# 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
#  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_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H8 Al Ge3 N O8'
_chemical_formula_weight         418.84

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'
Al Al 0.0645 0.0514 '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           Tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2'
_symmetry_space_group_name_HALL  'P 4abw 2nw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   10.3388(7)
_cell_length_b                   10.3388(7)
_cell_length_c                   9.4073(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1005.55(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7600
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      26.65

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    9.021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3649
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7149
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         25.01
_reflns_number_total             901
_reflns_number_gt                855
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_number_reflns         901
_refine_ls_number_parameters     74
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.56792(7) 0.43208(7) 0.2500 0.0089(3) Uani 0.75 2 d SP . .
Al1 Al 0.56792(7) 0.43208(7) 0.2500 0.0089(3) Uani 0.25 2 d SP . .
Ge2 Ge 0.86750(8) 0.13250(8) 0.2500 0.0122(3) Uani 0.75 2 d SP . .
Al2 Al 0.86750(8) 0.13250(8) 0.2500 0.0122(3) Uani 0.25 2 d SP . .
Ge3 Ge 0.86507(8) 0.42921(9) 0.34345(9) 0.0170(3) Uani 0.75 1 d P . .
Al3 Al 0.86507(8) 0.42921(9) 0.34345(9) 0.0170(3) Uani 0.25 1 d P . .
O1 O 0.6956(5) 0.4324(6) 0.3691(6) 0.0258(12) Uani 1 1 d U . .
O2 O 0.9286(5) 0.4206(5) 0.5149(6) 0.0226(11) Uani 1 1 d . . .
O3 O 0.5572(5) 0.5747(5) 0.1542(6) 0.0240(12) Uani 1 1 d U . .
C1 C 0.7089(14) 0.8043(12) 0.3934(12) 0.073(4) Uani 1 1 d . . .
H1A H 0.6409 0.7399 0.3868 0.088 Uiso 1 1 calc R . .
H1B H 0.7086 0.8718 0.3217 0.088 Uiso 1 1 calc R . .
O4 O 0.9055(6) 0.2933(5) 0.2442(7) 0.0282(13) Uani 1 1 d U . .
N1 N 0.832(2) 0.770(2) 0.463(2) 0.061(5) Uani 0.50 1 d PU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0077(4) 0.0077(4) 0.0115(6) 0.0016(3) 0.0016(3) 0.0003(4)
Al1 0.0077(4) 0.0077(4) 0.0115(6) 0.0016(3) 0.0016(3) 0.0003(4)
Ge2 0.0110(4) 0.0110(4) 0.0147(6) -0.0028(3) -0.0028(3) 0.0006(5)
Al2 0.0110(4) 0.0110(4) 0.0147(6) -0.0028(3) -0.0028(3) 0.0006(5)
Ge3 0.0154(5) 0.0140(5) 0.0216(5) 0.0008(4) -0.0010(4) 0.0006(4)
Al3 0.0154(5) 0.0140(5) 0.0216(5) 0.0008(4) -0.0010(4) 0.0006(4)
O1 0.013(3) 0.037(3) 0.027(3) 0.002(3) -0.003(2) 0.001(2)
O2 0.017(3) 0.024(3) 0.027(3) 0.001(2) -0.008(2) 0.000(2)
O3 0.030(3) 0.013(3) 0.029(3) 0.011(2) 0.007(2) 0.006(2)
C1 0.093(10) 0.065(8) 0.061(7) 0.036(6) 0.043(7) 0.030(7)
O4 0.031(3) 0.016(2) 0.037(3) -0.010(2) 0.009(3) -0.002(2)
N1 0.048(8) 0.070(9) 0.065(9) -0.030(7) 0.020(7) -0.004(7)

_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 O1 1.731(5) 8_665 ?
Ge1 O1 1.731(5) . ?
Ge1 O3 1.732(5) . ?
Ge1 O3 1.732(5) 8_665 ?
Ge2 O4 1.709(5) . ?
Ge2 O4 1.709(5) 8_665 ?
Ge2 O3 1.751(5) 5_645 ?
Ge2 O3 1.751(5) 3_645 ?
Ge3 O2 1.743(5) . ?
Ge3 O4 1.738(5) . ?
Ge3 O2 1.743(5) 4_564 ?
Ge3 O1 1.769(5) . ?
O2 Al3 1.743(5) 3_645 ?
O2 Ge3 1.743(5) 3_645 ?
O3 Al2 1.751(5) 4_564 ?
O3 Ge2 1.751(5) 4_564 ?
C1 N1 1.47(2) . ?
C1 N1 1.52(3) 7_556 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 N1 1.14(3) 7_556 ?
N1 C1 1.52(3) 7_556 ?

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
O1 Ge1 O1 114.9(4) 8_665 . ?
O1 Ge1 O3 108.2(2) 8_665 . ?
O1 Ge1 O3 112.6(3) . . ?
O1 Ge1 O3 112.6(3) 8_665 8_665 ?
O1 Ge1 O3 108.2(2) . 8_665 ?
O3 Ge1 O3 99.3(4) . 8_665 ?
O4 Ge2 O4 116.6(4) . 8_665 ?
O4 Ge2 O3 101.7(3) . 5_645 ?
O4 Ge2 O3 112.3(3) 8_665 5_645 ?
O4 Ge2 O3 112.3(3) . 3_645 ?
O4 Ge2 O3 101.7(3) 8_665 3_645 ?
O3 Ge2 O3 112.5(4) 5_645 3_645 ?
O2 Ge3 O4 111.4(3) . . ?
O2 Ge3 O2 108.2(3) . 4_564 ?
O4 Ge3 O2 112.0(3) . 4_564 ?
O2 Ge3 O1 104.4(2) . . ?
O4 Ge3 O1 109.1(3) . . ?
O2 Ge3 O1 111.6(3) 4_564 . ?
Ge1 O1 Ge3 131.9(3) . . ?
Ge3 O2 Al3 136.6(3) . 3_645 ?
Ge3 O2 Ge3 136.6(3) . 3_645 ?
Al3 O2 Ge3 0.00(8) 3_645 3_645 ?
Ge1 O3 Al2 133.9(3) . 4_564 ?
Ge1 O3 Ge2 133.9(3) . 4_564 ?
Al2 O3 Ge2 0.00(5) 4_564 4_564 ?
N1 C1 N1 45.0(13) . 7_556 ?
N1 C1 H1A 119.1 . . ?
N1 C1 H1A 119.1 7_556 . ?
N1 C1 H1B 119.1 . . ?
N1 C1 H1B 119.1 7_556 . ?
H1A C1 H1B 116.6 . . ?
Ge2 O4 Ge3 135.5(4) . . ?
N1 N1 C1 69.5(19) 7_556 . ?
N1 N1 C1 65.5(16) 7_556 7_556 ?
C1 N1 C1 109.5(14) . 7_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.135
_database_code_depnum_ccdc_archive 'CCDC 977877'
#######################################################################
#
#                 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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H8 Al Ge3 N O8'
_chemical_formula_sum            'C2 H8 Al Ge3 N O8'

_chemical_formula_weight         418.84

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'
Al Al 0.0645 0.0514 '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           Tetragonal
_symmetry_space_group_name_H-M   'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   10.3404(3)
_cell_length_b                   10.3404(3)
_cell_length_c                   9.4021(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1005.31(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7740
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      25.96

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    9.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3867
_exptl_absorpt_correction_T_max  0.4107
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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 Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7403
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         25.50
_reflns_number_total             940
_reflns_number_gt                892
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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)+(0.0326P)²+6.5035P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_number_reflns         940
_refine_ls_number_parameters     77
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0765
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.133
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.007

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 0.36506(8) 0.07082(8) 0.09367(8) 0.0152(2) Uani 0.75 1 d P . .
Al1 Al 0.36506(8) 0.07082(8) 0.09367(8) 0.0152(2) Uani 0.25 1 d P . .
Ge2 Ge 0.43200(7) 0.56800(7) -0.2500 0.0069(2) Uani 0.75 2 d SP . .
Al2 Al 0.43200(7) 0.56800(7) -0.2500 0.0069(2) Uani 0.25 2 d SP . .
Ge3 Ge 0.36732(7) 0.36732(7) 0.0000 0.0099(2) Uani 0.75 2 d SP . .
Al3 Al 0.36732(7) 0.36732(7) 0.0000 0.0099(2) Uani 0.25 2 d SP . .
O1 O 0.4199(5) -0.0712(4) 0.0147(5) 0.0192(10) Uani 1 1 d . . .
O2 O 0.4414(5) 0.4264(4) -0.1533(5) 0.0231(10) Uani 1 1 d . . .
O3 O 0.1969(4) 0.0666(5) 0.1176(5) 0.0216(10) Uani 1 1 d . . .
O4 O 0.4053(5) 0.2058(4) -0.0062(6) 0.0255(11) Uani 1 1 d . . .
C1 C 0.6956(10) 0.2079(11) -0.1448(12) 0.069(4) Uani 1 1 d D . .
H1A H 0.7403 0.2400 -0.0633 0.104 Uiso 1 1 d R . .
H1B H 0.6069 0.1932 -0.1212 0.104 Uiso 1 1 d R . .
H1C H 0.7342 0.1285 -0.1747 0.104 Uiso 1 1 d R . .
N1 N 0.7309(16) 0.3288(13) -0.2164(17) 0.051(4) Uani 0.50 1 d PDU . .
H1D H 0.7860 0.3728 -0.1612 0.061 Uiso 0.50 1 d PR . .
H1E H 0.6597 0.3772 -0.2269 0.061 Uiso 0.50 1 d PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0155(4) 0.0134(4) 0.0166(4) -0.0005(3) -0.0012(3) -0.0001(4)
Al1 0.0155(4) 0.0134(4) 0.0166(4) -0.0005(3) -0.0012(3) -0.0001(4)
Ge2 0.0064(3) 0.0064(3) 0.0079(5) 0.0019(3) 0.0019(3) -0.0003(4)
Al2 0.0064(3) 0.0064(3) 0.0079(5) 0.0019(3) 0.0019(3) -0.0003(4)
Ge3 0.0096(3) 0.0096(3) 0.0103(5) 0.0034(3) -0.0034(3) -0.0011(4)
Al3 0.0096(3) 0.0096(3) 0.0103(5) 0.0034(3) -0.0034(3) -0.0011(4)
O1 0.025(2) 0.020(2) 0.012(2) -0.0081(19) 0.0036(19) 0.004(2)
O2 0.034(3) 0.012(2) 0.023(2) 0.005(2) 0.009(2) 0.003(2)
O3 0.013(2) 0.031(3) 0.021(2) 0.004(2) -0.0042(19) -0.001(2)
O4 0.029(3) 0.016(2) 0.031(3) 0.008(2) 0.008(2) 0.0043(19)
C1 0.054(6) 0.086(9) 0.067(7) -0.051(7) 0.029(6) -0.032(6)
N1 0.048(7) 0.042(7) 0.063(8) -0.026(6) -0.034(6) 0.010(6)

_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 O4 1.733(5) . ?
Ge1 O1 1.741(4) 4 ?
Ge1 O1 1.740(4) . ?
Ge1 O3 1.754(4) . ?
Ge2 O2 1.727(5) . ?
Ge2 O2 1.727(5) 8_664 ?
Ge2 O3 1.731(4) 5_554 ?
Ge2 O3 1.731(4) 3_554 ?
Ge3 O4 1.717(5) 7 ?
Ge3 O4 1.717(5) . ?
Ge3 O2 1.743(4) 7 ?
Ge3 O2 1.743(4) . ?
O1 Al1 1.741(4) 3_544 ?
O1 Ge1 1.741(4) 3_544 ?
O3 Al2 1.731(4) 4_455 ?
O3 Ge2 1.731(4) 4_455 ?
C1 N1 1.466(15) . ?
C1 N1 1.47(2) 8_664 ?
N1 N1 1.08(3) 8_664 ?
N1 C1 1.47(2) 8_664 ?

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
O4 Ge1 O1 111.4(2) . 4 ?
O4 Ge1 O1 111.7(2) . . ?
O1 Ge1 O1 108.5(3) 4 . ?
O4 Ge1 O3 109.1(2) . . ?
O1 Ge1 O3 105.0(2) 4 . ?
O1 Ge1 O3 110.9(2) . . ?
O2 Ge2 O2 100.5(3) . 8_664 ?
O2 Ge2 O3 111.9(2) . 5_554 ?
O2 Ge2 O3 108.4(2) 8_664 5_554 ?
O2 Ge2 O3 108.4(2) . 3_554 ?
O2 Ge2 O3 111.9(3) 8_664 3_554 ?
O3 Ge2 O3 114.9(3) 5_554 3_554 ?
O4 Ge3 O4 116.5(3) 7 . ?
O4 Ge3 O2 102.2(2) 7 7 ?
O4 Ge3 O2 112.1(2) . 7 ?
O4 Ge3 O2 112.1(2) 7 . ?
O4 Ge3 O2 102.2(2) . . ?
O2 Ge3 O2 112.1(3) 7 . ?
Al1 O1 Ge1 0.00(5) 3_544 3_544 ?
Al1 O1 Ge1 137.0(3) 3_544 . ?
Ge1 O1 Ge1 137.0(3) 3_544 . ?
Ge2 O2 Ge3 135.1(3) . . ?
Al2 O3 Ge2 0.00(3) 4_455 4_455 ?
Al2 O3 Ge1 132.9(3) 4_455 . ?
Ge2 O3 Ge1 132.9(3) 4_455 . ?
Ge3 O4 Ge1 135.2(3) . . ?
N1 C1 N1 43.0(11) . 8_664 ?
N1 N1 C1 68.8(15) 8_664 . ?
N1 N1 C1 68.2(14) 8_664 8_664 ?
C1 N1 C1 111.6(12) . 8_664 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.131
_database_code_depnum_ccdc_archive 'CCDC 977878'
#######################################################################
#
#                 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_zhp9b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H29 Al3 Ge3 N7 Ni O12'
_chemical_formula_weight         760.79

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'
Al Al 0.0645 0.0514 '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           Cubic
_symmetry_space_group_name_H-M   'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'

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

_cell_length_a                   16.4699(7)
_cell_length_b                   16.4699(7)
_cell_length_c                   16.4699(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4467.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9999
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      25.66


_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3032
_exptl_absorpt_coefficient_mu    5.018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'

_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 Apex2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22677
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.94
_reflns_number_total             1466
_reflns_number_gt                1216
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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)+(0.0679P)²+12.7126P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1466
_refine_ls_number_parameters     115
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1243
_refine_ls_wR_factor_gt          0.1193
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.07764(3) 0.84110(3) 0.06607(3) 0.01567(12) Uani 0.50 1 d P . .
Al1 Al 0.07764(3) 0.84110(3) 0.06607(3) 0.01567(12) Uani 0.50 1 d P . .
Ge2 Ge 0.13863(3) 0.74352(3) -0.08924(3) 0.01608(12) Uani 0.50 1 d P . .
Al2 Al 0.13863(3) 0.74352(3) -0.08924(3) 0.01608(12) Uani 0.50 1 d P . .
Ni1 Ni 0.33410(3) 0.66590(3) 0.16590(3) 0.03110(19) Uani 1 3 d S A .
O1 O 0.08551(16) 0.75740(16) 0.00135(16) 0.0355(7) Uani 1 1 d . . .
O2 O 0.11662(17) 0.81892(17) 0.16238(15) 0.0346(7) Uani 1 1 d . . .
O3 O -0.02420(16) 0.86735(18) 0.07860(15) 0.0343(7) Uani 1 1 d . . .
O4 O 0.21199(18) 0.66782(16) -0.07544(17) 0.0363(7) Uani 1 1 d . . .
N2 N 0.3381(3) 0.6630(3) 0.2952(2) 0.0661(15) Uani 1 1 d . . .
N1 N 0.4594(2) 0.6525(2) 0.1812(2) 0.0434(10) Uani 1 1 d . . .
H1A H 0.4771 0.6111 0.1502 0.052 Uiso 1 1 calc R A .
H1B H 0.4846 0.6980 0.1644 0.052 Uiso 1 1 calc R . .
C1 C 0.4805(3) 0.6369(5) 0.2656(3) 0.079(2) Uani 1 1 d . A .
C2 C 0.4298(6) 0.6796(6) 0.3162(6) 0.049(3) Uani 0.50 1 d P A 1
H2A H 0.4409 0.7372 0.3110 0.059 Uiso 0.50 1 calc PR A 1
H2B H 0.4402 0.6640 0.3721 0.059 Uiso 0.50 1 calc PR A 1
C2A C 0.4108(8) 0.6353(10) 0.3208(7) 0.080(5) Uani 0.50 1 d P A 2
H2AA H 0.4033 0.5795 0.3381 0.096 Uiso 0.50 1 calc PR A 2
H2AB H 0.4256 0.6662 0.3687 0.096 Uiso 0.50 1 calc PR A 2
C3 C 0.4689(8) 0.4689(8) 0.4689(8) 0.190(10) Uani 1 3 d S . .
N3 N 0.5362(17) 0.4605(18) 0.4051(16) 0.158(6) Uani 0.33 1 d PU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0170(2) 0.0162(2) 0.0138(2) -0.00149(18) 0.00161(19) 0.00003(19)
Al1 0.0170(2) 0.0162(2) 0.0138(2) -0.00149(18) 0.00161(19) 0.00003(19)
Ge2 0.0174(2) 0.0153(2) 0.0156(2) -0.00227(19) -0.00012(18) 0.00169(19)
Al2 0.0174(2) 0.0153(2) 0.0156(2) -0.00227(19) -0.00012(18) 0.00169(19)
Ni1 0.03110(19) 0.03110(19) 0.03110(19) -0.0022(2) 0.0022(2) 0.0022(2)
O1 0.0415(15) 0.0295(13) 0.0356(14) -0.0072(12) 0.0130(12) -0.0035(12)
O2 0.0346(14) 0.0411(15) 0.0281(13) -0.0009(12) -0.0011(11) 0.0073(13)
O3 0.0279(13) 0.0482(16) 0.0267(13) -0.0066(12) 0.0011(11) 0.0051(13)
O4 0.0407(15) 0.0357(14) 0.0324(14) -0.0086(12) -0.0097(12) 0.0135(12)
N2 0.054(3) 0.112(4) 0.031(2) -0.005(2) 0.0084(19) -0.004(3)
N1 0.0318(18) 0.046(2) 0.052(2) 0.0044(18) 0.0018(17) -0.0024(16)
C1 0.048(3) 0.141(6) 0.049(3) 0.028(3) -0.012(3) -0.009(3)
C2 0.064(6) 0.042(5) 0.042(5) -0.007(4) -0.013(5) -0.011(5)
C2A 0.076(8) 0.131(13) 0.032(5) -0.003(7) -0.012(6) 0.021(9)
C3 0.190(10) 0.190(10) 0.190(10) 0.005(10) 0.005(10) 0.005(10)
N3 0.158(9) 0.168(9) 0.148(9) -0.005(7) 0.011(7) 0.000(7)

_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 O3 1.744(3) . ?
Ge1 O3 1.745(3) 21_665 ?
Ge1 O1 1.747(3) . ?
Ge1 O2 1.750(3) . ?
Ge2 O4 1.740(3) 8 ?
Ge2 O1 1.745(3) . ?
Ge2 O4 1.751(3) . ?
Ge2 O2 1.759(3) 21_665 ?
Ni1 N1 2.091(4) . ?
Ni1 N1 2.091(3) 7_564 ?
Ni1 N1 2.091(3) 10_655 ?
Ni1 N2 2.132(4) 7_564 ?
Ni1 N2 2.132(4) . ?
Ni1 N2 2.132(4) 10_655 ?
O2 Al2 1.759(3) 17_566 ?
O2 Ge2 1.759(3) 17_566 ?
O3 Al1 1.745(3) 17_566 ?
O3 Ge1 1.745(3) 17_566 ?
O4 Al2 1.740(3) 11_455 ?
O4 Ge2 1.740(3) 11_455 ?
N2 C2A 1.349(14) . ?
N2 C2 1.573(11) . ?
N1 C1 1.455(7) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
C1 C2 1.375(12) . ?
C1 C2A 1.464(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C3 N3 1.53(3) 9 ?
C3 N3 1.53(3) . ?
C3 N3 1.53(3) 5 ?
C3 C3 1.78(4) 13_666 ?

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
O3 Ge1 O3 110.99(19) . 21_665 ?
O3 Ge1 O1 109.81(13) . . ?
O3 Ge1 O1 108.57(13) 21_665 . ?
O3 Ge1 O2 107.29(13) . . ?
O3 Ge1 O2 109.02(14) 21_665 . ?
O1 Ge1 O2 111.17(13) . . ?
O4 Ge2 O1 112.04(13) 8 . ?
O4 Ge2 O4 107.26(17) 8 . ?
O1 Ge2 O4 109.17(13) . . ?
O4 Ge2 O2 108.06(14) 8 21_665 ?
O1 Ge2 O2 107.65(13) . 21_665 ?
O4 Ge2 O2 112.73(14) . 21_665 ?
N1 Ni1 N1 91.56(15) . 7_564 ?
N1 Ni1 N1 91.56(15) . 10_655 ?
N1 Ni1 N1 91.56(15) 7_564 10_655 ?
N1 Ni1 N2 170.32(17) . 7_564 ?
N1 Ni1 N2 81.17(16) 7_564 7_564 ?
N1 Ni1 N2 95.00(18) 10_655 7_564 ?
N1 Ni1 N2 81.17(16) . . ?
N1 Ni1 N2 95.00(18) 7_564 . ?
N1 Ni1 N2 170.32(17) 10_655 . ?
N2 Ni1 N2 93.03(19) 7_564 . ?
N1 Ni1 N2 95.00(18) . 10_655 ?
N1 Ni1 N2 170.32(17) 7_564 10_655 ?
N1 Ni1 N2 81.17(16) 10_655 10_655 ?
N2 Ni1 N2 93.03(19) 7_564 10_655 ?
N2 Ni1 N2 93.03(19) . 10_655 ?
Ge2 O1 Ge1 131.47(16) . . ?
Ge1 O2 Al2 128.44(16) . 17_566 ?
Ge1 O2 Ge2 128.44(16) . 17_566 ?
Al2 O2 Ge2 0.00(3) 17_566 17_566 ?
Ge1 O3 Al1 126.74(16) . 17_566 ?
Ge1 O3 Ge1 126.74(16) . 17_566 ?
Al1 O3 Ge1 0.00(3) 17_566 17_566 ?
Al2 O4 Ge2 0.00(3) 11_455 11_455 ?
Al2 O4 Ge2 131.14(17) 11_455 . ?
Ge2 O4 Ge2 131.14(17) 11_455 . ?
C2A N2 C2 30.5(8) . . ?
C2A N2 Ni1 110.3(6) . . ?
C2 N2 Ni1 104.2(4) . . ?
C1 N1 Ni1 111.7(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 . . ?
C2 C1 N1 110.1(6) . . ?
C2 C1 C2A 32.4(7) . . ?
N1 C1 C2A 114.1(6) . . ?
C1 C2 N2 111.1(7) . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
N2 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C2A C1 119.7(9) . . ?
N2 C2A H2AA 107.4 . . ?
C1 C2A H2AA 107.4 . . ?
N2 C2A H2AB 107.4 . . ?
C1 C2A H2AB 107.4 . . ?
H2AA C2A H2AB 106.9 . . ?
N3 C3 N3 119.91(14) 9 . ?
N3 C3 N3 119.91(15) 9 5 ?
N3 C3 N3 119.91(14) . 5 ?
N3 C3 C3 91.7(14) 9 13_666 ?
N3 C3 C3 91.7(14) . 13_666 ?
N3 C3 C3 91.7(14) 5 13_666 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.94
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.721
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.121
_database_code_depnum_ccdc_archive 'CCDC 977879'
