# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_Et3NH_2_H3L-Si
_database_code_depnum_ccdc_archive 'CCDC 2331262'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2024-02-06 deposited with the CCDC.	2024-07-14 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         'C21 H12 O12 Si, 2(C6 H16 N), 3(C3 H7 N O)'
_chemical_formula_sum            'C42 H65 N5 O15 Si'
_chemical_formula_weight         908.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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                   9.8788(4)
_cell_length_b                   14.7468(7)
_cell_length_c                   16.5789(8)
_cell_angle_alpha                95.373(4)
_cell_angle_beta                 90.577(4)
_cell_angle_gamma                97.219(4)
_cell_volume                     2384.97(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2482
_cell_measurement_theta_min      2.5600
_cell_measurement_theta_max      26.0030

_exptl_crystal_description       tablets
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.066
_exptl_absorpt_coefficient_mu    0.119
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            13899
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.353
_diffrn_reflns_theta_max         28.269
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             9373
_reflns_number_gt                4837
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _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, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          SQUEEZE
_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_number_reflns         9373
_refine_ls_number_parameters     505
_refine_ls_number_restraints     302
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.1042
_refine_ls_wR_factor_ref         0.3578
_refine_ls_wR_factor_gt          0.3102
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.144
_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
Si1 Si 0.53560(12) 0.30308(8) 0.29761(7) 0.0497(4) Uani 1 1 d . . . . .
O1 O 0.4247(3) 0.29242(19) 0.21101(18) 0.0550(8) Uani 1 1 d . . . . .
C2 C 0.3618(4) 0.3680(3) 0.2065(3) 0.0470(10) Uani 1 1 d . . . . .
C3 C 0.2733(4) 0.3822(3) 0.1462(3) 0.0537(11) Uani 1 1 d . . . . .
H3A H 0.250553 0.336500 0.102253 0.064 Uiso 1 1 calc R U . . .
C4 C 0.2167(4) 0.4652(3) 0.1502(3) 0.0504(10) Uani 1 1 d . . . . .
C5 C 0.2486(4) 0.5300(3) 0.2139(3) 0.0528(11) Uani 1 1 d . . . . .
H5A H 0.207323 0.584940 0.216655 0.063 Uiso 1 1 calc R U . . .
C6 C 0.3399(4) 0.5176(3) 0.2748(3) 0.0510(11) Uani 1 1 d . . . . .
H6A H 0.362846 0.563759 0.318376 0.061 Uiso 1 1 calc R U . . .
C7 C 0.3964(4) 0.4365(3) 0.2704(2) 0.0460(10) Uani 1 1 d . . . . .
O8 O 0.4867(3) 0.41458(18) 0.32416(17) 0.0511(7) Uani 1 1 d . . . . .
C9 C 0.1239(5) 0.4807(3) 0.0857(3) 0.0567(11) Uani 1 1 d . . . . .
O10 O 0.1080(3) 0.4236(2) 0.0218(2) 0.0710(10) Uani 1 1 d . . . . .
O11 O 0.0587(4) 0.5511(2) 0.0944(2) 0.0760(10) Uani 1 1 d . . . . .
O21 O 0.6364(3) 0.3163(2) 0.38758(18) 0.0571(8) Uani 1 1 d D . . . .
C22 C 0.5713(9) 0.2803(5) 0.4480(3) 0.059(3) Uani 0.643(15) 1 d DG U P A 1
C23 C 0.6275(8) 0.2838(6) 0.5256(4) 0.059(2) Uani 0.643(15) 1 d G U P A 1
H23A H 0.718672 0.311628 0.536693 0.070 Uiso 0.643(15) 1 calc R U P A 1
C24 C 0.5503(11) 0.2468(5) 0.5870(3) 0.071(3) Uani 0.643(15) 1 d DG U P A 1
C25 C 0.4169(11) 0.2061(5) 0.5708(4) 0.064(2) Uani 0.643(15) 1 d G U P A 1
H25A H 0.364158 0.180758 0.612772 0.077 Uiso 0.643(15) 1 calc R U P A 1
C26 C 0.3607(8) 0.2026(5) 0.4932(5) 0.074(3) Uani 0.643(15) 1 d G U P A 1
H26A H 0.269559 0.174775 0.482122 0.089 Uiso 0.643(15) 1 calc R U P A 1
C27 C 0.4379(9) 0.2396(5) 0.4318(3) 0.047(2) Uani 0.643(15) 1 d DG U P A 1
C29 C 0.5899(14) 0.2400(7) 0.6671(7) 0.081(3) Uani 0.643(15) 1 d D U P A 1
O30 O 0.7225(15) 0.2615(6) 0.6848(5) 0.110(3) Uani 0.643(15) 1 d D U P A 1
O31 O 0.4946(14) 0.2140(7) 0.7221(4) 0.116(3) Uani 0.643(15) 1 d D U P A 1
C22' C 0.5586(18) 0.2848(15) 0.4549(8) 0.062(6) Uiso 0.357(15) 1 d DG U P A 2
C23' C 0.5928(13) 0.2754(15) 0.5349(9) 0.084(6) Uiso 0.357(15) 1 d G U P A 2
H23B H 0.681640 0.298479 0.555886 0.101 Uiso 0.357(15) 1 calc R U P A 2
C24' C 0.4971(15) 0.2323(13) 0.5844(6) 0.059(4) Uiso 0.357(15) 1 d DG U P A 2
C25' C 0.3672(13) 0.1985(10) 0.5537(9) 0.066(5) Uiso 0.357(15) 1 d G U P A 2
H25B H 0.301756 0.169076 0.587500 0.079 Uiso 0.357(15) 1 calc R U P A 2
C26' C 0.3330(15) 0.2079(12) 0.4737(9) 0.060(4) Uiso 0.357(15) 1 d G U P A 2
H26B H 0.244190 0.184859 0.452721 0.072 Uiso 0.357(15) 1 calc R U P A 2
C27' C 0.429(2) 0.2510(15) 0.4242(6) 0.080(7) Uiso 0.357(15) 1 d DG U P A 2
C29' C 0.517(2) 0.230(2) 0.6676(12) 0.116(7) Uiso 0.357(15) 1 d D U P A 2
O30' O 0.652(2) 0.2496(16) 0.6906(10) 0.089(5) Uiso 0.357(15) 1 d D U P A 2
O31' O 0.4160(18) 0.1789(12) 0.7054(8) 0.104(5) Uiso 0.357(15) 1 d D U P A 2
O28 O 0.4015(3) 0.2450(2) 0.3501(2) 0.0597(8) Uani 1 1 d D . . . .
O51 O 0.5884(3) 0.19570(19) 0.26192(18) 0.0536(8) Uani 1 1 d . . . . .
C52 C 0.6931(4) 0.2083(3) 0.2091(3) 0.0550(11) Uani 1 1 d . . . . .
C53 C 0.7480(5) 0.1389(3) 0.1651(3) 0.0608(12) Uani 1 1 d . . . . .
H53A H 0.715564 0.076427 0.170791 0.073 Uiso 1 1 calc R U . . .
C54 C 0.8549(5) 0.1625(3) 0.1105(3) 0.0647(13) Uani 1 1 d . . . . .
C55 C 0.9030(6) 0.2529(3) 0.1061(3) 0.0750(15) Uani 1 1 d . . . . .
H55A H 0.976698 0.268568 0.071536 0.090 Uiso 1 1 calc R U . . .
C56 C 0.8469(5) 0.3218(3) 0.1509(3) 0.0707(14) Uani 1 1 d . . . . .
H56A H 0.880724 0.384342 0.146532 0.085 Uiso 1 1 calc R U . . .
C57 C 0.7434(5) 0.2999(3) 0.2011(3) 0.0581(12) Uani 1 1 d . . . . .
O58 O 0.6777(3) 0.3594(2) 0.24679(18) 0.0579(8) Uani 1 1 d . . . . .
C59 C 0.9185(6) 0.0907(4) 0.0648(4) 0.0798(16) Uani 1 1 d . . . . .
O60 O 0.8707(4) 0.0064(2) 0.0730(2) 0.0860(12) Uani 1 1 d . . . . .
O61 O 1.0128(5) 0.1117(3) 0.0166(3) 0.1056(16) Uani 1 1 d . . . . .
N70 N 0.8030(12) 0.5139(9) 0.3614(4) 0.100(4) Uani 0.686(7) 1 d D U P B 1
H70A H 0.748094 0.462067 0.344409 0.120 Uiso 0.686(7) 1 calc R U P B 1
C71 C 0.9402(10) 0.5033(7) 0.3293(7) 0.105(3) Uani 0.686(7) 1 d D U P B 1
H71A H 1.006514 0.554976 0.353329 0.126 Uiso 0.686(7) 1 calc R U P B 1
H71B H 0.937980 0.506236 0.269874 0.126 Uiso 0.686(7) 1 calc R U P B 1
C72 C 0.9891(18) 0.4107(13) 0.3483(9) 0.110(4) Uani 0.686(7) 1 d D U P B 1
H72A H 1.079932 0.406577 0.326008 0.165 Uiso 0.686(7) 1 calc R U P B 1
H72B H 0.993338 0.408021 0.407077 0.165 Uiso 0.686(7) 1 calc R U P B 1
H72C H 0.924815 0.359289 0.323636 0.165 Uiso 0.686(7) 1 calc R U P B 1
C73 C 0.8126(9) 0.5182(7) 0.4538(5) 0.098(3) Uani 0.686(7) 1 d D U P B 1
H73A H 0.842623 0.460790 0.469970 0.117 Uiso 0.686(7) 1 calc R U P B 1
H73B H 0.881093 0.570092 0.474764 0.117 Uiso 0.686(7) 1 calc R U P B 1
C74 C 0.6757(11) 0.5305(9) 0.4899(6) 0.088(3) Uani 0.686(7) 1 d D U P B 1
H74A H 0.683156 0.533198 0.549076 0.133 Uiso 0.686(7) 1 calc R U P B 1
H74B H 0.646687 0.587794 0.474407 0.133 Uiso 0.686(7) 1 calc R U P B 1
H74C H 0.608286 0.478688 0.469621 0.133 Uiso 0.686(7) 1 calc R U P B 1
C75 C 0.7383(11) 0.5919(8) 0.3331(7) 0.117(3) Uani 0.686(7) 1 d D U P B 1
H75A H 0.792282 0.650944 0.353178 0.140 Uiso 0.686(7) 1 calc R U P B 1
H75B H 0.644937 0.591216 0.354373 0.140 Uiso 0.686(7) 1 calc R U P B 1
C76 C 0.7323(13) 0.5815(8) 0.2366(7) 0.108(4) Uani 0.686(7) 1 d D U P B 1
H76A H 0.689946 0.632353 0.217320 0.162 Uiso 0.686(7) 1 calc R U P B 1
H76B H 0.825002 0.582651 0.215967 0.162 Uiso 0.686(7) 1 calc R U P B 1
H76C H 0.678100 0.523104 0.217158 0.162 Uiso 0.686(7) 1 calc R U P B 1
N70' N 0.799(3) 0.509(2) 0.3670(10) 0.081(7) Uiso 0.314(7) 1 d D U P B 2
H70B H 0.738301 0.459594 0.351495 0.097 Uiso 0.314(7) 1 calc R U P B 2
C71' C 0.9224(19) 0.4723(15) 0.3988(12) 0.092(6) Uiso 0.314(7) 1 d D U P B 2
H71C H 0.896341 0.435227 0.444320 0.110 Uiso 0.314(7) 1 calc R U P B 2
H71D H 0.991857 0.523891 0.419176 0.110 Uiso 0.314(7) 1 calc R U P B 2
C72' C 0.983(5) 0.411(3) 0.329(2) 0.126(9) Uiso 0.314(7) 1 d D U P B 2
H72D H 1.063442 0.387453 0.349951 0.189 Uiso 0.314(7) 1 calc R U P B 2
H72E H 0.914256 0.360090 0.309669 0.189 Uiso 0.314(7) 1 calc R U P B 2
H72F H 1.009539 0.448537 0.284586 0.189 Uiso 0.314(7) 1 calc R U P B 2
C73' C 0.7218(18) 0.5730(11) 0.4258(9) 0.070(4) Uiso 0.314(7) 1 d D U P B 2
H73C H 0.630116 0.578380 0.403513 0.084 Uiso 0.314(7) 1 calc R U P B 2
H73D H 0.773768 0.635123 0.435345 0.084 Uiso 0.314(7) 1 calc R U P B 2
C74' C 0.711(3) 0.524(2) 0.5061(11) 0.067(6) Uiso 0.314(7) 1 d D U P B 2
H74D H 0.663184 0.560355 0.546659 0.101 Uiso 0.314(7) 1 calc R U P B 2
H74E H 0.660026 0.462750 0.495103 0.101 Uiso 0.314(7) 1 calc R U P B 2
H74F H 0.802700 0.519107 0.526718 0.101 Uiso 0.314(7) 1 calc R U P B 2
C75' C 0.836(2) 0.5548(18) 0.2904(14) 0.122(5) Uiso 0.314(7) 1 d D U P B 2
H75C H 0.851841 0.508150 0.245729 0.146 Uiso 0.314(7) 1 calc R U P B 2
H75D H 0.919900 0.598972 0.299742 0.146 Uiso 0.314(7) 1 calc R U P B 2
C76' C 0.712(3) 0.606(2) 0.2684(17) 0.109(7) Uiso 0.314(7) 1 d D U P B 2
H76D H 0.731799 0.636514 0.219075 0.163 Uiso 0.314(7) 1 calc R U P B 2
H76E H 0.629672 0.561425 0.259348 0.163 Uiso 0.314(7) 1 calc R U P B 2
H76F H 0.697420 0.651832 0.313114 0.163 Uiso 0.314(7) 1 calc R U P B 2
N80 N 0.2850(8) 0.0920(5) 0.2412(6) 0.099(3) Uani 0.663(10) 1 d D U P C 1
H80A H 0.338276 0.142691 0.262777 0.119 Uiso 0.663(10) 1 calc R U P C 1
C81 C 0.3522(13) 0.0633(9) 0.1646(9) 0.133(4) Uani 0.663(10) 1 d D U P C 1
H81A H 0.361690 0.115682 0.130983 0.159 Uiso 0.663(10) 1 calc R U P C 1
H81B H 0.445384 0.050884 0.178473 0.159 Uiso 0.663(10) 1 calc R U P C 1
C82 C 0.2842(13) -0.0169(9) 0.1154(7) 0.143(5) Uani 0.663(10) 1 d D U P C 1
H82A H 0.337368 -0.029146 0.066870 0.214 Uiso 0.663(10) 1 calc R U P C 1
H82B H 0.276721 -0.070220 0.146889 0.214 Uiso 0.663(10) 1 calc R U P C 1
H82C H 0.192729 -0.005191 0.099230 0.214 Uiso 0.663(10) 1 calc R U P C 1
C83 C 0.1478(11) 0.1235(9) 0.2253(9) 0.115(4) Uani 0.663(10) 1 d D U P C 1
H83A H 0.157747 0.164631 0.181297 0.138 Uiso 0.663(10) 1 calc R U P C 1
H83B H 0.082661 0.069098 0.205721 0.138 Uiso 0.663(10) 1 calc R U P C 1
C84 C 0.0901(12) 0.1707(10) 0.2938(8) 0.122(4) Uani 0.663(10) 1 d D U P C 1
H84A H 0.001995 0.188268 0.277839 0.183 Uiso 0.663(10) 1 calc R U P C 1
H84B H 0.076894 0.130093 0.337374 0.183 Uiso 0.663(10) 1 calc R U P C 1
H84C H 0.152156 0.225849 0.312893 0.183 Uiso 0.663(10) 1 calc R U P C 1
C85 C 0.2794(16) 0.0258(9) 0.3058(10) 0.153(5) Uani 0.663(10) 1 d D U P C 1
H85A H 0.228835 0.050679 0.352339 0.183 Uiso 0.663(10) 1 calc R U P C 1
H85B H 0.226996 -0.033139 0.283790 0.183 Uiso 0.663(10) 1 calc R U P C 1
C86 C 0.4136(13) 0.0073(8) 0.3356(11) 0.128(5) Uani 0.663(10) 1 d D U P C 1
H86A H 0.400383 -0.036056 0.377075 0.192 Uiso 0.663(10) 1 calc R U P C 1
H86B H 0.463763 -0.019191 0.290476 0.192 Uiso 0.663(10) 1 calc R U P C 1
H86C H 0.465606 0.064799 0.359165 0.192 Uiso 0.663(10) 1 calc R U P C 1
N80' N 0.296(2) 0.0912(17) 0.1930(13) 0.127(6) Uiso 0.337(10) 1 d D U P C 2
H80B H 0.340424 0.147006 0.209624 0.152 Uiso 0.337(10) 1 calc R U P C 2
C81' C 0.373(4) 0.055(2) 0.1217(17) 0.145(7) Uiso 0.337(10) 1 d D U P C 2
H81C H 0.462981 0.042769 0.141786 0.174 Uiso 0.337(10) 1 calc R U P C 2
H81D H 0.322892 -0.004389 0.099253 0.174 Uiso 0.337(10) 1 calc R U P C 2
C82' C 0.396(2) 0.1130(15) 0.0564(11) 0.109(7) Uiso 0.337(10) 1 d D . P C 2
H82D H 0.446596 0.082468 0.013723 0.163 Uiso 0.337(10) 1 calc R U P C 2
H82E H 0.307690 0.124267 0.034210 0.163 Uiso 0.337(10) 1 calc R U P C 2
H82F H 0.448284 0.171595 0.076897 0.163 Uiso 0.337(10) 1 calc R U P C 2
C83' C 0.147(2) 0.102(2) 0.194(2) 0.141(9) Uiso 0.337(10) 1 d D U P C 2
H83C H 0.119656 0.114841 0.138510 0.169 Uiso 0.337(10) 1 calc R U P C 2
H83D H 0.095378 0.042948 0.204660 0.169 Uiso 0.337(10) 1 calc R U P C 2
C84' C 0.106(3) 0.173(2) 0.2507(19) 0.120(7) Uiso 0.337(10) 1 d D U P C 2
H84D H 0.007565 0.173932 0.245642 0.179 Uiso 0.337(10) 1 calc R U P C 2
H84E H 0.129632 0.160692 0.305881 0.179 Uiso 0.337(10) 1 calc R U P C 2
H84F H 0.153994 0.232834 0.239502 0.179 Uiso 0.337(10) 1 calc R U P C 2
C85' C 0.299(3) 0.036(3) 0.2636(18) 0.143(7) Uiso 0.337(10) 1 d D U P C 2
H85C H 0.290959 0.076945 0.313526 0.171 Uiso 0.337(10) 1 calc R U P C 2
H85D H 0.217857 -0.011024 0.259447 0.171 Uiso 0.337(10) 1 calc R U P C 2
C86' C 0.418(3) -0.0105(18) 0.2731(17) 0.124(8) Uiso 0.337(10) 1 d D U P C 2
H86D H 0.408577 -0.044402 0.321275 0.186 Uiso 0.337(10) 1 calc R U P C 2
H86E H 0.426497 -0.053425 0.225142 0.186 Uiso 0.337(10) 1 calc R U P C 2
H86F H 0.499874 0.034875 0.279425 0.186 Uiso 0.337(10) 1 calc R U P C 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
Si1 O21 1.767(3) . ?
Si1 O28 1.768(3) . ?
Si1 O1 1.780(3) . ?
Si1 O51 1.780(3) . ?
Si1 O8 1.788(3) . ?
Si1 O58 1.798(3) . ?
O1 C2 1.350(5) . ?
C2 C3 1.369(6) . ?
C2 C7 1.402(5) . ?
C3 C4 1.404(6) . ?
C4 C5 1.363(6) . ?
C4 C9 1.454(6) . ?
C5 C6 1.387(6) . ?
C6 C7 1.377(6) . ?
C7 O8 1.344(5) . ?
C9 O10 1.286(5) . ?
C9 O11 1.286(5) . ?
O21 C22 1.314(6) . ?
O21 C22' 1.441(9) . ?
C22 C23 1.3900 . ?
C22 C27 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C24 C29 1.397(11) . ?
C25 C26 1.3900 . ?
C26 C27 1.3900 . ?
C27 O28 1.410(6) . ?
C29 O30 1.331(11) . ?
C29 O31 1.361(10) . ?
C22' C23' 1.3900 . ?
C22' C27' 1.3900 . ?
C23' C24' 1.3900 . ?
C24' C25' 1.3900 . ?
C24' C29' 1.396(18) . ?
C25' C26' 1.3900 . ?
C26' C27' 1.3900 . ?
C27' O28 1.248(9) . ?
C29' O30' 1.365(14) . ?
C29' O31' 1.370(14) . ?
O51 C52 1.369(5) . ?
C52 C53 1.371(6) . ?
C52 C57 1.399(7) . ?
C53 C54 1.429(7) . ?
C54 C55 1.367(7) . ?
C54 C59 1.455(7) . ?
C55 C56 1.379(6) . ?
C56 C57 1.352(7) . ?
C57 O58 1.338(5) . ?
C59 O61 1.262(7) . ?
C59 O60 1.292(6) . ?
N70 C71 1.483(10) . ?
N70 C75 1.494(11) . ?
N70 C73 1.528(10) . ?
C71 C72 1.563(14) . ?
C73 C74 1.509(11) . ?
C75 C76 1.592(12) . ?
N70' C71' 1.504(14) . ?
N70' C75' 1.519(15) . ?
N70' C73' 1.564(14) . ?
C71' C72' 1.566(16) . ?
C73' C74' 1.570(15) . ?
C75' C76' 1.574(16) . ?
N80 C81 1.490(11) . ?
N80 C85 1.513(12) . ?
N80 C83 1.516(11) . ?
C81 C82 1.457(13) . ?
C83 C84 1.436(12) . ?
C85 C86 1.476(13) . ?
N80' C85' 1.491(16) . ?
N80' C83' 1.498(15) . ?
N80' C81' 1.504(16) . ?
C81' C82' 1.442(17) . ?
C83' C84' 1.443(17) . ?
C85' C86' 1.445(16) . ?

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
O21 Si1 O28 88.80(16) . . ?
O21 Si1 O1 176.06(15) . . ?
O28 Si1 O1 88.53(15) . . ?
O21 Si1 O51 94.67(14) . . ?
O28 Si1 O51 89.77(14) . . ?
O1 Si1 O51 88.21(13) . . ?
O21 Si1 O8 88.78(14) . . ?
O28 Si1 O8 94.60(14) . . ?
O1 Si1 O8 88.55(13) . . ?
O51 Si1 O8 174.50(16) . . ?
O21 Si1 O58 89.06(15) . . ?
O28 Si1 O58 177.24(16) . . ?
O1 Si1 O58 93.69(15) . . ?
O51 Si1 O58 88.67(14) . . ?
O8 Si1 O58 87.10(14) . . ?
C2 O1 Si1 111.8(2) . . ?
O1 C2 C3 126.1(4) . . ?
O1 C2 C7 114.0(4) . . ?
C3 C2 C7 119.9(4) . . ?
C2 C3 C4 119.2(4) . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 C9 120.7(4) . . ?
C3 C4 C9 119.2(4) . . ?
C4 C5 C6 121.6(4) . . ?
C7 C6 C5 118.2(4) . . ?
O8 C7 C6 125.3(4) . . ?
O8 C7 C2 113.7(4) . . ?
C6 C7 C2 121.0(4) . . ?
C7 O8 Si1 111.9(2) . . ?
O10 C9 O11 121.5(4) . . ?
O10 C9 C4 119.5(4) . . ?
O11 C9 C4 119.0(4) . . ?
C22 O21 Si1 112.5(4) . . ?
C22' O21 Si1 111.4(8) . . ?
O21 C22 C23 123.5(6) . . ?
O21 C22 C27 116.5(6) . . ?
C23 C22 C27 120.0 . . ?
C24 C23 C22 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 C29 111.4(6) . . ?
C23 C24 C29 128.5(6) . . ?
C24 C25 C26 120.0 . . ?
C25 C26 C27 120.0 . . ?
C26 C27 C22 120.0 . . ?
C26 C27 O28 129.6(6) . . ?
C22 C27 O28 110.4(6) . . ?
O30 C29 O31 124.0(10) . . ?
O30 C29 C24 116.0(8) . . ?
O31 C29 C24 120.0(9) . . ?
C23' C22' C27' 120.0 . . ?
C23' C22' O21 133.2(12) . . ?
C27' C22' O21 106.5(12) . . ?
C22' C23' C24' 120.0 . . ?
C25' C24' C23' 120.0 . . ?
C25' C24' C29' 116.1(10) . . ?
C23' C24' C29' 123.5(10) . . ?
C26' C25' C24' 120.0 . . ?
C25' C26' C27' 120.0 . . ?
O28 C27' C26' 117.6(14) . . ?
O28 C27' C22' 121.4(14) . . ?
C26' C27' C22' 120.0 . . ?
O30' C29' O31' 127.5(18) . . ?
O30' C29' C24' 112.3(13) . . ?
O31' C29' C24' 115.3(13) . . ?
C27' O28 Si1 110.8(9) . . ?
C27 O28 Si1 111.8(4) . . ?
C52 O51 Si1 110.4(3) . . ?
O51 C52 C53 124.8(4) . . ?
O51 C52 C57 115.1(4) . . ?
C53 C52 C57 120.1(4) . . ?
C52 C53 C54 118.6(4) . . ?
C55 C54 C53 119.3(4) . . ?
C55 C54 C59 120.5(5) . . ?
C53 C54 C59 120.1(5) . . ?
C54 C55 C56 121.3(5) . . ?
C57 C56 C55 119.6(5) . . ?
O58 C57 C56 126.0(4) . . ?
O58 C57 C52 113.0(4) . . ?
C56 C57 C52 121.0(4) . . ?
C57 O58 Si1 112.3(3) . . ?
O61 C59 O60 122.3(5) . . ?
O61 C59 C54 119.9(5) . . ?
O60 C59 C54 117.7(5) . . ?
C71 N70 C75 115.4(9) . . ?
C71 N70 C73 108.0(9) . . ?
C75 N70 C73 112.4(9) . . ?
N70 C71 C72 112.2(9) . . ?
C74 C73 N70 110.2(8) . . ?
N70 C75 C76 108.8(7) . . ?
C71' N70' C75' 109.2(18) . . ?
C71' N70' C73' 118.7(16) . . ?
C75' N70' C73' 110.2(16) . . ?
N70' C71' C72' 109.5(13) . . ?
N70' C73' C74' 104.2(11) . . ?
N70' C75' C76' 106.9(13) . . ?
C81 N80 C85 116.0(11) . . ?
C81 N80 C83 111.9(10) . . ?
C85 N80 C83 112.6(10) . . ?
C82 C81 N80 116.8(10) . . ?
C84 C83 N80 115.3(9) . . ?
C86 C85 N80 115.0(11) . . ?
C85' N80' C83' 98(2) . . ?
C85' N80' C81' 113.2(16) . . ?
C83' N80' C81' 126(2) . . ?
C82' C81' N80' 116.9(17) . . ?
C84' C83' N80' 116.7(16) . . ?
C86' C85' N80' 117.1(17) . . ?

_refine_diff_density_max         0.768
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.080




#===END

# start Validation Reply Form
_vrf_PLAT084_Et3NH_2_H3L-Si      
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: ...
The structure (including the solvent) is highly disordered, with ca. 62% of
the total electrons being disordered. This has a marked impact on the
intensity distribution of the data set, with the drop off at higher angles
being significantly steeper than would otherwise be expected to be the case.
Given this, it is unsurprising that the final R-factors are somewhat higher
than would be desired. See the supporting information for more details.
;
_vrf_PLAT430_Et3NH_2_H3L-Si      
;
PROBLEM: Short Inter D...A Contact  O10      ..O11      .       2.61 Ang.  
RESPONSE: ...
The hydrogen atoms of the three presumed -COOH groups could not be located
from delta-F maps, and so were omitted from the atom list. See the supporting
information for more details.
;
# end Validation Reply Form



####################################################################### 
# 
# 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_IMP34Dy
_database_code_depnum_ccdc_archive 'CCDC 2348719'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-07-14 downloaded from the CCDC.
;

#2022ncs0180r1_twin1b_twin1_hklf4

_audit_creation_date             2022-06-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
r.davies@imperial.ac.uk
pnh@soton.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H26 Dy2 Ge2 O28, Dy H16 O8, H2 O'
_chemical_formula_sum            'C42 H44 Dy3 Ge2 O37'
_chemical_formula_weight         1773.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H43 Ge N2 O12 Dy'
_chemical_oxdiff_usercomment     'ST L3-Ge + Dy '
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'
Dy Dy -9.8046 9.8477 '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'
O O 0.0492 0.0322 '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                   19.5343(3)
_cell_length_b                   14.22670(10)
_cell_length_c                   30.9853(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.9100(10)
_cell_angle_gamma                90
_cell_volume                     8548.53(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    42259
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1600
_cell_measurement_theta_min      2.8760
_shelx_estimated_absorpt_T_max   0.863
_shelx_estimated_absorpt_T_min   0.171
_exptl_absorpt_coefficient_mu    15.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
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    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             3416
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of water and MeCN'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            13640
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.051
_diffrn_reflns_theta_min         2.873
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  32.00   0.25    2.00    --  -45.09  27.00 155.00  144
  2  ω   -122.00 -39.00   0.25    2.00    --  -45.09 -27.00  -6.00  332
  3  ω     39.00 122.00   0.25    2.00    --   45.09  27.00 155.00  332
  4  ω    -31.00  -4.00   0.25    2.00    --   45.09 -27.00  -6.00  108
  5  ω   -167.00 -91.00   0.25    8.00    --  -97.00 -27.00  -6.00  304
  6  ω    104.00 159.00   0.25    8.00    --  109.75  27.00 155.00  220
  7  ω    -23.00  30.00   0.25    2.00    --  -45.09  38.00 -90.00  212
  8  ω    -90.00 -16.00   0.25    2.00    --  -45.09 125.00 -90.00  296
  9  ω    -30.00  15.00   0.25    2.00    --   45.09 -38.00-150.00  180
 10  ω    -30.00  15.00   0.25    2.00    --   45.09 -38.00-120.00  180
 11  ω    -30.00  15.00   0.25    2.00    --   45.09 -38.00  30.00  180
 12  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00 120.00  128
 13  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00 150.00  128
 14  ω   -140.00 -90.00   0.25    8.00    --  -97.00 -15.00-150.00  200
 15  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00 -90.00  128
 16  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00 -30.00  128
 17  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00 -60.00  128
 18  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00   0.00  128
 19  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00  90.00  128
 20  ω    -79.00 -23.00   0.25    8.00    --  -97.00  77.00  90.00  224
 21  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00  60.00  128
 22  ω    104.00 132.00   0.25    8.00    --  109.75  15.00  30.00  112
 23  ω     37.00  71.00   0.25    8.00    --  109.75 -77.00 -30.00  136
 24  ω     37.00  93.00   0.25    8.00    --  109.75 -95.00-120.00  224
 25  ω     37.00 100.00   0.25    8.00    --  109.75-125.00  30.00  252
 26  ω     37.00  71.00   0.25    8.00    --  109.75 -77.00 120.00  136
 27  ω     44.00  70.00   0.25    8.00    --  109.75 -77.00  60.00  104
 28  ω    106.00 132.00   0.25    8.00    --  109.75  15.00-120.00  104
 29  ω     58.00  84.00   0.25    8.00    --  109.75 -95.00-150.00  104
 30  ω     40.00  91.00   0.25    8.00    --  109.75 -95.00 -60.00  204
 31  ω     37.00  90.00   0.25    8.00    --  109.75 -95.00 -90.00  212
 32  ω    106.00 132.00   0.25    8.00    --  109.75  15.00  60.00  104
 33  ω     61.00  90.00   0.25    8.00    --  109.75-125.00 -90.00  116
 34  ω     41.00  67.00   0.25    8.00    --  109.75 -77.00 -60.00  104
 35  ω    105.00 131.00   0.25    8.00    --  109.75  15.00 -60.00  104
 36  ω    104.00 129.00   0.25    8.00    --  109.75  15.00  90.00  100
 37  ω     75.00 100.00   0.25    8.00    --  109.75-125.00 -60.00  100
 38  ω    104.00 132.00   0.25    8.00    --  109.75  15.00 150.00  112
 39  ω   -105.00 -80.00   0.25    2.00    --  -45.09 -27.00  -6.00  100
 40  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00 -90.00  324
 41  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00-120.00  324
 42  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00-150.00  324
 43  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00 150.00  324
 44  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00 120.00  324
 45  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00  90.00  324
 46  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00 -60.00  324
 47  ω   -120.00 -39.00   0.25    2.00    --  -45.09 -38.00 -30.00  324
 48  ω     39.00 120.00   0.25    2.00    --   45.09  38.00  90.00  324
 49  ω     -6.00  76.00   0.25    2.00    --   45.09 -99.00-180.00  328
 50  ω   -170.00 -86.00   0.25    8.00    --  -97.00 -61.00-150.00  336
 51  ω   -171.00 -89.00   0.25    8.00    --  -97.00 -45.00  90.00  328
 52  ω   -170.00 -86.00   0.25    8.00    --  -97.00 -61.00 -60.00  336
 53  ω    -55.00 -23.00   0.25    8.00    --  -97.00  61.00  30.00  128
 54  ω   -171.00 -89.00   0.25    8.00    --  -97.00 -45.00  60.00  328
 55  ω    104.00 132.00   0.25    8.00    --  109.75  15.00 -90.00  112
 56  ω     37.00  71.00   0.25    8.00    --  109.75 -77.00-180.00  136
 57  ω    104.00 132.00   0.25    8.00    --  109.75  15.00-150.00  112
 58  ω    104.00 132.00   0.25    8.00    --  109.75  15.00 -30.00  112
 59  ω     37.00  62.00   0.25    8.00    --  109.75 -95.00 150.00  100
 60  ω    104.00 132.00   0.25    8.00    --  109.75  15.00 120.00  112
 61  ω    104.00 132.00   0.25    8.00    --  109.75  15.00   0.00  112
 62  ω     37.00  71.00   0.25    8.00    --  109.75 -77.00 150.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 κ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF diffractometer with HF Varimax confocal mirrors, an UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0162825000
_diffrn_orient_matrix_UB_12      -0.0137884000
_diffrn_orient_matrix_UB_13      0.0494886000
_diffrn_orient_matrix_UB_21      -0.0220521000
_diffrn_orient_matrix_UB_22      0.1021017000
_diffrn_orient_matrix_UB_23      0.0074183000
_diffrn_orient_matrix_UB_31      -0.0745491000
_diffrn_orient_matrix_UB_32      -0.0333405000
_diffrn_orient_matrix_UB_33      0.0021942000
_diffrn_radiation_collimation    'HF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13100
_reflns_number_total             13640
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         13640
_refine_ls_number_restraints     377
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0823P)²+63.2670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1511
_refine_special_details          
'The system as currently presented does not charge balance (currently -0.5 for the asymmetric unit) with the required +0.5 charge assumed to come from a disordered Et3NH cation mixed in with the solvent water. Highly disordered solvent (assumed water (9 per asymmetric unit) along with half a EtNH cation) removed using SQUEEZE. The disordered hydrated Dy that lies over a symmetry site required the use of various restraints (DELU, SIMU) and in the end was held as a rigid body.,Twin,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5388(10)
 0.4612(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
3. Restrained distances
 O32-H32A = O32-H32B = O31-H31A = O31-H31B
 0.87 with sigma of 0.01
 Dy1-H31B = Dy1-H31A
 -2.7 with sigma of 0.02
 Dy1-H31A \\sim Dy1-H31B
 with sigma of 0.02
4. Rigid bond restraints
 Dy5, O58, O51, O53, O52, O57, O55, O56, O54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(O55) = Uanis(O61)
6. Rigid body (RIGU) restrains
 Dy5, O51, O58, O53, O57, O52, O55, O56, O54, O61
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: Dy5(0.5) O53(0.5) H53A(0.5) H53B(0.5) O51(0.5) O52(0.5) O54(0.5)
 O55(0.5) O56(0.5) O57(0.5) O58(0.5) H51A(0.5) H51B(0.5) H52A(0.5) H52B(0.5)
 H54A(0.5) H54B(0.5) H55A(0.5) H55B(0.5) H56A(0.5) H56B(0.5) H57A(0.5)
 H57B(0.5) H58A(0.5) H58B(0.5) O61(0.5) H61A(0.5) H61B(0.5)
8.a Free rotating group:
 O31(H31A,H31B), Dy5(O53,H53A,H53B,O51,O52,O54,O55,O56,O57,O58,H51A,H51B,H52A,
 H52B,H54A,H54B,H55A,H55B,H56A,H56B,H57A,H57B,H58A,H58B), O61(H61A,H61B)
8.b Rotating group:
 O32(H32A,H32B)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C13(H13), C15(H15), C16(H16), C23(H23), C25(H25),
 C26(H26)
;
_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
Dy1 Dy 0.43500(2) 0.62599(3) 0.48097(2) 0.03544(13) Uani 1 1 d D . . . .
Ge1 Ge 0.26279(5) 0.14686(5) 0.29915(2) 0.0354(2) Uani 1 1 d . U . . .
O1 O 0.2603(3) 0.2796(3) 0.30086(15) 0.0414(12) Uani 1 1 d . U . . .
O2 O 0.3413(3) 0.1573(3) 0.34078(15) 0.0408(12) Uani 1 1 d . U . . .
O3 O 0.4968(3) 0.3381(4) 0.45450(16) 0.0513(14) Uani 1 1 d . U . . .
O4 O 0.4512(3) 0.4810(3) 0.45280(15) 0.0431(12) Uani 1 1 d . U . . .
O11 O 0.2671(3) 0.0141(3) 0.30415(14) 0.0367(10) Uani 1 1 d . U . . .
O12 O 0.2030(3) 0.1413(3) 0.34223(15) 0.0435(13) Uani 1 1 d . U . . .
O13 O 0.1169(3) -0.0200(3) 0.47306(15) 0.0430(12) Uani 1 1 d . U . . .
O14 O 0.1448(3) -0.1670(4) 0.46570(15) 0.0454(12) Uani 1 1 d . U . . .
O21 O 0.3199(3) 0.1390(4) 0.25473(15) 0.0413(12) Uani 1 1 d . U . . .
O22 O 0.1879(2) 0.1491(4) 0.25490(14) 0.0378(12) Uani 1 1 d . U . . .
O23 O 0.0886(3) 0.1704(4) 0.09531(15) 0.0459(12) Uani 1 1 d . U . . .
O24 O 0.1752(3) 0.1417(4) 0.05977(16) 0.0527(14) Uani 1 1 d . U . . .
O31 O 0.4451(4) 0.7926(4) 0.4813(2) 0.0674(18) Uani 1 1 d DG . . . .
H31A H 0.425458 0.807104 0.455471 0.101 Uiso 1 1 d DG U . . .
H31B H 0.415359 0.808964 0.498638 0.101 Uiso 1 1 d DG U . . .
O32 O 0.5461(3) 0.6413(4) 0.45833(18) 0.0472(12) Uani 1 1 d D . . . .
H32A H 0.545128 0.667169 0.430106 0.071 Uiso 1 1 d DR U . . .
H32B H 0.567149 0.582552 0.454728 0.071 Uiso 1 1 d DR U . . .
C1 C 0.3058(5) 0.3121(5) 0.3330(2) 0.0469(19) Uani 1 1 d . U . . .
C2 C 0.3499(4) 0.2460(5) 0.3548(2) 0.0382(16) Uani 1 1 d . U . . .
C3 C 0.3984(4) 0.2738(5) 0.3896(2) 0.0418(17) Uani 1 1 d . U . . .
H3 H 0.427899 0.228646 0.404899 0.050 Uiso 1 1 calc R U . . .
C4 C 0.4028(4) 0.3664(5) 0.4013(2) 0.0460(18) Uani 1 1 d . U . . .
C5 C 0.3598(6) 0.4323(6) 0.3787(3) 0.076(3) Uani 1 1 d . U . . .
H5 H 0.364321 0.496722 0.386510 0.091 Uiso 1 1 calc R U . . .
C6 C 0.3100(5) 0.4055(5) 0.3446(3) 0.064(3) Uani 1 1 d . U . . .
H6 H 0.279797 0.450599 0.329888 0.076 Uiso 1 1 calc R U . . .
C7 C 0.4521(4) 0.3982(5) 0.4384(2) 0.0445(18) Uani 1 1 d . U . . .
C11 C 0.2383(4) -0.0147(5) 0.3389(2) 0.0345(14) Uani 1 1 d . U . . .
C12 C 0.2042(3) 0.0556(4) 0.36067(19) 0.0316(14) Uani 1 1 d . U . . .
C13 C 0.1751(4) 0.0338(5) 0.3973(2) 0.0362(15) Uani 1 1 d . U . . .
H13 H 0.152811 0.081339 0.412059 0.043 Uiso 1 1 calc R U . . .
C14 C 0.1781(4) -0.0591(5) 0.4134(2) 0.0393(16) Uani 1 1 d . U . . .
C15 C 0.2102(5) -0.1284(5) 0.3919(3) 0.0483(19) Uani 1 1 d . U . . .
H15 H 0.210714 -0.191412 0.402118 0.058 Uiso 1 1 calc R U . . .
C16 C 0.2423(5) -0.1056(5) 0.3545(2) 0.0449(18) Uani 1 1 d . U . . .
H16 H 0.266303 -0.152372 0.340412 0.054 Uiso 1 1 calc R U . . .
C17 C 0.1456(4) -0.0837(5) 0.4519(2) 0.0418(16) Uani 1 1 d . U . . .
C21 C 0.2823(4) 0.1434(4) 0.2150(2) 0.0345(14) Uani 1 1 d . U . . .
C22 C 0.2120(4) 0.1510(4) 0.2153(2) 0.0363(16) Uani 1 1 d . U . . .
C23 C 0.1677(4) 0.1591(5) 0.1762(2) 0.0375(16) Uani 1 1 d . U . . .
H23 H 0.119433 0.167383 0.176051 0.045 Uiso 1 1 calc R U . . .
C24 C 0.1985(4) 0.1542(5) 0.1370(2) 0.0381(16) Uani 1 1 d . U . . .
C25 C 0.2682(4) 0.1440(5) 0.1376(2) 0.0384(16) Uani 1 1 d . U . . .
H25 H 0.287348 0.139720 0.110909 0.046 Uiso 1 1 calc R U . . .
C26 C 0.3110(4) 0.1397(5) 0.1762(2) 0.0409(16) Uani 1 1 d . U . . .
H26 H 0.359526 0.134244 0.176227 0.049 Uiso 1 1 calc R U . . .
C27 C 0.1526(4) 0.1575(5) 0.0954(2) 0.0402(16) Uani 1 1 d . U . . .
Dy5 Dy 0.04386(5) 0.38795(11) 0.24601(4) 0.0762(4) Uani 0.5 1 d G U P A -1
O53 O 0.0827(3) 0.2447(2) 0.2789(2) 0.069(3) Uani 0.5 1 d G U P A -1
H53A H 0.051448 0.201066 0.272671 0.103 Uiso 0.5 1 d G U P A -1
H53B H 0.118538 0.224386 0.267241 0.103 Uiso 0.5 1 d G U P A -1
O51 O 0.0621(3) 0.54322(17) 0.2280(2) 0.077(3) Uani 0.5 1 d G U P A -1
O52 O 0.0865(3) 0.4293(5) 0.31989(8) 0.065(3) Uani 0.5 1 d G U P A -1
O54 O -0.0030(3) 0.2451(3) 0.2063(2) 0.099(4) Uani 0.5 1 d G U P A -1
O55 O 0.16851(6) 0.4042(4) 0.25339(19) 0.0417(15) Uani 0.5 1 d G U P A -1
O56 O -0.0459(2) 0.3434(5) 0.29199(16) 0.070(3) Uani 0.5 1 d G U P A -1
O57 O -0.05887(17) 0.4509(4) 0.20791(17) 0.071(3) Uani 0.5 1 d G U P A -1
O58 O 0.0612(3) 0.3732(5) 0.17108(6) 0.087(3) Uani 0.5 1 d G U P A -1
H51A H 0.103918 0.549997 0.220821 0.130 Uiso 0.5 1 d G U P A -1
H51B H 0.061698 0.578916 0.251101 0.130 Uiso 0.5 1 d G U P A -1
H52A H 0.078398 0.383655 0.337401 0.130 Uiso 0.5 1 d G U P A -1
H52B H 0.062797 0.476575 0.328171 0.130 Uiso 0.5 1 d G U P A -1
H54A H 0.030609 0.204857 0.203291 0.130 Uiso 0.5 1 d G U P A -1
H54B H -0.030172 0.214136 0.222270 0.130 Uiso 0.5 1 d G U P A -1
H55A H 0.192938 0.439247 0.238091 0.130 Uiso 0.5 1 d G U P A -1
H55B H 0.198818 0.374377 0.271251 0.130 Uiso 0.5 1 d G U P A -1
H56A H -0.090392 0.347885 0.285780 0.130 Uiso 0.5 1 d G U P A -1
H56B H -0.039982 0.319825 0.318081 0.130 Uiso 0.5 1 d G U P A -1
H57A H -0.079102 0.486886 0.225241 0.130 Uiso 0.5 1 d G U P A -1
H57B H -0.088222 0.405756 0.201051 0.130 Uiso 0.5 1 d G U P A -1
H58A H 0.066308 0.428817 0.160231 0.130 Uiso 0.5 1 d G U P A -1
H58B H 0.024049 0.351147 0.156251 0.130 Uiso 0.5 1 d G U P A -1
O61 O -0.1699(7) 0.3832(9) 0.2551(4) 0.0417(15) Uani 0.5 1 d G . P B -1
H61A H -0.193288 0.427222 0.266225 0.063 Uiso 0.5 1 d G U P B -1
H61B H -0.163616 0.404482 0.229503 0.063 Uiso 0.5 1 d G U P B -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
Dy1 O3 2.322(5) 5_666 ?
Dy1 O4 2.277(4) . ?
Dy1 O13 2.383(5) 7_556 ?
Dy1 O14 2.474(5) 7_556 ?
Dy1 O23 2.436(5) 4 ?
Dy1 O24 2.372(5) 4 ?
Dy1 O31 2.378(6) . ?
Dy1 O32 2.369(6) . ?
Dy1 C17 2.821(7) 7_556 ?
Dy1 C27 2.786(7) 4 ?
Ge1 O1 1.891(4) . ?
Ge1 O2 1.888(5) . ?
Ge1 O11 1.896(4) . ?
Ge1 O12 1.877(5) . ?
Ge1 O21 1.876(5) . ?
Ge1 O22 1.882(4) . ?
O1 C1 1.335(8) . ?
O2 C2 1.339(8) . ?
O3 C7 1.280(10) . ?
O4 C7 1.261(8) . ?
O11 C11 1.337(8) . ?
O12 C12 1.345(8) . ?
O13 C17 1.287(9) . ?
O14 C17 1.261(9) . ?
O21 C21 1.357(8) . ?
O22 C22 1.368(8) . ?
O23 C27 1.263(9) . ?
O24 C27 1.259(9) . ?
O31 H31A 0.8698 . ?
O31 H31B 0.8698 . ?
O32 H32A 0.9468 . ?
O32 H32B 0.9445 . ?
C1 C2 1.393(10) . ?
C1 C6 1.377(10) . ?
C2 C3 1.404(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.367(10) . ?
C4 C5 1.389(11) . ?
C4 C7 1.480(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.400(11) . ?
C6 H6 0.9500 . ?
C11 C12 1.417(9) . ?
C11 C16 1.380(10) . ?
C12 C13 1.366(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.411(10) . ?
C14 C15 1.383(10) . ?
C14 C17 1.459(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.420(11) . ?
C16 H16 0.9500 . ?
C21 C22 1.380(10) . ?
C21 C26 1.389(11) . ?
C22 C23 1.404(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.422(10) . ?
C24 C25 1.367(11) . ?
C24 C27 1.478(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.376(10) . ?
C26 H26 0.9500 . ?
Dy5 O53 2.3628 . ?
Dy5 O51 2.3164 . ?
Dy5 O52 2.4130 . ?
Dy5 O54 2.4919 . ?
Dy5 O55 2.4291 . ?
Dy5 O56 2.4705 . ?
Dy5 O57 2.3778 . ?
Dy5 O58 2.3957 . ?
O53 H53A 0.8751 . ?
O53 H53B 0.8755 . ?
O51 H51A 0.8772 . ?
O51 H51B 0.8782 . ?
O52 H52A 0.8730 . ?
O52 H52B 0.8728 . ?
O54 H54A 0.8848 . ?
O54 H54B 0.8848 . ?
O55 H55A 0.8696 . ?
O55 H55B 0.8703 . ?
O56 H56A 0.8703 . ?
O56 H56B 0.8701 . ?
O57 H57A 0.8701 . ?
O57 H57B 0.8706 . ?
O58 H58A 0.8697 . ?
O58 H58B 0.8702 . ?
O61 H61A 0.8704 . ?
O61 H61B 0.8708 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Dy1 O13 82.29(19) 5_666 7_556 ?
O3 Dy1 O14 73.5(2) 5_666 7_556 ?
O3 Dy1 O23 143.14(19) 5_666 4 ?
O3 Dy1 O24 145.9(2) 5_666 4 ?
O3 Dy1 O31 74.8(2) 5_666 . ?
O3 Dy1 O32 77.5(2) 5_666 . ?
O3 Dy1 C17 74.0(2) 5_666 7_556 ?
O3 Dy1 C27 157.9(2) 5_666 4 ?
O4 Dy1 O3 115.96(19) . 5_666 ?
O4 Dy1 O13 75.21(17) . 7_556 ?
O4 Dy1 O14 126.70(18) . 7_556 ?
O4 Dy1 O23 83.20(18) . 4 ?
O4 Dy1 O24 92.3(2) . 4 ?
O4 Dy1 O31 152.8(2) . . ?
O4 Dy1 O32 78.19(18) . . ?
O4 Dy1 C17 101.9(2) . 7_556 ?
O4 Dy1 C27 85.37(19) . 4 ?
O13 Dy1 O14 53.30(16) 7_556 7_556 ?
O13 Dy1 O23 134.39(17) 7_556 4 ?
O13 Dy1 C17 26.98(19) 7_556 7_556 ?
O13 Dy1 C27 110.4(2) 7_556 4 ?
O14 Dy1 C17 26.52(19) 7_556 7_556 ?
O14 Dy1 C27 99.1(2) 7_556 4 ?
O23 Dy1 O14 121.74(18) 4 7_556 ?
O23 Dy1 C17 135.5(2) 4 7_556 ?
O23 Dy1 C27 26.9(2) 4 4 ?
O24 Dy1 O13 87.32(19) 4 7_556 ?
O24 Dy1 O14 74.26(18) 4 7_556 ?
O24 Dy1 O23 53.54(18) 4 4 ?
O24 Dy1 O31 88.8(2) 4 . ?
O24 Dy1 C17 82.0(2) 4 7_556 ?
O24 Dy1 C27 26.8(2) 4 4 ?
O31 Dy1 O13 132.01(19) . 7_556 ?
O31 Dy1 O14 79.7(2) . 7_556 ?
O31 Dy1 O23 75.62(19) . 4 ?
O31 Dy1 C17 105.2(2) . 7_556 ?
O31 Dy1 C27 83.4(2) . 4 ?
O32 Dy1 O13 134.91(18) . 7_556 ?
O32 Dy1 O14 148.12(19) . 7_556 ?
O32 Dy1 O23 76.21(19) . 4 ?
O32 Dy1 O24 129.70(18) . 4 ?
O32 Dy1 O31 80.3(2) . . ?
O32 Dy1 C17 148.2(2) . 7_556 ?
O32 Dy1 C27 102.9(2) . 4 ?
C27 Dy1 C17 108.7(2) 4 7_556 ?
O1 Ge1 O11 173.75(19) . . ?
O2 Ge1 O1 85.66(19) . . ?
O2 Ge1 O11 89.9(2) . . ?
O12 Ge1 O1 90.1(2) . . ?
O12 Ge1 O2 92.4(2) . . ?
O12 Ge1 O11 85.7(2) . . ?
O12 Ge1 O22 91.3(2) . . ?
O21 Ge1 O1 95.7(2) . . ?
O21 Ge1 O2 90.0(2) . . ?
O21 Ge1 O11 88.6(2) . . ?
O21 Ge1 O12 173.9(2) . . ?
O21 Ge1 O22 86.9(2) . . ?
O22 Ge1 O1 89.0(2) . . ?
O22 Ge1 O2 173.5(2) . . ?
O22 Ge1 O11 95.7(2) . . ?
C1 O1 Ge1 110.4(4) . . ?
C2 O2 Ge1 110.8(4) . . ?
C7 O3 Dy1 118.9(4) . 5_666 ?
C7 O4 Dy1 172.3(6) . . ?
C11 O11 Ge1 110.6(4) . . ?
C12 O12 Ge1 111.1(4) . . ?
C17 O13 Dy1 95.9(4) . 7_556 ?
C17 O14 Dy1 92.3(4) . 7_556 ?
C21 O21 Ge1 111.0(5) . . ?
C22 O22 Ge1 109.5(4) . . ?
C27 O23 Dy1 92.1(4) . 4_545 ?
C27 O24 Dy1 95.3(5) . 4_545 ?
Dy1 O31 H31A 101.8 . . ?
Dy1 O31 H31B 102.0 . . ?
H31A O31 H31B 104.5 . . ?
Dy1 O32 H32A 113.1 . . ?
Dy1 O32 H32B 112.4 . . ?
H32A O32 H32B 101.2 . . ?
O1 C1 C2 116.5(6) . . ?
O1 C1 C6 122.8(7) . . ?
C6 C1 C2 120.7(7) . . ?
O2 C2 C1 115.6(6) . . ?
O2 C2 C3 124.1(6) . . ?
C1 C2 C3 120.3(6) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.2(7) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 120.2(7) . . ?
C3 C4 C7 120.9(7) . . ?
C5 C4 C7 118.9(7) . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.3(7) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 118.3(7) . . ?
C1 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
O3 C7 C4 116.7(6) . . ?
O4 C7 O3 121.6(7) . . ?
O4 C7 C4 121.7(7) . . ?
O11 C11 C12 115.8(6) . . ?
O11 C11 C16 123.9(6) . . ?
C16 C11 C12 120.3(6) . . ?
O12 C12 C11 114.9(6) . . ?
O12 C12 C13 124.9(6) . . ?
C13 C12 C11 120.2(6) . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.2(6) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C17 120.7(6) . . ?
C15 C14 C13 120.0(7) . . ?
C15 C14 C17 119.3(7) . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.0(7) . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 119.3(7) . . ?
C11 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
O13 C17 Dy1 57.2(4) . 7_556 ?
O13 C17 C14 120.4(7) . . ?
O14 C17 Dy1 61.2(4) . 7_556 ?
O14 C17 O13 117.7(6) . . ?
O14 C17 C14 121.9(6) . . ?
C14 C17 Dy1 171.9(5) . 7_556 ?
O21 C21 C22 115.4(6) . . ?
O21 C21 C26 123.6(7) . . ?
C22 C21 C26 121.0(7) . . ?
O22 C22 C21 117.0(6) . . ?
O22 C22 C23 122.2(7) . . ?
C21 C22 C23 120.8(7) . . ?
C22 C23 H23 121.5 . . ?
C22 C23 C24 116.9(7) . . ?
C24 C23 H23 121.5 . . ?
C23 C24 C27 117.9(7) . . ?
C25 C24 C23 121.1(7) . . ?
C25 C24 C27 121.0(7) . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.2(7) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 H26 120.5 . . ?
C25 C26 C21 119.0(7) . . ?
C25 C26 H26 120.5 . . ?
O23 C27 Dy1 60.9(4) . 4_545 ?
O23 C27 C24 120.3(7) . . ?
O24 C27 Dy1 58.0(4) . 4_545 ?
O24 C27 O23 118.4(6) . . ?
O24 C27 C24 121.2(7) . . ?
C24 C27 Dy1 168.9(5) . 4_545 ?
O53 Dy5 O52 75.2 . . ?
O53 Dy5 O54 65.7 . . ?
O53 Dy5 O55 77.0 . . ?
O53 Dy5 O56 75.1 . . ?
O53 Dy5 O57 138.3 . . ?
O53 Dy5 O58 105.5 . . ?
O51 Dy5 O53 151.1 . . ?
O51 Dy5 O52 87.1 . . ?
O51 Dy5 O54 135.8 . . ?
O51 Dy5 O55 75.6 . . ?
O51 Dy5 O56 121.6 . . ?
O51 Dy5 O57 70.5 . . ?
O51 Dy5 O58 78.8 . . ?
O52 Dy5 O54 137.0 . . ?
O52 Dy5 O55 70.1 . . ?
O52 Dy5 O56 72.8 . . ?
O55 Dy5 O54 115.4 . . ?
O55 Dy5 O56 138.0 . . ?
O56 Dy5 O54 80.3 . . ?
O57 Dy5 O52 123.6 . . ?
O57 Dy5 O54 79.9 . . ?
O57 Dy5 O55 142.0 . . ?
O57 Dy5 O56 76.6 . . ?
O57 Dy5 O58 76.2 . . ?
O58 Dy5 O52 150.2 . . ?
O58 Dy5 O54 62.4 . . ?
O58 Dy5 O55 80.9 . . ?
O58 Dy5 O56 136.8 . . ?
Dy5 O53 H53A 109.7 . . ?
Dy5 O53 H53B 109.7 . . ?
H53A O53 H53B 104.2 . . ?
Dy5 O51 H51A 109.9 . . ?
Dy5 O51 H51B 109.8 . . ?
H51A O51 H51B 104.1 . . ?
Dy5 O52 H52A 109.9 . . ?
Dy5 O52 H52B 109.4 . . ?
H52A O52 H52B 104.3 . . ?
Dy5 O54 H54A 110.3 . . ?
Dy5 O54 H54B 109.9 . . ?
H54A O54 H54B 103.9 . . ?
Dy5 O55 H55A 127.8 . . ?
Dy5 O55 H55B 127.7 . . ?
H55A O55 H55B 104.5 . . ?
Dy5 O56 H56A 127.8 . . ?
Dy5 O56 H56B 127.7 . . ?
H56A O56 H56B 104.5 . . ?
Dy5 O57 H57A 109.5 . . ?
Dy5 O57 H57B 109.5 . . ?
H57A O57 H57B 104.5 . . ?
Dy5 O58 H58A 109.3 . . ?
Dy5 O58 H58B 109.7 . . ?
H58A O58 H58B 104.5 . . ?
H61A O61 H61B 104.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O3 C7 O4 10.8(10) 5_666 . . . ?
Dy1 O3 C7 C4 -170.7(5) 5_666 . . . ?
Dy1 O13 C17 O14 -9.5(7) 7_556 . . . ?
Dy1 O13 C17 C14 170.9(6) 7_556 . . . ?
Dy1 O14 C17 O13 9.1(7) 7_556 . . . ?
Dy1 O14 C17 C14 -171.3(6) 7_556 . . . ?
Dy1 O23 C27 O24 8.3(7) 4_545 . . . ?
Dy1 O23 C27 C24 -167.3(6) 4_545 . . . ?
Dy1 O24 C27 O23 -8.5(7) 4_545 . . . ?
Dy1 O24 C27 C24 167.0(6) 4_545 . . . ?
Ge1 O1 C1 C2 6.9(9) . . . . ?
Ge1 O1 C1 C6 -173.0(8) . . . . ?
Ge1 O2 C2 C1 -7.0(9) . . . . ?
Ge1 O2 C2 C3 171.6(6) . . . . ?
Ge1 O11 C11 C12 7.4(7) . . . . ?
Ge1 O11 C11 C16 -170.4(6) . . . . ?
Ge1 O12 C12 C11 -11.5(7) . . . . ?
Ge1 O12 C12 C13 169.1(6) . . . . ?
Ge1 O21 C21 C22 -0.9(7) . . . . ?
Ge1 O21 C21 C26 179.7(5) . . . . ?
Ge1 O22 C22 C21 5.0(7) . . . . ?
Ge1 O22 C22 C23 -175.8(5) . . . . ?
O1 Ge1 O2 C2 8.6(5) . . . . ?
O1 Ge1 O12 C12 -163.0(4) . . . . ?
O1 Ge1 O21 C21 -85.7(4) . . . . ?
O1 Ge1 O22 C22 91.5(4) . . . . ?
O1 C1 C2 O2 0.0(11) . . . . ?
O1 C1 C2 C3 -178.7(7) . . . . ?
O1 C1 C6 C5 -179.7(10) . . . . ?
O2 Ge1 O1 C1 -8.5(6) . . . . ?
O2 Ge1 O11 C11 81.5(4) . . . . ?
O2 Ge1 O12 C12 -77.3(4) . . . . ?
O2 Ge1 O21 C21 -171.4(4) . . . . ?
O2 C2 C3 C4 -179.9(8) . . . . ?
O11 Ge1 O2 C2 -167.0(5) . . . . ?
O11 Ge1 O12 C12 12.4(4) . . . . ?
O11 Ge1 O21 C21 98.8(4) . . . . ?
O11 Ge1 O22 C22 -92.6(4) . . . . ?
O11 C11 C12 O12 2.7(9) . . . . ?
O11 C11 C12 C13 -177.9(6) . . . . ?
O11 C11 C16 C15 179.5(7) . . . . ?
O12 Ge1 O1 C1 83.8(6) . . . . ?
O12 Ge1 O2 C2 -81.3(5) . . . . ?
O12 Ge1 O11 C11 -10.9(4) . . . . ?
O12 Ge1 O22 C22 -178.4(4) . . . . ?
O12 C12 C13 C14 178.6(6) . . . . ?
O21 Ge1 O1 C1 -98.1(6) . . . . ?
O21 Ge1 O2 C2 104.3(5) . . . . ?
O21 Ge1 O11 C11 171.5(4) . . . . ?
O21 Ge1 O22 C22 -4.3(4) . . . . ?
O21 C21 C22 O22 -2.8(8) . . . . ?
O21 C21 C22 C23 178.0(6) . . . . ?
O21 C21 C26 C25 179.5(6) . . . . ?
O22 Ge1 O1 C1 175.2(6) . . . . ?
O22 Ge1 O11 C11 -101.8(4) . . . . ?
O22 Ge1 O12 C12 108.0(4) . . . . ?
O22 Ge1 O21 C21 3.0(4) . . . . ?
O22 C22 C23 C24 -176.1(6) . . . . ?
C1 C2 C3 C4 -1.3(13) . . . . ?
C2 C1 C6 C5 0.3(16) . . . . ?
C2 C3 C4 C5 -0.3(14) . . . . ?
C2 C3 C4 C7 178.6(8) . . . . ?
C3 C4 C5 C6 2.0(17) . . . . ?
C3 C4 C7 O3 10.1(12) . . . . ?
C3 C4 C7 O4 -171.4(8) . . . . ?
C4 C5 C6 C1 -1.9(18) . . . . ?
C5 C4 C7 O3 -170.9(9) . . . . ?
C5 C4 C7 O4 7.5(14) . . . . ?
C6 C1 C2 O2 -180.0(9) . . . . ?
C6 C1 C2 C3 1.3(14) . . . . ?
C7 C4 C5 C6 -177.0(10) . . . . ?
C11 C12 C13 C14 -0.8(10) . . . . ?
C12 C11 C16 C15 1.9(12) . . . . ?
C12 C13 C14 C15 -0.4(11) . . . . ?
C12 C13 C14 C17 -178.4(7) . . . . ?
C13 C14 C15 C16 2.2(12) . . . . ?
C13 C14 C17 O13 -3.7(11) . . . . ?
C13 C14 C17 O14 176.7(7) . . . . ?
C14 C15 C16 C11 -3.0(13) . . . . ?
C15 C14 C17 O13 178.3(7) . . . . ?
C15 C14 C17 O14 -1.3(12) . . . . ?
C16 C11 C12 O12 -179.4(7) . . . . ?
C16 C11 C12 C13 0.0(10) . . . . ?
C17 C14 C15 C16 -179.7(8) . . . . ?
C21 C22 C23 C24 3.0(9) . . . . ?
C22 C21 C26 C25 0.2(10) . . . . ?
C22 C23 C24 C25 -1.2(10) . . . . ?
C22 C23 C24 C27 176.8(6) . . . . ?
C23 C24 C25 C26 -1.2(10) . . . . ?
C23 C24 C27 Dy1 -89(3) . . . 4_545 ?
C23 C24 C27 O23 4.5(10) . . . . ?
C23 C24 C27 O24 -170.9(7) . . . . ?
C24 C25 C26 C21 1.7(10) . . . . ?
C25 C24 C27 Dy1 89(3) . . . 4_545 ?
C25 C24 C27 O23 -177.5(7) . . . . ?
C25 C24 C27 O24 7.1(11) . . . . ?
C26 C21 C22 O22 176.6(6) . . . . ?
C26 C21 C22 C23 -2.6(10) . . . . ?
C27 C24 C25 C26 -179.2(6) . . . . ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_original_sample_id 'ST L3-Ge + Dy'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.843
_oxdiff_exptl_absorpt_empirical_full_min 0.645
_oxdiff_twin_integration_method  simultaneous
_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 0.5388(10) 28481 50661 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4612(10) 28405 50661 nmt -1.0001 0.0000 0.0001 -0.0001 -1.0001 -0.0000
0.3812 -0.0011 1.0000

_twin_special_details            
;
Component 2 rotated by -179.9961° 
around [-0.00 -0.00 1.00] (reciprocal) or [0.19 -0.00 0.98] (direct)
;
####################################################################### 
# 
# 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_IMP34Y
_database_code_depnum_ccdc_archive 'CCDC 2348718'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-07-14 downloaded from the CCDC.
;

#2021ncs0370t
_audit_creation_date             2022-06-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
r.davies@imperial.ac.uk
pnh@soton.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H26 Ge2 O28 Y2, 5(H2 O), H16 O8 Y'
_chemical_formula_sum            'C42 H52 Ge2 O41 Y3'
_chemical_formula_weight         1624.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H43 Ge N2 O12 Y'
_chemical_oxdiff_usercomment     'ST L3-Ge + Y'
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'
Ge Ge -1.0885 0.8855 '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'
Y Y -0.2670 2.0244 '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                   19.9205(2)
_cell_length_b                   14.33510(10)
_cell_length_c                   30.7566(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.0890(10)
_cell_angle_gamma                90
_cell_volume                     8715.79(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    92409
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.4850
_cell_measurement_theta_min      2.8380
_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.472
_exptl_absorpt_coefficient_mu    4.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
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    1.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             3252
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of MeCN and water'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            27185
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.273
_diffrn_reflns_theta_min         2.896
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  94.00   0.25    0.25    --    5.00  49.00 -60.00  712
  2  ω    -84.00  94.00   0.25    0.25    --    5.00  36.00-158.66  712
  3  ω    -84.00  94.00   0.25    0.25    --    5.00  30.00 -90.00  712
  4  ω    -84.00  94.00   0.25    0.25    --    5.00  49.00 150.00  712
  5  ω    -84.00  94.00   0.25    0.25    --    5.00  30.00  60.00  712
  6  ω    -84.00  94.00   0.25    0.25    --    5.00  49.00  30.00  712
  7  ω    -84.00  94.00   0.25    0.25    --    5.00  49.00 -60.00  712
  8  ω     56.00  92.00   0.25    0.25    --    5.00  30.00 -90.00  144
  9  ω    -33.00  -1.00   0.25    0.40    --  -90.00  58.00  -2.19  128
 10  ω    -89.00 -58.00   0.25    0.40    --  -90.00  58.00  -2.19  124
 11  ω    -27.00  -1.00   0.25    0.40    --  -90.00  58.00  46.61  104
 12  ω    -27.00  -1.00   0.25    0.40    --  -90.00  58.00 -38.45  104
 13  ω   -135.00 -31.00   0.25    0.40    --  -90.00  58.00 -38.45  416
 14  ω   -168.00-142.00   0.25    0.40    --  -90.00  58.00  46.61  104
 15  ω   -160.00-133.00   0.25    0.40    --  -90.00  58.00   6.86  108
 16  ω    -32.00  -1.00   0.25    0.40    --  -90.00  59.00 147.02  124
 17  ω    -96.00 -70.00   0.25    0.40    --  -90.00  59.00 166.60  104
 18  ω    -26.00  -1.00   0.25    0.40    --  -90.00  59.00 166.60  100
 19  ω    -29.00  -1.00   0.25    0.40    --  -90.00  57.00  57.23  112
 20  ω    -89.00 -63.00   0.25    0.40    --  -90.00  58.00  12.14  104
 21  ω    -26.00  -1.00   0.25    0.40    --  -90.00  58.00  12.14  100
 22  ω    -27.00  -1.00   0.25    0.40    --  -90.00  58.00-161.94  104
 23  ω   -178.00-153.00   0.25    0.40    --  -90.00  59.00 -29.47  100
 24  ω    -94.00 -68.00   0.25    0.40    --  -90.00  59.00 147.02  104
 25  ω   -166.00-140.00   0.25    0.40    --  -90.00  59.00 147.02  104
 26  ω    -37.00  -1.00   0.25    0.40    --  -90.00  56.00 -89.58  144
 27  ω    -26.00  -1.00   0.25    0.40    --  -90.00  59.00-139.18  100
 28  ω   -101.00 -73.00   0.25    0.40    --  -90.00  59.00-139.18  112
 29  ω   -171.00-136.00   0.25    0.40    --  -90.00  56.00 -89.58  140
 30  ω    -39.00  -1.00   0.25    0.40    --  -90.00  58.00   6.86  152
 31  ω   -177.00-132.00   0.25    0.40    --  -90.00  59.00  72.77  180
 32  ω   -103.00 -69.00   0.25    0.40    --  -90.00  59.00  72.77  136
 33  ω    -63.00 -37.00   0.25    0.40    --  -90.00  59.00  72.77  104
 34  ω    -32.00  -1.00   0.25    0.40    --  -90.00  59.00  72.77  124
 35  ω    -93.00 -67.00   0.25    0.40    --  -90.00  59.00-132.79  104
 36  ω    -26.00  -1.00   0.25    0.40    --  -90.00  59.00-132.79  100
 37  ω   -165.00-139.00   0.25    0.40    --  -90.00  59.00  99.81  104
 38  ω    -59.00  -1.00   0.25    0.40    --  -90.00  59.00  99.81  232
 39  ω   -175.00-150.00   0.25    0.40    --  -90.00  59.00-174.95  100
 40  ω    -27.00  -1.00   0.25    0.40    --  -90.00  59.00-174.95  104
 41  ω    -26.00  -1.00   0.25    0.40    --  -90.00  59.00 -55.66  100
 42  ω   -129.00  -1.00   0.25    0.40    --  -90.00  56.00 135.76  512
 43  ω   -108.00 -81.00   0.25    0.40    --  -90.00  59.00 -55.66  108
 44  ω    -26.00  -1.00   0.25    0.40    --  -90.00  59.00 116.56  100
 45  ω    -34.00  -2.00   0.25    0.40    --  -90.00  59.00-151.78  128
 46  ω   -179.00  -1.00   0.25    0.40    --  -90.00  57.00  22.16  712
 47  ω    -72.00 -47.00   0.25    0.40    --  -90.00  58.00 157.00  100
 48  ω    -40.00  -1.00   0.25    0.40    --  -90.00  58.00 157.00  156
 49  ω    -27.00  -1.00   0.25    0.40    --  -90.00  57.00  85.87  104
 50  ω   -171.00  -2.00   0.25    0.40    --  -90.00  52.00 164.92  676
 51  ω    -26.00  -1.00   0.25    0.40    --  -90.00  59.00  32.89  100
 52  ω    -28.00  -1.00   0.25    0.40    --  -90.00  58.00  80.21  108
 53  ω   -104.00 -42.00   0.25    0.40    --  -90.00  59.00-151.78  248
 54  ω    -33.00  -1.00   0.25    0.40    --  -90.00  59.00  41.85  128
 55  ω   -106.00 -80.00   0.25    0.40    --  -90.00  57.00 -96.67  104
 56  ω    -27.00  -1.00   0.25    0.40    --  -90.00  56.00 -21.88  104
 57  ω    -94.00 -47.00   0.25    0.40    --  -90.00  58.00-107.33  188
 58  ω    -27.00  -1.00   0.25    0.40    --  -90.00  59.00 126.32  104
 59  ω   -125.00  -1.00   0.25    0.40    --  -90.00  54.00 -20.07  496
 60  ω    -26.00  -1.00   0.25    0.40    --  -90.00  58.00-107.33  100
 61  ω   -125.00  -1.00   0.25    0.40    --  -90.00  55.00  47.09  496
 62  ω   -136.00  -1.00   0.25    0.40    --  -90.00  57.00-170.25  540
 63  ω    -32.00  -1.00   0.25    0.40    --  -90.00  57.00 -96.67  124
 64  ω   -179.00  -2.00   0.25    0.40    --  -90.00  49.00 120.00  708
 65  ω   -178.00  -2.00   0.25    0.40    --  -90.00  58.00-127.37  704
 66  ω    -27.00  -1.00   0.25    0.40    --  -90.00  59.00 -29.47  104
 67  ω   -126.00  -1.00   0.25    0.40    --  -90.00  58.00  64.49  500
 68  ω   -105.00 -79.00   0.25    0.40    --  -90.00  58.00  80.21  104
 69  ω    -27.00  -1.00   0.25    0.40    --  -90.00  59.00-144.63  104
 70  ω   -154.00  -1.00   0.25    0.40    --  -90.00  49.00 -90.00  612
 71  ω   -134.00  -2.00   0.25    0.40    --  -90.00  49.00 -60.00  528
 72  ω    -86.00 -60.00   0.25    0.40    --  -90.00  58.00 105.68  104
 73  ω    -29.00  -2.00   0.25    0.40    --  -90.00  58.00 105.68  108
 74  ω    -79.00 -54.00   0.25    0.40    --  -90.00  58.00 -64.78  100
 75  ω    -30.00  -1.00   0.25    0.40    --  -90.00  58.00 -64.78  116
 76  ω    -27.00  -1.00   0.25    0.40    --  -90.00  59.00-117.41  104
 77  ω   -100.00 -56.00   0.25    0.40    --  -90.00  58.00   6.86  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with HF Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0044796000
_diffrn_orient_matrix_UB_12      -0.0009912000
_diffrn_orient_matrix_UB_13      -0.0496475000
_diffrn_orient_matrix_UB_21      -0.0020849000
_diffrn_orient_matrix_UB_22      -0.1074382000
_diffrn_orient_matrix_UB_23      0.0002185000
_diffrn_orient_matrix_UB_31      -0.0777694000
_diffrn_orient_matrix_UB_32      0.0027990000
_diffrn_orient_matrix_UB_33      -0.0090921000
_diffrn_radiation_collimation    'HF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                26231
_reflns_number_total             27185
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.812
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         27185
_refine_ls_number_restraints     656
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0658
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1084P)²+51.9555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1842
_refine_special_details          
'The system as currently presented does not charge balance (currently -0.5 for the asymmetric unit) with the required +0.5 charge assumed to come from a disordered Et3NH cation mixed in with the solvent water. Highly disordered solvent (assumed water (8 per asymmetric unit) along with half a EtNH cation) removed using SQUEEZE. The disordered hydrated Y that lies over a symmetry site required the use of various restraints (SADI, BUMP, RIGU, SIMU) and in the end was held as a rigid body.,Twin,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5197(13)
 0.4803(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Y1-H31A \\sim Y1-H31B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(O63) = Uanis(O58)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Y5, O56, O51, O52, O53, O57, O55, O54, O58, O62
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
6. Others
 Fixed Sof: Y5(0.5) O56(0.5) H56A(0.5) H56B(0.5) O51(0.5) H51A(0.5) H51B(0.5)
 O52(0.5) H52A(0.5) H52B(0.5) O53(0.5) H53A(0.5) H53B(0.5) O57(0.5) H57A(0.5)
 H57B(0.5) O55(0.5) H55A(0.5) H55B(0.5) O54(0.5) H54A(0.5) H54B(0.5) O58(0.5)
 H58A(0.5) H58B(0.5) O62(0.5) H62A(0.5) H62B(0.5) O63(0.5) H63A(0.5) H63B(0.5)
 O61(0.5) H61A(0.5) H61B(0.5)
7.a Free rotating group:
 O31(H31A,H31B), O64(H64A,H64B), Y5(O56,H56A,H56B,O51,H51A,H51B,O52,H52A,H52B,
 O53,H53A,H53B,O57,H57A,H57B,O55,H55A,H55B,O54,H54A,H54B,O58,H58A,H58B),
 O62(H62A,H62B,O63,H63A,H63B,O61,H61A,H61B)
7.b Rotating group:
 O32(H32A,H32B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C13(H13), C15(H15), C16(H16), C23(H23), C25(H25),
 C26(H26)
;
_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
Y1 Y 0.56539(3) 0.37442(3) 0.51756(2) 0.02955(16) Uani 1 1 d D . . . .
Ge1 Ge 0.26230(4) 0.15151(4) 0.29865(2) 0.03063(19) Uani 1 1 d . U . . .
O1 O 0.2590(2) 0.2833(3) 0.30024(13) 0.0367(10) Uani 1 1 d . U . . .
O2 O 0.3399(2) 0.1617(3) 0.34035(13) 0.0365(10) Uani 1 1 d . U . . .
O3 O 0.4959(2) 0.3442(3) 0.45316(13) 0.0375(10) Uani 1 1 d . U . . .
O4 O 0.4487(2) 0.4839(3) 0.45281(13) 0.0378(10) Uani 1 1 d . U . . .
O11 O 0.2672(2) 0.0191(3) 0.30353(12) 0.0323(9) Uani 1 1 d . U . . .
O12 O 0.2037(2) 0.1457(3) 0.34180(14) 0.0377(10) Uani 1 1 d . U . . .
O13 O 0.1142(2) -0.0189(3) 0.47142(13) 0.0357(9) Uani 1 1 d . U . . .
O14 O 0.1406(2) -0.1654(3) 0.46322(13) 0.0354(9) Uani 1 1 d . U . . .
O21 O 0.3183(2) 0.1437(3) 0.25367(13) 0.0367(10) Uani 1 1 d . U . . .
O22 O 0.1881(2) 0.1553(3) 0.25452(13) 0.0365(11) Uani 1 1 d . U . . .
O23 O 0.0898(2) 0.1732(3) 0.09316(13) 0.0409(10) Uani 1 1 d . U . . .
O24 O 0.1750(2) 0.1409(3) 0.05734(13) 0.0429(11) Uani 1 1 d . U . . .
O31 O 0.5544(3) 0.2110(3) 0.51587(15) 0.0493(12) Uani 1 1 d G . . . .
H31A H 0.565250 0.177281 0.539190 0.074 Uiso 1 1 d DG U . . .
H31B H 0.518946 0.183503 0.502331 0.074 Uiso 1 1 d DG U . . .
O32 O 0.4585(2) 0.3609(3) 0.54261(15) 0.0408(10) Uani 1 1 d . . . . .
H32A H 0.434951 0.414811 0.538637 0.061 Uiso 1 1 d R U . . .
H32B H 0.431950 0.319852 0.526105 0.061 Uiso 1 1 d R U . . .
C1 C 0.3054(3) 0.3175(4) 0.33209(19) 0.0348(13) Uani 1 1 d . U . . .
C2 C 0.3491(3) 0.2502(4) 0.35453(18) 0.0329(12) Uani 1 1 d . U . . .
C3 C 0.3964(3) 0.2772(4) 0.38911(18) 0.0340(13) Uani 1 1 d . U . . .
H3 H 0.425281 0.232558 0.404689 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4007(3) 0.3720(4) 0.4006(2) 0.0380(14) Uani 1 1 d . U . . .
C5 C 0.3594(4) 0.4363(4) 0.3776(2) 0.057(2) Uani 1 1 d . U . . .
H5 H 0.364650 0.500442 0.385126 0.068 Uiso 1 1 calc R U . . .
C6 C 0.3103(4) 0.4105(4) 0.3438(3) 0.058(2) Uani 1 1 d . U . . .
H6 H 0.280901 0.455690 0.329025 0.069 Uiso 1 1 calc R U . . .
C7 C 0.4508(3) 0.4031(4) 0.43727(18) 0.0346(13) Uani 1 1 d . U . . .
C11 C 0.2383(3) -0.0102(4) 0.33806(17) 0.0302(12) Uani 1 1 d . U . . .
C12 C 0.2040(3) 0.0595(4) 0.36015(18) 0.0315(12) Uani 1 1 d . U . . .
C13 C 0.1740(3) 0.0378(4) 0.39607(18) 0.0338(12) Uani 1 1 d . U . . .
H13 H 0.151840 0.084869 0.410749 0.041 Uiso 1 1 calc R U . . .
C14 C 0.1757(3) -0.0556(4) 0.41165(18) 0.0341(12) Uani 1 1 d . U . . .
C15 C 0.2098(4) -0.1235(4) 0.3902(2) 0.0394(14) Uani 1 1 d . U . . .
H15 H 0.211503 -0.185771 0.400769 0.047 Uiso 1 1 calc R U . . .
C16 C 0.2412(4) -0.1015(4) 0.3538(2) 0.0381(14) Uani 1 1 d . U . . .
H16 H 0.264468 -0.148218 0.339673 0.046 Uiso 1 1 calc R U . . .
C17 C 0.1436(3) -0.0824(4) 0.45045(18) 0.0369(13) Uani 1 1 d . U . . .
C21 C 0.2813(4) 0.1476(4) 0.21404(19) 0.0360(13) Uani 1 1 d . U . . .
C22 C 0.2122(4) 0.1557(4) 0.21370(19) 0.0361(13) Uani 1 1 d . U . . .
C23 C 0.1695(3) 0.1640(4) 0.17458(19) 0.0345(13) Uani 1 1 d . U . . .
H23 H 0.122216 0.173360 0.174269 0.041 Uiso 1 1 calc R U . . .
C24 C 0.1994(3) 0.1579(4) 0.13510(18) 0.0335(13) Uani 1 1 d . U . . .
C25 C 0.2666(4) 0.1461(4) 0.1353(2) 0.0400(14) Uani 1 1 d . U . . .
H25 H 0.284899 0.140026 0.108289 0.048 Uiso 1 1 calc R U . . .
C26 C 0.3101(4) 0.1427(4) 0.1751(2) 0.0385(14) Uani 1 1 d . U . . .
H26 H 0.357651 0.137208 0.175324 0.046 Uiso 1 1 calc R U . . .
C27 C 0.1538(3) 0.1593(4) 0.0932(2) 0.0385(14) Uani 1 1 d . U . . .
O64 O 0.4092(4) 0.0236(6) 0.3851(3) 0.108(3) Uani 1 1 d G . . . .
H64A H 0.450916 0.038024 0.382708 0.162 Uiso 1 1 d G U . . .
H64B H 0.385456 0.067273 0.370888 0.162 Uiso 1 1 d G U . . .
Y5 Y 0.45577(6) -0.10898(10) 0.25319(5) 0.0575(4) Uani 0.5 1 d G . P A -1
O56 O 0.4157(2) -0.2478(2) 0.22016(17) 0.064(2) Uani 0.5 1 d G . P A -1
H56A H 0.409559 -0.278400 0.196469 0.096 Uiso 0.5 1 d G U P A -1
H56B H 0.398700 -0.278979 0.239819 0.096 Uiso 0.5 1 d G U P A -1
O51 O 0.4356(2) 0.04754(14) 0.26850(18) 0.063(2) Uani 0.5 1 d G . P A -1
H51A H 0.453824 0.100261 0.265597 0.094 Uiso 0.5 1 d G U P A -1
H51B H 0.399204 0.056222 0.279967 0.094 Uiso 0.5 1 d G U P A -1
O52 O 0.4374(2) -0.1139(4) 0.32757(6) 0.066(2) Uani 0.5 1 d G . P A -1
H52A H 0.430011 -0.171077 0.332338 0.099 Uiso 0.5 1 d G U P A -1
H52B H 0.404423 -0.082336 0.335258 0.099 Uiso 0.5 1 d G U P A -1
O53 O 0.55751(14) -0.0424(3) 0.28928(16) 0.064(2) Uani 0.5 1 d G . P A -1
H53A H 0.547444 0.015049 0.289637 0.097 Uiso 0.5 1 d G U P A -1
H53B H 0.584402 -0.050272 0.269957 0.097 Uiso 0.5 1 d G U P A -1
O57 O 0.4170(2) -0.0646(4) 0.17955(7) 0.074(3) Uani 0.5 1 d G . P A -1
H57A H 0.450052 -0.030692 0.174467 0.112 Uiso 0.5 1 d G U P A -1
H57B H 0.382092 -0.046901 0.162548 0.112 Uiso 0.5 1 d G U P A -1
O55 O 0.54290(17) -0.1528(4) 0.20970(14) 0.055(2) Uani 0.5 1 d G . P A -1
H55A H 0.571900 -0.196124 0.209948 0.083 Uiso 0.5 1 d G U P A -1
H55B H 0.521191 -0.149963 0.183968 0.083 Uiso 0.5 1 d G U P A -1
O54 O 0.5081(2) -0.2415(3) 0.29234(16) 0.076(2) Uani 0.5 1 d G . P A -1
H54A H 0.506590 -0.252989 0.319228 0.114 Uiso 0.5 1 d G U P A -1
H54B H 0.523530 -0.289791 0.280679 0.114 Uiso 0.5 1 d G U P A -1
O58 O 0.33310(7) -0.1105(4) 0.25343(16) 0.0365(11) Uani 0.5 1 d G . P A -1
H58A H 0.315413 -0.056966 0.254678 0.055 Uiso 0.5 1 d G U P A -1
H58B H 0.309841 -0.141387 0.233158 0.055 Uiso 0.5 1 d G U P A -1
O62 O 0.5475(6) -0.1550(6) 0.1249(3) 0.086(4) Uani 0.5 1 d G . P B -1
H62A H 0.536601 -0.190053 0.101971 0.130 Uiso 0.5 1 d G U P B -1
H62B H 0.521501 -0.106243 0.120301 0.130 Uiso 0.5 1 d G U P B -1
O63 O 0.6678(4) -0.0913(6) 0.2538(3) 0.0365(11) Uani 0.5 1 d G . P B -1
H63A H 0.670110 -0.046133 0.272932 0.055 Uiso 0.5 1 d G U P B -1
H63B H 0.690380 -0.070903 0.233362 0.055 Uiso 0.5 1 d G U P B -1
O61 O 0.2950(4) 0.1614(5) 0.0206(3) 0.041(2) Uani 0.5 1 d G . P . .
H61A H 0.336442 0.161888 0.033411 0.061 Uiso 0.5 1 d G U P . .
H61B H 0.294512 0.144178 -0.006549 0.061 Uiso 0.5 1 d G 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
Y1 O3 2.313(4) . ?
Y1 O4 2.258(4) 5_666 ?
Y1 O13 2.375(4) 3 ?
Y1 O14 2.446(4) 3 ?
Y1 O23 2.415(4) 8_556 ?
Y1 O24 2.378(4) 8_556 ?
Y1 O31 2.352(4) . ?
Y1 O32 2.359(4) . ?
Y1 C17 2.805(6) 3 ?
Y1 C27 2.781(6) 8_556 ?
Ge1 O1 1.891(4) . ?
Ge1 O2 1.888(4) . ?
Ge1 O11 1.905(4) . ?
Ge1 O12 1.875(5) . ?
Ge1 O21 1.884(4) . ?
Ge1 O22 1.880(4) . ?
O1 C1 1.353(7) . ?
O2 C2 1.346(7) . ?
O3 C7 1.285(7) . ?
O4 C7 1.256(7) . ?
O11 C11 1.337(7) . ?
O12 C12 1.359(7) . ?
O13 C17 1.297(7) . ?
O14 C17 1.257(8) . ?
O21 C21 1.346(7) . ?
O22 C22 1.398(8) . ?
O23 C27 1.291(8) . ?
O24 C27 1.257(8) . ?
O31 H31A 0.8703 . ?
O31 H31B 0.8686 . ?
O32 H32A 0.9048 . ?
O32 H32B 0.9045 . ?
C1 C2 1.420(8) . ?
C1 C6 1.382(8) . ?
C2 C3 1.386(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.405(8) . ?
C4 C5 1.371(9) . ?
C4 C7 1.479(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(9) . ?
C6 H6 0.9500 . ?
C11 C12 1.428(8) . ?
C11 C16 1.394(8) . ?
C12 C13 1.356(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.421(8) . ?
C14 C15 1.398(8) . ?
C14 C17 1.473(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.383(9) . ?
C16 H16 0.9500 . ?
C21 C22 1.381(10) . ?
C21 C26 1.392(9) . ?
C22 C23 1.390(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.420(9) . ?
C24 C25 1.349(10) . ?
C24 C27 1.482(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.411(9) . ?
C26 H26 0.9500 . ?
O64 H64A 0.8694 . ?
O64 H64B 0.8698 . ?
Y5 O56 2.3296 . ?
Y5 O51 2.3376 . ?
Y5 O52 2.3621 . ?
Y5 O53 2.3866 . ?
Y5 O57 2.3874 . ?
Y5 O55 2.4018 . ?
Y5 O54 2.4152 . ?
Y5 O58 2.4447 . ?
O56 H56A 0.8466 . ?
O56 H56B 0.8552 . ?
O51 H51A 0.8480 . ?
O51 H51B 0.8534 . ?
O52 H52A 0.8483 . ?
O52 H52B 0.8548 . ?
O53 H53A 0.8477 . ?
O53 H53B 0.8552 . ?
O57 H57A 0.8485 . ?
O57 H57B 0.8550 . ?
O55 H55A 0.8479 . ?
O55 H55B 0.8547 . ?
O54 H54A 0.8473 . ?
O54 H54B 0.8546 . ?
O58 H58A 0.8473 . ?
O58 H58B 0.8533 . ?
O62 H62A 0.8711 . ?
O62 H62B 0.8711 . ?
O63 H63A 0.8715 . ?
O63 H63B 0.8681 . ?
O61 H61A 0.8701 . ?
O61 H61B 0.8699 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Y1 O13 81.66(15) . 3 ?
O3 Y1 O14 73.96(15) . 3 ?
O3 Y1 O23 143.09(16) . 8_556 ?
O3 Y1 O24 146.92(16) . 8_556 ?
O3 Y1 O31 75.52(16) . . ?
O3 Y1 O32 78.20(16) . . ?
O3 Y1 C17 74.90(17) . 3 ?
O3 Y1 C27 159.05(17) . 8_556 ?
O4 Y1 O3 115.03(15) 5_666 . ?
O4 Y1 O13 75.06(14) 5_666 3 ?
O4 Y1 O14 127.08(15) 5_666 3 ?
O4 Y1 O23 83.45(15) 5_666 8_556 ?
O4 Y1 O24 91.57(16) 5_666 8_556 ?
O4 Y1 O31 152.70(17) 5_666 . ?
O4 Y1 O32 77.28(16) 5_666 . ?
O4 Y1 C17 101.92(17) 5_666 3 ?
O4 Y1 C27 85.19(17) 5_666 8_556 ?
O13 Y1 O14 53.96(13) 3 3 ?
O13 Y1 O23 135.16(14) 3 8_556 ?
O13 Y1 O24 87.09(15) 3 8_556 ?
O13 Y1 C17 27.42(16) 3 3 ?
O13 Y1 C27 110.37(17) 3 8_556 ?
O14 Y1 C17 26.60(16) 3 3 ?
O14 Y1 C27 98.79(17) 3 8_556 ?
O23 Y1 O14 121.64(15) 8_556 3 ?
O23 Y1 C17 135.00(16) 8_556 3 ?
O23 Y1 C27 27.63(18) 8_556 8_556 ?
O24 Y1 O14 74.27(14) 8_556 3 ?
O24 Y1 O23 54.24(15) 8_556 8_556 ?
O24 Y1 C17 80.83(16) 8_556 3 ?
O24 Y1 C27 26.76(18) 8_556 8_556 ?
O31 Y1 O13 132.24(16) . 3 ?
O31 Y1 O14 79.40(16) . 3 ?
O31 Y1 O23 75.33(16) . 8_556 ?
O31 Y1 O24 89.83(18) . 8_556 ?
O31 Y1 O32 80.78(17) . . ?
O31 Y1 C17 105.22(18) . 3 ?
O31 Y1 C27 83.88(17) . 8_556 ?
O32 Y1 O13 134.46(15) . 3 ?
O32 Y1 O14 149.04(15) . 3 ?
O32 Y1 O23 75.21(16) . 8_556 ?
O32 Y1 O24 129.24(16) . 8_556 ?
O32 Y1 C17 149.78(17) . 3 ?
O32 Y1 C27 102.49(18) . 8_556 ?
C27 Y1 C17 107.57(19) 8_556 3 ?
O1 Ge1 O11 174.04(16) . . ?
O2 Ge1 O1 86.18(16) . . ?
O2 Ge1 O11 89.66(17) . . ?
O12 Ge1 O1 89.94(19) . . ?
O12 Ge1 O2 93.0(2) . . ?
O12 Ge1 O11 86.01(17) . . ?
O12 Ge1 O21 173.65(19) . . ?
O12 Ge1 O22 90.54(19) . . ?
O21 Ge1 O1 96.0(2) . . ?
O21 Ge1 O2 89.70(19) . . ?
O21 Ge1 O11 88.24(18) . . ?
O22 Ge1 O1 87.85(18) . . ?
O22 Ge1 O2 173.1(2) . . ?
O22 Ge1 O11 96.54(18) . . ?
O22 Ge1 O21 87.44(19) . . ?
C1 O1 Ge1 110.9(3) . . ?
C2 O2 Ge1 111.1(3) . . ?
C7 O3 Y1 121.3(3) . . ?
C7 O4 Y1 174.3(4) . 5_666 ?
C11 O11 Ge1 110.7(3) . . ?
C12 O12 Ge1 111.3(4) . . ?
C17 O13 Y1 95.1(4) . 3_445 ?
C17 O14 Y1 92.8(4) . 3_445 ?
C21 O21 Ge1 110.8(4) . . ?
C22 O22 Ge1 108.8(4) . . ?
C27 O23 Y1 92.2(4) . 8_455 ?
C27 O24 Y1 94.8(4) . 8_455 ?
Y1 O31 H31A 121.5 . . ?
Y1 O31 H31B 122.1 . . ?
H31A O31 H31B 104.3 . . ?
Y1 O32 H32A 111.1 . . ?
Y1 O32 H32B 111.1 . . ?
H32A O32 H32B 102.8 . . ?
O1 C1 C2 115.4(5) . . ?
O1 C1 C6 124.0(5) . . ?
C6 C1 C2 120.6(5) . . ?
O2 C2 C1 115.5(5) . . ?
O2 C2 C3 124.3(5) . . ?
C3 C2 C1 120.1(5) . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.5(5) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 C7 119.8(6) . . ?
C5 C4 C3 120.4(5) . . ?
C5 C4 C7 119.7(5) . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 122.0(6) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 118.2(6) . . ?
C1 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
O3 C7 C4 117.8(5) . . ?
O4 C7 O3 121.0(5) . . ?
O4 C7 C4 121.1(6) . . ?
O11 C11 C12 115.8(5) . . ?
O11 C11 C16 124.6(5) . . ?
C16 C11 C12 119.5(5) . . ?
O12 C12 C11 114.7(5) . . ?
C13 C12 O12 124.5(5) . . ?
C13 C12 C11 120.8(5) . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.7(5) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C17 121.6(5) . . ?
C15 C14 C13 119.3(6) . . ?
C15 C14 C17 119.1(6) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.2(6) . . ?
C16 C15 H15 119.4 . . ?
C11 C16 H16 120.3 . . ?
C15 C16 C11 119.4(5) . . ?
C15 C16 H16 120.3 . . ?
O13 C17 Y1 57.5(3) . 3_445 ?
O13 C17 C14 119.2(6) . . ?
O14 C17 Y1 60.6(3) . 3_445 ?
O14 C17 O13 117.9(6) . . ?
O14 C17 C14 122.8(5) . . ?
C14 C17 Y1 172.0(4) . 3_445 ?
O21 C21 C22 116.4(6) . . ?
O21 C21 C26 122.7(6) . . ?
C22 C21 C26 120.9(6) . . ?
C21 C22 O22 116.4(5) . . ?
C21 C22 C23 121.1(6) . . ?
C23 C22 O22 122.5(6) . . ?
C22 C23 H23 121.4 . . ?
C22 C23 C24 117.3(6) . . ?
C24 C23 H23 121.4 . . ?
C23 C24 C27 117.7(6) . . ?
C25 C24 C23 121.7(6) . . ?
C25 C24 C27 120.4(6) . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.6(6) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 118.1(7) . . ?
C21 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
O23 C27 Y1 60.2(3) . 8_455 ?
O23 C27 C24 120.2(6) . . ?
O24 C27 Y1 58.4(3) . 8_455 ?
O24 C27 O23 118.1(6) . . ?
O24 C27 C24 121.6(6) . . ?
C24 C27 Y1 169.0(4) . 8_455 ?
H64A O64 H64B 104.5 . . ?
O56 Y5 O51 148.1 . . ?
O56 Y5 O52 108.1 . . ?
O56 Y5 O53 140.3 . . ?
O56 Y5 O57 76.1 . . ?
O56 Y5 O55 76.5 . . ?
O56 Y5 O54 69.5 . . ?
O56 Y5 O58 72.8 . . ?
O51 Y5 O52 77.4 . . ?
O51 Y5 O53 71.3 . . ?
O51 Y5 O57 83.8 . . ?
O51 Y5 O55 121.1 . . ?
O51 Y5 O54 136.8 . . ?
O51 Y5 O58 79.1 . . ?
O52 Y5 O53 77.6 . . ?
O52 Y5 O57 148.9 . . ?
O52 Y5 O55 137.8 . . ?
O52 Y5 O54 66.6 . . ?
O52 Y5 O58 73.9 . . ?
O53 Y5 O57 119.4 . . ?
O53 Y5 O55 74.5 . . ?
O53 Y5 O54 78.1 . . ?
O53 Y5 O58 142.6 . . ?
O57 Y5 O55 73.3 . . ?
O57 Y5 O54 138.7 . . ?
O57 Y5 O58 78.4 . . ?
O55 Y5 O54 77.0 . . ?
O55 Y5 O58 142.2 . . ?
O54 Y5 O58 111.2 . . ?
Y5 O56 H56A 145.5 . . ?
Y5 O56 H56B 106.4 . . ?
H56A O56 H56B 108.0 . . ?
Y5 O51 H51A 138.4 . . ?
Y5 O51 H51B 113.5 . . ?
H51A O51 H51B 108.1 . . ?
Y5 O52 H52A 104.3 . . ?
Y5 O52 H52B 117.9 . . ?
H52A O52 H52B 108.0 . . ?
Y5 O53 H53A 101.9 . . ?
Y5 O53 H53B 101.1 . . ?
H53A O53 H53B 107.9 . . ?
Y5 O57 H57A 99.2 . . ?
Y5 O57 H57B 143.4 . . ?
H57A O57 H57B 108.0 . . ?
Y5 O55 H55A 136.5 . . ?
Y5 O55 H55B 100.7 . . ?
H55A O55 H55B 108.0 . . ?
Y5 O54 H54A 125.1 . . ?
Y5 O54 H54B 125.7 . . ?
H54A O54 H54B 108.0 . . ?
Y5 O58 H58A 114.4 . . ?
Y5 O58 H58B 117.1 . . ?
H58A O58 H58B 108.2 . . ?
H62A O62 H62B 104.3 . . ?
H63A O63 H63B 104.5 . . ?
H61A O61 H61B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O3 C7 O4 9.5(8) . . . . ?
Y1 O3 C7 C4 -169.4(4) . . . . ?
Y1 O13 C17 O14 -5.3(6) 3_445 . . . ?
Y1 O13 C17 C14 171.4(5) 3_445 . . . ?
Y1 O14 C17 O13 5.2(5) 3_445 . . . ?
Y1 O14 C17 C14 -171.5(5) 3_445 . . . ?
Y1 O23 C27 O24 8.0(6) 8_455 . . . ?
Y1 O23 C27 C24 -167.3(5) 8_455 . . . ?
Y1 O24 C27 O23 -8.1(6) 8_455 . . . ?
Y1 O24 C27 C24 167.1(5) 8_455 . . . ?
Ge1 O1 C1 C2 4.8(7) . . . . ?
Ge1 O1 C1 C6 -173.5(7) . . . . ?
Ge1 O2 C2 C1 -7.4(7) . . . . ?
Ge1 O2 C2 C3 171.3(5) . . . . ?
Ge1 O11 C11 C12 6.9(6) . . . . ?
Ge1 O11 C11 C16 -171.4(5) . . . . ?
Ge1 O12 C12 C11 -10.4(6) . . . . ?
Ge1 O12 C12 C13 170.7(5) . . . . ?
Ge1 O21 C21 C22 -0.3(6) . . . . ?
Ge1 O21 C21 C26 -179.6(5) . . . . ?
Ge1 O22 C22 C21 3.9(6) . . . . ?
Ge1 O22 C22 C23 -176.0(4) . . . . ?
O1 Ge1 O2 C2 8.0(4) . . . . ?
O1 Ge1 O12 C12 -164.3(4) . . . . ?
O1 Ge1 O21 C21 -85.6(4) . . . . ?
O1 Ge1 O22 C22 92.9(4) . . . . ?
O1 C1 C2 O2 1.8(9) . . . . ?
O1 C1 C2 C3 -177.0(6) . . . . ?
O1 C1 C6 C5 178.8(8) . . . . ?
O2 Ge1 O1 C1 -7.0(4) . . . . ?
O2 Ge1 O12 C12 -78.1(4) . . . . ?
O2 Ge1 O21 C21 -171.7(4) . . . . ?
O2 C2 C3 C4 -179.9(6) . . . . ?
O11 Ge1 O2 C2 -167.7(4) . . . . ?
O11 Ge1 O12 C12 11.4(4) . . . . ?
O11 Ge1 O21 C21 98.6(4) . . . . ?
O11 Ge1 O22 C22 -91.1(4) . . . . ?
O11 C11 C12 O12 2.3(7) . . . . ?
O11 C11 C12 C13 -178.8(5) . . . . ?
O11 C11 C16 C15 179.3(6) . . . . ?
O12 Ge1 O1 C1 85.9(4) . . . . ?
O12 Ge1 O2 C2 -81.7(4) . . . . ?
O12 Ge1 O22 C22 -177.2(4) . . . . ?
O12 C12 C13 C14 178.0(5) . . . . ?
O21 Ge1 O1 C1 -96.3(4) . . . . ?
O21 Ge1 O2 C2 104.0(4) . . . . ?
O21 Ge1 O22 C22 -3.2(4) . . . . ?
O21 C21 C22 O22 -2.5(7) . . . . ?
O21 C21 C22 C23 177.5(5) . . . . ?
O21 C21 C26 C25 179.1(5) . . . . ?
O22 Ge1 O1 C1 176.5(4) . . . . ?
O22 Ge1 O12 C12 107.9(4) . . . . ?
O22 Ge1 O21 C21 2.0(4) . . . . ?
O22 C22 C23 C24 -176.3(5) . . . . ?
C1 C2 C3 C4 -1.2(10) . . . . ?
C2 C1 C6 C5 0.6(12) . . . . ?
C2 C3 C4 C5 -0.9(11) . . . . ?
C2 C3 C4 C7 -179.8(6) . . . . ?
C3 C4 C5 C6 2.9(13) . . . . ?
C3 C4 C7 O3 10.4(9) . . . . ?
C3 C4 C7 O4 -168.5(6) . . . . ?
C4 C5 C6 C1 -2.7(14) . . . . ?
C5 C4 C7 O3 -168.5(7) . . . . ?
C5 C4 C7 O4 12.6(11) . . . . ?
C6 C1 C2 O2 -179.9(7) . . . . ?
C6 C1 C2 C3 1.4(11) . . . . ?
C7 C4 C5 C6 -178.2(8) . . . . ?
C11 C12 C13 C14 -0.8(9) . . . . ?
C12 C11 C16 C15 1.1(9) . . . . ?
C12 C13 C14 C15 1.4(9) . . . . ?
C12 C13 C14 C17 -179.8(5) . . . . ?
C13 C14 C15 C16 -0.7(10) . . . . ?
C13 C14 C17 O13 -1.4(9) . . . . ?
C13 C14 C17 O14 175.3(6) . . . . ?
C14 C15 C16 C11 -0.5(10) . . . . ?
C15 C14 C17 O13 177.4(6) . . . . ?
C15 C14 C17 O14 -6.0(9) . . . . ?
C16 C11 C12 O12 -179.4(5) . . . . ?
C16 C11 C12 C13 -0.4(9) . . . . ?
C17 C14 C15 C16 -179.5(6) . . . . ?
C21 C22 C23 C24 3.8(8) . . . . ?
C22 C21 C26 C25 -0.2(9) . . . . ?
C22 C23 C24 C25 -1.1(8) . . . . ?
C22 C23 C24 C27 175.4(5) . . . . ?
C23 C24 C25 C26 -2.2(9) . . . . ?
C23 C24 C27 Y1 -83(3) . . . 8_455 ?
C23 C24 C27 O23 5.4(8) . . . . ?
C23 C24 C27 O24 -169.6(6) . . . . ?
C24 C25 C26 C21 2.9(9) . . . . ?
C25 C24 C27 Y1 93(3) . . . 8_455 ?
C25 C24 C27 O23 -178.0(6) . . . . ?
C25 C24 C27 O24 6.9(9) . . . . ?
C26 C21 C22 O22 176.9(5) . . . . ?
C26 C21 C22 C23 -3.2(8) . . . . ?
C27 C24 C25 C26 -178.6(5) . . . . ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 'ST L3-Ge + Y'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_oxdiff_twin_integration_method  simultaneous
_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 0.5197(13) 64953 90779 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4803(13) 65035 90779 nmt -0.9995 0.0001 0.0001 -0.0000 -1.0001 -0.0000
0.3808 -0.0001 1.0000

_twin_special_details            
;
Component 2 rotated by 179.9990° 
around [0.00 -0.00 1.00] (reciprocal) or [0.19 -0.00 0.98] (direct)
;
####################################################################### 
# 
# 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_IMP33Sc
_database_code_depnum_ccdc_archive 'CCDC 2348717'
loop_
_audit_author_name
_audit_author_address
'Peter Horton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-07-14 downloaded from the CCDC.
;

#2022ncs0357_3b

_audit_creation_date             2023-04-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
r.davies@imperial.ac.uk
pnh@soton.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C42 H30 Ge2 O30 Sc3, C6 H16 N, 6[C2H3N], 9[H2O]'
_chemical_formula_sum            'C60 H82 Ge2 N7 O39 Sc3'
_chemical_formula_weight         1805.38
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H43 Ge N2 O12 Sc'
_chemical_oxdiff_usercomment     'ST L3-Ge + Sc'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   25.1090(8)
_cell_length_b                   13.1102(2)
_cell_length_c                   27.1137(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.410(3)
_cell_angle_gamma                90
_cell_volume                     8516.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    57319
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9910
_cell_measurement_theta_min      2.2410
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.888
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.66a (Rigaku Oxford Diffraction, 2022)
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    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3720
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of MeCN and water'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            203984
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.701
_diffrn_reflns_theta_min         2.076
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     58.00  97.00   0.25   16.00    --   15.93  12.00 118.00  156
  2  ω    -56.00   2.00   0.25   16.00    --  -12.81 -57.00-120.00  232
  3  ω     21.00  68.00   0.25   16.00    --  -12.81  19.00 -90.00  188
  4  ω    -56.00   2.00   0.25   16.00    --  -12.81 -57.00-180.00  232
  5  ω     21.00  68.00   0.25   16.00    --  -12.81  19.00-150.00  188
  6  ω    -36.00  24.00   0.25   16.00    --  -12.81  77.00-120.00  240
  7  ω    -56.00   2.00   0.25   16.00    --  -12.81 -57.00  90.00  232
  8  ω      1.00  62.00   0.25   16.00    --   15.93  57.00 120.00  244
  9  ω     10.00  43.00   0.25   16.00    --   15.93 -99.00   0.00  132
 10  ω      6.00  33.00   0.25   16.00    --   15.93  57.00-180.00  108
 11  ω    -64.00 -39.00   0.25   16.00    --  -12.81 132.00 150.08  100
 12  ω    -68.00 -43.00   0.25   16.00    --  -12.81 137.00  96.90  100
 13  ω    -64.00 -39.00   0.25   16.00    --  -12.81 132.00 179.03  100
 14  ω    -48.00 -23.00   0.25   16.00    --  -12.81 103.00 151.90  100
 15  ω    -32.00  13.00   0.25   16.00    --  -12.81  88.00 125.10  180
 16  ω    -65.00 -40.00   0.25   16.00    --  -12.81 134.00-149.65  100
 17  ω    -68.00 -43.00   0.25   16.00    --  -12.81 137.00-167.14  100
 18  ω    -68.00 -43.00   0.25   16.00    --  -12.81 138.00 117.87  100
 19  ω     27.00  91.00   0.25   16.00    --   15.93  19.00-150.00  256
 20  ω    -13.00  12.00   0.25   16.00    --   15.93  89.00   0.15  100
 21  ω    -15.00  10.00   0.25   16.00    --   15.93  93.00  75.27  100
 22  ω    -42.00  -9.00   0.25   16.00    --  -12.81  90.00  32.57  132
 23  ω      0.00  49.00   0.25   16.00    --   15.93 -99.00  60.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ diffractometer with Arc)Sec VHF Varimax confocal mirrors, a UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0293036000
_diffrn_orient_matrix_UB_12      0.0073515000
_diffrn_orient_matrix_UB_13      -0.0093297000
_diffrn_orient_matrix_UB_21      0.0017802000
_diffrn_orient_matrix_UB_22      0.0049275000
_diffrn_orient_matrix_UB_23      -0.0254972000
_diffrn_orient_matrix_UB_31      -0.0038983000
_diffrn_orient_matrix_UB_32      -0.0533845000
_diffrn_orient_matrix_UB_33      -0.0036645000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, Arc)Sec VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                37435
_reflns_number_total             43773
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.66a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.66a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.66a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.366
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.499(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1534
_refine_ls_number_reflns         43773
_refine_ls_number_restraints     5139
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0683
_refine_ls_restrained_S_all      1.368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1195P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.1823
_refine_special_details          
;Solvent masking was employed. Crystal was an inversion twin.
Various restraints (DFIX, SADI, RIGU and SIMU) were employed,SQUEEZE
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.501(8)
 0.499(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O153-H15E = O153-H15F = O152-H15C = O152-H15D = O151-H15B = O151-H15A = O154-
 H15H = O154-H15G = O155-H15I = O155-H15J = O156-H15K = O156-H15L = O157-H15N =
 O157-H15M = O158-H15O = O158-H15P = O159-H15Q = O159-H15R = O161-H16C = O161-
 H16D = O160-H16B = O160-H16A = O162-H16E = O162-H16F
 0.87 with sigma of 0.02
 Sc4-H15K \\sim Sc4-H15L
 with sigma of 0.02
 C52-C51 \\sim C42-C41 \\sim C32-C31 \\sim C72-C71 \\sim C12-C11 \\sim C22-C21
\\sim C102-C101 \\sim C112-
 C111 \\sim C92-C91 \\sim C82-C81 \\sim C62-C61 \\sim C2-C1
 with sigma of 0.02
 C73-C72 \\sim C77-C72 \\sim C77-C76 \\sim C76-C75 \\sim C75-C74 \\sim C74-C73
\\sim C84-C83 \\sim C85-C84
 \\sim C86-C85 \\sim C87-C86 \\sim C87-C82 \\sim C83-C82 \\sim C66-C65 \\sim
C67-C66 \\sim C67-C62 \\sim C63-
 C62 \\sim C64-C63 \\sim C65-C64 \\sim C113-C112 \\sim C114-C113 \\sim
C115-C114 \\sim C116-C115 \\sim C117-
 C116 \\sim C117-C112 \\sim C106-C105 \\sim C105-C104 \\sim C104-C103 \\sim
C103-C102 \\sim C107-C102 ~
 C107-C106 \\sim C96-C95 \\sim C97-C96 \\sim C97-C92 \\sim C93-C92 \\sim
C94-C93 \\sim C95-C94 \\sim C16-
 C15 \\sim C15-C14 \\sim C14-C13 \\sim C13-C12 \\sim C17-C12 \\sim C17-C16
\\sim C26-C25 \\sim C25-C24 ~
 C24-C23 \\sim C23-C22 \\sim C27-C22 \\sim C27-C26 \\sim C4-C3 \\sim C3-C2
\\sim C7-C2 \\sim C7-C6 \\sim C6-C5
 \\sim C5-C4 \\sim C33-C32 \\sim C34-C33 \\sim C35-C34 \\sim C36-C35 \\sim
C37-C36 \\sim C37-C32 \\sim C46-C45
 \\sim C47-C46 \\sim C47-C42 \\sim C43-C42 \\sim C44-C43 \\sim C45-C44 \\sim
C54-C53 \\sim C55-C54 \\sim C56-
 C55 \\sim C57-C56 \\sim C57-C52 \\sim C53-C52
 with sigma of 0.02
 C122-C121 \\sim C124-C123 \\sim C126-C125 \\sim C136-C135 \\sim C134-C133
\\sim C132-C131
 with sigma of 0.02
 N131-C131 \\sim N131-C135 \\sim N131-C133 \\sim N121-C121 \\sim N121-C123
\\sim N121-C125
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
6.a Free rotating group:
 O156(H15K,H15L)
6.b Rotating group:
 O151(H15A,H15B), O152(H15C,H15D), O153(H15E,H15F), O154(H15G,H15H), O155(H15I,
 H15J), O157(H15M,H15N), O158(H15O,H15P), O159(H15Q,H15R), O160(H16A,H16B),
 O161(H16C,H16D), O162(H16E,H16F)
6.c Ternary CH refined with riding coordinates:
 N121(H121), N131(H131)
6.d Secondary CH2 refined with riding coordinates:
 C121(H12A,H12B), C123(H12F,H12G), C125(H12K,H12L), C131(H13A,H13B), C133(H13F,
 H13G), C135(H13K,H13L)
6.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C13(H13), C16(H16), C17(H17), C23(H23), C26(H26),
 C27(H27), C33(H33), C36(H36), C37(H37), C43(H43), C46(H46), C47(H47), C53(H53),
  C56(H56), C57(H57), C63(H63), C66(H66), C67(H67), C73(H73), C76(H76),
 C77(H77), C83(H83), C86(H86), C87(H87), C93(H93), C96(H96), C97(H97),
 C103(H103), C106(H106), C107(H107), C113(H113), C116(H116), C117(H117)
6.f Idealised Me refined as rotating group:
 C122(H12C,H12D,H12E), C124(H12H,H12I,H12J), C126(H12M,H12N,H12O), C132(H13C,
 H13D,H13E), C134(H13H,H13I,H13J), C136(H13M,H13N,H13O)
;
_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 0.83952(3) 0.42692(5) 0.39575(3) 0.01811(15) Uani 1 1 d . U . . .
Ge2 Ge 0.61622(5) 0.11273(7) 0.11800(3) 0.0393(2) Uani 1 1 d . U . . .
Ge3 Ge 0.08135(3) 0.56832(5) 0.09641(3) 0.02128(16) Uani 1 1 d . U . . .
Ge4 Ge 0.37860(3) 0.98432(5) 0.40546(3) 0.02009(16) Uani 1 1 d . U . . .
Sc1 Sc 0.46788(6) 0.54491(9) 0.24018(5) 0.0185(3) Uani 1 1 d . U . . .
Sc2 Sc 1.10319(5) 0.28863(9) 0.66652(5) 0.0158(2) Uani 1 1 d . . . . .
Sc3 Sc 0.98904(6) -0.00535(9) 0.26329(5) 0.0172(2) Uani 1 1 d . U . . .
Sc4 Sc 0.43466(7) 0.24602(10) -0.17227(6) 0.0251(3) Uani 1 1 d D . . . .
Sc5 Sc -0.07745(6) 0.72586(9) -0.20065(5) 0.0184(3) Uani 1 1 d . . . . .
Sc6 Sc 0.60810(6) 0.82915(10) 0.68168(5) 0.0220(3) Uani 1 1 d . U . . .
O1 O 0.5475(2) 0.5684(4) 0.2533(2) 0.0315(11) Uani 1 1 d . U . . .
O2 O 0.6142(2) 0.6504(5) 0.2293(2) 0.0333(13) Uani 1 1 d . U . . .
O3 O 0.7964(2) 0.4976(4) 0.33988(18) 0.0191(7) Uani 1 1 d . U . . .
O4 O 0.7725(2) 0.3565(3) 0.39504(18) 0.0171(7) Uani 1 1 d . U . . .
O11 O 1.0164(2) 0.5098(3) 0.66136(18) 0.0205(9) Uani 1 1 d . U . . .
O12 O 1.0376(2) 0.3748(3) 0.62515(18) 0.0196(8) Uani 1 1 d . U . . .
O13 O 0.8784(2) 0.3496(4) 0.45481(19) 0.0205(8) Uani 1 1 d . U . . .
O14 O 0.8323(2) 0.5261(3) 0.44007(19) 0.0185(7) Uani 1 1 d . U . . .
O21 O 1.0306(2) 0.2650(4) 0.2484(2) 0.0268(10) Uani 1 1 d . U . . .
O22 O 0.9707(2) 0.1422(4) 0.2518(2) 0.0228(9) Uani 1 1 d . U . . .
O23 O 0.8526(2) 0.3135(3) 0.35370(19) 0.0198(7) Uani 1 1 d . U . . .
O24 O 0.9035(2) 0.4839(4) 0.38707(19) 0.0209(7) Uani 1 1 d . U . . .
O31 O 0.4243(3) 0.2729(4) 0.2611(2) 0.0361(12) Uani 1 1 d . U . . .
O32 O 0.4878(3) 0.3876(4) 0.2544(2) 0.0301(10) Uani 1 1 d . U . . .
O33 O 0.6000(3) 0.2164(4) 0.1523(2) 0.0331(9) Uani 1 1 d . U . . .
O34 O 0.5535(3) 0.0400(4) 0.1302(2) 0.0291(8) Uani 1 1 d . U . . .
O41 O 0.9057(2) -0.0480(4) 0.2374(2) 0.0267(9) Uani 1 1 d . U . . .
O42 O 0.8503(2) -0.1116(4) 0.2807(2) 0.0258(10) Uani 1 1 d . U . . .
O43 O 0.6605(3) 0.0350(4) 0.1754(2) 0.0308(9) Uani 1 1 d . U . . .
O44 O 0.6813(3) 0.1677(5) 0.1155(2) 0.0346(9) Uani 1 1 d . U . . .
O51 O 0.5399(3) 0.0147(5) -0.1612(2) 0.0476(16) Uani 1 1 d . U . . .
O52 O 0.4923(3) 0.1345(4) -0.1372(2) 0.0333(11) Uani 1 1 d . U . . .
O53 O 0.5716(3) 0.1577(5) 0.0545(2) 0.0377(11) Uani 1 1 d . U . . .
O54 O 0.6295(3) -0.0119(5) 0.0820(2) 0.0411(11) Uani 1 1 d . U . . .
O61 O 0.3851(2) 0.5068(4) 0.2281(2) 0.0304(10) Uani 1 1 d . U . . .
O62 O 0.3334(2) 0.4128(5) 0.2650(2) 0.0359(13) Uani 1 1 d . U . . .
O63 O 0.1321(2) 0.5012(4) 0.15534(19) 0.0261(8) Uani 1 1 d . U . . .
O64 O 0.1424(2) 0.6240(4) 0.08663(18) 0.0232(8) Uani 1 1 d . U . . .
O71 O 0.0093(3) 0.4734(4) -0.1886(2) 0.0322(12) Uani 1 1 d . U . . .
O72 O -0.0325(2) 0.5981(4) -0.16574(19) 0.0241(9) Uani 1 1 d . U . . .
O73 O 0.0359(2) 0.6098(3) 0.03430(18) 0.0213(8) Uani 1 1 d . U . . .
O74 O 0.0888(2) 0.4397(4) 0.05718(18) 0.0216(8) Uani 1 1 d . U . . .
O81 O -0.0570(3) 0.7319(4) 0.2881(3) 0.0367(13) Uani 1 1 d . U . . .
O82 O 0.0026(2) 0.8351(4) 0.2747(2) 0.0264(11) Uani 1 1 d . U . . .
O83 O 0.0675(2) 0.6728(4) 0.13458(19) 0.0224(8) Uani 1 1 d . U . . .
O84 O 0.0229(2) 0.4994(3) 0.11767(19) 0.0212(7) Uani 1 1 d . U . . .
O91 O 0.5213(2) 0.7990(3) 0.2199(2) 0.0219(9) Uani 1 1 d . U . . .
O92 O 0.4537(2) 0.6941(3) 0.22555(19) 0.0209(9) Uani 1 1 d . U . . .
O93 O 0.3870(2) 0.8666(3) 0.3668(2) 0.0221(8) Uani 1 1 d . U . . .
O94 O 0.4346(2) 1.0410(4) 0.3824(2) 0.0221(8) Uani 1 1 d . U . . .
O101 O 0.5201(2) 1.0745(4) 0.6808(2) 0.0253(10) Uani 1 1 d . U . . .
O102 O 0.5538(2) 0.9404(4) 0.6510(2) 0.0289(10) Uani 1 1 d . U . . .
O103 O 0.4297(2) 0.9206(4) 0.46497(19) 0.0219(8) Uani 1 1 d . U . . .
O104 O 0.3753(2) 1.0834(4) 0.44693(19) 0.0238(8) Uani 1 1 d . U . . .
O111 O 0.0731(2) 1.0243(3) 0.29078(19) 0.0208(9) Uani 1 1 d . U . . .
O112 O 0.1244(2) 1.1355(4) 0.2609(2) 0.0274(11) Uani 1 1 d . U . . .
O113 O 0.3219(2) 1.0372(4) 0.34961(19) 0.0214(8) Uani 1 1 d . U . . .
O114 O 0.3193(2) 0.9084(3) 0.42379(19) 0.0200(7) Uani 1 1 d . U . . .
O151 O 1.0754(2) 0.1703(4) 0.60687(19) 0.0244(10) Uani 1 1 d D . . . .
H15A H 1.073406 0.110865 0.621081 0.037 Uiso 1 1 d DR U . . .
H15B H 1.100802 0.161443 0.590969 0.037 Uiso 1 1 d DR U . . .
O152 O 1.1493(2) 0.3445(4) 0.6177(2) 0.0289(11) Uani 1 1 d D . . . .
H15C H 1.169176 0.403264 0.621158 0.043 Uiso 1 1 d DR U . . .
H15D H 1.153206 0.315883 0.588537 0.043 Uiso 1 1 d DR U . . .
O153 O 1.1649(3) 0.1712(5) 0.6977(2) 0.0350(13) Uani 1 1 d D . . . .
H15E H 1.150784 0.109555 0.687538 0.053 Uiso 1 1 d DR U . . .
H15F H 1.173056 0.168267 0.732063 0.053 Uiso 1 1 d DR U . . .
O154 O 0.4700(3) 0.3439(4) -0.1124(3) 0.0426(15) Uani 1 1 d D . . . .
H15G H 0.498590 0.377088 -0.118448 0.064 Uiso 1 1 d DR U . . .
H15H H 0.486191 0.309980 -0.083097 0.064 Uiso 1 1 d DR U . . .
O155 O 0.3893(3) 0.1855(4) -0.1246(3) 0.0390(14) Uani 1 1 d D . . . .
H15I H 0.395767 0.194915 -0.090806 0.059 Uiso 1 1 d DR U . . .
H15J H 0.359086 0.146015 -0.133744 0.059 Uiso 1 1 d DR U . . .
O156 O 0.3726(3) 0.3544(4) -0.2032(2) 0.0291(11) Uani 1 1 d DG . . . .
H15K H 0.353489 0.367269 -0.181922 0.044 Uiso 1 1 d DG U . . .
H15L H 0.348146 0.330430 -0.230658 0.044 Uiso 1 1 d DG U . . .
O157 O -0.0272(2) 0.7929(4) -0.13330(19) 0.0244(10) Uani 1 1 d D . . . .
H15M H -0.014305 0.853982 -0.139898 0.037 Uiso 1 1 d DR U . . .
H15N H 0.004410 0.757062 -0.119555 0.037 Uiso 1 1 d DR U . . .
O158 O -0.1161(3) 0.8687(4) -0.2238(2) 0.0317(12) Uani 1 1 d D . . . .
H15O H -0.104128 0.913317 -0.198482 0.048 Uiso 1 1 d DR U . . .
H15P H -0.152318 0.864902 -0.228054 0.048 Uiso 1 1 d DR U . . .
O159 O -0.1436(2) 0.6968(4) -0.1686(2) 0.0287(10) Uani 1 1 d D . . . .
H15Q H -0.142457 0.701223 -0.135812 0.043 Uiso 1 1 d DR U . . .
H15R H -0.178111 0.677222 -0.184651 0.043 Uiso 1 1 d DR U . . .
O160 O 0.5517(2) 0.7340(4) 0.62730(19) 0.0266(10) Uani 1 1 d D . . . .
H16A H 0.528344 0.700475 0.641968 0.040 Uiso 1 1 d DR U . . .
H16B H 0.568546 0.681153 0.615838 0.040 Uiso 1 1 d DR U . . .
O161 O 0.6544(3) 0.8688(4) 0.6323(2) 0.0316(11) Uani 1 1 d D . . . .
H16C H 0.691146 0.869655 0.638253 0.047 Uiso 1 1 d DR U . . .
H16D H 0.640688 0.888129 0.599675 0.047 Uiso 1 1 d DR U . . .
O162 O 0.6644(2) 0.6996(4) 0.7017(2) 0.0331(12) Uani 1 1 d D . . . .
H16E H 0.667397 0.671299 0.673284 0.050 Uiso 1 1 d DR U . . .
H16F H 0.649873 0.651174 0.716118 0.050 Uiso 1 1 d DR U . . .
C1 C 0.6035(3) 0.5838(6) 0.2587(3) 0.0277(13) Uani 1 1 d D U . . .
C2 C 0.6452(3) 0.5219(5) 0.2902(2) 0.0163(9) Uani 1 1 d D U . . .
C3 C 0.7003(3) 0.5360(6) 0.2966(3) 0.0247(12) Uani 1 1 d D U . . .
H3 H 0.710778 0.587119 0.276433 0.030 Uiso 1 1 calc R U . . .
C4 C 0.7425(3) 0.4800(5) 0.3309(2) 0.0185(10) Uani 1 1 d D U . . .
C5 C 0.7268(3) 0.4036(5) 0.3595(2) 0.0169(10) Uani 1 1 d D U . . .
C6 C 0.6724(3) 0.3753(5) 0.3503(3) 0.0175(10) Uani 1 1 d D U . . .
H6 H 0.662768 0.315794 0.365688 0.021 Uiso 1 1 calc R U . . .
C7 C 0.6301(3) 0.4388(5) 0.3164(2) 0.0187(10) Uani 1 1 d D U . . .
H7 H 0.591817 0.424595 0.311731 0.022 Uiso 1 1 calc R U . . .
C11 C 1.0074(3) 0.4475(5) 0.6235(3) 0.0199(10) Uani 1 1 d D U . . .
C12 C 0.9566(3) 0.4669(5) 0.5772(3) 0.0198(11) Uani 1 1 d D U . . .
C13 C 0.9388(3) 0.3890(5) 0.5381(2) 0.0196(11) Uani 1 1 d D U . . .
H13 H 0.955148 0.323015 0.542685 0.023 Uiso 1 1 calc R U . . .
C14 C 0.8976(3) 0.4139(5) 0.4944(3) 0.0187(10) Uani 1 1 d D U . . .
C15 C 0.8695(3) 0.5099(5) 0.4879(3) 0.0204(11) Uani 1 1 d D U . . .
C16 C 0.8869(3) 0.5819(5) 0.5275(2) 0.0203(11) Uani 1 1 d D U . . .
H16 H 0.867463 0.644787 0.524955 0.024 Uiso 1 1 calc R U . . .
C17 C 0.9319(3) 0.5626(5) 0.5703(3) 0.0203(11) Uani 1 1 d D U . . .
H17 H 0.946038 0.614913 0.594970 0.024 Uiso 1 1 calc R U . . .
C21 C 0.9886(3) 0.2345(5) 0.2599(3) 0.0201(10) Uani 1 1 d D U . . .
C22 C 0.9691(3) 0.2959(5) 0.2957(3) 0.0246(12) Uani 1 1 d D U . . .
C23 C 0.9230(3) 0.2714(5) 0.3093(2) 0.0182(10) Uani 1 1 d D U . . .
H23 H 0.905099 0.208216 0.297630 0.022 Uiso 1 1 calc R U . . .
C24 C 0.9000(3) 0.3350(5) 0.3398(2) 0.0171(9) Uani 1 1 d D U . . .
C25 C 0.9245(3) 0.4252(5) 0.3547(3) 0.0235(11) Uani 1 1 d D U . . .
C26 C 0.9729(3) 0.4548(5) 0.3445(3) 0.0236(12) Uani 1 1 d D U . . .
H26 H 0.991016 0.516257 0.358981 0.028 Uiso 1 1 calc R U . . .
C27 C 0.9955(3) 0.3945(5) 0.3129(3) 0.0182(10) Uani 1 1 d D U . . .
H27 H 1.026854 0.416914 0.303059 0.022 Uiso 1 1 calc R U . . .
C31 C 0.4647(3) 0.3025(5) 0.2458(3) 0.0261(11) Uani 1 1 d D U . . .
C32 C 0.4928(4) 0.2339(6) 0.2135(3) 0.0321(12) Uani 1 1 d D U . . .
C33 C 0.5332(4) 0.2650(6) 0.1984(3) 0.0318(13) Uani 1 1 d D U . . .
H33 H 0.550476 0.329515 0.207846 0.038 Uiso 1 1 calc R U . . .
C34 C 0.5500(4) 0.1966(5) 0.1670(3) 0.0331(13) Uani 1 1 d D U . . .
C35 C 0.5284(3) 0.1001(5) 0.1552(3) 0.0285(12) Uani 1 1 d D U . . .
C36 C 0.4843(4) 0.0674(6) 0.1702(3) 0.0334(13) Uani 1 1 d D U . . .
H36 H 0.468538 0.002012 0.160213 0.040 Uiso 1 1 calc R U . . .
C37 C 0.4611(4) 0.1354(5) 0.2025(3) 0.0317(13) Uani 1 1 d D U . . .
H37 H 0.430359 0.118659 0.214613 0.038 Uiso 1 1 calc R U . . .
C41 C 0.8630(3) -0.0537(6) 0.2470(3) 0.0279(12) Uani 1 1 d D U . . .
C42 C 0.8122(3) 0.0091(6) 0.2134(3) 0.0299(12) Uani 1 1 d D U . . .
C43 C 0.7631(3) -0.0063(6) 0.2174(3) 0.0285(12) Uani 1 1 d D U . . .
H43 H 0.758140 -0.051018 0.243225 0.034 Uiso 1 1 calc R U . . .
C44 C 0.7159(4) 0.0437(6) 0.1829(3) 0.0302(12) Uani 1 1 d D U . . .
C45 C 0.7272(4) 0.1163(6) 0.1476(3) 0.0326(13) Uani 1 1 d D U . . .
C46 C 0.7830(3) 0.1445(6) 0.1501(3) 0.0314(13) Uani 1 1 d D U . . .
H46 H 0.790643 0.202779 0.132524 0.038 Uiso 1 1 calc R U . . .
C47 C 0.8236(4) 0.0843(6) 0.1783(3) 0.0331(14) Uani 1 1 d D U . . .
H47 H 0.860262 0.090569 0.175489 0.040 Uiso 1 1 calc R U . . .
C51 C 0.5334(4) 0.0699(7) -0.1274(3) 0.0385(16) Uani 1 1 d D U . . .
C52 C 0.5554(5) 0.0441(7) -0.0726(3) 0.0462(19) Uani 1 1 d D U . . .
C53 C 0.5440(5) 0.1105(7) -0.0365(3) 0.0436(19) Uani 1 1 d D U . . .
H53 H 0.518150 0.164844 -0.047660 0.052 Uiso 1 1 calc R U . . .
C54 C 0.5708(4) 0.0961(6) 0.0152(3) 0.0373(16) Uani 1 1 d D U . . .
C55 C 0.6025(5) 0.0042(7) 0.0283(3) 0.0445(19) Uani 1 1 d D U . . .
C56 C 0.6200(5) -0.0651(8) -0.0019(3) 0.048(2) Uani 1 1 d D U . . .
H56 H 0.647772 -0.115553 0.011308 0.058 Uiso 1 1 calc R U . . .
C57 C 0.5893(5) -0.0504(7) -0.0591(3) 0.049(2) Uani 1 1 d D U . . .
H57 H 0.591577 -0.098684 -0.084482 0.059 Uiso 1 1 calc R U . . .
C61 C 0.3399(3) 0.4819(6) 0.2291(3) 0.0269(12) Uani 1 1 d D U . . .
C62 C 0.2871(3) 0.5207(5) 0.1901(3) 0.0249(11) Uani 1 1 d D U . . .
C63 C 0.2313(3) 0.4855(6) 0.1910(3) 0.0248(11) Uani 1 1 d D U . . .
H63 H 0.228099 0.436930 0.215886 0.030 Uiso 1 1 calc R U . . .
C64 C 0.1859(3) 0.5223(6) 0.1566(3) 0.0266(12) Uani 1 1 d D U . . .
C65 C 0.1922(3) 0.5949(6) 0.1194(3) 0.0287(13) Uani 1 1 d D U . . .
C66 C 0.2462(3) 0.6260(6) 0.1184(3) 0.0294(13) Uani 1 1 d D U . . .
H66 H 0.250090 0.674226 0.093562 0.035 Uiso 1 1 calc R U . . .
C67 C 0.2905(3) 0.5877(6) 0.1521(3) 0.0292(14) Uani 1 1 d D U . . .
H67 H 0.326360 0.606895 0.150238 0.035 Uiso 1 1 calc R U . . .
C71 C -0.0013(4) 0.5302(6) -0.1547(3) 0.0285(13) Uani 1 1 d D U . . .
C72 C 0.0246(4) 0.5009(5) -0.0982(3) 0.0280(13) Uani 1 1 d D U . . .
C73 C 0.0147(3) 0.5691(5) -0.0605(2) 0.0250(13) Uani 1 1 d D U . . .
H73 H -0.009379 0.626048 -0.071365 0.030 Uiso 1 1 calc R U . . .
C74 C 0.0412(3) 0.5514(5) -0.0058(3) 0.0242(12) Uani 1 1 d D U . . .
C75 C 0.0688(3) 0.4611(5) 0.0063(3) 0.0256(13) Uani 1 1 d D U . . .
C76 C 0.0824(4) 0.3960(5) -0.0287(3) 0.0296(14) Uani 1 1 d D U . . .
H76 H 0.106952 0.340105 -0.016609 0.035 Uiso 1 1 calc R U . . .
C77 C 0.0592(4) 0.4139(6) -0.0827(3) 0.0410(19) Uani 1 1 d D U . . .
H77 H 0.066638 0.369279 -0.107452 0.049 Uiso 1 1 calc R U . . .
C81 C -0.0211(3) 0.7563(5) 0.2644(3) 0.0229(11) Uani 1 1 d D U . . .
C82 C -0.0056(3) 0.6812(5) 0.2282(3) 0.0256(13) Uani 1 1 d D U . . .
C83 C 0.0247(4) 0.7111(5) 0.1990(3) 0.0316(16) Uani 1 1 d D U . . .
H83 H 0.038862 0.778740 0.203834 0.038 Uiso 1 1 calc R U . . .
C84 C 0.0380(4) 0.6519(5) 0.1615(3) 0.0253(13) Uani 1 1 d D U . . .
C85 C 0.0149(3) 0.5531(5) 0.1564(3) 0.0235(12) Uani 1 1 d D U . . .
C86 C -0.0232(4) 0.5232(5) 0.1820(3) 0.0300(15) Uani 1 1 d D U . . .
H86 H -0.039940 0.457692 0.174794 0.036 Uiso 1 1 calc R U . . .
C87 C -0.0377(4) 0.5845(5) 0.2171(3) 0.0283(14) Uani 1 1 d D U . . .
H87 H -0.065596 0.566644 0.232780 0.034 Uiso 1 1 calc R U . . .
C91 C 0.4858(3) 0.7768(5) 0.2386(3) 0.0183(10) Uani 1 1 d D U . . .
C92 C 0.4734(3) 0.8429(5) 0.2768(3) 0.0184(10) Uani 1 1 d D U . . .
C93 C 0.4296(3) 0.8133(5) 0.3005(2) 0.0172(10) Uani 1 1 d D U . . .
H93 H 0.407061 0.753996 0.291231 0.021 Uiso 1 1 calc R U . . .
C94 C 0.4253(3) 0.8855(5) 0.3395(3) 0.0227(11) Uani 1 1 d D U . . .
C95 C 0.4499(3) 0.9752(5) 0.3481(3) 0.0201(10) Uani 1 1 d D U . . .
C96 C 0.4876(3) 1.0131(5) 0.3205(3) 0.0245(12) Uani 1 1 d D U . . .
H96 H 0.504601 1.078459 0.326152 0.029 Uiso 1 1 calc R U . . .
C97 C 0.4958(3) 0.9431(5) 0.2851(3) 0.0247(12) Uani 1 1 d D U . . .
H97 H 0.518501 0.964081 0.264540 0.030 Uiso 1 1 calc R U . . .
C101 C 0.5217(3) 1.0171(4) 0.6461(3) 0.0185(10) Uani 1 1 d D U . . .
C102 C 0.4792(3) 1.0325(5) 0.5956(3) 0.0225(12) Uani 1 1 d D U . . .
C103 C 0.4797(3) 0.9615(5) 0.5530(2) 0.0170(10) Uani 1 1 d D U . . .
H103 H 0.504649 0.905378 0.557647 0.020 Uiso 1 1 calc R U . . .
C104 C 0.4394(3) 0.9851(5) 0.5043(3) 0.0170(9) Uani 1 1 d D U . . .
C105 C 0.4088(3) 1.0747(5) 0.4955(3) 0.0192(10) Uani 1 1 d D U . . .
C106 C 0.4094(3) 1.1438(6) 0.5368(3) 0.0254(13) Uani 1 1 d D U . . .
H106 H 0.386339 1.202662 0.531786 0.030 Uiso 1 1 calc R U . . .
C107 C 0.4472(3) 1.1173(5) 0.5857(3) 0.0169(10) Uani 1 1 d D U . . .
H107 H 0.450227 1.163009 0.613604 0.020 Uiso 1 1 calc R U . . .
C111 C 0.1187(3) 1.0606(5) 0.2903(3) 0.0199(10) Uani 1 1 d D U . . .
C112 C 0.1718(3) 1.0172(5) 0.3257(3) 0.0250(12) Uani 1 1 d D U . . .
C113 C 0.2236(3) 1.0485(5) 0.3202(3) 0.0254(13) Uani 1 1 d D U . . .
H113 H 0.224736 1.092691 0.292798 0.030 Uiso 1 1 calc R U . . .
C114 C 0.2728(3) 1.0139(5) 0.3553(3) 0.0223(11) Uani 1 1 d D U . . .
C115 C 0.2716(3) 0.9416(5) 0.3923(3) 0.0183(10) Uani 1 1 d D U . . .
C116 C 0.2213(3) 0.9137(5) 0.4011(3) 0.0203(11) Uani 1 1 d D U . . .
H116 H 0.220958 0.873652 0.430161 0.024 Uiso 1 1 calc R U . . .
C117 C 0.1704(3) 0.9478(6) 0.3645(3) 0.0265(13) Uani 1 1 d D U . . .
H117 H 0.135632 0.923118 0.366585 0.032 Uiso 1 1 calc R U . . .
N121 N 0.3266(3) 0.6777(5) 0.3810(3) 0.0457(14) Uani 1 1 d D U . . .
H121 H 0.333034 0.752668 0.379202 0.055 Uiso 1 1 calc R U . . .
C121 C 0.3158(4) 0.6437(6) 0.3256(4) 0.0436(16) Uani 1 1 d D U . . .
H12A H 0.304055 0.571289 0.321540 0.052 Uiso 1 1 calc R U . . .
H12B H 0.349787 0.651560 0.314644 0.052 Uiso 1 1 calc R U . . .
C122 C 0.2689(4) 0.7128(6) 0.2933(4) 0.044(2) Uani 1 1 d D U . . .
H12C H 0.257603 0.690165 0.257202 0.066 Uiso 1 1 calc R U . . .
H12D H 0.282259 0.783352 0.295319 0.066 Uiso 1 1 calc R U . . .
H12E H 0.236795 0.709038 0.306775 0.066 Uiso 1 1 calc R U . . .
C123 C 0.2830(4) 0.6722(6) 0.4073(4) 0.0465(18) Uani 1 1 d D U . . .
H12F H 0.250682 0.713307 0.387392 0.056 Uiso 1 1 calc R U . . .
H12G H 0.297754 0.703921 0.441854 0.056 Uiso 1 1 calc R U . . .
C124 C 0.2630(5) 0.5680(6) 0.4140(5) 0.050(2) Uani 1 1 d D U . . .
H12H H 0.228212 0.572678 0.423168 0.074 Uiso 1 1 calc R U . . .
H12I H 0.291314 0.532701 0.441602 0.074 Uiso 1 1 calc R U . . .
H12J H 0.256390 0.529845 0.381631 0.074 Uiso 1 1 calc R U . . .
C125 C 0.3868(4) 0.6356(6) 0.4113(4) 0.0465(17) Uani 1 1 d D U . . .
H12K H 0.386692 0.561053 0.405351 0.056 Uiso 1 1 calc R U . . .
H12L H 0.413745 0.665871 0.395298 0.056 Uiso 1 1 calc R U . . .
C126 C 0.4072(5) 0.6518(7) 0.4642(4) 0.047(2) Uani 1 1 d D U . . .
H12M H 0.425485 0.718602 0.470794 0.070 Uiso 1 1 calc R U . . .
H12N H 0.434261 0.598390 0.479933 0.070 Uiso 1 1 calc R U . . .
H12O H 0.376271 0.649904 0.479274 0.070 Uiso 1 1 calc R U . . .
N131 N 0.1247(3) 0.8589(6) 0.1014(3) 0.0436(14) Uani 1 1 d D U . . .
H131 H 0.119028 0.783523 0.102398 0.052 Uiso 1 1 calc R U . . .
C131 C 0.0787(4) 0.8967(7) 0.0550(3) 0.0429(17) Uani 1 1 d D U . . .
H13A H 0.079959 0.971981 0.052989 0.052 Uiso 1 1 calc R U . . .
H13B H 0.041833 0.876546 0.058035 0.052 Uiso 1 1 calc R U . . .
C132 C 0.0879(4) 0.8471(7) 0.0041(3) 0.045(2) Uani 1 1 d D U . . .
H13C H 0.094431 0.773616 0.009440 0.067 Uiso 1 1 calc R U . . .
H13D H 0.120279 0.878798 -0.002774 0.067 Uiso 1 1 calc R U . . .
H13E H 0.054610 0.858406 -0.025357 0.067 Uiso 1 1 calc R U . . .
C133 C 0.1822(4) 0.8728(6) 0.0913(4) 0.0441(16) Uani 1 1 d D U . . .
H13F H 0.212589 0.841412 0.119212 0.053 Uiso 1 1 calc R U . . .
H13G H 0.181822 0.841965 0.057817 0.053 Uiso 1 1 calc R U . . .
C134 C 0.1887(4) 0.9792(6) 0.0904(4) 0.0429(19) Uani 1 1 d D U . . .
H13H H 0.194522 0.999414 0.057527 0.064 Uiso 1 1 calc R U . . .
H13I H 0.221114 0.999856 0.119039 0.064 Uiso 1 1 calc R U . . .
H13J H 0.155146 1.012644 0.093862 0.064 Uiso 1 1 calc R U . . .
C135 C 0.1237(5) 0.8950(6) 0.1498(3) 0.0448(18) Uani 1 1 d D U . . .
H13K H 0.084968 0.888214 0.151212 0.054 Uiso 1 1 calc R U . . .
H13L H 0.132295 0.968803 0.151066 0.054 Uiso 1 1 calc R U . . .
C136 C 0.1617(5) 0.8474(7) 0.1985(4) 0.050(3) Uani 1 1 d D U . . .
H13M H 0.198264 0.880828 0.207569 0.075 Uiso 1 1 calc R U . . .
H13N H 0.166132 0.774538 0.192654 0.075 Uiso 1 1 calc R U . . .
H13O H 0.145285 0.856026 0.226776 0.075 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 O3 1.829(5) . ?
Ge1 O4 1.915(5) . ?
Ge1 O13 1.900(5) . ?
Ge1 O14 1.817(5) . ?
Ge1 O23 1.960(5) . ?
Ge1 O24 1.850(5) . ?
Ge2 O33 1.762(5) . ?
Ge2 O34 1.951(6) . ?
Ge2 O43 1.913(5) . ?
Ge2 O44 1.807(7) . ?
Ge2 O53 1.847(6) . ?
Ge2 O54 1.981(6) . ?
Ge3 O63 1.931(5) . ?
Ge3 O64 1.787(5) . ?
Ge3 O73 1.812(5) . ?
Ge3 O74 2.032(5) . ?
Ge3 O83 1.812(5) . ?
Ge3 O84 1.952(5) . ?
Ge4 O93 1.912(5) . ?
Ge4 O94 1.857(5) . ?
Ge4 O103 1.926(5) . ?
Ge4 O104 1.736(5) . ?
Ge4 O113 1.874(5) . ?
Ge4 O114 1.974(5) . ?
Sc1 O1 1.947(6) . ?
Sc1 O32 2.130(5) . ?
Sc1 O51 2.128(7) 2_655 ?
Sc1 O61 2.066(6) . ?
Sc1 O92 2.006(5) . ?
Sc1 O101 2.108(5) 2_646 ?
Sc2 O12 2.035(5) . ?
Sc2 O42 2.030(5) 2_756 ?
Sc2 O81 2.067(6) 2_646 ?
Sc2 O151 2.199(5) . ?
Sc2 O152 2.132(6) . ?
Sc2 O153 2.169(6) . ?
Sc3 O11 2.097(5) 2_746 ?
Sc3 O22 1.991(5) . ?
Sc3 O41 2.075(6) . ?
Sc3 O71 2.057(5) 2_645 ?
Sc3 O82 2.127(5) 1_645 ?
Sc3 O111 2.054(5) 1_645 ?
Sc4 O2 2.081(5) 2_645 ?
Sc4 O52 2.077(6) . ?
Sc4 O91 2.058(5) 2_645 ?
Sc4 O154 2.050(6) . ?
Sc4 O155 2.117(6) . ?
Sc4 O156 2.091(5) . ?
Sc5 O21 2.058(5) 2_655 ?
Sc5 O72 2.082(5) . ?
Sc5 O112 2.077(5) 2_545 ?
Sc5 O157 2.078(5) . ?
Sc5 O158 2.116(5) . ?
Sc5 O159 2.127(6) . ?
Sc6 O31 2.090(6) 2_656 ?
Sc6 O62 2.044(6) 2_656 ?
Sc6 O102 1.999(5) . ?
Sc6 O160 2.118(5) . ?
Sc6 O161 2.083(6) . ?
Sc6 O162 2.172(5) . ?
O1 C1 1.383(10) . ?
O2 C1 1.265(9) . ?
O3 C4 1.320(8) . ?
O4 C5 1.401(8) . ?
O11 C11 1.279(8) . ?
O12 C11 1.210(9) . ?
O13 C14 1.336(8) . ?
O14 C15 1.369(8) . ?
O21 C21 1.251(9) . ?
O22 C21 1.286(9) . ?
O23 C24 1.382(8) . ?
O24 C25 1.384(8) . ?
O31 C31 1.267(10) . ?
O32 C31 1.246(10) . ?
O33 C34 1.448(11) . ?
O34 C35 1.317(9) . ?
O41 C41 1.179(10) . ?
O42 C41 1.299(9) . ?
O43 C44 1.349(11) . ?
O44 C45 1.394(10) . ?
O51 C51 1.215(10) . ?
O52 C51 1.301(10) . ?
O53 C54 1.333(10) . ?
O54 C55 1.428(11) . ?
O61 C61 1.191(10) . ?
O62 C61 1.375(9) . ?
O63 C64 1.369(10) . ?
O64 C65 1.355(9) . ?
O71 C71 1.272(9) . ?
O72 C71 1.164(9) . ?
O73 C74 1.368(9) . ?
O74 C75 1.350(8) . ?
O81 C81 1.294(9) . ?
O82 C81 1.181(9) . ?
O83 C84 1.218(9) . ?
O84 C85 1.328(8) . ?
O91 C91 1.185(9) . ?
O92 C91 1.334(8) . ?
O93 C94 1.399(9) . ?
O94 C95 1.403(8) . ?
O101 C101 1.215(8) . ?
O102 C101 1.271(8) . ?
O103 C104 1.326(8) . ?
O104 C105 1.339(8) . ?
O111 C111 1.245(9) . ?
O112 C111 1.298(8) . ?
O113 C114 1.324(9) . ?
O114 C115 1.319(8) . ?
O151 H15A 0.8774 . ?
O151 H15B 0.8773 . ?
O152 H15C 0.9068 . ?
O152 H15D 0.9071 . ?
O153 H15E 0.8919 . ?
O153 H15F 0.8919 . ?
O154 H15G 0.8947 . ?
O154 H15H 0.8955 . ?
O155 H15I 0.8889 . ?
O155 H15J 0.8898 . ?
O156 H15K 0.8703 . ?
O156 H15L 0.8688 . ?
O157 H15M 0.9024 . ?
O157 H15N 0.9021 . ?
O158 H15O 0.8831 . ?
O158 H15P 0.8836 . ?
O159 H15Q 0.8829 . ?
O159 H15R 0.8825 . ?
O160 H16A 0.9129 . ?
O160 H16B 0.9142 . ?
O161 H16C 0.8886 . ?
O161 H16D 0.8859 . ?
O162 H16E 0.8797 . ?
O162 H16F 0.8790 . ?
C1 C2 1.396(9) . ?
C2 C3 1.354(9) . ?
C2 C7 1.415(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(9) . ?
C4 C5 1.395(8) . ?
C5 C6 1.364(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.442(8) . ?
C7 H7 0.9500 . ?
C11 C12 1.519(9) . ?
C12 C13 1.445(8) . ?
C12 C17 1.387(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.358(9) . ?
C14 C15 1.428(8) . ?
C15 C16 1.398(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(9) . ?
C17 H17 0.9500 . ?
C21 C22 1.454(9) . ?
C22 C23 1.353(9) . ?
C22 C27 1.465(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.413(8) . ?
C24 C25 1.338(9) . ?
C25 C26 1.380(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.405(9) . ?
C27 H27 0.9500 . ?
C31 C32 1.562(10) . ?
C32 C33 1.270(11) . ?
C32 C37 1.500(10) . ?
C33 H33 0.9500 . ?
C33 C34 1.386(9) . ?
C34 C35 1.377(9) . ?
C35 C36 1.358(11) . ?
C36 H36 0.9500 . ?
C36 C37 1.485(10) . ?
C37 H37 0.9500 . ?
C41 C42 1.562(10) . ?
C42 C43 1.286(10) . ?
C42 C47 1.456(10) . ?
C43 H43 0.9500 . ?
C43 C44 1.430(10) . ?
C44 C45 1.436(10) . ?
C45 C46 1.430(11) . ?
C46 H46 0.9500 . ?
C46 C47 1.335(10) . ?
C47 H47 0.9500 . ?
C51 C52 1.463(11) . ?
C52 C53 1.400(10) . ?
C52 C57 1.486(11) . ?
C53 H53 0.9500 . ?
C53 C54 1.374(11) . ?
C54 C55 1.428(10) . ?
C55 C56 1.380(11) . ?
C56 H56 0.9500 . ?
C56 C57 1.523(11) . ?
C57 H57 0.9500 . ?
C61 C62 1.515(9) . ?
C62 C63 1.480(10) . ?
C62 C67 1.376(9) . ?
C63 H63 0.9500 . ?
C63 C64 1.329(9) . ?
C64 C65 1.431(9) . ?
C65 C66 1.423(10) . ?
C66 H66 0.9500 . ?
C66 C67 1.310(10) . ?
C67 H67 0.9500 . ?
C71 C72 1.523(9) . ?
C72 C73 1.436(9) . ?
C72 C77 1.418(10) . ?
C73 H73 0.9500 . ?
C73 C74 1.450(9) . ?
C74 C75 1.362(9) . ?
C75 C76 1.392(9) . ?
C76 H76 0.9500 . ?
C76 C77 1.425(10) . ?
C77 H77 0.9500 . ?
C81 C82 1.521(9) . ?
C82 C83 1.311(9) . ?
C82 C87 1.484(9) . ?
C83 H83 0.9500 . ?
C83 C84 1.396(9) . ?
C84 C85 1.408(8) . ?
C85 C86 1.397(9) . ?
C86 H86 0.9500 . ?
C86 C87 1.376(9) . ?
C87 H87 0.9500 . ?
C91 C92 1.453(9) . ?
C92 C93 1.482(9) . ?
C92 C97 1.420(8) . ?
C93 H93 0.9500 . ?
C93 C94 1.447(9) . ?
C94 C95 1.318(8) . ?
C95 C96 1.456(9) . ?
C96 H96 0.9500 . ?
C96 C97 1.387(9) . ?
C97 H97 0.9500 . ?
C101 C102 1.477(9) . ?
C102 C103 1.486(9) . ?
C102 C107 1.350(8) . ?
C103 H103 0.9500 . ?
C103 C104 1.437(9) . ?
C104 C105 1.386(8) . ?
C105 C106 1.435(9) . ?
C106 H106 0.9500 . ?
C106 C107 1.425(9) . ?
C107 H107 0.9500 . ?
C111 C112 1.503(9) . ?
C112 C113 1.413(9) . ?
C112 C117 1.397(9) . ?
C113 H113 0.9500 . ?
C113 C114 1.391(9) . ?
C114 C115 1.388(8) . ?
C115 C116 1.401(9) . ?
C116 H116 0.9500 . ?
C116 C117 1.435(9) . ?
C117 H117 0.9500 . ?
N121 H121 1.0000 . ?
N121 C121 1.512(11) . ?
N121 C123 1.476(11) . ?
N121 C125 1.588(11) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
C121 C122 1.535(12) . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C122 H12E 0.9800 . ?
C123 H12F 0.9900 . ?
C123 H12G 0.9900 . ?
C123 C124 1.485(11) . ?
C124 H12H 0.9800 . ?
C124 H12I 0.9800 . ?
C124 H12J 0.9800 . ?
C125 H12K 0.9900 . ?
C125 H12L 0.9900 . ?
C125 C126 1.387(12) . ?
C126 H12M 0.9800 . ?
C126 H12N 0.9800 . ?
C126 H12O 0.9800 . ?
N131 H131 1.0000 . ?
N131 C131 1.514(10) . ?
N131 C133 1.560(12) . ?
N131 C135 1.401(11) . ?
C131 H13A 0.9900 . ?
C131 H13B 0.9900 . ?
C131 C132 1.602(12) . ?
C132 H13C 0.9800 . ?
C132 H13D 0.9800 . ?
C132 H13E 0.9800 . ?
C133 H13F 0.9900 . ?
C133 H13G 0.9900 . ?
C133 C134 1.406(11) . ?
C134 H13H 0.9800 . ?
C134 H13I 0.9800 . ?
C134 H13J 0.9800 . ?
C135 H13K 0.9900 . ?
C135 H13L 0.9900 . ?
C135 C136 1.513(11) . ?
C136 H13M 0.9800 . ?
C136 H13N 0.9800 . ?
C136 H13O 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ge1 O4 86.3(2) . . ?
O3 Ge1 O13 174.9(2) . . ?
O3 Ge1 O23 93.6(2) . . ?
O3 Ge1 O24 90.7(2) . . ?
O4 Ge1 O23 85.9(2) . . ?
O13 Ge1 O4 88.8(2) . . ?
O13 Ge1 O23 87.3(2) . . ?
O14 Ge1 O3 91.9(2) . . ?
O14 Ge1 O4 95.2(2) . . ?
O14 Ge1 O13 87.3(2) . . ?
O14 Ge1 O23 174.4(2) . . ?
O14 Ge1 O24 93.3(2) . . ?
O24 Ge1 O4 171.1(2) . . ?
O24 Ge1 O13 94.4(2) . . ?
O24 Ge1 O23 86.0(2) . . ?
O33 Ge2 O34 87.8(3) . . ?
O33 Ge2 O43 98.7(3) . . ?
O33 Ge2 O44 93.9(3) . . ?
O33 Ge2 O53 94.2(3) . . ?
O33 Ge2 O54 174.4(3) . . ?
O34 Ge2 O54 86.8(3) . . ?
O43 Ge2 O34 84.5(2) . . ?
O43 Ge2 O54 79.5(2) . . ?
O44 Ge2 O34 170.6(2) . . ?
O44 Ge2 O43 86.1(3) . . ?
O44 Ge2 O53 98.0(3) . . ?
O44 Ge2 O54 91.3(3) . . ?
O53 Ge2 O34 91.1(3) . . ?
O53 Ge2 O43 166.1(3) . . ?
O53 Ge2 O54 87.1(3) . . ?
O63 Ge3 O74 85.1(2) . . ?
O63 Ge3 O84 85.0(2) . . ?
O64 Ge3 O63 85.8(2) . . ?
O64 Ge3 O73 93.9(2) . . ?
O64 Ge3 O74 92.5(2) . . ?
O64 Ge3 O83 95.5(2) . . ?
O64 Ge3 O84 170.7(2) . . ?
O73 Ge3 O63 168.9(2) . . ?
O73 Ge3 O74 83.9(2) . . ?
O73 Ge3 O84 95.4(2) . . ?
O83 Ge3 O63 93.6(2) . . ?
O83 Ge3 O73 97.4(2) . . ?
O83 Ge3 O74 171.8(2) . . ?
O83 Ge3 O84 83.8(2) . . ?
O84 Ge3 O74 88.1(2) . . ?
O93 Ge4 O103 87.3(2) . . ?
O93 Ge4 O114 86.9(2) . . ?
O94 Ge4 O93 85.4(2) . . ?
O94 Ge4 O103 94.2(2) . . ?
O94 Ge4 O113 92.8(2) . . ?
O94 Ge4 O114 172.3(2) . . ?
O103 Ge4 O114 86.2(2) . . ?
O104 Ge4 O93 173.3(2) . . ?
O104 Ge4 O94 96.1(2) . . ?
O104 Ge4 O103 86.0(2) . . ?
O104 Ge4 O113 94.3(2) . . ?
O104 Ge4 O114 91.6(2) . . ?
O113 Ge4 O93 92.2(2) . . ?
O113 Ge4 O103 172.9(2) . . ?
O113 Ge4 O114 86.7(2) . . ?
O1 Sc1 O32 87.0(2) . . ?
O1 Sc1 O51 89.7(3) . 2_655 ?
O1 Sc1 O61 175.0(2) . . ?
O1 Sc1 O92 89.6(2) . . ?
O1 Sc1 O101 87.6(2) . 2_646 ?
O51 Sc1 O32 87.0(2) 2_655 . ?
O61 Sc1 O32 88.0(2) . . ?
O61 Sc1 O51 90.6(3) . 2_655 ?
O61 Sc1 O101 92.1(2) . 2_646 ?
O92 Sc1 O32 176.3(2) . . ?
O92 Sc1 O51 91.4(2) . 2_655 ?
O92 Sc1 O61 95.4(2) . . ?
O92 Sc1 O101 89.1(2) . 2_646 ?
O101 Sc1 O32 92.3(2) 2_646 . ?
O101 Sc1 O51 177.2(3) 2_646 2_655 ?
O12 Sc2 O81 91.3(2) . 2_646 ?
O12 Sc2 O151 87.7(2) . . ?
O12 Sc2 O152 88.1(2) . . ?
O12 Sc2 O153 167.2(2) . . ?
O42 Sc2 O12 103.4(2) 2_756 . ?
O42 Sc2 O81 96.9(2) 2_756 2_646 ?
O42 Sc2 O151 164.1(2) 2_756 . ?
O42 Sc2 O152 84.9(2) 2_756 . ?
O42 Sc2 O153 89.4(2) 2_756 . ?
O81 Sc2 O151 94.2(2) 2_646 . ?
O81 Sc2 O152 178.2(3) 2_646 . ?
O81 Sc2 O153 88.5(2) 2_646 . ?
O152 Sc2 O151 84.1(2) . . ?
O152 Sc2 O153 91.7(2) . . ?
O153 Sc2 O151 79.5(2) . . ?
O11 Sc3 O82 90.33(19) 2_746 1_645 ?
O22 Sc3 O11 88.9(2) . 2_746 ?
O22 Sc3 O41 92.7(2) . . ?
O22 Sc3 O71 92.8(2) . 2_645 ?
O22 Sc3 O82 176.0(2) . 1_645 ?
O22 Sc3 O111 92.1(2) . 1_645 ?
O41 Sc3 O11 90.1(2) . 2_746 ?
O41 Sc3 O82 83.4(2) . 1_645 ?
O71 Sc3 O11 176.6(2) 2_645 2_746 ?
O71 Sc3 O41 86.9(2) 2_645 . ?
O71 Sc3 O82 87.7(2) 2_645 1_645 ?
O111 Sc3 O11 89.3(2) 1_645 2_746 ?
O111 Sc3 O41 175.2(2) 1_645 . ?
O111 Sc3 O71 93.6(2) 1_645 2_645 ?
O111 Sc3 O82 91.8(2) 1_645 1_645 ?
O2 Sc4 O155 85.5(3) 2_645 . ?
O2 Sc4 O156 84.7(2) 2_645 . ?
O52 Sc4 O2 95.2(2) . 2_645 ?
O52 Sc4 O155 83.4(2) . . ?
O52 Sc4 O156 174.9(2) . . ?
O91 Sc4 O2 92.6(2) 2_645 2_645 ?
O91 Sc4 O52 95.4(2) 2_645 . ?
O91 Sc4 O155 177.7(2) 2_645 . ?
O91 Sc4 O156 89.7(2) 2_645 . ?
O154 Sc4 O2 169.7(3) . 2_645 ?
O154 Sc4 O52 90.0(2) . . ?
O154 Sc4 O91 95.7(3) . 2_645 ?
O154 Sc4 O155 86.3(3) . . ?
O154 Sc4 O156 89.2(2) . . ?
O156 Sc4 O155 91.5(2) . . ?
O21 Sc5 O72 98.7(2) 2_655 . ?
O21 Sc5 O112 86.8(2) 2_655 2_545 ?
O21 Sc5 O157 97.9(2) 2_655 . ?
O21 Sc5 O158 83.7(2) 2_655 . ?
O21 Sc5 O159 164.8(2) 2_655 . ?
O72 Sc5 O158 170.0(2) . . ?
O72 Sc5 O159 93.1(2) . . ?
O112 Sc5 O72 90.1(2) 2_545 . ?
O112 Sc5 O157 170.1(2) 2_545 . ?
O112 Sc5 O158 99.8(2) 2_545 . ?
O112 Sc5 O159 83.7(2) 2_545 . ?
O157 Sc5 O72 80.6(2) . . ?
O157 Sc5 O158 89.4(2) . . ?
O157 Sc5 O159 93.4(2) . . ?
O158 Sc5 O159 86.3(2) . . ?
O31 Sc6 O160 88.9(2) 2_656 . ?
O31 Sc6 O162 84.6(2) 2_656 . ?
O62 Sc6 O31 91.2(3) 2_656 2_656 ?
O62 Sc6 O160 175.9(2) 2_656 . ?
O62 Sc6 O161 84.2(2) 2_656 . ?
O62 Sc6 O162 88.1(2) 2_656 . ?
O102 Sc6 O31 101.4(3) . 2_656 ?
O102 Sc6 O62 99.1(2) . 2_656 ?
O102 Sc6 O160 84.8(2) . . ?
O102 Sc6 O161 89.6(2) . . ?
O102 Sc6 O162 170.4(2) . . ?
O160 Sc6 O162 87.9(2) . . ?
O161 Sc6 O31 168.6(3) . 2_656 ?
O161 Sc6 O160 94.9(2) . . ?
O161 Sc6 O162 84.8(2) . . ?
C1 O1 Sc1 175.6(6) . . ?
C1 O2 Sc4 133.9(5) . 2_655 ?
C4 O3 Ge1 112.6(4) . . ?
C5 O4 Ge1 109.3(4) . . ?
C11 O11 Sc3 132.5(4) . 2_756 ?
C11 O12 Sc2 148.5(5) . . ?
C14 O13 Ge1 108.1(4) . . ?
C15 O14 Ge1 109.9(4) . . ?
C21 O21 Sc5 139.5(5) . 2_645 ?
C21 O22 Sc3 146.6(5) . . ?
C24 O23 Ge1 108.2(4) . . ?
C25 O24 Ge1 111.5(4) . . ?
C31 O31 Sc6 131.5(5) . 2_646 ?
C31 O32 Sc1 139.7(5) . . ?
C34 O33 Ge2 111.3(4) . . ?
C35 O34 Ge2 109.3(5) . . ?
C41 O41 Sc3 146.5(5) . . ?
C41 O42 Sc2 131.4(5) . 2_746 ?
C44 O43 Ge2 113.5(5) . . ?
C45 O44 Ge2 111.8(5) . . ?
C51 O51 Sc1 130.9(6) . 2_645 ?
C51 O52 Sc4 162.5(6) . . ?
C54 O53 Ge2 114.3(5) . . ?
C55 O54 Ge2 106.4(5) . . ?
C61 O61 Sc1 169.8(5) . . ?
C61 O62 Sc6 129.9(5) . 2_646 ?
C64 O63 Ge3 109.3(4) . . ?
C65 O64 Ge3 116.9(4) . . ?
C71 O71 Sc3 134.7(5) . 2_655 ?
C71 O72 Sc5 164.6(6) . . ?
C74 O73 Ge3 112.8(4) . . ?
C75 O74 Ge3 107.4(4) . . ?
C81 O81 Sc2 143.6(5) . 2_656 ?
C81 O82 Sc3 141.1(6) . 1_465 ?
C84 O83 Ge3 115.4(4) . . ?
C85 O84 Ge3 107.0(4) . . ?
C91 O91 Sc4 143.1(5) . 2_655 ?
C91 O92 Sc1 133.1(4) . . ?
C94 O93 Ge4 110.7(4) . . ?
C95 O94 Ge4 111.3(4) . . ?
C101 O101 Sc1 130.1(4) . 2_656 ?
C101 O102 Sc6 162.4(5) . . ?
C104 O103 Ge4 108.3(4) . . ?
C105 O104 Ge4 115.9(4) . . ?
C111 O111 Sc3 156.6(5) . 1_465 ?
C111 O112 Sc5 140.6(5) . 2 ?
C114 O113 Ge4 109.2(4) . . ?
C115 O114 Ge4 106.2(4) . . ?
Sc2 O151 H15A 110.5 . . ?
Sc2 O151 H15B 109.8 . . ?
H15A O151 H15B 104.1 . . ?
Sc2 O152 H15C 127.7 . . ?
Sc2 O152 H15D 128.2 . . ?
H15C O152 H15D 104.0 . . ?
Sc2 O153 H15E 110.5 . . ?
Sc2 O153 H15F 110.6 . . ?
H15E O153 H15F 103.4 . . ?
Sc4 O154 H15G 110.0 . . ?
Sc4 O154 H15H 111.5 . . ?
H15G O154 H15H 103.2 . . ?
Sc4 O155 H15I 127.6 . . ?
Sc4 O155 H15J 128.0 . . ?
H15I O155 H15J 104.3 . . ?
Sc4 O156 H15K 110.9 . . ?
Sc4 O156 H15L 110.4 . . ?
H15K O156 H15L 104.5 . . ?
Sc5 O157 H15M 111.1 . . ?
Sc5 O157 H15N 111.8 . . ?
H15M O157 H15N 102.6 . . ?
Sc5 O158 H15O 109.6 . . ?
Sc5 O158 H15P 110.5 . . ?
H15O O158 H15P 103.7 . . ?
Sc5 O159 H15Q 127.2 . . ?
Sc5 O159 H15R 128.4 . . ?
H15Q O159 H15R 104.4 . . ?
Sc6 O160 H16A 111.3 . . ?
Sc6 O160 H16B 113.6 . . ?
H16A O160 H16B 101.9 . . ?
Sc6 O161 H16C 129.5 . . ?
Sc6 O161 H16D 126.1 . . ?
H16C O161 H16D 104.4 . . ?
Sc6 O162 H16E 109.3 . . ?
Sc6 O162 H16F 110.5 . . ?
H16E O162 H16F 103.9 . . ?
O1 C1 C2 122.2(7) . . ?
O2 C1 O1 115.9(6) . . ?
O2 C1 C2 121.5(7) . . ?
C1 C2 C7 119.3(6) . . ?
C3 C2 C1 123.4(6) . . ?
C3 C2 C7 117.2(6) . . ?
C2 C3 H3 118.0 . . ?
C2 C3 C4 124.0(7) . . ?
C4 C3 H3 118.0 . . ?
O3 C4 C3 124.4(6) . . ?
O3 C4 C5 117.9(6) . . ?
C3 C4 C5 117.7(6) . . ?
C4 C5 O4 112.9(6) . . ?
C6 C5 O4 125.1(6) . . ?
C6 C5 C4 121.9(6) . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.8(6) . . ?
C7 C6 H6 121.1 . . ?
C2 C7 C6 120.5(6) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
O11 C11 C12 117.3(6) . . ?
O12 C11 O11 121.0(6) . . ?
O12 C11 C12 121.7(6) . . ?
C13 C12 C11 119.2(6) . . ?
C17 C12 C11 119.7(6) . . ?
C17 C12 C13 120.8(6) . . ?
C12 C13 H13 121.3 . . ?
C14 C13 C12 117.3(6) . . ?
C14 C13 H13 121.3 . . ?
O13 C14 C13 123.2(6) . . ?
O13 C14 C15 114.3(6) . . ?
C13 C14 C15 122.5(6) . . ?
O14 C15 C14 115.2(6) . . ?
O14 C15 C16 126.2(6) . . ?
C16 C15 C14 118.1(6) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 C15 120.7(6) . . ?
C17 C16 H16 119.6 . . ?
C12 C17 H17 120.0 . . ?
C16 C17 C12 120.1(6) . . ?
C16 C17 H17 120.0 . . ?
O21 C21 O22 122.3(6) . . ?
O21 C21 C22 117.9(6) . . ?
O22 C21 C22 117.7(6) . . ?
C21 C22 C27 119.3(6) . . ?
C23 C22 C21 122.4(6) . . ?
C23 C22 C27 117.8(6) . . ?
C22 C23 H23 118.3 . . ?
C22 C23 C24 123.4(6) . . ?
C24 C23 H23 118.3 . . ?
O23 C24 C23 125.1(6) . . ?
C25 C24 O23 117.0(6) . . ?
C25 C24 C23 117.8(6) . . ?
C24 C25 O24 117.1(6) . . ?
C24 C25 C26 122.7(7) . . ?
C26 C25 O24 119.7(6) . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.3(7) . . ?
C27 C26 H26 119.9 . . ?
C22 C27 H27 121.2 . . ?
C26 C27 C22 117.6(6) . . ?
C26 C27 H27 121.2 . . ?
O31 C31 C32 123.2(7) . . ?
O32 C31 O31 125.9(7) . . ?
O32 C31 C32 111.0(7) . . ?
C33 C32 C31 122.3(7) . . ?
C33 C32 C37 129.8(7) . . ?
C37 C32 C31 107.8(7) . . ?
C32 C33 H33 122.9 . . ?
C32 C33 C34 114.2(8) . . ?
C34 C33 H33 122.9 . . ?
C33 C34 O33 120.1(7) . . ?
C35 C34 O33 114.5(6) . . ?
C35 C34 C33 124.4(8) . . ?
O34 C35 C34 116.9(7) . . ?
O34 C35 C36 121.7(7) . . ?
C36 C35 C34 121.4(7) . . ?
C35 C36 H36 120.4 . . ?
C35 C36 C37 119.2(7) . . ?
C37 C36 H36 120.4 . . ?
C32 C37 H37 124.6 . . ?
C36 C37 C32 110.8(7) . . ?
C36 C37 H37 124.6 . . ?
O41 C41 O42 128.6(7) . . ?
O41 C41 C42 118.3(7) . . ?
O42 C41 C42 112.9(7) . . ?
C43 C42 C41 120.2(7) . . ?
C43 C42 C47 122.8(7) . . ?
C47 C42 C41 116.9(7) . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 120.0(7) . . ?
C44 C43 H43 120.0 . . ?
O43 C44 C43 132.4(7) . . ?
O43 C44 C45 110.9(7) . . ?
C43 C44 C45 116.7(7) . . ?
O44 C45 C44 116.5(7) . . ?
O44 C45 C46 121.2(7) . . ?
C46 C45 C44 121.8(7) . . ?
C45 C46 H46 121.9 . . ?
C47 C46 C45 116.3(7) . . ?
C47 C46 H46 121.9 . . ?
C42 C47 H47 119.7 . . ?
C46 C47 C42 120.6(8) . . ?
C46 C47 H47 119.7 . . ?
O51 C51 O52 120.8(8) . . ?
O51 C51 C52 122.3(8) . . ?
O52 C51 C52 113.1(7) . . ?
C51 C52 C57 117.2(7) . . ?
C53 C52 C51 118.2(7) . . ?
C53 C52 C57 124.6(8) . . ?
C52 C53 H53 120.5 . . ?
C54 C53 C52 119.1(8) . . ?
C54 C53 H53 120.5 . . ?
O53 C54 C53 128.1(7) . . ?
O53 C54 C55 116.0(7) . . ?
C53 C54 C55 115.9(8) . . ?
O54 C55 C54 116.0(7) . . ?
C56 C55 O54 111.7(7) . . ?
C56 C55 C54 131.3(8) . . ?
C55 C56 H56 124.3 . . ?
C55 C56 C57 111.5(8) . . ?
C57 C56 H56 124.3 . . ?
C52 C57 C56 115.8(7) . . ?
C52 C57 H57 122.1 . . ?
C56 C57 H57 122.1 . . ?
O61 C61 O62 120.9(7) . . ?
O61 C61 C62 122.2(7) . . ?
O62 C61 C62 116.9(6) . . ?
C63 C62 C61 121.2(6) . . ?
C67 C62 C61 120.0(7) . . ?
C67 C62 C63 118.8(7) . . ?
C62 C63 H63 120.2 . . ?
C64 C63 C62 119.6(7) . . ?
C64 C63 H63 120.2 . . ?
O63 C64 C65 115.7(6) . . ?
C63 C64 O63 125.4(7) . . ?
C63 C64 C65 118.8(7) . . ?
O64 C65 C64 111.9(7) . . ?
O64 C65 C66 127.2(6) . . ?
C66 C65 C64 120.8(7) . . ?
C65 C66 H66 120.3 . . ?
C67 C66 C65 119.5(7) . . ?
C67 C66 H66 120.3 . . ?
C62 C67 H67 118.8 . . ?
C66 C67 C62 122.4(8) . . ?
C66 C67 H67 118.8 . . ?
O71 C71 C72 117.4(7) . . ?
O72 C71 O71 122.1(7) . . ?
O72 C71 C72 120.3(7) . . ?
C73 C72 C71 116.5(6) . . ?
C77 C72 C71 122.7(7) . . ?
C77 C72 C73 120.8(6) . . ?
C72 C73 H73 119.9 . . ?
C72 C73 C74 120.3(6) . . ?
C74 C73 H73 119.9 . . ?
O73 C74 C73 126.8(6) . . ?
C75 C74 O73 117.2(6) . . ?
C75 C74 C73 115.5(6) . . ?
O74 C75 C74 115.7(6) . . ?
O74 C75 C76 118.4(6) . . ?
C74 C75 C76 125.5(7) . . ?
C75 C76 H76 120.3 . . ?
C75 C76 C77 119.4(7) . . ?
C77 C76 H76 120.3 . . ?
C72 C77 C76 117.6(7) . . ?
C72 C77 H77 121.2 . . ?
C76 C77 H77 121.2 . . ?
O81 C81 C82 120.6(6) . . ?
O82 C81 O81 118.4(6) . . ?
O82 C81 C82 120.7(7) . . ?
C83 C82 C81 120.1(6) . . ?
C83 C82 C87 120.8(6) . . ?
C87 C82 C81 117.1(6) . . ?
C82 C83 H83 117.2 . . ?
C82 C83 C84 125.6(7) . . ?
C84 C83 H83 117.2 . . ?
O83 C84 C83 129.3(6) . . ?
O83 C84 C85 117.0(6) . . ?
C83 C84 C85 113.7(6) . . ?
O84 C85 C84 114.3(6) . . ?
O84 C85 C86 122.1(6) . . ?
C86 C85 C84 122.1(6) . . ?
C85 C86 H86 118.6 . . ?
C87 C86 C85 122.9(7) . . ?
C87 C86 H86 118.6 . . ?
C82 C87 H87 123.3 . . ?
C86 C87 C82 113.5(6) . . ?
C86 C87 H87 123.3 . . ?
O91 C91 O92 123.9(6) . . ?
O91 C91 C92 120.4(6) . . ?
O92 C91 C92 115.7(6) . . ?
C91 C92 C93 119.9(6) . . ?
C97 C92 C91 120.3(6) . . ?
C97 C92 C93 118.9(6) . . ?
C92 C93 H93 124.0 . . ?
C94 C93 C92 111.9(6) . . ?
C94 C93 H93 124.0 . . ?
O93 C94 C93 119.0(6) . . ?
C95 C94 O93 115.1(6) . . ?
C95 C94 C93 125.4(7) . . ?
O94 C95 C96 118.7(5) . . ?
C94 C95 O94 117.3(6) . . ?
C94 C95 C96 123.8(6) . . ?
C95 C96 H96 123.7 . . ?
C97 C96 C95 112.6(6) . . ?
C97 C96 H96 123.7 . . ?
C92 C97 H97 117.0 . . ?
C96 C97 C92 126.0(7) . . ?
C96 C97 H97 117.0 . . ?
O101 C101 O102 125.2(6) . . ?
O101 C101 C102 116.7(6) . . ?
O102 C101 C102 117.8(6) . . ?
C101 C102 C103 117.5(6) . . ?
C107 C102 C101 121.3(6) . . ?
C107 C102 C103 120.3(6) . . ?
C102 C103 H103 122.8 . . ?
C104 C103 C102 114.3(6) . . ?
C104 C103 H103 122.8 . . ?
O103 C104 C103 120.8(6) . . ?
O103 C104 C105 116.3(6) . . ?
C105 C104 C103 122.9(6) . . ?
O104 C105 C104 113.2(6) . . ?
O104 C105 C106 124.8(6) . . ?
C104 C105 C106 121.7(6) . . ?
C105 C106 H106 122.6 . . ?
C107 C106 C105 114.9(6) . . ?
C107 C106 H106 122.6 . . ?
C102 C107 C106 125.2(6) . . ?
C102 C107 H107 117.4 . . ?
C106 C107 H107 117.4 . . ?
O111 C111 O112 124.5(6) . . ?
O111 C111 C112 119.5(6) . . ?
O112 C111 C112 116.0(6) . . ?
C113 C112 C111 119.4(6) . . ?
C117 C112 C111 120.7(6) . . ?
C117 C112 C113 119.9(6) . . ?
C112 C113 H113 120.3 . . ?
C114 C113 C112 119.4(6) . . ?
C114 C113 H113 120.3 . . ?
O113 C114 C113 120.9(6) . . ?
O113 C114 C115 117.7(6) . . ?
C115 C114 C113 120.7(7) . . ?
O114 C115 C114 118.8(6) . . ?
O114 C115 C116 119.6(6) . . ?
C114 C115 C116 121.1(6) . . ?
C115 C116 H116 121.2 . . ?
C115 C116 C117 117.6(6) . . ?
C117 C116 H116 121.2 . . ?
C112 C117 C116 120.4(7) . . ?
C112 C117 H117 119.8 . . ?
C116 C117 H117 119.8 . . ?
C121 N121 H121 103.0 . . ?
C121 N121 C125 105.9(7) . . ?
C123 N121 H121 103.0 . . ?
C123 N121 C121 121.8(8) . . ?
C123 N121 C125 117.5(8) . . ?
C125 N121 H121 103.0 . . ?
N121 C121 H12A 110.6 . . ?
N121 C121 H12B 110.6 . . ?
N121 C121 C122 105.8(7) . . ?
H12A C121 H12B 108.7 . . ?
C122 C121 H12A 110.6 . . ?
C122 C121 H12B 110.6 . . ?
C121 C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
C121 C122 H12E 109.5 . . ?
H12C C122 H12D 109.5 . . ?
H12C C122 H12E 109.5 . . ?
H12D C122 H12E 109.5 . . ?
N121 C123 H12F 108.4 . . ?
N121 C123 H12G 108.4 . . ?
N121 C123 C124 115.5(7) . . ?
H12F C123 H12G 107.5 . . ?
C124 C123 H12F 108.4 . . ?
C124 C123 H12G 108.4 . . ?
C123 C124 H12H 109.5 . . ?
C123 C124 H12I 109.5 . . ?
C123 C124 H12J 109.5 . . ?
H12H C124 H12I 109.5 . . ?
H12H C124 H12J 109.5 . . ?
H12I C124 H12J 109.5 . . ?
N121 C125 H12K 107.6 . . ?
N121 C125 H12L 107.6 . . ?
H12K C125 H12L 107.0 . . ?
C126 C125 N121 118.8(8) . . ?
C126 C125 H12K 107.6 . . ?
C126 C125 H12L 107.6 . . ?
C125 C126 H12M 109.5 . . ?
C125 C126 H12N 109.5 . . ?
C125 C126 H12O 109.5 . . ?
H12M C126 H12N 109.5 . . ?
H12M C126 H12O 109.5 . . ?
H12N C126 H12O 109.5 . . ?
C131 N131 H131 105.4 . . ?
C131 N131 C133 109.3(7) . . ?
C133 N131 H131 105.4 . . ?
C135 N131 H131 105.4 . . ?
C135 N131 C131 116.5(7) . . ?
C135 N131 C133 113.7(8) . . ?
N131 C131 H13A 110.1 . . ?
N131 C131 H13B 110.1 . . ?
N131 C131 C132 108.2(7) . . ?
H13A C131 H13B 108.4 . . ?
C132 C131 H13A 110.1 . . ?
C132 C131 H13B 110.1 . . ?
C131 C132 H13C 109.5 . . ?
C131 C132 H13D 109.5 . . ?
C131 C132 H13E 109.5 . . ?
H13C C132 H13D 109.5 . . ?
H13C C132 H13E 109.5 . . ?
H13D C132 H13E 109.5 . . ?
N131 C133 H13F 111.0 . . ?
N131 C133 H13G 111.0 . . ?
H13F C133 H13G 109.0 . . ?
C134 C133 N131 103.8(8) . . ?
C134 C133 H13F 111.0 . . ?
C134 C133 H13G 111.0 . . ?
C133 C134 H13H 109.5 . . ?
C133 C134 H13I 109.5 . . ?
C133 C134 H13J 109.5 . . ?
H13H C134 H13I 109.5 . . ?
H13H C134 H13J 109.5 . . ?
H13I C134 H13J 109.5 . . ?
N131 C135 H13K 107.4 . . ?
N131 C135 H13L 107.4 . . ?
N131 C135 C136 119.7(8) . . ?
H13K C135 H13L 106.9 . . ?
C136 C135 H13K 107.4 . . ?
C136 C135 H13L 107.4 . . ?
C135 C136 H13M 109.5 . . ?
C135 C136 H13N 109.5 . . ?
C135 C136 H13O 109.5 . . ?
H13M C136 H13N 109.5 . . ?
H13M C136 H13O 109.5 . . ?
H13N C136 H13O 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ge1 O3 C4 C3 168.8(6) . . . . ?
Ge1 O3 C4 C5 -7.7(7) . . . . ?
Ge1 O4 C5 C4 6.5(6) . . . . ?
Ge1 O4 C5 C6 -177.8(5) . . . . ?
Ge1 O13 C14 C13 -162.3(6) . . . . ?
Ge1 O13 C14 C15 20.4(7) . . . . ?
Ge1 O14 C15 C14 -9.9(7) . . . . ?
Ge1 O14 C15 C16 161.7(6) . . . . ?
Ge1 O23 C24 C23 -179.9(5) . . . . ?
Ge1 O23 C24 C25 -3.0(7) . . . . ?
Ge1 O24 C25 C24 -6.8(8) . . . . ?
Ge1 O24 C25 C26 -178.7(6) . . . . ?
Ge2 O33 C34 C33 174.0(6) . . . . ?
Ge2 O33 C34 C35 4.9(9) . . . . ?
Ge2 O34 C35 C34 0.2(9) . . . . ?
Ge2 O34 C35 C36 -177.8(7) . . . . ?
Ge2 O43 C44 C43 -173.8(7) . . . . ?
Ge2 O43 C44 C45 4.5(8) . . . . ?
Ge2 O44 C45 C44 -10.6(9) . . . . ?
Ge2 O44 C45 C46 177.5(6) . . . . ?
Ge2 O53 C54 C53 -176.8(9) . . . . ?
Ge2 O53 C54 C55 2.2(11) . . . . ?
Ge2 O54 C55 C54 -4.7(11) . . . . ?
Ge2 O54 C55 C56 164.9(8) . . . . ?
Ge3 O63 C64 C63 -177.5(7) . . . . ?
Ge3 O63 C64 C65 6.5(8) . . . . ?
Ge3 O64 C65 C64 0.3(9) . . . . ?
Ge3 O64 C65 C66 178.0(7) . . . . ?
Ge3 O73 C74 C73 -174.3(6) . . . . ?
Ge3 O73 C74 C75 13.8(9) . . . . ?
Ge3 O74 C75 C74 -10.5(8) . . . . ?
Ge3 O74 C75 C76 163.1(6) . . . . ?
Ge3 O83 C84 C83 172.2(8) . . . . ?
Ge3 O83 C84 C85 -5.0(10) . . . . ?
Ge3 O84 C85 C84 15.6(8) . . . . ?
Ge3 O84 C85 C86 -178.1(7) . . . . ?
Ge4 O93 C94 C93 -168.4(5) . . . . ?
Ge4 O93 C94 C95 4.2(8) . . . . ?
Ge4 O94 C95 C94 -2.8(8) . . . . ?
Ge4 O94 C95 C96 171.4(5) . . . . ?
Ge4 O103 C104 C103 -174.8(5) . . . . ?
Ge4 O103 C104 C105 5.1(7) . . . . ?
Ge4 O104 C105 C104 -1.7(8) . . . . ?
Ge4 O104 C105 C106 -175.0(6) . . . . ?
Ge4 O113 C114 C113 176.9(6) . . . . ?
Ge4 O113 C114 C115 -12.8(8) . . . . ?
Ge4 O114 C115 C114 1.7(7) . . . . ?
Ge4 O114 C115 C116 -170.0(5) . . . . ?
Sc1 O32 C31 O31 -60.5(12) . . . . ?
Sc1 O32 C31 C32 120.2(7) . . . . ?
Sc1 O51 C51 O52 41.1(15) 2_645 . . . ?
Sc1 O51 C51 C52 -162.5(8) 2_645 . . . ?
Sc1 O61 C61 O62 -30(4) . . . . ?
Sc1 O61 C61 C62 153(3) . . . . ?
Sc1 O92 C91 O91 73.8(9) . . . . ?
Sc1 O92 C91 C92 -108.3(7) . . . . ?
Sc1 O101 C101 O102 -34.0(11) 2_656 . . . ?
Sc1 O101 C101 C102 139.8(5) 2_656 . . . ?
Sc2 O12 C11 O11 5.0(13) . . . . ?
Sc2 O12 C11 C12 -173.1(6) . . . . ?
Sc2 O42 C41 O41 3.3(13) 2_746 . . . ?
Sc2 O42 C41 C42 178.6(5) 2_746 . . . ?
Sc2 O81 C81 O82 14.4(14) 2_656 . . . ?
Sc2 O81 C81 C82 -171.4(7) 2_656 . . . ?
Sc3 O11 C11 O12 -68.0(9) 2_756 . . . ?
Sc3 O11 C11 C12 110.2(6) 2_756 . . . ?
Sc3 O22 C21 O21 54.8(12) . . . . ?
Sc3 O22 C21 C22 -108.4(9) . . . . ?
Sc3 O41 C41 O42 -67.4(13) . . . . ?
Sc3 O41 C41 C42 117.6(9) . . . . ?
Sc3 O71 C71 O72 30.0(14) 2_655 . . . ?
Sc3 O71 C71 C72 -155.0(6) 2_655 . . . ?
Sc3 O82 C81 O81 -73.3(11) 1_465 . . . ?
Sc3 O82 C81 C82 112.5(8) 1_465 . . . ?
Sc3 O111 C111 O112 19.2(16) 1_465 . . . ?
Sc3 O111 C111 C112 -161.3(8) 1_465 . . . ?
Sc4 O2 C1 O1 -0.1(12) 2_655 . . . ?
Sc4 O2 C1 C2 172.8(6) 2_655 . . . ?
Sc4 O52 C51 O51 -45(3) . . . . ?
Sc4 O52 C51 C52 156.6(16) . . . . ?
Sc4 O91 C91 O92 -9.4(13) 2_655 . . . ?
Sc4 O91 C91 C92 172.9(5) 2_655 . . . ?
Sc5 O21 C21 O22 20.8(12) 2_645 . . . ?
Sc5 O21 C21 C22 -176.1(6) 2_645 . . . ?
Sc5 O72 C71 O71 -42(3) . . . . ?
Sc5 O72 C71 C72 143.2(17) . . . . ?
Sc5 O112 C111 O111 -6.9(12) 2 . . . ?
Sc5 O112 C111 C112 173.5(5) 2 . . . ?
Sc6 O31 C31 O32 -16.9(12) 2_646 . . . ?
Sc6 O31 C31 C32 162.4(5) 2_646 . . . ?
Sc6 O62 C61 O61 -5.6(12) 2_646 . . . ?
Sc6 O62 C61 C62 171.9(5) 2_646 . . . ?
Sc6 O102 C101 O101 11(2) . . . . ?
Sc6 O102 C101 C102 -162.3(14) . . . . ?
O1 C1 C2 C3 -179.2(7) . . . . ?
O1 C1 C2 C7 1.8(11) . . . . ?
O2 C1 C2 C3 8.4(12) . . . . ?
O2 C1 C2 C7 -170.6(7) . . . . ?
O3 Ge1 O14 C15 -167.9(4) . . . . ?
O3 Ge1 O24 C25 -89.7(5) . . . . ?
O3 C4 C5 O4 0.5(8) . . . . ?
O3 C4 C5 C6 -175.3(6) . . . . ?
O4 Ge1 O3 C4 9.1(4) . . . . ?
O4 Ge1 O13 C14 -116.5(4) . . . . ?
O4 Ge1 O14 C15 105.7(4) . . . . ?
O4 C5 C6 C7 173.6(6) . . . . ?
O11 C11 C12 C13 -168.4(6) . . . . ?
O11 C11 C12 C17 18.8(10) . . . . ?
O12 C11 C12 C13 9.9(10) . . . . ?
O12 C11 C12 C17 -163.0(7) . . . . ?
O13 Ge1 O14 C15 17.1(4) . . . . ?
O13 Ge1 O24 C25 90.8(5) . . . . ?
O13 C14 C15 O14 -7.7(9) . . . . ?
O13 C14 C15 C16 179.9(6) . . . . ?
O14 Ge1 O3 C4 -86.0(5) . . . . ?
O14 Ge1 O13 C14 -21.3(4) . . . . ?
O14 Ge1 O24 C25 178.4(4) . . . . ?
O14 C15 C16 C17 -167.9(7) . . . . ?
O21 C21 C22 C23 177.7(7) . . . . ?
O21 C21 C22 C27 5.6(11) . . . . ?
O22 C21 C22 C23 -18.4(11) . . . . ?
O22 C21 C22 C27 169.5(6) . . . . ?
O23 Ge1 O3 C4 94.7(4) . . . . ?
O23 Ge1 O13 C14 157.6(4) . . . . ?
O23 Ge1 O24 C25 3.9(4) . . . . ?
O23 C24 C25 O24 6.6(9) . . . . ?
O23 C24 C25 C26 178.2(7) . . . . ?
O24 Ge1 O3 C4 -179.3(4) . . . . ?
O24 Ge1 O13 C14 71.8(4) . . . . ?
O24 Ge1 O14 C15 -77.1(4) . . . . ?
O24 C25 C26 C27 178.2(6) . . . . ?
O31 C31 C32 C33 179.8(8) . . . . ?
O31 C31 C32 C37 3.4(10) . . . . ?
O32 C31 C32 C33 -0.8(11) . . . . ?
O32 C31 C32 C37 -177.2(6) . . . . ?
O33 Ge2 O44 C45 108.7(5) . . . . ?
O33 Ge2 O53 C54 -178.6(7) . . . . ?
O33 C34 C35 O34 -3.3(11) . . . . ?
O33 C34 C35 C36 174.8(7) . . . . ?
O34 Ge2 O33 C34 -3.8(5) . . . . ?
O34 Ge2 O53 C54 -90.7(7) . . . . ?
O34 C35 C36 C37 174.4(7) . . . . ?
O41 C41 C42 C43 169.6(8) . . . . ?
O41 C41 C42 C47 -10.5(11) . . . . ?
O42 C41 C42 C43 -6.2(11) . . . . ?
O42 C41 C42 C47 173.6(7) . . . . ?
O43 Ge2 O33 C34 -87.9(5) . . . . ?
O43 Ge2 O44 C45 10.1(5) . . . . ?
O43 Ge2 O53 C54 -19.5(16) . . . . ?
O43 C44 C45 O44 3.7(10) . . . . ?
O43 C44 C45 C46 175.7(7) . . . . ?
O44 Ge2 O33 C34 -174.5(5) . . . . ?
O44 Ge2 O53 C54 86.9(7) . . . . ?
O44 C45 C46 C47 -173.8(8) . . . . ?
O51 C51 C52 C53 -177.7(11) . . . . ?
O51 C51 C52 C57 3.4(17) . . . . ?
O52 C51 C52 C53 -19.7(15) . . . . ?
O52 C51 C52 C57 161.4(10) . . . . ?
O53 Ge2 O33 C34 87.2(5) . . . . ?
O53 Ge2 O44 C45 -156.5(5) . . . . ?
O53 C54 C55 O54 2.0(14) . . . . ?
O53 C54 C55 C56 -165.2(12) . . . . ?
O54 Ge2 O44 C45 -69.3(5) . . . . ?
O54 Ge2 O53 C54 -4.0(7) . . . . ?
O54 C55 C56 C57 177.6(9) . . . . ?
O61 C61 C62 C63 177.6(7) . . . . ?
O61 C61 C62 C67 -0.6(12) . . . . ?
O62 C61 C62 C63 0.0(11) . . . . ?
O62 C61 C62 C67 -178.1(7) . . . . ?
O63 Ge3 O64 C65 2.7(5) . . . . ?
O63 Ge3 O73 C74 -11.1(15) . . . . ?
O63 Ge3 O83 C84 -73.5(6) . . . . ?
O63 C64 C65 O64 -4.7(10) . . . . ?
O63 C64 C65 C66 177.4(7) . . . . ?
O64 Ge3 O73 C74 77.0(5) . . . . ?
O64 Ge3 O83 C84 -159.6(6) . . . . ?
O64 C65 C66 C67 -177.6(8) . . . . ?
O71 C71 C72 C73 176.6(8) . . . . ?
O71 C71 C72 C77 -0.4(13) . . . . ?
O72 C71 C72 C73 -8.3(12) . . . . ?
O72 C71 C72 C77 174.8(9) . . . . ?
O73 Ge3 O64 C65 -166.2(5) . . . . ?
O73 Ge3 O83 C84 105.7(6) . . . . ?
O73 C74 C75 O74 -1.0(11) . . . . ?
O73 C74 C75 C76 -174.1(8) . . . . ?
O74 Ge3 O64 C65 -82.2(5) . . . . ?
O74 Ge3 O73 C74 -15.1(5) . . . . ?
O74 C75 C76 C77 176.6(8) . . . . ?
O81 C81 C82 C83 170.5(8) . . . . ?
O81 C81 C82 C87 6.5(11) . . . . ?
O82 C81 C82 C83 -15.4(12) . . . . ?
O82 C81 C82 C87 -179.5(8) . . . . ?
O83 Ge3 O64 C65 95.9(5) . . . . ?
O83 Ge3 O73 C74 173.1(5) . . . . ?
O83 C84 C85 O84 -8.2(11) . . . . ?
O83 C84 C85 C86 -174.6(8) . . . . ?
O84 Ge3 O73 C74 -102.5(5) . . . . ?
O84 Ge3 O83 C84 11.0(6) . . . . ?
O84 C85 C86 C87 -170.8(8) . . . . ?
O91 C91 C92 C93 -178.9(6) . . . . ?
O91 C91 C92 C97 12.0(10) . . . . ?
O92 C91 C92 C93 3.2(9) . . . . ?
O92 C91 C92 C97 -165.9(6) . . . . ?
O93 Ge4 O94 C95 4.0(4) . . . . ?
O93 Ge4 O113 C114 97.6(5) . . . . ?
O93 C94 C95 O94 -1.0(10) . . . . ?
O93 C94 C95 C96 -174.9(7) . . . . ?
O94 Ge4 O104 C105 -90.2(5) . . . . ?
O94 Ge4 O113 C114 -177.0(5) . . . . ?
O94 C95 C96 C97 -175.4(6) . . . . ?
O101 C101 C102 C103 -178.7(6) . . . . ?
O101 C101 C102 C107 12.4(10) . . . . ?
O102 C101 C102 C103 -4.4(10) . . . . ?
O102 C101 C102 C107 -173.4(7) . . . . ?
O103 Ge4 O94 C95 91.0(4) . . . . ?
O103 Ge4 O104 C105 3.6(5) . . . . ?
O103 C104 C105 O104 -2.6(9) . . . . ?
O103 C104 C105 C106 170.9(6) . . . . ?
O104 Ge4 O94 C95 177.4(4) . . . . ?
O104 Ge4 O113 C114 -80.6(5) . . . . ?
O104 C105 C106 C107 178.0(6) . . . . ?
O111 C111 C112 C113 171.3(7) . . . . ?
O111 C111 C112 C117 -9.7(11) . . . . ?
O112 C111 C112 C113 -9.1(10) . . . . ?
O112 C111 C112 C117 169.9(7) . . . . ?
O113 Ge4 O94 C95 -88.0(4) . . . . ?
O113 Ge4 O104 C105 176.5(5) . . . . ?
O113 C114 C115 O114 7.6(10) . . . . ?
O113 C114 C115 C116 179.2(6) . . . . ?
O114 Ge4 O104 C105 89.7(5) . . . . ?
O114 Ge4 O113 C114 10.8(5) . . . . ?
O114 C115 C116 C117 -177.2(6) . . . . ?
C1 C2 C3 C4 174.7(7) . . . . ?
C1 C2 C7 C6 -178.2(7) . . . . ?
C2 C3 C4 O3 -175.3(7) . . . . ?
C2 C3 C4 C5 1.3(11) . . . . ?
C3 C2 C7 C6 2.7(9) . . . . ?
C3 C4 C5 O4 -176.2(6) . . . . ?
C3 C4 C5 C6 7.9(10) . . . . ?
C4 C5 C6 C7 -11.1(9) . . . . ?
C5 C6 C7 C2 5.7(9) . . . . ?
C7 C2 C3 C4 -6.3(11) . . . . ?
C11 C12 C13 C14 -172.0(6) . . . . ?
C11 C12 C17 C16 177.9(6) . . . . ?
C12 C13 C14 O13 178.3(6) . . . . ?
C12 C13 C14 C15 -4.6(10) . . . . ?
C13 C12 C17 C16 5.2(11) . . . . ?
C13 C14 C15 O14 175.0(6) . . . . ?
C13 C14 C15 C16 2.6(11) . . . . ?
C14 C15 C16 C17 3.5(10) . . . . ?
C15 C16 C17 C12 -7.3(11) . . . . ?
C17 C12 C13 C14 0.7(10) . . . . ?
C21 C22 C23 C24 -173.5(6) . . . . ?
C21 C22 C27 C26 175.6(7) . . . . ?
C22 C23 C24 O23 178.9(7) . . . . ?
C22 C23 C24 C25 2.0(10) . . . . ?
C23 C22 C27 C26 3.1(10) . . . . ?
C23 C24 C25 O24 -176.3(6) . . . . ?
C23 C24 C25 C26 -4.7(11) . . . . ?
C24 C25 C26 C27 6.8(12) . . . . ?
C25 C26 C27 C22 -5.8(10) . . . . ?
C27 C22 C23 C24 -1.3(11) . . . . ?
C31 C32 C33 C34 -175.4(7) . . . . ?
C31 C32 C37 C36 178.0(6) . . . . ?
C32 C33 C34 O33 -172.3(8) . . . . ?
C32 C33 C34 C35 -4.3(13) . . . . ?
C33 C32 C37 C36 2.0(12) . . . . ?
C33 C34 C35 O34 -171.8(8) . . . . ?
C33 C34 C35 C36 6.2(14) . . . . ?
C34 C35 C36 C37 -3.5(12) . . . . ?
C35 C36 C37 C32 -0.2(11) . . . . ?
C37 C32 C33 C34 0.2(14) . . . . ?
C41 C42 C43 C44 -173.6(7) . . . . ?
C41 C42 C47 C46 -176.8(8) . . . . ?
C42 C43 C44 O43 173.3(8) . . . . ?
C42 C43 C44 C45 -4.9(12) . . . . ?
C43 C42 C47 C46 3.1(13) . . . . ?
C43 C44 C45 O44 -177.6(7) . . . . ?
C43 C44 C45 C46 -5.7(12) . . . . ?
C44 C45 C46 C47 14.6(12) . . . . ?
C45 C46 C47 C42 -13.2(12) . . . . ?
C47 C42 C43 C44 6.5(13) . . . . ?
C51 C52 C53 C54 -170.5(10) . . . . ?
C51 C52 C57 C56 169.4(10) . . . . ?
C52 C53 C54 O53 170.2(10) . . . . ?
C52 C53 C54 C55 -8.8(15) . . . . ?
C53 C52 C57 C56 -9.4(18) . . . . ?
C53 C54 C55 O54 -178.9(9) . . . . ?
C53 C54 C55 C56 13.9(19) . . . . ?
C54 C55 C56 C57 -14.8(18) . . . . ?
C55 C56 C57 C52 11.0(15) . . . . ?
C57 C52 C53 C54 8.3(18) . . . . ?
C61 C62 C63 C64 179.0(7) . . . . ?
C61 C62 C67 C66 -177.8(8) . . . . ?
C62 C63 C64 O63 -175.5(7) . . . . ?
C62 C63 C64 C65 0.4(11) . . . . ?
C63 C62 C67 C66 4.0(12) . . . . ?
C63 C64 C65 O64 179.0(7) . . . . ?
C63 C64 C65 C66 1.1(12) . . . . ?
C64 C65 C66 C67 -0.1(13) . . . . ?
C65 C66 C67 C62 -2.5(13) . . . . ?
C67 C62 C63 C64 -2.9(11) . . . . ?
C71 C72 C73 C74 -175.3(7) . . . . ?
C71 C72 C77 C76 178.2(8) . . . . ?
C72 C73 C74 O73 179.6(7) . . . . ?
C72 C73 C74 C75 -8.4(11) . . . . ?
C73 C72 C77 C76 1.4(14) . . . . ?
C73 C74 C75 O74 -173.8(7) . . . . ?
C73 C74 C75 C76 13.1(13) . . . . ?
C74 C75 C76 C77 -10.4(14) . . . . ?
C75 C76 C77 C72 2.4(14) . . . . ?
C77 C72 C73 C74 1.7(13) . . . . ?
C81 C82 C83 C84 -174.7(8) . . . . ?
C81 C82 C87 C86 176.7(7) . . . . ?
C82 C83 C84 O83 -176.6(9) . . . . ?
C82 C83 C84 C85 0.7(14) . . . . ?
C83 C82 C87 C86 12.7(12) . . . . ?
C83 C84 C85 O84 174.1(7) . . . . ?
C83 C84 C85 C86 7.8(12) . . . . ?
C84 C85 C86 C87 -5.5(14) . . . . ?
C85 C86 C87 C82 -4.7(13) . . . . ?
C87 C82 C83 C84 -11.2(15) . . . . ?
C91 C92 C93 C94 177.0(6) . . . . ?
C91 C92 C97 C96 -179.5(7) . . . . ?
C92 C93 C94 O93 -177.8(6) . . . . ?
C92 C93 C94 C95 10.4(10) . . . . ?
C93 C92 C97 C96 11.4(11) . . . . ?
C93 C94 C95 O94 171.1(6) . . . . ?
C93 C94 C95 C96 -2.8(12) . . . . ?
C94 C95 C96 C97 -1.6(11) . . . . ?
C95 C96 C97 C92 -3.0(11) . . . . ?
C97 C92 C93 C94 -13.8(9) . . . . ?
C101 C102 C103 C104 -176.4(6) . . . . ?
C101 C102 C107 C106 173.1(7) . . . . ?
C102 C103 C104 O103 -170.3(6) . . . . ?
C102 C103 C104 C105 9.7(9) . . . . ?
C103 C102 C107 C106 4.5(11) . . . . ?
C103 C104 C105 O104 177.3(6) . . . . ?
C103 C104 C105 C106 -9.1(10) . . . . ?
C104 C105 C106 C107 5.2(10) . . . . ?
C105 C106 C107 C102 -3.1(11) . . . . ?
C107 C102 C103 C104 -7.3(9) . . . . ?
C111 C112 C113 C114 175.5(7) . . . . ?
C111 C112 C117 C116 -174.4(7) . . . . ?
C112 C113 C114 O113 176.3(7) . . . . ?
C112 C113 C114 C115 6.4(11) . . . . ?
C113 C112 C117 C116 4.5(12) . . . . ?
C113 C114 C115 O114 177.8(7) . . . . ?
C113 C114 C115 C116 -10.5(11) . . . . ?
C114 C115 C116 C117 11.2(10) . . . . ?
C115 C116 C117 C112 -8.2(11) . . . . ?
C117 C112 C113 C114 -3.4(12) . . . . ?
C121 N121 C123 C124 63.4(12) . . . . ?
C121 N121 C125 C126 -177.4(8) . . . . ?
C123 N121 C121 C122 61.4(10) . . . . ?
C123 N121 C125 C126 -37.6(11) . . . . ?
C125 N121 C121 C122 -160.9(7) . . . . ?
C125 N121 C123 C124 -69.7(12) . . . . ?
C131 N131 C133 C134 67.3(9) . . . . ?
C131 N131 C135 C136 169.4(9) . . . . ?
C133 N131 C131 C132 49.1(9) . . . . ?
C133 N131 C135 C136 -62.1(12) . . . . ?
C135 N131 C131 C132 179.6(8) . . . . ?
C135 N131 C133 C134 -64.7(9) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 908 electrons were 
found in a volume of 3887Å³ in 1 void per unit cell. 
This is consistent with the presence of 
6[C2H3N], 9[H2O] per Asymmetric Unit 
which account for 888 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.756 -0.732 -0.799 3886.8 907.7 '24 MeCN,36 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_original_sample_id 'ST L3-Ge + Sc'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.947
_oxdiff_exptl_absorpt_empirical_full_min 0.612
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.501(8)
2 0.499(8)

