# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_Ia

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H39 N9 Pr, 0.5(Ge2 S6), Cl '
_chemical_formula_sum            'C12 H39 Cl Ge N9 Pr S3'
_chemical_formula_weight         654.70

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'
Ge Ge 0.1547 1.8001 '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'
Cl Cl 0.1484 0.1585 '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/n'
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   11.637(3)
_cell_length_b                   14.143(3)
_cell_length_c                   15.120(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.149(5)
_cell_angle_gamma                90.00
_cell_volume                     2463.5(10)
_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          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    3.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3121
_exptl_absorpt_correction_T_max  0.5454
_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            17095
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4249
_reflns_number_gt                3818
_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)+(0.0202P)²+3.4646P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4249
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0570
_refine_ls_wR_factor_gt          0.0546
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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 0.010724(14) 0.735847(12) 0.191683(12) 0.02646(7) Uani 1 1 d . . .
Ge1 Ge 0.36336(3) 0.50262(2) -0.01098(2) 0.02445(9) Uani 1 1 d . . .
S3 S 0.50482(7) 0.58352(7) 0.07511(7) 0.0414(2) Uani 1 1 d . . .
S2 S 0.26052(8) 0.41471(8) 0.06474(7) 0.0466(3) Uani 1 1 d . . .
C8 C 0.0057(4) 0.7083(3) 0.4256(3) 0.0490(10) Uani 1 1 d . . .
H8A H -0.0358 0.7257 0.4745 0.059 Uiso 1 1 calc R . .
H8B H 0.0867 0.6991 0.4497 0.059 Uiso 1 1 calc R . .
S1 S 0.25363(8) 0.59028(7) -0.10383(9) 0.0554(3) Uani 1 1 d . . .
N2 N 0.1758(2) 0.7438(2) 0.0847(2) 0.0362(7) Uani 1 1 d . . .
H2C H 0.1861 0.6833 0.0668 0.043 Uiso 1 1 calc R . .
N5 N 0.0177(2) 0.59528(19) 0.3083(2) 0.0362(7) Uani 1 1 d . . .
H5C H 0.0938 0.5911 0.3324 0.043 Uiso 1 1 calc R . .
N3 N 0.2306(2) 0.7325(2) 0.2744(2) 0.0358(7) Uani 1 1 d . . .
H3A H 0.2448 0.7870 0.3045 0.043 Uiso 1 1 calc R . .
H3B H 0.2374 0.6853 0.3147 0.043 Uiso 1 1 calc R . .
N6 N -0.0043(3) 0.7844(2) 0.3595(2) 0.0370(7) Uani 1 1 d . . .
H6A H 0.0516 0.8272 0.3769 0.044 Uiso 1 1 calc R . .
H6B H -0.0730 0.8134 0.3603 0.044 Uiso 1 1 calc R . .
N4 N 0.0196(3) 0.5576(2) 0.1232(2) 0.0454(8) Uani 1 1 d . . .
H4A H -0.0504 0.5429 0.0929 0.054 Uiso 1 1 calc R . .
H4B H 0.0714 0.5567 0.0843 0.054 Uiso 1 1 calc R . .
N1 N -0.0647(3) 0.7593(2) 0.0175(2) 0.0446(8) Uani 1 1 d . . .
H1A H -0.1175 0.7141 0.0001 0.054 Uiso 1 1 calc R . .
H1B H -0.1014 0.8154 0.0102 0.054 Uiso 1 1 calc R . .
N8 N -0.1551(3) 0.8654(2) 0.1839(3) 0.0545(9) Uani 1 1 d . . .
H8C H -0.1599 0.8736 0.2430 0.065 Uiso 1 1 calc R . .
C2 C 0.1363(3) 0.7978(3) 0.0027(3) 0.0472(10) Uani 1 1 d . . .
H2A H 0.1949 0.7954 -0.0369 0.057 Uiso 1 1 calc R . .
H2B H 0.1244 0.8635 0.0176 0.057 Uiso 1 1 calc R . .
C7 C -0.0433(4) 0.6177(3) 0.3843(3) 0.0493(10) Uani 1 1 d . . .
H7A H -0.0325 0.5670 0.4280 0.059 Uiso 1 1 calc R . .
H7B H -0.1257 0.6247 0.3642 0.059 Uiso 1 1 calc R . .
C3 C 0.2894(3) 0.7752(3) 0.1305(3) 0.0429(9) Uani 1 1 d . . .
H3C H 0.2864 0.8421 0.1442 0.051 Uiso 1 1 calc R . .
H3D H 0.3483 0.7657 0.0919 0.051 Uiso 1 1 calc R . .
C4 C 0.3200(3) 0.7196(3) 0.2155(3) 0.0447(9) Uani 1 1 d . . .
H4C H 0.3263 0.6531 0.2013 0.054 Uiso 1 1 calc R . .
H4D H 0.3946 0.7406 0.2460 0.054 Uiso 1 1 calc R . .
C6 C -0.0111(3) 0.5009(2) 0.2704(3) 0.0453(10) Uani 1 1 d . . .
H6C H -0.0941 0.4962 0.2515 0.054 Uiso 1 1 calc R . .
H6D H 0.0111 0.4529 0.3153 0.054 Uiso 1 1 calc R . .
C5 C 0.0522(4) 0.4857(3) 0.1924(3) 0.0502(11) Uani 1 1 d . . .
H5A H 0.1352 0.4887 0.2121 0.060 Uiso 1 1 calc R . .
H5B H 0.0342 0.4233 0.1676 0.060 Uiso 1 1 calc R . .
C1 C 0.0252(4) 0.7564(3) -0.0427(3) 0.0531(11) Uani 1 1 d . . .
H1C H -0.0012 0.7917 -0.0968 0.064 Uiso 1 1 calc R . .
H1D H 0.0381 0.6914 -0.0594 0.064 Uiso 1 1 calc R . .
N9 N 0.0792(3) 0.9173(2) 0.2070(2) 0.0424(7) Uani 1 1 d . . .
H9A H 0.1236 0.9244 0.2603 0.051 Uiso 1 1 calc R . .
H9B H 0.1246 0.9289 0.1647 0.051 Uiso 1 1 calc R . .
N7 N -0.2072(2) 0.6693(2) 0.1699(2) 0.0455(8) Uani 1 1 d . . .
H7C H -0.2266 0.6508 0.1128 0.055 Uiso 1 1 calc R . .
H7D H -0.2102 0.6181 0.2049 0.055 Uiso 1 1 calc R . .
C10 C -0.2709(4) 0.8316(3) 0.1516(4) 0.0707(16) Uani 1 1 d . . .
H10A H -0.2803 0.8259 0.0870 0.085 Uiso 1 1 calc R . .
H10B H -0.3275 0.8770 0.1668 0.085 Uiso 1 1 calc R . .
C9 C -0.2920(4) 0.7384(4) 0.1915(4) 0.0769(18) Uani 1 1 d . . .
H9C H -0.2866 0.7446 0.2559 0.092 Uiso 1 1 calc R . .
H9D H -0.3697 0.7167 0.1687 0.092 Uiso 1 1 calc R . .
C11 C -0.1219(5) 0.9575(3) 0.1599(4) 0.0801(17) Uani 1 1 d . . .
H11A H -0.1244 0.9595 0.0955 0.096 Uiso 1 1 calc R . .
H11B H -0.1793 1.0021 0.1753 0.096 Uiso 1 1 calc R . .
C12 C -0.0112(4) 0.9888(3) 0.1995(4) 0.0726(15) Uani 1 1 d . . .
H12A H -0.0174 1.0125 0.2588 0.087 Uiso 1 1 calc R . .
H12B H 0.0122 1.0412 0.1647 0.087 Uiso 1 1 calc R . .
Cl1 Cl 0.27601(9) 0.55198(7) 0.41982(8) 0.0555(3) Uani 1 1 d . . .


_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 2.651(3) . ?
Pr1 N8 2.651(3) . ?
Pr1 N6 2.658(3) . ?
Pr1 N1 2.676(3) . ?
Pr1 N7 2.682(3) . ?
Pr1 N2 2.684(3) . ?
Pr1 N3 2.684(3) . ?
Pr1 N9 2.688(3) . ?
Pr1 N4 2.733(3) . ?
Ge1 S1 2.1518(10) . ?
Ge1 S2 2.1627(10) . ?
Ge1 S3 2.2596(10) . ?
Ge1 S3 2.2803(10) 3_665 ?
S3 Ge1 2.2803(10) 3_665 ?
C8 N6 1.463(5) . ?
C8 C7 1.501(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
N2 C3 1.472(5) . ?
N2 C2 1.472(5) . ?
N2 H2C 0.9100 . ?
N5 C7 1.468(5) . ?
N5 C6 1.472(4) . ?
N5 H5C 0.9100 . ?
N3 C4 1.474(5) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N4 C5 1.471(5) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N1 C1 1.482(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N8 C11 1.422(6) . ?
N8 C10 1.447(5) . ?
N8 H8C 0.9100 . ?
C2 C1 1.495(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C3 C4 1.505(6) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C6 C5 1.492(6) . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
N9 C12 1.452(5) . ?
N9 H9A 0.9000 . ?
N9 H9B 0.9000 . ?
N7 C9 1.458(5) . ?
N7 H7C 0.9000 . ?
N7 H7D 0.9000 . ?
C10 C9 1.485(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C11 C12 1.413(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 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 N8 120.07(11) . . ?
N5 Pr1 N6 63.83(9) . . ?
N8 Pr1 N6 73.60(11) . . ?
N5 Pr1 N1 136.27(9) . . ?
N8 Pr1 N1 74.66(11) . . ?
N6 Pr1 N1 148.25(10) . . ?
N5 Pr1 N7 75.97(10) . . ?
N8 Pr1 N7 64.35(10) . . ?
N6 Pr1 N7 91.06(10) . . ?
N1 Pr1 N7 75.54(10) . . ?
N5 Pr1 N2 118.39(9) . . ?
N8 Pr1 N2 121.54(11) . . ?
N6 Pr1 N2 135.60(9) . . ?
N1 Pr1 N2 64.17(10) . . ?
N7 Pr1 N2 133.33(10) . . ?
N5 Pr1 N3 74.89(9) . . ?
N8 Pr1 N3 132.28(10) . . ?
N6 Pr1 N3 75.37(9) . . ?
N1 Pr1 N3 128.23(10) . . ?
N7 Pr1 N3 150.85(10) . . ?
N2 Pr1 N3 64.24(9) . . ?
N5 Pr1 N9 132.70(9) . . ?
N8 Pr1 N9 63.21(10) . . ?
N6 Pr1 N9 74.33(9) . . ?
N1 Pr1 N9 91.03(10) . . ?
N7 Pr1 N9 127.55(10) . . ?
N2 Pr1 N9 77.47(9) . . ?
N3 Pr1 N9 74.07(9) . . ?
N5 Pr1 N4 63.96(10) . . ?
N8 Pr1 N4 133.37(10) . . ?
N6 Pr1 N4 127.68(10) . . ?
N1 Pr1 N4 76.49(10) . . ?
N7 Pr1 N4 73.48(9) . . ?
N2 Pr1 N4 75.02(9) . . ?
N3 Pr1 N4 94.33(9) . . ?
N9 Pr1 N4 152.48(10) . . ?
S1 Ge1 S2 110.78(4) . . ?
S1 Ge1 S3 113.62(4) . . ?
S2 Ge1 S3 113.50(4) . . ?
S1 Ge1 S3 113.78(5) . 3_665 ?
S2 Ge1 S3 111.97(5) . 3_665 ?
S3 Ge1 S3 92.09(4) . 3_665 ?
Ge1 S3 Ge1 87.91(4) . 3_665 ?
N6 C8 C7 110.8(3) . . ?
N6 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N6 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C3 N2 C2 113.1(3) . . ?
C3 N2 Pr1 113.6(2) . . ?
C2 N2 Pr1 111.4(2) . . ?
C3 N2 H2C 106.0 . . ?
C2 N2 H2C 106.0 . . ?
Pr1 N2 H2C 106.0 . . ?
C7 N5 C6 113.1(3) . . ?
C7 N5 Pr1 112.7(2) . . ?
C6 N5 Pr1 115.9(2) . . ?
C7 N5 H5C 104.6 . . ?
C6 N5 H5C 104.6 . . ?
Pr1 N5 H5C 104.6 . . ?
C4 N3 Pr1 115.4(2) . . ?
C4 N3 H3A 108.4 . . ?
Pr1 N3 H3A 108.4 . . ?
C4 N3 H3B 108.4 . . ?
Pr1 N3 H3B 108.4 . . ?
H3A N3 H3B 107.5 . . ?
C8 N6 Pr1 116.9(2) . . ?
C8 N6 H6A 108.1 . . ?
Pr1 N6 H6A 108.1 . . ?
C8 N6 H6B 108.1 . . ?
Pr1 N6 H6B 108.1 . . ?
H6A N6 H6B 107.3 . . ?
C5 N4 Pr1 112.8(2) . . ?
C5 N4 H4A 109.0 . . ?
Pr1 N4 H4A 109.0 . . ?
C5 N4 H4B 109.0 . . ?
Pr1 N4 H4B 109.0 . . ?
H4A N4 H4B 107.8 . . ?
C1 N1 Pr1 116.1(2) . . ?
C1 N1 H1A 108.3 . . ?
Pr1 N1 H1A 108.3 . . ?
C1 N1 H1B 108.3 . . ?
Pr1 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C11 N8 C10 119.3(4) . . ?
C11 N8 Pr1 115.0(3) . . ?
C10 N8 Pr1 115.1(2) . . ?
C11 N8 H8C 101.0 . . ?
C10 N8 H8C 101.0 . . ?
Pr1 N8 H8C 101.0 . . ?
N2 C2 C1 109.2(3) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
N5 C7 C8 108.2(3) . . ?
N5 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
N5 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N2 C3 C4 109.4(3) . . ?
N2 C3 H3C 109.8 . . ?
C4 C3 H3C 109.8 . . ?
N2 C3 H3D 109.8 . . ?
C4 C3 H3D 109.8 . . ?
H3C C3 H3D 108.2 . . ?
N3 C4 C3 110.5(3) . . ?
N3 C4 H4C 109.6 . . ?
C3 C4 H4C 109.6 . . ?
N3 C4 H4D 109.6 . . ?
C3 C4 H4D 109.6 . . ?
H4C C4 H4D 108.1 . . ?
N5 C6 C5 109.2(3) . . ?
N5 C6 H6C 109.8 . . ?
C5 C6 H6C 109.8 . . ?
N5 C6 H6D 109.8 . . ?
C5 C6 H6D 109.8 . . ?
H6C C6 H6D 108.3 . . ?
N4 C5 C6 110.8(3) . . ?
N4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N1 C1 C2 110.3(3) . . ?
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 . . ?
C12 N9 Pr1 117.1(3) . . ?
C12 N9 H9A 108.0 . . ?
Pr1 N9 H9A 108.0 . . ?
C12 N9 H9B 108.0 . . ?
Pr1 N9 H9B 108.0 . . ?
H9A N9 H9B 107.3 . . ?
C9 N7 Pr1 113.3(2) . . ?
C9 N7 H7C 108.9 . . ?
Pr1 N7 H7C 108.9 . . ?
C9 N7 H7D 108.9 . . ?
Pr1 N7 H7D 108.9 . . ?
H7C N7 H7D 107.7 . . ?
N8 C10 C9 110.8(4) . . ?
N8 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
N8 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N7 C9 C10 110.3(4) . . ?
N7 C9 H9C 109.6 . . ?
C10 C9 H9C 109.6 . . ?
N7 C9 H9D 109.6 . . ?
C10 C9 H9D 109.6 . . ?
H9C C9 H9D 108.1 . . ?
C12 C11 N8 116.3(4) . . ?
C12 C11 H11A 108.2 . . ?
N8 C11 H11A 108.2 . . ?
C12 C11 H11B 108.2 . . ?
N8 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 N9 115.0(4) . . ?
C11 C12 H12A 108.5 . . ?
N9 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
N9 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 1005128'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ib

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H39 N9 Sm, 0.5(Ge2 S6), Cl'
_chemical_formula_sum            'C12 H39 Cl Ge N9 S3 Sm'
_chemical_formula_weight         664.15

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.532(3)
_cell_length_b                   14.423(4)
_cell_length_c                   14.573(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.105(5)
_cell_angle_gamma                90.00
_cell_volume                     2405.3(10)
_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            'light yellow'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1332
_exptl_absorpt_coefficient_mu    4.056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3199
_exptl_absorpt_correction_T_max  0.6159
_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            16607
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4206
_reflns_number_gt                3864
_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)+(0.0274P)²+5.5956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4206
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0667
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.004121(15) 0.259501(13) 0.189443(13) 0.02800(8) Uani 1 1 d . . .
Ge1 Ge -0.36303(3) 0.50052(3) 0.00764(2) 0.02570(10) Uani 1 1 d . . .
S1 S -0.24816(9) 0.59671(9) 0.08459(10) 0.0561(3) Uani 1 1 d . . .
S2 S -0.50570(9) 0.56674(10) -0.09034(9) 0.0534(3) Uani 1 1 d . . .
S3 S -0.26609(9) 0.39901(9) -0.05963(8) 0.0510(3) Uani 1 1 d . . .
Cl1 Cl 0.26888(11) 0.44902(9) 0.41609(10) 0.0610(3) Uani 1 1 d . . .
N1 N -0.2085(3) 0.3278(3) 0.1726(3) 0.0447(9) Uani 1 1 d . . .
H1A H -0.2082 0.3792 0.2076 0.054 Uiso 1 1 calc R . .
H1B H -0.2284 0.3449 0.1133 0.054 Uiso 1 1 calc R . .
N2 N -0.1649(3) 0.1373(3) 0.1895(4) 0.0667(13) Uani 1 1 d . . .
H2C H -0.1667 0.1336 0.2517 0.080 Uiso 1 1 calc R . .
N3 N 0.0648(3) 0.0852(3) 0.2041(2) 0.0468(9) Uani 1 1 d . . .
H3A H 0.1275 0.0763 0.1740 0.056 Uiso 1 1 calc R . .
H3B H 0.0864 0.0721 0.2642 0.056 Uiso 1 1 calc R . .
N4 N 0.0146(3) 0.4252(3) 0.1094(3) 0.0527(10) Uani 1 1 d . . .
H4A H 0.0658 0.4222 0.0676 0.063 Uiso 1 1 calc R . .
H4B H -0.0560 0.4386 0.0787 0.063 Uiso 1 1 calc R . .
N5 N 0.0146(3) 0.4002(2) 0.3016(2) 0.0406(8) Uani 1 1 d . . .
H5C H 0.0916 0.4043 0.3242 0.049 Uiso 1 1 calc R . .
N6 N -0.0118(3) 0.2187(3) 0.3611(3) 0.0445(9) Uani 1 1 d . . .
H6A H -0.0824 0.1931 0.3641 0.053 Uiso 1 1 calc R . .
H6B H 0.0423 0.1753 0.3792 0.053 Uiso 1 1 calc R . .
N7 N -0.0718(3) 0.2298(3) 0.0153(3) 0.0504(10) Uani 1 1 d . . .
H7A H -0.1083 0.1745 0.0108 0.061 Uiso 1 1 calc R . .
H7B H -0.1255 0.2734 -0.0033 0.061 Uiso 1 1 calc R . .
N8 N 0.1687(3) 0.2470(3) 0.0805(2) 0.0392(8) Uani 1 1 d . . .
H8C H 0.1796 0.3055 0.0599 0.047 Uiso 1 1 calc R . .
N9 N 0.2192(3) 0.2649(2) 0.2730(2) 0.0366(8) Uani 1 1 d . . .
H9A H 0.2253 0.3130 0.3126 0.044 Uiso 1 1 calc R . .
H9B H 0.2324 0.2128 0.3066 0.044 Uiso 1 1 calc R . .
C1 C -0.2818(4) 0.1730(4) 0.1634(5) 0.080(2) Uani 1 1 d . . .
H1C H -0.2979 0.1741 0.0964 0.096 Uiso 1 1 calc R . .
H1D H -0.3377 0.1314 0.1864 0.096 Uiso 1 1 calc R . .
C2 C -0.2976(5) 0.2652(5) 0.1987(5) 0.083(2) Uani 1 1 d . . .
H2A H -0.2933 0.2629 0.2656 0.100 Uiso 1 1 calc R . .
H2B H -0.3743 0.2882 0.1744 0.100 Uiso 1 1 calc R . .
C3 C -0.1432(6) 0.0447(4) 0.1725(5) 0.082(2) Uani 1 1 d . . .
H3C H -0.1885 0.0275 0.1144 0.098 Uiso 1 1 calc R . .
H3D H -0.1716 0.0078 0.2207 0.098 Uiso 1 1 calc R . .
C4 C -0.0261(6) 0.0209(4) 0.1679(6) 0.094(2) Uani 1 1 d . . .
H4C H -0.0175 0.0097 0.1034 0.113 Uiso 1 1 calc R . .
H4D H -0.0113 -0.0375 0.2002 0.113 Uiso 1 1 calc R . .
C5 C 0.0493(4) 0.4995(3) 0.1741(4) 0.0623(15) Uani 1 1 d . . .
H5A H 0.0307 0.5588 0.1446 0.075 Uiso 1 1 calc R . .
H5B H 0.1331 0.4970 0.1922 0.075 Uiso 1 1 calc R . .
C6 C -0.0129(4) 0.4907(3) 0.2583(4) 0.0532(12) Uani 1 1 d . . .
H6C H 0.0119 0.5399 0.3017 0.064 Uiso 1 1 calc R . .
H6D H -0.0965 0.4962 0.2409 0.064 Uiso 1 1 calc R . .
C7 C -0.0445(4) 0.3830(4) 0.3835(3) 0.0562(12) Uani 1 1 d . . .
H7C H -0.1281 0.3775 0.3658 0.067 Uiso 1 1 calc R . .
H7D H -0.0305 0.4341 0.4268 0.067 Uiso 1 1 calc R . .
C8 C 0.0031(4) 0.2951(4) 0.4272(3) 0.0552(13) Uani 1 1 d . . .
H8A H 0.0854 0.3029 0.4489 0.066 Uiso 1 1 calc R . .
H8B H -0.0372 0.2807 0.4801 0.066 Uiso 1 1 calc R . .
C9 C 0.0169(5) 0.2302(4) -0.0482(3) 0.0531(12) Uani 1 1 d . . .
H9C H 0.0293 0.2933 -0.0680 0.064 Uiso 1 1 calc R . .
H9D H -0.0105 0.1938 -0.1026 0.064 Uiso 1 1 calc R . .
C10 C 0.1299(4) 0.1911(4) -0.0031(3) 0.0480(11) Uani 1 1 d . . .
H10A H 0.1194 0.1269 0.0140 0.058 Uiso 1 1 calc R . .
H10B H 0.1883 0.1933 -0.0455 0.058 Uiso 1 1 calc R . .
C11 C 0.2824(4) 0.2171(4) 0.1268(3) 0.0487(11) Uani 1 1 d . . .
H11A H 0.3419 0.2255 0.0859 0.058 Uiso 1 1 calc R . .
H11B H 0.2796 0.1519 0.1426 0.058 Uiso 1 1 calc R . .
C12 C 0.3116(4) 0.2737(4) 0.2126(3) 0.0482(11) Uani 1 1 d . . .
H12A H 0.3854 0.2528 0.2453 0.058 Uiso 1 1 calc R . .
H12B H 0.3201 0.3383 0.1960 0.058 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 N6 2.599(4) . ?
Sm1 N5 2.599(4) . ?
Sm1 N3 2.612(4) . ?
Sm1 N7 2.615(4) . ?
Sm1 N9 2.626(3) . ?
Sm1 N1 2.626(3) . ?
Sm1 N8 2.628(3) . ?
Sm1 N2 2.628(4) . ?
Sm1 N4 2.668(4) . ?
Ge1 S1 2.1377(12) . ?
Ge1 S3 2.1507(12) . ?
Ge1 S2 2.2531(11) . ?
Ge1 S2 2.2664(11) 3_465 ?
S2 Ge1 2.2664(11) 3_465 ?
N1 C2 1.454(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.387(7) . ?
N2 C1 1.450(7) . ?
N2 H2C 0.9100 . ?
N3 C4 1.450(7) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.451(7) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.467(6) . ?
N5 C6 1.467(6) . ?
N5 H5C 0.9100 . ?
N6 C8 1.459(7) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 C9 1.462(7) . ?
N7 H7A 0.9000 . ?
N7 H7B 0.9000 . ?
N8 C11 1.463(5) . ?
N8 C10 1.483(5) . ?
N8 H8C 0.9100 . ?
N9 C12 1.469(5) . ?
N9 H9A 0.9000 . ?
N9 H9B 0.9000 . ?
C1 C2 1.446(10) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.403(9) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.501(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.493(7) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.497(7) . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.496(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 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 Sm1 N5 64.83(12) . . ?
N6 Sm1 N3 75.72(12) . . ?
N5 Sm1 N3 135.17(11) . . ?
N6 Sm1 N7 147.35(13) . . ?
N5 Sm1 N7 136.21(12) . . ?
N3 Sm1 N7 88.62(12) . . ?
N6 Sm1 N9 74.67(11) . . ?
N5 Sm1 N9 73.61(11) . . ?
N3 Sm1 N9 76.24(11) . . ?
N7 Sm1 N9 129.67(12) . . ?
N6 Sm1 N1 89.93(12) . . ?
N5 Sm1 N1 74.70(11) . . ?
N3 Sm1 N1 127.33(12) . . ?
N7 Sm1 N1 76.92(12) . . ?
N9 Sm1 N1 148.24(12) . . ?
N6 Sm1 N8 135.13(11) . . ?
N5 Sm1 N8 116.93(11) . . ?
N3 Sm1 N8 77.11(12) . . ?
N7 Sm1 N8 65.33(12) . . ?
N9 Sm1 N8 64.56(11) . . ?
N1 Sm1 N8 134.86(11) . . ?
N6 Sm1 N2 72.96(15) . . ?
N5 Sm1 N2 120.00(14) . . ?
N3 Sm1 N2 62.97(13) . . ?
N7 Sm1 N2 74.41(15) . . ?
N9 Sm1 N2 132.67(12) . . ?
N1 Sm1 N2 64.37(13) . . ?
N8 Sm1 N2 123.07(15) . . ?
N6 Sm1 N4 129.52(13) . . ?
N5 Sm1 N4 64.84(13) . . ?
N3 Sm1 N4 150.65(12) . . ?
N7 Sm1 N4 75.52(14) . . ?
N9 Sm1 N4 94.88(12) . . ?
N1 Sm1 N4 73.48(11) . . ?
N8 Sm1 N4 73.85(12) . . ?
N2 Sm1 N4 132.41(13) . . ?
S1 Ge1 S3 110.96(5) . . ?
S1 Ge1 S2 114.45(6) . . ?
S3 Ge1 S2 112.31(5) . . ?
S1 Ge1 S2 114.21(6) . 3_465 ?
S3 Ge1 S2 111.72(6) . 3_465 ?
S2 Ge1 S2 92.01(4) . 3_465 ?
Ge1 S2 Ge1 87.99(4) . 3_465 ?
C2 N1 Sm1 115.1(3) . . ?
C2 N1 H1A 108.5 . . ?
Sm1 N1 H1A 108.5 . . ?
C2 N1 H1B 108.5 . . ?
Sm1 N1 H1B 108.5 . . ?
H1A N1 H1B 107.5 . . ?
C3 N2 C1 118.5(5) . . ?
C3 N2 Sm1 119.7(4) . . ?
C1 N2 Sm1 115.3(3) . . ?
C3 N2 H2C 98.5 . . ?
C1 N2 H2C 98.5 . . ?
Sm1 N2 H2C 98.5 . . ?
C4 N3 Sm1 114.3(4) . . ?
C4 N3 H3A 108.7 . . ?
Sm1 N3 H3A 108.7 . . ?
C4 N3 H3B 108.7 . . ?
Sm1 N3 H3B 108.7 . . ?
H3A N3 H3B 107.6 . . ?
C5 N4 Sm1 113.6(3) . . ?
C5 N4 H4A 108.8 . . ?
Sm1 N4 H4A 108.8 . . ?
C5 N4 H4B 108.8 . . ?
Sm1 N4 H4B 108.8 . . ?
H4A N4 H4B 107.7 . . ?
C7 N5 C6 113.7(4) . . ?
C7 N5 Sm1 112.9(3) . . ?
C6 N5 Sm1 115.7(3) . . ?
C7 N5 H5C 104.3 . . ?
C6 N5 H5C 104.3 . . ?
Sm1 N5 H5C 104.3 . . ?
C8 N6 Sm1 116.6(3) . . ?
C8 N6 H6A 108.1 . . ?
Sm1 N6 H6A 108.1 . . ?
C8 N6 H6B 108.1 . . ?
Sm1 N6 H6B 108.1 . . ?
H6A N6 H6B 107.3 . . ?
C9 N7 Sm1 115.9(3) . . ?
C9 N7 H7A 108.3 . . ?
Sm1 N7 H7A 108.3 . . ?
C9 N7 H7B 108.3 . . ?
Sm1 N7 H7B 108.3 . . ?
H7A N7 H7B 107.4 . . ?
C11 N8 C10 112.4(3) . . ?
C11 N8 Sm1 114.5(2) . . ?
C10 N8 Sm1 111.5(3) . . ?
C11 N8 H8C 105.9 . . ?
C10 N8 H8C 105.9 . . ?
Sm1 N8 H8C 105.9 . . ?
C12 N9 Sm1 116.0(2) . . ?
C12 N9 H9A 108.3 . . ?
Sm1 N9 H9A 108.3 . . ?
C12 N9 H9B 108.3 . . ?
Sm1 N9 H9B 108.3 . . ?
H9A N9 H9B 107.4 . . ?
C2 C1 N2 112.7(5) . . ?
C2 C1 H1C 109.0 . . ?
N2 C1 H1C 109.0 . . ?
C2 C1 H1D 109.0 . . ?
N2 C1 H1D 109.0 . . ?
H1C C1 H1D 107.8 . . ?
C1 C2 N1 110.7(5) . . ?
C1 C2 H2A 109.5 . . ?
N1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 116.1(5) . . ?
N2 C3 H3C 108.3 . . ?
C4 C3 H3C 108.3 . . ?
N2 C3 H3D 108.3 . . ?
C4 C3 H3D 108.3 . . ?
H3C C3 H3D 107.4 . . ?
C3 C4 N3 118.9(5) . . ?
C3 C4 H4C 107.6 . . ?
N3 C4 H4C 107.6 . . ?
C3 C4 H4D 107.6 . . ?
N3 C4 H4D 107.6 . . ?
H4C C4 H4D 107.0 . . ?
N4 C5 C6 110.4(4) . . ?
N4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N5 C6 C5 109.1(4) . . ?
N5 C6 H6C 109.9 . . ?
C5 C6 H6C 109.9 . . ?
N5 C6 H6D 109.9 . . ?
C5 C6 H6D 109.9 . . ?
H6C C6 H6D 108.3 . . ?
N5 C7 C8 107.9(4) . . ?
N5 C7 H7C 110.1 . . ?
C8 C7 H7C 110.1 . . ?
N5 C7 H7D 110.1 . . ?
C8 C7 H7D 110.1 . . ?
H7C C7 H7D 108.4 . . ?
N6 C8 C7 110.7(4) . . ?
N6 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N6 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N7 C9 C10 111.1(4) . . ?
N7 C9 H9C 109.4 . . ?
C10 C9 H9C 109.4 . . ?
N7 C9 H9D 109.4 . . ?
C10 C9 H9D 109.4 . . ?
H9C C9 H9D 108.0 . . ?
N8 C10 C9 108.3(4) . . ?
N8 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
N8 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N8 C11 C12 108.8(4) . . ?
N8 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
N8 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N9 C12 C11 110.4(4) . . ?
N9 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
N9 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 1005129'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ic

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H39 Gd N9, 0.5(Ge2 S6), Cl'
_chemical_formula_sum            'C12 H39 Cl Gd Ge N9 S3'
_chemical_formula_weight         671.04

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   11.5484(14)
_cell_length_b                   14.6767(17)
_cell_length_c                   14.4271(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.332(2)
_cell_angle_gamma                90.00
_cell_volume                     2430.4(5)
_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          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1340
_exptl_absorpt_coefficient_mu    4.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2435
_exptl_absorpt_correction_T_max  0.3536
_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            20881
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.39
_reflns_number_total             5982
_reflns_number_gt                5450
_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)+(0.0294P)²+2.4354P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5982
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0640
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd -0.000202(11) 0.241750(8) 0.310278(9) 0.02362(5) Uani 1 1 d . . .
Ge1 Ge -0.13701(2) 0.499341(19) -0.00633(2) 0.02378(7) Uani 1 1 d . . .
S2 S -0.23075(7) 0.39200(6) 0.05597(6) 0.03898(18) Uani 1 1 d . . .
S3 S 0.00499(6) 0.55821(6) 0.09809(6) 0.03673(17) Uani 1 1 d . . .
S1 S -0.25367(7) 0.59831(6) -0.07708(6) 0.03786(17) Uani 1 1 d . . .
Cl1 Cl -0.26708(8) 0.04934(6) 0.08614(7) 0.0487(2) Uani 1 1 d . . .
N1 N 0.2087(2) 0.17273(19) 0.3244(2) 0.0390(6) Uani 1 1 d . . .
H1A H 0.2289 0.1572 0.3844 0.047 Uiso 1 1 calc R . .
H1B H 0.2065 0.1212 0.2905 0.047 Uiso 1 1 calc R . .
N2 N 0.1697(2) 0.3597(2) 0.3015(3) 0.0500(8) Uani 1 1 d . . .
H2C H 0.1723 0.3629 0.2388 0.060 Uiso 1 1 calc R . .
N3 N -0.0578(2) 0.41262(18) 0.2953(2) 0.0375(6) Uani 1 1 d . . .
H3A H -0.0689 0.4276 0.2345 0.045 Uiso 1 1 calc R . .
H3B H -0.1257 0.4209 0.3193 0.045 Uiso 1 1 calc R . .
N4 N 0.0146(2) 0.2772(2) 0.1349(2) 0.0401(6) Uani 1 1 d . . .
H4A H -0.0382 0.3204 0.1163 0.048 Uiso 1 1 calc R . .
H4B H 0.0856 0.3007 0.1297 0.048 Uiso 1 1 calc R . .
N5 N -0.0134(2) 0.10022(18) 0.20176(18) 0.0341(5) Uani 1 1 d . . .
H5C H -0.0903 0.0960 0.1805 0.041 Uiso 1 1 calc R . .
N6 N -0.0110(2) 0.08271(18) 0.39745(19) 0.0389(6) Uani 1 1 d . . .
H6A H 0.0595 0.0700 0.4276 0.047 Uiso 1 1 calc R . .
H6B H -0.0615 0.0876 0.4404 0.047 Uiso 1 1 calc R . .
N7 N 0.0766(3) 0.2749(2) 0.4815(2) 0.0417(6) Uani 1 1 d . . .
H7A H 0.1315 0.2332 0.5000 0.050 Uiso 1 1 calc R . .
H7B H 0.1114 0.3298 0.4840 0.050 Uiso 1 1 calc R . .
N8 N -0.1637(2) 0.25656(17) 0.42077(18) 0.0323(5) Uani 1 1 d . . .
H8C H -0.1741 0.1992 0.4424 0.039 Uiso 1 1 calc R . .
N9 N -0.2126(2) 0.23674(17) 0.22714(19) 0.0320(5) Uani 1 1 d . . .
H9A H -0.2254 0.2883 0.1937 0.038 Uiso 1 1 calc R . .
H9B H -0.2179 0.1899 0.1866 0.038 Uiso 1 1 calc R . .
C1 C 0.3003(4) 0.2317(3) 0.2945(4) 0.0672(14) Uani 1 1 d . . .
H1C H 0.2944 0.2336 0.2270 0.081 Uiso 1 1 calc R . .
H1D H 0.3763 0.2076 0.3174 0.081 Uiso 1 1 calc R . .
C2 C 0.2865(3) 0.3253(3) 0.3322(3) 0.0540(10) Uani 1 1 d . . .
H2A H 0.2986 0.3239 0.3998 0.065 Uiso 1 1 calc R . .
H2B H 0.3444 0.3655 0.3103 0.065 Uiso 1 1 calc R . .
C3 C 0.1507(3) 0.4541(2) 0.3232(3) 0.0535(10) Uani 1 1 d . . .
H3C H 0.1684 0.4913 0.2710 0.064 Uiso 1 1 calc R . .
H3D H 0.2043 0.4711 0.3769 0.064 Uiso 1 1 calc R . .
C4 C 0.0306(3) 0.4740(2) 0.3432(3) 0.0508(9) Uani 1 1 d . . .
H4C H 0.0272 0.4695 0.4100 0.061 Uiso 1 1 calc R . .
H4D H 0.0115 0.5362 0.3248 0.061 Uiso 1 1 calc R . .
C5 C -0.0036(3) 0.1991(3) 0.0706(2) 0.0500(9) Uani 1 1 d . . .
H5A H 0.0344 0.2109 0.0151 0.060 Uiso 1 1 calc R . .
H5B H -0.0863 0.1914 0.0518 0.060 Uiso 1 1 calc R . .
C6 C 0.0451(3) 0.1133(3) 0.1170(3) 0.0500(9) Uani 1 1 d . . .
H6C H 0.0303 0.0617 0.0754 0.060 Uiso 1 1 calc R . .
H6D H 0.1285 0.1190 0.1331 0.060 Uiso 1 1 calc R . .
C7 C 0.0144(3) 0.0117(2) 0.2481(3) 0.0449(8) Uani 1 1 d . . .
H7C H 0.0978 0.0063 0.2646 0.054 Uiso 1 1 calc R . .
H7D H -0.0108 -0.0379 0.2062 0.054 Uiso 1 1 calc R . .
C8 C -0.0475(3) 0.0067(2) 0.3344(3) 0.0467(8) Uani 1 1 d . . .
H8A H -0.1310 0.0094 0.3172 0.056 Uiso 1 1 calc R . .
H8B H -0.0295 -0.0507 0.3661 0.056 Uiso 1 1 calc R . .
C9 C -0.0120(3) 0.2743(2) 0.5492(2) 0.0433(8) Uani 1 1 d . . .
H9C H 0.0154 0.3111 0.6031 0.052 Uiso 1 1 calc R . .
H9D H -0.0231 0.2125 0.5703 0.052 Uiso 1 1 calc R . .
C10 C -0.1264(3) 0.3116(2) 0.5043(2) 0.0379(7) Uani 1 1 d . . .
H10A H -0.1846 0.3086 0.5478 0.046 Uiso 1 1 calc R . .
H10B H -0.1171 0.3748 0.4869 0.046 Uiso 1 1 calc R . .
C11 C -0.2783(3) 0.2840(3) 0.3743(2) 0.0425(8) Uani 1 1 d . . .
H11A H -0.2770 0.3480 0.3576 0.051 Uiso 1 1 calc R . .
H11B H -0.3376 0.2752 0.4161 0.051 Uiso 1 1 calc R . .
C12 C -0.3057(3) 0.2271(3) 0.2882(2) 0.0435(8) Uani 1 1 d . . .
H12A H -0.3130 0.1637 0.3056 0.052 Uiso 1 1 calc R . .
H12B H -0.3793 0.2465 0.2552 0.052 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 N7 2.577(3) . ?
Gd1 N5 2.595(3) . ?
Gd1 N3 2.597(3) . ?
Gd1 N1 2.604(3) . ?
Gd1 N4 2.608(3) . ?
Gd1 N9 2.609(3) . ?
Gd1 N8 2.611(3) . ?
Gd1 N2 2.630(3) . ?
Gd1 N6 2.661(3) . ?
Ge1 S1 2.1595(8) . ?
Ge1 S2 2.1625(8) . ?
Ge1 S3 2.2716(8) . ?
Ge1 S3 2.2882(8) 3_565 ?
S3 Ge1 2.2882(8) 3_565 ?
N1 C1 1.468(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.442(5) . ?
N2 C2 1.463(4) . ?
N2 H2C 0.9100 . ?
N3 C4 1.475(5) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.475(5) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C6 1.473(4) . ?
N5 C7 1.480(4) . ?
N5 H5C 0.9100 . ?
N6 C8 1.472(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 C9 1.491(5) . ?
N7 H7A 0.9000 . ?
N7 H7B 0.9000 . ?
N8 C11 1.472(4) . ?
N8 C10 1.476(4) . ?
N8 H8C 0.9100 . ?
N9 C12 1.471(4) . ?
N9 H9A 0.9000 . ?
N9 H9B 0.9000 . ?
C1 C2 1.493(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.477(5) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.506(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.504(6) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.508(5) . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.501(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 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
N7 Gd1 N5 136.08(9) . . ?
N7 Gd1 N3 87.44(9) . . ?
N5 Gd1 N3 136.48(8) . . ?
N7 Gd1 N1 77.31(9) . . ?
N5 Gd1 N1 74.22(9) . . ?
N3 Gd1 N1 127.49(9) . . ?
N7 Gd1 N4 147.15(10) . . ?
N5 Gd1 N4 65.17(9) . . ?
N3 Gd1 N4 76.72(9) . . ?
N1 Gd1 N4 89.67(9) . . ?
N7 Gd1 N9 130.72(9) . . ?
N5 Gd1 N9 73.18(8) . . ?
N3 Gd1 N9 76.71(8) . . ?
N1 Gd1 N9 147.22(9) . . ?
N4 Gd1 N9 73.65(8) . . ?
N7 Gd1 N8 66.08(9) . . ?
N5 Gd1 N8 115.89(8) . . ?
N3 Gd1 N8 76.98(8) . . ?
N1 Gd1 N8 135.29(9) . . ?
N4 Gd1 N8 134.85(8) . . ?
N9 Gd1 N8 64.96(8) . . ?
N7 Gd1 N2 75.07(11) . . ?
N5 Gd1 N2 119.48(10) . . ?
N3 Gd1 N2 62.99(9) . . ?
N1 Gd1 N2 64.54(9) . . ?
N4 Gd1 N2 72.11(10) . . ?
N9 Gd1 N2 131.66(9) . . ?
N8 Gd1 N2 124.62(10) . . ?
N7 Gd1 N6 75.03(9) . . ?
N5 Gd1 N6 65.19(9) . . ?
N3 Gd1 N6 149.47(9) . . ?
N1 Gd1 N6 73.32(8) . . ?
N4 Gd1 N6 130.18(9) . . ?
N9 Gd1 N6 95.84(8) . . ?
N8 Gd1 N6 73.12(8) . . ?
N2 Gd1 N6 132.40(9) . . ?
S1 Ge1 S2 111.82(3) . . ?
S1 Ge1 S3 115.13(3) . . ?
S2 Ge1 S3 111.06(3) . . ?
S1 Ge1 S3 113.30(4) . 3_565 ?
S2 Ge1 S3 111.57(4) . 3_565 ?
S3 Ge1 S3 92.62(3) . 3_565 ?
Ge1 S3 Ge1 87.38(3) . 3_565 ?
C1 N1 Gd1 116.0(2) . . ?
C1 N1 H1A 108.3 . . ?
Gd1 N1 H1A 108.3 . . ?
C1 N1 H1B 108.3 . . ?
Gd1 N1 H1B 108.3 . . ?
H1A N1 H1B 107.4 . . ?
C3 N2 C2 115.0(3) . . ?
C3 N2 Gd1 119.3(2) . . ?
C2 N2 Gd1 115.3(2) . . ?
C3 N2 H2C 100.9 . . ?
C2 N2 H2C 100.9 . . ?
Gd1 N2 H2C 100.9 . . ?
C4 N3 Gd1 113.2(2) . . ?
C4 N3 H3A 108.9 . . ?
Gd1 N3 H3A 108.9 . . ?
C4 N3 H3B 108.9 . . ?
Gd1 N3 H3B 108.9 . . ?
H3A N3 H3B 107.8 . . ?
C5 N4 Gd1 115.8(2) . . ?
C5 N4 H4A 108.3 . . ?
Gd1 N4 H4A 108.3 . . ?
C5 N4 H4B 108.3 . . ?
Gd1 N4 H4B 108.3 . . ?
H4A N4 H4B 107.4 . . ?
C6 N5 C7 113.2(3) . . ?
C6 N5 Gd1 113.2(2) . . ?
C7 N5 Gd1 115.8(2) . . ?
C6 N5 H5C 104.4 . . ?
C7 N5 H5C 104.4 . . ?
Gd1 N5 H5C 104.4 . . ?
C8 N6 Gd1 113.47(19) . . ?
C8 N6 H6A 108.9 . . ?
Gd1 N6 H6A 108.9 . . ?
C8 N6 H6B 108.9 . . ?
Gd1 N6 H6B 108.9 . . ?
H6A N6 H6B 107.7 . . ?
C9 N7 Gd1 116.0(2) . . ?
C9 N7 H7A 108.3 . . ?
Gd1 N7 H7A 108.3 . . ?
C9 N7 H7B 108.3 . . ?
Gd1 N7 H7B 108.3 . . ?
H7A N7 H7B 107.4 . . ?
C11 N8 C10 112.9(3) . . ?
C11 N8 Gd1 114.75(19) . . ?
C10 N8 Gd1 112.23(19) . . ?
C11 N8 H8C 105.3 . . ?
C10 N8 H8C 105.3 . . ?
Gd1 N8 H8C 105.3 . . ?
C12 N9 Gd1 116.09(19) . . ?
C12 N9 H9A 108.3 . . ?
Gd1 N9 H9A 108.3 . . ?
C12 N9 H9B 108.3 . . ?
Gd1 N9 H9B 108.3 . . ?
H9A N9 H9B 107.4 . . ?
N1 C1 C2 109.1(4) . . ?
N1 C1 H1C 109.9 . . ?
C2 C1 H1C 109.9 . . ?
N1 C1 H1D 109.9 . . ?
C2 C1 H1D 109.9 . . ?
H1C C1 H1D 108.3 . . ?
N2 C2 C1 109.8(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 113.7(3) . . ?
N2 C3 H3C 108.8 . . ?
C4 C3 H3C 108.8 . . ?
N2 C3 H3D 108.8 . . ?
C4 C3 H3D 108.8 . . ?
H3C C3 H3D 107.7 . . ?
N3 C4 C3 113.8(3) . . ?
N3 C4 H4C 108.8 . . ?
C3 C4 H4C 108.8 . . ?
N3 C4 H4D 108.8 . . ?
C3 C4 H4D 108.8 . . ?
H4C C4 H4D 107.7 . . ?
N4 C5 C6 110.5(3) . . ?
N4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N5 C6 C5 107.2(3) . . ?
N5 C6 H6C 110.3 . . ?
C5 C6 H6C 110.3 . . ?
N5 C6 H6D 110.3 . . ?
C5 C6 H6D 110.3 . . ?
H6C C6 H6D 108.5 . . ?
N5 C7 C8 108.5(3) . . ?
N5 C7 H7C 110.0 . . ?
C8 C7 H7C 110.0 . . ?
N5 C7 H7D 110.0 . . ?
C8 C7 H7D 110.0 . . ?
H7C C7 H7D 108.4 . . ?
N6 C8 C7 110.2(3) . . ?
N6 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N6 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N7 C9 C10 110.4(3) . . ?
N7 C9 H9C 109.6 . . ?
C10 C9 H9C 109.6 . . ?
N7 C9 H9D 109.6 . . ?
C10 C9 H9D 109.6 . . ?
H9C C9 H9D 108.1 . . ?
N8 C10 C9 108.4(3) . . ?
N8 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
N8 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
N8 C11 C12 108.8(3) . . ?
N8 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
N8 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N9 C12 C11 109.9(3) . . ?
N9 C12 H12A 109.7 . . ?
C11 C12 H12A 109.7 . . ?
N9 C12 H12B 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.426
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.128
_database_code_depnum_ccdc_archive 'CCDC 1005130'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Id

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H39 Dy N9, 0.5(Ge2 S6), Cl'
_chemical_formula_sum            'C12 H39 Cl Dy Ge N9 S3'
_chemical_formula_weight         676.29

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'
Ge Ge 0.1547 1.8001 '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/n'
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   11.5035(11)
_cell_length_b                   14.6453(14)
_cell_length_c                   14.3396(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.178(2)
_cell_angle_gamma                90.00
_cell_volume                     2401.8(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            'light 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    1.870
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1348
_exptl_absorpt_coefficient_mu    4.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2759
_exptl_absorpt_correction_T_max  0.4048
_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            16686
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4237
_reflns_number_gt                3810
_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)+(0.1281P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4237
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1568
_refine_ls_wR_factor_gt          0.1476
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
Dy1 Dy 0.00057(2) 0.241827(19) 0.308519(19) 0.02162(17) Uani 1 1 d . . .
Ge1 Ge 0.36275(5) 0.00092(4) 0.49329(4) 0.0223(2) Uani 1 1 d . . .
S1 S 0.49580(12) 0.05567(12) 0.39985(11) 0.0327(4) Uani 1 1 d . . .
S2 S 0.26950(13) 0.11035(12) 0.55319(11) 0.0350(4) Uani 1 1 d . . .
S3 S 0.24660(12) -0.09938(12) 0.42454(11) 0.0337(4) Uani 1 1 d . . .
Cl1 Cl -0.26724(15) 0.04826(13) 0.08765(13) 0.0457(4) Uani 1 1 d . . .
N1 N 0.0160(5) 0.2747(5) 0.1336(4) 0.0370(13) Uani 1 1 d . . .
H1A H -0.0356 0.3189 0.1148 0.044 Uiso 1 1 calc R . .
H1B H 0.0880 0.2969 0.1281 0.044 Uiso 1 1 calc R . .
N2 N -0.0135(4) 0.0998(4) 0.2027(3) 0.0313(12) Uani 1 1 d . . .
H2C H -0.0909 0.0959 0.1817 0.038 Uiso 1 1 calc R . .
N3 N -0.0105(5) 0.0860(4) 0.3983(4) 0.0352(12) Uani 1 1 d . . .
H3A H 0.0607 0.0734 0.4278 0.042 Uiso 1 1 calc R . .
H3B H -0.0599 0.0925 0.4423 0.042 Uiso 1 1 calc R . .
N4 N -0.0557(4) 0.4107(4) 0.2946(4) 0.0331(11) Uani 1 1 d . . .
H4A H -0.0639 0.4265 0.2336 0.040 Uiso 1 1 calc R . .
H4B H -0.1253 0.4186 0.3167 0.040 Uiso 1 1 calc R . .
N5 N 0.1707(5) 0.3590(4) 0.2979(4) 0.0375(13) Uani 1 1 d . . .
H5C H 0.1728 0.3637 0.2348 0.045 Uiso 1 1 calc R . .
N6 N 0.2072(4) 0.1708(4) 0.3209(4) 0.0354(12) Uani 1 1 d . . .
H6A H 0.2276 0.1543 0.3809 0.042 Uiso 1 1 calc R . .
H6B H 0.2042 0.1197 0.2859 0.042 Uiso 1 1 calc R . .
N7 N 0.0779(5) 0.2764(4) 0.4778(4) 0.0356(12) Uani 1 1 d . . .
H7A H 0.1340 0.2354 0.4960 0.043 Uiso 1 1 calc R . .
H7B H 0.1120 0.3318 0.4794 0.043 Uiso 1 1 calc R . .
N8 N -0.1619(5) 0.2568(3) 0.4191(4) 0.0287(12) Uani 1 1 d . . .
H8C H -0.1722 0.1993 0.4408 0.034 Uiso 1 1 calc R . .
N9 N -0.2101(5) 0.2377(4) 0.2259(4) 0.0300(12) Uani 1 1 d . . .
H9A H -0.2231 0.2899 0.1934 0.036 Uiso 1 1 calc R . .
H9B H -0.2152 0.1915 0.1843 0.036 Uiso 1 1 calc R . .
C1 C -0.0046(6) 0.1970(6) 0.0695(5) 0.0462(19) Uani 1 1 d . . .
H1C H 0.0328 0.2079 0.0131 0.055 Uiso 1 1 calc R . .
H1D H -0.0879 0.1898 0.0517 0.055 Uiso 1 1 calc R . .
C2 C 0.0440(6) 0.1119(6) 0.1169(5) 0.0457(18) Uani 1 1 d . . .
H2A H 0.0288 0.0597 0.0758 0.055 Uiso 1 1 calc R . .
H2B H 0.1279 0.1176 0.1324 0.055 Uiso 1 1 calc R . .
C3 C 0.0132(6) 0.0118(5) 0.2479(5) 0.0413(16) Uani 1 1 d . . .
H3C H 0.0969 0.0054 0.2634 0.050 Uiso 1 1 calc R . .
H3D H -0.0141 -0.0375 0.2061 0.050 Uiso 1 1 calc R . .
C4 C -0.0492(6) 0.0083(5) 0.3381(5) 0.0422(16) Uani 1 1 d . . .
H4C H -0.1332 0.0109 0.3220 0.051 Uiso 1 1 calc R . .
H4D H -0.0304 -0.0485 0.3712 0.051 Uiso 1 1 calc R . .
C5 C 0.0308(6) 0.4718(5) 0.3461(5) 0.0426(16) Uani 1 1 d . . .
H5A H 0.0270 0.4646 0.4129 0.051 Uiso 1 1 calc R . .
H5B H 0.0110 0.5347 0.3299 0.051 Uiso 1 1 calc R . .
C6 C 0.1525(6) 0.4529(5) 0.3244(5) 0.0439(17) Uani 1 1 d . . .
H6C H 0.1704 0.4926 0.2737 0.053 Uiso 1 1 calc R . .
H6D H 0.2065 0.4675 0.3791 0.053 Uiso 1 1 calc R . .
C7 C 0.2871(6) 0.3240(6) 0.3290(6) 0.0482(19) Uani 1 1 d . . .
H7C H 0.2989 0.3226 0.3970 0.058 Uiso 1 1 calc R . .
H7D H 0.3459 0.3637 0.3069 0.058 Uiso 1 1 calc R . .
C8 C 0.2992(7) 0.2301(6) 0.2911(8) 0.054(2) Uani 1 1 d . . .
H8A H 0.2932 0.2323 0.2231 0.065 Uiso 1 1 calc R . .
H8B H 0.3754 0.2056 0.3137 0.065 Uiso 1 1 calc R . .
C9 C -0.0082(7) 0.2757(5) 0.5472(5) 0.0383(15) Uani 1 1 d . . .
H9C H 0.0201 0.3133 0.6006 0.046 Uiso 1 1 calc R . .
H9D H -0.0178 0.2139 0.5693 0.046 Uiso 1 1 calc R . .
C10 C -0.1248(5) 0.3120(5) 0.5037(4) 0.0337(14) Uani 1 1 d . . .
H10A H -0.1825 0.3074 0.5481 0.040 Uiso 1 1 calc R . .
H10B H -0.1174 0.3756 0.4866 0.040 Uiso 1 1 calc R . .
C11 C -0.2777(5) 0.2844(6) 0.3737(5) 0.0393(15) Uani 1 1 d . . .
H11A H -0.2772 0.3485 0.3568 0.047 Uiso 1 1 calc R . .
H11B H -0.3369 0.2750 0.4161 0.047 Uiso 1 1 calc R . .
C12 C -0.3039(6) 0.2265(6) 0.2870(5) 0.0412(17) Uani 1 1 d . . .
H12A H -0.3098 0.1629 0.3046 0.049 Uiso 1 1 calc R . .
H12B H -0.3781 0.2449 0.2536 0.049 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 N7 2.544(6) . ?
Dy1 N4 2.558(5) . ?
Dy1 N2 2.570(6) . ?
Dy1 N1 2.579(6) . ?
Dy1 N9 2.581(6) . ?
Dy1 N6 2.583(5) . ?
Dy1 N8 2.587(5) . ?
Dy1 N5 2.619(5) . ?
Dy1 N3 2.629(6) . ?
Ge1 S3 2.1521(16) . ?
Ge1 S2 2.1576(16) . ?
Ge1 S1 2.2685(15) 3_656 ?
Ge1 S1 2.2852(15) . ?
S1 Ge1 2.2685(15) 3_656 ?
N1 C1 1.466(11) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.460(9) . ?
N2 C2 1.469(8) . ?
N2 H2C 0.9100 . ?
N3 C4 1.469(10) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.476(9) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C6 1.449(9) . ?
N5 C7 1.458(9) . ?
N5 H5C 0.9100 . ?
N6 C8 1.468(10) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 C9 1.478(9) . ?
N7 H7A 0.9000 . ?
N7 H7B 0.9000 . ?
N8 C11 1.475(9) . ?
N8 C10 1.481(9) . ?
N8 H8C 0.9100 . ?
N9 C12 1.470(9) . ?
N9 H9A 0.9000 . ?
N9 H9B 0.9000 . ?
C1 C2 1.499(11) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.545(11) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.492(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.490(13) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.513(9) . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.508(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 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
N7 Dy1 N4 86.64(18) . . ?
N7 Dy1 N2 135.88(18) . . ?
N4 Dy1 N2 137.49(17) . . ?
N7 Dy1 N1 146.8(2) . . ?
N4 Dy1 N1 77.69(19) . . ?
N2 Dy1 N1 65.40(19) . . ?
N7 Dy1 N9 131.06(18) . . ?
N4 Dy1 N9 76.70(17) . . ?
N2 Dy1 N9 73.36(16) . . ?
N1 Dy1 N9 73.61(18) . . ?
N7 Dy1 N6 77.88(18) . . ?
N4 Dy1 N6 128.14(17) . . ?
N2 Dy1 N6 73.37(17) . . ?
N1 Dy1 N6 89.02(18) . . ?
N9 Dy1 N6 146.49(18) . . ?
N7 Dy1 N8 66.41(19) . . ?
N4 Dy1 N8 76.85(16) . . ?
N2 Dy1 N8 115.26(17) . . ?
N1 Dy1 N8 135.25(19) . . ?
N9 Dy1 N8 65.07(19) . . ?
N6 Dy1 N8 135.41(18) . . ?
N7 Dy1 N5 74.85(19) . . ?
N4 Dy1 N5 63.04(17) . . ?
N2 Dy1 N5 119.73(18) . . ?
N1 Dy1 N5 71.98(19) . . ?
N9 Dy1 N5 131.24(18) . . ?
N6 Dy1 N5 65.16(18) . . ?
N8 Dy1 N5 125.01(18) . . ?
N7 Dy1 N3 74.71(19) . . ?
N4 Dy1 N3 148.40(17) . . ?
N2 Dy1 N3 65.36(18) . . ?
N1 Dy1 N3 130.6(2) . . ?
N9 Dy1 N3 96.41(17) . . ?
N6 Dy1 N3 73.12(17) . . ?
N8 Dy1 N3 72.40(16) . . ?
N5 Dy1 N3 132.28(17) . . ?
S3 Ge1 S2 112.25(7) . . ?
S3 Ge1 S1 115.15(7) . 3_656 ?
S2 Ge1 S1 110.72(7) . 3_656 ?
S3 Ge1 S1 113.13(7) . . ?
S2 Ge1 S1 111.46(7) . . ?
S1 Ge1 S1 92.71(5) 3_656 . ?
Ge1 S1 Ge1 87.29(5) 3_656 . ?
C1 N1 Dy1 116.2(4) . . ?
C1 N1 H1A 108.2 . . ?
Dy1 N1 H1A 108.2 . . ?
C1 N1 H1B 108.2 . . ?
Dy1 N1 H1B 108.2 . . ?
H1A N1 H1B 107.4 . . ?
C3 N2 C2 112.7(5) . . ?
C3 N2 Dy1 117.1(4) . . ?
C2 N2 Dy1 113.0(4) . . ?
C3 N2 H2C 104.1 . . ?
C2 N2 H2C 104.1 . . ?
Dy1 N2 H2C 104.1 . . ?
C4 N3 Dy1 114.4(4) . . ?
C4 N3 H3A 108.7 . . ?
Dy1 N3 H3A 108.7 . . ?
C4 N3 H3B 108.7 . . ?
Dy1 N3 H3B 108.7 . . ?
H3A N3 H3B 107.6 . . ?
C5 N4 Dy1 113.4(4) . . ?
C5 N4 H4A 108.9 . . ?
Dy1 N4 H4A 108.9 . . ?
C5 N4 H4B 108.9 . . ?
Dy1 N4 H4B 108.9 . . ?
H4A N4 H4B 107.7 . . ?
C6 N5 C7 114.0(6) . . ?
C6 N5 Dy1 118.5(4) . . ?
C7 N5 Dy1 114.8(4) . . ?
C6 N5 H5C 102.0 . . ?
C7 N5 H5C 102.0 . . ?
Dy1 N5 H5C 102.0 . . ?
C8 N6 Dy1 115.4(4) . . ?
C8 N6 H6A 108.4 . . ?
Dy1 N6 H6A 108.4 . . ?
C8 N6 H6B 108.4 . . ?
Dy1 N6 H6B 108.4 . . ?
H6A N6 H6B 107.5 . . ?
C9 N7 Dy1 116.8(4) . . ?
C9 N7 H7A 108.1 . . ?
Dy1 N7 H7A 108.1 . . ?
C9 N7 H7B 108.1 . . ?
Dy1 N7 H7B 108.1 . . ?
H7A N7 H7B 107.3 . . ?
C11 N8 C10 112.3(5) . . ?
C11 N8 Dy1 115.5(4) . . ?
C10 N8 Dy1 112.6(4) . . ?
C11 N8 H8C 105.1 . . ?
C10 N8 H8C 105.1 . . ?
Dy1 N8 H8C 105.1 . . ?
C12 N9 Dy1 116.3(4) . . ?
C12 N9 H9A 108.2 . . ?
Dy1 N9 H9A 108.2 . . ?
C12 N9 H9B 108.2 . . ?
Dy1 N9 H9B 108.2 . . ?
H9A N9 H9B 107.4 . . ?
N1 C1 C2 109.5(6) . . ?
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 . . ?
N2 C2 C1 107.5(5) . . ?
N2 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
N2 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
N2 C3 C4 107.9(5) . . ?
N2 C3 H3C 110.1 . . ?
C4 C3 H3C 110.1 . . ?
N2 C3 H3D 110.1 . . ?
C4 C3 H3D 110.1 . . ?
H3C C3 H3D 108.4 . . ?
N3 C4 C3 109.1(5) . . ?
N3 C4 H4C 109.9 . . ?
C3 C4 H4C 109.9 . . ?
N3 C4 H4D 109.9 . . ?
C3 C4 H4D 109.9 . . ?
H4C C4 H4D 108.3 . . ?
N4 C5 C6 112.3(6) . . ?
N4 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N4 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
N5 C6 C5 113.3(5) . . ?
N5 C6 H6C 108.9 . . ?
C5 C6 H6C 108.9 . . ?
N5 C6 H6D 108.9 . . ?
C5 C6 H6D 108.9 . . ?
H6C C6 H6D 107.7 . . ?
N5 C7 C8 109.3(6) . . ?
N5 C7 H7C 109.8 . . ?
C8 C7 H7C 109.8 . . ?
N5 C7 H7D 109.8 . . ?
C8 C7 H7D 109.8 . . ?
H7C C7 H7D 108.3 . . ?
N6 C8 C7 109.9(7) . . ?
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 . . ?
N7 C9 C10 110.4(5) . . ?
N7 C9 H9C 109.6 . . ?
C10 C9 H9C 109.6 . . ?
N7 C9 H9D 109.6 . . ?
C10 C9 H9D 109.6 . . ?
H9C C9 H9D 108.1 . . ?
N8 C10 C9 108.1(5) . . ?
N8 C10 H10A 110.1 . . ?
C9 C10 H10A 110.1 . . ?
N8 C10 H10B 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N8 C11 C12 107.5(6) . . ?
N8 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
N8 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
N9 C12 C11 109.5(6) . . ?
N9 C12 H12A 109.8 . . ?
C11 C12 H12A 109.8 . . ?
N9 C12 H12B 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         4.950
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.328
_database_code_depnum_ccdc_archive 'CCDC 1005131'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_II

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H54 Er2 N12 O2, Ge2 S6'
_chemical_formula_sum            'C16 H54 Er2 Ge2 N12 O2 S6'
_chemical_formula_weight         1118.87

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn '

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

_cell_length_a                   11.710(2)
_cell_length_b                   11.318(2)
_cell_length_c                   13.548(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.635(3)
_cell_angle_gamma                90.00
_cell_volume                     1779.6(5)
_cell_formula_units_Z            2
_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          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    6.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_T_max  0.663
_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            12194
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3110
_reflns_number_gt                2946
_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)+(0.0179P)²+1.5534P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3110
_refine_ls_number_parameters     185
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0171
_refine_ls_wR_factor_ref         0.0418
_refine_ls_wR_factor_gt          0.0413
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.975202(9) 0.415313(11) 0.113013(9) 0.01691(5) Uani 1 1 d . . .
Ge1 Ge 1.01242(2) 0.02586(3) 0.38576(2) 0.01977(8) Uani 1 1 d . . .
S1 S 0.93827(7) 0.12892(7) 0.50955(6) 0.02875(17) Uani 1 1 d . . .
S2 S 0.88599(6) -0.00602(7) 0.25799(6) 0.02859(17) Uani 1 1 d . . .
S3 S 1.16373(6) 0.11155(8) 0.34111(6) 0.02925(18) Uani 1 1 d . . .
O1W O 0.91447(17) 0.4517(2) -0.04604(15) 0.0252(4) Uani 1 1 d D . .
N1 N 0.8617(2) 0.5845(2) 0.1609(2) 0.0317(6) Uani 1 1 d . . .
H1A H 0.8426 0.6297 0.1066 0.038 Uiso 1 1 calc R . .
H1B H 0.7958 0.5564 0.1793 0.038 Uiso 1 1 calc R . .
N2 N 1.0851(2) 0.5269(2) 0.26071(18) 0.0279(6) Uani 1 1 d . . .
H2C H 1.1602 0.5281 0.2501 0.034 Uiso 1 1 calc R . .
N3 N 0.9499(3) 0.3237(3) 0.2778(2) 0.0364(7) Uani 1 1 d . . .
H3A H 0.8776 0.2956 0.2742 0.044 Uiso 1 1 calc R . .
H3B H 0.9984 0.2619 0.2886 0.044 Uiso 1 1 calc R . .
N4 N 0.7696(2) 0.3423(2) 0.08768(19) 0.0244(5) Uani 1 1 d . . .
H4A H 0.7365 0.3608 0.1419 0.029 Uiso 1 1 calc R . .
H4B H 0.7309 0.3808 0.0355 0.029 Uiso 1 1 calc R . .
N5 N 0.9631(2) 0.1990(2) 0.06796(19) 0.0260(5) Uani 1 1 d . . .
H5C H 0.9731 0.1548 0.1246 0.031 Uiso 1 1 calc R . .
N6 N 1.1677(2) 0.3082(2) 0.1340(2) 0.0343(6) Uani 1 1 d . . .
H6A H 1.2215 0.3577 0.1163 0.041 Uiso 1 1 calc R . .
H6B H 1.1870 0.2912 0.1990 0.041 Uiso 1 1 calc R . .
C1 C 0.9175(3) 0.6613(3) 0.2422(3) 0.0411(9) Uani 1 1 d . . .
H1C H 0.8890 0.6402 0.3039 0.049 Uiso 1 1 calc R . .
H1D H 0.8964 0.7428 0.2273 0.049 Uiso 1 1 calc R . .
C2 C 1.0461(3) 0.6506(3) 0.2563(3) 0.0370(8) Uani 1 1 d . . .
H2A H 1.0762 0.6901 0.2016 0.044 Uiso 1 1 calc R . .
H2B H 1.0771 0.6903 0.3174 0.044 Uiso 1 1 calc R . .
C3 C 1.0828(3) 0.4688(4) 0.3570(2) 0.0432(9) Uani 1 1 d . . .
H3C H 1.0935 0.5277 0.4094 0.052 Uiso 1 1 calc R . .
H3D H 1.1463 0.4133 0.3684 0.052 Uiso 1 1 calc R . .
C4 C 0.9706(4) 0.4035(3) 0.3624(3) 0.0412(9) Uani 1 1 d . . .
H4C H 0.9755 0.3591 0.4241 0.049 Uiso 1 1 calc R . .
H4D H 0.9076 0.4595 0.3608 0.049 Uiso 1 1 calc R . .
C5 C 0.7575(3) 0.2149(3) 0.0699(2) 0.0304(7) Uani 1 1 d . . .
H5A H 0.6822 0.1982 0.0335 0.037 Uiso 1 1 calc R . .
H5B H 0.7637 0.1735 0.1331 0.037 Uiso 1 1 calc R . .
C6 C 0.8501(3) 0.1718(3) 0.0109(3) 0.0302(7) Uani 1 1 d . . .
H6C H 0.8426 0.0873 0.0000 0.036 Uiso 1 1 calc R . .
H6D H 0.8426 0.2108 -0.0533 0.036 Uiso 1 1 calc R . .
C7 C 1.0587(3) 0.1773(3) 0.0106(3) 0.0343(8) Uani 1 1 d . . .
H7A H 1.0528 0.2302 -0.0461 0.041 Uiso 1 1 calc R . .
H7B H 1.0550 0.0967 -0.0140 0.041 Uiso 1 1 calc R . .
C8 C 1.1712(3) 0.1972(3) 0.0760(3) 0.0360(8) Uani 1 1 d . . .
H8A H 1.1868 0.1311 0.1214 0.043 Uiso 1 1 calc R . .
H8B H 1.2331 0.2017 0.0351 0.043 Uiso 1 1 calc R . .
H1W H 0.850(2) 0.430(3) -0.072(3) 0.049(12) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1W 2.216(2) . ?
Er1 O1W 2.251(2) 3_765 ?
Er1 N1 2.466(3) . ?
Er1 N3 2.514(3) . ?
Er1 N5 2.523(3) . ?
Er1 N4 2.525(2) . ?
Er1 N6 2.542(3) . ?
Er1 N2 2.563(3) . ?
Er1 Er1 3.7231(5) 3_765 ?
Ge1 S2 2.1535(8) . ?
Ge1 S3 2.1750(8) . ?
Ge1 S1 2.2795(9) 3_756 ?
Ge1 S1 2.3053(8) . ?
S1 Ge1 2.2795(9) 3_756 ?
O1W Er1 2.251(2) 3_765 ?
O1W H1W 0.833(19) . ?
N1 C1 1.485(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.464(4) . ?
N2 C2 1.471(5) . ?
N2 H2C 0.9100 . ?
N3 C4 1.455(5) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.466(4) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.465(4) . ?
N5 C6 1.474(4) . ?
N5 H5C 0.9100 . ?
N6 C8 1.485(4) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.498(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.518(5) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.510(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.505(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
O1W Er1 O1W 67.11(8) . 3_765 ?
O1W Er1 N1 89.83(9) . . ?
O1W Er1 N1 86.87(9) 3_765 . ?
O1W Er1 N3 151.59(8) . . ?
O1W Er1 N3 140.81(8) 3_765 . ?
N1 Er1 N3 87.44(10) . . ?
O1W Er1 N5 86.84(8) . . ?
O1W Er1 N5 124.60(8) 3_765 . ?
N1 Er1 N5 143.35(8) . . ?
N3 Er1 N5 78.77(9) . . ?
O1W Er1 N4 75.62(8) . . ?
O1W Er1 N4 138.74(8) 3_765 . ?
N1 Er1 N4 75.67(8) . . ?
N3 Er1 N4 76.30(9) . . ?
N5 Er1 N4 68.14(8) . . ?
O1W Er1 N6 111.27(9) . . ?
O1W Er1 N6 79.41(9) 3_765 . ?
N1 Er1 N6 147.32(9) . . ?
N3 Er1 N6 84.90(10) . . ?
N5 Er1 N6 65.45(8) . . ?
N4 Er1 N6 132.40(9) . . ?
O1W Er1 N2 136.91(8) . . ?
O1W Er1 N2 74.32(8) 3_765 . ?
N1 Er1 N2 69.16(9) . . ?
N3 Er1 N2 67.43(8) . . ?
N5 Er1 N2 132.32(8) . . ?
N4 Er1 N2 129.65(8) . . ?
N6 Er1 N2 78.58(9) . . ?
O1W Er1 Er1 33.85(5) . 3_765 ?
O1W Er1 Er1 33.26(5) 3_765 3_765 ?
N1 Er1 Er1 88.01(7) . 3_765 ?
N3 Er1 Er1 172.84(7) . 3_765 ?
N5 Er1 Er1 108.09(6) . 3_765 ?
N4 Er1 Er1 107.86(6) . 3_765 ?
N6 Er1 Er1 96.01(7) . 3_765 ?
N2 Er1 Er1 105.74(6) . 3_765 ?
S2 Ge1 S3 110.47(3) . . ?
S2 Ge1 S1 117.50(3) . 3_756 ?
S3 Ge1 S1 111.55(3) . 3_756 ?
S2 Ge1 S1 112.60(3) . . ?
S3 Ge1 S1 112.10(4) . . ?
S1 Ge1 S1 91.42(3) 3_756 . ?
Ge1 S1 Ge1 88.58(3) 3_756 . ?
Er1 O1W Er1 112.89(8) . 3_765 ?
Er1 O1W H1W 121(3) . . ?
Er1 O1W H1W 124(3) 3_765 . ?
C1 N1 Er1 116.8(2) . . ?
C1 N1 H1A 108.1 . . ?
Er1 N1 H1A 108.1 . . ?
C1 N1 H1B 108.1 . . ?
Er1 N1 H1B 108.1 . . ?
H1A N1 H1B 107.3 . . ?
C3 N2 C2 114.9(3) . . ?
C3 N2 Er1 114.0(2) . . ?
C2 N2 Er1 108.42(19) . . ?
C3 N2 H2C 106.3 . . ?
C2 N2 H2C 106.3 . . ?
Er1 N2 H2C 106.3 . . ?
C4 N3 Er1 114.7(2) . . ?
C4 N3 H3A 108.6 . . ?
Er1 N3 H3A 108.6 . . ?
C4 N3 H3B 108.6 . . ?
Er1 N3 H3B 108.6 . . ?
H3A N3 H3B 107.6 . . ?
C5 N4 Er1 114.46(17) . . ?
C5 N4 H4A 108.6 . . ?
Er1 N4 H4A 108.6 . . ?
C5 N4 H4B 108.6 . . ?
Er1 N4 H4B 108.6 . . ?
H4A N4 H4B 107.6 . . ?
C7 N5 C6 112.5(3) . . ?
C7 N5 Er1 105.59(19) . . ?
C6 N5 Er1 110.31(18) . . ?
C7 N5 H5C 109.4 . . ?
C6 N5 H5C 109.4 . . ?
Er1 N5 H5C 109.4 . . ?
C8 N6 Er1 115.54(19) . . ?
C8 N6 H6A 108.4 . . ?
Er1 N6 H6A 108.4 . . ?
C8 N6 H6B 108.4 . . ?
Er1 N6 H6B 108.4 . . ?
H6A N6 H6B 107.5 . . ?
N1 C1 C2 112.5(3) . . ?
N1 C1 H1C 109.1 . . ?
C2 C1 H1C 109.1 . . ?
N1 C1 H1D 109.1 . . ?
C2 C1 H1D 109.1 . . ?
H1C C1 H1D 107.8 . . ?
N2 C2 C1 112.5(3) . . ?
N2 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N2 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 C4 112.3(3) . . ?
N2 C3 H3C 109.1 . . ?
C4 C3 H3C 109.1 . . ?
N2 C3 H3D 109.1 . . ?
C4 C3 H3D 109.1 . . ?
H3C C3 H3D 107.9 . . ?
N3 C4 C3 108.6(3) . . ?
N3 C4 H4C 110.0 . . ?
C3 C4 H4C 110.0 . . ?
N3 C4 H4D 110.0 . . ?
C3 C4 H4D 110.0 . . ?
H4C C4 H4D 108.4 . . ?
N4 C5 C6 110.1(2) . . ?
N4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N5 C6 C5 108.2(3) . . ?
N5 C6 H6C 110.0 . . ?
C5 C6 H6C 110.0 . . ?
N5 C6 H6D 110.0 . . ?
C5 C6 H6D 110.0 . . ?
H6C C6 H6D 108.4 . . ?
N5 C7 C8 109.5(3) . . ?
N5 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N5 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
N6 C8 C7 110.8(3) . . ?
N6 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N6 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.119
_database_code_depnum_ccdc_archive 'CCDC 1005132'
