.67(15) . . ?
N1 Tb1 S1 76.95(14) . . ?
N5 Tb1 S2' 85.7(7) . . ?
N4 Tb1 S2' 131.7(3) . . ?
N2 Tb1 S2' 69.5(7) . . ?
N6 Tb1 S2' 147.9(6) . . ?
N3 Tb1 S2' 68.4(3) . . ?
N1 Tb1 S2' 125.9(7) . . ?
S1 Tb1 S2' 73.8(2) . . ?
N5 Tb1 S2 72.2(7) . . ?
N4 Tb1 S2 132.99(17) . . ?
N2 Tb1 S2 83.0(7) . . ?
N6 Tb1 S2 136.5(6) . . ?
N3 Tb1 S2 67.39(17) . . ?
N1 Tb1 S2 137.4(6) . . ?
S1 Tb1 S2 74.40(10) . . ?
S2' Tb1 S2 13.63(18) . . ?
S3 As1 S4 112.04(9) . . ?
S3 As1 S2 105.5(9) . . ?
S4 As1 S2 114.7(8) . . ?
S3 As1 S1 109.32(8) . . ?
S4 As1 S1 109.93(7) . . ?
S2 As1 S1 104.91(14) . . ?
S3 As1 S2' 122.8(9) . . ?
S4 As1 S2' 100.6(6) . . ?
S2 As1 S2' 18.0(2) . . ?
S1 As1 S2' 101.1(5) . . ?
S2' S2 As1 84.0(14) . . ?
S2' S2 Tb1 78.3(12) . . ?
As1 S2 Tb1 89.3(2) . . ?
S2 S2' As1 78.0(14) . . ?
S2 S2' Tb1 88.1(12) . . ?
As1 S2' Tb1 90.1(4) . . ?
As1 S1 Tb1 91.39(5) . . ?
C5 N3 Tb1 120.9(5) . . ?
C5 N3 H3A 107.1 . . ?
Tb1 N3 H3A 107.1 . . ?
C5 N3 H3B 107.1 . . ?
Tb1 N3 H3B 107.1 . . ?
H3A N3 H3B 106.8 . . ?
C6 N4 Tb1 114.8(5) . . ?
C6 N4 H4A 108.6 . . ?
Tb1 N4 H4A 108.6 . . ?
C6 N4 H4B 108.6 . . ?
Tb1 N4 H4B 108.6 . . ?
H4A N4 H4B 107.5 . . ?
C9 N5 Tb1 113.4(5) . . ?
C9 N5 H5A 108.9 . . ?
Tb1 N5 H5A 108.9 . . ?
C9 N5 H5B 108.9 . . ?
Tb1 N5 H5B 108.9 . . ?
H5A N5 H5B 107.7 . . ?
C8 N6 Tb1 113.7(4) . . ?
C8 N6 H6A 108.8 . . ?
Tb1 N6 H6A 108.8 . . ?
C8 N6 H6B 108.8 . . ?
Tb1 N6 H6B 108.8 . . ?
H6A N6 H6B 107.7 . . ?
C5 C4 H4C 109.5 . . ?
C5 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C5 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N3 C5 C6 110.6(7) . . ?
N3 C5 C4 115.0(7) . . ?
C6 C5 C4 113.9(8) . . ?
N3 C5 H5C 105.5 . . ?
C6 C5 H5C 105.5 . . ?
C4 C5 H5C 105.5 . . ?
N4 C6 C5 115.2(6) . . ?
N4 C6 H6C 108.5 . . ?
C5 C6 H6C 108.5 . . ?
N4 C6 H6D 108.5 . . ?
C5 C6 H6D 108.5 . . ?
H6C C6 H6D 107.5 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 C8 C9 105.8(6) . . ?
N6 C8 C7 112.1(6) . . ?
C9 C8 C7 112.9(7) . . ?
N6 C8 H8A 108.6 . . ?
C9 C8 H8A 108.6 . . ?
C7 C8 H8A 108.6 . . ?
N5 C9 C8 109.3(7) . . ?
N5 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
N5 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
C2 N1 Tb1 113.8(4) . . ?
C2 N1 H1A 108.8 . . ?
Tb1 N1 H1A 108.8 . . ?
C2 N1 H1B 108.8 . . ?
Tb1 N1 H1B 108.8 . . ?
H1A N1 H1B 107.7 . . ?
C3 N2 Tb1 112.6(7) . . ?
C3 N2 H2A 109.1 . . ?
Tb1 N2 H2A 109.1 . . ?
C3 N2 H2B 109.1 . . ?
Tb1 N2 H2B 109.1 . . ?
H2A N2 H2B 107.8 . . ?
N1 C2 C1 114.5(7) . . ?
N1 C2 C3 111.0(8) . . ?
C1 C2 C3 127.0(9) . . ?
N1 C2 H2C 99.1 . . ?
C1 C2 H2C 99.1 . . ?
C3 C2 H2C 99.1 . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
C2 C3 N2 105.1(9) . . ?
C2 C3 H3C 110.7 . . ?
N2 C3 H3C 110.7 . . ?
C2 C3 H3D 110.7 . . ?
N2 C3 H3D 110.7 . . ?
H3C C3 H3D 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.170
####################################################################### 
# 
# 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_IIb
_database_code_depnum_ccdc_archive 'CCDC 1403236'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H30 As Dy N6 S4'
_chemical_formula_sum            'C9 H30 As Dy N6 S4'
_chemical_formula_weight         588.05

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.3353(9)
_cell_length_b                   19.5603(18)
_cell_length_c                   14.2064(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.973(4)
_cell_angle_gamma                90.00
_cell_volume                     2016.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9139
_cell_measurement_theta_min      2.4187
_cell_measurement_theta_max      28.3356

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    5.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5219
_exptl_absorpt_correction_T_max  0.6257
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16146
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4125
_reflns_number_gt                3675
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The DELU restraint prevents the thermal ellipsoids of 
all adjacent C and N atoms from adopting different 
orientations, and the DFIX restraint makes all the CCC 
and CCN distances approximately equal. 
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)+(0.0626P)²+21.2363P] 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         4125
_refine_ls_number_parameters     209
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1309
_refine_ls_wR_factor_gt          0.1263
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.061
_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
Dy1 Dy 0.33725(4) 0.175672(17) 0.53506(3) 0.02583(13) Uani 1 1 d . A 1
As1 As 0.65588(9) 0.18379(4) 0.47381(7) 0.02432(18) Uani 1 1 d . A 1
S1 S 0.3637(2) 0.20971(10) 0.35583(16) 0.0284(4) Uani 1 1 d . A 1
S2 S 0.723(2) 0.1559(17) 0.6454(17) 0.054(4) Uani 0.69(7) 1 d P A 1
S2' S 0.685(4) 0.126(2) 0.616(2) 0.034(6) Uani 0.31(7) 1 d P A 1
S3 S 0.8131(3) 0.27403(12) 0.5114(3) 0.0662(9) Uani 1 1 d . A 1
S4 S 0.7047(3) 0.10564(12) 0.3914(2) 0.0496(6) Uani 1 1 d . A 1
N1 N 0.5224(11) 0.1254(5) 0.7444(8) 0.0504(16) Uani 1 1 d DU A 1
H1A H 0.5727 0.0863 0.7437 0.060 Uiso 1 1 calc R A 1
H1B H 0.6162 0.1543 0.7947 0.060 Uiso 1 1 calc R A 1
N2 N 0.1559(10) 0.1554(4) 0.6070(7) 0.0417(13) Uani 1 1 d DU A 1
H2A H 0.1479 0.1951 0.6357 0.050 Uiso 1 1 calc R A 1
H2B H 0.0408 0.1430 0.5434 0.050 Uiso 1 1 calc R A 1
N3 N 0.5069(12) 0.2841(4) 0.6329(9) 0.068(2) Uani 1 1 d DU A 1
H3A H 0.5438 0.2854 0.7086 0.082 Uiso 1 1 calc R A 1
H3B H 0.6084 0.2845 0.6385 0.082 Uiso 1 1 calc R A 1
N4 N 0.1247(10) 0.2770(3) 0.4579(7) 0.0411(15) Uani 1 1 d DU A 1
H4A H 0.0863 0.2880 0.3837 0.049 Uiso 1 1 calc R A 1
H4B H 0.0249 0.2652 0.4505 0.049 Uiso 1 1 calc R A 1
N5 N 0.3097(13) 0.0504(5) 0.4812(9) 0.071(2) Uani 1 1 d DU A 1
H5A H 0.3533 0.0440 0.4405 0.085 Uiso 1 1 calc R A 1
H5B H 0.3799 0.0257 0.5498 0.085 Uiso 1 1 calc R A 1
N6 N 0.0234(10) 0.1438(3) 0.3403(7) 0.0386(13) Uani 1 1 d DU A 1
H6A H -0.0617 0.1502 0.3503 0.046 Uiso 1 1 calc R A 1
H6B H -0.0039 0.1722 0.2811 0.046 Uiso 1 1 calc R A 1
C1 C 0.5185(17) 0.0488(6) 0.8823(11) 0.066(3) Uani 1 1 d DU A 1
H1C H 0.6489 0.0551 0.9433 0.098 Uiso 1 1 calc R A 1
H1D H 0.4955 0.0083 0.8364 0.098 Uiso 1 1 calc R A 1
H1E H 0.4628 0.0441 0.9203 0.098 Uiso 1 1 calc R A 1
C2 C 0.4370(11) 0.1099(5) 0.7989(8) 0.057(2) Uani 1 1 d DU A 1
H2C H 0.4574 0.1496 0.8482 0.068 Uiso 1 1 calc R A 1
C3 C 0.2322(12) 0.1036(5) 0.7006(9) 0.057(2) Uani 1 1 d DU A 1
H3C H 0.2051 0.0588 0.6635 0.068 Uiso 1 1 calc R A 1
H3D H 0.1721 0.1068 0.7366 0.068 Uiso 1 1 calc R A 1
C4 C 0.0930(15) 0.4019(4) 0.4774(10) 0.058(3) Uani 1 1 d DU A 1
H4C H -0.0239 0.3951 0.4593 0.087 Uiso 1 1 calc R A 1
H4D H 0.0739 0.4112 0.4038 0.087 Uiso 1 1 calc R A 1
H4E H 0.1551 0.4399 0.5317 0.087 Uiso 1 1 calc R A 1
C5 C 0.2102(11) 0.3378(4) 0.5365(9) 0.050(2) Uani 1 1 d DU A 1
H5C H 0.2281 0.3289 0.6112 0.059 Uiso 1 1 calc R A 1
C6 C 0.3981(12) 0.3452(5) 0.5680(10) 0.058(2) Uani 1 1 d DU A 1
H6C H 0.3837 0.3506 0.4945 0.070 Uiso 1 1 calc R A 1
H6D H 0.4605 0.3853 0.6181 0.070 Uiso 1 1 calc R A 1
C8 C 0.0115(14) 0.0734(4) 0.3018(9) 0.064(2) Uani 1 1 d DU A 1
H8A H 0.0993 0.0767 0.2859 0.077 Uiso 1 1 calc R A 1
C7 C -0.1583(18) 0.0598(7) 0.1760(11) 0.089(4) Uani 1 1 d DU A 1
H7A H -0.1954 0.1008 0.1287 0.133 Uiso 1 1 calc R A 1
H7B H -0.2551 0.0452 0.1774 0.133 Uiso 1 1 calc R A 1
H7C H -0.1340 0.0246 0.1406 0.133 Uiso 1 1 calc R A 1
C9 C 0.1164(17) 0.0250(8) 0.4060(14) 0.062(3) Uani 0.55 1 d PDU A 1
H9A H 0.0707 0.0260 0.4512 0.075 Uiso 0.55 1 calc PR A 1
H9B H 0.1076 -0.0213 0.3784 0.075 Uiso 0.55 1 calc PR A 1
C9' C 0.207(3) 0.0421(11) 0.360(2) 0.053(3) Uani 0.45 1 d PU B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 N3 2.484(9) . ?
Dy1 N2 2.499(7) . ?
Dy1 N4 2.517(7) . ?
Dy1 N1 2.517(8) . ?
Dy1 N5 2.532(9) . ?
Dy1 N6 2.536(8) . ?
Dy1 S1 2.7891(18) . ?
Dy1 S2' 2.843(11) . ?
Dy1 S2 2.909(7) . ?
As1 S3 2.138(2) . ?
As1 S4 2.142(2) . ?
As1 S2 2.172(9) . ?
As1 S2' 2.173(16) . ?
As1 S1 2.1805(18) . ?
S2 S2' 0.667(15) . ?
N1 C2 1.450(8) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.452(8) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N3 C6 1.460(8) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.476(8) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C9 1.490(10) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.459(8) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.509(8) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 C3 1.504(8) . ?
C2 H2C 0.9800 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 C5 1.523(8) . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C5 C6 1.521(8) . ?
C5 H5C 0.9800 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C8 C7 1.489(9) . ?
C8 C9 1.491(9) . ?
C8 H8A 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

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
N3 Dy1 N2 105.3(3) . . ?
N3 Dy1 N4 67.8(2) . . ?
N2 Dy1 N4 75.6(2) . . ?
N3 Dy1 N1 87.2(3) . . ?
N2 Dy1 N1 66.0(2) . . ?
N4 Dy1 N1 126.2(3) . . ?
N3 Dy1 N5 154.6(3) . . ?
N2 Dy1 N5 90.2(3) . . ?
N4 Dy1 N5 136.8(3) . . ?
N1 Dy1 N5 80.9(3) . . ?
N3 Dy1 N6 135.5(2) . . ?
N2 Dy1 N6 78.0(2) . . ?
N4 Dy1 N6 70.4(2) . . ?
N1 Dy1 N6 131.1(3) . . ?
N5 Dy1 N6 66.7(3) . . ?
N3 Dy1 S1 85.2(3) . . ?
N2 Dy1 S1 152.02(17) . . ?
N4 Dy1 S1 84.97(19) . . ?
N1 Dy1 S1 141.52(16) . . ?
N5 Dy1 S1 90.3(3) . . ?
N6 Dy1 S1 76.54(16) . . ?
N3 Dy1 S2' 84.2(10) . . ?
N2 Dy1 S2' 132.5(4) . . ?
N4 Dy1 S2' 146.0(9) . . ?
N1 Dy1 S2' 68.2(3) . . ?
N5 Dy1 S2' 70.6(10) . . ?
N6 Dy1 S2' 126.8(9) . . ?
S1 Dy1 S2' 73.5(2) . . ?
N3 Dy1 S2 71.0(8) . . ?
N2 Dy1 S2 133.3(2) . . ?
N4 Dy1 S2 135.1(7) . . ?
N1 Dy1 S2 67.3(2) . . ?
N5 Dy1 S2 83.7(8) . . ?
N6 Dy1 S2 138.1(6) . . ?
S1 Dy1 S2 74.56(16) . . ?
S2' Dy1 S2 13.3(3) . . ?
S3 As1 S4 112.15(11) . . ?
S3 As1 S2 105.1(9) . . ?
S4 As1 S2 115.1(8) . . ?
S3 As1 S2' 122.0(13) . . ?
S4 As1 S2' 101.3(10) . . ?
S2 As1 S2' 17.7(4) . . ?
S3 As1 S1 109.29(9) . . ?
S4 As1 S1 109.83(9) . . ?
S2 As1 S1 105.00(17) . . ?
S2' As1 S1 101.4(5) . . ?
As1 S1 Dy1 91.66(6) . . ?
S2' S2 As1 81.2(19) . . ?
S2' S2 Dy1 77.7(12) . . ?
As1 S2 Dy1 88.7(3) . . ?
S2 S2' As1 81(2) . . ?
S2 S2' Dy1 89.1(13) . . ?
As1 S2' Dy1 90.4(4) . . ?
C2 N1 Dy1 120.8(5) . . ?
C2 N1 H1A 107.1 . . ?
Dy1 N1 H1A 107.1 . . ?
C2 N1 H1B 107.1 . . ?
Dy1 N1 H1B 107.1 . . ?
H1A N1 H1B 106.8 . . ?
C3 N2 Dy1 114.6(5) . . ?
C3 N2 H2A 108.6 . . ?
Dy1 N2 H2A 108.6 . . ?
C3 N2 H2B 108.6 . . ?
Dy1 N2 H2B 108.6 . . ?
H2A N2 H2B 107.6 . . ?
C6 N3 Dy1 113.6(6) . . ?
C6 N3 H3A 108.8 . . ?
Dy1 N3 H3A 108.8 . . ?
C6 N3 H3B 108.8 . . ?
Dy1 N3 H3B 108.8 . . ?
H3A N3 H3B 107.7 . . ?
C5 N4 Dy1 113.7(5) . . ?
C5 N4 H4A 108.8 . . ?
Dy1 N4 H4A 108.8 . . ?
C5 N4 H4B 108.8 . . ?
Dy1 N4 H4B 108.8 . . ?
H4A N4 H4B 107.7 . . ?
C9 N5 Dy1 112.7(8) . . ?
C9 N5 H5A 109.0 . . ?
Dy1 N5 H5A 109.0 . . ?
C9 N5 H5B 109.0 . . ?
Dy1 N5 H5B 109.0 . . ?
H5A N5 H5B 107.8 . . ?
C8 N6 Dy1 113.8(5) . . ?
C8 N6 H6A 108.8 . . ?
Dy1 N6 H6A 108.8 . . ?
C8 N6 H6B 108.8 . . ?
Dy1 N6 H6B 108.8 . . ?
H6A N6 H6B 107.7 . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N1 C2 C3 109.0(7) . . ?
N1 C2 C1 114.2(8) . . ?
C3 C2 C1 112.5(8) . . ?
N1 C2 H2C 106.9 . . ?
C3 C2 H2C 106.9 . . ?
C1 C2 H2C 106.9 . . ?
N2 C3 C2 113.5(7) . . ?
N2 C3 H3C 108.9 . . ?
C2 C3 H3C 108.9 . . ?
N2 C3 H3D 108.9 . . ?
C2 C3 H3D 108.9 . . ?
H3C C3 H3D 107.7 . . ?
C5 C4 H4C 109.5 . . ?
C5 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C5 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N4 C5 C6 105.8(7) . . ?
N4 C5 C4 112.8(7) . . ?
C6 C5 C4 112.3(8) . . ?
N4 C5 H5C 108.6 . . ?
C6 C5 H5C 108.6 . . ?
C4 C5 H5C 108.6 . . ?
N3 C6 C5 108.9(8) . . ?
N3 C6 H6C 109.9 . . ?
C5 C6 H6C 109.9 . . ?
N3 C6 H6D 109.9 . . ?
C5 C6 H6D 109.9 . . ?
H6C C6 H6D 108.3 . . ?
N6 C8 C7 113.0(9) . . ?
N6 C8 C9 112.4(10) . . ?
C7 C8 C9 128.1(10) . . ?
N6 C8 H8A 98.5 . . ?
C7 C8 H8A 98.5 . . ?
C9 C8 H8A 98.5 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C9 C8 104.1(10) . . ?
N5 C9 H9A 110.9 . . ?
C8 C9 H9A 110.9 . . ?
N5 C9 H9B 110.9 . . ?
C8 C9 H9B 110.9 . . ?
H9A C9 H9B 109.0 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         3.049
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.206
####################################################################### 
# 
# 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_IIc
_database_code_depnum_ccdc_archive 'CCDC 1403237'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H30 As Ho N6 S4'
_chemical_formula_sum            'C9 H30 As Ho N6 S4'
_chemical_formula_weight         590.48

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.3226(6)
_cell_length_b                   19.5184(12)
_cell_length_c                   14.1847(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.966(3)
_cell_angle_gamma                90.00
_cell_volume                     2006.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      2.4224
_cell_measurement_theta_max      28.3868

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    5.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5583
_exptl_absorpt_correction_T_max  0.7149
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16799
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4152
_reflns_number_gt                3853
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The DELU restraint prevents the thermal ellipsoids of 
all adjacent C and N atoms from adopting different 
orientations, and the DFIX restraint makes all the CCC 
and CCN distances approximately equal. 
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)+(0.0639P)²+14.3698P] 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         4152
_refine_ls_number_parameters     203
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1032
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.151
_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
Ho1 Ho 0.33694(4) 0.675728(15) 0.53572(2) 0.02410(12) Uani 1 1 d . . .
As1 As 0.65524(8) 0.68344(3) 0.47392(6) 0.02280(16) Uani 1 1 d . . .
S1 S 0.3628(2) 0.70978(9) 0.35687(14) 0.0265(3) Uani 1 1 d . . .
S2 S 0.7226(13) 0.6563(12) 0.6460(11) 0.048(3) Uani 0.68(5) 1 d P . .
S2' S 0.683(3) 0.6245(17) 0.6159(18) 0.036(5) Uani 0.32(5) 1 d P . .
S3 S 0.8123(3) 0.77386(11) 0.5104(3) 0.0668(8) Uani 1 1 d . . .
S4 S 0.7037(3) 0.60475(10) 0.3922(2) 0.0465(5) Uani 1 1 d . . .
N1 N 0.3250(13) 0.5535(4) 0.4859(7) 0.072(2) Uani 1 1 d DU . .
H1A H 0.4387 0.5396 0.5161 0.086 Uiso 1 1 d R . .
H1B H 0.2902 0.5288 0.5220 0.086 Uiso 1 1 d R . .
N2 N 0.0238(9) 0.6436(3) 0.3409(6) 0.0362(11) Uani 1 1 d DU . .
H2A H -0.0628 0.6518 0.3491 0.043 Uiso 1 1 d R . .
H2B H -0.0011 0.6702 0.2804 0.043 Uiso 1 1 d R . .
N3 N 0.1533(9) 0.6554(3) 0.6063(6) 0.0394(12) Uani 1 1 d DU . .
H3A H 0.1436 0.6952 0.6339 0.047 Uiso 1 1 d R . .
H3B H 0.0386 0.6424 0.5424 0.047 Uiso 1 1 d R . .
N4 N 0.5203(9) 0.6254(4) 0.7437(6) 0.0484(14) Uani 1 1 d DU . .
H4A H 0.5749 0.5872 0.7442 0.058 Uiso 1 1 d R . .
H4B H 0.6110 0.6553 0.7948 0.058 Uiso 1 1 d R . .
N5 N 0.5039(12) 0.7827(4) 0.6344(8) 0.070(2) Uani 1 1 d U . .
H5A H 0.5399 0.7838 0.7100 0.084 Uiso 1 1 d R . .
H5B H 0.6063 0.7830 0.6408 0.084 Uiso 1 1 d R . .
N6 N 0.1230(9) 0.7765(3) 0.4571(6) 0.0382(13) Uani 1 1 d U . .
H6A H 0.0844 0.7873 0.3827 0.046 Uiso 1 1 d R . .
H6B H 0.0231 0.7647 0.4498 0.046 Uiso 1 1 d R . .
C1 C -0.1515(17) 0.5585(6) 0.1799(9) 0.085(3) Uani 1 1 d DU . .
H1C H -0.2593 0.5544 0.1743 0.128 Uiso 1 1 calc R . .
H1D H -0.1342 0.5168 0.1522 0.128 Uiso 1 1 calc R . .
H1E H -0.1671 0.5960 0.1304 0.128 Uiso 1 1 calc R . .
C2 C 0.0127(12) 0.5712(4) 0.3082(9) 0.068(2) Uani 1 1 d DU . .
H2C H -0.0191 0.5479 0.3540 0.082 Uiso 1 1 calc R . .
C3 C 0.1959(15) 0.5399(7) 0.3582(9) 0.099(4) Uani 1 1 d DU . .
H3C H 0.1824 0.4909 0.3440 0.119 Uiso 1 1 calc R . .
H3D H 0.2403 0.5594 0.3179 0.119 Uiso 1 1 calc R . .
C4 C 0.5177(15) 0.5488(5) 0.8830(9) 0.063(2) Uani 1 1 d DU . .
H4C H 0.6424 0.5597 0.9517 0.094 Uiso 1 1 calc R . .
H4D H 0.5167 0.5090 0.8429 0.094 Uiso 1 1 calc R . .
H4E H 0.4470 0.5399 0.9097 0.094 Uiso 1 1 calc R . .
C5 C 0.4342(10) 0.6084(5) 0.7963(7) 0.0551(18) Uani 1 1 d DU . .
H5C H 0.4551 0.6482 0.8456 0.066 Uiso 1 1 calc R . .
C6 C 0.2302(10) 0.6043(5) 0.7001(7) 0.0557(18) Uani 1 1 d DU . .
H6C H 0.1991 0.5593 0.6629 0.067 Uiso 1 1 calc R . .
H6D H 0.1728 0.6088 0.7378 0.067 Uiso 1 1 calc R . .
C7 C 0.0898(14) 0.9015(4) 0.4772(9) 0.060(2) Uani 1 1 d U . .
H7A H -0.0281 0.8920 0.4564 0.090 Uiso 1 1 calc R . .
H7B H 0.0737 0.9123 0.4050 0.090 Uiso 1 1 calc R . .
H7C H 0.1456 0.9397 0.5319 0.090 Uiso 1 1 calc R . .
C8 C 0.2146(12) 0.8385(4) 0.5384(8) 0.0459(17) Uani 1 1 d U . .
H8A H 0.2328 0.8294 0.6132 0.055 Uiso 1 1 calc R . .
C9 C 0.3999(13) 0.8448(5) 0.5699(10) 0.057(2) Uani 1 1 d U . .
H9A H 0.3868 0.8499 0.4968 0.068 Uiso 1 1 calc R . .
H9B H 0.4640 0.8847 0.6207 0.068 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
Ho1 N5 2.450(8) . ?
Ho1 N1 2.471(8) . ?
Ho1 N4 2.500(6) . ?
Ho1 N3 2.499(6) . ?
Ho1 N6 2.508(6) . ?
Ho1 N2 2.531(6) . ?
Ho1 S1 2.7761(15) . ?
Ho1 S2' 2.847(8) . ?
Ho1 S2 2.906(5) . ?
As1 S4 2.1368(19) . ?
As1 S3 2.139(2) . ?
As1 S2 2.169(5) . ?
As1 S1 2.1816(15) . ?
As1 S2' 2.187(11) . ?
S2 S2' 0.710(14) . ?
N1 C3 1.434(9) . ?
N1 H1A 0.8998 . ?
N1 H1B 0.8992 . ?
N2 C2 1.470(7) . ?
N2 H2A 0.8995 . ?
N2 H2B 0.8996 . ?
N3 C6 1.442(7) . ?
N3 H3A 0.8994 . ?
N3 H3B 0.8997 . ?
N4 C5 1.437(7) . ?
N4 H4A 0.9003 . ?
N4 H4B 0.9001 . ?
N5 C9 1.458(13) . ?
N5 H5A 0.9002 . ?
N5 H5B 0.9003 . ?
N6 C8 1.512(9) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.8999 . ?
C1 C2 1.487(9) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 C3 1.506(9) . ?
C2 H2C 0.9800 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 C5 1.505(8) . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C5 C6 1.490(8) . ?
C5 H5C 0.9800 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.533(12) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.493(13) . ?
C8 H8A 0.9800 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

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
N5 Ho1 N1 152.2(3) . . ?
N5 Ho1 N4 86.8(3) . . ?
N1 Ho1 N4 80.4(3) . . ?
N5 Ho1 N3 104.8(3) . . ?
N1 Ho1 N3 92.4(3) . . ?
N4 Ho1 N3 66.2(2) . . ?
N5 Ho1 N6 68.1(2) . . ?
N1 Ho1 N6 138.6(2) . . ?
N4 Ho1 N6 126.5(2) . . ?
N3 Ho1 N6 75.5(2) . . ?
N5 Ho1 N2 135.8(2) . . ?
N1 Ho1 N2 68.6(2) . . ?
N4 Ho1 N2 130.9(2) . . ?
N3 Ho1 N2 77.7(2) . . ?
N6 Ho1 N2 70.13(19) . . ?
N5 Ho1 S1 85.9(3) . . ?
N1 Ho1 S1 89.1(2) . . ?
N4 Ho1 S1 141.70(14) . . ?
N3 Ho1 S1 151.54(15) . . ?
N6 Ho1 S1 84.70(16) . . ?
N2 Ho1 S1 76.40(14) . . ?
N5 Ho1 S2' 85.3(8) . . ?
N1 Ho1 S2' 67.1(8) . . ?
N4 Ho1 S2' 68.2(2) . . ?
N3 Ho1 S2' 132.5(3) . . ?
N6 Ho1 S2' 146.9(6) . . ?
N2 Ho1 S2' 126.1(7) . . ?
S1 Ho1 S2' 73.76(16) . . ?
N5 Ho1 S2 71.2(5) . . ?
N1 Ho1 S2 81.1(6) . . ?
N4 Ho1 S2 67.48(16) . . ?
N3 Ho1 S2 133.71(16) . . ?
N6 Ho1 S2 135.3(5) . . ?
N2 Ho1 S2 137.9(4) . . ?
S1 Ho1 S2 74.58(10) . . ?
S2' Ho1 S2 14.1(3) . . ?
S4 As1 S3 112.22(10) . . ?
S4 As1 S2 115.1(6) . . ?
S3 As1 S2 105.0(6) . . ?
S4 As1 S1 110.24(7) . . ?
S3 As1 S1 109.11(8) . . ?
S2 As1 S1 104.66(12) . . ?
S4 As1 S2' 100.2(8) . . ?
S3 As1 S2' 122.9(10) . . ?
S2 As1 S2' 18.7(3) . . ?
S1 As1 S2' 101.2(4) . . ?
As1 S1 Ho1 91.90(5) . . ?
S2' S2 As1 82.0(11) . . ?
S2' S2 Ho1 78.2(9) . . ?
As1 S2 Ho1 88.7(2) . . ?
S2 S2' As1 79.2(14) . . ?
S2 S2' Ho1 87.7(9) . . ?
As1 S2' Ho1 89.9(3) . . ?
C3 N1 Ho1 113.0(6) . . ?
C3 N1 H1A 110.3 . . ?
Ho1 N1 H1A 109.1 . . ?
C3 N1 H1B 107.6 . . ?
Ho1 N1 H1B 108.8 . . ?
H1A N1 H1B 107.8 . . ?
C2 N2 Ho1 112.7(5) . . ?
C2 N2 H2A 108.7 . . ?
Ho1 N2 H2A 109.1 . . ?
C2 N2 H2B 109.2 . . ?
Ho1 N2 H2B 109.1 . . ?
H2A N2 H2B 107.8 . . ?
C6 N3 Ho1 114.3(5) . . ?
C6 N3 H3A 108.9 . . ?
Ho1 N3 H3A 108.5 . . ?
C6 N3 H3B 108.7 . . ?
Ho1 N3 H3B 108.7 . . ?
H3A N3 H3B 107.6 . . ?
C5 N4 Ho1 120.9(5) . . ?
C5 N4 H4A 107.6 . . ?
Ho1 N4 H4A 107.4 . . ?
C5 N4 H4B 106.3 . . ?
Ho1 N4 H4B 107.1 . . ?
H4A N4 H4B 106.9 . . ?
C9 N5 Ho1 114.6(6) . . ?
C9 N5 H5A 109.3 . . ?
Ho1 N5 H5A 109.1 . . ?
C9 N5 H5B 107.7 . . ?
Ho1 N5 H5B 108.3 . . ?
H5A N5 H5B 107.6 . . ?
C8 N6 Ho1 112.3(5) . . ?
C8 N6 H6A 108.9 . . ?
Ho1 N6 H6A 109.0 . . ?
C8 N6 H6B 109.9 . . ?
Ho1 N6 H6B 109.1 . . ?
H6A N6 H6B 107.7 . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N2 C2 C1 111.1(8) . . ?
N2 C2 C3 114.0(8) . . ?
C1 C2 C3 119.9(9) . . ?
N2 C2 H2C 103.1 . . ?
C1 C2 H2C 103.1 . . ?
C3 C2 H2C 103.1 . . ?
N1 C3 C2 108.8(9) . . ?
N1 C3 H3C 109.9 . . ?
C2 C3 H3C 109.9 . . ?
N1 C3 H3D 109.9 . . ?
C2 C3 H3D 109.9 . . ?
H3C C3 H3D 108.3 . . ?
C5 C4 H4C 109.5 . . ?
C5 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
C5 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
N4 C5 C6 110.1(6) . . ?
N4 C5 C4 115.7(7) . . ?
C6 C5 C4 114.4(7) . . ?
N4 C5 H5C 105.2 . . ?
C6 C5 H5C 105.2 . . ?
C4 C5 H5C 105.2 . . ?
N3 C6 C5 114.6(6) . . ?
N3 C6 H6C 108.6 . . ?
C5 C6 H6C 108.6 . . ?
N3 C6 H6D 108.6 . . ?
C5 C6 H6D 108.6 . . ?
H6C C6 H6D 107.6 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N6 106.6(7) . . ?
C9 C8 C7 115.3(8) . . ?
N6 C8 C7 110.3(7) . . ?
C9 C8 H8A 108.1 . . ?
N6 C8 H8A 108.1 . . ?
C7 C8 H8A 108.1 . . ?
N5 C9 C8 107.9(8) . . ?
N5 C9 H9A 110.1 . . ?
C8 C9 H9A 110.1 . . ?
N5 C9 H9B 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.248
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.273
####################################################################### 
# 
# 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_IId
_database_code_depnum_ccdc_archive 'CCDC 1403238'
_audit_update_record             
;
2015-08-03 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H24 As Er N6 S4'
_chemical_formula_sum            'C9 H24 As Er N6 S4'
_chemical_formula_weight         586.76

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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.2966(8)
_cell_length_b                   19.4847(16)
_cell_length_c                   14.1712(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.834(4)
_cell_angle_gamma                90.00
_cell_volume                     1999.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    16420
_cell_measurement_theta_min      2.09
_cell_measurement_theta_max      26.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    6.258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4967
_exptl_absorpt_correction_T_max  0.5460
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16419
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4098
_reflns_number_gt                3614
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The DELU restraint prevents the thermal ellipsoids of 
all adjacent C and N atoms from adopting different 
orientations, and the DFIX restraint makes all the CCC 
and CCN distances approximately equal. 
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)+(0.0488P)²+15.0356P] 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         4098
_refine_ls_number_parameters     203
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.072
_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 0.16292(4) 0.324026(15) 0.46348(3) 0.02486(11) Uani 1 1 d . . .
As1 As -0.15543(8) 0.31627(3) 0.52561(6) 0.02370(16) Uani 1 1 d . . .
S1 S 0.1370(2) 0.29021(9) 0.64176(14) 0.0280(3) Uani 1 1 d . . .
S2 S -0.183(3) 0.3755(18) 0.3839(19) 0.033(5) Uani 0.29(4) 1 d P . .
S2' S -0.2233(12) 0.3428(11) 0.3533(10) 0.047(3) Uani 0.71(4) 1 d P . .
S3 S -0.3114(3) 0.22564(11) 0.4916(3) 0.0642(8) Uani 1 1 d . . .
S4 S -0.2040(3) 0.39581(10) 0.6062(2) 0.0464(5) Uani 1 1 d . . .
N1 N -0.0045(11) 0.2178(4) 0.3623(8) 0.074(2) Uani 1 1 d U . .
H1C H -0.1161 0.2171 0.2957 0.088 Uiso 1 1 d R . .
N2 N 0.3753(8) 0.2234(3) 0.5431(6) 0.0384(13) Uani 1 1 d U . .
H2B H 0.4866 0.2242 0.6099 0.046 Uiso 1 1 d R . .
N3 N -0.0187(9) 0.3746(4) 0.2568(6) 0.0493(14) Uani 1 1 d U . .
H3D H -0.1359 0.3803 0.2144 0.059 Uiso 1 1 d R . .
N4 N 0.3450(9) 0.3442(3) 0.3933(6) 0.0391(12) Uani 1 1 d U . .
H4D H 0.4472 0.3234 0.4237 0.047 Uiso 1 1 d R . .
N5 N 0.1720(13) 0.4464(4) 0.5129(8) 0.072(2) Uani 1 1 d U . .
H5B H 0.1030 0.4774 0.4596 0.086 Uiso 1 1 d R . .
N6 N 0.4732(8) 0.3561(3) 0.6567(6) 0.0355(12) Uani 1 1 d U . .
H6C H 0.5637 0.3276 0.6984 0.043 Uiso 1 1 d R . .
C1 C 0.1009(13) 0.1549(5) 0.4279(9) 0.059(2) Uani 1 1 d U . .
H1A H 0.0385 0.1150 0.3765 0.071 Uiso 1 1 calc R . .
H1B H 0.1109 0.1492 0.4998 0.071 Uiso 1 1 calc R . .
C2 C 0.2886(12) 0.1617(4) 0.4625(9) 0.0499(19) Uani 1 1 d U . .
H2A H 0.2736 0.1711 0.3888 0.060 Uiso 1 1 calc R . .
C3 C 0.4077(14) 0.0979(4) 0.5218(10) 0.061(2) Uani 1 1 d U . .
H3A H 0.5265 0.1061 0.5428 0.091 Uiso 1 1 calc R . .
H3B H 0.3492 0.0600 0.4664 0.091 Uiso 1 1 calc R . .
H3C H 0.4228 0.0873 0.5937 0.091 Uiso 1 1 calc R . .
C4 C -0.0149(14) 0.4509(5) 0.1177(9) 0.062(2) Uani 1 1 d DU . .
H4A H 0.0741 0.4682 0.1101 0.093 Uiso 1 1 calc R . .
H4B H -0.0505 0.4869 0.1455 0.093 Uiso 1 1 calc R . .
H4C H -0.1217 0.4347 0.0403 0.093 Uiso 1 1 calc R . .
C5 C 0.0683(10) 0.3929(5) 0.2068(8) 0.0558(18) Uani 1 1 d DU . .
H5A H 0.0460 0.3530 0.1572 0.067 Uiso 1 1 calc R . .
C6 C 0.2701(10) 0.3938(5) 0.2998(8) 0.0570(19) Uani 1 1 d DU . .
H6A H 0.3244 0.3869 0.2603 0.068 Uiso 1 1 calc R . .
H6B H 0.3071 0.4390 0.3366 0.068 Uiso 1 1 calc R . .
C7 C 0.2998(15) 0.4602(6) 0.6350(12) 0.096(4) Uani 1 1 d DU . .
H7A H 0.2559 0.4419 0.6764 0.116 Uiso 1 1 calc R . .
H7B H 0.3123 0.5095 0.6471 0.116 Uiso 1 1 calc R . .
C8 C 0.4846(11) 0.4300(5) 0.6892(8) 0.063(2) Uani 1 1 d DU . .
H8A H 0.5190 0.4528 0.6442 0.076 Uiso 1 1 calc R . .
C9 C 0.6465(16) 0.4427(6) 0.8172(8) 0.079(3) Uani 1 1 d DU . .
H9A H 0.6594 0.4912 0.8330 0.119 Uiso 1 1 calc R . .
H9B H 0.7558 0.4254 0.8322 0.119 Uiso 1 1 calc R . .
H9C H 0.6291 0.4199 0.8694 0.119 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 N1 2.442(8) . ?
Er1 N5 2.471(8) . ?
Er1 N4 2.475(6) . ?
Er1 N3 2.490(7) . ?
Er1 N2 2.494(6) . ?
Er1 N6 2.511(6) . ?
Er1 S1 2.7639(15) . ?
Er1 S2 2.838(8) . ?
Er1 S2' 2.904(5) . ?
As1 S4 2.135(2) . ?
As1 S3 2.139(2) . ?
As1 S2' 2.166(5) . ?
As1 S1 2.1784(16) . ?
As1 S2 2.188(12) . ?
S2 S2' 0.728(19) . ?
N1 C1 1.478(13) . ?
N1 H1C 0.8598 . ?
N2 C2 1.500(10) . ?
N2 H2B 0.8594 . ?
N3 C5 1.415(10) . ?
N3 H3D 0.8599 . ?
N4 C6 1.420(9) . ?
N4 H4D 0.8598 . ?
N5 C7 1.378(15) . ?
N5 H5B 0.8598 . ?
N6 C8 1.494(10) . ?
N6 H6C 0.8613 . ?
C1 C2 1.494(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.520(12) . ?
C2 H2A 0.9800 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.498(8) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.469(8) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.495(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.481(8) . ?
C8 H8A 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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
N1 Er1 N5 151.6(3) . . ?
N1 Er1 N4 104.1(3) . . ?
N5 Er1 N4 92.9(3) . . ?
N1 Er1 N3 86.1(3) . . ?
N5 Er1 N3 80.2(3) . . ?
N4 Er1 N3 66.1(2) . . ?
N1 Er1 N2 68.4(2) . . ?
N5 Er1 N2 138.9(2) . . ?
N4 Er1 N2 76.1(2) . . ?
N3 Er1 N2 127.1(2) . . ?
N1 Er1 N6 136.5(2) . . ?
N5 Er1 N6 68.8(2) . . ?
N4 Er1 N6 77.9(2) . . ?
N3 Er1 N6 130.7(2) . . ?
N2 Er1 N6 70.14(19) . . ?
N1 Er1 S1 86.9(3) . . ?
N5 Er1 S1 88.7(2) . . ?
N4 Er1 S1 151.55(15) . . ?
N3 Er1 S1 141.83(15) . . ?
N2 Er1 S1 84.09(16) . . ?
N6 Er1 S1 76.21(14) . . ?
N1 Er1 S2 85.4(9) . . ?
N5 Er1 S2 66.5(9) . . ?
N4 Er1 S2 132.3(3) . . ?
N3 Er1 S2 68.2(2) . . ?
N2 Er1 S2 146.6(7) . . ?
N6 Er1 S2 125.8(7) . . ?
S1 Er1 S2 73.83(18) . . ?
N1 Er1 S2' 70.9(5) . . ?
N5 Er1 S2' 80.9(5) . . ?
N4 Er1 S2' 133.71(16) . . ?
N3 Er1 S2' 67.67(17) . . ?
N2 Er1 S2' 134.7(4) . . ?
N6 Er1 S2' 137.9(4) . . ?
S1 Er1 S2' 74.58(9) . . ?
S2 Er1 S2' 14.5(4) . . ?
S4 As1 S3 112.27(9) . . ?
S4 As1 S2' 114.8(5) . . ?
S3 As1 S2' 105.4(6) . . ?
S4 As1 S1 110.33(8) . . ?
S3 As1 S1 109.04(8) . . ?
S2' As1 S1 104.52(12) . . ?
S4 As1 S2 99.6(8) . . ?
S3 As1 S2 123.8(10) . . ?
S2' As1 S2 19.2(5) . . ?
S1 As1 S2 100.8(4) . . ?
As1 S1 Er1 92.10(6) . . ?
S2' S2 As1 78.6(14) . . ?
S2' S2 Er1 87.9(10) . . ?
As1 S2 Er1 89.9(3) . . ?
S2 S2' As1 82.1(11) . . ?
S2 S2' Er1 77.6(8) . . ?
As1 S2' Er1 88.6(2) . . ?
C1 N1 Er1 114.0(5) . . ?
C1 N1 H1C 123.0 . . ?
Er1 N1 H1C 122.9 . . ?
C2 N2 Er1 113.1(5) . . ?
C2 N2 H2B 123.7 . . ?
Er1 N2 H2B 123.3 . . ?
C5 N3 Er1 120.7(5) . . ?
C5 N3 H3D 119.3 . . ?
Er1 N3 H3D 120.0 . . ?
C6 N4 Er1 115.1(5) . . ?
C6 N4 H4D 122.0 . . ?
Er1 N4 H4D 122.9 . . ?
C7 N5 Er1 113.2(6) . . ?
C7 N5 H5B 123.1 . . ?
Er1 N5 H5B 123.7 . . ?
C8 N6 Er1 112.8(4) . . ?
C8 N6 H6C 124.0 . . ?
Er1 N6 H6C 123.2 . . ?
N1 C1 C2 108.1(8) . . ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
C1 C2 N2 106.2(7) . . ?
C1 C2 C3 113.9(8) . . ?
N2 C2 C3 112.2(7) . . ?
C1 C2 H2A 108.1 . . ?
N2 C2 H2A 108.1 . . ?
C3 C2 H2A 108.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 C6 111.3(7) . . ?
N3 C5 C4 117.3(7) . . ?
C6 C5 C4 116.2(8) . . ?
N3 C5 H5A 103.2 . . ?
C6 C5 H5A 103.2 . . ?
C4 C5 H5A 103.2 . . ?
N4 C6 C5 115.6(7) . . ?
N4 C6 H6A 108.4 . . ?
C5 C6 H6A 108.4 . . ?
N4 C6 H6B 108.4 . . ?
C5 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
N5 C7 C8 112.1(10) . . ?
N5 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N5 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 N6 111.1(8) . . ?
C9 C8 C7 121.4(9) . . ?
N6 C8 C7 112.6(8) . . ?
C9 C8 H8A 103.0 . . ?
N6 C8 H8A 103.0 . . ?
C7 C8 H8A 103.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.844
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.183
####################################################################### 
# 
# 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_III
_database_code_depnum_ccdc_archive 'CCDC 1403239'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As Er N6 S4'
_chemical_formula_sum            'C8 H26 As Er N6 S4'
_chemical_formula_weight         576.77

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'
As As 0.0499 2.0058 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   8.9342(8)
_cell_length_b                   15.4964(14)
_cell_length_c                   25.966(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3594.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    6775
_cell_measurement_theta_min      2.6287
_cell_measurement_theta_max      28.4198

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2248
_exptl_absorpt_coefficient_mu    6.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4890
_exptl_absorpt_correction_T_max  0.6061
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14423
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3180
_reflns_number_gt                2803
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
The DFIX 
restraint makes all the CCC and CCN distances approximately equal. 
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)+(0.0311P)²+10.8298P] 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         3180
_refine_ls_number_parameters     181
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.095
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.59527(2) 0.255675(11) 0.373873(6) 0.00860(9) Uani 1 1 d . . .
As1 As 0.98352(5) 0.25043(2) 0.383075(17) 0.01011(12) Uani 1 1 d . . .
S1 S 0.83276(11) 0.33883(6) 0.42270(4) 0.0122(2) Uani 1 1 d . . .
S2 S 0.84148(11) 0.15616(6) 0.34383(4) 0.0120(2) Uani 1 1 d . . .
S3 S 1.10738(12) 0.31945(7) 0.32449(4) 0.0182(2) Uani 1 1 d . . .
S4 S 1.12177(12) 0.18662(7) 0.43910(4) 0.0154(2) Uani 1 1 d . . .
N1 N 0.7178(4) 0.3436(2) 0.30314(13) 0.0136(7) Uani 1 1 d . . .
H1A H 0.8178 0.3416 0.3073 0.016 Uiso 1 1 calc R . .
H1B H 0.6964 0.3193 0.2725 0.016 Uiso 1 1 calc R . .
N2 N 0.4535(4) 0.3915(2) 0.35412(14) 0.0122(7) Uani 1 1 d . . .
H2C H 0.3562 0.3760 0.3494 0.015 Uiso 1 1 calc R . .
N3 N 0.4400(4) 0.3086(2) 0.44648(13) 0.0129(7) Uani 1 1 d . . .
H3A H 0.3621 0.2723 0.4502 0.015 Uiso 1 1 calc R . .
H3B H 0.4951 0.3050 0.4754 0.015 Uiso 1 1 calc R . .
N4 N 0.6576(4) 0.1655(2) 0.45292(14) 0.0137(7) Uani 1 1 d . . .
H4A H 0.7538 0.1486 0.4505 0.016 Uiso 1 1 calc R . .
H4B H 0.6503 0.1996 0.4808 0.016 Uiso 1 1 calc R . .
N5 N 0.4368(5) 0.1205(2) 0.38149(13) 0.0166(8) Uani 1 1 d . . .
H5C H 0.3571 0.1362 0.4012 0.020 Uiso 1 1 calc R . .
N6 N 0.4611(5) 0.2162(2) 0.29233(15) 0.0235(9) Uani 1 1 d . . .
H6A H 0.3683 0.2388 0.2926 0.028 Uiso 1 1 calc R . .
H6B H 0.5106 0.2377 0.2650 0.028 Uiso 1 1 calc R . .
C1 C 0.6698(5) 0.4344(3) 0.30220(16) 0.0142(9) Uani 1 1 d . . .
H1C H 0.7013 0.4614 0.2703 0.017 Uiso 1 1 calc R . .
H1D H 0.7151 0.4656 0.3306 0.017 Uiso 1 1 calc R . .
C2 C 0.5012(5) 0.4374(3) 0.30668(16) 0.0143(9) Uani 1 1 d . . .
H2A H 0.4678 0.4969 0.3080 0.017 Uiso 1 1 calc R . .
H2B H 0.4562 0.4103 0.2768 0.017 Uiso 1 1 calc R . .
C3 C 0.4580(5) 0.4468(3) 0.40064(16) 0.0150(9) Uani 1 1 d . . .
H3C H 0.4077 0.5012 0.3941 0.018 Uiso 1 1 calc R . .
H3D H 0.5608 0.4588 0.4103 0.018 Uiso 1 1 calc R . .
C4 C 0.3795(5) 0.3979(3) 0.44303(17) 0.0165(9) Uani 1 1 d . . .
H4C H 0.3942 0.4274 0.4756 0.020 Uiso 1 1 calc R . .
H4D H 0.2729 0.3958 0.4360 0.020 Uiso 1 1 calc R . .
C5 C 0.5651(5) 0.0883(3) 0.46179(17) 0.0197(10) Uani 1 1 d . . .
H5A H 0.4791 0.1034 0.4827 0.024 Uiso 1 1 calc R . .
H5B H 0.6230 0.0452 0.4802 0.024 Uiso 1 1 calc R . .
C6 C 0.5134(5) 0.0519(3) 0.41133(18) 0.0197(10) Uani 1 1 d . . .
H6C H 0.5985 0.0304 0.3921 0.024 Uiso 1 1 calc R . .
H6D H 0.4452 0.0043 0.4173 0.024 Uiso 1 1 calc R . .
C7 C 0.3711(7) 0.0879(3) 0.33311(18) 0.0374(15) Uani 1 1 d D . .
H7A H 0.3739 0.0254 0.3331 0.045 Uiso 1 1 calc R . .
H7B H 0.2672 0.1057 0.3310 0.045 Uiso 1 1 calc R . .
C8 C 0.4521(7) 0.1204(3) 0.2882(2) 0.0421(15) Uani 1 1 d D . .
H8A H 0.4001 0.1042 0.2569 0.051 Uiso 1 1 calc R . .
H8B H 0.5519 0.0959 0.2872 0.051 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 N3 2.480(3) . ?
Er1 N6 2.509(4) . ?
Er1 N2 2.509(3) . ?
Er1 N1 2.535(3) . ?
Er1 N5 2.536(4) . ?
Er1 N4 2.545(3) . ?
Er1 S1 2.7874(10) . ?
Er1 S2 2.7974(10) . ?
As1 S4 2.1494(11) . ?
As1 S3 2.1640(12) . ?
As1 S1 2.1793(11) . ?
As1 S2 2.1869(11) . ?
N1 C1 1.472(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.482(5) . ?
N2 C2 1.485(5) . ?
N2 H2C 0.9100 . ?
N3 C4 1.488(5) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.472(5) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.476(6) . ?
N5 C6 1.483(5) . ?
N5 H5C 0.9100 . ?
N6 C8 1.490(6) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.512(6) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.509(6) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.499(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.461(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
N3 Er1 N6 117.05(14) . . ?
N3 Er1 N2 66.16(11) . . ?
N6 Er1 N2 77.92(12) . . ?
N3 Er1 N1 127.94(11) . . ?
N6 Er1 N1 74.10(12) . . ?
N2 Er1 N1 67.63(11) . . ?
N3 Er1 N5 84.34(12) . . ?
N6 Er1 N5 66.27(12) . . ?
N2 Er1 N5 115.27(13) . . ?
N1 Er1 N5 137.84(11) . . ?
N3 Er1 N4 72.00(11) . . ?
N6 Er1 N4 130.65(11) . . ?
N2 Er1 N4 137.39(11) . . ?
N1 Er1 N4 141.69(11) . . ?
N5 Er1 N4 66.78(11) . . ?
N3 Er1 S1 85.83(8) . . ?
N6 Er1 S1 149.35(9) . . ?
N2 Er1 S1 95.13(8) . . ?
N1 Er1 S1 75.66(8) . . ?
N5 Er1 S1 140.48(8) . . ?
N4 Er1 S1 73.76(8) . . ?
N3 Er1 S2 146.52(8) . . ?
N6 Er1 S2 90.35(10) . . ?
N2 Er1 S2 143.35(8) . . ?
N1 Er1 S2 75.79(8) . . ?
N5 Er1 S2 90.31(10) . . ?
N4 Er1 S2 75.52(8) . . ?
S1 Er1 S2 77.47(3) . . ?
S4 As1 S3 114.16(5) . . ?
S4 As1 S1 108.95(4) . . ?
S3 As1 S1 109.71(4) . . ?
S4 As1 S2 109.97(4) . . ?
S3 As1 S2 107.42(4) . . ?
S1 As1 S2 106.33(4) . . ?
As1 S1 Er1 88.00(3) . . ?
As1 S2 Er1 87.60(3) . . ?
C1 N1 Er1 113.6(2) . . ?
C1 N1 H1A 108.9 . . ?
Er1 N1 H1A 108.9 . . ?
C1 N1 H1B 108.9 . . ?
Er1 N1 H1B 108.9 . . ?
H1A N1 H1B 107.7 . . ?
C3 N2 C2 113.0(3) . . ?
C3 N2 Er1 107.7(2) . . ?
C2 N2 Er1 115.3(2) . . ?
C3 N2 H2C 106.8 . . ?
C2 N2 H2C 106.8 . . ?
Er1 N2 H2C 106.8 . . ?
C4 N3 Er1 117.7(2) . . ?
C4 N3 H3A 107.9 . . ?
Er1 N3 H3A 107.9 . . ?
C4 N3 H3B 107.9 . . ?
Er1 N3 H3B 107.9 . . ?
H3A N3 H3B 107.2 . . ?
C5 N4 Er1 116.7(3) . . ?
C5 N4 H4A 108.1 . . ?
Er1 N4 H4A 108.1 . . ?
C5 N4 H4B 108.1 . . ?
Er1 N4 H4B 108.1 . . ?
H4A N4 H4B 107.3 . . ?
C7 N5 C6 112.6(4) . . ?
C7 N5 Er1 116.0(3) . . ?
C6 N5 Er1 112.0(3) . . ?
C7 N5 H5C 105.0 . . ?
C6 N5 H5C 105.0 . . ?
Er1 N5 H5C 105.0 . . ?
C8 N6 Er1 109.2(3) . . ?
C8 N6 H6A 109.8 . . ?
Er1 N6 H6A 109.8 . . ?
C8 N6 H6B 109.8 . . ?
Er1 N6 H6B 109.8 . . ?
H6A N6 H6B 108.3 . . ?
N1 C1 C2 108.6(3) . . ?
N1 C1 H1C 110.0 . . ?
C2 C1 H1C 110.0 . . ?
N1 C1 H1D 110.0 . . ?
C2 C1 H1D 110.0 . . ?
H1C C1 H1D 108.4 . . ?
N2 C2 C1 109.6(3) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 106.9(3) . . ?
N2 C3 H3C 110.3 . . ?
C4 C3 H3C 110.3 . . ?
N2 C3 H3D 110.3 . . ?
C4 C3 H3D 110.3 . . ?
H3C C3 H3D 108.6 . . ?
N3 C4 C3 110.0(3) . . ?
N3 C4 H4C 109.7 . . ?
C3 C4 H4C 109.7 . . ?
N3 C4 H4D 109.7 . . ?
C3 C4 H4D 109.7 . . ?
H4C C4 H4D 108.2 . . ?
N4 C5 C6 110.0(3) . . ?
N4 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
N4 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N5 C6 C5 109.3(4) . . ?
N5 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N5 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.3 . . ?
C8 C7 N5 111.4(4) . . ?
C8 C7 H7A 109.4 . . ?
N5 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
N5 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 N6 108.2(4) . . ?
C7 C8 H8A 110.1 . . ?
N6 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
N6 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.036
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.162
