# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_km777-3
_database_code_depnum_ccdc_archive 'CCDC 2247475'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H69 N31 Nd2 O49'
_chemical_formula_weight         2008.70

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.3393(3)
_cell_length_b                   13.6235(3)
_cell_length_c                   18.0779(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.504(2)
_cell_angle_gamma                90
_cell_volume                     3403.03(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    16669
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.92

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_F_000             2028
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.649
_shelx_estimated_absorpt_T_min   0.629
_shelx_estimated_absorpt_T_max   0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6
_diffrn_reflns_number            28760
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.898
_diffrn_reflns_theta_max         29.103
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7905
_reflns_number_gt                7174
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)²+3.2292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7905
_refine_ls_number_parameters     634
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0535
_refine_ls_wR_factor_gt          0.0521
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.003
_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
Nd1 Nd 0.58193(2) 0.46637(2) 0.21959(2) 0.01117(4) Uani 1 1 d . . . . .
O1M O 0.66487(11) 0.30037(11) 0.23144(9) 0.0197(3) Uani 1 1 d D . . . .
H11M H 0.6385(13) 0.2502(12) 0.2442(14) 0.024 Uiso 1 1 d D U . . .
H12M H 0.7247(7) 0.3003(16) 0.2530(13) 0.024 Uiso 1 1 d D U . . .
O2M O 0.50550(11) 0.38898(12) 0.30957(10) 0.0232(3) Uani 1 1 d D . . . .
H21M H 0.5348(14) 0.3439(14) 0.3381(13) 0.028 Uiso 1 1 d D U . . .
H22M H 0.4461(8) 0.3744(17) 0.2933(14) 0.028 Uiso 1 1 d D U . . .
O3M O 0.41200(11) 0.52041(12) 0.18374(9) 0.0205(3) Uani 1 1 d D . . . .
H31M H 0.3711(14) 0.5115(18) 0.1411(8) 0.025 Uiso 1 1 d D U . . .
H32M H 0.3870(15) 0.5531(17) 0.2130(10) 0.025 Uiso 1 1 d D U . . .
O4M O 0.58036(13) 0.60317(12) 0.13018(9) 0.0257(4) Uani 1 1 d D . . . .
H41M H 0.5952(19) 0.5936(16) 0.0885(9) 0.031 Uiso 1 1 d D U . . .
H42M H 0.5681(19) 0.6632(9) 0.1337(13) 0.031 Uiso 1 1 d D U . . .
O5M O 0.74548(10) 0.49585(12) 0.20662(9) 0.0182(3) Uani 1 1 d D . . . .
H51M H 0.7551(17) 0.5157(16) 0.1650(9) 0.022 Uiso 1 1 d D U . . .
H52M H 0.7883(14) 0.4550(14) 0.2278(12) 0.022 Uiso 1 1 d D U . . .
O11 O 0.57659(10) 0.61594(10) 0.28955(8) 0.0155(3) Uani 1 1 d . . . . .
O12 O 0.65812(11) 0.79693(11) 0.60935(8) 0.0199(3) Uani 1 1 d . . . . .
C11 C 0.60354(14) 0.68158(14) 0.33767(11) 0.0131(4) Uani 1 1 d . . . . .
C12 C 0.65474(15) 0.79335(15) 0.54119(12) 0.0162(4) Uani 1 1 d . . . . .
C13 C 0.60120(14) 0.82249(15) 0.40952(11) 0.0143(4) Uani 1 1 d . . . . .
H13 H 0.596931 0.888033 0.383924 0.017 Uiso 1 1 calc R U . . .
C14 C 0.70560(14) 0.78107(15) 0.42940(12) 0.0147(4) Uani 1 1 d . . . . .
H14 H 0.753009 0.830912 0.421125 0.018 Uiso 1 1 calc R U . . .
N11 N 0.54512(12) 0.74827(12) 0.35810(10) 0.0138(3) Uani 1 1 d . . . . .
N12 N 0.69678(12) 0.69912(12) 0.37721(10) 0.0142(3) Uani 1 1 d . . . . .
N13 N 0.72363(12) 0.75471(13) 0.51013(10) 0.0164(4) Uani 1 1 d . . . . .
N14 N 0.58118(12) 0.82925(13) 0.48309(10) 0.0155(3) Uani 1 1 d . . . . .
C15 C 0.77643(14) 0.63799(15) 0.37143(11) 0.0143(4) Uani 1 1 d . . . . .
H15A H 0.762251 0.610569 0.318880 0.017 Uiso 1 1 calc R U . . .
H15B H 0.835339 0.678963 0.379644 0.017 Uiso 1 1 calc R U . . .
C16 C 0.81668(15) 0.72139(15) 0.55776(12) 0.0173(4) Uani 1 1 d . . . . .
H16A H 0.868892 0.751289 0.538856 0.021 Uiso 1 1 calc R U . . .
H16B H 0.824581 0.744319 0.611052 0.021 Uiso 1 1 calc R U . . .
O21 O 0.70039(10) 0.44303(10) 0.34752(8) 0.0153(3) Uani 1 1 d . . . . .
O22 O 0.81455(11) 0.58409(11) 0.68077(8) 0.0191(3) Uani 1 1 d . . . . .
C21 C 0.75729(14) 0.46752(14) 0.40871(12) 0.0130(4) Uani 1 1 d . . . . .
C22 C 0.82695(14) 0.55712(15) 0.61932(12) 0.0152(4) Uani 1 1 d . . . . .
C23 C 0.86208(14) 0.56335(15) 0.50095(12) 0.0150(4) Uani 1 1 d . . . . .
H23 H 0.926902 0.588213 0.498747 0.018 Uiso 1 1 calc R U . . .
C24 C 0.86753(14) 0.45565(15) 0.52904(12) 0.0143(4) Uani 1 1 d . . . . .
H24 H 0.933123 0.426850 0.534260 0.017 Uiso 1 1 calc R U . . .
N21 N 0.79534(12) 0.55854(13) 0.42577(10) 0.0142(3) Uani 1 1 d . . . . .
N22 N 0.79383(12) 0.40672(12) 0.46886(10) 0.0142(3) Uani 1 1 d . . . . .
N23 N 0.84631(12) 0.46318(12) 0.60202(10) 0.0146(3) Uani 1 1 d . . . . .
N24 N 0.82679(12) 0.61530(13) 0.55797(10) 0.0157(4) Uani 1 1 d . . . . .
C25 C 0.78155(14) 0.30094(15) 0.46294(12) 0.0148(4) Uani 1 1 d . . . . .
H25A H 0.756796 0.283017 0.408107 0.018 Uiso 1 1 calc R U . . .
H25B H 0.845562 0.269340 0.482699 0.018 Uiso 1 1 calc R U . . .
C26 C 0.84858(14) 0.38079(15) 0.65281(12) 0.0162(4) Uani 1 1 d . . . . .
H26A H 0.902085 0.336380 0.649796 0.019 Uiso 1 1 calc R U . . .
H26B H 0.862082 0.405069 0.706249 0.019 Uiso 1 1 calc R U . . .
O31 O 0.58673(10) 0.23297(10) 0.40016(8) 0.0166(3) Uani 1 1 d . . . . .
O32 O 0.69118(10) 0.39471(11) 0.72425(8) 0.0194(3) Uani 1 1 d . . . . .
C31 C 0.62674(14) 0.22906(14) 0.46900(12) 0.0136(4) Uani 1 1 d . . . . .
C32 C 0.69168(14) 0.33296(15) 0.67501(11) 0.0144(4) Uani 1 1 d . . . . .
C33 C 0.74585(14) 0.24062(15) 0.58593(11) 0.0144(4) Uani 1 1 d . . . . .
H33 H 0.803287 0.196005 0.599638 0.017 Uiso 1 1 calc R U . . .
C34 C 0.65503(14) 0.19161(15) 0.59928(11) 0.0147(4) Uani 1 1 d . . . . .
H34 H 0.669340 0.124556 0.621987 0.018 Uiso 1 1 calc R U . . .
N31 N 0.71663(12) 0.26288(13) 0.50424(10) 0.0152(4) Uani 1 1 d . . . . .
N32 N 0.58887(12) 0.18827(12) 0.52364(10) 0.0150(3) Uani 1 1 d . . . . .
N33 N 0.62633(12) 0.25871(13) 0.65151(10) 0.0151(3) Uani 1 1 d . . . . .
N34 N 0.75931(12) 0.32614(12) 0.63459(10) 0.0148(3) Uani 1 1 d . . . . .
C35 C 0.50445(15) 0.12603(14) 0.50477(12) 0.0162(4) Uani 1 1 d . . . . .
H35A H 0.491106 0.106477 0.450195 0.019 Uiso 1 1 calc R U . . .
H35B H 0.518838 0.065585 0.536161 0.019 Uiso 1 1 calc R U . . .
C36 C 0.55267(14) 0.23493(16) 0.68944(12) 0.0155(4) Uani 1 1 d . . . . .
H36A H 0.563216 0.274983 0.736650 0.019 Uiso 1 1 calc R U . . .
H36B H 0.559332 0.165046 0.704981 0.019 Uiso 1 1 calc R U . . .
N1 N 0.52365(12) 0.32965(13) 0.08894(10) 0.0165(4) Uani 1 1 d . . . . .
O11N O 0.47980(10) 0.33147(11) 0.14090(8) 0.0172(3) Uani 1 1 d . . . . .
O12N O 0.58161(10) 0.39924(11) 0.08771(8) 0.0191(3) Uani 1 1 d . . . . .
O13N O 0.51189(11) 0.26215(12) 0.04205(9) 0.0251(4) Uani 1 1 d . . . . .
N2 N 0.72437(13) 0.53100(12) 0.00688(10) 0.0157(4) Uani 1 1 d . . . . .
O21N O 0.78716(11) 0.52701(11) 0.07018(9) 0.0229(3) Uani 1 1 d . . . . .
O22N O 0.64542(11) 0.57218(12) 0.00104(9) 0.0225(3) Uani 1 1 d . . . . .
O23N O 0.74300(12) 0.49528(14) -0.05109(9) 0.0306(4) Uani 1 1 d . . . . .
N3 N 0.92444(12) 0.37188(13) 0.33100(10) 0.0174(4) Uani 1 1 d . . . . .
O31N O 0.86903(11) 0.34557(12) 0.26718(9) 0.0241(3) Uani 1 1 d . . . . .
O32N O 0.94244(12) 0.46037(11) 0.34415(11) 0.0299(4) Uani 1 1 d . . . . .
O33N O 0.95955(12) 0.30921(12) 0.38020(10) 0.0312(4) Uani 1 1 d . . . . .
N4 N 0.4691(7) 0.5195(6) 0.4653(5) 0.073(2) Uani 0.25 1 d D U P A -1
O41N O 0.5341(8) 0.5174(7) 0.4300(6) 0.055(2) Uani 0.25 1 d D U P A -1
O42N O 0.4726(10) 0.5814(7) 0.5154(6) 0.069(3) Uani 0.25 1 d D U P A -1
O43N O 0.4031(8) 0.4567(9) 0.4482(6) 0.077(2) Uani 0.25 1 d D U P A -1
N5 N 0.4518(6) 0.4948(6) 0.4688(5) 0.068(2) Uani 0.25 1 d D U P B -2
O51N O 0.4450(11) 0.4031(6) 0.4699(7) 0.075(3) Uani 0.25 1 d D U P B -2
O52N O 0.4886(10) 0.5317(7) 0.4193(7) 0.064(2) Uani 0.25 1 d D U P B -2
O53N O 0.4243(10) 0.5456(8) 0.5146(7) 0.074(3) Uani 0.25 1 d D U P B -2
O1W O 0.32666(11) 0.32545(12) 0.26681(9) 0.0225(3) Uani 1 1 d D . . . .
H11W H 0.3301(18) 0.2791(13) 0.3003(12) 0.027 Uiso 1 1 d D U . . .
H12W H 0.2874(15) 0.3685(13) 0.2769(13) 0.027 Uiso 1 1 d D U . . .
O2W O 0.57159(13) 0.13916(12) 0.25733(10) 0.0278(4) Uani 1 1 d D . . . .
H21W H 0.565(2) 0.1346(17) 0.3032(8) 0.033 Uiso 1 1 d D U . . .
H22W H 0.575(2) 0.0801(10) 0.2407(13) 0.033 Uiso 1 1 d D U . . .
O3W O 0.39227(15) 0.01707(13) 0.33131(10) 0.0342(4) Uani 1 1 d D . . . .
H31W H 0.3544(16) -0.0042(19) 0.2887(10) 0.041 Uiso 1 1 d D U . . .
H32W H 0.3605(17) 0.0624(16) 0.3478(14) 0.041 Uiso 1 1 d D 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
Nd1 O1M 2.5374(15) . yes
Nd1 O2M 2.4314(16) . yes
Nd1 O3M 2.4607(15) . yes
Nd1 O4M 2.4632(15) . yes
Nd1 O5M 2.4516(14) . yes
Nd1 O11 2.4103(14) . yes
Nd1 O21 2.4969(14) . yes
Nd1 N1 2.9481(17) . ?
Nd1 O11N 2.5362(14) . yes
Nd1 O12N 2.5524(15) . yes
O1M H11M 0.842(9) . ?
O1M H12M 0.842(9) . ?
O2M H21M 0.840(9) . ?
O2M H22M 0.847(9) . ?
O3M H31M 0.843(9) . ?
O3M H32M 0.842(9) . ?
O4M H41M 0.846(9) . ?
O4M H42M 0.843(9) . ?
O5M H51M 0.845(9) . ?
O5M H52M 0.842(9) . ?
O11 C11 1.235(2) . ?
O12 C12 1.221(3) . ?
C11 N11 1.352(3) . ?
C11 N12 1.358(2) . ?
C12 N13 1.366(3) . ?
C12 N14 1.365(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.549(3) . ?
C13 N11 1.461(2) . ?
C13 N14 1.437(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.445(3) . ?
C14 N13 1.457(3) . ?
N11 C36 1.454(2) 3_666 ?
N12 C15 1.440(3) . ?
N13 C16 1.454(3) . ?
N14 C35 1.439(3) 3_666 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.438(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.453(3) . ?
O21 C21 1.232(2) . ?
O22 C22 1.227(3) . ?
C21 N21 1.357(3) . ?
C21 N22 1.356(3) . ?
C22 N23 1.364(3) . ?
C22 N24 1.363(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.548(3) . ?
C23 N21 1.439(3) . ?
C23 N24 1.449(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.459(2) . ?
C24 N23 1.435(3) . ?
N22 C25 1.452(3) . ?
N23 C26 1.445(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 N31 1.437(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 N34 1.441(3) . ?
O31 C31 1.224(2) . ?
O32 C32 1.226(2) . ?
C31 N31 1.357(3) . ?
C31 N32 1.366(3) . ?
C32 N33 1.367(3) . ?
C32 N34 1.365(3) . ?
C33 H33 1.0000 . ?
C33 C34 1.539(3) . ?
C33 N31 1.455(3) . ?
C33 N34 1.441(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.442(3) . ?
C34 N33 1.451(3) . ?
N32 C35 1.442(3) . ?
N33 C36 1.441(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.263(2) . ?
N1 O12N 1.265(2) . ?
N1 O13N 1.231(2) . ?
N2 O21N 1.254(2) . ?
N2 O22N 1.242(2) . ?
N2 O23N 1.247(2) . ?
N3 O31N 1.265(2) . ?
N3 O32N 1.242(2) . ?
N3 O33N 1.239(2) . ?
N4 O41N 1.263(7) . ?
N4 O42N 1.230(7) . ?
N4 O43N 1.252(7) . ?
N5 O51N 1.254(7) . ?
N5 O52N 1.259(7) . ?
N5 O53N 1.223(7) . ?
O1W H11W 0.867(9) . ?
O1W H12W 0.866(9) . ?
O2W H21W 0.862(9) . ?
O2W H22W 0.865(10) . ?
O3W H31W 0.865(10) . ?
O3W H32W 0.866(10) . ?

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
O1M Nd1 N1 62.00(5) . . ?
O1M Nd1 O12N 69.10(5) . . yes
O2M Nd1 O1M 80.91(5) . . yes
O2M Nd1 O3M 73.40(5) . . yes
O2M Nd1 O4M 147.19(5) . . yes
O2M Nd1 O5M 138.49(5) . . yes
O2M Nd1 O21 69.01(5) . . yes
O2M Nd1 N1 100.37(5) . . ?
O2M Nd1 O11N 76.41(5) . . yes
O2M Nd1 O12N 125.52(5) . . yes
O3M Nd1 O1M 134.24(5) . . yes
O3M Nd1 O4M 76.47(6) . . yes
O3M Nd1 O21 131.50(5) . . yes
O3M Nd1 N1 85.95(5) . . ?
O3M Nd1 O11N 71.72(5) . . yes
O3M Nd1 O12N 96.13(5) . . yes
O4M Nd1 O1M 130.66(5) . . yes
O4M Nd1 O21 126.07(5) . . yes
O4M Nd1 N1 90.08(5) . . ?
O4M Nd1 O11N 106.12(5) . . yes
O4M Nd1 O12N 70.17(5) . . yes
O5M Nd1 O1M 73.46(5) . . yes
O5M Nd1 O3M 146.20(5) . . yes
O5M Nd1 O4M 69.78(5) . . yes
O5M Nd1 O21 71.22(5) . . yes
O5M Nd1 N1 95.76(5) . . ?
O5M Nd1 O11N 119.26(5) . . yes
O5M Nd1 O12N 74.47(5) . . yes
O11 Nd1 O1M 142.10(5) . . yes
O11 Nd1 O2M 86.12(5) . . yes
O11 Nd1 O3M 73.57(5) . . yes
O11 Nd1 O4M 73.06(5) . . yes
O11 Nd1 O5M 94.42(5) . . yes
O11 Nd1 O21 74.39(5) . . yes
O11 Nd1 N1 155.86(5) . . ?
O11 Nd1 O11N 144.33(5) . . yes
O11 Nd1 O12N 143.19(5) . . yes
O21 Nd1 O1M 67.72(5) . . yes
O21 Nd1 N1 129.68(5) . . ?
O21 Nd1 O11N 125.10(5) . . yes
O21 Nd1 O12N 130.57(5) . . yes
O11N Nd1 O1M 65.72(5) . . yes
O11N Nd1 N1 25.21(5) . . ?
O11N Nd1 O12N 50.19(5) . . yes
O12N Nd1 N1 25.30(5) . . ?
Nd1 O1M H11M 120.8(16) . . ?
Nd1 O1M H12M 115.9(16) . . ?
H11M O1M H12M 110.3(15) . . ?
Nd1 O2M H21M 119.2(17) . . ?
Nd1 O2M H22M 117.4(16) . . ?
H21M O2M H22M 109.5(15) . . ?
Nd1 O3M H31M 126.6(15) . . ?
Nd1 O3M H32M 123.4(15) . . ?
H31M O3M H32M 110.0(15) . . ?
Nd1 O4M H41M 120.5(15) . . ?
Nd1 O4M H42M 130.6(16) . . ?
H41M O4M H42M 108.9(15) . . ?
Nd1 O5M H51M 121.8(16) . . ?
Nd1 O5M H52M 116.6(16) . . ?
H51M O5M H52M 110.1(15) . . ?
C11 O11 Nd1 159.01(13) . . ?
O11 C11 N11 125.36(18) . . ?
O11 C11 N12 125.21(19) . . ?
N11 C11 N12 109.42(17) . . ?
O12 C12 N13 126.32(19) . . ?
O12 C12 N14 125.2(2) . . ?
N14 C12 N13 108.49(18) . . ?
C14 C13 H13 111.6 . . ?
N11 C13 H13 111.6 . . ?
N11 C13 C14 103.23(16) . . ?
N14 C13 H13 111.6 . . ?
N14 C13 C14 103.20(16) . . ?
N14 C13 N11 114.91(16) . . ?
C13 C14 H14 111.8 . . ?
N12 C14 C13 102.68(15) . . ?
N12 C14 H14 111.8 . . ?
N12 C14 N13 115.12(17) . . ?
N13 C14 C13 102.93(16) . . ?
N13 C14 H14 111.8 . . ?
C11 N11 C13 111.29(16) . . ?
C11 N11 C36 120.96(16) . 3_666 ?
C36 N11 C13 123.18(16) 3_666 . ?
C11 N12 C14 112.43(16) . . ?
C11 N12 C15 123.26(17) . . ?
C15 N12 C14 124.17(16) . . ?
C12 N13 C14 111.26(17) . . ?
C12 N13 C16 121.81(17) . . ?
C16 N13 C14 124.00(17) . . ?
C12 N14 C13 112.63(17) . . ?
C12 N14 C35 123.36(18) . 3_666 ?
C13 N14 C35 123.92(17) . 3_666 ?
N12 C15 H15A 108.9 . . ?
N12 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
N21 C15 N12 113.22(16) . . ?
N21 C15 H15A 108.9 . . ?
N21 C15 H15B 108.9 . . ?
N13 C16 H16A 109.0 . . ?
N13 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
N24 C16 N13 112.79(16) . . ?
N24 C16 H16A 109.0 . . ?
N24 C16 H16B 109.0 . . ?
C21 O21 Nd1 156.97(13) . . ?
O21 C21 N21 125.54(19) . . ?
O21 C21 N22 125.15(18) . . ?
N22 C21 N21 109.28(17) . . ?
O22 C22 N23 125.2(2) . . ?
O22 C22 N24 126.4(2) . . ?
N24 C22 N23 108.38(18) . . ?
C24 C23 H23 111.6 . . ?
N21 C23 H23 111.6 . . ?
N21 C23 C24 103.24(16) . . ?
N21 C23 N24 115.05(16) . . ?
N24 C23 H23 111.6 . . ?
N24 C23 C24 103.08(16) . . ?
C23 C24 H24 111.5 . . ?
N22 C24 C23 103.03(16) . . ?
N22 C24 H24 111.5 . . ?
N23 C24 C23 103.26(16) . . ?
N23 C24 H24 111.5 . . ?
N23 C24 N22 115.40(16) . . ?
C15 N21 C23 124.55(17) . . ?
C21 N21 C15 122.80(17) . . ?
C21 N21 C23 112.45(17) . . ?
C21 N22 C24 111.50(16) . . ?
C21 N22 C25 122.27(17) . . ?
C25 N22 C24 123.88(16) . . ?
C22 N23 C24 112.60(17) . . ?
C22 N23 C26 123.69(18) . . ?
C24 N23 C26 123.68(17) . . ?
C22 N24 C16 124.00(18) . . ?
C22 N24 C23 111.72(17) . . ?
C23 N24 C16 122.55(17) . . ?
N22 C25 H25A 108.8 . . ?
N22 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N31 C25 N22 113.73(17) . . ?
N31 C25 H25A 108.8 . . ?
N31 C25 H25B 108.8 . . ?
N23 C26 H26A 109.0 . . ?
N23 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
N34 C26 N23 112.86(16) . . ?
N34 C26 H26A 109.0 . . ?
N34 C26 H26B 109.0 . . ?
O31 C31 N31 126.22(19) . . ?
O31 C31 N32 125.72(18) . . ?
N31 C31 N32 108.05(17) . . ?
O32 C32 N33 126.63(19) . . ?
O32 C32 N34 125.34(19) . . ?
N34 C32 N33 108.02(17) . . ?
C34 C33 H33 111.9 . . ?
N31 C33 H33 111.9 . . ?
N31 C33 C34 102.91(16) . . ?
N34 C33 H33 111.9 . . ?
N34 C33 C34 103.64(16) . . ?
N34 C33 N31 113.96(17) . . ?
C33 C34 H34 111.8 . . ?
N32 C34 C33 103.58(16) . . ?
N32 C34 H34 111.8 . . ?
N32 C34 N33 114.08(16) . . ?
N33 C34 C33 103.18(16) . . ?
N33 C34 H34 111.8 . . ?
C25 N31 C33 123.49(16) . . ?
C31 N31 C25 123.00(17) . . ?
C31 N31 C33 112.68(17) . . ?
C31 N32 C34 112.65(16) . . ?
C31 N32 C35 122.61(17) . . ?
C34 N32 C35 122.74(17) . . ?
C32 N33 C34 112.24(16) . . ?
C32 N33 C36 123.16(17) . . ?
C36 N33 C34 122.65(17) . . ?
C26 N34 C33 121.54(16) . . ?
C32 N34 C26 123.88(17) . . ?
C32 N34 C33 112.55(17) . . ?
N14 C35 N32 114.30(16) 3_666 . ?
N14 C35 H35A 108.7 3_666 . ?
N14 C35 H35B 108.7 3_666 . ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
N11 C36 H36A 108.9 3_666 . ?
N11 C36 H36B 108.9 3_666 . ?
N33 C36 N11 113.40(16) . 3_666 ?
N33 C36 H36A 108.9 . . ?
N33 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
O11N N1 Nd1 58.83(9) . . ?
O11N N1 O12N 117.30(16) . . ?
O12N N1 Nd1 59.58(9) . . ?
O13N N1 Nd1 168.73(13) . . ?
O13N N1 O11N 121.54(18) . . ?
O13N N1 O12N 121.15(18) . . ?
N1 O11N Nd1 95.96(11) . . ?
N1 O12N Nd1 95.12(11) . . ?
O22N N2 O21N 120.86(18) . . ?
O22N N2 O23N 119.98(18) . . ?
O23N N2 O21N 119.14(18) . . ?
O32N N3 O31N 119.81(18) . . ?
O33N N3 O31N 119.68(18) . . ?
O33N N3 O32N 120.51(18) . . ?
O42N N4 O41N 119.8(7) . . ?
O42N N4 O43N 122.0(7) . . ?
O43N N4 O41N 118.1(6) . . ?
O51N N5 O52N 117.3(6) . . ?
O53N N5 O51N 120.8(7) . . ?
O53N N5 O52N 121.9(7) . . ?
H11W O1W H12W 105.3(14) . . ?
H21W O2W H22W 107.3(14) . . ?
H31W O3W H32W 106.4(15) . . ?

_refine_diff_density_max         0.582
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.076



####################################################################### 
# 
# 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_km777-4
_database_code_depnum_ccdc_archive 'CCDC 2247476'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H69 N31 O49 Sm2'
_chemical_formula_weight         2020.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.3566(4)
_cell_length_b                   13.5936(4)
_cell_length_c                   18.0138(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.343(3)
_cell_angle_gamma                90
_cell_volume                     3390.24(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    10065
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      29.13

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_F_000             2036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    1.856
_shelx_estimated_absorpt_T_min   0.397
_shelx_estimated_absorpt_T_max   0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6
_diffrn_reflns_number            17023
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.902
_diffrn_reflns_theta_max         29.316
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8021
_reflns_number_gt                7146
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0239P)²+2.3855P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8021
_refine_ls_number_parameters     650
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0591
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_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
Sm1 Sm 0.58238(2) 0.46643(2) 0.21995(2) 0.01144(4) Uani 1 1 d . . . . .
O1M O 0.50696(12) 0.39018(13) 0.30911(10) 0.0220(4) Uani 1 1 d D . . . .
H11M H 0.5351(18) 0.3439(16) 0.3373(15) 0.042(10) Uiso 1 1 d D . . . .
H12M H 0.4474(8) 0.377(2) 0.2927(18) 0.060(12) Uiso 1 1 d D . . . .
O2M O 0.66350(13) 0.30154(13) 0.23169(10) 0.0201(4) Uani 1 1 d D . . . .
H21M H 0.7237(8) 0.298(2) 0.2528(19) 0.060(12) Uiso 1 1 d D . . . .
H22M H 0.6359(18) 0.2511(16) 0.2437(18) 0.047(10) Uiso 1 1 d D . . . .
O3M O 0.74383(12) 0.49576(14) 0.20677(10) 0.0195(4) Uani 1 1 d D . . . .
H31M H 0.753(2) 0.513(2) 0.1643(12) 0.059(12) Uiso 1 1 d D . . . .
H32M H 0.785(2) 0.452(2) 0.2273(18) 0.078(15) Uiso 1 1 d D . . . .
O4M O 0.57987(15) 0.60194(13) 0.13112(10) 0.0260(4) Uani 1 1 d D . . . .
H41M H 0.593(2) 0.589(2) 0.0893(11) 0.044(10) Uiso 1 1 d D . . . .
H42M H 0.573(3) 0.6633(9) 0.1347(17) 0.055(11) Uiso 1 1 d D . . . .
O5M O 0.41443(12) 0.52006(13) 0.18432(10) 0.0205(4) Uani 1 1 d D . . . .
H51M H 0.3892(19) 0.554(2) 0.2135(13) 0.046(10) Uiso 1 1 d D . . . .
H52M H 0.3732(16) 0.512(2) 0.1414(9) 0.037(9) Uiso 1 1 d D . . . .
O11 O 0.57664(11) 0.61460(11) 0.28937(9) 0.0157(3) Uani 1 1 d . . . . .
O12 O 0.65761(12) 0.79727(13) 0.60924(9) 0.0211(4) Uani 1 1 d . . . . .
C11 C 0.60353(16) 0.68099(16) 0.33723(12) 0.0134(4) Uani 1 1 d . . . . .
C12 C 0.65416(17) 0.79360(16) 0.54070(13) 0.0164(5) Uani 1 1 d . . . . .
C13 C 0.60058(17) 0.82261(17) 0.40850(13) 0.0150(5) Uani 1 1 d . . . . .
H13 H 0.595965 0.888219 0.382663 0.018 Uiso 1 1 calc R U . . .
C14 C 0.70490(17) 0.78154(17) 0.42841(13) 0.0148(5) Uani 1 1 d . . . . .
H14 H 0.752003 0.831605 0.419805 0.018 Uiso 1 1 calc R U . . .
N11 N 0.54468(13) 0.74772(14) 0.35738(11) 0.0138(4) Uani 1 1 d . . . . .
N12 N 0.69661(13) 0.69923(14) 0.37653(11) 0.0139(4) Uani 1 1 d . . . . .
N13 N 0.72328(14) 0.75534(15) 0.50953(11) 0.0174(4) Uani 1 1 d . . . . .
N14 N 0.58090(14) 0.82932(14) 0.48258(11) 0.0158(4) Uani 1 1 d . . . . .
C15 C 0.77642(16) 0.63830(17) 0.37063(13) 0.0148(5) Uani 1 1 d . . . . .
H15A H 0.835078 0.679596 0.378865 0.018 Uiso 1 1 calc R U . . .
H15B H 0.762505 0.610897 0.317911 0.018 Uiso 1 1 calc R U . . .
C16 C 0.81621(17) 0.72251(17) 0.55716(13) 0.0185(5) Uani 1 1 d . . . . .
H16A H 0.824024 0.745697 0.610557 0.022 Uiso 1 1 calc R U . . .
H16B H 0.868195 0.752556 0.537960 0.022 Uiso 1 1 calc R U . . .
O21 O 0.70041(11) 0.44306(12) 0.34709(9) 0.0156(3) Uani 1 1 d . . . . .
O22 O 0.81452(12) 0.58487(13) 0.68087(9) 0.0205(4) Uani 1 1 d . . . . .
C21 C 0.75743(16) 0.46764(16) 0.40824(13) 0.0137(4) Uani 1 1 d . . . . .
C22 C 0.82703(16) 0.55779(18) 0.61930(13) 0.0165(5) Uani 1 1 d . . . . .
C23 C 0.86218(16) 0.56372(18) 0.50061(13) 0.0159(5) Uani 1 1 d . . . . .
H23 H 0.926807 0.588764 0.498202 0.019 Uiso 1 1 calc R U . . .
C24 C 0.86784(17) 0.45580(17) 0.52897(13) 0.0157(5) Uani 1 1 d . . . . .
H24 H 0.933361 0.427001 0.534222 0.019 Uiso 1 1 calc R U . . .
N21 N 0.79545(14) 0.55847(14) 0.42519(11) 0.0146(4) Uani 1 1 d . . . . .
N22 N 0.79439(14) 0.40675(14) 0.46869(11) 0.0154(4) Uani 1 1 d . . . . .
N23 N 0.84628(14) 0.46349(14) 0.60209(11) 0.0157(4) Uani 1 1 d . . . . .
N24 N 0.82662(14) 0.61604(14) 0.55760(11) 0.0169(4) Uani 1 1 d . . . . .
C25 C 0.78233(17) 0.30080(17) 0.46285(13) 0.0154(5) Uani 1 1 d . . . . .
H25A H 0.757714 0.282703 0.407896 0.019 Uiso 1 1 calc R U . . .
H25B H 0.846218 0.269183 0.482662 0.019 Uiso 1 1 calc R U . . .
C26 C 0.84885(17) 0.38131(18) 0.65313(13) 0.0184(5) Uani 1 1 d . . . . .
H26A H 0.862299 0.405776 0.706684 0.022 Uiso 1 1 calc R U . . .
H26B H 0.902288 0.336834 0.650011 0.022 Uiso 1 1 calc R U . . .
O31 O 0.58721(12) 0.23358(12) 0.40021(9) 0.0174(3) Uani 1 1 d . . . . .
O32 O 0.69102(12) 0.39567(13) 0.72476(9) 0.0205(4) Uani 1 1 d . . . . .
C31 C 0.62722(16) 0.22923(16) 0.46922(13) 0.0144(4) Uani 1 1 d . . . . .
C32 C 0.69179(16) 0.33352(17) 0.67563(13) 0.0152(5) Uani 1 1 d . . . . .
C33 C 0.74653(16) 0.24075(17) 0.58636(12) 0.0146(5) Uani 1 1 d . . . . .
H33 H 0.803856 0.196046 0.600100 0.017 Uiso 1 1 calc R U . . .
C34 C 0.65512(16) 0.19165(17) 0.59996(13) 0.0157(5) Uani 1 1 d . . . . .
H34 H 0.669108 0.124352 0.622581 0.019 Uiso 1 1 calc R U . . .
N31 N 0.71721(14) 0.26284(15) 0.50459(11) 0.0160(4) Uani 1 1 d . . . . .
N32 N 0.58897(14) 0.18874(14) 0.52398(11) 0.0150(4) Uani 1 1 d . . . . .
N33 N 0.62677(14) 0.25894(14) 0.65256(11) 0.0156(4) Uani 1 1 d . . . . .
N34 N 0.75954(14) 0.32644(14) 0.63498(11) 0.0155(4) Uani 1 1 d . . . . .
C35 C 0.50507(17) 0.12589(16) 0.50536(13) 0.0174(5) Uani 1 1 d . . . . .
H35A H 0.519628 0.065554 0.537105 0.021 Uiso 1 1 calc R U . . .
H35B H 0.491994 0.105918 0.450712 0.021 Uiso 1 1 calc R U . . .
C36 C 0.55281(16) 0.23550(18) 0.69006(13) 0.0165(5) Uani 1 1 d . . . . .
H36A H 0.563135 0.275650 0.737397 0.020 Uiso 1 1 calc R U . . .
H36B H 0.559268 0.165485 0.705708 0.020 Uiso 1 1 calc R U . . .
N1 N 0.52416(14) 0.33086(14) 0.08979(11) 0.0175(4) Uani 1 1 d . . . . .
O11N O 0.48049(11) 0.33275(12) 0.14227(9) 0.0180(3) Uani 1 1 d . . . . .
O12N O 0.58227(12) 0.40027(13) 0.08883(9) 0.0198(4) Uani 1 1 d . . . . .
O13N O 0.51189(12) 0.26345(13) 0.04273(10) 0.0263(4) Uani 1 1 d . . . . .
N2 N 0.92451(14) 0.37143(15) 0.33066(11) 0.0178(4) Uani 1 1 d . . . . .
O21N O 0.86804(12) 0.34537(13) 0.26695(10) 0.0244(4) Uani 1 1 d . . . . .
O22N O 0.94273(14) 0.45984(13) 0.34419(12) 0.0290(4) Uani 1 1 d . . . . .
O23N O 0.96071(14) 0.30818(13) 0.37954(11) 0.0313(5) Uani 1 1 d . . . . .
N3 N 0.72360(15) 0.53088(14) 0.00664(11) 0.0167(4) Uani 1 1 d . . . . .
O31N O 0.64451(12) 0.57271(13) 0.00122(10) 0.0229(4) Uani 1 1 d . . . . .
O32N O 0.78611(13) 0.52662(13) 0.07010(10) 0.0232(4) Uani 1 1 d . . . . .
O33N O 0.74206(14) 0.49575(16) -0.05173(11) 0.0324(5) Uani 1 1 d . . . . .
N4 N 0.4688(9) 0.5194(8) 0.4645(6) 0.076(3) Uani 0.25 1 d D U P A -1
O41N O 0.5342(9) 0.5183(8) 0.4301(7) 0.059(3) Uani 0.25 1 d D U P A -1
O42N O 0.4714(11) 0.5801(8) 0.5155(7) 0.075(3) Uani 0.25 1 d D U P A -1
O43N O 0.4050(9) 0.4551(10) 0.4483(7) 0.079(3) Uani 0.25 1 d D U P A -1
N5 N 0.4508(9) 0.4937(7) 0.4687(6) 0.071(3) Uani 0.25 1 d D U P B -2
O51N O 0.4477(13) 0.4019(7) 0.4707(7) 0.077(3) Uani 0.25 1 d D U P B -2
O52N O 0.4878(11) 0.5321(8) 0.4203(8) 0.068(3) Uani 0.25 1 d D U P B -2
O53N O 0.4219(12) 0.5429(8) 0.5146(8) 0.078(3) Uani 0.25 1 d D U P B -2
O1W O 0.57191(15) 0.13841(14) 0.25750(11) 0.0285(4) Uani 1 1 d D . . . .
H11W H 0.577(3) 0.0789(12) 0.2414(18) 0.069(13) Uiso 1 1 d D . . . .
H12W H 0.565(3) 0.132(3) 0.3037(11) 0.083(15) Uiso 1 1 d D . . . .
O2W O 0.32856(13) 0.32625(14) 0.26731(10) 0.0235(4) Uani 1 1 d D . . . .
H21W H 0.2895(19) 0.3702(16) 0.2762(17) 0.047(10) Uiso 1 1 d D . . . .
H22W H 0.333(2) 0.2806(15) 0.3013(14) 0.043(10) Uiso 1 1 d D . . . .
O3W O 0.39388(17) 0.01730(15) 0.33139(11) 0.0360(5) Uani 1 1 d D . . . .
H31W H 0.357(2) -0.005(3) 0.2895(14) 0.071(13) Uiso 1 1 d D . . . .
H32W H 0.366(2) 0.0670(19) 0.3457(19) 0.069(14) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1M 2.3972(17) . yes
Sm1 O2M 2.5089(17) . yes
Sm1 O3M 2.4246(17) . yes
Sm1 O4M 2.4340(17) . yes
Sm1 O5M 2.4369(17) . yes
Sm1 O11 2.3837(15) . yes
Sm1 O21 2.4827(15) . yes
Sm1 N1 2.9250(19) . ?
Sm1 O11N 2.5133(16) . yes
Sm1 O12N 2.5269(16) . yes
O1M H11M 0.842(10) . ?
O1M H12M 0.846(10) . ?
O2M H21M 0.848(10) . ?
O2M H22M 0.848(10) . ?
O3M H31M 0.845(10) . ?
O3M H32M 0.847(10) . ?
O4M H41M 0.843(10) . ?
O4M H42M 0.846(10) . ?
O5M H51M 0.846(10) . ?
O5M H52M 0.848(10) . ?
O11 C11 1.237(3) . ?
O12 C12 1.224(3) . ?
C11 N11 1.353(3) . ?
C11 N12 1.359(3) . ?
C12 N13 1.366(3) . ?
C12 N14 1.362(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.549(3) . ?
C13 N11 1.462(3) . ?
C13 N14 1.438(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.442(3) . ?
C14 N13 1.459(3) . ?
N11 C36 1.452(3) 3_666 ?
N12 C15 1.440(3) . ?
N13 C16 1.452(3) . ?
N14 C35 1.443(3) 3_666 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.441(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.455(3) . ?
O21 C21 1.232(3) . ?
O22 C22 1.226(3) . ?
C21 N21 1.352(3) . ?
C21 N22 1.359(3) . ?
C22 N23 1.364(3) . ?
C22 N24 1.364(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.549(3) . ?
C23 N21 1.442(3) . ?
C23 N24 1.448(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.459(3) . ?
C24 N23 1.434(3) . ?
N22 C25 1.451(3) . ?
N23 C26 1.441(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 N31 1.441(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 N34 1.444(3) . ?
O31 C31 1.225(3) . ?
O32 C32 1.226(3) . ?
C31 N31 1.359(3) . ?
C31 N32 1.365(3) . ?
C32 N33 1.366(3) . ?
C32 N34 1.367(3) . ?
C33 H33 1.0000 . ?
C33 C34 1.548(3) . ?
C33 N31 1.452(3) . ?
C33 N34 1.440(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.445(3) . ?
C34 N33 1.451(3) . ?
N32 C35 1.442(3) . ?
N33 C36 1.437(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.265(2) . ?
N1 O12N 1.263(3) . ?
N1 O13N 1.229(2) . ?
N2 O21N 1.268(2) . ?
N2 O22N 1.240(3) . ?
N2 O23N 1.242(3) . ?
N3 O31N 1.250(3) . ?
N3 O32N 1.254(3) . ?
N3 O33N 1.246(3) . ?
N4 O41N 1.254(7) . ?
N4 O42N 1.228(7) . ?
N4 O43N 1.244(7) . ?
N5 O51N 1.249(7) . ?
N5 O52N 1.250(7) . ?
N5 O53N 1.218(7) . ?
O1W H11W 0.869(10) . ?
O1W H12W 0.869(10) . ?
O2W H21W 0.863(10) . ?
O2W H22W 0.864(10) . ?
O3W H31W 0.859(10) . ?
O3W H32W 0.860(10) . ?

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
O1M Sm1 O2M 80.74(6) . . ?
O1M Sm1 O3M 138.56(6) . . ?
O1M Sm1 O4M 146.82(6) . . ?
O1M Sm1 O5M 73.44(6) . . ?
O1M Sm1 O21 69.25(6) . . ?
O1M Sm1 N1 100.41(6) . . ?
O1M Sm1 O11N 76.16(6) . . ?
O1M Sm1 O12N 125.71(6) . . ?
O2M Sm1 N1 62.13(5) . . ?
O2M Sm1 O11N 65.78(5) . . ?
O2M Sm1 O12N 69.29(6) . . ?
O3M Sm1 O2M 73.78(6) . . ?
O3M Sm1 O4M 70.09(6) . . ?
O3M Sm1 O5M 146.09(6) . . ?
O3M Sm1 O21 71.01(6) . . ?
O3M Sm1 N1 95.91(6) . . ?
O3M Sm1 O11N 119.67(6) . . ?
O3M Sm1 O12N 74.41(6) . . ?
O4M Sm1 O2M 131.09(6) . . ?
O4M Sm1 O5M 76.05(7) . . ?
O4M Sm1 O21 126.24(6) . . ?
O4M Sm1 N1 89.91(6) . . ?
O4M Sm1 O11N 106.02(6) . . ?
O4M Sm1 O12N 70.04(6) . . ?
O5M Sm1 O2M 133.97(6) . . ?
O5M Sm1 O21 131.87(6) . . ?
O5M Sm1 N1 85.66(6) . . ?
O5M Sm1 O11N 71.34(6) . . ?
O5M Sm1 O12N 95.99(6) . . ?
O11 Sm1 O1M 85.95(6) . . ?
O11 Sm1 O2M 142.22(5) . . ?
O11 Sm1 O3M 94.54(6) . . ?
O11 Sm1 O4M 73.07(6) . . ?
O11 Sm1 O5M 73.52(6) . . ?
O11 Sm1 O21 74.58(5) . . ?
O11 Sm1 N1 155.60(5) . . ?
O11 Sm1 O11N 143.82(5) . . ?
O11 Sm1 O12N 143.08(5) . . ?
O21 Sm1 O2M 67.64(5) . . ?
O21 Sm1 N1 129.75(5) . . ?
O21 Sm1 O11N 125.15(5) . . ?
O21 Sm1 O12N 130.41(5) . . ?
O11N Sm1 N1 25.49(5) . . ?
O11N Sm1 O12N 50.65(5) . . ?
O12N Sm1 N1 25.46(5) . . ?
Sm1 O1M H11M 120(2) . . ?
Sm1 O1M H12M 117(2) . . ?
H11M O1M H12M 109.5(16) . . ?
Sm1 O2M H21M 119(2) . . ?
Sm1 O2M H22M 120(2) . . ?
H21M O2M H22M 109.1(16) . . ?
Sm1 O3M H31M 121(2) . . ?
Sm1 O3M H32M 114(3) . . ?
H31M O3M H32M 109.6(17) . . ?
Sm1 O4M H41M 117.8(19) . . ?
Sm1 O4M H42M 133(2) . . ?
H41M O4M H42M 109.2(16) . . ?
Sm1 O5M H51M 123.6(19) . . ?
Sm1 O5M H52M 127.2(18) . . ?
H51M O5M H52M 109.1(16) . . ?
C11 O11 Sm1 159.10(15) . . ?
O11 C11 N11 125.0(2) . . ?
O11 C11 N12 125.3(2) . . ?
N11 C11 N12 109.60(19) . . ?
O12 C12 N13 126.2(2) . . ?
O12 C12 N14 125.3(2) . . ?
N14 C12 N13 108.5(2) . . ?
C14 C13 H13 111.7 . . ?
N11 C13 H13 111.7 . . ?
N11 C13 C14 103.34(18) . . ?
N14 C13 H13 111.7 . . ?
N14 C13 C14 102.91(18) . . ?
N14 C13 N11 114.75(19) . . ?
C13 C14 H14 111.8 . . ?
N12 C14 C13 102.75(18) . . ?
N12 C14 H14 111.8 . . ?
N12 C14 N13 114.94(19) . . ?
N13 C14 C13 103.15(18) . . ?
N13 C14 H14 111.8 . . ?
C11 N11 C13 110.99(18) . . ?
C11 N11 C36 121.36(19) . 3_666 ?
C36 N11 C13 122.98(19) 3_666 . ?
C11 N12 C14 112.34(19) . . ?
C11 N12 C15 123.25(19) . . ?
C15 N12 C14 124.27(19) . . ?
C12 N13 C14 111.12(19) . . ?
C12 N13 C16 121.86(19) . . ?
C16 N13 C14 124.14(19) . . ?
C12 N14 C13 112.91(19) . . ?
C12 N14 C35 123.5(2) . 3_666 ?
C13 N14 C35 123.52(19) . 3_666 ?
N12 C15 H15A 108.9 . . ?
N12 C15 H15B 108.9 . . ?
N12 C15 N21 113.18(18) . . ?
H15A C15 H15B 107.8 . . ?
N21 C15 H15A 108.9 . . ?
N21 C15 H15B 108.9 . . ?
N13 C16 H16A 109.1 . . ?
N13 C16 H16B 109.1 . . ?
N13 C16 N24 112.70(19) . . ?
H16A C16 H16B 107.8 . . ?
N24 C16 H16A 109.1 . . ?
N24 C16 H16B 109.1 . . ?
C21 O21 Sm1 156.91(15) . . ?
O21 C21 N21 125.6(2) . . ?
O21 C21 N22 125.3(2) . . ?
N21 C21 N22 109.07(19) . . ?
O22 C22 N23 125.1(2) . . ?
O22 C22 N24 126.4(2) . . ?
N24 C22 N23 108.5(2) . . ?
C24 C23 H23 111.6 . . ?
N21 C23 H23 111.6 . . ?
N21 C23 C24 103.17(18) . . ?
N21 C23 N24 114.91(19) . . ?
N24 C23 H23 111.6 . . ?
N24 C23 C24 103.24(18) . . ?
C23 C24 H24 111.6 . . ?
N22 C24 C23 102.88(18) . . ?
N22 C24 H24 111.6 . . ?
N23 C24 C23 103.22(18) . . ?
N23 C24 H24 111.6 . . ?
N23 C24 N22 115.31(19) . . ?
C15 N21 C23 124.34(19) . . ?
C21 N21 C15 122.79(19) . . ?
C21 N21 C23 112.69(19) . . ?
C21 N22 C24 111.72(18) . . ?
C21 N22 C25 122.18(18) . . ?
C25 N22 C24 123.80(18) . . ?
C22 N23 C24 112.53(19) . . ?
C22 N23 C26 123.8(2) . . ?
C24 N23 C26 123.64(19) . . ?
C22 N24 C16 124.1(2) . . ?
C22 N24 C23 111.48(19) . . ?
C23 N24 C16 122.7(2) . . ?
N22 C25 H25A 108.9 . . ?
N22 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
N31 C25 N22 113.50(19) . . ?
N31 C25 H25A 108.9 . . ?
N31 C25 H25B 108.9 . . ?
N23 C26 H26A 109.1 . . ?
N23 C26 H26B 109.1 . . ?
N23 C26 N34 112.62(18) . . ?
H26A C26 H26B 107.8 . . ?
N34 C26 H26A 109.1 . . ?
N34 C26 H26B 109.1 . . ?
O31 C31 N31 126.3(2) . . ?
O31 C31 N32 125.6(2) . . ?
N31 C31 N32 108.11(19) . . ?
O32 C32 N33 126.5(2) . . ?
O32 C32 N34 125.4(2) . . ?
N33 C32 N34 108.10(19) . . ?
C34 C33 H33 112.0 . . ?
N31 C33 H33 112.0 . . ?
N31 C33 C34 102.67(18) . . ?
N34 C33 H33 112.0 . . ?
N34 C33 C34 103.38(18) . . ?
N34 C33 N31 113.94(19) . . ?
C33 C34 H34 111.8 . . ?
N32 C34 C33 103.53(18) . . ?
N32 C34 H34 111.8 . . ?
N32 C34 N33 114.09(18) . . ?
N33 C34 C33 103.16(18) . . ?
N33 C34 H34 111.8 . . ?
C25 N31 C33 123.31(19) . . ?
C31 N31 C25 122.89(19) . . ?
C31 N31 C33 112.97(19) . . ?
C31 N32 C34 112.59(18) . . ?
C31 N32 C35 122.79(19) . . ?
C35 N32 C34 122.39(19) . . ?
C32 N33 C34 112.29(19) . . ?
C32 N33 C36 123.50(19) . . ?
C36 N33 C34 122.49(19) . . ?
C32 N34 C26 123.88(19) . . ?
C32 N34 C33 112.75(19) . . ?
C33 N34 C26 121.34(19) . . ?
N14 C35 H35A 108.7 3_666 . ?
N14 C35 H35B 108.7 3_666 . ?
N32 C35 N14 114.20(18) . 3_666 ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
N11 C36 H36A 108.8 3_666 . ?
N11 C36 H36B 108.8 3_666 . ?
N33 C36 N11 113.93(18) . 3_666 ?
N33 C36 H36A 108.8 . . ?
N33 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
O11N N1 Sm1 58.75(11) . . ?
O12N N1 Sm1 59.36(11) . . ?
O12N N1 O11N 117.05(18) . . ?
O13N N1 Sm1 168.85(15) . . ?
O13N N1 O11N 121.4(2) . . ?
O13N N1 O12N 121.5(2) . . ?
N1 O11N Sm1 95.76(12) . . ?
N1 O12N Sm1 95.18(12) . . ?
O22N N2 O21N 120.0(2) . . ?
O22N N2 O23N 120.3(2) . . ?
O23N N2 O21N 119.7(2) . . ?
O31N N3 O32N 120.6(2) . . ?
O33N N3 O31N 120.0(2) . . ?
O33N N3 O32N 119.4(2) . . ?
O42N N4 O41N 119.9(7) . . ?
O42N N4 O43N 121.5(7) . . ?
O43N N4 O41N 118.6(7) . . ?
O51N N5 O52N 117.5(7) . . ?
O53N N5 O51N 120.5(7) . . ?
O53N N5 O52N 121.9(7) . . ?
H11W O1W H12W 105.8(15) . . ?
H21W O2W H22W 107.0(15) . . ?
H31W O3W H32W 108.4(16) . . ?

_refine_diff_density_max         0.688
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.086




####################################################################### 
# 
# 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_km777-6
_database_code_depnum_ccdc_archive 'CCDC 2247478'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H69 Gd2 N31 O49'
_chemical_formula_weight         2034.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0039 0.0019 'Calculated with ShelXle (H\"ubschle, 2011)'
H H 0.0000 0.0000 'Calculated with ShelXle (H\"ubschle, 2011)'
N N 0.0075 0.0038 'Calculated with ShelXle (H\"ubschle, 2011)'
O O 0.0128 0.0069 'Calculated with ShelXle (H\"ubschle, 2011)'
Gd Gd -0.0886 4.2819 'Calculated with ShelXle (H\"ubschle, 2011)'

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

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

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

_cell_length_a                   14.360(2)
_cell_length_b                   13.586(3)
_cell_length_c                   17.933(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.395(2)
_cell_angle_gamma                90
_cell_volume                     3373.1(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30747
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      31.0

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_F_000             2044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.356
_shelx_estimated_absorpt_T_min   0.538
_shelx_estimated_absorpt_T_max   0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7392
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_absorpt_special_details   ?

_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.74500
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       'φ scan'
_diffrn_detector_area_resol_mean 12.4
_diffrn_reflns_number            31820
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.998
_diffrn_reflns_theta_max         31.077
_diffrn_reflns_theta_full        26.551
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             9256
_reflns_number_gt                8985
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²+5.6376P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9256
_refine_ls_number_parameters     634
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0800
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_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
Gd1 Gd 0.41635(2) 0.53340(2) 0.77962(2) 0.01323(4) Uani 1 1 d . . . . .
O1M O 0.33667(13) 0.69766(13) 0.76846(10) 0.0210(3) Uani 1 1 d D . . . .
H11M H 0.2777(9) 0.699(2) 0.7429(17) 0.025 Uiso 1 1 d D U . . .
H12M H 0.3640(18) 0.7498(15) 0.7586(18) 0.025 Uiso 1 1 d D U . . .
O2M O 0.25631(13) 0.50464(14) 0.79253(10) 0.0203(3) Uani 1 1 d D . . . .
H21M H 0.2143(19) 0.5485(19) 0.7742(16) 0.024 Uiso 1 1 d D U . . .
H22M H 0.247(2) 0.484(2) 0.8351(11) 0.024 Uiso 1 1 d D U . . .
O3M O 0.41893(16) 0.39888(14) 0.86805(11) 0.0276(4) Uani 1 1 d D . . . .
H31M H 0.431(3) 0.3379(10) 0.8652(18) 0.033 Uiso 1 1 d D U . . .
H32M H 0.406(3) 0.410(2) 0.9107(12) 0.033 Uiso 1 1 d D U . . .
O4M O 0.58240(14) 0.47912(14) 0.81591(10) 0.0222(3) Uani 1 1 d D . . . .
H41M H 0.6235(18) 0.487(3) 0.8593(10) 0.027 Uiso 1 1 d D U . . .
H42M H 0.608(2) 0.447(2) 0.7862(14) 0.027 Uiso 1 1 d D U . . .
O5M O 0.49151(13) 0.60809(13) 0.69066(10) 0.0223(3) Uani 1 1 d D . . . .
H51M H 0.4599(17) 0.6515(18) 0.6603(16) 0.027 Uiso 1 1 d D U . . .
H52M H 0.5505(9) 0.626(2) 0.7050(18) 0.027 Uiso 1 1 d D U . . .
O11 O 0.29929(12) 0.55769(13) 0.65291(9) 0.0181(3) Uani 1 1 d . . . . .
O12 O 0.18478(14) 0.41584(14) 0.31750(10) 0.0234(3) Uani 1 1 d . . . . .
C11 C 0.24246(17) 0.53299(15) 0.59166(13) 0.0157(4) Uani 1 1 d . . . . .
C12 C 0.17218(16) 0.44311(19) 0.37960(13) 0.0188(4) Uani 1 1 d . . . . .
C13 C 0.13177(17) 0.54568(18) 0.47020(13) 0.0186(4) Uani 1 1 d . . . . .
H13 H 0.066530 0.575102 0.465045 0.022 Uiso 1 1 calc R U . . .
C14 C 0.13648(16) 0.43729(19) 0.49852(12) 0.0186(4) Uani 1 1 d . . . . .
H14 H 0.071689 0.412558 0.500759 0.022 Uiso 1 1 calc R U . . .
N11 N 0.20569(14) 0.59407(14) 0.53072(11) 0.0175(3) Uani 1 1 d . . . . .
N12 N 0.20351(14) 0.44200(15) 0.57442(11) 0.0175(3) Uani 1 1 d . . . . .
N13 N 0.17235(15) 0.38470(16) 0.44142(11) 0.0197(4) Uani 1 1 d . . . . .
N14 N 0.15292(16) 0.53750(15) 0.39654(12) 0.0206(4) Uani 1 1 d . . . . .
C15 C 0.22202(16) 0.36233(17) 0.62934(12) 0.0171(4) Uani 1 1 d . . . . .
H15A H 0.163318 0.321057 0.620839 0.021 Uiso 1 1 calc R U . . .
H15B H 0.235680 0.389847 0.682262 0.021 Uiso 1 1 calc R U . . .
C16 C 0.18253(17) 0.27816(18) 0.44175(13) 0.0199(4) Uani 1 1 d . . . . .
H16A H 0.130462 0.248196 0.460958 0.024 Uiso 1 1 calc R U . . .
H16B H 0.174643 0.255040 0.388076 0.024 Uiso 1 1 calc R U . . .
O21 O 0.42197(12) 0.38651(12) 0.71051(9) 0.0177(3) Uani 1 1 d . . . . .
O22 O 0.34118(14) 0.20306(14) 0.38947(10) 0.0233(3) Uani 1 1 d . . . . .
C21 C 0.39495(16) 0.31982(15) 0.66261(12) 0.0146(4) Uani 1 1 d . . . . .
C22 C 0.34479(17) 0.20683(17) 0.45864(13) 0.0185(4) Uani 1 1 d . . . . .
C23 C 0.29335(17) 0.21898(16) 0.57119(12) 0.0170(4) Uani 1 1 d . . . . .
H23 H 0.246243 0.168874 0.579778 0.020 Uiso 1 1 calc R U . . .
C24 C 0.39785(17) 0.17786(16) 0.59112(12) 0.0169(4) Uani 1 1 d . . . . .
H24 H 0.402499 0.112314 0.617225 0.020 Uiso 1 1 calc R U . . .
N21 N 0.30218(14) 0.30120(14) 0.62371(11) 0.0165(3) Uani 1 1 d . . . . .
N22 N 0.45391(14) 0.25304(14) 0.64255(11) 0.0162(3) Uani 1 1 d . . . . .
N23 N 0.41817(15) 0.17077(15) 0.51685(11) 0.0186(4) Uani 1 1 d . . . . .
N24 N 0.27533(15) 0.24497(15) 0.48959(11) 0.0193(4) Uani 1 1 d . . . . .
C25 C 0.55113(17) 0.23576(17) 0.69079(12) 0.0185(4) Uani 1 1 d . . . . .
H25A H 0.561368 0.276114 0.738253 0.022 Uiso 1 1 calc R U . . .
H25B H 0.557091 0.165739 0.706635 0.022 Uiso 1 1 calc R U . . .
C26 C 0.50383(18) 0.12610(16) 0.50497(14) 0.0195(4) Uani 1 1 d . . . . .
H26A H 0.490883 0.106262 0.450046 0.023 Uiso 1 1 calc R U . . .
H26B H 0.518167 0.065630 0.536765 0.023 Uiso 1 1 calc R U . . .
O31 O 0.68944(14) 0.39620(14) 0.72513(10) 0.0228(3) Uani 1 1 d . . . . .
O32 O 0.58701(13) 0.23321(12) 0.39943(10) 0.0193(3) Uani 1 1 d . . . . .
C31 C 0.69052(17) 0.33356(17) 0.67634(12) 0.0180(4) Uani 1 1 d . . . . .
C32 C 0.62648(17) 0.22870(16) 0.46911(13) 0.0175(4) Uani 1 1 d . . . . .
C33 C 0.65369(17) 0.19112(17) 0.60052(13) 0.0182(4) Uani 1 1 d . . . . .
H33 H 0.667175 0.123659 0.623100 0.022 Uiso 1 1 calc R U . . .
C34 C 0.74533(17) 0.23953(17) 0.58700(13) 0.0184(4) Uani 1 1 d . . . . .
H34 H 0.802470 0.194603 0.601359 0.022 Uiso 1 1 calc R U . . .
N31 N 0.62560(15) 0.25857(15) 0.65338(11) 0.0192(4) Uani 1 1 d . . . . .
N32 N 0.75845(15) 0.32589(15) 0.63552(11) 0.0190(4) Uani 1 1 d . . . . .
N33 N 0.71699(14) 0.26114(16) 0.50470(11) 0.0192(4) Uani 1 1 d . . . . .
N34 N 0.58801(15) 0.18878(15) 0.52401(11) 0.0184(4) Uani 1 1 d . . . . .
C35 C 0.84799(17) 0.37978(19) 0.65438(13) 0.0215(4) Uani 1 1 d . . . . .
H35A H 0.901103 0.334718 0.651497 0.026 Uiso 1 1 calc R U . . .
H35B H 0.861196 0.403959 0.708256 0.026 Uiso 1 1 calc R U . . .
C36 C 0.78268(16) 0.29953(17) 0.46331(13) 0.0176(4) Uani 1 1 d . . . . .
H36A H 0.758691 0.281396 0.408050 0.021 Uiso 1 1 calc R U . . .
H36B H 0.846622 0.268156 0.483670 0.021 Uiso 1 1 calc R U . . .
N1 N 0.47563(14) 0.66785(15) 0.90984(11) 0.0184(4) Uani 1 1 d . . . . .
O11N O 0.51896(12) 0.66650(12) 0.85656(10) 0.0198(3) Uani 1 1 d . . . . .
O12N O 0.41743(13) 0.59817(13) 0.91068(10) 0.0210(3) Uani 1 1 d . . . . .
O13N O 0.48815(13) 0.73530(14) 0.95750(11) 0.0252(4) Uani 1 1 d . . . . .
N2 N 0.07585(14) 0.62875(15) 0.66929(11) 0.0176(3) Uani 1 1 d . . . . .
O21N O 0.13240(13) 0.65520(14) 0.73310(10) 0.0238(3) Uani 1 1 d . . . . .
O22N O 0.05727(15) 0.54018(13) 0.65600(12) 0.0266(4) Uani 1 1 d . . . . .
O23N O 0.03978(15) 0.69244(14) 0.61997(11) 0.0287(4) Uani 1 1 d . . . . .
N3 N 0.77647(16) 0.03146(13) 0.49390(12) 0.0175(4) Uani 1 1 d . . . . .
O31N O 0.85581(13) 0.07234(14) 0.49916(10) 0.0231(3) Uani 1 1 d . . . . .
O32N O 0.71378(14) 0.02677(13) 0.42991(10) 0.0233(4) Uani 1 1 d . . . . .
O33N O 0.75804(15) -0.00304(17) 0.55296(11) 0.0300(4) Uani 1 1 d . . . . .
N4 N 0.5526(8) 0.5067(7) 0.5335(6) 0.048(2) Uani 0.25 1 d D U P A -1
O41N O 0.5139(12) 0.4674(9) 0.5814(8) 0.055(2) Uani 0.25 1 d D U P A -1
O42N O 0.5826(12) 0.4562(8) 0.4878(8) 0.060(3) Uani 0.25 1 d D U P A -1
O43N O 0.5577(12) 0.5989(7) 0.5326(7) 0.063(2) Uani 0.25 1 d D U P A -1
N5 N 0.5393(8) 0.4845(7) 0.5367(6) 0.056(2) Uani 0.25 1 d D U P B -2
O51N O 0.5409(11) 0.4234(8) 0.4859(7) 0.059(2) Uani 0.25 1 d D U P B -2
O52N O 0.5991(9) 0.5532(10) 0.5535(7) 0.059(2) Uani 0.25 1 d D U P B -2
O53N O 0.4740(9) 0.4790(8) 0.5721(6) 0.041(2) Uani 0.25 1 d D U P B -2
O1W O 0.67035(14) 0.67148(15) 0.73338(10) 0.0249(4) Uani 1 1 d D . . . .
H11W H 0.668(3) 0.7181(17) 0.7000(16) 0.030 Uiso 1 1 d D U . . .
H12W H 0.705(2) 0.6256(17) 0.7202(18) 0.030 Uiso 1 1 d D U . . .
O2W O 0.42831(15) 0.86150(14) 0.74337(11) 0.0276(4) Uani 1 1 d D . . . .
H21W H 0.430(3) 0.870(2) 0.6958(9) 0.033 Uiso 1 1 d D U . . .
H22W H 0.419(3) 0.9195(13) 0.7609(17) 0.033 Uiso 1 1 d D U . . .
O3W O 0.1040(2) 0.51712(16) 0.16823(12) 0.0373(5) Uani 1 1 d D . . . .
H31W H 0.138(2) 0.491(3) 0.2114(14) 0.045 Uiso 1 1 d D U . . .
H32W H 0.133(3) 0.5712(18) 0.161(2) 0.045 Uiso 1 1 d D 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
Gd1 O1M 2.4915(18) . yes
Gd1 O2M 2.4021(18) . yes
Gd1 O3M 2.4136(18) . yes
Gd1 O4M 2.4144(19) . yes
Gd1 O5M 2.3778(18) . yes
Gd1 O11 2.4636(17) . yes
Gd1 O21 2.3618(17) . yes
Gd1 N1 2.9084(19) . ?
Gd1 O11N 2.5031(17) . yes
Gd1 O12N 2.5058(17) . yes
O1M H11M 0.850(10) . ?
O1M H12M 0.851(10) . ?
O2M H21M 0.850(10) . ?
O2M H22M 0.854(10) . ?
O3M H31M 0.849(10) . ?
O3M H32M 0.848(10) . ?
O4M H41M 0.850(10) . ?
O4M H42M 0.845(10) . ?
O5M H51M 0.847(10) . ?
O5M H52M 0.852(10) . ?
O11 C11 1.228(3) . ?
O12 C12 1.232(3) . ?
C11 N11 1.362(3) . ?
C11 N12 1.358(3) . ?
C12 N13 1.363(3) . ?
C12 N14 1.363(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.553(3) . ?
C13 N11 1.458(3) . ?
C13 N14 1.436(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.445(3) . ?
C14 N13 1.451(3) . ?
N11 C36 1.456(3) 3_666 ?
N12 C15 1.440(3) . ?
N13 C16 1.455(3) . ?
N14 C35 1.446(3) 3_666 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.444(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.452(3) . ?
O21 C21 1.238(3) . ?
O22 C22 1.229(3) . ?
C21 N21 1.354(3) . ?
C21 N22 1.353(3) . ?
C22 N23 1.362(3) . ?
C22 N24 1.366(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.552(3) . ?
C23 N21 1.445(3) . ?
C23 N24 1.460(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.466(3) . ?
C24 N23 1.440(3) . ?
N22 C25 1.453(3) . ?
N23 C26 1.437(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 N31 1.439(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 N34 1.443(3) . ?
O31 C31 1.224(3) . ?
O32 C32 1.229(3) . ?
C31 N31 1.368(3) . ?
C31 N32 1.370(3) . ?
C32 N33 1.360(3) . ?
C32 N34 1.363(3) . ?
C33 H33 1.0000 . ?
C33 C34 1.547(3) . ?
C33 N31 1.451(3) . ?
C33 N34 1.444(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.443(3) . ?
C34 N33 1.453(3) . ?
N32 C35 1.440(3) . ?
N33 C36 1.444(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.271(3) . ?
N1 O12N 1.266(3) . ?
N1 O13N 1.233(3) . ?
N2 O21N 1.267(2) . ?
N2 O22N 1.242(3) . ?
N2 O23N 1.247(3) . ?
N3 O31N 1.249(3) . ?
N3 O32N 1.258(3) . ?
N3 O33N 1.249(3) . ?
N4 O41N 1.259(8) . ?
N4 O42N 1.231(7) . ?
N4 O43N 1.255(7) . ?
N5 O51N 1.237(7) . ?
N5 O52N 1.249(8) . ?
N5 O53N 1.267(7) . ?
O1W H11W 0.866(10) . ?
O1W H12W 0.869(10) . ?
O2W H21W 0.866(10) . ?
O2W H22W 0.872(10) . ?
O3W H31W 0.874(10) . ?
O3W H32W 0.872(10) . ?

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
O1M Gd1 N1 62.11(6) . . ?
O1M Gd1 O11N 65.66(6) . . ?
O1M Gd1 O12N 69.46(6) . . ?
O2M Gd1 O1M 73.90(6) . . ?
O2M Gd1 O3M 70.22(7) . . ?
O2M Gd1 O4M 145.69(6) . . ?
O2M Gd1 O11 71.02(6) . . ?
O2M Gd1 N1 96.22(6) . . ?
O2M Gd1 O11N 120.18(6) . . ?
O2M Gd1 O12N 74.61(6) . . ?
O3M Gd1 O1M 131.12(6) . . ?
O3M Gd1 O4M 75.51(7) . . ?
O3M Gd1 O11 126.52(7) . . ?
O3M Gd1 N1 89.88(6) . . ?
O3M Gd1 O11N 106.30(7) . . ?
O3M Gd1 O12N 69.78(6) . . ?
O4M Gd1 O1M 134.02(6) . . ?
O4M Gd1 O11 132.28(6) . . ?
O4M Gd1 N1 85.28(6) . . ?
O4M Gd1 O11N 71.17(6) . . ?
O4M Gd1 O12N 95.43(6) . . ?
O5M Gd1 O1M 81.05(6) . . ?
O5M Gd1 O2M 138.62(6) . . ?
O5M Gd1 O3M 146.46(6) . . ?
O5M Gd1 O4M 73.71(6) . . ?
O5M Gd1 O11 69.16(6) . . ?
O5M Gd1 N1 100.51(6) . . ?
O5M Gd1 O11N 75.87(6) . . ?
O5M Gd1 O12N 126.05(6) . . ?
O11 Gd1 O1M 67.64(6) . . ?
O11 Gd1 N1 129.72(6) . . ?
O11 Gd1 O11N 124.70(6) . . ?
O11 Gd1 O12N 130.61(6) . . ?
O21 Gd1 O1M 142.52(6) . . ?
O21 Gd1 O2M 94.59(6) . . ?
O21 Gd1 O3M 73.04(6) . . ?
O21 Gd1 O4M 73.41(6) . . ?
O21 Gd1 O5M 85.62(6) . . ?
O21 Gd1 O11 74.88(6) . . ?
O21 Gd1 N1 155.30(6) . . ?
O21 Gd1 O11N 143.37(6) . . ?
O21 Gd1 O12N 142.78(6) . . ?
O11N Gd1 N1 25.80(6) . . ?
O11N Gd1 O12N 51.18(6) . . ?
O12N Gd1 N1 25.68(6) . . ?
Gd1 O1M H11M 115(2) . . ?
Gd1 O1M H12M 122(2) . . ?
H11M O1M H12M 109.0(16) . . ?
Gd1 O2M H21M 117(2) . . ?
Gd1 O2M H22M 121(2) . . ?
H21M O2M H22M 108.0(16) . . ?
Gd1 O3M H31M 132(2) . . ?
Gd1 O3M H32M 119(2) . . ?
H31M O3M H32M 108.7(16) . . ?
Gd1 O4M H41M 127(2) . . ?
Gd1 O4M H42M 124(2) . . ?
H41M O4M H42M 109.1(16) . . ?
Gd1 O5M H51M 118(2) . . ?
Gd1 O5M H52M 121(2) . . ?
H51M O5M H52M 108.5(16) . . ?
C11 O11 Gd1 156.45(15) . . ?
O11 C11 N11 125.1(2) . . ?
O11 C11 N12 126.0(2) . . ?
N12 C11 N11 108.9(2) . . ?
O12 C12 N13 126.3(2) . . ?
O12 C12 N14 124.9(2) . . ?
N13 C12 N14 108.9(2) . . ?
C14 C13 H13 111.6 . . ?
N11 C13 H13 111.6 . . ?
N11 C13 C14 102.96(18) . . ?
N14 C13 H13 111.6 . . ?
N14 C13 C14 103.05(18) . . ?
N14 C13 N11 115.4(2) . . ?
C13 C14 H14 111.8 . . ?
N12 C14 C13 103.08(19) . . ?
N12 C14 H14 111.8 . . ?
N12 C14 N13 114.47(19) . . ?
N13 C14 C13 103.23(18) . . ?
N13 C14 H14 111.8 . . ?
C11 N11 C13 111.91(19) . . ?
C11 N11 C36 122.24(19) . 3_666 ?
C36 N11 C13 123.31(19) 3_666 . ?
C11 N12 C14 112.7(2) . . ?
C11 N12 C15 122.58(19) . . ?
C15 N12 C14 124.53(19) . . ?
C12 N13 C14 111.3(2) . . ?
C12 N13 C16 124.1(2) . . ?
C14 N13 C16 122.8(2) . . ?
C12 N14 C13 112.5(2) . . ?
C12 N14 C35 124.0(2) . 3_666 ?
C13 N14 C35 123.5(2) . 3_666 ?
N12 C15 H15A 109.0 . . ?
N12 C15 H15B 109.0 . . ?
N12 C15 N21 112.97(18) . . ?
H15A C15 H15B 107.8 . . ?
N21 C15 H15A 109.0 . . ?
N21 C15 H15B 109.0 . . ?
N13 C16 H16A 109.0 . . ?
N13 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
N24 C16 N13 112.76(19) . . ?
N24 C16 H16A 109.0 . . ?
N24 C16 H16B 109.0 . . ?
C21 O21 Gd1 159.15(16) . . ?
O21 C21 N21 125.4(2) . . ?
O21 C21 N22 124.9(2) . . ?
N22 C21 N21 109.72(19) . . ?
O22 C22 N23 125.1(2) . . ?
O22 C22 N24 125.9(2) . . ?
N23 C22 N24 108.95(19) . . ?
C24 C23 H23 111.8 . . ?
N21 C23 H23 111.8 . . ?
N21 C23 C24 102.48(17) . . ?
N21 C23 N24 115.34(19) . . ?
N24 C23 H23 111.8 . . ?
N24 C23 C24 102.78(18) . . ?
C23 C24 H24 111.6 . . ?
N22 C24 C23 103.30(17) . . ?
N22 C24 H24 111.6 . . ?
N23 C24 C23 103.42(18) . . ?
N23 C24 H24 111.6 . . ?
N23 C24 N22 114.60(19) . . ?
C15 N21 C23 123.81(19) . . ?
C21 N21 C15 123.38(18) . . ?
C21 N21 C23 112.61(19) . . ?
C21 N22 C24 110.90(19) . . ?
C21 N22 C25 121.34(18) . . ?
C25 N22 C24 122.85(18) . . ?
C22 N23 C24 112.29(19) . . ?
C22 N23 C26 123.82(19) . . ?
C26 N23 C24 123.8(2) . . ?
C16 N24 C23 123.92(19) . . ?
C22 N24 C16 122.16(19) . . ?
C22 N24 C23 111.2(2) . . ?
N22 C25 H25A 108.8 . . ?
N22 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N31 C25 N22 113.77(18) . . ?
N31 C25 H25A 108.8 . . ?
N31 C25 H25B 108.8 . . ?
N23 C26 H26A 108.7 . . ?
N23 C26 H26B 108.7 . . ?
N23 C26 N34 114.31(18) . . ?
H26A C26 H26B 107.6 . . ?
N34 C26 H26A 108.7 . . ?
N34 C26 H26B 108.7 . . ?
O31 C31 N31 126.6(2) . . ?
O31 C31 N32 125.5(2) . . ?
N31 C31 N32 107.91(19) . . ?
O32 C32 N33 125.9(2) . . ?
O32 C32 N34 126.0(2) . . ?
N33 C32 N34 108.07(19) . . ?
C34 C33 H33 111.8 . . ?
N31 C33 H33 111.8 . . ?
N31 C33 C34 103.27(19) . . ?
N34 C33 H33 111.8 . . ?
N34 C33 C34 103.22(18) . . ?
N34 C33 N31 114.21(19) . . ?
C33 C34 H34 112.0 . . ?
N32 C34 C33 103.39(18) . . ?
N32 C34 H34 112.0 . . ?
N32 C34 N33 113.88(19) . . ?
N33 C34 C33 102.98(18) . . ?
N33 C34 H34 112.0 . . ?
C25 N31 C33 122.59(19) . . ?
C31 N31 C25 123.46(19) . . ?
C31 N31 C33 112.43(19) . . ?
C31 N32 C34 112.74(19) . . ?
C31 N32 C35 123.6(2) . . ?
C35 N32 C34 121.4(2) . . ?
C32 N33 C34 112.71(19) . . ?
C32 N33 C36 123.32(19) . . ?
C36 N33 C34 123.38(19) . . ?
C26 N34 C33 122.17(19) . . ?
C32 N34 C26 122.58(19) . . ?
C32 N34 C33 112.94(19) . . ?
N14 C35 H35A 109.0 3_666 . ?
N14 C35 H35B 109.0 3_666 . ?
N32 C35 N14 112.90(19) . 3_666 ?
N32 C35 H35A 109.0 . . ?
N32 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
N11 C36 H36A 108.9 3_666 . ?
N11 C36 H36B 108.9 3_666 . ?
N33 C36 N11 113.50(19) . 3_666 ?
N33 C36 H36A 108.9 . . ?
N33 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
O11N N1 Gd1 58.99(11) . . ?
O12N N1 Gd1 59.09(11) . . ?
O12N N1 O11N 117.05(18) . . ?
O13N N1 Gd1 168.77(16) . . ?
O13N N1 O11N 121.4(2) . . ?
O13N N1 O12N 121.5(2) . . ?
N1 O11N Gd1 95.21(13) . . ?
N1 O12N Gd1 95.23(12) . . ?
O22N N2 O21N 120.1(2) . . ?
O22N N2 O23N 120.6(2) . . ?
O23N N2 O21N 119.3(2) . . ?
O31N N3 O32N 120.6(2) . . ?
O31N N3 O33N 119.8(2) . . ?
O33N N3 O32N 119.5(2) . . ?
O42N N4 O41N 120.9(7) . . ?
O42N N4 O43N 121.0(7) . . ?
O43N N4 O41N 118.1(6) . . ?
O51N N5 O52N 122.2(7) . . ?
O51N N5 O53N 119.3(7) . . ?
O52N N5 O53N 118.4(6) . . ?
H11W O1W H12W 105(2) . . ?
H21W O2W H22W 107(2) . . ?
H31W O3W H32W 107(2) . . ?

_refine_diff_density_max         0.759
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.118



####################################################################### 
# 
# 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_km777-10
_database_code_depnum_ccdc_archive 'CCDC 2247480'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_km777-10            
;
PROBLEM: Short Inter D...A Contact  O1M      ..O9W      .       2.49 Ang.
RESPONSE: Hydrogen bonds
;
_vrf_PLAT043_km777-10            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      56.45 Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT306_km777-10            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT430_km777-10_2          
;
PROBLEM: Short Inter D...A Contact  O1M      ..O8W      .       2.68 Ang.
RESPONSE: Hydrogen bonds
;
# Added during the CSD deposition process: Thursday 09 March 2023 03:57 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H92 Dy2 N32 O63'
_chemical_formula_weight         2306.41

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.7641(4)
_cell_length_b                   25.7641(4)
_cell_length_c                   31.6786(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18210.7(7)
_cell_formula_units_Z            9
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    16952
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      28.17

_exptl_crystal_description       brick
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_F_000             10512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.974
_shelx_estimated_absorpt_T_min   0.491
_shelx_estimated_absorpt_T_max   0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6
_diffrn_reflns_number            30539
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.233
_diffrn_reflns_theta_max         28.390
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8927
_reflns_number_gt                8252
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0513P)²+98.0100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8927
_refine_ls_number_parameters     770
_refine_ls_number_restraints     394
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0891
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.003
_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
Dy1 Dy 0.38191(2) 0.36608(2) 0.66354(2) 0.01894(6) Uani 1 1 d . . . . .
O1M O 0.43110(13) 0.47155(12) 0.66994(8) 0.0412(6) Uani 1 1 d . . . . .
O2M O 0.41201(10) 0.40059(11) 0.59493(7) 0.0297(5) Uani 1 1 d . . . . .
O3M O 0.30774(13) 0.39272(14) 0.65869(10) 0.0452(7) Uani 1 1 d . . . . .
O4M O 0.31176(11) 0.29628(12) 0.61404(8) 0.0385(6) Uani 1 1 d . . . . .
O5M O 0.48731(10) 0.40394(11) 0.66301(8) 0.0333(5) Uani 1 1 d . . . . .
O6M O 0.40338(10) 0.38797(11) 0.73573(7) 0.0297(5) Uani 1 1 d . . . . .
O7M O 0.30237(11) 0.29161(11) 0.70482(8) 0.0359(6) Uani 1 1 d . . . . .
O8M O 0.39828(12) 0.28561(12) 0.66627(11) 0.0445(7) Uani 1 1 d . . . . .
O11 O 0.49069(11) 0.74882(10) 0.59579(7) 0.0309(5) Uani 1 1 d . . . . .
O12 O 0.47835(11) 0.74465(10) 0.40636(7) 0.0279(5) Uani 1 1 d . . . . .
C11 C 0.51361(13) 0.76172(13) 0.56048(9) 0.0212(6) Uani 1 1 d . . . . .
C12 C 0.50559(13) 0.75886(13) 0.43995(9) 0.0199(5) Uani 1 1 d . . . . .
C13 C 0.56017(13) 0.75794(12) 0.49833(8) 0.0184(5) Uani 1 1 d . . . . .
H13 H 0.602546 0.766673 0.496529 0.022 Uiso 1 1 calc R U . . .
C14 C 0.55638(12) 0.81608(12) 0.49887(8) 0.0168(5) Uani 1 1 d . . . . .
H14 H 0.596927 0.852832 0.497805 0.020 Uiso 1 1 calc R U . . .
N11 N 0.53228(12) 0.72945(11) 0.53789(7) 0.0216(5) Uani 1 1 d . . . . .
N12 N 0.52580(11) 0.81159(11) 0.53814(7) 0.0194(5) Uani 1 1 d . . . . .
N13 N 0.52151(11) 0.81008(11) 0.46172(7) 0.0186(5) Uani 1 1 d . . . . .
N14 N 0.52610(11) 0.72685(10) 0.46150(7) 0.0191(5) Uani 1 1 d . . . . .
C15 C 0.51584(13) 0.85822(13) 0.55432(9) 0.0207(6) Uani 1 1 d . . . . .
H15A H 0.552243 0.897493 0.549252 0.025 Uiso 1 1 calc R U . . .
H15B H 0.509757 0.853053 0.585227 0.025 Uiso 1 1 calc R U . . .
C16 C 0.51820(12) 0.85992(12) 0.44368(8) 0.0170(5) Uani 1 1 d . . . . .
H16A H 0.555865 0.897478 0.450093 0.020 Uiso 1 1 calc R U . . .
H16B H 0.515039 0.855251 0.412608 0.020 Uiso 1 1 calc R U . . .
O21 O 0.40073(11) 0.81615(12) 0.59212(7) 0.0333(5) Uani 1 1 d . . . . .
O22 O 0.40453(9) 0.82277(9) 0.40218(6) 0.0214(4) Uani 1 1 d . . . . .
C21 C 0.41349(13) 0.84205(14) 0.55774(9) 0.0222(6) Uani 1 1 d . . . . .
C22 C 0.41693(12) 0.84724(12) 0.43687(8) 0.0170(5) Uani 1 1 d . . . . .
C23 C 0.46903(12) 0.89379(12) 0.49856(8) 0.0165(5) Uani 1 1 d . . . . .
H23 H 0.503669 0.935652 0.500270 0.020 Uiso 1 1 calc R U . . .
C24 C 0.40814(12) 0.89241(12) 0.49829(8) 0.0165(5) Uani 1 1 d . . . . .
H24 H 0.413685 0.933676 0.499232 0.020 Uiso 1 1 calc R U . . .
N21 N 0.46500(11) 0.85900(11) 0.53571(7) 0.0196(5) Uani 1 1 d . . . . .
N22 N 0.37880(11) 0.85857(11) 0.53586(7) 0.0199(5) Uani 1 1 d . . . . .
N23 N 0.38111(10) 0.86227(10) 0.45897(7) 0.0167(4) Uani 1 1 d . . . . .
N24 N 0.46836(10) 0.86522(10) 0.45898(7) 0.0171(5) Uani 1 1 d . . . . .
C25 C 0.32466(13) 0.85395(14) 0.55321(9) 0.0220(6) Uani 1 1 d . . . . .
H25A H 0.325863 0.851445 0.584343 0.026 Uiso 1 1 calc R U . . .
H25B H 0.323619 0.890855 0.546156 0.026 Uiso 1 1 calc R U . . .
C26 C 0.32416(12) 0.85165(12) 0.44360(9) 0.0181(5) Uani 1 1 d . . . . .
H26A H 0.323230 0.847038 0.412540 0.022 Uiso 1 1 calc R U . . .
H26B H 0.320334 0.887242 0.449864 0.022 Uiso 1 1 calc R U . . .
O31 O 0.40720(10) 0.82580(10) 0.26465(6) 0.0257(5) Uani 1 1 d . . . . .
O32 O 0.40092(10) 0.81078(10) 0.07517(6) 0.0264(5) Uani 1 1 d . . . . .
C31 C 0.41867(13) 0.84876(13) 0.22946(9) 0.0193(5) Uani 1 1 d . . . . .
C32 C 0.41410(13) 0.83791(13) 0.10867(9) 0.0194(5) Uani 1 1 d . . . . .
C33 C 0.47005(13) 0.89315(12) 0.16692(9) 0.0182(5) Uani 1 1 d . . . . .
H33 H 0.504270 0.935178 0.164684 0.022 Uiso 1 1 calc R U . . .
C34 C 0.40889(12) 0.89095(12) 0.16689(8) 0.0181(5) Uani 1 1 d . . . . .
H34 H 0.413786 0.931856 0.164436 0.022 Uiso 1 1 calc R U . . .
N31 N 0.47005(11) 0.86619(11) 0.20707(7) 0.0196(5) Uani 1 1 d . . . . .
N32 N 0.38307(11) 0.86333(11) 0.20692(7) 0.0190(5) Uani 1 1 d . . . . .
N33 N 0.37861(11) 0.85410(11) 0.13050(7) 0.0192(5) Uani 1 1 d . . . . .
N34 N 0.46638(11) 0.85776(11) 0.13037(7) 0.0190(5) Uani 1 1 d . . . . .
C35 C 0.32539(12) 0.85210(13) 0.22145(9) 0.0187(5) Uani 1 1 d . . . . .
H35A H 0.321402 0.887536 0.214974 0.022 Uiso 1 1 calc R U . . .
H35B H 0.323603 0.847232 0.252507 0.022 Uiso 1 1 calc R U . . .
C36 C 0.32678(13) 0.85222(13) 0.11179(9) 0.0204(6) Uani 1 1 d . . . . .
H36A H 0.327826 0.890397 0.117992 0.025 Uiso 1 1 calc R U . . .
H36B H 0.329053 0.849172 0.080763 0.025 Uiso 1 1 calc R U . . .
N1 N 0.54273(11) 0.53593(11) 0.58783(8) 0.0223(5) Uani 1 1 d . . . . .
O11N O 0.55425(10) 0.51262(10) 0.61843(7) 0.0307(5) Uani 1 1 d . . . . .
O12N O 0.49593(11) 0.50624(12) 0.56675(8) 0.0376(6) Uani 1 1 d . . . . .
O13N O 0.57958(11) 0.58747(10) 0.57673(8) 0.0324(5) Uani 1 1 d . . . . .
N2 N 0.53632(12) 0.53448(11) 0.75208(8) 0.0238(5) Uani 1 1 d . . . . .
O21N O 0.53765(15) 0.53138(13) 0.71274(8) 0.0601(10) Uani 1 1 d . . . . .
O22N O 0.57789(10) 0.57741(10) 0.77078(7) 0.0260(4) Uani 1 1 d . . . . .
O23N O 0.49347(10) 0.49405(10) 0.77209(7) 0.0270(5) Uani 1 1 d . . . . .
N3 N 0.33706(11) 0.33510(11) 0.49538(8) 0.0208(5) Uani 1 1 d . . . . .
O31N O 0.36577(10) 0.38254(10) 0.51600(7) 0.0277(5) Uani 1 1 d . . . . .
O32N O 0.30473(10) 0.33264(10) 0.46542(7) 0.0281(5) Uani 1 1 d . . . . .
O33N O 0.34147(14) 0.29089(11) 0.50453(11) 0.0473(7) Uani 1 1 d . . . . .
N4 N 0.3270(3) 0.1665(2) 0.59270(14) 0.0381(12) Uani 0.604(6) 1 d D U P A 1
O41N O 0.2900(5) 0.1457(4) 0.6217(3) 0.054(2) Uani 0.302(3) 1 d D U P A 1
O41' O 0.3315(5) 0.1699(4) 0.63263(18) 0.0390(17) Uani 0.302(3) 1 d D U P A 1
O42N O 0.3424(3) 0.1324(3) 0.57555(18) 0.0619(16) Uani 0.604(6) 1 d D U P A 1
O43N O 0.3287(3) 0.2082(3) 0.5722(2) 0.0419(15) Uani 0.604(6) 1 d D U P A 1
N5 N 0.3444(6) 0.1693(6) 0.5921(4) 0.048(3) Uani 0.196(6) 1 d D U P A 2
O51N O 0.3904(6) 0.1974(6) 0.6147(4) 0.043(3) Uani 0.196(6) 1 d D U P A 2
O52N O 0.3205(9) 0.1973(9) 0.5775(8) 0.049(3) Uani 0.196(6) 1 d D U P A 2
O53N O 0.3209(9) 0.1148(6) 0.5843(5) 0.052(3) Uani 0.196(6) 1 d D U P A 2
O1W O 0.51158(11) 0.30917(11) 0.66728(7) 0.0311(5) Uani 1 1 d . . . . .
O2W O 0.44541(12) 0.79698(11) 0.33325(7) 0.0306(5) Uani 1 1 d . . . . .
O3W O 0.56116(18) 0.85032(16) 0.33257(12) 0.0654(9) Uani 1 1 d . . . . .
O4W O 0.3717(3) 0.6863(3) 0.3335(2) 0.0324(15) Uani 0.3333 1 d . . P B -1
O5W O 0.3083(3) 0.6560(4) 0.4021(2) 0.0376(19) Uani 0.3333 1 d . . P C -1
O6W O 0.3053(4) 0.6532(4) 0.2665(3) 0.0421(19) Uani 0.3333 1 d . . P D -1
O7W O 0.3215(4) 0.4990(4) 0.66707(18) 0.0352(16) Uani 0.355(3) 1 d . U P E 1
O8W O 0.3696(4) 0.5298(3) 0.66460(16) 0.0373(13) Uani 0.441(3) 1 d . U P F 2
O9W O 0.4617(4) 0.5794(4) 0.6613(3) 0.0153(19) Uani 0.204(3) 1 d . U P G 3
O10W O 0.3234(5) 0.6289(4) 0.5892(3) 0.055(2) Uani 0.3333 1 d . U P H -1
O11W O 0.3291(9) 0.7137(8) 0.6320(7) 0.054(2) Uani 0.1667 1 d . U P I -1
N6 N 0.3098(6) 0.6860(7) 0.1689(4) 0.034(4) Uani 0.12 1 d D U P J -1
O61N O 0.3078(12) 0.6874(13) 0.1296(4) 0.036(4) Uani 0.12 1 d D U P J -1
O62N O 0.2688(10) 0.6433(11) 0.1882(9) 0.036(5) Uani 0.12 1 d D U P J -1
O63N O 0.3525(10) 0.7275(11) 0.1879(8) 0.029(5) Uani 0.12 1 d D U P J -1
N7 N 0.3752(7) 0.6807(7) 0.5018(5) 0.033(4) Uani 0.08 1 d D U P K -1
O71N O 0.3495(11) 0.7103(10) 0.4985(8) 0.032(4) Uani 0.08 1 d D U P K -1
O72N O 0.3668(12) 0.6418(11) 0.4751(7) 0.032(4) Uani 0.08 1 d D U P K -1
O73N O 0.4086(12) 0.6888(13) 0.5322(7) 0.036(4) Uani 0.08 1 d D U P K -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 O1M 2.364(3) . yes
Dy1 O2M 2.330(2) . yes
Dy1 O3M 2.336(3) . yes
Dy1 O4M 2.390(2) . yes
Dy1 O5M 2.383(2) . yes
Dy1 O6M 2.354(2) . yes
Dy1 O7M 2.379(2) . yes
Dy1 O8M 2.315(3) . yes
O11 C11 1.230(4) . ?
O12 C12 1.225(4) . ?
C11 N11 1.354(4) . ?
C11 N12 1.359(4) . ?
C12 N13 1.358(4) . ?
C12 N14 1.364(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.549(4) . ?
C13 N11 1.449(4) . ?
C13 N14 1.439(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.446(4) . ?
C14 N13 1.441(3) . ?
N11 C25 1.441(4) 3_565 ?
N12 C15 1.442(4) . ?
N13 C16 1.446(3) . ?
N14 C26 1.448(4) 3_565 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.446(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.442(3) . ?
O21 C21 1.233(4) . ?
O22 C22 1.227(3) . ?
C21 N21 1.364(4) . ?
C21 N22 1.357(4) . ?
C22 N23 1.360(4) . ?
C22 N24 1.359(4) . ?
C23 H23 1.0000 . ?
C23 C24 1.551(4) . ?
C23 N21 1.451(3) . ?
C23 N24 1.450(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.445(3) . ?
C24 N23 1.449(3) . ?
N22 C25 1.448(4) . ?
N23 C26 1.437(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O31 C31 1.227(4) . ?
O32 C32 1.222(4) . ?
C31 N31 1.365(4) . ?
C31 N32 1.355(4) . ?
C32 N33 1.367(4) . ?
C32 N34 1.364(4) . ?
C33 H33 1.0000 . ?
C33 C34 1.548(4) . ?
C33 N31 1.449(4) . ?
C33 N34 1.447(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.444(3) . ?
C34 N33 1.448(4) . ?
N31 C36 1.439(4) 14_455 ?
N32 C35 1.440(4) . ?
N33 C36 1.440(4) . ?
N34 C35 1.445(4) 14_455 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.252(3) . ?
N1 O12N 1.250(4) . ?
N1 O13N 1.236(3) . ?
N2 O21N 1.250(4) . ?
N2 O22N 1.240(3) . ?
N2 O23N 1.247(3) . ?
N3 O31N 1.250(3) . ?
N3 O32N 1.243(3) . ?
N3 O33N 1.234(3) . ?
N4 O41N 1.236(6) . ?
N4 O41' 1.269(6) . ?
N4 O42N 1.255(5) . ?
N4 O43N 1.238(5) . ?
N5 O51N 1.257(7) . ?
N5 O52N 1.248(7) . ?
N5 O53N 1.245(7) . ?
N6 O61N 1.248(7) . ?
N6 O62N 1.240(7) . ?
N6 O63N 1.241(7) . ?
N7 O71N 1.240(7) . ?
N7 O72N 1.244(7) . ?
N7 O73N 1.235(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1M Dy1 O4M 133.66(10) . . ?
O1M Dy1 O5M 71.57(10) . . ?
O1M Dy1 O7M 129.10(9) . . ?
O2M Dy1 O1M 75.90(9) . . ?
O2M Dy1 O3M 89.52(10) . . ?
O2M Dy1 O4M 69.95(9) . . ?
O2M Dy1 O5M 75.13(8) . . ?
O2M Dy1 O6M 145.23(8) . . ?
O2M Dy1 O7M 143.98(8) . . ?
O3M Dy1 O1M 73.44(11) . . ?
O3M Dy1 O4M 75.87(10) . . ?
O3M Dy1 O5M 144.25(10) . . ?
O3M Dy1 O6M 97.02(9) . . ?
O3M Dy1 O7M 76.81(11) . . ?
O5M Dy1 O4M 125.58(9) . . ?
O6M Dy1 O1M 73.42(9) . . ?
O6M Dy1 O4M 144.74(9) . . ?
O6M Dy1 O5M 79.96(8) . . ?
O6M Dy1 O7M 70.35(8) . . ?
O7M Dy1 O4M 74.41(9) . . ?
O7M Dy1 O5M 132.84(9) . . ?
O8M Dy1 O1M 142.51(10) . . ?
O8M Dy1 O2M 101.63(10) . . ?
O8M Dy1 O3M 143.87(10) . . ?
O8M Dy1 O4M 76.02(11) . . ?
O8M Dy1 O5M 71.71(9) . . ?
O8M Dy1 O6M 92.99(10) . . ?
O8M Dy1 O7M 74.12(10) . . ?
O11 C11 N11 125.7(3) . . ?
O11 C11 N12 125.6(3) . . ?
N11 C11 N12 108.7(2) . . ?
O12 C12 N13 125.5(3) . . ?
O12 C12 N14 126.2(3) . . ?
N13 C12 N14 108.3(2) . . ?
C14 C13 H13 111.9 . . ?
N11 C13 H13 111.9 . . ?
N11 C13 C14 103.0(2) . . ?
N14 C13 H13 111.9 . . ?
N14 C13 C14 103.4(2) . . ?
N14 C13 N11 114.2(2) . . ?
C13 C14 H14 112.0 . . ?
N12 C14 C13 103.1(2) . . ?
N12 C14 H14 112.0 . . ?
N13 C14 C13 103.0(2) . . ?
N13 C14 H14 112.0 . . ?
N13 C14 N12 114.1(2) . . ?
C11 N11 C13 112.6(2) . . ?
C11 N11 C25 123.5(2) . 3_565 ?
C25 N11 C13 123.7(2) 3_565 . ?
C11 N12 C14 112.5(2) . . ?
C11 N12 C15 123.3(2) . . ?
C15 N12 C14 123.8(2) . . ?
C12 N13 C14 112.8(2) . . ?
C12 N13 C16 122.6(2) . . ?
C14 N13 C16 122.5(2) . . ?
C12 N14 C13 112.5(2) . . ?
C12 N14 C26 123.1(2) . 3_565 ?
C13 N14 C26 122.5(2) . 3_565 ?
N12 C15 H15A 108.8 . . ?
N12 C15 H15B 108.8 . . ?
N12 C15 N21 114.0(2) . . ?
H15A C15 H15B 107.7 . . ?
N21 C15 H15A 108.8 . . ?
N21 C15 H15B 108.8 . . ?
N13 C16 H16A 108.8 . . ?
N13 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N24 C16 N13 113.7(2) . . ?
N24 C16 H16A 108.8 . . ?
N24 C16 H16B 108.8 . . ?
O21 C21 N21 125.4(3) . . ?
O21 C21 N22 125.6(3) . . ?
N22 C21 N21 109.1(2) . . ?
O22 C22 N23 124.6(3) . . ?
O22 C22 N24 126.6(3) . . ?
N24 C22 N23 108.8(2) . . ?
C24 C23 H23 111.8 . . ?
N21 C23 H23 111.8 . . ?
N21 C23 C24 103.4(2) . . ?
N24 C23 H23 111.8 . . ?
N24 C23 C24 103.2(2) . . ?
N24 C23 N21 114.1(2) . . ?
C23 C24 H24 111.7 . . ?
N22 C24 C23 103.1(2) . . ?
N22 C24 H24 111.7 . . ?
N22 C24 N23 114.7(2) . . ?
N23 C24 C23 103.1(2) . . ?
N23 C24 H24 111.7 . . ?
C15 N21 C23 123.6(2) . . ?
C21 N21 C15 122.0(2) . . ?
C21 N21 C23 111.7(2) . . ?
C21 N22 C24 112.5(2) . . ?
C21 N22 C25 122.6(2) . . ?
C24 N22 C25 123.6(2) . . ?
C22 N23 C24 112.5(2) . . ?
C22 N23 C26 123.0(2) . . ?
C26 N23 C24 124.4(2) . . ?
C16 N24 C23 123.6(2) . . ?
C22 N24 C16 123.9(2) . . ?
C22 N24 C23 112.4(2) . . ?
N11 C25 N22 113.5(2) 2_665 . ?
N11 C25 H25A 108.9 2_665 . ?
N11 C25 H25B 108.9 2_665 . ?
N22 C25 H25A 108.9 . . ?
N22 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
N14 C26 H26A 108.7 2_665 . ?
N14 C26 H26B 108.7 2_665 . ?
N23 C26 N14 114.2(2) . 2_665 ?
N23 C26 H26A 108.7 . . ?
N23 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
O31 C31 N31 126.2(3) . . ?
O31 C31 N32 125.4(3) . . ?
N32 C31 N31 108.3(2) . . ?
O32 C32 N33 125.2(3) . . ?
O32 C32 N34 126.3(3) . . ?
N34 C32 N33 108.4(2) . . ?
C34 C33 H33 111.7 . . ?
N31 C33 H33 111.7 . . ?
N31 C33 C34 103.1(2) . . ?
N34 C33 H33 111.7 . . ?
N34 C33 C34 103.4(2) . . ?
N34 C33 N31 114.6(2) . . ?
C33 C34 H34 111.8 . . ?
N32 C34 C33 103.1(2) . . ?
N32 C34 H34 111.8 . . ?
N32 C34 N33 114.3(2) . . ?
N33 C34 C33 103.3(2) . . ?
N33 C34 H34 111.8 . . ?
C31 N31 C33 112.4(2) . . ?
C31 N31 C36 124.0(2) . 14_455 ?
C36 N31 C33 123.6(2) 14_455 . ?
C31 N32 C34 113.0(2) . . ?
C31 N32 C35 123.3(2) . . ?
C35 N32 C34 123.7(2) . . ?
C32 N33 C34 112.3(2) . . ?
C32 N33 C36 122.1(2) . . ?
C36 N33 C34 122.4(2) . . ?
C32 N34 C33 112.4(2) . . ?
C32 N34 C35 122.6(2) . 14_455 ?
C35 N34 C33 122.2(2) 14_455 . ?
N32 C35 N34 114.1(2) . 15 ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
N34 C35 H35A 108.7 15 . ?
N34 C35 H35B 108.7 15 . ?
H35A C35 H35B 107.6 . . ?
N31 C36 N33 114.2(2) 15 . ?
N31 C36 H36A 108.7 15 . ?
N31 C36 H36B 108.7 15 . ?
N33 C36 H36A 108.7 . . ?
N33 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
O12N N1 O11N 120.5(3) . . ?
O13N N1 O11N 119.8(3) . . ?
O13N N1 O12N 119.6(3) . . ?
O22N N2 O21N 119.6(3) . . ?
O22N N2 O23N 120.8(3) . . ?
O23N N2 O21N 119.6(3) . . ?
O32N N3 O31N 120.2(3) . . ?
O33N N3 O31N 119.8(3) . . ?
O33N N3 O32N 120.0(3) . . ?
O41N N4 O41' 46.7(7) . . ?
O41N N4 O42N 117.7(6) . . ?
O41N N4 O43N 116.9(7) . . ?
O42N N4 O41' 115.5(5) . . ?
O43N N4 O41' 120.1(5) . . ?
O43N N4 O42N 119.6(5) . . ?
O52N N5 O51N 118.3(9) . . ?
O53N N5 O51N 123.3(13) . . ?
O53N N5 O52N 118.4(9) . . ?
O62N N6 O61N 119.3(7) . . ?
O62N N6 O63N 121.5(7) . . ?
O63N N6 O61N 119.2(7) . . ?
O71N N7 O72N 120.4(7) . . ?
O73N N7 O71N 120.1(7) . . ?
O73N N7 O72N 119.5(7) . . ?

_refine_diff_density_max         1.607
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.113



####################################################################### 
# 
# 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_km777-5
_database_code_depnum_ccdc_archive 'CCDC 2247477'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H69 Eu2 N31 O49'
_chemical_formula_weight         2024.14

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'
Eu Eu -0.1578 3.6682 '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                   13.42009(18)
_cell_length_b                   14.43599(18)
_cell_length_c                   18.2561(2)
_cell_angle_alpha                73.8067(11)
_cell_angle_beta                 87.3433(11)
_cell_angle_gamma                87.7224(11)
_cell_volume                     3391.50(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    26938
_cell_measurement_temperature    140(2)
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      28.59

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_F_000             2040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    1.973
_shelx_estimated_absorpt_T_min   0.682
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6
_diffrn_reflns_number            46829
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.879
_diffrn_reflns_theta_max         28.742
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15953
_reflns_number_gt                14217
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0166P)²+5.1611P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15953
_refine_ls_number_parameters     1270
_refine_ls_number_restraints     380
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0564
_refine_ls_wR_factor_gt          0.0549
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.003
_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
Eu1 Eu 0.95224(2) 0.91746(2) 0.22472(2) 0.01130(3) Uani 1 1 d . . . . .
O11M O 0.78669(13) 0.83970(14) 0.24415(11) 0.0210(4) Uani 1 1 d D . . . .
H111 H 0.7859(19) 0.7808(8) 0.2683(16) 0.025 Uiso 1 1 d D U . . .
H112 H 0.7310(12) 0.8667(16) 0.2490(17) 0.025 Uiso 1 1 d D U . . .
O12M O 0.99055(14) 0.75851(13) 0.21122(10) 0.0175(4) Uani 1 1 d D . . . .
H121 H 0.9462(16) 0.7167(16) 0.2268(14) 0.021 Uiso 1 1 d D U . . .
H122 H 1.0157(19) 0.7534(19) 0.1690(10) 0.021 Uiso 1 1 d D U . . .
O13M O 1.08718(14) 0.92554(15) 0.12978(11) 0.0239(4) Uani 1 1 d D . . . .
H131 H 1.1475(10) 0.935(2) 0.1361(15) 0.029 Uiso 1 1 d D U . . .
H132 H 1.0834(19) 0.909(2) 0.0887(11) 0.029 Uiso 1 1 d D U . . .
O14M O 1.00548(14) 1.08384(13) 0.18840(10) 0.0195(4) Uani 1 1 d D . . . .
H141 H 1.003(2) 1.1209(17) 0.1437(7) 0.023 Uiso 1 1 d D U . . .
H142 H 1.0411(19) 1.1076(18) 0.2150(12) 0.023 Uiso 1 1 d D U . . .
O15M O 0.87366(16) 0.99710(14) 0.31154(12) 0.0283(5) Uani 1 1 d D . . . .
H151 H 0.8286(16) 0.9695(16) 0.3439(15) 0.034 Uiso 1 1 d D U . . .
H152 H 0.860(2) 1.0571(7) 0.2972(17) 0.034 Uiso 1 1 d D U . . .
N1 N 0.81915(16) 0.97399(15) 0.09667(12) 0.0178(4) Uani 1 1 d . . . . .
O11N O 0.82169(13) 1.02003(13) 0.14650(10) 0.0187(4) Uani 1 1 d . . . . .
O12N O 0.88615(14) 0.91043(13) 0.09810(10) 0.0205(4) Uani 1 1 d . . . . .
O13N O 0.75211(15) 0.98994(14) 0.05057(12) 0.0281(5) Uani 1 1 d . . . . .
O11 O 1.10499(12) 0.91549(12) 0.28607(10) 0.0151(4) Uani 1 1 d . . . . .
O12 O 1.29010(13) 0.83040(13) 0.59563(10) 0.0181(4) Uani 1 1 d D . . . .
C11 C 1.17194(17) 0.88399(17) 0.33145(13) 0.0121(5) Uani 1 1 d . . . . .
C12 C 1.28720(17) 0.83065(17) 0.52891(14) 0.0136(5) Uani 1 1 d . . . . .
C13 C 1.31794(17) 0.87700(17) 0.39694(13) 0.0119(5) Uani 1 1 d . . . . .
H13 H 1.384258 0.875760 0.369850 0.014 Uiso 1 1 calc R U . . .
C14 C 1.27082(17) 0.77635(17) 0.42074(13) 0.0122(5) Uani 1 1 d . . . . .
H14 H 1.318389 0.725175 0.411805 0.015 Uiso 1 1 calc R U . . .
N11 N 1.24460(15) 0.93740(14) 0.34699(11) 0.0122(4) Uani 1 1 d . . . . .
N12 N 1.18589(15) 0.79035(14) 0.37224(11) 0.0125(4) Uani 1 1 d . . . . .
N13 N 1.24633(15) 0.76190(15) 0.50161(11) 0.0136(4) Uani 1 1 d . . . . .
N14 N 1.32688(15) 0.89927(15) 0.46798(11) 0.0130(4) Uani 1 1 d . . . . .
C15 C 1.12016(17) 0.71389(17) 0.37094(13) 0.0124(5) Uani 1 1 d . . . . .
H15A H 1.091251 0.728572 0.319910 0.015 Uiso 1 1 calc R U . . .
H15B H 1.159743 0.652772 0.378923 0.015 Uiso 1 1 calc R U . . .
C16 C 1.20972(17) 0.67272(17) 0.55238(13) 0.0139(5) Uani 1 1 d . . . . .
H16A H 1.234212 0.665027 0.604126 0.017 Uiso 1 1 calc R U . . .
H16B H 1.237209 0.617884 0.534444 0.017 Uiso 1 1 calc R U . . .
O21 O 0.92702(13) 0.80476(13) 0.35353(10) 0.0162(4) Uani 1 1 d . . . . .
O22 O 1.07611(13) 0.68535(13) 0.67876(10) 0.0179(4) Uani 1 1 d . . . . .
C21 C 0.95052(17) 0.74762(17) 0.41433(13) 0.0122(5) Uani 1 1 d . . . . .
C22 C 1.04534(18) 0.67300(17) 0.62020(14) 0.0137(5) Uani 1 1 d . . . . .
C23 C 1.04484(17) 0.63588(17) 0.50397(13) 0.0120(5) Uani 1 1 d . . . . .
H23 H 1.066358 0.569073 0.503081 0.014 Uiso 1 1 calc R U . . .
C24 C 0.93578(17) 0.63956(17) 0.53586(13) 0.0125(5) Uani 1 1 d . . . . .
H24 H 0.901667 0.577395 0.541853 0.015 Uiso 1 1 calc R U . . .
N21 N 1.04034(15) 0.70071(15) 0.42791(11) 0.0129(4) Uani 1 1 d . . . . .
N22 N 0.88961(15) 0.71923(15) 0.47749(11) 0.0131(4) Uani 1 1 d . . . . .
N23 N 0.94811(15) 0.65797(15) 0.60829(11) 0.0130(4) Uani 1 1 d . . . . .
N24 N 1.10140(15) 0.66936(15) 0.55676(11) 0.0136(4) Uani 1 1 d . . . . .
C25 C 0.78201(17) 0.73753(18) 0.47440(14) 0.0139(5) Uani 1 1 d . . . . .
H25A H 0.764279 0.764544 0.420411 0.017 Uiso 1 1 calc R U . . .
H25B H 0.748037 0.675409 0.494457 0.017 Uiso 1 1 calc R U . . .
C26 C 0.86644(18) 0.66342(17) 0.66149(14) 0.0140(5) Uani 1 1 d . . . . .
H26A H 0.892571 0.649866 0.713367 0.017 Uiso 1 1 calc R U . . .
H26B H 0.818301 0.612953 0.662141 0.017 Uiso 1 1 calc R U . . .
O31 O 0.71487(13) 0.93586(13) 0.41523(10) 0.0175(4) Uani 1 1 d D . . . .
O32 O 0.89100(13) 0.82128(13) 0.72705(10) 0.0186(4) Uani 1 1 d . . . . .
C31 C 0.71063(17) 0.89394(18) 0.48410(14) 0.0137(5) Uani 1 1 d . . . . .
C32 C 0.82587(18) 0.82335(17) 0.68175(13) 0.0137(5) Uani 1 1 d . . . . .
C33 C 0.72572(17) 0.77342(17) 0.59929(13) 0.0128(5) Uani 1 1 d . . . . .
H33 H 0.680027 0.717690 0.615252 0.015 Uiso 1 1 calc R U . . .
C34 C 0.67803(18) 0.86579(17) 0.61535(13) 0.0130(5) Uani 1 1 d . . . . .
H34 H 0.611946 0.852805 0.643311 0.016 Uiso 1 1 calc R U . . .
N31 N 0.74522(15) 0.80318(15) 0.51723(11) 0.0137(4) Uani 1 1 d . . . . .
N32 N 0.66792(15) 0.93090(14) 0.53956(11) 0.0138(4) Uani 1 1 d . . . . .
N33 N 0.75137(15) 0.89239(15) 0.66148(11) 0.0139(4) Uani 1 1 d . . . . .
N34 N 0.81482(15) 0.75637(14) 0.64293(11) 0.0130(4) Uani 1 1 d . . . . .
C35 C 0.61466(18) 1.02297(17) 0.52472(14) 0.0145(5) Uani 1 1 d . . . . .
H35A H 0.589634 1.039696 0.472341 0.017 Uiso 1 1 calc R U . . .
H35B H 0.556005 1.016414 0.560558 0.017 Uiso 1 1 calc R U . . .
C36 C 0.73313(18) 0.96603(17) 0.70040(13) 0.0139(5) Uani 1 1 d . . . . .
H36A H 0.774355 0.950877 0.746057 0.017 Uiso 1 1 calc R U . . .
H36B H 0.662205 0.964933 0.718049 0.017 Uiso 1 1 calc R U . . .
Eu2 Eu 0.53421(2) 0.42761(2) 0.71533(2) 0.01146(3) Uani 1 1 d . . . . .
O21M O 0.40340(14) 0.43399(16) 0.62615(11) 0.0258(4) Uani 1 1 d D . . . .
H211 H 0.4156(19) 0.414(2) 0.5868(12) 0.031 Uiso 1 1 d D U . . .
H212 H 0.3409(8) 0.438(2) 0.6331(16) 0.031 Uiso 1 1 d D U . . .
O22M O 0.50880(14) 0.26791(13) 0.70386(10) 0.0188(4) Uani 1 1 d D . . . .
H221 H 0.5449(19) 0.2221(15) 0.7294(13) 0.023 Uiso 1 1 d D U . . .
H222 H 0.488(2) 0.2535(19) 0.6655(11) 0.023 Uiso 1 1 d D U . . .
O23M O 0.70180(13) 0.34347(13) 0.72767(10) 0.0171(4) Uani 1 1 d D . . . .
H231 H 0.7049(19) 0.2844(8) 0.7522(14) 0.020 Uiso 1 1 d D U . . .
H232 H 0.7489(16) 0.3722(15) 0.7405(15) 0.020 Uiso 1 1 d D U . . .
O24M O 0.60498(14) 0.49520(13) 0.80628(11) 0.0213(4) Uani 1 1 d D . . . .
H241 H 0.625(2) 0.5525(9) 0.7918(16) 0.026 Uiso 1 1 d D U . . .
H242 H 0.6448(18) 0.4612(15) 0.8382(14) 0.026 Uiso 1 1 d D U . . .
O25M O 0.48050(15) 0.59564(13) 0.68059(11) 0.0224(4) Uani 1 1 d D . . . .
H251 H 0.492(2) 0.6344(16) 0.6370(8) 0.027 Uiso 1 1 d D U . . .
H252 H 0.457(2) 0.6274(17) 0.7103(12) 0.027 Uiso 1 1 d D U . . .
N2 N 0.67627(15) 0.48605(15) 0.58678(12) 0.0154(4) Uani 1 1 d . . . . .
O21N O 0.67190(13) 0.52855(12) 0.63887(10) 0.0173(4) Uani 1 1 d . . . . .
O22N O 0.60645(13) 0.42967(13) 0.58652(10) 0.0163(4) Uani 1 1 d . . . . .
O23N O 0.74573(14) 0.49795(14) 0.53929(11) 0.0234(4) Uani 1 1 d D . . . .
O41 O 0.55165(13) 0.30772(12) 0.84050(9) 0.0154(4) Uani 1 1 d . . . . .
O42 O 0.38885(13) 0.18511(13) 1.17103(10) 0.0195(4) Uani 1 1 d . . . . .
C41 C 0.52420(18) 0.24907(17) 0.90031(14) 0.0130(5) Uani 1 1 d . . . . .
C42 C 0.42067(18) 0.17581(17) 1.10959(14) 0.0142(5) Uani 1 1 d . . . . .
C43 C 0.53119(18) 0.13636(17) 1.01956(14) 0.0138(5) Uani 1 1 d . . . . .
H43 H 0.560855 0.069895 1.026881 0.017 Uiso 1 1 calc R U . . .
C44 C 0.42275(18) 0.14414(17) 0.99121(14) 0.0139(5) Uani 1 1 d . . . . .
H44 H 0.399766 0.080682 0.987329 0.017 Uiso 1 1 calc R U . . .
N41 N 0.58381(15) 0.20689(15) 0.95907(11) 0.0140(4) Uani 1 1 d . . . . .
N42 N 0.43101(15) 0.21421(15) 0.91708(12) 0.0146(4) Uani 1 1 d . . . . .
N43 N 0.36556(15) 0.17659(15) 1.04866(12) 0.0152(4) Uani 1 1 d . . . . .
N44 N 0.51874(15) 0.16089(15) 1.09084(11) 0.0142(4) Uani 1 1 d . . . . .
C45 C 0.35216(18) 0.23817(17) 0.86335(14) 0.0140(5) Uani 1 1 d . . . . .
H45A H 0.309225 0.181716 0.871500 0.017 Uiso 1 1 calc R U . . .
H45B H 0.381928 0.252046 0.810909 0.017 Uiso 1 1 calc R U . . .
C46 C 0.25840(18) 0.19350(18) 1.04751(15) 0.0162(5) Uani 1 1 d . . . . .
H46A H 0.231638 0.183768 1.100486 0.019 Uiso 1 1 calc R U . . .
H46B H 0.227823 0.145696 1.026341 0.019 Uiso 1 1 calc R U . . .
O51 O 0.38265(12) 0.43624(12) 0.78404(10) 0.0161(4) Uani 1 1 d . . . . .
O52 O 0.19390(13) 0.35281(13) 1.10438(10) 0.0190(4) Uani 1 1 d . . . . .
C51 C 0.31401(17) 0.41214(17) 0.83219(13) 0.0129(5) Uani 1 1 d . . . . .
C52 C 0.19618(17) 0.35975(18) 1.03569(14) 0.0147(5) Uani 1 1 d . . . . .
C53 C 0.20617(17) 0.31517(18) 0.92226(14) 0.0142(5) Uani 1 1 d . . . . .
H53 H 0.153698 0.272958 0.912870 0.017 Uiso 1 1 calc R U . . .
C54 C 0.16910(17) 0.42192(18) 0.90534(14) 0.0138(5) Uani 1 1 d . . . . .
H54 H 0.103222 0.432514 0.880405 0.017 Uiso 1 1 calc R U . . .
N51 N 0.29124(15) 0.32027(15) 0.87002(12) 0.0136(4) Uani 1 1 d . . . . .
N52 N 0.24853(15) 0.47413(14) 0.85426(11) 0.0133(4) Uani 1 1 d . . . . .
N53 N 0.16177(15) 0.43742(15) 0.98028(11) 0.0140(4) Uani 1 1 d . . . . .
N54 N 0.23025(15) 0.29023(15) 1.00228(12) 0.0147(4) Uani 1 1 d . . . . .
C55 C 0.24135(18) 0.57476(17) 0.81036(13) 0.0137(5) Uani 1 1 d . . . . .
H55A H 0.283908 0.584135 0.763245 0.016 Uiso 1 1 calc R U . . .
H55B H 0.171558 0.590837 0.795052 0.016 Uiso 1 1 calc R U . . .
C56 C 0.12285(18) 0.52522(17) 0.99595(14) 0.0146(5) Uani 1 1 d . . . . .
H56A H 0.062711 0.547573 0.965782 0.018 Uiso 1 1 calc R U . . .
H56B H 0.101950 0.510419 1.050614 0.018 Uiso 1 1 calc R U . . .
O61 O 0.40850(13) 0.70397(14) 0.77476(10) 0.0208(4) Uani 1 1 d . . . . .
O62 O 0.23665(13) 0.58964(12) 1.10199(9) 0.0161(4) Uani 1 1 d . . . . .
C61 C 0.34631(18) 0.70405(18) 0.82637(14) 0.0153(5) Uani 1 1 d . . . . .
C62 C 0.23615(17) 0.63306(17) 1.03390(14) 0.0132(5) Uani 1 1 d . . . . .
C63 C 0.20194(18) 0.67126(17) 0.90423(13) 0.0127(5) Uani 1 1 d . . . . .
H63 H 0.135509 0.691443 0.881362 0.015 Uiso 1 1 calc R U . . .
C64 C 0.25471(18) 0.75638(18) 0.92000(13) 0.0133(5) Uani 1 1 d . . . . .
H64 H 0.210644 0.815730 0.910238 0.016 Uiso 1 1 calc R U . . .
N61 N 0.27139(15) 0.64009(15) 0.85192(11) 0.0146(4) Uani 1 1 d . . . . .
N62 N 0.34044(15) 0.76947(15) 0.86797(11) 0.0149(4) Uani 1 1 d . . . . .
N63 N 0.27778(15) 0.71990(15) 1.00015(11) 0.0138(4) Uani 1 1 d . . . . .
N64 N 0.19254(15) 0.60256(15) 0.97877(11) 0.0137(4) Uani 1 1 d . . . . .
C65 C 0.40389(19) 0.85146(18) 0.85465(14) 0.0163(5) Uani 1 1 d . . . . .
H65A H 0.435345 0.863836 0.802821 0.020 Uiso 1 1 calc R U . . .
H65B H 0.362076 0.908998 0.856176 0.020 Uiso 1 1 calc R U . . .
C66 C 0.30908(18) 0.78133(18) 1.04472(14) 0.0140(5) Uani 1 1 d . . . . .
H66A H 0.287016 0.753546 1.098647 0.017 Uiso 1 1 calc R U . . .
H66B H 0.275801 0.845587 1.026256 0.017 Uiso 1 1 calc R U . . .
N3 N 1.03268(15) 0.78602(16) 0.00780(12) 0.0174(4) Uani 1 1 d . . . . .
O31N O 1.07200(15) 0.86513(14) -0.00002(11) 0.0264(4) Uani 1 1 d . . . . .
O32N O 1.03030(14) 0.72354(14) 0.07152(10) 0.0232(4) Uani 1 1 d . . . . .
O33N O 0.99676(15) 0.76737(15) -0.04835(11) 0.0278(5) Uani 1 1 d . . . . .
N4 N 0.87150(17) 0.57852(17) 0.33095(13) 0.0235(5) Uani 1 1 d . U . . .
O41N O 0.81036(18) 0.5494(2) 0.38353(14) 0.0556(8) Uani 1 1 d D U . . .
H41N H 0.803(2) 0.5346(10) 0.4325(6) 0.067 Uiso 1 1 d D U . . .
O42N O 0.84382(16) 0.63343(16) 0.26882(12) 0.0329(5) Uani 1 1 d . U . . .
O43N O 0.96127(16) 0.55545(16) 0.34116(13) 0.0351(5) Uani 1 1 d . U . . .
N5 N 0.46925(15) 0.27603(16) 0.50844(12) 0.0170(4) Uani 1 1 d . . . . .
O51N O 0.44157(15) 0.36157(14) 0.50021(11) 0.0258(4) Uani 1 1 d . . . . .
O52N O 0.46924(15) 0.21675(14) 0.57357(10) 0.0255(4) Uani 1 1 d . . . . .
O53N O 0.49552(15) 0.24772(15) 0.45114(11) 0.0267(4) Uani 1 1 d . . . . .
N6 N 0.63624(16) 0.07478(15) 0.83958(12) 0.0179(4) Uani 1 1 d . . . . .
O61N O 0.65437(15) 0.13844(14) 0.77788(11) 0.0264(4) Uani 1 1 d . . . . .
O62N O 0.54766(15) 0.05194(15) 0.85941(13) 0.0319(5) Uani 1 1 d . . . . .
O63N O 0.70470(16) 0.03495(15) 0.88071(12) 0.0317(5) Uani 1 1 d . . . . .
N7 N 1.0209(12) 1.0179(12) 0.4661(11) 0.080(3) Uani 0.25 1 d D U P A -1
O71N O 1.0129(13) 0.9578(11) 0.4290(10) 0.067(3) Uani 0.25 1 d D U P A -1
O72N O 1.0924(10) 1.0099(14) 0.5071(9) 0.070(3) Uani 0.25 1 d D U P A -1
O73N O 0.9701(12) 1.0936(10) 0.4481(9) 0.085(3) Uani 0.25 1 d D U P A -1
N7A N 1.0051(10) 1.0357(10) 0.4677(8) 0.075(3) Uani 0.25 1 d D U P B -2
O71A O 1.0635(12) 1.0493(14) 0.5125(10) 0.078(3) Uani 0.25 1 d D U P B -2
O72A O 1.0255(15) 0.9903(14) 0.4202(11) 0.071(3) Uani 0.25 1 d D U P B -2
O73A O 0.9194(11) 1.0689(15) 0.4688(10) 0.086(3) Uani 0.25 1 d D U P B -2
N8 N 0.4650(12) 0.5070(11) 0.9708(8) 0.077(3) Uani 0.25 1 d D U P C -1
O81N O 0.4769(11) 0.4493(10) 0.9318(8) 0.063(3) Uani 0.25 1 d D U P C -1
O82N O 0.5181(14) 0.5787(10) 0.9560(9) 0.082(3) Uani 0.25 1 d D U P C -1
O83N O 0.4052(9) 0.4912(13) 1.0253(7) 0.071(3) Uani 0.25 1 d D U P C -1
N8A N 0.4992(10) 0.5346(19) 0.9699(10) 0.077(3) Uani 0.25 1 d D U P D -2
O81A O 0.5822(12) 0.5709(14) 0.9581(9) 0.077(3) Uani 0.25 1 d D U P D -2
O82A O 0.4471(10) 0.5522(13) 1.0214(8) 0.078(3) Uani 0.25 1 d D U P D -2
O83A O 0.4684(12) 0.4958(13) 0.9229(9) 0.070(3) Uani 0.25 1 d D U P D -2
O1W O 0.82240(15) 1.18166(14) 0.27216(11) 0.0242(4) Uani 1 1 d D . . . .
H11W H 0.8745(13) 1.213(2) 0.2763(16) 0.029 Uiso 1 1 d D U . . .
H12W H 0.7823(16) 1.183(2) 0.3103(12) 0.029 Uiso 1 1 d D U . . .
O2W O 0.60322(17) 0.92085(17) 0.25308(16) 0.0404(6) Uani 1 1 d D . . . .
H21W H 0.5707(17) 0.955(2) 0.2783(16) 0.048 Uiso 1 1 d D U . . .
H22W H 0.570(2) 0.926(3) 0.2120(12) 0.048 Uiso 1 1 d D U . . .
O3W O 1.42778(17) 0.9303(2) 0.66904(13) 0.0426(6) Uani 1 1 d D . . . .
H31W H 1.4054(19) 0.8742(11) 0.6568(19) 0.051 Uiso 1 1 d D U . . .
H32W H 1.3781(13) 0.9681(12) 0.6445(6) 0.051 Uiso 1 1 d D U . . .
O4W O 0.86035(14) 0.43450(15) 0.75504(11) 0.0255(4) Uani 1 1 d D . . . .
H41W H 0.9224(10) 0.429(2) 0.7409(14) 0.031 Uiso 1 1 d D U . . .
H42W H 0.8599(19) 0.436(2) 0.8019(8) 0.031 Uiso 1 1 d D U . . .
O5W O 0.67665(15) 0.66618(14) 0.77615(11) 0.0238(4) Uani 1 1 d D . . . .
H51W H 0.7214(16) 0.657(2) 0.8102(14) 0.029 Uiso 1 1 d D U . . .
H52W H 0.6356(17) 0.7106(17) 0.7842(16) 0.029 Uiso 1 1 d D U . . .
O6W O 0.00478(16) 0.39241(19) 1.16646(12) 0.0389(6) Uani 1 1 d D . . . .
H61W H 0.0602(16) 0.368(2) 1.1539(17) 0.047 Uiso 1 1 d D U . . .
H62W H -0.0155(11) 0.357(2) 1.2102(6) 0.047 Uiso 1 1 d D 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
Eu1 O11M 2.4950(18) . yes
Eu1 O12M 2.4084(18) . yes
Eu1 O13M 2.4310(18) . yes
Eu1 O14M 2.4337(18) . yes
Eu1 O15M 2.3899(19) . yes
Eu1 N1 2.920(2) . ?
Eu1 O11N 2.4795(17) . yes
Eu1 O12N 2.5434(18) . yes
Eu1 O11 2.3764(16) . yes
Eu1 O21 2.4753(17) . yes
O11M H111 0.842(10) . ?
O11M H112 0.842(10) . ?
O12M H121 0.847(10) . ?
O12M H122 0.848(10) . ?
O13M H131 0.844(10) . ?
O13M H132 0.849(10) . ?
O14M H141 0.843(10) . ?
O14M H142 0.843(10) . ?
O15M H151 0.853(7) . ?
O15M H152 0.847(7) . ?
N1 O11N 1.270(3) . ?
N1 O12N 1.255(3) . ?
N1 O13N 1.231(3) . ?
O11 C11 1.236(3) . ?
O12 C12 1.219(3) . ?
C11 N11 1.354(3) . ?
C11 N12 1.360(3) . ?
C12 N13 1.371(3) . ?
C12 N14 1.369(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.548(3) . ?
C13 N11 1.460(3) . ?
C13 N14 1.432(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.449(3) . ?
C14 N13 1.456(3) . ?
N11 C36 1.455(3) 2_776 ?
N12 C15 1.446(3) . ?
N13 C16 1.449(3) . ?
N14 C35 1.434(3) 2_776 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.438(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.454(3) . ?
O21 C21 1.230(3) . ?
O22 C22 1.224(3) . ?
C21 N21 1.357(3) . ?
C21 N22 1.357(3) . ?
C22 N23 1.368(3) . ?
C22 N24 1.364(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.554(3) . ?
C23 N21 1.444(3) . ?
C23 N24 1.448(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.471(3) . ?
C24 N23 1.437(3) . ?
N22 C25 1.458(3) . ?
N23 C26 1.445(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 N31 1.447(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 N34 1.446(3) . ?
O31 C31 1.234(3) . ?
O32 C32 1.225(3) . ?
C31 N31 1.354(3) . ?
C31 N32 1.364(3) . ?
C32 N33 1.371(3) . ?
C32 N34 1.365(3) . ?
C33 H33 1.0000 . ?
C33 C34 1.551(3) . ?
C33 N31 1.453(3) . ?
C33 N34 1.442(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.448(3) . ?
C34 N33 1.454(3) . ?
N32 C35 1.447(3) . ?
N33 C36 1.442(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
Eu2 O21M 2.4309(18) . yes
Eu2 O22M 2.4111(18) . yes
Eu2 O23M 2.5023(17) . yes
Eu2 O24M 2.3946(18) . yes
Eu2 O25M 2.4188(18) . yes
Eu2 N2 2.909(2) . ?
Eu2 O21N 2.5152(18) . yes
Eu2 O22N 2.4945(17) . yes
Eu2 O41 2.4664(17) . yes
Eu2 O51 2.3572(17) . yes
O21M H211 0.851(10) . ?
O21M H212 0.845(10) . ?
O22M H221 0.844(10) . ?
O22M H222 0.844(10) . ?
O23M H231 0.846(10) . ?
O23M H232 0.845(10) . ?
O24M H241 0.845(10) . ?
O24M H242 0.845(10) . ?
O25M H251 0.848(10) . ?
O25M H252 0.847(10) . ?
N2 O21N 1.266(3) . ?
N2 O22N 1.266(3) . ?
N2 O23N 1.227(3) . ?
O41 C41 1.232(3) . ?
O42 C42 1.222(3) . ?
C41 N41 1.356(3) . ?
C41 N42 1.356(3) . ?
C42 N43 1.361(3) . ?
C42 N44 1.368(3) . ?
C43 H43 1.0000 . ?
C43 C44 1.556(3) . ?
C43 N41 1.453(3) . ?
C43 N44 1.442(3) . ?
C44 H44 1.0000 . ?
C44 N42 1.449(3) . ?
C44 N43 1.442(3) . ?
N41 C66 1.450(3) 2_667 ?
N42 C45 1.442(3) . ?
N43 C46 1.449(3) . ?
N44 C65 1.443(3) 2_667 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 N51 1.443(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 N54 1.455(3) . ?
O51 C51 1.234(3) . ?
O52 C52 1.229(3) . ?
C51 N51 1.353(3) . ?
C51 N52 1.357(3) . ?
C52 N53 1.365(3) . ?
C52 N54 1.366(3) . ?
C53 H53 1.0000 . ?
C53 C54 1.551(3) . ?
C53 N51 1.444(3) . ?
C53 N54 1.453(3) . ?
C54 H54 1.0000 . ?
C54 N52 1.467(3) . ?
C54 N53 1.445(3) . ?
N52 C55 1.452(3) . ?
N53 C56 1.448(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 N61 1.444(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 N64 1.442(3) . ?
O61 C61 1.230(3) . ?
O62 C62 1.226(3) . ?
C61 N61 1.368(3) . ?
C61 N62 1.365(3) . ?
C62 N63 1.362(3) . ?
C62 N64 1.368(3) . ?
C63 H63 1.0000 . ?
C63 C64 1.543(3) . ?
C63 N61 1.452(3) . ?
C63 N64 1.447(3) . ?
C64 H64 1.0000 . ?
C64 N62 1.441(3) . ?
C64 N63 1.454(3) . ?
N62 C65 1.444(3) . ?
N63 C66 1.445(3) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
N3 O31N 1.246(3) . ?
N3 O32N 1.258(3) . ?
N3 O33N 1.251(3) . ?
N4 O41N 1.225(3) . ?
N4 O42N 1.252(3) . ?
N4 O43N 1.245(3) . ?
O41N H41N 0.862(9) . ?
N5 O51N 1.245(3) . ?
N5 O52N 1.256(3) . ?
N5 O53N 1.256(3) . ?
N6 O61N 1.260(3) . ?
N6 O62N 1.256(3) . ?
N6 O63N 1.233(3) . ?
N7 O71N 1.250(7) . ?
N7 O72N 1.227(7) . ?
N7 O73N 1.236(7) . ?
N7A O71A 1.218(7) . ?
N7A O72A 1.241(8) . ?
N7A O73A 1.229(8) . ?
N8 O81N 1.240(7) . ?
N8 O82N 1.238(7) . ?
N8 O83N 1.225(7) . ?
N8A O81A 1.234(8) . ?
N8A O82A 1.223(8) . ?
N8A O83A 1.239(8) . ?
O1W H11W 0.862(10) . ?
O1W H12W 0.866(10) . ?
O2W H21W 0.856(10) . ?
O2W H22W 0.875(10) . ?
O3W H31W 0.960(8) . ?
O3W H32W 0.898(8) . ?
O4W H41W 0.868(10) . ?
O4W H42W 0.862(10) . ?
O5W H51W 0.863(10) . ?
O5W H52W 0.868(10) . ?
O6W H61W 0.862(10) . ?
O6W H62W 0.860(10) . ?

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
O11M Eu1 N1 63.47(6) . . ?
O11M Eu1 O12N 69.23(6) . . ?
O12M Eu1 O11M 76.43(6) . . ?
O12M Eu1 O13M 70.37(7) . . ?
O12M Eu1 O14M 144.32(6) . . ?
O12M Eu1 N1 95.14(6) . . ?
O12M Eu1 O11N 119.70(6) . . ?
O12M Eu1 O12N 72.26(6) . . ?
O12M Eu1 O21 73.99(6) . . ?
O13M Eu1 O11M 132.50(6) . . ?
O13M Eu1 O14M 74.27(7) . . ?
O13M Eu1 N1 86.45(6) . . ?
O13M Eu1 O11N 101.17(6) . . ?
O13M Eu1 O12N 68.88(6) . . ?
O13M Eu1 O21 130.52(6) . . ?
O14M Eu1 O11M 134.25(6) . . ?
O14M Eu1 N1 87.20(6) . . ?
O14M Eu1 O11N 71.62(6) . . ?
O14M Eu1 O12N 99.40(6) . . ?
O14M Eu1 O21 129.39(6) . . ?
O15M Eu1 O11M 80.37(7) . . ?
O15M Eu1 O12M 141.35(6) . . ?
O15M Eu1 O13M 144.52(7) . . ?
O15M Eu1 O14M 71.73(7) . . ?
O15M Eu1 N1 101.62(7) . . ?
O15M Eu1 O11N 77.50(7) . . ?
O15M Eu1 O12N 126.55(7) . . ?
O15M Eu1 O21 68.57(6) . . ?
O11N Eu1 O11M 67.34(6) . . ?
O11N Eu1 N1 25.57(6) . . ?
O11N Eu1 O12N 50.72(6) . . ?
O12N Eu1 N1 25.36(6) . . ?
O11 Eu1 O11M 141.64(6) . . ?
O11 Eu1 O12M 90.56(6) . . ?
O11 Eu1 O13M 72.32(6) . . ?
O11 Eu1 O14M 74.17(6) . . ?
O11 Eu1 O15M 88.81(7) . . ?
O11 Eu1 N1 154.73(6) . . ?
O11 Eu1 O11N 145.62(6) . . ?
O11 Eu1 O12N 140.90(6) . . ?
O11 Eu1 O21 74.89(6) . . ?
O21 Eu1 O11M 66.87(6) . . ?
O21 Eu1 N1 130.32(6) . . ?
O21 Eu1 O11N 126.26(6) . . ?
O21 Eu1 O12N 129.33(6) . . ?
Eu1 O11M H111 116.7(18) . . ?
Eu1 O11M H112 126.3(19) . . ?
H111 O11M H112 110.4(16) . . ?
Eu1 O12M H121 117.0(19) . . ?
Eu1 O12M H122 118.6(19) . . ?
H121 O12M H122 108.9(15) . . ?
Eu1 O13M H131 125.1(18) . . ?
Eu1 O13M H132 125.3(18) . . ?
H131 O13M H132 108.8(16) . . ?
Eu1 O14M H141 123.9(17) . . ?
Eu1 O14M H142 124.5(17) . . ?
H141 O14M H142 110.1(16) . . ?
Eu1 O15M H151 120.8(19) . . ?
Eu1 O15M H152 121(2) . . ?
H151 O15M H152 108.9(13) . . ?
O11N N1 Eu1 57.43(11) . . ?
O12N N1 Eu1 60.27(12) . . ?
O12N N1 O11N 116.99(19) . . ?
O13N N1 Eu1 170.07(17) . . ?
O13N N1 O11N 120.9(2) . . ?
O13N N1 O12N 122.1(2) . . ?
N1 O11N Eu1 97.01(13) . . ?
N1 O12N Eu1 94.36(14) . . ?
C11 O11 Eu1 157.93(16) . . ?
O11 C11 N11 125.1(2) . . ?
O11 C11 N12 125.7(2) . . ?
N11 C11 N12 109.2(2) . . ?
O12 C12 N13 126.5(2) . . ?
O12 C12 N14 125.5(2) . . ?
N14 C12 N13 107.9(2) . . ?
C14 C13 H13 111.7 . . ?
N11 C13 H13 111.7 . . ?
N11 C13 C14 103.40(18) . . ?
N14 C13 H13 111.7 . . ?
N14 C13 C14 103.49(18) . . ?
N14 C13 N11 114.28(19) . . ?
C13 C14 H14 111.8 . . ?
N12 C14 C13 102.60(18) . . ?
N12 C14 H14 111.8 . . ?
N12 C14 N13 115.19(19) . . ?
N13 C14 C13 102.91(18) . . ?
N13 C14 H14 111.8 . . ?
C11 N11 C13 111.48(19) . . ?
C11 N11 C36 123.0(2) . 2_776 ?
C36 N11 C13 122.07(19) 2_776 . ?
C11 N12 C14 112.53(19) . . ?
C11 N12 C15 123.93(19) . . ?
C15 N12 C14 123.45(19) . . ?
C12 N13 C14 111.78(19) . . ?
C12 N13 C16 121.7(2) . . ?
C16 N13 C14 124.3(2) . . ?
C12 N14 C13 112.9(2) . . ?
C12 N14 C35 123.6(2) . 2_776 ?
C13 N14 C35 122.7(2) . 2_776 ?
N12 C15 H15A 108.9 . . ?
N12 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
N21 C15 N12 113.33(19) . . ?
N21 C15 H15A 108.9 . . ?
N21 C15 H15B 108.9 . . ?
N13 C16 H16A 109.0 . . ?
N13 C16 H16B 109.0 . . ?
N13 C16 N24 112.91(19) . . ?
H16A C16 H16B 107.8 . . ?
N24 C16 H16A 109.0 . . ?
N24 C16 H16B 109.0 . . ?
C21 O21 Eu1 157.27(16) . . ?
O21 C21 N21 125.3(2) . . ?
O21 C21 N22 125.3(2) . . ?
N22 C21 N21 109.4(2) . . ?
O22 C22 N23 125.3(2) . . ?
O22 C22 N24 126.4(2) . . ?
N24 C22 N23 108.3(2) . . ?
C24 C23 H23 111.7 . . ?
N21 C23 H23 111.7 . . ?
N21 C23 C24 102.89(18) . . ?
N21 C23 N24 115.25(19) . . ?
N24 C23 H23 111.7 . . ?
N24 C23 C24 102.92(18) . . ?
C23 C24 H24 111.7 . . ?
N22 C24 C23 102.78(18) . . ?
N22 C24 H24 111.7 . . ?
N23 C24 C23 103.04(18) . . ?
N23 C24 H24 111.7 . . ?
N23 C24 N22 115.36(19) . . ?
C15 N21 C23 124.81(19) . . ?
C21 N21 C15 122.5(2) . . ?
C21 N21 C23 112.7(2) . . ?
C21 N22 C24 111.21(19) . . ?
C21 N22 C25 121.6(2) . . ?
C25 N22 C24 122.82(19) . . ?
C22 N23 C24 112.5(2) . . ?
C22 N23 C26 123.7(2) . . ?
C24 N23 C26 123.76(19) . . ?
C22 N24 C16 123.2(2) . . ?
C22 N24 C23 111.85(19) . . ?
C23 N24 C16 122.9(2) . . ?
N22 C25 H25A 108.8 . . ?
N22 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N31 C25 N22 113.79(19) . . ?
N31 C25 H25A 108.8 . . ?
N31 C25 H25B 108.8 . . ?
N23 C26 H26A 109.0 . . ?
N23 C26 H26B 109.0 . . ?
N23 C26 N34 113.03(19) . . ?
H26A C26 H26B 107.8 . . ?
N34 C26 H26A 109.0 . . ?
N34 C26 H26B 109.0 . . ?
O31 C31 N31 126.0(2) . . ?
O31 C31 N32 125.4(2) . . ?
N31 C31 N32 108.5(2) . . ?
O32 C32 N33 126.3(2) . . ?
O32 C32 N34 125.5(2) . . ?
N34 C32 N33 108.1(2) . . ?
C34 C33 H33 112.0 . . ?
N31 C33 H33 112.0 . . ?
N31 C33 C34 102.95(18) . . ?
N34 C33 H33 112.0 . . ?
N34 C33 C34 103.47(18) . . ?
N34 C33 N31 113.73(19) . . ?
C33 C34 H34 111.7 . . ?
N32 C34 C33 102.99(19) . . ?
N32 C34 H34 111.7 . . ?
N32 C34 N33 115.27(19) . . ?
N33 C34 C33 102.93(18) . . ?
N33 C34 H34 111.7 . . ?
C25 N31 C33 123.2(2) . . ?
C31 N31 C25 123.4(2) . . ?
C31 N31 C33 112.7(2) . . ?
C31 N32 C34 112.5(2) . . ?
C31 N32 C35 124.1(2) . . ?
C35 N32 C34 123.3(2) . . ?
C32 N33 C34 112.14(19) . . ?
C32 N33 C36 122.0(2) . . ?
C36 N33 C34 123.3(2) . . ?
C32 N34 C26 123.4(2) . . ?
C32 N34 C33 112.69(19) . . ?
C33 N34 C26 121.23(19) . . ?
N14 C35 N32 114.34(19) 2_776 . ?
N14 C35 H35A 108.7 2_776 . ?
N14 C35 H35B 108.7 2_776 . ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
N11 C36 H36A 108.9 2_776 . ?
N11 C36 H36B 108.9 2_776 . ?
N33 C36 N11 113.38(19) . 2_776 ?
N33 C36 H36A 108.9 . . ?
N33 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
O21M Eu2 O23M 130.67(6) . . ?
O21M Eu2 N2 89.16(6) . . ?
O21M Eu2 O21N 105.71(7) . . ?
O21M Eu2 O22N 68.98(6) . . ?
O21M Eu2 O41 126.04(7) . . ?
O22M Eu2 O21M 70.35(7) . . ?
O22M Eu2 O23M 73.66(6) . . ?
O22M Eu2 O25M 147.11(7) . . ?
O22M Eu2 N2 96.64(6) . . ?
O22M Eu2 O21N 120.41(6) . . ?
O22M Eu2 O22N 75.14(6) . . ?
O22M Eu2 O41 70.07(6) . . ?
O23M Eu2 N2 62.68(6) . . ?
O23M Eu2 O21N 66.09(6) . . ?
O24M Eu2 O21M 148.29(7) . . ?
O24M Eu2 O22M 136.40(6) . . ?
O24M Eu2 O23M 79.93(6) . . ?
O24M Eu2 O25M 74.38(7) . . ?
O24M Eu2 N2 101.27(6) . . ?
O24M Eu2 O21N 76.94(6) . . ?
O24M Eu2 O22N 126.72(6) . . ?
O24M Eu2 O41 68.02(6) . . ?
O25M Eu2 O21M 76.85(7) . . ?
O25M Eu2 O23M 133.49(6) . . ?
O25M Eu2 N2 85.06(6) . . ?
O25M Eu2 O21N 70.66(6) . . ?
O25M Eu2 O22N 95.60(6) . . ?
O25M Eu2 O41 131.78(6) . . ?
O21N Eu2 N2 25.69(6) . . ?
O22N Eu2 O23M 70.01(6) . . ?
O22N Eu2 N2 25.66(6) . . ?
O22N Eu2 O21N 51.05(5) . . ?
O41 Eu2 O23M 67.77(6) . . ?
O41 Eu2 N2 130.43(6) . . ?
O41 Eu2 O21N 125.58(6) . . ?
O41 Eu2 O22N 130.96(6) . . ?
O51 Eu2 O21M 74.30(6) . . ?
O51 Eu2 O22M 94.90(6) . . ?
O51 Eu2 O23M 141.89(6) . . ?
O51 Eu2 O24M 84.96(6) . . ?
O51 Eu2 O25M 73.52(6) . . ?
O51 Eu2 N2 155.29(6) . . ?
O51 Eu2 O21N 143.02(6) . . ?
O51 Eu2 O22N 143.20(6) . . ?
O51 Eu2 O41 74.15(6) . . ?
Eu2 O21M H211 120.1(18) . . ?
Eu2 O21M H212 129.1(19) . . ?
H211 O21M H212 108.5(16) . . ?
Eu2 O22M H221 117.9(18) . . ?
Eu2 O22M H222 127.0(18) . . ?
H221 O22M H222 109.6(15) . . ?
Eu2 O23M H231 118.1(18) . . ?
Eu2 O23M H232 116.8(18) . . ?
H231 O23M H232 109.0(15) . . ?
Eu2 O24M H241 119.0(19) . . ?
Eu2 O24M H242 119.5(19) . . ?
H241 O24M H242 109.3(16) . . ?
Eu2 O25M H251 123.4(18) . . ?
Eu2 O25M H252 127.0(18) . . ?
H251 O25M H252 108.8(16) . . ?
O21N N2 Eu2 59.49(11) . . ?
O21N N2 O22N 117.0(2) . . ?
O22N N2 Eu2 58.55(11) . . ?
O23N N2 Eu2 169.30(16) . . ?
O23N N2 O21N 121.5(2) . . ?
O23N N2 O22N 121.5(2) . . ?
N2 O21N Eu2 94.82(13) . . ?
N2 O22N Eu2 95.78(13) . . ?
C41 O41 Eu2 157.10(16) . . ?
O41 C41 N41 125.0(2) . . ?
O41 C41 N42 125.8(2) . . ?
N41 C41 N42 109.2(2) . . ?
O42 C42 N43 126.5(2) . . ?
O42 C42 N44 125.4(2) . . ?
N43 C42 N44 108.1(2) . . ?
C44 C43 H43 111.7 . . ?
N41 C43 H43 111.7 . . ?
N41 C43 C44 103.33(19) . . ?
N44 C43 H43 111.7 . . ?
N44 C43 C44 103.03(19) . . ?
N44 C43 N41 114.8(2) . . ?
C43 C44 H44 111.7 . . ?
N42 C44 C43 102.68(19) . . ?
N42 C44 H44 111.7 . . ?
N43 C44 C43 103.11(19) . . ?
N43 C44 H44 111.7 . . ?
N43 C44 N42 115.1(2) . . ?
C41 N41 C43 112.00(19) . . ?
C41 N41 C66 123.1(2) . 2_667 ?
C66 N41 C43 124.0(2) 2_667 . ?
C41 N42 C44 112.7(2) . . ?
C41 N42 C45 122.9(2) . . ?
C45 N42 C44 124.2(2) . . ?
C42 N43 C44 112.3(2) . . ?
C42 N43 C46 123.2(2) . . ?
C44 N43 C46 123.8(2) . . ?
C42 N44 C43 112.4(2) . . ?
C42 N44 C65 122.0(2) . 2_667 ?
C43 N44 C65 124.0(2) . 2_667 ?
N42 C45 H45A 109.0 . . ?
N42 C45 H45B 109.0 . . ?
N42 C45 N51 113.0(2) . . ?
H45A C45 H45B 107.8 . . ?
N51 C45 H45A 109.0 . . ?
N51 C45 H45B 109.0 . . ?
N43 C46 H46A 109.1 . . ?
N43 C46 H46B 109.1 . . ?
N43 C46 N54 112.6(2) . . ?
H46A C46 H46B 107.8 . . ?
N54 C46 H46A 109.1 . . ?
N54 C46 H46B 109.1 . . ?
C51 O51 Eu2 159.78(16) . . ?
O51 C51 N51 125.5(2) . . ?
O51 C51 N52 124.9(2) . . ?
N51 C51 N52 109.6(2) . . ?
O52 C52 N53 125.4(2) . . ?
O52 C52 N54 125.9(2) . . ?
N53 C52 N54 108.7(2) . . ?
C54 C53 H53 111.7 . . ?
N51 C53 H53 111.7 . . ?
N51 C53 C54 102.95(19) . . ?
N51 C53 N54 114.7(2) . . ?
N54 C53 H53 111.7 . . ?
N54 C53 C54 103.33(19) . . ?
C53 C54 H54 111.7 . . ?
N52 C54 C53 102.96(18) . . ?
N52 C54 H54 111.7 . . ?
N53 C54 C53 102.88(19) . . ?
N53 C54 H54 111.7 . . ?
N53 C54 N52 115.24(19) . . ?
C45 N51 C53 124.5(2) . . ?
C51 N51 C45 122.7(2) . . ?
C51 N51 C53 112.6(2) . . ?
C51 N52 C54 111.1(2) . . ?
C51 N52 C55 120.6(2) . . ?
C55 N52 C54 124.8(2) . . ?
C52 N53 C54 112.5(2) . . ?
C52 N53 C56 123.0(2) . . ?
C54 N53 C56 124.5(2) . . ?
C52 N54 C46 121.6(2) . . ?
C52 N54 C53 111.5(2) . . ?
C53 N54 C46 124.4(2) . . ?
N52 C55 H55A 109.0 . . ?
N52 C55 H55B 109.0 . . ?
H55A C55 H55B 107.8 . . ?
N61 C55 N52 113.06(19) . . ?
N61 C55 H55A 109.0 . . ?
N61 C55 H55B 109.0 . . ?
N53 C56 H56A 108.7 . . ?
N53 C56 H56B 108.7 . . ?
H56A C56 H56B 107.6 . . ?
N64 C56 N53 114.3(2) . . ?
N64 C56 H56A 108.7 . . ?
N64 C56 H56B 108.7 . . ?
O61 C61 N61 126.6(2) . . ?
O61 C61 N62 125.2(2) . . ?
N62 C61 N61 108.2(2) . . ?
O62 C62 N63 126.2(2) . . ?
O62 C62 N64 125.5(2) . . ?
N63 C62 N64 108.2(2) . . ?
C64 C63 H63 111.9 . . ?
N61 C63 H63 111.9 . . ?
N61 C63 C64 103.36(19) . . ?
N64 C63 H63 111.9 . . ?
N64 C63 C64 103.49(19) . . ?
N64 C63 N61 113.81(19) . . ?
C63 C64 H64 111.8 . . ?
N62 C64 C63 103.24(19) . . ?
N62 C64 H64 111.8 . . ?
N62 C64 N63 114.7(2) . . ?
N63 C64 C63 103.01(19) . . ?
N63 C64 H64 111.8 . . ?
C55 N61 C63 120.9(2) . . ?
C61 N61 C55 122.9(2) . . ?
C61 N61 C63 111.6(2) . . ?
C61 N62 C64 112.6(2) . . ?
C61 N62 C65 124.3(2) . . ?
C64 N62 C65 122.5(2) . . ?
C62 N63 C64 112.38(19) . . ?
C62 N63 C66 121.4(2) . . ?
C66 N63 C64 122.8(2) . . ?
C56 N64 C63 122.6(2) . . ?
C62 N64 C56 123.0(2) . . ?
C62 N64 C63 112.4(2) . . ?
N44 C65 N62 113.8(2) 2_667 . ?
N44 C65 H65A 108.8 2_667 . ?
N44 C65 H65B 108.8 2_667 . ?
N62 C65 H65A 108.8 . . ?
N62 C65 H65B 108.8 . . ?
H65A C65 H65B 107.7 . . ?
N41 C66 H66A 108.9 2_667 . ?
N41 C66 H66B 108.9 2_667 . ?
N63 C66 N41 113.2(2) . 2_667 ?
N63 C66 H66A 108.9 . . ?
N63 C66 H66B 108.9 . . ?
H66A C66 H66B 107.7 . . ?
O31N N3 O32N 120.6(2) . . ?
O31N N3 O33N 120.0(2) . . ?
O33N N3 O32N 119.3(2) . . ?
O41N N4 O42N 119.9(2) . . ?
O41N N4 O43N 119.1(2) . . ?
O43N N4 O42N 120.9(2) . . ?
N4 O41N H41N 143(2) . . ?
O51N N5 O52N 120.7(2) . . ?
O51N N5 O53N 120.0(2) . . ?
O52N N5 O53N 119.3(2) . . ?
O62N N6 O61N 119.7(2) . . ?
O63N N6 O61N 120.5(2) . . ?
O63N N6 O62N 119.8(2) . . ?
O72N N7 O71N 118.7(7) . . ?
O72N N7 O73N 121.0(8) . . ?
O73N N7 O71N 118.5(7) . . ?
O71A N7A O72A 124.7(15) . . ?
O71A N7A O73A 118.7(15) . . ?
O73A N7A O72A 116.6(14) . . ?
O82N N8 O81N 118.8(7) . . ?
O83N N8 O81N 120.6(7) . . ?
O83N N8 O82N 120.5(7) . . ?
O81A N8A O83A 118.7(14) . . ?
O82A N8A O81A 116.4(15) . . ?
O82A N8A O83A 124.0(15) . . ?
H11W O1W H12W 106.8(15) . . ?
H21W O2W H22W 106.4(15) . . ?
H31W O3W H32W 93.1(10) . . ?
H41W O4W H42W 106.7(15) . . ?
H51W O5W H52W 106.4(15) . . ?
H61W O6W H62W 108.1(16) . . ?

_refine_diff_density_max         0.790
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.084




####################################################################### 
# 
# 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_km777-7
_database_code_depnum_ccdc_archive 'CCDC 2247479'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H69 N31 O49 Tb2'
_chemical_formula_weight         2038.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0039 0.0019 'Calculated with ShelXle (H\"ubschle, 2011)'
H H 0.0000 0.0000 'Calculated with ShelXle (H\"ubschle, 2011)'
N N 0.0075 0.0038 'Calculated with ShelXle (H\"ubschle, 2011)'
O O 0.0128 0.0069 'Calculated with ShelXle (H\"ubschle, 2011)'
Tb Tb -0.1100 4.5464 'Calculated with ShelXle (H\"ubschle, 2011)'

_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                   13.386(3)
_cell_length_b                   14.4235(13)
_cell_length_c                   18.1775(13)
_cell_angle_alpha                73.769(2)
_cell_angle_beta                 87.340(4)
_cell_angle_gamma                87.608(5)
_cell_volume                     3364.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    59990
_cell_measurement_theta_min      1.2
_cell_measurement_theta_max      31.0

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_F_000             2048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    2.500
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_absorpt_special_details   ?

_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.74500
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       'φ scan'
_diffrn_detector_area_resol_mean 12.4
_diffrn_reflns_number            67138
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.224
_diffrn_reflns_theta_max         31.057
_diffrn_reflns_theta_full        26.551
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             18484
_reflns_number_gt                17140
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0513P)²+2.0590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18484
_refine_ls_number_parameters     1270
_refine_ls_number_restraints     386
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0994
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.003
_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
Tb1 Tb 0.95315(2) 0.91663(2) 0.22476(2) 0.01328(4) Uani 1 1 d . . . . .
O11M O 0.78839(14) 0.83986(14) 0.24335(11) 0.0225(4) Uani 1 1 d D . . . .
H111 H 0.789(2) 0.7797(8) 0.265(2) 0.027 Uiso 1 1 d D U . . .
H112 H 0.7295(12) 0.863(2) 0.247(2) 0.027 Uiso 1 1 d D U . . .
O12M O 0.99116(14) 0.75922(13) 0.21163(10) 0.0182(3) Uani 1 1 d D . . . .
H121 H 0.9480(19) 0.7158(18) 0.2285(16) 0.022 Uiso 1 1 d D U . . .
H122 H 1.013(2) 0.756(2) 0.1679(10) 0.022 Uiso 1 1 d D U . . .
O13M O 1.08666(14) 0.92501(16) 0.13045(11) 0.0233(4) Uani 1 1 d D . . . .
H131 H 1.1465(12) 0.939(3) 0.1354(18) 0.028 Uiso 1 1 d D U . . .
H132 H 1.082(2) 0.914(3) 0.0873(11) 0.028 Uiso 1 1 d D U . . .
O14M O 1.00587(14) 1.08163(13) 0.18894(10) 0.0200(3) Uani 1 1 d D . . . .
H141 H 1.006(3) 1.1220(18) 0.1449(9) 0.024 Uiso 1 1 d D U . . .
H142 H 1.040(2) 1.104(2) 0.2182(13) 0.024 Uiso 1 1 d D U . . .
O15M O 0.87544(16) 0.99547(14) 0.31109(12) 0.0273(4) Uani 1 1 d D . . . .
H151 H 0.8277(19) 0.9685(18) 0.3415(17) 0.033 Uiso 1 1 d D U . . .
H152 H 0.865(2) 1.0561(7) 0.299(2) 0.033 Uiso 1 1 d D U . . .
N1 N 0.82009(16) 0.97340(15) 0.09743(12) 0.0181(4) Uani 1 1 d . . . . .
O11N O 0.82320(14) 1.01916(13) 0.14781(10) 0.0197(3) Uani 1 1 d . . . . .
O12N O 0.88778(14) 0.90990(13) 0.09820(10) 0.0203(3) Uani 1 1 d . . . . .
O13N O 0.75297(15) 0.98973(15) 0.05119(12) 0.0259(4) Uani 1 1 d . . . . .
O11 O 1.10434(13) 0.91367(13) 0.28625(10) 0.0165(3) Uani 1 1 d . . . . .
O12 O 1.29002(13) 0.82874(13) 0.59702(10) 0.0188(3) Uani 1 1 d D . . . .
C11 C 1.17191(17) 0.88223(16) 0.33188(12) 0.0134(4) Uani 1 1 d . . . . .
C12 C 1.28705(17) 0.82904(17) 0.52993(13) 0.0151(4) Uani 1 1 d . . . . .
C13 C 1.31758(17) 0.87543(16) 0.39728(13) 0.0147(4) Uani 1 1 d . . . . .
H13 H 1.384105 0.874281 0.370095 0.018 Uiso 1 1 calc R U . . .
C14 C 1.27098(17) 0.77427(16) 0.42165(13) 0.0139(4) Uani 1 1 d . . . . .
H14 H 1.318932 0.723061 0.412849 0.017 Uiso 1 1 calc R U . . .
N11 N 1.24435(15) 0.93583(14) 0.34730(11) 0.0150(4) Uani 1 1 d . . . . .
N12 N 1.18614(15) 0.78861(14) 0.37243(11) 0.0149(4) Uani 1 1 d . . . . .
N13 N 1.24621(15) 0.76017(14) 0.50262(11) 0.0153(4) Uani 1 1 d . . . . .
N14 N 1.32645(15) 0.89791(15) 0.46875(11) 0.0154(4) Uani 1 1 d . . . . .
C15 C 1.12012(17) 0.71218(17) 0.37133(13) 0.0139(4) Uani 1 1 d . . . . .
H15A H 1.091104 0.726897 0.320078 0.017 Uiso 1 1 calc R U . . .
H15B H 1.159843 0.650944 0.379362 0.017 Uiso 1 1 calc R U . . .
C16 C 1.20973(17) 0.67088(17) 0.55325(13) 0.0150(4) Uani 1 1 d . . . . .
H16A H 1.234499 0.662762 0.605223 0.018 Uiso 1 1 calc R U . . .
H16B H 1.237292 0.616205 0.534924 0.018 Uiso 1 1 calc R U . . .
O21 O 0.92737(13) 0.80435(13) 0.35334(10) 0.0175(3) Uani 1 1 d . . . . .
O22 O 1.07531(13) 0.68419(13) 0.68026(10) 0.0184(3) Uani 1 1 d . . . . .
C21 C 0.95028(18) 0.74684(17) 0.41435(13) 0.0143(4) Uani 1 1 d . . . . .
C22 C 1.04439(18) 0.67186(16) 0.62137(13) 0.0151(4) Uani 1 1 d . . . . .
C23 C 1.04369(17) 0.63419(16) 0.50494(13) 0.0142(4) Uani 1 1 d . . . . .
H23 H 1.064714 0.567077 0.504250 0.017 Uiso 1 1 calc R U . . .
C24 C 0.93461(17) 0.63890(17) 0.53643(13) 0.0141(4) Uani 1 1 d . . . . .
H24 H 0.899986 0.576987 0.542344 0.017 Uiso 1 1 calc R U . . .
N21 N 1.04012(15) 0.69891(14) 0.42844(11) 0.0145(4) Uani 1 1 d . . . . .
N22 N 0.88885(15) 0.71860(14) 0.47835(11) 0.0151(4) Uani 1 1 d . . . . .
N23 N 0.94725(15) 0.65691(15) 0.60939(11) 0.0152(4) Uani 1 1 d . . . . .
N24 N 1.10113(15) 0.66740(15) 0.55792(11) 0.0153(4) Uani 1 1 d . . . . .
C25 C 0.78133(17) 0.73767(17) 0.47441(13) 0.0155(4) Uani 1 1 d . . . . .
H25A H 0.764295 0.764858 0.420018 0.019 Uiso 1 1 calc R U . . .
H25B H 0.746871 0.675728 0.494277 0.019 Uiso 1 1 calc R U . . .
C26 C 0.86512(18) 0.66332(17) 0.66251(13) 0.0155(4) Uani 1 1 d . . . . .
H26A H 0.891111 0.650060 0.714664 0.019 Uiso 1 1 calc R U . . .
H26B H 0.816694 0.612972 0.663343 0.019 Uiso 1 1 calc R U . . .
O31 O 0.71487(13) 0.93643(13) 0.41448(10) 0.0190(3) Uani 1 1 d D . . . .
O32 O 0.89096(14) 0.82206(14) 0.72733(11) 0.0201(3) Uani 1 1 d . . . . .
C31 C 0.70967(17) 0.89498(17) 0.48364(14) 0.0162(4) Uani 1 1 d . . . . .
C32 C 0.82569(18) 0.82413(17) 0.68183(13) 0.0156(4) Uani 1 1 d . . . . .
C33 C 0.72425(17) 0.77418(17) 0.59962(13) 0.0148(4) Uani 1 1 d . . . . .
H33 H 0.678255 0.718632 0.615809 0.018 Uiso 1 1 calc R U . . .
C34 C 0.67666(17) 0.86724(16) 0.61522(13) 0.0152(4) Uani 1 1 d . . . . .
H34 H 0.610450 0.854873 0.643417 0.018 Uiso 1 1 calc R U . . .
N31 N 0.74402(15) 0.80352(15) 0.51708(11) 0.0159(4) Uani 1 1 d . . . . .
N32 N 0.66688(16) 0.93214(15) 0.53910(12) 0.0168(4) Uani 1 1 d . . . . .
N33 N 0.75094(15) 0.89373(14) 0.66115(11) 0.0154(4) Uani 1 1 d . . . . .
N34 N 0.81364(15) 0.75677(15) 0.64316(12) 0.0152(4) Uani 1 1 d . . . . .
C35 C 0.61389(17) 1.02500(17) 0.52400(14) 0.0166(4) Uani 1 1 d . . . . .
H35A H 0.588756 1.041949 0.471379 0.020 Uiso 1 1 calc R U . . .
H35B H 0.555175 1.019051 0.560007 0.020 Uiso 1 1 calc R U . . .
C36 C 0.73318(18) 0.96776(16) 0.70008(13) 0.0156(4) Uani 1 1 d . . . . .
H36A H 0.774588 0.952341 0.745926 0.019 Uiso 1 1 calc R U . . .
H36B H 0.662114 0.967028 0.717874 0.019 Uiso 1 1 calc R U . . .
Tb2 Tb 0.53316(2) 0.42708(2) 0.71553(2) 0.01320(4) Uani 1 1 d . . . . .
O21M O 0.40323(14) 0.43379(16) 0.62674(11) 0.0241(4) Uani 1 1 d D . . . .
H211 H 0.419(2) 0.416(3) 0.5868(13) 0.029 Uiso 1 1 d D U . . .
H212 H 0.3403(9) 0.444(3) 0.6282(18) 0.029 Uiso 1 1 d D U . . .
O22M O 0.50785(14) 0.26916(13) 0.70433(10) 0.0193(3) Uani 1 1 d D . . . .
H221 H 0.543(2) 0.2225(16) 0.7303(15) 0.023 Uiso 1 1 d D U . . .
H222 H 0.487(2) 0.255(2) 0.6656(12) 0.023 Uiso 1 1 d D U . . .
O23M O 0.70003(13) 0.34418(13) 0.72773(10) 0.0190(3) Uani 1 1 d D . . . .
H231 H 0.707(2) 0.2840(8) 0.7508(17) 0.023 Uiso 1 1 d D U . . .
H232 H 0.7498(17) 0.3724(18) 0.7385(19) 0.023 Uiso 1 1 d D U . . .
O24M O 0.60306(14) 0.49363(13) 0.80593(11) 0.0207(3) Uani 1 1 d D . . . .
H241 H 0.623(2) 0.5513(10) 0.7939(18) 0.025 Uiso 1 1 d D U . . .
H242 H 0.639(2) 0.4582(17) 0.8397(15) 0.025 Uiso 1 1 d D U . . .
O25M O 0.47942(15) 0.59361(13) 0.68063(11) 0.0216(4) Uani 1 1 d D . . . .
H251 H 0.487(3) 0.6351(18) 0.6372(9) 0.026 Uiso 1 1 d D U . . .
H252 H 0.452(3) 0.621(2) 0.7122(13) 0.026 Uiso 1 1 d D U . . .
N2 N 0.67426(15) 0.48628(14) 0.58777(12) 0.0155(4) Uani 1 1 d . . . . .
O21N O 0.67009(13) 0.52781(12) 0.64040(10) 0.0175(3) Uani 1 1 d . . . . .
O22N O 0.60459(13) 0.42939(12) 0.58727(10) 0.0170(3) Uani 1 1 d . . . . .
O23N O 0.74351(14) 0.49814(13) 0.53944(11) 0.0216(4) Uani 1 1 d D . . . .
O41 O 0.55168(13) 0.30722(13) 0.84075(10) 0.0171(3) Uani 1 1 d . . . . .
O42 O 0.38867(14) 0.18413(13) 1.17254(10) 0.0200(3) Uani 1 1 d . . . . .
C41 C 0.52407(18) 0.24832(17) 0.90046(14) 0.0152(4) Uani 1 1 d . . . . .
C42 C 0.42099(18) 0.17503(17) 1.11081(14) 0.0165(4) Uani 1 1 d . . . . .
C43 C 0.53161(18) 0.13549(17) 1.02055(14) 0.0163(4) Uani 1 1 d . . . . .
H43 H 0.561281 0.068832 1.028207 0.020 Uiso 1 1 calc R U . . .
C44 C 0.42325(18) 0.14313(17) 0.99195(13) 0.0158(4) Uani 1 1 d . . . . .
H44 H 0.400712 0.079558 0.987912 0.019 Uiso 1 1 calc R U . . .
N41 N 0.58441(15) 0.20528(15) 0.95956(12) 0.0165(4) Uani 1 1 d . . . . .
N42 N 0.43069(15) 0.21340(15) 0.91764(12) 0.0161(4) Uani 1 1 d . . . . .
N43 N 0.36541(15) 0.17493(15) 1.04970(12) 0.0170(4) Uani 1 1 d . . . . .
N44 N 0.51939(16) 0.16039(16) 1.09212(12) 0.0164(4) Uani 1 1 d . . . . .
C45 C 0.35192(18) 0.23640(17) 0.86382(13) 0.0164(4) Uani 1 1 d . . . . .
H45A H 0.309002 0.179786 0.872589 0.020 Uiso 1 1 calc R U . . .
H45B H 0.381746 0.249525 0.811188 0.020 Uiso 1 1 calc R U . . .
C46 C 0.25808(17) 0.19284(17) 1.04796(14) 0.0173(4) Uani 1 1 d . . . . .
H46A H 0.230837 0.182991 1.101067 0.021 Uiso 1 1 calc R U . . .
H46B H 0.227319 0.145425 1.026349 0.021 Uiso 1 1 calc R U . . .
O51 O 0.38299(13) 0.43492(13) 0.78357(10) 0.0177(3) Uani 1 1 d . . . . .
O52 O 0.19449(13) 0.35283(13) 1.10513(10) 0.0189(3) Uani 1 1 d . . . . .
C51 C 0.31383(17) 0.41095(17) 0.83224(13) 0.0146(4) Uani 1 1 d . . . . .
C52 C 0.19644(17) 0.35941(17) 1.03640(14) 0.0163(4) Uani 1 1 d . . . . .
C53 C 0.20581(17) 0.31452(17) 0.92253(13) 0.0154(4) Uani 1 1 d . . . . .
H53 H 0.152973 0.272351 0.913483 0.018 Uiso 1 1 calc R U . . .
C54 C 0.16870(17) 0.42169(17) 0.90528(13) 0.0148(4) Uani 1 1 d . . . . .
H54 H 0.102710 0.432456 0.880121 0.018 Uiso 1 1 calc R U . . .
N51 N 0.29047(15) 0.31923(15) 0.86972(12) 0.0158(4) Uani 1 1 d . . . . .
N52 N 0.24854(15) 0.47365(15) 0.85401(11) 0.0152(4) Uani 1 1 d . . . . .
N53 N 0.16120(15) 0.43712(15) 0.98043(11) 0.0158(4) Uani 1 1 d . . . . .
N54 N 0.23060(15) 0.28967(15) 1.00280(11) 0.0161(4) Uani 1 1 d . . . . .
C55 C 0.24166(18) 0.57423(17) 0.80981(13) 0.0163(4) Uani 1 1 d . . . . .
H55A H 0.284469 0.583253 0.762588 0.020 Uiso 1 1 calc R U . . .
H55B H 0.171761 0.590479 0.794200 0.020 Uiso 1 1 calc R U . . .
C56 C 0.12269(17) 0.52503(17) 0.99629(13) 0.0158(4) Uani 1 1 d . . . . .
H56A H 0.062129 0.547585 0.966297 0.019 Uiso 1 1 calc R U . . .
H56B H 0.102239 0.510233 1.051290 0.019 Uiso 1 1 calc R U . . .
O61 O 0.40883(14) 0.70388(15) 0.77386(11) 0.0221(4) Uani 1 1 d . . . . .
O62 O 0.23743(13) 0.59025(13) 1.10225(10) 0.0169(3) Uani 1 1 d . . . . .
C61 C 0.34663(18) 0.70398(18) 0.82547(13) 0.0173(4) Uani 1 1 d . . . . .
C62 C 0.23633(17) 0.63309(17) 1.03382(13) 0.0142(4) Uani 1 1 d . . . . .
C63 C 0.20119(17) 0.67070(17) 0.90373(13) 0.0152(4) Uani 1 1 d . . . . .
H63 H 0.134401 0.690296 0.880844 0.018 Uiso 1 1 calc R U . . .
C64 C 0.25382(17) 0.75700(17) 0.91891(13) 0.0149(4) Uani 1 1 d . . . . .
H64 H 0.209329 0.816296 0.909033 0.018 Uiso 1 1 calc R U . . .
N61 N 0.27154(15) 0.63983(15) 0.85102(11) 0.0165(4) Uani 1 1 d . . . . .
N62 N 0.34003(15) 0.77002(15) 0.86674(11) 0.0164(4) Uani 1 1 d . . . . .
N63 N 0.27728(16) 0.72013(15) 0.99982(11) 0.0165(4) Uani 1 1 d . . . . .
N64 N 0.19258(15) 0.60230(15) 0.97869(11) 0.0153(4) Uani 1 1 d . . . . .
C65 C 0.40347(18) 0.85204(17) 0.85310(13) 0.0176(4) Uani 1 1 d . . . . .
H65A H 0.435135 0.864153 0.801111 0.021 Uiso 1 1 calc R U . . .
H65B H 0.361506 0.909766 0.854401 0.021 Uiso 1 1 calc R U . . .
C66 C 0.30881(18) 0.78222(17) 1.04430(14) 0.0164(4) Uani 1 1 d . . . . .
H66A H 0.274966 0.846363 1.025660 0.020 Uiso 1 1 calc R U . . .
H66B H 0.286953 0.754548 1.098544 0.020 Uiso 1 1 calc R U . . .
N3 N 1.03289(15) 0.78698(16) 0.00734(12) 0.0167(4) Uani 1 1 d . . . . .
O31N O 1.07219(16) 0.86612(15) -0.00036(11) 0.0240(4) Uani 1 1 d . . . . .
O32N O 1.03121(15) 0.72413(14) 0.07186(11) 0.0223(4) Uani 1 1 d . . . . .
O33N O 0.99710(15) 0.76824(15) -0.04858(11) 0.0245(4) Uani 1 1 d . . . . .
N4 N 0.87236(17) 0.57920(16) 0.33164(13) 0.0211(4) Uani 1 1 d . U . . .
O41N O 0.81058(17) 0.55199(19) 0.38527(13) 0.0374(5) Uani 1 1 d D U . . .
H41N H 0.808(2) 0.5351(10) 0.4347(6) 0.045 Uiso 1 1 d D U . . .
O42N O 0.84363(16) 0.63430(15) 0.26829(11) 0.0268(4) Uani 1 1 d . U . . .
O43N O 0.96224(15) 0.55502(15) 0.34068(12) 0.0278(4) Uani 1 1 d . U . . .
N5 N 0.46906(15) 0.27593(16) 0.50830(12) 0.0168(4) Uani 1 1 d . . . . .
O51N O 0.44234(16) 0.36188(14) 0.50012(11) 0.0239(4) Uani 1 1 d . . . . .
O52N O 0.46861(16) 0.21659(15) 0.57416(11) 0.0236(4) Uani 1 1 d . . . . .
O53N O 0.49550(15) 0.24799(15) 0.45092(11) 0.0245(4) Uani 1 1 d . . . . .
N6 N 0.63577(16) 0.07542(15) 0.83927(12) 0.0182(4) Uani 1 1 d . . . . .
O61N O 0.65455(15) 0.13938(14) 0.77738(11) 0.0239(4) Uani 1 1 d . . . . .
O62N O 0.54723(15) 0.05206(16) 0.85891(13) 0.0283(4) Uani 1 1 d . . . . .
O63N O 0.70493(15) 0.03531(15) 0.88101(12) 0.0274(4) Uani 1 1 d . . . . .
N7 N 1.0250(11) 1.0222(10) 0.4609(10) 0.051(2) Uani 0.25 1 d D U P A -1
O71N O 1.0147(11) 0.9595(10) 0.4262(9) 0.038(2) Uani 0.25 1 d D U P A -1
O72N O 1.0915(10) 1.0095(11) 0.5078(9) 0.051(3) Uani 0.25 1 d D U P A -1
O73N O 0.9708(10) 1.0959(9) 0.4460(8) 0.057(2) Uani 0.25 1 d D U P A -1
N7A N 1.0071(8) 1.0409(8) 0.4647(7) 0.041(2) Uani 0.25 1 d D U P B -2
O71A O 1.0719(11) 1.0448(11) 0.5090(9) 0.050(2) Uani 0.25 1 d D U P B -2
O72A O 1.0258(14) 0.9867(12) 0.4228(11) 0.048(2) Uani 0.25 1 d D U P B -2
O73A O 0.9264(9) 1.0855(11) 0.4589(9) 0.057(2) Uani 0.25 1 d D U P B -2
N8 N 0.4611(10) 0.5080(9) 0.9690(7) 0.053(2) Uani 0.25 1 d D U P C -1
O81N O 0.4750(9) 0.4493(9) 0.9303(6) 0.040(2) Uani 0.25 1 d D U P C -1
O82N O 0.5123(11) 0.5813(9) 0.9527(7) 0.057(2) Uani 0.25 1 d D U P C -1
O83N O 0.4053(8) 0.4886(10) 1.0267(5) 0.049(2) Uani 0.25 1 d D U P C -1
N8A N 0.4975(9) 0.5372(13) 0.9698(8) 0.052(2) Uani 0.25 1 d D U P D -2
O81A O 0.5778(11) 0.5784(12) 0.9522(8) 0.058(2) Uani 0.25 1 d D U P D -2
O82A O 0.4417(10) 0.5533(12) 1.0207(7) 0.059(2) Uani 0.25 1 d D U P D -2
O83A O 0.4675(10) 0.4958(11) 0.9240(7) 0.044(2) Uani 0.25 1 d D U P D -2
O1W O 0.82411(16) 1.17993(14) 0.27224(11) 0.0232(4) Uani 1 1 d D . . . .
H11W H 0.8749(16) 1.212(2) 0.2801(18) 0.028 Uiso 1 1 d D U . . .
H12W H 0.7803(18) 1.182(3) 0.3086(15) 0.028 Uiso 1 1 d D U . . .
O2W O 0.60363(17) 0.92006(16) 0.25335(14) 0.0325(5) Uani 1 1 d D . . . .
H21W H 0.5626(16) 0.930(2) 0.2887(14) 0.039 Uiso 1 1 d D U . . .
H22W H 0.566(2) 0.923(3) 0.2138(12) 0.039 Uiso 1 1 d D U . . .
O3W O 1.42722(17) 0.93226(19) 0.66832(13) 0.0333(5) Uani 1 1 d D . . . .
H31W H 1.400(2) 0.8807(12) 0.656(2) 0.040 Uiso 1 1 d D U . . .
H32W H 1.3871(15) 0.9782(12) 0.6435(6) 0.040 Uiso 1 1 d D U . . .
O4W O 0.85894(14) 0.43504(15) 0.75496(11) 0.0225(4) Uani 1 1 d D . . . .
H41W H 0.9210(11) 0.427(3) 0.7416(17) 0.027 Uiso 1 1 d D U . . .
H42W H 0.859(2) 0.442(3) 0.8008(10) 0.027 Uiso 1 1 d D U . . .
O5W O 0.67454(16) 0.66473(14) 0.77607(11) 0.0226(4) Uani 1 1 d D . . . .
H51W H 0.7199(18) 0.658(2) 0.8104(16) 0.027 Uiso 1 1 d D U . . .
H52W H 0.6309(19) 0.707(2) 0.7863(18) 0.027 Uiso 1 1 d D U . . .
O6W O 0.00464(16) 0.3951(2) 1.16580(12) 0.0345(5) Uani 1 1 d D . . . .
H61W H 0.0637(15) 0.373(3) 1.1559(19) 0.041 Uiso 1 1 d D U . . .
H62W H -0.0163(12) 0.359(2) 1.2094(7) 0.041 Uiso 1 1 d D 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
Tb1 O11M 2.4757(19) . yes
Tb1 O12M 2.3803(18) . yes
Tb1 O13M 2.4012(19) . yes
Tb1 O14M 2.4119(18) . yes
Tb1 O15M 2.363(2) . yes
Tb1 N1 2.899(2) . ?
Tb1 O11N 2.4545(18) . yes
Tb1 O12N 2.5270(18) . yes
Tb1 O11 2.3502(18) . yes
Tb1 O21 2.4617(17) . yes
O11M H111 0.848(10) . ?
O11M H112 0.851(10) . ?
O12M H121 0.852(10) . ?
O12M H122 0.850(10) . ?
O13M H131 0.848(10) . ?
O13M H132 0.846(10) . ?
O14M H141 0.849(10) . ?
O14M H142 0.848(10) . ?
O15M H151 0.857(8) . ?
O15M H152 0.847(7) . ?
N1 O11N 1.273(3) . ?
N1 O12N 1.259(3) . ?
N1 O13N 1.229(3) . ?
O11 C11 1.240(3) . ?
O12 C12 1.221(3) . ?
C11 N11 1.351(3) . ?
C11 N12 1.356(3) . ?
C12 N13 1.370(3) . ?
C12 N14 1.369(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.550(3) . ?
C13 N11 1.454(3) . ?
C13 N14 1.435(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.451(3) . ?
C14 N13 1.453(3) . ?
N11 C36 1.452(3) 2_776 ?
N12 C15 1.446(3) . ?
N13 C16 1.447(3) . ?
N14 C35 1.434(3) 2_776 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.437(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.454(3) . ?
O21 C21 1.228(3) . ?
O22 C22 1.226(3) . ?
C21 N21 1.360(3) . ?
C21 N22 1.367(3) . ?
C22 N23 1.364(3) . ?
C22 N24 1.367(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.549(3) . ?
C23 N21 1.444(3) . ?
C23 N24 1.451(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.461(3) . ?
C24 N23 1.440(3) . ?
N22 C25 1.455(3) . ?
N23 C26 1.447(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 N31 1.446(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 N34 1.447(3) . ?
O31 C31 1.232(3) . ?
O32 C32 1.225(3) . ?
C31 N31 1.359(3) . ?
C31 N32 1.362(3) . ?
C32 N33 1.375(3) . ?
C32 N34 1.367(3) . ?
C33 H33 1.0000 . ?
C33 C34 1.553(3) . ?
C33 N31 1.455(3) . ?
C33 N34 1.440(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.446(3) . ?
C34 N33 1.456(3) . ?
N32 C35 1.451(3) . ?
N33 C36 1.443(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
Tb2 O21M 2.4080(19) . yes
Tb2 O22M 2.3820(18) . yes
Tb2 O23M 2.4786(19) . yes
Tb2 O24M 2.3657(18) . yes
Tb2 O25M 2.3950(19) . yes
Tb2 N2 2.882(2) . ?
Tb2 O21N 2.4933(18) . yes
Tb2 O22N 2.4705(18) . yes
Tb2 O41 2.4592(17) . yes
Tb2 O51 2.3263(18) . yes
O21M H211 0.847(10) . ?
O21M H212 0.851(10) . ?
O22M H221 0.845(10) . ?
O22M H222 0.846(10) . ?
O23M H231 0.855(10) . ?
O23M H232 0.853(10) . ?
O24M H241 0.850(10) . ?
O24M H242 0.841(10) . ?
O25M H251 0.852(10) . ?
O25M H252 0.842(10) . ?
N2 O21N 1.261(3) . ?
N2 O22N 1.270(3) . ?
N2 O23N 1.231(3) . ?
O41 C41 1.229(3) . ?
O42 C42 1.223(3) . ?
C41 N41 1.363(3) . ?
C41 N42 1.357(3) . ?
C42 N43 1.366(3) . ?
C42 N44 1.368(3) . ?
C43 H43 1.0000 . ?
C43 C44 1.553(3) . ?
C43 N41 1.451(3) . ?
C43 N44 1.444(3) . ?
C44 H44 1.0000 . ?
C44 N42 1.446(3) . ?
C44 N43 1.441(3) . ?
N41 C66 1.444(3) 2_667 ?
N42 C45 1.437(3) . ?
N43 C46 1.449(3) . ?
N44 C65 1.439(3) 2_667 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 N51 1.448(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 N54 1.451(3) . ?
O51 C51 1.241(3) . ?
O52 C52 1.225(3) . ?
C51 N51 1.350(3) . ?
C51 N52 1.357(3) . ?
C52 N53 1.370(3) . ?
C52 N54 1.369(3) . ?
C53 H53 1.0000 . ?
C53 C54 1.554(3) . ?
C53 N51 1.442(3) . ?
C53 N54 1.453(3) . ?
C54 H54 1.0000 . ?
C54 N52 1.468(3) . ?
C54 N53 1.443(3) . ?
N52 C55 1.450(3) . ?
N53 C56 1.447(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 N61 1.440(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 N64 1.442(3) . ?
O61 C61 1.225(3) . ?
O62 C62 1.225(3) . ?
C61 N61 1.370(3) . ?
C61 N62 1.365(3) . ?
C62 N63 1.360(3) . ?
C62 N64 1.367(3) . ?
C63 H63 1.0000 . ?
C63 C64 1.551(3) . ?
C63 N61 1.457(3) . ?
C63 N64 1.444(3) . ?
C64 H64 1.0000 . ?
C64 N62 1.443(3) . ?
C64 N63 1.462(3) . ?
N62 C65 1.443(3) . ?
N63 C66 1.450(3) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
N3 O31N 1.246(3) . ?
N3 O32N 1.266(3) . ?
N3 O33N 1.243(3) . ?
N4 O41N 1.235(3) . ?
N4 O42N 1.269(3) . ?
N4 O43N 1.244(3) . ?
O41N H41N 0.863(9) . ?
N5 O51N 1.246(3) . ?
N5 O52N 1.262(3) . ?
N5 O53N 1.251(3) . ?
N6 O61N 1.262(3) . ?
N6 O62N 1.254(3) . ?
N6 O63N 1.242(3) . ?
N7 O71N 1.253(7) . ?
N7 O72N 1.234(7) . ?
N7 O73N 1.234(7) . ?
N7A O71A 1.224(7) . ?
N7A O72A 1.245(8) . ?
N7A O73A 1.228(7) . ?
N8 O81N 1.246(7) . ?
N8 O82N 1.242(7) . ?
N8 O83N 1.231(7) . ?
N8A O81A 1.235(8) . ?
N8A O82A 1.227(7) . ?
N8A O83A 1.241(8) . ?
O1W H11W 0.874(10) . ?
O1W H12W 0.869(10) . ?
O2W H21W 0.865(10) . ?
O2W H22W 0.882(10) . ?
O3W H31W 0.931(8) . ?
O3W H32W 0.870(7) . ?
O4W H41W 0.868(10) . ?
O4W H42W 0.866(10) . ?
O5W H51W 0.874(10) . ?
O5W H52W 0.874(10) . ?
O6W H61W 0.869(10) . ?
O6W H62W 0.861(10) . ?

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
O11M Tb1 N1 63.08(6) . . ?
O11M Tb1 O12N 69.08(6) . . ?
O12M Tb1 O11M 76.38(7) . . ?
O12M Tb1 O13M 70.61(7) . . ?
O12M Tb1 O14M 144.50(6) . . ?
O12M Tb1 N1 95.39(6) . . ?
O12M Tb1 O11N 120.19(6) . . ?
O12M Tb1 O12N 72.32(6) . . ?
O12M Tb1 O21 73.90(6) . . ?
O13M Tb1 O11M 132.32(7) . . ?
O13M Tb1 O14M 74.23(7) . . ?
O13M Tb1 N1 86.58(7) . . ?
O13M Tb1 O11N 101.39(7) . . ?
O13M Tb1 O12N 68.70(6) . . ?
O13M Tb1 O21 130.84(7) . . ?
O14M Tb1 O11M 134.15(7) . . ?
O14M Tb1 N1 87.25(6) . . ?
O14M Tb1 O11N 71.48(6) . . ?
O14M Tb1 O12N 99.46(6) . . ?
O14M Tb1 O21 129.35(6) . . ?
O15M Tb1 O11M 80.62(7) . . ?
O15M Tb1 O12M 141.24(6) . . ?
O15M Tb1 O13M 144.35(7) . . ?
O15M Tb1 O14M 71.58(6) . . ?
O15M Tb1 N1 101.48(7) . . ?
O15M Tb1 O11N 77.11(7) . . ?
O15M Tb1 O12N 126.76(7) . . ?
O15M Tb1 O21 68.48(6) . . ?
O11N Tb1 O11M 67.16(6) . . ?
O11N Tb1 N1 25.84(6) . . ?
O11N Tb1 O12N 51.29(6) . . ?
O11N Tb1 O21 125.80(6) . . ?
O12N Tb1 N1 25.68(6) . . ?
O11 Tb1 O11M 141.62(6) . . ?
O11 Tb1 O12M 90.36(6) . . ?
O11 Tb1 O13M 72.55(6) . . ?
O11 Tb1 O14M 74.39(6) . . ?
O11 Tb1 O15M 88.68(7) . . ?
O11 Tb1 N1 155.14(6) . . ?
O11 Tb1 O11N 145.64(6) . . ?
O11 Tb1 O12N 140.90(6) . . ?
O11 Tb1 O21 74.82(6) . . ?
O21 Tb1 O11M 66.94(6) . . ?
O21 Tb1 N1 130.00(6) . . ?
O21 Tb1 O12N 129.27(6) . . ?
Tb1 O11M H111 116(2) . . ?
Tb1 O11M H112 131(2) . . ?
H111 O11M H112 108.8(16) . . ?
Tb1 O12M H121 118(2) . . ?
Tb1 O12M H122 117(2) . . ?
H121 O12M H122 108.3(16) . . ?
Tb1 O13M H131 125(2) . . ?
Tb1 O13M H132 126(2) . . ?
H131 O13M H132 108.9(16) . . ?
Tb1 O14M H141 128(2) . . ?
Tb1 O14M H142 122(2) . . ?
H141 O14M H142 108.9(16) . . ?
Tb1 O15M H151 120(2) . . ?
Tb1 O15M H152 122(2) . . ?
H151 O15M H152 108.4(13) . . ?
O11N N1 Tb1 57.20(11) . . ?
O12N N1 Tb1 60.44(12) . . ?
O12N N1 O11N 116.9(2) . . ?
O13N N1 Tb1 170.27(17) . . ?
O13N N1 O11N 121.2(2) . . ?
O13N N1 O12N 121.9(2) . . ?
N1 O11N Tb1 96.96(14) . . ?
N1 O12N Tb1 93.88(13) . . ?
C11 O11 Tb1 158.48(16) . . ?
O11 C11 N11 125.1(2) . . ?
O11 C11 N12 125.4(2) . . ?
N11 C11 N12 109.51(19) . . ?
O12 C12 N13 126.5(2) . . ?
O12 C12 N14 125.5(2) . . ?
N14 C12 N13 108.03(19) . . ?
C14 C13 H13 111.7 . . ?
N11 C13 H13 111.7 . . ?
N11 C13 C14 103.88(18) . . ?
N14 C13 H13 111.7 . . ?
N14 C13 C14 103.32(18) . . ?
N14 C13 N11 114.13(19) . . ?
C13 C14 H14 111.9 . . ?
N12 C14 C13 101.99(18) . . ?
N12 C14 H14 111.9 . . ?
N12 C14 N13 115.38(19) . . ?
N13 C14 C13 102.98(18) . . ?
N13 C14 H14 111.9 . . ?
C11 N11 C13 111.17(19) . . ?
C11 N11 C36 123.38(19) . 2_776 ?
C36 N11 C13 121.95(19) 2_776 . ?
C11 N12 C14 112.61(18) . . ?
C11 N12 C15 124.00(19) . . ?
C15 N12 C14 123.25(19) . . ?
C12 N13 C14 111.80(19) . . ?
C12 N13 C16 121.98(19) . . ?
C16 N13 C14 123.85(19) . . ?
C12 N14 C13 112.83(19) . . ?
C12 N14 C35 123.7(2) . 2_776 ?
C35 N14 C13 122.6(2) 2_776 . ?
N12 C15 H15A 108.8 . . ?
N12 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
N21 C15 N12 113.62(19) . . ?
N21 C15 H15A 108.8 . . ?
N21 C15 H15B 108.8 . . ?
N13 C16 H16A 109.0 . . ?
N13 C16 H16B 109.0 . . ?
N13 C16 N24 113.06(19) . . ?
H16A C16 H16B 107.8 . . ?
N24 C16 H16A 109.0 . . ?
N24 C16 H16B 109.0 . . ?
C21 O21 Tb1 157.46(16) . . ?
O21 C21 N21 125.4(2) . . ?
O21 C21 N22 125.6(2) . . ?
N21 C21 N22 109.0(2) . . ?
O22 C22 N23 125.3(2) . . ?
O22 C22 N24 126.2(2) . . ?
N23 C22 N24 108.5(2) . . ?
C24 C23 H23 111.6 . . ?
N21 C23 H23 111.6 . . ?
N21 C23 C24 103.02(18) . . ?
N21 C23 N24 115.03(18) . . ?
N24 C23 H23 111.6 . . ?
N24 C23 C24 103.27(18) . . ?
C23 C24 H24 111.6 . . ?
N22 C24 C23 103.17(18) . . ?
N22 C24 H24 111.6 . . ?
N23 C24 C23 102.85(18) . . ?
N23 C24 H24 111.6 . . ?
N23 C24 N22 115.3(2) . . ?
C15 N21 C23 125.37(19) . . ?
C21 N21 C15 122.06(19) . . ?
C21 N21 C23 112.56(19) . . ?
C21 N22 C24 111.15(19) . . ?
C21 N22 C25 121.0(2) . . ?
C25 N22 C24 123.26(19) . . ?
C22 N23 C24 112.71(19) . . ?
C22 N23 C26 123.6(2) . . ?
C24 N23 C26 123.58(19) . . ?
C22 N24 C16 123.6(2) . . ?
C22 N24 C23 111.39(19) . . ?
C23 N24 C16 123.18(19) . . ?
N22 C25 H25A 108.8 . . ?
N22 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N31 C25 N22 113.91(19) . . ?
N31 C25 H25A 108.8 . . ?
N31 C25 H25B 108.8 . . ?
N23 C26 H26A 109.0 . . ?
N23 C26 H26B 109.0 . . ?
N23 C26 N34 113.05(19) . . ?
H26A C26 H26B 107.8 . . ?
N34 C26 H26A 109.0 . . ?
N34 C26 H26B 109.0 . . ?
O31 C31 N31 125.5(2) . . ?
O31 C31 N32 125.9(2) . . ?
N31 C31 N32 108.6(2) . . ?
O32 C32 N33 126.3(2) . . ?
O32 C32 N34 125.9(2) . . ?
N34 C32 N33 107.8(2) . . ?
C34 C33 H33 112.0 . . ?
N31 C33 H33 112.0 . . ?
N31 C33 C34 102.88(18) . . ?
N34 C33 H33 112.0 . . ?
N34 C33 C34 103.75(18) . . ?
N34 C33 N31 113.44(19) . . ?
C33 C34 H34 111.8 . . ?
N32 C34 C33 103.11(18) . . ?
N32 C34 H34 111.8 . . ?
N32 C34 N33 115.00(19) . . ?
N33 C34 C33 102.61(18) . . ?
N33 C34 H34 111.8 . . ?
C25 N31 C33 123.29(19) . . ?
C31 N31 C25 123.6(2) . . ?
C31 N31 C33 112.4(2) . . ?
C31 N32 C34 112.59(19) . . ?
C31 N32 C35 124.2(2) . . ?
C34 N32 C35 123.2(2) . . ?
C32 N33 C34 112.36(19) . . ?
C32 N33 C36 121.84(19) . . ?
C36 N33 C34 123.22(19) . . ?
C32 N34 C26 123.0(2) . . ?
C32 N34 C33 112.8(2) . . ?
C33 N34 C26 121.49(19) . . ?
N14 C35 N32 114.04(19) 2_776 . ?
N14 C35 H35A 108.7 2_776 . ?
N14 C35 H35B 108.7 2_776 . ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
N11 C36 H36A 108.8 2_776 . ?
N11 C36 H36B 108.8 2_776 . ?
N33 C36 N11 113.66(19) . 2_776 ?
N33 C36 H36A 108.8 . . ?
N33 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
O21M Tb2 O23M 130.84(6) . . ?
O21M Tb2 N2 89.26(6) . . ?
O21M Tb2 O21N 106.06(7) . . ?
O21M Tb2 O22N 68.89(6) . . ?
O21M Tb2 O41 126.31(7) . . ?
O22M Tb2 O21M 70.39(7) . . ?
O22M Tb2 O23M 73.99(6) . . ?
O22M Tb2 O25M 146.92(7) . . ?
O22M Tb2 N2 97.16(6) . . ?
O22M Tb2 O21N 120.97(6) . . ?
O22M Tb2 O22N 75.30(6) . . ?
O22M Tb2 O41 70.01(6) . . ?
O23M Tb2 N2 62.71(6) . . ?
O23M Tb2 O21N 65.91(6) . . ?
O24M Tb2 O21M 148.24(7) . . ?
O24M Tb2 O22M 136.32(6) . . ?
O24M Tb2 O23M 79.78(6) . . ?
O24M Tb2 O25M 74.58(7) . . ?
O24M Tb2 N2 101.06(6) . . ?
O24M Tb2 O21N 76.50(6) . . ?
O24M Tb2 O22N 126.83(6) . . ?
O24M Tb2 O41 67.89(6) . . ?
O25M Tb2 O21M 76.62(7) . . ?
O25M Tb2 O23M 133.31(6) . . ?
O25M Tb2 N2 84.67(6) . . ?
O25M Tb2 O21N 70.48(6) . . ?
O25M Tb2 O22N 95.39(6) . . ?
O25M Tb2 O41 132.07(6) . . ?
O21N Tb2 N2 25.85(5) . . ?
O22N Tb2 O23M 70.10(6) . . ?
O22N Tb2 N2 26.01(5) . . ?
O22N Tb2 O21N 51.58(5) . . ?
O41 Tb2 O23M 67.60(6) . . ?
O41 Tb2 N2 130.28(6) . . ?
O41 Tb2 O21N 125.05(6) . . ?
O41 Tb2 O22N 130.85(6) . . ?
O51 Tb2 O21M 74.17(6) . . ?
O51 Tb2 O22M 94.48(6) . . ?
O51 Tb2 O23M 141.93(6) . . ?
O51 Tb2 O24M 85.12(7) . . ?
O51 Tb2 O25M 73.78(6) . . ?
O51 Tb2 N2 155.23(6) . . ?
O51 Tb2 O21N 142.98(6) . . ?
O51 Tb2 O22N 143.00(6) . . ?
O51 Tb2 O41 74.35(6) . . ?
Tb2 O21M H211 117(2) . . ?
Tb2 O21M H212 134(2) . . ?
H211 O21M H212 108.6(16) . . ?
Tb2 O22M H221 119(2) . . ?
Tb2 O22M H222 127(2) . . ?
H221 O22M H222 109.4(16) . . ?
Tb2 O23M H231 121(2) . . ?
Tb2 O23M H232 119(2) . . ?
H231 O23M H232 107.5(15) . . ?
Tb2 O24M H241 122(2) . . ?
Tb2 O24M H242 119(2) . . ?
H241 O24M H242 109.8(16) . . ?
Tb2 O25M H251 128(2) . . ?
Tb2 O25M H252 123(2) . . ?
H251 O25M H252 109.5(16) . . ?
O21N N2 Tb2 59.57(11) . . ?
O21N N2 O22N 117.21(19) . . ?
O22N N2 Tb2 58.57(11) . . ?
O23N N2 Tb2 169.38(16) . . ?
O23N N2 O21N 122.1(2) . . ?
O23N N2 O22N 120.6(2) . . ?
N2 O21N Tb2 94.59(13) . . ?
N2 O22N Tb2 95.43(13) . . ?
C41 O41 Tb2 156.63(17) . . ?
O41 C41 N41 124.8(2) . . ?
O41 C41 N42 126.2(2) . . ?
N42 C41 N41 109.0(2) . . ?
O42 C42 N43 126.2(2) . . ?
O42 C42 N44 125.5(2) . . ?
N43 C42 N44 108.3(2) . . ?
C44 C43 H43 111.5 . . ?
N41 C43 H43 111.5 . . ?
N41 C43 C44 103.30(19) . . ?
N44 C43 H43 111.5 . . ?
N44 C43 C44 103.35(19) . . ?
N44 C43 N41 115.1(2) . . ?
C43 C44 H44 111.6 . . ?
N42 C44 C43 103.08(18) . . ?
N42 C44 H44 111.6 . . ?
N43 C44 C43 103.18(19) . . ?
N43 C44 H44 111.6 . . ?
N43 C44 N42 115.1(2) . . ?
C41 N41 C43 112.0(2) . . ?
C41 N41 C66 123.0(2) . 2_667 ?
C66 N41 C43 124.4(2) 2_667 . ?
C41 N42 C44 112.6(2) . . ?
C41 N42 C45 122.9(2) . . ?
C45 N42 C44 124.22(19) . . ?
C42 N43 C44 112.2(2) . . ?
C42 N43 C46 123.4(2) . . ?
C44 N43 C46 123.9(2) . . ?
C42 N44 C43 112.0(2) . . ?
C42 N44 C65 122.0(2) . 2_667 ?
C65 N44 C43 124.2(2) 2_667 . ?
N42 C45 H45A 109.0 . . ?
N42 C45 H45B 109.0 . . ?
N42 C45 N51 112.92(19) . . ?
H45A C45 H45B 107.8 . . ?
N51 C45 H45A 109.0 . . ?
N51 C45 H45B 109.0 . . ?
N43 C46 H46A 109.1 . . ?
N43 C46 H46B 109.1 . . ?
N43 C46 N54 112.69(19) . . ?
H46A C46 H46B 107.8 . . ?
N54 C46 H46A 109.1 . . ?
N54 C46 H46B 109.1 . . ?
C51 O51 Tb2 160.09(17) . . ?
O51 C51 N51 125.4(2) . . ?
O51 C51 N52 124.6(2) . . ?
N51 C51 N52 109.9(2) . . ?
O52 C52 N53 125.4(2) . . ?
O52 C52 N54 126.1(2) . . ?
N54 C52 N53 108.5(2) . . ?
C54 C53 H53 111.7 . . ?
N51 C53 H53 111.7 . . ?
N51 C53 C54 102.90(18) . . ?
N51 C53 N54 114.82(19) . . ?
N54 C53 H53 111.7 . . ?
N54 C53 C54 103.43(18) . . ?
C53 C54 H54 111.7 . . ?
N52 C54 C53 102.94(18) . . ?
N52 C54 H54 111.7 . . ?
N53 C54 C53 102.76(18) . . ?
N53 C54 H54 111.7 . . ?
N53 C54 N52 115.34(19) . . ?
C51 N51 C45 122.8(2) . . ?
C51 N51 C53 112.47(19) . . ?
C53 N51 C45 124.28(19) . . ?
C51 N52 C54 110.80(19) . . ?
C51 N52 C55 120.8(2) . . ?
C55 N52 C54 124.9(2) . . ?
C52 N53 C54 112.7(2) . . ?
C52 N53 C56 122.7(2) . . ?
C54 N53 C56 124.6(2) . . ?
C46 N54 C53 124.1(2) . . ?
C52 N54 C46 121.7(2) . . ?
C52 N54 C53 111.5(2) . . ?
N52 C55 H55A 108.9 . . ?
N52 C55 H55B 108.9 . . ?
H55A C55 H55B 107.7 . . ?
N61 C55 N52 113.36(19) . . ?
N61 C55 H55A 108.9 . . ?
N61 C55 H55B 108.9 . . ?
N53 C56 H56A 108.7 . . ?
N53 C56 H56B 108.7 . . ?
H56A C56 H56B 107.6 . . ?
N64 C56 N53 114.37(19) . . ?
N64 C56 H56A 108.7 . . ?
N64 C56 H56B 108.7 . . ?
O61 C61 N61 126.5(2) . . ?
O61 C61 N62 125.1(2) . . ?
N62 C61 N61 108.3(2) . . ?
O62 C62 N63 125.8(2) . . ?
O62 C62 N64 125.9(2) . . ?
N63 C62 N64 108.3(2) . . ?
C64 C63 H63 111.9 . . ?
N61 C63 H63 111.9 . . ?
N61 C63 C64 102.94(18) . . ?
N64 C63 H63 111.9 . . ?
N64 C63 C64 103.61(18) . . ?
N64 C63 N61 113.89(19) . . ?
C63 C64 H64 111.9 . . ?
N62 C64 C63 103.41(18) . . ?
N62 C64 H64 111.9 . . ?
N62 C64 N63 114.42(19) . . ?
N63 C64 C63 102.45(18) . . ?
N63 C64 H64 111.9 . . ?
C55 N61 C63 120.50(19) . . ?
C61 N61 C55 123.3(2) . . ?
C61 N61 C63 111.84(19) . . ?
C61 N62 C64 112.6(2) . . ?
C61 N62 C65 124.2(2) . . ?
C65 N62 C64 122.7(2) . . ?
C62 N63 C64 112.59(19) . . ?
C62 N63 C66 121.7(2) . . ?
C66 N63 C64 122.43(19) . . ?
C56 N64 C63 122.32(19) . . ?
C62 N64 C56 123.00(19) . . ?
C62 N64 C63 112.57(19) . . ?
N44 C65 N62 113.6(2) 2_667 . ?
N44 C65 H65A 108.8 2_667 . ?
N44 C65 H65B 108.8 2_667 . ?
N62 C65 H65A 108.8 . . ?
N62 C65 H65B 108.8 . . ?
H65A C65 H65B 107.7 . . ?
N41 C66 N63 113.66(19) 2_667 . ?
N41 C66 H66A 108.8 2_667 . ?
N41 C66 H66B 108.8 2_667 . ?
N63 C66 H66A 108.8 . . ?
N63 C66 H66B 108.8 . . ?
H66A C66 H66B 107.7 . . ?
O31N N3 O32N 120.2(2) . . ?
O33N N3 O31N 120.3(2) . . ?
O33N N3 O32N 119.5(2) . . ?
O41N N4 O42N 119.3(2) . . ?
O41N N4 O43N 120.1(2) . . ?
O43N N4 O42N 120.5(2) . . ?
N4 O41N H41N 139.4(18) . . ?
O51N N5 O52N 120.3(2) . . ?
O51N N5 O53N 119.9(2) . . ?
O53N N5 O52N 119.8(2) . . ?
O62N N6 O61N 120.2(2) . . ?
O63N N6 O61N 120.1(2) . . ?
O63N N6 O62N 119.7(2) . . ?
O72N N7 O71N 118.6(7) . . ?
O73N N7 O71N 119.7(7) . . ?
O73N N7 O72N 121.6(7) . . ?
O71A N7A O72A 116.4(13) . . ?
O71A N7A O73A 125.1(13) . . ?
O73A N7A O72A 118.5(12) . . ?
O82N N8 O81N 118.5(7) . . ?
O83N N8 O81N 120.3(7) . . ?
O83N N8 O82N 120.8(7) . . ?
O81A N8A O83A 116.1(11) . . ?
O82A N8A O81A 120.9(13) . . ?
O82A N8A O83A 121.3(13) . . ?
H11W O1W H12W 105.3(15) . . ?
H21W O2W H22W 105.4(15) . . ?
H31W O3W H32W 98.6(10) . . ?
H41W O4W H42W 106.6(15) . . ?
H51W O5W H52W 104.6(15) . . ?
H61W O6W H62W 107.4(16) . . ?

_refine_diff_density_max         0.787
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.150



####################################################################### 
# 
# 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_km777-8
_database_code_depnum_ccdc_archive 'CCDC 2247482'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_km777-8             
;
PROBLEM: Short Inter D...A Contact  O1M      ..O9W      .       2.50 Ang.
RESPONSE: Hydrogen bonds
;
_vrf_PLAT043_km777-8             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      56.44 Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT306_km777-8             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT430_km777-8_2           
;
PROBLEM: Short Inter D...A Contact  O1M      ..O8W      .       2.68 Ang.
RESPONSE: Hydrogen bonds
;
# Added during the CSD deposition process: Thursday 09 March 2023 03:57 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H92 Er2 N32 O63'
_chemical_formula_weight         2315.93

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.8081(6)
_cell_length_b                   25.8081(6)
_cell_length_c                   31.7446(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18311.0(10)
_cell_formula_units_Z            9
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    13118
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.11

_exptl_crystal_description       plank
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_F_000             10548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.189
_shelx_estimated_absorpt_T_min   0.589
_shelx_estimated_absorpt_T_max   0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6
_diffrn_reflns_number            20707
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.229
_diffrn_reflns_theta_max         28.291
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8730
_reflns_number_gt                8490
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          
;
 Refined as a 2-component twin.
 Twin law: 0 1 0  1 0 0  0 0 -1 
 BASF: 0.3513(6)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+16.5480P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8730
_refine_ls_number_parameters     771
_refine_ls_number_restraints     400
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.38172(2) 0.36632(2) 0.66375(2) 0.01947(5) Uani 1 1 d . . . . .
O1M O 0.43054(15) 0.47120(14) 0.66984(10) 0.0425(7) Uani 1 1 d . . . . .
O2M O 0.41128(12) 0.40001(12) 0.59562(8) 0.0307(6) Uani 1 1 d . . . . .
O3M O 0.30817(14) 0.39271(16) 0.65893(11) 0.0452(8) Uani 1 1 d . . . . .
O4M O 0.31168(13) 0.29673(14) 0.61485(9) 0.0389(7) Uani 1 1 d . . . . .
O5M O 0.48602(12) 0.40375(13) 0.66326(9) 0.0339(7) Uani 1 1 d . . . . .
O6M O 0.40291(12) 0.38772(13) 0.73521(8) 0.0306(6) Uani 1 1 d . . . . .
O7M O 0.30227(13) 0.29251(13) 0.70479(9) 0.0367(7) Uani 1 1 d . . . . .
O8M O 0.39762(14) 0.28600(14) 0.66673(12) 0.0460(8) Uani 1 1 d . . . . .
O11 O 0.49068(13) 0.74880(12) 0.59589(7) 0.0318(6) Uani 1 1 d . . . . .
O12 O 0.47825(13) 0.74439(12) 0.40615(8) 0.0302(6) Uani 1 1 d . . . . .
C11 C 0.51382(16) 0.76165(16) 0.56052(10) 0.0218(7) Uani 1 1 d . . . . .
C12 C 0.50583(16) 0.75878(15) 0.43987(10) 0.0213(6) Uani 1 1 d . . . . .
C13 C 0.56028(16) 0.75779(14) 0.49850(11) 0.0192(7) Uani 1 1 d . . . . .
H13 H 0.602568 0.766478 0.496703 0.023 Uiso 1 1 calc R U . . .
C14 C 0.55656(15) 0.81618(15) 0.49887(10) 0.0190(6) Uani 1 1 d . . . . .
H14 H 0.597062 0.852840 0.497828 0.023 Uiso 1 1 calc R U . . .
N11 N 0.53250(14) 0.72944(13) 0.53795(9) 0.0222(6) Uani 1 1 d . . . . .
N12 N 0.52603(13) 0.81164(13) 0.53816(9) 0.0208(6) Uani 1 1 d . . . . .
N13 N 0.52166(13) 0.81019(13) 0.46160(8) 0.0199(6) Uani 1 1 d . . . . .
N14 N 0.52620(14) 0.72687(13) 0.46144(9) 0.0206(6) Uani 1 1 d . . . . .
C15 C 0.51630(16) 0.85829(16) 0.55415(10) 0.0218(7) Uani 1 1 d . . . . .
H15A H 0.552619 0.897429 0.548864 0.026 Uiso 1 1 calc R U . . .
H15B H 0.510499 0.853425 0.585023 0.026 Uiso 1 1 calc R U . . .
C16 C 0.51841(15) 0.86017(15) 0.44365(10) 0.0191(7) Uani 1 1 d . . . . .
H16A H 0.556010 0.897627 0.450108 0.023 Uiso 1 1 calc R U . . .
H16B H 0.515282 0.855623 0.412635 0.023 Uiso 1 1 calc R U . . .
O21 O 0.40081(13) 0.81632(14) 0.59223(8) 0.0353(6) Uani 1 1 d . . . . .
O22 O 0.40467(11) 0.82289(11) 0.40231(7) 0.0220(5) Uani 1 1 d . . . . .
C21 C 0.41358(16) 0.84221(16) 0.55776(10) 0.0225(7) Uani 1 1 d . . . . .
C22 C 0.41716(15) 0.84726(14) 0.43685(10) 0.0180(6) Uani 1 1 d . . . . .
C23 C 0.46915(15) 0.89383(15) 0.49845(11) 0.0179(7) Uani 1 1 d . . . . .
H23 H 0.503743 0.935607 0.500172 0.021 Uiso 1 1 calc R U . . .
C24 C 0.40828(15) 0.89264(15) 0.49828(10) 0.0181(6) Uani 1 1 d . . . . .
H24 H 0.413899 0.933875 0.499214 0.022 Uiso 1 1 calc R U . . .
N21 N 0.46529(13) 0.85898(13) 0.53568(8) 0.0202(6) Uani 1 1 d . . . . .
N22 N 0.37902(13) 0.85882(14) 0.53588(8) 0.0211(6) Uani 1 1 d . . . . .
N23 N 0.38136(12) 0.86257(13) 0.45905(8) 0.0177(5) Uani 1 1 d . . . . .
N24 N 0.46869(12) 0.86546(13) 0.45893(8) 0.0180(5) Uani 1 1 d . . . . .
C25 C 0.32467(15) 0.85429(17) 0.55304(11) 0.0247(7) Uani 1 1 d . . . . .
H25A H 0.325850 0.852137 0.584140 0.030 Uiso 1 1 calc R U . . .
H25B H 0.323623 0.891051 0.545739 0.030 Uiso 1 1 calc R U . . .
C26 C 0.32416(14) 0.85207(15) 0.44357(10) 0.0189(6) Uani 1 1 d . . . . .
H26A H 0.323271 0.847659 0.412559 0.023 Uiso 1 1 calc R U . . .
H26B H 0.320293 0.887525 0.449985 0.023 Uiso 1 1 calc R U . . .
O31 O 0.40738(11) 0.82606(12) 0.26479(7) 0.0267(5) Uani 1 1 d . . . . .
O32 O 0.40124(12) 0.81073(12) 0.07510(7) 0.0266(5) Uani 1 1 d . . . . .
C31 C 0.41935(16) 0.84915(15) 0.22942(10) 0.0206(7) Uani 1 1 d . . . . .
C32 C 0.41457(16) 0.83794(15) 0.10893(10) 0.0206(6) Uani 1 1 d . . . . .
C33 C 0.47036(15) 0.89292(16) 0.16697(11) 0.0193(7) Uani 1 1 d . . . . .
H33 H 0.504631 0.934810 0.164731 0.023 Uiso 1 1 calc R U . . .
C34 C 0.40965(16) 0.89126(15) 0.16678(10) 0.0201(7) Uani 1 1 d . . . . .
H34 H 0.414850 0.932223 0.164253 0.024 Uiso 1 1 calc R U . . .
N31 N 0.47055(13) 0.86618(14) 0.20703(9) 0.0201(6) Uani 1 1 d . . . . .
N32 N 0.38381(13) 0.86376(14) 0.20714(8) 0.0202(5) Uani 1 1 d . . . . .
N33 N 0.37934(13) 0.85443(13) 0.13048(9) 0.0209(6) Uani 1 1 d . . . . .
N34 N 0.46691(12) 0.85760(13) 0.13041(8) 0.0193(6) Uani 1 1 d . . . . .
C35 C 0.32618(16) 0.85280(16) 0.22160(10) 0.0212(7) Uani 1 1 d . . . . .
H35A H 0.322329 0.888238 0.215081 0.025 Uiso 1 1 calc R U . . .
H35B H 0.324268 0.847928 0.252599 0.025 Uiso 1 1 calc R U . . .
C36 C 0.32769(15) 0.85302(16) 0.11192(10) 0.0221(7) Uani 1 1 d . . . . .
H36A H 0.329971 0.850309 0.080937 0.026 Uiso 1 1 calc R U . . .
H36B H 0.328901 0.891141 0.118390 0.026 Uiso 1 1 calc R U . . .
N1 N 0.54228(14) 0.53582(14) 0.58764(9) 0.0239(6) Uani 1 1 d . . . . .
O11N O 0.55383(13) 0.51256(13) 0.61877(8) 0.0330(6) Uani 1 1 d . . . . .
O12N O 0.49537(14) 0.50544(14) 0.56669(9) 0.0385(7) Uani 1 1 d . . . . .
O13N O 0.57878(13) 0.58655(12) 0.57628(9) 0.0341(6) Uani 1 1 d . . . . .
N2 N 0.53618(14) 0.53435(13) 0.75177(10) 0.0242(6) Uani 1 1 d . . . . .
O21N O 0.53793(18) 0.53139(16) 0.71257(9) 0.0633(13) Uani 1 1 d . . . . .
O22N O 0.57787(11) 0.57751(11) 0.77031(8) 0.0266(6) Uani 1 1 d . . . . .
O23N O 0.49358(12) 0.49397(13) 0.77154(8) 0.0288(6) Uani 1 1 d . . . . .
N3 N 0.33699(13) 0.33474(12) 0.49545(9) 0.0231(6) Uani 1 1 d . . . . .
O31N O 0.36581(12) 0.38212(11) 0.51629(9) 0.0298(6) Uani 1 1 d . . . . .
O32N O 0.30472(12) 0.33235(12) 0.46536(8) 0.0304(6) Uani 1 1 d . . . . .
O33N O 0.34106(16) 0.29017(14) 0.50408(12) 0.0523(10) Uani 1 1 d . . . . .
N4 N 0.3284(3) 0.1670(3) 0.59356(17) 0.0413(15) Uani 0.576(6) 1 d D U P A 1
O41N O 0.2919(6) 0.1465(5) 0.6234(3) 0.059(3) Uani 0.288(3) 1 d D U P A 1
O41' O 0.3353(6) 0.1725(4) 0.63308(19) 0.0372(18) Uani 0.288(3) 1 d D U P A 1
O42N O 0.3415(4) 0.1309(3) 0.5761(2) 0.0632(18) Uani 0.576(6) 1 d D U P A 1
O43N O 0.3291(4) 0.2079(4) 0.5724(3) 0.046(2) Uani 0.576(6) 1 d D U P A 1
N5 N 0.3435(6) 0.1707(6) 0.5925(4) 0.051(3) Uani 0.224(6) 1 d D U P A 2
O51N O 0.3909(6) 0.1967(6) 0.6139(4) 0.047(3) Uani 0.224(6) 1 d D U P A 2
O52N O 0.3223(11) 0.2013(9) 0.5781(8) 0.050(3) Uani 0.224(6) 1 d D U P A 2
O53N O 0.3163(9) 0.1155(6) 0.5855(5) 0.056(3) Uani 0.224(6) 1 d D U P A 2
O1W O 0.51137(14) 0.30922(14) 0.66741(8) 0.0349(6) Uani 1 1 d . . . . .
O2W O 0.44587(14) 0.79738(14) 0.33332(8) 0.0317(6) Uani 1 1 d . . . . .
O3W O 0.5621(2) 0.85117(18) 0.33247(13) 0.0628(11) Uani 1 1 d . . . . .
O4W O 0.3721(4) 0.6865(4) 0.3337(3) 0.0371(18) Uani 0.3333 1 d . . P B -1
O5W O 0.3082(4) 0.6566(6) 0.4020(3) 0.036(2) Uani 0.3333 1 d . . P C -1
O6W O 0.3061(4) 0.6541(5) 0.2675(3) 0.043(2) Uani 0.3333 1 d . . P D -1
O7W O 0.3225(4) 0.4996(4) 0.6677(2) 0.0343(13) Uani 0.379(3) 1 d . U P E 1
O8W O 0.3697(4) 0.5300(3) 0.66508(18) 0.0344(12) Uani 0.431(3) 1 d . U P F 2
O9W O 0.4622(8) 0.5795(6) 0.6616(4) 0.0329(14) Uani 0.190(3) 1 d . U P G 3
O10W O 0.3230(6) 0.6290(5) 0.5884(4) 0.063(3) Uani 0.3333 1 d . U P H -1
O11W O 0.3275(9) 0.7137(7) 0.6349(7) 0.041(4) Uani 0.1667 1 d . U P I -1
N6 N 0.3122(7) 0.6862(7) 0.1686(4) 0.029(3) Uani 0.12 1 d D U P J -1
O61N O 0.3069(12) 0.6837(12) 0.1294(4) 0.031(4) Uani 0.12 1 d D U P J -1
O62N O 0.2745(11) 0.6444(10) 0.1905(8) 0.031(4) Uani 0.12 1 d D U P J -1
O63N O 0.3551(10) 0.7307(9) 0.1851(7) 0.027(4) Uani 0.12 1 d D U P J -1
N7 N 0.3755(8) 0.6791(8) 0.5021(6) 0.029(4) Uani 0.08 1 d D U P K -1
O71N O 0.3493(12) 0.7084(11) 0.4993(8) 0.028(4) Uani 0.08 1 d D U P K -1
O72N O 0.3672(13) 0.6408(12) 0.4748(8) 0.027(4) Uani 0.08 1 d D U P K -1
O73N O 0.4094(13) 0.6872(14) 0.5322(7) 0.033(4) Uani 0.08 1 d D U P K -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
Er1 O1M 2.354(3) . yes
Er1 O2M 2.314(3) . yes
Er1 O3M 2.320(3) . yes
Er1 O4M 2.378(3) . yes
Er1 O5M 2.362(3) . yes
Er1 O6M 2.334(3) . yes
Er1 O7M 2.371(3) . yes
Er1 O8M 2.307(3) . yes
O11 C11 1.237(4) . ?
O12 C12 1.235(4) . ?
C11 N11 1.356(5) . ?
C11 N12 1.364(4) . ?
C12 N13 1.364(4) . ?
C12 N14 1.363(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.557(4) . ?
C13 N11 1.447(4) . ?
C13 N14 1.446(4) . ?
C14 H14 1.0000 . ?
C14 N12 1.448(4) . ?
C14 N13 1.448(4) . ?
N11 C25 1.443(4) 3_565 ?
N12 C15 1.440(4) . ?
N13 C16 1.451(4) . ?
N14 C26 1.455(4) 3_565 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.449(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.441(4) . ?
O21 C21 1.238(4) . ?
O22 C22 1.224(4) . ?
C21 N21 1.372(4) . ?
C21 N22 1.358(5) . ?
C22 N23 1.368(4) . ?
C22 N24 1.362(4) . ?
C23 H23 1.0000 . ?
C23 C24 1.556(5) . ?
C23 N21 1.458(4) . ?
C23 N24 1.449(4) . ?
C24 H24 1.0000 . ?
C24 N22 1.448(4) . ?
C24 N23 1.448(4) . ?
N22 C25 1.454(4) . ?
N23 C26 1.447(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O31 C31 1.236(4) . ?
O32 C32 1.234(4) . ?
C31 N31 1.365(5) . ?
C31 N32 1.352(4) . ?
C32 N33 1.365(5) . ?
C32 N34 1.365(4) . ?
C33 H33 1.0000 . ?
C33 C34 1.546(5) . ?
C33 N31 1.448(4) . ?
C33 N34 1.451(4) . ?
C34 H34 1.0000 . ?
C34 N32 1.455(4) . ?
C34 N33 1.449(4) . ?
N31 C36 1.449(4) 14_455 ?
N32 C35 1.443(4) . ?
N33 C36 1.441(4) . ?
N34 C35 1.454(4) 14_455 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.267(4) . ?
N1 O12N 1.254(4) . ?
N1 O13N 1.224(4) . ?
N2 O21N 1.249(4) . ?
N2 O22N 1.243(4) . ?
N2 O23N 1.242(4) . ?
N3 O31N 1.256(4) . ?
N3 O32N 1.249(4) . ?
N3 O33N 1.237(4) . ?
N4 O41N 1.250(7) . ?
N4 O41' 1.265(6) . ?
N4 O42N 1.266(6) . ?
N4 O43N 1.243(6) . ?
N5 O51N 1.259(7) . ?
N5 O52N 1.253(7) . ?
N5 O53N 1.252(7) . ?
N6 O61N 1.250(7) . ?
N6 O62N 1.242(7) . ?
N6 O63N 1.245(7) . ?
N7 O71N 1.244(7) . ?
N7 O72N 1.248(7) . ?
N7 O73N 1.241(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1M Er1 O4M 133.61(12) . . ?
O1M Er1 O5M 71.63(11) . . ?
O1M Er1 O7M 128.99(11) . . ?
O2M Er1 O1M 76.01(10) . . ?
O2M Er1 O3M 89.57(11) . . ?
O2M Er1 O4M 69.94(10) . . ?
O2M Er1 O5M 75.28(10) . . ?
O2M Er1 O6M 145.63(10) . . ?
O2M Er1 O7M 143.67(10) . . ?
O3M Er1 O1M 73.38(13) . . ?
O3M Er1 O4M 75.77(11) . . ?
O3M Er1 O5M 144.27(11) . . ?
O3M Er1 O6M 97.12(11) . . ?
O3M Er1 O7M 76.49(12) . . ?
O5M Er1 O4M 125.81(11) . . ?
O5M Er1 O7M 133.08(10) . . ?
O6M Er1 O1M 73.78(10) . . ?
O6M Er1 O4M 144.36(10) . . ?
O6M Er1 O5M 79.94(10) . . ?
O6M Er1 O7M 70.27(10) . . ?
O7M Er1 O4M 74.13(10) . . ?
O8M Er1 O1M 142.77(12) . . ?
O8M Er1 O2M 101.69(12) . . ?
O8M Er1 O3M 143.65(11) . . ?
O8M Er1 O4M 75.98(12) . . ?
O8M Er1 O5M 71.92(10) . . ?
O8M Er1 O6M 92.68(12) . . ?
O8M Er1 O7M 74.13(12) . . ?
O11 C11 N11 126.0(3) . . ?
O11 C11 N12 125.3(3) . . ?
N11 C11 N12 108.7(3) . . ?
O12 C12 N13 125.3(3) . . ?
O12 C12 N14 126.3(3) . . ?
N14 C12 N13 108.4(3) . . ?
C14 C13 H13 111.8 . . ?
N11 C13 H13 111.8 . . ?
N11 C13 C14 103.2(3) . . ?
N14 C13 H13 111.8 . . ?
N14 C13 C14 103.0(3) . . ?
N14 C13 N11 114.5(3) . . ?
C13 C14 H14 112.0 . . ?
N12 C14 C13 102.9(3) . . ?
N12 C14 H14 112.0 . . ?
N13 C14 C13 103.1(3) . . ?
N13 C14 H14 112.0 . . ?
N13 C14 N12 114.3(3) . . ?
C11 N11 C13 112.7(3) . . ?
C11 N11 C25 123.8(3) . 3_565 ?
C25 N11 C13 123.4(3) 3_565 . ?
C11 N12 C14 112.6(3) . . ?
C11 N12 C15 123.6(3) . . ?
C15 N12 C14 123.5(3) . . ?
C12 N13 C14 112.6(3) . . ?
C12 N13 C16 123.0(3) . . ?
C14 N13 C16 122.4(3) . . ?
C12 N14 C13 112.8(3) . . ?
C12 N14 C26 123.1(3) . 3_565 ?
C13 N14 C26 122.1(3) . 3_565 ?
N12 C15 H15A 108.8 . . ?
N12 C15 H15B 108.8 . . ?
N12 C15 N21 114.0(3) . . ?
H15A C15 H15B 107.6 . . ?
N21 C15 H15A 108.8 . . ?
N21 C15 H15B 108.8 . . ?
N13 C16 H16A 108.8 . . ?
N13 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N24 C16 N13 113.7(3) . . ?
N24 C16 H16A 108.8 . . ?
N24 C16 H16B 108.8 . . ?
O21 C21 N21 125.2(3) . . ?
O21 C21 N22 125.7(3) . . ?
N22 C21 N21 109.1(3) . . ?
O22 C22 N23 124.6(3) . . ?
O22 C22 N24 126.8(3) . . ?
N24 C22 N23 108.6(3) . . ?
C24 C23 H23 111.7 . . ?
N21 C23 H23 111.7 . . ?
N21 C23 C24 103.5(3) . . ?
N24 C23 H23 111.7 . . ?
N24 C23 C24 103.5(3) . . ?
N24 C23 N21 114.2(3) . . ?
C23 C24 H24 111.8 . . ?
N22 C24 C23 103.1(3) . . ?
N22 C24 H24 111.8 . . ?
N23 C24 C23 102.9(3) . . ?
N23 C24 H24 111.8 . . ?
N23 C24 N22 114.8(3) . . ?
C15 N21 C23 123.6(3) . . ?
C21 N21 C15 122.4(3) . . ?
C21 N21 C23 111.4(3) . . ?
C21 N22 C24 112.6(3) . . ?
C21 N22 C25 122.9(3) . . ?
C24 N22 C25 123.3(3) . . ?
C22 N23 C24 112.7(3) . . ?
C22 N23 C26 123.0(3) . . ?
C26 N23 C24 124.3(3) . . ?
C16 N24 C23 123.8(3) . . ?
C22 N24 C16 123.8(3) . . ?
C22 N24 C23 112.3(3) . . ?
N11 C25 N22 113.7(3) 2_665 . ?
N11 C25 H25A 108.8 2_665 . ?
N11 C25 H25B 108.8 2_665 . ?
N22 C25 H25A 108.8 . . ?
N22 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N14 C26 H26A 108.8 2_665 . ?
N14 C26 H26B 108.8 2_665 . ?
N23 C26 N14 113.8(3) . 2_665 ?
N23 C26 H26A 108.8 . . ?
N23 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
O31 C31 N31 126.6(3) . . ?
O31 C31 N32 124.7(3) . . ?
N32 C31 N31 108.7(3) . . ?
O32 C32 N33 125.0(3) . . ?
O32 C32 N34 126.1(3) . . ?
N34 C32 N33 108.9(3) . . ?
C34 C33 H33 111.5 . . ?
N31 C33 H33 111.5 . . ?
N31 C33 C34 103.6(3) . . ?
N31 C33 N34 114.7(3) . . ?
N34 C33 H33 111.5 . . ?
N34 C33 C34 103.7(3) . . ?
C33 C34 H34 111.9 . . ?
N32 C34 C33 102.8(3) . . ?
N32 C34 H34 111.9 . . ?
N33 C34 C33 103.2(3) . . ?
N33 C34 H34 111.9 . . ?
N33 C34 N32 114.5(3) . . ?
C31 N31 C33 112.2(3) . . ?
C31 N31 C36 124.3(3) . 14_455 ?
C33 N31 C36 123.5(3) . 14_455 ?
C31 N32 C34 112.8(3) . . ?
C31 N32 C35 123.7(3) . . ?
C35 N32 C34 123.5(3) . . ?
C32 N33 C34 112.2(3) . . ?
C32 N33 C36 122.6(3) . . ?
C36 N33 C34 122.1(3) . . ?
C32 N34 C33 111.8(3) . . ?
C32 N34 C35 122.8(3) . 14_455 ?
C33 N34 C35 122.5(3) . 14_455 ?
N32 C35 N34 113.8(3) . 15 ?
N32 C35 H35A 108.8 . . ?
N32 C35 H35B 108.8 . . ?
N34 C35 H35A 108.8 15 . ?
N34 C35 H35B 108.8 15 . ?
H35A C35 H35B 107.7 . . ?
N31 C36 H36A 108.7 15 . ?
N31 C36 H36B 108.7 15 . ?
N33 C36 N31 114.1(3) . 15 ?
N33 C36 H36A 108.7 . . ?
N33 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
O12N N1 O11N 120.0(3) . . ?
O13N N1 O11N 119.9(3) . . ?
O13N N1 O12N 119.9(3) . . ?
O22N N2 O21N 119.0(3) . . ?
O23N N2 O21N 119.7(3) . . ?
O23N N2 O22N 121.2(3) . . ?
O32N N3 O31N 120.5(3) . . ?
O33N N3 O31N 120.3(3) . . ?
O33N N3 O32N 119.2(3) . . ?
O41N N4 O41' 48.0(8) . . ?
O41N N4 O42N 116.4(7) . . ?
O41' N4 O42N 116.3(6) . . ?
O43N N4 O41N 117.1(9) . . ?
O43N N4 O41' 119.9(6) . . ?
O43N N4 O42N 119.4(6) . . ?
O52N N5 O51N 118.3(9) . . ?
O53N N5 O51N 123.1(13) . . ?
O53N N5 O52N 118.5(9) . . ?
O62N N6 O61N 119.6(7) . . ?
O62N N6 O63N 121.1(7) . . ?
O63N N6 O61N 119.3(7) . . ?
O71N N7 O72N 120.2(7) . . ?
O73N N7 O71N 120.1(7) . . ?
O73N N7 O72N 119.7(7) . . ?

_refine_diff_density_max         1.078
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.102



####################################################################### 
# 
# 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_km774-4
_database_code_depnum_ccdc_archive 'CCDC 2247481'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_km774-4             
;
PROBLEM: Short Inter D...A Contact  O1M      ..O9W      .       2.51 Ang.
RESPONSE: Hydrogen bonds
;
_vrf_PLAT043_km774-4             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      56.48 Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT306_km774-4             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT430_km774-4_2           
;
PROBLEM: Short Inter D...A Contact  O1M      ..O8W      .       2.68 Ang.
RESPONSE: Hydrogen bonds
;
# Added during the CSD deposition process: Thursday 09 March 2023 03:57 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H92 Ho2 N32 O63'
_chemical_formula_weight         2311.27

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.8703(6)
_cell_length_b                   25.8703(6)
_cell_length_c                   31.8766(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18475.9(10)
_cell_formula_units_Z            9
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    22747
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.44

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_F_000             10530
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.053
_shelx_estimated_absorpt_T_min   0.607
_shelx_estimated_absorpt_T_max   0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6
_diffrn_reflns_number            45645
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.222
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9787
_reflns_number_gt                8785
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0521P)²+64.8100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9787
_refine_ls_number_parameters     770
_refine_ls_number_restraints     394
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0882
_refine_ls_wR_factor_gt          0.0858
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.073
_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
Ho1 Ho 0.38180(2) 0.36649(2) 0.66391(2) 0.02164(5) Uani 1 1 d . . . . .
O1M O 0.43058(12) 0.47140(11) 0.67004(8) 0.0459(6) Uani 1 1 d . . . . .
O2M O 0.41147(10) 0.40070(10) 0.59561(6) 0.0352(5) Uani 1 1 d . . . . .
O3M O 0.30797(12) 0.39274(14) 0.65937(9) 0.0511(7) Uani 1 1 d . . . . .
O4M O 0.31192(11) 0.29657(12) 0.61486(8) 0.0422(6) Uani 1 1 d . . . . .
O5M O 0.48647(10) 0.40405(11) 0.66338(8) 0.0398(5) Uani 1 1 d . . . . .
O6M O 0.40358(10) 0.38861(11) 0.73558(6) 0.0358(5) Uani 1 1 d . . . . .
O7M O 0.30275(10) 0.29231(11) 0.70504(7) 0.0404(5) Uani 1 1 d . . . . .
O8M O 0.39806(12) 0.28643(11) 0.66693(10) 0.0499(7) Uani 1 1 d . . . . .
O11 O 0.49041(11) 0.74877(10) 0.59556(6) 0.0356(5) Uani 1 1 d . . . . .
O12 O 0.47871(10) 0.74453(10) 0.40633(6) 0.0312(5) Uani 1 1 d . . . . .
C11 C 0.51328(13) 0.76134(13) 0.56029(8) 0.0247(5) Uani 1 1 d . . . . .
C12 C 0.50588(12) 0.75854(12) 0.43991(8) 0.0222(5) Uani 1 1 d . . . . .
C13 C 0.56005(12) 0.75756(11) 0.49852(8) 0.0205(5) Uani 1 1 d . . . . .
H13 H 0.602200 0.766089 0.496861 0.025 Uiso 1 1 calc R U . . .
C14 C 0.55650(12) 0.81570(12) 0.49886(8) 0.0198(5) Uani 1 1 d . . . . .
H14 H 0.596959 0.852201 0.497834 0.024 Uiso 1 1 calc R U . . .
N11 N 0.53189(11) 0.72906(10) 0.53780(7) 0.0247(5) Uani 1 1 d . . . . .
N12 N 0.52591(11) 0.81138(10) 0.53805(7) 0.0226(5) Uani 1 1 d . . . . .
N13 N 0.52174(11) 0.80986(10) 0.46169(7) 0.0218(4) Uani 1 1 d . . . . .
N14 N 0.52589(11) 0.72643(10) 0.46147(7) 0.0220(5) Uani 1 1 d . . . . .
C15 C 0.51648(13) 0.85834(13) 0.55414(8) 0.0243(5) Uani 1 1 d . . . . .
H15A H 0.552810 0.897298 0.548873 0.029 Uiso 1 1 calc R U . . .
H15B H 0.510730 0.853466 0.584892 0.029 Uiso 1 1 calc R U . . .
C16 C 0.51823(12) 0.85949(12) 0.44370(8) 0.0198(5) Uani 1 1 d . . . . .
H16A H 0.555776 0.896940 0.449901 0.024 Uiso 1 1 calc R U . . .
H16B H 0.514834 0.854672 0.412836 0.024 Uiso 1 1 calc R U . . .
O21 O 0.40162(11) 0.81670(12) 0.59215(6) 0.0383(5) Uani 1 1 d . . . . .
O22 O 0.40484(9) 0.82272(9) 0.40234(6) 0.0256(4) Uani 1 1 d . . . . .
C21 C 0.41416(13) 0.84216(13) 0.55777(8) 0.0251(6) Uani 1 1 d . . . . .
C22 C 0.41722(12) 0.84709(11) 0.43697(8) 0.0197(5) Uani 1 1 d . . . . .
C23 C 0.46927(11) 0.89351(11) 0.49847(8) 0.0188(5) Uani 1 1 d . . . . .
H23 H 0.503777 0.935209 0.499969 0.023 Uiso 1 1 calc R U . . .
C24 C 0.40862(11) 0.89239(12) 0.49836(8) 0.0192(5) Uani 1 1 d . . . . .
H24 H 0.414221 0.933519 0.499343 0.023 Uiso 1 1 calc R U . . .
N21 N 0.46563(10) 0.85928(11) 0.53578(7) 0.0224(5) Uani 1 1 d . . . . .
N22 N 0.37925(10) 0.85836(11) 0.53588(7) 0.0228(5) Uani 1 1 d . . . . .
N23 N 0.38154(10) 0.86222(10) 0.45911(7) 0.0199(4) Uani 1 1 d . . . . .
N24 N 0.46854(10) 0.86489(10) 0.45910(7) 0.0202(4) Uani 1 1 d . . . . .
C25 C 0.32520(12) 0.85387(13) 0.55325(9) 0.0259(6) Uani 1 1 d . . . . .
H25A H 0.326351 0.851183 0.584180 0.031 Uiso 1 1 calc R U . . .
H25B H 0.324306 0.890729 0.546363 0.031 Uiso 1 1 calc R U . . .
C26 C 0.32473(11) 0.85197(12) 0.44371(8) 0.0208(5) Uani 1 1 d . . . . .
H26A H 0.323868 0.847553 0.412826 0.025 Uiso 1 1 calc R U . . .
H26B H 0.321038 0.887454 0.450052 0.025 Uiso 1 1 calc R U . . .
O31 O 0.40767(10) 0.82582(10) 0.26448(6) 0.0301(4) Uani 1 1 d . . . . .
O32 O 0.40143(9) 0.81095(10) 0.07518(6) 0.0304(5) Uani 1 1 d . . . . .
C31 C 0.41933(12) 0.84873(12) 0.22932(8) 0.0223(5) Uani 1 1 d . . . . .
C32 C 0.41456(12) 0.83797(12) 0.10867(8) 0.0221(5) Uani 1 1 d . . . . .
C33 C 0.47047(12) 0.89274(12) 0.16683(8) 0.0205(5) Uani 1 1 d . . . . .
H33 H 0.504668 0.934531 0.164641 0.025 Uiso 1 1 calc R U . . .
C34 C 0.40964(12) 0.89100(12) 0.16686(8) 0.0209(5) Uani 1 1 d . . . . .
H34 H 0.414766 0.931852 0.164507 0.025 Uiso 1 1 calc R U . . .
N31 N 0.47045(11) 0.86579(11) 0.20691(7) 0.0230(5) Uani 1 1 d . . . . .
N32 N 0.38371(10) 0.86327(10) 0.20680(7) 0.0217(4) Uani 1 1 d . . . . .
N33 N 0.37943(10) 0.85442(11) 0.13048(7) 0.0216(4) Uani 1 1 d . . . . .
N34 N 0.46684(10) 0.85752(10) 0.13033(7) 0.0224(5) Uani 1 1 d . . . . .
C35 C 0.32627(12) 0.85238(12) 0.22137(8) 0.0218(5) Uani 1 1 d . . . . .
H35A H 0.322501 0.887803 0.214969 0.026 Uiso 1 1 calc R U . . .
H35B H 0.324559 0.847551 0.252239 0.026 Uiso 1 1 calc R U . . .
C36 C 0.32763(12) 0.85261(12) 0.11180(8) 0.0228(5) Uani 1 1 d . . . . .
H36A H 0.329792 0.849420 0.080976 0.027 Uiso 1 1 calc R U . . .
H36B H 0.328756 0.890687 0.117898 0.027 Uiso 1 1 calc R U . . .
N1 N 0.54222(11) 0.53568(11) 0.58778(7) 0.0270(5) Uani 1 1 d . . . . .
O11N O 0.55376(11) 0.51271(11) 0.61844(7) 0.0404(6) Uani 1 1 d . . . . .
O12N O 0.49565(11) 0.50568(11) 0.56678(8) 0.0448(6) Uani 1 1 d . . . . .
O13N O 0.57922(11) 0.58673(10) 0.57617(8) 0.0395(5) Uani 1 1 d . . . . .
N2 N 0.53683(11) 0.53463(11) 0.75175(8) 0.0281(5) Uani 1 1 d . . . . .
O21N O 0.53817(15) 0.53106(14) 0.71262(8) 0.0728(11) Uani 1 1 d . . . . .
O22N O 0.57825(10) 0.57757(9) 0.77012(7) 0.0314(5) Uani 1 1 d . . . . .
O23N O 0.49380(10) 0.49445(10) 0.77169(7) 0.0335(5) Uani 1 1 d . . . . .
N3 N 0.33716(11) 0.33483(10) 0.49554(7) 0.0248(5) Uani 1 1 d . . . . .
O31N O 0.36592(11) 0.38167(10) 0.51646(7) 0.0348(5) Uani 1 1 d . . . . .
O32N O 0.30482(10) 0.33268(11) 0.46589(7) 0.0359(5) Uani 1 1 d . . . . .
O33N O 0.34112(14) 0.29039(12) 0.50428(12) 0.0618(9) Uani 1 1 d . . . . .
N4 N 0.3271(3) 0.1666(2) 0.59327(15) 0.0457(13) Uani 0.585(6) 1 d D U P A 1
O41N O 0.2897(5) 0.1456(4) 0.6219(3) 0.063(2) Uani 0.292(3) 1 d D U P A 1
O41' O 0.3333(5) 0.1711(4) 0.63282(18) 0.0444(17) Uani 0.292(3) 1 d D U P A 1
O42N O 0.3416(3) 0.1320(3) 0.57585(18) 0.0708(17) Uani 0.585(6) 1 d D U P A 1
O43N O 0.3292(3) 0.2084(3) 0.57283(19) 0.0503(16) Uani 0.585(6) 1 d D U P A 1
N5 N 0.3430(5) 0.1695(5) 0.5930(4) 0.056(3) Uani 0.215(6) 1 d D U P A 2
O51N O 0.3901(6) 0.1976(5) 0.6142(4) 0.050(2) Uani 0.215(6) 1 d D U P A 2
O52N O 0.3190(8) 0.1978(8) 0.5793(7) 0.056(3) Uani 0.215(6) 1 d D U P A 2
O53N O 0.3183(8) 0.1150(5) 0.5854(5) 0.061(3) Uani 0.215(6) 1 d D U P A 2
O1W O 0.51174(11) 0.30976(11) 0.66728(6) 0.0364(5) Uani 1 1 d . . . . .
O2W O 0.44581(11) 0.79761(11) 0.33329(6) 0.0354(5) Uani 1 1 d . . . . .
O3W O 0.56188(17) 0.85086(15) 0.33242(11) 0.0681(9) Uani 1 1 d . . . . .
O4W O 0.3720(3) 0.6861(3) 0.3335(2) 0.0385(16) Uani 0.3333 1 d . . P B -1
O5W O 0.3078(3) 0.6561(5) 0.4022(2) 0.0456(19) Uani 0.3333 1 d . . P C -1
O6W O 0.3053(4) 0.6537(5) 0.2665(2) 0.050(2) Uani 0.3333 1 d . . P D -1
O7W O 0.3210(4) 0.4983(4) 0.66702(17) 0.0405(16) Uani 0.358(3) 1 d . U P E 1
O8W O 0.3692(3) 0.5295(3) 0.66470(15) 0.0426(13) Uani 0.443(3) 1 d . U P F 2
O9W O 0.4607(4) 0.5795(4) 0.6618(3) 0.022(2) Uani 0.199(3) 1 d . U P G 3
O10W O 0.3222(6) 0.6287(5) 0.5900(4) 0.084(3) Uani 0.3333 1 d . U P H -1
O11W O 0.3296(9) 0.7143(8) 0.6328(7) 0.063(5) Uani 0.1667 1 d . U P I -1
N6 N 0.3102(7) 0.6866(7) 0.1688(4) 0.048(4) Uani 0.12 1 d D U P J -1
O61N O 0.3076(14) 0.6868(13) 0.1297(4) 0.050(5) Uani 0.12 1 d D U P J -1
O62N O 0.2702(12) 0.6442(11) 0.1888(10) 0.048(5) Uani 0.12 1 d D U P J -1
O63N O 0.3524(11) 0.7291(11) 0.1872(9) 0.046(5) Uani 0.12 1 d D U P J -1
N7 N 0.3713(8) 0.6818(8) 0.5009(6) 0.044(4) Uani 0.08 1 d D U P K -1
O71N O 0.3449(13) 0.7105(11) 0.4967(8) 0.044(4) Uani 0.08 1 d D U P K -1
O72N O 0.3636(13) 0.6425(11) 0.4750(8) 0.043(4) Uani 0.08 1 d D U P K -1
O73N O 0.4047(12) 0.6916(13) 0.5312(7) 0.046(4) Uani 0.08 1 d D U P K -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
Ho1 O1M 2.360(3) . yes
Ho1 O2M 2.331(2) . yes
Ho1 O3M 2.330(3) . yes
Ho1 O4M 2.391(2) . yes
Ho1 O5M 2.376(2) . yes
Ho1 O6M 2.354(2) . yes
Ho1 O7M 2.379(2) . yes
Ho1 O8M 2.312(2) . yes
O11 C11 1.236(3) . ?
O12 C12 1.231(3) . ?
C11 N11 1.359(4) . ?
C11 N12 1.365(4) . ?
C12 N13 1.367(3) . ?
C12 N14 1.364(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.552(4) . ?
C13 N11 1.451(3) . ?
C13 N14 1.454(3) . ?
C14 H14 1.0000 . ?
C14 N12 1.453(3) . ?
C14 N13 1.449(3) . ?
N11 C25 1.450(3) 3_565 ?
N12 C15 1.447(3) . ?
N13 C16 1.450(3) . ?
N14 C26 1.456(3) 3_565 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.451(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.447(3) . ?
O21 C21 1.235(3) . ?
O22 C22 1.232(3) . ?
C21 N21 1.368(4) . ?
C21 N22 1.363(4) . ?
C22 N23 1.366(3) . ?
C22 N24 1.364(3) . ?
C23 H23 1.0000 . ?
C23 C24 1.555(4) . ?
C23 N21 1.457(3) . ?
C23 N24 1.452(3) . ?
C24 H24 1.0000 . ?
C24 N22 1.454(3) . ?
C24 N23 1.455(3) . ?
N22 C25 1.453(3) . ?
N23 C26 1.443(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O31 C31 1.233(3) . ?
O32 C32 1.227(3) . ?
C31 N31 1.367(4) . ?
C31 N32 1.361(3) . ?
C32 N33 1.370(4) . ?
C32 N34 1.370(3) . ?
C33 H33 1.0000 . ?
C33 C34 1.552(4) . ?
C33 N31 1.455(3) . ?
C33 N34 1.451(3) . ?
C34 H34 1.0000 . ?
C34 N32 1.451(3) . ?
C34 N33 1.453(3) . ?
N31 C36 1.447(3) 14_455 ?
N32 C35 1.444(3) . ?
N33 C36 1.446(3) . ?
N34 C35 1.450(3) 14_455 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.255(3) . ?
N1 O12N 1.252(3) . ?
N1 O13N 1.238(3) . ?
N2 O21N 1.253(3) . ?
N2 O22N 1.239(3) . ?
N2 O23N 1.251(3) . ?
N3 O31N 1.251(3) . ?
N3 O32N 1.245(3) . ?
N3 O33N 1.236(3) . ?
N4 O41N 1.240(6) . ?
N4 O41' 1.269(6) . ?
N4 O42N 1.259(6) . ?
N4 O43N 1.239(5) . ?
N5 O51N 1.260(7) . ?
N5 O52N 1.251(7) . ?
N5 O53N 1.247(7) . ?
N6 O61N 1.247(7) . ?
N6 O62N 1.242(7) . ?
N6 O63N 1.243(7) . ?
N7 O71N 1.241(7) . ?
N7 O72N 1.247(7) . ?
N7 O73N 1.236(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1M Ho1 O4M 133.74(9) . . yes
O1M Ho1 O5M 71.68(10) . . yes
O1M Ho1 O7M 129.18(9) . . yes
O2M Ho1 O1M 75.85(8) . . yes
O2M Ho1 O4M 69.95(8) . . yes
O2M Ho1 O5M 75.31(8) . . yes
O2M Ho1 O6M 145.17(8) . . yes
O2M Ho1 O7M 143.91(8) . . yes
O3M Ho1 O1M 73.44(10) . . yes
O3M Ho1 O2M 89.63(10) . . yes
O3M Ho1 O4M 76.11(10) . . yes
O3M Ho1 O5M 144.41(10) . . yes
O3M Ho1 O6M 96.95(9) . . yes
O3M Ho1 O7M 76.70(10) . . yes
O5M Ho1 O4M 125.50(9) . . yes
O5M Ho1 O7M 132.69(9) . . yes
O6M Ho1 O1M 73.43(9) . . yes
O6M Ho1 O4M 144.81(8) . . yes
O6M Ho1 O5M 79.76(8) . . yes
O6M Ho1 O7M 70.49(8) . . yes
O7M Ho1 O4M 74.35(8) . . yes
O8M Ho1 O1M 142.59(10) . . yes
O8M Ho1 O2M 101.89(10) . . yes
O8M Ho1 O3M 143.75(10) . . yes
O8M Ho1 O4M 75.93(10) . . yes
O8M Ho1 O5M 71.70(9) . . yes
O8M Ho1 O6M 92.79(10) . . yes
O8M Ho1 O7M 73.89(10) . . yes
O11 C11 N11 126.0(3) . . ?
O11 C11 N12 125.3(3) . . ?
N11 C11 N12 108.6(2) . . ?
O12 C12 N13 125.3(2) . . ?
O12 C12 N14 126.4(3) . . ?
N14 C12 N13 108.3(2) . . ?
C14 C13 H13 111.9 . . ?
N11 C13 H13 111.9 . . ?
N11 C13 C14 103.2(2) . . ?
N11 C13 N14 114.1(2) . . ?
N14 C13 H13 111.9 . . ?
N14 C13 C14 103.2(2) . . ?
C13 C14 H14 111.9 . . ?
N12 C14 C13 103.0(2) . . ?
N12 C14 H14 111.9 . . ?
N13 C14 C13 103.2(2) . . ?
N13 C14 H14 111.9 . . ?
N13 C14 N12 114.2(2) . . ?
C11 N11 C13 112.7(2) . . ?
C11 N11 C25 123.3(2) . 3_565 ?
C25 N11 C13 123.8(2) 3_565 . ?
C11 N12 C14 112.5(2) . . ?
C11 N12 C15 123.4(2) . . ?
C15 N12 C14 123.6(2) . . ?
C12 N13 C14 112.7(2) . . ?
C12 N13 C16 122.6(2) . . ?
C14 N13 C16 122.8(2) . . ?
C12 N14 C13 112.5(2) . . ?
C12 N14 C26 123.1(2) . 3_565 ?
C13 N14 C26 122.4(2) . 3_565 ?
N12 C15 H15A 108.8 . . ?
N12 C15 H15B 108.8 . . ?
N12 C15 N21 113.9(2) . . ?
H15A C15 H15B 107.7 . . ?
N21 C15 H15A 108.8 . . ?
N21 C15 H15B 108.8 . . ?
N13 C16 H16A 108.8 . . ?
N13 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N24 C16 N13 113.8(2) . . ?
N24 C16 H16A 108.8 . . ?
N24 C16 H16B 108.8 . . ?
O21 C21 N21 125.5(3) . . ?
O21 C21 N22 125.5(3) . . ?
N22 C21 N21 109.0(2) . . ?
O22 C22 N23 124.8(2) . . ?
O22 C22 N24 126.6(2) . . ?
N24 C22 N23 108.6(2) . . ?
C24 C23 H23 111.6 . . ?
N21 C23 H23 111.6 . . ?
N21 C23 C24 103.4(2) . . ?
N24 C23 H23 111.6 . . ?
N24 C23 C24 103.4(2) . . ?
N24 C23 N21 114.5(2) . . ?
C23 C24 H24 111.9 . . ?
N22 C24 C23 103.1(2) . . ?
N22 C24 H24 111.9 . . ?
N22 C24 N23 114.6(2) . . ?
N23 C24 C23 102.9(2) . . ?
N23 C24 H24 111.9 . . ?
C15 N21 C23 123.7(2) . . ?
C21 N21 C15 122.1(2) . . ?
C21 N21 C23 111.8(2) . . ?
C21 N22 C24 112.4(2) . . ?
C21 N22 C25 122.7(2) . . ?
C25 N22 C24 123.5(2) . . ?
C22 N23 C24 112.6(2) . . ?
C22 N23 C26 122.9(2) . . ?
C26 N23 C24 124.3(2) . . ?
C16 N24 C23 123.8(2) . . ?
C22 N24 C16 123.6(2) . . ?
C22 N24 C23 112.4(2) . . ?
N11 C25 N22 113.5(2) 2_665 . ?
N11 C25 H25A 108.9 2_665 . ?
N11 C25 H25B 108.9 2_665 . ?
N22 C25 H25A 108.9 . . ?
N22 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
N14 C26 H26A 108.8 2_665 . ?
N14 C26 H26B 108.8 2_665 . ?
N23 C26 N14 114.0(2) . 2_665 ?
N23 C26 H26A 108.8 . . ?
N23 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
O31 C31 N31 126.5(3) . . ?
O31 C31 N32 125.1(3) . . ?
N32 C31 N31 108.3(2) . . ?
O32 C32 N33 125.5(3) . . ?
O32 C32 N34 126.1(3) . . ?
N33 C32 N34 108.4(2) . . ?
C34 C33 H33 111.6 . . ?
N31 C33 H33 111.6 . . ?
N31 C33 C34 103.2(2) . . ?
N34 C33 H33 111.6 . . ?
N34 C33 C34 103.6(2) . . ?
N34 C33 N31 114.7(2) . . ?
C33 C34 H34 111.9 . . ?
N32 C34 C33 103.1(2) . . ?
N32 C34 H34 111.9 . . ?
N32 C34 N33 114.4(2) . . ?
N33 C34 C33 103.0(2) . . ?
N33 C34 H34 111.9 . . ?
C31 N31 C33 112.5(2) . . ?
C31 N31 C36 123.8(2) . 14_455 ?
C36 N31 C33 123.7(2) 14_455 . ?
C31 N32 C34 113.0(2) . . ?
C31 N32 C35 123.3(2) . . ?
C35 N32 C34 123.7(2) . . ?
C32 N33 C34 112.5(2) . . ?
C32 N33 C36 121.9(2) . . ?
C36 N33 C34 122.5(2) . . ?
C32 N34 C33 112.2(2) . . ?
C32 N34 C35 122.7(2) . 14_455 ?
C35 N34 C33 122.4(2) 14_455 . ?
N32 C35 N34 114.1(2) . 15 ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
N34 C35 H35A 108.7 15 . ?
N34 C35 H35B 108.7 15 . ?
H35A C35 H35B 107.6 . . ?
N31 C36 H36A 108.7 15 . ?
N31 C36 H36B 108.7 15 . ?
N33 C36 N31 114.1(2) . 15 ?
N33 C36 H36A 108.7 . . ?
N33 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
O12N N1 O11N 120.4(3) . . ?
O13N N1 O11N 119.8(3) . . ?
O13N N1 O12N 119.5(2) . . ?
O22N N2 O21N 119.6(3) . . ?
O22N N2 O23N 121.1(2) . . ?
O23N N2 O21N 119.4(3) . . ?
O32N N3 O31N 120.6(3) . . ?
O33N N3 O31N 119.7(3) . . ?
O33N N3 O32N 119.7(3) . . ?
O41N N4 O41' 49.0(7) . . ?
O41N N4 O42N 117.2(6) . . ?
O42N N4 O41' 115.8(5) . . ?
O43N N4 O41N 116.9(8) . . ?
O43N N4 O41' 119.5(5) . . ?
O43N N4 O42N 119.3(5) . . ?
O52N N5 O51N 118.1(8) . . ?
O53N N5 O51N 123.9(12) . . ?
O53N N5 O52N 118.1(9) . . ?
O62N N6 O61N 119.5(7) . . ?
O62N N6 O63N 120.9(7) . . ?
O63N N6 O61N 119.5(7) . . ?
O71N N7 O72N 120.3(7) . . ?
O73N N7 O71N 119.9(7) . . ?
O73N N7 O72N 119.7(7) . . ?

_refine_diff_density_max         1.147
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.102



####################################################################### 
# 
# 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_km785-5
_database_code_depnum_ccdc_archive 'CCDC 2247483'
loop_
_audit_author_name
_audit_author_address
'Denis Samsonenko'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2023-03-09 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_km785-5             
;
PROBLEM: Short Inter D...A Contact  O1M      ..O9W      .       2.51 Ang.
RESPONSE: Hydrogen bonds
;
_vrf_PLAT043_km785-5             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      56.41 Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT306_km785-5             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check
RESPONSE: Hydrogen atoms of water molecules were not localized
;
_vrf_PLAT430_km785-5_2           
;
PROBLEM: Short Inter D...A Contact  O1M      ..O8W      .       2.66 Ang.
RESPONSE: Hydrogen bonds
;
# Added during the CSD deposition process: Thursday 09 March 2023 03:57 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H92 N32 O63 Yb2'
_chemical_formula_weight         2327.49

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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   25.7946(4)
_cell_length_b                   25.7946(4)
_cell_length_c                   31.7638(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18302.9(7)
_cell_formula_units_Z            9
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9222
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.66

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_F_000             10584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.426
_shelx_estimated_absorpt_T_min   0.793
_shelx_estimated_absorpt_T_max   0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7077
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?

_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_detector                 PIXEL
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 7.41
_diffrn_reflns_number            95542
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.573
_diffrn_reflns_theta_max         28.704
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10486
_reflns_number_gt                8714
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'APEX3 (Bruker-AXS, 2016)'
_computing_cell_refinement       'SAINT (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2016)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0544P)²+52.7150P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10486
_refine_ls_number_parameters     770
_refine_ls_number_restraints     388
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0923
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.090
_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
Yb1 Yb 0.38143(2) 0.36667(2) 0.66413(2) 0.02022(6) Uani 1 1 d . . . . .
O1M O 0.42977(14) 0.47059(13) 0.66975(9) 0.0431(7) Uani 1 1 d . . . . .
O2M O 0.41058(12) 0.40004(12) 0.59673(8) 0.0329(6) Uani 1 1 d . . . . .
O3M O 0.30831(14) 0.39248(15) 0.65996(11) 0.0479(8) Uani 1 1 d . . . . .
O4M O 0.31216(12) 0.29715(13) 0.61564(9) 0.0393(6) Uani 1 1 d . . . . .
O5M O 0.48493(11) 0.40390(13) 0.66380(9) 0.0386(7) Uani 1 1 d . . . . .
O6M O 0.40316(12) 0.38869(12) 0.73482(8) 0.0337(6) Uani 1 1 d . . . . .
O7M O 0.30312(12) 0.29369(12) 0.70492(9) 0.0383(6) Uani 1 1 d . . . . .
O8M O 0.39708(14) 0.28752(13) 0.66711(11) 0.0467(7) Uani 1 1 d . . . . .
O11 O 0.49076(13) 0.74887(12) 0.59586(8) 0.0347(6) Uani 1 1 d . . . . .
O12 O 0.47874(12) 0.74437(11) 0.40632(7) 0.0297(5) Uani 1 1 d . . . . .
C11 C 0.51355(16) 0.76146(15) 0.56047(10) 0.0238(7) Uani 1 1 d . . . . .
C12 C 0.50605(15) 0.75847(14) 0.43986(10) 0.0220(6) Uani 1 1 d . . . . .
C13 C 0.56058(14) 0.75753(13) 0.49852(9) 0.0192(6) Uani 1 1 d . . . . .
H13 H 0.602889 0.766197 0.496830 0.023 Uiso 1 1 calc R U . . .
C14 C 0.55661(14) 0.81570(14) 0.49888(10) 0.0194(6) Uani 1 1 d . . . . .
H14 H 0.597132 0.852384 0.497837 0.023 Uiso 1 1 calc R U . . .
N11 N 0.53232(13) 0.72914(12) 0.53797(8) 0.0234(6) Uani 1 1 d . . . . .
N12 N 0.52612(13) 0.81146(12) 0.53818(8) 0.0219(6) Uani 1 1 d . . . . .
N13 N 0.52196(13) 0.80997(12) 0.46174(8) 0.0209(5) Uani 1 1 d . . . . .
N14 N 0.52621(12) 0.72625(12) 0.46149(8) 0.0213(5) Uani 1 1 d . . . . .
C15 C 0.51680(15) 0.85837(15) 0.55429(10) 0.0225(6) Uani 1 1 d . . . . .
H15A H 0.553302 0.897412 0.549054 0.027 Uiso 1 1 calc R U . . .
H15B H 0.510984 0.853424 0.585142 0.027 Uiso 1 1 calc R U . . .
C16 C 0.51848(14) 0.85968(14) 0.44363(9) 0.0182(6) Uani 1 1 d . . . . .
H16A H 0.556152 0.897238 0.449815 0.022 Uiso 1 1 calc R U . . .
H16B H 0.515029 0.854766 0.412669 0.022 Uiso 1 1 calc R U . . .
O21 O 0.40168(12) 0.81691(14) 0.59234(7) 0.0377(6) Uani 1 1 d . . . . .
O22 O 0.40511(11) 0.82317(11) 0.40220(7) 0.0245(5) Uani 1 1 d . . . . .
C21 C 0.41423(15) 0.84244(16) 0.55788(10) 0.0255(7) Uani 1 1 d . . . . .
C22 C 0.41740(14) 0.84731(14) 0.43695(9) 0.0191(6) Uani 1 1 d . . . . .
C23 C 0.46973(14) 0.89407(14) 0.49854(9) 0.0182(6) Uani 1 1 d . . . . .
H23 H 0.504377 0.935876 0.500053 0.022 Uiso 1 1 calc R U . . .
C24 C 0.40889(14) 0.89277(14) 0.49840(9) 0.0186(6) Uani 1 1 d . . . . .
H24 H 0.414483 0.934011 0.499408 0.022 Uiso 1 1 calc R U . . .
N21 N 0.46582(12) 0.85955(12) 0.53584(8) 0.0214(5) Uani 1 1 d . . . . .
N22 N 0.37947(12) 0.85883(13) 0.53587(8) 0.0225(6) Uani 1 1 d . . . . .
N23 N 0.38185(11) 0.86279(12) 0.45916(8) 0.0184(5) Uani 1 1 d . . . . .
N24 N 0.46875(12) 0.86513(12) 0.45907(8) 0.0185(5) Uani 1 1 d . . . . .
C25 C 0.32523(14) 0.85438(16) 0.55323(10) 0.0259(7) Uani 1 1 d . . . . .
H25A H 0.326454 0.851943 0.584290 0.031 Uiso 1 1 calc R U . . .
H25B H 0.324295 0.891278 0.546158 0.031 Uiso 1 1 calc R U . . .
C26 C 0.32495(13) 0.85247(14) 0.44364(10) 0.0192(6) Uani 1 1 d . . . . .
H26A H 0.324124 0.847922 0.412660 0.023 Uiso 1 1 calc R U . . .
H26B H 0.321239 0.888066 0.449909 0.023 Uiso 1 1 calc R U . . .
O31 O 0.40837(11) 0.82629(12) 0.26476(7) 0.0284(5) Uani 1 1 d . . . . .
O32 O 0.40207(11) 0.81101(12) 0.07521(7) 0.0286(5) Uani 1 1 d . . . . .
C31 C 0.42044(15) 0.84944(14) 0.22949(10) 0.0212(6) Uani 1 1 d . . . . .
C32 C 0.41519(15) 0.83807(14) 0.10871(10) 0.0217(6) Uani 1 1 d . . . . .
C33 C 0.47150(14) 0.89317(14) 0.16682(10) 0.0202(6) Uani 1 1 d . . . . .
H33 H 0.505865 0.935041 0.164574 0.024 Uiso 1 1 calc R U . . .
C34 C 0.41042(14) 0.89133(14) 0.16680(10) 0.0198(6) Uani 1 1 d . . . . .
H34 H 0.415656 0.932322 0.164261 0.024 Uiso 1 1 calc R U . . .
N31 N 0.47118(12) 0.86600(12) 0.20703(8) 0.0213(5) Uani 1 1 d . . . . .
N32 N 0.38449(12) 0.86407(12) 0.20700(8) 0.0205(5) Uani 1 1 d . . . . .
N33 N 0.38006(12) 0.85464(12) 0.13043(8) 0.0206(5) Uani 1 1 d . . . . .
N34 N 0.46749(12) 0.85765(12) 0.13040(8) 0.0210(5) Uani 1 1 d . . . . .
C35 C 0.32686(14) 0.85313(14) 0.22133(10) 0.0205(6) Uani 1 1 d . . . . .
H35A H 0.323120 0.888636 0.214765 0.025 Uiso 1 1 calc R U . . .
H35B H 0.324974 0.848374 0.252315 0.025 Uiso 1 1 calc R U . . .
C36 C 0.32839(14) 0.85332(15) 0.11183(10) 0.0218(6) Uani 1 1 d . . . . .
H36A H 0.330593 0.850395 0.080876 0.026 Uiso 1 1 calc R U . . .
H36B H 0.329755 0.891562 0.118167 0.026 Uiso 1 1 calc R U . . .
N1 N 0.54161(13) 0.53531(13) 0.58772(9) 0.0257(6) Uani 1 1 d . . . . .
O11N O 0.55294(13) 0.51248(13) 0.61881(9) 0.0396(7) Uani 1 1 d . . . . .
O12N O 0.49485(12) 0.50471(13) 0.56687(9) 0.0417(7) Uani 1 1 d . . . . .
O13N O 0.57876(12) 0.58616(12) 0.57592(9) 0.0373(6) Uani 1 1 d . . . . .
N2 N 0.53693(13) 0.53472(13) 0.75101(9) 0.0262(6) Uani 1 1 d . . . . .
O21N O 0.53814(18) 0.53123(16) 0.71205(9) 0.0744(13) Uani 1 1 d . . . . .
O22N O 0.57844(11) 0.57787(11) 0.76948(8) 0.0287(5) Uani 1 1 d . . . . .
O23N O 0.49378(11) 0.49427(12) 0.77124(8) 0.0310(6) Uani 1 1 d . . . . .
N3 N 0.33686(12) 0.33431(12) 0.49558(9) 0.0232(6) Uani 1 1 d . . . . .
O31N O 0.36567(12) 0.38080(11) 0.51699(8) 0.0329(6) Uani 1 1 d . . . . .
O32N O 0.30504(12) 0.33309(12) 0.46598(8) 0.0336(6) Uani 1 1 d . . . . .
O33N O 0.34050(16) 0.28960(13) 0.50414(13) 0.0599(10) Uani 1 1 d . . . . .
N4 N 0.3282(4) 0.1670(3) 0.59422(18) 0.0452(16) Uani 0.541(6) 1 d D U P A 1
O41N O 0.2931(6) 0.1474(5) 0.6245(4) 0.065(3) Uani 0.271(3) 1 d D U P A 1
O41' O 0.3385(6) 0.1749(4) 0.6334(2) 0.0356(18) Uani 0.271(3) 1 d D U P A 1
O42N O 0.3409(4) 0.1311(3) 0.5764(2) 0.065(2) Uani 0.541(6) 1 d D U P A 1
O43N O 0.3294(4) 0.2081(4) 0.5731(2) 0.047(2) Uani 0.541(6) 1 d D U P A 1
N5 N 0.3430(5) 0.1704(5) 0.5933(3) 0.051(3) Uani 0.259(6) 1 d D U P A 2
O51N O 0.3903(5) 0.1980(5) 0.6146(4) 0.048(2) Uani 0.259(6) 1 d D U P A 2
O52N O 0.3199(8) 0.1996(7) 0.5796(6) 0.051(3) Uani 0.259(6) 1 d D U P A 2
O53N O 0.3169(8) 0.1155(5) 0.5857(5) 0.057(3) Uani 0.259(6) 1 d D U P A 2
O1W O 0.51145(13) 0.31003(13) 0.66730(8) 0.0369(6) Uani 1 1 d . . . . .
O2W O 0.44620(13) 0.79762(13) 0.33349(8) 0.0350(6) Uani 1 1 d . . . . .
O3W O 0.56283(19) 0.85150(17) 0.33286(12) 0.0635(10) Uani 1 1 d . . . . .
O4W O 0.3724(4) 0.6864(4) 0.3335(3) 0.0363(18) Uani 0.3333 1 d . . P B -1
O5W O 0.3086(4) 0.6561(6) 0.4016(3) 0.043(2) Uani 0.3333 1 d . . P C -1
O6W O 0.3064(4) 0.6544(5) 0.2670(3) 0.046(2) Uani 0.3333 1 d . . P D -1
O7W O 0.3202(4) 0.4975(4) 0.6668(2) 0.0350(14) Uani 0.363(3) 1 d . U P E 1
O8W O 0.3687(4) 0.5282(3) 0.66467(17) 0.0399(13) Uani 0.464(3) 1 d . U P F 2
O9W O 0.4602(8) 0.5790(7) 0.6620(4) 0.034(2) Uani 0.173(3) 1 d . U P G 3
O10W O 0.3229(7) 0.6294(5) 0.5900(4) 0.077(3) Uani 0.3333 1 d . U P H -1
O11W O 0.3303(9) 0.7158(8) 0.6337(7) 0.053(5) Uani 0.1667 1 d . U P I -1
N6 N 0.3096(7) 0.6866(8) 0.1691(4) 0.044(5) Uani 0.12 1 d D U P J -1
O61N O 0.3102(14) 0.6901(16) 0.1299(4) 0.044(5) Uani 0.12 1 d D U P J -1
O62N O 0.2677(11) 0.6427(13) 0.1868(10) 0.041(5) Uani 0.12 1 d D U P J -1
O63N O 0.3505(12) 0.7272(13) 0.1898(11) 0.043(6) Uani 0.12 1 d D U P J -1
N7 N 0.3742(8) 0.6805(8) 0.5016(6) 0.035(4) Uani 0.08 1 d D U P K -1
O71N O 0.3491(13) 0.7106(11) 0.4984(9) 0.035(4) Uani 0.08 1 d D U P K -1
O72N O 0.3653(14) 0.6415(12) 0.4749(8) 0.034(4) Uani 0.08 1 d D U P K -1
O73N O 0.4077(13) 0.6884(14) 0.5318(8) 0.039(4) Uani 0.08 1 d D U P K -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
Yb1 O1M 2.330(3) . yes
Yb1 O2M 2.290(2) . yes
Yb1 O3M 2.296(3) . yes
Yb1 O4M 2.362(3) . yes
Yb1 O5M 2.342(3) . yes
Yb1 O6M 2.315(2) . yes
Yb1 O7M 2.345(3) . yes
Yb1 O8M 2.273(3) . yes
O11 C11 1.235(4) . ?
O12 C12 1.228(4) . ?
C11 N11 1.358(4) . ?
C11 N12 1.361(4) . ?
C12 N13 1.368(4) . ?
C12 N14 1.366(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.554(4) . ?
C13 N11 1.451(4) . ?
C13 N14 1.451(4) . ?
C14 H14 1.0000 . ?
C14 N12 1.450(4) . ?
C14 N13 1.442(4) . ?
N11 C25 1.447(4) 3_565 ?
N12 C15 1.441(4) . ?
N13 C16 1.448(4) . ?
N14 C26 1.453(4) 3_565 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N21 1.454(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N24 1.444(4) . ?
O21 C21 1.234(4) . ?
O22 C22 1.229(4) . ?
C21 N21 1.367(4) . ?
C21 N22 1.360(4) . ?
C22 N23 1.365(4) . ?
C22 N24 1.360(4) . ?
C23 H23 1.0000 . ?
C23 C24 1.553(4) . ?
C23 N21 1.455(4) . ?
C23 N24 1.453(4) . ?
C24 H24 1.0000 . ?
C24 N22 1.447(4) . ?
C24 N23 1.449(4) . ?
N22 C25 1.454(4) . ?
N23 C26 1.441(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O31 C31 1.234(4) . ?
O32 C32 1.224(4) . ?
C31 N31 1.358(4) . ?
C31 N32 1.365(4) . ?
C32 N33 1.367(4) . ?
C32 N34 1.367(4) . ?
C33 H33 1.0000 . ?
C33 C34 1.552(4) . ?
C33 N31 1.455(4) . ?
C33 N34 1.447(4) . ?
C34 H34 1.0000 . ?
C34 N32 1.450(4) . ?
C34 N33 1.450(4) . ?
N31 C36 1.445(4) 14_455 ?
N32 C35 1.441(4) . ?
N33 C36 1.443(4) . ?
N34 C35 1.448(4) 14_455 ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 O11N 1.257(4) . ?
N1 O12N 1.251(4) . ?
N1 O13N 1.234(4) . ?
N2 O21N 1.242(4) . ?
N2 O22N 1.240(4) . ?
N2 O23N 1.257(4) . ?
N3 O31N 1.250(4) . ?
N3 O32N 1.238(4) . ?
N3 O33N 1.234(4) . ?
N4 O41N 1.243(7) . ?
N4 O41' 1.267(6) . ?
N4 O42N 1.258(6) . ?
N4 O43N 1.244(6) . ?
N5 O51N 1.260(7) . ?
N5 O52N 1.251(7) . ?
N5 O53N 1.249(7) . ?
N6 O61N 1.247(7) . ?
N6 O62N 1.242(7) . ?
N6 O63N 1.241(7) . ?
N7 O71N 1.240(7) . ?
N7 O72N 1.246(7) . ?
N7 O73N 1.237(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1M Yb1 O4M 133.63(11) . . ?
O1M Yb1 O5M 71.58(11) . . ?
O1M Yb1 O7M 129.19(10) . . ?
O2M Yb1 O1M 75.70(10) . . ?
O2M Yb1 O3M 90.00(11) . . ?
O2M Yb1 O4M 69.95(10) . . ?
O2M Yb1 O5M 75.46(10) . . ?
O2M Yb1 O6M 145.18(10) . . ?
O2M Yb1 O7M 143.84(10) . . ?
O3M Yb1 O1M 73.47(12) . . ?
O3M Yb1 O4M 76.31(11) . . ?
O3M Yb1 O5M 144.47(12) . . ?
O3M Yb1 O6M 96.78(11) . . ?
O3M Yb1 O7M 76.23(12) . . ?
O5M Yb1 O4M 125.66(11) . . ?
O5M Yb1 O7M 132.79(10) . . ?
O6M Yb1 O1M 73.67(10) . . ?
O6M Yb1 O4M 144.82(10) . . ?
O6M Yb1 O5M 79.47(10) . . ?
O6M Yb1 O7M 70.54(10) . . ?
O7M Yb1 O4M 74.32(10) . . ?
O8M Yb1 O1M 142.85(12) . . ?
O8M Yb1 O2M 101.78(12) . . ?
O8M Yb1 O3M 143.46(12) . . ?
O8M Yb1 O4M 75.63(11) . . ?
O8M Yb1 O5M 71.97(11) . . ?
O8M Yb1 O6M 92.87(11) . . ?
O8M Yb1 O7M 74.01(11) . . ?
O11 C11 N11 125.9(3) . . ?
O11 C11 N12 125.4(3) . . ?
N11 C11 N12 108.6(3) . . ?
O12 C12 N13 125.3(3) . . ?
O12 C12 N14 126.4(3) . . ?
N14 C12 N13 108.4(3) . . ?
C14 C13 H13 112.1 . . ?
N11 C13 H13 112.1 . . ?
N11 C13 C14 102.8(2) . . ?
N11 C13 N14 114.0(3) . . ?
N14 C13 H13 112.1 . . ?
N14 C13 C14 103.1(2) . . ?
C13 C14 H14 111.8 . . ?
N12 C14 C13 103.2(2) . . ?
N12 C14 H14 111.8 . . ?
N13 C14 C13 103.4(2) . . ?
N13 C14 H14 111.8 . . ?
N13 C14 N12 114.3(3) . . ?
C11 N11 C13 112.8(3) . . ?
C11 N11 C25 123.6(3) . 3_565 ?
C25 N11 C13 123.3(3) 3_565 . ?
C11 N12 C14 112.5(3) . . ?
C11 N12 C15 123.4(3) . . ?
C15 N12 C14 123.7(3) . . ?
C12 N13 C14 112.6(3) . . ?
C12 N13 C16 122.5(3) . . ?
C14 N13 C16 122.9(3) . . ?
C12 N14 C13 112.5(3) . . ?
C12 N14 C26 123.1(3) . 3_565 ?
C13 N14 C26 122.4(3) . 3_565 ?
N12 C15 H15A 108.7 . . ?
N12 C15 H15B 108.7 . . ?
N12 C15 N21 114.0(3) . . ?
H15A C15 H15B 107.6 . . ?
N21 C15 H15A 108.7 . . ?
N21 C15 H15B 108.7 . . ?
N13 C16 H16A 108.8 . . ?
N13 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N24 C16 N13 113.8(3) . . ?
N24 C16 H16A 108.8 . . ?
N24 C16 H16B 108.8 . . ?
O21 C21 N21 125.4(3) . . ?
O21 C21 N22 125.7(3) . . ?
N22 C21 N21 108.8(3) . . ?
O22 C22 N23 124.9(3) . . ?
O22 C22 N24 126.6(3) . . ?
N24 C22 N23 108.5(3) . . ?
C24 C23 H23 111.8 . . ?
N21 C23 H23 111.8 . . ?
N21 C23 C24 103.2(2) . . ?
N24 C23 H23 111.8 . . ?
N24 C23 C24 103.2(2) . . ?
N24 C23 N21 114.2(3) . . ?
C23 C24 H24 111.7 . . ?
N22 C24 C23 103.3(2) . . ?
N22 C24 H24 111.7 . . ?
N22 C24 N23 114.7(3) . . ?
N23 C24 C23 103.0(2) . . ?
N23 C24 H24 111.7 . . ?
C15 N21 C23 123.7(3) . . ?
C21 N21 C15 122.1(3) . . ?
C21 N21 C23 111.9(3) . . ?
C21 N22 C24 112.5(3) . . ?
C21 N22 C25 122.6(3) . . ?
C24 N22 C25 123.5(3) . . ?
C22 N23 C24 112.7(3) . . ?
C22 N23 C26 122.7(3) . . ?
C26 N23 C24 124.5(3) . . ?
C16 N24 C23 123.7(2) . . ?
C22 N24 C16 123.6(3) . . ?
C22 N24 C23 112.5(2) . . ?
N11 C25 N22 113.6(3) 2_665 . ?
N11 C25 H25A 108.8 2_665 . ?
N11 C25 H25B 108.8 2_665 . ?
N22 C25 H25A 108.8 . . ?
N22 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N14 C26 H26A 108.8 2_665 . ?
N14 C26 H26B 108.8 2_665 . ?
N23 C26 N14 113.9(3) . 2_665 ?
N23 C26 H26A 108.8 . . ?
N23 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
O31 C31 N31 126.8(3) . . ?
O31 C31 N32 124.6(3) . . ?
N31 C31 N32 108.6(3) . . ?
O32 C32 N33 125.4(3) . . ?
O32 C32 N34 126.1(3) . . ?
N33 C32 N34 108.4(3) . . ?
C34 C33 H33 111.8 . . ?
N31 C33 H33 111.8 . . ?
N31 C33 C34 103.0(2) . . ?
N34 C33 H33 111.8 . . ?
N34 C33 C34 103.3(2) . . ?
N34 C33 N31 114.5(3) . . ?
C33 C34 H34 111.7 . . ?
N32 C34 C33 103.3(2) . . ?
N32 C34 H34 111.7 . . ?
N32 C34 N33 114.7(3) . . ?
N33 C34 C33 103.2(2) . . ?
N33 C34 H34 111.7 . . ?
C31 N31 C33 112.6(3) . . ?
C31 N31 C36 124.0(3) . 14_455 ?
C36 N31 C33 123.4(3) 14_455 . ?
C31 N32 C34 112.5(3) . . ?
C31 N32 C35 123.9(3) . . ?
C35 N32 C34 123.6(3) . . ?
C32 N33 C34 112.3(3) . . ?
C32 N33 C36 122.4(3) . . ?
C36 N33 C34 122.2(3) . . ?
C32 N34 C33 112.4(3) . . ?
C32 N34 C35 122.7(3) . 14_455 ?
C33 N34 C35 122.0(3) . 14_455 ?
N32 C35 N34 114.3(3) . 15 ?
N32 C35 H35A 108.7 . . ?
N32 C35 H35B 108.7 . . ?
N34 C35 H35A 108.7 15 . ?
N34 C35 H35B 108.7 15 . ?
H35A C35 H35B 107.6 . . ?
N31 C36 H36A 108.7 15 . ?
N31 C36 H36B 108.7 15 . ?
N33 C36 N31 114.1(3) . 15 ?
N33 C36 H36A 108.7 . . ?
N33 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
O12N N1 O11N 119.8(3) . . ?
O13N N1 O11N 119.9(3) . . ?
O13N N1 O12N 120.1(3) . . ?
O21N N2 O23N 119.6(3) . . ?
O22N N2 O21N 119.6(3) . . ?
O22N N2 O23N 120.8(3) . . ?
O32N N3 O31N 120.4(3) . . ?
O33N N3 O31N 119.4(3) . . ?
O33N N3 O32N 120.2(3) . . ?
O41N N4 O41' 49.9(8) . . ?
O41N N4 O42N 117.0(7) . . ?
O41N N4 O43N 117.9(9) . . ?
O42N N4 O41' 116.7(6) . . ?
O43N N4 O41' 118.5(6) . . ?
O43N N4 O42N 118.7(6) . . ?
O52N N5 O51N 117.7(8) . . ?
O53N N5 O51N 124.4(11) . . ?
O53N N5 O52N 117.9(8) . . ?
O62N N6 O61N 119.6(7) . . ?
O63N N6 O61N 119.5(7) . . ?
O63N N6 O62N 120.9(7) . . ?
O71N N7 O72N 120.4(7) . . ?
O73N N7 O71N 120.1(7) . . ?
O73N N7 O72N 119.5(7) . . ?

_refine_diff_density_max         1.309
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.122



