# 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.
#
#  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_a

_audit_update_record             
;
2014-07-20 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Ni (C4H14N3)2]2 Cl [Ge7O13(OH)2F3)]'
_chemical_formula_sum            'C16 H54 Cl F3 Ge7 N12 Ni2 O15'
_chemical_formula_weight         1372.71

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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   P2/n


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

_cell_length_a                   8.8785(7)
_cell_length_b                   17.4501(14)
_cell_length_c                   13.1922(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.292(2)
_cell_angle_gamma                90.00
_cell_volume                     2004.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356
_exptl_absorpt_coefficient_mu    6.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5579
_exptl_absorpt_correction_T_max  0.7883
_exptl_absorpt_process_details   SADABS

_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            11746
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_sigmaI/netI    0.1069
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.17
_diffrn_reflns_theta_max         26.35
_reflns_number_total             4088
_reflns_number_gt                2416
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0091P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4088
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Ge1 Ge 0.2500 0.33605(6) 0.7500 0.0207(3) Uani 1 2 d S . .
Ge2 Ge 0.31991(9) 0.14227(4) 0.66166(6) 0.0219(2) Uani 1 1 d . . .
Ge3 Ge 0.07913(8) 0.25656(5) 0.54910(6) 0.0249(2) Uani 1 1 d . . .
Ge4 Ge -0.06651(8) 0.25603(4) 0.73824(6) 0.0226(2) Uani 1 1 d . . .
Ni1 Ni 0.7500 -0.06113(8) 0.7500 0.0311(4) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.5000 0.5000 0.0284(4) Uani 1 2 d S . .
Cl1 Cl 0.7500 -0.32835(18) 0.7500 0.0530(9) Uani 1 2 d S . .
F1 F 0.2500 0.4396(3) 0.7500 0.0323(16) Uani 1 2 d S . .
F2 F 0.3722(4) 0.0602(2) 0.5912(3) 0.0348(11) Uani 1 1 d . . .
O1 O 0.2500 0.2215(3) 0.7500 0.0180(16) Uani 1 2 d S . .
O2 O 0.1738(5) 0.3359(3) 0.6070(3) 0.0233(12) Uani 1 1 d . . .
O3 O 0.0487(5) 0.3345(3) 0.7770(3) 0.0248(12) Uani 1 1 d . . .
O4 O 0.5134(5) 0.1738(3) 0.6872(4) 0.0268(12) Uani 1 1 d . . .
O5 O 0.2500 0.0806(3) 0.7500 0.0214(17) Uani 1 2 d S . .
O6 O 0.1967(5) 0.1765(3) 0.5481(3) 0.0290(13) Uani 1 1 d . . .
O7 O -0.0001(5) 0.2770(3) 0.4196(4) 0.0391(15) Uani 1 1 d . . .
H7 H 0.0690 0.2872 0.3886 0.080 Uiso 1 1 calc . . .
O8 O -0.0760(5) 0.2332(3) 0.6077(4) 0.0289(13) Uani 1 1 d . . .
O9 O -0.2500 0.2846(4) 0.7500 0.0310(19) Uani 1 2 d S . .
N1 N 0.6702(7) -0.1510(4) 0.6393(5) 0.0395(18) Uani 1 1 d . . .
H1A H 0.7064 -0.1435 0.5809 0.047 Uiso 1 1 calc . . .
H1B H 0.7032 -0.1970 0.6657 0.047 Uiso 1 1 calc . . .
N2 N 0.5192(7) -0.0568(4) 0.7560(5) 0.0394(19) Uani 1 1 d . . .
H2 H 0.4756 -0.0184 0.7135 0.047 Uiso 1 1 calc . . .
N3 N 0.7678(8) 0.0193(4) 0.8731(5) 0.0446(19) Uani 1 1 d . . .
H3A H 0.8256 -0.0001 0.9311 0.053 Uiso 1 1 calc . . .
H3B H 0.8121 0.0628 0.8569 0.053 Uiso 1 1 calc . . .
N4 N 0.5517(7) 0.4609(4) 0.3563(5) 0.0441(19) Uani 1 1 d . . .
H4A H 0.4640 0.4482 0.3127 0.053 Uiso 1 1 calc . . .
H4B H 0.5971 0.4988 0.3271 0.053 Uiso 1 1 calc . . .
N5 N 0.6460(8) 0.4116(4) 0.5587(6) 0.0441(19) Uani 1 1 d . . .
H5 H 0.6091 0.3886 0.6107 0.053 Uiso 1 1 calc . . .
N6 N 0.7001(7) 0.5647(4) 0.5301(5) 0.0388(18) Uani 1 1 d . . .
H6A H 0.7051 0.5948 0.4754 0.047 Uiso 1 1 calc . . .
H6B H 0.7001 0.5951 0.5852 0.047 Uiso 1 1 calc . . .
C1 C 0.5006(10) -0.1484(5) 0.6171(7) 0.054(3) Uani 1 1 d . . .
H1C H 0.4595 -0.1974 0.5900 0.064 Uiso 1 1 calc . . .
H1D H 0.4649 -0.1093 0.5658 0.064 Uiso 1 1 calc . . .
C2 C 0.4468(9) -0.1307(5) 0.7144(8) 0.052(3) Uani 1 1 d . . .
H2A H 0.4763 -0.1715 0.7643 0.062 Uiso 1 1 calc . . .
H2B H 0.3358 -0.1261 0.7008 0.062 Uiso 1 1 calc . . .
C3 C 0.5117(10) -0.0354(6) 0.8624(7) 0.050(3) Uani 1 1 d . . .
H3C H 0.5496 -0.0769 0.9094 0.060 Uiso 1 1 calc . . .
H3D H 0.4064 -0.0245 0.8678 0.060 Uiso 1 1 calc . . .
C4 C 0.6103(11) 0.0352(5) 0.8893(7) 0.051(3) Uani 1 1 d . . .
H4C H 0.5666 0.0777 0.8460 0.061 Uiso 1 1 calc . . .
H4D H 0.6135 0.0491 0.9609 0.061 Uiso 1 1 calc . . .
C5 C 0.6535(10) 0.3943(6) 0.3733(8) 0.059(3) Uani 1 1 d . . .
H5A H 0.7586 0.4102 0.3749 0.070 Uiso 1 1 calc . . .
H5B H 0.6245 0.3579 0.3173 0.070 Uiso 1 1 calc . . .
C6 C 0.6408(9) 0.3572(5) 0.4752(8) 0.055(3) Uani 1 1 d . . .
H6C H 0.5451 0.3289 0.4662 0.066 Uiso 1 1 calc . . .
H6D H 0.7242 0.3208 0.4942 0.066 Uiso 1 1 calc . . .
C7 C 0.7983(10) 0.4423(6) 0.6005(8) 0.062(3) Uani 1 1 d . . .
H7A H 0.8745 0.4040 0.5929 0.074 Uiso 1 1 calc . . .
H7B H 0.8064 0.4518 0.6738 0.074 Uiso 1 1 calc . . .
C8 C 0.8332(10) 0.5134(6) 0.5505(8) 0.058(3) Uani 1 1 d . . .
H8A H 0.9182 0.5393 0.5946 0.070 Uiso 1 1 calc . . .
H8B H 0.8642 0.5012 0.4858 0.070 Uiso 1 1 calc . . .


_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 F1 1.807(6) . ?
Ge1 O2 1.875(4) . ?
Ge1 O2 1.875(4) 2_556 ?
Ge1 O3 1.890(4) . ?
Ge1 O3 1.890(4) 2_556 ?
Ge1 O1 1.999(6) . ?
Ge2 O4 1.772(4) . ?
Ge2 O6 1.776(4) . ?
Ge2 O5 1.785(4) . ?
Ge2 F2 1.817(4) . ?
Ge2 O1 1.984(4) . ?
Ge2 Ge2 2.8472(16) 2_556 ?
Ge3 O2 1.719(4) . ?
Ge3 O6 1.745(5) . ?
Ge3 O7 1.752(5) . ?
Ge3 O8 1.754(5) . ?
Ge4 O3 1.725(4) . ?
Ge4 O9 1.740(2) . ?
Ge4 O4 1.751(5) 2_556 ?
Ge4 O8 1.754(5) . ?
Ni1 N2 2.067(6) . ?
Ni1 N2 2.067(6) 2_656 ?
Ni1 N3 2.129(7) 2_656 ?
Ni1 N3 2.129(7) . ?
Ni1 N1 2.166(7) . ?
Ni1 N1 2.166(7) 2_656 ?
Ni2 N5 2.065(6) 3_666 ?
Ni2 N5 2.065(6) . ?
Ni2 N6 2.077(6) . ?
Ni2 N6 2.077(6) 3_666 ?
Ni2 N4 2.147(7) . ?
Ni2 N4 2.147(7) 3_666 ?
O1 Ge2 1.984(4) 2_556 ?
O4 Ge4 1.751(5) 2_556 ?
O5 Ge2 1.785(4) 2_556 ?
O7 H7 0.8200 . ?
O9 Ge4 1.740(2) 2_456 ?
N1 C1 1.478(10) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.466(10) . ?
N2 C2 1.497(10) . ?
N2 H2 0.9100 . ?
N3 C4 1.481(10) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.462(11) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C6 1.449(11) . ?
N5 C7 1.459(10) . ?
N5 H5 0.9100 . ?
N6 C8 1.465(10) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.487(12) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.511(12) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.516(13) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.467(12) . ?
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
F1 Ge1 O2 90.08(14) . . ?
F1 Ge1 O2 90.08(14) . 2_556 ?
O2 Ge1 O2 179.8(3) . 2_556 ?
F1 Ge1 O3 90.84(14) . . ?
O2 Ge1 O3 91.21(19) . . ?
O2 Ge1 O3 88.79(19) 2_556 . ?
F1 Ge1 O3 90.84(14) . 2_556 ?
O2 Ge1 O3 88.79(19) . 2_556 ?
O2 Ge1 O3 91.21(19) 2_556 2_556 ?
O3 Ge1 O3 178.3(3) . 2_556 ?
F1 Ge1 O1 180 . . ?
O2 Ge1 O1 89.92(14) . . ?
O2 Ge1 O1 89.92(14) 2_556 . ?
O3 Ge1 O1 89.16(14) . . ?
O3 Ge1 O1 89.16(14) 2_556 . ?
O4 Ge2 O6 118.1(2) . . ?
O4 Ge2 O5 120.73(16) . . ?
O6 Ge2 O5 121.18(16) . . ?
O4 Ge2 F2 90.4(2) . . ?
O6 Ge2 F2 90.61(19) . . ?
O5 Ge2 F2 90.9(2) . . ?
O4 Ge2 O1 94.30(17) . . ?
O6 Ge2 O1 92.81(17) . . ?
O5 Ge2 O1 81.3(2) . . ?
F2 Ge2 O1 172.07(19) . . ?
O4 Ge2 Ge2 113.95(16) . 2_556 ?
O6 Ge2 Ge2 113.25(16) . 2_556 ?
O5 Ge2 Ge2 37.09(16) . 2_556 ?
F2 Ge2 Ge2 127.94(14) . 2_556 ?
O1 Ge2 Ge2 44.16(13) . 2_556 ?
O2 Ge3 O6 114.0(2) . . ?
O2 Ge3 O7 109.7(2) . . ?
O6 Ge3 O7 106.4(2) . . ?
O2 Ge3 O8 110.4(2) . . ?
O6 Ge3 O8 109.8(2) . . ?
O7 Ge3 O8 106.1(2) . . ?
O3 Ge4 O9 104.9(3) . . ?
O3 Ge4 O4 113.9(2) . 2_556 ?
O9 Ge4 O4 109.8(2) . 2_556 ?
O3 Ge4 O8 112.5(2) . . ?
O9 Ge4 O8 106.69(15) . . ?
O4 Ge4 O8 108.7(2) 2_556 . ?
N2 Ni1 N2 175.8(4) . 2_656 ?
N2 Ni1 N3 94.5(3) . 2_656 ?
N2 Ni1 N3 82.7(3) 2_656 2_656 ?
N2 Ni1 N3 82.7(3) . . ?
N2 Ni1 N3 94.5(3) 2_656 . ?
N3 Ni1 N3 97.5(4) 2_656 . ?
N2 Ni1 N1 81.8(3) . . ?
N2 Ni1 N1 101.3(2) 2_656 . ?
N3 Ni1 N1 89.9(2) 2_656 . ?
N3 Ni1 N1 163.3(3) . . ?
N2 Ni1 N1 101.3(2) . 2_656 ?
N2 Ni1 N1 81.8(3) 2_656 2_656 ?
N3 Ni1 N1 163.3(2) 2_656 2_656 ?
N3 Ni1 N1 89.9(2) . 2_656 ?
N1 Ni1 N1 87.2(3) . 2_656 ?
N5 Ni2 N5 180 3_666 . ?
N5 Ni2 N6 96.7(3) 3_666 . ?
N5 Ni2 N6 83.3(3) . . ?
N5 Ni2 N6 83.3(3) 3_666 3_666 ?
N5 Ni2 N6 96.7(3) . 3_666 ?
N6 Ni2 N6 180 . 3_666 ?
N5 Ni2 N4 97.7(3) 3_666 . ?
N5 Ni2 N4 82.3(3) . . ?
N6 Ni2 N4 91.1(2) . . ?
N6 Ni2 N4 88.9(2) 3_666 . ?
N5 Ni2 N4 82.3(3) 3_666 3_666 ?
N5 Ni2 N4 97.7(3) . 3_666 ?
N6 Ni2 N4 88.9(2) . 3_666 ?
N6 Ni2 N4 91.1(2) 3_666 3_666 ?
N4 Ni2 N4 180 . 3_666 ?
Ge2 O1 Ge2 91.7(3) . 2_556 ?
Ge2 O1 Ge1 134.16(13) . . ?
Ge2 O1 Ge1 134.16(13) 2_556 . ?
Ge3 O2 Ge1 119.8(2) . . ?
Ge4 O3 Ge1 118.9(3) . . ?
Ge4 O4 Ge2 120.4(3) 2_556 . ?
Ge2 O5 Ge2 105.8(3) 2_556 . ?
Ge3 O6 Ge2 122.2(3) . . ?
Ge3 O7 H7 109.5 . . ?
Ge4 O8 Ge3 119.3(2) . . ?
Ge4 O9 Ge4 146.7(4) . 2_456 ?
C1 N1 Ni1 107.3(5) . . ?
C1 N1 H1A 110.3 . . ?
Ni1 N1 H1A 110.3 . . ?
C1 N1 H1B 110.3 . . ?
Ni1 N1 H1B 110.3 . . ?
H1A N1 H1B 108.5 . . ?
C3 N2 C2 118.3(7) . . ?
C3 N2 Ni1 106.1(5) . . ?
C2 N2 Ni1 108.2(5) . . ?
C3 N2 H2 108.0 . . ?
C2 N2 H2 108.0 . . ?
Ni1 N2 H2 108.0 . . ?
C4 N3 Ni1 107.6(5) . . ?
C4 N3 H3A 110.2 . . ?
Ni1 N3 H3A 110.2 . . ?
C4 N3 H3B 110.2 . . ?
Ni1 N3 H3B 110.2 . . ?
H3A N3 H3B 108.5 . . ?
C5 N4 Ni2 110.5(5) . . ?
C5 N4 H4A 109.6 . . ?
Ni2 N4 H4A 109.6 . . ?
C5 N4 H4B 109.6 . . ?
Ni2 N4 H4B 109.6 . . ?
H4A N4 H4B 108.1 . . ?
C6 N5 C7 114.6(7) . . ?
C6 N5 Ni2 106.3(5) . . ?
C7 N5 Ni2 109.6(5) . . ?
C6 N5 H5 108.7 . . ?
C7 N5 H5 108.7 . . ?
Ni2 N5 H5 108.7 . . ?
C8 N6 Ni2 109.4(5) . . ?
C8 N6 H6A 109.8 . . ?
Ni2 N6 H6A 109.8 . . ?
C8 N6 H6B 109.8 . . ?
Ni2 N6 H6B 109.8 . . ?
H6A N6 H6B 108.2 . . ?
N1 C1 C2 108.8(7) . . ?
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 . . ?
C1 C2 N2 107.9(7) . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2B 110.1 . . ?
N2 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 107.4(7) . . ?
N2 C3 H3C 110.2 . . ?
C4 C3 H3C 110.2 . . ?
N2 C3 H3D 110.2 . . ?
C4 C3 H3D 110.2 . . ?
H3C C3 H3D 108.5 . . ?
N3 C4 C3 109.5(7) . . ?
N3 C4 H4C 109.8 . . ?
C3 C4 H4C 109.8 . . ?
N3 C4 H4D 109.8 . . ?
C3 C4 H4D 109.8 . . ?
H4C C4 H4D 108.2 . . ?
N4 C5 C6 108.9(7) . . ?
N4 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N4 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N5 C6 C5 113.4(7) . . ?
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 113.7(7) . . ?
N5 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N5 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N6 C8 C7 111.5(7) . . ?
N6 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
N6 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O6 0.90 2.13 2.975(8) 155.6 3_656
N2 H2 F2 0.91 2.18 3.080(7) 170.6 .
N3 H3A F2 0.90 2.32 3.165(8) 156.0 4_656
N4 H4B F1 0.90 2.14 3.008(7) 162.3 3_666
N5 H5 O3 0.91 2.42 3.311(9) 166.1 2_556
N6 H6A O2 0.90 2.06 2.885(8) 151.2 3_666

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.146

_database_code_depnum_ccdc_archive 'CCDC 992864'
#######################################################################
#
#                 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Ni(C3N2H11)3] [Ge7O14F2(OC2NH7)] (H2O)0.5'
_chemical_formula_sum            'C11 H38 F2 Ge7 N7 Ni O15.50'
_chemical_formula_weight         1121.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1550 1.8000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   8.829(3)
_cell_length_b                   16.632(5)
_cell_length_c                   20.933(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.992(6)
_cell_angle_gamma                90.00
_cell_volume                     3051.0(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17507
_cell_measurement_theta_min      1.57
_cell_measurement_theta_max      26.35

_exptl_crystal_description       'hexagonal rod'
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2188
_exptl_absorpt_coefficient_mu    7.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1536
_exptl_absorpt_correction_T_max  0.2561
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 5.00
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17507
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_sigmaI/netI    0.1189
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         26.35
_reflns_number_total             6206
_reflns_number_gt                3637
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0414P)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         6206
_refine_ls_number_parameters     427
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1142
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.899
_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 0.23120(9) 0.87834(5) 0.19692(4) 0.0186(2) Uani 1 1 d . . .
Ge2 Ge 0.18292(10) 0.90843(6) 0.36466(4) 0.0218(2) Uani 1 1 d . . .
Ge3 Ge 0.37651(10) 0.77258(6) 0.34697(4) 0.0228(2) Uani 1 1 d . . .
Ge4 Ge -0.06577(9) 0.85351(6) 0.26090(4) 0.0207(2) Uani 1 1 d . . .
Ge5 Ge 0.36973(9) 1.01741(5) 0.28532(4) 0.0197(2) Uani 1 1 d . . .
Ge6 Ge 0.56356(9) 0.87311(6) 0.26172(4) 0.0204(2) Uani 1 1 d . . .
Ge7 Ge 0.13359(9) 0.71029(5) 0.23941(4) 0.0200(2) Uani 1 1 d . . .
Ni1 Ni -0.07446(15) 0.78533(8) 0.53076(6) 0.0438(4) Uani 1 1 d . A .
F1 F 0.1988(5) 0.8999(3) 0.1112(2) 0.0316(13) Uani 1 1 d . . .
F2 F 0.1324(5) 0.9462(3) 0.4402(2) 0.0346(13) Uani 1 1 d . . .
O1 O 0.2590(6) 0.8572(3) 0.2901(2) 0.0172(12) Uani 1 1 d . . .
O2 O 0.0236(6) 0.8991(3) 0.2007(3) 0.0220(14) Uani 1 1 d . . .
O3 O 0.2689(6) 0.9895(3) 0.2132(3) 0.0244(14) Uani 1 1 d . . .
O4 O 0.4368(6) 0.8585(3) 0.1938(3) 0.0231(14) Uani 1 1 d . . .
O5 O 0.1899(6) 0.7702(3) 0.1788(3) 0.0217(13) Uani 1 1 d . . .
O6 O 0.2854(6) 0.8289(4) 0.4047(3) 0.0265(14) Uani 1 1 d . . .
O7 O -0.0127(6) 0.8952(3) 0.3369(3) 0.0253(14) Uani 1 1 d . . .
O8 O 0.2623(6) 1.0022(3) 0.3502(3) 0.0297(15) Uani 1 1 d . . .
O9 O 0.4769(6) 0.7056(4) 0.4058(3) 0.0287(15) Uani 1 1 d . . .
O10 O 0.5531(6) 0.7992(3) 0.3204(3) 0.0260(14) Uani 1 1 d . . .
O11 O 0.2747(6) 0.6940(3) 0.3036(3) 0.0262(14) Uani 1 1 d . . .
O12 O -0.2573(6) 0.8676(4) 0.2356(3) 0.0305(15) Uani 1 1 d . . .
O13 O -0.0315(6) 0.7502(3) 0.2672(3) 0.0243(14) Uani 1 1 d . . .
O14 O 0.5460(6) 0.9669(3) 0.2970(3) 0.0237(14) Uani 1 1 d . . .
O15 O 0.0796(6) 0.6177(3) 0.2078(3) 0.0287(15) Uani 1 1 d . . .
O1W O -0.1841(17) 0.8890(11) 0.0916(7) 0.077(5) Uani 0.50 1 d PU . .
C1 C 0.196(5) 0.869(2) 0.603(2) 0.076(12) Uani 0.50 1 d PU A 1
H1A H 0.1685 0.9243 0.5936 0.091 Uiso 0.50 1 d PR A 1
H1B H 0.3020 0.8616 0.6184 0.091 Uiso 0.50 1 d PR A 1
C1' C 0.212(3) 0.8286(18) 0.604(2) 0.061(10) Uani 0.50 1 d P A 2
H1'A H 0.3091 0.8561 0.6145 0.074 Uiso 0.50 1 d PR A 2
H1'B H 0.2213 0.7767 0.6301 0.074 Uiso 0.50 1 d PR A 2
C2' C 0.090(3) 0.8792(15) 0.6414(13) 0.040(6) Uani 0.50 1 d PU A 2
H2' H 0.0777 0.9317 0.6202 0.048 Uiso 0.50 1 d PR A 2
C2 C 0.109(3) 0.8354(17) 0.6506(12) 0.046(7) Uani 0.50 1 d PU A 1
H2 H 0.1459 0.7813 0.6626 0.055 Uiso 0.50 1 d PR A 1
C3 C 0.1334(13) 0.8881(8) 0.7115(6) 0.075(4) Uani 1 1 d . . .
H3BD H 0.1371 0.8365 0.7333 0.113 Uiso 0.50 1 d PR A .
H3BE H 0.2295 0.9147 0.7219 0.113 Uiso 0.50 1 d PR . .
H3BF H 0.0557 0.9205 0.7301 0.113 Uiso 0.50 1 d PR . .
H3AA H 0.2384 0.8903 0.7298 0.113 Uiso 0.50 1 d PR B 1
H3AB H 0.0971 0.9418 0.7016 0.113 Uiso 0.50 1 d PR C 1
H3AC H 0.0746 0.8675 0.7455 0.113 Uiso 0.50 1 d PR D 1
C4 C -0.3845(12) 0.8476(7) 0.5226(6) 0.058(3) Uani 1 1 d . A .
H4A H -0.3695 0.8792 0.5618 0.070 Uiso 1 1 d R . .
H4B H -0.4929 0.8404 0.5095 0.070 Uiso 1 1 d R . .
C5 C -0.3146(12) 0.8896(7) 0.4704(5) 0.050(3) Uani 1 1 d . A .
H5 H -0.3289 0.8555 0.4320 0.060 Uiso 1 1 d R . .
C6 C -0.3802(16) 0.9724(10) 0.4509(7) 0.106(6) Uani 1 1 d . . .
H6A H -0.3299 0.9933 0.4163 0.159 Uiso 1 1 calc R . .
H6B H -0.3642 1.0082 0.4871 0.159 Uiso 1 1 calc R . .
H6C H -0.4876 0.9676 0.4371 0.159 Uiso 1 1 calc R . .
C7 C -0.081(5) 0.611(3) 0.496(2) 0.105(10) Uani 0.50 1 d PU A 1
H7A H -0.1908 0.6057 0.4922 0.126 Uiso 0.50 1 d PR A 1
H7B H -0.0324 0.5617 0.5080 0.126 Uiso 0.50 1 d PR A 1
C7' C -0.011(4) 0.618(2) 0.505(2) 0.077(10) Uani 0.50 1 d PU A 2
H7'A H -0.0399 0.5592 0.5084 0.092 Uiso 0.50 1 d PR A 2
H7'B H 0.0937 0.6168 0.4928 0.092 Uiso 0.50 1 d PR A 2
C8' C -0.086(3) 0.6520(13) 0.4341(9) 0.039(6) Uani 0.50 1 d PU A 2
H8' H -0.1919 0.6435 0.4425 0.047 Uiso 0.50 1 d PR A 2
C8 C 0.007(5) 0.654(2) 0.4556(19) 0.105(10) Uani 0.50 1 d PU A 1
H8 H 0.1190 0.6567 0.4595 0.126 Uiso 0.50 1 d PR A 1
C9 C -0.088(2) 0.6021(9) 0.3774(7) 0.117(6) Uani 1 1 d . . .
H9BD H 0.0161 0.6056 0.3684 0.175 Uiso 0.50 1 d PR A 2
H9BE H -0.1144 0.5468 0.3827 0.175 Uiso 0.50 1 d PR A 2
H9BF H -0.1539 0.6250 0.3423 0.175 Uiso 0.50 1 d PR A 2
H9AA H -0.0440 0.5493 0.3816 0.175 Uiso 0.50 1 d PR A 1
H9AB H -0.1969 0.5981 0.3731 0.175 Uiso 0.50 1 d PR A 1
H9AC H -0.0572 0.6279 0.3400 0.175 Uiso 0.50 1 d PR A 1
C10 C 0.4008(18) 0.6481(11) 0.4359(8) 0.109(6) Uani 1 1 d . . .
H10A H 0.2933 0.6509 0.4195 0.131 Uiso 1 1 calc R . .
H10B H 0.4104 0.6604 0.4815 0.131 Uiso 1 1 calc R . .
C11 C 0.4573(19) 0.5604(10) 0.4274(8) 0.107(5) Uani 1 1 d . . .
H11A H 0.5561 0.5520 0.4522 0.128 Uiso 1 1 d R . .
H11B H 0.3845 0.5223 0.4410 0.128 Uiso 1 1 d R . .
N1 N 0.1605(10) 0.8151(6) 0.5402(5) 0.061(3) Uani 1 1 d . . .
H1C H 0.2099 0.7708 0.5470 0.073 Uiso 0.50 1 d PR A 1
H1D H 0.1745 0.8445 0.5076 0.073 Uiso 0.50 1 d PR A 1
N2 N -0.0539(8) 0.8281(5) 0.6281(4) 0.039(2) Uani 1 1 d . . .
H2A H -0.0885 0.8764 0.6271 0.047 Uiso 0.50 1 d PR A 1
H2B H -0.0930 0.7921 0.6506 0.047 Uiso 0.50 1 d PR A 1
N3 N -0.3126(9) 0.7691(5) 0.5340(4) 0.046(2) Uani 1 1 d . . .
H3A H -0.3459 0.7388 0.5020 0.055 Uiso 1 1 d R A .
H3B H -0.3243 0.7549 0.5726 0.055 Uiso 1 1 d R . .
N4 N -0.1500(9) 0.8950(5) 0.4913(4) 0.042(2) Uani 1 1 d . . .
H4C H -0.1379 0.9298 0.5219 0.050 Uiso 1 1 d R A .
H4D H -0.1062 0.9020 0.4572 0.050 Uiso 1 1 d R . .
N5 N -0.0885(14) 0.7334(6) 0.4338(5) 0.083(4) Uani 1 1 d . . .
H5BC H -0.1773 0.7407 0.4158 0.100 Uiso 0.50 1 d PR A 2
H5BD H -0.0147 0.7511 0.4166 0.100 Uiso 0.50 1 d PR A 2
N6 N -0.0239(12) 0.6666(6) 0.5570(5) 0.071(3) Uani 1 1 d . . .
H6AA H 0.0683 0.6650 0.5723 0.085 Uiso 0.50 1 d PR A 1
H6AB H -0.0908 0.6513 0.5795 0.085 Uiso 0.50 1 d PR A 1
N7 N 0.4689(10) 0.5510(5) 0.3606(5) 0.059(3) Uani 1 1 d . . .
H7C H 0.3892 0.5743 0.3377 0.071 Uiso 1 1 d R . .
H7D H 0.5546 0.5738 0.3511 0.071 Uiso 1 1 d R . .
H7E H 0.4699 0.4989 0.3511 0.071 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 F1 1.817(5) . ?
Ge1 O4 1.854(5) . ?
Ge1 O5 1.865(5) . ?
Ge1 O2 1.876(5) . ?
Ge1 O3 1.901(6) . ?
Ge1 O1 1.968(5) . ?
Ge2 O8 1.752(6) . ?
Ge2 O6 1.756(6) . ?
Ge2 O7 1.768(5) . ?
Ge2 F2 1.808(4) . ?
Ge2 O1 1.967(5) . ?
Ge2 Ge3 2.8840(14) . ?
Ge3 O11 1.773(6) . ?
Ge3 O10 1.774(5) . ?
Ge3 O6 1.794(5) . ?
Ge3 O9 1.810(6) . ?
Ge3 O1 2.042(5) . ?
Ge4 O12 1.725(5) . ?
Ge4 O2 1.740(5) . ?
Ge4 O7 1.747(5) . ?
Ge4 O13 1.747(6) . ?
Ge5 O3 1.721(6) . ?
Ge5 O15 1.728(6) 2 ?
Ge5 O14 1.759(5) . ?
Ge5 O8 1.766(5) . ?
Ge6 O4 1.716(6) . ?
Ge6 O12 1.738(5) 1_655 ?
Ge6 O14 1.741(6) . ?
Ge6 O10 1.749(6) . ?
Ge7 O15 1.720(6) . ?
Ge7 O5 1.733(5) . ?
Ge7 O11 1.738(6) . ?
Ge7 O13 1.763(5) . ?
Ni1 N4 2.079(8) . ?
Ni1 N6 2.083(10) . ?
Ni1 N1 2.119(9) . ?
Ni1 N3 2.129(8) . ?
Ni1 N2 2.145(8) . ?
Ni1 N5 2.195(10) . ?
O9 C10 1.366(16) . ?
O12 Ge6 1.738(5) 1_455 ?
O15 Ge5 1.728(6) 2_545 ?
C1 C2 1.45(5) . ?
C1 N1 1.58(4) . ?
C1 H1A 0.9701 . ?
C1 H1B 0.9586 . ?
C1 H1'A 1.0190 . ?
C1 H2' 1.5554 . ?
C1' N1 1.39(4) . ?
C1' C2' 1.63(4) . ?
C1' H1B 0.9775 . ?
C1' H1'A 0.9679 . ?
C1' H1'B 1.0147 . ?
C1' H1C 1.5385 . ?
C2' C3 1.48(3) . ?
C2' N2 1.53(3) . ?
C2' H1A 1.4851 . ?
C2' H2' 0.9800 . ?
C2' H2A 1.5731 . ?
C2 N2 1.46(3) . ?
C2 C3 1.54(3) . ?
C2 H1'B 1.4933 . ?
C2 H2 0.9800 . ?
C3 H3BD 0.9706 . ?
C3 H3BE 0.9571 . ?
C3 H3BF 0.9886 . ?
C3 H3AA 0.9596 . ?
C3 H3AB 0.9624 . ?
C3 H3AC 0.9924 . ?
C4 N3 1.459(13) . ?
C4 C5 1.492(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N4 1.469(12) . ?
C5 C6 1.529(17) . ?
C5 H5 0.9799 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.41(5) . ?
C7 N6 1.60(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9509 . ?
C7 H7'A 0.9645 . ?
C7 H7'B 1.5524 . ?
C7 H8' 1.4929 . ?
C7' N6 1.37(4) . ?
C7' C8' 1.65(5) . ?
C7' H7B 0.9630 . ?
C7' H7'A 1.0195 . ?
C7' H7'B 0.9892 . ?
C8' N5 1.35(2) . ?
C8' C9 1.45(2) . ?
C8' H8' 0.9801 . ?
C8 N5 1.60(4) . ?
C8 C9 1.95(4) . ?
C8 H7'B 1.1943 . ?
C8 H8 0.9800 . ?
C9 H9BD 0.9599 . ?
C9 H9BE 0.9598 . ?
C9 H9BF 0.9601 . ?
C9 H9AA 0.9598 . ?
C9 H9AB 0.9600 . ?
C9 H9AC 0.9598 . ?
C10 C11 1.56(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N7 1.422(17) . ?
C11 H11A 0.9699 . ?
C11 H11B 0.9701 . ?
N1 H1C 0.8602 . ?
N1 H1D 0.8598 . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8597 . ?
N3 H3A 0.8601 . ?
N3 H3B 0.8600 . ?
N4 H4C 0.8600 . ?
N4 H4D 0.8598 . ?
N5 H5BC 0.8363 . ?
N5 H5BD 0.8357 . ?
N6 H6AA 0.8376 . ?
N6 H6AB 0.8388 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8899 . ?
N7 H7E 0.8899 . ?

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
F1 Ge1 O4 92.2(2) . . ?
F1 Ge1 O5 89.2(2) . . ?
O4 Ge1 O5 89.4(2) . . ?
F1 Ge1 O2 88.2(2) . . ?
O4 Ge1 O2 179.5(3) . . ?
O5 Ge1 O2 91.0(2) . . ?
F1 Ge1 O3 89.3(2) . . ?
O4 Ge1 O3 91.7(2) . . ?
O5 Ge1 O3 178.2(2) . . ?
O2 Ge1 O3 87.9(2) . . ?
F1 Ge1 O1 177.8(2) . . ?
O4 Ge1 O1 89.9(2) . . ?
O5 Ge1 O1 91.5(2) . . ?
O2 Ge1 O1 89.8(2) . . ?
O3 Ge1 O1 89.9(2) . . ?
O8 Ge2 O6 124.0(3) . . ?
O8 Ge2 O7 116.7(3) . . ?
O6 Ge2 O7 119.3(3) . . ?
O8 Ge2 F2 89.4(2) . . ?
O6 Ge2 F2 90.7(2) . . ?
O7 Ge2 F2 89.7(2) . . ?
O8 Ge2 O1 93.8(2) . . ?
O6 Ge2 O1 81.1(2) . . ?
O7 Ge2 O1 95.8(2) . . ?
F2 Ge2 O1 171.6(2) . . ?
O8 Ge2 Ge3 114.80(18) . . ?
O6 Ge2 Ge3 36.13(17) . . ?
O7 Ge2 Ge3 115.53(19) . . ?
F2 Ge2 Ge3 126.71(18) . . ?
O1 Ge2 Ge3 45.05(15) . . ?
O11 Ge3 O10 115.7(3) . . ?
O11 Ge3 O6 119.3(3) . . ?
O10 Ge3 O6 124.3(3) . . ?
O11 Ge3 O9 94.0(3) . . ?
O10 Ge3 O9 89.4(3) . . ?
O6 Ge3 O9 94.9(3) . . ?
O11 Ge3 O1 91.1(2) . . ?
O10 Ge3 O1 92.8(2) . . ?
O6 Ge3 O1 78.2(2) . . ?
O9 Ge3 O1 172.8(2) . . ?
O11 Ge3 Ge2 111.84(18) . . ?
O10 Ge3 Ge2 113.71(19) . . ?
O6 Ge3 Ge2 35.25(18) . . ?
O9 Ge3 Ge2 130.08(19) . . ?
O1 Ge3 Ge2 42.97(14) . . ?
O12 Ge4 O2 103.4(3) . . ?
O12 Ge4 O7 111.7(3) . . ?
O2 Ge4 O7 113.1(3) . . ?
O12 Ge4 O13 108.1(3) . . ?
O2 Ge4 O13 113.1(2) . . ?
O7 Ge4 O13 107.3(3) . . ?
O3 Ge5 O15 115.7(3) . 2 ?
O3 Ge5 O14 110.4(3) . . ?
O15 Ge5 O14 103.5(3) 2 . ?
O3 Ge5 O8 111.5(3) . . ?
O15 Ge5 O8 103.4(3) 2 . ?
O14 Ge5 O8 111.9(3) . . ?
O4 Ge6 O12 105.0(3) . 1_655 ?
O4 Ge6 O14 113.3(3) . . ?
O12 Ge6 O14 108.2(3) 1_655 . ?
O4 Ge6 O10 113.4(3) . . ?
O12 Ge6 O10 108.2(3) 1_655 . ?
O14 Ge6 O10 108.4(3) . . ?
O15 Ge7 O5 108.9(3) . . ?
O15 Ge7 O11 107.2(3) . . ?
O5 Ge7 O11 114.4(3) . . ?
O15 Ge7 O13 105.2(3) . . ?
O5 Ge7 O13 110.3(3) . . ?
O11 Ge7 O13 110.3(3) . . ?
N4 Ni1 N6 170.0(4) . . ?
N4 Ni1 N1 95.4(4) . . ?
N6 Ni1 N1 91.2(4) . . ?
N4 Ni1 N3 81.6(3) . . ?
N6 Ni1 N3 93.0(4) . . ?
N1 Ni1 N3 170.5(4) . . ?
N4 Ni1 N2 94.1(3) . . ?
N6 Ni1 N2 94.2(4) . . ?
N1 Ni1 N2 82.3(3) . . ?
N3 Ni1 N2 89.0(3) . . ?
N4 Ni1 N5 89.9(4) . . ?
N6 Ni1 N5 81.8(4) . . ?
N1 Ni1 N5 97.0(4) . . ?
N3 Ni1 N5 92.0(4) . . ?
N2 Ni1 N5 175.9(4) . . ?
Ge1 O1 Ge2 134.1(3) . . ?
Ge1 O1 Ge3 134.0(3) . . ?
Ge2 O1 Ge3 92.0(2) . . ?
Ge4 O2 Ge1 118.8(3) . . ?
Ge5 O3 Ge1 118.7(3) . . ?
Ge6 O4 Ge1 119.2(3) . . ?
Ge7 O5 Ge1 118.2(3) . . ?
Ge2 O6 Ge3 108.6(3) . . ?
Ge4 O7 Ge2 119.4(3) . . ?
Ge2 O8 Ge5 121.6(3) . . ?
C10 O9 Ge3 121.1(8) . . ?
Ge6 O10 Ge3 121.3(3) . . ?
Ge7 O11 Ge3 123.5(3) . . ?
Ge4 O12 Ge6 143.7(4) . 1_455 ?
Ge4 O13 Ge7 119.2(3) . . ?
Ge6 O14 Ge5 119.5(3) . . ?
Ge7 O15 Ge5 140.9(4) . 2_545 ?
C2 C1 N1 107(2) . . ?
C2 C1 H1A 111.1 . . ?
N1 C1 H1A 110.6 . . ?
C2 C1 H1B 107.4 . . ?
N1 C1 H1B 107.5 . . ?
H1A C1 H1B 113.3 . . ?
C2 C1 H1'A 110.1 . . ?
N1 C1 H1'A 100.0 . . ?
H1A C1 H1'A 117.3 . . ?
H1B C1 H1'A 7.4 . . ?
C2 C1 H2' 70.4 . . ?
N1 C1 H2' 120.0 . . ?
H1A C1 H2' 40.8 . . ?
H1B C1 H2' 131.2 . . ?
H1'A C1 H2' 138.5 . . ?
N1 C1' C2' 113(2) . . ?
N1 C1' H1B 122.8 . . ?
C2' C1' H1B 97.2 . . ?
N1 C1' H1'A 117.9 . . ?
C2' C1' H1'A 105.5 . . ?
H1B C1' H1'A 8.3 . . ?
N1 C1' H1'B 111.8 . . ?
C2' C1' H1'B 101.5 . . ?
H1B C1' H1'B 108.2 . . ?
H1'A C1' H1'B 106.0 . . ?
N1 C1' H1C 33.7 . . ?
C2' C1' H1C 138.1 . . ?
H1B C1' H1C 121.3 . . ?
H1'A C1' H1C 113.3 . . ?
H1'B C1' H1C 82.8 . . ?
C3 C2' N2 110.1(18) . . ?
C3 C2' C1' 115(2) . . ?
N2 C2' C1' 102.1(18) . . ?
C3 C2' H1A 122.3 . . ?
N2 C2' H1A 127.1 . . ?
C1' C2' H1A 63.5 . . ?
C3 C2' H2' 111.3 . . ?
N2 C2' H2' 111.4 . . ?
C1' C2' H2' 106.9 . . ?
H1A C2' H2' 44.1 . . ?
C3 C2' H2A 108.9 . . ?
N2 C2' H2A 32.1 . . ?
C1' C2' H2A 126.8 . . ?
H1A C2' H2A 115.1 . . ?
H2' C2' H2A 83.2 . . ?
C1 C2 N2 113(2) . . ?
C1 C2 C3 109(2) . . ?
N2 C2 C3 110.4(18) . . ?
C1 C2 H1'B 67.7 . . ?
N2 C2 H1'B 121.0 . . ?
C3 C2 H1'B 125.3 . . ?
C1 C2 H2 109.7 . . ?
N2 C2 H2 107.0 . . ?
C3 C2 H2 107.5 . . ?
H1'B C2 H2 42.2 . . ?
C2' C3 C2 29.3(11) . . ?
C2' C3 H3BD 111.6 . . ?
C2 C3 H3BD 83.1 . . ?
C2' C3 H3BE 112.6 . . ?
C2 C3 H3BE 118.8 . . ?
H3BD C3 H3BE 108.8 . . ?
C2' C3 H3BF 109.8 . . ?
C2 C3 H3BF 126.9 . . ?
H3BD C3 H3BF 106.3 . . ?
H3BE C3 H3BF 107.3 . . ?
C2' C3 H3AA 121.3 . . ?
C2 C3 H3AA 112.7 . . ?
H3BD C3 H3AA 82.5 . . ?
H3BE C3 H3AA 26.6 . . ?
H3BF C3 H3AA 120.3 . . ?
C2' C3 H3AB 80.8 . . ?
C2 C3 H3AB 109.9 . . ?
H3BD C3 H3AB 155.9 . . ?
H3BE C3 H3AB 83.3 . . ?
H3BF C3 H3AB 49.6 . . ?
H3AA C3 H3AB 109.3 . . ?
C2' C3 H3AC 125.8 . . ?
C2 C3 H3AC 111.3 . . ?
H3BD C3 H3AC 49.2 . . ?
H3BE C3 H3AC 121.5 . . ?
H3BF C3 H3AC 57.1 . . ?
H3AA C3 H3AC 106.8 . . ?
H3AB C3 H3AC 106.6 . . ?
N3 C4 C5 109.2(9) . . ?
N3 C4 H4A 109.6 . . ?
C5 C4 H4A 109.8 . . ?
N3 C4 H4B 109.3 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C5 C4 107.1(9) . . ?
N4 C5 C6 110.7(10) . . ?
C4 C5 C6 116.1(10) . . ?
N4 C5 H5 107.7 . . ?
C4 C5 H5 107.8 . . ?
C6 C5 H5 107.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N6 93(3) . . ?
C8 C7 H7A 128.5 . . ?
N6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.6 . . ?
N6 C7 H7B 101.5 . . ?
H7A C7 H7B 110.4 . . ?
C8 C7 H7'A 113.6 . . ?
N6 C7 H7'A 103.3 . . ?
H7A C7 H7'A 105.7 . . ?
H7B C7 H7'A 4.7 . . ?
C8 C7 H7'B 47.3 . . ?
N6 C7 H7'B 77.6 . . ?
H7A C7 H7'B 172.6 . . ?
H7B C7 H7'B 69.2 . . ?
H7'A C7 H7'B 73.9 . . ?
C8 C7 H8' 74.5 . . ?
N6 C7 H8' 120.4 . . ?
H7A C7 H8' 54.1 . . ?
H7B C7 H8' 138.0 . . ?
H7'A C7 H8' 135.6 . . ?
H7'B C7 H8' 120.9 . . ?
N6 C7' C8' 117(3) . . ?
N6 C7' H7B 118.9 . . ?
C8' C7' H7B 109.5 . . ?
N6 C7' H7'A 117.6 . . ?
C8' C7' H7'A 108.4 . . ?
H7B C7' H7'A 3.2 . . ?
N6 C7' H7'B 112.8 . . ?
C8' C7' H7'B 93.7 . . ?
H7B C7' H7'B 100.9 . . ?
H7'A C7' H7'B 104.1 . . ?
N5 C8' C9 124.8(17) . . ?
N5 C8' C7' 110.4(19) . . ?
C9 C8' C7' 120(2) . . ?
N5 C8' H8' 97.5 . . ?
C9 C8' H8' 98.7 . . ?
C7' C8' H8' 94.4 . . ?
C7 C8 N5 106(3) . . ?
C7 C8 C9 94(3) . . ?
N5 C8 C9 88(2) . . ?
C7 C8 H7'B 72.8 . . ?
N5 C8 H7'B 152.4 . . ?
C9 C8 H7'B 119.4 . . ?
C7 C8 H8 126.7 . . ?
N5 C8 H8 118.6 . . ?
C9 C8 H8 114.5 . . ?
H7'B C8 H8 54.1 . . ?
C8' C9 C8 25.4(13) . . ?
C8' C9 H9BD 102.3 . . ?
C8 C9 H9BD 79.3 . . ?
C8' C9 H9BE 115.6 . . ?
C8 C9 H9BE 114.5 . . ?
H9BD C9 H9BE 109.5 . . ?
C8' C9 H9BF 110.2 . . ?
C8 C9 H9BF 128.8 . . ?
H9BD C9 H9BF 109.5 . . ?
H9BE C9 H9BF 109.5 . . ?
C8' C9 H9AA 119.1 . . ?
C8 C9 H9AA 101.7 . . ?
H9BD C9 H9AA 71.9 . . ?
H9BE C9 H9AA 38.1 . . ?
H9BF C9 H9AA 129.3 . . ?
C8' C9 H9AB 91.4 . . ?
C8 C9 H9AB 115.7 . . ?
H9BD C9 H9AB 163.4 . . ?
H9BE C9 H9AB 71.7 . . ?
H9BF C9 H9AB 56.3 . . ?
H9AA C9 H9AB 109.5 . . ?
C8' C9 H9AC 116.0 . . ?
C8 C9 H9AC 110.6 . . ?
H9BD C9 H9AC 56.2 . . ?
H9BE C9 H9AC 128.3 . . ?
H9BF C9 H9AC 53.4 . . ?
H9AA C9 H9AC 109.5 . . ?
H9AB C9 H9AC 109.5 . . ?
O9 C10 C11 114.8(12) . . ?
O9 C10 H10A 108.6 . . ?
C11 C10 H10A 108.6 . . ?
O9 C10 H10B 108.6 . . ?
C11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.5 . . ?
N7 C11 C10 106.1(12) . . ?
N7 C11 H11A 110.1 . . ?
C10 C11 H11A 110.6 . . ?
N7 C11 H11B 110.4 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 109.5 . . ?
C1' N1 C1 25.4(18) . . ?
C1' N1 Ni1 109.4(14) . . ?
C1 N1 Ni1 107.6(15) . . ?
C1' N1 H1C 82.9 . . ?
C1 N1 H1C 107.4 . . ?
Ni1 N1 H1C 106.6 . . ?
C1' N1 H1D 128.0 . . ?
C1 N1 H1D 107.7 . . ?
Ni1 N1 H1D 107.0 . . ?
H1C N1 H1D 120.0 . . ?
C2 N2 C2' 29.6(11) . . ?
C2 N2 Ni1 107.5(11) . . ?
C2' N2 Ni1 109.3(11) . . ?
C2 N2 H2A 105.2 . . ?
C2' N2 H2A 76.7 . . ?
Ni1 N2 H2A 107.3 . . ?
C2 N2 H2B 109.0 . . ?
C2' N2 H2B 131.9 . . ?
Ni1 N2 H2B 107.3 . . ?
H2A N2 H2B 120.0 . . ?
C4 N3 Ni1 107.1(6) . . ?
C4 N3 H3A 107.2 . . ?
Ni1 N3 H3A 107.2 . . ?
C4 N3 H3B 107.5 . . ?
Ni1 N3 H3B 107.3 . . ?
H3A N3 H3B 120.0 . . ?
C5 N4 Ni1 108.8(6) . . ?
C5 N4 H4C 107.0 . . ?
Ni1 N4 H4C 106.9 . . ?
C5 N4 H4D 106.8 . . ?
Ni1 N4 H4D 107.0 . . ?
H4C N4 H4D 120.0 . . ?
C8' N5 C8 33.8(15) . . ?
C8' N5 Ni1 113.0(10) . . ?
C8 N5 Ni1 95.2(15) . . ?
C8' N5 H5BC 99.2 . . ?
C8 N5 H5BC 133.0 . . ?
Ni1 N5 H5BC 107.7 . . ?
C8' N5 H5BD 109.9 . . ?
C8 N5 H5BD 90.0 . . ?
Ni1 N5 H5BD 107.6 . . ?
H5BC N5 H5BD 119.4 . . ?
C7' N6 C7 23(2) . . ?
C7' N6 Ni1 112.5(16) . . ?
C7 N6 Ni1 107.2(18) . . ?
C7' N6 H6AA 96.6 . . ?
C7 N6 H6AA 118.8 . . ?
Ni1 N6 H6AA 107.4 . . ?
C7' N6 H6AB 113.6 . . ?
C7 N6 H6AB 95.7 . . ?
Ni1 N6 H6AB 107.0 . . ?
H6AA N6 H6AB 119.5 . . ?
C11 N7 H7C 109.5 . . ?
C11 N7 H7D 109.7 . . ?
H7C N7 H7D 109.5 . . ?
C11 N7 H7E 109.2 . . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1D F2 0.86 2.20 3.010(11) 156.0 .
N1 H1D O6 0.86 2.49 3.174(10) 137.5 .
N2 H2A O8 0.86 2.61 3.430(10) 158.8 3_576
N2 H2B O5 0.86 2.32 3.082(9) 148.2 4_576
N3 H3A O9 0.86 2.46 3.249(10) 153.1 1_455
N3 H3B O5 0.86 2.25 3.099(9) 168.6 4_576
N4 H4C F2 0.86 2.21 2.999(9) 153.0 3_576
N4 H4D F2 0.86 2.30 2.955(9) 133.1 .
N6 H6AA O1W 0.84 2.35 3.139(17) 156.5 4_676
N6 H6AB F1 0.84 2.22 3.031(10) 163.3 4_576
N6 H6AB O4 0.84 2.38 2.957(10) 126.3 4_576
N7 H7C O3 0.89 2.17 2.655(10) 113.6 2_545
N7 H7C O11 0.89 2.31 3.085(10) 146.1 .
N7 H7E O2 0.89 1.99 2.838(11) 159.5 2_545
N7 H7E F1 0.89 2.42 3.012(10) 124.6 2_545

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.199
_database_code_depnum_ccdc_archive 'CCDC 992865'
#######################################################################
#
#                 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_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Ni2(C6N4H18)3]0.5 [Ge7O14F2(OC2NH7)] H2O'
_chemical_formula_sum            'C11 H36 F2 Ge7 N7 Ni O16'
_chemical_formula_weight         1127.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1550 1.8000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c


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

_cell_length_a                   8.8029(18)
_cell_length_b                   16.671(3)
_cell_length_c                   21.293(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.21(3)
_cell_angle_gamma                90.00
_cell_volume                     3065.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17842
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      26.35

_exptl_crystal_description       'hexagonal rod'
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2196
_exptl_absorpt_coefficient_mu    7.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3171
_exptl_absorpt_correction_T_max  0.5226
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 5.00
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17842
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         26.35
_reflns_number_total             6232
_reflns_number_gt                4636
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.1000P)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         6232
_refine_ls_number_parameters     418
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1974
_refine_ls_wR_factor_gt          0.1765
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_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 0.52731(11) 0.35399(6) 0.80056(5) 0.0184(3) Uani 1 1 d . . .
Ge2 Ge 0.35416(13) 0.38074(7) 0.63237(6) 0.0317(3) Uani 1 1 d . . .
Ge3 Ge 0.56063(14) 0.24476(7) 0.65064(6) 0.0343(3) Uani 1 1 d . . .
Ge4 Ge 0.59275(11) 0.49314(6) 0.71141(5) 0.0210(3) Uani 1 1 d . . .
Ge5 Ge 0.18322(11) 0.32895(6) 0.73657(6) 0.0233(3) Uani 1 1 d . . .
Ge6 Ge 0.39846(12) 0.18583(6) 0.75897(5) 0.0210(3) Uani 1 1 d . . .
Ge7 Ge 0.80819(11) 0.35032(6) 0.73351(6) 0.0240(3) Uani 1 1 d . . .
Ni1 Ni 0.86996(18) 0.30699(10) 0.46065(9) 0.0442(4) Uani 1 1 d . C .
F1 F 0.5699(7) 0.3747(3) 0.8851(3) 0.0323(14) Uani 1 1 d . . .
F2 F 0.2492(10) 0.4141(5) 0.5556(4) 0.066(3) Uani 1 1 d . . .
O1 O 0.4837(7) 0.3316(4) 0.7079(3) 0.0222(15) Uani 1 1 d . . .
O2 O 0.5512(7) 0.4653(4) 0.7843(3) 0.0236(15) Uani 1 1 d . . .
O3 O 0.3168(7) 0.3732(4) 0.7971(3) 0.0229(15) Uani 1 1 d . . .
O4 O 0.5034(7) 0.2447(4) 0.8176(3) 0.0217(15) Uani 1 1 d . . .
O5 O 0.7371(7) 0.3363(4) 0.8024(4) 0.0269(16) Uani 1 1 d . . .
O6 O 0.4276(10) 0.3000(5) 0.5935(4) 0.045(2) Uani 1 1 d . . .
O7 O 0.4431(8) 0.4768(4) 0.6458(4) 0.0302(18) Uani 1 1 d . . .
O8 O 0.1781(8) 0.3696(4) 0.6608(4) 0.0337(18) Uani 1 1 d . . .
O9 O 0.6206(12) 0.1789(5) 0.5922(4) 0.051(3) Uani 1 1 d . . .
O10 O 0.4924(9) 0.1669(4) 0.6948(4) 0.0321(18) Uani 1 1 d . . .
O11 O 0.7543(8) 0.2768(4) 0.6751(4) 0.037(2) Uani 1 1 d . . .
O12 O 0.7635(8) 0.4455(4) 0.6992(4) 0.0279(17) Uani 1 1 d . . .
O13 O 0.0059(8) 0.3458(5) 0.7589(4) 0.039(2) Uani 1 1 d . . .
O14 O 0.2118(7) 0.2249(4) 0.7312(4) 0.0286(17) Uani 1 1 d . . .
O15 O 0.3652(8) 0.0947(4) 0.7928(4) 0.0295(17) Uani 1 1 d . . .
N1 N 0.9438(12) 0.2676(7) 0.5557(6) 0.055(3) Uani 1 1 d . . .
H1A H 1.0212 0.2974 0.5719 0.066 Uiso 1 1 d R . .
H1B H 0.8625 0.2669 0.5725 0.066 Uiso 1 1 d R . .
N2 N 0.9216(13) 0.1873(7) 0.4436(7) 0.057(3) Uani 1 1 d . C .
H2 H 0.8519 0.1673 0.4101 0.068 Uiso 1 1 d R . .
N3 N 1.1009(18) 0.3227(11) 0.4435(8) 0.088(5) Uani 1 1 d U . .
H3A H 1.1819 0.3376 0.4747 0.106 Uiso 0.50 1 d PR A 1
H3B H 1.1531 0.3630 0.4673 0.106 Uiso 0.50 1 d PR A 2
N4 N 0.8062(16) 0.3428(8) 0.3648(6) 0.071(4) Uani 1 1 d . . .
H4A H 0.7781 0.2999 0.3432 0.085 Uiso 1 1 d R C .
H4B H 0.7414 0.3814 0.3649 0.085 Uiso 1 1 d R . .
N5 N 0.6355(12) 0.2891(7) 0.4648(6) 0.050(3) Uani 1 1 d . . .
H5A H 0.5907 0.2698 0.4285 0.060 Uiso 1 1 d R C .
H5B H 0.6330 0.2630 0.4995 0.060 Uiso 1 1 d R . .
N6 N 0.8196(19) 0.4250(9) 0.4934(10) 0.101(5) Uani 1 1 d . . .
H6 H 0.8022 0.4624 0.4617 0.121 Uiso 1 1 d R C .
N7 N 0.6716(17) 0.0261(7) 0.6494(8) 0.080(5) Uani 1 1 d . . .
H7C H 0.7713 0.0126 0.6565 0.096 Uiso 1 1 d R . .
H7D H 0.6612 0.0738 0.6668 0.096 Uiso 1 1 d R . .
H7E H 0.6188 -0.0105 0.6668 0.096 Uiso 1 1 d R . .
C1 C 1.003(3) 0.1873(11) 0.5573(12) 0.116(9) Uani 1 1 d . . .
H1C H 1.1128 0.1873 0.5559 0.139 Uiso 1 1 d R . .
H1D H 0.9877 0.1622 0.5966 0.139 Uiso 1 1 d R . .
C2 C 0.914(3) 0.1435(11) 0.5019(10) 0.097(7) Uani 1 1 d . . .
H2A H 0.8064 0.1385 0.5059 0.116 Uiso 1 1 d R . .
H2B H 0.9583 0.0905 0.5000 0.116 Uiso 1 1 d R . .
C3 C 1.069(2) 0.1779(13) 0.4221(12) 0.097(7) Uani 1 1 d . . .
H3AA H 1.1140 0.1272 0.4376 0.116 Uiso 0.50 1 d PR B 1
H3AB H 1.0501 0.1782 0.3761 0.116 Uiso 0.50 1 d PR B 1
C4 C 1.180(4) 0.263(2) 0.438(2) 0.057(9) Uani 0.50 1 d PU C 1
H4C H 1.2364 0.2673 0.4038 0.068 Uiso 0.50 1 d PR C 1
H4D H 1.2513 0.2513 0.4781 0.068 Uiso 0.50 1 d PR C 1
C4' C 1.182(5) 0.226(2) 0.453(2) 0.070(12) Uani 0.50 1 d PU C 2
H4'A H 1.2788 0.2245 0.4370 0.084 Uiso 0.50 1 d PR C 2
H4'B H 1.2033 0.2153 0.4984 0.084 Uiso 0.50 1 d PR C 2
C5 C 1.056(6) 0.404(3) 0.393(3) 0.112(16) Uani 0.50 1 d PU C 1
C5' C 1.093(4) 0.339(3) 0.3757(19) 0.079(10) Uani 0.50 1 d PU C 2
H5'A H 1.1766 0.3741 0.3695 0.094 Uiso 0.50 1 d PR C 2
H5'B H 1.1017 0.2881 0.3548 0.094 Uiso 0.50 1 d PR C 2
C6 C 0.934(3) 0.3768(18) 0.3389(12) 0.127(9) Uani 1 1 d . C .
H6AA H 0.9653 0.3390 0.3091 0.152 Uiso 0.50 1 d PR D 1
H6AB H 0.9014 0.4266 0.3167 0.152 Uiso 0.50 1 d PR D 1
H6BC H 0.9152 0.3670 0.2931 0.152 Uiso 0.50 1 d PR D 2
H6BD H 0.9404 0.4342 0.3468 0.152 Uiso 0.50 1 d PR D 2
C7 C 0.5685(18) 0.3683(8) 0.4714(8) 0.058(4) Uani 1 1 d . C .
H7A H 0.5455 0.3942 0.4299 0.070 Uiso 1 1 d R . .
H7B H 0.4738 0.3620 0.4878 0.070 Uiso 1 1 d R . .
C8 C 0.677(2) 0.4168(9) 0.5161(9) 0.068(5) Uani 1 1 d . C .
H8A H 0.6979 0.3915 0.5579 0.081 Uiso 1 1 d R . .
H8B H 0.6332 0.4696 0.5194 0.081 Uiso 1 1 d R . .
C9 C 0.944(2) 0.4761(11) 0.5218(12) 0.101(5) Uani 1 1 d . . .
H9A H 1.0082 0.4462 0.5508 0.121 Uiso 1 1 d R . .
H9B H 0.9038 0.5138 0.5440 0.121 Uiso 1 1 d R . .
C10 C 0.528(3) 0.1116(10) 0.5677(8) 0.088(6) Uani 1 1 d . . .
H10A H 0.4351 0.1109 0.5859 0.106 Uiso 1 1 d R . .
H10B H 0.4996 0.1175 0.5216 0.106 Uiso 1 1 d R . .
C11 C 0.613(3) 0.0291(11) 0.5812(11) 0.104(8) Uani 1 1 d . . .
H11A H 0.6980 0.0250 0.5582 0.125 Uiso 1 1 d R . .
H11B H 0.5407 -0.0143 0.5683 0.125 Uiso 1 1 d R . .
O1W O 1.011(2) 0.0726(15) 0.6949(11) 0.080(7) Uani 0.50 1 d P . .
O2W O 0.798(3) -0.0149(14) 0.4001(14) 0.104(10) Uani 0.50 1 d P . .


_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 F1 1.799(6) . ?
Ge1 O5 1.863(7) . ?
Ge1 O3 1.867(6) . ?
Ge1 O4 1.878(6) . ?
Ge1 O2 1.906(7) . ?
Ge1 O1 1.972(7) . ?
Ge2 O6 1.768(9) . ?
Ge2 O8 1.780(8) . ?
Ge2 O7 1.782(7) . ?
Ge2 F2 1.801(7) . ?
Ge2 O1 1.960(7) . ?
Ge2 Ge3 2.8842(18) . ?
Ge3 O11 1.766(7) . ?
Ge3 O6 1.774(9) . ?
Ge3 O10 1.775(7) . ?
Ge3 O9 1.814(8) . ?
Ge3 O1 2.088(7) . ?
Ge4 O2 1.727(7) . ?
Ge4 O15 1.740(6) 2_656 ?
Ge4 O7 1.745(7) . ?
Ge4 O12 1.764(6) . ?
Ge5 O3 1.732(7) . ?
Ge5 O13 1.741(7) . ?
Ge5 O8 1.743(8) . ?
Ge5 O14 1.760(7) . ?
Ge6 O4 1.710(7) . ?
Ge6 O15 1.730(7) . ?
Ge6 O10 1.757(7) . ?
Ge6 O14 1.760(7) . ?
Ge7 O5 1.719(8) . ?
Ge7 O13 1.721(7) 1_655 ?
Ge7 O11 1.745(8) . ?
Ge7 O12 1.759(7) . ?
Ni1 N4 2.096(13) . ?
Ni1 N2 2.093(11) . ?
Ni1 N5 2.105(11) . ?
Ni1 N1 2.106(12) . ?
Ni1 N3 2.150(15) . ?
Ni1 N6 2.162(15) . ?
O9 C10 1.425(19) . ?
O13 Ge7 1.721(7) 1_455 ?
O15 Ge4 1.740(6) 2_646 ?
N1 C1 1.44(2) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 C2 1.45(2) . ?
N2 C3 1.47(2) . ?
N2 H2 0.9099 . ?
N3 C4 1.24(3) . ?
N3 C5' 1.46(4) . ?
N3 C5 1.72(5) . ?
N3 C4' 1.77(4) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9101 . ?
N4 C6 1.46(2) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N5 C7 1.463(17) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N6 C9 1.43(2) . ?
N6 C8 1.43(2) . ?
N6 H6 0.9100 . ?
N7 C11 1.44(2) . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8899 . ?
N7 H7E 0.8898 . ?
C1 C2 1.48(3) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9701 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9699 . ?
C3 C4' 1.34(4) . ?
C3 C4 1.71(4) . ?
C3 H3AA 0.9644 . ?
C3 H3AB 0.9615 . ?
C4 H3A 1.4681 . ?
C4 H4C 0.9699 . ?
C4 H4D 0.9700 . ?
C4 H4'A 1.0846 . ?
C4 H4'B 1.4818 . ?
C4' H4C 1.4089 . ?
C4' H4D 0.8470 . ?
C4' H4'A 0.9701 . ?
C4' H4'B 0.9701 . ?
C5 C6 1.48(5) . ?
C5 H5'A 1.3565 . ?
C5 H6BD 1.3695 . ?
C5' C6 1.59(4) . ?
C5' H5'A 0.9701 . ?
C5' H5'B 0.9701 . ?
C6 H6AA 0.9704 . ?
C6 H6AB 0.9700 . ?
C6 H6BC 0.9701 . ?
C6 H6BD 0.9699 . ?
C7 C8 1.46(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9699 . ?
C8 H8A 0.9699 . ?
C8 H8B 0.9700 . ?
C9 C9 1.68(4) 3_766 ?
C9 H9A 0.9001 . ?
C9 H9B 0.9000 . ?
C10 C11 1.57(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9698 . ?
C11 H11A 0.9700 . ?
C11 H11B 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
F1 Ge1 O5 89.8(3) . . ?
F1 Ge1 O3 91.1(3) . . ?
O5 Ge1 O3 178.7(3) . . ?
F1 Ge1 O4 90.1(3) . . ?
O5 Ge1 O4 89.5(3) . . ?
O3 Ge1 O4 91.5(3) . . ?
F1 Ge1 O2 89.2(3) . . ?
O5 Ge1 O2 90.8(3) . . ?
O3 Ge1 O2 88.3(3) . . ?
O4 Ge1 O2 179.3(3) . . ?
F1 Ge1 O1 179.2(3) . . ?
O5 Ge1 O1 89.5(3) . . ?
O3 Ge1 O1 89.7(3) . . ?
O4 Ge1 O1 90.1(3) . . ?
O2 Ge1 O1 90.6(3) . . ?
O6 Ge2 O8 120.1(4) . . ?
O6 Ge2 O7 124.8(4) . . ?
O8 Ge2 O7 115.1(4) . . ?
O6 Ge2 F2 88.9(4) . . ?
O8 Ge2 F2 90.8(4) . . ?
O7 Ge2 F2 90.0(3) . . ?
O6 Ge2 O1 81.9(4) . . ?
O8 Ge2 O1 94.8(3) . . ?
O7 Ge2 O1 94.4(3) . . ?
F2 Ge2 O1 170.6(4) . . ?
O6 Ge2 Ge3 35.5(3) . . ?
O8 Ge2 Ge3 116.1(2) . . ?
O7 Ge2 Ge3 116.0(2) . . ?
F2 Ge2 Ge3 124.3(3) . . ?
O1 Ge2 Ge3 46.4(2) . . ?
O11 Ge3 O6 121.1(4) . . ?
O11 Ge3 O10 118.2(4) . . ?
O6 Ge3 O10 119.8(4) . . ?
O11 Ge3 O9 89.6(4) . . ?
O6 Ge3 O9 94.8(4) . . ?
O10 Ge3 O9 95.5(3) . . ?
O11 Ge3 O1 91.3(3) . . ?
O6 Ge3 O1 78.1(3) . . ?
O10 Ge3 O1 90.9(3) . . ?
O9 Ge3 O1 172.3(4) . . ?
O11 Ge3 Ge2 110.4(2) . . ?
O6 Ge3 Ge2 35.4(3) . . ?
O10 Ge3 Ge2 112.1(3) . . ?
O9 Ge3 Ge2 130.0(3) . . ?
O1 Ge3 Ge2 42.80(19) . . ?
O2 Ge4 O15 113.1(3) . 2_656 ?
O2 Ge4 O7 114.8(3) . . ?
O15 Ge4 O7 104.2(3) 2_656 . ?
O2 Ge4 O12 110.3(3) . . ?
O15 Ge4 O12 103.6(3) 2_656 . ?
O7 Ge4 O12 110.2(4) . . ?
O3 Ge5 O13 104.1(4) . . ?
O3 Ge5 O8 114.5(3) . . ?
O13 Ge5 O8 109.1(4) . . ?
O3 Ge5 O14 112.5(3) . . ?
O13 Ge5 O14 108.9(3) . . ?
O8 Ge5 O14 107.5(4) . . ?
O4 Ge6 O15 108.1(3) . . ?
O4 Ge6 O10 113.6(3) . . ?
O15 Ge6 O10 108.0(3) . . ?
O4 Ge6 O14 111.7(3) . . ?
O15 Ge6 O14 104.0(3) . . ?
O10 Ge6 O14 110.8(4) . . ?
O5 Ge7 O13 103.9(4) . 1_655 ?
O5 Ge7 O11 114.8(3) . . ?
O13 Ge7 O11 108.2(4) 1_655 . ?
O5 Ge7 O12 112.8(3) . . ?
O13 Ge7 O12 107.5(3) 1_655 . ?
O11 Ge7 O12 109.3(4) . . ?
N4 Ni1 N2 97.4(6) . . ?
N4 Ni1 N5 90.1(5) . . ?
N2 Ni1 N5 96.9(5) . . ?
N4 Ni1 N1 177.0(5) . . ?
N2 Ni1 N1 80.3(5) . . ?
N5 Ni1 N1 92.1(4) . . ?
N4 Ni1 N3 83.3(6) . . ?
N2 Ni1 N3 80.9(6) . . ?
N5 Ni1 N3 172.7(5) . . ?
N1 Ni1 N3 94.4(5) . . ?
N4 Ni1 N6 91.3(7) . . ?
N2 Ni1 N6 171.1(7) . . ?
N5 Ni1 N6 81.4(5) . . ?
N1 Ni1 N6 91.0(6) . . ?
N3 Ni1 N6 101.8(7) . . ?
Ge2 O1 Ge1 135.3(4) . . ?
Ge2 O1 Ge3 90.8(3) . . ?
Ge1 O1 Ge3 133.9(3) . . ?
Ge4 O2 Ge1 118.4(4) . . ?
Ge5 O3 Ge1 118.8(4) . . ?
Ge6 O4 Ge1 118.7(4) . . ?
Ge7 O5 Ge1 119.0(4) . . ?
Ge2 O6 Ge3 109.1(4) . . ?
Ge4 O7 Ge2 120.6(4) . . ?
Ge5 O8 Ge2 119.2(4) . . ?
C10 O9 Ge3 120.3(10) . . ?
Ge6 O10 Ge3 122.7(4) . . ?
Ge7 O11 Ge3 122.4(4) . . ?
Ge7 O12 Ge4 118.3(4) . . ?
Ge7 O13 Ge5 145.8(6) 1_455 . ?
Ge6 O14 Ge5 118.6(4) . . ?
Ge6 O15 Ge4 141.1(4) . 2_646 ?
C1 N1 Ni1 110.9(12) . . ?
C1 N1 H1A 105.8 . . ?
Ni1 N1 H1A 106.1 . . ?
C1 N1 H1B 107.8 . . ?
Ni1 N1 H1B 106.2 . . ?
H1A N1 H1B 120.0 . . ?
C2 N2 C3 113.8(16) . . ?
C2 N2 Ni1 106.5(11) . . ?
C3 N2 Ni1 113.0(11) . . ?
C2 N2 H2 110.5 . . ?
C3 N2 H2 102.6 . . ?
Ni1 N2 H2 110.4 . . ?
C4 N3 C5' 89(3) . . ?
C4 N3 C5 130(3) . . ?
C5' N3 C5 44(2) . . ?
C4 N3 C4' 17(3) . . ?
C5' N3 C4' 103(3) . . ?
C5 N3 C4' 146(3) . . ?
C4 N3 Ni1 119(2) . . ?
C5' N3 Ni1 109.0(15) . . ?
C5 N3 Ni1 95.2(19) . . ?
C4' N3 Ni1 104.3(16) . . ?
C4 N3 H3A 84.9 . . ?
C5' N3 H3A 123.6 . . ?
C5 N3 H3A 107.1 . . ?
C4' N3 H3A 85.7 . . ?
Ni1 N3 H3A 122.8 . . ?
C4 N3 H3B 114.6 . . ?
C5' N3 H3B 109.6 . . ?
C5 N3 H3B 78.3 . . ?
C4' N3 H3B 117.7 . . ?
Ni1 N3 H3B 112.8 . . ?
H3A N3 H3B 32.1 . . ?
C6 N4 Ni1 113.4(13) . . ?
C6 N4 H4A 106.4 . . ?
Ni1 N4 H4A 106.2 . . ?
C6 N4 H4B 105.8 . . ?
Ni1 N4 H4B 105.3 . . ?
H4A N4 H4B 120.0 . . ?
C7 N5 Ni1 107.0(8) . . ?
C7 N5 H5A 107.5 . . ?
Ni1 N5 H5A 107.3 . . ?
C7 N5 H5B 107.2 . . ?
Ni1 N5 H5B 107.2 . . ?
H5A N5 H5B 120.0 . . ?
C9 N6 C8 124.3(17) . . ?
C9 N6 Ni1 119.4(13) . . ?
C8 N6 Ni1 105.6(10) . . ?
C9 N6 H6 84.8 . . ?
C8 N6 H6 106.4 . . ?
Ni1 N6 H6 113.5 . . ?
C11 N7 H7C 109.0 . . ?
C11 N7 H7D 110.0 . . ?
H7C N7 H7D 109.5 . . ?
C11 N7 H7E 109.3 . . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?
N1 C1 C2 107.9(15) . . ?
N1 C1 H1C 111.1 . . ?
C2 C1 H1C 110.8 . . ?
N1 C1 H1D 108.2 . . ?
C2 C1 H1D 109.4 . . ?
H1C C1 H1D 109.5 . . ?
N2 C2 C1 109.0(17) . . ?
N2 C2 H2A 109.1 . . ?
C1 C2 H2A 110.5 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 109.5 . . ?
C4' C3 N2 114(2) . . ?
C4' C3 C4 22(2) . . ?
N2 C3 C4 110.6(17) . . ?
C4' C3 H3AA 97.9 . . ?
N2 C3 H3AA 108.4 . . ?
C4 C3 H3AA 118.4 . . ?
C4' C3 H3AB 117.2 . . ?
N2 C3 H3AB 109.2 . . ?
C4 C3 H3AB 100.5 . . ?
H3AA C3 H3AB 109.4 . . ?
N3 C4 C3 112(2) . . ?
N3 C4 H3A 38.1 . . ?
C3 C4 H3A 139.3 . . ?
N3 C4 H4C 112.5 . . ?
C3 C4 H4C 105.6 . . ?
H3A C4 H4C 112.0 . . ?
N3 C4 H4D 111.2 . . ?
C3 C4 H4D 105.3 . . ?
H3A C4 H4D 76.5 . . ?
H4C C4 H4D 109.5 . . ?
N3 C4 H4'A 161.1 . . ?
C3 C4 H4'A 86.5 . . ?
H3A C4 H4'A 125.8 . . ?
H4C C4 H4'A 59.4 . . ?
H4D C4 H4'A 61.3 . . ?
N3 C4 H4'B 110.1 . . ?
C3 C4 H4'B 73.4 . . ?
H3A C4 H4'B 90.8 . . ?
H4C C4 H4'B 133.6 . . ?
H4D C4 H4'B 35.5 . . ?
H4'A C4 H4'B 74.4 . . ?
C3 C4' N3 104(3) . . ?
C3 C4' H4C 105.1 . . ?
N3 C4' H4C 69.7 . . ?
C3 C4' H4D 169.5 . . ?
N3 C4' H4D 80.3 . . ?
H4C C4' H4D 85.3 . . ?
C3 C4' H4'A 116.1 . . ?
N3 C4' H4'A 110.0 . . ?
H4C C4' H4'A 46.5 . . ?
H4D C4' H4'A 70.4 . . ?
C3 C4' H4'B 111.1 . . ?
N3 C4' H4'B 105.5 . . ?
H4C C4' H4'B 143.4 . . ?
H4D C4' H4'B 58.4 . . ?
H4'A C4' H4'B 109.5 . . ?
C6 C5 N3 107(3) . . ?
C6 C5 H5'A 95.6 . . ?
N3 C5 H5'A 80.9 . . ?
C6 C5 H6BD 39.5 . . ?
N3 C5 H6BD 142.0 . . ?
H5'A C5 H6BD 113.0 . . ?
N3 C5' C6 116(2) . . ?
N3 C5' H5'A 110.8 . . ?
C6 C5' H5'A 108.2 . . ?
N3 C5' H5'B 107.4 . . ?
C6 C5' H5'B 105.2 . . ?
H5'A C5' H5'B 109.4 . . ?
C5 C6 N4 108(3) . . ?
C5 C6 C5' 46(2) . . ?
N4 C6 C5' 109(2) . . ?
C5 C6 H6AA 117.1 . . ?
N4 C6 H6AA 109.2 . . ?
C5' C6 H6AA 74.6 . . ?
C5 C6 H6AB 102.9 . . ?
N4 C6 H6AB 109.6 . . ?
C5' C6 H6AB 136.8 . . ?
H6AA C6 H6AB 109.4 . . ?
C5 C6 H6BC 142.5 . . ?
N4 C6 H6BC 108.5 . . ?
C5' C6 H6BC 113.2 . . ?
H6AA C6 H6BC 41.4 . . ?
H6AB C6 H6BC 71.2 . . ?
C5 C6 H6BD 63.9 . . ?
N4 C6 H6BD 109.7 . . ?
C5' C6 H6BD 107.0 . . ?
H6AA C6 H6BD 137.8 . . ?
H6AB C6 H6BD 40.8 . . ?
H6BC C6 H6BD 109.4 . . ?
C8 C7 N5 109.7(13) . . ?
C8 C7 H7A 110.0 . . ?
N5 C7 H7A 109.4 . . ?
C8 C7 H7B 109.1 . . ?
N5 C7 H7B 109.1 . . ?
H7A C7 H7B 109.5 . . ?
N6 C8 C7 109.9(15) . . ?
N6 C8 H8A 109.4 . . ?
C7 C8 H8A 109.9 . . ?
N6 C8 H8B 109.1 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 109.5 . . ?
N6 C9 C9 122(2) . 3_766 ?
N6 C9 H9A 106.7 . . ?
C9 C9 H9A 106.7 3_766 . ?
N6 C9 H9B 106.8 . . ?
C9 C9 H9B 107.0 3_766 . ?
H9A C9 H9B 106.6 . . ?
O9 C10 C11 113.9(17) . . ?
O9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.2 . . ?
O9 C10 H10B 107.8 . . ?
C11 C10 H10B 107.1 . . ?
H10A C10 H10B 109.5 . . ?
N7 C11 C10 106.2(16) . . ?
N7 C11 H11A 110.3 . . ?
C10 C11 H11A 111.0 . . ?
N7 C11 H11B 110.1 . . ?
C10 C11 H11B 109.7 . . ?
H11A C11 H11B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O8 0.86 2.43 3.218(13) 152.1 1_655
N1 H1B O11 0.86 2.55 3.304(14) 146.6 .
N2 H2 O5 0.91 2.32 3.152(15) 152.1 4_565
N2 H2 F1 0.91 2.53 3.272(13) 138.5 4_565
N3 H3B F2 0.91 2.09 2.918(17) 151.0 1_655
N3 H3B F2 0.91 2.09 2.918(17) 151.0 1_655
N4 H4A O5 0.86 2.43 3.277(14) 166.9 4_565
N4 H4A O4 0.86 2.49 3.033(14) 122.1 4_565
N5 H5A O4 0.86 2.35 3.175(14) 161.1 4_565
N5 H5A F1 0.86 2.57 3.208(13) 131.4 4_565
N5 H5B O9 0.86 2.44 3.298(14) 175.1 .
N6 H6 F2 0.91 2.13 2.901(19) 142.4 3_666
N7 H7C O1W 0.89 2.34 3.06(3) 138.2 .
N7 H7D O10 0.89 2.31 3.088(15) 146.5 .
N7 H7D O9 0.89 2.35 2.822(16) 113.6 .
N7 H7E O2 0.89 2.02 2.819(14) 148.2 2_646
N7 H7E O3 0.89 2.12 2.786(14) 130.7 2_646
N7 H7E F1 0.89 2.63 3.290(15) 131.4 2_646

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         5.541
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.255
_database_code_depnum_ccdc_archive 'CCDC 992866'
#######################################################################
#
#                 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_b_sqd

_audit_update_record             
;
2014-07-20 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[C2H8NO]2 [Ni2 (C8N5H23)2 (C2N2H8)] [Ge7O14F3]2 H2O'
_chemical_formula_sum            'C22 H72 F6 Ge14 N14 Ni2 O31'
_chemical_formula_weight         2276.62

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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   Pbcm


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

_cell_length_a                   8.8089(18)
_cell_length_b                   22.436(5)
_cell_length_c                   31.193(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6165(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4432
_exptl_absorpt_coefficient_mu    7.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2134
_exptl_absorpt_correction_T_max  0.4026
_exptl_absorpt_process_details   SADABS

_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            34855
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         26.35
_reflns_number_total             6400
_reflns_number_gt                5534
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0517P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6400
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0774
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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 0.79203(4) 0.276623(15) 0.138325(11) 0.01707(9) Uani 1 1 d . . .
Ge2 Ge 0.89786(4) 0.439075(17) 0.133540(12) 0.02261(10) Uani 1 1 d . . .
Ge3 Ge 0.70421(4) 0.396307(16) 0.065121(12) 0.02024(9) Uani 1 1 d . . .
Ge4 Ge 1.10559(4) 0.331642(15) 0.118233(11) 0.01861(9) Uani 1 1 d . . .
Ge5 Ge 0.68131(4) 0.378696(16) 0.198302(11) 0.01857(9) Uani 1 1 d . . .
Ge6 Ge 0.47955(4) 0.337812(16) 0.125979(11) 0.01883(9) Uani 1 1 d . . .
Ge7 Ge 0.90703(4) 0.289311(15) 0.044945(11) 0.01862(9) Uani 1 1 d . . .
Ni1 Ni 0.42815(6) 0.11901(2) 0.078027(16) 0.02945(12) Uani 1 1 d . . .
F1 F 0.7906(2) 0.20284(9) 0.16062(7) 0.0299(5) Uani 1 1 d . . .
F2 F 0.9654(3) 0.51322(10) 0.14301(8) 0.0444(6) Uani 1 1 d . . .
F3 F 0.6376(2) 0.44260(9) 0.02176(7) 0.0328(5) Uani 1 1 d . . .
O1 O 0.7951(2) 0.35901(10) 0.11524(7) 0.0189(5) Uani 1 1 d . . .
O2 O 0.7939(3) 0.46053(11) 0.08761(8) 0.0270(6) Uani 1 1 d . . .
O3 O 1.0806(2) 0.40716(11) 0.13036(8) 0.0255(5) Uani 1 1 d . . .
O4 O 0.8080(3) 0.43548(11) 0.18437(8) 0.0259(5) Uani 1 1 d . . .
O5 O 0.5139(3) 0.37731(11) 0.07866(8) 0.0255(5) Uani 1 1 d . . .
O6 O 0.7914(3) 0.34798(11) 0.02744(8) 0.0258(5) Uani 1 1 d . . .
O7 O 0.9990(2) 0.28384(10) 0.14949(8) 0.0223(5) Uani 1 1 d . . .
O8 O 1.0803(3) 0.31858(11) 0.06324(8) 0.0252(5) Uani 1 1 d . . .
O9 O 0.7566(3) 0.30791(10) 0.19482(7) 0.0228(5) Uani 1 1 d . . .
O10 O 0.5109(3) 0.38572(10) 0.16948(7) 0.0243(5) Uani 1 1 d . . .
O11 O 0.6245(4) 0.39743(15) 0.2500 0.0258(8) Uani 1 2 d S . .
O12 O 0.5828(2) 0.27254(10) 0.12977(8) 0.0217(5) Uani 1 1 d . . .
O13 O 0.2937(2) 0.31383(12) 0.12872(8) 0.0292(6) Uani 1 1 d . . .
O14 O 0.8218(3) 0.24508(10) 0.08301(8) 0.0227(5) Uani 1 1 d . . .
O15 O 0.9640(4) 0.2500 0.0000 0.0279(8) Uani 1 2 d S . .
N1 N 0.3557(4) 0.07780(14) 0.01936(11) 0.0362(8) Uani 1 1 d . . .
H1A H 0.3941 0.0982 -0.0030 0.054 Uiso 1 1 calc . . .
H1B H 0.3923 0.0404 0.0182 0.054 Uiso 1 1 calc . . .
N2 N 0.1917(4) 0.11521(16) 0.08806(13) 0.0458(10) Uani 1 1 d . . .
H2 H 0.1678 0.0790 0.0994 0.069 Uiso 1 1 calc . . .
N3 N 0.4251(5) 0.15253(16) 0.14247(12) 0.0508(11) Uani 1 1 d . . .
H3A H 0.4280 0.1405 0.1150 0.076 Uiso 1 1 calc . . .
H3B H 0.4705 0.1884 0.1440 0.076 Uiso 1 1 calc . . .
N4 N 0.4809(4) 0.03783(14) 0.10924(11) 0.0359(8) Uani 1 1 d . . .
H4 H 0.4089 0.0106 0.1019 0.054 Uiso 1 1 calc . . .
N5 N 0.6672(4) 0.11867(14) 0.06636(11) 0.0342(8) Uani 1 1 d . . .
H5A H 0.6845 0.1163 0.0380 0.051 Uiso 1 1 calc . . .
H5B H 0.7081 0.1529 0.0760 0.051 Uiso 1 1 calc . . .
N6 N 0.4262(4) 0.20879(14) 0.05325(10) 0.0358(8) Uani 1 1 d . . .
H6A H 0.3409 0.2266 0.0627 0.054 Uiso 1 1 calc . . .
H6B H 0.5050 0.2284 0.0650 0.054 Uiso 1 1 calc . . .
C1 C 0.1895(5) 0.0761(2) 0.01583(16) 0.0471(12) Uani 1 1 d . . .
H1C H 0.1531 0.0364 0.0227 0.071 Uiso 1 1 calc . . .
H1D H 0.1595 0.0853 -0.0134 0.071 Uiso 1 1 calc . . .
C2 C 0.1203(5) 0.1205(2) 0.04596(19) 0.0541(13) Uani 1 1 d . . .
H2A H 0.1349 0.1605 0.0349 0.081 Uiso 1 1 calc . . .
H2B H 0.0121 0.1133 0.0484 0.081 Uiso 1 1 calc . . .
C3 C 0.1549(7) 0.1612(2) 0.1191(2) 0.0679(17) Uani 1 1 d . . .
H3C H 0.0523 0.1553 0.1295 0.102 Uiso 1 1 calc . . .
H3D H 0.1599 0.2000 0.1055 0.102 Uiso 1 1 calc . . .
C4 C 0.2641(8) 0.1589(2) 0.15584(19) 0.0703(17) Uani 1 1 d . . .
H4A H 0.2537 0.1951 0.1726 0.105 Uiso 1 1 calc . . .
H4B H 0.2375 0.1256 0.1742 0.105 Uiso 1 1 calc . . .
C5 C 0.5106(6) 0.1101(2) 0.16867(15) 0.0556(13) Uani 1 1 d . . .
H5C H 0.4861 0.1162 0.1987 0.083 Uiso 1 1 calc . . .
H5D H 0.6185 0.1171 0.1650 0.083 Uiso 1 1 calc . . .
C6 C 0.4733(6) 0.0466(2) 0.15616(16) 0.0532(12) Uani 1 1 d . . .
H6C H 0.5443 0.0197 0.1700 0.080 Uiso 1 1 calc . . .
H6D H 0.3721 0.0368 0.1662 0.080 Uiso 1 1 calc . . .
C7 C 0.6281(5) 0.01682(19) 0.09244(17) 0.0469(11) Uani 1 1 d . . .
H7A H 0.6129 -0.0017 0.0647 0.070 Uiso 1 1 calc . . .
H7B H 0.6699 -0.0129 0.1117 0.070 Uiso 1 1 calc . . .
C8 C 0.7389(5) 0.0680(2) 0.08805(16) 0.0467(11) Uani 1 1 d . . .
H8A H 0.7733 0.0802 0.1163 0.070 Uiso 1 1 calc . . .
H8B H 0.8267 0.0551 0.0718 0.070 Uiso 1 1 calc . . .
C9 C 0.4341(5) 0.21742(17) 0.00661(13) 0.0365(9) Uani 1 1 d . . .
H9A H 0.3481 0.1977 -0.0066 0.055 Uiso 1 1 calc . . .
H9B H 0.5257 0.1986 -0.0041 0.055 Uiso 1 1 calc . . .
O2W O 0.5416(9) 0.2348(3) 0.2500 0.107(2) Uani 1 2 d S . .


_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 F1 1.796(2) . ?
Ge1 O7 1.864(2) . ?
Ge1 O12 1.865(2) . ?
Ge1 O14 1.883(2) . ?
Ge1 O9 1.922(2) . ?
Ge1 O1 1.984(2) . ?
Ge2 O3 1.765(2) . ?
Ge2 O2 1.767(2) . ?
Ge2 O4 1.774(2) . ?
Ge2 F2 1.791(2) . ?
Ge2 O1 2.091(2) . ?
Ge3 O6 1.774(2) . ?
Ge3 O5 1.780(2) . ?
Ge3 O2 1.787(2) . ?
Ge3 F3 1.804(2) . ?
Ge3 O1 1.945(2) . ?
Ge4 O7 1.727(2) . ?
Ge4 O13 1.735(2) 1_655 ?
Ge4 O3 1.750(2) . ?
Ge4 O8 1.755(2) . ?
Ge5 O9 1.725(2) . ?
Ge5 O11 1.7402(13) . ?
Ge5 O4 1.749(2) . ?
Ge5 O10 1.757(2) . ?
Ge6 O13 1.726(2) . ?
Ge6 O12 1.728(2) . ?
Ge6 O5 1.748(2) . ?
Ge6 O10 1.753(2) . ?
Ge7 O14 1.720(2) . ?
Ge7 O15 1.7307(11) . ?
Ge7 O6 1.752(2) . ?
Ge7 O8 1.757(2) . ?
Ni1 N2 2.108(4) . ?
Ni1 N4 2.117(3) . ?
Ni1 N5 2.137(3) . ?
Ni1 N3 2.146(4) . ?
Ni1 N1 2.147(3) . ?
Ni1 N6 2.157(3) . ?
O11 Ge5 1.7402(13) 6_556 ?
O13 Ge4 1.735(2) 1_455 ?
O15 Ge7 1.7307(11) 4 ?
N1 C1 1.469(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.451(6) . ?
N2 C2 1.461(6) . ?
N2 H2 0.9100 . ?
N3 C5 1.463(6) . ?
N3 C4 1.485(7) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C7 1.476(5) . ?
N4 C6 1.478(6) . ?
N4 H4 0.9100 . ?
N5 C8 1.466(5) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C9 1.469(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.499(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.498(9) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.514(6) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.514(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C9 1.519(7) 4 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Ge1 O7 90.82(9) . . ?
F1 Ge1 O12 90.19(10) . . ?
O7 Ge1 O12 176.64(11) . . ?
F1 Ge1 O14 90.54(10) . . ?
O7 Ge1 O14 93.87(10) . . ?
O12 Ge1 O14 89.33(10) . . ?
F1 Ge1 O9 88.88(10) . . ?
O7 Ge1 O9 87.46(10) . . ?
O12 Ge1 O9 89.36(10) . . ?
O14 Ge1 O9 178.56(10) . . ?
F1 Ge1 O1 178.45(10) . . ?
O7 Ge1 O1 88.50(9) . . ?
O12 Ge1 O1 90.41(9) . . ?
O14 Ge1 O1 90.89(10) . . ?
O9 Ge1 O1 89.70(10) . . ?
O3 Ge2 O2 122.54(11) . . ?
O3 Ge2 O4 116.02(11) . . ?
O2 Ge2 O4 120.38(11) . . ?
O3 Ge2 F2 94.78(11) . . ?
O2 Ge2 F2 93.02(11) . . ?
O4 Ge2 F2 92.46(11) . . ?
O3 Ge2 O1 91.79(10) . . ?
O2 Ge2 O1 77.77(10) . . ?
O4 Ge2 O1 90.68(10) . . ?
F2 Ge2 O1 170.61(10) . . ?
O3 Ge2 Ge3 111.19(8) . . ?
O2 Ge2 Ge3 35.65(8) . . ?
O4 Ge2 Ge3 112.39(8) . . ?
F2 Ge2 Ge3 128.67(8) . . ?
O1 Ge2 Ge3 42.18(6) . . ?
O6 Ge3 O5 114.73(11) . . ?
O6 Ge3 O2 124.19(11) . . ?
O5 Ge3 O2 121.07(11) . . ?
O6 Ge3 F3 89.77(10) . . ?
O5 Ge3 F3 90.53(10) . . ?
O2 Ge3 F3 88.50(10) . . ?
O6 Ge3 O1 95.25(10) . . ?
O5 Ge3 O1 95.38(10) . . ?
O2 Ge3 O1 81.34(10) . . ?
F3 Ge3 O1 169.81(10) . . ?
O6 Ge3 Ge2 115.84(8) . . ?
O5 Ge3 Ge2 117.33(8) . . ?
O2 Ge3 Ge2 35.21(8) . . ?
F3 Ge3 Ge2 123.61(7) . . ?
O1 Ge3 Ge2 46.20(7) . . ?
O7 Ge4 O13 105.64(12) . 1_655 ?
O7 Ge4 O3 114.26(11) . . ?
O13 Ge4 O3 107.59(12) 1_655 . ?
O7 Ge4 O8 112.30(11) . . ?
O13 Ge4 O8 105.48(12) 1_655 . ?
O3 Ge4 O8 110.92(12) . . ?
O9 Ge5 O11 113.05(13) . . ?
O9 Ge5 O4 114.18(11) . . ?
O11 Ge5 O4 103.77(14) . . ?
O9 Ge5 O10 112.28(11) . . ?
O11 Ge5 O10 101.92(13) . . ?
O4 Ge5 O10 110.67(12) . . ?
O13 Ge6 O12 103.40(12) . . ?
O13 Ge6 O5 111.36(12) . . ?
O12 Ge6 O5 113.35(11) . . ?
O13 Ge6 O10 107.59(12) . . ?
O12 Ge6 O10 112.57(11) . . ?
O5 Ge6 O10 108.39(12) . . ?
O14 Ge7 O15 113.06(9) . . ?
O14 Ge7 O6 113.26(11) . . ?
O15 Ge7 O6 107.41(10) . . ?
O14 Ge7 O8 111.76(11) . . ?
O15 Ge7 O8 101.62(13) . . ?
O6 Ge7 O8 109.01(11) . . ?
N2 Ni1 N4 96.53(13) . . ?
N2 Ni1 N5 177.18(14) . . ?
N4 Ni1 N5 81.90(13) . . ?
N2 Ni1 N3 82.11(16) . . ?
N4 Ni1 N3 82.73(14) . . ?
N5 Ni1 N3 99.97(15) . . ?
N2 Ni1 N1 79.37(15) . . ?
N4 Ni1 N1 94.98(13) . . ?
N5 Ni1 N1 98.40(13) . . ?
N3 Ni1 N1 160.96(14) . . ?
N2 Ni1 N6 94.77(14) . . ?
N4 Ni1 N6 165.88(13) . . ?
N5 Ni1 N6 87.14(13) . . ?
N3 Ni1 N6 90.48(13) . . ?
N1 Ni1 N6 95.41(13) . . ?
Ge3 O1 Ge1 133.39(12) . . ?
Ge3 O1 Ge2 91.61(9) . . ?
Ge1 O1 Ge2 134.99(11) . . ?
Ge2 O2 Ge3 109.13(13) . . ?
Ge4 O3 Ge2 121.32(13) . . ?
Ge5 O4 Ge2 122.68(13) . . ?
Ge6 O5 Ge3 119.00(13) . . ?
Ge7 O6 Ge3 120.30(13) . . ?
Ge4 O7 Ge1 118.71(12) . . ?
Ge4 O8 Ge7 119.35(13) . . ?
Ge5 O9 Ge1 117.16(12) . . ?
Ge6 O10 Ge5 118.39(12) . . ?
Ge5 O11 Ge5 135.9(2) . 6_556 ?
Ge6 O12 Ge1 119.23(13) . . ?
Ge6 O13 Ge4 145.57(18) . 1_455 ?
Ge7 O14 Ge1 118.46(13) . . ?
Ge7 O15 Ge7 146.3(2) 4 . ?
C1 N1 Ni1 111.8(3) . . ?
C1 N1 H1A 109.3 . . ?
Ni1 N1 H1A 109.3 . . ?
C1 N1 H1B 109.3 . . ?
Ni1 N1 H1B 109.3 . . ?
H1A N1 H1B 107.9 . . ?
C3 N2 C2 116.4(4) . . ?
C3 N2 Ni1 106.9(3) . . ?
C2 N2 Ni1 106.8(3) . . ?
C3 N2 H2 108.8 . . ?
C2 N2 H2 108.8 . . ?
Ni1 N2 H2 108.8 . . ?
C5 N3 C4 113.4(4) . . ?
C5 N3 Ni1 106.8(3) . . ?
C4 N3 Ni1 108.0(3) . . ?
C5 N3 H3A 108.9 . . ?
C4 N3 H3A 108.9 . . ?
Ni1 N3 H3A 3.2 . . ?
C5 N3 H3B 108.9 . . ?
C4 N3 H3B 108.9 . . ?
Ni1 N3 H3B 110.9 . . ?
H3A N3 H3B 107.7 . . ?
C7 N4 C6 115.7(4) . . ?
C7 N4 Ni1 107.7(3) . . ?
C6 N4 Ni1 109.3(3) . . ?
C7 N4 H4 107.9 . . ?
C6 N4 H4 107.9 . . ?
Ni1 N4 H4 107.9 . . ?
C8 N5 Ni1 110.4(2) . . ?
C8 N5 H5A 109.6 . . ?
Ni1 N5 H5A 109.6 . . ?
C8 N5 H5B 109.6 . . ?
Ni1 N5 H5B 109.6 . . ?
H5A N5 H5B 108.1 . . ?
C9 N6 Ni1 118.5(2) . . ?
C9 N6 H6A 107.7 . . ?
Ni1 N6 H6A 107.7 . . ?
C9 N6 H6B 107.7 . . ?
Ni1 N6 H6B 107.7 . . ?
H6A N6 H6B 107.1 . . ?
N1 C1 C2 109.9(4) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N2 C2 C1 109.5(4) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 110.0(5) . . ?
N2 C3 H3C 109.7 . . ?
C4 C3 H3C 109.7 . . ?
N2 C3 H3D 109.7 . . ?
C4 C3 H3D 109.7 . . ?
H3C C3 H3D 108.2 . . ?
N3 C4 C3 113.7(4) . . ?
N3 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
N3 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N3 C5 C6 110.9(4) . . ?
N3 C5 H5C 109.5 . . ?
C6 C5 H5C 109.5 . . ?
N3 C5 H5D 109.5 . . ?
C6 C5 H5D 109.5 . . ?
H5C C5 H5D 108.0 . . ?
N4 C6 C5 111.8(4) . . ?
N4 C6 H6C 109.3 . . ?
C5 C6 H6C 109.3 . . ?
N4 C6 H6D 109.3 . . ?
C5 C6 H6D 109.3 . . ?
H6C C6 H6D 107.9 . . ?
N4 C7 C8 110.9(3) . . ?
N4 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N5 C8 C7 110.6(3) . . ?
N5 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N5 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N6 C9 C9 113.3(4) . 4 ?
N6 C9 H9A 108.9 . . ?
C9 C9 H9A 108.9 4 . ?
N6 C9 H9B 108.9 . . ?
C9 C9 H9B 108.9 4 . ?
H9A C9 H9B 107.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N6 H6B O12 0.90 2.35 3.106(4) 141.4 .
N5 H5B O14 0.90 2.31 3.189(4) 166.0 .
N5 H5A O6 0.90 2.39 3.212(4) 152.7 4
N5 H5A F3 0.90 2.32 3.084(4) 142.5 4
N4 H4 O2 0.91 2.16 3.053(4) 168.2 8_655
N3 H3B O12 0.90 2.18 3.056(4) 165.2 .
N3 H3A N5 0.90 2.64 3.281(5) 128.7 .
N3 H3A N6 0.90 2.46 3.056(5) 124.0 .
N3 H3A N4 0.90 2.36 2.817(5) 111.7 .
N3 H3A N2 0.90 2.31 2.794(6) 113.2 .
N2 H2 F2 0.91 2.33 3.176(4) 155.6 8_655
N1 H1B F3 0.90 2.21 3.035(4) 151.7 8_655

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.133
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.015 0.104 0.250 530 235 ' '
2 0.015 0.326 0.750 530 235 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The remaining charge balancing organic species cations were disordered and assigned as eight protonated ethanolamine cations per unit cell, which were determined by TGA and elemental analysis. Then, the formula can be get as (NH3CH2CH2OH)2 [Ni2(TEPA)2(en)] [Ge7O14F3]2 H2O, with elemental analysis of C 11.61 (calcd wt%) 11.45 (found wt%), N 8.62 (calcd wt%) 8.86 (found wt%), N 3.19 (calcd wt%) 3.25 (found wt%). The contributions of these disordered protonated ethanolamine cations to the scattering values have been removed by using the PLATON SQUEEZE program.
;

_database_code_depnum_ccdc_archive 'CCDC 992867'
