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

#######################################################################
#
#                 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.
#
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#  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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data_jlgeo16

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H41 Co Ge2 N9 S6'
_chemical_formula_weight         708.01

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3224(3)
_cell_length_b                   14.6492(4)
_cell_length_c                   18.3710(5)
_cell_angle_alpha                71.000(2)
_cell_angle_beta                 78.352(2)
_cell_angle_gamma                73.441(2)
_cell_volume                     2741.51(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      4
_cell_measurement_theta_max      26

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_absorpt_coefficient_mu    3.254
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5285
_exptl_absorpt_correction_T_max  0.6177
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38362
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         27.97
_reflns_number_total             13102
_reflns_number_gt                10537
_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)+(0.0415P)²+1.8145P] 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       0.00077(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13102
_refine_ls_number_parameters     552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0908
_refine_ls_wR_factor_gt          0.0854
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Ge1 Ge 0.14038(3) 0.68746(3) -0.01091(2) 0.03081(8) Uani 1 1 d . . .
Ge2 Ge -0.11220(3) 0.79427(2) 0.061902(19) 0.02882(8) Uani 1 1 d . . .
S1 S 0.24264(9) 0.54549(7) 0.05302(6) 0.0474(2) Uani 1 1 d . . .
S2 S 0.22822(8) 0.75591(7) -0.12328(5) 0.03772(18) Uani 1 1 d . . .
S3 S 0.08811(7) 0.79056(7) 0.06686(5) 0.03462(17) Uani 1 1 d . . .
S4 S -0.05957(8) 0.68884(7) -0.01287(5) 0.03802(19) Uani 1 1 d . . .
S5 S -0.20072(8) 0.72953(7) 0.17578(5) 0.03844(19) Uani 1 1 d . . .
S6 S -0.20871(8) 0.94065(7) 0.00048(6) 0.0407(2) Uani 1 1 d . . .
Ge11 Ge 0.13739(3) 0.27109(2) 0.475258(19) 0.02915(8) Uani 1 1 d . . .
Ge12 Ge -0.12784(3) 0.23568(2) 0.539074(19) 0.02910(8) Uani 1 1 d . . .
S11 S 0.24576(8) 0.28833(8) 0.55172(6) 0.0427(2) Uani 1 1 d . . .
S12 S 0.23325(8) 0.27092(7) 0.36120(5) 0.03788(19) Uani 1 1 d . . .
S13 S -0.05488(7) 0.37447(6) 0.47376(5) 0.03589(18) Uani 1 1 d . . .
S14 S 0.06415(7) 0.13190(6) 0.53420(5) 0.03382(17) Uani 1 1 d . . .
S15 S -0.21126(8) 0.23996(7) 0.65463(5) 0.04001(19) Uani 1 1 d . . .
S16 S -0.24345(8) 0.21385(8) 0.46908(6) 0.0430(2) Uani 1 1 d . . .
Co1 Co 0.46874(4) 0.25354(3) -0.00339(2) 0.03042(10) Uani 1 1 d . . .
N1 N 0.6054(3) 0.1334(2) 0.06100(17) 0.0386(6) Uani 1 1 d . . .
H1N H 0.6441 0.0917 0.0322 0.046 Uiso 1 1 calc R . .
H2N H 0.6627 0.1586 0.0703 0.046 Uiso 1 1 calc R . .
C1 C 0.5475(4) 0.0782(3) 0.1348(2) 0.0453(9) Uani 1 1 d . . .
H1A H 0.5563 0.1025 0.1762 0.054 Uiso 1 1 calc R . .
H1B H 0.5900 0.0084 0.1461 0.054 Uiso 1 1 calc R . .
C2 C 0.4114(4) 0.0891(3) 0.1323(2) 0.0455(9) Uani 1 1 d . . .
H2A H 0.4034 0.0470 0.1032 0.055 Uiso 1 1 calc R . .
H2B H 0.3716 0.0667 0.1847 0.055 Uiso 1 1 calc R . .
N2 N 0.3469(3) 0.1928(2) 0.09625(16) 0.0354(6) Uani 1 1 d . . .
H3N H 0.2770 0.1919 0.0795 0.042 Uiso 1 1 calc R . .
C3 C 0.3117(3) 0.2595(3) 0.1463(2) 0.0439(8) Uani 1 1 d . . .
H3A H 0.2853 0.2228 0.1986 0.053 Uiso 1 1 calc R . .
H3B H 0.2419 0.3132 0.1277 0.053 Uiso 1 1 calc R . .
C4 C 0.4165(4) 0.3029(3) 0.1484(2) 0.0431(8) Uani 1 1 d . . .
H4A H 0.3846 0.3559 0.1731 0.052 Uiso 1 1 calc R . .
H4B H 0.4778 0.2520 0.1788 0.052 Uiso 1 1 calc R . .
N3 N 0.4752(3) 0.3424(2) 0.06915(16) 0.0350(6) Uani 1 1 d . . .
H4N H 0.5546 0.3411 0.0706 0.042 Uiso 1 1 calc R . .
H5N H 0.4352 0.4058 0.0491 0.042 Uiso 1 1 calc R . .
N11 N 0.4765(3) 0.1577(3) -0.07490(19) 0.0494(8) Uani 1 1 d . . .
H6N H 0.5070 0.0940 -0.0490 0.059 Uiso 1 1 calc R . .
H7N H 0.3993 0.1634 -0.0842 0.059 Uiso 1 1 calc R . .
C11 C 0.5522(6) 0.1834(4) -0.1463(3) 0.0744(15) Uani 1 1 d . . .
H11A H 0.4988 0.2211 -0.1865 0.089 Uiso 1 1 calc R . .
H11B H 0.5991 0.1227 -0.1589 0.089 Uiso 1 1 calc R . .
C12 C 0.6377(5) 0.2402(5) -0.1481(3) 0.0827(19) Uani 1 1 d . . .
H12A H 0.6614 0.2742 -0.2017 0.099 Uiso 1 1 calc R . .
H12B H 0.7120 0.1946 -0.1275 0.099 Uiso 1 1 calc R . .
N12 N 0.5898(3) 0.3153(3) -0.10382(17) 0.0435(7) Uani 1 1 d . . .
H8N H 0.6551 0.3241 -0.0872 0.052 Uiso 1 1 calc R . .
C13 C 0.5218(5) 0.4111(5) -0.1467(4) 0.114(3) Uani 1 1 d . . .
H13A H 0.5658 0.4600 -0.1486 0.137 Uiso 1 1 calc R . .
H13B H 0.5266 0.4093 -0.1995 0.137 Uiso 1 1 calc R . .
C14 C 0.3999(5) 0.4458(4) -0.1222(3) 0.086(2) Uani 1 1 d . . .
H14A H 0.3555 0.4727 -0.1674 0.103 Uiso 1 1 calc R . .
H14B H 0.3948 0.5008 -0.1024 0.103 Uiso 1 1 calc R . .
N13 N 0.3340(3) 0.3787(2) -0.06427(17) 0.0404(7) Uani 1 1 d . . .
H9N H 0.2876 0.3575 -0.0868 0.048 Uiso 1 1 calc R . .
H10N H 0.2834 0.4100 -0.0307 0.048 Uiso 1 1 calc R . .
Co2 Co 0.5000 0.5000 0.5000 0.02949(13) Uani 1 2 d S . .
N21 N 0.5049(3) 0.6482(2) 0.42672(16) 0.0351(6) Uani 1 1 d . . .
H11N H 0.4272 0.6865 0.4242 0.042 Uiso 1 1 calc R . .
H12N H 0.5479 0.6753 0.4469 0.042 Uiso 1 1 calc R . .
C21 C 0.5642(4) 0.6443(3) 0.3483(2) 0.0410(8) Uani 1 1 d . . .
H21A H 0.6047 0.6989 0.3245 0.049 Uiso 1 1 calc R . .
H21B H 0.5014 0.6516 0.3165 0.049 Uiso 1 1 calc R . .
C22 C 0.6585(3) 0.5471(3) 0.3516(2) 0.0433(8) Uani 1 1 d . . .
H22A H 0.6850 0.5409 0.2995 0.052 Uiso 1 1 calc R . .
H22B H 0.7307 0.5471 0.3725 0.052 Uiso 1 1 calc R . .
N22 N 0.6085(3) 0.4613(2) 0.39994(16) 0.0357(6) Uani 1 1 d . . .
H13N H 0.6735 0.4095 0.4161 0.043 Uiso 1 1 calc R . .
C23 C 0.5314(4) 0.4275(3) 0.3631(2) 0.0444(8) Uani 1 1 d . . .
H23A H 0.5354 0.3576 0.3886 0.053 Uiso 1 1 calc R . .
H23B H 0.5656 0.4343 0.3093 0.053 Uiso 1 1 calc R . .
C24 C 0.3974(4) 0.4840(3) 0.3663(2) 0.0454(9) Uani 1 1 d . . .
H24A H 0.3897 0.5479 0.3272 0.054 Uiso 1 1 calc R . .
H24B H 0.3480 0.4474 0.3546 0.054 Uiso 1 1 calc R . .
N23 N 0.3494(3) 0.4996(2) 0.44234(17) 0.0383(6) Uani 1 1 d . . .
H14N H 0.3118 0.4509 0.4716 0.046 Uiso 1 1 calc R . .
H15N H 0.2928 0.5579 0.4369 0.046 Uiso 1 1 calc R . .
Co3 Co 0.5000 0.0000 0.5000 0.03074(13) Uani 1 2 d S . .
N31 N 0.5148(3) 0.1471(2) 0.42788(17) 0.0406(7) Uani 1 1 d . . .
H16N H 0.4390 0.1888 0.4262 0.049 Uiso 1 1 calc R . .
H17N H 0.5622 0.1703 0.4482 0.049 Uiso 1 1 calc R . .
C31 C 0.5700(4) 0.1433(3) 0.3495(2) 0.0533(10) Uani 1 1 d . . .
H31A H 0.6165 0.1943 0.3266 0.064 Uiso 1 1 calc R . .
H31B H 0.5047 0.1570 0.3178 0.064 Uiso 1 1 calc R . .
C32 C 0.6554(4) 0.0428(4) 0.3502(2) 0.0535(10) Uani 1 1 d . . .
H32A H 0.6762 0.0379 0.2975 0.064 Uiso 1 1 calc R . .
H32B H 0.7318 0.0372 0.3693 0.064 Uiso 1 1 calc R . .
N32 N 0.6004(3) -0.0399(2) 0.39853(17) 0.0427(7) Uani 1 1 d . . .
H18N H 0.6634 -0.0940 0.4137 0.051 Uiso 1 1 calc R . .
C33 C 0.5168(4) -0.0685(3) 0.3623(2) 0.0540(10) Uani 1 1 d . . .
H33A H 0.5158 -0.1376 0.3880 0.065 Uiso 1 1 calc R . .
H33B H 0.5496 -0.0628 0.3084 0.065 Uiso 1 1 calc R . .
C34 C 0.3870(4) -0.0069(3) 0.3661(2) 0.0526(10) Uani 1 1 d . . .
H34A H 0.3832 0.0572 0.3275 0.063 Uiso 1 1 calc R . .
H34B H 0.3329 -0.0394 0.3540 0.063 Uiso 1 1 calc R . .
N33 N 0.3433(3) 0.0078(2) 0.44277(17) 0.0390(6) Uani 1 1 d . . .
H19N H 0.3030 -0.0392 0.4719 0.047 Uiso 1 1 calc R . .
H20N H 0.2897 0.0675 0.4382 0.047 Uiso 1 1 calc R . .
N41 N 0.0555(3) 0.9750(2) -0.10497(17) 0.0423(7) Uani 1 1 d . . .
H21N H -0.0234 0.9727 -0.0886 0.063 Uiso 1 1 calc R . .
H22N H 0.0855 0.9915 -0.0711 0.063 Uiso 1 1 calc R . .
H23N H 0.0997 0.9157 -0.1093 0.063 Uiso 1 1 calc R . .
C41 C 0.0634(5) 1.0500(4) -0.1814(2) 0.0637(13) Uani 1 1 d . . .
H41A H 0.0003 1.1103 -0.1796 0.076 Uiso 1 1 calc R . .
H41B H 0.1438 1.0661 -0.1922 0.076 Uiso 1 1 calc R . .
C42 C 0.0465(5) 1.0151(4) -0.2446(3) 0.0619(11) Uani 1 1 d . . .
H42A H 0.0577 1.0648 -0.2938 0.074 Uiso 1 1 calc R . .
H42B H 0.1090 0.9544 -0.2462 0.074 Uiso 1 1 calc R . .
N42 N -0.0744(4) 0.9966(3) -0.2338(2) 0.0622(10) Uani 1 1 d . . .
H24N H -0.1223 1.0485 -0.2652 0.075 Uiso 1 1 d R . .
C43 C -0.0743(5) 0.9077(4) -0.2507(3) 0.0674(13) Uani 1 1 d . . .
H43A H -0.1589 0.8999 -0.2403 0.081 Uiso 1 1 calc R . .
H43B H -0.0259 0.8516 -0.2152 0.081 Uiso 1 1 calc R . .
C44 C -0.0227(5) 0.9027(4) -0.3347(3) 0.0604(11) Uani 1 1 d . . .
H44A H -0.0822 0.9466 -0.3697 0.072 Uiso 1 1 calc R . .
H44B H 0.0536 0.9254 -0.3504 0.072 Uiso 1 1 calc R . .
N43 N 0.0016(3) 0.8011(3) -0.34012(18) 0.0487(8) Uani 1 1 d . . .
H25N H 0.0285 0.7580 -0.2965 0.073 Uiso 1 1 calc R . .
H26N H 0.0592 0.7936 -0.3800 0.073 Uiso 1 1 calc R . .
H27N H -0.0680 0.7900 -0.3471 0.073 Uiso 1 1 calc R . .
N51 N -0.0238(3) 0.6965(3) 0.31519(18) 0.0454(7) Uani 1 1 d . . .
H28N H 0.0318 0.7304 0.3123 0.068 Uiso 1 1 calc R . .
H29N H -0.0833 0.7049 0.3539 0.068 Uiso 1 1 calc R . .
H30N H -0.0568 0.7186 0.2708 0.068 Uiso 1 1 calc R . .
C51 C 0.0378(4) 0.5898(3) 0.3293(2) 0.0459(9) Uani 1 1 d . . .
H51A H -0.0252 0.5517 0.3461 0.055 Uiso 1 1 calc R . .
H51B H 0.0886 0.5699 0.3711 0.055 Uiso 1 1 calc R . .
C52 C 0.1179(3) 0.5650(3) 0.2592(2) 0.0436(8) Uani 1 1 d . . .
H52A H 0.1606 0.6175 0.2320 0.052 Uiso 1 1 calc R . .
H52B H 0.1804 0.5041 0.2762 0.052 Uiso 1 1 calc R . .
N52 N 0.0477(3) 0.5521(2) 0.20428(16) 0.0372(6) Uani 1 1 d . . .
H31N H -0.0181 0.6042 0.1946 0.045 Uiso 1 1 calc R . .
H32N H 0.0968 0.5520 0.1592 0.045 Uiso 1 1 calc R . .
C53 C 0.0033(4) 0.4588(3) 0.2344(2) 0.0476(9) Uani 1 1 d . B .
H53A H -0.0522 0.4600 0.2819 0.057 Uiso 1 1 calc R . .
H53B H 0.0738 0.4027 0.2467 0.057 Uiso 1 1 calc R . .
C54 C -0.0629(5) 0.4445(3) 0.1778(3) 0.0592(12) Uani 1 1 d . . .
H54A H -0.0049 0.4301 0.1340 0.071 Uiso 0.80 1 calc PR A 1
H54B H -0.1261 0.5040 0.1588 0.071 Uiso 0.80 1 calc PR A 1
H54C H -0.1482 0.4827 0.1815 0.071 Uiso 0.20 1 d PR A 2
H54D H -0.0240 0.4702 0.1257 0.071 Uiso 0.20 1 d PR A 2
N53 N -0.1211(5) 0.3585(4) 0.2206(4) 0.0660(15) Uani 0.80 1 d P B 1
H33N H -0.1279 0.3365 0.1822 0.099 Uiso 1 1 d R . .
H34N H -0.2035 0.3761 0.2291 0.099 Uiso 0.80 1 d PR C 1
N53' N -0.0605(15) 0.3502(12) 0.1895(9) 0.035(3) Uiso 0.20 1 d P B 2
H35N H -0.0364 0.3355 0.1446 0.052 Uiso 0.20 1 d PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 S1 2.1521(10) . ?
Ge1 S2 2.1559(9) . ?
Ge1 S4 2.2658(9) . ?
Ge1 S3 2.2862(9) . ?
Ge2 S6 2.1569(9) . ?
Ge2 S5 2.1643(9) . ?
Ge2 S4 2.2701(9) . ?
Ge2 S3 2.2727(8) . ?
Ge11 S11 2.1555(9) . ?
Ge11 S12 2.1568(9) . ?
Ge11 S13 2.2697(9) . ?
Ge11 S14 2.2762(8) . ?
Ge12 S15 2.1554(9) . ?
Ge12 S16 2.1576(9) . ?
Ge12 S14 2.2740(9) . ?
Ge12 S13 2.2858(9) . ?
Co1 N2 2.160(3) . ?
Co1 N3 2.167(3) . ?
Co1 N12 2.168(3) . ?
Co1 N13 2.168(3) . ?
Co1 N1 2.173(3) . ?
Co1 N11 2.188(3) . ?
N1 C1 1.467(5) . ?
C1 C2 1.512(5) . ?
C2 N2 1.478(5) . ?
N2 C3 1.475(5) . ?
C3 C4 1.509(5) . ?
C4 N3 1.475(4) . ?
N11 C11 1.416(5) . ?
C11 C12 1.434(7) . ?
C12 N12 1.494(6) . ?
N12 C13 1.446(6) . ?
C13 C14 1.365(7) . ?
C14 N13 1.439(5) . ?
Co2 N22 2.140(3) . ?
Co2 N22 2.140(3) 2_666 ?
Co2 N21 2.160(3) . ?
Co2 N21 2.160(3) 2_666 ?
Co2 N23 2.184(3) 2_666 ?
Co2 N23 2.184(3) . ?
N21 C21 1.474(4) . ?
C21 C22 1.508(5) . ?
C22 N22 1.472(5) . ?
N22 C23 1.472(4) . ?
C23 C24 1.507(6) . ?
C24 N23 1.459(5) . ?
Co3 N32 2.141(3) . ?
Co3 N32 2.141(3) 2_656 ?
Co3 N31 2.165(3) 2_656 ?
Co3 N31 2.165(3) . ?
Co3 N33 2.197(3) . ?
Co3 N33 2.197(3) 2_656 ?
N31 C31 1.461(5) . ?
C31 C32 1.512(6) . ?
C32 N32 1.466(5) . ?
N32 C33 1.475(5) . ?
C33 C34 1.491(6) . ?
C34 N33 1.460(5) . ?
N41 C41 1.479(5) . ?
C41 C42 1.477(6) . ?
C42 N42 1.433(6) . ?
N42 C43 1.435(6) . ?
C43 C44 1.553(7) . ?
C44 N43 1.467(6) . ?
N51 C51 1.479(5) . ?
C51 C52 1.504(6) . ?
C52 N52 1.489(4) . ?
N52 C53 1.488(5) . ?
C53 C54 1.494(5) . ?
C54 N53' 1.321(17) . ?
C54 N53 1.503(7) . ?

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
S1 Ge1 S2 116.67(4) . . ?
S1 Ge1 S4 112.55(4) . . ?
S2 Ge1 S4 112.73(4) . . ?
S1 Ge1 S3 107.70(4) . . ?
S2 Ge1 S3 111.17(4) . . ?
S4 Ge1 S3 93.50(3) . . ?
S6 Ge2 S5 115.92(4) . . ?
S6 Ge2 S4 111.47(4) . . ?
S5 Ge2 S4 111.80(4) . . ?
S6 Ge2 S3 110.89(4) . . ?
S5 Ge2 S3 110.89(3) . . ?
S4 Ge2 S3 93.75(3) . . ?
Ge2 S3 Ge1 86.09(3) . . ?
Ge1 S4 Ge2 86.63(3) . . ?
S11 Ge11 S12 114.38(4) . . ?
S11 Ge11 S13 112.70(4) . . ?
S12 Ge11 S13 113.56(3) . . ?
S11 Ge11 S14 108.97(4) . . ?
S12 Ge11 S14 111.71(4) . . ?
S13 Ge11 S14 93.60(3) . . ?
S15 Ge12 S16 115.66(4) . . ?
S15 Ge12 S14 114.01(4) . . ?
S16 Ge12 S14 111.14(4) . . ?
S15 Ge12 S13 111.04(4) . . ?
S16 Ge12 S13 109.50(4) . . ?
S14 Ge12 S13 93.23(3) . . ?
Ge11 S13 Ge12 86.44(3) . . ?
Ge12 S14 Ge11 86.56(3) . . ?
N2 Co1 N3 81.46(11) . . ?
N2 Co1 N12 179.56(12) . . ?
N3 Co1 N12 98.59(12) . . ?
N2 Co1 N13 99.16(11) . . ?
N3 Co1 N13 88.15(12) . . ?
N12 Co1 N13 80.40(12) . . ?
N2 Co1 N1 80.83(11) . . ?
N3 Co1 N1 88.68(11) . . ?
N12 Co1 N1 99.61(12) . . ?
N13 Co1 N1 176.79(12) . . ?
N2 Co1 N11 99.82(12) . . ?
N3 Co1 N11 175.67(12) . . ?
N12 Co1 N11 80.17(13) . . ?
N13 Co1 N11 95.71(13) . . ?
N1 Co1 N11 87.44(13) . . ?
C1 N1 Co1 111.4(2) . . ?
N1 C1 C2 111.4(3) . . ?
N2 C2 C1 112.5(3) . . ?
C3 N2 C2 115.9(3) . . ?
C3 N2 Co1 108.2(2) . . ?
C2 N2 Co1 107.4(2) . . ?
N2 C3 C4 112.8(3) . . ?
N3 C4 C3 110.5(3) . . ?
C4 N3 Co1 109.9(2) . . ?
C11 N11 Co1 111.3(3) . . ?
N11 C11 C12 115.4(4) . . ?
C11 C12 N12 115.1(4) . . ?
C13 N12 C12 115.0(5) . . ?
C13 N12 Co1 108.8(3) . . ?
C12 N12 Co1 107.1(3) . . ?
C14 C13 N12 119.8(4) . . ?
C13 C14 N13 119.1(4) . . ?
C14 N13 Co1 108.4(3) . . ?
N22 Co2 N22 180.000(1) . 2_666 ?
N22 Co2 N21 81.81(11) . . ?
N22 Co2 N21 98.19(11) 2_666 . ?
N22 Co2 N21 98.19(11) . 2_666 ?
N22 Co2 N21 81.81(11) 2_666 2_666 ?
N21 Co2 N21 180.000(1) . 2_666 ?
N22 Co2 N23 98.60(11) . 2_666 ?
N22 Co2 N23 81.40(11) 2_666 2_666 ?
N21 Co2 N23 89.60(11) . 2_666 ?
N21 Co2 N23 90.40(11) 2_666 2_666 ?
N22 Co2 N23 81.40(11) . . ?
N22 Co2 N23 98.60(11) 2_666 . ?
N21 Co2 N23 90.40(11) . . ?
N21 Co2 N23 89.60(11) 2_666 . ?
N23 Co2 N23 180.000(1) 2_666 . ?
C21 N21 Co2 109.7(2) . . ?
N21 C21 C22 110.7(3) . . ?
N22 C22 C21 112.1(3) . . ?
C22 N22 C23 116.4(3) . . ?
C22 N22 Co2 107.5(2) . . ?
C23 N22 Co2 108.5(2) . . ?
N22 C23 C24 113.6(3) . . ?
N23 C24 C23 111.7(3) . . ?
C24 N23 Co2 110.4(2) . . ?
N32 Co3 N32 180.0 . 2_656 ?
N32 Co3 N31 98.05(12) . 2_656 ?
N32 Co3 N31 81.95(12) 2_656 2_656 ?
N32 Co3 N31 81.95(12) . . ?
N32 Co3 N31 98.05(12) 2_656 . ?
N31 Co3 N31 180.00(16) 2_656 . ?
N32 Co3 N33 80.64(11) . . ?
N32 Co3 N33 99.36(11) 2_656 . ?
N31 Co3 N33 88.91(11) 2_656 . ?
N31 Co3 N33 91.09(11) . . ?
N32 Co3 N33 99.36(11) . 2_656 ?
N32 Co3 N33 80.64(11) 2_656 2_656 ?
N31 Co3 N33 91.09(11) 2_656 2_656 ?
N31 Co3 N33 88.91(11) . 2_656 ?
N33 Co3 N33 180.00(13) . 2_656 ?
C31 N31 Co3 109.8(2) . . ?
N31 C31 C32 111.3(3) . . ?
N32 C32 C31 112.9(3) . . ?
C32 N32 C33 116.4(3) . . ?
C32 N32 Co3 107.4(3) . . ?
C33 N32 Co3 108.7(2) . . ?
N32 C33 C34 113.6(3) . . ?
N33 C34 C33 111.4(3) . . ?
C34 N33 Co3 110.5(2) . . ?
C42 C41 N41 112.3(4) . . ?
N42 C42 C41 111.2(4) . . ?
C42 N42 C43 113.7(4) . . ?
N42 C43 C44 116.2(4) . . ?
N43 C44 C43 111.2(4) . . ?
N51 C51 C52 113.4(3) . . ?
N52 C52 C51 113.7(3) . . ?
C53 N52 C52 113.0(3) . . ?
N52 C53 C54 112.7(3) . . ?
N53' C54 C53 112.5(8) . . ?
N53' C54 N53 32.4(7) . . ?
C53 C54 N53 106.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.97
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 985614'
#######################################################################
#
#                 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_jl33

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H41 Co Ge2 N9 S6'
_chemical_formula_weight         708.01

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2034(5)
_cell_length_b                   9.2773(6)
_cell_length_c                   11.4365(8)
_cell_angle_alpha                74.107(5)
_cell_angle_beta                 73.402(5)
_cell_angle_gamma                71.293(5)
_cell_volume                     679.62(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7633
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      27.9

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             363
_exptl_absorpt_coefficient_mu    3.282
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5423
_exptl_absorpt_correction_T_max  0.6735
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7633
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         27.88
_reflns_number_total             3205
_reflns_number_gt                2933
_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)+(0.0332P)²+0.6343P] 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         3205
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_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
Ge1 Ge 0.61106(4) 0.57601(3) 0.87121(2) 0.02760(8) Uani 1 1 d . . .
S1 S 0.47795(12) 0.79369(8) 0.76345(7) 0.04101(16) Uani 1 1 d . . .
S2 S 0.91607(10) 0.46218(9) 0.79262(7) 0.04195(17) Uani 1 1 d . . .
S3 S 0.41586(10) 0.40718(8) 0.92929(6) 0.03283(14) Uani 1 1 d . . .
Co1 Co 0.5000 0.5000 0.5000 0.02784(11) Uani 1 2 d S . .
N1 N 0.2932(4) 0.3633(3) 0.5162(2) 0.0367(5) Uani 1 1 d . . .
H1N H 0.1696 0.4079 0.5564 0.044 Uiso 1 1 calc R . .
H2N H 0.2859 0.3595 0.4399 0.044 Uiso 1 1 calc R . .
C1 C 0.3667(5) 0.2047(3) 0.5858(3) 0.0429(6) Uani 1 1 d . . .
H1A H 0.4661 0.1421 0.5294 0.052 Uiso 1 1 calc R . .
H1B H 0.2561 0.1570 0.6225 0.052 Uiso 1 1 calc R . .
C2 C 0.4588(5) 0.2107(3) 0.6869(3) 0.0440(7) Uani 1 1 d . . .
H2A H 0.3529 0.2541 0.7520 0.053 Uiso 1 1 calc R . .
H2B H 0.5247 0.1057 0.7233 0.053 Uiso 1 1 calc R . .
N2 N 0.6058(4) 0.3043(3) 0.6407(2) 0.0346(5) Uani 1 1 d . . .
H3N H 0.6100 0.3418 0.7053 0.042 Uiso 1 1 calc R . .
C3 C 0.8120(5) 0.2246(4) 0.5863(3) 0.0489(7) Uani 1 1 d . . .
H3A H 0.8477 0.1210 0.6361 0.059 Uiso 1 1 calc R . .
H3B H 0.9031 0.2804 0.5893 0.059 Uiso 1 1 calc R . .
C4 C 0.8385(5) 0.2127(4) 0.4533(3) 0.0481(7) Uani 1 1 d . . .
H4A H 0.9803 0.1894 0.4143 0.058 Uiso 1 1 calc R . .
H4B H 0.7878 0.1281 0.4524 0.058 Uiso 1 1 calc R . .
N3 N 0.7321(3) 0.3576(3) 0.3818(2) 0.0361(5) Uani 1 1 d . . .
H4N H 0.6770 0.3346 0.3302 0.043 Uiso 1 1 calc R . .
H5N H 0.8209 0.4117 0.3349 0.043 Uiso 1 1 calc R . .
N11 N 0.9718(4) 0.2731(3) 1.0767(2) 0.0418(5) Uani 1 1 d . . .
H6N H 0.8475 0.2629 1.1151 0.063 Uiso 1 1 d R A .
H7N H 0.9676 0.3081 0.9957 0.063 Uiso 1 1 d R . .
H8N H 0.9933 0.3436 1.1084 0.063 Uiso 1 1 d R . .
C11 C 1.111(2) 0.1236(16) 1.1184(9) 0.051(3) Uani 0.50 1 d P A 1
H11A H 1.0960 0.1060 1.2078 0.061 Uiso 0.50 1 calc PR A 1
H11B H 1.2477 0.1282 1.0792 0.061 Uiso 0.50 1 calc PR A 1
C11' C 1.135(2) 0.1261(17) 1.0665(11) 0.055(3) Uani 0.50 1 d P A 2
H11C H 1.2209 0.1395 0.9840 0.066 Uiso 0.50 1 calc PR A 2
H11D H 1.2159 0.1104 1.1260 0.066 Uiso 0.50 1 calc PR A 2
C12 C 1.0720(7) -0.0093(5) 1.0870(5) 0.108(2) Uani 1 1 d . . .
H12A H 0.9357 -0.0158 1.1265 0.130 Uiso 0.50 1 d PR A 1
H12B H 1.1639 -0.1063 1.1163 0.130 Uiso 0.50 1 d PR A 1
H12C H 1.0466 -0.0474 1.1764 0.130 Uiso 0.50 1 d PR A 2
H12D H 1.1956 -0.0762 1.0258 0.130 Uiso 0.50 1 d PR A 2
N12 N 1.1013(7) 0.0198(5) 0.9517(5) 0.0616(16) Uani 0.50 1 d PR . .
H9N H 0.9944 0.0852 0.9204 0.074 Uiso 0.50 1 d PR . .


_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
Ge1 S1 2.1416(8) . ?
Ge1 S2 2.1572(7) . ?
Ge1 S3 2.2762(7) . ?
Ge1 S3 2.2783(7) 2_667 ?
S3 Ge1 2.2783(7) 2_667 ?
Co1 N3 2.153(2) . ?
Co1 N3 2.153(2) 2_666 ?
Co1 N2 2.163(2) 2_666 ?
Co1 N2 2.163(2) . ?
Co1 N1 2.188(2) 2_666 ?
Co1 N1 2.188(2) . ?
N1 C1 1.476(4) . ?
C1 C2 1.509(4) . ?
C2 N2 1.475(4) . ?
N2 C3 1.469(4) . ?
C3 C4 1.508(5) . ?
C4 N3 1.469(4) . ?
N11 C11 1.474(13) . ?
N11 C11' 1.496(14) . ?
C11 C12 1.499(14) . ?
C11' C12 1.408(15) . ?
C12 N12 1.4609 . ?
C12 N12 1.476(9) 2_757 ?
N12 C12 1.476(9) 2_757 ?
N12 N12 1.639(10) 2_757 ?

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
S1 Ge1 S2 116.37(3) . . ?
S1 Ge1 S3 112.35(3) . . ?
S2 Ge1 S3 110.11(3) . . ?
S1 Ge1 S3 112.05(3) . 2_667 ?
S2 Ge1 S3 110.02(3) . 2_667 ?
S3 Ge1 S3 93.68(2) . 2_667 ?
Ge1 S3 Ge1 86.32(2) . 2_667 ?
N3 Co1 N3 180.000(1) . 2_666 ?
N3 Co1 N2 99.45(9) . 2_666 ?
N3 Co1 N2 80.55(9) 2_666 2_666 ?
N3 Co1 N2 80.55(9) . . ?
N3 Co1 N2 99.45(9) 2_666 . ?
N2 Co1 N2 180.00(10) 2_666 . ?
N3 Co1 N1 89.41(9) . 2_666 ?
N3 Co1 N1 90.59(9) 2_666 2_666 ?
N2 Co1 N1 81.16(9) 2_666 2_666 ?
N2 Co1 N1 98.84(9) . 2_666 ?
N3 Co1 N1 90.59(9) . . ?
N3 Co1 N1 89.41(9) 2_666 . ?
N2 Co1 N1 98.84(9) 2_666 . ?
N2 Co1 N1 81.16(9) . . ?
N1 Co1 N1 180.0 2_666 . ?
C1 N1 Co1 109.00(17) . . ?
N1 C1 C2 109.9(2) . . ?
N2 C2 C1 112.8(2) . . ?
C3 N2 C2 116.5(2) . . ?
C3 N2 Co1 107.52(18) . . ?
C2 N2 Co1 108.39(17) . . ?
N2 C3 C4 112.9(2) . . ?
N3 C4 C3 111.5(2) . . ?
C4 N3 Co1 112.33(17) . . ?
C11 N11 C11' 21.9(5) . . ?
N11 C11 C12 111.9(9) . . ?
C12 C11' N11 116.0(9) . . ?
C11' C12 N12 85.6(5) . . ?
C11' C12 N12 126.0(7) . 2_757 ?
N12 C12 N12 67.8(4) . 2_757 ?
C11' C12 C11 22.1(5) . . ?
N12 C12 C11 107.4(5) . . ?
N12 C12 C11 131.0(7) 2_757 . ?
C12 N12 C12 112.2(4) . 2_757 ?
C12 N12 N12 56.5(3) . 2_757 ?
C12 N12 N12 55.6(3) 2_757 2_757 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.071
_database_code_depnum_ccdc_archive 'CCDC 985615'
#######################################################################
#
#                 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_jl34_ge

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H41 Co Ge2 N9 S6'
_chemical_formula_weight         708.01

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-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                   15.2110(3)
_cell_length_b                   16.7025(4)
_cell_length_c                   21.8821(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5559.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    45318
_cell_measurement_theta_min      4
_cell_measurement_theta_max      28

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2904
_exptl_absorpt_coefficient_mu    3.209
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5149
_exptl_absorpt_correction_T_max  0.7110
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42958
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         27.97
_reflns_number_total             6648
_reflns_number_gt                5672
_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)+(0.0149P)²+10.4708P] 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       0.00014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6648
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_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
Ge1 Ge 0.64399(2) 0.75201(2) 0.672560(16) 0.02834(9) Uani 1 1 d . . .
Ge2 Ge 0.60637(3) 0.73060(2) 0.812281(17) 0.03103(10) Uani 1 1 d . . .
S1 S 0.61912(7) 0.66172(6) 0.60390(4) 0.0361(2) Uani 1 1 d . . .
S2 S 0.69631(7) 0.86186(6) 0.63517(4) 0.0366(2) Uani 1 1 d . . .
S3 S 0.52289(7) 0.77136(6) 0.73107(5) 0.0378(2) Uani 1 1 d . . .
S4 S 0.72660(6) 0.70866(6) 0.75237(5) 0.0363(2) Uani 1 1 d . . .
S5 S 0.55288(8) 0.62236(6) 0.85056(5) 0.0411(2) Uani 1 1 d . . .
S6 S 0.62865(7) 0.82758(6) 0.87653(4) 0.0397(2) Uani 1 1 d . . .
Co1 Co 0.37927(3) 0.76190(3) 0.48569(2) 0.02815(11) Uani 1 1 d . . .
N1 N 0.2461(2) 0.72637(17) 0.50559(14) 0.0340(7) Uani 1 1 d . . .
H1N H 0.2213 0.7626 0.5307 0.041 Uiso 1 1 calc R . .
H2N H 0.2148 0.7254 0.4707 0.041 Uiso 1 1 calc R . .
C1 C 0.2433(3) 0.6473(2) 0.53430(19) 0.0393(9) Uani 1 1 d . . .
H1A H 0.2439 0.6061 0.5031 0.047 Uiso 1 1 calc R . .
H1B H 0.1895 0.6418 0.5577 0.047 Uiso 1 1 calc R . .
C2 C 0.3218(3) 0.6371(3) 0.5759(2) 0.0443(10) Uani 1 1 d . . .
H2A H 0.3144 0.6708 0.6116 0.053 Uiso 1 1 calc R . .
H2B H 0.3245 0.5819 0.5896 0.053 Uiso 1 1 calc R . .
N2 N 0.4044(2) 0.65770(17) 0.54543(15) 0.0345(7) Uani 1 1 d . . .
H3N H 0.4442 0.6723 0.5744 0.041 Uiso 1 1 calc R . .
C3 C 0.4432(3) 0.5937(2) 0.5079(2) 0.0463(10) Uani 1 1 d . . .
H3A H 0.4318 0.5425 0.5272 0.056 Uiso 1 1 calc R . .
H3B H 0.5064 0.6011 0.5062 0.056 Uiso 1 1 calc R . .
C4 C 0.4070(3) 0.5920(2) 0.4433(2) 0.0473(10) Uani 1 1 d . . .
H4A H 0.4433 0.5577 0.4180 0.057 Uiso 1 1 calc R . .
H4B H 0.3479 0.5702 0.4436 0.057 Uiso 1 1 calc R . .
N3 N 0.4055(2) 0.67314(19) 0.41761(15) 0.0400(7) Uani 1 1 d . . .
H4N H 0.3640 0.6758 0.3884 0.048 Uiso 1 1 calc R . .
H5N H 0.4578 0.6835 0.4000 0.048 Uiso 1 1 calc R . .
N11 N 0.5138(2) 0.79801(18) 0.49591(15) 0.0348(7) Uani 1 1 d . . .
H6N H 0.5418 0.7635 0.5208 0.042 Uiso 1 1 calc R . .
H7N H 0.5406 0.7969 0.4593 0.042 Uiso 1 1 calc R . .
C11 C 0.5191(3) 0.8791(2) 0.52157(19) 0.0397(9) Uani 1 1 d . . .
H11A H 0.5107 0.9183 0.4894 0.048 Uiso 1 1 calc R . .
H11B H 0.5768 0.8876 0.5393 0.048 Uiso 1 1 calc R . .
C12 C 0.4493(3) 0.8895(3) 0.5700(2) 0.0456(10) Uani 1 1 d . . .
H12A H 0.4650 0.8583 0.6057 0.055 Uiso 1 1 calc R . .
H12B H 0.4468 0.9454 0.5821 0.055 Uiso 1 1 calc R . .
N12 N 0.3621(2) 0.86426(17) 0.54819(15) 0.0374(7) Uani 1 1 d . . .
H8N H 0.3301 0.8476 0.5809 0.045 Uiso 1 1 calc R . .
C13 C 0.3110(3) 0.9254(2) 0.5151(2) 0.0517(11) Uani 1 1 d . . .
H13A H 0.3190 0.9768 0.5350 0.062 Uiso 1 1 calc R . .
H13B H 0.2491 0.9119 0.5173 0.062 Uiso 1 1 calc R . .
C14 C 0.3378(3) 0.9325(2) 0.4489(2) 0.0531(12) Uani 1 1 d . . .
H14A H 0.2949 0.9645 0.4271 0.064 Uiso 1 1 calc R . .
H14B H 0.3943 0.9592 0.4462 0.064 Uiso 1 1 calc R . .
N13 N 0.3440(2) 0.85297(18) 0.42077(16) 0.0402(7) Uani 1 1 d . . .
H9N H 0.3844 0.8543 0.3908 0.048 Uiso 1 1 calc R . .
H10N H 0.2919 0.8404 0.4038 0.048 Uiso 1 1 calc R . .
N21 N 0.5382(2) 0.55489(19) 0.71248(15) 0.0394(8) Uani 1 1 d . . .
H11N H 0.5428 0.5808 0.7479 0.059 Uiso 1 1 calc R . .
H12N H 0.5593 0.5854 0.6826 0.059 Uiso 1 1 calc R . .
H13N H 0.5686 0.5095 0.7143 0.059 Uiso 1 1 calc R . .
C21 C 0.4452(3) 0.5368(3) 0.70038(19) 0.0421(9) Uani 1 1 d . . .
H21A H 0.4404 0.5035 0.6642 0.050 Uiso 1 1 calc R . .
H21B H 0.4132 0.5861 0.6930 0.050 Uiso 1 1 calc R . .
C22 C 0.4060(3) 0.4936(2) 0.75466(19) 0.0417(9) Uani 1 1 d . . .
H22A H 0.4507 0.4601 0.7732 0.050 Uiso 1 1 calc R . .
H22B H 0.3878 0.5328 0.7848 0.050 Uiso 1 1 calc R . .
N22 N 0.3298(2) 0.44352(17) 0.73800(14) 0.0329(7) Uani 1 1 d . . .
H14N H 0.3143 0.4147 0.7711 0.040 Uiso 1 1 calc R . .
H15N H 0.3471 0.4087 0.7090 0.040 Uiso 1 1 calc R . .
C23 C 0.2503(3) 0.4858(2) 0.7153(2) 0.0438(9) Uani 1 1 d . . .
H23A H 0.2629 0.5096 0.6758 0.053 Uiso 1 1 calc R . .
H23B H 0.2351 0.5285 0.7433 0.053 Uiso 1 1 calc R . .
C24 C 0.1740(3) 0.4294(3) 0.7093(2) 0.0467(10) Uani 1 1 d . . .
H24A H 0.1307 0.4524 0.6819 0.056 Uiso 1 1 calc R . .
H24B H 0.1941 0.3794 0.6916 0.056 Uiso 1 1 calc R . .
N23 N 0.1334(2) 0.4136(2) 0.76843(17) 0.0450(8) Uani 1 1 d . . .
H16N H 0.1704 0.3918 0.7951 0.067 Uiso 1 1 d R . .
H17N H 0.0908 0.3778 0.7631 0.067 Uiso 1 1 d 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
Ge1 S2 2.1608(10) . ?
Ge1 S1 2.1621(10) . ?
Ge1 S3 2.2664(10) . ?
Ge1 S4 2.2701(10) . ?
Ge2 S5 2.1522(10) . ?
Ge2 S6 2.1714(10) . ?
Ge2 S4 2.2797(11) . ?
Ge2 S3 2.2878(11) . ?
Co1 N3 2.139(3) . ?
Co1 N11 2.145(3) . ?
Co1 N13 2.150(3) . ?
Co1 N1 2.155(3) . ?
Co1 N12 2.205(3) . ?
Co1 N2 2.210(3) . ?
N1 C1 1.463(5) . ?
C1 C2 1.510(6) . ?
C2 N2 1.464(5) . ?
N2 C3 1.471(5) . ?
C3 C4 1.517(6) . ?
C4 N3 1.467(5) . ?
N11 C11 1.468(5) . ?
C11 C12 1.511(6) . ?
C12 N12 1.471(5) . ?
N12 C13 1.474(5) . ?
C13 C14 1.510(7) . ?
C14 N13 1.467(5) . ?
N21 C21 1.470(5) . ?
C21 C22 1.512(5) . ?
C22 N22 1.475(5) . ?
N22 C23 1.485(5) . ?
C23 C24 1.500(6) . ?
C24 N23 1.459(6) . ?

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
S2 Ge1 S1 113.18(4) . . ?
S2 Ge1 S3 113.09(4) . . ?
S1 Ge1 S3 110.48(4) . . ?
S2 Ge1 S4 110.99(4) . . ?
S1 Ge1 S4 114.14(4) . . ?
S3 Ge1 S4 93.48(4) . . ?
S5 Ge2 S6 115.70(4) . . ?
S5 Ge2 S4 113.09(4) . . ?
S6 Ge2 S4 111.53(4) . . ?
S5 Ge2 S3 110.03(4) . . ?
S6 Ge2 S3 111.56(4) . . ?
S4 Ge2 S3 92.66(4) . . ?
Ge1 S3 Ge2 86.86(4) . . ?
Ge1 S4 Ge2 86.97(4) . . ?
N3 Co1 N11 95.12(13) . . ?
N3 Co1 N13 94.40(13) . . ?
N11 Co1 N13 96.22(13) . . ?
N3 Co1 N1 97.21(13) . . ?
N11 Co1 N1 162.35(13) . . ?
N13 Co1 N1 95.37(12) . . ?
N3 Co1 N12 172.46(13) . . ?
N11 Co1 N12 80.22(12) . . ?
N13 Co1 N12 80.31(13) . . ?
N1 Co1 N12 88.68(12) . . ?
N3 Co1 N2 80.44(12) . . ?
N11 Co1 N2 89.68(12) . . ?
N13 Co1 N2 172.51(13) . . ?
N1 Co1 N2 80.01(12) . . ?
N12 Co1 N2 105.32(12) . . ?
C1 N1 Co1 111.2(2) . . ?
N1 C1 C2 109.8(3) . . ?
N2 C2 C1 112.2(3) . . ?
C2 N2 C3 115.2(3) . . ?
C2 N2 Co1 107.8(2) . . ?
C3 N2 Co1 108.1(2) . . ?
N2 C3 C4 112.8(3) . . ?
N3 C4 C3 110.2(3) . . ?
C4 N3 Co1 112.1(3) . . ?
C11 N11 Co1 110.6(2) . . ?
N11 C11 C12 109.6(3) . . ?
N12 C12 C11 111.9(3) . . ?
C12 N12 C13 115.8(3) . . ?
C12 N12 Co1 108.5(2) . . ?
C13 N12 Co1 107.2(3) . . ?
N12 C13 C14 112.5(3) . . ?
N13 C14 C13 110.5(3) . . ?
C14 N13 Co1 112.3(3) . . ?
N21 C21 C22 109.7(3) . . ?
N22 C22 C21 112.7(3) . . ?
C22 N22 C23 116.9(3) . . ?
N22 C23 C24 111.1(3) . . ?
N23 C24 C23 111.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.97
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.082
_database_code_depnum_ccdc_archive 'CCDC 985616'
#######################################################################
#
#                 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_jl2geco

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H41 Co Ge2 N9 S6'
_chemical_formula_weight         708.01

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P ca21'

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

_cell_length_a                   14.7043(3)
_cell_length_b                   9.0099(2)
_cell_length_c                   21.4540(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2842.32(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    38098
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      26.0

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_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    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1452
_exptl_absorpt_coefficient_mu    3.139
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5386
_exptl_absorpt_correction_T_max  0.7204
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38098
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         26.01
_reflns_number_total             5573
_reflns_number_gt                5486
_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)+(0.0277P)²+0.9420P] 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       0.00184(13)
_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   0.000(17)
_refine_ls_number_reflns         5573
_refine_ls_number_parameters     283
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0479
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
Ge1 Ge 0.335858(16) 0.34040(3) 0.475540(11) 0.02864(6) Uani 1 1 d . . .
Ge2 Ge 0.283565(17) 0.30635(3) 0.617147(11) 0.03000(6) Uani 1 1 d . . .
S1 S 0.40280(5) 0.16759(7) 0.42304(3) 0.03956(15) Uani 1 1 d . . .
S2 S 0.30586(5) 0.53498(7) 0.42040(3) 0.03576(13) Uani 1 1 d . . .
S3 S 0.20995(4) 0.25731(8) 0.52579(3) 0.03829(15) Uani 1 1 d . . .
S4 S 0.40955(4) 0.39485(8) 0.56586(3) 0.03504(14) Uani 1 1 d . . .
S5 S 0.31623(5) 0.10973(8) 0.66950(3) 0.04303(16) Uani 1 1 d . . .
S6 S 0.21687(5) 0.47948(8) 0.66942(3) 0.03979(15) Uani 1 1 d . . .
Co1 Co 0.54430(2) 0.52886(4) 0.298239(16) 0.03077(8) Uani 1 1 d . B .
N1 N 0.49303(17) 0.6677(3) 0.22180(11) 0.0419(5) Uani 1 1 d . . .
H1N H 0.5380 0.6864 0.1945 0.050 Uiso 0.50 1 calc PR A 1
H2N H 0.4481 0.6199 0.2015 0.050 Uiso 0.50 1 calc PR A 1
H1NA H 0.5373 0.7278 0.2076 0.050 Uiso 0.50 1 calc PR A 2
H2NB H 0.4737 0.6104 0.1901 0.050 Uiso 0.50 1 calc PR A 2
C1 C 0.4579(6) 0.8103(9) 0.2483(3) 0.0480(16) Uani 0.50 1 d P B 1
H1A H 0.5046 0.8856 0.2436 0.058 Uiso 0.50 1 calc PR B 1
H1B H 0.4057 0.8415 0.2240 0.058 Uiso 0.50 1 calc PR B 1
C1' C 0.4186(5) 0.7543(10) 0.2463(4) 0.0492(16) Uani 0.50 1 d P B 2
H1C H 0.3634 0.6955 0.2443 0.059 Uiso 0.50 1 calc PR B 2
H1D H 0.4099 0.8408 0.2200 0.059 Uiso 0.50 1 calc PR B 2
C2 C 0.4324(3) 0.8039(5) 0.31092(19) 0.0731(12) Uani 1 1 d . . .
H2A H 0.3695 0.7722 0.3129 0.088 Uiso 0.50 1 calc PR B 1
H2B H 0.4353 0.9037 0.3279 0.088 Uiso 0.50 1 calc PR B 1
H2C H 0.4618 0.9003 0.3098 0.088 Uiso 0.50 1 calc PR B 2
H2D H 0.3732 0.8176 0.3300 0.088 Uiso 0.50 1 calc PR B 2
N2 N 0.48569(15) 0.7071(3) 0.35099(11) 0.0386(5) Uani 1 1 d . B .
H3N H 0.4474 0.6668 0.3797 0.046 Uiso 1 1 calc R . .
C3 C 0.5593(2) 0.7820(4) 0.38488(15) 0.0491(7) Uani 1 1 d . . .
H3A H 0.5759 0.7232 0.4210 0.059 Uiso 1 1 calc R B .
H3B H 0.5380 0.8777 0.3995 0.059 Uiso 1 1 calc R . .
C4 C 0.6424(2) 0.8042(4) 0.34407(17) 0.0516(7) Uani 1 1 d . B .
H4A H 0.6305 0.8821 0.3139 0.062 Uiso 1 1 calc R . .
H4B H 0.6935 0.8348 0.3696 0.062 Uiso 1 1 calc R . .
N3 N 0.66532(15) 0.6657(3) 0.31121(12) 0.0407(5) Uani 1 1 d . . .
H4N H 0.7069 0.6149 0.3334 0.049 Uiso 1 1 calc R B .
H5N H 0.6897 0.6874 0.2738 0.049 Uiso 1 1 calc R . .
N11 N 0.42683(15) 0.3842(3) 0.28643(10) 0.0380(5) Uani 1 1 d . . .
H6N H 0.4020 0.3647 0.3239 0.046 Uiso 1 1 calc R B .
H7N H 0.3847 0.4304 0.2630 0.046 Uiso 1 1 calc R . .
C11 C 0.4536(2) 0.2442(3) 0.25618(15) 0.0465(7) Uani 1 1 d . B .
H11A H 0.4036 0.2072 0.2312 0.056 Uiso 1 1 calc R . .
H11B H 0.4677 0.1705 0.2877 0.056 Uiso 1 1 calc R . .
C12 C 0.5357(2) 0.2691(4) 0.21531(15) 0.0518(8) Uani 1 1 d . . .
H12A H 0.5604 0.1736 0.2031 0.062 Uiso 1 1 calc R B .
H12B H 0.5169 0.3205 0.1777 0.062 Uiso 1 1 calc R . .
N12 N 0.60735(17) 0.3557(3) 0.24609(11) 0.0428(5) Uani 1 1 d . B .
H8N H 0.6423 0.3982 0.2160 0.051 Uiso 1 1 calc R . .
C13 C 0.6678(2) 0.2715(4) 0.28819(17) 0.0525(8) Uani 1 1 d . . .
H13A H 0.7250 0.3243 0.2923 0.063 Uiso 1 1 calc R B .
H13B H 0.6807 0.1755 0.2697 0.063 Uiso 1 1 calc R . .
C14 C 0.6274(2) 0.2481(4) 0.35242(15) 0.0484(7) Uani 1 1 d . B .
H14A H 0.5804 0.1727 0.3504 0.058 Uiso 1 1 calc R . .
H14B H 0.6743 0.2137 0.3808 0.058 Uiso 1 1 calc R . .
N13 N 0.58834(15) 0.3878(3) 0.37596(11) 0.0400(5) Uani 1 1 d . . .
H9N H 0.6302 0.4363 0.3988 0.048 Uiso 1 1 calc R B .
H10N H 0.5405 0.3676 0.4007 0.048 Uiso 1 1 calc R . .
N21 N 0.59020(18) 0.1058(3) 0.51898(15) 0.0570(7) Uani 1 1 d . . .
H11N H 0.6058 0.0392 0.4896 0.086 Uiso 1 1 d R . .
H12N H 0.5461 0.1522 0.4974 0.086 Uiso 1 1 d R . .
C21 C 0.5580(2) 0.0290(4) 0.57514(15) 0.0471(7) Uani 1 1 d . . .
H21A H 0.5306 0.1012 0.6030 0.057 Uiso 1 1 calc R . .
H21B H 0.6097 -0.0143 0.5965 0.057 Uiso 1 1 calc R . .
C22 C 0.48905(19) -0.0924(3) 0.56162(15) 0.0433(6) Uani 1 1 d . . .
H22A H 0.5110 -0.1542 0.5278 0.052 Uiso 1 1 calc R . .
H22B H 0.4818 -0.1546 0.5982 0.052 Uiso 1 1 calc R . .
N22 N 0.40005(15) -0.0275(2) 0.54435(11) 0.0351(5) Uani 1 1 d . . .
H13N H 0.4095 0.0421 0.5150 0.042 Uiso 1 1 calc R . .
H14N H 0.3770 0.0186 0.5780 0.042 Uiso 1 1 calc R . .
C23 C 0.3310(2) -0.1332(3) 0.52069(14) 0.0421(6) Uani 1 1 d . . .
H23A H 0.3573 -0.1919 0.4873 0.051 Uiso 1 1 calc R . .
H23B H 0.2800 -0.0783 0.5037 0.051 Uiso 1 1 calc R . .
C24 C 0.2978(2) -0.2347(3) 0.57135(15) 0.0427(6) Uani 1 1 d . . .
H24A H 0.3467 -0.2995 0.5847 0.051 Uiso 1 1 calc R . .
H24B H 0.2780 -0.1767 0.6070 0.051 Uiso 1 1 calc R . .
N23 N 0.22158(16) -0.3237(3) 0.54751(12) 0.0404(5) Uani 1 1 d . . .
H15N H 0.1744 -0.2646 0.5397 0.061 Uiso 1 1 calc R . .
H16N H 0.2058 -0.3911 0.5758 0.061 Uiso 1 1 calc R . .
H17N H 0.2384 -0.3693 0.5125 0.061 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
Ge1 S1 2.1592(7) . ?
Ge1 S2 2.1604(7) . ?
Ge1 S3 2.2694(6) . ?
Ge1 S4 2.2737(7) . ?
Ge2 S5 2.1519(7) . ?
Ge2 S6 2.1570(7) . ?
Ge2 S3 2.2822(7) . ?
Ge2 S4 2.2975(7) . ?
Co1 N12 2.132(2) . ?
Co1 N2 2.146(2) . ?
Co1 N11 2.178(2) . ?
Co1 N3 2.183(2) . ?
Co1 N13 2.194(2) . ?
Co1 N1 2.196(2) . ?
N1 C1' 1.444(8) . ?
N1 C1 1.497(8) . ?
C1 C2 1.396(9) . ?
C1' C2 1.471(8) . ?
C2 N2 1.454(4) . ?
N2 C3 1.469(4) . ?
C3 C4 1.516(5) . ?
C4 N3 1.472(4) . ?
N11 C11 1.472(4) . ?
C11 C12 1.509(5) . ?
C12 N12 1.468(4) . ?
N12 C13 1.478(4) . ?
C13 C14 1.515(5) . ?
C14 N13 1.473(4) . ?
N21 C21 1.468(4) . ?
C21 C22 1.520(4) . ?
C22 N22 1.481(3) . ?
N22 C23 1.481(4) . ?
C23 C24 1.502(4) . ?
C24 N23 1.470(4) . ?

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
S1 Ge1 S2 113.12(3) . . ?
S1 Ge1 S3 112.45(3) . . ?
S2 Ge1 S3 111.18(3) . . ?
S1 Ge1 S4 112.51(3) . . ?
S2 Ge1 S4 112.88(3) . . ?
S3 Ge1 S4 93.16(2) . . ?
S5 Ge2 S6 115.18(3) . . ?
S5 Ge2 S3 113.25(3) . . ?
S6 Ge2 S3 111.77(3) . . ?
S5 Ge2 S4 110.84(3) . . ?
S6 Ge2 S4 111.39(3) . . ?
S3 Ge2 S4 92.20(2) . . ?
Ge1 S3 Ge2 87.55(2) . . ?
Ge1 S4 Ge2 87.07(2) . . ?
N12 Co1 N2 177.86(9) . . ?
N12 Co1 N11 81.14(9) . . ?
N2 Co1 N11 100.99(9) . . ?
N12 Co1 N3 97.22(9) . . ?
N2 Co1 N3 80.64(9) . . ?
N11 Co1 N3 177.62(9) . . ?
N12 Co1 N13 81.17(10) . . ?
N2 Co1 N13 98.71(9) . . ?
N11 Co1 N13 88.62(9) . . ?
N3 Co1 N13 89.41(9) . . ?
N12 Co1 N1 100.03(9) . . ?
N2 Co1 N1 80.19(9) . . ?
N11 Co1 N1 88.95(9) . . ?
N3 Co1 N1 93.06(9) . . ?
N13 Co1 N1 177.09(9) . . ?
C1' N1 C1 30.2(3) . . ?
C1' N1 Co1 107.2(3) . . ?
C1 N1 Co1 108.9(3) . . ?
C2 C1 N1 115.0(5) . . ?
N1 C1' C2 113.7(5) . . ?
C1 C2 N2 116.7(4) . . ?
C1 C2 C1' 31.0(4) . . ?
N2 C2 C1' 116.7(4) . . ?
C2 N2 C3 114.5(3) . . ?
C2 N2 Co1 110.72(19) . . ?
C3 N2 Co1 107.99(17) . . ?
N2 C3 C4 111.6(2) . . ?
N3 C4 C3 110.4(2) . . ?
C4 N3 Co1 110.70(17) . . ?
C11 N11 Co1 110.59(17) . . ?
N11 C11 C12 110.1(2) . . ?
N12 C12 C11 113.1(2) . . ?
C12 N12 C13 115.7(3) . . ?
C12 N12 Co1 108.24(18) . . ?
C13 N12 Co1 108.48(19) . . ?
N12 C13 C14 113.0(2) . . ?
N13 C14 C13 110.3(2) . . ?
C14 N13 Co1 110.47(17) . . ?
N21 C21 C22 113.5(2) . . ?
N22 C22 C21 110.6(2) . . ?
C22 N22 C23 115.9(2) . . ?
N22 C23 C24 111.5(2) . . ?
N23 C24 C23 109.2(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.050
_database_code_depnum_ccdc_archive 'CCDC 985617'
