# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_193xzek17
_database_code_depnum_ccdc_archive 'CCDC 1952091'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H24 Br Ge N3'
_chemical_formula_sum            'C13 H24 Br Ge N3'
_chemical_formula_weight         374.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.3994(15)
_cell_length_b                   10.027(2)
_cell_length_c                   21.820(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.18(3)
_cell_angle_gamma                90
_cell_volume                     1618.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8142
_cell_measurement_theta_min      4.0120
_cell_measurement_theta_max      76.2560

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    5.361
_shelx_estimated_absorpt_T_min   0.590
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_reflns_number            17119
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.053
_diffrn_reflns_theta_max         76.174
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3374
_reflns_number_gt                3274
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0991P)²+46.2831P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3374
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0977
_refine_ls_wR_factor_ref         0.2661
_refine_ls_wR_factor_gt          0.2646
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.8588(2) 0.10196(14) 0.63811(6) 0.0413(4) Uani 1 1 d . . . . .
Ge1 Ge 0.78706(18) 0.33694(14) 0.59244(6) 0.0295(4) Uani 1 1 d . . . . .
N1 N 0.6416(13) 0.2835(9) 0.5260(4) 0.0289(19) Uani 1 1 d . . . . .
N2 N 0.3909(12) 0.3404(9) 0.6262(4) 0.0286(19) Uani 1 1 d . . . . .
N3 N 0.5431(12) 0.4298(10) 0.7015(4) 0.0280(19) Uani 1 1 d . . . . .
C1 C 0.7218(17) 0.2597(12) 0.4648(5) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.888(2) 0.3481(16) 0.4584(6) 0.047(3) Uani 1 1 d . . . . .
H2A H 0.855403 0.441164 0.466255 0.070 Uiso 1 1 calc R U . . .
H2B H 0.934383 0.340061 0.416771 0.070 Uiso 1 1 calc R U . . .
H2C H 0.981915 0.319974 0.488056 0.070 Uiso 1 1 calc R U . . .
C3 C 0.779(2) 0.1165(13) 0.4571(7) 0.045(3) Uani 1 1 d . . . . .
H3A H 0.843596 0.086650 0.494228 0.067 Uiso 1 1 calc R U . . .
H3B H 0.857985 0.109032 0.421873 0.067 Uiso 1 1 calc R U . . .
H3C H 0.671339 0.060767 0.450285 0.067 Uiso 1 1 calc R U . . .
C4 C 0.587(2) 0.2998(15) 0.4151(6) 0.047(3) Uani 1 1 d . . . . .
H4A H 0.481933 0.240324 0.416101 0.071 Uiso 1 1 calc R U . . .
H4B H 0.643650 0.293148 0.374994 0.071 Uiso 1 1 calc R U . . .
H4C H 0.547863 0.391877 0.421929 0.071 Uiso 1 1 calc R U . . .
C5 C 0.4837(17) 0.2025(14) 0.5396(6) 0.039(3) Uani 1 1 d . . . . .
H5A H 0.521383 0.128791 0.567255 0.047 Uiso 1 1 calc R U . . .
H5B H 0.436711 0.162266 0.501034 0.047 Uiso 1 1 calc R U . . .
C6 C 0.3377(15) 0.2773(13) 0.5683(6) 0.034(3) Uani 1 1 d . . . . .
H6A H 0.294330 0.347044 0.539466 0.041 Uiso 1 1 calc R U . . .
H6B H 0.235631 0.215923 0.575667 0.041 Uiso 1 1 calc R U . . .
C7 C 0.5609(14) 0.3655(11) 0.6449(5) 0.025(2) Uani 1 1 d . . . . .
C8 C 0.2638(16) 0.3884(12) 0.6666(6) 0.036(3) Uani 1 1 d . . . . .
H8 H 0.135838 0.383969 0.662507 0.043 Uiso 1 1 calc R U . . .
C9 C 0.3645(17) 0.4439(12) 0.7138(5) 0.034(2) Uani 1 1 d . . . . .
H9 H 0.317106 0.485275 0.749247 0.041 Uiso 1 1 calc R U . . .
C10 C 0.6982(17) 0.4825(12) 0.7404(5) 0.033(2) Uani 1 1 d . . . . .
C11 C 0.6196(18) 0.5389(15) 0.7982(6) 0.040(3) Uani 1 1 d . . . . .
H11A H 0.522849 0.601911 0.787438 0.061 Uiso 1 1 calc R U . . .
H11B H 0.714531 0.585084 0.821878 0.061 Uiso 1 1 calc R U . . .
H11C H 0.570358 0.466176 0.822822 0.061 Uiso 1 1 calc R U . . .
C12 C 0.8265(17) 0.3674(13) 0.7562(6) 0.036(3) Uani 1 1 d . . . . .
H12A H 0.765959 0.304373 0.783288 0.054 Uiso 1 1 calc R U . . .
H12B H 0.935117 0.402522 0.777012 0.054 Uiso 1 1 calc R U . . .
H12C H 0.860719 0.321698 0.718498 0.054 Uiso 1 1 calc R U . . .
C13 C 0.793(2) 0.5950(14) 0.7061(6) 0.042(3) Uani 1 1 d . . . . .
H13A H 0.853182 0.558280 0.670266 0.063 Uiso 1 1 calc R U . . .
H13B H 0.883024 0.637111 0.733439 0.063 Uiso 1 1 calc R U . . .
H13C H 0.703603 0.661549 0.692785 0.063 Uiso 1 1 calc R U . . .


_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
Br1 Ge1 2.6088(19) . ?
Ge1 N1 1.866(9) . ?
Ge1 C7 2.067(10) . ?
N1 C5 1.459(15) . ?
N1 C1 1.493(14) . ?
N2 C7 1.338(14) . ?
N2 C8 1.388(15) . ?
N2 C6 1.460(14) . ?
N3 C9 1.362(16) . ?
N3 C7 1.401(14) . ?
N3 C10 1.509(14) . ?
C1 C3 1.506(18) . ?
C1 C4 1.513(18) . ?
C1 C2 1.527(18) . ?
C5 C6 1.466(18) . ?
C8 C9 1.377(18) . ?
C10 C11 1.510(17) . ?
C10 C12 1.529(17) . ?
C10 C13 1.532(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C7 90.5(4) . . ?
N1 Ge1 Br1 98.5(3) . . ?
C7 Ge1 Br1 94.2(3) . . ?
C5 N1 C1 115.3(9) . . ?
C5 N1 Ge1 117.0(7) . . ?
C1 N1 Ge1 120.5(8) . . ?
C7 N2 C8 112.7(10) . . ?
C7 N2 C6 125.5(9) . . ?
C8 N2 C6 121.7(10) . . ?
C9 N3 C7 109.4(9) . . ?
C9 N3 C10 125.6(10) . . ?
C7 N3 C10 124.9(9) . . ?
N1 C1 C3 111.6(10) . . ?
N1 C1 C4 109.3(11) . . ?
C3 C1 C4 110.8(11) . . ?
N1 C1 C2 109.0(10) . . ?
C3 C1 C2 108.4(12) . . ?
C4 C1 C2 107.6(11) . . ?
N1 C5 C6 113.7(11) . . ?
N2 C6 C5 113.8(10) . . ?
N2 C7 N3 104.5(9) . . ?
N2 C7 Ge1 124.8(8) . . ?
N3 C7 Ge1 130.1(8) . . ?
C9 C8 N2 104.6(10) . . ?
N3 C9 C8 108.8(10) . . ?
N3 C10 C11 107.5(10) . . ?
N3 C10 C12 108.9(9) . . ?
C11 C10 C12 110.0(10) . . ?
N3 C10 C13 109.5(10) . . ?
C11 C10 C13 108.7(11) . . ?
C12 C10 C13 112.2(11) . . ?

_refine_diff_density_max         2.553
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.211


_vrf_PLAT341_193xzek17           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.02 Ang.  
RESPONSE: The crystal was extremely small and weakly diffracting.  Furthermore
the crystal was twinned which have affected quality of the data. This 
is reflected in the high wR2 factor and in the low precision of C-C bonds. 
However, the thermal parameters are reasonable and actual molecule is well 
behaved.
;

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_307xzjh19_a
_database_code_depnum_ccdc_archive 'CCDC 2005217'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;Australian National University
United Kingdom
;
_audit_update_record             
;
2020-05-22 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H33 Cl Ge N P'
_chemical_formula_sum            'C31 H33 Cl Ge N P'
_chemical_formula_weight         558.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1837(3)
_cell_length_b                   11.0396(4)
_cell_length_c                   14.5439(5)
_cell_angle_alpha                111.357(3)
_cell_angle_beta                 92.618(3)
_cell_angle_gamma                90.475(3)
_cell_volume                     1371.34(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7455
_cell_measurement_theta_min      3.2610
_cell_measurement_theta_max      76.4670

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             580
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.105
_shelx_estimated_absorpt_T_min   0.812
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_reflns_number            11314
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.267
_diffrn_reflns_theta_max         76.460
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5691
_reflns_number_gt                5273
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0330P)²+0.5624P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5691
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0672
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.62067(2) 0.55600(2) 0.66662(2) 0.02152(6) Uani 1 1 d . . . . .
Cl1 Cl 0.87024(4) 0.55041(4) 0.64225(3) 0.03296(9) Uani 1 1 d . . . . .
P1 P 0.59972(4) 0.31741(3) 0.58442(2) 0.01803(8) Uani 1 1 d . . . . .
N1 N 0.62450(13) 0.52097(12) 0.78454(8) 0.0192(2) Uani 1 1 d . . . . .
C1 C 0.56501(16) 0.62551(14) 0.86500(10) 0.0206(3) Uani 1 1 d . . . . .
C2 C 0.41913(16) 0.61285(15) 0.88862(11) 0.0230(3) Uani 1 1 d . . . . .
C3 C 0.36121(18) 0.71478(17) 0.96531(12) 0.0299(3) Uani 1 1 d . . . . .
H3 H 0.263601 0.707282 0.981992 0.036 Uiso 1 1 calc R U . . .
C4 C 0.44301(19) 0.82686(17) 1.01777(12) 0.0333(4) Uani 1 1 d . . . . .
H4 H 0.401515 0.895164 1.069839 0.040 Uiso 1 1 calc R U . . .
C5 C 0.58458(19) 0.83893(16) 0.99419(12) 0.0309(3) Uani 1 1 d . . . . .
H5 H 0.639797 0.916181 1.030294 0.037 Uiso 1 1 calc R U . . .
C6 C 0.64862(17) 0.73989(14) 0.91826(11) 0.0242(3) Uani 1 1 d . . . . .
C7 C 0.80586(17) 0.75923(15) 0.89688(12) 0.0274(3) Uani 1 1 d . . . . .
H7 H 0.834148 0.678969 0.841806 0.033 Uiso 1 1 calc R U . . .
C8 C 0.8243(2) 0.8743(2) 0.8632(2) 0.0489(5) Uani 1 1 d . . . . .
H8A H 0.757989 0.862057 0.805585 0.073 Uiso 1 1 calc R U . . .
H8B H 0.925124 0.879494 0.845402 0.073 Uiso 1 1 calc R U . . .
H8C H 0.801430 0.954950 0.917020 0.073 Uiso 1 1 calc R U . . .
C9 C 0.9081(2) 0.7757(2) 0.98726(15) 0.0442(5) Uani 1 1 d . . . . .
H9A H 0.881860 0.853251 1.042777 0.066 Uiso 1 1 calc R U . . .
H9B H 1.009021 0.785578 0.971351 0.066 Uiso 1 1 calc R U . . .
H9C H 0.898785 0.698887 1.005404 0.066 Uiso 1 1 calc R U . . .
C10 C 0.32818(16) 0.48958(16) 0.83401(11) 0.0262(3) Uani 1 1 d . . . . .
H10 H 0.351635 0.459233 0.762809 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3721(2) 0.38187(19) 0.87285(14) 0.0417(4) Uani 1 1 d . . . . .
H11A H 0.359169 0.412076 0.944134 0.063 Uiso 1 1 calc R U . . .
H11B H 0.474554 0.361121 0.860081 0.063 Uiso 1 1 calc R U . . .
H11C H 0.310611 0.303882 0.839035 0.063 Uiso 1 1 calc R U . . .
C12 C 0.1643(2) 0.5083(2) 0.83891(17) 0.0493(5) Uani 1 1 d . . . . .
H12A H 0.136470 0.530250 0.907231 0.074 Uiso 1 1 calc R U . . .
H12B H 0.113180 0.427689 0.796403 0.074 Uiso 1 1 calc R U . . .
H12C H 0.137796 0.578989 0.816237 0.074 Uiso 1 1 calc R U . . .
C13 C 0.73576(17) 0.44802(15) 0.81549(11) 0.0255(3) Uani 1 1 d . . . . .
H13A H 0.713754 0.451643 0.882435 0.031 Uiso 1 1 calc R U . . .
H13B H 0.830373 0.494739 0.821824 0.031 Uiso 1 1 calc R U . . .
C14 C 0.75657(15) 0.30643(14) 0.75195(10) 0.0194(3) Uani 1 1 d . . . . .
C15 C 0.84343(16) 0.23857(15) 0.79797(11) 0.0246(3) Uani 1 1 d . . . . .
H15 H 0.881684 0.283053 0.863674 0.029 Uiso 1 1 calc R U . . .
C16 C 0.87502(18) 0.10893(16) 0.75056(13) 0.0293(3) Uani 1 1 d . . . . .
H16 H 0.933858 0.065657 0.783800 0.035 Uiso 1 1 calc R U . . .
C17 C 0.82067(18) 0.04202(15) 0.65431(13) 0.0299(3) Uani 1 1 d . . . . .
H17 H 0.840490 -0.047413 0.621725 0.036 Uiso 1 1 calc R U . . .
C18 C 0.73743(16) 0.10728(14) 0.60666(12) 0.0249(3) Uani 1 1 d . . . . .
H18 H 0.701581 0.062256 0.540444 0.030 Uiso 1 1 calc R U . . .
C19 C 0.70470(14) 0.23902(14) 0.65419(10) 0.0191(3) Uani 1 1 d . . . . .
C20 C 0.64295(16) 0.24128(14) 0.45532(10) 0.0222(3) Uani 1 1 d . . . . .
C21 C 0.7688(2) 0.2819(2) 0.42380(13) 0.0426(5) Uani 1 1 d . . . . .
H21 H 0.833583 0.344374 0.470215 0.051 Uiso 1 1 calc R U . . .
C22 C 0.7998(3) 0.2313(3) 0.32457(16) 0.0635(8) Uani 1 1 d . . . . .
H22 H 0.885819 0.259358 0.303382 0.076 Uiso 1 1 calc R U . . .
C23 C 0.7066(3) 0.1406(2) 0.25662(14) 0.0517(6) Uani 1 1 d . . . . .
H23 H 0.728401 0.106117 0.188852 0.062 Uiso 1 1 calc R U . . .
C24 C 0.5814(2) 0.09991(18) 0.28732(12) 0.0361(4) Uani 1 1 d . . . . .
H24 H 0.517115 0.037380 0.240543 0.043 Uiso 1 1 calc R U . . .
C25 C 0.54920(17) 0.14996(15) 0.38612(11) 0.0268(3) Uani 1 1 d . . . . .
H25 H 0.462717 0.121819 0.406717 0.032 Uiso 1 1 calc R U . . .
C26 C 0.41026(15) 0.27437(14) 0.58764(10) 0.0212(3) Uani 1 1 d . . . . .
C27 C 0.30631(17) 0.34026(17) 0.55212(12) 0.0279(3) Uani 1 1 d . . . . .
H27 H 0.336693 0.403113 0.525981 0.034 Uiso 1 1 calc R U . . .
C28 C 0.15916(18) 0.31446(19) 0.55480(13) 0.0346(4) Uani 1 1 d . . . . .
H28 H 0.088751 0.359476 0.530488 0.042 Uiso 1 1 calc R U . . .
C29 C 0.11451(18) 0.22266(19) 0.59309(14) 0.0363(4) Uani 1 1 d . . . . .
H29 H 0.013478 0.205161 0.595045 0.044 Uiso 1 1 calc R U . . .
C30 C 0.21681(18) 0.15651(17) 0.62843(13) 0.0330(3) Uani 1 1 d . . . . .
H30 H 0.185736 0.093494 0.654212 0.040 Uiso 1 1 calc R U . . .
C31 C 0.36523(17) 0.18227(15) 0.62623(12) 0.0260(3) Uani 1 1 d . . . . .
H31 H 0.435375 0.137377 0.650860 0.031 Uiso 1 1 calc R U . . .


_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 N1 1.8894(12) . ?
Ge1 Cl1 2.3330(4) . ?
Ge1 P1 2.4659(4) . ?
P1 C26 1.8071(14) . ?
P1 C19 1.8089(14) . ?
P1 C20 1.8203(15) . ?
N1 C1 1.4440(17) . ?
N1 C13 1.4598(17) . ?
C1 C6 1.415(2) . ?
C1 C2 1.416(2) . ?
C2 C3 1.394(2) . ?
C2 C10 1.521(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.377(2) . ?
C5 C6 1.397(2) . ?
C6 C7 1.520(2) . ?
C7 C8 1.529(2) . ?
C7 C9 1.534(2) . ?
C10 C12 1.522(2) . ?
C10 C11 1.540(2) . ?
C13 C14 1.5175(19) . ?
C14 C19 1.4014(19) . ?
C14 C15 1.404(2) . ?
C15 C16 1.384(2) . ?
C16 C17 1.390(2) . ?
C17 C18 1.381(2) . ?
C18 C19 1.406(2) . ?
C20 C21 1.392(2) . ?
C20 C25 1.392(2) . ?
C21 C22 1.389(3) . ?
C22 C23 1.378(3) . ?
C23 C24 1.381(3) . ?
C24 C25 1.386(2) . ?
C26 C27 1.396(2) . ?
C26 C31 1.396(2) . ?
C27 C28 1.384(2) . ?
C28 C29 1.389(3) . ?
C29 C30 1.386(3) . ?
C30 C31 1.394(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 Cl1 98.96(4) . . ?
N1 Ge1 P1 84.39(4) . . ?
Cl1 Ge1 P1 90.494(14) . . ?
C26 P1 C19 107.05(7) . . ?
C26 P1 C20 104.98(7) . . ?
C19 P1 C20 107.73(7) . . ?
C26 P1 Ge1 106.09(5) . . ?
C19 P1 Ge1 110.45(5) . . ?
C20 P1 Ge1 119.75(5) . . ?
C1 N1 C13 114.19(11) . . ?
C1 N1 Ge1 112.05(9) . . ?
C13 N1 Ge1 125.68(10) . . ?
C6 C1 C2 120.18(13) . . ?
C6 C1 N1 121.17(13) . . ?
C2 C1 N1 118.64(13) . . ?
C3 C2 C1 118.53(14) . . ?
C3 C2 C10 120.29(14) . . ?
C1 C2 C10 121.16(13) . . ?
C4 C3 C2 121.41(15) . . ?
C5 C4 C3 119.83(15) . . ?
C4 C5 C6 121.34(15) . . ?
C5 C6 C1 118.71(14) . . ?
C5 C6 C7 118.53(14) . . ?
C1 C6 C7 122.75(13) . . ?
C6 C7 C8 111.93(14) . . ?
C6 C7 C9 110.78(14) . . ?
C8 C7 C9 110.69(16) . . ?
C2 C10 C12 114.14(14) . . ?
C2 C10 C11 109.99(13) . . ?
C12 C10 C11 110.02(16) . . ?
N1 C13 C14 119.09(12) . . ?
C19 C14 C15 117.62(13) . . ?
C19 C14 C13 128.15(13) . . ?
C15 C14 C13 114.19(13) . . ?
C16 C15 C14 122.03(14) . . ?
C15 C16 C17 119.99(14) . . ?
C18 C17 C16 119.11(15) . . ?
C17 C18 C19 121.32(14) . . ?
C14 C19 C18 119.89(13) . . ?
C14 C19 P1 122.02(11) . . ?
C18 C19 P1 118.07(11) . . ?
C21 C20 C25 119.08(14) . . ?
C21 C20 P1 118.87(12) . . ?
C25 C20 P1 121.91(11) . . ?
C22 C21 C20 120.09(17) . . ?
C23 C22 C21 120.42(18) . . ?
C22 C23 C24 119.82(17) . . ?
C23 C24 C25 120.26(16) . . ?
C24 C25 C20 120.33(15) . . ?
C27 C26 C31 119.70(14) . . ?
C27 C26 P1 117.31(11) . . ?
C31 C26 P1 122.96(11) . . ?
C28 C27 C26 120.31(15) . . ?
C27 C28 C29 119.93(16) . . ?
C30 C29 C28 120.25(15) . . ?
C29 C30 C31 120.13(16) . . ?
C30 C31 C26 119.68(15) . . ?

_refine_diff_density_max         0.503
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.048



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_274xzjh18_a
_database_code_depnum_ccdc_archive 'CCDC 1952092'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H26 Br Ge N3'
_chemical_formula_sum            'C18 H26 Br Ge N3'
_chemical_formula_weight         436.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.8454(3)
_cell_length_b                   13.2083(3)
_cell_length_c                   21.4808(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3928.28(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3404
_cell_measurement_theta_min      4.0570
_cell_measurement_theta_max      75.8220

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.510
_shelx_estimated_absorpt_T_min   0.614
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_reflns_number            13468
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.116
_diffrn_reflns_theta_max         76.211
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4070
_reflns_number_gt                3229
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0347P)²+4.0183P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4070
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0983
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.62393(3) 0.28395(3) 0.47438(2) 0.03342(12) Uani 1 1 d . . . . .
Ge1 Ge 0.60069(3) 0.34548(3) 0.35980(2) 0.02431(11) Uani 1 1 d . . . . .
N1 N 0.4645(2) 0.3559(2) 0.35889(16) 0.0255(6) Uani 1 1 d . . . . .
N2 N 0.5381(2) 0.5589(2) 0.39804(15) 0.0261(7) Uani 1 1 d . . . . .
N3 N 0.6926(2) 0.5493(2) 0.39310(14) 0.0222(6) Uani 1 1 d . . . . .
C1 C 0.4067(3) 0.2640(3) 0.3421(2) 0.0321(9) Uani 1 1 d . . . . .
C2 C 0.4642(3) 0.2018(3) 0.2947(3) 0.0490(13) Uani 1 1 d . . . . .
H2A H 0.481591 0.244872 0.259281 0.073 Uiso 1 1 calc R U . . .
H2B H 0.424757 0.144978 0.280150 0.073 Uiso 1 1 calc R U . . .
H2C H 0.523080 0.175908 0.314390 0.073 Uiso 1 1 calc R U . . .
C3 C 0.3123(3) 0.2960(3) 0.3110(2) 0.0412(10) Uani 1 1 d . . . . .
H3A H 0.277077 0.342056 0.338638 0.062 Uiso 1 1 calc R U . . .
H3B H 0.272743 0.235979 0.302747 0.062 Uiso 1 1 calc R U . . .
H3C H 0.326583 0.330551 0.271690 0.062 Uiso 1 1 calc R U . . .
C4 C 0.3849(4) 0.1994(4) 0.3987(3) 0.0622(16) Uani 1 1 d . . . . .
H4A H 0.445580 0.176564 0.417464 0.093 Uiso 1 1 calc R U . . .
H4B H 0.346554 0.140539 0.386067 0.093 Uiso 1 1 calc R U . . .
H4C H 0.348454 0.239496 0.429037 0.093 Uiso 1 1 calc R U . . .
C5 C 0.4200(3) 0.4200(3) 0.4061(2) 0.0322(9) Uani 1 1 d . . . . .
H5A H 0.447322 0.402432 0.447361 0.039 Uiso 1 1 calc R U . . .
H5B H 0.349825 0.405969 0.407458 0.039 Uiso 1 1 calc R U . . .
C6 C 0.4355(3) 0.5320(3) 0.3942(2) 0.0315(9) Uani 1 1 d . . . . .
H6A H 0.410585 0.549442 0.352376 0.038 Uiso 1 1 calc R U . . .
H6B H 0.398738 0.571773 0.425271 0.038 Uiso 1 1 calc R U . . .
C7 C 0.6105(2) 0.4939(3) 0.38838(17) 0.0225(7) Uani 1 1 d . . . . .
C8 C 0.5730(3) 0.6547(3) 0.4096(2) 0.0316(8) Uani 1 1 d . . . . .
H8 H 0.535656 0.713426 0.418194 0.038 Uiso 1 1 calc R U . . .
C9 C 0.6701(3) 0.6495(3) 0.4064(2) 0.0300(8) Uani 1 1 d . . . . .
H9 H 0.714378 0.703645 0.412171 0.036 Uiso 1 1 calc R U . . .
C10 C 0.7892(2) 0.5097(2) 0.38415(17) 0.0218(7) Uani 1 1 d . . . . .
C11 C 0.8233(3) 0.5013(3) 0.32362(18) 0.0250(7) Uani 1 1 d . . . . .
C12 C 0.9158(3) 0.4604(3) 0.31528(19) 0.0284(8) Uani 1 1 d . . . . .
H12 H 0.940927 0.453414 0.274351 0.034 Uiso 1 1 calc R U . . .
C13 C 0.9711(3) 0.4299(3) 0.36540(19) 0.0275(8) Uani 1 1 d . . . . .
C14 C 0.9349(3) 0.4415(3) 0.42556(19) 0.0264(8) Uani 1 1 d . . . . .
H14 H 0.973060 0.421419 0.460160 0.032 Uiso 1 1 calc R U . . .
C15 C 0.8426(2) 0.4825(3) 0.43564(17) 0.0235(7) Uani 1 1 d . . . . .
C16 C 0.8055(3) 0.4989(3) 0.50087(19) 0.0307(8) Uani 1 1 d . . . . .
H16A H 0.790839 0.570864 0.506921 0.046 Uiso 1 1 calc R U . . .
H16B H 0.854763 0.477771 0.530923 0.046 Uiso 1 1 calc R U . . .
H16C H 0.746712 0.458880 0.507150 0.046 Uiso 1 1 calc R U . . .
C17 C 1.0717(3) 0.3879(3) 0.3552(2) 0.0370(9) Uani 1 1 d . . . . .
H17A H 1.072987 0.348655 0.316458 0.055 Uiso 1 1 calc R U . . .
H17B H 1.089207 0.343917 0.390164 0.055 Uiso 1 1 calc R U . . .
H17C H 1.117929 0.443840 0.352315 0.055 Uiso 1 1 calc R U . . .
C18 C 0.7638(3) 0.5367(3) 0.26896(19) 0.0374(9) Uani 1 1 d . . . . .
H18A H 0.705910 0.494384 0.265255 0.056 Uiso 1 1 calc R U . . .
H18B H 0.802110 0.531297 0.230751 0.056 Uiso 1 1 calc R U . . .
H18C H 0.744625 0.607357 0.275363 0.056 Uiso 1 1 calc R U . . .


_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
Br1 Ge1 2.6118(6) . ?
Ge1 N1 1.891(3) . ?
Ge1 C7 2.059(3) . ?
N1 C5 1.458(5) . ?
N1 C1 1.498(4) . ?
N2 C7 1.335(4) . ?
N2 C8 1.378(5) . ?
N2 C6 1.467(5) . ?
N3 C7 1.356(4) . ?
N3 C9 1.390(4) . ?
N3 C10 1.449(4) . ?
C1 C4 1.515(6) . ?
C1 C3 1.527(5) . ?
C1 C2 1.530(6) . ?
C5 C6 1.516(5) . ?
C8 C9 1.348(5) . ?
C10 C15 1.378(5) . ?
C10 C11 1.388(5) . ?
C11 C12 1.402(5) . ?
C11 C18 1.509(5) . ?
C12 C13 1.381(5) . ?
C13 C14 1.395(6) . ?
C13 C17 1.515(5) . ?
C14 C15 1.403(5) . ?
C15 C16 1.508(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C7 89.96(13) . . ?
N1 Ge1 Br1 98.93(10) . . ?
C7 Ge1 Br1 90.42(10) . . ?
C5 N1 C1 114.4(3) . . ?
C5 N1 Ge1 117.1(2) . . ?
C1 N1 Ge1 118.4(2) . . ?
C7 N2 C8 110.8(3) . . ?
C7 N2 C6 124.2(3) . . ?
C8 N2 C6 124.9(3) . . ?
C7 N3 C9 109.9(3) . . ?
C7 N3 C10 124.7(3) . . ?
C9 N3 C10 125.3(3) . . ?
N1 C1 C4 111.7(4) . . ?
N1 C1 C3 109.7(3) . . ?
C4 C1 C3 109.6(4) . . ?
N1 C1 C2 108.5(3) . . ?
C4 C1 C2 109.6(4) . . ?
C3 C1 C2 107.6(4) . . ?
N1 C5 C6 112.9(3) . . ?
N2 C6 C5 111.3(3) . . ?
N2 C7 N3 105.7(3) . . ?
N2 C7 Ge1 127.5(3) . . ?
N3 C7 Ge1 126.2(2) . . ?
C9 C8 N2 107.1(3) . . ?
C8 C9 N3 106.4(3) . . ?
C15 C10 C11 123.3(3) . . ?
C15 C10 N3 118.9(3) . . ?
C11 C10 N3 117.8(3) . . ?
C10 C11 C12 117.5(3) . . ?
C10 C11 C18 121.2(3) . . ?
C12 C11 C18 121.3(4) . . ?
C13 C12 C11 121.3(4) . . ?
C12 C13 C14 119.4(3) . . ?
C12 C13 C17 120.2(4) . . ?
C14 C13 C17 120.4(4) . . ?
C13 C14 C15 120.8(3) . . ?
C10 C15 C14 117.7(3) . . ?
C10 C15 C16 121.6(3) . . ?
C14 C15 C16 120.6(3) . . ?

_refine_diff_density_max         0.940
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.088



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_032xzjh17_a
_database_code_depnum_ccdc_archive 'CCDC 1952093'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H24 Ge N3, C16 Al F36 O4'
_chemical_formula_sum            'C29 H24 Al F36 Ge N3 O4'
_chemical_formula_weight         1262.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2433(6)
_cell_length_b                   14.4020(8)
_cell_length_c                   16.1962(9)
_cell_angle_alpha                95.690(5)
_cell_angle_beta                 107.389(5)
_cell_angle_gamma                100.633(5)
_cell_volume                     2210.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8508
_cell_measurement_theta_min      4.5770
_cell_measurement_theta_max      76.0640

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    2.958
_shelx_estimated_absorpt_T_min   0.525
_shelx_estimated_absorpt_T_max   0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_reflns_number            21959
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.926
_diffrn_reflns_theta_max         76.289
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9104
_reflns_number_gt                7732
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1440P)²+6.8423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9104
_refine_ls_number_parameters     783
_refine_ls_number_restraints     134
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.2304
_refine_ls_wR_factor_gt          0.2158
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge -0.00839(5) 0.13302(3) 0.13260(3) 0.03461(17) Uani 1 1 d . . . . .
Al1 Al 0.80250(11) 0.69562(7) 0.28549(7) 0.0219(2) Uani 1 1 d . . . . .
F101 F 0.5829(4) 0.6162(3) 0.4263(2) 0.0673(10) Uani 1 1 d . . . . .
F102 F 0.7303(4) 0.5270(2) 0.4362(2) 0.0598(9) Uani 1 1 d . . . . .
F103 F 0.5121(4) 0.4635(3) 0.4062(2) 0.0756(12) Uani 1 1 d . . . . .
F104 F 0.3612(3) 0.5666(3) 0.2784(3) 0.0691(10) Uani 1 1 d . . . . .
F105 F 0.3592(3) 0.4222(2) 0.2281(2) 0.0589(8) Uani 1 1 d . . . . .
F106 F 0.4078(3) 0.5378(2) 0.16058(19) 0.0528(7) Uani 1 1 d . . . . .
F107 F 0.6097(4) 0.3689(2) 0.2914(3) 0.0719(11) Uani 1 1 d . . . . .
F108 F 0.6007(4) 0.4290(3) 0.1744(2) 0.0648(9) Uani 1 1 d . . . . .
F109 F 0.7842(3) 0.4746(2) 0.2878(3) 0.0623(9) Uani 1 1 d . . . . .
F110 F 0.5960(6) 0.6517(8) 0.0842(4) 0.0637(19) Uani 0.6 1 d D . P A 1
F111 F 0.6602(11) 0.5266(5) 0.0474(5) 0.095(3) Uani 0.6 1 d D . P A 1
F112 F 0.6640(10) 0.6418(7) -0.0288(4) 0.064(2) Uani 0.6 1 d D U P A 1
F113 F 1.0757(8) 0.6609(7) 0.1277(5) 0.0833(14) Uani 0.6 1 d D . P B 1
F114 F 0.9382(10) 0.5309(7) 0.1207(5) 0.0833(14) Uani 0.6 1 d D . P B 1
F115 F 0.9182(9) 0.5922(7) 0.0016(5) 0.0833(14) Uani 0.6 1 d D . P B 1
F119 F 1.2203(4) 0.7191(5) 0.5726(3) 0.0540(14) Uani 0.6 1 d D . P C 1
F120 F 1.0043(6) 0.6559(5) 0.5428(3) 0.0663(18) Uani 0.6 1 d D . P C 1
F121 F 1.0697(8) 0.8043(4) 0.5472(4) 0.080(2) Uani 0.6 1 d D . P C 1
F122 F 1.2834(4) 0.8293(5) 0.4581(5) 0.0520(19) Uani 0.6 1 d D . P D 1
F123 F 1.1703(7) 0.7803(5) 0.3255(3) 0.079(2) Uani 0.6 1 d D . P D 1
F124 F 1.0907(6) 0.8668(4) 0.3981(5) 0.0700(17) Uani 0.6 1 d D U P D 1
F125 F 1.2724(4) 0.6342(5) 0.4303(5) 0.0585(17) Uani 0.6 1 d D . P E 1
F126 F 1.0790(5) 0.5455(3) 0.4265(5) 0.0634(18) Uani 0.6 1 d D . P E 1
F127 F 1.0968(6) 0.5933(5) 0.3145(3) 0.0690(19) Uani 0.6 1 d D . P E 1
F128 F 0.7779(10) 0.8402(8) 0.4518(4) 0.084(4) Uani 0.7 1 d . . P F 1
F129 F 0.6830(12) 0.9649(7) 0.4345(6) 0.074(3) Uani 0.7 1 d . . P F 1
F130 F 0.8844(5) 0.9707(4) 0.4266(4) 0.0710(16) Uani 0.7 1 d . U P F 1
F131 F 0.5087(5) 0.7766(3) 0.3403(4) 0.0550(11) Uani 0.7 1 d . . P F 1
F132 F 0.4905(6) 0.7699(3) 0.2087(4) 0.0473(16) Uani 0.7 1 d . . P F 1
F133 F 0.4611(5) 0.8948(3) 0.2782(3) 0.0461(10) Uani 0.7 1 d . U P F 1
F134 F 0.6391(7) 0.9312(4) 0.1715(3) 0.0607(13) Uani 0.7 1 d . . P F 1
F135 F 0.6844(6) 1.0349(3) 0.2827(4) 0.0569(13) Uani 0.7 1 d . U P F 1
F136 F 0.8577(9) 0.9822(6) 0.2596(7) 0.080(3) Uani 0.7 1 d . . P F 1
O101 O 0.6502(3) 0.6174(2) 0.2809(2) 0.0334(6) Uani 1 1 d . . . . .
O102 O 0.8552(3) 0.6672(2) 0.1965(2) 0.0386(7) Uani 1 1 d . . . . .
O103 O 0.9347(3) 0.6878(2) 0.37886(18) 0.0297(6) Uani 1 1 d . . . . .
O104 O 0.7690(3) 0.8093(2) 0.2864(2) 0.0359(6) Uani 1 1 d D . . . .
N1 N -0.1483(4) 0.1960(3) 0.1292(2) 0.0338(7) Uani 1 1 d . . . . .
N2 N 0.1014(4) 0.2962(2) 0.2844(2) 0.0326(7) Uani 1 1 d . . . . .
N3 N 0.2396(3) 0.1987(2) 0.3074(2) 0.0279(6) Uani 1 1 d . . . . .
C1 C -0.2780(4) 0.1758(4) 0.0502(3) 0.0390(9) Uani 1 1 d . . . . .
C2 C -0.2842(6) 0.2672(5) 0.0087(4) 0.0578(14) Uani 1 1 d . . . . .
H2A H -0.2930 0.3180 0.0502 0.087 Uiso 1 1 calc R U . . .
H2B H -0.3655 0.2540 -0.0450 0.087 Uiso 1 1 calc R U . . .
H2C H -0.1981 0.2878 -0.0057 0.087 Uiso 1 1 calc R U . . .
C3 C -0.4088(5) 0.1468(5) 0.0765(4) 0.0565(13) Uani 1 1 d . . . . .
H3A H -0.4071 0.0871 0.1007 0.085 Uiso 1 1 calc R U . . .
H3B H -0.4927 0.1372 0.0249 0.085 Uiso 1 1 calc R U . . .
H3C H -0.4108 0.1975 0.1210 0.085 Uiso 1 1 calc R U . . .
C4 C -0.2724(6) 0.0952(5) -0.0163(4) 0.0595(15) Uani 1 1 d . . . . .
H4A H -0.1864 0.1126 -0.0315 0.089 Uiso 1 1 calc R U . . .
H4B H -0.3543 0.0850 -0.0693 0.089 Uiso 1 1 calc R U . . .
H4C H -0.2729 0.0362 0.0091 0.089 Uiso 1 1 calc R U . . .
C5 C -0.1496(5) 0.2653(4) 0.2014(3) 0.0452(11) Uani 1 1 d . . . . .
H5A H -0.1686 0.2305 0.2478 0.054 Uiso 1 1 calc R U . . .
H5B H -0.2270 0.2981 0.1796 0.054 Uiso 1 1 calc R U . . .
C6 C -0.0142(6) 0.3389(3) 0.2404(4) 0.0475(12) Uani 1 1 d . . . . .
H6A H 0.0087 0.3708 0.1935 0.057 Uiso 1 1 calc R U . . .
H6B H -0.0255 0.3883 0.2832 0.057 Uiso 1 1 calc R U . . .
C7 C 0.1194(4) 0.2113(3) 0.2512(3) 0.0282(7) Uani 1 1 d . . . . .
C8 C 0.2076(5) 0.3356(3) 0.3605(3) 0.0379(9) Uani 1 1 d . . . . .
H8 H 0.2183 0.3948 0.3962 0.046 Uiso 1 1 calc R U . . .
C9 C 0.2940(4) 0.2751(3) 0.3755(3) 0.0360(9) Uani 1 1 d . . . . .
H9 H 0.3772 0.2834 0.4240 0.043 Uiso 1 1 calc R U . . .
C10 C 0.3075(4) 0.1161(3) 0.2967(3) 0.0333(8) Uani 1 1 d . . . . .
C11 C 0.2023(5) 0.0233(3) 0.2874(4) 0.0508(12) Uani 1 1 d . . . . .
H11A H 0.1645 0.0262 0.3362 0.076 Uiso 1 1 calc R U . . .
H11B H 0.2489 -0.0304 0.2880 0.076 Uiso 1 1 calc R U . . .
H11C H 0.1255 0.0140 0.2318 0.076 Uiso 1 1 calc R U . . .
C12 C 0.3546(6) 0.1218(4) 0.2166(4) 0.0478(11) Uani 1 1 d . . . . .
H12A H 0.4065 0.0720 0.2112 0.072 Uiso 1 1 calc R U . . .
H12B H 0.4155 0.1849 0.2229 0.072 Uiso 1 1 calc R U . . .
H12C H 0.2722 0.1120 0.1641 0.072 Uiso 1 1 calc R U . . .
C13 C 0.4357(6) 0.1253(4) 0.3778(4) 0.0578(14) Uani 1 1 d . . . . .
H13A H 0.4057 0.1211 0.4296 0.087 Uiso 1 1 calc R U . . .
H13B H 0.5007 0.1872 0.3857 0.087 Uiso 1 1 calc R U . . .
H13C H 0.4831 0.0735 0.3699 0.087 Uiso 1 1 calc R U . . .
C101 C 0.5845(4) 0.5322(3) 0.2925(3) 0.0297(8) Uani 1 1 d . . . . .
C102 C 0.6020(6) 0.5347(4) 0.3918(3) 0.0475(12) Uani 1 1 d . . . . .
C103 C 0.4258(5) 0.5151(4) 0.2386(3) 0.0418(10) Uani 1 1 d . . . . .
C104 C 0.6441(5) 0.4493(3) 0.2612(4) 0.0459(11) Uani 1 1 d . . . . .
C105 C 0.8427(5) 0.6680(3) 0.1114(3) 0.0383(9) Uani 1 1 d D . . . .
C106 C 0.6881(9) 0.6213(6) 0.0523(5) 0.058(3) Uani 0.6 1 d D . P A 1
C107 C 0.9434(10) 0.6113(8) 0.0880(6) 0.081(4) Uani 0.6 1 d D . P B 1
C109 C 1.0733(4) 0.7078(3) 0.4243(3) 0.0287(8) Uani 1 1 d . . . . .
C110 C 1.0907(4) 0.7188(3) 0.5229(3) 0.0483(11) Uani 1 1 d D . . . .
C111 C 1.1503(4) 0.8028(4) 0.4055(3) 0.0574(15) Uani 1 1 d D . . . .
C112 C 1.1375(5) 0.6257(4) 0.4006(3) 0.0555(13) Uani 1 1 d D . . . .
C113 C 0.7007(5) 0.8721(3) 0.3092(3) 0.0209(10) Uani 0.7 1 d . . P F 1
C114 C 0.7601(9) 0.9119(6) 0.4070(4) 0.0506(19) Uani 0.7 1 d . . P F 1
C115 C 0.5381(6) 0.8287(4) 0.2838(4) 0.0347(12) Uani 0.7 1 d . . P F 1
C116 C 0.7189(7) 0.9564(4) 0.2551(5) 0.0420(15) Uani 0.7 1 d . . P F 1
F118 F 0.9862(8) 0.8228(5) 0.1607(4) 0.0818(13) Uani 0.6 1 d D . P A 1
C108 C 0.8717(8) 0.7709(6) 0.0938(5) 0.061(3) Uani 0.6 1 d D . P A 1
F117 F 0.9142(9) 0.7815(6) 0.0232(4) 0.0818(13) Uani 0.6 1 d D . P A 1
F116 F 0.7733(7) 0.8169(5) 0.0888(4) 0.0818(13) Uani 0.6 1 d D . P A 1
C214 C 0.6822(16) 0.8699(12) 0.3925(8) 0.084(4) Uiso 0.3 1 d D . P F 2
C215 C 0.5659(11) 0.8648(8) 0.2323(7) 0.084(4) Uiso 0.3 1 d D . P F 2
F233 F 0.4904(11) 0.9128(9) 0.2580(8) 0.058(4) Uiso 0.3 1 d D . P F 2
F232 F 0.5184(16) 0.7759(7) 0.2217(13) 0.101(11) Uiso 0.3 1 d D . P F 2
F231 F 0.5999(17) 0.8928(14) 0.1683(8) 0.104(8) Uiso 0.3 1 d D . P F 2
F228 F 0.783(2) 0.850(2) 0.4569(17) 0.109(14) Uiso 0.3 1 d D . P F 2
F229 F 0.652(3) 0.9448(11) 0.4324(18) 0.064(6) Uiso 0.3 1 d D . P F 2
C216 C 0.7938(10) 0.9805(8) 0.3124(7) 0.084(4) Uiso 0.3 1 d D . P F 2
F236 F 0.8906(13) 0.9876(11) 0.3843(9) 0.118(8) Uiso 0.3 1 d D . P F 2
F235 F 0.7143(12) 1.0374(7) 0.3159(8) 0.054(3) Uiso 0.3 1 d D . P F 2
F234 F 0.8310(17) 0.9761(12) 0.2460(9) 0.053(5) Uiso 0.3 1 d D . P F 2
F223 F 1.1005(8) 0.8183(6) 0.3273(4) 0.0536(19) Uiso 0.4 1 d D . P D 2
F224 F 1.1104(9) 0.8744(6) 0.4521(5) 0.062(2) Uiso 0.4 1 d D . P D 2
F222 F 1.2850(7) 0.8290(11) 0.4365(7) 0.063(4) Uiso 0.4 1 d D . P D 2
F221 F 1.0007(8) 0.7611(6) 0.5465(7) 0.066(3) Uiso 0.4 1 d D . P C 2
F220 F 1.0605(10) 0.6307(5) 0.5430(7) 0.070(3) Uiso 0.4 1 d D . P C 2
F219 F 1.2142(7) 0.7598(6) 0.5792(7) 0.060(3) Uiso 0.4 1 d D . P C 2
F227 F 1.1653(12) 0.6449(8) 0.3274(5) 0.081(3) Uiso 0.4 1 d D . P E 2
F226 F 1.0839(17) 0.5366(7) 0.3886(10) 0.142(9) Uiso 0.4 1 d D . P E 2
F225 F 1.2680(8) 0.6405(9) 0.4584(6) 0.058(3) Uiso 0.4 1 d D . P E 2
C206 C 0.6928(6) 0.6534(7) 0.0525(7) 0.044(4) Uiso 0.4 1 d D . P A 2
C208 C 0.9326(7) 0.7603(5) 0.0978(6) 0.047(3) Uiso 0.4 1 d D . P A 2
C207 C 0.9084(8) 0.5866(5) 0.0836(6) 0.038(3) Uiso 0.4 1 d D . P A 2
F211 F 0.637(2) 0.5601(7) 0.0426(11) 0.104(6) Uiso 0.4 1 d D . P A 2
F210 F 0.6139(17) 0.6950(9) 0.0868(9) 0.091(6) Uiso 0.4 1 d D . P A 2
F212 F 0.6663(16) 0.6721(9) -0.0278(7) 0.064(4) Uiso 0.4 1 d D . P A 2
F216 F 0.8528(12) 0.8267(9) 0.0996(8) 0.096(4) Uiso 0.4 1 d D . P A 2
F218 F 1.0513(9) 0.7981(8) 0.1520(6) 0.082(3) Uiso 0.4 1 d D . P A 2
F217 F 0.9359(11) 0.7535(7) 0.0175(5) 0.063(3) Uiso 0.4 1 d D . P A 2
F215 F 0.8763(10) 0.5598(7) -0.0010(5) 0.064(3) Uiso 0.4 1 d D . P A 2
F213 F 1.0500(8) 0.6141(7) 0.1116(6) 0.066(3) Uiso 0.4 1 d D . P A 2
F214 F 0.8828(10) 0.5091(6) 0.1166(6) 0.059(2) Uiso 0.4 1 d D . P A 2
F230 F 0.5719(19) 0.7994(12) 0.3839(15) 0.118(8) Uiso 0.3 1 d D . P F 2
C213 C 0.7023(9) 0.8838(6) 0.3028(7) 0.084(4) Uiso 0.3 1 d D . P F 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.822(4) . ?
Ge1 C7 2.049(4) . ?
Al1 O102 1.723(3) . ?
Al1 O101 1.725(3) . ?
Al1 O103 1.732(3) . ?
Al1 O104 1.733(3) . ?
F101 C102 1.322(7) . ?
F102 C102 1.327(6) . ?
F103 C102 1.334(6) . ?
F104 C103 1.320(6) . ?
F105 C103 1.354(6) . ?
F106 C103 1.305(6) . ?
F107 C104 1.330(6) . ?
F108 C104 1.325(6) . ?
F109 C104 1.336(6) . ?
F110 C106 1.321(7) . ?
F111 C106 1.331(7) . ?
F112 C106 1.335(7) . ?
F113 C107 1.338(7) . ?
F114 C107 1.318(8) . ?
F115 C107 1.335(7) . ?
F119 C110 1.330(5) . ?
F120 C110 1.280(5) . ?
F121 C110 1.332(5) . ?
F122 C111 1.334(5) . ?
F123 C111 1.386(5) . ?
F124 C111 1.192(7) . ?
F125 C112 1.298(5) . ?
F126 C112 1.364(6) . ?
F127 C112 1.336(6) . ?
F128 C114 1.328(12) . ?
F129 C114 1.331(10) . ?
F130 C114 1.321(11) . ?
F131 C115 1.307(8) . ?
F132 C115 1.313(8) . ?
F133 C115 1.336(7) . ?
F134 C116 1.328(9) . ?
F135 C116 1.322(8) . ?
F136 C116 1.379(10) . ?
O101 C101 1.345(5) . ?
O102 C105 1.346(5) . ?
O103 C109 1.350(4) . ?
O104 C113 1.329(6) . ?
O104 C213 1.418(7) . ?
N1 C5 1.465(6) . ?
N1 C1 1.501(5) . ?
N2 C7 1.353(5) . ?
N2 C8 1.363(6) . ?
N2 C6 1.462(6) . ?
N3 C7 1.350(5) . ?
N3 C9 1.380(5) . ?
N3 C10 1.504(5) . ?
C1 C3 1.524(7) . ?
C1 C4 1.524(7) . ?
C1 C2 1.540(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.500(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C8 C9 1.342(6) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C12 1.517(7) . ?
C10 C11 1.518(6) . ?
C10 C13 1.529(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C101 C104 1.546(6) . ?
C101 C102 1.561(6) . ?
C101 C103 1.558(6) . ?
C105 C206 1.509(6) . ?
C105 C108 1.528(9) . ?
C105 C107 1.536(12) . ?
C105 C208 1.546(6) . ?
C105 C207 1.549(6) . ?
C105 C106 1.565(10) . ?
C109 C112 1.525(6) . ?
C109 C110 1.542(6) . ?
C109 C111 1.554(6) . ?
C110 F219 1.307(6) . ?
C110 F221 1.319(6) . ?
C110 F220 1.345(6) . ?
C111 F223 1.274(6) . ?
C111 F222 1.287(7) . ?
C111 F224 1.409(6) . ?
C112 F226 1.270(7) . ?
C112 F227 1.342(7) . ?
C112 F225 1.348(7) . ?
C113 C114 1.525(8) . ?
C113 C116 1.581(8) . ?
C113 C115 1.578(8) . ?
F118 C108 1.366(7) . ?
C108 F116 1.292(7) . ?
C108 F117 1.352(7) . ?
C214 F228 1.329(8) . ?
C214 F230 1.335(8) . ?
C214 F229 1.338(8) . ?
C214 C213 1.553(7) . ?
C215 F232 1.258(7) . ?
C215 F233 1.258(7) . ?
C215 F231 1.266(7) . ?
C215 C213 1.475(7) . ?
C216 F234 1.244(7) . ?
C216 F235 1.266(7) . ?
C216 F236 1.264(7) . ?
C216 C213 1.494(7) . ?
C206 F210 1.305(7) . ?
C206 F212 1.312(7) . ?
C206 F211 1.333(7) . ?
C208 F218 1.252(7) . ?
C208 F217 1.306(7) . ?
C208 F216 1.372(7) . ?
C207 F214 1.301(7) . ?
C207 F215 1.310(7) . ?
C207 F213 1.350(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C7 93.13(15) . . ?
O102 Al1 O101 111.78(16) . . ?
O102 Al1 O103 107.65(15) . . ?
O101 Al1 O103 108.48(14) . . ?
O102 Al1 O104 109.21(16) . . ?
O101 Al1 O104 107.47(15) . . ?
O103 Al1 O104 112.29(15) . . ?
C101 O101 Al1 150.0(3) . . ?
C105 O102 Al1 150.3(3) . . ?
C109 O103 Al1 148.1(3) . . ?
C113 O104 Al1 149.1(3) . . ?
C213 O104 Al1 156.6(5) . . ?
C5 N1 C1 114.3(3) . . ?
C5 N1 Ge1 124.9(3) . . ?
C1 N1 Ge1 120.8(3) . . ?
C7 N2 C8 110.4(4) . . ?
C7 N2 C6 123.1(4) . . ?
C8 N2 C6 126.4(4) . . ?
C7 N3 C9 109.5(3) . . ?
C7 N3 C10 125.8(3) . . ?
C9 N3 C10 124.7(3) . . ?
N1 C1 C3 110.4(4) . . ?
N1 C1 C4 109.8(4) . . ?
C3 C1 C4 109.3(5) . . ?
N1 C1 C2 108.6(4) . . ?
C3 C1 C2 109.3(4) . . ?
C4 C1 C2 109.4(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 113.0(4) . . ?
N1 C5 H5A 109.0 . . ?
C6 C5 H5A 109.0 . . ?
N1 C5 H5B 109.0 . . ?
C6 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
N2 C6 C5 111.7(4) . . ?
N2 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N3 C7 N2 105.7(3) . . ?
N3 C7 Ge1 130.9(3) . . ?
N2 C7 Ge1 123.1(3) . . ?
C9 C8 N2 107.1(4) . . ?
C9 C8 H8 126.5 . . ?
N2 C8 H8 126.5 . . ?
C8 C9 N3 107.4(4) . . ?
C8 C9 H9 126.3 . . ?
N3 C9 H9 126.3 . . ?
N3 C10 C12 107.9(3) . . ?
N3 C10 C11 108.9(3) . . ?
C12 C10 C11 112.0(4) . . ?
N3 C10 C13 109.1(4) . . ?
C12 C10 C13 109.2(4) . . ?
C11 C10 C13 109.7(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O101 C101 C104 111.8(4) . . ?
O101 C101 C102 109.3(3) . . ?
C104 C101 C102 109.0(4) . . ?
O101 C101 C103 108.0(3) . . ?
C104 C101 C103 109.1(3) . . ?
C102 C101 C103 109.6(4) . . ?
F102 C102 F101 107.6(4) . . ?
F102 C102 F103 107.0(4) . . ?
F101 C102 F103 107.7(5) . . ?
F102 C102 C101 110.6(4) . . ?
F101 C102 C101 111.0(4) . . ?
F103 C102 C101 112.7(4) . . ?
F106 C103 F104 107.8(5) . . ?
F106 C103 F105 107.4(4) . . ?
F104 C103 F105 107.1(4) . . ?
F106 C103 C101 111.5(4) . . ?
F104 C103 C101 111.2(4) . . ?
F105 C103 C101 111.5(4) . . ?
F108 C104 F107 107.7(4) . . ?
F108 C104 F109 107.1(5) . . ?
F107 C104 F109 106.9(4) . . ?
F108 C104 C101 111.0(4) . . ?
F107 C104 C101 113.7(5) . . ?
F109 C104 C101 110.0(4) . . ?
O102 C105 C206 113.6(5) . . ?
O102 C105 C108 110.5(4) . . ?
O102 C105 C107 108.5(5) . . ?
C108 C105 C107 112.0(5) . . ?
O102 C105 C208 112.1(5) . . ?
C206 C105 C208 109.8(5) . . ?
O102 C105 C207 106.5(5) . . ?
C206 C105 C207 109.9(5) . . ?
C208 C105 C207 104.5(4) . . ?
O102 C105 C106 110.0(4) . . ?
C108 C105 C106 105.8(5) . . ?
C107 C105 C106 109.9(5) . . ?
F110 C106 F111 106.2(10) . . ?
F110 C106 F112 107.7(7) . . ?
F111 C106 F112 108.6(8) . . ?
F110 C106 C105 111.8(6) . . ?
F111 C106 C105 111.3(7) . . ?
F112 C106 C105 111.1(7) . . ?
F114 C107 F115 109.7(9) . . ?
F114 C107 F113 104.1(9) . . ?
F115 C107 F113 110.0(8) . . ?
F114 C107 C105 111.2(7) . . ?
F115 C107 C105 112.4(8) . . ?
F113 C107 C105 109.1(8) . . ?
O103 C109 C112 109.9(3) . . ?
O103 C109 C110 108.2(3) . . ?
C112 C109 C110 108.9(3) . . ?
O103 C109 C111 111.1(3) . . ?
C112 C109 C111 110.0(4) . . ?
C110 C109 C111 108.7(3) . . ?
F219 C110 F221 105.8(6) . . ?
F120 C110 F121 107.5(5) . . ?
F120 C110 F119 108.5(5) . . ?
F121 C110 F119 105.3(5) . . ?
F219 C110 F220 105.1(6) . . ?
F221 C110 F220 102.7(5) . . ?
F120 C110 C109 114.3(4) . . ?
F219 C110 C109 118.4(6) . . ?
F221 C110 C109 115.2(6) . . ?
F121 C110 C109 107.9(4) . . ?
F119 C110 C109 112.8(4) . . ?
F220 C110 C109 108.0(6) . . ?
F223 C111 F222 113.1(7) . . ?
F124 C111 F122 113.7(5) . . ?
F124 C111 F123 106.0(5) . . ?
F122 C111 F123 100.3(5) . . ?
F223 C111 F224 100.6(5) . . ?
F222 C111 F224 101.4(6) . . ?
F124 C111 C109 117.4(4) . . ?
F223 C111 C109 114.3(5) . . ?
F222 C111 C109 120.0(8) . . ?
F122 C111 C109 111.4(4) . . ?
F123 C111 C109 106.1(4) . . ?
F224 C111 C109 103.9(5) . . ?
F125 C112 F127 106.8(5) . . ?
F226 C112 F227 107.4(7) . . ?
F226 C112 F225 106.8(7) . . ?
F227 C112 F225 101.4(6) . . ?
F125 C112 F126 106.3(5) . . ?
F127 C112 F126 98.7(5) . . ?
F226 C112 C109 127.2(10) . . ?
F125 C112 C109 120.0(5) . . ?
F127 C112 C109 113.8(4) . . ?
F227 C112 C109 103.6(6) . . ?
F225 C112 C109 107.6(6) . . ?
F126 C112 C109 108.9(4) . . ?
O104 C113 C114 111.7(4) . . ?
O104 C113 C116 106.6(4) . . ?
C114 C113 C116 109.5(5) . . ?
O104 C113 C115 112.5(4) . . ?
C114 C113 C115 109.2(5) . . ?
C116 C113 C115 107.1(4) . . ?
F128 C114 F130 107.2(7) . . ?
F128 C114 F129 111.5(9) . . ?
F130 C114 F129 104.2(7) . . ?
F128 C114 C113 109.3(6) . . ?
F130 C114 C113 110.9(7) . . ?
F129 C114 C113 113.4(7) . . ?
F131 C115 F132 104.7(6) . . ?
F131 C115 F133 106.7(5) . . ?
F132 C115 F133 108.0(5) . . ?
F131 C115 C113 112.0(5) . . ?
F132 C115 C113 111.2(5) . . ?
F133 C115 C113 113.7(5) . . ?
F135 C116 F134 104.7(6) . . ?
F135 C116 F136 106.9(6) . . ?
F134 C116 F136 109.1(8) . . ?
F135 C116 C113 115.0(6) . . ?
F134 C116 C113 111.8(5) . . ?
F136 C116 C113 109.1(5) . . ?
F116 C108 F117 107.6(6) . . ?
F116 C108 F118 106.1(6) . . ?
F117 C108 F118 101.8(6) . . ?
F116 C108 C105 117.0(6) . . ?
F117 C108 C105 114.7(6) . . ?
F118 C108 C105 108.2(6) . . ?
F228 C214 F230 102.9(8) . . ?
F228 C214 F229 102.3(8) . . ?
F230 C214 F229 102.3(8) . . ?
F228 C214 C213 121.0(18) . . ?
F230 C214 C213 112.1(13) . . ?
F229 C214 C213 114.2(16) . . ?
F232 C215 F233 112.9(7) . . ?
F232 C215 F231 114.0(8) . . ?
F233 C215 F231 113.6(8) . . ?
F232 C215 C213 105.1(7) . . ?
F233 C215 C213 107.4(6) . . ?
F231 C215 C213 102.8(6) . . ?
F234 C216 F235 115.2(8) . . ?
F234 C216 F236 115.3(8) . . ?
F235 C216 F236 112.9(8) . . ?
F234 C216 C213 103.9(7) . . ?
F235 C216 C213 104.0(6) . . ?
F236 C216 C213 103.6(7) . . ?
F210 C206 F212 106.2(7) . . ?
F210 C206 F211 104.2(7) . . ?
F212 C206 F211 104.7(7) . . ?
F210 C206 C105 114.4(10) . . ?
F212 C206 C105 120.0(9) . . ?
F211 C206 C105 105.8(10) . . ?
F218 C208 F217 111.2(7) . . ?
F218 C208 F216 105.6(6) . . ?
F217 C208 F216 102.0(6) . . ?
F218 C208 C105 120.9(8) . . ?
F217 C208 C105 111.1(7) . . ?
F216 C208 C105 103.8(7) . . ?
F214 C207 F215 106.6(6) . . ?
F214 C207 F213 104.1(6) . . ?
F215 C207 F213 103.6(6) . . ?
F214 C207 C105 114.7(7) . . ?
F215 C207 C105 115.7(7) . . ?
F213 C207 C105 110.9(7) . . ?
O104 C213 C215 106.9(7) . . ?
O104 C213 C216 111.9(7) . . ?
C215 C213 C216 114.5(6) . . ?
O104 C213 C214 102.9(9) . . ?
C215 C213 C214 111.2(6) . . ?
C216 C213 C214 109.0(6) . . ?

_refine_diff_density_max         1.665
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.119



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_099xzjh17_a
_database_code_depnum_ccdc_archive 'CCDC 1952094'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H26 Ge N3, C16 Al F36 O4'
_chemical_formula_sum            'C34 H26 Al F36 Ge N3 O4'
_chemical_formula_weight         1324.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   10.52460(10)
_cell_length_b                   18.4838(3)
_cell_length_c                   24.2497(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.7470(10)
_cell_angle_gamma                90
_cell_volume                     4662.54(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11189
_cell_measurement_theta_min      2.9660
_cell_measurement_theta_max      76.1410

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.844
_shelx_estimated_absorpt_T_min   0.573
_shelx_estimated_absorpt_T_max   0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_reflns_number            27806
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.019
_diffrn_reflns_theta_max         76.215
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9656
_reflns_number_gt                7840
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1518P)²+17.2616P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9656
_refine_ls_number_parameters     957
_refine_ls_number_restraints     212
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0938
_refine_ls_wR_factor_ref         0.2713
_refine_ls_wR_factor_gt          0.2517
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.011
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.20161(5) 0.13811(3) 0.45039(2) 0.0274(2) Uani 1 1 d . . . . .
Al1 Al 0.53931(11) 0.55848(7) 0.30783(5) 0.0206(3) Uani 1 1 d . . . . .
N3 N 0.4436(4) 0.2015(2) 0.41517(17) 0.0293(8) Uani 1 1 d . . . . .
N1 N 0.1103(4) 0.2060(2) 0.48283(17) 0.0288(8) Uani 1 1 d . . . . .
N2 N 0.3118(4) 0.2854(2) 0.42977(17) 0.0299(8) Uani 1 1 d . . . . .
F15 F 0.9403(19) 0.5472(5) 0.3203(8) 0.089(8) Uani 0.5 1 d D . P A 1
F12 F 0.6499(11) 0.4222(7) 0.4146(5) 0.056(3) Uani 0.5 1 d D . P B 1
O1 O 0.5509(5) 0.6352(3) 0.2703(3) 0.0645(15) Uani 1 1 d . . . . .
C15 C 0.4942(4) 0.1046(3) 0.3543(2) 0.0309(10) Uani 1 1 d . . . . .
C10 C 0.5000(4) 0.1316(3) 0.4084(2) 0.0279(9) Uani 1 1 d . . . . .
F7 F 0.7466(5) 0.6841(4) 0.1722(3) 0.0972(18) Uani 1 1 d . U . . .
C14 C 0.5502(5) 0.0374(3) 0.3482(2) 0.0377(11) Uani 1 1 d . . . . .
H14 H 0.5458 0.0172 0.3120 0.045 Uiso 1 1 calc R U . . .
C11 C 0.5601(5) 0.0947(3) 0.4555(2) 0.0311(10) Uani 1 1 d . . . . .
F9 F 0.7179(7) 0.5828(3) 0.2122(3) 0.097(2) Uani 1 1 d . . . . .
F30 F 0.3290(8) 0.5509(3) 0.1822(3) 0.0736(13) Uani 0.6 1 d D . P C 1
C31 C 0.3949(5) 0.4479(3) 0.2343(2) 0.0321(10) Uani 1 1 d . . . . .
F29 F 0.4494(6) 0.4763(5) 0.1418(3) 0.0736(13) Uani 0.6 1 d D . P C 1
C12 C 0.6155(5) 0.0279(3) 0.4467(2) 0.0373(11) Uani 1 1 d . . . . .
H12 H 0.6569 0.0014 0.4779 0.045 Uiso 1 1 calc R U . . .
O2A O 0.6933(10) 0.5399(5) 0.3358(5) 0.034(2) Uani 0.5 1 d . . P D 2
F3 F 0.8214(5) 0.6810(4) 0.2845(3) 0.104(2) Uani 1 1 d . . . . .
F4 F 0.5399(6) 0.7736(3) 0.1713(3) 0.099(2) Uani 1 1 d . . . . .
C6 C 0.1943(5) 0.3190(3) 0.4436(2) 0.0367(11) Uani 1 1 d . . . . .
H6A H 0.1259 0.3163 0.4108 0.044 Uiso 1 1 calc R U . . .
H6B H 0.2111 0.3707 0.4526 0.044 Uiso 1 1 calc R U . . .
C23 C 0.7847(4) 0.4955(3) 0.36481(19) 0.0277(9) Uani 1 1 d . . . . .
F13 F 0.8649(7) 0.4444(6) 0.2871(4) 0.053(2) Uani 0.5 1 d D . P A 1
C13 C 0.6121(5) -0.0009(3) 0.3937(2) 0.0396(12) Uani 1 1 d . . . . .
C7 C 0.3303(4) 0.2137(2) 0.43220(19) 0.0267(9) Uani 1 1 d . . . . .
F6 F 0.3954(5) 0.7067(4) 0.1951(4) 0.122(3) Uani 1 1 d . . . . .
O3A O 0.4366(11) 0.5709(8) 0.3550(6) 0.043(3) Uani 0.5 1 d . . P D 2
C1 C -0.0070(5) 0.1853(3) 0.5071(2) 0.0341(10) Uani 1 1 d . . . . .
F14 F 0.9962(7) 0.4471(5) 0.3648(4) 0.051(2) Uani 0.5 1 d D . P A 1
F10 F 0.8553(12) 0.4126(10) 0.4411(5) 0.088(5) Uani 0.5 1 d D . P B 1
C5 C 0.1485(5) 0.2823(3) 0.4926(2) 0.0346(10) Uani 1 1 d . . . . .
H5A H 0.2180 0.2847 0.5250 0.041 Uiso 1 1 calc R U . . .
H5B H 0.0741 0.3096 0.5024 0.041 Uiso 1 1 calc R U . . .
F36 F 0.6125(6) 0.4163(3) 0.2281(3) 0.0598(17) Uani 0.6 1 d D . P D 1
F8 F 0.5662(8) 0.6284(5) 0.1514(3) 0.124(3) Uani 1 1 d . . . . .
F20 F 0.2610(14) 0.6545(6) 0.3089(4) 0.094(3) Uani 0.5 1 d D . P D 1
C8 C 0.4130(6) 0.3187(3) 0.4107(2) 0.0405(12) Uani 1 1 d . . . . .
H8 H 0.4225 0.3691 0.4049 0.049 Uiso 1 1 calc R U . . .
C27 C 0.3831(4) 0.6126(2) 0.39094(17) 0.0348(11) Uani 1 1 d D . . . .
F1 F 0.6849(8) 0.7380(5) 0.3273(3) 0.132(3) Uani 1 1 d . . . . .
C16 C 0.4308(6) 0.1456(4) 0.3041(2) 0.0426(13) Uani 1 1 d . . . . .
H16A H 0.4759 0.1915 0.3012 0.064 Uiso 1 1 calc R U . . .
H16B H 0.3410 0.1553 0.3078 0.064 Uiso 1 1 calc R U . . .
H16C H 0.4340 0.1167 0.2704 0.064 Uiso 1 1 calc R U . . .
C18 C 0.5658(6) 0.1243(3) 0.5137(2) 0.0415(12) Uani 1 1 d . . . . .
H18A H 0.6061 0.1722 0.5158 0.062 Uiso 1 1 calc R U . . .
H18B H 0.6165 0.0917 0.5403 0.062 Uiso 1 1 calc R U . . .
H18C H 0.4784 0.1283 0.5228 0.062 Uiso 1 1 calc R U . . .
C19 C 0.6059(5) 0.6836(3) 0.2413(2) 0.0385(12) Uani 1 1 d . . . . .
F17 F 0.7410(8) 0.5510(7) 0.4494(4) 0.057(3) Uani 0.5 1 d D . P D 1
F32 F 0.2816(8) 0.3987(6) 0.3087(3) 0.0972(18) Uani 0.6 1 d D . P D 1
C9 C 0.4964(6) 0.2663(3) 0.4018(2) 0.0395(12) Uani 1 1 d . . . . .
H9 H 0.5763 0.2727 0.3888 0.047 Uiso 1 1 calc R U . . .
O4A O 0.4751(11) 0.4945(7) 0.2605(4) 0.052(3) Uani 0.5 1 d . U P D 2
F34 F 0.5187(8) 0.3558(5) 0.2865(3) 0.070(2) Uani 0.6 1 d D . P D 1
C3 C 0.0129(7) 0.2026(4) 0.5694(3) 0.0500(15) Uani 1 1 d . . . . .
H3A H 0.0885 0.1765 0.5881 0.075 Uiso 1 1 calc R U . . .
H3B H -0.0631 0.1876 0.5854 0.075 Uiso 1 1 calc R U . . .
H3C H 0.0261 0.2548 0.5749 0.075 Uiso 1 1 calc R U . . .
C4 C -0.0310(6) 0.1041(3) 0.4996(3) 0.0454(13) Uani 1 1 d . . . . .
H4A H -0.0371 0.0916 0.4600 0.068 Uiso 1 1 calc R U . . .
H4B H -0.1115 0.0913 0.5129 0.068 Uiso 1 1 calc R U . . .
H4C H 0.0403 0.0774 0.5211 0.068 Uiso 1 1 calc R U . . .
F21 F 0.4013(9) 0.7293(6) 0.3524(4) 0.094(3) Uani 0.5 1 d D . P D 1
F16 F 0.9410(6) 0.5498(5) 0.4360(4) 0.058(2) Uani 0.5 1 d D . P D 1
C2 C -0.1234(5) 0.2257(4) 0.4764(3) 0.0480(14) Uani 1 1 d . . . . .
H2A H -0.1114 0.2779 0.4823 0.072 Uiso 1 1 calc R U . . .
H2B H -0.2011 0.2102 0.4907 0.072 Uiso 1 1 calc R U . . .
H2C H -0.1323 0.2151 0.4364 0.072 Uiso 1 1 calc R U . . .
F5 F 0.4805(8) 0.7851(4) 0.2516(4) 0.131(3) Uani 1 1 d . . . . .
F35 F 0.4680(8) 0.3365(4) 0.1977(3) 0.081(3) Uani 0.6 1 d D . P D 1
F28 F 0.2549(6) 0.4494(4) 0.1455(3) 0.0736(13) Uani 0.6 1 d D . P C 1
F18 F 0.8017(9) 0.6199(4) 0.3867(3) 0.059(2) Uani 0.5 1 d D . P D 1
C17 C 0.6737(8) -0.0733(4) 0.3846(3) 0.0629(19) Uani 1 1 d . . . . .
H17A H 0.6085 -0.1063 0.3657 0.094 Uiso 1 1 calc R U . . .
H17B H 0.7108 -0.0938 0.4208 0.094 Uiso 1 1 calc R U . . .
H17C H 0.7417 -0.0664 0.3616 0.094 Uiso 1 1 calc R U . . .
C32 C 0.3614(5) 0.4795(3) 0.1756(2) 0.0591(18) Uani 1 1 d D . . . .
F23 F 0.3626(12) 0.4949(6) 0.4258(6) 0.107(5) Uani 0.5 1 d D U P D 1
F2 F 0.7403(8) 0.7863(4) 0.2545(4) 0.147(3) Uani 1 1 d . U . . .
F11 F 0.7674(9) 0.3653(4) 0.3625(4) 0.058(2) Uani 0.5 1 d D . P B 1
F25 F 0.4969(11) 0.5891(4) 0.4826(4) 0.0778(17) Uani 0.5 1 d D . P D 1
C25 C 0.8978(13) 0.4822(6) 0.3344(5) 0.052(5) Uani 0.5 1 d D . P A 1
F22 F 0.2186(11) 0.5714(7) 0.4436(5) 0.106(4) Uani 0.5 1 d D U P D 1
C22 C 0.6649(9) 0.6425(6) 0.1931(4) 0.078(3) Uani 1 1 d . . . . .
C24 C 0.7640(12) 0.4223(7) 0.3966(5) 0.042(4) Uani 0.5 1 d D . P B 1
C33 C 0.2775(8) 0.4160(5) 0.2543(4) 0.053(3) Uani 0.6 1 d D . P D 1
C34 C 0.4994(8) 0.3874(4) 0.2363(3) 0.039(2) Uani 0.6 1 d D . P D 1
F27 F 0.5419(8) 0.6895(5) 0.4432(4) 0.0778(17) Uani 0.5 1 d D . P D 1
F19 F 0.2269(10) 0.7097(6) 0.3848(5) 0.094(4) Uani 0.5 1 d D U P D 1
C26 C 0.8191(9) 0.5541(5) 0.4102(5) 0.043(4) Uani 0.5 1 d D . P D 1
F26 F 0.3631(8) 0.6790(5) 0.4760(4) 0.0778(17) Uani 0.5 1 d D . P D 1
C20 C 0.7144(10) 0.7242(5) 0.2787(6) 0.095(4) Uani 1 1 d . . . . .
F31 F 0.1753(8) 0.4610(5) 0.2430(4) 0.0972(18) Uani 0.6 1 d D . P D 1
C28 C 0.3143(9) 0.6760(4) 0.3592(3) 0.074(3) Uani 0.5 1 d D . P D 1
F24 F 0.2130(12) 0.5295(8) 0.3595(5) 0.119(5) Uani 0.5 1 d D U P D 1
F33 F 0.2411(9) 0.3524(4) 0.2277(4) 0.0972(18) Uani 0.6 1 d D . P D 1
C30 C 0.4468(8) 0.6429(4) 0.4489(3) 0.074(3) Uani 0.5 1 d D . P D 1
C29 C 0.2916(8) 0.5530(4) 0.4040(4) 0.074(3) Uani 0.5 1 d D . P D 1
C21 C 0.5033(8) 0.7348(5) 0.2121(4) 0.075(3) Uani 1 1 d . . . . .
F18A F 0.8890(9) 0.6044(4) 0.3972(3) 0.063(2) Uani 0.5 1 d D . P D 2
F16A F 0.9767(7) 0.5043(6) 0.4307(4) 0.075(3) Uani 0.5 1 d D . P D 2
F17A F 0.7987(10) 0.5414(7) 0.4558(5) 0.068(3) Uani 0.5 1 d D . P D 2
C26A C 0.8636(10) 0.5365(5) 0.4121(5) 0.047(4) Uani 0.5 1 d D . P D 2
F14A F 0.9583(12) 0.4237(6) 0.3390(4) 0.090(4) Uani 0.5 1 d D . P D 2
F13A F 0.8040(11) 0.4533(6) 0.2729(4) 0.067(3) Uani 0.5 1 d D . P D 2
F15A F 0.9433(15) 0.5342(6) 0.3080(7) 0.052(3) Uani 0.5 1 d D . P D 2
C25A C 0.8757(11) 0.4765(6) 0.3201(5) 0.043(4) Uani 0.5 1 d D . P D 2
F11A F 0.6940(12) 0.3798(5) 0.3447(4) 0.071(3) Uani 0.5 1 d D . P D 2
F10A F 0.8124(10) 0.3948(7) 0.4254(5) 0.070(4) Uani 0.5 1 d D . P D 2
F12A F 0.6247(14) 0.4451(7) 0.4080(6) 0.066(4) Uani 0.5 1 d D . P D 2
C24A C 0.7298(13) 0.4281(7) 0.3856(5) 0.049(5) Uani 0.5 1 d D . P D 2
F30A F 0.2794(8) 0.5331(5) 0.1657(4) 0.055(2) Uiso 0.4 1 d D . P C 2
F29A F 0.4778(7) 0.5012(6) 0.1634(5) 0.063(3) Uiso 0.4 1 d D . P C 2
F28A F 0.3198(12) 0.4261(6) 0.1389(6) 0.099(5) Uiso 0.4 1 d D . P C 2
F36A F 0.5571(8) 0.3741(6) 0.2081(4) 0.060(3) Uani 0.4 1 d D . P D 2
F35A F 0.3624(10) 0.3341(6) 0.1863(4) 0.077(4) Uani 0.4 1 d D . P D 2
F34A F 0.4541(12) 0.3343(5) 0.2726(3) 0.060(3) Uani 0.4 1 d D . P D 2
C34A C 0.4407(10) 0.3722(6) 0.2247(4) 0.046(4) Uani 0.4 1 d D . P D 2
F31A F 0.2117(9) 0.5099(4) 0.2613(4) 0.052(2) Uiso 0.4 1 d D . P D 2
F32A F 0.3133(7) 0.4285(4) 0.3151(3) 0.0334(16) Uiso 0.4 1 d D . P D 2
F33A F 0.1815(13) 0.3973(6) 0.2397(5) 0.088(4) Uiso 0.4 1 d D . P D 2
C33A C 0.2718(11) 0.4452(5) 0.2612(4) 0.041(4) Uiso 0.4 1 d D . P D 2
C29A C 0.2799(9) 0.5694(7) 0.4153(5) 0.059(8) Uiso 0.25 1 d D . P D 2
C28A C 0.3158(12) 0.6791(6) 0.3607(6) 0.046(6) Uiso 0.25 1 d D . P D 2
C30A C 0.4894(8) 0.6368(5) 0.4363(4) 0.038(5) Uiso 0.25 1 d D . P D 2
F27A F 0.5923(12) 0.6614(8) 0.4141(6) 0.054(4) Uiso 0.25 1 d D . P D 2
F25A F 0.5346(19) 0.5832(7) 0.4717(8) 0.088(8) Uiso 0.25 1 d D . P D 2
F26A F 0.4529(11) 0.6912(6) 0.4677(4) 0.044(3) Uiso 0.25 1 d D . P D 2
F20A F 0.287(2) 0.6825(12) 0.3045(6) 0.069(4) Uiso 0.25 1 d D . P D 2
F21A F 0.363(3) 0.7443(11) 0.3781(10) 0.119(10) Uiso 0.25 1 d D . P D 2
F19A F 0.2007(18) 0.6718(13) 0.3794(9) 0.069(4) Uiso 0.25 1 d D . P D 2
F24A F 0.244(2) 0.5932(15) 0.4629(6) 0.063(3) Uiso 0.25 1 d D . P D 2
F22A F 0.1708(9) 0.5681(9) 0.3766(6) 0.063(3) Uiso 0.25 1 d D . P D 2
F23A F 0.316(2) 0.4997(9) 0.4236(9) 0.063(3) Uiso 0.25 1 d D . P D 2
C29B C 0.3475(12) 0.5683(6) 0.4398(4) 0.053(6) Uiso 0.25 1 d D . P D 3
C28B C 0.2596(9) 0.6253(6) 0.3487(4) 0.053(6) Uiso 0.25 1 d D . P D 3
C30B C 0.4382(12) 0.6853(4) 0.4122(5) 0.059(7) Uiso 0.25 1 d D . P D 3
F23B F 0.4512(12) 0.5644(9) 0.4790(6) 0.049(3) Uiso 0.25 1 d D . P D 3
F22B F 0.2567(16) 0.6062(13) 0.4604(9) 0.074(8) Uiso 0.25 1 d D . P D 3
F24B F 0.304(3) 0.5023(10) 0.4262(15) 0.126(15) Uiso 0.25 1 d D . P D 3
F27B F 0.3771(17) 0.7131(11) 0.4515(6) 0.074(5) Uiso 0.25 1 d D . P D 3
F26B F 0.5579(17) 0.6671(14) 0.4337(9) 0.102(10) Uiso 0.25 1 d D . P D 3
F25B F 0.4377(13) 0.7320(7) 0.3708(5) 0.040(3) Uiso 0.25 1 d D . P D 3
F20B F 0.1969(18) 0.5618(7) 0.3369(8) 0.070(5) Uiso 0.25 1 d D . P D 3
F21B F 0.2882(19) 0.6506(10) 0.3000(7) 0.058(5) Uiso 0.25 1 d D . P D 3
F19B F 0.1731(15) 0.6713(8) 0.3653(7) 0.056(5) Uiso 0.25 1 d D . P D 3
O2 O 0.6789(11) 0.5096(6) 0.3306(5) 0.037(2) Uani 0.5 1 d . . P D 1
O3 O 0.4800(10) 0.5839(9) 0.3678(5) 0.042(3) Uani 0.5 1 d . . P D 1
O4 O 0.4370(12) 0.4954(7) 0.2756(5) 0.058(3) Uani 0.5 1 d . U P D 1


_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 N1 1.830(4) . ?
Ge1 C7 2.040(4) . ?
Al1 O2A 1.694(11) . ?
Al1 O4 1.695(11) . ?
Al1 O1 1.699(4) . ?
Al1 O3A 1.704(13) . ?
Al1 O4A 1.713(10) . ?
Al1 O3 1.733(12) . ?
Al1 O2 1.741(11) . ?
N3 C7 1.339(6) . ?
N3 C9 1.380(6) . ?
N3 C10 1.443(6) . ?
N1 C5 1.475(6) . ?
N1 C1 1.497(6) . ?
N2 C7 1.339(6) . ?
N2 C8 1.369(7) . ?
N2 C6 1.467(7) . ?
F15 C25 1.344(8) . ?
F12 C24 1.338(8) . ?
O1 C19 1.323(6) . ?
C15 C14 1.391(8) . ?
C15 C10 1.396(7) . ?
C15 C16 1.502(7) . ?
C10 C11 1.396(7) . ?
F7 C22 1.312(10) . ?
C14 C13 1.386(8) . ?
C11 C12 1.395(8) . ?
C11 C18 1.507(7) . ?
F9 C22 1.292(11) . ?
F30 C32 1.378(6) . ?
C31 O4A 1.303(11) . ?
C31 O4 1.355(12) . ?
C31 C34A 1.509(13) . ?
C31 C33 1.513(10) . ?
C31 C32 1.531(7) . ?
C31 C33A 1.537(13) . ?
C31 C34 1.564(10) . ?
F29 C32 1.328(6) . ?
C12 C13 1.387(8) . ?
O2A C23 1.373(12) . ?
F3 C20 1.369(13) . ?
F4 C21 1.326(10) . ?
C6 C5 1.507(8) . ?
C23 O2 1.310(12) . ?
C23 C24A 1.494(16) . ?
C23 C26A 1.512(13) . ?
C23 C25 1.513(17) . ?
C23 C26 1.546(13) . ?
C23 C24 1.589(15) . ?
C23 C25A 1.591(14) . ?
F13 C25 1.342(8) . ?
C13 C17 1.517(8) . ?
F6 C21 1.260(11) . ?
O3A C27 1.349(13) . ?
C1 C3 1.527(8) . ?
C1 C4 1.528(8) . ?
C1 C2 1.529(8) . ?
F14 C25 1.344(8) . ?
F10 C24 1.343(8) . ?
F36 C34 1.347(7) . ?
F8 C22 1.361(13) . ?
F20 C28 1.324(7) . ?
C8 C9 1.346(8) . ?
C27 O3 1.345(12) . ?
C27 C30A 1.513(6) . ?
C27 C30B 1.522(5) . ?
C27 C28 1.522(5) . ?
C27 C29 1.528(6) . ?
C27 C29B 1.532(5) . ?
C27 C29A 1.536(7) . ?
C27 C28B 1.545(6) . ?
C27 C28A 1.546(7) . ?
C27 C30 1.566(6) . ?
F1 C20 1.290(16) . ?
C19 C21 1.526(9) . ?
C19 C20 1.540(11) . ?
C19 C22 1.597(12) . ?
F17 C26 1.350(8) . ?
F32 C33 1.352(7) . ?
F34 C34 1.338(7) . ?
F21 C28 1.372(7) . ?
F16 C26 1.341(7) . ?
F5 C21 1.381(13) . ?
F35 C34 1.334(7) . ?
F28 C32 1.360(6) . ?
F18 C26 1.344(7) . ?
C32 F30A 1.311(7) . ?
C32 F28A 1.357(7) . ?
C32 F29A 1.363(7) . ?
F23 C29 1.368(7) . ?
F2 C20 1.336(12) . ?
F11 C24 1.344(7) . ?
F25 C30 1.343(5) . ?
F22 C29 1.360(7) . ?
C33 F31 1.354(7) . ?
C33 F33 1.366(7) . ?
F27 C30 1.343(5) . ?
F19 C28 1.339(7) . ?
F26 C30 1.353(5) . ?
F24 C29 1.328(7) . ?
F18A C26A 1.343(8) . ?
F16A C26A 1.347(8) . ?
F17A C26A 1.348(8) . ?
F14A C25A 1.341(7) . ?
F13A C25A 1.341(8) . ?
F15A C25A 1.340(8) . ?
F11A C24A 1.346(8) . ?
F10A C24A 1.344(8) . ?
F12A C24A 1.342(8) . ?
F36A C34A 1.347(8) . ?
F35A C34A 1.345(8) . ?
F34A C34A 1.345(8) . ?
F31A C33A 1.353(8) . ?
F32A C33A 1.349(8) . ?
F33A C33A 1.344(8) . ?
C29A F24A 1.345(8) . ?
C29A F23A 1.349(8) . ?
C29A F22A 1.368(7) . ?
C28A F21A 1.346(8) . ?
C28A F20A 1.351(8) . ?
C28A F19A 1.363(8) . ?
C30A F26A 1.350(6) . ?
C30A F25A 1.351(6) . ?
C30A F27A 1.359(6) . ?
C29B F24B 1.328(8) . ?
C29B F23B 1.336(8) . ?
C29B F22B 1.342(8) . ?
C28B F21B 1.347(8) . ?
C28B F19B 1.351(8) . ?
C28B F20B 1.355(8) . ?
C30B F25B 1.324(7) . ?
C30B F27B 1.331(8) . ?
C30B F26B 1.331(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 C7 91.84(19) . . ?
O2A Al1 O1 104.0(4) . . ?
O4 Al1 O1 114.8(5) . . ?
O2A Al1 O3A 115.1(6) . . ?
O1 Al1 O3A 110.6(5) . . ?
O2A Al1 O4A 112.6(6) . . ?
O1 Al1 O4A 105.7(5) . . ?
O3A Al1 O4A 108.4(5) . . ?
O4 Al1 O3 106.8(6) . . ?
O1 Al1 O3 106.7(6) . . ?
O4 Al1 O2 103.6(6) . . ?
O1 Al1 O2 118.5(5) . . ?
O3 Al1 O2 105.6(5) . . ?
C7 N3 C9 109.6(4) . . ?
C7 N3 C10 126.0(4) . . ?
C9 N3 C10 124.3(4) . . ?
C5 N1 C1 113.7(4) . . ?
C5 N1 Ge1 125.2(3) . . ?
C1 N1 Ge1 120.8(3) . . ?
C7 N2 C8 110.1(4) . . ?
C7 N2 C6 122.0(4) . . ?
C8 N2 C6 127.8(4) . . ?
C19 O1 Al1 157.1(5) . . ?
C14 C15 C10 117.3(5) . . ?
C14 C15 C16 120.6(5) . . ?
C10 C15 C16 122.1(5) . . ?
C15 C10 C11 123.0(5) . . ?
C15 C10 N3 117.9(4) . . ?
C11 C10 N3 119.1(4) . . ?
C13 C14 C15 121.8(5) . . ?
C12 C11 C10 117.0(5) . . ?
C12 C11 C18 120.5(5) . . ?
C10 C11 C18 122.5(5) . . ?
O4A C31 C34A 119.4(8) . . ?
O4 C31 C33 102.0(7) . . ?
O4A C31 C32 104.0(7) . . ?
O4 C31 C32 116.3(7) . . ?
C34A C31 C32 104.1(5) . . ?
C33 C31 C32 111.3(5) . . ?
O4A C31 C33A 109.9(7) . . ?
C34A C31 C33A 110.2(6) . . ?
C32 C31 C33A 108.5(5) . . ?
O4 C31 C34 106.9(7) . . ?
C33 C31 C34 108.4(5) . . ?
C32 C31 C34 111.3(4) . . ?
C13 C12 C11 122.0(5) . . ?
C23 O2A Al1 151.6(7) . . ?
N2 C6 C5 111.8(4) . . ?
O2A C23 C24A 113.2(7) . . ?
O2A C23 C26A 110.5(7) . . ?
C24A C23 C26A 111.0(6) . . ?
O2 C23 C25 112.3(7) . . ?
O2 C23 C26 113.4(6) . . ?
C25 C23 C26 110.1(6) . . ?
O2 C23 C24 108.1(8) . . ?
C25 C23 C24 106.0(7) . . ?
C26 C23 C24 106.5(6) . . ?
O2A C23 C25A 103.3(7) . . ?
C24A C23 C25A 110.5(7) . . ?
C26A C23 C25A 108.0(6) . . ?
C14 C13 C12 118.9(5) . . ?
C14 C13 C17 119.7(6) . . ?
C12 C13 C17 121.4(6) . . ?
N3 C7 N2 106.5(4) . . ?
N3 C7 Ge1 127.0(3) . . ?
N2 C7 Ge1 126.2(4) . . ?
C27 O3A Al1 151.6(10) . . ?
N1 C1 C3 109.8(5) . . ?
N1 C1 C4 109.6(4) . . ?
C3 C1 C4 108.6(5) . . ?
N1 C1 C2 109.3(4) . . ?
C3 C1 C2 111.1(5) . . ?
C4 C1 C2 108.4(5) . . ?
N1 C5 C6 114.6(4) . . ?
C9 C8 N2 106.9(5) . . ?
O3A C27 C30A 107.7(7) . . ?
O3 C27 C28 115.2(8) . . ?
O3 C27 C29 110.1(8) . . ?
C28 C27 C29 113.1(5) . . ?
C30B C27 C29B 109.6(5) . . ?
O3A C27 C29A 109.9(9) . . ?
C30A C27 C29A 111.3(5) . . ?
C30B C27 C28B 109.2(5) . . ?
C29B C27 C28B 108.3(5) . . ?
O3A C27 C28A 110.7(9) . . ?
C30A C27 C28A 110.1(5) . . ?
C29A C27 C28A 107.2(5) . . ?
O3 C27 C30 105.5(6) . . ?
C28 C27 C30 106.5(4) . . ?
C29 C27 C30 105.6(4) . . ?
O1 C19 C21 109.3(5) . . ?
O1 C19 C20 111.2(7) . . ?
C21 C19 C20 112.3(7) . . ?
O1 C19 C22 108.5(6) . . ?
C21 C19 C22 106.3(6) . . ?
C20 C19 C22 109.0(8) . . ?
C8 C9 N3 106.9(5) . . ?
C31 O4A Al1 160.7(8) . . ?
F30A C32 F28A 107.0(6) . . ?
F29 C32 F28 104.2(5) . . ?
F30A C32 F29A 109.1(6) . . ?
F28A C32 F29A 106.5(6) . . ?
F29 C32 F30 108.9(6) . . ?
F28 C32 F30 104.9(5) . . ?
F30A C32 C31 120.7(6) . . ?
F29 C32 C31 118.3(5) . . ?
F28A C32 C31 109.7(8) . . ?
F28 C32 C31 113.4(5) . . ?
F29A C32 C31 103.1(6) . . ?
F30 C32 C31 106.4(5) . . ?
F13 C25 F15 107.5(8) . . ?
F13 C25 F14 107.1(8) . . ?
F15 C25 F14 108.2(8) . . ?
F13 C25 C23 112.4(9) . . ?
F15 C25 C23 107.2(12) . . ?
F14 C25 C23 114.1(10) . . ?
F9 C22 F7 111.5(8) . . ?
F9 C22 F8 109.9(10) . . ?
F7 C22 F8 107.3(8) . . ?
F9 C22 C19 109.8(7) . . ?
F7 C22 C19 110.8(9) . . ?
F8 C22 C19 107.3(7) . . ?
F12 C24 F10 107.8(8) . . ?
F12 C24 F11 108.0(8) . . ?
F10 C24 F11 107.9(8) . . ?
F12 C24 C23 110.8(10) . . ?
F10 C24 C23 111.7(10) . . ?
F11 C24 C23 110.5(9) . . ?
F32 C33 F31 104.4(7) . . ?
F32 C33 F33 102.8(6) . . ?
F31 C33 F33 106.0(7) . . ?
F32 C33 C31 119.8(7) . . ?
F31 C33 C31 111.0(7) . . ?
F33 C33 C31 111.7(7) . . ?
F35 C34 F34 108.6(6) . . ?
F35 C34 F36 107.8(7) . . ?
F34 C34 F36 107.1(6) . . ?
F35 C34 C31 112.6(7) . . ?
F34 C34 C31 110.4(6) . . ?
F36 C34 C31 110.2(6) . . ?
F16 C26 F18 108.1(7) . . ?
F16 C26 F17 108.1(8) . . ?
F18 C26 F17 106.2(7) . . ?
F16 C26 C23 113.3(7) . . ?
F18 C26 C23 109.2(8) . . ?
F17 C26 C23 111.7(8) . . ?
F1 C20 F2 108.9(11) . . ?
F1 C20 F3 109.2(9) . . ?
F2 C20 F3 109.1(10) . . ?
F1 C20 C19 112.0(9) . . ?
F2 C20 C19 110.1(8) . . ?
F3 C20 C19 107.6(9) . . ?
F20 C28 F19 110.0(7) . . ?
F20 C28 F21 107.5(7) . . ?
F19 C28 F21 103.8(6) . . ?
F20 C28 C27 109.7(8) . . ?
F19 C28 C27 115.6(7) . . ?
F21 C28 C27 109.8(7) . . ?
F25 C30 F27 107.9(5) . . ?
F25 C30 F26 107.1(5) . . ?
F27 C30 F26 106.5(5) . . ?
F25 C30 C27 110.9(7) . . ?
F27 C30 C27 111.2(6) . . ?
F26 C30 C27 113.0(6) . . ?
F24 C29 F22 107.8(7) . . ?
F24 C29 F23 107.1(7) . . ?
F22 C29 F23 105.0(7) . . ?
F24 C29 C27 113.6(8) . . ?
F22 C29 C27 114.0(7) . . ?
F23 C29 C27 108.7(8) . . ?
F6 C21 F4 109.1(9) . . ?
F6 C21 F5 105.2(8) . . ?
F4 C21 F5 104.6(8) . . ?
F6 C21 C19 115.8(7) . . ?
F4 C21 C19 114.6(6) . . ?
F5 C21 C19 106.3(8) . . ?
F18A C26A F16A 107.5(8) . . ?
F18A C26A F17A 107.1(7) . . ?
F16A C26A F17A 107.1(7) . . ?
F18A C26A C23 111.9(8) . . ?
F16A C26A C23 112.8(8) . . ?
F17A C26A C23 110.1(9) . . ?
F15A C25A F14A 108.4(8) . . ?
F15A C25A F13A 108.5(8) . . ?
F14A C25A F13A 108.0(8) . . ?
F15A C25A C23 111.6(12) . . ?
F14A C25A C23 110.7(9) . . ?
F13A C25A C23 109.5(8) . . ?
F12A C24A F10A 107.5(8) . . ?
F12A C24A F11A 107.4(8) . . ?
F10A C24A F11A 107.7(8) . . ?
F12A C24A C23 109.0(11) . . ?
F10A C24A C23 112.5(10) . . ?
F11A C24A C23 112.6(10) . . ?
F34A C34A F35A 107.3(8) . . ?
F34A C34A F36A 106.9(8) . . ?
F35A C34A F36A 107.2(8) . . ?
F34A C34A C31 110.1(8) . . ?
F35A C34A C31 114.6(8) . . ?
F36A C34A C31 110.4(8) . . ?
F33A C33A F32A 109.3(8) . . ?
F33A C33A F31A 106.2(8) . . ?
F32A C33A F31A 106.5(7) . . ?
F33A C33A C31 116.6(9) . . ?
F32A C33A C31 104.4(7) . . ?
F31A C33A C31 113.3(8) . . ?
F24A C29A F23A 107.1(8) . . ?
F24A C29A F22A 106.0(8) . . ?
F23A C29A F22A 105.9(7) . . ?
F24A C29A C27 118.0(17) . . ?
F23A C29A C27 110.7(16) . . ?
F22A C29A C27 108.4(7) . . ?
F21A C28A F20A 106.7(8) . . ?
F21A C28A F19A 106.6(8) . . ?
F20A C28A F19A 105.6(8) . . ?
F21A C28A C27 116.4(15) . . ?
F20A C28A C27 122.0(14) . . ?
F19A C28A C27 97.5(12) . . ?
F26A C30A F25A 106.9(6) . . ?
F26A C30A F27A 106.7(6) . . ?
F25A C30A F27A 105.8(6) . . ?
F26A C30A C27 112.8(6) . . ?
F25A C30A C27 113.3(12) . . ?
F27A C30A C27 110.9(9) . . ?
F24B C29B F23B 109.9(8) . . ?
F24B C29B F22B 109.5(9) . . ?
F23B C29B F22B 108.3(8) . . ?
F24B C29B C27 114.5(19) . . ?
F23B C29B C27 108.1(9) . . ?
F22B C29B C27 106.4(14) . . ?
F21B C28B F19B 107.0(8) . . ?
F21B C28B F20B 106.4(7) . . ?
F19B C28B F20B 106.2(7) . . ?
F21B C28B C27 110.9(12) . . ?
F19B C28B C27 115.8(11) . . ?
F20B C28B C27 110.0(11) . . ?
F25B C30B F27B 110.2(8) . . ?
F25B C30B F26B 110.9(8) . . ?
F27B C30B F26B 110.4(8) . . ?
F25B C30B C27 111.2(9) . . ?
F27B C30B C27 112.5(12) . . ?
F26B C30B C27 101.5(15) . . ?
C23 O2 Al1 154.0(8) . . ?
C27 O3 Al1 148.2(8) . . ?
C31 O4 Al1 154.2(10) . . ?

_refine_diff_density_max         2.035
_refine_diff_density_min         -1.517
_refine_diff_density_rms         0.134



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_334xzjh19_twin_comp1_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 2005219'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;Australian National University
United Kingdom
;
_audit_update_record             
;
2020-05-22 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 Al F36 O4, C31 H33 Ge N P'
_chemical_formula_sum            'C47 H33 Al F36 Ge N O4 P'
_chemical_formula_weight         1490.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1911(3)
_cell_length_b                   15.3762(6)
_cell_length_c                   29.9659(10)
_cell_angle_alpha                83.214(3)
_cell_angle_beta                 88.694(2)
_cell_angle_gamma                87.381(2)
_cell_volume                     5571.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12973
_cell_measurement_theta_min      5.7740
_cell_measurement_theta_max      76.0850

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_F_000             2952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.718
_shelx_estimated_absorpt_T_min   0.550
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_reflns_number            24700
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.630
_diffrn_reflns_theta_max         76.701
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             24700
_reflns_number_gt                19220
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component perfect twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1321P)²] where P=(Fo²+2Fc²)/3'
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5687 41136 22314 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4313 0 22314 nmt 1.0001 -0.0675 -0.0144 0.0002 -1.0000 -0.0000 0.0004
0.0001 -1.0001
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by 179.9971° 
 around [1.00 0.00 0.00] (reciprocal) or [1.00 -0.03 -0.01] (direct)
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         24700
_refine_ls_number_parameters     1838
_refine_ls_number_restraints     372
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1824
_refine_ls_wR_factor_gt          0.1707
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.072
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.66384(4) 0.81029(3) 0.68356(2) 0.02979(11) Uani 1 1 d . . . . .
Ge2 Ge 0.82203(3) 0.32948(3) 0.17468(2) 0.02383(10) Uani 1 1 d . . . . .
P1 P 0.50912(7) 0.81335(6) 0.63299(3) 0.02554(19) Uani 1 1 d . . . . .
P2 P 0.98351(7) 0.33447(6) 0.12446(3) 0.02038(17) Uani 1 1 d . . . . .
Al1 Al 0.20142(8) 0.74335(7) 0.38902(3) 0.0214(2) Uani 1 1 d . . . . .
Al2 Al 0.66822(8) 0.76214(7) 0.11311(3) 0.0200(2) Uani 1 1 d . . . . .
F1 F 0.0512(3) 0.5304(3) 0.45671(12) 0.0663(10) Uani 1 1 d . . . . .
F2 F -0.1155(3) 0.5331(3) 0.43639(15) 0.0767(12) Uani 1 1 d . . . . .
F3 F -0.0598(3) 0.6362(3) 0.47180(12) 0.0715(11) Uani 1 1 d . . . . .
F4 F -0.1860(2) 0.6884(3) 0.39104(16) 0.0705(11) Uani 1 1 d . . . . .
F5 F -0.0698(3) 0.7776(2) 0.40902(16) 0.0722(11) Uani 1 1 d . . . . .
F6 F -0.0745(3) 0.7463(3) 0.34150(14) 0.0681(11) Uani 1 1 d . . . . .
F7 F 0.0607(3) 0.6161(3) 0.32181(11) 0.0650(9) Uani 1 1 d . . . . .
F8 F 0.0672(3) 0.5034(2) 0.37073(14) 0.0631(9) Uani 1 1 d . . . . .
F9 F -0.0890(3) 0.5559(3) 0.34629(15) 0.0748(11) Uani 1 1 d . . . . .
F10 F 0.0496(3) 0.9604(3) 0.43653(12) 0.0692(11) Uani 1 1 d . . . . .
F11 F 0.0208(3) 0.8541(3) 0.48760(12) 0.0674(10) Uani 1 1 d . . . . .
F12 F 0.1094(4) 0.9640(3) 0.50337(14) 0.0915(16) Uani 1 1 d . . . . .
F13 F 0.1792(3) 0.7198(2) 0.49302(10) 0.0512(7) Uani 1 1 d . . . . .
F14 F 0.2144(3) 0.8141(2) 0.53725(10) 0.0565(8) Uani 1 1 d . . . . .
F15 F 0.3421(2) 0.7689(2) 0.49364(10) 0.0488(7) Uani 1 1 d . . . . .
F16 F 0.2584(4) 1.0065(2) 0.42832(15) 0.0796(13) Uani 1 1 d . . . . .
F17 F 0.3308(4) 0.9499(2) 0.49158(13) 0.0676(10) Uani 1 1 d . . . . .
F18 F 0.3805(3) 0.8987(3) 0.42972(12) 0.0632(9) Uani 1 1 d . . . . .
F19 F 0.1781(5) 0.7437(3) 0.25075(11) 0.0763(12) Uani 1 1 d . . . . .
F20 F 0.1781(4) 0.8771(3) 0.22029(10) 0.0767(12) Uani 1 1 d . . . . .
F21 F 0.0395(3) 0.8298(3) 0.26062(14) 0.0770(12) Uani 1 1 d . . . . .
F22 F 0.1201(3) 0.9950(2) 0.27794(12) 0.0630(9) Uani 1 1 d . . . . .
F23 F 0.0447(3) 0.9179(2) 0.33379(13) 0.0622(9) Uani 1 1 d . . . . .
F24 F 0.1993(3) 0.97382(19) 0.34170(11) 0.0581(8) Uani 1 1 d . . . . .
F25 F 0.3364(3) 0.9477(2) 0.26815(14) 0.0678(10) Uani 1 1 d . . . . .
F26 F 0.3741(3) 0.8659(3) 0.33020(13) 0.0640(10) Uani 1 1 d . . . . .
F27 F 0.3709(3) 0.8097(3) 0.26849(14) 0.0752(12) Uani 1 1 d . . . . .
F28 F 0.2769(4) 0.5375(6) 0.4455(3) 0.076(3) Uani 0.482(6) 1 d D U P A 1
F28A F 0.3361(9) 0.5732(5) 0.4781(2) 0.076(2) Uani 0.518(6) 1 d D U P A 2
F29 F 0.4188(8) 0.5836(5) 0.4750(2) 0.074(2) Uani 0.482(6) 1 d D U P A 1
F29A F 0.4500(7) 0.4869(7) 0.4468(4) 0.066(3) Uani 0.518(6) 1 d D U P A 2
F30 F 0.4380(8) 0.4815(6) 0.4329(3) 0.051(2) Uani 0.482(6) 1 d D U P A 1
F30A F 0.2863(5) 0.5093(4) 0.4241(3) 0.063(2) Uani 0.518(6) 1 d D U P A 2
F31 F 0.5286(6) 0.7212(5) 0.4277(3) 0.066(2) Uani 0.482(6) 1 d D U P A 1
F31A F 0.5372(7) 0.7352(4) 0.3922(4) 0.097(3) Uani 0.518(6) 1 d D U P A 2
F32 F 0.5948(13) 0.5967(8) 0.4123(4) 0.076(3) Uani 0.482(6) 1 d D U P A 1
F32A F 0.5966(10) 0.6001(6) 0.3988(4) 0.073(3) Uani 0.518(6) 1 d D U P A 2
F33 F 0.5425(7) 0.6993(5) 0.3606(2) 0.0757(18) Uani 0.482(6) 1 d D U P A 1
F33A F 0.5235(7) 0.6570(6) 0.4541(3) 0.103(3) Uani 0.518(6) 1 d D U P A 2
F34 F 0.4482(7) 0.5157(5) 0.3546(5) 0.058(3) Uani 0.482(6) 1 d D U P A 1
F34A F 0.2982(4) 0.5428(5) 0.3570(3) 0.0564(17) Uani 0.518(6) 1 d D U P A 2
F35 F 0.4539(7) 0.6510(4) 0.3298(3) 0.0732(18) Uani 0.482(6) 1 d D U P A 1
F35A F 0.3791(7) 0.6468(3) 0.31925(19) 0.0581(18) Uani 0.518(6) 1 d D U P A 2
F36 F 0.2977(5) 0.5935(6) 0.3417(3) 0.065(2) Uani 0.482(6) 1 d D U P A 1
F36A F 0.4711(6) 0.5316(5) 0.3456(4) 0.052(2) Uani 0.518(6) 1 d D U P A 2
F37 F 0.3416(3) 0.7664(2) 0.14653(15) 0.0676(10) Uani 1 1 d . . . . .
F38 F 0.3126(3) 0.7917(3) 0.07751(17) 0.0785(13) Uani 1 1 d . . . . .
F39 F 0.2664(2) 0.8900(2) 0.12026(16) 0.0663(10) Uani 1 1 d . . . . .
F40 F 0.4226(3) 1.00502(18) 0.13251(11) 0.0492(7) Uani 1 1 d . . . . .
F41 F 0.4460(3) 0.8928(2) 0.18128(10) 0.0567(8) Uani 1 1 d . . . . .
F42 F 0.5829(2) 0.9442(2) 0.14280(12) 0.0532(8) Uani 1 1 d . . . . .
F43 F 0.5508(4) 0.9713(2) 0.05462(12) 0.0699(11) Uani 1 1 d . . . . .
F44 F 0.4767(5) 0.8662(3) 0.02592(12) 0.0905(16) Uani 1 1 d . . . . .
F45 F 0.3751(4) 0.9696(3) 0.04842(14) 0.0868(14) Uani 1 1 d . . . . .
F46 F 0.8180(4) 0.6002(3) 0.25682(16) 0.0921(16) Uani 1 1 d . . . . .
F47 F 0.8935(3) 0.6669(4) 0.2003(2) 0.122(2) Uani 1 1 d . . . . .
F48 F 0.7805(5) 0.5662(4) 0.1931(2) 0.1076(19) Uani 1 1 d . . . . .
F49 F 0.5711(4) 0.6137(4) 0.18565(16) 0.0988(18) Uani 1 1 d . . . . .
F50 F 0.5133(3) 0.7111(3) 0.2232(2) 0.0978(17) Uani 1 1 d . . . . .
F51 F 0.5967(3) 0.6006(3) 0.25620(13) 0.0747(12) Uani 1 1 d . . . . .
F52 F 0.6496(6) 0.8375(4) 0.2360(2) 0.120(2) Uani 1 1 d . . . . .
F53 F 0.7010(5) 0.7347(3) 0.28618(12) 0.0874(14) Uani 1 1 d . . . . .
F54 F 0.8160(5) 0.7981(4) 0.24318(18) 0.0998(17) Uani 1 1 d . . . . .
F55 F 0.6340(4) 0.4838(2) 0.12076(13) 0.0702(10) Uani 1 1 d . . . . .
F56 F 0.7965(3) 0.5132(2) 0.09587(14) 0.0657(10) Uani 1 1 d . . . . .
F57 F 0.6858(3) 0.4539(2) 0.05531(15) 0.0661(10) Uani 1 1 d . . . . .
F58 F 0.8088(3) 0.6078(3) 0.01688(13) 0.0643(10) Uani 1 1 d . . . . .
F59 F 0.6556(3) 0.5844(3) -0.01342(11) 0.0731(12) Uani 1 1 d . . . . .
F60 F 0.6857(3) 0.7132(3) 0.00405(13) 0.0689(11) Uani 1 1 d . . . . .
F61 F 0.4899(2) 0.53447(19) 0.04493(11) 0.0452(6) Uani 1 1 d . . . . .
F62 F 0.4844(2) 0.6755(2) 0.03514(12) 0.0524(7) Uani 1 1 d . . . . .
F63 F 0.4753(2) 0.6093(2) 0.10083(11) 0.0511(7) Uani 1 1 d . . . . .
F64 F 0.7906(6) 1.0196(5) 0.0507(2) 0.068(2) Uani 0.643(6) 1 d D U P B 1
F64A F 0.8014(10) 0.9616(11) 0.1282(6) 0.069(4) Uani 0.357(6) 1 d D U P B 2
F65 F 0.8079(8) 0.9800(6) 0.1207(2) 0.064(2) Uani 0.643(6) 1 d D U P B 1
F65A F 0.9334(14) 0.8687(8) 0.1435(5) 0.082(4) Uani 0.357(6) 1 d D U P B 2
F66 F 0.9494(5) 0.9988(5) 0.0777(3) 0.072(2) Uani 0.643(6) 1 d D U P B 1
F66A F 0.9600(11) 0.9822(10) 0.0978(5) 0.074(4) Uani 0.357(6) 1 d D U P B 2
F67 F 0.7814(5) 0.8922(5) -0.0035(2) 0.0617(19) Uani 0.643(6) 1 d D U P B 1
F67A F 0.7591(13) 1.0080(9) 0.0418(6) 0.082(4) Uani 0.357(6) 1 d D U P B 2
F68 F 0.8935(8) 0.7838(4) 0.0130(3) 0.0533(19) Uani 0.643(6) 1 d D U P B 1
F68A F 0.7545(13) 0.8967(11) 0.0060(6) 0.094(5) Uani 0.357(6) 1 d D U P B 2
F69 F 0.9501(5) 0.9149(4) 0.0038(2) 0.0712(18) Uani 0.643(6) 1 d D U P B 1
F69A F 0.9021(11) 0.9663(10) 0.0060(5) 0.107(4) Uani 0.357(6) 1 d D U P B 2
F70 F 0.9203(6) 0.7312(4) 0.1004(3) 0.0560(19) Uani 0.643(6) 1 d D U P B 1
F70A F 1.0333(9) 0.8412(9) 0.0569(5) 0.078(3) Uani 0.357(6) 1 d D U P B 2
F71 F 1.0403(5) 0.8266(5) 0.0799(2) 0.0688(19) Uani 0.643(6) 1 d D U P B 1
F71A F 0.9164(15) 0.7779(11) 0.0206(4) 0.062(4) Uani 0.357(6) 1 d D U P B 2
F72 F 0.9433(7) 0.8344(5) 0.1402(2) 0.070(2) Uani 0.643(6) 1 d D U P B 1
F72A F 0.9436(15) 0.7356(9) 0.0896(5) 0.077(4) Uani 0.357(6) 1 d D U P B 2
O1 O 0.1028(2) 0.66772(19) 0.40210(10) 0.0297(6) Uani 1 1 d . . . . .
O2 O 0.1862(2) 0.83345(18) 0.41840(9) 0.0285(5) Uani 1 1 d . . . . .
O3 O 0.1890(2) 0.78208(19) 0.33283(9) 0.0293(6) Uani 1 1 d . . . . .
O4 O 0.3287(2) 0.69574(19) 0.40386(11) 0.0345(6) Uani 1 1 d . . . . .
O5 O 0.5332(2) 0.79846(19) 0.10768(11) 0.0347(6) Uani 1 1 d . . . . .
O6 O 0.7068(3) 0.7482(2) 0.16851(11) 0.0411(7) Uani 1 1 d . . . . .
O7 O 0.6821(2) 0.6615(2) 0.09253(11) 0.0349(6) Uani 1 1 d . . . . .
O8 O 0.7502(3) 0.8379(2) 0.08428(12) 0.0401(7) Uani 1 1 d . . . . .
N1 N 0.7226(3) 0.7165(2) 0.65849(11) 0.0264(6) Uani 1 1 d . . . . .
N2 N 0.7758(2) 0.2392(2) 0.14731(10) 0.0227(6) Uani 1 1 d . . . . .
C1 C 0.8190(3) 0.6758(2) 0.68154(13) 0.0262(7) Uani 1 1 d . . . . .
C2 C 0.8055(3) 0.6153(3) 0.72008(13) 0.0306(8) Uani 1 1 d . . . . .
C3 C 0.8996(4) 0.5803(3) 0.74186(15) 0.0386(10) Uani 1 1 d . . . . .
H3 H 0.892776 0.539765 0.768181 0.046 Uiso 1 1 calc R U . . .
C4 C 1.0031(4) 0.6030(3) 0.72605(17) 0.0395(10) Uani 1 1 d . . . . .
H4 H 1.066337 0.578912 0.741777 0.047 Uiso 1 1 calc R U . . .
C5 C 1.0149(3) 0.6612(3) 0.68721(17) 0.0366(9) Uani 1 1 d . . . . .
H5 H 1.086307 0.676118 0.676496 0.044 Uiso 1 1 calc R U . . .
C6 C 0.9233(3) 0.6978(3) 0.66376(14) 0.0288(8) Uani 1 1 d . . . . .
C7 C 0.9388(3) 0.7552(3) 0.61923(15) 0.0340(9) Uani 1 1 d . . . . .
H7 H 0.864297 0.775695 0.608009 0.041 Uiso 1 1 calc R U . . .
C8 C 1.0031(5) 0.8363(3) 0.62449(19) 0.0504(12) Uani 1 1 d . . . . .
H8A H 0.960278 0.874252 0.643126 0.076 Uiso 1 1 calc R U . . .
H8B H 1.016980 0.868441 0.594814 0.076 Uiso 1 1 calc R U . . .
H8C H 1.073167 0.818257 0.638888 0.076 Uiso 1 1 calc R U . . .
C9 C 0.9939(5) 0.7010(4) 0.58441(18) 0.0516(13) Uani 1 1 d . . . . .
H9A H 1.067587 0.680556 0.594396 0.077 Uiso 1 1 calc R U . . .
H9B H 0.999258 0.737400 0.555381 0.077 Uiso 1 1 calc R U . . .
H9C H 0.949863 0.650360 0.581227 0.077 Uiso 1 1 calc R U . . .
C10 C 0.6931(4) 0.5866(3) 0.73713(15) 0.0413(10) Uani 1 1 d . . . . .
H10 H 0.641292 0.598483 0.711520 0.050 Uiso 1 1 calc R U . . .
C11 C 0.6501(5) 0.6395(4) 0.77457(18) 0.0558(14) Uani 1 1 d . . . . .
H11A H 0.699904 0.629614 0.800045 0.084 Uiso 1 1 calc R U . . .
H11B H 0.576741 0.620639 0.784354 0.084 Uiso 1 1 calc R U . . .
H11C H 0.645968 0.701982 0.763274 0.084 Uiso 1 1 calc R U . . .
C12 C 0.6937(5) 0.4886(4) 0.75319(19) 0.0568(15) Uani 1 1 d . . . . .
H12A H 0.732028 0.456056 0.730835 0.085 Uiso 1 1 calc R U . . .
H12B H 0.617967 0.469905 0.757101 0.085 Uiso 1 1 calc R U . . .
H12C H 0.731542 0.476867 0.781921 0.085 Uiso 1 1 calc R U . . .
C13 C 0.6879(3) 0.6736(3) 0.61976(13) 0.0275(7) Uani 1 1 d . . . . .
H13A H 0.623498 0.638424 0.629120 0.033 Uiso 1 1 calc R U . . .
H13B H 0.748064 0.632632 0.611596 0.033 Uiso 1 1 calc R U . . .
C14 C 0.6583(3) 0.7362(3) 0.57847(14) 0.0297(8) Uani 1 1 d . . . . .
C15 C 0.7127(4) 0.7271(3) 0.53777(15) 0.0372(9) Uani 1 1 d . . . . .
H15 H 0.768193 0.682042 0.536236 0.045 Uiso 1 1 calc R U . . .
C16 C 0.6864(4) 0.7834(4) 0.49943(15) 0.0445(11) Uani 1 1 d . . . . .
H16 H 0.723653 0.776440 0.471803 0.053 Uiso 1 1 calc R U . . .
C17 C 0.6059(4) 0.8496(4) 0.50127(15) 0.0434(11) Uani 1 1 d . . . . .
H17 H 0.588597 0.888128 0.474980 0.052 Uiso 1 1 calc R U . . .
C18 C 0.5508(4) 0.8596(3) 0.54144(15) 0.0343(9) Uani 1 1 d . . . . .
H18 H 0.496167 0.905339 0.542823 0.041 Uiso 1 1 calc R U . . .
C19 C 0.5757(3) 0.8023(3) 0.57970(13) 0.0285(7) Uani 1 1 d . . . . .
C20 C 0.4249(3) 0.7205(3) 0.64725(15) 0.0288(8) Uani 1 1 d . . . . .
C21 C 0.3863(3) 0.6740(3) 0.61370(16) 0.0346(9) Uani 1 1 d . . . . .
H21 H 0.403222 0.691652 0.582959 0.041 Uiso 1 1 calc R U . . .
C22 C 0.3228(4) 0.6014(3) 0.6260(2) 0.0425(11) Uani 1 1 d . . . . .
H22 H 0.295522 0.569854 0.603435 0.051 Uiso 1 1 calc R U . . .
C23 C 0.2993(4) 0.5752(3) 0.6708(2) 0.0474(12) Uani 1 1 d . . . . .
H23 H 0.256745 0.525456 0.679068 0.057 Uiso 1 1 calc R U . . .
C24 C 0.3379(4) 0.6216(3) 0.70361(19) 0.0473(12) Uani 1 1 d . . . . .
H24 H 0.321141 0.603648 0.734349 0.057 Uiso 1 1 calc R U . . .
C25 C 0.4007(4) 0.6939(3) 0.69204(17) 0.0404(10) Uani 1 1 d . . . . .
H25 H 0.427050 0.725323 0.714778 0.048 Uiso 1 1 calc R U . . .
C26 C 0.4214(3) 0.9121(3) 0.62988(13) 0.0275(7) Uani 1 1 d . . . . .
C27 C 0.4642(3) 0.9882(3) 0.64189(16) 0.0360(9) Uani 1 1 d . . . . .
H27 H 0.538573 0.988673 0.650660 0.043 Uiso 1 1 calc R U . . .
C28 C 0.3965(4) 1.0633(3) 0.6408(2) 0.0475(12) Uani 1 1 d . . . . .
H28 H 0.424522 1.115589 0.649255 0.057 Uiso 1 1 calc R U . . .
C29 C 0.2888(4) 1.0630(3) 0.6277(2) 0.0495(12) Uani 1 1 d . . . . .
H29 H 0.243441 1.115018 0.626779 0.059 Uiso 1 1 calc R U . . .
C30 C 0.2466(4) 0.9871(3) 0.6157(2) 0.0492(12) Uani 1 1 d . . . . .
H30 H 0.172491 0.987026 0.606659 0.059 Uiso 1 1 calc R U . . .
C31 C 0.3128(4) 0.9114(3) 0.61712(18) 0.0403(10) Uani 1 1 d . . . . .
H31 H 0.283985 0.858912 0.609342 0.048 Uiso 1 1 calc R U . . .
C32 C 0.6883(3) 0.1923(2) 0.17227(12) 0.0232(7) Uani 1 1 d . . . . .
C33 C 0.5802(3) 0.2044(2) 0.15641(13) 0.0260(7) Uani 1 1 d . . . . .
C34 C 0.4976(3) 0.1627(3) 0.18255(15) 0.0328(8) Uani 1 1 d . . . . .
H34 H 0.423734 0.170618 0.172956 0.039 Uiso 1 1 calc R U . . .
C35 C 0.5209(4) 0.1099(3) 0.22219(16) 0.0375(9) Uani 1 1 d . . . . .
H35 H 0.463078 0.083287 0.239847 0.045 Uiso 1 1 calc R U . . .
C36 C 0.6281(4) 0.0959(3) 0.23606(14) 0.0359(9) Uani 1 1 d . . . . .
H36 H 0.643422 0.058364 0.262900 0.043 Uiso 1 1 calc R U . . .
C37 C 0.7142(3) 0.1359(3) 0.21139(13) 0.0289(8) Uani 1 1 d . . . . .
C38 C 0.8318(4) 0.1137(3) 0.22603(14) 0.0363(9) Uani 1 1 d . . . . .
H38 H 0.881548 0.138307 0.201171 0.044 Uiso 1 1 calc R U . . .
C39 C 0.8586(5) 0.1548(4) 0.26779(19) 0.0548(13) Uani 1 1 d . . . . .
H39A H 0.849177 0.218756 0.261742 0.082 Uiso 1 1 calc R U . . .
H39B H 0.934850 0.138933 0.276103 0.082 Uiso 1 1 calc R U . . .
H39C H 0.809270 0.133434 0.292535 0.082 Uiso 1 1 calc R U . . .
C40 C 0.8552(6) 0.0142(4) 0.2334(3) 0.0647(17) Uani 1 1 d . . . . .
H40A H 0.934054 0.001915 0.237893 0.097 Uiso 1 1 calc R U . . .
H40B H 0.832285 -0.011976 0.207070 0.097 Uiso 1 1 calc R U . . .
H40C H 0.814335 -0.010790 0.260068 0.097 Uiso 1 1 calc R U . . .
C41 C 0.5531(3) 0.2567(3) 0.11154(13) 0.0282(7) Uani 1 1 d . . . . .
H41 H 0.620845 0.286129 0.099472 0.034 Uiso 1 1 calc R U . . .
C42 C 0.5192(4) 0.1953(3) 0.07789(16) 0.0410(10) Uani 1 1 d . . . . .
H42A H 0.572835 0.145804 0.078158 0.062 Uiso 1 1 calc R U . . .
H42B H 0.516764 0.227566 0.047667 0.062 Uiso 1 1 calc R U . . .
H42C H 0.446502 0.173486 0.086352 0.062 Uiso 1 1 calc R U . . .
C43 C 0.4630(4) 0.3271(3) 0.11574(17) 0.0423(10) Uani 1 1 d . . . . .
H43A H 0.395735 0.299575 0.127594 0.064 Uiso 1 1 calc R U . . .
H43B H 0.448957 0.359389 0.086091 0.064 Uiso 1 1 calc R U . . .
H43C H 0.486254 0.367596 0.136228 0.064 Uiso 1 1 calc R U . . .
C44 C 0.8179(3) 0.1978(2) 0.10786(12) 0.0237(7) Uani 1 1 d . . . . .
H44A H 0.760931 0.160121 0.098532 0.028 Uiso 1 1 calc R U . . .
H44B H 0.882874 0.159363 0.117008 0.028 Uiso 1 1 calc R U . . .
C45 C 0.8501(3) 0.2616(2) 0.06761(12) 0.0236(7) Uani 1 1 d . . . . .
C46 C 0.8027(3) 0.2565(3) 0.02635(13) 0.0294(8) Uani 1 1 d . . . . .
H46 H 0.750188 0.213621 0.023789 0.035 Uiso 1 1 calc R U . . .
C47 C 0.8313(4) 0.3134(3) -0.01126(14) 0.0361(9) Uani 1 1 d . . . . .
H47 H 0.797793 0.309265 -0.039198 0.043 Uiso 1 1 calc R U . . .
C48 C 0.9082(4) 0.3759(3) -0.00838(14) 0.0341(9) Uani 1 1 d . . . . .
H48 H 0.927399 0.414323 -0.034285 0.041 Uiso 1 1 calc R U . . .
C49 C 0.9571(3) 0.3823(2) 0.03229(13) 0.0264(7) Uani 1 1 d . . . . .
H49 H 1.009742 0.425293 0.034465 0.032 Uiso 1 1 calc R U . . .
C50 C 0.9284(3) 0.3250(2) 0.07024(12) 0.0218(7) Uani 1 1 d . . . . .
C51 C 1.0678(3) 0.4282(2) 0.12270(12) 0.0223(7) Uani 1 1 d . . . . .
C52 C 1.1753(3) 0.4234(3) 0.10597(14) 0.0288(8) Uani 1 1 d . . . . .
H52 H 1.203032 0.371888 0.094218 0.035 Uiso 1 1 calc R U . . .
C53 C 1.2415(3) 0.4939(3) 0.10651(15) 0.0320(8) Uani 1 1 d . . . . .
H53 H 1.314351 0.490904 0.094718 0.038 Uiso 1 1 calc R U . . .
C54 C 1.2020(3) 0.5689(3) 0.12416(14) 0.0308(8) Uani 1 1 d . . . . .
H54 H 1.248447 0.616603 0.125234 0.037 Uiso 1 1 calc R U . . .
C55 C 1.0950(3) 0.5741(3) 0.14018(14) 0.0302(8) Uani 1 1 d . . . . .
H55 H 1.067641 0.626001 0.151682 0.036 Uiso 1 1 calc R U . . .
C56 C 1.0267(3) 0.5039(3) 0.13965(14) 0.0275(7) Uani 1 1 d . . . . .
H56 H 0.953156 0.507748 0.150690 0.033 Uiso 1 1 calc R U . . .
C57 C 1.0708(3) 0.2390(2) 0.14114(13) 0.0255(7) Uani 1 1 d . . . . .
C58 C 1.1010(3) 0.2233(3) 0.18622(14) 0.0306(8) Uani 1 1 d . . . . .
H58 H 1.077781 0.263463 0.206688 0.037 Uiso 1 1 calc R U . . .
C59 C 1.1650(4) 0.1491(3) 0.20091(16) 0.0375(9) Uani 1 1 d . . . . .
H59 H 1.184573 0.137647 0.231624 0.045 Uiso 1 1 calc R U . . .
C60 C 1.2005(4) 0.0914(3) 0.17082(18) 0.0404(10) Uani 1 1 d . . . . .
H60 H 1.244472 0.040731 0.181062 0.048 Uiso 1 1 calc R U . . .
C61 C 1.1725(4) 0.1069(3) 0.12607(18) 0.0433(10) Uani 1 1 d . . . . .
H61 H 1.197116 0.067141 0.105649 0.052 Uiso 1 1 calc R U . . .
C62 C 1.1076(3) 0.1817(3) 0.11097(15) 0.0338(9) Uani 1 1 d . . . . .
H62 H 1.088800 0.193188 0.080178 0.041 Uiso 1 1 calc R U . . .
C63 C 0.0033(3) 0.6374(3) 0.39634(14) 0.0314(8) Uani 1 1 d . . . . .
C64 C -0.0320(4) 0.5826(4) 0.44104(18) 0.0466(12) Uani 1 1 d . . . . .
C65 C -0.0844(4) 0.7128(4) 0.3846(2) 0.0476(12) Uani 1 1 d . . . . .
C66 C 0.0090(4) 0.5781(4) 0.35809(17) 0.0443(11) Uani 1 1 d . . . . .
C67 C 0.2009(4) 0.8647(3) 0.45792(14) 0.0338(8) Uani 1 1 d . . . . .
C68 C 0.0922(5) 0.9102(4) 0.47205(18) 0.0538(14) Uani 1 1 d . . . . .
C69 C 0.2350(4) 0.7899(3) 0.49628(15) 0.0386(9) Uani 1 1 d . . . . .
C70 C 0.2936(5) 0.9305(4) 0.4520(2) 0.0541(13) Uani 1 1 d . U . . .
C71 C 0.1993(4) 0.8496(3) 0.30019(14) 0.0335(9) Uani 1 1 d . . . . .
C72 C 0.1469(6) 0.8243(4) 0.25717(17) 0.0539(14) Uani 1 1 d . . . . .
C73 C 0.1396(4) 0.9351(3) 0.31368(17) 0.0443(11) Uani 1 1 d . . . . .
C74 C 0.3215(4) 0.8686(4) 0.29117(19) 0.0485(12) Uani 1 1 d . . . . .
C75 C 0.4000(4) 0.6259(3) 0.40129(17) 0.0457(10) Uani 1 1 d D U . . .
C76 C 0.3763(4) 0.5519(3) 0.43859(15) 0.0569(12) Uani 1 1 d D U . . .
C77 C 0.5163(4) 0.6571(3) 0.4058(2) 0.0741(13) Uani 1 1 d D U . . .
C78 C 0.3937(4) 0.5905(3) 0.35558(14) 0.0557(11) Uani 1 1 d D U . . .
C79 C 0.4594(3) 0.8668(2) 0.10458(13) 0.0271(7) Uani 1 1 d . . . . .
C80 C 0.3434(4) 0.8281(3) 0.1137(2) 0.0483(12) Uani 1 1 d . . . . .
C81 C 0.4788(4) 0.9283(3) 0.14056(15) 0.0337(8) Uani 1 1 d . . . . .
C82 C 0.4628(6) 0.9192(3) 0.05779(18) 0.0543(14) Uani 1 1 d . . . . .
C83 C 0.7053(3) 0.7038(3) 0.20943(13) 0.0308(8) Uani 1 1 d . . . . .
C84 C 0.8032(5) 0.6357(4) 0.2155(2) 0.0539(13) Uani 1 1 d . . . . .
C85 C 0.5961(4) 0.6542(4) 0.21948(17) 0.0459(11) Uani 1 1 d . . . . .
C86 C 0.7119(5) 0.7696(4) 0.2451(2) 0.0531(13) Uani 1 1 d . . . . .
C87 C 0.6501(3) 0.6064(2) 0.06442(13) 0.0255(7) Uani 1 1 d . . . . .
C88 C 0.6918(4) 0.5128(3) 0.0840(2) 0.0472(12) Uani 1 1 d . . . . .
C89 C 0.7001(4) 0.6277(4) 0.01676(18) 0.0471(12) Uani 1 1 d . . . . .
C90 C 0.5230(3) 0.6060(3) 0.06062(16) 0.0340(8) Uani 1 1 d . . . . .
C91 C 0.8473(4) 0.8711(3) 0.07206(15) 0.0437(9) Uani 1 1 d D U . . .
C92 C 0.8499(5) 0.9669(3) 0.0805(2) 0.0548(16) Uani 0.643(6) 1 d D U P B 1
C92A C 0.8874(9) 0.9214(6) 0.1098(3) 0.059(2) Uani 0.357(6) 1 d D U P B 2
C93 C 0.8683(5) 0.8652(4) 0.02119(17) 0.0511(16) Uani 0.643(6) 1 d D U P B 1
C93A C 0.8177(9) 0.9381(6) 0.0314(3) 0.067(2) Uani 0.357(6) 1 d D U P B 2
C94 C 0.9403(5) 0.8165(4) 0.0978(2) 0.0541(16) Uani 0.643(6) 1 d D U P B 1
C94A C 0.9358(7) 0.8061(6) 0.0595(4) 0.054(2) Uani 0.357(6) 1 d D U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.815(3) . ?
Ge1 P1 2.4418(10) . ?
Ge2 N2 1.811(3) . ?
Ge2 P2 2.4491(9) . ?
P1 C19 1.797(4) . ?
P1 C20 1.802(4) . ?
P1 C26 1.811(4) . ?
P2 C50 1.796(4) . ?
P2 C57 1.802(4) . ?
P2 C51 1.803(4) . ?
Al1 O1 1.718(3) . ?
Al1 O3 1.726(3) . ?
Al1 O2 1.728(3) . ?
Al1 O4 1.730(3) . ?
Al2 O8 1.712(3) . ?
Al2 O5 1.719(3) . ?
Al2 O6 1.722(3) . ?
Al2 O7 1.732(3) . ?
F1 C64 1.324(7) . ?
F2 C64 1.318(6) . ?
F3 C64 1.336(7) . ?
F4 C65 1.314(6) . ?
F5 C65 1.323(7) . ?
F6 C65 1.339(7) . ?
F7 C66 1.331(6) . ?
F8 C66 1.341(7) . ?
F9 C66 1.325(6) . ?
F10 C68 1.339(6) . ?
F11 C68 1.295(8) . ?
F12 C68 1.348(7) . ?
F13 C69 1.315(6) . ?
F14 C69 1.339(6) . ?
F15 C69 1.333(6) . ?
F16 C70 1.350(7) . ?
F17 C70 1.350(7) . ?
F18 C70 1.343(8) . ?
F19 C72 1.314(7) . ?
F20 C72 1.351(6) . ?
F21 C72 1.310(8) . ?
F22 C73 1.345(5) . ?
F23 C73 1.315(6) . ?
F24 C73 1.332(7) . ?
F25 C74 1.342(6) . ?
F26 C74 1.342(7) . ?
F27 C74 1.313(7) . ?
F28 C76 1.250(6) . ?
F28A C76 1.342(6) . ?
F29 C76 1.367(6) . ?
F29A C76 1.318(6) . ?
F30 C76 1.316(6) . ?
F30A C76 1.405(6) . ?
F31 C77 1.264(6) . ?
F31A C77 1.258(6) . ?
F32 C77 1.304(7) . ?
F32A C77 1.314(7) . ?
F33 C77 1.464(7) . ?
F33 F35 1.689(14) . ?
F33A C77 1.452(7) . ?
F34 C78 1.305(6) . ?
F34A C78 1.402(6) . ?
F35 C78 1.367(6) . ?
F35A C78 1.318(5) . ?
F36 C78 1.248(6) . ?
F36A C78 1.331(6) . ?
F37 C80 1.284(7) . ?
F38 C80 1.347(7) . ?
F39 C80 1.334(6) . ?
F40 C81 1.336(5) . ?
F41 C81 1.337(5) . ?
F42 C81 1.309(5) . ?
F43 C82 1.363(8) . ?
F44 C82 1.330(7) . ?
F45 C82 1.307(8) . ?
F46 C84 1.307(7) . ?
F47 C84 1.274(8) . ?
F48 C84 1.368(8) . ?
F49 C85 1.299(7) . ?
F50 C85 1.318(7) . ?
F51 C85 1.294(6) . ?
F52 C86 1.269(8) . ?
F53 C86 1.291(7) . ?
F54 C86 1.359(8) . ?
F55 C88 1.335(7) . ?
F56 C88 1.334(6) . ?
F57 C88 1.327(6) . ?
F58 C89 1.346(6) . ?
F59 C89 1.324(6) . ?
F60 C89 1.329(7) . ?
F61 C90 1.328(5) . ?
F62 C90 1.314(5) . ?
F63 C90 1.331(6) . ?
F64 C92 1.335(7) . ?
F64A C92A 1.334(8) . ?
F65 C92 1.331(6) . ?
F65A C92A 1.334(8) . ?
F66 C92 1.327(6) . ?
F66A C92A 1.330(8) . ?
F67 C93 1.328(7) . ?
F67A C93A 1.326(8) . ?
F68 C93 1.326(7) . ?
F68A C93A 1.330(8) . ?
F69 C93 1.343(6) . ?
F69A C93A 1.325(8) . ?
F70 C94 1.338(6) . ?
F70A C94A 1.325(8) . ?
F71 C94 1.329(6) . ?
F71A C94A 1.320(8) . ?
F72 C94 1.331(6) . ?
F72A C94A 1.328(8) . ?
O1 C63 1.341(5) . ?
O2 C67 1.348(5) . ?
O3 C71 1.348(5) . ?
O4 C75 1.359(5) . ?
O5 C79 1.347(5) . ?
O6 C83 1.332(5) . ?
O7 C87 1.339(5) . ?
O8 C91 1.337(5) . ?
N1 C1 1.455(5) . ?
N1 C13 1.480(5) . ?
N2 C32 1.457(4) . ?
N2 C44 1.479(5) . ?
C1 C2 1.406(5) . ?
C1 C6 1.408(5) . ?
C2 C3 1.389(6) . ?
C2 C10 1.517(6) . ?
C3 C4 1.383(7) . ?
C4 C5 1.390(7) . ?
C5 C6 1.393(6) . ?
C6 C7 1.523(6) . ?
C7 C8 1.529(6) . ?
C7 C9 1.535(7) . ?
C10 C12 1.527(8) . ?
C10 C11 1.531(7) . ?
C13 C14 1.515(6) . ?
C14 C15 1.393(6) . ?
C14 C19 1.402(6) . ?
C15 C16 1.389(7) . ?
C16 C17 1.386(8) . ?
C17 C18 1.387(7) . ?
C18 C19 1.391(6) . ?
C20 C25 1.385(6) . ?
C20 C21 1.402(6) . ?
C21 C22 1.397(6) . ?
C22 C23 1.384(8) . ?
C23 C24 1.383(9) . ?
C24 C25 1.385(7) . ?
C26 C31 1.387(6) . ?
C26 C27 1.391(6) . ?
C27 C28 1.387(7) . ?
C28 C29 1.380(8) . ?
C29 C30 1.384(8) . ?
C30 C31 1.384(7) . ?
C32 C37 1.406(5) . ?
C32 C33 1.407(5) . ?
C33 C34 1.394(5) . ?
C33 C41 1.518(5) . ?
C34 C35 1.384(7) . ?
C35 C36 1.380(7) . ?
C36 C37 1.394(6) . ?
C37 C38 1.521(6) . ?
C38 C39 1.516(7) . ?
C38 C40 1.534(7) . ?
C41 C43 1.520(6) . ?
C41 C42 1.535(6) . ?
C44 C45 1.518(5) . ?
C45 C46 1.389(5) . ?
C45 C50 1.405(5) . ?
C46 C47 1.391(6) . ?
C47 C48 1.384(6) . ?
C48 C49 1.385(6) . ?
C49 C50 1.403(5) . ?
C51 C56 1.394(5) . ?
C51 C52 1.395(5) . ?
C52 C53 1.381(6) . ?
C53 C54 1.387(6) . ?
C54 C55 1.383(6) . ?
C55 C56 1.394(5) . ?
C57 C62 1.388(6) . ?
C57 C58 1.399(6) . ?
C58 C59 1.387(6) . ?
C59 C60 1.386(7) . ?
C60 C61 1.382(7) . ?
C61 C62 1.401(6) . ?
C63 C66 1.545(7) . ?
C63 C65 1.556(6) . ?
C63 C64 1.559(6) . ?
C67 C68 1.545(7) . ?
C67 C70 1.545(7) . ?
C67 C69 1.575(6) . ?
C71 C74 1.542(6) . ?
C71 C72 1.550(7) . ?
C71 C73 1.564(7) . ?
C75 C77 1.530(5) . ?
C75 C76 1.531(5) . ?
C75 C78 1.537(6) . ?
C79 C82 1.533(6) . ?
C79 C81 1.545(6) . ?
C79 C80 1.565(6) . ?
C83 C84 1.550(6) . ?
C83 C86 1.561(7) . ?
C83 C85 1.569(7) . ?
C87 C89 1.545(6) . ?
C87 C88 1.556(6) . ?
C87 C90 1.557(5) . ?
C91 C94A 1.508(6) . ?
C91 C92 1.525(5) . ?
C91 C93A 1.537(6) . ?
C91 C92A 1.544(6) . ?
C91 C94 1.545(6) . ?
C91 C93 1.552(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 P1 88.61(11) . . ?
N2 Ge2 P2 88.55(10) . . ?
C19 P1 C20 108.22(19) . . ?
C19 P1 C26 110.86(19) . . ?
C20 P1 C26 108.38(17) . . ?
C19 P1 Ge1 102.63(13) . . ?
C20 P1 Ge1 111.56(13) . . ?
C26 P1 Ge1 114.94(14) . . ?
C50 P2 C57 108.90(18) . . ?
C50 P2 C51 111.36(17) . . ?
C57 P2 C51 106.88(17) . . ?
C50 P2 Ge2 103.89(11) . . ?
C57 P2 Ge2 107.85(12) . . ?
C51 P2 Ge2 117.70(12) . . ?
O1 Al1 O3 107.50(14) . . ?
O1 Al1 O2 113.66(15) . . ?
O3 Al1 O2 106.62(14) . . ?
O1 Al1 O4 109.18(15) . . ?
O3 Al1 O4 114.90(16) . . ?
O2 Al1 O4 105.13(15) . . ?
O8 Al2 O5 109.17(16) . . ?
O8 Al2 O6 108.16(18) . . ?
O5 Al2 O6 111.53(17) . . ?
O8 Al2 O7 111.93(17) . . ?
O5 Al2 O7 107.79(15) . . ?
O6 Al2 O7 108.30(17) . . ?
C77 F33 F35 100.5(5) . . ?
C78 F35 F33 112.2(7) . . ?
C63 O1 Al1 151.2(3) . . ?
C67 O2 Al1 145.7(3) . . ?
C71 O3 Al1 147.6(3) . . ?
C75 O4 Al1 146.2(3) . . ?
C79 O5 Al2 147.9(3) . . ?
C83 O6 Al2 151.0(3) . . ?
C87 O7 Al2 149.7(3) . . ?
C91 O8 Al2 153.4(3) . . ?
C1 N1 C13 115.1(3) . . ?
C1 N1 Ge1 113.6(3) . . ?
C13 N1 Ge1 131.3(2) . . ?
C32 N2 C44 114.0(3) . . ?
C32 N2 Ge2 113.1(2) . . ?
C44 N2 Ge2 132.5(2) . . ?
C2 C1 C6 122.2(4) . . ?
C2 C1 N1 119.5(3) . . ?
C6 C1 N1 118.2(3) . . ?
C3 C2 C1 117.6(4) . . ?
C3 C2 C10 120.3(4) . . ?
C1 C2 C10 122.1(4) . . ?
C4 C3 C2 121.4(4) . . ?
C3 C4 C5 120.1(4) . . ?
C4 C5 C6 120.9(4) . . ?
C5 C6 C1 117.6(4) . . ?
C5 C6 C7 119.7(4) . . ?
C1 C6 C7 122.6(4) . . ?
C6 C7 C8 112.1(4) . . ?
C6 C7 C9 110.0(4) . . ?
C8 C7 C9 111.4(4) . . ?
C2 C10 C12 111.9(5) . . ?
C2 C10 C11 111.3(4) . . ?
C12 C10 C11 110.3(4) . . ?
N1 C13 C14 114.6(3) . . ?
C15 C14 C19 118.6(4) . . ?
C15 C14 C13 119.5(4) . . ?
C19 C14 C13 121.8(4) . . ?
C16 C15 C14 120.5(4) . . ?
C17 C16 C15 120.3(4) . . ?
C16 C17 C18 120.1(4) . . ?
C17 C18 C19 119.7(4) . . ?
C18 C19 C14 120.8(4) . . ?
C18 C19 P1 121.8(3) . . ?
C14 C19 P1 117.4(3) . . ?
C25 C20 C21 120.1(4) . . ?
C25 C20 P1 119.2(3) . . ?
C21 C20 P1 120.7(3) . . ?
C22 C21 C20 119.3(4) . . ?
C23 C22 C21 120.2(5) . . ?
C24 C23 C22 120.0(4) . . ?
C23 C24 C25 120.6(5) . . ?
C20 C25 C24 119.9(5) . . ?
C31 C26 C27 120.6(4) . . ?
C31 C26 P1 120.8(3) . . ?
C27 C26 P1 118.6(3) . . ?
C28 C27 C26 118.9(4) . . ?
C29 C28 C27 120.6(5) . . ?
C28 C29 C30 120.3(5) . . ?
C29 C30 C31 119.7(5) . . ?
C30 C31 C26 119.9(5) . . ?
C37 C32 C33 121.8(3) . . ?
C37 C32 N2 119.1(3) . . ?
C33 C32 N2 119.0(3) . . ?
C34 C33 C32 117.5(4) . . ?
C34 C33 C41 120.1(4) . . ?
C32 C33 C41 122.3(3) . . ?
C35 C34 C33 121.5(4) . . ?
C36 C35 C34 120.0(4) . . ?
C35 C36 C37 121.2(4) . . ?
C36 C37 C32 117.9(4) . . ?
C36 C37 C38 119.5(4) . . ?
C32 C37 C38 122.5(3) . . ?
C39 C38 C37 112.1(4) . . ?
C39 C38 C40 110.4(4) . . ?
C37 C38 C40 111.3(4) . . ?
C33 C41 C43 112.4(3) . . ?
C33 C41 C42 110.3(3) . . ?
C43 C41 C42 109.7(4) . . ?
N2 C44 C45 114.8(3) . . ?
C46 C45 C50 118.3(3) . . ?
C46 C45 C44 119.3(3) . . ?
C50 C45 C44 122.3(3) . . ?
C45 C46 C47 120.7(4) . . ?
C48 C47 C46 120.6(4) . . ?
C47 C48 C49 119.9(4) . . ?
C48 C49 C50 119.5(4) . . ?
C49 C50 C45 120.9(3) . . ?
C49 C50 P2 121.3(3) . . ?
C45 C50 P2 117.7(3) . . ?
C56 C51 C52 120.2(3) . . ?
C56 C51 P2 119.8(3) . . ?
C52 C51 P2 119.9(3) . . ?
C53 C52 C51 119.9(4) . . ?
C52 C53 C54 120.4(4) . . ?
C55 C54 C53 119.7(4) . . ?
C54 C55 C56 120.7(4) . . ?
C51 C56 C55 119.0(4) . . ?
C62 C57 C58 120.1(4) . . ?
C62 C57 P2 122.2(3) . . ?
C58 C57 P2 117.7(3) . . ?
C59 C58 C57 119.7(4) . . ?
C60 C59 C58 120.0(4) . . ?
C61 C60 C59 120.7(4) . . ?
C60 C61 C62 119.6(4) . . ?
C57 C62 C61 119.8(4) . . ?
O1 C63 C66 109.8(4) . . ?
O1 C63 C65 112.1(4) . . ?
C66 C63 C65 108.8(4) . . ?
O1 C63 C64 108.1(4) . . ?
C66 C63 C64 109.4(4) . . ?
C65 C63 C64 108.7(4) . . ?
F2 C64 F1 107.6(5) . . ?
F2 C64 F3 108.4(5) . . ?
F1 C64 F3 108.0(5) . . ?
F2 C64 C63 113.3(4) . . ?
F1 C64 C63 109.7(4) . . ?
F3 C64 C63 109.7(4) . . ?
F4 C65 F5 108.2(5) . . ?
F4 C65 F6 107.1(5) . . ?
F5 C65 F6 106.8(5) . . ?
F4 C65 C63 113.7(4) . . ?
F5 C65 C63 110.1(4) . . ?
F6 C65 C63 110.6(4) . . ?
F9 C66 F7 108.7(5) . . ?
F9 C66 F8 107.1(4) . . ?
F7 C66 F8 105.9(5) . . ?
F9 C66 C63 112.9(5) . . ?
F7 C66 C63 111.5(4) . . ?
F8 C66 C63 110.5(4) . . ?
O2 C67 C68 108.6(4) . . ?
O2 C67 C70 108.9(4) . . ?
C68 C67 C70 110.5(5) . . ?
O2 C67 C69 112.3(4) . . ?
C68 C67 C69 108.7(4) . . ?
C70 C67 C69 108.0(4) . . ?
F11 C68 F10 108.6(5) . . ?
F11 C68 F12 108.9(5) . . ?
F10 C68 F12 106.6(5) . . ?
F11 C68 C67 111.9(5) . . ?
F10 C68 C67 109.6(4) . . ?
F12 C68 C67 111.1(5) . . ?
F13 C69 F15 109.1(4) . . ?
F13 C69 F14 107.5(4) . . ?
F15 C69 F14 107.3(4) . . ?
F13 C69 C67 110.0(4) . . ?
F15 C69 C67 110.8(4) . . ?
F14 C69 C67 112.0(4) . . ?
F18 C70 F16 107.6(5) . . ?
F18 C70 F17 106.8(5) . . ?
F16 C70 F17 107.5(5) . . ?
F18 C70 C67 111.3(5) . . ?
F16 C70 C67 110.7(5) . . ?
F17 C70 C67 112.7(5) . . ?
O3 C71 C74 110.5(4) . . ?
O3 C71 C72 107.8(4) . . ?
C74 C71 C72 110.2(4) . . ?
O3 C71 C73 111.3(4) . . ?
C74 C71 C73 107.9(4) . . ?
C72 C71 C73 109.2(4) . . ?
F21 C72 F19 109.0(5) . . ?
F21 C72 F20 108.4(5) . . ?
F19 C72 F20 107.2(5) . . ?
F21 C72 C71 110.5(5) . . ?
F19 C72 C71 110.3(5) . . ?
F20 C72 C71 111.5(4) . . ?
F23 C73 F24 107.6(5) . . ?
F23 C73 F22 107.6(4) . . ?
F24 C73 F22 106.5(4) . . ?
F23 C73 C71 111.0(4) . . ?
F24 C73 C71 111.6(4) . . ?
F22 C73 C71 112.3(4) . . ?
F27 C74 F26 107.0(5) . . ?
F27 C74 F25 107.6(4) . . ?
F26 C74 F25 107.5(5) . . ?
F27 C74 C71 111.5(5) . . ?
F26 C74 C71 110.0(4) . . ?
F25 C74 C71 113.0(4) . . ?
O4 C75 C77 107.8(4) . . ?
O4 C75 C76 111.0(4) . . ?
C77 C75 C76 110.1(4) . . ?
O4 C75 C78 111.2(4) . . ?
C77 C75 C78 107.9(4) . . ?
C76 C75 C78 108.8(4) . . ?
F28 C76 F30 114.0(7) . . ?
F29A C76 F28A 108.0(6) . . ?
F28 C76 F29 110.0(6) . . ?
F30 C76 F29 105.1(5) . . ?
F29A C76 F30A 102.4(6) . . ?
F28A C76 F30A 100.0(5) . . ?
F28 C76 C75 115.1(5) . . ?
F30 C76 C75 110.3(6) . . ?
F29A C76 C75 118.9(7) . . ?
F28A C76 C75 118.5(5) . . ?
F29 C76 C75 101.1(5) . . ?
F30A C76 C75 105.9(5) . . ?
F31 C77 F32 112.9(8) . . ?
F31A C77 F32A 113.9(7) . . ?
F31A C77 F33A 101.1(6) . . ?
F32A C77 F33A 100.2(6) . . ?
F31 C77 F33 98.9(5) . . ?
F32 C77 F33 102.4(6) . . ?
F31A C77 C75 119.6(5) . . ?
F31 C77 C75 118.2(5) . . ?
F32 C77 C75 117.0(9) . . ?
F32A C77 C75 115.8(7) . . ?
F33A C77 C75 101.7(5) . . ?
F33 C77 C75 103.5(5) . . ?
F36 C78 F34 115.6(7) . . ?
F35A C78 F36A 107.2(5) . . ?
F36 C78 F35 109.9(5) . . ?
F34 C78 F35 105.6(5) . . ?
F35A C78 F34A 102.1(5) . . ?
F36A C78 F34A 102.4(5) . . ?
F36 C78 C75 112.1(5) . . ?
F34 C78 C75 112.6(8) . . ?
F35A C78 C75 118.7(4) . . ?
F36A C78 C75 117.5(6) . . ?
F35 C78 C75 99.6(5) . . ?
F34A C78 C75 106.5(4) . . ?
O5 C79 C82 111.4(4) . . ?
O5 C79 C81 111.3(3) . . ?
C82 C79 C81 109.5(4) . . ?
O5 C79 C80 107.0(3) . . ?
C82 C79 C80 109.6(4) . . ?
C81 C79 C80 108.0(4) . . ?
F37 C80 F39 109.9(5) . . ?
F37 C80 F38 105.4(5) . . ?
F39 C80 F38 106.1(5) . . ?
F37 C80 C79 113.3(4) . . ?
F39 C80 C79 112.1(4) . . ?
F38 C80 C79 109.5(4) . . ?
F42 C81 F40 108.0(4) . . ?
F42 C81 F41 107.6(4) . . ?
F40 C81 F41 106.3(4) . . ?
F42 C81 C79 111.2(3) . . ?
F40 C81 C79 112.3(4) . . ?
F41 C81 C79 111.2(4) . . ?
F45 C82 F44 108.0(5) . . ?
F45 C82 F43 107.7(5) . . ?
F44 C82 F43 106.6(6) . . ?
F45 C82 C79 114.0(5) . . ?
F44 C82 C79 111.0(4) . . ?
F43 C82 C79 109.2(5) . . ?
O6 C83 C84 111.1(4) . . ?
O6 C83 C86 108.9(4) . . ?
C84 C83 C86 109.3(4) . . ?
O6 C83 C85 112.1(4) . . ?
C84 C83 C85 108.3(4) . . ?
C86 C83 C85 107.0(4) . . ?
F47 C84 F46 108.3(6) . . ?
F47 C84 F48 108.9(6) . . ?
F46 C84 F48 103.6(6) . . ?
F47 C84 C83 112.7(5) . . ?
F46 C84 C83 114.6(5) . . ?
F48 C84 C83 108.2(5) . . ?
F51 C85 F49 110.3(5) . . ?
F51 C85 F50 106.6(5) . . ?
F49 C85 F50 104.3(6) . . ?
F51 C85 C83 114.4(4) . . ?
F49 C85 C83 110.7(4) . . ?
F50 C85 C83 109.9(5) . . ?
F52 C86 F53 112.7(6) . . ?
F52 C86 F54 105.9(6) . . ?
F53 C86 F54 103.3(5) . . ?
F52 C86 C83 112.4(5) . . ?
F53 C86 C83 114.4(5) . . ?
F54 C86 C83 107.1(5) . . ?
O7 C87 C89 111.9(3) . . ?
O7 C87 C88 106.8(3) . . ?
C89 C87 C88 108.8(4) . . ?
O7 C87 C90 112.8(3) . . ?
C89 C87 C90 108.5(3) . . ?
C88 C87 C90 107.9(3) . . ?
F57 C88 F56 107.1(4) . . ?
F57 C88 F55 107.1(5) . . ?
F56 C88 F55 107.3(5) . . ?
F57 C88 C87 113.3(4) . . ?
F56 C88 C87 110.5(4) . . ?
F55 C88 C87 111.2(4) . . ?
F59 C89 F60 108.7(5) . . ?
F59 C89 F58 107.9(5) . . ?
F60 C89 F58 107.9(4) . . ?
F59 C89 C87 113.0(4) . . ?
F60 C89 C87 108.9(5) . . ?
F58 C89 C87 110.3(4) . . ?
F62 C90 F61 109.1(4) . . ?
F62 C90 F63 105.8(4) . . ?
F61 C90 F63 107.2(4) . . ?
F62 C90 C87 111.5(3) . . ?
F61 C90 C87 112.7(3) . . ?
F63 C90 C87 110.2(4) . . ?
O8 C91 C94A 115.8(5) . . ?
O8 C91 C92 111.1(4) . . ?
O8 C91 C93A 102.5(5) . . ?
C94A C91 C93A 110.7(5) . . ?
O8 C91 C92A 109.0(5) . . ?
C94A C91 C92A 110.1(5) . . ?
C93A C91 C92A 108.2(5) . . ?
O8 C91 C94 110.0(4) . . ?
C92 C91 C94 110.2(4) . . ?
O8 C91 C93 109.3(4) . . ?
C92 C91 C93 108.7(4) . . ?
C94 C91 C93 107.5(4) . . ?
F66 C92 F65 107.1(6) . . ?
F66 C92 F64 105.1(6) . . ?
F65 C92 F64 105.8(6) . . ?
F66 C92 C91 114.2(5) . . ?
F65 C92 C91 112.1(6) . . ?
F64 C92 C91 111.9(5) . . ?
F66A C92A F64A 106.9(7) . . ?
F66A C92A F65A 105.4(7) . . ?
F64A C92A F65A 105.5(7) . . ?
F66A C92A C91 116.3(9) . . ?
F64A C92A C91 109.2(11) . . ?
F65A C92A C91 112.9(9) . . ?
F68 C93 F67 106.5(6) . . ?
F68 C93 F69 107.1(6) . . ?
F67 C93 F69 105.3(5) . . ?
F68 C93 C91 111.9(6) . . ?
F67 C93 C91 112.7(5) . . ?
F69 C93 C91 113.0(5) . . ?
F69A C93A F67A 107.6(8) . . ?
F69A C93A F68A 107.1(7) . . ?
F67A C93A F68A 106.5(8) . . ?
F69A C93A C91 115.3(8) . . ?
F67A C93A C91 114.2(10) . . ?
F68A C93A C91 105.7(11) . . ?
F71 C94 F72 107.7(6) . . ?
F71 C94 F70 107.2(6) . . ?
F72 C94 F70 105.6(6) . . ?
F71 C94 C91 115.2(5) . . ?
F72 C94 C91 111.0(6) . . ?
F70 C94 C91 109.7(6) . . ?
F71A C94A F70A 108.6(8) . . ?
F71A C94A F72A 106.6(7) . . ?
F70A C94A F72A 106.7(7) . . ?
F71A C94A C91 111.8(10) . . ?
F70A C94A C91 111.1(8) . . ?
F72A C94A C91 112.0(10) . . ?

_refine_diff_density_max         1.843
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.108



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_207xzjh18-F_a
_database_code_depnum_ccdc_archive 'CCDC 1952097'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H35 Ge N4, C16 Al F36 O4, 0.5(C6 H5 F)'
_chemical_formula_sum            'C49 H37.50 Al F36.50 Ge N4 O4'
_chemical_formula_weight         1539.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   80.2560(12)
_cell_length_b                   29.4338(5)
_cell_length_c                   10.7141(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     25309.3(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    56577
_cell_measurement_theta_min      4.3900
_cell_measurement_theta_max      76.0610

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             12240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.208
_shelx_estimated_absorpt_T_min   0.512
_shelx_estimated_absorpt_T_max   0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_reflns_number            131887
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -100
_diffrn_reflns_limit_h_max       98
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.725
_diffrn_reflns_theta_max         77.137
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13230
_reflns_number_gt                12751
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_max     0.982
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13230
_refine_ls_number_parameters     1116
_refine_ls_number_restraints     675
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.1155
_refine_ls_wR_factor_ref         0.3316
_refine_ls_wR_factor_gt          0.3260
_refine_ls_goodness_of_fit_ref   1.650
_refine_ls_restrained_S_all      1.792
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.45975(2) 0.29794(3) 0.2095(2) 0.0427(3) Uani 1 1 d . . . . .
Al1 Al 0.34814(2) 0.35212(6) 0.6369(3) 0.0323(4) Uani 1 1 d . . . . .
F1 F 0.34751(19) 0.3397(5) 0.2639(17) 0.156(5) Uani 1 1 d D U . . .
F2 F 0.33555(15) 0.2948(5) 0.3885(15) 0.143(5) Uani 1 1 d D U . . .
F3 F 0.3526(2) 0.2685(5) 0.2539(16) 0.163(5) Uani 1 1 d D U . . .
F4 F 0.35800(17) 0.2310(6) 0.490(2) 0.166(5) Uani 1 1 d D U . . .
F5 F 0.37983(18) 0.2392(5) 0.3782(14) 0.153(5) Uani 1 1 d D U . . .
F6 F 0.3798(2) 0.2612(6) 0.5665(14) 0.157(5) Uani 1 1 d D U . . .
F7 F 0.3758(2) 0.3751(5) 0.347(2) 0.185(6) Uani 1 1 d D U . . .
F8 F 0.3817(2) 0.3146(7) 0.2451(14) 0.173(6) Uani 1 1 d D U . . .
F9 F 0.39242(15) 0.3262(5) 0.4243(15) 0.138(4) Uani 1 1 d D U . . .
F10 F 0.35740(15) 0.4634(5) 0.5395(15) 0.078(4) Uani 0.518(10) 1 d D U P A 1
F11 F 0.34513(18) 0.4734(5) 0.7107(12) 0.065(4) Uani 0.518(10) 1 d D U P A 1
F12 F 0.3375(2) 0.5117(5) 0.5514(18) 0.103(5) Uani 0.518(10) 1 d D U P A 1
F13 F 0.32018(18) 0.4166(5) 0.7590(12) 0.083(4) Uani 0.518(10) 1 d D U P A 1
F14 F 0.30957(16) 0.4755(4) 0.6779(17) 0.087(4) Uani 0.518(10) 1 d D U P A 1
F15 F 0.30241(15) 0.4098(5) 0.6120(16) 0.078(4) Uani 0.518(10) 1 d D U P A 1
F16 F 0.3124(3) 0.4736(5) 0.417(3) 0.096(6) Uani 0.518(10) 1 d D U P A 1
F17 F 0.3157(2) 0.4023(5) 0.3842(16) 0.061(4) Uani 0.518(10) 1 d D U P A 1
F18 F 0.33544(17) 0.4490(6) 0.3442(14) 0.088(4) Uani 0.518(10) 1 d D U P A 1
F19 F 0.3255(2) 0.2048(5) 0.7509(15) 0.160(5) Uani 1 1 d D U . . .
F20 F 0.34850(18) 0.2389(6) 0.722(2) 0.180(6) Uani 1 1 d D U . . .
F21 F 0.3298(3) 0.2407(6) 0.5808(13) 0.175(6) Uani 1 1 d D U . . .
F22 F 0.3071(3) 0.3119(7) 0.6086(16) 0.179(6) Uani 1 1 d D U . . .
F23 F 0.3009(3) 0.3210(6) 0.8003(19) 0.187(7) Uani 1 1 d D U . . .
F24 F 0.2978(2) 0.2561(5) 0.716(2) 0.178(6) Uani 1 1 d D U . . .
F25 F 0.3229(2) 0.3167(4) 0.9615(18) 0.165(5) Uani 1 1 d D U . . .
F26 F 0.3147(2) 0.2473(5) 0.9405(15) 0.162(6) Uani 1 1 d D U . . .
F27 F 0.34065(17) 0.2635(5) 0.9374(19) 0.162(5) Uani 1 1 d D U . . .
F28 F 0.3737(3) 0.3026(7) 0.8085(19) 0.084(6) Uani 0.431(13) 1 d D U P B 1
F29 F 0.3651(2) 0.3330(8) 0.9773(17) 0.091(5) Uani 0.431(13) 1 d D U P B 1
F30 F 0.3909(2) 0.3251(8) 0.947(2) 0.083(6) Uani 0.431(13) 1 d D U P B 1
F31 F 0.3733(3) 0.4591(6) 0.8523(18) 0.082(5) Uani 0.431(13) 1 d D U P B 1
F32 F 0.38363(19) 0.4181(7) 0.9967(17) 0.092(5) Uani 0.431(13) 1 d D U P B 1
F33 F 0.35722(18) 0.4205(8) 0.9693(19) 0.088(5) Uani 0.431(13) 1 d D U P B 1
F34 F 0.3833(3) 0.4192(7) 0.647(2) 0.101(6) Uani 0.431(13) 1 d D U P B 1
F35 F 0.3938(3) 0.3530(6) 0.671(2) 0.091(5) Uani 0.431(13) 1 d D U P B 1
F36 F 0.4020(2) 0.4079(7) 0.785(2) 0.092(5) Uani 0.431(13) 1 d D U P B 1
F10A F 0.34306(16) 0.4827(8) 0.687(2) 0.076(5) Uani 0.482(10) 1 d D U P A 2
F11A F 0.3206(2) 0.5069(4) 0.6047(12) 0.079(4) Uani 0.482(10) 1 d D U P A 2
F12A F 0.3194(2) 0.4537(4) 0.7387(11) 0.073(4) Uani 0.482(10) 1 d D U P A 2
F13A F 0.30089(17) 0.4302(6) 0.5535(16) 0.083(4) Uani 0.482(10) 1 d D U P A 2
F14A F 0.3120(3) 0.3927(6) 0.4033(19) 0.075(5) Uani 0.482(10) 1 d D U P A 2
F15A F 0.3108(3) 0.4646(6) 0.396(2) 0.095(6) Uani 0.482(10) 1 d D U P A 2
F16A F 0.34196(17) 0.4929(3) 0.4125(16) 0.075(4) Uani 0.482(10) 1 d D U P A 2
F17A F 0.34208(19) 0.4264(4) 0.3372(11) 0.064(3) Uani 0.482(10) 1 d D U P A 2
F18A F 0.35853(17) 0.4426(5) 0.4859(19) 0.090(5) Uani 0.482(10) 1 d D U P A 2
F28A F 0.3545(2) 0.4175(7) 0.939(2) 0.116(6) Uani 0.569(13) 1 d D U P B 2
F29A F 0.3769(2) 0.3984(7) 1.0355(17) 0.104(5) Uani 0.569(13) 1 d D U P B 2
F30A F 0.3583(3) 0.3489(6) 0.9934(18) 0.109(5) Uani 0.569(13) 1 d D U P B 2
F31A F 0.3795(2) 0.4589(5) 0.816(2) 0.093(5) Uani 0.569(13) 1 d D U P B 2
F32A F 0.3917(2) 0.4178(7) 0.6822(14) 0.109(5) Uani 0.569(13) 1 d D U P B 2
F33A F 0.39977(18) 0.4167(6) 0.8711(18) 0.104(5) Uani 0.569(13) 1 d D U P B 2
F34A F 0.3945(3) 0.3363(7) 0.9163(17) 0.103(6) Uani 0.569(13) 1 d D U P B 2
F35A F 0.3931(3) 0.3321(6) 0.7187(16) 0.108(5) Uani 0.569(13) 1 d D U P B 2
F36A F 0.3756(3) 0.2960(7) 0.831(2) 0.102(6) Uani 0.569(13) 1 d D U P B 2
O1 O 0.35945(16) 0.3248(4) 0.5206(11) 0.088(3) Uani 1 1 d . U . . .
O2 O 0.33578(9) 0.3922(2) 0.5700(8) 0.0562(16) Uani 1 1 d . . . . .
O3 O 0.33619(13) 0.3146(4) 0.7200(14) 0.089(3) Uani 1 1 d . U . . .
O4 O 0.36158(12) 0.3787(3) 0.7389(8) 0.069(2) Uani 1 1 d . . . . .
N1 N 0.43545(8) 0.3272(3) 0.2173(8) 0.0493(16) Uani 1 1 d . . . . .
H1 H 0.432707 0.331470 0.307579 0.059 Uiso 1 1 calc R U . . .
N2 N 0.43332(8) 0.2259(3) 0.2816(8) 0.0489(17) Uani 1 1 d . . . . .
N3 N 0.45832(9) 0.2022(2) 0.3057(8) 0.0431(15) Uani 1 1 d . . . . .
N4 N 0.46712(8) 0.3210(2) 0.3694(6) 0.0375(12) Uani 1 1 d . . . . .
C1 C 0.43429(12) 0.3727(4) 0.1577(9) 0.057(2) Uani 1 1 d . . . . .
C2 C 0.41802(14) 0.3957(4) 0.1885(11) 0.068(3) Uani 1 1 d . . . . .
H2A H 0.409113 0.382504 0.137386 0.102 Uiso 1 1 calc R U . . .
H2B H 0.418911 0.428251 0.170987 0.102 Uiso 1 1 calc R U . . .
H2C H 0.415452 0.391131 0.277006 0.102 Uiso 1 1 calc R U . . .
C3 C 0.44822(15) 0.4023(3) 0.2100(12) 0.063(3) Uani 1 1 d . . . . .
H3A H 0.449463 0.396405 0.299530 0.095 Uiso 1 1 calc R U . . .
H3B H 0.445480 0.434404 0.196948 0.095 Uiso 1 1 calc R U . . .
H3C H 0.458685 0.395134 0.167143 0.095 Uiso 1 1 calc R U . . .
C4 C 0.43635(16) 0.3676(6) 0.0132(11) 0.074(3) Uani 1 1 d . . . . .
H4A H 0.446888 0.352149 -0.005001 0.111 Uiso 1 1 calc R U . . .
H4B H 0.436364 0.397713 -0.025685 0.111 Uiso 1 1 calc R U . . .
H4C H 0.427071 0.349651 -0.020134 0.111 Uiso 1 1 calc R U . . .
C5 C 0.42334(12) 0.2930(4) 0.1669(11) 0.062(3) Uani 1 1 d . . . . .
H5A H 0.412939 0.308836 0.142607 0.074 Uiso 1 1 calc R U . . .
H5B H 0.428102 0.278978 0.090944 0.074 Uiso 1 1 calc R U . . .
C6 C 0.41930(11) 0.2570(4) 0.2578(12) 0.064(3) Uani 1 1 d . . . . .
H6A H 0.415889 0.271227 0.337483 0.077 Uiso 1 1 calc R U . . .
H6B H 0.409724 0.239181 0.226124 0.077 Uiso 1 1 calc R U . . .
C7 C 0.44953(9) 0.2398(3) 0.2767(8) 0.0446(17) Uani 1 1 d . . . . .
C8 C 0.43255(13) 0.1798(4) 0.3198(11) 0.059(2) Uani 1 1 d . . . . .
H8 H 0.422785 0.162380 0.335019 0.071 Uiso 1 1 calc R U . . .
C9 C 0.44820(12) 0.1658(3) 0.3299(10) 0.0528(19) Uani 1 1 d . . . . .
H9 H 0.451751 0.135900 0.350218 0.063 Uiso 1 1 calc R U . . .
C10 C 0.47646(10) 0.2021(3) 0.3066(8) 0.0406(15) Uani 1 1 d . . . . .
C11 C 0.48428(11) 0.2094(3) 0.4190(8) 0.0438(16) Uani 1 1 d . . . . .
C12 C 0.50170(10) 0.2095(3) 0.4178(8) 0.0427(15) Uani 1 1 d . . . . .
H12 H 0.507550 0.213303 0.494151 0.051 Uiso 1 1 calc R U . . .
C13 C 0.51078(10) 0.2042(3) 0.3065(9) 0.0440(16) Uani 1 1 d . . . . .
C14 C 0.50225(10) 0.1963(3) 0.1965(9) 0.0445(16) Uani 1 1 d . . . . .
H14 H 0.508279 0.191483 0.121398 0.053 Uiso 1 1 calc R U . . .
C15 C 0.48479(10) 0.1953(3) 0.1948(8) 0.0429(15) Uani 1 1 d . . . . .
C16 C 0.47584(11) 0.1858(4) 0.0737(9) 0.053(2) Uani 1 1 d . . . . .
H16A H 0.464336 0.196829 0.079487 0.080 Uiso 1 1 calc R U . . .
H16B H 0.475806 0.153059 0.057812 0.080 Uiso 1 1 calc R U . . .
H16C H 0.481556 0.201479 0.005268 0.080 Uiso 1 1 calc R U . . .
C17 C 0.52958(12) 0.2064(4) 0.3097(10) 0.057(2) Uani 1 1 d . . . . .
H17A H 0.534071 0.194502 0.231164 0.085 Uiso 1 1 calc R U . . .
H17B H 0.533714 0.187992 0.379432 0.085 Uiso 1 1 calc R U . . .
H17C H 0.533139 0.237954 0.320675 0.085 Uiso 1 1 calc R U . . .
C18 C 0.47483(12) 0.2150(4) 0.5401(9) 0.0520(19) Uani 1 1 d . . . . .
H18A H 0.467438 0.241437 0.533971 0.078 Uiso 1 1 calc R U . . .
H18B H 0.482745 0.219641 0.608664 0.078 Uiso 1 1 calc R U . . .
H18C H 0.468196 0.187717 0.556290 0.078 Uiso 1 1 calc R U . . .
C19 C 0.45725(9) 0.3358(2) 0.4687(7) 0.0374(13) Uani 1 1 d . . . . .
C20 C 0.44230(10) 0.3172(3) 0.5136(8) 0.0406(14) Uani 1 1 d . . . . .
H20 H 0.437696 0.290475 0.478019 0.049 Uiso 1 1 calc R U . . .
C21 C 0.43443(11) 0.3396(3) 0.6128(8) 0.0471(17) Uani 1 1 d . . . . .
H21 H 0.424325 0.327635 0.645295 0.057 Uiso 1 1 calc R U . . .
C22 C 0.44103(15) 0.3785(3) 0.6644(9) 0.055(2) Uani 1 1 d . . . . .
H22 H 0.435215 0.393559 0.729632 0.067 Uiso 1 1 calc R U . . .
C23 C 0.45579(13) 0.3958(3) 0.6229(8) 0.0504(18) Uani 1 1 d . . . . .
H23 H 0.460220 0.422397 0.660428 0.060 Uiso 1 1 calc R U . . .
C24 C 0.46451(10) 0.3746(3) 0.5253(7) 0.0419(15) Uani 1 1 d . . . . .
C25 C 0.47979(11) 0.3834(3) 0.4584(9) 0.0488(18) Uani 1 1 d . . . . .
C26 C 0.49244(16) 0.4165(4) 0.4718(13) 0.071(3) Uani 1 1 d . . . . .
H26 H 0.491606 0.439521 0.533697 0.085 Uiso 1 1 calc R U . . .
C27 C 0.50572(16) 0.4148(5) 0.3945(13) 0.086(5) Uani 1 1 d D . . . .
H27 H 0.514247 0.436990 0.402393 0.103 Uiso 1 1 calc R U . . .
C28 C 0.50723(14) 0.3808(5) 0.3025(13) 0.081(4) Uani 1 1 d D . . . .
H28 H 0.516862 0.380129 0.250928 0.097 Uiso 1 1 calc R U . . .
C29 C 0.49467(11) 0.3476(4) 0.2855(11) 0.057(2) Uani 1 1 d . . . . .
H29 H 0.495361 0.324850 0.222963 0.069 Uiso 1 1 calc R U . . .
C30 C 0.48094(10) 0.3509(3) 0.3688(8) 0.0457(17) Uani 1 1 d . . . . .
C31 C 0.36456(18) 0.3067(5) 0.4218(17) 0.125(3) Uani 1 1 d D U . . .
C32 C 0.34993(14) 0.3019(5) 0.3316(13) 0.130(4) Uani 1 1 d D U . . .
C33 C 0.37048(16) 0.2595(4) 0.4643(13) 0.135(4) Uani 1 1 d D U . . .
C34 C 0.37888(16) 0.3313(5) 0.3577(15) 0.142(4) Uani 1 1 d D U . . .
C35 C 0.32998(10) 0.4334(3) 0.5486(8) 0.0621(17) Uani 1 1 d D U . . .
C36 C 0.34241(13) 0.4708(4) 0.5870(12) 0.066(3) Uani 0.518(10) 1 d D U P A 1
C37 C 0.31561(13) 0.4344(4) 0.6475(11) 0.072(3) Uani 0.518(10) 1 d D U P A 1
C38 C 0.32317(17) 0.4399(5) 0.4212(9) 0.071(3) Uani 0.518(10) 1 d D U P A 1
C39 C 0.3257(2) 0.2856(6) 0.7619(15) 0.153(4) Uani 1 1 d D U . . .
C40 C 0.33229(19) 0.2411(5) 0.7023(14) 0.162(4) Uani 1 1 d D U . . .
C41 C 0.30759(17) 0.2920(5) 0.7186(16) 0.164(4) Uani 1 1 d D U . . .
C42 C 0.32561(19) 0.2780(5) 0.9040(12) 0.157(4) Uani 1 1 d D U . . .
C43 C 0.37403(12) 0.3796(3) 0.8184(9) 0.077(2) Uani 1 1 d D U . . .
C44 C 0.3768(2) 0.3356(4) 0.8900(14) 0.080(3) Uani 0.431(13) 1 d D U P B 1
C45 C 0.37181(19) 0.4192(4) 0.9101(13) 0.081(3) Uani 0.431(13) 1 d D U P B 1
C46 C 0.38867(17) 0.3894(5) 0.7319(13) 0.085(4) Uani 0.431(13) 1 d D U P B 1
C36A C 0.32839(17) 0.4699(4) 0.6451(10) 0.066(3) Uani 0.482(10) 1 d D U P A 2
C37A C 0.31329(13) 0.4295(5) 0.4736(13) 0.073(3) Uani 0.482(10) 1 d D U P A 2
C38A C 0.34292(13) 0.4490(4) 0.4465(11) 0.070(3) Uani 0.482(10) 1 d D U P A 2
C44A C 0.36606(17) 0.3853(5) 0.9493(11) 0.090(3) Uani 0.569(13) 1 d D U P B 2
C45A C 0.38636(16) 0.4186(4) 0.7982(14) 0.089(3) Uani 0.569(13) 1 d D U P B 2
C46A C 0.38401(18) 0.3348(4) 0.8214(14) 0.087(3) Uani 0.569(13) 1 d D U P B 2
C48 C 0.4974(4) 0.4223(9) 0.797(4) 0.182(12) Uani 0.5 1 d D U P . .
H48 H 0.489267 0.412639 0.738501 0.218 Uiso 0.5 1 calc R U P . .
C50 C 0.5247(4) 0.4514(10) 0.848(6) 0.183(12) Uani 0.5 1 d D U P . .
H50 H 0.535356 0.461737 0.821767 0.220 Uiso 0.5 1 calc R U P . .
C52 C 0.5050(5) 0.4350(12) 1.011(4) 0.182(12) Uani 0.5 1 d D U P . .
H52 H 0.501909 0.433713 1.096788 0.219 Uiso 0.5 1 calc R U P . .
C47 C 0.4944(3) 0.4220(7) 0.921(4) 0.181(12) Uani 0.5 1 d D U P . .
C49 C 0.5134(5) 0.4378(11) 0.757(4) 0.183(12) Uani 0.5 1 d D U P . .
H49 H 0.516208 0.438728 0.671415 0.220 Uiso 0.5 1 calc R U P . .
C51 C 0.5210(4) 0.4505(13) 0.974(5) 0.183(12) Uani 0.5 1 d D U P . .
H51 H 0.529006 0.460077 1.034140 0.220 Uiso 0.5 1 calc R U P . .
F37 F 0.4806(4) 0.4086(10) 0.954(5) 0.175(12) Uani 0.5 1 d D U 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 N4 1.934(6) . ?
Ge1 C7 2.030(9) . ?
Ge1 N1 2.134(6) . ?
Al1 O2 1.700(6) . ?
Al1 O3 1.713(10) . ?
Al1 O4 1.723(7) . ?
Al1 O1 1.738(11) . ?
F1 C32 1.341(10) . ?
F2 C32 1.322(10) . ?
F3 C32 1.307(11) . ?
F4 C33 1.333(10) . ?
F5 C33 1.331(11) . ?
F6 C33 1.325(10) . ?
F7 C34 1.316(10) . ?
F8 C34 1.321(11) . ?
F9 C34 1.309(10) . ?
F10 C36 1.324(10) . ?
F11 C36 1.345(10) . ?
F12 C36 1.322(10) . ?
F13 C37 1.354(10) . ?
F14 C37 1.344(10) . ?
F15 C37 1.338(10) . ?
F16 C38 1.319(11) . ?
F17 C38 1.318(10) . ?
F18 C38 1.312(10) . ?
F19 C40 1.309(11) . ?
F20 C40 1.320(11) . ?
F21 C40 1.318(11) . ?
F22 C41 1.316(11) . ?
F23 C41 1.335(11) . ?
F24 C41 1.321(11) . ?
F25 C42 1.313(10) . ?
F26 C42 1.320(11) . ?
F27 C42 1.329(11) . ?
F28 C44 1.332(11) . ?
F29 C44 1.332(11) . ?
F30 C44 1.320(11) . ?
F31 C45 1.331(11) . ?
F32 C45 1.328(11) . ?
F33 C45 1.332(11) . ?
F34 C46 1.332(11) . ?
F35 C46 1.324(11) . ?
F36 C46 1.328(11) . ?
F10A C36A 1.316(10) . ?
F11A C36A 1.328(10) . ?
F12A C36A 1.325(10) . ?
F13A C37A 1.313(10) . ?
F14A C37A 1.324(10) . ?
F15A C37A 1.343(11) . ?
F16A C38A 1.344(10) . ?
F17A C38A 1.349(10) . ?
F18A C38A 1.335(10) . ?
F28A C44A 1.331(10) . ?
F29A C44A 1.325(11) . ?
F30A C44A 1.327(10) . ?
F31A C45A 1.322(10) . ?
F32A C45A 1.316(10) . ?
F33A C45A 1.330(10) . ?
F34A C46A 1.320(11) . ?
F35A C46A 1.322(11) . ?
F36A C46A 1.328(10) . ?
O1 C31 1.25(2) . ?
O2 C35 1.317(10) . ?
O3 C39 1.28(2) . ?
O4 C43 1.313(12) . ?
N1 C1 1.487(15) . ?
N1 C5 1.500(12) . ?
N2 C7 1.364(10) . ?
N2 C8 1.421(16) . ?
N2 C6 1.472(13) . ?
N3 C7 1.349(12) . ?
N3 C9 1.369(12) . ?
N3 C10 1.457(10) . ?
N4 C19 1.397(10) . ?
N4 C30 1.416(10) . ?
C1 C2 1.506(12) . ?
C1 C3 1.524(16) . ?
C1 C4 1.564(14) . ?
C5 C6 1.48(2) . ?
C8 C9 1.326(15) . ?
C10 C11 1.375(12) . ?
C10 C15 1.386(12) . ?
C11 C12 1.398(12) . ?
C11 C18 1.512(11) . ?
C12 C13 1.406(12) . ?
C13 C14 1.382(12) . ?
C13 C17 1.510(12) . ?
C14 C15 1.401(11) . ?
C15 C16 1.509(11) . ?
C19 C20 1.404(11) . ?
C19 C24 1.417(11) . ?
C20 C21 1.401(12) . ?
C21 C22 1.378(15) . ?
C22 C23 1.363(16) . ?
C23 C24 1.404(12) . ?
C24 C25 1.444(12) . ?
C25 C30 1.359(14) . ?
C25 C26 1.415(13) . ?
C26 C27 1.35(2) . ?
C27 C28 1.410(11) . ?
C28 C29 1.415(16) . ?
C29 C30 1.421(13) . ?
C31 C34 1.522(11) . ?
C31 C32 1.527(11) . ?
C31 C33 1.538(11) . ?
C35 C38 1.483(9) . ?
C35 C36A 1.498(9) . ?
C35 C36 1.542(9) . ?
C35 C37 1.566(9) . ?
C35 C37A 1.566(9) . ?
C35 C38A 1.577(9) . ?
C39 C41 1.536(11) . ?
C39 C42 1.539(11) . ?
C39 C40 1.548(11) . ?
C43 C44 1.522(10) . ?
C43 C46 1.525(10) . ?
C43 C45A 1.532(10) . ?
C43 C45 1.535(9) . ?
C43 C46A 1.544(10) . ?
C43 C44A 1.550(10) . ?
C48 C47 1.347(10) . ?
C48 C49 1.423(10) . ?
C50 C49 1.384(10) . ?
C50 C51 1.387(10) . ?
C52 C47 1.347(10) . ?
C52 C51 1.422(10) . ?
C47 F37 1.229(9) . ?

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
N4 Ge1 C7 96.0(3) . . ?
N4 Ge1 N1 95.9(3) . . ?
C7 Ge1 N1 87.6(3) . . ?
O2 Al1 O3 109.9(5) . . ?
O2 Al1 O4 108.5(4) . . ?
O3 Al1 O4 108.2(6) . . ?
O2 Al1 O1 108.9(5) . . ?
O3 Al1 O1 111.5(6) . . ?
O4 Al1 O1 109.7(5) . . ?
C31 O1 Al1 166.4(12) . . ?
C35 O2 Al1 156.5(7) . . ?
C39 O3 Al1 168.6(13) . . ?
C43 O4 Al1 153.8(7) . . ?
C1 N1 C5 114.2(8) . . ?
C1 N1 Ge1 113.9(6) . . ?
C5 N1 Ge1 107.9(5) . . ?
C7 N2 C8 109.8(8) . . ?
C7 N2 C6 122.5(9) . . ?
C8 N2 C6 127.6(8) . . ?
C7 N3 C9 112.1(7) . . ?
C7 N3 C10 121.7(7) . . ?
C9 N3 C10 126.3(7) . . ?
C19 N4 C30 104.6(6) . . ?
C19 N4 Ge1 127.7(5) . . ?
C30 N4 Ge1 117.0(5) . . ?
N1 C1 C2 111.3(10) . . ?
N1 C1 C3 108.1(7) . . ?
C2 C1 C3 107.5(9) . . ?
N1 C1 C4 109.3(9) . . ?
C2 C1 C4 110.6(8) . . ?
C3 C1 C4 110.0(11) . . ?
C6 C5 N1 112.8(9) . . ?
N2 C6 C5 113.1(8) . . ?
N3 C7 N2 104.1(8) . . ?
N3 C7 Ge1 124.2(6) . . ?
N2 C7 Ge1 130.6(7) . . ?
C9 C8 N2 106.2(9) . . ?
C8 C9 N3 107.7(9) . . ?
C11 C10 C15 124.0(8) . . ?
C11 C10 N3 117.5(8) . . ?
C15 C10 N3 118.5(7) . . ?
C10 C11 C12 116.7(8) . . ?
C10 C11 C18 122.7(8) . . ?
C12 C11 C18 120.6(8) . . ?
C11 C12 C13 121.7(8) . . ?
C14 C13 C12 119.0(7) . . ?
C14 C13 C17 121.4(8) . . ?
C12 C13 C17 119.6(8) . . ?
C13 C14 C15 120.7(8) . . ?
C10 C15 C14 117.9(8) . . ?
C10 C15 C16 122.7(7) . . ?
C14 C15 C16 119.4(8) . . ?
N4 C19 C20 128.5(7) . . ?
N4 C19 C24 110.2(7) . . ?
C20 C19 C24 121.3(7) . . ?
C21 C20 C19 117.5(7) . . ?
C22 C21 C20 121.4(8) . . ?
C23 C22 C21 120.9(8) . . ?
C22 C23 C24 120.7(8) . . ?
C23 C24 C19 118.1(8) . . ?
C23 C24 C25 135.5(8) . . ?
C19 C24 C25 106.4(7) . . ?
C30 C25 C26 120.5(10) . . ?
C30 C25 C24 106.4(7) . . ?
C26 C25 C24 133.1(11) . . ?
C27 C26 C25 118.6(13) . . ?
C26 C27 C28 121.6(11) . . ?
C29 C28 C27 121.2(11) . . ?
C28 C29 C30 115.2(11) . . ?
C25 C30 C29 122.9(9) . . ?
C25 C30 N4 112.4(7) . . ?
C29 C30 N4 124.6(9) . . ?
O1 C31 C34 115.2(14) . . ?
O1 C31 C32 108.8(13) . . ?
C34 C31 C32 109.8(10) . . ?
O1 C31 C33 103.5(13) . . ?
C34 C31 C33 109.3(10) . . ?
C32 C31 C33 110.0(10) . . ?
F3 C32 F2 108.6(10) . . ?
F3 C32 F1 107.7(11) . . ?
F2 C32 F1 104.7(9) . . ?
F3 C32 C31 110.2(13) . . ?
F2 C32 C31 113.2(12) . . ?
F1 C32 C31 112.1(12) . . ?
F6 C33 F5 105.8(10) . . ?
F6 C33 F4 106.1(10) . . ?
F5 C33 F4 106.5(10) . . ?
F6 C33 C31 112.6(13) . . ?
F5 C33 C31 112.0(11) . . ?
F4 C33 C31 113.3(12) . . ?
F9 C34 F7 108.5(10) . . ?
F9 C34 F8 108.3(11) . . ?
F7 C34 F8 108.3(11) . . ?
F9 C34 C31 109.0(11) . . ?
F7 C34 C31 111.3(14) . . ?
F8 C34 C31 111.2(13) . . ?
O2 C35 C38 114.1(9) . . ?
O2 C35 C36A 124.8(9) . . ?
O2 C35 C36 112.5(8) . . ?
C38 C35 C36 113.0(7) . . ?
O2 C35 C37 99.2(8) . . ?
C38 C35 C37 110.4(7) . . ?
C36 C35 C37 106.4(7) . . ?
O2 C35 C37A 108.9(8) . . ?
C36A C35 C37A 109.5(7) . . ?
O2 C35 C38A 99.0(8) . . ?
C36A C35 C38A 109.0(7) . . ?
C37A C35 C38A 103.2(7) . . ?
F12 C36 F10 108.1(10) . . ?
F12 C36 F11 106.4(10) . . ?
F10 C36 F11 103.9(9) . . ?
F12 C36 C35 112.3(11) . . ?
F10 C36 C35 111.5(10) . . ?
F11 C36 C35 114.1(10) . . ?
F15 C37 F14 105.7(9) . . ?
F15 C37 F13 104.9(9) . . ?
F14 C37 F13 103.3(9) . . ?
F15 C37 C35 112.4(10) . . ?
F14 C37 C35 116.5(10) . . ?
F13 C37 C35 113.0(10) . . ?
F18 C38 F17 108.9(10) . . ?
F18 C38 F16 108.4(10) . . ?
F17 C38 F16 108.9(11) . . ?
F18 C38 C35 109.2(11) . . ?
F17 C38 C35 109.5(12) . . ?
F16 C38 C35 111.9(15) . . ?
O3 C39 C41 115.7(13) . . ?
O3 C39 C42 116.4(14) . . ?
C41 C39 C42 108.2(10) . . ?
O3 C39 C40 101.2(13) . . ?
C41 C39 C40 107.7(10) . . ?
C42 C39 C40 106.7(9) . . ?
F19 C40 F21 108.7(11) . . ?
F19 C40 F20 107.6(11) . . ?
F21 C40 F20 108.2(11) . . ?
F19 C40 C39 112.7(12) . . ?
F21 C40 C39 111.3(14) . . ?
F20 C40 C39 108.2(13) . . ?
F22 C41 F24 108.6(11) . . ?
F22 C41 F23 107.0(11) . . ?
F24 C41 F23 106.7(11) . . ?
F22 C41 C39 110.6(14) . . ?
F24 C41 C39 118.2(14) . . ?
F23 C41 C39 105.1(14) . . ?
F25 C42 F26 110.3(11) . . ?
F25 C42 F27 107.5(10) . . ?
F26 C42 F27 107.8(11) . . ?
F25 C42 C39 109.8(14) . . ?
F26 C42 C39 113.2(12) . . ?
F27 C42 C39 108.0(13) . . ?
O4 C43 C44 115.0(10) . . ?
O4 C43 C46 101.3(10) . . ?
C44 C43 C46 110.7(8) . . ?
O4 C43 C45A 114.6(10) . . ?
O4 C43 C45 110.0(9) . . ?
C44 C43 C45 110.0(8) . . ?
C46 C43 C45 109.5(8) . . ?
O4 C43 C46A 113.0(9) . . ?
C45A C43 C46A 108.0(8) . . ?
O4 C43 C44A 106.0(9) . . ?
C45A C43 C44A 108.2(8) . . ?
C46A C43 C44A 106.8(8) . . ?
F30 C44 F28 107.1(10) . . ?
F30 C44 F29 105.8(10) . . ?
F28 C44 F29 106.4(11) . . ?
F30 C44 C43 123.9(15) . . ?
F28 C44 C43 105.2(14) . . ?
F29 C44 C43 107.3(14) . . ?
F32 C45 F33 107.2(10) . . ?
F32 C45 F31 106.5(11) . . ?
F33 C45 F31 105.8(10) . . ?
F32 C45 C43 110.2(12) . . ?
F33 C45 C43 115.4(15) . . ?
F31 C45 C43 111.2(13) . . ?
F35 C46 F36 106.9(11) . . ?
F35 C46 F34 107.2(11) . . ?
F36 C46 F34 106.2(11) . . ?
F35 C46 C43 112.9(15) . . ?
F36 C46 C43 116.2(15) . . ?
F34 C46 C43 107.0(16) . . ?
F10A C36A F12A 109.3(10) . . ?
F10A C36A F11A 107.5(10) . . ?
F12A C36A F11A 106.6(9) . . ?
F10A C36A C35 111.4(14) . . ?
F12A C36A C35 108.0(10) . . ?
F11A C36A C35 113.8(9) . . ?
F13A C37A F14A 108.9(10) . . ?
F13A C37A F15A 106.4(10) . . ?
F14A C37A F15A 105.4(11) . . ?
F13A C37A C35 108.2(11) . . ?
F14A C37A C35 114.7(14) . . ?
F15A C37A C35 112.8(16) . . ?
F18A C38A F16A 105.9(9) . . ?
F18A C38A F17A 104.6(10) . . ?
F16A C38A F17A 103.7(9) . . ?
F18A C38A C35 110.9(12) . . ?
F16A C38A C35 115.5(10) . . ?
F17A C38A C35 115.1(10) . . ?
F29A C44A F30A 107.0(10) . . ?
F29A C44A F28A 108.0(10) . . ?
F30A C44A F28A 106.2(10) . . ?
F29A C44A C43 113.1(13) . . ?
F30A C44A C43 115.3(12) . . ?
F28A C44A C43 107.0(14) . . ?
F32A C45A F31A 106.8(10) . . ?
F32A C45A F33A 106.8(10) . . ?
F31A C45A F33A 107.0(10) . . ?
F32A C45A C43 109.3(12) . . ?
F31A C45A C43 112.4(13) . . ?
F33A C45A C43 114.1(11) . . ?
F34A C46A F35A 107.1(11) . . ?
F34A C46A F36A 106.8(10) . . ?
F35A C46A F36A 107.1(10) . . ?
F34A C46A C43 108.5(13) . . ?
F35A C46A C43 108.6(12) . . ?
F36A C46A C43 118.3(15) . . ?
C47 C48 C49 117.2(8) . . ?
C49 C50 C51 122.5(9) . . ?
C47 C52 C51 117.4(8) . . ?
F37 C47 C52 116.7(10) . . ?
F37 C47 C48 116.9(10) . . ?
C52 C47 C48 126.4(8) . . ?
C50 C49 C48 118.4(8) . . ?
C50 C51 C52 118.1(8) . . ?

_refine_diff_density_max         1.405
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.166



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_069xzah19
_database_code_depnum_ccdc_archive 'CCDC 2005218'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;Australian National University
United Kingdom
;
_audit_update_record             
;
2020-05-22 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;
_audit_creation_date             2019-12-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C43 H42 Ge N2 P, Al C16 F36 O4'
_chemical_formula_sum            'C59 H42 Al F36 Ge N2 O4 P'
_chemical_formula_weight         1657.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         C50H50P1N1Ge1Al1O4F40
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.6853(7)
_cell_length_b                   18.4131(3)
_cell_length_c                   29.1049(8)
_cell_angle_alpha                90
_cell_angle_beta                 120.236(4)
_cell_angle_gamma                90
_cell_volume                     13281.4(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8817
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      74.9490
_cell_measurement_theta_min      3.8500
_shelx_estimated_absorpt_T_max   0.933
_shelx_estimated_absorpt_T_min   0.799
_exptl_absorpt_coefficient_mu    2.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            38546
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.164
_diffrn_reflns_theta_min         3.529
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  28.00   1.00   25.00    --  -42.66  38.00 -30.00   43
  2  ω    -22.00  21.00   1.00   25.00    --  -42.66  38.00 -60.00   43
  3  ω    -44.00  -4.00   1.00   25.00    --  -42.66  38.00-150.00   40
  4  ω    -10.00  27.00   1.00   25.00    --  -42.66  38.00  30.00   37
  5  ω     85.00 126.00   1.00   25.00    --   42.66 178.00  30.00   41
  6  ω     68.00 116.00   1.00   25.00    --   42.66 178.00-120.00   48
  7  ω     62.00  88.00   1.00   90.00    --  111.00 -95.00 150.00   26
  8  ω     88.00 119.00   1.00   90.00    --  111.00  45.00 -60.00   31
  9  ω     40.00  96.00   1.00   90.00    --  111.00 -45.00-180.00   56
 10  ω    140.00 166.00   1.00   90.00    --  111.00  15.00 -90.00   26
 11  ω    112.00 138.00   1.00   90.00    --  111.00 -61.00-180.00   26
 12  ω    126.00 175.00   1.00   90.00    --  111.00  45.00 -60.00   49
 13  ω     48.00  79.00   1.00   90.00    --  111.00 -30.00 -60.00   31
 14  ω     58.00  85.00   1.00   90.00    --  111.00 -61.00-180.00   27
 15  ω    128.00 154.00   1.00   90.00    --  111.00  30.00   0.00   26
 16  ω     88.00 116.00   1.00   90.00    --  111.00  30.00   0.00   28
 17  ω     69.00  95.00   1.00   90.00    --  111.00 -45.00 120.00   26
 18  ω    111.00 177.00   1.00   90.00    --  111.00 125.00 150.00   66
 19  ω     37.00  90.00   1.00   90.00    --  111.00 -30.00  30.00   53
 20  ω     67.00 107.00   1.00   90.00    --  111.00  15.00 -90.00   40
 21  ω     42.00  78.00   1.00   90.00    --  111.00-125.00-180.00   36
 22  ω     41.00  99.00   1.00   90.00    --  111.00 -77.00 150.00   58
 23  ω     38.00  82.00   1.00   90.00    --  111.00 -30.00 120.00   44
 24  ω     66.00 107.00   1.00   90.00    --  111.00  15.00 120.00   41
 25  ω     -6.00  -5.00   1.00   25.00    --  -42.66  38.00-150.00    1
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0055357000
_diffrn_orient_matrix_UB_12      -0.0742770000
_diffrn_orient_matrix_UB_13      0.0266887000
_diffrn_orient_matrix_UB_21      -0.0616667000
_diffrn_orient_matrix_UB_22      -0.0029597000
_diffrn_orient_matrix_UB_23      -0.0239602000
_diffrn_orient_matrix_UB_31      -0.0058724000
_diffrn_orient_matrix_UB_32      -0.0384204000
_diffrn_orient_matrix_UB_33      -0.0496135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10222
_reflns_number_total             13689
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1290
_refine_ls_number_reflns         13689
_refine_ls_number_restraints     1001
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0669
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1044P)²+35.1211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1958
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F8A-C47A = F9A-C47A = F7A-C47A = F3A-C45A = F2A-C45A = F1A-C45A = F6A-C46A =
 F4A-C46A = F5A-C46A
 1.33 with sigma of 0.008
 C59A-C56A = C57A-C56A = C58A-C56A
 1.53 with sigma of 0.008
 F36A-C59A = F34A-C59A = F35A-C59A = F28A-C57A = F30A-C57A = F29A-C57A = F31A-
 C58A = F33A-C58A = F32A-C58A
 1.33 with sigma of 0.008
 C45-F1 = C45-F2 = C45-F3
 1.33 with sigma of 0.008
 C47-C44 = C47A-C44 = C45-C44 = C45A-C44 = C46-C44 = C46A-C44
 1.53 with sigma of 0.008
 F8-C47 = F9-C47 = F7-C47 = F6-C46 = F4-C46 = F5-C46 = F1-C45 = F2-C45 = F3-C45
 1.33 with sigma of 0.008
 C58-C56 = C59-C56 = C57-C56
 1.53 with sigma of 0.008
 F36-C59 = F34-C59 = F35-C59 = F32-C58 = F33-C58 = F31-C58 = F30-C57 = F29-C57
 = F28-C57
 1.33 with sigma of 0.008
 O4-C56A = O4-C56
 1.33 with sigma of 0.008
 C53-C52 = C55-C52 = C54-C52
 1.53 with sigma of 0.008
 C55A-C52A = C54A-C52A = C53A-C52A
 1.53 with sigma of 0.008
 F26-C55 = F26A-C55A = F25A-C55A = F25-C55 = F27A-C55A = F27-C55 = F21-C53 =
 F19-C53 = F19A-C53A = F20A-C53A = F21A-C53A = F22A-C54A = F22-C54 = F23A-C54A =
  F23-C54 = F24A-C54A = F24-C54
 1.33 with sigma of 0.008
 F26A-F25A
 2.13 with sigma of 0.008
 F25A-F27A
 2.13 with sigma of 0.008
 F27A-F26A
 2.13 with sigma of 0.008
 F21A-F19A
 2.13 with sigma of 0.008
 F6A-F5A
 2.13 with sigma of 0.008
 F5A-F4A
 2.13 with sigma of 0.008
 F4A-F6A
 2.13 with sigma of 0.008
 F1A-F3A
 2.13 with sigma of 0.008
 F3A-F2A
 2.13 with sigma of 0.008
 F2A-F1A
 2.13 with sigma of 0.008
 F9A-F7A
 2.13 with sigma of 0.008
 F7A-F8A
 2.13 with sigma of 0.008
 F8A-F9A
 2.13 with sigma of 0.008
 C47A-C45A
 2.5 with sigma of 0.008
 C45A-C46A
 2.5 with sigma of 0.008
 C46A-C47A
 2.5 with sigma of 0.008
 C59A-C57A
 2.5 with sigma of 0.008
 C57A-C58A
 2.5 with sigma of 0.008
 C58A-C59A
 2.5 with sigma of 0.008
 F7-F8
 2.13 with sigma of 0.008
 F8-F9
 2.13 with sigma of 0.008
 F9-F7
 2.13 with sigma of 0.008
 F6-F4
 2.13 with sigma of 0.008
 F6-F5
 2.13 with sigma of 0.008
 F5-F4
 2.13 with sigma of 0.008
 C47-C45
 2.5 with sigma of 0.008
 C47-C46
 2.5 with sigma of 0.008
 C46-C45
 2.5 with sigma of 0.008
 C57-C59
 2.5 with sigma of 0.008
 C58-C59
 2.5 with sigma of 0.008
 C58-C57
 2.5 with sigma of 0.008
 F36-F35
 2.13 with sigma of 0.008
 F36-F34
 2.13 with sigma of 0.008
 F35-F34
 2.13 with sigma of 0.008
 F32A-F31A
 2.13 with sigma of 0.008
 F31A-F33A
 2.13 with sigma of 0.008
 F33A-F32A
 2.13 with sigma of 0.008
 F35A-F34A
 2.13 with sigma of 0.008
 F34A-F36A
 2.13 with sigma of 0.008
 F36A-F35A
 2.13 with sigma of 0.008
 F29A-F28A
 2.13 with sigma of 0.008
 F28A-F30A
 2.13 with sigma of 0.008
 F30A-F29A
 2.13 with sigma of 0.008
 F23A-F22A
 2.13 with sigma of 0.008
 F20A-F21A
 2.13 with sigma of 0.008
 F19A-F20A
 2.13 with sigma of 0.008
 C54A-C53A = C53A-C55A = C55A-C54A
 2.5 with sigma of 0.008
 C54-C53 = C53-C55 = C55-C54
 2.5 with sigma of 0.008
 F22A-F24A
 2.13 with sigma of 0.008
 F24A-F23A
 2.13 with sigma of 0.008
 F23A-F24A
 2.13 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
F9A \\sim F7A \\sim F8A \\sim F3A \\sim F2A \\sim F1A \\sim F5A \\sim F6A \\sim
F4A: within 10A with sigma of 0.005 and sigma for terminal atoms of 0.01
F21 \\sim F19 \\sim F20 \\sim F24 \\sim F22 \\sim F23 \\sim F26 \\sim F25 \\sim
F27: within 10A with sigma of 0.005 and sigma for terminal atoms of 0.01
F8 \\sim F9 \\sim F7 \\sim F3 \\sim F2 \\sim F1 \\sim F5 \\sim F6 \\sim F4:
within 10A with sigma of 0.005 and sigma for terminal atoms of 0.01
C45 \\sim C45A \\sim C46 \\sim C46A \\sim C47 \\sim C47A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
C47 \\sim C47A \\sim C45 \\sim C45A \\sim C44 \\sim C46 \\sim C46A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
C58A \\sim C56A \\sim C59A \\sim C57A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
F31A \\sim C58A \\sim F33A \\sim F32A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
F30A \\sim C57A \\sim F29A \\sim F28A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C59A \\sim F36A \\sim F35A \\sim F34A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C54 \\sim C52 \\sim C53 \\sim C55: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C53A \\sim C52A \\sim C55A \\sim C54A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C55A \\sim F26A \\sim F27A \\sim F25A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C54A \\sim F23A \\sim F22A \\sim F24A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
C53A \\sim F21A \\sim F20A \\sim F19A: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
4. Others
 Sof(F26A)=Sof(F25A)=Sof(F20A)=Sof(F27A)=Sof(F21A)=Sof(F19A)=Sof(F24A)=
 Sof(F22A)=Sof(F23A)=Sof(C55A)=Sof(C54A)=Sof(C53A)=Sof(C52A)=1-FVAR(1)
 Sof(F26)=Sof(F25)=Sof(C52)=Sof(F20)=Sof(F27)=Sof(F21)=Sof(F19)=Sof(F24)=
 Sof(F22)=Sof(F23)=Sof(C55)=Sof(C54)=Sof(C53)=FVAR(1)
 Sof(F7A)=Sof(F9A)=Sof(F8A)=Sof(C46A)=Sof(F5A)=Sof(F1A)=Sof(F6A)=Sof(C47A)=
 Sof(C45A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(F7)=Sof(F9)=Sof(F8)=Sof(C46)=Sof(F5)=Sof(F1)=Sof(F6)=Sof(C47)=Sof(C45)=
 Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2)
 Sof(F35A)=Sof(F36A)=Sof(F31A)=Sof(F34A)=Sof(F33A)=Sof(F32A)=Sof(C59A)=
 Sof(C56A)=Sof(F28A)=Sof(F29A)=Sof(F30A)=Sof(C57A)=Sof(C58A)=1-FVAR(3)
 Sof(F35)=Sof(F36)=Sof(F31)=Sof(F34)=Sof(F33)=Sof(F32)=Sof(C59)=Sof(C56)=
 Sof(F28)=Sof(F29)=Sof(F30)=Sof(C57)=Sof(C58)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C33(H33), C42(H42), C2(H2), C34(H34), C19(H19), C18(H18), C16(H16),
 C11(H11), C17(H17), C36(H36), C39(H39), C22(H22), C10(H10), C5(H5), C9(H9),
 C4(H4), C13(H13), C3(H3), C41(H41), C12(H12), C35(H35), C40(H40), C23(H23),
 C24(H24)
5.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C27(H27A,H27B,
 H27C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.33653(2) 0.54628(2) 0.33320(2) 0.02843(12) Uani 1 1 d . . . . .
P1 P 0.28019(3) 0.61844(4) 0.25154(4) 0.02925(19) Uani 1 1 d . . . . .
Al1 Al 0.13651(4) 0.49955(6) 0.41545(4) 0.0338(2) Uani 1 1 d . . . . .
O1 O 0.12490(13) 0.46788(19) 0.35485(12) 0.0508(8) Uani 1 1 d . . . . .
N2 N 0.34778(12) 0.45701(16) 0.30587(12) 0.0310(6) Uani 1 1 d . . . . .
O3 O 0.11143(16) 0.58431(18) 0.40962(13) 0.0592(9) Uani 1 1 d . . . . .
N1 N 0.40473(12) 0.59926(18) 0.33716(13) 0.0323(6) Uani 1 1 d . . . . .
F16 F 0.18581(13) 0.5439(3) 0.53529(13) 0.0872(12) Uani 1 1 d . . . . .
O2 O 0.20494(12) 0.5021(3) 0.45802(13) 0.0660(11) Uani 1 1 d . . . . .
C32 C 0.36975(14) 0.43891(19) 0.27367(15) 0.0327(7) Uani 1 1 d . . . . .
C43 C 0.35723(14) 0.39612(19) 0.33940(15) 0.0341(7) Uani 1 1 d . . . . .
F14 F 0.31540(13) 0.4840(3) 0.48695(16) 0.0938(13) Uani 1 1 d . . . . .
O4 O 0.10648(18) 0.4414(2) 0.43859(15) 0.0686(11) Uani 1 1 d D . . . .
F13 F 0.27604(17) 0.3996(3) 0.50507(17) 0.0965(12) Uani 1 1 d . . . . .
C15 C 0.25974(16) 0.7658(2) 0.25546(16) 0.0385(8) Uani 1 1 d . . . . .
H15 H 0.268594 0.772224 0.229075 0.046 Uiso 1 1 calc R . . . .
C38 C 0.38608(16) 0.3428(2) 0.32992(17) 0.0406(8) Uani 1 1 d . . . . .
C1 C 0.31675(16) 0.65139(19) 0.21995(16) 0.0351(7) Uani 1 1 d . . . . .
C14 C 0.26192(14) 0.69689(19) 0.27622(15) 0.0334(7) Uani 1 1 d . . . . .
F7 F 0.1111(3) 0.4077(5) 0.2361(3) 0.0797(18) Uani 0.501(5) 1 d D U P A 1
C33 C 0.36902(15) 0.4776(2) 0.23253(16) 0.0364(8) Uani 1 1 d . . . . .
H33 H 0.353027 0.523267 0.223179 0.044 Uiso 1 1 calc R . . . .
C8 C 0.21874(15) 0.5752(2) 0.20203(14) 0.0344(7) Uani 1 1 d . . . . .
C42 C 0.33968(17) 0.3852(2) 0.37569(16) 0.0428(9) Uani 1 1 d . . . . .
H42 H 0.320212 0.420576 0.381684 0.051 Uiso 1 1 calc R . . . .
F35 F 0.0100(3) 0.4086(3) 0.3530(3) 0.088(2) Uani 0.673(7) 1 d D . P B 1
F18 F 0.22860(17) 0.4439(3) 0.55997(15) 0.0974(13) Uani 1 1 d . . . . .
C37 C 0.39389(15) 0.3694(2) 0.28787(17) 0.0399(8) Uani 1 1 d . . . . .
F15 F 0.33295(14) 0.4668(3) 0.56739(15) 0.1033(15) Uani 1 1 d . . . . .
C2 C 0.2925(2) 0.6520(2) 0.16488(17) 0.0462(9) Uani 1 1 d . . . . .
H2 H 0.256289 0.639818 0.143808 0.055 Uiso 1 1 calc R . . . .
F9 F 0.0588(4) 0.4711(4) 0.2531(4) 0.084(2) Uani 0.501(5) 1 d D U P A 1
C34 C 0.39245(19) 0.4473(2) 0.20566(19) 0.0472(10) Uani 1 1 d . . . . .
H34 H 0.392173 0.472862 0.177975 0.057 Uiso 1 1 calc R . . . .
C20 C 0.44822(15) 0.5964(2) 0.39316(16) 0.0424(9) Uani 1 1 d . . . . .
C19 C 0.24874(17) 0.6878(2) 0.31596(18) 0.0423(9) Uani 1 1 d . . . . .
H19 H 0.250686 0.642054 0.330355 0.051 Uiso 1 1 calc R . . . .
C18 C 0.23280(19) 0.7471(2) 0.3338(2) 0.0498(10) Uani 1 1 d . . . . .
H18 H 0.223408 0.741074 0.359842 0.060 Uiso 1 1 calc R . . . .
F17 F 0.26934(15) 0.5428(3) 0.59568(14) 0.1111(17) Uani 1 1 d . . . . .
C6 C 0.37165(17) 0.66965(19) 0.25235(17) 0.0385(8) Uani 1 1 d . . . . .
C16 C 0.24436(18) 0.8242(2) 0.27429(18) 0.0462(10) Uani 1 1 d . . . . .
H16 H 0.243135 0.870309 0.260656 0.055 Uiso 1 1 calc R . . . .
C11 C 0.1256(2) 0.5048(3) 0.1292(2) 0.0613(13) Uani 1 1 d . . . . .
H11 H 0.094144 0.481045 0.104789 0.074 Uiso 1 1 calc R . . . .
F12 F 0.2626(2) 0.6122(3) 0.4581(2) 0.1246(19) Uani 1 1 d . . . . .
F8 F 0.0767(3) 0.3603(4) 0.2795(3) 0.0800(19) Uani 0.501(5) 1 d D U P A 1
F26 F -0.0155(3) 0.6599(4) 0.3273(3) 0.0843(17) Uani 0.580(6) 1 d D U P C 1
C21 C 0.49294(17) 0.5526(3) 0.4061(2) 0.0536(11) Uani 1 1 d . . . . .
C17 C 0.23080(18) 0.8152(2) 0.31302(19) 0.0468(10) Uani 1 1 d . . . . .
H17 H 0.220261 0.855066 0.325247 0.056 Uiso 1 1 calc R . . . .
C36 C 0.41741(19) 0.3398(3) 0.2598(2) 0.0542(11) Uani 1 1 d . . . . .
H36 H 0.433426 0.294172 0.268677 0.065 Uiso 1 1 calc R . . . .
C7 C 0.39869(16) 0.6729(2) 0.31187(17) 0.0379(8) Uani 1 1 d . . . . .
H7A H 0.377772 0.704112 0.321612 0.046 Uiso 1 1 calc R . . . .
H7B H 0.434122 0.694586 0.325898 0.046 Uiso 1 1 calc R . . . .
C39 C 0.3990(2) 0.2775(2) 0.3581(2) 0.0552(12) Uani 1 1 d . . . . .
H39 H 0.418578 0.241901 0.352480 0.066 Uiso 1 1 calc R . . . .
C22 C 0.5340(2) 0.5512(4) 0.4595(3) 0.0781(18) Uani 1 1 d . . . . .
H22 H 0.564231 0.522366 0.469732 0.094 Uiso 1 1 calc R . . . .
C10 C 0.1747(2) 0.4729(3) 0.1453(2) 0.0554(11) Uani 1 1 d . . . . .
H10 H 0.176536 0.428082 0.131606 0.066 Uiso 1 1 calc R . . . .
F25 F 0.0220(4) 0.5640(5) 0.3205(5) 0.100(2) Uani 0.580(6) 1 d D U P C 1
C5 C 0.4010(2) 0.6878(2) 0.2278(2) 0.0496(11) Uani 1 1 d . . . . .
H5 H 0.437273 0.700114 0.248403 0.060 Uiso 1 1 calc R . . . .
C26 C 0.49907(17) 0.5102(3) 0.3649(2) 0.0578(12) Uani 1 1 d . . . . .
H26 H 0.462737 0.495201 0.337523 0.069 Uiso 1 1 calc R . . . .
C9 C 0.22177(17) 0.5081(2) 0.18221(17) 0.0446(9) Uani 1 1 d . . . . .
H9 H 0.255172 0.486655 0.193519 0.054 Uiso 1 1 calc R . . . .
C4 C 0.3766(2) 0.6879(3) 0.1728(2) 0.0594(13) Uani 1 1 d . . . . .
H4 H 0.396873 0.699356 0.156922 0.071 Uiso 1 1 calc R . . . .
F10 F 0.2346(2) 0.6450(3) 0.5108(3) 0.1257(18) Uani 1 1 d . . . . .
C44 C 0.14293(17) 0.4539(2) 0.32182(18) 0.0571(10) Uani 1 1 d D U . . .
C13 C 0.16924(19) 0.6069(3) 0.1852(2) 0.0567(12) Uani 1 1 d . . . . .
H13 H 0.167141 0.652142 0.198257 0.068 Uiso 1 1 calc R . . . .
C3 C 0.3227(3) 0.6710(3) 0.1414(2) 0.0588(13) Uani 1 1 d . . . . .
H3 H 0.306488 0.672232 0.104573 0.071 Uiso 1 1 calc R . . . .
F36 F 0.0064(3) 0.3021(4) 0.3812(3) 0.100(2) Uani 0.673(7) 1 d D . P B 1
C41 C 0.3524(2) 0.3194(3) 0.40244(19) 0.0566(12) Uani 1 1 d . . . . .
H41 H 0.340716 0.310214 0.426412 0.068 Uiso 1 1 calc R . . . .
C12 C 0.1225(2) 0.5709(3) 0.1488(2) 0.0733(17) Uani 1 1 d . . . . .
H12 H 0.088966 0.591949 0.137669 0.088 Uiso 1 1 calc R . . . .
C46 C 0.1933(2) 0.4119(4) 0.3391(3) 0.0674(18) Uani 0.501(5) 1 d D U P A 1
C35 C 0.4166(2) 0.3787(3) 0.2194(2) 0.0580(12) Uani 1 1 d . . . . .
H35 H 0.432234 0.359336 0.200829 0.070 Uiso 1 1 calc R . . . .
F5 F 0.2336(3) 0.4524(4) 0.3722(3) 0.0860(17) Uani 0.501(5) 1 d D U P A 1
C25 C 0.4432(2) 0.6373(3) 0.43121(19) 0.0543(11) Uani 1 1 d . . . . .
C29 C 0.3945(2) 0.6828(3) 0.4200(2) 0.0544(12) Uani 1 1 d . . . . .
H29 H 0.366594 0.673578 0.382975 0.065 Uiso 1 1 calc R . . . .
C52 C 0.0758(3) 0.6358(4) 0.3961(2) 0.0477(16) Uani 0.580(6) 1 d D U P C 1
F11 F 0.31737(19) 0.6084(3) 0.5439(3) 0.135(2) Uani 1 1 d . . . . .
F20 F 0.1388(3) 0.7180(4) 0.3971(3) 0.0963(19) Uani 0.580(6) 1 d . U P C 1
F31 F 0.0852(4) 0.4188(6) 0.5151(3) 0.130(4) Uani 0.673(7) 1 d D . P B 1
F1 F 0.1753(3) 0.5753(4) 0.3463(2) 0.0693(15) Uani 0.501(5) 1 d D U P A 1
C28 C 0.5328(2) 0.4408(4) 0.3858(3) 0.0788(18) Uani 1 1 d . . . . .
H28A H 0.569522 0.453355 0.410808 0.118 Uiso 1 1 calc GR . . . .
H28B H 0.531288 0.414331 0.356735 0.118 Uiso 1 1 calc GR . . . .
H28C H 0.518587 0.411262 0.403162 0.118 Uiso 1 1 calc GR . . . .
F27 F 0.0522(3) 0.6654(5) 0.3112(3) 0.0952(18) Uani 0.580(6) 1 d D U P C 1
F6 F 0.1881(4) 0.3561(4) 0.3633(3) 0.090(2) Uani 0.501(5) 1 d D U P A 1
C40 C 0.3823(2) 0.2669(3) 0.3943(2) 0.0650(14) Uani 1 1 d . . . . .
H40 H 0.391154 0.223931 0.413692 0.078 Uiso 1 1 calc R . . . .
C47 C 0.0956(3) 0.4200(4) 0.2711(3) 0.062(2) Uani 0.501(5) 1 d D U P A 1
F34 F 0.0618(3) 0.3259(3) 0.3546(4) 0.112(3) Uani 0.673(7) 1 d D . P B 1
C23 C 0.5302(3) 0.5920(5) 0.4973(3) 0.093(2) Uani 1 1 d . . . . .
H23 H 0.558097 0.590935 0.532524 0.112 Uiso 1 1 calc R . . . .
F33 F 0.0404(3) 0.3226(5) 0.4838(3) 0.135(4) Uani 0.673(7) 1 d D . P B 1
F21 F 0.1298(4) 0.7167(5) 0.4653(3) 0.104(2) Uani 0.580(6) 1 d D U P C 1
F32 F 0.0045(2) 0.4190(4) 0.4422(3) 0.096(2) Uani 0.673(7) 1 d D . P B 1
C59 C 0.0385(3) 0.3539(4) 0.3806(2) 0.069(2) Uani 0.673(7) 1 d D . P B 1
C48 C 0.24728(18) 0.5209(4) 0.5056(2) 0.0626(14) Uani 1 1 d . . . . .
C56 C 0.0807(2) 0.3804(3) 0.4376(2) 0.0524(19) Uani 0.673(7) 1 d D . P B 1
C31 C 0.3712(3) 0.6602(4) 0.4551(2) 0.0712(16) Uani 1 1 d . . . . .
H31A H 0.360714 0.610021 0.448796 0.107 Uiso 1 1 calc GR . . . .
H31B H 0.340324 0.689605 0.446726 0.107 Uiso 1 1 calc GR . . . .
H31C H 0.398114 0.666731 0.491850 0.107 Uiso 1 1 calc GR . . . .
C51 C 0.2327(2) 0.5127(5) 0.5499(2) 0.0780(19) Uani 1 1 d . . . . .
C24 C 0.4858(2) 0.6339(4) 0.4835(2) 0.0807(19) Uani 1 1 d . . . . .
H24 H 0.483966 0.660741 0.509616 0.097 Uiso 1 1 calc R . . . .
C45 C 0.1500(3) 0.5325(3) 0.3041(3) 0.0626(18) Uani 0.501(5) 1 d D U P A 1
F19 F 0.0668(3) 0.7633(4) 0.3888(3) 0.103(2) Uani 0.580(6) 1 d D U P C 1
F28 F 0.1533(3) 0.3202(6) 0.5118(4) 0.139(4) Uani 0.673(7) 1 d D . P B 1
F24 F 0.0840(3) 0.6048(4) 0.4804(2) 0.0858(16) Uani 0.580(6) 1 d D U P C 1
F22 F 0.0219(3) 0.6811(4) 0.4325(3) 0.0876(17) Uani 0.580(6) 1 d D U P C 1
F2 F 0.1803(3) 0.5322(5) 0.2808(3) 0.0784(16) Uani 0.501(5) 1 d D U P A 1
C30 C 0.4071(3) 0.7647(3) 0.4250(3) 0.0753(18) Uani 1 1 d . . . . .
H30A H 0.436825 0.774896 0.459878 0.113 Uiso 1 1 calc GR . . . .
H30B H 0.375943 0.791449 0.419462 0.113 Uiso 1 1 calc GR . . . .
H30C H 0.416300 0.778746 0.398801 0.113 Uiso 1 1 calc GR . . . .
C50 C 0.2936(2) 0.4663(5) 0.5167(2) 0.0780(19) Uani 1 1 d . . . . .
F23 F 0.0148(2) 0.5672(4) 0.4122(3) 0.0872(17) Uani 0.580(6) 1 d D U P C 1
C27 C 0.5212(2) 0.5571(4) 0.3373(3) 0.0767(17) Uani 1 1 d . . . . .
H27A H 0.498381 0.598754 0.321869 0.115 Uiso 1 1 calc GR . . . .
H27B H 0.522247 0.529487 0.309883 0.115 Uiso 1 1 calc GR . . . .
H27C H 0.557024 0.572875 0.362792 0.115 Uiso 1 1 calc GR . . . .
F3 F 0.1048(3) 0.5681(4) 0.2701(3) 0.0796(17) Uani 0.501(5) 1 d D U P A 1
F4 F 0.2000(3) 0.3912(5) 0.2998(3) 0.0887(18) Uani 0.501(5) 1 d D U P A 1
F29 F 0.1601(3) 0.3269(4) 0.4471(5) 0.168(5) Uani 0.673(7) 1 d D . P B 1
F30 F 0.1051(3) 0.2511(4) 0.4512(5) 0.171(5) Uani 0.673(7) 1 d D . P B 1
C57 C 0.1227(3) 0.3185(4) 0.4607(4) 0.146(10) Uani 0.673(7) 1 d D . P B 1
C49 C 0.2662(3) 0.5969(5) 0.5048(4) 0.099(2) Uani 1 1 d . . . . .
C55 C 0.0317(3) 0.6317(4) 0.3383(2) 0.060(2) Uani 0.580(6) 1 d D U P C 1
C58 C 0.0520(3) 0.3860(4) 0.4699(2) 0.093(4) Uani 0.673(7) 1 d D . P B 1
C54 C 0.0492(3) 0.6230(4) 0.4312(2) 0.064(2) Uani 0.580(6) 1 d D U P C 1
C53 C 0.1027(3) 0.7103(3) 0.4115(3) 0.072(2) Uani 0.580(6) 1 d D U P C 1
F26A F 0.0073(6) 0.6919(7) 0.3140(6) 0.194(7) Uani 0.420(6) 1 d D U P C 2
F25A F 0.0132(6) 0.5761(7) 0.3214(7) 0.196(8) Uani 0.420(6) 1 d D U P C 2
F20A F 0.1638(6) 0.6682(8) 0.3946(6) 0.156(5) Uani 0.420(6) 1 d D U P C 2
F27A F 0.0667(7) 0.6350(9) 0.3043(6) 0.164(5) Uani 0.420(6) 1 d D U P C 2
F21A F 0.1482(6) 0.7230(9) 0.4501(5) 0.158(6) Uani 0.420(6) 1 d D U P C 2
F19A F 0.1071(6) 0.7549(8) 0.3688(6) 0.181(6) Uani 0.420(6) 1 d D U P C 2
F24A F 0.0833(5) 0.6627(8) 0.4699(4) 0.149(5) Uani 0.420(6) 1 d D U P C 2
F22A F 0.0387(5) 0.7419(5) 0.4092(5) 0.156(6) Uani 0.420(6) 1 d D U P C 2
F23A F 0.0053(4) 0.6367(8) 0.4045(7) 0.165(5) Uani 0.420(6) 1 d D U P C 2
C55A C 0.0412(5) 0.6364(7) 0.3314(4) 0.173(5) Uani 0.420(6) 1 d D U P C 2
C54A C 0.0506(4) 0.6720(6) 0.4185(5) 0.151(4) Uani 0.420(6) 1 d D U P C 2
C53A C 0.1250(4) 0.6982(8) 0.4004(5) 0.162(5) Uani 0.420(6) 1 d D U P C 2
F7A F 0.0996(3) 0.4367(4) 0.2243(3) 0.0699(16) Uani 0.499(5) 1 d D U P A 2
F9A F 0.0463(3) 0.4481(4) 0.2547(3) 0.0671(16) Uani 0.499(5) 1 d D U P A 2
F8A F 0.0930(4) 0.3532(3) 0.2713(3) 0.079(2) Uani 0.499(5) 1 d D U P A 2
C46A C 0.1832(3) 0.3876(3) 0.3523(3) 0.062(2) Uani 0.499(5) 1 d D U P A 2
F5A F 0.2335(2) 0.4067(4) 0.3916(3) 0.0713(15) Uani 0.499(5) 1 d D U P A 2
F1A F 0.2135(3) 0.5411(4) 0.3605(2) 0.0871(18) Uani 0.499(5) 1 d D U P A 2
F6A F 0.1671(3) 0.3426(3) 0.3789(3) 0.0729(16) Uani 0.499(5) 1 d D U P A 2
C47A C 0.0974(3) 0.4261(4) 0.2691(3) 0.062(2) Uani 0.499(5) 1 d D U P A 2
C45A C 0.1787(3) 0.5086(3) 0.3151(3) 0.0670(18) Uani 0.499(5) 1 d D U P A 2
F2A F 0.2082(3) 0.4793(4) 0.2964(3) 0.0823(16) Uani 0.499(5) 1 d D U P A 2
F3A F 0.1464(3) 0.5568(4) 0.2814(3) 0.092(2) Uani 0.499(5) 1 d D U P A 2
F4A F 0.1931(3) 0.3420(4) 0.3223(3) 0.0781(17) Uani 0.499(5) 1 d D U P A 2
F35A F 0.0277(7) 0.4182(9) 0.3520(8) 0.106(5) Uani 0.327(7) 1 d D U P B 2
F36A F -0.0086(5) 0.3464(10) 0.3822(6) 0.105(4) Uani 0.327(7) 1 d D U P B 2
F31A F 0.0802(5) 0.4843(9) 0.5067(5) 0.118(5) Uani 0.327(7) 1 d D U P B 2
F34A F 0.0631(7) 0.3144(9) 0.3815(8) 0.135(5) Uani 0.327(7) 1 d D U P B 2
F33A F 0.0252(6) 0.3959(9) 0.4863(6) 0.120(4) Uani 0.327(7) 1 d D U P B 2
F32A F 0.0125(5) 0.4775(10) 0.4283(5) 0.135(5) Uani 0.327(7) 1 d D U P B 2
C59A C 0.0380(5) 0.3697(8) 0.3894(4) 0.115(4) Uani 0.327(7) 1 d D U P B 2
C56A C 0.0768(5) 0.3939(6) 0.4457(5) 0.115(4) Uani 0.327(7) 1 d D U P B 2
F28A F 0.1347(7) 0.3531(10) 0.5316(5) 0.133(5) Uani 0.327(7) 1 d D U P B 2
F29A F 0.1413(8) 0.3027(12) 0.4687(9) 0.147(7) Uani 0.327(7) 1 d D U P B 2
F30A F 0.0716(7) 0.2827(10) 0.4754(6) 0.137(6) Uani 0.327(7) 1 d D U P B 2
C57A C 0.1077(5) 0.3314(7) 0.4816(5) 0.126(4) Uani 0.327(7) 1 d D U P B 2
C58A C 0.0492(5) 0.4390(7) 0.4685(5) 0.116(4) Uani 0.327(7) 1 d D U P B 2
C52A C 0.0805(5) 0.6437(8) 0.3910(5) 0.156(4) Uani 0.420(6) 1 d D U P C 2
H1 H 0.4140(16) 0.571(2) 0.3224(16) 0.026(10) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 P1 2.4815(10) . ?
Ge1 N2 1.923(3) . ?
Ge1 N1 2.137(3) . ?
P1 C1 1.812(4) . ?
P1 C14 1.805(4) . ?
P1 C8 1.806(4) . ?
Al1 O1 1.723(3) . ?
Al1 O3 1.691(3) . ?
Al1 O2 1.715(3) . ?
Al1 O4 1.711(3) . ?
O1 C44 1.326(5) . ?
N2 C32 1.407(5) . ?
N2 C43 1.420(5) . ?
O3 C52 1.301(7) . ?
O3 C52A 1.339(16) . ?
N1 C20 1.472(5) . ?
N1 C7 1.511(5) . ?
F16 C51 1.320(7) . ?
O2 C48 1.348(6) . ?
C32 C33 1.384(5) . ?
C32 C37 1.414(5) . ?
C43 C38 1.399(6) . ?
C43 C42 1.395(6) . ?
F14 C50 1.337(7) . ?
O4 C56 1.337(6) . ?
O4 C56A 1.306(8) . ?
F13 C50 1.307(9) . ?
C15 C14 1.392(5) . ?
C15 C16 1.377(6) . ?
C38 C37 1.437(6) . ?
C38 C39 1.395(6) . ?
C1 C2 1.389(6) . ?
C1 C6 1.410(6) . ?
C14 C19 1.396(6) . ?
F7 C47 1.321(7) . ?
C33 C34 1.380(6) . ?
C8 C9 1.384(6) . ?
C8 C13 1.377(6) . ?
C42 C41 1.385(6) . ?
F35 C59 1.292(6) . ?
F18 C51 1.318(9) . ?
C37 C36 1.405(6) . ?
F15 C50 1.333(7) . ?
C2 C3 1.389(7) . ?
F9 C47 1.309(7) . ?
C34 C35 1.398(7) . ?
C20 C21 1.397(7) . ?
C20 C25 1.405(7) . ?
C19 C18 1.382(6) . ?
C18 C17 1.381(6) . ?
F17 C51 1.333(7) . ?
C6 C7 1.501(6) . ?
C6 C5 1.393(6) . ?
C16 C17 1.375(7) . ?
C11 C10 1.372(8) . ?
C11 C12 1.367(8) . ?
F12 C49 1.339(10) . ?
F8 C47 1.303(6) . ?
F26 C55 1.332(6) . ?
C21 C22 1.401(7) . ?
C21 C26 1.513(8) . ?
C36 C35 1.367(8) . ?
C39 C40 1.374(8) . ?
C22 C23 1.381(11) . ?
C10 C9 1.391(6) . ?
F25 C55 1.325(7) . ?
C5 C4 1.386(8) . ?
C26 C28 1.531(7) . ?
C26 C27 1.519(8) . ?
C4 C3 1.380(8) . ?
F10 C49 1.341(10) . ?
C44 C46 1.487(6) . ?
C44 C47 1.547(6) . ?
C44 C45 1.582(6) . ?
C44 C46A 1.606(6) . ?
C44 C47A 1.519(6) . ?
C44 C45A 1.519(6) . ?
C13 C12 1.389(7) . ?
F36 C59 1.331(6) . ?
C41 C40 1.389(8) . ?
C46 F5 1.303(6) . ?
C46 F6 1.295(7) . ?
C46 F4 1.309(6) . ?
C25 C29 1.516(8) . ?
C25 C24 1.393(7) . ?
C29 C31 1.534(7) . ?
C29 C30 1.540(7) . ?
C52 C55 1.513(6) . ?
C52 C54 1.573(6) . ?
C52 C53 1.527(6) . ?
F11 C49 1.346(9) . ?
F20 C53 1.305(12) . ?
F31 C58 1.320(6) . ?
F1 C45 1.327(5) . ?
F27 C55 1.349(7) . ?
F34 C59 1.338(6) . ?
C23 C24 1.363(11) . ?
F33 C58 1.332(7) . ?
F21 C53 1.356(7) . ?
F32 C58 1.331(7) . ?
C59 C56 1.560(6) . ?
C48 C51 1.552(8) . ?
C48 C50 1.565(9) . ?
C48 C49 1.505(10) . ?
C56 C57 1.545(6) . ?
C56 C58 1.533(6) . ?
C45 F2 1.345(5) . ?
C45 F3 1.341(5) . ?
F19 C53 1.328(7) . ?
F28 C57 1.291(7) . ?
F24 C54 1.311(6) . ?
F22 C54 1.337(6) . ?
F23 C54 1.336(7) . ?
F29 C57 1.326(7) . ?
F30 C57 1.316(7) . ?
F26A C55A 1.323(8) . ?
F25A C55A 1.314(7) . ?
F20A C53A 1.326(8) . ?
F27A C55A 1.320(8) . ?
F21A C53A 1.330(8) . ?
F19A C53A 1.314(8) . ?
F24A C54A 1.318(8) . ?
F22A C54A 1.324(8) . ?
F23A C54A 1.320(8) . ?
C55A C52A 1.526(8) . ?
C54A C52A 1.530(8) . ?
C53A C52A 1.536(8) . ?
F7A C47A 1.350(7) . ?
F9A C47A 1.367(7) . ?
F8A C47A 1.352(7) . ?
C46A F5A 1.360(6) . ?
C46A F6A 1.364(7) . ?
C46A F4A 1.342(7) . ?
F1A C45A 1.331(6) . ?
C45A F2A 1.331(7) . ?
C45A F3A 1.302(7) . ?
F35A C59A 1.320(8) . ?
F36A C59A 1.317(8) . ?
F31A C58A 1.314(8) . ?
F34A C59A 1.331(8) . ?
F33A C58A 1.316(8) . ?
F32A C58A 1.318(8) . ?
C59A C56A 1.511(8) . ?
C56A C57A 1.507(7) . ?
C56A C58A 1.513(8) . ?
F28A C57A 1.321(8) . ?
F29A C57A 1.307(8) . ?
F30A C57A 1.313(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge1 P1 103.02(9) . . ?
N2 Ge1 N1 94.16(13) . . ?
N1 Ge1 P1 86.80(9) . . ?
C1 P1 Ge1 113.65(13) . . ?
C14 P1 Ge1 103.12(13) . . ?
C14 P1 C1 106.99(16) . . ?
C14 P1 C8 107.96(18) . . ?
C8 P1 Ge1 115.55(12) . . ?
C8 P1 C1 108.94(18) . . ?
O3 Al1 O1 110.88(16) . . ?
O3 Al1 O2 108.7(2) . . ?
O3 Al1 O4 110.1(2) . . ?
O2 Al1 O1 108.05(18) . . ?
O4 Al1 O1 108.36(19) . . ?
O4 Al1 O2 110.7(2) . . ?
C44 O1 Al1 149.6(3) . . ?
C32 N2 Ge1 134.6(2) . . ?
C32 N2 C43 106.0(3) . . ?
C43 N2 Ge1 113.8(2) . . ?
C52 O3 Al1 158.9(4) . . ?
C52A O3 Al1 163.0(6) . . ?
C20 N1 Ge1 106.6(2) . . ?
C20 N1 C7 113.3(3) . . ?
C7 N1 Ge1 120.4(2) . . ?
C48 O2 Al1 149.4(4) . . ?
N2 C32 C37 109.7(3) . . ?
C33 C32 N2 129.6(3) . . ?
C33 C32 C37 120.7(4) . . ?
C38 C43 N2 110.3(3) . . ?
C42 C43 N2 128.1(3) . . ?
C42 C43 C38 121.5(4) . . ?
C56 O4 Al1 154.2(4) . . ?
C56A O4 Al1 167.9(6) . . ?
C16 C15 C14 119.5(4) . . ?
C43 C38 C37 106.8(3) . . ?
C39 C38 C43 119.8(4) . . ?
C39 C38 C37 133.3(4) . . ?
C2 C1 P1 120.5(3) . . ?
C2 C1 C6 120.7(4) . . ?
C6 C1 P1 118.5(3) . . ?
C15 C14 P1 121.0(3) . . ?
C15 C14 C19 119.8(3) . . ?
C19 C14 P1 119.2(3) . . ?
C34 C33 C32 118.8(4) . . ?
C9 C8 P1 119.0(3) . . ?
C13 C8 P1 120.9(3) . . ?
C13 C8 C9 120.0(4) . . ?
C41 C42 C43 117.2(4) . . ?
C32 C37 C38 107.1(3) . . ?
C36 C37 C32 119.3(4) . . ?
C36 C37 C38 133.6(4) . . ?
C1 C2 C3 119.7(5) . . ?
C33 C34 C35 121.1(4) . . ?
C21 C20 N1 118.0(4) . . ?
C21 C20 C25 122.8(4) . . ?
C25 C20 N1 119.2(4) . . ?
C18 C19 C14 119.7(4) . . ?
C19 C18 C17 120.1(4) . . ?
C1 C6 C7 122.4(3) . . ?
C5 C6 C1 118.3(4) . . ?
C5 C6 C7 119.3(4) . . ?
C17 C16 C15 120.8(4) . . ?
C12 C11 C10 120.7(4) . . ?
C20 C21 C22 116.9(5) . . ?
C20 C21 C26 122.8(4) . . ?
C22 C21 C26 120.2(5) . . ?
C16 C17 C18 120.1(4) . . ?
C35 C36 C37 119.5(4) . . ?
C6 C7 N1 113.1(3) . . ?
C40 C39 C38 118.8(5) . . ?
C23 C22 C21 121.1(6) . . ?
C11 C10 C9 119.7(5) . . ?
C4 C5 C6 120.6(5) . . ?
C21 C26 C28 114.6(5) . . ?
C21 C26 C27 111.8(5) . . ?
C27 C26 C28 109.7(4) . . ?
C8 C9 C10 119.8(4) . . ?
C3 C4 C5 120.6(4) . . ?
O1 C44 C46 121.6(4) . . ?
O1 C44 C47 107.1(4) . . ?
O1 C44 C45 102.7(4) . . ?
O1 C44 C46A 100.4(4) . . ?
O1 C44 C47A 110.3(4) . . ?
O1 C44 C45A 120.0(4) . . ?
C46 C44 C47 110.5(4) . . ?
C46 C44 C45 108.9(4) . . ?
C47 C44 C45 104.6(4) . . ?
C47A C44 C46A 108.4(4) . . ?
C45A C44 C46A 103.3(4) . . ?
C45A C44 C47A 112.8(4) . . ?
C8 C13 C12 119.7(5) . . ?
C4 C3 C2 120.0(5) . . ?
C42 C41 C40 121.6(5) . . ?
C11 C12 C13 120.1(5) . . ?
F5 C46 C44 107.5(6) . . ?
F5 C46 F4 110.4(6) . . ?
F6 C46 C44 103.8(6) . . ?
F6 C46 F5 110.7(6) . . ?
F6 C46 F4 110.6(6) . . ?
F4 C46 C44 113.7(6) . . ?
C36 C35 C34 120.7(4) . . ?
C20 C25 C29 125.0(4) . . ?
C24 C25 C20 117.1(5) . . ?
C24 C25 C29 117.8(5) . . ?
C25 C29 C31 111.7(5) . . ?
C25 C29 C30 111.9(4) . . ?
C31 C29 C30 111.2(4) . . ?
O3 C52 C55 112.9(5) . . ?
O3 C52 C54 105.0(5) . . ?
O3 C52 C53 111.3(5) . . ?
C55 C52 C54 107.9(5) . . ?
C55 C52 C53 112.8(5) . . ?
C53 C52 C54 106.4(5) . . ?
C39 C40 C41 121.0(4) . . ?
F7 C47 C44 109.3(6) . . ?
F9 C47 F7 109.3(6) . . ?
F9 C47 C44 103.7(6) . . ?
F8 C47 F7 109.5(6) . . ?
F8 C47 F9 110.7(6) . . ?
F8 C47 C44 114.2(7) . . ?
C24 C23 C22 120.6(5) . . ?
F35 C59 F36 109.9(6) . . ?
F35 C59 F34 106.8(6) . . ?
F35 C59 C56 109.1(6) . . ?
F36 C59 F34 106.0(5) . . ?
F36 C59 C56 112.4(6) . . ?
F34 C59 C56 112.5(6) . . ?
O2 C48 C51 110.3(4) . . ?
O2 C48 C50 106.2(5) . . ?
O2 C48 C49 111.6(5) . . ?
C51 C48 C50 108.8(5) . . ?
C49 C48 C51 110.8(6) . . ?
C49 C48 C50 108.9(5) . . ?
O4 C56 C59 114.2(5) . . ?
O4 C56 C57 108.0(5) . . ?
O4 C56 C58 113.1(5) . . ?
C57 C56 C59 104.4(5) . . ?
C58 C56 C59 107.7(4) . . ?
C58 C56 C57 109.0(5) . . ?
F16 C51 F17 107.7(6) . . ?
F16 C51 C48 110.3(5) . . ?
F18 C51 F16 107.4(5) . . ?
F18 C51 F17 106.9(5) . . ?
F18 C51 C48 111.8(6) . . ?
F17 C51 C48 112.5(5) . . ?
C23 C24 C25 121.5(6) . . ?
F1 C45 C44 110.0(5) . . ?
F1 C45 F2 106.1(6) . . ?
F1 C45 F3 105.5(6) . . ?
F2 C45 C44 112.5(5) . . ?
F3 C45 C44 116.9(5) . . ?
F3 C45 F2 105.0(7) . . ?
F14 C50 C48 109.6(5) . . ?
F13 C50 F14 107.9(6) . . ?
F13 C50 F15 107.0(6) . . ?
F13 C50 C48 112.0(5) . . ?
F15 C50 F14 107.7(5) . . ?
F15 C50 C48 112.5(6) . . ?
F28 C57 C56 114.3(7) . . ?
F28 C57 F29 99.1(9) . . ?
F28 C57 F30 103.3(9) . . ?
F29 C57 C56 110.9(6) . . ?
F30 C57 C56 118.1(6) . . ?
F30 C57 F29 109.2(8) . . ?
F12 C49 F10 106.3(7) . . ?
F12 C49 F11 108.8(7) . . ?
F12 C49 C48 111.5(7) . . ?
F10 C49 C48 109.7(6) . . ?
F11 C49 F10 107.9(8) . . ?
F11 C49 C48 112.4(7) . . ?
F26 C55 C52 115.3(6) . . ?
F26 C55 F27 111.7(7) . . ?
F25 C55 F26 106.6(7) . . ?
F25 C55 C52 112.1(8) . . ?
F25 C55 F27 105.8(8) . . ?
F27 C55 C52 105.1(6) . . ?
F31 C58 F33 105.2(7) . . ?
F31 C58 F32 113.5(8) . . ?
F31 C58 C56 107.6(5) . . ?
F33 C58 C56 115.0(6) . . ?
F32 C58 F33 104.4(7) . . ?
F32 C58 C56 111.2(5) . . ?
F24 C54 C52 113.3(6) . . ?
F24 C54 F22 108.1(6) . . ?
F24 C54 F23 104.7(7) . . ?
F22 C54 C52 112.4(6) . . ?
F22 C54 F23 107.8(7) . . ?
F23 C54 C52 110.1(5) . . ?
F20 C53 C52 111.5(6) . . ?
F20 C53 F21 105.9(7) . . ?
F20 C53 F19 107.6(8) . . ?
F21 C53 C52 109.1(7) . . ?
F19 C53 C52 111.3(6) . . ?
F19 C53 F21 111.2(8) . . ?
F26A C55A C52A 110.3(10) . . ?
F25A C55A F26A 108.6(8) . . ?
F25A C55A F27A 108.1(8) . . ?
F25A C55A C52A 110.3(11) . . ?
F27A C55A F26A 108.0(8) . . ?
F27A C55A C52A 111.4(10) . . ?
F24A C54A F22A 108.7(8) . . ?
F24A C54A F23A 108.3(7) . . ?
F24A C54A C52A 106.5(10) . . ?
F22A C54A C52A 112.2(9) . . ?
F23A C54A F22A 107.7(8) . . ?
F23A C54A C52A 113.4(10) . . ?
F20A C53A F21A 106.8(8) . . ?
F20A C53A C52A 112.3(11) . . ?
F21A C53A C52A 109.5(10) . . ?
F19A C53A F20A 107.3(8) . . ?
F19A C53A F21A 107.1(8) . . ?
F19A C53A C52A 113.4(12) . . ?
F5A C46A C44 115.6(6) . . ?
F5A C46A F6A 101.5(5) . . ?
F6A C46A C44 114.9(5) . . ?
F4A C46A C44 116.4(6) . . ?
F4A C46A F5A 103.1(5) . . ?
F4A C46A F6A 103.4(5) . . ?
F7A C47A C44 119.5(6) . . ?
F7A C47A F9A 103.1(5) . . ?
F7A C47A F8A 103.9(6) . . ?
F9A C47A C44 116.9(7) . . ?
F8A C47A C44 109.9(6) . . ?
F8A C47A F9A 101.4(5) . . ?
F1A C45A C44 112.9(6) . . ?
F2A C45A C44 113.2(5) . . ?
F2A C45A F1A 105.9(6) . . ?
F3A C45A C44 106.2(6) . . ?
F3A C45A F1A 109.6(6) . . ?
F3A C45A F2A 109.0(6) . . ?
F35A C59A F34A 107.0(8) . . ?
F35A C59A C56A 115.5(13) . . ?
F36A C59A F35A 107.4(8) . . ?
F36A C59A F34A 108.4(8) . . ?
F36A C59A C56A 113.8(10) . . ?
F34A C59A C56A 104.3(11) . . ?
O4 C56A C59A 102.1(9) . . ?
O4 C56A C57A 114.7(10) . . ?
O4 C56A C58A 103.2(9) . . ?
C59A C56A C58A 112.0(7) . . ?
C57A C56A C59A 112.4(7) . . ?
C57A C56A C58A 111.8(7) . . ?
F28A C57A C56A 110.3(11) . . ?
F29A C57A C56A 111.9(13) . . ?
F29A C57A F28A 109.4(8) . . ?
F29A C57A F30A 109.1(8) . . ?
F30A C57A C56A 106.2(10) . . ?
F30A C57A F28A 109.9(8) . . ?
F31A C58A F33A 108.3(8) . . ?
F31A C58A F32A 107.9(8) . . ?
F31A C58A C56A 116.0(11) . . ?
F33A C58A F32A 109.4(8) . . ?
F33A C58A C56A 109.6(9) . . ?
F32A C58A C56A 105.5(10) . . ?
O3 C52A C55A 110.4(10) . . ?
O3 C52A C54A 119.8(11) . . ?
O3 C52A C53A 98.1(10) . . ?
C55A C52A C54A 109.6(8) . . ?
C55A C52A C53A 109.5(8) . . ?
C54A C52A C53A 108.6(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.874
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_147xzjh18_a
_database_code_depnum_ccdc_archive 'CCDC 1952095'
loop_
_audit_author_name
_audit_author_address
'Jamie Hicks'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2019-09-07 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H52 Br Ge2 N6, C16 Al F36 O4'
_chemical_formula_sum            'C52 H52 Al Br F36 Ge2 N6 O4'
_chemical_formula_weight         1761.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.06330(10)
_cell_length_b                   18.7791(2)
_cell_length_c                   18.8201(2)
_cell_angle_alpha                61.9680(10)
_cell_angle_beta                 80.5190(10)
_cell_angle_gamma                80.4240(10)
_cell_volume                     3386.38(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    87305
_cell_measurement_theta_min      4.0350
_cell_measurement_theta_max      76.2760

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_F_000             1748
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    3.265
_shelx_estimated_absorpt_T_min   0.591
_shelx_estimated_absorpt_T_max   0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_reflns_number            171625
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.073
_diffrn_reflns_theta_max         76.443
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14100
_reflns_number_gt                13008
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²+2.4444P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14100
_refine_ls_number_parameters     1107
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.046
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.45541(2) 0.22441(2) 0.83031(2) 0.03599(5) Uani 1 1 d . . . . .
Ge1 Ge 0.62176(2) 0.25760(2) 0.90305(2) 0.02232(5) Uani 1 1 d . . . . .
Ge2 Ge 0.45416(2) 0.33277(2) 0.67040(2) 0.02388(5) Uani 1 1 d . . . . .
Al1 Al 0.91734(4) 0.18510(2) 0.26839(3) 0.01750(9) Uani 1 1 d . . . . .
F1 F 0.7150(3) 0.12984(18) 0.47909(19) 0.0687(8) Uani 0.732(4) 1 d D . P A 1
F2 F 0.6761(6) 0.0136(3) 0.4996(3) 0.0695(14) Uani 0.732(4) 1 d D . P A 1
F3 F 0.8527(4) 0.0555(4) 0.4437(4) 0.0472(15) Uani 0.732(4) 1 d D . P A 1
F5A F 0.567(2) 0.2319(7) 0.3544(11) 0.063(5) Uani 0.268(4) 1 d D . P A 2
F6A F 0.5049(11) 0.1220(11) 0.4502(7) 0.065(4) Uani 0.268(4) 1 d D . P A 2
F7 F 0.5757(3) 0.0123(2) 0.3745(3) 0.0618(11) Uani 0.732(4) 1 d D . P A 1
F8 F 0.7728(3) -0.0068(2) 0.3604(2) 0.0503(8) Uani 0.732(4) 1 d D . P A 1
F9 F 0.6768(6) 0.0807(4) 0.2598(3) 0.0601(19) Uani 0.732(4) 1 d D . P A 1
F10 F 1.24043(12) 0.10130(9) 0.28557(10) 0.0611(4) Uani 1 1 d . . . . .
F11 F 1.12128(14) 0.01936(8) 0.38071(8) 0.0581(4) Uani 1 1 d . . . . .
F12 F 1.26350(14) -0.02559(9) 0.31513(10) 0.0687(5) Uani 1 1 d . . . . .
F13 F 0.94868(12) -0.01375(7) 0.22353(8) 0.0448(3) Uani 1 1 d . . . . .
F14 F 1.02485(13) -0.07603(7) 0.33683(8) 0.0508(3) Uani 1 1 d . . . . .
F15 F 1.13790(12) -0.06485(7) 0.22831(8) 0.0511(3) Uani 1 1 d . . . . .
F16 F 1.26429(12) 0.06588(8) 0.15023(9) 0.0591(4) Uani 1 1 d . . . . .
F17 F 1.08637(13) 0.09848(8) 0.10581(7) 0.0524(3) Uani 1 1 d . . . . .
F18 F 1.15799(13) 0.17674(7) 0.13925(9) 0.0547(3) Uani 1 1 d . . . . .
F19 F 0.82620(14) 0.19792(6) 0.11216(8) 0.0524(3) Uani 1 1 d . . . . .
F20 F 0.96111(16) 0.26922(9) 0.02207(8) 0.0653(4) Uani 1 1 d . . . . .
F21 F 0.76882(15) 0.30773(8) 0.00886(8) 0.0608(4) Uani 1 1 d . . . . .
F22 F 1.04253(12) 0.37794(8) 0.05462(8) 0.0590(4) Uani 1 1 d . . . . .
F23 F 0.88905(14) 0.43646(7) -0.01670(7) 0.0552(3) Uani 1 1 d . . . . .
F24 F 0.89670(13) 0.44881(6) 0.09070(8) 0.0514(3) Uani 1 1 d . . . . .
F25 F 0.64574(11) 0.28847(8) 0.15770(8) 0.0512(3) Uani 1 1 d . . . . .
F26 F 0.66996(11) 0.41266(7) 0.07319(7) 0.0459(3) Uani 1 1 d . . . . .
F27 F 0.71243(11) 0.36399(8) 0.19584(7) 0.0460(3) Uani 1 1 d . . . . .
F28 F 0.82696(12) 0.30754(8) 0.34714(10) 0.0608(4) Uani 1 1 d . . . . .
F29 F 0.95566(16) 0.37972(7) 0.25662(8) 0.0612(4) Uani 1 1 d . . . . .
F30 F 0.94944(13) 0.36504(7) 0.37658(8) 0.0488(3) Uani 1 1 d . . . . .
F31 F 1.2445(3) 0.2083(4) 0.3574(5) 0.0891(16) Uani 0.735(12) 1 d D U P B 1
F32 F 1.1793(7) 0.2902(4) 0.2435(4) 0.0899(18) Uani 0.735(12) 1 d D . P B 1
F33 F 1.1890(7) 0.3327(4) 0.3304(5) 0.0855(19) Uani 0.735(12) 1 d D . P B 1
F34 F 0.9093(5) 0.1954(2) 0.4834(2) 0.0610(10) Uani 0.735(12) 1 d D . P B 1
F35 F 1.0762(6) 0.1246(2) 0.4738(2) 0.0699(13) Uani 0.735(12) 1 d D . P B 1
F36 F 1.0804(5) 0.2343(2) 0.4818(3) 0.0691(11) Uani 0.735(12) 1 d D . P B 1
O1 O 0.76591(10) 0.16872(7) 0.30648(7) 0.0274(2) Uani 1 1 d . . . . .
O2 O 0.98499(10) 0.10085(6) 0.25710(7) 0.0239(2) Uani 1 1 d . . . . .
O3 O 0.91428(10) 0.27355(6) 0.17807(6) 0.0221(2) Uani 1 1 d . . . . .
O4 O 1.00310(11) 0.19995(7) 0.32790(7) 0.0273(2) Uani 1 1 d . . . . .
N1 N 0.63041(13) 0.15618(8) 0.99208(8) 0.0239(3) Uani 1 1 d . . . . .
N2 N 0.44622(14) 0.26370(9) 1.04345(9) 0.0286(3) Uani 1 1 d . . . . .
N3 N 0.42270(13) 0.37676(8) 0.93630(9) 0.0271(3) Uani 1 1 d . . . . .
N4 N 0.60383(13) 0.29407(8) 0.63341(9) 0.0249(3) Uani 1 1 d . . . . .
N5 N 0.41425(14) 0.20643(8) 0.61958(9) 0.0272(3) Uani 1 1 d . . . . .
N6 N 0.24250(13) 0.25183(8) 0.66252(9) 0.0256(3) Uani 1 1 d . . . . .
C1 C 0.72330(16) 0.08917(10) 0.99167(11) 0.0272(3) Uani 1 1 d . . . . .
C2 C 0.8245(2) 0.12407(13) 0.92398(16) 0.0558(7) Uani 1 1 d . . . . .
H2A H 0.7902 0.1492 0.8718 0.084 Uiso 1 1 calc R U . . .
H2B H 0.8888 0.0806 0.9261 0.084 Uiso 1 1 calc R U . . .
H2C H 0.8601 0.1650 0.9303 0.084 Uiso 1 1 calc R U . . .
C3 C 0.6658(2) 0.02781(13) 0.97909(15) 0.0442(5) Uani 1 1 d . . . . .
H3A H 0.6026 0.0031 1.0238 0.066 Uiso 1 1 calc R U . . .
H3B H 0.7298 -0.0144 0.9775 0.066 Uiso 1 1 calc R U . . .
H3C H 0.6282 0.0555 0.9279 0.066 Uiso 1 1 calc R U . . .
C4 C 0.7818(2) 0.04562(12) 1.07161(14) 0.0479(5) Uani 1 1 d . . . . .
H4A H 0.8201 0.0846 1.0794 0.072 Uiso 1 1 calc R U . . .
H4B H 0.8446 0.0027 1.0703 0.072 Uiso 1 1 calc R U . . .
H4C H 0.7181 0.0217 1.1163 0.072 Uiso 1 1 calc R U . . .
C5 C 0.52363(17) 0.12992(10) 1.05216(11) 0.0303(4) Uani 1 1 d . . . . .
H5A H 0.5415 0.0723 1.0912 0.036 Uiso 1 1 calc R U . . .
H5B H 0.4519 0.1342 1.0246 0.036 Uiso 1 1 calc R U . . .
C6 C 0.49137(18) 0.18021(10) 1.09756(10) 0.0327(4) Uani 1 1 d . . . . .
H6A H 0.4272 0.1556 1.1427 0.039 Uiso 1 1 calc R U . . .
H6B H 0.5652 0.1805 1.1208 0.039 Uiso 1 1 calc R U . . .
C7 C 0.48156(15) 0.30086(10) 0.96402(10) 0.0239(3) Uani 1 1 d . . . . .
C8 C 0.3647(2) 0.31513(12) 1.06630(13) 0.0423(5) Uani 1 1 d . . . . .
H8 H 0.3266 0.3029 1.1193 0.051 Uiso 1 1 calc R U . . .
C9 C 0.34950(19) 0.38580(12) 0.99915(13) 0.0410(5) Uani 1 1 d . . . . .
H9 H 0.2982 0.4330 0.9956 0.049 Uiso 1 1 calc R U . . .
C10 C 0.43489(15) 0.43843(10) 0.85305(10) 0.0255(3) Uani 1 1 d . . . . .
C11 C 0.34981(17) 0.44702(11) 0.80184(12) 0.0339(4) Uani 1 1 d . . . . .
C12 C 0.3686(2) 0.50425(12) 0.72125(13) 0.0404(5) Uani 1 1 d . . . . .
H12 H 0.3126 0.5109 0.6848 0.048 Uiso 1 1 calc R U . . .
C13 C 0.4651(2) 0.55153(11) 0.69219(11) 0.0375(4) Uani 1 1 d . . . . .
C14 C 0.54393(18) 0.54378(10) 0.74631(11) 0.0315(4) Uani 1 1 d . . . . .
H14 H 0.6091 0.5775 0.7273 0.038 Uiso 1 1 calc R U . . .
C15 C 0.52965(15) 0.48782(10) 0.82773(10) 0.0253(3) Uani 1 1 d . . . . .
C16 C 0.61198(17) 0.48332(11) 0.88603(11) 0.0325(4) Uani 1 1 d . . . . .
H16A H 0.5622 0.4954 0.9279 0.049 Uiso 1 1 calc R U . . .
H16B H 0.6723 0.5229 0.8569 0.049 Uiso 1 1 calc R U . . .
H16C H 0.6552 0.4287 0.9113 0.049 Uiso 1 1 calc R U . . .
C17 C 0.4841(3) 0.61079(14) 0.60366(13) 0.0574(7) Uani 1 1 d . . . . .
H17A H 0.4891 0.5822 0.5709 0.086 Uiso 1 1 calc R U . . .
H17B H 0.5608 0.6354 0.5930 0.086 Uiso 1 1 calc R U . . .
H17C H 0.4148 0.6533 0.5895 0.086 Uiso 1 1 calc R U . . .
C18 C 0.2411(2) 0.39863(14) 0.83146(17) 0.0519(6) Uani 1 1 d . . . . .
H18A H 0.1773 0.4216 0.8598 0.078 Uiso 1 1 calc R U . . .
H18B H 0.2669 0.3423 0.8686 0.078 Uiso 1 1 calc R U . . .
H18C H 0.2082 0.4004 0.7853 0.078 Uiso 1 1 calc R U . . .
C19 C 0.71798(15) 0.33106(10) 0.62421(10) 0.0251(3) Uani 1 1 d . . . . .
C20 C 0.7870(2) 0.34950(13) 0.54098(12) 0.0422(5) Uani 1 1 d . . . . .
H20A H 0.8053 0.2995 0.5352 0.063 Uiso 1 1 calc R U . . .
H20B H 0.8642 0.3715 0.5357 0.063 Uiso 1 1 calc R U . . .
H20C H 0.7358 0.3893 0.4988 0.063 Uiso 1 1 calc R U . . .
C21 C 0.80151(18) 0.27523(12) 0.69059(12) 0.0370(4) Uani 1 1 d . . . . .
H21A H 0.7561 0.2628 0.7437 0.056 Uiso 1 1 calc R U . . .
H21B H 0.8738 0.3023 0.6843 0.056 Uiso 1 1 calc R U . . .
H21C H 0.8282 0.2248 0.6863 0.056 Uiso 1 1 calc R U . . .
C22 C 0.68455(17) 0.41056(11) 0.63004(12) 0.0342(4) Uani 1 1 d . . . . .
H22A H 0.6282 0.4467 0.5895 0.051 Uiso 1 1 calc R U . . .
H22B H 0.7595 0.4366 0.6201 0.051 Uiso 1 1 calc R U . . .
H22C H 0.6445 0.3994 0.6842 0.051 Uiso 1 1 calc R U . . .
C23 C 0.62432(16) 0.21038(10) 0.64481(11) 0.0279(3) Uani 1 1 d . . . . .
H23A H 0.6060 0.1731 0.7029 0.033 Uiso 1 1 calc R U . . .
H23B H 0.7123 0.1982 0.6292 0.033 Uiso 1 1 calc R U . . .
C24 C 0.54617(17) 0.19456(10) 0.59600(11) 0.0298(4) Uani 1 1 d . . . . .
H24A H 0.5644 0.2316 0.5379 0.036 Uiso 1 1 calc R U . . .
H24B H 0.5678 0.1382 0.6038 0.036 Uiso 1 1 calc R U . . .
C25 C 0.36555(15) 0.25399(9) 0.65459(10) 0.0229(3) Uani 1 1 d . . . . .
C26 C 0.32258(19) 0.17469(12) 0.60505(13) 0.0394(4) Uani 1 1 d . . . . .
H26 H 0.3336 0.1396 0.5805 0.047 Uiso 1 1 calc R U . . .
C27 C 0.21504(19) 0.20281(12) 0.63209(13) 0.0386(4) Uani 1 1 d . . . . .
H27 H 0.1353 0.1913 0.6306 0.046 Uiso 1 1 calc R U . . .
C28 C 0.15224(14) 0.29933(10) 0.69206(10) 0.0241(3) Uani 1 1 d . . . . .
C29 C 0.10289(15) 0.26355(10) 0.77244(10) 0.0265(3) Uani 1 1 d . . . . .
C30 C 0.01593(16) 0.31137(11) 0.79826(11) 0.0307(4) Uani 1 1 d . . . . .
H30 H -0.0191 0.2885 0.8530 0.037 Uiso 1 1 calc R U . . .
C31 C -0.02128(16) 0.39143(11) 0.74655(12) 0.0327(4) Uani 1 1 d . . . . .
C32 C 0.02987(16) 0.42408(10) 0.66676(12) 0.0323(4) Uani 1 1 d . . . . .
H32 H 0.0048 0.4788 0.6310 0.039 Uiso 1 1 calc R U . . .
C33 C 0.11666(16) 0.37919(10) 0.63746(11) 0.0289(3) Uani 1 1 d . . . . .
C34 C 0.1691(2) 0.41523(13) 0.55027(12) 0.0440(5) Uani 1 1 d . . . . .
H34A H 0.2562 0.4220 0.5466 0.066 Uiso 1 1 calc R U . . .
H34B H 0.1238 0.4682 0.5199 0.066 Uiso 1 1 calc R U . . .
H34C H 0.1615 0.3790 0.5274 0.066 Uiso 1 1 calc R U . . .
C35 C -0.1161(2) 0.44087(14) 0.77685(16) 0.0486(5) Uani 1 1 d . . . . .
H35A H -0.0859 0.4441 0.8213 0.073 Uiso 1 1 calc R U . . .
H35B H -0.1930 0.4151 0.7963 0.073 Uiso 1 1 calc R U . . .
H35C H -0.1310 0.4956 0.7327 0.073 Uiso 1 1 calc R U . . .
C36 C 0.13993(18) 0.17651(11) 0.82915(12) 0.0374(4) Uani 1 1 d . . . . .
H36A H 0.1057 0.1409 0.8144 0.056 Uiso 1 1 calc R U . . .
H36B H 0.1083 0.1656 0.8847 0.056 Uiso 1 1 calc R U . . .
H36C H 0.2300 0.1663 0.8253 0.056 Uiso 1 1 calc R U . . .
C37 C 0.68761(15) 0.11625(10) 0.36147(10) 0.0290(4) Uani 1 1 d D . . . .
C38 C 0.7329(3) 0.07790(17) 0.44764(15) 0.0442(8) Uani 0.732(4) 1 d D . P A 1
C39A C 0.6045(6) 0.1568(4) 0.4063(4) 0.050(2) Uani 0.268(4) 1 d D . P A 2
C40 C 0.6776(3) 0.05002(16) 0.33926(18) 0.0416(7) Uani 0.732(4) 1 d D . P A 1
C41 C 1.08756(15) 0.05546(9) 0.24666(10) 0.0252(3) Uani 1 1 d . . . . .
C42 C 1.1794(2) 0.03685(13) 0.30846(14) 0.0442(5) Uani 1 1 d . . . . .
C43 C 1.04891(19) -0.02578(10) 0.25857(12) 0.0347(4) Uani 1 1 d . . . . .
C44 C 1.15033(19) 0.09953(12) 0.15908(13) 0.0403(5) Uani 1 1 d . . . . .
C45 C 0.85412(16) 0.32010(9) 0.11183(9) 0.0247(3) Uani 1 1 d . . . . .
C46 C 0.8517(2) 0.27339(11) 0.06286(12) 0.0413(5) Uani 1 1 d . . . . .
C47 C 0.9217(2) 0.39676(11) 0.05918(12) 0.0386(4) Uani 1 1 d . . . . .
C48 C 0.71845(18) 0.34674(11) 0.13519(11) 0.0341(4) Uani 1 1 d . . . . .
C49 C 1.03386(17) 0.24986(11) 0.35372(11) 0.0308(4) Uani 1 1 d . . . . .
C50 C 0.93994(19) 0.32636(11) 0.33426(12) 0.0361(4) Uani 1 1 d . . . . .
C51 C 1.1614(5) 0.2726(4) 0.3195(4) 0.0602(13) Uani 0.735(12) 1 d D . P B 1
C52 C 1.0267(6) 0.1993(3) 0.4501(3) 0.0431(14) Uani 0.735(12) 1 d D . P B 1
F4 F 0.5049(2) 0.1808(2) 0.29930(18) 0.0717(9) Uani 0.732(4) 1 d D . P A 1
F5 F 0.5701(9) 0.2355(3) 0.3608(4) 0.073(2) Uani 0.732(4) 1 d D . P A 1
C39 C 0.5611(3) 0.16509(18) 0.3632(2) 0.0508(9) Uani 0.732(4) 1 d D . P A 1
F6 F 0.4863(4) 0.1245(3) 0.4291(3) 0.0689(13) Uani 0.732(4) 1 d D . P A 1
F4A F 0.6717(7) 0.1618(5) 0.4554(4) 0.0571(19) Uani 0.268(4) 1 d D . P A 2
C40A C 0.6013(5) 0.0909(3) 0.3184(3) 0.0341(17) Uani 0.268(4) 1 d D . P A 2
C38A C 0.7531(5) 0.0349(3) 0.4206(3) 0.0361(18) Uani 0.268(4) 1 d D . P A 2
F8A F 0.5167(6) 0.1519(4) 0.2802(4) 0.0517(17) Uani 0.268(4) 1 d D . P A 2
F9A F 0.5386(8) 0.0281(5) 0.3702(6) 0.0435(19) Uani 0.268(4) 1 d D . P A 2
F7A F 0.6625(15) 0.0705(9) 0.2619(6) 0.042(2) Uani 0.268(4) 1 d D . P A 2
F1A F 0.7910(10) -0.0158(6) 0.3885(5) 0.046(2) Uani 0.268(4) 1 d D . P A 2
F3A F 0.6857(13) -0.0058(7) 0.4896(6) 0.051(3) Uani 0.268(4) 1 d D . P A 2
F2A F 0.8542(9) 0.0490(11) 0.4398(11) 0.048(5) Uani 0.268(4) 1 d D . P A 2
F31A F 1.2584(8) 0.2362(6) 0.3133(10) 0.069(3) Uani 0.265(12) 1 d D U P B 2
F33A F 1.1845(15) 0.3539(7) 0.3000(10) 0.058(3) Uani 0.265(12) 1 d D . P B 2
F32A F 1.1552(14) 0.3134(10) 0.2156(8) 0.061(3) Uani 0.265(12) 1 d D . P B 2
C51A C 1.1604(12) 0.2908(8) 0.2928(9) 0.0602(13) Uani 0.265(12) 1 d D . P B 2
F35A F 1.1378(14) 0.1425(6) 0.4475(8) 0.071(3) Uani 0.265(12) 1 d D U P B 2
F36A F 1.1328(13) 0.2515(6) 0.4563(8) 0.070(3) Uani 0.265(12) 1 d D U P B 2
F34A F 0.9686(15) 0.1950(6) 0.4826(6) 0.072(3) Uani 0.265(12) 1 d D U P B 2
C52A C 1.0716(12) 0.2126(6) 0.4321(8) 0.046(4) Uani 0.265(12) 1 d D . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ge2 2.7289(3) . ?
Br1 Ge1 2.7682(3) . ?
Ge1 N1 1.8538(13) . ?
Ge1 C7 2.0624(16) . ?
Ge2 N4 1.8574(14) . ?
Ge2 C25 2.0568(15) . ?
Al1 O4 1.7217(12) . ?
Al1 O2 1.7257(11) . ?
Al1 O1 1.7274(12) . ?
Al1 O3 1.7309(11) . ?
F1 C38 1.335(4) . ?
F2 C38 1.323(4) . ?
F3 C38 1.323(5) . ?
F5A C39A 1.326(7) . ?
F6A C39A 1.325(7) . ?
F7 C40 1.338(4) . ?
F8 C40 1.332(4) . ?
F9 C40 1.328(5) . ?
F10 C42 1.339(3) . ?
F11 C42 1.316(3) . ?
F12 C42 1.339(2) . ?
F13 C43 1.316(2) . ?
F14 C43 1.334(2) . ?
F15 C43 1.342(2) . ?
F16 C44 1.335(2) . ?
F17 C44 1.328(3) . ?
F18 C44 1.331(2) . ?
F19 C46 1.327(2) . ?
F20 C46 1.334(3) . ?
F21 C46 1.336(2) . ?
F22 C47 1.324(2) . ?
F23 C47 1.344(2) . ?
F24 C47 1.336(2) . ?
F25 C48 1.330(2) . ?
F26 C48 1.345(2) . ?
F27 C48 1.314(2) . ?
F28 C50 1.309(2) . ?
F29 C50 1.330(2) . ?
F30 C50 1.330(2) . ?
F31 C51 1.360(5) . ?
F32 C51 1.294(5) . ?
F33 C51 1.326(4) . ?
F34 C52 1.344(5) . ?
F35 C52 1.305(4) . ?
F36 C52 1.325(4) . ?
O1 C37 1.350(2) . ?
O2 C41 1.3473(18) . ?
O3 C45 1.3478(18) . ?
O4 C49 1.349(2) . ?
N1 C5 1.465(2) . ?
N1 C1 1.489(2) . ?
N2 C7 1.339(2) . ?
N2 C8 1.380(2) . ?
N2 C6 1.467(2) . ?
N3 C7 1.353(2) . ?
N3 C9 1.382(2) . ?
N3 C10 1.446(2) . ?
N4 C23 1.4656(19) . ?
N4 C19 1.488(2) . ?
N5 C25 1.341(2) . ?
N5 C26 1.380(2) . ?
N5 C24 1.466(2) . ?
N6 C25 1.350(2) . ?
N6 C27 1.383(2) . ?
N6 C28 1.445(2) . ?
C1 C2 1.515(3) . ?
C1 C3 1.529(2) . ?
C1 C4 1.529(3) . ?
C5 C6 1.515(2) . ?
C8 C9 1.344(3) . ?
C10 C15 1.389(2) . ?
C10 C11 1.394(2) . ?
C11 C12 1.392(3) . ?
C11 C18 1.500(3) . ?
C12 C13 1.376(3) . ?
C13 C14 1.390(3) . ?
C13 C17 1.509(3) . ?
C14 C15 1.393(2) . ?
C15 C16 1.502(2) . ?
C19 C22 1.528(2) . ?
C19 C21 1.530(2) . ?
C19 C20 1.530(2) . ?
C23 C24 1.511(2) . ?
C26 C27 1.341(3) . ?
C28 C29 1.390(2) . ?
C28 C33 1.396(2) . ?
C29 C30 1.392(3) . ?
C29 C36 1.503(2) . ?
C30 C31 1.388(3) . ?
C31 C32 1.386(3) . ?
C31 C35 1.504(3) . ?
C32 C33 1.389(3) . ?
C33 C34 1.504(3) . ?
C37 C39A 1.501(5) . ?
C37 C40 1.511(3) . ?
C37 C39 1.545(3) . ?
C37 C38A 1.548(5) . ?
C37 C38 1.565(3) . ?
C37 C40A 1.602(5) . ?
C39A F4A 1.322(6) . ?
C41 C42 1.548(3) . ?
C41 C44 1.554(3) . ?
C41 C43 1.557(2) . ?
C45 C47 1.545(2) . ?
C45 C46 1.548(2) . ?
C45 C48 1.561(3) . ?
C49 C52A 1.405(12) . ?
C49 C51 1.494(6) . ?
C49 C50 1.553(3) . ?
C49 C52 1.599(5) . ?
C49 C51A 1.692(15) . ?
F4 C39 1.332(4) . ?
F5 C39 1.322(5) . ?
C39 F6 1.337(4) . ?
C40A F9A 1.338(7) . ?
C40A F7A 1.340(7) . ?
C40A F8A 1.340(6) . ?
C38A F3A 1.328(7) . ?
C38A F1A 1.332(7) . ?
C38A F2A 1.332(7) . ?
F31A C51A 1.331(8) . ?
F33A C51A 1.328(8) . ?
F32A C51A 1.318(8) . ?
F35A C52A 1.321(8) . ?
F36A C52A 1.334(8) . ?
F34A C52A 1.337(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ge2 Br1 Ge1 111.296(9) . . ?
N1 Ge1 C7 90.99(6) . . ?
N1 Ge1 Br1 95.64(4) . . ?
C7 Ge1 Br1 91.68(4) . . ?
N4 Ge2 C25 90.20(6) . . ?
N4 Ge2 Br1 97.92(4) . . ?
C25 Ge2 Br1 88.62(4) . . ?
O4 Al1 O2 108.44(6) . . ?
O4 Al1 O1 115.15(6) . . ?
O2 Al1 O1 107.01(6) . . ?
O4 Al1 O3 106.23(6) . . ?
O2 Al1 O3 113.40(6) . . ?
O1 Al1 O3 106.79(6) . . ?
C37 O1 Al1 146.55(11) . . ?
C41 O2 Al1 149.44(11) . . ?
C45 O3 Al1 145.67(11) . . ?
C49 O4 Al1 148.88(11) . . ?
C5 N1 C1 114.75(13) . . ?
C5 N1 Ge1 120.50(11) . . ?
C1 N1 Ge1 121.36(11) . . ?
C7 N2 C8 110.63(15) . . ?
C7 N2 C6 123.62(14) . . ?
C8 N2 C6 125.73(15) . . ?
C7 N3 C9 109.85(15) . . ?
C7 N3 C10 124.54(14) . . ?
C9 N3 C10 125.61(14) . . ?
C23 N4 C19 114.67(13) . . ?
C23 N4 Ge2 120.50(11) . . ?
C19 N4 Ge2 120.08(10) . . ?
C25 N5 C26 110.52(15) . . ?
C25 N5 C24 123.98(14) . . ?
C26 N5 C24 125.40(14) . . ?
C25 N6 C27 110.15(14) . . ?
C25 N6 C28 124.79(13) . . ?
C27 N6 C28 124.85(15) . . ?
N1 C1 C2 109.36(14) . . ?
N1 C1 C3 111.64(15) . . ?
C2 C1 C3 108.70(18) . . ?
N1 C1 C4 109.88(15) . . ?
C2 C1 C4 107.98(18) . . ?
C3 C1 C4 109.20(15) . . ?
N1 C5 C6 112.14(14) . . ?
N2 C6 C5 110.67(14) . . ?
N2 C7 N3 105.74(14) . . ?
N2 C7 Ge1 125.94(12) . . ?
N3 C7 Ge1 127.35(12) . . ?
C9 C8 N2 106.74(17) . . ?
C8 C9 N3 107.04(16) . . ?
C15 C10 C11 122.62(16) . . ?
C15 C10 N3 118.60(14) . . ?
C11 C10 N3 118.78(16) . . ?
C12 C11 C10 116.88(18) . . ?
C12 C11 C18 120.83(18) . . ?
C10 C11 C18 122.28(19) . . ?
C13 C12 C11 122.64(17) . . ?
C12 C13 C14 118.44(18) . . ?
C12 C13 C17 120.68(19) . . ?
C14 C13 C17 120.9(2) . . ?
C13 C14 C15 121.57(18) . . ?
C10 C15 C14 117.65(16) . . ?
C10 C15 C16 121.63(15) . . ?
C14 C15 C16 120.69(16) . . ?
N4 C19 C22 109.78(13) . . ?
N4 C19 C21 111.54(14) . . ?
C22 C19 C21 107.74(15) . . ?
N4 C19 C20 109.25(14) . . ?
C22 C19 C20 108.47(15) . . ?
C21 C19 C20 109.99(16) . . ?
N4 C23 C24 113.20(14) . . ?
N5 C24 C23 111.95(14) . . ?
N5 C25 N6 105.56(13) . . ?
N5 C25 Ge2 127.14(12) . . ?
N6 C25 Ge2 126.11(11) . . ?
C27 C26 N5 106.96(16) . . ?
C26 C27 N6 106.80(16) . . ?
C29 C28 C33 122.92(16) . . ?
C29 C28 N6 119.11(14) . . ?
C33 C28 N6 117.96(15) . . ?
C28 C29 C30 117.21(15) . . ?
C28 C29 C36 121.72(16) . . ?
C30 C29 C36 121.07(17) . . ?
C31 C30 C29 122.05(17) . . ?
C32 C31 C30 118.54(17) . . ?
C32 C31 C35 121.13(18) . . ?
C30 C31 C35 120.32(19) . . ?
C31 C32 C33 121.99(16) . . ?
C32 C33 C28 117.29(16) . . ?
C32 C33 C34 121.16(16) . . ?
C28 C33 C34 121.55(17) . . ?
O1 C37 C39A 109.1(3) . . ?
O1 C37 C40 110.56(16) . . ?
O1 C37 C39 107.49(16) . . ?
C40 C37 C39 110.8(2) . . ?
O1 C37 C38A 113.6(3) . . ?
C39A C37 C38A 111.2(3) . . ?
O1 C37 C38 110.16(16) . . ?
C40 C37 C38 109.74(18) . . ?
C39 C37 C38 108.00(19) . . ?
O1 C37 C40A 111.1(2) . . ?
C39A C37 C40A 107.1(3) . . ?
C38A C37 C40A 104.5(3) . . ?
F2 C38 F3 108.3(4) . . ?
F2 C38 F1 107.0(3) . . ?
F3 C38 F1 106.7(3) . . ?
F2 C38 C37 112.1(4) . . ?
F3 C38 C37 109.9(4) . . ?
F1 C38 C37 112.6(2) . . ?
F4A C39A F6A 107.6(6) . . ?
F4A C39A F5A 107.3(7) . . ?
F6A C39A F5A 107.3(8) . . ?
F4A C39A C37 107.0(5) . . ?
F6A C39A C37 117.9(9) . . ?
F5A C39A C37 109.3(13) . . ?
F9 C40 F8 107.1(3) . . ?
F9 C40 F7 107.8(4) . . ?
F8 C40 F7 106.8(3) . . ?
F9 C40 C37 110.2(4) . . ?
F8 C40 C37 111.7(3) . . ?
F7 C40 C37 113.1(3) . . ?
O2 C41 C42 111.46(14) . . ?
O2 C41 C44 110.04(13) . . ?
C42 C41 C44 109.95(16) . . ?
O2 C41 C43 108.07(14) . . ?
C42 C41 C43 109.10(14) . . ?
C44 C41 C43 108.14(14) . . ?
F11 C42 F10 108.08(17) . . ?
F11 C42 F12 107.88(19) . . ?
F10 C42 F12 107.27(18) . . ?
F11 C42 C41 110.89(17) . . ?
F10 C42 C41 110.24(17) . . ?
F12 C42 C41 112.30(16) . . ?
F13 C43 F14 107.11(17) . . ?
F13 C43 F15 107.99(15) . . ?
F14 C43 F15 106.96(14) . . ?
F13 C43 C41 111.44(14) . . ?
F14 C43 C41 111.16(15) . . ?
F15 C43 C41 111.94(16) . . ?
F17 C44 F18 107.65(18) . . ?
F17 C44 F16 107.46(17) . . ?
F18 C44 F16 107.52(17) . . ?
F17 C44 C41 111.24(16) . . ?
F18 C44 C41 110.34(15) . . ?
F16 C44 C41 112.42(17) . . ?
O3 C45 C47 108.19(14) . . ?
O3 C45 C46 110.62(13) . . ?
C47 C45 C46 109.77(15) . . ?
O3 C45 C48 111.25(14) . . ?
C47 C45 C48 108.66(14) . . ?
C46 C45 C48 108.32(15) . . ?
F19 C46 F20 107.32(16) . . ?
F19 C46 F21 107.96(18) . . ?
F20 C46 F21 106.99(17) . . ?
F19 C46 C45 110.33(15) . . ?
F20 C46 C45 110.95(18) . . ?
F21 C46 C45 113.06(15) . . ?
F22 C47 F24 107.64(17) . . ?
F22 C47 F23 107.64(17) . . ?
F24 C47 F23 107.17(15) . . ?
F22 C47 C45 110.91(15) . . ?
F24 C47 C45 110.78(16) . . ?
F23 C47 C45 112.49(16) . . ?
F27 C48 F25 107.54(17) . . ?
F27 C48 F26 107.76(15) . . ?
F25 C48 F26 106.96(15) . . ?
F27 C48 C45 110.71(15) . . ?
F25 C48 C45 111.57(15) . . ?
F26 C48 C45 112.07(15) . . ?
O4 C49 C52A 116.1(4) . . ?
O4 C49 C51 110.4(2) . . ?
O4 C49 C50 112.37(14) . . ?
C52A C49 C50 115.0(4) . . ?
C51 C49 C50 111.1(3) . . ?
O4 C49 C52 105.5(2) . . ?
C51 C49 C52 110.4(3) . . ?
C50 C49 C52 106.8(2) . . ?
O4 C49 C51A 105.8(4) . . ?
C52A C49 C51A 104.1(6) . . ?
C50 C49 C51A 101.5(4) . . ?
F28 C50 F29 106.00(17) . . ?
F28 C50 F30 108.82(17) . . ?
F29 C50 F30 106.60(15) . . ?
F28 C50 C49 110.84(15) . . ?
F29 C50 C49 111.09(16) . . ?
F30 C50 C49 113.15(16) . . ?
F32 C51 F33 110.4(4) . . ?
F32 C51 F31 106.4(4) . . ?
F33 C51 F31 105.9(4) . . ?
F32 C51 C49 111.0(4) . . ?
F33 C51 C49 113.3(4) . . ?
F31 C51 C49 109.5(4) . . ?
F35 C52 F36 109.1(3) . . ?
F35 C52 F34 106.6(4) . . ?
F36 C52 F34 105.9(3) . . ?
F35 C52 C49 112.3(3) . . ?
F36 C52 C49 111.3(3) . . ?
F34 C52 C49 111.2(3) . . ?
F5 C39 F4 107.2(3) . . ?
F5 C39 F6 107.4(4) . . ?
F4 C39 F6 107.0(3) . . ?
F5 C39 C37 112.8(5) . . ?
F4 C39 C37 109.8(3) . . ?
F6 C39 C37 112.3(3) . . ?
F9A C40A F7A 106.2(7) . . ?
F9A C40A F8A 106.0(5) . . ?
F7A C40A F8A 105.5(6) . . ?
F9A C40A C37 113.2(6) . . ?
F7A C40A C37 113.9(10) . . ?
F8A C40A C37 111.5(5) . . ?
F3A C38A F1A 106.6(6) . . ?
F3A C38A F2A 107.0(7) . . ?
F1A C38A F2A 105.8(6) . . ?
F3A C38A C37 114.6(7) . . ?
F1A C38A C37 113.0(5) . . ?
F2A C38A C37 109.3(9) . . ?
F32A C51A F33A 108.3(8) . . ?
F32A C51A F31A 105.1(8) . . ?
F33A C51A F31A 106.9(8) . . ?
F32A C51A C49 114.5(10) . . ?
F33A C51A C49 111.7(10) . . ?
F31A C51A C49 109.8(9) . . ?
F35A C52A F36A 106.1(8) . . ?
F35A C52A F34A 106.0(7) . . ?
F36A C52A F34A 105.5(7) . . ?
F35A C52A C49 111.1(8) . . ?
F36A C52A C49 121.1(8) . . ?
F34A C52A C49 105.9(8) . . ?

_refine_diff_density_max         0.656
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.048



