# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033469'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 As Ce N4 S3'
_chemical_formula_sum            'C6 H18 As Ce N4 S3'
_chemical_formula_weight         457.46

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'
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'
As As 0.0499 2.0058 '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           Orthorhombic
_symmetry_space_group_name_H-M   'A b a 2'
_symmetry_space_group_name_Hall  'A 2 -2ac '

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

_cell_length_a                   19.7580(5)
_cell_length_b                   9.6623(2)
_cell_length_c                   14.9521(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2854.47(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    5.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5627
_exptl_absorpt_correction_T_max  0.6826
_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            3387
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         25.08
_reflns_number_total             2265
_reflns_number_gt                2159
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0241P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         2265
_refine_ls_number_parameters     136
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_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 0.684843(16) 0.59194(3) 0.49147(3) 0.02219(11) Uani 1 1 d . . .
S1 S 0.57778(8) 0.39335(17) 0.4921(3) 0.0384(4) Uani 1 1 d . . .
S2 S 0.74617(9) 0.34018(17) 0.41560(12) 0.0293(4) Uani 1 1 d . . .
S3 S 0.68605(10) 0.1380(2) 0.58476(12) 0.0333(5) Uani 1 1 d . . .
As1 As 0.64888(4) 0.22442(7) 0.45615(5) 0.02884(18) Uani 1 1 d . . .
N1 N 0.6748(4) 0.4902(7) 0.6572(4) 0.0479(19) Uani 1 1 d . . .
H1A H 0.6589 0.4029 0.6546 0.058 Uiso 1 1 calc R . .
H1B H 0.7162 0.4876 0.6824 0.058 Uiso 1 1 calc R . .
N2 N 0.6380(3) 0.7739(6) 0.6120(4) 0.0342(15) Uani 1 1 d . . .
H2C H 0.6644 0.8508 0.6068 0.041 Uiso 1 1 calc R . .
N3 N 0.5760(3) 0.7310(6) 0.4403(4) 0.0297(14) Uani 1 1 d . . .
H3C H 0.5413 0.6717 0.4514 0.036 Uiso 1 1 calc R . .
N4 N 0.6552(4) 0.5876(6) 0.3161(4) 0.0400(17) Uani 1 1 d . . .
H4C H 0.6847 0.6426 0.2871 0.048 Uiso 1 1 calc R . .
H4D H 0.6611 0.5008 0.2955 0.048 Uiso 1 1 calc R . .
C1 C 0.6297(7) 0.5739(8) 0.7129(6) 0.061(3) Uani 1 1 d . . .
H1C H 0.6347 0.5463 0.7750 0.073 Uiso 1 1 calc R . .
H1D H 0.5832 0.5572 0.6954 0.073 Uiso 1 1 calc R . .
C2 C 0.6453(5) 0.7262(8) 0.7041(6) 0.052(3) Uani 1 1 d . . .
H2A H 0.6149 0.7784 0.7422 0.062 Uiso 1 1 calc R . .
H2B H 0.6912 0.7433 0.7241 0.062 Uiso 1 1 calc R . .
C3 C 0.5680(4) 0.8185(9) 0.5929(6) 0.045(2) Uani 1 1 d . . .
H3A H 0.5570 0.8992 0.6287 0.054 Uiso 1 1 calc R . .
H3B H 0.5367 0.7450 0.6087 0.054 Uiso 1 1 calc R . .
C4 C 0.5608(4) 0.8523(7) 0.4967(7) 0.0464(19) Uani 1 1 d . . .
H4A H 0.5149 0.8831 0.4850 0.056 Uiso 1 1 calc R . .
H4B H 0.5913 0.9273 0.4815 0.056 Uiso 1 1 calc R . .
C5 C 0.5703(5) 0.7602(10) 0.3445(6) 0.051(2) Uani 1 1 d . . .
H5A H 0.6014 0.8335 0.3280 0.062 Uiso 1 1 calc R . .
H5B H 0.5247 0.7903 0.3305 0.062 Uiso 1 1 calc R . .
C6 C 0.5865(4) 0.6322(10) 0.2942(6) 0.047(2) Uani 1 1 d . . .
H6A H 0.5546 0.5598 0.3097 0.057 Uiso 1 1 calc R . .
H6B H 0.5830 0.6496 0.2305 0.057 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
Ce1 N3 2.648(6) . ?
Ce1 N1 2.674(6) . ?
Ce1 N2 2.682(6) . ?
Ce1 N4 2.688(7) . ?
Ce1 S1 2.8560(16) . ?
Ce1 S3 2.9413(19) 4_655 ?
Ce1 S2 2.9449(17) . ?
Ce1 S2 2.9830(18) 4_655 ?
S1 As1 2.219(2) . ?
S2 As1 2.305(2) . ?
S2 Ce1 2.9830(18) 4_645 ?
S3 As1 2.221(2) . ?
S3 Ce1 2.9413(19) 4_645 ?
N1 C1 1.463(12) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.460(10) . ?
N2 C3 1.478(10) . ?
N2 H2C 0.9100 . ?
N3 C5 1.463(11) . ?
N3 C4 1.475(10) . ?
N3 H3C 0.9100 . ?
N4 C6 1.460(10) . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
C1 C2 1.509(11) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.482(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.483(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 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 Ce1 N1 113.2(2) . . ?
N3 Ce1 N2 65.26(19) . . ?
N1 Ce1 N2 65.98(19) . . ?
N3 Ce1 N4 63.2(2) . . ?
N1 Ce1 N4 152.0(2) . . ?
N2 Ce1 N4 126.20(19) . . ?
N3 Ce1 S1 74.97(13) . . ?
N1 Ce1 S1 72.25(17) . . ?
N2 Ce1 S1 100.55(15) . . ?
N4 Ce1 S1 80.26(16) . . ?
N3 Ce1 S3 139.84(14) . 4_655 ?
N1 Ce1 S3 71.36(17) . 4_655 ?
N2 Ce1 S3 83.18(15) . 4_655 ?
N4 Ce1 S3 130.87(16) . 4_655 ?
S1 Ce1 S3 137.95(7) . 4_655 ?
N3 Ce1 S2 129.93(14) . . ?
N1 Ce1 S2 94.81(16) . . ?
N2 Ce1 S2 160.43(14) . . ?
N4 Ce1 S2 72.60(14) . . ?
S1 Ce1 S2 75.58(6) . . ?
S3 Ce1 S2 87.19(5) 4_655 . ?
N3 Ce1 S2 81.55(14) . 4_655 ?
N1 Ce1 S2 133.01(15) . 4_655 ?
N2 Ce1 S2 83.44(13) . 4_655 ?
N4 Ce1 S2 75.00(14) . 4_655 ?
S1 Ce1 S2 151.63(7) . 4_655 ?
S3 Ce1 S2 70.26(5) 4_655 4_655 ?
S2 Ce1 S2 109.25(4) . 4_655 ?
As1 S1 Ce1 91.41(6) . . ?
As1 S2 Ce1 87.50(6) . . ?
As1 S2 Ce1 83.73(5) . 4_645 ?
Ce1 S2 Ce1 134.89(7) . 4_645 ?
As1 S3 Ce1 86.16(6) . 4_645 ?
S1 As1 S3 106.03(11) . . ?
S1 As1 S2 103.57(7) . . ?
S3 As1 S2 97.73(8) . . ?
C1 N1 Ce1 111.7(5) . . ?
C1 N1 H1A 109.3 . . ?
Ce1 N1 H1A 109.3 . . ?
C1 N1 H1B 109.3 . . ?
Ce1 N1 H1B 109.3 . . ?
H1A N1 H1B 107.9 . . ?
C2 N2 C3 111.5(7) . . ?
C2 N2 Ce1 113.1(5) . . ?
C3 N2 Ce1 112.6(4) . . ?
C2 N2 H2C 106.4 . . ?
C3 N2 H2C 106.4 . . ?
Ce1 N2 H2C 106.4 . . ?
C5 N3 C4 113.0(7) . . ?
C5 N3 Ce1 116.3(5) . . ?
C4 N3 Ce1 113.8(5) . . ?
C5 N3 H3C 103.9 . . ?
C4 N3 H3C 103.9 . . ?
Ce1 N3 H3C 103.9 . . ?
C6 N4 Ce1 114.6(5) . . ?
C6 N4 H4C 108.6 . . ?
Ce1 N4 H4C 108.6 . . ?
C6 N4 H4D 108.6 . . ?
Ce1 N4 H4D 108.6 . . ?
H4C N4 H4D 107.6 . . ?
N1 C1 C2 111.4(8) . . ?
N1 C1 H1C 109.3 . . ?
C2 C1 H1C 109.3 . . ?
N1 C1 H1D 109.3 . . ?
C2 C1 H1D 109.3 . . ?
H1C C1 H1D 108.0 . . ?
N2 C2 C1 111.8(7) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 C4 110.0(7) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 111.1(6) . . ?
N3 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 C6 108.6(6) . . ?
N3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.3 . . ?
N4 C6 C5 109.5(7) . . ?
N4 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N4 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.08
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.117
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033470'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 As N4 Pr S3'
_chemical_formula_sum            'C6 H18 As N4 Pr S3'
_chemical_formula_weight         458.25

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'
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'
As As 0.0499 2.0058 '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           Orthorhombic
_symmetry_space_group_name_H-M   'A b a 2'
_symmetry_space_group_name_Hall  'A 2 -2ac '

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

_cell_length_a                   19.7203(5)
_cell_length_b                   9.6404(2)
_cell_length_c                   14.9599(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2844.05(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.1411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1776
_exptl_absorpt_coefficient_mu    6.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2721
_exptl_absorpt_correction_T_max  0.4005
_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            3365
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         25.10
_reflns_number_total             1647
_reflns_number_gt                1533
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0183P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.00153(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1647
_refine_ls_number_parameters     137
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0596
_refine_ls_wR_factor_gt          0.0570
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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
Pr1 Pr 0.31530(2) 0.09233(4) 0.84311(4) 0.02412(16) Uani 1 1 d . . .
As1 As 0.35069(5) -0.27539(8) 0.80719(8) 0.0310(3) Uani 1 1 d . . .
S1 S 0.42211(11) -0.1060(2) 0.8434(4) 0.0396(5) Uani 1 1 d . . .
S2 S 0.25300(13) -0.1588(2) 0.76787(16) 0.0312(6) Uani 1 1 d . . .
S3 S 0.31323(14) -0.3627(2) 0.93585(17) 0.0354(6) Uani 1 1 d . . .
C3 C 0.4408(5) 0.3529(8) 0.8477(10) 0.047(3) Uani 1 1 d . . .
H3A H 0.4113 0.4296 0.8321 0.056 Uiso 1 1 calc R . .
H3B H 0.4872 0.3808 0.8363 0.056 Uiso 1 1 calc R . .
N2 N 0.4239(4) 0.2314(7) 0.7927(6) 0.034(2) Uani 1 1 d . . .
H2C H 0.4586 0.1714 0.8034 0.040 Uiso 1 1 calc R . .
N3 N 0.3618(4) 0.2735(7) 0.9620(5) 0.036(2) Uani 1 1 d . . .
H3C H 0.3355 0.3506 0.9563 0.043 Uiso 1 1 calc R . .
N1 N 0.3432(5) 0.0887(7) 0.6681(6) 0.040(2) Uani 1 1 d . . .
H1A H 0.3359 0.0025 0.6472 0.048 Uiso 1 1 calc R . .
H1B H 0.3141 0.1460 0.6399 0.048 Uiso 1 1 calc R . .
N4 N 0.3248(5) -0.0109(8) 1.0083(5) 0.045(2) Uani 1 1 d . . .
H4A H 0.2835 -0.0119 1.0337 0.054 Uiso 1 1 calc R . .
H4B H 0.3399 -0.0989 1.0054 0.054 Uiso 1 1 calc R . .
C1 C 0.4132(6) 0.1303(12) 0.6451(8) 0.050(3) Uani 1 1 d . . .
H1C H 0.4168 0.1483 0.5815 0.060 Uiso 1 1 calc R . .
H1D H 0.4447 0.0570 0.6606 0.060 Uiso 1 1 calc R . .
C4 C 0.4325(6) 0.3187(11) 0.9436(9) 0.050(3) Uani 1 1 d . . .
H4C H 0.4431 0.3995 0.9796 0.060 Uiso 1 1 calc R . .
H4D H 0.4637 0.2452 0.9599 0.060 Uiso 1 1 calc R . .
C5 C 0.3530(7) 0.2257(9) 1.0548(7) 0.050(3) Uani 1 1 d . . .
H5A H 0.3065 0.2409 1.0734 0.060 Uiso 1 1 calc R . .
H5B H 0.3823 0.2789 1.0940 0.060 Uiso 1 1 calc R . .
C2 C 0.4288(6) 0.2586(11) 0.6969(8) 0.048(3) Uani 1 1 d . . .
H2A H 0.4742 0.2901 0.6826 0.058 Uiso 1 1 calc R . .
H2B H 0.3972 0.3314 0.6806 0.058 Uiso 1 1 calc R . .
C6 C 0.3704(9) 0.0698(10) 1.0632(8) 0.067(5) Uani 1 1 d . . .
H6A H 0.4168 0.0541 1.0443 0.080 Uiso 1 1 calc R . .
H6B H 0.3663 0.0410 1.1251 0.080 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
Pr1 N2 2.637(7) . ?
Pr1 N3 2.656(8) . ?
Pr1 N4 2.671(8) . ?
Pr1 N1 2.676(9) . ?
Pr1 S1 2.844(2) . ?
Pr1 S3 2.922(3) 4 ?
Pr1 S2 2.939(2) . ?
Pr1 S2 2.972(2) 4 ?
As1 S1 2.224(3) . ?
As1 S3 2.227(3) . ?
As1 S2 2.306(3) . ?
S2 Pr1 2.972(2) 4_545 ?
S3 Pr1 2.922(3) 4_545 ?
C3 N2 1.470(13) . ?
C3 C4 1.481(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N2 C2 1.459(15) . ?
N2 H2C 0.9100 . ?
N3 C5 1.473(13) . ?
N3 C4 1.486(13) . ?
N3 H3C 0.9100 . ?
N1 C1 1.478(14) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N4 C6 1.444(15) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
C1 C2 1.492(15) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.546(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 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
N2 Pr1 N3 65.0(3) . . ?
N2 Pr1 N4 113.4(3) . . ?
N3 Pr1 N4 66.5(2) . . ?
N2 Pr1 N1 63.9(3) . . ?
N3 Pr1 N1 126.4(3) . . ?
N4 Pr1 N1 152.4(2) . . ?
N2 Pr1 S1 74.98(16) . . ?
N3 Pr1 S1 100.7(2) . . ?
N4 Pr1 S1 72.3(2) . . ?
N1 Pr1 S1 80.8(2) . . ?
N2 Pr1 S3 139.91(17) . 4 ?
N3 Pr1 S3 83.3(2) . 4 ?
N4 Pr1 S3 71.2(2) . 4 ?
N1 Pr1 S3 130.1(2) . 4 ?
S1 Pr1 S3 137.84(10) . 4 ?
N2 Pr1 S2 130.45(19) . . ?
N3 Pr1 S2 160.47(18) . . ?
N4 Pr1 S2 94.41(18) . . ?
N1 Pr1 S2 72.57(17) . . ?
S1 Pr1 S2 75.91(8) . . ?
S3 Pr1 S2 86.64(7) 4 . ?
N2 Pr1 S2 81.33(17) . 4 ?
N3 Pr1 S2 83.07(17) . 4 ?
N4 Pr1 S2 133.08(18) . 4 ?
N1 Pr1 S2 74.51(18) . 4 ?
S1 Pr1 S2 151.46(11) . 4 ?
S3 Pr1 S2 70.55(7) 4 4 ?
S2 Pr1 S2 109.29(5) . 4 ?
S1 As1 S3 106.10(16) . . ?
S1 As1 S2 103.50(8) . . ?
S3 As1 S2 97.33(10) . . ?
As1 S1 Pr1 91.38(8) . . ?
As1 S2 Pr1 87.39(8) . . ?
As1 S2 Pr1 83.62(7) . 4_545 ?
Pr1 S2 Pr1 135.17(9) . 4_545 ?
As1 S3 Pr1 86.18(8) . 4_545 ?
N2 C3 C4 109.9(8) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C2 N2 C3 113.1(8) . . ?
C2 N2 Pr1 115.2(7) . . ?
C3 N2 Pr1 115.4(6) . . ?
C2 N2 H2C 103.7 . . ?
C3 N2 H2C 103.7 . . ?
Pr1 N2 H2C 103.7 . . ?
C5 N3 C4 112.1(9) . . ?
C5 N3 Pr1 112.6(5) . . ?
C4 N3 Pr1 113.1(6) . . ?
C5 N3 H3C 106.1 . . ?
C4 N3 H3C 106.1 . . ?
Pr1 N3 H3C 106.1 . . ?
C1 N1 Pr1 114.6(7) . . ?
C1 N1 H1A 108.6 . . ?
Pr1 N1 H1A 108.6 . . ?
C1 N1 H1B 108.6 . . ?
Pr1 N1 H1B 108.6 . . ?
H1A N1 H1B 107.6 . . ?
C6 N4 Pr1 111.7(6) . . ?
C6 N4 H4A 109.3 . . ?
Pr1 N4 H4A 109.3 . . ?
C6 N4 H4B 109.3 . . ?
Pr1 N4 H4B 109.3 . . ?
H4A N4 H4B 107.9 . . ?
N1 C1 C2 107.3(9) . . ?
N1 C1 H1C 110.3 . . ?
C2 C1 H1C 110.3 . . ?
N1 C1 H1D 110.3 . . ?
C2 C1 H1D 110.3 . . ?
H1C C1 H1D 108.5 . . ?
C3 C4 N3 110.4(10) . . ?
C3 C4 H4C 109.6 . . ?
N3 C4 H4C 109.6 . . ?
C3 C4 H4D 109.6 . . ?
N3 C4 H4D 109.6 . . ?
H4C C4 H4D 108.1 . . ?
N3 C5 C6 110.8(9) . . ?
N3 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N2 C2 C1 110.4(8) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N4 C6 C5 109.8(10) . . ?
N4 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N4 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.132
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033471'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 As N4 Nd S3'
_chemical_formula_sum            'C6 H18 As N4 Nd S3'
_chemical_formula_weight         461.58

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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           Orthorhombic
_symmetry_space_group_name_H-M   'A b a 2'
_symmetry_space_group_name_Hall  'A 2 -2ac '

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

_cell_length_a                   19.648(4)
_cell_length_b                   9.625(3)
_cell_length_c                   14.947(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2826.9(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    6.417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5387
_exptl_absorpt_correction_T_max  0.6622
_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            11560
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.36
_reflns_number_total             3376
_reflns_number_gt                3290
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.6421P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(9)
_refine_ls_number_reflns         3376
_refine_ls_number_parameters     137
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_ref         0.0401
_refine_ls_wR_factor_gt          0.0399
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
Nd1 Nd 0.684489(6) 0.907689(12) 0.940917(13) 0.02139(4) Uani 1 1 d . . .
As1 As 0.649613(15) 1.27525(3) 0.97740(3) 0.02766(7) Uani 1 1 d . . .
S1 S 0.57794(3) 1.10573(6) 0.94085(12) 0.03662(16) Uani 1 1 d . . .
S2 S 0.74750(4) 1.15818(6) 1.01489(6) 0.02808(16) Uani 1 1 d . . .
S3 S 0.68653(4) 1.36377(8) 0.84913(6) 0.03057(17) Uani 1 1 d . . .
N1 N 0.67644(18) 1.0121(3) 0.7773(2) 0.0429(7) Uani 1 1 d . . .
H1A H 0.6617 1.1005 0.7802 0.051 Uiso 1 1 calc R . .
H1B H 0.7180 1.0124 0.7521 0.051 Uiso 1 1 calc R . .
N2 N 0.63839(15) 0.7285(3) 0.8212(2) 0.0338(6) Uani 1 1 d . . .
H2C H 0.6650 0.6516 0.8269 0.041 Uiso 1 1 calc R . .
N3 N 0.57616(14) 0.7700(2) 0.9910(2) 0.0301(6) Uani 1 1 d . . .
H3C H 0.5412 0.8295 0.9797 0.036 Uiso 1 1 calc R . .
N4 N 0.65759(17) 0.9133(3) 1.1148(2) 0.0349(6) Uani 1 1 d . . .
H4A H 0.6874 0.8575 1.1430 0.042 Uiso 1 1 calc R . .
H4B H 0.6645 1.0003 1.1349 0.042 Uiso 1 1 calc R . .
C1 C 0.6296(3) 0.9299(4) 0.7217(3) 0.0578(13) Uani 1 1 d . . .
H1C H 0.6329 0.9598 0.6598 0.069 Uiso 1 1 calc R . .
H1D H 0.5832 0.9443 0.7416 0.069 Uiso 1 1 calc R . .
C2 C 0.6478(3) 0.7764(4) 0.7287(3) 0.0493(11) Uani 1 1 d . . .
H2A H 0.6189 0.7228 0.6889 0.059 Uiso 1 1 calc R . .
H2B H 0.6947 0.7625 0.7107 0.059 Uiso 1 1 calc R . .
C3 C 0.5679(2) 0.6816(4) 0.8396(3) 0.0475(10) Uani 1 1 d . . .
H3A H 0.5577 0.6002 0.8038 0.057 Uiso 1 1 calc R . .
H3B H 0.5360 0.7543 0.8234 0.057 Uiso 1 1 calc R . .
C4 C 0.56014(16) 0.6473(3) 0.9365(4) 0.0452(8) Uani 1 1 d . . .
H4C H 0.5138 0.6176 0.9483 0.054 Uiso 1 1 calc R . .
H4D H 0.5905 0.5717 0.9522 0.054 Uiso 1 1 calc R . .
C5 C 0.5706(2) 0.7422(4) 1.0881(3) 0.0472(10) Uani 1 1 d . . .
H5A H 0.6012 0.6673 1.1045 0.057 Uiso 1 1 calc R . .
H5B H 0.5245 0.7135 1.1024 0.057 Uiso 1 1 calc R . .
C6 C 0.58834(19) 0.8704(5) 1.1399(3) 0.0438(9) Uani 1 1 d . . .
H6A H 0.5563 0.9441 1.1262 0.053 Uiso 1 1 calc R . .
H6B H 0.5862 0.8515 1.2035 0.053 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
Nd1 N3 2.617(3) . ?
Nd1 N2 2.645(3) . ?
Nd1 N1 2.649(3) . ?
Nd1 N4 2.653(3) . ?
Nd1 S1 2.8313(8) . ?
Nd1 S3 2.9126(9) 4_645 ?
Nd1 S2 2.9272(9) . ?
Nd1 S2 2.9624(9) 4_645 ?
As1 S3 2.2199(10) . ?
As1 S1 2.2235(9) . ?
As1 S2 2.2986(9) . ?
S2 Nd1 2.9624(9) 4_655 ?
S3 Nd1 2.9126(9) 4_655 ?
N1 C1 1.471(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.470(5) . ?
N2 C3 1.483(5) . ?
N2 H2C 0.9100 . ?
N3 C4 1.469(5) . ?
N3 C5 1.479(6) . ?
N3 H3C 0.9100 . ?
N4 C6 1.470(5) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
C1 C2 1.524(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.493(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.498(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 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 Nd1 N2 65.46(10) . . ?
N3 Nd1 N1 114.06(10) . . ?
N2 Nd1 N1 66.58(9) . . ?
N3 Nd1 N4 64.40(10) . . ?
N2 Nd1 N4 127.43(9) . . ?
N1 Nd1 N4 152.24(9) . . ?
N3 Nd1 S1 74.91(6) . . ?
N2 Nd1 S1 100.70(7) . . ?
N1 Nd1 S1 72.55(8) . . ?
N4 Nd1 S1 80.75(7) . . ?
N3 Nd1 S3 140.27(6) . 4_645 ?
N2 Nd1 S3 83.38(7) . 4_645 ?
N1 Nd1 S3 70.86(8) . 4_645 ?
N4 Nd1 S3 129.63(7) . 4_645 ?
S1 Nd1 S3 137.81(3) . 4_645 ?
N3 Nd1 S2 130.77(7) . . ?
N2 Nd1 S2 159.63(7) . . ?
N1 Nd1 S2 93.53(7) . . ?
N4 Nd1 S2 72.38(6) . . ?
S1 Nd1 S2 76.02(3) . . ?
S3 Nd1 S2 85.95(3) 4_645 . ?
N3 Nd1 S2 81.35(6) . 4_645 ?
N2 Nd1 S2 83.00(6) . 4_645 ?
N1 Nd1 S2 132.78(7) . 4_645 ?
N4 Nd1 S2 74.98(6) . 4_645 ?
S1 Nd1 S2 151.58(3) . 4_645 ?
S3 Nd1 S2 70.47(2) 4_645 4_645 ?
S2 Nd1 S2 109.63(3) . 4_645 ?
S3 As1 S1 106.05(5) . . ?
S3 As1 S2 97.20(3) . . ?
S1 As1 S2 103.30(3) . . ?
As1 S1 Nd1 91.47(3) . . ?
As1 S2 Nd1 87.58(3) . . ?
As1 S2 Nd1 83.63(3) . 4_655 ?
Nd1 S2 Nd1 135.85(3) . 4_655 ?
As1 S3 Nd1 86.17(3) . 4_655 ?
C1 N1 Nd1 110.8(3) . . ?
C1 N1 H1A 109.5 . . ?
Nd1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
Nd1 N1 H1B 109.5 . . ?
H1A N1 H1B 108.1 . . ?
C2 N2 C3 112.8(3) . . ?
C2 N2 Nd1 112.9(2) . . ?
C3 N2 Nd1 113.1(2) . . ?
C2 N2 H2C 105.7 . . ?
C3 N2 H2C 105.7 . . ?
Nd1 N2 H2C 105.7 . . ?
C4 N3 C5 112.5(3) . . ?
C4 N3 Nd1 115.0(2) . . ?
C5 N3 Nd1 115.6(2) . . ?
C4 N3 H3C 104.0 . . ?
C5 N3 H3C 104.0 . . ?
Nd1 N3 H3C 104.0 . . ?
C6 N4 Nd1 115.4(2) . . ?
C6 N4 H4A 108.4 . . ?
Nd1 N4 H4A 108.4 . . ?
C6 N4 H4B 108.4 . . ?
Nd1 N4 H4B 108.4 . . ?
H4A N4 H4B 107.5 . . ?
N1 C1 C2 109.6(4) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N2 C2 C1 109.9(3) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 110.0(3) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 109.8(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 . . ?
N3 C5 C6 109.9(3) . . ?
N3 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
N3 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N4 C6 C5 108.4(3) . . ?
N4 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
N4 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033472'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 As N4 S3 Sm '
_chemical_formula_sum            'C6 H18 As N4 S3 Sm '
_chemical_formula_weight         467.70

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'A b a 2'
_symmetry_space_group_name_Hall  'A 2 -2ac '

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

_cell_length_a                   19.4659(18)
_cell_length_b                   9.5700(9)
_cell_length_c                   14.7915(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2755.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    7.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2896
_exptl_absorpt_correction_T_max  0.3638
_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            5148
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         25.09
_reflns_number_total             2131
_reflns_number_gt                2108
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0269P)²+4.4858P] 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     SHELXL
_refine_ls_extinction_coef       0.00044(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.031(15)
_refine_ls_number_reflns         2131
_refine_ls_number_parameters     137
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0540
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
Sm1 Sm 0.315605(11) 0.09141(2) 0.35558(2) 0.01218(10) Uani 1 1 d . . .
As1 As 0.34983(3) -0.27608(5) 0.39361(4) 0.01430(14) Uani 1 1 d . . .
S1 S 0.42211(6) -0.10582(11) 0.35634(19) 0.0182(3) Uani 1 1 d . . .
S2 S 0.25071(7) -0.15835(12) 0.42902(10) 0.0150(3) Uani 1 1 d . . .
S3 S 0.31284(7) -0.36542(14) 0.26369(10) 0.0155(3) Uani 1 1 d . . .
C4 C 0.4395(3) 0.3523(5) 0.3530(6) 0.0222(11) Uani 1 1 d . . .
H4A H 0.4862 0.3815 0.3656 0.027 Uiso 1 1 calc R . .
H4B H 0.4089 0.4283 0.3693 0.027 Uiso 1 1 calc R . .
N3 N 0.4226(3) 0.2270(4) 0.4076(4) 0.0163(11) Uani 1 1 d . . .
H3C H 0.4578 0.1673 0.3955 0.020 Uiso 1 1 calc R . .
N1 N 0.3234(3) -0.0133(5) 0.1939(4) 0.0220(11) Uani 1 1 d . . .
H1A H 0.3380 -0.1025 0.1974 0.026 Uiso 1 1 calc R . .
H1B H 0.2814 -0.0134 0.1685 0.026 Uiso 1 1 calc R . .
N2 N 0.3608(2) 0.2710(4) 0.2370(3) 0.0167(10) Uani 1 1 d . . .
H2C H 0.3335 0.3477 0.2426 0.020 Uiso 1 1 calc R . .
N4 N 0.3402(3) 0.0802(5) 0.5290(4) 0.0173(11) Uani 1 1 d . . .
H4C H 0.3099 0.1358 0.5577 0.021 Uiso 1 1 calc R . .
H4D H 0.3328 -0.0078 0.5482 0.021 Uiso 1 1 calc R . .
C3 C 0.4322(3) 0.3202(6) 0.2552(5) 0.0246(14) Uani 1 1 d . . .
H3A H 0.4648 0.2484 0.2380 0.030 Uiso 1 1 calc R . .
H3B H 0.4417 0.4033 0.2197 0.030 Uiso 1 1 calc R . .
C5 C 0.4290(3) 0.2528(6) 0.5052(5) 0.0233(14) Uani 1 1 d . . .
H5A H 0.3985 0.3282 0.5229 0.028 Uiso 1 1 calc R . .
H5B H 0.4757 0.2800 0.5196 0.028 Uiso 1 1 calc R . .
C6 C 0.4106(3) 0.1226(6) 0.5558(5) 0.0204(13) Uani 1 1 d . . .
H6A H 0.4429 0.0487 0.5415 0.024 Uiso 1 1 calc R . .
H6B H 0.4124 0.1398 0.6204 0.024 Uiso 1 1 calc R . .
C2 C 0.3519(3) 0.2224(6) 0.1436(5) 0.0261(14) Uani 1 1 d . . .
H2A H 0.3810 0.2766 0.1035 0.031 Uiso 1 1 calc R . .
H2B H 0.3046 0.2358 0.1251 0.031 Uiso 1 1 calc R . .
C1 C 0.3709(4) 0.0668(6) 0.1366(5) 0.0279(15) Uani 1 1 d . . .
H1C H 0.3672 0.0358 0.0744 0.033 Uiso 1 1 calc R . .
H1D H 0.4178 0.0525 0.1566 0.033 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
Sm1 N3 2.573(5) . ?
Sm1 N1 2.598(5) . ?
Sm1 N2 2.609(5) . ?
Sm1 N4 2.612(5) . ?
Sm1 S1 2.8037(12) . ?
Sm1 S3 2.8756(14) 4 ?
Sm1 S2 2.9136(13) . ?
Sm1 S2 2.9294(13) 4 ?
Sm1 As1 3.5065(6) 4 ?
As1 S1 2.2223(14) . ?
As1 S3 2.2231(16) . ?
As1 S2 2.2950(14) . ?
As1 Sm1 3.5065(6) 4_545 ?
S2 Sm1 2.9294(13) 4_545 ?
S3 Sm1 2.8756(14) 4_545 ?
C4 N3 1.482(7) . ?
C4 C3 1.487(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N3 C5 1.470(9) . ?
N3 H3C 0.9100 . ?
N1 C1 1.469(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.467(9) . ?
N2 C3 1.491(8) . ?
N2 H2C 0.9100 . ?
N4 C6 1.484(8) . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 C6 1.497(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2 C1 1.538(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 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 Sm1 N1 114.99(16) . . ?
N3 Sm1 N2 66.15(15) . . ?
N1 Sm1 N2 67.37(15) . . ?
N3 Sm1 N4 65.09(16) . . ?
N1 Sm1 N4 151.37(15) . . ?
N2 Sm1 N4 128.75(15) . . ?
N3 Sm1 S1 74.91(10) . . ?
N1 Sm1 S1 72.57(13) . . ?
N2 Sm1 S1 101.35(11) . . ?
N4 Sm1 S1 80.39(12) . . ?
N3 Sm1 S3 140.63(11) . 4 ?
N1 Sm1 S3 70.82(12) . 4 ?
N2 Sm1 S3 83.15(11) . 4 ?
N4 Sm1 S3 128.99(12) . 4 ?
S1 Sm1 S3 137.86(5) . 4 ?
N3 Sm1 S2 130.81(12) . . ?
N1 Sm1 S2 92.99(12) . . ?
N2 Sm1 S2 159.62(11) . . ?
N4 Sm1 S2 71.30(11) . . ?
S1 Sm1 S2 76.52(4) . . ?
S3 Sm1 S2 85.24(4) 4 . ?
N3 Sm1 S2 80.42(10) . 4 ?
N1 Sm1 S2 133.06(12) . 4 ?
N2 Sm1 S2 81.92(10) . 4 ?
N4 Sm1 S2 75.52(11) . 4 ?
S1 Sm1 S2 151.01(6) . 4 ?
S3 Sm1 S2 71.02(4) 4 4 ?
S2 Sm1 S2 109.96(3) . 4 ?
N3 Sm1 As1 120.89(10) . 4 ?
N1 Sm1 As1 109.95(12) . 4 ?
N2 Sm1 As1 100.33(10) . 4 ?
N4 Sm1 As1 91.45(11) . 4 ?
S1 Sm1 As1 157.21(3) . 4 ?
S3 Sm1 As1 39.23(3) 4 4 ?
S2 Sm1 As1 80.72(3) . 4 ?
S2 Sm1 As1 40.55(3) 4 4 ?
S1 As1 S3 105.82(8) . . ?
S1 As1 S2 103.24(5) . . ?
S3 As1 S2 96.53(5) . . ?
S1 As1 Sm1 143.79(5) . 4_545 ?
S3 As1 Sm1 54.88(4) . 4_545 ?
S2 As1 Sm1 56.08(3) . 4_545 ?
As1 S1 Sm1 91.51(4) . . ?
As1 S2 Sm1 87.31(4) . . ?
As1 S2 Sm1 83.37(4) . 4_545 ?
Sm1 S2 Sm1 136.34(6) . 4_545 ?
As1 S3 Sm1 85.89(5) . 4_545 ?
N3 C4 C3 110.0(5) . . ?
N3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C5 N3 C4 112.4(5) . . ?
C5 N3 Sm1 116.5(4) . . ?
C4 N3 Sm1 115.1(4) . . ?
C5 N3 H3C 103.6 . . ?
C4 N3 H3C 103.6 . . ?
Sm1 N3 H3C 103.6 . . ?
C1 N1 Sm1 111.5(4) . . ?
C1 N1 H1A 109.3 . . ?
Sm1 N1 H1A 109.3 . . ?
C1 N1 H1B 109.3 . . ?
Sm1 N1 H1B 109.3 . . ?
H1A N1 H1B 108.0 . . ?
C2 N2 C3 112.3(5) . . ?
C2 N2 Sm1 112.6(3) . . ?
C3 N2 Sm1 113.6(3) . . ?
C2 N2 H2C 105.8 . . ?
C3 N2 H2C 105.8 . . ?
Sm1 N2 H2C 105.8 . . ?
C6 N4 Sm1 114.8(4) . . ?
C6 N4 H4C 108.6 . . ?
Sm1 N4 H4C 108.6 . . ?
C6 N4 H4D 108.6 . . ?
Sm1 N4 H4D 108.6 . . ?
H4C N4 H4D 107.5 . . ?
C4 C3 N2 109.3(5) . . ?
C4 C3 H3A 109.8 . . ?
N2 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
N2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N3 C5 C6 109.4(5) . . ?
N3 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N3 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N4 C6 C5 108.4(5) . . ?
N4 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
N4 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
N2 C2 C1 110.0(5) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N1 C1 C2 108.4(5) . . ?
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 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.127
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033473'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As La N6 S4'
_chemical_formula_sum            'C8 H26 As La N6 S4'
_chemical_formula_weight         548.42

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_chemical_absolute_configuration unk

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'

_cell_length_a                   8.3601(2)
_cell_length_b                   11.2089(3)
_cell_length_c                   19.8455(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1859.67(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    4.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6379
_exptl_absorpt_correction_T_max  0.7152
_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            5938
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3574
_reflns_number_gt                3306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0086P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.165(15)
_refine_ls_number_reflns         3574
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0477
_refine_ls_wR_factor_gt          0.0460
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
La1 La 0.21391(3) 0.53495(2) 0.907874(13) 0.01761(7) Uani 1 1 d . . .
As1 As 0.76669(5) 0.50343(4) 0.90861(3) 0.02110(11) Uani 1 1 d . . .
S1 S 0.56608(12) 0.62635(10) 0.91107(8) 0.0281(3) Uani 1 1 d . . .
S2 S 0.91386(14) 0.54095(14) 0.82151(6) 0.0307(3) Uani 1 1 d . . .
S3 S 0.91746(14) 0.53547(14) 0.99512(6) 0.0314(3) Uani 1 1 d . . .
S4 S 0.68404(13) 0.32188(10) 0.90718(8) 0.0302(3) Uani 1 1 d . . .
N1 N 0.1518(5) 0.7716(3) 0.90001(19) 0.0326(10) Uani 1 1 d . . .
H1A H 0.0449 0.7809 0.9014 0.039 Uiso 1 1 calc R . .
H1B H 0.1917 0.8061 0.9374 0.039 Uiso 1 1 calc R . .
N2 N 0.2964(5) 0.6499(3) 0.79359(17) 0.0259(10) Uani 1 1 d . . .
H2C H 0.3991 0.6734 0.8011 0.031 Uiso 1 1 calc R . .
N3 N 0.3631(5) 0.4006(3) 0.81155(19) 0.0263(10) Uani 1 1 d . . .
H3C H 0.4530 0.3712 0.8313 0.032 Uiso 1 1 calc R . .
N4 N 0.1196(5) 0.3032(3) 0.8986(2) 0.0361(11) Uani 1 1 d . . .
H4A H 0.1201 0.2713 0.9402 0.043 Uiso 1 1 calc R . .
H4B H 0.0182 0.3014 0.8835 0.043 Uiso 1 1 calc R . .
N6 N 0.2739(5) 0.6405(3) 1.02471(17) 0.0243(9) Uani 1 1 d . . .
H6A H 0.3633 0.6846 1.0205 0.029 Uiso 1 1 calc R . .
H6B H 0.1929 0.6905 1.0343 0.029 Uiso 1 1 calc R . .
N7 N 0.3610(5) 0.4005(3) 1.00104(18) 0.0280(11) Uani 1 1 d . . .
H7A H 0.2940 0.3414 1.0132 0.034 Uiso 1 1 calc R . .
H7B H 0.4470 0.3663 0.9818 0.034 Uiso 1 1 calc R . .
C1 C 0.2111(7) 0.8385(4) 0.8421(2) 0.0398(14) Uani 1 1 d . . .
H1C H 0.3190 0.8659 0.8511 0.048 Uiso 1 1 calc R . .
H1D H 0.1440 0.9079 0.8347 0.048 Uiso 1 1 calc R . .
C2 C 0.2105(7) 0.7618(4) 0.7805(2) 0.0367(13) Uani 1 1 d . . .
H2A H 0.1012 0.7444 0.7675 0.044 Uiso 1 1 calc R . .
H2B H 0.2615 0.8040 0.7436 0.044 Uiso 1 1 calc R . .
C3 C 0.3081(7) 0.5714(4) 0.7356(2) 0.0381(14) Uani 1 1 d . . .
H3A H 0.3493 0.6154 0.6972 0.046 Uiso 1 1 calc R . .
H3B H 0.2028 0.5414 0.7239 0.046 Uiso 1 1 calc R . .
C4 C 0.4181(6) 0.4684(5) 0.7516(2) 0.0370(13) Uani 1 1 d . . .
H4C H 0.4231 0.4152 0.7131 0.044 Uiso 1 1 calc R . .
H4D H 0.5250 0.4986 0.7599 0.044 Uiso 1 1 calc R . .
C5 C 0.2661(7) 0.2959(4) 0.7931(3) 0.0477(16) Uani 1 1 d . . .
H5A H 0.3270 0.2449 0.7631 0.057 Uiso 1 1 calc R . .
H5B H 0.1709 0.3219 0.7693 0.057 Uiso 1 1 calc R . .
C6 C 0.2189(7) 0.2274(4) 0.8541(3) 0.0490(15) Uani 1 1 d . . .
H6C H 0.1589 0.1571 0.8409 0.059 Uiso 1 1 calc R . .
H6D H 0.3138 0.2015 0.8781 0.059 Uiso 1 1 calc R . .
C7 C 0.4135(5) 0.4621(4) 1.0620(2) 0.0317(12) Uani 1 1 d . . .
H7C H 0.5174 0.4981 1.0544 0.038 Uiso 1 1 calc R . .
H7D H 0.4239 0.4051 1.0986 0.038 Uiso 1 1 calc R . .
C8 C 0.2947(6) 0.5573(4) 1.0813(2) 0.0304(11) Uani 1 1 d . . .
H8A H 0.1928 0.5209 1.0926 0.037 Uiso 1 1 calc R . .
H8B H 0.3329 0.6002 1.1206 0.037 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
La1 N6 2.651(3) . ?
La1 N7 2.684(4) . ?
La1 N2 2.698(4) . ?
La1 N1 2.708(3) . ?
La1 N4 2.721(4) . ?
La1 N3 2.734(4) . ?
La1 S3 3.0232(12) 1_455 ?
La1 S2 3.0388(12) 1_455 ?
La1 S1 3.1180(11) . ?
As1 S4 2.1493(12) . ?
As1 S3 2.1599(12) . ?
As1 S2 2.1629(13) . ?
As1 S1 2.1711(11) . ?
S2 La1 3.0388(12) 1_655 ?
S3 La1 3.0232(12) 1_655 ?
N1 C1 1.458(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.453(5) . ?
N2 C2 1.469(5) . ?
N2 H2C 0.9100 . ?
N3 C5 1.472(6) . ?
N3 C4 1.484(6) . ?
N3 H3C 0.9100 . ?
N4 C6 1.481(6) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N6 C8 1.471(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 C7 1.461(5) . ?
N7 H7A 0.9000 . ?
N7 H7B 0.9000 . ?
C1 C2 1.495(6) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.510(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.488(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.508(6) . ?
C7 H7C 0.9700 . ?
C7 H7D 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
N6 La1 N7 63.98(11) . . ?
N6 La1 N2 118.28(11) . . ?
N7 La1 N2 136.90(13) . . ?
N6 La1 N1 69.48(11) . . ?
N7 La1 N1 132.67(12) . . ?
N2 La1 N1 62.15(12) . . ?
N6 La1 N4 122.68(12) . . ?
N7 La1 N4 69.08(12) . . ?
N2 La1 N4 118.24(13) . . ?
N1 La1 N4 151.16(12) . . ?
N6 La1 N3 140.44(12) . . ?
N7 La1 N3 87.91(10) . . ?
N2 La1 N3 63.81(11) . . ?
N1 La1 N3 125.93(11) . . ?
N4 La1 N3 63.84(12) . . ?
N6 La1 S3 69.72(9) . 1_455 ?
N7 La1 S3 88.97(9) . 1_455 ?
N2 La1 S3 133.64(9) . 1_455 ?
N1 La1 S3 82.75(9) . 1_455 ?
N4 La1 S3 78.63(9) . 1_455 ?
N3 La1 S3 140.83(9) . 1_455 ?
N6 La1 S2 129.77(9) . 1_455 ?
N7 La1 S2 141.19(9) . 1_455 ?
N2 La1 S2 74.12(10) . 1_455 ?
N1 La1 S2 77.73(9) . 1_455 ?
N4 La1 S2 75.17(9) . 1_455 ?
N3 La1 S2 89.67(9) . 1_455 ?
S3 La1 S2 69.29(3) 1_455 1_455 ?
N6 La1 S1 69.93(9) . . ?
N7 La1 S1 74.81(9) . . ?
N2 La1 S1 67.59(10) . . ?
N1 La1 S1 81.98(9) . . ?
N4 La1 S1 126.06(8) . . ?
N3 La1 S1 76.38(9) . . ?
S3 La1 S1 139.62(4) 1_455 . ?
S2 La1 S1 141.60(4) 1_455 . ?
S4 As1 S3 110.83(6) . . ?
S4 As1 S2 110.88(6) . . ?
S3 As1 S2 105.72(4) . . ?
S4 As1 S1 110.66(5) . . ?
S3 As1 S1 109.11(6) . . ?
S2 As1 S1 109.51(6) . . ?
As1 S1 La1 121.36(5) . . ?
As1 S2 La1 90.83(4) . 1_655 ?
As1 S3 La1 91.31(4) . 1_655 ?
C1 N1 La1 118.9(3) . . ?
C1 N1 H1A 107.6 . . ?
La1 N1 H1A 107.6 . . ?
C1 N1 H1B 107.6 . . ?
La1 N1 H1B 107.6 . . ?
H1A N1 H1B 107.0 . . ?
C3 N2 C2 114.2(4) . . ?
C3 N2 La1 113.2(3) . . ?
C2 N2 La1 115.6(3) . . ?
C3 N2 H2C 104.0 . . ?
C2 N2 H2C 104.0 . . ?
La1 N2 H2C 104.0 . . ?
C5 N3 C4 112.3(4) . . ?
C5 N3 La1 111.2(3) . . ?
C4 N3 La1 114.8(3) . . ?
C5 N3 H3C 105.9 . . ?
C4 N3 H3C 105.9 . . ?
La1 N3 H3C 105.9 . . ?
C6 N4 La1 115.2(3) . . ?
C6 N4 H4A 108.5 . . ?
La1 N4 H4A 108.5 . . ?
C6 N4 H4B 108.5 . . ?
La1 N4 H4B 108.5 . . ?
H4A N4 H4B 107.5 . . ?
C8 N6 La1 114.1(3) . . ?
C8 N6 H6A 108.7 . . ?
La1 N6 H6A 108.7 . . ?
C8 N6 H6B 108.7 . . ?
La1 N6 H6B 108.7 . . ?
H6A N6 H6B 107.6 . . ?
C7 N7 La1 116.3(3) . . ?
C7 N7 H7A 108.2 . . ?
La1 N7 H7A 108.2 . . ?
C7 N7 H7B 108.2 . . ?
La1 N7 H7B 108.2 . . ?
H7A N7 H7B 107.4 . . ?
N1 C1 C2 110.4(4) . . ?
N1 C1 H1C 109.6 . . ?
C2 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
C2 C1 H1D 109.6 . . ?
H1C C1 H1D 108.1 . . ?
N2 C2 C1 110.2(4) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 109.6(4) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 111.8(4) . . ?
N3 C4 H4C 109.2 . . ?
C3 C4 H4C 109.2 . . ?
N3 C4 H4D 109.2 . . ?
C3 C4 H4D 109.2 . . ?
H4C C4 H4D 107.9 . . ?
N3 C5 C6 110.8(4) . . ?
N3 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N4 C6 C5 109.8(4) . . ?
N4 C6 H6C 109.7 . . ?
C5 C6 H6C 109.7 . . ?
N4 C6 H6D 109.7 . . ?
C5 C6 H6D 109.7 . . ?
H6C C6 H6D 108.2 . . ?
N7 C7 C8 110.3(4) . . ?
N7 C7 H7C 109.6 . . ?
C8 C7 H7C 109.6 . . ?
N7 C7 H7D 109.6 . . ?
C8 C7 H7D 109.6 . . ?
H7C C7 H7D 108.1 . . ?
N6 C8 C7 109.4(4) . . ?
N6 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N6 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.098
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033474'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As Ce N6 S4'
_chemical_formula_sum            'C8 H26 As Ce N6 S4'
_chemical_formula_weight         549.63

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'
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'
As As 0.0499 2.0058 '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           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_chemical_absolute_configuration unk

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

_cell_length_a                   8.3413(2)
_cell_length_b                   11.1822(3)
_cell_length_c                   19.7987(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1846.71(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1084
_exptl_absorpt_coefficient_mu    4.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3307
_exptl_absorpt_correction_T_max  0.4911
_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            5011
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.08
_reflns_number_total             3054
_reflns_number_gt                2891
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0094P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         3054
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0509
_refine_ls_wR_factor_gt          0.0495
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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 0.71348(3) 0.46460(2) 0.092398(15) 0.01741(8) Uani 1 1 d . . .
As1 As 0.26748(6) 0.49642(4) 0.09158(3) 0.02099(13) Uani 1 1 d . . .
S1 S 0.41953(17) 0.46375(17) 0.00513(7) 0.0309(4) Uani 1 1 d . . .
S2 S 0.41531(17) 0.45860(17) 0.17882(7) 0.0297(4) Uani 1 1 d . . .
S3 S 0.06605(15) 0.37353(12) 0.08905(9) 0.0270(3) Uani 1 1 d . . .
S4 S 0.18529(16) 0.67839(12) 0.09272(8) 0.0304(3) Uani 1 1 d . . .
N1 N 0.6184(5) 0.6953(4) 0.1015(2) 0.0345(13) Uani 1 1 d . . .
H1A H 0.6169 0.7268 0.0597 0.041 Uiso 1 1 calc R . .
H1B H 0.5173 0.6969 0.1174 0.041 Uiso 1 1 calc R . .
N2 N 0.8621(5) 0.5992(4) 0.1876(2) 0.0246(12) Uani 1 1 d . . .
H2C H 0.9522 0.6279 0.1674 0.030 Uiso 1 1 calc R . .
N3 N 0.7938(6) 0.3503(4) 0.2062(2) 0.0259(11) Uani 1 1 d . . .
H3C H 0.8965 0.3264 0.1985 0.031 Uiso 1 1 calc R . .
N4 N 0.6511(5) 0.2299(4) 0.0995(2) 0.0317(12) Uani 1 1 d . . .
H4A H 0.5440 0.2208 0.0978 0.038 Uiso 1 1 calc R . .
H4B H 0.6914 0.1956 0.0621 0.038 Uiso 1 1 calc R . .
N5 N 0.8603(6) 0.5991(4) 0.0006(2) 0.0277(13) Uani 1 1 d . . .
H5A H 0.7937 0.6590 -0.0110 0.033 Uiso 1 1 calc R . .
H5B H 0.9470 0.6324 0.0201 0.033 Uiso 1 1 calc R . .
N6 N 0.7744(6) 0.3590(4) -0.02371(19) 0.0262(11) Uani 1 1 d . . .
H6A H 0.8648 0.3157 -0.0195 0.031 Uiso 1 1 calc R . .
H6B H 0.6939 0.3081 -0.0332 0.031 Uiso 1 1 calc R . .
C1 C 0.7178(8) 0.7714(5) 0.1446(3) 0.0482(18) Uani 1 1 d . . .
H1C H 0.6575 0.8419 0.1577 0.058 Uiso 1 1 calc R . .
H1D H 0.8117 0.7974 0.1197 0.058 Uiso 1 1 calc R . .
C2 C 0.7688(8) 0.7047(5) 0.2063(3) 0.0448(18) Uani 1 1 d . . .
H2A H 0.8331 0.7565 0.2348 0.054 Uiso 1 1 calc R . .
H2B H 0.6750 0.6804 0.2317 0.054 Uiso 1 1 calc R . .
C3 C 0.9194(7) 0.5309(6) 0.2474(3) 0.0343(15) Uani 1 1 d . . .
H3A H 0.9279 0.5843 0.2858 0.041 Uiso 1 1 calc R . .
H3B H 1.0253 0.4990 0.2381 0.041 Uiso 1 1 calc R . .
C4 C 0.8081(8) 0.4301(5) 0.2645(3) 0.0356(16) Uani 1 1 d . . .
H4C H 0.8493 0.3861 0.3030 0.043 Uiso 1 1 calc R . .
H4D H 0.7034 0.4616 0.2763 0.043 Uiso 1 1 calc R . .
C5 C 0.7098(8) 0.2394(5) 0.2195(3) 0.0370(15) Uani 1 1 d . . .
H5C H 0.6002 0.2567 0.2326 0.044 Uiso 1 1 calc R . .
H5D H 0.7613 0.1978 0.2566 0.044 Uiso 1 1 calc R . .
C6 C 0.7101(8) 0.1612(5) 0.1581(3) 0.0383(16) Uani 1 1 d . . .
H6C H 0.8180 0.1328 0.1493 0.046 Uiso 1 1 calc R . .
H6D H 0.6418 0.0923 0.1657 0.046 Uiso 1 1 calc R . .
C7 C 0.9124(7) 0.5381(6) -0.0617(3) 0.0341(15) Uani 1 1 d . . .
H7A H 1.0172 0.5026 -0.0548 0.041 Uiso 1 1 calc R . .
H7B H 0.9207 0.5956 -0.0982 0.041 Uiso 1 1 calc R . .
C8 C 0.7933(7) 0.4423(5) -0.0802(2) 0.0281(13) Uani 1 1 d . . .
H8A H 0.6908 0.4786 -0.0909 0.034 Uiso 1 1 calc R . .
H8B H 0.8305 0.3995 -0.1198 0.034 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
Ce1 N6 2.634(4) . ?
Ce1 N5 2.657(4) . ?
Ce1 N3 2.676(4) . ?
Ce1 N4 2.679(4) . ?
Ce1 N1 2.705(4) . ?
Ce1 N2 2.713(4) . ?
Ce1 S1 2.9996(14) . ?
Ce1 S2 3.0196(14) . ?
Ce1 S3 3.1129(13) 1_655 ?
As1 S4 2.1474(14) . ?
As1 S1 2.1614(15) . ?
As1 S2 2.1640(15) . ?
As1 S3 2.1712(13) . ?
S3 Ce1 3.1129(13) 1_455 ?
N1 C1 1.462(7) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.461(7) . ?
N2 C3 1.487(7) . ?
N2 H2C 0.9100 . ?
N3 C5 1.448(7) . ?
N3 C4 1.463(6) . ?
N3 H3C 0.9100 . ?
N4 C6 1.476(6) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.475(6) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.464(6) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.493(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.499(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.497(7) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.506(7) . ?
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
N6 Ce1 N5 64.41(13) . . ?
N6 Ce1 N3 118.20(12) . . ?
N5 Ce1 N3 136.95(15) . . ?
N6 Ce1 N4 69.15(13) . . ?
N5 Ce1 N4 132.82(14) . . ?
N3 Ce1 N4 62.39(13) . . ?
N6 Ce1 N1 122.85(14) . . ?
N5 Ce1 N1 68.96(14) . . ?
N3 Ce1 N1 118.21(14) . . ?
N4 Ce1 N1 150.91(14) . . ?
N6 Ce1 N2 140.12(15) . . ?
N5 Ce1 N2 87.18(12) . . ?
N3 Ce1 N2 64.23(13) . . ?
N4 Ce1 N2 126.56(13) . . ?
N1 Ce1 N2 63.79(14) . . ?
N6 Ce1 S1 69.73(12) . . ?
N5 Ce1 S1 89.11(11) . . ?
N3 Ce1 S1 133.49(11) . . ?
N4 Ce1 S1 82.44(10) . . ?
N1 Ce1 S1 78.58(10) . . ?
N2 Ce1 S1 140.88(10) . . ?
N6 Ce1 S2 130.05(12) . . ?
N5 Ce1 S2 141.21(11) . . ?
N3 Ce1 S2 73.65(12) . . ?
N4 Ce1 S2 77.79(11) . . ?
N1 Ce1 S2 75.04(10) . . ?
N2 Ce1 S2 89.70(10) . . ?
S1 Ce1 S2 69.70(3) . . ?
N6 Ce1 S3 69.66(12) . 1_655 ?
N5 Ce1 S3 74.65(11) . 1_655 ?
N3 Ce1 S3 67.98(12) . 1_655 ?
N4 Ce1 S3 82.19(10) . 1_655 ?
N1 Ce1 S3 126.18(10) . 1_655 ?
N2 Ce1 S3 76.38(10) . 1_655 ?
S1 Ce1 S3 139.37(4) . 1_655 ?
S2 Ce1 S3 141.53(4) . 1_655 ?
S4 As1 S1 110.84(7) . . ?
S4 As1 S2 111.02(7) . . ?
S1 As1 S2 105.35(5) . . ?
S4 As1 S3 110.67(5) . . ?
S1 As1 S3 109.20(7) . . ?
S2 As1 S3 109.61(7) . . ?
As1 S1 Ce1 91.32(5) . . ?
As1 S2 Ce1 90.73(5) . . ?
As1 S3 Ce1 121.57(5) . 1_455 ?
C1 N1 Ce1 115.3(3) . . ?
C1 N1 H1A 108.4 . . ?
Ce1 N1 H1A 108.4 . . ?
C1 N1 H1B 108.4 . . ?
Ce1 N1 H1B 108.4 . . ?
H1A N1 H1B 107.5 . . ?
C2 N2 C3 112.7(4) . . ?
C2 N2 Ce1 112.3(3) . . ?
C3 N2 Ce1 114.5(4) . . ?
C2 N2 H2C 105.4 . . ?
C3 N2 H2C 105.4 . . ?
Ce1 N2 H2C 105.4 . . ?
C5 N3 C4 114.7(4) . . ?
C5 N3 Ce1 116.2(3) . . ?
C4 N3 Ce1 113.1(3) . . ?
C5 N3 H3C 103.6 . . ?
C4 N3 H3C 103.6 . . ?
Ce1 N3 H3C 103.6 . . ?
C6 N4 Ce1 119.1(3) . . ?
C6 N4 H4A 107.5 . . ?
Ce1 N4 H4A 107.5 . . ?
C6 N4 H4B 107.5 . . ?
Ce1 N4 H4B 107.5 . . ?
H4A N4 H4B 107.0 . . ?
C7 N5 Ce1 116.5(3) . . ?
C7 N5 H5A 108.2 . . ?
Ce1 N5 H5A 108.2 . . ?
C7 N5 H5B 108.2 . . ?
Ce1 N5 H5B 108.2 . . ?
H5A N5 H5B 107.3 . . ?
C8 N6 Ce1 113.7(3) . . ?
C8 N6 H6A 108.8 . . ?
Ce1 N6 H6A 108.8 . . ?
C8 N6 H6B 108.8 . . ?
Ce1 N6 H6B 108.8 . . ?
H6A N6 H6B 107.7 . . ?
N1 C1 C2 110.4(5) . . ?
N1 C1 H1C 109.6 . . ?
C2 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
C2 C1 H1D 109.6 . . ?
H1C C1 H1D 108.1 . . ?
N2 C2 C1 110.4(5) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 111.5(4) . . ?
N2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
N3 C4 C3 109.3(5) . . ?
N3 C4 H4C 109.8 . . ?
C3 C4 H4C 109.8 . . ?
N3 C4 H4D 109.8 . . ?
C3 C4 H4D 109.8 . . ?
H4C C4 H4D 108.3 . . ?
N3 C5 C6 110.6(5) . . ?
N3 C5 H5C 109.5 . . ?
C6 C5 H5C 109.5 . . ?
N3 C5 H5D 109.5 . . ?
C6 C5 H5D 109.5 . . ?
H5C C5 H5D 108.1 . . ?
N4 C6 C5 109.5(5) . . ?
N4 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N4 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.2 . . ?
N5 C7 C8 109.7(4) . . ?
N5 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N5 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N6 C8 C7 109.7(4) . . ?
N6 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
N6 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.08
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.101
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033475'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As N6 Pr S4'
_chemical_formula_sum            'C8 H26 As N6 Pr S4'
_chemical_formula_weight         550.42

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'
Pr Pr -0.2180 2.8214 '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   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_chemical_absolute_configuration unk

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'

_cell_length_a                   8.3354(2)
_cell_length_b                   11.1590(2)
_cell_length_c                   19.7264(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1834.85(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    4.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6148
_exptl_absorpt_correction_T_max  0.7576
_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            4451
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         25.10
_reflns_number_total             2638
_reflns_number_gt                2493
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0131P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(2)
_refine_ls_number_reflns         2638
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0573
_refine_ls_wR_factor_gt          0.0548
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.71320(4) 0.46431(3) 0.592526(16) 0.01813(10) Uani 1 1 d . . .
As1 As 0.26780(7) 0.49614(5) 0.59166(3) 0.02093(15) Uani 1 1 d . . .
S1 S 0.4204(2) 0.4635(2) 0.50516(8) 0.0310(4) Uani 1 1 d . . .
S2 S 0.4163(2) 0.45861(19) 0.67907(8) 0.0297(4) Uani 1 1 d . . .
S3 S 0.06596(17) 0.37348(14) 0.58911(10) 0.0272(4) Uani 1 1 d . . .
S4 S 0.18608(19) 0.67892(13) 0.59267(9) 0.0295(4) Uani 1 1 d . . .
N1 N 0.6491(7) 0.2305(4) 0.5992(2) 0.0337(14) Uani 1 1 d . . .
H1A H 0.5418 0.2219 0.5983 0.040 Uiso 1 1 d R . .
H1B H 0.6876 0.1963 0.5612 0.040 Uiso 1 1 d R . .
N2 N 0.7959(8) 0.3505(4) 0.7063(2) 0.0256(13) Uani 1 1 d . . .
H2C H 0.8988 0.3266 0.6988 0.031 Uiso 1 1 d R . .
N3 N 0.8621(7) 0.5993(5) 0.6868(3) 0.0273(14) Uani 1 1 d . . .
H3C H 0.9525 0.6276 0.6665 0.033 Uiso 1 1 d R . .
N4 N 0.6157(6) 0.6930(4) 0.6002(3) 0.0362(14) Uani 1 1 d . . .
H4A H 0.6128 0.7237 0.5581 0.043 Uiso 1 1 d R . .
H4B H 0.5150 0.6944 0.6167 0.043 Uiso 1 1 d R . .
N5 N 0.7733(7) 0.3590(4) 0.4765(2) 0.0256(13) Uani 1 1 d . . .
H5A H 0.8630 0.3149 0.4809 0.031 Uiso 1 1 d R . .
H5B H 0.6921 0.3086 0.4669 0.031 Uiso 1 1 d R . .
N6 N 0.8601(7) 0.5994(5) 0.5019(2) 0.0281(14) Uani 1 1 d . . .
H6A H 0.7933 0.6591 0.4899 0.034 Uiso 1 1 d R . .
H6B H 0.9462 0.6330 0.5218 0.034 Uiso 1 1 d R . .
C1 C 0.7095(10) 0.1615(5) 0.6570(3) 0.0392(18) Uani 1 1 d . . .
H1C H 0.8178 0.1342 0.6477 0.047 Uiso 1 1 calc R . .
H1D H 0.6424 0.0916 0.6641 0.047 Uiso 1 1 calc R . .
C2 C 0.7089(10) 0.2383(5) 0.7197(3) 0.0343(17) Uani 1 1 d . . .
H2A H 0.5993 0.2561 0.7327 0.041 Uiso 1 1 calc R . .
H2B H 0.7598 0.1955 0.7567 0.041 Uiso 1 1 calc R . .
C3 C 0.8075(9) 0.4296(6) 0.7635(3) 0.0337(17) Uani 1 1 d . . .
H3A H 0.8472 0.3858 0.8025 0.040 Uiso 1 1 calc R . .
H3B H 0.7021 0.4608 0.7745 0.040 Uiso 1 1 calc R . .
C4 C 0.9188(8) 0.5309(7) 0.7476(3) 0.0341(17) Uani 1 1 d . . .
H4C H 1.0255 0.4997 0.7390 0.041 Uiso 1 1 calc R . .
H4D H 0.9250 0.5844 0.7862 0.041 Uiso 1 1 calc R . .
C5 C 0.7692(10) 0.7053(6) 0.7052(3) 0.042(2) Uani 1 1 d . . .
H5C H 0.8338 0.7578 0.7333 0.050 Uiso 1 1 calc R . .
H5D H 0.6755 0.6815 0.7311 0.050 Uiso 1 1 calc R . .
C6 C 0.7176(10) 0.7705(6) 0.6429(4) 0.048(2) Uani 1 1 d . . .
H6C H 0.6583 0.8419 0.6556 0.058 Uiso 1 1 calc R . .
H6D H 0.8114 0.7953 0.6174 0.058 Uiso 1 1 calc R . .
C7 C 0.9139(8) 0.5382(6) 0.4397(3) 0.0320(16) Uani 1 1 d . . .
H7A H 1.0181 0.5020 0.4473 0.038 Uiso 1 1 calc R . .
H7B H 0.9246 0.5962 0.4033 0.038 Uiso 1 1 calc R . .
C8 C 0.7942(8) 0.4424(5) 0.4194(3) 0.0299(15) Uani 1 1 d . . .
H8A H 0.6922 0.4790 0.4079 0.036 Uiso 1 1 calc R . .
H8B H 0.8331 0.3994 0.3800 0.036 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
Pr1 N5 2.621(5) . ?
Pr1 N6 2.640(5) . ?
Pr1 N1 2.666(5) . ?
Pr1 N2 2.670(5) . ?
Pr1 N4 2.682(5) . ?
Pr1 N3 2.696(5) . ?
Pr1 S1 2.9881(17) . ?
Pr1 S2 3.0071(16) . ?
Pr1 S3 3.1110(15) 1_655 ?
As1 S4 2.1505(16) . ?
As1 S1 2.1590(17) . ?
As1 S2 2.1635(17) . ?
As1 S3 2.1695(16) . ?
S3 Pr1 3.1110(15) 1_455 ?
N1 C1 1.465(7) . ?
N1 H1A 0.8997 . ?
N1 H1B 0.9003 . ?
N2 C3 1.436(7) . ?
N2 C2 1.471(8) . ?
N2 H2C 0.9104 . ?
N3 C5 1.460(8) . ?
N3 C4 1.497(8) . ?
N3 H3C 0.9099 . ?
N4 C6 1.477(7) . ?
N4 H4A 0.8987 . ?
N4 H4B 0.9004 . ?
N5 C8 1.472(6) . ?
N5 H5A 0.8994 . ?
N5 H5B 0.9002 . ?
N6 C7 1.475(7) . ?
N6 H6A 0.8999 . ?
N6 H6B 0.8999 . ?
C1 C2 1.504(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.496(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.492(8) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.516(8) . ?
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
N5 Pr1 N6 64.91(15) . . ?
N5 Pr1 N1 69.07(15) . . ?
N6 Pr1 N1 133.26(16) . . ?
N5 Pr1 N2 118.13(14) . . ?
N6 Pr1 N2 136.16(18) . . ?
N1 Pr1 N2 62.91(16) . . ?
N5 Pr1 N4 122.26(17) . . ?
N6 Pr1 N4 68.62(17) . . ?
N1 Pr1 N4 150.15(16) . . ?
N2 Pr1 N4 118.91(17) . . ?
N5 Pr1 N3 139.88(17) . . ?
N6 Pr1 N3 86.24(15) . . ?
N1 Pr1 N3 127.22(15) . . ?
N2 Pr1 N3 64.34(15) . . ?
N4 Pr1 N3 64.47(16) . . ?
N5 Pr1 S1 69.59(13) . . ?
N6 Pr1 S1 89.43(12) . . ?
N1 Pr1 S1 82.06(12) . . ?
N2 Pr1 S1 133.99(14) . . ?
N4 Pr1 S1 77.76(12) . . ?
N3 Pr1 S1 140.87(12) . . ?
N5 Pr1 S2 130.06(13) . . ?
N6 Pr1 S2 141.11(12) . . ?
N1 Pr1 S2 77.66(13) . . ?
N2 Pr1 S2 74.05(14) . . ?
N4 Pr1 S2 74.86(13) . . ?
N3 Pr1 S2 89.95(12) . . ?
S1 Pr1 S2 69.83(4) . . ?
N5 Pr1 S3 69.77(13) . 1_655 ?
N6 Pr1 S3 74.51(12) . 1_655 ?
N1 Pr1 S3 82.63(12) . 1_655 ?
N2 Pr1 S3 67.61(14) . 1_655 ?
N4 Pr1 S3 126.69(12) . 1_655 ?
N3 Pr1 S3 76.22(12) . 1_655 ?
S1 Pr1 S3 139.34(5) . 1_655 ?
S2 Pr1 S3 141.56(5) . 1_655 ?
S4 As1 S1 110.73(8) . . ?
S4 As1 S2 110.94(8) . . ?
S1 As1 S2 105.09(6) . . ?
S4 As1 S3 110.67(6) . . ?
S1 As1 S3 109.39(8) . . ?
S2 As1 S3 109.88(8) . . ?
As1 S1 Pr1 91.42(5) . . ?
As1 S2 Pr1 90.82(6) . . ?
As1 S3 Pr1 121.80(6) . 1_455 ?
C1 N1 Pr1 119.0(4) . . ?
C1 N1 H1A 107.5 . . ?
Pr1 N1 H1A 107.6 . . ?
C1 N1 H1B 107.6 . . ?
Pr1 N1 H1B 107.6 . . ?
H1A N1 H1B 107.0 . . ?
C3 N2 C2 114.6(5) . . ?
C3 N2 Pr1 112.7(3) . . ?
C2 N2 Pr1 115.3(4) . . ?
C3 N2 H2C 104.2 . . ?
C2 N2 H2C 104.1 . . ?
Pr1 N2 H2C 104.2 . . ?
C5 N3 C4 112.4(5) . . ?
C5 N3 Pr1 112.3(4) . . ?
C4 N3 Pr1 114.4(4) . . ?
C5 N3 H3C 105.5 . . ?
C4 N3 H3C 105.5 . . ?
Pr1 N3 H3C 105.8 . . ?
C6 N4 Pr1 114.6(4) . . ?
C6 N4 H4A 108.6 . . ?
Pr1 N4 H4A 108.6 . . ?
C6 N4 H4B 108.7 . . ?
Pr1 N4 H4B 108.6 . . ?
H4A N4 H4B 107.6 . . ?
C8 N5 Pr1 114.1(3) . . ?
C8 N5 H5A 108.7 . . ?
Pr1 N5 H5A 108.7 . . ?
C8 N5 H5B 108.9 . . ?
Pr1 N5 H5B 108.7 . . ?
H5A N5 H5B 107.7 . . ?
C7 N6 Pr1 116.1(4) . . ?
C7 N6 H6A 108.2 . . ?
Pr1 N6 H6A 108.3 . . ?
C7 N6 H6B 108.3 . . ?
Pr1 N6 H6B 108.2 . . ?
H6A N6 H6B 107.4 . . ?
N1 C1 C2 109.8(5) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N2 C2 C1 109.7(5) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 110.0(5) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 N3 111.0(5) . . ?
C3 C4 H4C 109.4 . . ?
N3 C4 H4C 109.4 . . ?
C3 C4 H4D 109.4 . . ?
N3 C4 H4D 109.4 . . ?
H4C C4 H4D 108.0 . . ?
N3 C5 C6 110.1(5) . . ?
N3 C5 H5C 109.6 . . ?
C6 C5 H5C 109.6 . . ?
N3 C5 H5D 109.6 . . ?
C6 C5 H5D 109.6 . . ?
H5C C5 H5D 108.2 . . ?
N4 C6 C5 110.5(5) . . ?
N4 C6 H6C 109.6 . . ?
C5 C6 H6C 109.6 . . ?
N4 C6 H6D 109.6 . . ?
C5 C6 H6D 109.6 . . ?
H6C C6 H6D 108.1 . . ?
N6 C7 C8 110.3(5) . . ?
N6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
N6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N5 C8 C7 108.8(5) . . ?
N5 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
N5 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.120
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033476'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As N6 Nd S4'
_chemical_formula_sum            'C8 H26 As N6 Nd S4'
_chemical_formula_weight         553.75

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'
Nd Nd -0.1943 3.0179 '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   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_chemical_absolute_configuration unk

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'

_cell_length_a                   8.491(10)
_cell_length_b                   11.211(13)
_cell_length_c                   19.69(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1874(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    4.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5431
_exptl_absorpt_correction_T_max  0.6634
_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            7881
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.60
_diffrn_reflns_theta_max         26.49
_reflns_number_total             3620
_reflns_number_gt                3518
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0361P)²+0.6583P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.111(15)
_refine_ls_number_reflns         3620
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0688
_refine_ls_wR_factor_gt          0.0682
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.000
_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 0.21279(2) 0.535966(19) 0.407308(11) 0.01806(8) Uani 1 1 d . . .
As1 As -0.23229(4) 0.50378(4) 0.40829(2) 0.02136(11) Uani 1 1 d . . .
S1 S -0.07860(13) 0.53774(15) 0.49468(6) 0.0310(3) Uani 1 1 d . . .
S2 S -0.08324(13) 0.54151(14) 0.32075(6) 0.0303(3) Uani 1 1 d . . .
S3 S -0.43469(11) 0.62638(10) 0.41089(7) 0.0272(2) Uani 1 1 d . . .
S4 S -0.31347(13) 0.32071(10) 0.40743(7) 0.0293(2) Uani 1 1 d . . .
N1 N 0.1466(6) 0.7687(4) 0.4007(2) 0.0332(9) Uani 1 1 d . . .
H1A H 0.0411 0.7762 0.4007 0.040 Uiso 1 1 d R . .
H1B H 0.1822 0.8029 0.4391 0.040 Uiso 1 1 d R . .
N2 N 0.2959(6) 0.6500(4) 0.29398(17) 0.0269(9) Uani 1 1 d . . .
H2C H 0.3964 0.6745 0.3020 0.032 Uiso 1 1 d R . .
N3 N 0.3629(5) 0.4012(4) 0.3141(2) 0.0285(9) Uani 1 1 d . . .
H3C H 0.4505 0.3726 0.3351 0.034 Uiso 1 1 d R . .
N4 N 0.1151(5) 0.3089(4) 0.3997(2) 0.0336(9) Uani 1 1 d . . .
H4A H 0.1109 0.2787 0.4420 0.040 Uiso 1 1 d R . .
H4B H 0.0167 0.3079 0.3827 0.040 Uiso 1 1 d R . .
N5 N 0.3592(5) 0.4013(4) 0.4975(2) 0.0281(9) Uani 1 1 d . . .
H5A H 0.2938 0.3417 0.5094 0.034 Uiso 1 1 d R . .
H5B H 0.4432 0.3679 0.4771 0.034 Uiso 1 1 d R . .
N6 N 0.2723(5) 0.6405(3) 0.52275(17) 0.0235(8) Uani 1 1 d . . .
H6A H 0.3597 0.6852 0.5182 0.028 Uiso 1 1 d R . .
H6B H 0.1920 0.6900 0.5327 0.028 Uiso 1 1 d R . .
C1 C 0.2083(8) 0.8377(4) 0.3430(2) 0.0366(11) Uani 1 1 d . . .
H1C H 0.3146 0.8642 0.3528 0.044 Uiso 1 1 calc R . .
H1D H 0.1432 0.9076 0.3356 0.044 Uiso 1 1 calc R . .
C2 C 0.2084(7) 0.7623(5) 0.2812(2) 0.0343(11) Uani 1 1 d . . .
H2A H 0.2574 0.8054 0.2441 0.041 Uiso 1 1 calc R . .
H2B H 0.1009 0.7440 0.2683 0.041 Uiso 1 1 calc R . .
C3 C 0.3099(7) 0.5695(5) 0.2363(2) 0.0379(12) Uani 1 1 d . . .
H3A H 0.3503 0.6128 0.1973 0.045 Uiso 1 1 calc R . .
H3B H 0.2069 0.5382 0.2245 0.045 Uiso 1 1 calc R . .
C4 C 0.4201(6) 0.4674(6) 0.2535(2) 0.0325(11) Uani 1 1 d . . .
H4C H 0.4269 0.4134 0.2151 0.039 Uiso 1 1 calc R . .
H4D H 0.5247 0.4985 0.2624 0.039 Uiso 1 1 calc R . .
C5 C 0.2693(8) 0.2947(5) 0.2951(3) 0.0453(15) Uani 1 1 d . . .
H5C H 0.3327 0.2417 0.2674 0.054 Uiso 1 1 calc R . .
H5D H 0.1783 0.3189 0.2687 0.054 Uiso 1 1 calc R . .
C6 C 0.2156(8) 0.2299(5) 0.3584(3) 0.0437(13) Uani 1 1 d . . .
H6C H 0.1571 0.1590 0.3458 0.052 Uiso 1 1 calc R . .
H6D H 0.3066 0.2054 0.3847 0.052 Uiso 1 1 calc R . .
C7 C 0.4133(6) 0.4611(5) 0.5600(2) 0.0315(10) Uani 1 1 d . . .
H7A H 0.5158 0.4970 0.5524 0.038 Uiso 1 1 calc R . .
H7B H 0.4230 0.4034 0.5964 0.038 Uiso 1 1 calc R . .
C8 C 0.2940(6) 0.5576(4) 0.5798(2) 0.0291(10) Uani 1 1 d . . .
H8A H 0.1941 0.5209 0.5914 0.035 Uiso 1 1 calc R . .
H8B H 0.3318 0.6008 0.6192 0.035 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
Nd1 N6 2.607(4) . ?
Nd1 N5 2.642(4) . ?
Nd1 N2 2.667(4) . ?
Nd1 N1 2.673(5) . ?
Nd1 N4 2.681(5) . ?
Nd1 N3 2.697(4) . ?
Nd1 S1 3.014(3) . ?
Nd1 S2 3.038(3) . ?
Nd1 S3 3.161(4) 1_655 ?
As1 S4 2.165(3) . ?
As1 S1 2.178(2) . ?
As1 S2 2.180(2) . ?
As1 S3 2.201(2) . ?
S3 Nd1 3.161(4) 1_455 ?
N1 C1 1.472(6) . ?
N1 H1A 0.8997 . ?
N1 H1B 0.9000 . ?
N2 C3 1.456(6) . ?
N2 C2 1.483(7) . ?
N2 H2C 0.9102 . ?
N3 C5 1.482(7) . ?
N3 C4 1.487(6) . ?
N3 H3C 0.9094 . ?
N4 C6 1.475(7) . ?
N4 H4A 0.8998 . ?
N4 H4B 0.9001 . ?
N5 C7 1.474(6) . ?
N5 H5A 0.8999 . ?
N5 H5B 0.9002 . ?
N6 C8 1.469(6) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9005 . ?
C1 C2 1.481(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.517(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.512(8) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.532(7) . ?
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
N6 Nd1 N5 65.13(14) . . ?
N6 Nd1 N2 117.57(14) . . ?
N5 Nd1 N2 135.41(14) . . ?
N6 Nd1 N1 69.15(13) . . ?
N5 Nd1 N1 133.60(13) . . ?
N2 Nd1 N1 63.06(13) . . ?
N6 Nd1 N4 122.37(13) . . ?
N5 Nd1 N4 68.93(14) . . ?
N2 Nd1 N4 119.36(13) . . ?
N1 Nd1 N4 149.22(14) . . ?
N6 Nd1 N3 138.89(14) . . ?
N5 Nd1 N3 85.12(14) . . ?
N2 Nd1 N3 64.80(14) . . ?
N1 Nd1 N3 127.83(13) . . ?
N4 Nd1 N3 64.94(14) . . ?
N6 Nd1 S1 70.03(11) . . ?
N5 Nd1 S1 90.35(12) . . ?
N2 Nd1 S1 133.77(11) . . ?
N1 Nd1 S1 81.30(10) . . ?
N4 Nd1 S1 77.53(10) . . ?
N3 Nd1 S1 141.26(10) . . ?
N6 Nd1 S2 129.83(10) . . ?
N5 Nd1 S2 141.10(10) . . ?
N2 Nd1 S2 74.90(12) . . ?
N1 Nd1 S2 77.22(11) . . ?
N4 Nd1 S2 74.46(10) . . ?
N3 Nd1 S2 91.19(12) . . ?
S1 Nd1 S2 68.95(9) . . ?
N6 Nd1 S3 69.68(10) . 1_655 ?
N5 Nd1 S3 73.91(11) . 1_655 ?
N2 Nd1 S3 67.33(11) . 1_655 ?
N1 Nd1 S3 83.52(12) . 1_655 ?
N4 Nd1 S3 126.78(9) . 1_655 ?
N3 Nd1 S3 75.37(11) . 1_655 ?
S1 Nd1 S3 139.69(6) . 1_655 ?
S2 Nd1 S3 142.15(6) . 1_655 ?
S4 As1 S1 111.26(6) . . ?
S4 As1 S2 111.26(6) . . ?
S1 As1 S2 103.64(9) . . ?
S4 As1 S3 110.09(9) . . ?
S1 As1 S3 109.91(8) . . ?
S2 As1 S3 110.52(8) . . ?
As1 S1 Nd1 92.57(9) . . ?
As1 S2 Nd1 91.88(9) . . ?
As1 S3 Nd1 122.58(9) . 1_455 ?
C1 N1 Nd1 118.4(3) . . ?
C1 N1 H1A 107.8 . . ?
Nd1 N1 H1A 107.5 . . ?
C1 N1 H1B 107.8 . . ?
Nd1 N1 H1B 107.7 . . ?
H1A N1 H1B 107.1 . . ?
C3 N2 C2 115.8(4) . . ?
C3 N2 Nd1 112.2(3) . . ?
C2 N2 Nd1 114.6(3) . . ?
C3 N2 H2C 104.2 . . ?
C2 N2 H2C 104.0 . . ?
Nd1 N2 H2C 104.3 . . ?
C5 N3 C4 112.0(4) . . ?
C5 N3 Nd1 111.7(3) . . ?
C4 N3 Nd1 114.9(3) . . ?
C5 N3 H3C 105.6 . . ?
C4 N3 H3C 105.9 . . ?
Nd1 N3 H3C 105.9 . . ?
C6 N4 Nd1 114.9(3) . . ?
C6 N4 H4A 107.9 . . ?
Nd1 N4 H4A 108.5 . . ?
C6 N4 H4B 108.9 . . ?
Nd1 N4 H4B 108.7 . . ?
H4A N4 H4B 107.6 . . ?
C7 N5 Nd1 116.6(3) . . ?
C7 N5 H5A 108.2 . . ?
Nd1 N5 H5A 108.0 . . ?
C7 N5 H5B 108.3 . . ?
Nd1 N5 H5B 108.1 . . ?
H5A N5 H5B 107.2 . . ?
C8 N6 Nd1 114.0(3) . . ?
C8 N6 H6A 109.0 . . ?
Nd1 N6 H6A 108.8 . . ?
C8 N6 H6B 108.6 . . ?
Nd1 N6 H6B 108.6 . . ?
H6A N6 H6B 107.6 . . ?
N1 C1 C2 109.5(4) . . ?
N1 C1 H1C 109.8 . . ?
C2 C1 H1C 109.8 . . ?
N1 C1 H1D 109.8 . . ?
C2 C1 H1D 109.8 . . ?
H1C C1 H1D 108.2 . . ?
C1 C2 N2 110.2(4) . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
N2 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 110.1(4) . . ?
N2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 110.8(4) . . ?
N3 C4 H4C 109.5 . . ?
C3 C4 H4C 109.5 . . ?
N3 C4 H4D 109.5 . . ?
C3 C4 H4D 109.5 . . ?
H4C C4 H4D 108.1 . . ?
N3 C5 C6 109.9(4) . . ?
N3 C5 H5C 109.7 . . ?
C6 C5 H5C 109.7 . . ?
N3 C5 H5D 109.7 . . ?
C6 C5 H5D 109.7 . . ?
H5C C5 H5D 108.2 . . ?
N4 C6 C5 109.9(5) . . ?
N4 C6 H6C 109.7 . . ?
C5 C6 H6C 109.7 . . ?
N4 C6 H6D 109.7 . . ?
C5 C6 H6D 109.7 . . ?
H6C C6 H6D 108.2 . . ?
N5 C7 C8 109.1(4) . . ?
N5 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N5 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N6 C8 C7 109.6(4) . . ?
N6 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N6 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        26.49
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.173
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033477'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As Dy N6 S4'
_chemical_formula_sum            'C8 H26 As Dy N6 S4'
_chemical_formula_weight         572.01

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'
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'
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'

_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                   9.6438(5)
_cell_length_b                   13.1563(7)
_cell_length_c                   14.5845(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4360(10)
_cell_angle_gamma                90.00
_cell_volume                     1834.87(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_absorpt_coefficient_mu    6.316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1593
_exptl_absorpt_correction_T_max  0.2877
_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            13540
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3680
_reflns_number_gt                3285
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0458P)²+3.0069P] 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         3680
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_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 0.338151(19) 0.482800(15) 0.715531(13) 0.01690(9) Uani 1 1 d . . .
As1 As 0.71326(5) 0.51682(3) 0.74032(3) 0.02090(12) Uani 1 1 d . . .
S1 S 0.59173(11) 0.38563(9) 0.68531(9) 0.0274(3) Uani 1 1 d . . .
S2 S 0.55713(12) 0.60249(10) 0.80447(9) 0.0300(3) Uani 1 1 d . . .
S3 S 0.88161(14) 0.47403(11) 0.84112(10) 0.0350(3) Uani 1 1 d . . .
S4 S 0.77466(14) 0.60373(10) 0.62660(9) 0.0337(3) Uani 1 1 d . . .
N1 N 0.3648(5) 0.5626(3) 0.5633(3) 0.0333(10) Uani 1 1 d . . .
H1A H 0.4547 0.5563 0.5535 0.040 Uiso 1 1 calc R . .
H1B H 0.3125 0.5272 0.5186 0.040 Uiso 1 1 calc R . .
N2 N 0.2497(4) 0.6634(3) 0.7049(3) 0.0233(8) Uani 1 1 d . . .
H2C H 0.3262 0.7019 0.7244 0.028 Uiso 1 1 calc R . .
N3 N 0.2241(4) 0.5344(3) 0.8541(3) 0.0243(8) Uani 1 1 d . . .
H3C H 0.1364 0.5076 0.8449 0.029 Uiso 1 1 calc R . .
N4 N 0.3649(5) 0.3511(3) 0.8414(3) 0.0380(11) Uani 1 1 d . . .
H4A H 0.3295 0.2922 0.8174 0.046 Uiso 1 1 calc R . .
H4B H 0.4568 0.3414 0.8591 0.046 Uiso 1 1 calc R . .
N5 N 0.0795(4) 0.4555(4) 0.6668(3) 0.0315(9) Uani 1 1 d . . .
H5A H 0.0405 0.4351 0.7165 0.038 Uiso 1 1 calc R . .
H5B H 0.0407 0.5155 0.6485 0.038 Uiso 1 1 calc R . .
N6 N 0.2855(4) 0.3259(3) 0.6165(3) 0.0254(8) Uani 1 1 d . . .
H6A H 0.3063 0.3392 0.5593 0.030 Uiso 1 1 calc R . .
H6B H 0.3418 0.2753 0.6401 0.030 Uiso 1 1 calc R . .
C1 C 0.3256(6) 0.6703(4) 0.5531(4) 0.0369(12) Uani 1 1 d . . .
H1C H 0.2967 0.6854 0.4883 0.044 Uiso 1 1 calc R . .
H1D H 0.4061 0.7123 0.5742 0.044 Uiso 1 1 calc R . .
C2 C 0.2076(6) 0.6955(4) 0.6084(3) 0.0324(11) Uani 1 1 d . . .
H2A H 0.1891 0.7680 0.6059 0.039 Uiso 1 1 calc R . .
H2B H 0.1231 0.6601 0.5828 0.039 Uiso 1 1 calc R . .
C3 C 0.1498(5) 0.6883(4) 0.7685(4) 0.0294(11) Uani 1 1 d . . .
H3A H 0.0592 0.6588 0.7469 0.035 Uiso 1 1 calc R . .
H3B H 0.1390 0.7614 0.7724 0.035 Uiso 1 1 calc R . .
C4 C 0.2049(5) 0.6458(4) 0.8619(4) 0.0309(11) Uani 1 1 d . . .
H4C H 0.2935 0.6776 0.8844 0.037 Uiso 1 1 calc R . .
H4D H 0.1396 0.6600 0.9055 0.037 Uiso 1 1 calc R . .
C5 C 0.2925(7) 0.4883(4) 0.9405(4) 0.0409(14) Uani 1 1 d . . .
H5C H 0.2397 0.5032 0.9912 0.049 Uiso 1 1 calc R . .
H5D H 0.3863 0.5152 0.9558 0.049 Uiso 1 1 calc R . .
C6 C 0.2980(7) 0.3740(5) 0.9249(4) 0.0450(14) Uani 1 1 d . . .
H6C H 0.3505 0.3418 0.9783 0.054 Uiso 1 1 calc R . .
H6D H 0.2039 0.3465 0.9175 0.054 Uiso 1 1 calc R . .
C7 C 0.0441(5) 0.3816(4) 0.5927(4) 0.0314(11) Uani 1 1 d . . .
H7A H 0.0547 0.4123 0.5336 0.038 Uiso 1 1 calc R . .
H7B H -0.0525 0.3604 0.5914 0.038 Uiso 1 1 calc R . .
C8 C 0.1395(5) 0.2907(4) 0.6091(4) 0.0384(13) Uani 1 1 d . . .
H8A H 0.1233 0.2564 0.6657 0.046 Uiso 1 1 calc R . .
H8B H 0.1207 0.2430 0.5583 0.046 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
Dy1 N1 2.499(4) . ?
Dy1 N4 2.513(4) . ?
Dy1 N3 2.517(4) . ?
Dy1 N2 2.523(4) . ?
Dy1 N5 2.529(4) . ?
Dy1 N6 2.532(4) . ?
Dy1 S2 2.8129(12) . ?
Dy1 S1 2.8439(11) . ?
As1 S3 2.1204(14) . ?
As1 S4 2.1594(13) . ?
As1 S1 2.1800(12) . ?
As1 S2 2.1858(12) . ?
N1 C1 1.470(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.459(6) . ?
N2 C2 1.475(6) . ?
N2 H2C 0.9100 . ?
N3 C5 1.475(7) . ?
N3 C4 1.483(6) . ?
N3 H3C 0.9100 . ?
N4 C6 1.480(7) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.461(6) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.473(6) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.514(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.504(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.523(8) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.509(7) . ?
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
N1 Dy1 N4 157.80(14) . . ?
N1 Dy1 N3 134.94(14) . . ?
N4 Dy1 N3 67.25(14) . . ?
N1 Dy1 N2 67.83(13) . . ?
N4 Dy1 N2 134.13(14) . . ?
N3 Dy1 N2 67.41(13) . . ?
N1 Dy1 N5 91.21(16) . . ?
N4 Dy1 N5 96.40(16) . . ?
N3 Dy1 N5 75.32(14) . . ?
N2 Dy1 N5 78.67(14) . . ?
N1 Dy1 N6 82.62(14) . . ?
N4 Dy1 N6 81.31(15) . . ?
N3 Dy1 N6 126.99(13) . . ?
N2 Dy1 N6 133.73(12) . . ?
N5 Dy1 N6 66.79(13) . . ?
N1 Dy1 S2 90.99(11) . . ?
N4 Dy1 S2 92.81(12) . . ?
N3 Dy1 S2 81.86(9) . . ?
N2 Dy1 S2 74.26(9) . . ?
N5 Dy1 S2 149.70(10) . . ?
N6 Dy1 S2 143.36(9) . . ?
N1 Dy1 S1 82.05(11) . . ?
N4 Dy1 S1 78.13(11) . . ?
N3 Dy1 S1 136.03(10) . . ?
N2 Dy1 S1 134.79(9) . . ?
N5 Dy1 S1 136.80(10) . . ?
N6 Dy1 S1 70.03(9) . . ?
S2 Dy1 S1 73.37(3) . . ?
S3 As1 S4 114.30(6) . . ?
S3 As1 S1 111.83(5) . . ?
S4 As1 S1 108.93(6) . . ?
S3 As1 S2 110.38(6) . . ?
S4 As1 S2 109.16(6) . . ?
S1 As1 S2 101.45(5) . . ?
As1 S1 Dy1 91.10(4) . . ?
As1 S2 Dy1 91.81(4) . . ?
C1 N1 Dy1 116.1(3) . . ?
C1 N1 H1A 108.3 . . ?
Dy1 N1 H1A 108.3 . . ?
C1 N1 H1B 108.3 . . ?
Dy1 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C3 N2 C2 114.8(4) . . ?
C3 N2 Dy1 114.7(3) . . ?
C2 N2 Dy1 112.2(3) . . ?
C3 N2 H2C 104.6 . . ?
C2 N2 H2C 104.6 . . ?
Dy1 N2 H2C 104.6 . . ?
C5 N3 C4 112.8(4) . . ?
C5 N3 Dy1 112.4(3) . . ?
C4 N3 Dy1 113.6(3) . . ?
C5 N3 H3C 105.7 . . ?
C4 N3 H3C 105.7 . . ?
Dy1 N3 H3C 105.7 . . ?
C6 N4 Dy1 116.5(3) . . ?
C6 N4 H4A 108.2 . . ?
Dy1 N4 H4A 108.2 . . ?
C6 N4 H4B 108.2 . . ?
Dy1 N4 H4B 108.2 . . ?
H4A N4 H4B 107.3 . . ?
C7 N5 Dy1 115.5(3) . . ?
C7 N5 H5A 108.4 . . ?
Dy1 N5 H5A 108.4 . . ?
C7 N5 H5B 108.4 . . ?
Dy1 N5 H5B 108.4 . . ?
H5A N5 H5B 107.5 . . ?
C8 N6 Dy1 114.7(3) . . ?
C8 N6 H6A 108.6 . . ?
Dy1 N6 H6A 108.6 . . ?
C8 N6 H6B 108.6 . . ?
Dy1 N6 H6B 108.6 . . ?
H6A N6 H6B 107.6 . . ?
N1 C1 C2 111.0(4) . . ?
N1 C1 H1C 109.4 . . ?
C2 C1 H1C 109.4 . . ?
N1 C1 H1D 109.4 . . ?
C2 C1 H1D 109.4 . . ?
H1C C1 H1D 108.0 . . ?
N2 C2 C1 108.2(4) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 107.9(4) . . ?
N2 C3 H3A 110.1 . . ?
C4 C3 H3A 110.1 . . ?
N2 C3 H3B 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
N3 C4 C3 109.4(4) . . ?
N3 C4 H4C 109.8 . . ?
C3 C4 H4C 109.8 . . ?
N3 C4 H4D 109.8 . . ?
C3 C4 H4D 109.8 . . ?
H4C C4 H4D 108.3 . . ?
N3 C5 C6 107.4(5) . . ?
N3 C5 H5C 110.2 . . ?
C6 C5 H5C 110.2 . . ?
N3 C5 H5D 110.2 . . ?
C6 C5 H5D 110.2 . . ?
H5C C5 H5D 108.5 . . ?
N4 C6 C5 110.5(5) . . ?
N4 C6 H6C 109.5 . . ?
C5 C6 H6C 109.5 . . ?
N4 C6 H6D 109.5 . . ?
C5 C6 H6D 109.5 . . ?
H6C C6 H6D 108.1 . . ?
N5 C7 C8 109.3(4) . . ?
N5 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N5 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
N6 C8 C7 108.6(4) . . ?
N6 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
N6 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.173
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033478'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As Ho N6 S4'
_chemical_formula_sum            'C8 H26 As Ho N6 S4'
_chemical_formula_weight         574.44

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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                   9.5522(14)
_cell_length_b                   13.0616(18)
_cell_length_c                   14.483(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.604(2)
_cell_angle_gamma                90.00
_cell_volume                     1791.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_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    2.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    6.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2443
_exptl_absorpt_correction_T_max  0.3436
_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            10397
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3135
_reflns_number_gt                2815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0285P)²+3.6797P] 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         3135
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0639
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_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 0.33785(2) 0.517801(14) 0.715884(13) 0.01113(8) Uani 1 1 d . . .
As1 As 0.71535(5) 0.48433(3) 0.74142(3) 0.01431(12) Uani 1 1 d . . .
S3 S 0.88329(14) 0.52704(10) 0.84214(10) 0.0281(3) Uani 1 1 d . . .
S2 S 0.55721(11) 0.39846(8) 0.80591(8) 0.0171(2) Uani 1 1 d . . .
S1 S 0.59178(11) 0.61594(8) 0.68579(8) 0.0160(2) Uani 1 1 d . . .
S4 S 0.77386(12) 0.39581(8) 0.62596(8) 0.0175(2) Uani 1 1 d . . .
N5 N 0.0784(4) 0.5435(3) 0.6678(3) 0.0193(8) Uani 1 1 d . . .
H5A H 0.0395 0.4828 0.6497 0.023 Uiso 1 1 calc R . .
H5B H 0.0393 0.5643 0.7178 0.023 Uiso 1 1 calc R . .
N6 N 0.2847(4) 0.6737(3) 0.6163(3) 0.0157(8) Uani 1 1 d . . .
H6A H 0.3419 0.7247 0.6397 0.019 Uiso 1 1 calc R . .
H6B H 0.3053 0.6599 0.5587 0.019 Uiso 1 1 calc R . .
N3 N 0.2236(4) 0.4661(3) 0.8549(3) 0.0157(8) Uani 1 1 d . . .
H3C H 0.1351 0.4933 0.8458 0.019 Uiso 1 1 calc R . .
N1 N 0.3663(4) 0.4392(3) 0.5636(3) 0.0172(8) Uani 1 1 d . . .
H1A H 0.3137 0.4749 0.5185 0.021 Uiso 1 1 calc R . .
H1B H 0.4572 0.4457 0.5544 0.021 Uiso 1 1 calc R . .
N2 N 0.2497(4) 0.3366(3) 0.7048(2) 0.0149(8) Uani 1 1 d . . .
H2C H 0.3269 0.2979 0.7248 0.018 Uiso 1 1 calc R . .
N4 N 0.3648(4) 0.6498(3) 0.8411(3) 0.0198(8) Uani 1 1 d . . .
H4A H 0.4578 0.6602 0.8583 0.024 Uiso 1 1 calc R . .
H4B H 0.3283 0.7089 0.8166 0.024 Uiso 1 1 calc R . .
C5 C 0.2945(5) 0.5137(3) 0.9408(3) 0.0217(10) Uani 1 1 d . . .
H5C H 0.3896 0.4869 0.9551 0.026 Uiso 1 1 calc R . .
H5D H 0.2431 0.4984 0.9925 0.026 Uiso 1 1 calc R . .
C3 C 0.1477(5) 0.3117(3) 0.7688(3) 0.0175(10) Uani 1 1 d . . .
H3A H 0.1367 0.2381 0.7730 0.021 Uiso 1 1 calc R . .
H3B H 0.0563 0.3414 0.7467 0.021 Uiso 1 1 calc R . .
C8 C 0.1373(5) 0.7098(3) 0.6086(3) 0.0192(10) Uani 1 1 d . . .
H8A H 0.1183 0.7577 0.5573 0.023 Uiso 1 1 calc R . .
H8B H 0.1210 0.7443 0.6655 0.023 Uiso 1 1 calc R . .
C2 C 0.2076(5) 0.3046(3) 0.6073(3) 0.0213(10) Uani 1 1 d . . .
H2A H 0.1226 0.3405 0.5812 0.026 Uiso 1 1 calc R . .
H2B H 0.1886 0.2316 0.6046 0.026 Uiso 1 1 calc R . .
C4 C 0.2043(5) 0.3553(3) 0.8632(3) 0.0176(10) Uani 1 1 d . . .
H4C H 0.1386 0.3414 0.9073 0.021 Uiso 1 1 calc R . .
H4D H 0.2939 0.3233 0.8861 0.021 Uiso 1 1 calc R . .
C6 C 0.2993(6) 0.6279(4) 0.9260(3) 0.0239(11) Uani 1 1 d . . .
H6C H 0.2043 0.6557 0.9193 0.029 Uiso 1 1 calc R . .
H6D H 0.3538 0.6601 0.9794 0.029 Uiso 1 1 calc R . .
C7 C 0.0415(5) 0.6179(3) 0.5920(3) 0.0164(9) Uani 1 1 d . . .
H7A H -0.0562 0.6389 0.5903 0.020 Uiso 1 1 calc R . .
H7B H 0.0526 0.5867 0.5326 0.020 Uiso 1 1 calc R . .
C1 C 0.3266(5) 0.3296(3) 0.5530(3) 0.0200(10) Uani 1 1 d . . .
H1C H 0.4077 0.2873 0.5749 0.024 Uiso 1 1 calc R . .
H1D H 0.2982 0.3144 0.4877 0.024 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 N1 2.480(4) . ?
Ho1 N4 2.491(4) . ?
Ho1 N5 2.507(4) . ?
Ho1 N3 2.507(4) . ?
Ho1 N6 2.508(4) . ?
Ho1 N2 2.510(4) . ?
Ho1 S2 2.7924(11) . ?
Ho1 S1 2.8278(11) . ?
As1 S3 2.0960(14) . ?
As1 S4 2.1663(12) . ?
As1 S1 2.1785(12) . ?
As1 S2 2.1876(12) . ?
N5 C7 1.472(5) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.475(6) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N3 C4 1.465(6) . ?
N3 C5 1.472(6) . ?
N3 H3C 0.9100 . ?
N1 C1 1.484(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.468(5) . ?
N2 C2 1.477(6) . ?
N2 H2C 0.9100 . ?
N4 C6 1.479(6) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
C5 C6 1.509(7) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C3 C4 1.514(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C8 C7 1.510(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 C1 1.500(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 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
N1 Ho1 N4 157.08(12) . . ?
N1 Ho1 N5 91.66(13) . . ?
N4 Ho1 N5 96.48(13) . . ?
N1 Ho1 N3 135.50(12) . . ?
N4 Ho1 N3 67.41(12) . . ?
N5 Ho1 N3 74.93(12) . . ?
N1 Ho1 N6 82.10(12) . . ?
N4 Ho1 N6 81.38(12) . . ?
N5 Ho1 N6 67.28(12) . . ?
N3 Ho1 N6 127.17(12) . . ?
N1 Ho1 N2 68.16(12) . . ?
N4 Ho1 N2 134.49(12) . . ?
N5 Ho1 N2 78.32(12) . . ?
N3 Ho1 N2 67.61(12) . . ?
N6 Ho1 N2 133.47(12) . . ?
N1 Ho1 S2 91.16(9) . . ?
N4 Ho1 S2 92.73(9) . . ?
N5 Ho1 S2 149.08(9) . . ?
N3 Ho1 S2 81.61(9) . . ?
N6 Ho1 S2 143.52(8) . . ?
N2 Ho1 S2 74.23(8) . . ?
N1 Ho1 S1 81.58(9) . . ?
N4 Ho1 S1 77.89(10) . . ?
N5 Ho1 S1 137.14(9) . . ?
N3 Ho1 S1 136.01(9) . . ?
N6 Ho1 S1 69.87(8) . . ?
N2 Ho1 S1 134.83(9) . . ?
S2 Ho1 S1 73.68(3) . . ?
S3 As1 S4 115.30(5) . . ?
S3 As1 S1 112.01(5) . . ?
S4 As1 S1 108.55(5) . . ?
S3 As1 S2 110.34(5) . . ?
S4 As1 S2 108.61(5) . . ?
S1 As1 S2 101.04(5) . . ?
As1 S2 Ho1 91.85(4) . . ?
As1 S1 Ho1 91.10(4) . . ?
C7 N5 Ho1 115.2(3) . . ?
C7 N5 H5A 108.5 . . ?
Ho1 N5 H5A 108.5 . . ?
C7 N5 H5B 108.5 . . ?
Ho1 N5 H5B 108.5 . . ?
H5A N5 H5B 107.5 . . ?
C8 N6 Ho1 114.9(3) . . ?
C8 N6 H6A 108.5 . . ?
Ho1 N6 H6A 108.5 . . ?
C8 N6 H6B 108.5 . . ?
Ho1 N6 H6B 108.5 . . ?
H6A N6 H6B 107.5 . . ?
C4 N3 C5 113.4(3) . . ?
C4 N3 Ho1 113.9(3) . . ?
C5 N3 Ho1 111.3(3) . . ?
C4 N3 H3C 105.8 . . ?
C5 N3 H3C 105.8 . . ?
Ho1 N3 H3C 105.8 . . ?
C1 N1 Ho1 115.8(3) . . ?
C1 N1 H1A 108.3 . . ?
Ho1 N1 H1A 108.3 . . ?
C1 N1 H1B 108.3 . . ?
Ho1 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C3 N2 C2 115.0(3) . . ?
C3 N2 Ho1 114.5(3) . . ?
C2 N2 Ho1 112.0(3) . . ?
C3 N2 H2C 104.7 . . ?
C2 N2 H2C 104.7 . . ?
Ho1 N2 H2C 104.7 . . ?
C6 N4 Ho1 117.1(3) . . ?
C6 N4 H4A 108.0 . . ?
Ho1 N4 H4A 108.0 . . ?
C6 N4 H4B 108.0 . . ?
Ho1 N4 H4B 108.0 . . ?
H4A N4 H4B 107.3 . . ?
N3 C5 C6 108.5(4) . . ?
N3 C5 H5C 110.0 . . ?
C6 C5 H5C 110.0 . . ?
N3 C5 H5D 110.0 . . ?
C6 C5 H5D 110.0 . . ?
H5C C5 H5D 108.4 . . ?
N2 C3 C4 107.4(3) . . ?
N2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
N2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
N6 C8 C7 108.1(4) . . ?
N6 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
N6 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
N2 C2 C1 108.1(4) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N3 C4 C3 109.4(3) . . ?
N3 C4 H4C 109.8 . . ?
C3 C4 H4C 109.8 . . ?
N3 C4 H4D 109.8 . . ?
C3 C4 H4D 109.8 . . ?
H4C C4 H4D 108.3 . . ?
N4 C6 C5 109.5(4) . . ?
N4 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N4 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.2 . . ?
N5 C7 C8 109.0(4) . . ?
N5 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N5 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N1 C1 C2 110.9(4) . . ?
N1 C1 H1C 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.308
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.132
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1033479'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 As N6 S4 Tm'
_chemical_formula_sum            'C8 H26 As N6 S4 Tm'
_chemical_formula_weight         578.44

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
Tm Tm -0.3139 5.2483 '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                   9.5588(6)
_cell_length_b                   13.0353(8)
_cell_length_c                   14.4749(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.6090(10)
_cell_angle_gamma                90.00
_cell_volume                     1787.72(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_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    2.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    7.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2446
_exptl_absorpt_correction_T_max  0.3549
_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            12751
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3110
_reflns_number_gt                2844
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0176P)²+1.6259P] 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     SHELXL
_refine_ls_extinction_coef       0.00029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3110
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0192
_refine_ls_wR_factor_ref         0.0458
_refine_ls_wR_factor_gt          0.0440
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Tm1 Tm 0.336295(15) 0.017450(11) 0.216243(9) 0.00855(7) Uani 1 1 d . . .
As1 As 0.71309(4) -0.01597(3) 0.24103(2) 0.01075(9) Uani 1 1 d . . .
S1 S 0.58975(9) 0.11576(6) 0.18566(5) 0.01274(18) Uani 1 1 d . . .
S2 S 0.55551(9) -0.10116(6) 0.30638(6) 0.01361(18) Uani 1 1 d . . .
S3 S 0.77295(9) -0.10497(6) 0.12651(6) 0.01462(19) Uani 1 1 d . . .
S4 S 0.88351(10) 0.02705(7) 0.34220(6) 0.0190(2) Uani 1 1 d . . .
N1 N 0.3653(3) -0.0585(2) 0.06452(18) 0.0149(6) Uani 1 1 d . . .
H1A H 0.3121 -0.0226 0.0198 0.018 Uiso 1 1 calc R . .
H1B H 0.4560 -0.0510 0.0553 0.018 Uiso 1 1 calc R . .
N2 N 0.2499(3) -0.1625(2) 0.20419(17) 0.0107(6) Uani 1 1 d . . .
H2C H 0.3275 -0.2009 0.2241 0.013 Uiso 1 1 calc R . .
N3 N 0.2257(3) -0.0344(2) 0.35487(18) 0.0117(6) Uani 1 1 d . . .
H3C H 0.1372 -0.0073 0.3458 0.014 Uiso 1 1 calc R . .
N4 N 0.3669(3) 0.1492(2) 0.34010(18) 0.0163(6) Uani 1 1 d . . .
H4A H 0.4600 0.1586 0.3571 0.020 Uiso 1 1 calc R . .
H4B H 0.3316 0.2087 0.3155 0.020 Uiso 1 1 calc R . .
N5 N 0.0799(3) 0.0413(2) 0.16725(19) 0.0144(6) Uani 1 1 d . . .
H5A H 0.0424 -0.0196 0.1481 0.017 Uiso 1 1 calc R . .
H5B H 0.0397 0.0607 0.2173 0.017 Uiso 1 1 calc R . .
N6 N 0.2845(3) 0.1730(2) 0.11842(18) 0.0119(6) Uani 1 1 d . . .
H6A H 0.3419 0.2239 0.1423 0.014 Uiso 1 1 calc R . .
H6B H 0.3054 0.1596 0.0608 0.014 Uiso 1 1 calc R . .
C1 C 0.3273(4) -0.1686(3) 0.0527(2) 0.0165(8) Uani 1 1 d . . .
H1C H 0.4090 -0.2105 0.0741 0.020 Uiso 1 1 calc R . .
H1D H 0.2989 -0.1831 -0.0128 0.020 Uiso 1 1 calc R . .
C2 C 0.2087(4) -0.1952(3) 0.1072(2) 0.0156(7) Uani 1 1 d . . .
H2A H 0.1229 -0.1603 0.0809 0.019 Uiso 1 1 calc R . .
H2B H 0.1914 -0.2685 0.1046 0.019 Uiso 1 1 calc R . .
C3 C 0.1478(4) -0.1891(3) 0.2690(2) 0.0141(7) Uani 1 1 d . . .
H3A H 0.1380 -0.2630 0.2731 0.017 Uiso 1 1 calc R . .
H3B H 0.0559 -0.1599 0.2474 0.017 Uiso 1 1 calc R . .
C4 C 0.2053(4) -0.1452(3) 0.3630(2) 0.0139(7) Uani 1 1 d . . .
H4C H 0.1398 -0.1588 0.4073 0.017 Uiso 1 1 calc R . .
H4D H 0.2945 -0.1777 0.3856 0.017 Uiso 1 1 calc R . .
C5 C 0.2954(4) 0.0139(3) 0.4407(2) 0.0178(8) Uani 1 1 d . . .
H5C H 0.3901 -0.0132 0.4560 0.021 Uiso 1 1 calc R . .
H5D H 0.2430 -0.0008 0.4922 0.021 Uiso 1 1 calc R . .
C6 C 0.3013(4) 0.1285(3) 0.4254(2) 0.0202(8) Uani 1 1 d . . .
H6C H 0.2067 0.1569 0.4187 0.024 Uiso 1 1 calc R . .
H6D H 0.3563 0.1608 0.4787 0.024 Uiso 1 1 calc R . .
C7 C 0.0420(4) 0.1172(3) 0.0922(2) 0.0144(7) Uani 1 1 d . . .
H7A H -0.0558 0.1376 0.0908 0.017 Uiso 1 1 calc R . .
H7B H 0.0535 0.0872 0.0324 0.017 Uiso 1 1 calc R . .
C8 C 0.1373(4) 0.2097(3) 0.1105(2) 0.0155(7) Uani 1 1 d . . .
H8A H 0.1190 0.2585 0.0597 0.019 Uiso 1 1 calc R . .
H8B H 0.1203 0.2434 0.1677 0.019 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
Tm1 N1 2.458(3) . ?
Tm1 N4 2.472(3) . ?
Tm1 N5 2.479(3) . ?
Tm1 N3 2.483(3) . ?
Tm1 N2 2.485(3) . ?
Tm1 N6 2.485(3) . ?
Tm1 S2 2.7856(8) . ?
Tm1 S1 2.8270(9) . ?
As1 S4 2.1168(10) . ?
As1 S3 2.1616(9) . ?
As1 S1 2.1750(9) . ?
As1 S2 2.1850(9) . ?
N1 C1 1.485(4) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.471(4) . ?
N2 C3 1.482(4) . ?
N2 H2C 0.9100 . ?
N3 C4 1.464(4) . ?
N3 C5 1.472(4) . ?
N3 H3C 0.9100 . ?
N4 C6 1.481(4) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.478(4) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.476(4) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.504(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.511(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.512(5) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.513(5) . ?
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
N1 Tm1 N4 155.69(10) . . ?
N1 Tm1 N5 91.09(10) . . ?
N4 Tm1 N5 97.91(10) . . ?
N1 Tm1 N3 136.30(9) . . ?
N4 Tm1 N3 67.99(9) . . ?
N5 Tm1 N3 75.80(9) . . ?
N1 Tm1 N2 68.46(9) . . ?
N4 Tm1 N2 135.48(9) . . ?
N5 Tm1 N2 77.98(9) . . ?
N3 Tm1 N2 68.07(9) . . ?
N1 Tm1 N6 81.78(9) . . ?
N4 Tm1 N6 80.89(9) . . ?
N5 Tm1 N6 67.65(9) . . ?
N3 Tm1 N6 127.49(9) . . ?
N2 Tm1 N6 133.70(9) . . ?
N1 Tm1 S2 91.62(7) . . ?
N4 Tm1 S2 92.10(7) . . ?
N5 Tm1 S2 149.04(7) . . ?
N3 Tm1 S2 81.07(7) . . ?
N2 Tm1 S2 74.42(6) . . ?
N6 Tm1 S2 143.18(7) . . ?
N1 Tm1 S1 80.92(7) . . ?
N4 Tm1 S1 77.13(7) . . ?
N5 Tm1 S1 137.18(7) . . ?
N3 Tm1 S1 135.69(7) . . ?
N2 Tm1 S1 134.47(7) . . ?
N6 Tm1 S1 69.58(7) . . ?
S2 Tm1 S1 73.61(2) . . ?
S4 As1 S3 114.53(4) . . ?
S4 As1 S1 112.07(4) . . ?
S3 As1 S1 109.07(3) . . ?
S4 As1 S2 110.28(4) . . ?
S3 As1 S2 109.08(4) . . ?
S1 As1 S2 100.93(3) . . ?
As1 S1 Tm1 91.05(3) . . ?
As1 S2 Tm1 91.95(3) . . ?
C1 N1 Tm1 115.9(2) . . ?
C1 N1 H1A 108.3 . . ?
Tm1 N1 H1A 108.3 . . ?
C1 N1 H1B 108.3 . . ?
Tm1 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C2 N2 C3 114.9(3) . . ?
C2 N2 Tm1 112.64(19) . . ?
C3 N2 Tm1 114.7(2) . . ?
C2 N2 H2C 104.4 . . ?
C3 N2 H2C 104.4 . . ?
Tm1 N2 H2C 104.4 . . ?
C4 N3 C5 113.9(3) . . ?
C4 N3 Tm1 114.2(2) . . ?
C5 N3 Tm1 111.8(2) . . ?
C4 N3 H3C 105.3 . . ?
C5 N3 H3C 105.3 . . ?
Tm1 N3 H3C 105.3 . . ?
C6 N4 Tm1 117.1(2) . . ?
C6 N4 H4A 108.0 . . ?
Tm1 N4 H4A 108.0 . . ?
C6 N4 H4B 108.0 . . ?
Tm1 N4 H4B 108.0 . . ?
H4A N4 H4B 107.3 . . ?
C7 N5 Tm1 115.5(2) . . ?
C7 N5 H5A 108.4 . . ?
Tm1 N5 H5A 108.4 . . ?
C7 N5 H5B 108.4 . . ?
Tm1 N5 H5B 108.4 . . ?
H5A N5 H5B 107.5 . . ?
C8 N6 Tm1 115.1(2) . . ?
C8 N6 H6A 108.5 . . ?
Tm1 N6 H6A 108.5 . . ?
C8 N6 H6B 108.5 . . ?
Tm1 N6 H6B 108.5 . . ?
H6A N6 H6B 107.5 . . ?
N1 C1 C2 110.6(3) . . ?
N1 C1 H1C 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 108.1 . . ?
N2 C2 C1 107.9(3) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 106.8(3) . . ?
N2 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N2 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N3 C4 C3 109.7(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 . . ?
N3 C5 C6 108.7(3) . . ?
N3 C5 H5C 110.0 . . ?
C6 C5 H5C 110.0 . . ?
N3 C5 H5D 110.0 . . ?
C6 C5 H5D 110.0 . . ?
H5C C5 H5D 108.3 . . ?
N4 C6 C5 109.3(3) . . ?
N4 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N4 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.3 . . ?
N5 C7 C8 108.8(3) . . ?
N5 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N5 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N6 C8 C7 107.5(3) . . ?
N6 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
N6 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.111
