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

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

data_Eu-phen
_database_code_depnum_ccdc_archive 'CCDC 2013253'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  EuCum3Fen
# Clave IF-UAP:  EuCum3Fen
# Solicitud: 127
# Firma en la Solicitud: Dra. Laura Gasque (UNAM)
# Clave datos : ... \BUAP\Sylvain\EuCum3Fen\40mm_1\

# start Validation Reply Form
_vrf_PLAT973_Eu-phen             
;
PROBLEM: Check Calcd Positive Resid. Density on       Eu1       2.63 eA-3  
RESPONSE: Bond lengths from Eu1 are within expectations (MOGUL check),
and the residual is not improved for models including other lanthanides.
The high residual could reflect a not optimized absorption correction
rather than a wrongly assigned lanthanide.

;
# end Validation Reply Form

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_audit_creation_date             2018-06-21

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H31 Eu N2 O13, 1.5(H2 O)'
_chemical_formula_sum            'C45 H34 Eu N2 O14.50'
_chemical_formula_weight         986.70
_chemical_absolute_configuration .
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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'
Eu Eu -0.3977 2.4351 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 '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       ?

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                   13.6208(3)
_cell_length_b                   17.3161(3)
_cell_length_c                   18.5812(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.983(2)
_cell_angle_gamma                90
_cell_volume                     4381.90(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    69972
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      26.03

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_F_000             1988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.806
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4784
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA 1.82 (Stoe & Cie, 2018)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1619 frames, 30-40 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            156004
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.048
_diffrn_reflns_theta_max         24.353
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14574
_reflns_number_gt                9832
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA 1.82 (Stoe & Cie, 2018)'
_computing_cell_refinement       'X-AREA 1.82'
_computing_data_reduction        'X-AREA 1.82'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'

_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)+(0.0767P)²+0.5036P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         14574
_refine_ls_number_parameters     604
_refine_ls_number_restraints     12
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1351
_refine_ls_wR_factor_gt          0.1095
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.004
_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 0.55060(2) 0.65244(2) 0.23695(2) 0.03490(6) Uani 1 1 d . . . . .
O1 O 0.1175(2) 0.6056(3) 0.1984(2) 0.0822(11) Uani 1 1 d . . . . .
O2 O 0.1264(3) 0.7290(3) 0.1739(3) 0.0983(13) Uani 1 1 d . . . . .
O3 O 0.41360(19) 0.57665(15) 0.19867(16) 0.0499(6) Uani 1 1 d . . . . .
O4 O 0.4283(2) 0.72547(16) 0.16401(16) 0.0562(7) Uani 1 1 d . . . . .
C3 C 0.2780(3) 0.6601(2) 0.1769(2) 0.0493(8) Uani 1 1 d . . . . .
C2 C 0.1735(4) 0.6696(3) 0.1811(3) 0.0659(12) Uani 1 1 d . . . . .
C4 C 0.3231(3) 0.5894(2) 0.19535(18) 0.0438(7) Uani 1 1 d . . . . .
C5 C 0.2576(3) 0.5231(3) 0.20821(18) 0.0499(9) Uani 1 1 d . . . . .
C6 C 0.2934(3) 0.4482(2) 0.2186(2) 0.0539(9) Uani 1 1 d . . . . .
H6A H 0.360782 0.439576 0.218318 0.065 Uiso 1 1 calc R U . . .
C7 C 0.2312(4) 0.3870(3) 0.2292(3) 0.0764(15) Uani 1 1 d . . . . .
H7A H 0.256124 0.337346 0.234854 0.092 Uiso 1 1 calc R U . . .
C8 C 0.1321(5) 0.4000(5) 0.2312(4) 0.105(2) Uani 1 1 d . . . . .
H8A H 0.089734 0.359019 0.239872 0.126 Uiso 1 1 calc R U . . .
C9 C 0.0944(4) 0.4729(5) 0.2207(4) 0.100(2) Uani 1 1 d . . . . .
H9A H 0.027038 0.481460 0.221922 0.120 Uiso 1 1 calc R U . . .
C10 C 0.1588(4) 0.5336(4) 0.2081(3) 0.0765(15) Uani 1 1 d . . . . .
C11 C 0.3399(3) 0.7222(2) 0.1504(2) 0.0528(9) Uani 1 1 d . . . . .
C12 C 0.2989(4) 0.7823(3) 0.0999(3) 0.0795(15) Uani 1 1 d . . . . .
H12A H 0.255222 0.758177 0.065522 0.119 Uiso 1 1 calc R U . . .
H12B H 0.351615 0.806858 0.075023 0.119 Uiso 1 1 calc R U . . .
H12C H 0.263493 0.820249 0.126743 0.119 Uiso 1 1 calc R U . . .
O21 O 0.4948(2) 0.6360(2) 0.56143(15) 0.0677(9) Uani 1 1 d . . . . .
O22 O 0.3773(3) 0.7155(3) 0.53216(19) 0.0883(12) Uani 1 1 d . . . . .
O23 O 0.5700(2) 0.59882(14) 0.35241(13) 0.0492(6) Uani 1 1 d . . . . .
O24 O 0.4127(2) 0.6824(2) 0.31413(15) 0.0609(7) Uani 1 1 d . . . . .
C22 C 0.4391(4) 0.6711(3) 0.5090(2) 0.0605(11) Uani 1 1 d . . . . .
C23 C 0.4594(3) 0.6561(2) 0.4340(2) 0.0469(8) Uani 1 1 d . . . . .
C24 C 0.5427(3) 0.61223(19) 0.41597(18) 0.0432(7) Uani 1 1 d . . . . .
C25 C 0.6004(3) 0.5774(2) 0.47472(18) 0.0456(8) Uani 1 1 d . . . . .
C26 C 0.6818(4) 0.5319(3) 0.4622(2) 0.0598(11) Uani 1 1 d . . . . .
H26A H 0.701880 0.523344 0.415300 0.072 Uiso 1 1 calc R U . . .
C27 C 0.7338(4) 0.4990(3) 0.5197(2) 0.0707(13) Uani 1 1 d . . . . .
H27A H 0.788466 0.468146 0.511528 0.085 Uiso 1 1 calc R U . . .
C28 C 0.7027(4) 0.5129(3) 0.5892(2) 0.0703(13) Uani 1 1 d . . . . .
H28A H 0.736905 0.490567 0.627695 0.084 Uiso 1 1 calc R U . . .
C29 C 0.6237(4) 0.5582(3) 0.6026(2) 0.0679(13) Uani 1 1 d . . . . .
H29A H 0.604466 0.567566 0.649607 0.082 Uiso 1 1 calc R U . . .
C30 C 0.5725(3) 0.5901(2) 0.54513(19) 0.0517(9) Uani 1 1 d . . . . .
C31 C 0.3932(3) 0.6852(3) 0.3786(2) 0.0547(9) Uani 1 1 d . . . . .
C32 C 0.2933(4) 0.7166(4) 0.3958(3) 0.0928(19) Uani 1 1 d . . . . .
H32A H 0.264194 0.685401 0.432424 0.139 Uiso 1 1 calc R U . . .
H32B H 0.252313 0.715578 0.353209 0.139 Uiso 1 1 calc R U . . .
H32C H 0.299542 0.768781 0.412638 0.139 Uiso 1 1 calc R U . . .
O41 O 0.6619(2) 0.98810(15) 0.31548(15) 0.0502(6) Uani 1 1 d . . . . .
O42 O 0.6924(3) 0.99053(16) 0.20186(17) 0.0612(8) Uani 1 1 d . . . . .
O43 O 0.5906(2) 0.75944(15) 0.31485(14) 0.0541(7) Uani 1 1 d . . . . .
O44 O 0.6299(2) 0.75751(14) 0.17707(14) 0.0499(6) Uani 1 1 d . . . . .
C42 C 0.6677(3) 0.9498(2) 0.2510(2) 0.0444(7) Uani 1 1 d . . . . .
C43 C 0.6429(2) 0.8690(2) 0.24810(19) 0.0395(7) Uani 1 1 d . . . . .
C44 C 0.6154(3) 0.8284(2) 0.31249(19) 0.0418(7) Uani 1 1 d . . . . .
C45 C 0.6158(3) 0.8741(2) 0.3794(2) 0.0467(8) Uani 1 1 d . . . . .
C46 C 0.5909(4) 0.8411(3) 0.4451(2) 0.0598(11) Uani 1 1 d . . . . .
H46A H 0.575375 0.788869 0.447121 0.072 Uiso 1 1 calc R U . . .
C47 C 0.5887(4) 0.8846(3) 0.5068(2) 0.0664(12) Uani 1 1 d . . . . .
H47A H 0.572180 0.862058 0.550344 0.080 Uiso 1 1 calc R U . . .
C48 C 0.6115(4) 0.9623(3) 0.5036(2) 0.0657(11) Uani 1 1 d . . . . .
H48A H 0.610586 0.991689 0.545414 0.079 Uiso 1 1 calc R U . . .
C49 C 0.6354(3) 0.9968(3) 0.4398(2) 0.0569(10) Uani 1 1 d . . . . .
H49A H 0.649471 1.049328 0.437762 0.068 Uiso 1 1 calc R U . . .
C50 C 0.6379(3) 0.9512(2) 0.37790(19) 0.0435(7) Uani 1 1 d . . . . .
C51 C 0.6488(3) 0.8269(2) 0.18126(19) 0.0437(7) Uani 1 1 d . . . . .
C52 C 0.6772(5) 0.8659(3) 0.1123(3) 0.0802(17) Uani 1 1 d . . . . .
H52A H 0.738748 0.892139 0.119295 0.120 Uiso 1 1 calc R U . . .
H52B H 0.627493 0.902653 0.098587 0.120 Uiso 1 1 calc R U . . .
H52C H 0.683468 0.827950 0.075032 0.120 Uiso 1 1 calc R U . . .
N1 N 0.5881(2) 0.50283(16) 0.21962(15) 0.0384(6) Uani 1 1 d . . . . .
N2 N 0.5940(2) 0.60453(18) 0.10650(15) 0.0439(6) Uani 1 1 d . . . . .
C61 C 0.5821(3) 0.4529(2) 0.2726(2) 0.0466(8) Uani 1 1 d . . . . .
H61A H 0.572560 0.472088 0.318720 0.056 Uiso 1 1 calc R U . . .
C62 C 0.5892(4) 0.3725(2) 0.2642(2) 0.0576(10) Uani 1 1 d . . . . .
H62A H 0.583381 0.339551 0.303435 0.069 Uiso 1 1 calc R U . . .
C63 C 0.6050(4) 0.3441(2) 0.1967(3) 0.0599(10) Uani 1 1 d . . . . .
H63A H 0.610556 0.291189 0.189462 0.072 Uiso 1 1 calc R U . . .
C64 C 0.6128(3) 0.3944(2) 0.1390(2) 0.0494(8) Uani 1 1 d . . . . .
C65 C 0.6314(4) 0.3680(3) 0.0671(3) 0.0627(11) Uani 1 1 d . . . . .
H65A H 0.639587 0.315483 0.058434 0.075 Uiso 1 1 calc R U . . .
C66 C 0.6368(4) 0.4179(3) 0.0128(2) 0.0641(12) Uani 1 1 d . . . . .
H66A H 0.649625 0.399425 -0.033095 0.077 Uiso 1 1 calc R U . . .
C67 C 0.6236(3) 0.4992(3) 0.0231(2) 0.0514(9) Uani 1 1 d . . . . .
C68 C 0.6286(4) 0.5517(3) -0.0330(2) 0.0638(11) Uani 1 1 d . . . . .
H68A H 0.640455 0.534638 -0.079520 0.077 Uiso 1 1 calc R U . . .
C69 C 0.6159(4) 0.6289(3) -0.0196(2) 0.0652(12) Uani 1 1 d . . . . .
H69A H 0.619174 0.664793 -0.056688 0.078 Uiso 1 1 calc R U . . .
C70 C 0.5979(4) 0.6528(3) 0.0515(2) 0.0582(10) Uani 1 1 d . . . . .
H70A H 0.588233 0.705138 0.060084 0.070 Uiso 1 1 calc R U . . .
C71 C 0.6068(2) 0.5278(2) 0.09331(17) 0.0412(7) Uani 1 1 d . . . . .
C72 C 0.6020(2) 0.47422(19) 0.15214(18) 0.0390(7) Uani 1 1 d . . . . .
O61 O 0.7304(2) 0.63524(16) 0.24862(16) 0.0489(6) Uani 1 1 d D . . . .
H611 H 0.770(3) 0.666(2) 0.231(3) 0.073 Uiso 1 1 d D U . . .
H612 H 0.758(3) 0.5933(15) 0.254(3) 0.073 Uiso 1 1 d D U . . .
O71 O 0.8858(3) 0.6903(3) 0.1600(2) 0.0842(11) Uani 1 1 d D . . . .
H711 H 0.890(5) 0.712(4) 0.120(2) 0.126 Uiso 1 1 d D U . . .
H712 H 0.946(2) 0.684(5) 0.174(4) 0.126 Uiso 1 1 d D U . . .
O72A O 0.6583(17) 0.1778(8) 0.1048(8) 0.116(8) Uani 0.25 1 d D . P A 1
H721 H 0.670(7) 0.208(4) 0.070(3) 0.174 Uiso 0.25 1 d D U P B 1
H722 H 0.607(4) 0.154(4) 0.092(5) 0.174 Uiso 0.25 1 d D U P C 1
O72B O 0.538(2) 0.1208(12) 0.103(2) 0.217(19) Uani 0.25 1 d D . P D 2
H723 H 0.516(6) 0.083(3) 0.079(4) 0.326 Uiso 0.25 1 d D U P E 2
H724 H 0.488(4) 0.140(4) 0.122(5) 0.326 Uiso 0.25 1 d D U P F 2


_geom_special_details            ?

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 O23 2.348(2) . ?
Eu1 O3 2.380(3) . ?
Eu1 O44 2.399(2) . ?
Eu1 O43 2.408(3) . ?
Eu1 O24 2.439(3) . ?
Eu1 O61 2.473(3) . ?
Eu1 O4 2.477(3) . ?
Eu1 N2 2.639(3) . ?
Eu1 N1 2.661(3) . ?
O1 C10 1.378(7) . ?
O1 C2 1.387(7) . ?
O2 C2 1.218(6) . ?
O3 C4 1.252(4) . ?
O4 C11 1.227(5) . ?
C3 C4 1.410(5) . ?
C3 C2 1.436(6) . ?
C3 C11 1.458(6) . ?
C4 C5 1.475(5) . ?
C5 C10 1.358(7) . ?
C5 C6 1.399(6) . ?
C6 C7 1.372(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.371(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.375(10) . ?
C8 H8A 0.9300 . ?
C9 C10 1.392(8) . ?
C9 H9A 0.9300 . ?
C11 C12 1.504(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.363(6) . ?
O21 C22 1.367(6) . ?
O22 C22 1.224(6) . ?
O23 C24 1.266(4) . ?
O24 C31 1.231(5) . ?
C22 C23 1.448(5) . ?
C23 C24 1.412(5) . ?
C23 C31 1.448(6) . ?
C24 C25 1.464(5) . ?
C25 C26 1.383(6) . ?
C25 C30 1.386(5) . ?
C26 C27 1.394(6) . ?
C26 H26A 0.9300 . ?
C27 C28 1.388(7) . ?
C27 H27A 0.9300 . ?
C28 C29 1.359(8) . ?
C28 H28A 0.9300 . ?
C29 C30 1.381(6) . ?
C29 H29A 0.9300 . ?
C31 C32 1.506(7) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.369(5) . ?
O41 C42 1.374(4) . ?
O42 C42 1.206(5) . ?
O43 C44 1.241(4) . ?
O44 C51 1.231(4) . ?
C42 C43 1.440(5) . ?
C43 C44 1.443(5) . ?
C43 C51 1.444(5) . ?
C44 C45 1.474(5) . ?
C45 C50 1.369(5) . ?
C45 C46 1.395(6) . ?
C46 C47 1.373(6) . ?
C46 H46A 0.9300 . ?
C47 C48 1.381(7) . ?
C47 H47A 0.9300 . ?
C48 C49 1.372(7) . ?
C48 H48A 0.9300 . ?
C49 C50 1.396(5) . ?
C49 H49A 0.9300 . ?
C51 C52 1.505(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N1 C61 1.314(5) . ?
N1 C72 1.364(4) . ?
N2 C70 1.323(5) . ?
N2 C71 1.362(5) . ?
C61 C62 1.404(5) . ?
C61 H61A 0.9300 . ?
C62 C63 1.369(6) . ?
C62 H62A 0.9300 . ?
C63 C64 1.387(6) . ?
C63 H63A 0.9300 . ?
C64 C72 1.412(5) . ?
C64 C65 1.438(6) . ?
C65 C66 1.331(7) . ?
C65 H65A 0.9300 . ?
C66 C67 1.433(6) . ?
C66 H66A 0.9300 . ?
C67 C68 1.386(6) . ?
C67 C71 1.418(5) . ?
C68 C69 1.371(7) . ?
C68 H68A 0.9300 . ?
C69 C70 1.409(6) . ?
C69 H69A 0.9300 . ?
C70 H70A 0.9300 . ?
C71 C72 1.437(5) . ?
O61 H611 0.829(19) . ?
O61 H612 0.825(18) . ?
O71 H711 0.845(19) . ?
O71 H712 0.859(19) . ?
O72A H721 0.850(2) . ?
O72A H722 0.850(2) . ?
O72B H723 0.850(2) . ?
O72B H724 0.850(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O23 Eu1 O3 97.51(10) . . ?
O23 Eu1 O44 132.75(10) . . ?
O3 Eu1 O44 129.53(10) . . ?
O23 Eu1 O43 74.59(9) . . ?
O3 Eu1 O43 140.54(10) . . ?
O44 Eu1 O43 66.18(9) . . ?
O23 Eu1 O24 67.84(10) . . ?
O3 Eu1 O24 71.64(10) . . ?
O44 Eu1 O24 117.97(11) . . ?
O43 Eu1 O24 69.60(11) . . ?
O23 Eu1 O61 77.07(10) . . ?
O3 Eu1 O61 136.89(9) . . ?
O44 Eu1 O61 71.27(10) . . ?
O43 Eu1 O61 80.01(10) . . ?
O24 Eu1 O61 138.23(10) . . ?
O23 Eu1 O4 140.00(10) . . ?
O3 Eu1 O4 66.51(10) . . ?
O44 Eu1 O4 70.30(10) . . ?
O43 Eu1 O4 94.54(10) . . ?
O24 Eu1 O4 72.27(10) . . ?
O61 Eu1 O4 139.93(10) . . ?
O23 Eu1 N2 133.74(9) . . ?
O3 Eu1 N2 74.87(10) . . ?
O44 Eu1 N2 72.70(9) . . ?
O43 Eu1 N2 137.92(9) . . ?
O24 Eu1 N2 142.57(10) . . ?
O61 Eu1 N2 78.78(10) . . ?
O4 Eu1 N2 79.46(10) . . ?
O23 Eu1 N1 72.95(8) . . ?
O3 Eu1 N1 65.05(9) . . ?
O44 Eu1 N1 126.39(9) . . ?
O43 Eu1 N1 141.26(10) . . ?
O24 Eu1 N1 115.44(10) . . ?
O61 Eu1 N1 72.64(9) . . ?
O4 Eu1 N1 124.02(9) . . ?
N2 Eu1 N1 62.37(9) . . ?
C10 O1 C2 121.9(4) . . ?
C4 O3 Eu1 133.1(2) . . ?
C11 O4 Eu1 137.5(3) . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 C11 118.0(4) . . ?
C2 C3 C11 120.9(4) . . ?
O2 C2 O1 114.2(5) . . ?
O2 C2 C3 127.7(5) . . ?
O1 C2 C3 118.1(4) . . ?
O3 C4 C3 126.1(4) . . ?
O3 C4 C5 116.9(3) . . ?
C3 C4 C5 116.9(3) . . ?
C10 C5 C6 117.9(4) . . ?
C10 C5 C4 119.8(4) . . ?
C6 C5 C4 122.3(4) . . ?
C7 C6 C5 121.4(5) . . ?
C7 C6 H6A 119.3 . . ?
C5 C6 H6A 119.3 . . ?
C6 C7 C8 119.2(6) . . ?
C6 C7 H7A 120.4 . . ?
C8 C7 H7A 120.4 . . ?
C7 C8 C9 120.8(5) . . ?
C7 C8 H8A 119.6 . . ?
C9 C8 H8A 119.6 . . ?
C8 C9 C10 118.9(6) . . ?
C8 C9 H9A 120.6 . . ?
C10 C9 H9A 120.6 . . ?
C5 C10 O1 121.6(5) . . ?
C5 C10 C9 121.7(6) . . ?
O1 C10 C9 116.6(5) . . ?
O4 C11 C3 122.5(4) . . ?
O4 C11 C12 116.7(4) . . ?
C3 C11 C12 120.7(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 121.6(3) . . ?
C24 O23 Eu1 138.5(2) . . ?
C31 O24 Eu1 139.5(3) . . ?
O22 C22 O21 113.9(4) . . ?
O22 C22 C23 126.5(5) . . ?
O21 C22 C23 119.6(4) . . ?
C24 C23 C22 119.5(4) . . ?
C24 C23 C31 120.8(3) . . ?
C22 C23 C31 119.7(4) . . ?
O23 C24 C23 124.8(4) . . ?
O23 C24 C25 117.2(3) . . ?
C23 C24 C25 117.9(3) . . ?
C26 C25 C30 118.8(4) . . ?
C26 C25 C24 122.0(3) . . ?
C30 C25 C24 119.1(4) . . ?
C25 C26 C27 120.2(4) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C28 C27 C26 118.9(5) . . ?
C28 C27 H27A 120.6 . . ?
C26 C27 H27A 120.6 . . ?
C29 C28 C27 121.7(5) . . ?
C29 C28 H28A 119.1 . . ?
C27 C28 H28A 119.1 . . ?
C28 C29 C30 118.7(4) . . ?
C28 C29 H29A 120.6 . . ?
C30 C29 H29A 120.6 . . ?
O21 C30 C29 116.5(4) . . ?
O21 C30 C25 121.9(4) . . ?
C29 C30 C25 121.6(4) . . ?
O24 C31 C23 122.5(4) . . ?
O24 C31 C32 115.5(4) . . ?
C23 C31 C32 121.9(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.1(3) . . ?
C44 O43 Eu1 141.0(2) . . ?
C51 O44 Eu1 143.7(2) . . ?
O42 C42 O41 113.5(3) . . ?
O42 C42 C43 127.5(4) . . ?
O41 C42 C43 119.0(3) . . ?
C42 C43 C44 120.5(3) . . ?
C42 C43 C51 120.4(3) . . ?
C44 C43 C51 119.1(3) . . ?
O43 C44 C43 124.9(3) . . ?
O43 C44 C45 118.9(3) . . ?
C43 C44 C45 116.1(3) . . ?
C50 C45 C46 118.3(3) . . ?
C50 C45 C44 120.3(3) . . ?
C46 C45 C44 121.4(4) . . ?
C47 C46 C45 121.0(4) . . ?
C47 C46 H46A 119.5 . . ?
C45 C46 H46A 119.5 . . ?
C46 C47 C48 119.3(4) . . ?
C46 C47 H47A 120.3 . . ?
C48 C47 H47A 120.3 . . ?
C49 C48 C47 121.3(4) . . ?
C49 C48 H48A 119.4 . . ?
C47 C48 H48A 119.4 . . ?
C48 C49 C50 118.3(4) . . ?
C48 C49 H49A 120.9 . . ?
C50 C49 H49A 120.9 . . ?
C45 C50 O41 121.9(3) . . ?
C45 C50 C49 121.8(4) . . ?
O41 C50 C49 116.3(3) . . ?
O44 C51 C43 122.2(3) . . ?
O44 C51 C52 116.2(3) . . ?
C43 C51 C52 121.6(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 N1 C72 117.5(3) . . ?
C61 N1 Eu1 122.4(2) . . ?
C72 N1 Eu1 119.6(2) . . ?
C70 N2 C71 118.0(3) . . ?
C70 N2 Eu1 121.6(3) . . ?
C71 N2 Eu1 120.2(2) . . ?
N1 C61 C62 124.3(4) . . ?
N1 C61 H61A 117.8 . . ?
C62 C61 H61A 117.8 . . ?
C63 C62 C61 118.0(4) . . ?
C63 C62 H62A 121.0 . . ?
C61 C62 H62A 121.0 . . ?
C62 C63 C64 120.0(4) . . ?
C62 C63 H63A 120.0 . . ?
C64 C63 H63A 120.0 . . ?
C63 C64 C72 118.1(3) . . ?
C63 C64 C65 122.4(4) . . ?
C72 C64 C65 119.6(4) . . ?
C66 C65 C64 120.7(4) . . ?
C66 C65 H65A 119.7 . . ?
C64 C65 H65A 119.7 . . ?
C65 C66 C67 121.8(4) . . ?
C65 C66 H66A 119.1 . . ?
C67 C66 H66A 119.1 . . ?
C68 C67 C71 118.2(4) . . ?
C68 C67 C66 122.4(4) . . ?
C71 C67 C66 119.4(4) . . ?
C69 C68 C67 119.6(4) . . ?
C69 C68 H68A 120.2 . . ?
C67 C68 H68A 120.2 . . ?
C68 C69 C70 118.8(4) . . ?
C68 C69 H69A 120.6 . . ?
C70 C69 H69A 120.6 . . ?
N2 C70 C69 123.3(4) . . ?
N2 C70 H70A 118.4 . . ?
C69 C70 H70A 118.4 . . ?
N2 C71 C67 122.0(3) . . ?
N2 C71 C72 119.0(3) . . ?
C67 C71 C72 118.9(3) . . ?
N1 C72 C64 122.1(3) . . ?
N1 C72 C71 118.3(3) . . ?
C64 C72 C71 119.6(3) . . ?
Eu1 O61 H611 123(3) . . ?
Eu1 O61 H612 125(3) . . ?
H611 O61 H612 108(3) . . ?
H711 O71 H712 104(3) . . ?
H721 O72A H722 104.1(3) . . ?
H723 O72B H724 104.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 179.6(5) . . . . ?
C10 O1 C2 C3 -3.1(7) . . . . ?
C4 C3 C2 O2 172.0(5) . . . . ?
C11 C3 C2 O2 -10.7(8) . . . . ?
C4 C3 C2 O1 -5.0(6) . . . . ?
C11 C3 C2 O1 172.4(4) . . . . ?
Eu1 O3 C4 C3 36.7(5) . . . . ?
Eu1 O3 C4 C5 -146.7(3) . . . . ?
C2 C3 C4 O3 -174.4(4) . . . . ?
C11 C3 C4 O3 8.2(6) . . . . ?
C2 C3 C4 C5 9.1(5) . . . . ?
C11 C3 C4 C5 -168.3(3) . . . . ?
O3 C4 C5 C10 177.5(4) . . . . ?
C3 C4 C5 C10 -5.6(5) . . . . ?
O3 C4 C5 C6 -4.5(5) . . . . ?
C3 C4 C5 C6 172.4(3) . . . . ?
C10 C5 C6 C7 -0.8(6) . . . . ?
C4 C5 C6 C7 -178.8(4) . . . . ?
C5 C6 C7 C8 -1.5(7) . . . . ?
C6 C7 C8 C9 2.0(10) . . . . ?
C7 C8 C9 C10 -0.2(11) . . . . ?
C6 C5 C10 O1 179.8(4) . . . . ?
C4 C5 C10 O1 -2.1(6) . . . . ?
C6 C5 C10 C9 2.6(7) . . . . ?
C4 C5 C10 C9 -179.3(5) . . . . ?
C2 O1 C10 C5 6.7(7) . . . . ?
C2 O1 C10 C9 -176.0(5) . . . . ?
C8 C9 C10 C5 -2.1(10) . . . . ?
C8 C9 C10 O1 -179.5(6) . . . . ?
Eu1 O4 C11 C3 -3.9(6) . . . . ?
Eu1 O4 C11 C12 -179.2(3) . . . . ?
C4 C3 C11 O4 -23.3(5) . . . . ?
C2 C3 C11 O4 159.3(4) . . . . ?
C4 C3 C11 C12 151.9(4) . . . . ?
C2 C3 C11 C12 -25.5(6) . . . . ?
C30 O21 C22 O22 -174.3(4) . . . . ?
C30 O21 C22 C23 3.4(6) . . . . ?
O22 C22 C23 C24 170.5(5) . . . . ?
O21 C22 C23 C24 -6.8(6) . . . . ?
O22 C22 C23 C31 -10.4(7) . . . . ?
O21 C22 C23 C31 172.2(4) . . . . ?
Eu1 O23 C24 C23 22.5(6) . . . . ?
Eu1 O23 C24 C25 -159.6(3) . . . . ?
C22 C23 C24 O23 -176.4(4) . . . . ?
C31 C23 C24 O23 4.6(6) . . . . ?
C22 C23 C24 C25 5.7(5) . . . . ?
C31 C23 C24 C25 -173.4(3) . . . . ?
O23 C24 C25 C26 0.3(5) . . . . ?
C23 C24 C25 C26 178.4(4) . . . . ?
O23 C24 C25 C30 -179.4(3) . . . . ?
C23 C24 C25 C30 -1.3(5) . . . . ?
C30 C25 C26 C27 0.6(7) . . . . ?
C24 C25 C26 C27 -179.0(4) . . . . ?
C25 C26 C27 C28 -0.3(8) . . . . ?
C26 C27 C28 C29 -0.6(8) . . . . ?
C27 C28 C29 C30 1.0(8) . . . . ?
C22 O21 C30 C29 179.5(4) . . . . ?
C22 O21 C30 C25 1.1(6) . . . . ?
C28 C29 C30 O21 -179.0(4) . . . . ?
C28 C29 C30 C25 -0.6(7) . . . . ?
C26 C25 C30 O21 178.1(4) . . . . ?
C24 C25 C30 O21 -2.2(5) . . . . ?
C26 C25 C30 C29 -0.2(6) . . . . ?
C24 C25 C30 C29 179.5(4) . . . . ?
Eu1 O24 C31 C23 -9.7(7) . . . . ?
Eu1 O24 C31 C32 173.9(4) . . . . ?
C24 C23 C31 O24 -9.9(6) . . . . ?
C22 C23 C31 O24 171.0(4) . . . . ?
C24 C23 C31 C32 166.3(5) . . . . ?
C22 C23 C31 C32 -12.8(7) . . . . ?
C50 O41 C42 O42 -178.0(3) . . . . ?
C50 O41 C42 C43 3.3(5) . . . . ?
O42 C42 C43 C44 179.5(4) . . . . ?
O41 C42 C43 C44 -2.0(5) . . . . ?
O42 C42 C43 C51 2.0(6) . . . . ?
O41 C42 C43 C51 -179.6(3) . . . . ?
Eu1 O43 C44 C43 -8.9(7) . . . . ?
Eu1 O43 C44 C45 169.9(3) . . . . ?
C42 C43 C44 O43 178.1(4) . . . . ?
C51 C43 C44 O43 -4.3(6) . . . . ?
C42 C43 C44 C45 -0.7(5) . . . . ?
C51 C43 C44 C45 176.9(3) . . . . ?
O43 C44 C45 C50 -176.6(4) . . . . ?
C43 C44 C45 C50 2.3(5) . . . . ?
O43 C44 C45 C46 1.2(6) . . . . ?
C43 C44 C45 C46 -179.9(4) . . . . ?
C50 C45 C46 C47 -0.2(7) . . . . ?
C44 C45 C46 C47 -178.1(4) . . . . ?
C45 C46 C47 C48 0.2(8) . . . . ?
C46 C47 C48 C49 0.5(8) . . . . ?
C47 C48 C49 C50 -1.1(7) . . . . ?
C46 C45 C50 O41 -179.1(4) . . . . ?
C44 C45 C50 O41 -1.2(6) . . . . ?
C46 C45 C50 C49 -0.4(6) . . . . ?
C44 C45 C50 C49 177.5(4) . . . . ?
C42 O41 C50 C45 -1.7(5) . . . . ?
C42 O41 C50 C49 179.5(3) . . . . ?
C48 C49 C50 C45 1.1(6) . . . . ?
C48 C49 C50 O41 179.9(4) . . . . ?
Eu1 O44 C51 C43 17.4(7) . . . . ?
Eu1 O44 C51 C52 -161.7(4) . . . . ?
C42 C43 C51 O44 178.7(4) . . . . ?
C44 C43 C51 O44 1.1(6) . . . . ?
C42 C43 C51 C52 -2.3(6) . . . . ?
C44 C43 C51 C52 -179.9(4) . . . . ?
C72 N1 C61 C62 0.1(6) . . . . ?
Eu1 N1 C61 C62 171.8(3) . . . . ?
N1 C61 C62 C63 1.1(7) . . . . ?
C61 C62 C63 C64 -0.5(7) . . . . ?
C62 C63 C64 C72 -1.3(7) . . . . ?
C62 C63 C64 C65 178.7(5) . . . . ?
C63 C64 C65 C66 178.9(5) . . . . ?
C72 C64 C65 C66 -1.1(7) . . . . ?
C64 C65 C66 C67 -0.7(8) . . . . ?
C65 C66 C67 C68 -179.7(5) . . . . ?
C65 C66 C67 C71 1.8(7) . . . . ?
C71 C67 C68 C69 -1.0(7) . . . . ?
C66 C67 C68 C69 -179.5(5) . . . . ?
C67 C68 C69 C70 -0.1(8) . . . . ?
C71 N2 C70 C69 -0.9(7) . . . . ?
Eu1 N2 C70 C69 -176.7(4) . . . . ?
C68 C69 C70 N2 1.1(8) . . . . ?
C70 N2 C71 C67 -0.2(6) . . . . ?
Eu1 N2 C71 C67 175.6(3) . . . . ?
C70 N2 C71 C72 -179.4(4) . . . . ?
Eu1 N2 C71 C72 -3.6(4) . . . . ?
C68 C67 C71 N2 1.2(6) . . . . ?
C66 C67 C71 N2 179.8(4) . . . . ?
C68 C67 C71 C72 -179.7(4) . . . . ?
C66 C67 C71 C72 -1.0(6) . . . . ?
C61 N1 C72 C64 -2.0(5) . . . . ?
Eu1 N1 C72 C64 -173.9(3) . . . . ?
C61 N1 C72 C71 178.8(3) . . . . ?
Eu1 N1 C72 C71 6.9(4) . . . . ?
C63 C64 C72 N1 2.6(6) . . . . ?
C65 C64 C72 N1 -177.4(4) . . . . ?
C63 C64 C72 C71 -178.3(4) . . . . ?
C65 C64 C72 C71 1.7(6) . . . . ?
N2 C71 C72 N1 -2.3(5) . . . . ?
C67 C71 C72 N1 178.5(3) . . . . ?
N2 C71 C72 C64 178.5(3) . . . . ?
C67 C71 C72 C64 -0.7(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C9 H9A O41 0.93 2.66 3.553(6) 162.2 2_545 yes
C61 H61A O23 0.93 2.28 2.936(4) 126.8 . yes
C70 H70A O44 0.93 2.41 2.982(5) 119.3 . yes
O61 H611 O71 0.829(19) 2.12(3) 2.868(4) 151(5) . yes
O61 H612 O41 0.825(18) 2.49(4) 3.182(4) 142(5) 2_645 yes
O61 H612 O42 0.825(18) 2.07(2) 2.864(4) 162(5) 2_645 yes
O71 H711 O22 0.845(19) 2.05(3) 2.882(5) 166(7) 4_675 yes
O71 H712 O2 0.859(19) 2.58(4) 3.351(6) 150(6) 1_655 yes

_refine_diff_density_max         2.021
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.127

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_Tm-phen
_database_code_depnum_ccdc_archive 'CCDC 2013256'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  TmCF
# Clave IF-UAP:  TmCF2
# Solicitud: 289
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM)
# Clave datos : ... \BUAP\Sylvain\TmCF2\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_audit_creation_date             2019-03-20

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H29 N2 O12 Tm'
_chemical_formula_sum            'C45 H29 N2 O12 Tm'
_chemical_formula_weight         958.63
_chemical_absolute_configuration .
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3084 3.5155 '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       ?

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

_cell_length_a                   11.2098(9)
_cell_length_b                   12.9725(9)
_cell_length_c                   14.1866(9)
_cell_angle_alpha                105.184(5)
_cell_angle_beta                 91.711(6)
_cell_angle_gamma                99.498(6)
_cell_volume                     1957.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    36522
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      23.39

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_F_000             956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.126
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 2 8 0.0440
3 -2 -10 0.0820
6 2 -1 0.2260
-6 -2 1 0.1960
1 -1 1 0.0950
-1 1 -1 0.0690

_exptl_absorpt_coefficient_mu    1.256
_shelx_estimated_absorpt_T_min   0.619
_shelx_estimated_absorpt_T_max   0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3469
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA 1.86 (Stoe & Cie, 2018)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.500
_diffrn_source_power             0.0325
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1270 frames, 40-60 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            57568
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.610
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10407
_reflns_number_gt                7008
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA 1.86 (Stoe & Cie, 2018)'
_computing_cell_refinement       'X-AREA 1.86'
_computing_data_reduction        'X-AREA 1.86'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'

_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)+(0.0350P)²] 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         10407
_refine_ls_number_parameters     544
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_restrained_S_all      0.865
_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
Tm1 Tm 0.28913(2) 0.25366(2) 0.78613(2) 0.04741(6) Uani 1 1 d . . . . .
O1 O 0.0939(4) 0.6481(3) 0.7905(3) 0.0963(12) Uani 1 1 d . . . . .
O2 O -0.0222(5) 0.5774(4) 0.8884(3) 0.1307(18) Uani 1 1 d . . . . .
O3 O 0.2541(2) 0.3801(2) 0.70745(18) 0.0536(6) Uani 1 1 d . . . . .
O4 O 0.0946(3) 0.2846(2) 0.8073(2) 0.0624(7) Uani 1 1 d . . . . .
C2 C 0.0497(6) 0.5606(5) 0.8277(4) 0.0928(18) Uani 1 1 d . . . . .
C3 C 0.0990(4) 0.4618(4) 0.7919(3) 0.0659(12) Uani 1 1 d . . . . .
C4 C 0.1988(4) 0.4595(3) 0.7330(3) 0.0567(10) Uani 1 1 d . . . . .
C5 C 0.2393(4) 0.5548(3) 0.6977(3) 0.0630(11) Uani 1 1 d . . . . .
C6 C 0.3334(5) 0.5591(4) 0.6374(4) 0.0814(14) Uani 1 1 d . . . . .
H6A H 0.373585 0.500530 0.618522 0.098 Uiso 1 1 calc R U . . .
C7 C 0.3680(6) 0.6510(5) 0.6051(5) 0.109(2) Uani 1 1 d . . . . .
H7A H 0.431235 0.653837 0.564328 0.131 Uiso 1 1 calc R U . . .
C8 C 0.3086(8) 0.7387(6) 0.6333(6) 0.121(2) Uani 1 1 d . . . . .
H8A H 0.331412 0.799462 0.610413 0.145 Uiso 1 1 calc R U . . .
C9 C 0.2174(7) 0.7366(4) 0.6941(5) 0.105(2) Uani 1 1 d . . . . .
H9A H 0.178368 0.795884 0.713509 0.127 Uiso 1 1 calc R U . . .
C10 C 0.1830(5) 0.6446(4) 0.7269(4) 0.0812(15) Uani 1 1 d . . . . .
C11 C 0.0438(4) 0.3644(5) 0.8177(3) 0.0704(13) Uani 1 1 d . . . . .
C12 C -0.0810(5) 0.3503(6) 0.8549(5) 0.119(2) Uani 1 1 d . . . . .
H12A H -0.111223 0.274484 0.846344 0.178 Uiso 1 1 calc R U . . .
H12B H -0.134737 0.379175 0.818753 0.178 Uiso 1 1 calc R U . . .
H12C H -0.076532 0.388210 0.923114 0.178 Uiso 1 1 calc R U . . .
O21 O 0.1300(3) -0.1451(2) 0.4446(2) 0.0741(8) Uani 1 1 d . . . . .
O22 O 0.2992(4) -0.0779(3) 0.3937(3) 0.1045(13) Uani 1 1 d . . . . .
O23 O 0.1690(2) 0.0942(2) 0.70247(18) 0.0582(7) Uani 1 1 d . . . . .
O24 O 0.3578(3) 0.1924(2) 0.63410(18) 0.0598(7) Uani 1 1 d . . . . .
C22 C 0.2318(5) -0.0650(4) 0.4587(3) 0.0708(12) Uani 1 1 d . . . . .
C23 C 0.2462(4) 0.0236(3) 0.5474(3) 0.0548(9) Uani 1 1 d . . . . .
C24 C 0.1606(4) 0.0240(3) 0.6203(3) 0.0505(9) Uani 1 1 d . . . . .
C25 C 0.0551(4) -0.0642(3) 0.5988(3) 0.0505(9) Uani 1 1 d . . . . .
C26 C -0.0359(4) -0.0680(3) 0.6619(3) 0.0651(11) Uani 1 1 d . . . . .
H26A H -0.030206 -0.014213 0.720796 0.078 Uiso 1 1 calc R U . . .
C27 C -0.1349(5) -0.1508(4) 0.6383(4) 0.0821(14) Uani 1 1 d . . . . .
H27A H -0.195522 -0.153505 0.681350 0.099 Uiso 1 1 calc R U . . .
C28 C -0.1437(5) -0.2303(4) 0.5499(4) 0.0826(15) Uani 1 1 d . . . . .
H28A H -0.210613 -0.286277 0.534138 0.099 Uiso 1 1 calc R U . . .
C29 C -0.0560(5) -0.2275(4) 0.4859(4) 0.0765(13) Uani 1 1 d . . . . .
H29A H -0.062933 -0.280550 0.426481 0.092 Uiso 1 1 calc R U . . .
C30 C 0.0439(4) -0.1442(3) 0.5109(3) 0.0581(10) Uani 1 1 d . . . . .
C31 C 0.3434(4) 0.1144(3) 0.5596(3) 0.0565(10) Uani 1 1 d . . . . .
C32 C 0.4317(5) 0.1252(4) 0.4836(3) 0.0826(15) Uani 1 1 d . . . . .
H32A H 0.488430 0.192134 0.506933 0.124 Uiso 1 1 calc R U . . .
H32B H 0.388450 0.125063 0.424114 0.124 Uiso 1 1 calc R U . . .
H32C H 0.474663 0.065429 0.471201 0.124 Uiso 1 1 calc R U . . .
O41 O 0.6412(3) 0.6510(2) 0.8194(3) 0.0769(9) Uani 1 1 d . . . . .
O42 O 0.5142(3) 0.7179(2) 0.9224(3) 0.0885(10) Uani 1 1 d . . . . .
O43 O 0.4831(2) 0.33660(19) 0.79266(19) 0.0547(6) Uani 1 1 d . . . . .
O44 O 0.3219(2) 0.4110(2) 0.91308(17) 0.0525(6) Uani 1 1 d . . . . .
C42 C 0.5417(4) 0.6349(3) 0.8729(3) 0.0640(11) Uani 1 1 d . . . . .
C43 C 0.4830(4) 0.5242(3) 0.8655(3) 0.0494(9) Uani 1 1 d . . . . .
C44 C 0.5268(4) 0.4360(3) 0.8031(3) 0.0512(9) Uani 1 1 d . . . . .
C45 C 0.6321(4) 0.4596(3) 0.7489(3) 0.0546(9) Uani 1 1 d . . . . .
C46 C 0.6809(4) 0.3784(4) 0.6842(3) 0.0692(12) Uani 1 1 d . . . . .
H46A H 0.646333 0.305961 0.675560 0.083 Uiso 1 1 calc R U . . .
C47 C 0.7787(5) 0.4039(4) 0.6334(4) 0.0856(15) Uani 1 1 d . . . . .
H47A H 0.809890 0.349182 0.590483 0.103 Uiso 1 1 calc R U . . .
C48 C 0.8310(5) 0.5123(5) 0.6466(4) 0.0939(17) Uani 1 1 d . . . . .
H48A H 0.898295 0.529815 0.613230 0.113 Uiso 1 1 calc R U . . .
C49 C 0.7843(5) 0.5930(5) 0.7080(4) 0.0886(16) Uani 1 1 d . . . . .
H49A H 0.818847 0.665278 0.715815 0.106 Uiso 1 1 calc R U . . .
C50 C 0.6845(4) 0.5668(4) 0.7589(3) 0.0663(11) Uani 1 1 d . . . . .
C51 C 0.3816(4) 0.5043(3) 0.9222(3) 0.0512(9) Uani 1 1 d . . . . .
C52 C 0.3368(4) 0.5942(3) 0.9957(3) 0.0683(12) Uani 1 1 d . . . . .
H52A H 0.282040 0.563381 1.035888 0.102 Uiso 1 1 calc R U . . .
H52B H 0.295336 0.634521 0.961612 0.102 Uiso 1 1 calc R U . . .
H52C H 0.404526 0.641842 1.036168 0.102 Uiso 1 1 calc R U . . .
N61 N 0.4067(3) 0.1177(2) 0.8203(2) 0.0551(8) Uani 1 1 d . . . . .
C62 C 0.5011(4) 0.0888(3) 0.7733(3) 0.0624(11) Uani 1 1 d . . . . .
H62A H 0.536313 0.130838 0.734064 0.075 Uiso 1 1 calc R U . . .
C63 C 0.5508(4) -0.0012(4) 0.7794(3) 0.0704(12) Uani 1 1 d . . . . .
H63A H 0.618988 -0.016879 0.746598 0.084 Uiso 1 1 calc R U . . .
C64 C 0.4985(5) -0.0654(4) 0.8336(3) 0.0717(13) Uani 1 1 d . . . . .
H64A H 0.529028 -0.127060 0.836529 0.086 Uiso 1 1 calc R U . . .
C65 C 0.3982(4) -0.0390(3) 0.8854(3) 0.0612(11) Uani 1 1 d . . . . .
C66 C 0.3407(5) -0.0999(4) 0.9469(4) 0.0765(13) Uani 1 1 d . . . . .
H66A H 0.365924 -0.163758 0.950109 0.092 Uiso 1 1 calc R U . . .
C67 C 0.2500(5) -0.0661(4) 1.0007(4) 0.0755(13) Uani 1 1 d . . . . .
H67A H 0.212299 -0.108521 1.038747 0.091 Uiso 1 1 calc R U . . .
C68 C 0.2106(4) 0.0328(3) 1.0004(3) 0.0595(10) Uani 1 1 d . . . . .
C69 C 0.1259(4) 0.0768(4) 1.0623(3) 0.0685(12) Uani 1 1 d . . . . .
H69A H 0.089874 0.039979 1.105189 0.082 Uiso 1 1 calc R U . . .
C70 C 0.0967(4) 0.1740(4) 1.0593(3) 0.0704(12) Uani 1 1 d . . . . .
H70A H 0.043012 0.205463 1.101671 0.084 Uiso 1 1 calc R U . . .
C71 C 0.1484(4) 0.2251(3) 0.9919(3) 0.0623(11) Uani 1 1 d . . . . .
H71A H 0.126875 0.290802 0.990019 0.075 Uiso 1 1 calc R U . . .
N72 N 0.2265(3) 0.1858(2) 0.9303(2) 0.0523(8) Uani 1 1 d . . . . .
C73 C 0.2609(4) 0.0922(3) 0.9363(3) 0.0524(9) Uani 1 1 d . . . . .
C74 C 0.3570(4) 0.0559(3) 0.8782(3) 0.0503(9) Uani 1 1 d . . . . .


_geom_special_details            ?

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
Tm1 O43 2.249(3) . ?
Tm1 O23 2.280(2) . ?
Tm1 O3 2.289(2) . ?
Tm1 O4 2.297(3) . ?
Tm1 O24 2.297(3) . ?
Tm1 O44 2.309(2) . ?
Tm1 N61 2.502(3) . ?
Tm1 N72 2.505(3) . ?
O1 C10 1.364(7) . ?
O1 C2 1.399(7) . ?
O2 C2 1.199(6) . ?
O3 C4 1.266(5) . ?
O4 C11 1.240(5) . ?
C2 C3 1.454(7) . ?
C3 C4 1.416(6) . ?
C3 C11 1.452(7) . ?
C4 C5 1.462(6) . ?
C5 C6 1.382(7) . ?
C5 C10 1.390(6) . ?
C6 C7 1.388(7) . ?
C6 H6A 0.9300 . ?
C7 C8 1.388(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.358(9) . ?
C8 H8A 0.9300 . ?
C9 C10 1.393(8) . ?
C9 H9A 0.9300 . ?
C11 C12 1.510(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.366(5) . ?
O21 C22 1.381(5) . ?
O22 C22 1.205(5) . ?
O23 C24 1.267(4) . ?
O24 C31 1.242(4) . ?
C22 C23 1.449(6) . ?
C23 C24 1.431(5) . ?
C23 C31 1.437(6) . ?
C24 C25 1.466(5) . ?
C25 C26 1.381(6) . ?
C25 C30 1.385(5) . ?
C26 C27 1.376(6) . ?
C26 H26A 0.9300 . ?
C27 C28 1.389(7) . ?
C27 H27A 0.9300 . ?
C28 C29 1.360(7) . ?
C28 H28A 0.9300 . ?
C29 C30 1.387(6) . ?
C29 H29A 0.9300 . ?
C31 C32 1.503(6) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.369(5) . ?
O41 C42 1.385(5) . ?
O42 C42 1.214(5) . ?
O43 C44 1.270(4) . ?
O44 C51 1.255(4) . ?
C42 C43 1.453(5) . ?
C43 C44 1.419(5) . ?
C43 C51 1.439(6) . ?
C44 C45 1.462(6) . ?
C45 C50 1.385(6) . ?
C45 C46 1.401(6) . ?
C46 C47 1.373(6) . ?
C46 H46A 0.9300 . ?
C47 C48 1.393(7) . ?
C47 H47A 0.9300 . ?
C48 C49 1.364(7) . ?
C48 H48A 0.9300 . ?
C49 C50 1.393(7) . ?
C49 H49A 0.9300 . ?
C51 C52 1.513(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N61 C62 1.321(5) . ?
N61 C74 1.361(5) . ?
C62 C63 1.395(6) . ?
C62 H62A 0.9300 . ?
C63 C64 1.353(6) . ?
C63 H63A 0.9300 . ?
C64 C65 1.402(6) . ?
C64 H64A 0.9300 . ?
C65 C74 1.411(5) . ?
C65 C66 1.424(6) . ?
C66 C67 1.352(7) . ?
C66 H66A 0.9300 . ?
C67 C68 1.425(6) . ?
C67 H67A 0.9300 . ?
C68 C69 1.401(6) . ?
C68 C73 1.413(5) . ?
C69 C70 1.365(6) . ?
C69 H69A 0.9300 . ?
C70 C71 1.388(6) . ?
C70 H70A 0.9300 . ?
C71 N72 1.323(5) . ?
C71 H71A 0.9300 . ?
N72 C73 1.355(5) . ?
C73 C74 1.442(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O43 Tm1 O23 138.10(9) . . ?
O43 Tm1 O3 82.89(9) . . ?
O23 Tm1 O3 106.28(9) . . ?
O43 Tm1 O4 143.41(10) . . ?
O23 Tm1 O4 75.43(10) . . ?
O3 Tm1 O4 70.93(10) . . ?
O43 Tm1 O24 72.75(9) . . ?
O23 Tm1 O24 70.16(9) . . ?
O3 Tm1 O24 76.40(9) . . ?
O4 Tm1 O24 122.56(10) . . ?
O43 Tm1 O44 71.03(9) . . ?
O23 Tm1 O44 150.41(10) . . ?
O3 Tm1 O44 78.16(9) . . ?
O4 Tm1 O44 78.75(10) . . ?
O24 Tm1 O44 137.71(9) . . ?
O43 Tm1 N61 76.82(10) . . ?
O23 Tm1 N61 78.51(10) . . ?
O3 Tm1 N61 152.91(10) . . ?
O4 Tm1 N61 134.87(11) . . ?
O24 Tm1 N61 80.53(10) . . ?
O44 Tm1 N61 111.15(9) . . ?
O43 Tm1 N72 116.69(10) . . ?
O23 Tm1 N72 81.99(10) . . ?
O3 Tm1 N72 140.96(10) . . ?
O4 Tm1 N72 74.72(10) . . ?
O24 Tm1 N72 139.81(10) . . ?
O44 Tm1 N72 77.46(9) . . ?
N61 Tm1 N72 65.59(10) . . ?
C10 O1 C2 122.6(4) . . ?
C4 O3 Tm1 130.7(2) . . ?
C11 O4 Tm1 135.5(3) . . ?
O2 C2 O1 115.5(5) . . ?
O2 C2 C3 127.5(6) . . ?
O1 C2 C3 116.9(5) . . ?
C4 C3 C11 120.1(4) . . ?
C4 C3 C2 121.2(5) . . ?
C11 C3 C2 118.7(5) . . ?
O3 C4 C3 124.7(4) . . ?
O3 C4 C5 117.8(4) . . ?
C3 C4 C5 117.5(4) . . ?
C6 C5 C10 118.8(5) . . ?
C6 C5 C4 122.0(4) . . ?
C10 C5 C4 119.2(5) . . ?
C5 C6 C7 119.9(5) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C8 C7 C6 120.3(7) . . ?
C8 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
C9 C8 C7 120.6(6) . . ?
C9 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
C8 C9 C10 119.1(6) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
O1 C10 C5 121.9(5) . . ?
O1 C10 C9 116.8(5) . . ?
C5 C10 C9 121.3(6) . . ?
O4 C11 C3 122.1(4) . . ?
O4 C11 C12 114.8(5) . . ?
C3 C11 C12 123.1(5) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 122.8(3) . . ?
C24 O23 Tm1 139.4(3) . . ?
C31 O24 Tm1 143.4(3) . . ?
O22 C22 O21 114.6(4) . . ?
O22 C22 C23 127.4(5) . . ?
O21 C22 C23 118.0(4) . . ?
C24 C23 C31 119.8(3) . . ?
C24 C23 C22 120.5(4) . . ?
C31 C23 C22 119.6(4) . . ?
O23 C24 C23 125.3(4) . . ?
O23 C24 C25 117.2(4) . . ?
C23 C24 C25 117.5(3) . . ?
C26 C25 C30 118.8(4) . . ?
C26 C25 C24 122.0(3) . . ?
C30 C25 C24 119.2(4) . . ?
C27 C26 C25 120.4(4) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C28 119.7(5) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
C29 C28 C27 121.0(5) . . ?
C29 C28 H28A 119.5 . . ?
C27 C28 H28A 119.5 . . ?
C28 C29 C30 118.9(4) . . ?
C28 C29 H29A 120.6 . . ?
C30 C29 H29A 120.6 . . ?
O21 C30 C25 121.9(4) . . ?
O21 C30 C29 116.8(4) . . ?
C25 C30 C29 121.3(4) . . ?
O24 C31 C23 121.4(4) . . ?
O24 C31 C32 114.9(4) . . ?
C23 C31 C32 123.6(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.5(3) . . ?
C44 O43 Tm1 129.9(2) . . ?
C51 O44 Tm1 132.9(2) . . ?
O42 C42 O41 114.4(4) . . ?
O42 C42 C43 127.2(5) . . ?
O41 C42 C43 118.4(4) . . ?
C44 C43 C51 120.2(3) . . ?
C44 C43 C42 119.8(4) . . ?
C51 C43 C42 120.0(4) . . ?
O43 C44 C43 124.7(4) . . ?
O43 C44 C45 116.8(3) . . ?
C43 C44 C45 118.6(3) . . ?
C50 C45 C46 118.0(4) . . ?
C50 C45 C44 119.1(4) . . ?
C46 C45 C44 122.9(4) . . ?
C47 C46 C45 121.2(4) . . ?
C47 C46 H46A 119.4 . . ?
C45 C46 H46A 119.4 . . ?
C46 C47 C48 119.5(5) . . ?
C46 C47 H47A 120.2 . . ?
C48 C47 H47A 120.2 . . ?
C49 C48 C47 120.5(5) . . ?
C49 C48 H48A 119.8 . . ?
C47 C48 H48A 119.8 . . ?
C48 C49 C50 119.8(5) . . ?
C48 C49 H49A 120.1 . . ?
C50 C49 H49A 120.1 . . ?
O41 C50 C45 121.6(4) . . ?
O41 C50 C49 117.3(4) . . ?
C45 C50 C49 121.1(5) . . ?
O44 C51 C43 122.6(3) . . ?
O44 C51 C52 114.7(4) . . ?
C43 C51 C52 122.7(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C62 N61 C74 117.4(3) . . ?
C62 N61 Tm1 124.5(3) . . ?
C74 N61 Tm1 117.0(3) . . ?
N61 C62 C63 123.6(4) . . ?
N61 C62 H62A 118.2 . . ?
C63 C62 H62A 118.2 . . ?
C64 C63 C62 119.1(4) . . ?
C64 C63 H63A 120.4 . . ?
C62 C63 H63A 120.4 . . ?
C63 C64 C65 120.0(4) . . ?
C63 C64 H64A 120.0 . . ?
C65 C64 H64A 120.0 . . ?
C64 C65 C74 117.1(4) . . ?
C64 C65 C66 123.5(4) . . ?
C74 C65 C66 119.4(4) . . ?
C67 C66 C65 120.9(4) . . ?
C67 C66 H66A 119.5 . . ?
C65 C66 H66A 119.5 . . ?
C66 C67 C68 121.6(4) . . ?
C66 C67 H67A 119.2 . . ?
C68 C67 H67A 119.2 . . ?
C69 C68 C73 117.3(4) . . ?
C69 C68 C67 123.7(4) . . ?
C73 C68 C67 119.0(4) . . ?
C70 C69 C68 119.6(4) . . ?
C70 C69 H69A 120.2 . . ?
C68 C69 H69A 120.2 . . ?
C69 C70 C71 118.9(4) . . ?
C69 C70 H70A 120.5 . . ?
C71 C70 H70A 120.5 . . ?
N72 C71 C70 123.8(4) . . ?
N72 C71 H71A 118.1 . . ?
C70 C71 H71A 118.1 . . ?
C71 N72 C73 117.6(3) . . ?
C71 N72 Tm1 124.7(3) . . ?
C73 N72 Tm1 116.9(2) . . ?
N72 C73 C68 122.6(4) . . ?
N72 C73 C74 118.0(3) . . ?
C68 C73 C74 119.3(3) . . ?
N61 C74 C65 122.7(4) . . ?
N61 C74 C73 117.7(3) . . ?
C65 C74 C73 119.5(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 174.8(5) . . . . ?
C10 O1 C2 C3 -3.0(7) . . . . ?
O2 C2 C3 C4 -168.8(6) . . . . ?
O1 C2 C3 C4 8.6(7) . . . . ?
O2 C2 C3 C11 11.2(8) . . . . ?
O1 C2 C3 C11 -171.4(4) . . . . ?
Tm1 O3 C4 C3 -31.6(6) . . . . ?
Tm1 O3 C4 C5 149.6(3) . . . . ?
C11 C3 C4 O3 -7.5(6) . . . . ?
C2 C3 C4 O3 172.5(4) . . . . ?
C11 C3 C4 C5 171.4(4) . . . . ?
C2 C3 C4 C5 -8.7(6) . . . . ?
O3 C4 C5 C6 0.9(6) . . . . ?
C3 C4 C5 C6 -178.0(4) . . . . ?
O3 C4 C5 C10 -178.0(4) . . . . ?
C3 C4 C5 C10 3.1(6) . . . . ?
C10 C5 C6 C7 -1.7(7) . . . . ?
C4 C5 C6 C7 179.4(5) . . . . ?
C5 C6 C7 C8 0.2(9) . . . . ?
C6 C7 C8 C9 1.1(11) . . . . ?
C7 C8 C9 C10 -0.8(10) . . . . ?
C2 O1 C10 C5 -2.5(7) . . . . ?
C2 O1 C10 C9 178.9(5) . . . . ?
C6 C5 C10 O1 -176.5(4) . . . . ?
C4 C5 C10 O1 2.4(6) . . . . ?
C6 C5 C10 C9 2.0(7) . . . . ?
C4 C5 C10 C9 -179.1(4) . . . . ?
C8 C9 C10 O1 177.8(5) . . . . ?
C8 C9 C10 C5 -0.8(9) . . . . ?
Tm1 O4 C11 C3 17.4(6) . . . . ?
Tm1 O4 C11 C12 -165.0(4) . . . . ?
C4 C3 C11 O4 15.0(6) . . . . ?
C2 C3 C11 O4 -165.0(4) . . . . ?
C4 C3 C11 C12 -162.4(5) . . . . ?
C2 C3 C11 C12 17.6(7) . . . . ?
C30 O21 C22 O22 179.7(4) . . . . ?
C30 O21 C22 C23 -0.5(6) . . . . ?
O22 C22 C23 C24 -176.7(5) . . . . ?
O21 C22 C23 C24 3.6(6) . . . . ?
O22 C22 C23 C31 6.7(8) . . . . ?
O21 C22 C23 C31 -173.0(4) . . . . ?
Tm1 O23 C24 C23 5.3(6) . . . . ?
Tm1 O23 C24 C25 -175.1(3) . . . . ?
C31 C23 C24 O23 -7.7(6) . . . . ?
C22 C23 C24 O23 175.8(4) . . . . ?
C31 C23 C24 C25 172.7(4) . . . . ?
C22 C23 C24 C25 -3.9(6) . . . . ?
O23 C24 C25 C26 3.9(6) . . . . ?
C23 C24 C25 C26 -176.5(4) . . . . ?
O23 C24 C25 C30 -178.4(3) . . . . ?
C23 C24 C25 C30 1.2(5) . . . . ?
C30 C25 C26 C27 0.9(6) . . . . ?
C24 C25 C26 C27 178.6(4) . . . . ?
C25 C26 C27 C28 -0.7(7) . . . . ?
C26 C27 C28 C29 -0.1(8) . . . . ?
C27 C28 C29 C30 0.7(8) . . . . ?
C22 O21 C30 C25 -2.2(6) . . . . ?
C22 O21 C30 C29 177.7(4) . . . . ?
C26 C25 C30 O21 179.5(4) . . . . ?
C24 C25 C30 O21 1.8(6) . . . . ?
C26 C25 C30 C29 -0.4(6) . . . . ?
C24 C25 C30 C29 -178.1(4) . . . . ?
C28 C29 C30 O21 179.6(4) . . . . ?
C28 C29 C30 C25 -0.5(7) . . . . ?
Tm1 O24 C31 C23 6.6(7) . . . . ?
Tm1 O24 C31 C32 -175.6(3) . . . . ?
C24 C23 C31 O24 2.5(6) . . . . ?
C22 C23 C31 O24 179.2(4) . . . . ?
C24 C23 C31 C32 -175.1(4) . . . . ?
C22 C23 C31 C32 1.5(6) . . . . ?
C50 O41 C42 O42 -179.5(4) . . . . ?
C50 O41 C42 C43 1.1(6) . . . . ?
O42 C42 C43 C44 179.6(4) . . . . ?
O41 C42 C43 C44 -1.1(5) . . . . ?
O42 C42 C43 C51 -1.1(6) . . . . ?
O41 C42 C43 C51 178.2(3) . . . . ?
Tm1 O43 C44 C43 38.6(5) . . . . ?
Tm1 O43 C44 C45 -143.6(3) . . . . ?
C51 C43 C44 O43 -0.5(6) . . . . ?
C42 C43 C44 O43 178.9(4) . . . . ?
C51 C43 C44 C45 -178.3(3) . . . . ?
C42 C43 C44 C45 1.0(5) . . . . ?
O43 C44 C45 C50 -179.0(3) . . . . ?
C43 C44 C45 C50 -1.0(5) . . . . ?
O43 C44 C45 C46 3.1(6) . . . . ?
C43 C44 C45 C46 -178.9(4) . . . . ?
C50 C45 C46 C47 1.0(7) . . . . ?
C44 C45 C46 C47 178.9(4) . . . . ?
C45 C46 C47 C48 0.3(8) . . . . ?
C46 C47 C48 C49 -1.3(9) . . . . ?
C47 C48 C49 C50 0.9(9) . . . . ?
C42 O41 C50 C45 -1.1(6) . . . . ?
C42 O41 C50 C49 179.3(4) . . . . ?
C46 C45 C50 O41 179.0(4) . . . . ?
C44 C45 C50 O41 1.0(6) . . . . ?
C46 C45 C50 C49 -1.4(6) . . . . ?
C44 C45 C50 C49 -179.4(4) . . . . ?
C48 C49 C50 O41 -179.9(5) . . . . ?
C48 C49 C50 C45 0.5(8) . . . . ?
Tm1 O44 C51 C43 -24.8(5) . . . . ?
Tm1 O44 C51 C52 153.9(3) . . . . ?
C44 C43 C51 O44 -6.2(5) . . . . ?
C42 C43 C51 O44 174.5(3) . . . . ?
C44 C43 C51 C52 175.2(3) . . . . ?
C42 C43 C51 C52 -4.2(5) . . . . ?
C74 N61 C62 C63 0.6(6) . . . . ?
Tm1 N61 C62 C63 -167.0(3) . . . . ?
N61 C62 C63 C64 2.1(7) . . . . ?
C62 C63 C64 C65 -2.1(7) . . . . ?
C63 C64 C65 C74 -0.4(6) . . . . ?
C63 C64 C65 C66 -177.6(4) . . . . ?
C64 C65 C66 C67 175.1(5) . . . . ?
C74 C65 C66 C67 -2.1(7) . . . . ?
C65 C66 C67 C68 -1.9(8) . . . . ?
C66 C67 C68 C69 -173.2(5) . . . . ?
C66 C67 C68 C73 5.3(7) . . . . ?
C73 C68 C69 C70 -0.7(6) . . . . ?
C67 C68 C69 C70 177.8(5) . . . . ?
C68 C69 C70 C71 2.5(7) . . . . ?
C69 C70 C71 N72 -0.8(7) . . . . ?
C70 C71 N72 C73 -2.6(6) . . . . ?
C70 C71 N72 Tm1 166.9(3) . . . . ?
C71 N72 C73 C68 4.4(5) . . . . ?
Tm1 N72 C73 C68 -165.9(3) . . . . ?
C71 N72 C73 C74 -172.4(3) . . . . ?
Tm1 N72 C73 C74 17.3(4) . . . . ?
C69 C68 C73 N72 -2.8(6) . . . . ?
C67 C68 C73 N72 178.6(4) . . . . ?
C69 C68 C73 C74 173.9(4) . . . . ?
C67 C68 C73 C74 -4.6(6) . . . . ?
C62 N61 C74 C65 -3.3(6) . . . . ?
Tm1 N61 C74 C65 165.2(3) . . . . ?
C62 N61 C74 C73 174.7(4) . . . . ?
Tm1 N61 C74 C73 -16.8(4) . . . . ?
C64 C65 C74 N61 3.2(6) . . . . ?
C66 C65 C74 N61 -179.4(4) . . . . ?
C64 C65 C74 C73 -174.7(4) . . . . ?
C66 C65 C74 C73 2.6(6) . . . . ?
N72 C73 C74 N61 -0.4(5) . . . . ?
C68 C73 C74 N61 -177.3(3) . . . . ?
N72 C73 C74 C65 177.7(3) . . . . ?
C68 C73 C74 C65 0.8(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C52 H52C O43 0.96 2.63 3.395(5) 137.1 2_667 yes
C71 H71A O2 0.93 2.55 3.242(6) 131.3 2_567 yes

_refine_diff_density_max         1.252
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.081

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_Dy-batho
_database_code_depnum_ccdc_archive 'CCDC 2013259'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  Dy(Cum)3BF
# Clave IF-UAP:  DyCum3BF
# Solicitud: 387
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM)
# Clave datos : ... \BUAP\Sylvain\DyCum3BF\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_audit_creation_date             2019-10-07

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H37 Dy N2 O12, 0.7(C2 H6 O)'
_chemical_formula_sum            'C58.40 H41.20 Dy N2 O12.70'
_chemical_formula_weight         1136.63
_chemical_absolute_configuration ?
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.3302 2.9404 '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       ?

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

_cell_length_a                   11.6542(3)
_cell_length_b                   13.2784(4)
_cell_length_c                   18.3379(6)
_cell_angle_alpha                78.449(2)
_cell_angle_beta                 76.214(2)
_cell_angle_gamma                68.738(2)
_cell_volume                     2548.04(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    61416
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      28.67

_exptl_crystal_recrystallization_method 
;
Re-crystallisation from solvent: ethanol
;

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_F_000             1146
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.081
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 5 -6 0.0340
3 -3 4 0.0460
0 -1 -2 0.0740
0 1 2 0.0750
4 7 -1 0.3900
-3 -5 1 0.3410

_exptl_absorpt_coefficient_mu    0.829
_shelx_estimated_absorpt_T_min   0.636
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3556
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA 1.86 (Stoe & Cie, 2018)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.55
_diffrn_source_power             0.03575
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1072 frames, 50 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            76435
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.662
_diffrn_reflns_theta_max         24.000
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             16269
_reflns_number_gt                11299
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA 1.86 (Stoe & Cie, 2018)'
_computing_cell_refinement       'X-AREA 1.86'
_computing_data_reduction        'X-AREA 1.86'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'

_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)+(0.0406P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16269
_refine_ls_number_parameters     681
_refine_ls_number_restraints     37
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_restrained_S_all      0.922
_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
Dy1 Dy 0.40860(2) 0.36212(2) 0.31619(2) 0.04275(4) Uani 1 1 d . . . . .
O1 O 0.3067(3) 0.0647(2) 0.59365(13) 0.0741(7) Uani 1 1 d . . . . .
O2 O 0.3832(3) 0.1560(2) 0.64363(14) 0.0898(8) Uani 1 1 d . . . . .
O3 O 0.4112(2) 0.19492(18) 0.37848(12) 0.0620(6) Uani 1 1 d . . . . .
O4 O 0.46563(19) 0.33536(17) 0.43592(12) 0.0540(5) Uani 1 1 d . . . . .
C2 C 0.3667(3) 0.1396(3) 0.58487(19) 0.0635(8) Uani 1 1 d . . . . .
C3 C 0.4010(3) 0.1908(2) 0.50937(16) 0.0482(6) Uani 1 1 d . . . . .
C4 C 0.3785(3) 0.1592(2) 0.44642(17) 0.0490(6) Uani 1 1 d . . . . .
C5 C 0.3131(3) 0.0796(2) 0.46013(18) 0.0546(7) Uani 1 1 d . . . . .
C6 C 0.2817(4) 0.0491(3) 0.4014(2) 0.0715(9) Uani 1 1 d . . . . .
H6 H 0.306816 0.075971 0.351577 0.086 Uiso 1 1 calc R U . . .
C7 C 0.2131(5) -0.0214(3) 0.4168(3) 0.0888(13) Uani 1 1 d . . . . .
H7 H 0.192077 -0.042036 0.377511 0.107 Uiso 1 1 calc R U . . .
C8 C 0.1764(5) -0.0602(3) 0.4906(3) 0.0965(14) Uani 1 1 d . . . . .
H8 H 0.128889 -0.106233 0.501073 0.116 Uiso 1 1 calc R U . . .
C9 C 0.2087(5) -0.0323(3) 0.5494(3) 0.0923(13) Uani 1 1 d . . . . .
H9 H 0.184847 -0.060540 0.599020 0.111 Uiso 1 1 calc R U . . .
C10 C 0.2768(3) 0.0380(3) 0.5340(2) 0.0637(8) Uani 1 1 d . . . . .
C11 C 0.4569(3) 0.2745(2) 0.49764(16) 0.0501(6) Uani 1 1 d . . . . .
C12 C 0.5090(4) 0.2945(3) 0.5589(2) 0.0738(10) Uani 1 1 d . . . . .
H12A H 0.566749 0.227371 0.577949 0.111 Uiso 1 1 calc R U . . .
H12B H 0.441776 0.322273 0.599333 0.111 Uiso 1 1 calc R U . . .
H12C H 0.551568 0.346582 0.538622 0.111 Uiso 1 1 calc R U . . .
O21 O -0.1462(2) 0.57802(19) 0.43193(15) 0.0683(6) Uani 1 1 d . . . . .
O22 O -0.0808(3) 0.7116(2) 0.4350(2) 0.0985(10) Uani 1 1 d . . . . .
O23 O 0.2024(2) 0.38253(19) 0.34566(16) 0.0763(7) Uani 1 1 d . . . . .
O24 O 0.29166(19) 0.53346(17) 0.35765(13) 0.0569(5) Uani 1 1 d . . . . .
C22 C -0.0490(3) 0.6206(3) 0.4198(2) 0.0633(8) Uani 1 1 d . . . . .
C23 C 0.0778(3) 0.5522(2) 0.38999(17) 0.0508(6) Uani 1 1 d . . . . .
C24 C 0.0972(3) 0.4479(2) 0.37230(18) 0.0534(7) Uani 1 1 d . . . . .
C25 C -0.0107(3) 0.4113(3) 0.38407(18) 0.0537(7) Uani 1 1 d . . . . .
C26 C 0.0020(3) 0.3099(3) 0.3662(2) 0.0629(8) Uani 1 1 d . . . . .
H26 H 0.080478 0.264214 0.346409 0.076 Uiso 1 1 calc R U . . .
C27 C -0.1013(3) 0.2773(3) 0.3779(2) 0.0673(9) Uani 1 1 d . . . . .
H27 H -0.092823 0.210202 0.365262 0.081 Uiso 1 1 calc R U . . .
C28 C -0.2178(3) 0.3451(3) 0.4085(2) 0.0726(10) Uani 1 1 d . . . . .
H28 H -0.287437 0.322993 0.416387 0.087 Uiso 1 1 calc R U . . .
C29 C -0.2316(3) 0.4438(3) 0.4271(2) 0.0721(10) Uani 1 1 d . . . . .
H29 H -0.309958 0.488271 0.448235 0.086 Uiso 1 1 calc R U . . .
C30 C -0.1278(3) 0.4776(3) 0.41432(19) 0.0580(8) Uani 1 1 d . . . . .
C31 C 0.1803(3) 0.5918(2) 0.37832(17) 0.0503(6) Uani 1 1 d . . . . .
C32 C 0.1623(4) 0.7072(3) 0.3885(3) 0.0776(11) Uani 1 1 d . . . . .
H32A H 0.119219 0.720737 0.439005 0.116 Uiso 1 1 calc R U . . .
H32B H 0.113718 0.757353 0.352796 0.116 Uiso 1 1 calc R U . . .
H32C H 0.242455 0.716627 0.380184 0.116 Uiso 1 1 calc R U . . .
O41 O 0.2418(2) 0.4900(2) 0.01399(14) 0.0801(7) Uani 1 1 d . . . . .
O42 O 0.1779(3) 0.3513(3) 0.05947(16) 0.1013(10) Uani 1 1 d . . . . .
O43 O 0.3921(2) 0.46426(18) 0.19962(12) 0.0621(6) Uani 1 1 d . . . . .
O44 O 0.3846(2) 0.26272(17) 0.23200(12) 0.0581(5) Uani 1 1 d . . . . .
C42 C 0.2378(3) 0.4035(4) 0.0688(2) 0.0720(10) Uani 1 1 d . . . . .
C43 C 0.3026(3) 0.3852(3) 0.13174(17) 0.0544(7) Uani 1 1 d . . . . .
C44 C 0.3500(3) 0.4652(3) 0.14155(17) 0.0546(7) Uani 1 1 d . . . . .
C45 C 0.3576(3) 0.5515(3) 0.07848(17) 0.0584(7) Uani 1 1 d . . . . .
C46 C 0.4199(4) 0.6228(3) 0.0772(2) 0.0688(9) Uani 1 1 d . . . . .
H46 H 0.455223 0.619135 0.118461 0.083 Uiso 1 1 calc R U . . .
C47 C 0.4301(4) 0.6997(3) 0.0150(2) 0.0793(11) Uani 1 1 d . . . . .
H47 H 0.473886 0.746421 0.013811 0.095 Uiso 1 1 calc R U . . .
C48 C 0.3745(4) 0.7063(3) -0.0456(2) 0.0867(13) Uani 1 1 d . . . . .
H48 H 0.379962 0.758619 -0.087186 0.104 Uiso 1 1 calc R U . . .
C49 C 0.3119(4) 0.6371(4) -0.0449(2) 0.0856(12) Uani 1 1 d . . . . .
H49 H 0.275014 0.642118 -0.085816 0.103 Uiso 1 1 calc R U . . .
C50 C 0.3035(3) 0.5595(3) 0.01669(18) 0.0667(9) Uani 1 1 d . . . . .
C51 C 0.3285(3) 0.2823(3) 0.17840(18) 0.0567(7) Uani 1 1 d . . . . .
C52 C 0.2978(5) 0.1885(3) 0.1633(3) 0.0969(15) Uani 1 1 d . . . . .
H52A H 0.324750 0.179774 0.110514 0.145 Uiso 1 1 calc R U . . .
H52B H 0.209001 0.202849 0.176759 0.145 Uiso 1 1 calc R U . . .
H52C H 0.339947 0.122936 0.192904 0.145 Uiso 1 1 calc R U . . .
N1 N 0.5755(2) 0.45408(18) 0.28046(13) 0.0457(5) Uani 1 1 d . . . . .
N2 N 0.6282(2) 0.24141(18) 0.26969(13) 0.0467(5) Uani 1 1 d . . . . .
C61 C 0.5494(3) 0.5592(2) 0.28511(18) 0.0551(7) Uani 1 1 d . . . . .
H61 H 0.470184 0.597143 0.309688 0.066 Uiso 1 1 calc R U . . .
C62 C 0.6334(3) 0.6152(2) 0.25546(18) 0.0552(7) Uani 1 1 d . . . . .
H62 H 0.609927 0.688422 0.261153 0.066 Uiso 1 1 calc R U . . .
C63 C 0.7517(3) 0.5632(2) 0.21754(16) 0.0486(6) Uani 1 1 d . . . . .
C64 C 0.7834(3) 0.4502(2) 0.21150(16) 0.0466(6) Uani 1 1 d . . . . .
C65 C 0.9045(3) 0.3853(2) 0.17645(17) 0.0529(7) Uani 1 1 d . . . . .
H65 H 0.965619 0.417617 0.155400 0.064 Uiso 1 1 calc R U . . .
C66 C 0.9317(3) 0.2789(3) 0.17338(18) 0.0545(7) Uani 1 1 d . . . . .
H66 H 1.011264 0.239096 0.150410 0.065 Uiso 1 1 calc R U . . .
C67 C 0.8411(2) 0.2253(2) 0.20457(16) 0.0466(6) Uani 1 1 d . . . . .
C68 C 0.8677(3) 0.1118(2) 0.20367(17) 0.0519(7) Uani 1 1 d . . . . .
C69 C 0.7741(3) 0.0688(2) 0.23580(19) 0.0587(8) Uani 1 1 d . . . . .
H69 H 0.789115 -0.005198 0.236814 0.070 Uiso 1 1 calc R U . . .
C70 C 0.6558(3) 0.1359(2) 0.26714(18) 0.0554(7) Uani 1 1 d . . . . .
H70 H 0.593250 0.104883 0.287212 0.066 Uiso 1 1 calc R U . . .
C71 C 0.7212(2) 0.2855(2) 0.23941(15) 0.0429(6) Uani 1 1 d . . . . .
C72 C 0.6923(2) 0.4004(2) 0.24378(15) 0.0427(5) Uani 1 1 d . . . . .
C73 C 0.8420(3) 0.6235(2) 0.18526(17) 0.0519(7) Uani 1 1 d . . . . .
C74 C 0.8719(3) 0.6769(3) 0.2321(2) 0.0678(9) Uani 1 1 d . . . . .
H74 H 0.835791 0.675235 0.283156 0.081 Uiso 1 1 calc R U . . .
C75 C 0.9559(4) 0.7327(3) 0.2022(3) 0.0857(12) Uani 1 1 d . . . . .
H75 H 0.976990 0.767377 0.233762 0.103 Uiso 1 1 calc R U . . .
C76 C 1.0082(4) 0.7376(3) 0.1272(3) 0.0919(13) Uani 1 1 d . . . . .
H76 H 1.065024 0.774959 0.107865 0.110 Uiso 1 1 calc R U . . .
C77 C 0.9766(4) 0.6874(3) 0.0807(3) 0.0829(11) Uani 1 1 d . . . . .
H77 H 1.010584 0.692356 0.029308 0.100 Uiso 1 1 calc R U . . .
C78 C 0.8949(3) 0.6291(3) 0.1089(2) 0.0655(8) Uani 1 1 d . . . . .
H78 H 0.875491 0.593918 0.076856 0.079 Uiso 1 1 calc R U . . .
C79 C 0.9929(3) 0.0442(3) 0.1695(3) 0.0733(10) Uani 1 1 d . . . . .
C80 C 1.0295(5) 0.0494(5) 0.0923(4) 0.134(2) Uani 1 1 d . . . . .
H80 H 0.972769 0.092998 0.061231 0.161 Uiso 1 1 calc R U . . .
C81 C 1.1476(8) -0.0083(8) 0.0605(6) 0.196(4) Uani 1 1 d . . . . .
H81 H 1.172838 -0.002761 0.008238 0.236 Uiso 1 1 calc R U . . .
C82 C 1.2291(7) -0.0751(7) 0.1072(7) 0.199(5) Uani 1 1 d . . . . .
H82 H 1.309642 -0.115165 0.085769 0.238 Uiso 1 1 calc R U . . .
C83 C 1.1957(7) -0.0840(7) 0.1825(7) 0.210(4) Uani 1 1 d . . . . .
H83 H 1.251791 -0.129447 0.213296 0.252 Uiso 1 1 calc R U . . .
C84 C 1.0738(5) -0.0230(4) 0.2139(4) 0.133(2) Uani 1 1 d . . . . .
H84 H 1.048539 -0.028982 0.266230 0.160 Uiso 1 1 calc R U . . .
C91 C 0.5898(8) -0.1073(10) 0.0911(5) 0.169(4) Uani 0.7 1 d . . P . .
H91A H 0.655323 -0.102880 0.048735 0.253 Uiso 0.7 1 calc R U P . .
H91B H 0.510882 -0.058376 0.079209 0.253 Uiso 0.7 1 calc R U P . .
H91C H 0.587602 -0.180459 0.102009 0.253 Uiso 0.7 1 calc R U P . .
C92 C 0.6121(8) -0.0793(7) 0.1527(5) 0.121(3) Uani 0.7 1 d D . P . .
H92A H 0.614484 -0.005471 0.141103 0.146 Uiso 0.7 1 calc R U P . .
H92B H 0.693616 -0.127073 0.162910 0.146 Uiso 0.7 1 calc R U P . .
O92 O 0.5200(7) -0.0857(5) 0.2192(4) 0.153(3) Uani 0.7 1 d D . P . .
H92 H 0.523513 -0.050063 0.249863 0.229 Uiso 0.7 1 calc R U P . .


_geom_special_details            ?

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 O23 2.259(2) . ?
Dy1 O3 2.277(2) . ?
Dy1 O43 2.300(2) . ?
Dy1 O44 2.344(2) . ?
Dy1 O24 2.358(2) . ?
Dy1 O4 2.367(2) . ?
Dy1 N2 2.526(2) . ?
Dy1 N1 2.549(2) . ?
O1 C10 1.368(4) . ?
O1 C2 1.375(4) . ?
O2 C2 1.212(4) . ?
O3 C4 1.261(3) . ?
O4 C11 1.258(3) . ?
C2 C3 1.448(4) . ?
C3 C4 1.413(4) . ?
C3 C11 1.438(4) . ?
C4 C5 1.465(4) . ?
C5 C10 1.383(4) . ?
C5 C6 1.389(5) . ?
C6 C7 1.387(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.373(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.377(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(5) . ?
C9 H9 0.9300 . ?
C11 C12 1.504(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.363(4) . ?
O21 C22 1.395(4) . ?
O22 C22 1.198(4) . ?
O23 C24 1.268(4) . ?
O24 C31 1.257(3) . ?
C22 C23 1.465(4) . ?
C23 C24 1.412(4) . ?
C23 C31 1.428(4) . ?
C24 C25 1.462(4) . ?
C25 C30 1.382(4) . ?
C25 C26 1.395(4) . ?
C26 C27 1.379(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.386(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.364(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.392(4) . ?
C29 H29 0.9300 . ?
C31 C32 1.513(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C42 1.374(5) . ?
O41 C50 1.374(5) . ?
O42 C42 1.205(4) . ?
O43 C44 1.271(3) . ?
O44 C51 1.241(3) . ?
C42 C43 1.460(4) . ?
C43 C44 1.419(4) . ?
C43 C51 1.430(4) . ?
C44 C45 1.467(4) . ?
C45 C46 1.380(5) . ?
C45 C50 1.391(5) . ?
C46 C47 1.383(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.388(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.361(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.379(5) . ?
C49 H49 0.9300 . ?
C51 C52 1.506(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N1 C61 1.332(3) . ?
N1 C72 1.366(3) . ?
N2 C70 1.327(4) . ?
N2 C71 1.366(3) . ?
C61 C62 1.386(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.380(4) . ?
C62 H62 0.9300 . ?
C63 C64 1.430(4) . ?
C63 C73 1.492(4) . ?
C64 C72 1.403(4) . ?
C64 C65 1.434(4) . ?
C65 C66 1.340(4) . ?
C65 H65 0.9300 . ?
C66 C67 1.429(4) . ?
C66 H66 0.9300 . ?
C67 C71 1.403(4) . ?
C67 C68 1.427(4) . ?
C68 C69 1.370(4) . ?
C68 C79 1.472(4) . ?
C69 C70 1.401(4) . ?
C69 H69 0.9300 . ?
C70 H70 0.9300 . ?
C71 C72 1.453(4) . ?
C73 C78 1.388(4) . ?
C73 C74 1.389(4) . ?
C74 C75 1.383(5) . ?
C74 H74 0.9300 . ?
C75 C76 1.365(6) . ?
C75 H75 0.9300 . ?
C76 C77 1.365(6) . ?
C76 H76 0.9300 . ?
C77 C78 1.383(5) . ?
C77 H77 0.9300 . ?
C78 H78 0.9300 . ?
C79 C84 1.346(7) . ?
C79 C80 1.374(7) . ?
C80 C81 1.361(8) . ?
C80 H80 0.9300 . ?
C81 C82 1.376(14) . ?
C81 H81 0.9300 . ?
C82 C83 1.335(14) . ?
C82 H82 0.9300 . ?
C83 C84 1.403(8) . ?
C83 H83 0.9300 . ?
C84 H84 0.9300 . ?
C91 C92 1.363(11) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C92 O92 1.430(7) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
O92 H92 0.8200 . ?

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
O23 Dy1 O3 78.21(9) . . ?
O23 Dy1 O43 93.26(10) . . ?
O3 Dy1 O43 141.44(8) . . ?
O23 Dy1 O44 76.63(8) . . ?
O3 Dy1 O44 71.82(7) . . ?
O43 Dy1 O44 69.62(7) . . ?
O23 Dy1 O24 69.54(7) . . ?
O3 Dy1 O24 127.70(8) . . ?
O43 Dy1 O24 81.67(8) . . ?
O44 Dy1 O24 133.82(7) . . ?
O23 Dy1 O4 103.22(9) . . ?
O3 Dy1 O4 69.16(7) . . ?
O43 Dy1 O4 148.52(7) . . ?
O44 Dy1 O4 140.02(7) . . ?
O24 Dy1 O4 79.34(7) . . ?
O23 Dy1 N2 147.23(8) . . ?
O3 Dy1 N2 77.07(8) . . ?
O43 Dy1 N2 92.80(8) . . ?
O44 Dy1 N2 75.43(7) . . ?
O24 Dy1 N2 143.23(7) . . ?
O4 Dy1 N2 87.67(7) . . ?
O23 Dy1 N1 147.30(8) . . ?
O3 Dy1 N1 131.64(8) . . ?
O43 Dy1 N1 71.18(7) . . ?
O44 Dy1 N1 120.98(8) . . ?
O24 Dy1 N1 79.62(7) . . ?
O4 Dy1 N1 80.83(7) . . ?
N2 Dy1 N1 64.32(7) . . ?
C10 O1 C2 122.5(3) . . ?
C4 O3 Dy1 134.40(19) . . ?
C11 O4 Dy1 138.02(18) . . ?
O2 C2 O1 114.2(3) . . ?
O2 C2 C3 127.3(3) . . ?
O1 C2 C3 118.6(3) . . ?
C4 C3 C11 119.5(2) . . ?
C4 C3 C2 119.8(3) . . ?
C11 C3 C2 120.7(3) . . ?
O3 C4 C3 124.3(3) . . ?
O3 C4 C5 117.2(3) . . ?
C3 C4 C5 118.5(3) . . ?
C10 C5 C6 119.4(3) . . ?
C10 C5 C4 118.8(3) . . ?
C6 C5 C4 121.7(3) . . ?
C7 C6 C5 120.2(4) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C8 C7 C6 119.3(4) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C7 C8 C9 121.2(4) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C10 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
O1 C10 C9 118.0(3) . . ?
O1 C10 C5 121.6(3) . . ?
C9 C10 C5 120.4(4) . . ?
O4 C11 C3 122.5(2) . . ?
O4 C11 C12 115.8(3) . . ?
C3 C11 C12 121.7(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 122.4(2) . . ?
C24 O23 Dy1 141.82(19) . . ?
C31 O24 Dy1 140.77(18) . . ?
O22 C22 O21 114.5(3) . . ?
O22 C22 C23 127.3(3) . . ?
O21 C22 C23 118.1(3) . . ?
C24 C23 C31 120.5(3) . . ?
C24 C23 C22 119.5(3) . . ?
C31 C23 C22 119.9(3) . . ?
O23 C24 C23 124.8(3) . . ?
O23 C24 C25 116.5(3) . . ?
C23 C24 C25 118.7(3) . . ?
C30 C25 C26 119.1(3) . . ?
C30 C25 C24 119.5(3) . . ?
C26 C25 C24 121.4(3) . . ?
C27 C26 C25 120.3(3) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 119.6(3) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 120.8(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 119.7(3) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
O21 C30 C25 121.7(3) . . ?
O21 C30 C29 117.8(3) . . ?
C25 C30 C29 120.5(3) . . ?
O24 C31 C23 122.2(3) . . ?
O24 C31 C32 115.5(3) . . ?
C23 C31 C32 122.3(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C42 O41 C50 122.4(3) . . ?
C44 O43 Dy1 137.4(2) . . ?
C51 O44 Dy1 137.0(2) . . ?
O42 C42 O41 114.7(3) . . ?
O42 C42 C43 127.1(4) . . ?
O41 C42 C43 118.2(3) . . ?
C44 C43 C51 120.5(2) . . ?
C44 C43 C42 119.8(3) . . ?
C51 C43 C42 119.4(3) . . ?
O43 C44 C43 124.5(3) . . ?
O43 C44 C45 117.6(3) . . ?
C43 C44 C45 117.7(3) . . ?
C46 C45 C50 118.8(3) . . ?
C46 C45 C44 122.4(3) . . ?
C50 C45 C44 118.8(3) . . ?
C45 C46 C47 120.6(4) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C46 C47 C48 119.3(4) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
C49 C48 C47 120.8(4) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C48 C49 C50 119.7(4) . . ?
C48 C49 H49 120.1 . . ?
C50 C49 H49 120.1 . . ?
O41 C50 C49 117.5(3) . . ?
O41 C50 C45 121.7(3) . . ?
C49 C50 C45 120.8(4) . . ?
O44 C51 C43 121.6(3) . . ?
O44 C51 C52 115.4(3) . . ?
C43 C51 C52 122.8(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 N1 C72 116.9(2) . . ?
C61 N1 Dy1 122.63(19) . . ?
C72 N1 Dy1 119.65(16) . . ?
C70 N2 C71 117.3(2) . . ?
C70 N2 Dy1 122.09(18) . . ?
C71 N2 Dy1 120.29(17) . . ?
N1 C61 C62 123.8(3) . . ?
N1 C61 H61 118.1 . . ?
C62 C61 H61 118.1 . . ?
C63 C62 C61 120.5(3) . . ?
C63 C62 H62 119.7 . . ?
C61 C62 H62 119.7 . . ?
C62 C63 C64 117.3(2) . . ?
C62 C63 C73 120.6(3) . . ?
C64 C63 C73 122.1(3) . . ?
C72 C64 C63 118.0(3) . . ?
C72 C64 C65 118.8(3) . . ?
C63 C64 C65 123.2(2) . . ?
C66 C65 C64 121.4(3) . . ?
C66 C65 H65 119.3 . . ?
C64 C65 H65 119.3 . . ?
C65 C66 C67 121.5(3) . . ?
C65 C66 H66 119.2 . . ?
C67 C66 H66 119.2 . . ?
C71 C67 C68 117.9(2) . . ?
C71 C67 C66 119.1(3) . . ?
C68 C67 C66 123.0(3) . . ?
C69 C68 C67 118.0(3) . . ?
C69 C68 C79 121.8(3) . . ?
C67 C68 C79 120.2(3) . . ?
C68 C69 C70 120.1(3) . . ?
C68 C69 H69 119.9 . . ?
C70 C69 H69 119.9 . . ?
N2 C70 C69 123.4(3) . . ?
N2 C70 H70 118.3 . . ?
C69 C70 H70 118.3 . . ?
N2 C71 C67 123.1(2) . . ?
N2 C71 C72 117.5(2) . . ?
C67 C71 C72 119.4(2) . . ?
N1 C72 C64 123.5(2) . . ?
N1 C72 C71 116.9(2) . . ?
C64 C72 C71 119.7(2) . . ?
C78 C73 C74 119.3(3) . . ?
C78 C73 C63 121.2(3) . . ?
C74 C73 C63 119.5(3) . . ?
C75 C74 C73 119.4(4) . . ?
C75 C74 H74 120.3 . . ?
C73 C74 H74 120.3 . . ?
C76 C75 C74 121.1(4) . . ?
C76 C75 H75 119.4 . . ?
C74 C75 H75 119.4 . . ?
C75 C76 C77 119.5(4) . . ?
C75 C76 H76 120.3 . . ?
C77 C76 H76 120.3 . . ?
C76 C77 C78 121.0(4) . . ?
C76 C77 H77 119.5 . . ?
C78 C77 H77 119.5 . . ?
C77 C78 C73 119.6(3) . . ?
C77 C78 H78 120.2 . . ?
C73 C78 H78 120.2 . . ?
C84 C79 C80 119.1(5) . . ?
C84 C79 C68 120.1(4) . . ?
C80 C79 C68 120.7(4) . . ?
C81 C80 C79 120.8(7) . . ?
C81 C80 H80 119.6 . . ?
C79 C80 H80 119.6 . . ?
C80 C81 C82 118.8(9) . . ?
C80 C81 H81 120.6 . . ?
C82 C81 H81 120.6 . . ?
C83 C82 C81 121.8(7) . . ?
C83 C82 H82 119.1 . . ?
C81 C82 H82 119.1 . . ?
C82 C83 C84 118.4(9) . . ?
C82 C83 H83 120.8 . . ?
C84 C83 H83 120.8 . . ?
C79 C84 C83 121.0(7) . . ?
C79 C84 H84 119.5 . . ?
C83 C84 H84 119.5 . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C91 C92 O92 113.4(8) . . ?
C91 C92 H92A 108.9 . . ?
O92 C92 H92A 108.9 . . ?
C91 C92 H92B 108.9 . . ?
O92 C92 H92B 108.9 . . ?
H92A C92 H92B 107.7 . . ?
C92 O92 H92 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 178.1(3) . . . . ?
C10 O1 C2 C3 -0.9(5) . . . . ?
O2 C2 C3 C4 177.8(4) . . . . ?
O1 C2 C3 C4 -3.3(5) . . . . ?
O2 C2 C3 C11 -2.7(5) . . . . ?
O1 C2 C3 C11 176.2(3) . . . . ?
Dy1 O3 C4 C3 -41.8(4) . . . . ?
Dy1 O3 C4 C5 138.4(2) . . . . ?
C11 C3 C4 O3 4.6(4) . . . . ?
C2 C3 C4 O3 -176.0(3) . . . . ?
C11 C3 C4 C5 -175.6(3) . . . . ?
C2 C3 C4 C5 3.8(4) . . . . ?
O3 C4 C5 C10 179.4(3) . . . . ?
C3 C4 C5 C10 -0.4(4) . . . . ?
O3 C4 C5 C6 -3.7(5) . . . . ?
C3 C4 C5 C6 176.5(3) . . . . ?
C10 C5 C6 C7 0.9(6) . . . . ?
C4 C5 C6 C7 -176.0(3) . . . . ?
C5 C6 C7 C8 0.1(7) . . . . ?
C6 C7 C8 C9 -1.3(8) . . . . ?
C7 C8 C9 C10 1.5(8) . . . . ?
C2 O1 C10 C9 -175.4(4) . . . . ?
C2 O1 C10 C5 4.5(5) . . . . ?
C8 C9 C10 O1 179.6(4) . . . . ?
C8 C9 C10 C5 -0.4(7) . . . . ?
C6 C5 C10 O1 179.3(3) . . . . ?
C4 C5 C10 O1 -3.8(5) . . . . ?
C6 C5 C10 C9 -0.8(5) . . . . ?
C4 C5 C10 C9 176.2(3) . . . . ?
Dy1 O4 C11 C3 1.4(5) . . . . ?
Dy1 O4 C11 C12 -178.6(2) . . . . ?
C4 C3 C11 O4 13.6(4) . . . . ?
C2 C3 C11 O4 -165.8(3) . . . . ?
C4 C3 C11 C12 -166.3(3) . . . . ?
C2 C3 C11 C12 14.3(4) . . . . ?
C30 O21 C22 O22 176.8(3) . . . . ?
C30 O21 C22 C23 -2.6(5) . . . . ?
O22 C22 C23 C24 -177.3(4) . . . . ?
O21 C22 C23 C24 2.0(5) . . . . ?
O22 C22 C23 C31 2.0(6) . . . . ?
O21 C22 C23 C31 -178.6(3) . . . . ?
Dy1 O23 C24 C23 5.4(6) . . . . ?
Dy1 O23 C24 C25 -175.5(3) . . . . ?
C31 C23 C24 O23 0.0(5) . . . . ?
C22 C23 C24 O23 179.3(3) . . . . ?
C31 C23 C24 C25 -179.1(3) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
O23 C24 C25 C30 178.8(3) . . . . ?
C23 C24 C25 C30 -2.1(5) . . . . ?
O23 C24 C25 C26 -0.5(5) . . . . ?
C23 C24 C25 C26 178.7(3) . . . . ?
C30 C25 C26 C27 0.8(5) . . . . ?
C24 C25 C26 C27 180.0(3) . . . . ?
C25 C26 C27 C28 -0.9(5) . . . . ?
C26 C27 C28 C29 0.1(5) . . . . ?
C27 C28 C29 C30 0.9(5) . . . . ?
C22 O21 C30 C25 0.8(5) . . . . ?
C22 O21 C30 C29 -178.6(3) . . . . ?
C26 C25 C30 O21 -179.1(3) . . . . ?
C24 C25 C30 O21 1.6(5) . . . . ?
C26 C25 C30 C29 0.2(5) . . . . ?
C24 C25 C30 C29 -179.0(3) . . . . ?
C28 C29 C30 O21 178.3(3) . . . . ?
C28 C29 C30 C25 -1.1(5) . . . . ?
Dy1 O24 C31 C23 7.4(5) . . . . ?
Dy1 O24 C31 C32 -171.5(2) . . . . ?
C24 C23 C31 O24 -5.5(5) . . . . ?
C22 C23 C31 O24 175.2(3) . . . . ?
C24 C23 C31 C32 173.3(3) . . . . ?
C22 C23 C31 C32 -6.0(5) . . . . ?
C50 O41 C42 O42 178.5(3) . . . . ?
C50 O41 C42 C43 -0.4(5) . . . . ?
O42 C42 C43 C44 -168.7(4) . . . . ?
O41 C42 C43 C44 10.1(5) . . . . ?
O42 C42 C43 C51 17.4(6) . . . . ?
O41 C42 C43 C51 -163.8(3) . . . . ?
Dy1 O43 C44 C43 -5.2(5) . . . . ?
Dy1 O43 C44 C45 178.5(2) . . . . ?
C51 C43 C44 O43 -16.3(5) . . . . ?
C42 C43 C44 O43 169.9(3) . . . . ?
C51 C43 C44 C45 160.0(3) . . . . ?
C42 C43 C44 C45 -13.9(4) . . . . ?
O43 C44 C45 C46 7.0(5) . . . . ?
C43 C44 C45 C46 -169.5(3) . . . . ?
O43 C44 C45 C50 -175.1(3) . . . . ?
C43 C44 C45 C50 8.4(4) . . . . ?
C50 C45 C46 C47 -1.1(5) . . . . ?
C44 C45 C46 C47 176.8(3) . . . . ?
C45 C46 C47 C48 1.5(6) . . . . ?
C46 C47 C48 C49 -1.0(6) . . . . ?
C47 C48 C49 C50 0.1(6) . . . . ?
C42 O41 C50 C49 173.8(3) . . . . ?
C42 O41 C50 C45 -5.2(5) . . . . ?
C48 C49 C50 O41 -178.6(4) . . . . ?
C48 C49 C50 C45 0.4(6) . . . . ?
C46 C45 C50 O41 179.0(3) . . . . ?
C44 C45 C50 O41 1.1(5) . . . . ?
C46 C45 C50 C49 0.1(5) . . . . ?
C44 C45 C50 C49 -177.9(3) . . . . ?
Dy1 O44 C51 C43 28.6(5) . . . . ?
Dy1 O44 C51 C52 -155.1(3) . . . . ?
C44 C43 C51 O44 5.4(5) . . . . ?
C42 C43 C51 O44 179.3(3) . . . . ?
C44 C43 C51 C52 -170.6(4) . . . . ?
C42 C43 C51 C52 3.3(5) . . . . ?
C72 N1 C61 C62 -0.3(4) . . . . ?
Dy1 N1 C61 C62 -169.7(2) . . . . ?
N1 C61 C62 C63 0.9(5) . . . . ?
C61 C62 C63 C64 -1.0(4) . . . . ?
C61 C62 C63 C73 179.7(3) . . . . ?
C62 C63 C64 C72 0.5(4) . . . . ?
C73 C63 C64 C72 179.9(3) . . . . ?
C62 C63 C64 C65 -177.3(3) . . . . ?
C73 C63 C64 C65 2.0(4) . . . . ?
C72 C64 C65 C66 0.6(4) . . . . ?
C63 C64 C65 C66 178.5(3) . . . . ?
C64 C65 C66 C67 0.3(5) . . . . ?
C65 C66 C67 C71 -0.2(4) . . . . ?
C65 C66 C67 C68 -178.6(3) . . . . ?
C71 C67 C68 C69 1.0(4) . . . . ?
C66 C67 C68 C69 179.4(3) . . . . ?
C71 C67 C68 C79 -178.5(3) . . . . ?
C66 C67 C68 C79 -0.1(5) . . . . ?
C67 C68 C69 C70 1.1(5) . . . . ?
C79 C68 C69 C70 -179.4(3) . . . . ?
C71 N2 C70 C69 0.5(4) . . . . ?
Dy1 N2 C70 C69 174.4(2) . . . . ?
C68 C69 C70 N2 -1.9(5) . . . . ?
C70 N2 C71 C67 1.8(4) . . . . ?
Dy1 N2 C71 C67 -172.31(19) . . . . ?
C70 N2 C71 C72 -178.5(2) . . . . ?
Dy1 N2 C71 C72 7.4(3) . . . . ?
C68 C67 C71 N2 -2.5(4) . . . . ?
C66 C67 C71 N2 179.0(3) . . . . ?
C68 C67 C71 C72 177.8(2) . . . . ?
C66 C67 C71 C72 -0.7(4) . . . . ?
C61 N1 C72 C64 -0.1(4) . . . . ?
Dy1 N1 C72 C64 169.6(2) . . . . ?
C61 N1 C72 C71 179.4(2) . . . . ?
Dy1 N1 C72 C71 -10.9(3) . . . . ?
C63 C64 C72 N1 0.0(4) . . . . ?
C65 C64 C72 N1 177.9(2) . . . . ?
C63 C64 C72 C71 -179.5(2) . . . . ?
C65 C64 C72 C71 -1.6(4) . . . . ?
N2 C71 C72 N1 2.4(3) . . . . ?
C67 C71 C72 N1 -177.9(2) . . . . ?
N2 C71 C72 C64 -178.1(2) . . . . ?
C67 C71 C72 C64 1.6(4) . . . . ?
C62 C63 C73 C78 -123.1(3) . . . . ?
C64 C63 C73 C78 57.6(4) . . . . ?
C62 C63 C73 C74 55.6(4) . . . . ?
C64 C63 C73 C74 -123.7(3) . . . . ?
C78 C73 C74 C75 -1.4(5) . . . . ?
C63 C73 C74 C75 179.9(3) . . . . ?
C73 C74 C75 C76 1.1(6) . . . . ?
C74 C75 C76 C77 0.5(7) . . . . ?
C75 C76 C77 C78 -1.7(7) . . . . ?
C76 C77 C78 C73 1.4(6) . . . . ?
C74 C73 C78 C77 0.2(5) . . . . ?
C63 C73 C78 C77 178.9(3) . . . . ?
C69 C68 C79 C84 -76.0(5) . . . . ?
C67 C68 C79 C84 103.5(5) . . . . ?
C69 C68 C79 C80 104.7(5) . . . . ?
C67 C68 C79 C80 -75.8(5) . . . . ?
C84 C79 C80 C81 -3.0(9) . . . . ?
C68 C79 C80 C81 176.2(5) . . . . ?
C79 C80 C81 C82 2.1(11) . . . . ?
C80 C81 C82 C83 -0.5(15) . . . . ?
C81 C82 C83 C84 0.0(15) . . . . ?
C80 C79 C84 C83 2.5(9) . . . . ?
C68 C79 C84 C83 -176.8(6) . . . . ?
C82 C83 C84 C79 -1.0(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C61 H61 O24 0.93 2.43 3.093(4) 127.9 . yes
C70 H70 O3 0.93 2.45 3.026(4) 120.1 . yes

_refine_diff_density_max         1.244
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_Tb-phen
_database_code_depnum_ccdc_archive 'CCDC 2013254'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  TbCum3Fen
# Clave IF-UAP:  TbCum3Fen
# Solicitud: 101
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM) 
# Clave datos : ... \BUAP\Sylvain\TbCum3Fen\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_audit_creation_date             2018-04-27

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H29 N2 O12 Tb, 0.5(H2 O)'
_chemical_formula_sum            'C45 H30 N2 O12.50 Tb'
_chemical_formula_weight         957.63
_chemical_absolute_configuration .
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.3496 2.7654 '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       ?

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

_cell_length_a                   11.0672(7)
_cell_length_b                   13.0523(8)
_cell_length_c                   14.2639(9)
_cell_angle_alpha                104.500(5)
_cell_angle_beta                 92.593(5)
_cell_angle_gamma                98.423(5)
_cell_volume                     1966.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    20255
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.90

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_F_000             958
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.064
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -5 -1 0.0340
-3 5 1 0.0300
-3 -1 0 0.1120
2 1 0 0.1440
1 1 -6 0.0690
0 -1 6 0.0970
-2 -1 1 0.1260
-3 -1 -5 0.1000

_exptl_absorpt_coefficient_mu    1.004
_shelx_estimated_absorpt_T_min   0.783
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4806
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA (Stoe & Cie, 2015)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1579 frames, 15-20 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            63684
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.336
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10452
_reflns_number_gt                6372
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_cell_refinement       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'

_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)+(0.0210P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         10452
_refine_ls_number_parameters     559
_refine_ls_number_restraints     5
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_restrained_S_all      0.789
_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
Tb1 Tb 0.28848(2) 0.25259(2) 0.78545(2) 0.04432(6) Uani 1 1 d . . . . .
O1 O 0.0957(3) 0.6532(3) 0.7895(3) 0.0988(11) Uani 1 1 d . . . . .
O2 O -0.0175(4) 0.5872(3) 0.8901(3) 0.1404(17) Uani 1 1 d . . . . .
O3 O 0.2481(2) 0.38080(19) 0.70494(16) 0.0528(6) Uani 1 1 d . . . . .
O4 O 0.0898(2) 0.2904(2) 0.80845(18) 0.0623(7) Uani 1 1 d . . . . .
C2 C 0.0534(5) 0.5685(5) 0.8280(3) 0.0939(16) Uani 1 1 d . . . . .
C3 C 0.0973(4) 0.4674(4) 0.7930(3) 0.0627(11) Uani 1 1 d . . . . .
C4 C 0.1953(3) 0.4613(3) 0.7315(2) 0.0534(9) Uani 1 1 d . . . . .
C5 C 0.2366(4) 0.5561(3) 0.6969(3) 0.0599(10) Uani 1 1 d . . . . .
C6 C 0.3295(4) 0.5582(4) 0.6359(3) 0.0784(13) Uani 1 1 d . . . . .
H6A H 0.366673 0.497917 0.615078 0.094 Uiso 1 1 calc R U . . .
C7 C 0.3673(5) 0.6483(5) 0.6057(4) 0.1060(17) Uani 1 1 d . . . . .
H7A H 0.431636 0.649441 0.566021 0.127 Uiso 1 1 calc R U . . .
C8 C 0.3116(6) 0.7371(5) 0.6330(5) 0.120(2) Uani 1 1 d . . . . .
H8A H 0.336387 0.796735 0.609863 0.143 Uiso 1 1 calc R U . . .
C9 C 0.2213(6) 0.7384(4) 0.6932(4) 0.1036(19) Uani 1 1 d . . . . .
H9A H 0.184141 0.798906 0.712889 0.124 Uiso 1 1 calc R U . . .
C10 C 0.1845(5) 0.6470(4) 0.7256(3) 0.0794(13) Uani 1 1 d . . . . .
C11 C 0.0424(4) 0.3737(4) 0.8206(3) 0.0690(12) Uani 1 1 d . . . . .
C12 C -0.0799(4) 0.3667(5) 0.8625(4) 0.129(2) Uani 1 1 d . . . . .
H12A H -0.121697 0.293921 0.842894 0.194 Uiso 1 1 calc DR U . . .
H12B H -0.128272 0.412051 0.839284 0.194 Uiso 1 1 calc R U . . .
H12C H -0.067808 0.389775 0.932175 0.194 Uiso 1 1 calc R U . . .
O21 O 0.1309(2) -0.1405(2) 0.44275(17) 0.0681(7) Uani 1 1 d . . . . .
O22 O 0.2980(3) -0.0713(2) 0.3920(2) 0.1004(11) Uani 1 1 d . . . . .
O23 O 0.1666(2) 0.09389(18) 0.69861(15) 0.0539(6) Uani 1 1 d . . . . .
O24 O 0.3579(2) 0.19113(18) 0.63262(16) 0.0562(7) Uani 1 1 d . . . . .
C22 C 0.2314(4) -0.0601(3) 0.4578(3) 0.0649(11) Uani 1 1 d . . . . .
C23 C 0.2459(3) 0.0255(3) 0.5456(2) 0.0477(8) Uani 1 1 d . . . . .
C24 C 0.1613(3) 0.0238(3) 0.6181(2) 0.0452(8) Uani 1 1 d . . . . .
C25 C 0.0575(3) -0.0653(2) 0.5967(2) 0.0451(8) Uani 1 1 d . . . . .
C26 C -0.0309(3) -0.0721(3) 0.6610(3) 0.0601(10) Uani 1 1 d . . . . .
H26A H -0.025120 -0.019943 0.719655 0.072 Uiso 1 1 calc R U . . .
C27 C -0.1283(4) -0.1563(3) 0.6382(3) 0.0781(13) Uani 1 1 d . . . . .
H27A H -0.187517 -0.161562 0.681736 0.094 Uiso 1 1 calc R U . . .
C28 C -0.1366(4) -0.2329(3) 0.5499(3) 0.0786(13) Uani 1 1 d . . . . .
H28A H -0.202485 -0.288997 0.534108 0.094 Uiso 1 1 calc R U . . .
C29 C -0.0502(4) -0.2271(3) 0.4864(3) 0.0704(12) Uani 1 1 d . . . . .
H29A H -0.056073 -0.278906 0.427539 0.084 Uiso 1 1 calc R U . . .
C30 C 0.0472(3) -0.1427(3) 0.5104(3) 0.0548(9) Uani 1 1 d . . . . .
C31 C 0.3424(3) 0.1157(3) 0.5588(3) 0.0545(9) Uani 1 1 d . . . . .
C32 C 0.4306(4) 0.1275(3) 0.4826(3) 0.0811(14) Uani 1 1 d . . . . .
H32A H 0.494120 0.187722 0.509112 0.122 Uiso 1 1 calc R U . . .
H32B H 0.387106 0.138673 0.427132 0.122 Uiso 1 1 calc R U . . .
H32C H 0.466303 0.063487 0.463084 0.122 Uiso 1 1 calc R U . . .
O41 O 0.6449(3) 0.6445(2) 0.8147(2) 0.0744(8) Uani 1 1 d . . . . .
O42 O 0.5188(3) 0.7118(2) 0.9167(2) 0.0876(9) Uani 1 1 d . . . . .
O43 O 0.4870(2) 0.33540(17) 0.79156(16) 0.0521(6) Uani 1 1 d . . . . .
O44 O 0.3265(2) 0.41158(17) 0.91123(15) 0.0489(6) Uani 1 1 d . . . . .
C42 C 0.5459(4) 0.6296(3) 0.8686(3) 0.0626(10) Uani 1 1 d . . . . .
C43 C 0.4862(3) 0.5209(3) 0.8614(2) 0.0468(8) Uani 1 1 d . . . . .
C44 C 0.5304(3) 0.4328(3) 0.8007(2) 0.0472(8) Uani 1 1 d . . . . .
C45 C 0.6345(3) 0.4553(3) 0.7455(3) 0.0528(9) Uani 1 1 d . . . . .
C46 C 0.6819(3) 0.3736(3) 0.6814(3) 0.0666(11) Uani 1 1 d . . . . .
H46A H 0.647134 0.302279 0.673379 0.080 Uiso 1 1 calc R U . . .
C47 C 0.7792(4) 0.3984(4) 0.6306(3) 0.0851(14) Uani 1 1 d . . . . .
H47A H 0.810222 0.343667 0.588559 0.102 Uiso 1 1 calc R U . . .
C48 C 0.8317(4) 0.5038(5) 0.6411(4) 0.0918(15) Uani 1 1 d . . . . .
H48A H 0.897873 0.519826 0.606475 0.110 Uiso 1 1 calc R U . . .
C49 C 0.7857(4) 0.5847(4) 0.7030(4) 0.0853(14) Uani 1 1 d . . . . .
H49A H 0.820456 0.655867 0.710466 0.102 Uiso 1 1 calc R U . . .
C50 C 0.6874(4) 0.5597(3) 0.7541(3) 0.0638(10) Uani 1 1 d . . . . .
C51 C 0.3851(3) 0.5033(3) 0.9187(2) 0.0476(9) Uani 1 1 d . . . . .
C52 C 0.3408(3) 0.5933(3) 0.9902(3) 0.0633(10) Uani 1 1 d . . . . .
H52A H 0.280886 0.563962 1.027057 0.095 Uiso 1 1 calc R U . . .
H52B H 0.304460 0.637079 0.955555 0.095 Uiso 1 1 calc R U . . .
H52C H 0.408795 0.636276 1.033329 0.095 Uiso 1 1 calc R U . . .
N61 N 0.4080(3) 0.1131(2) 0.82127(19) 0.0494(7) Uani 1 1 d . . . . .
C62 C 0.5038(3) 0.0830(3) 0.7745(3) 0.0582(10) Uani 1 1 d . . . . .
H62A H 0.539563 0.125194 0.736171 0.070 Uiso 1 1 calc R U . . .
C63 C 0.5537(4) -0.0075(3) 0.7794(3) 0.0661(11) Uani 1 1 d . . . . .
H63A H 0.621611 -0.024132 0.746170 0.079 Uiso 1 1 calc R U . . .
C64 C 0.5014(4) -0.0713(3) 0.8335(3) 0.0697(11) Uani 1 1 d . . . . .
H64A H 0.531903 -0.133330 0.836108 0.084 Uiso 1 1 calc R U . . .
C65 C 0.4005(4) -0.0432(3) 0.8859(3) 0.0562(10) Uani 1 1 d . . . . .
C66 C 0.3440(4) -0.1042(3) 0.9465(3) 0.0712(12) Uani 1 1 d . . . . .
H66A H 0.368949 -0.168707 0.948489 0.085 Uiso 1 1 calc R U . . .
C67 C 0.2553(4) -0.0699(3) 1.0006(3) 0.0682(11) Uani 1 1 d . . . . .
H67A H 0.219127 -0.111295 1.039385 0.082 Uiso 1 1 calc R U . . .
C68 C 0.2146(3) 0.0291(3) 1.0003(3) 0.0549(9) Uani 1 1 d . . . . .
C69 C 0.1293(4) 0.0732(3) 1.0622(3) 0.0651(11) Uani 1 1 d . . . . .
H69A H 0.094249 0.036622 1.105044 0.078 Uiso 1 1 calc R U . . .
C70 C 0.0982(4) 0.1695(3) 1.0593(3) 0.0666(11) Uani 1 1 d . . . . .
H70A H 0.044398 0.200766 1.101525 0.080 Uiso 1 1 calc R U . . .
C71 C 0.1490(3) 0.2204(3) 0.9914(3) 0.0598(10) Uani 1 1 d . . . . .
H71A H 0.126006 0.285525 0.989079 0.072 Uiso 1 1 calc R U . . .
N72 N 0.2277(3) 0.1817(2) 0.93025(19) 0.0491(7) Uani 1 1 d . . . . .
C73 C 0.2639(3) 0.0883(3) 0.9372(2) 0.0493(9) Uani 1 1 d . . . . .
C74 C 0.3595(3) 0.0513(3) 0.8784(2) 0.0471(8) Uani 1 1 d . . . . .
O81 O -0.1265(8) 0.1303(8) 0.8005(6) 0.158(3) Uani 0.5 1 d D . P . .
H81A H -0.145(5) 0.097(11) 0.739(3) 0.190 Uiso 0.5 1 d D U P . .
H81B H -0.199(2) 0.1323(19) 0.8208(17) 0.190 Uiso 0.5 1 d D U P . .


_geom_special_details            ?

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 O43 2.289(2) . ?
Tb1 O23 2.322(2) . ?
Tb1 O24 2.333(2) . ?
Tb1 O3 2.335(2) . ?
Tb1 O4 2.342(3) . ?
Tb1 O44 2.348(2) . ?
Tb1 N61 2.537(3) . ?
Tb1 N72 2.544(3) . ?
O1 C10 1.368(5) . ?
O1 C2 1.386(6) . ?
O2 C2 1.212(5) . ?
O3 C4 1.261(4) . ?
O4 C11 1.252(5) . ?
C2 C3 1.451(6) . ?
C3 C4 1.424(5) . ?
C3 C11 1.438(6) . ?
C4 C5 1.464(5) . ?
C5 C10 1.372(6) . ?
C5 C6 1.379(5) . ?
C6 C7 1.368(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.370(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.346(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.398(6) . ?
C9 H9A 0.9300 . ?
C11 C12 1.504(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.370(4) . ?
O21 C22 1.381(4) . ?
O22 C22 1.214(4) . ?
O23 C24 1.270(3) . ?
O24 C31 1.234(4) . ?
C22 C23 1.438(4) . ?
C23 C24 1.429(4) . ?
C23 C31 1.436(4) . ?
C24 C25 1.471(4) . ?
C25 C30 1.371(4) . ?
C25 C26 1.378(4) . ?
C26 C27 1.385(5) . ?
C26 H26A 0.9300 . ?
C27 C28 1.388(6) . ?
C27 H27A 0.9300 . ?
C28 C29 1.353(5) . ?
C28 H28A 0.9300 . ?
C29 C30 1.386(5) . ?
C29 H29A 0.9300 . ?
C31 C32 1.515(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.379(4) . ?
O41 C42 1.385(4) . ?
O42 C42 1.207(4) . ?
O43 C44 1.264(4) . ?
O44 C51 1.252(4) . ?
C42 C43 1.451(5) . ?
C43 C44 1.420(4) . ?
C43 C51 1.440(5) . ?
C44 C45 1.460(5) . ?
C45 C50 1.375(5) . ?
C45 C46 1.403(5) . ?
C46 C47 1.369(5) . ?
C46 H46A 0.9300 . ?
C47 C48 1.380(6) . ?
C47 H47A 0.9300 . ?
C48 C49 1.373(6) . ?
C48 H48A 0.9300 . ?
C49 C50 1.380(5) . ?
C49 H49A 0.9300 . ?
C51 C52 1.508(4) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N61 C62 1.334(4) . ?
N61 C74 1.357(4) . ?
C62 C63 1.391(5) . ?
C62 H62A 0.9300 . ?
C63 C64 1.358(5) . ?
C63 H63A 0.9300 . ?
C64 C65 1.413(5) . ?
C64 H64A 0.9300 . ?
C65 C74 1.402(5) . ?
C65 C66 1.421(5) . ?
C66 C67 1.336(5) . ?
C66 H66A 0.9300 . ?
C67 C68 1.430(5) . ?
C67 H67A 0.9300 . ?
C68 C73 1.405(5) . ?
C68 C69 1.408(5) . ?
C69 C70 1.360(5) . ?
C69 H69A 0.9300 . ?
C70 C71 1.400(5) . ?
C70 H70A 0.9300 . ?
C71 N72 1.323(4) . ?
C71 H71A 0.9300 . ?
N72 C73 1.363(4) . ?
C73 C74 1.444(5) . ?
O81 H81A 0.88(2) . ?
O81 H81B 0.87(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O43 Tb1 O23 137.55(8) . . ?
O43 Tb1 O24 72.70(8) . . ?
O23 Tb1 O24 69.12(7) . . ?
O43 Tb1 O3 83.02(8) . . ?
O23 Tb1 O3 105.15(8) . . ?
O24 Tb1 O3 76.68(8) . . ?
O43 Tb1 O4 141.59(9) . . ?
O23 Tb1 O4 77.37(9) . . ?
O24 Tb1 O4 123.39(9) . . ?
O3 Tb1 O4 69.69(9) . . ?
O43 Tb1 O44 69.55(8) . . ?
O23 Tb1 O44 152.67(8) . . ?
O24 Tb1 O44 136.37(8) . . ?
O3 Tb1 O44 77.78(8) . . ?
O4 Tb1 O44 78.41(8) . . ?
O43 Tb1 N61 78.04(8) . . ?
O23 Tb1 N61 78.23(9) . . ?
O24 Tb1 N61 80.81(9) . . ?
O3 Tb1 N61 154.05(8) . . ?
O4 Tb1 N61 135.00(9) . . ?
O44 Tb1 N61 111.26(8) . . ?
O43 Tb1 N72 116.88(9) . . ?
O23 Tb1 N72 82.70(8) . . ?
O24 Tb1 N72 139.01(9) . . ?
O3 Tb1 N72 141.33(9) . . ?
O4 Tb1 N72 75.55(9) . . ?
O44 Tb1 N72 79.17(8) . . ?
N61 Tb1 N72 64.27(9) . . ?
C10 O1 C2 121.9(4) . . ?
C4 O3 Tb1 130.6(2) . . ?
C11 O4 Tb1 134.3(3) . . ?
O2 C2 O1 115.5(5) . . ?
O2 C2 C3 125.8(6) . . ?
O1 C2 C3 118.8(4) . . ?
C4 C3 C11 120.0(4) . . ?
C4 C3 C2 119.8(4) . . ?
C11 C3 C2 120.1(4) . . ?
O3 C4 C3 124.9(4) . . ?
O3 C4 C5 118.2(4) . . ?
C3 C4 C5 116.9(4) . . ?
C10 C5 C6 117.7(4) . . ?
C10 C5 C4 120.7(4) . . ?
C6 C5 C4 121.6(4) . . ?
C7 C6 C5 120.4(5) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C6 C7 C8 120.9(6) . . ?
C6 C7 H7A 119.5 . . ?
C8 C7 H7A 119.5 . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 H8A 119.8 . . ?
C7 C8 H8A 119.8 . . ?
C8 C9 C10 118.5(6) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
O1 C10 C5 121.4(5) . . ?
O1 C10 C9 116.6(5) . . ?
C5 C10 C9 122.1(5) . . ?
O4 C11 C3 123.0(4) . . ?
O4 C11 C12 114.8(4) . . ?
C3 C11 C12 122.2(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 121.8(3) . . ?
C24 O23 Tb1 139.6(2) . . ?
C31 O24 Tb1 143.5(2) . . ?
O22 C22 O21 113.5(3) . . ?
O22 C22 C23 127.5(4) . . ?
O21 C22 C23 118.9(3) . . ?
C24 C23 C31 119.5(3) . . ?
C24 C23 C22 120.3(3) . . ?
C31 C23 C22 120.1(3) . . ?
O23 C24 C23 125.5(3) . . ?
O23 C24 C25 117.2(3) . . ?
C23 C24 C25 117.3(3) . . ?
C30 C25 C26 119.1(3) . . ?
C30 C25 C24 119.4(3) . . ?
C26 C25 C24 121.5(3) . . ?
C25 C26 C27 120.1(4) . . ?
C25 C26 H26A 120.0 . . ?
C27 C26 H26A 120.0 . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
C29 C28 C27 120.9(4) . . ?
C29 C28 H28A 119.5 . . ?
C27 C28 H28A 119.5 . . ?
C28 C29 C30 119.0(4) . . ?
C28 C29 H29A 120.5 . . ?
C30 C29 H29A 120.5 . . ?
O21 C30 C25 122.2(3) . . ?
O21 C30 C29 116.4(3) . . ?
C25 C30 C29 121.4(4) . . ?
O24 C31 C23 122.3(3) . . ?
O24 C31 C32 114.7(3) . . ?
C23 C31 C32 122.9(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.2(3) . . ?
C44 O43 Tb1 130.5(2) . . ?
C51 O44 Tb1 133.7(2) . . ?
O42 C42 O41 114.1(3) . . ?
O42 C42 C43 127.3(4) . . ?
O41 C42 C43 118.6(3) . . ?
C44 C43 C51 120.5(3) . . ?
C44 C43 C42 119.8(3) . . ?
C51 C43 C42 119.6(3) . . ?
O43 C44 C43 124.7(3) . . ?
O43 C44 C45 117.1(3) . . ?
C43 C44 C45 118.2(3) . . ?
C50 C45 C46 118.0(4) . . ?
C50 C45 C44 119.8(3) . . ?
C46 C45 C44 122.2(3) . . ?
C47 C46 C45 120.2(4) . . ?
C47 C46 H46A 119.9 . . ?
C45 C46 H46A 119.9 . . ?
C46 C47 C48 120.8(4) . . ?
C46 C47 H47A 119.6 . . ?
C48 C47 H47A 119.6 . . ?
C49 C48 C47 119.7(4) . . ?
C49 C48 H48A 120.2 . . ?
C47 C48 H48A 120.2 . . ?
C48 C49 C50 119.6(4) . . ?
C48 C49 H49A 120.2 . . ?
C50 C49 H49A 120.2 . . ?
C45 C50 O41 121.4(4) . . ?
C45 C50 C49 121.7(4) . . ?
O41 C50 C49 116.9(4) . . ?
O44 C51 C43 121.9(3) . . ?
O44 C51 C52 115.3(3) . . ?
C43 C51 C52 122.7(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C62 N61 C74 116.6(3) . . ?
C62 N61 Tb1 124.1(2) . . ?
C74 N61 Tb1 118.2(2) . . ?
N61 C62 C63 124.1(4) . . ?
N61 C62 H62A 117.9 . . ?
C63 C62 H62A 117.9 . . ?
C64 C63 C62 118.8(4) . . ?
C64 C63 H63A 120.6 . . ?
C62 C63 H63A 120.6 . . ?
C63 C64 C65 119.9(4) . . ?
C63 C64 H64A 120.1 . . ?
C65 C64 H64A 120.1 . . ?
C74 C65 C64 116.8(4) . . ?
C74 C65 C66 120.3(4) . . ?
C64 C65 C66 122.9(4) . . ?
C67 C66 C65 120.6(4) . . ?
C67 C66 H66A 119.7 . . ?
C65 C66 H66A 119.7 . . ?
C66 C67 C68 121.6(4) . . ?
C66 C67 H67A 119.2 . . ?
C68 C67 H67A 119.2 . . ?
C73 C68 C69 117.2(4) . . ?
C73 C68 C67 119.1(3) . . ?
C69 C68 C67 123.6(4) . . ?
C70 C69 C68 119.9(4) . . ?
C70 C69 H69A 120.1 . . ?
C68 C69 H69A 120.1 . . ?
C69 C70 C71 118.6(4) . . ?
C69 C70 H70A 120.7 . . ?
C71 C70 H70A 120.7 . . ?
N72 C71 C70 124.1(4) . . ?
N72 C71 H71A 117.9 . . ?
C70 C71 H71A 117.9 . . ?
C71 N72 C73 117.1(3) . . ?
C71 N72 Tb1 124.4(2) . . ?
C73 N72 Tb1 117.8(2) . . ?
N72 C73 C68 122.9(3) . . ?
N72 C73 C74 117.6(3) . . ?
C68 C73 C74 119.4(3) . . ?
N61 C74 C65 123.7(3) . . ?
N61 C74 C73 117.5(3) . . ?
C65 C74 C73 118.8(3) . . ?
H81A O81 H81B 100(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 173.8(4) . . . . ?
C10 O1 C2 C3 -5.4(7) . . . . ?
O2 C2 C3 C4 -169.8(5) . . . . ?
O1 C2 C3 C4 9.3(6) . . . . ?
O2 C2 C3 C11 10.0(7) . . . . ?
O1 C2 C3 C11 -170.9(4) . . . . ?
Tb1 O3 C4 C3 -32.9(5) . . . . ?
Tb1 O3 C4 C5 147.4(2) . . . . ?
C11 C3 C4 O3 -7.0(6) . . . . ?
C2 C3 C4 O3 172.7(3) . . . . ?
C11 C3 C4 C5 172.8(3) . . . . ?
C2 C3 C4 C5 -7.5(5) . . . . ?
O3 C4 C5 C10 -178.3(3) . . . . ?
C3 C4 C5 C10 1.9(5) . . . . ?
O3 C4 C5 C6 0.8(5) . . . . ?
C3 C4 C5 C6 -179.0(3) . . . . ?
C10 C5 C6 C7 0.0(6) . . . . ?
C4 C5 C6 C7 -179.1(4) . . . . ?
C5 C6 C7 C8 -1.9(8) . . . . ?
C6 C7 C8 C9 2.4(9) . . . . ?
C7 C8 C9 C10 -1.1(9) . . . . ?
C2 O1 C10 C5 -0.3(6) . . . . ?
C2 O1 C10 C9 -178.7(4) . . . . ?
C6 C5 C10 O1 -177.1(4) . . . . ?
C4 C5 C10 O1 2.1(6) . . . . ?
C6 C5 C10 C9 1.3(6) . . . . ?
C4 C5 C10 C9 -179.5(4) . . . . ?
C8 C9 C10 O1 177.6(5) . . . . ?
C8 C9 C10 C5 -0.8(8) . . . . ?
Tb1 O4 C11 C3 20.6(6) . . . . ?
Tb1 O4 C11 C12 -162.0(3) . . . . ?
C4 C3 C11 O4 13.5(6) . . . . ?
C2 C3 C11 O4 -166.3(4) . . . . ?
C4 C3 C11 C12 -163.7(4) . . . . ?
C2 C3 C11 C12 16.5(6) . . . . ?
C30 O21 C22 O22 178.3(4) . . . . ?
C30 O21 C22 C23 -2.2(6) . . . . ?
O22 C22 C23 C24 -177.1(4) . . . . ?
O21 C22 C23 C24 3.4(6) . . . . ?
O22 C22 C23 C31 5.7(7) . . . . ?
O21 C22 C23 C31 -173.7(3) . . . . ?
Tb1 O23 C24 C23 -0.4(6) . . . . ?
Tb1 O23 C24 C25 -178.9(2) . . . . ?
C31 C23 C24 O23 -4.1(5) . . . . ?
C22 C23 C24 O23 178.7(4) . . . . ?
C31 C23 C24 C25 174.3(3) . . . . ?
C22 C23 C24 C25 -2.8(5) . . . . ?
O23 C24 C25 C30 179.6(3) . . . . ?
C23 C24 C25 C30 1.0(5) . . . . ?
O23 C24 C25 C26 0.5(5) . . . . ?
C23 C24 C25 C26 -178.0(3) . . . . ?
C30 C25 C26 C27 0.2(6) . . . . ?
C24 C25 C26 C27 179.2(3) . . . . ?
C25 C26 C27 C28 -0.8(6) . . . . ?
C26 C27 C28 C29 0.9(7) . . . . ?
C27 C28 C29 C30 -0.4(7) . . . . ?
C22 O21 C30 C25 0.4(5) . . . . ?
C22 O21 C30 C29 179.5(4) . . . . ?
C26 C25 C30 O21 179.3(3) . . . . ?
C24 C25 C30 O21 0.3(5) . . . . ?
C26 C25 C30 C29 0.2(6) . . . . ?
C24 C25 C30 C29 -178.8(3) . . . . ?
C28 C29 C30 O21 -179.3(4) . . . . ?
C28 C29 C30 C25 -0.1(6) . . . . ?
Tb1 O24 C31 C23 4.4(7) . . . . ?
Tb1 O24 C31 C32 -177.3(3) . . . . ?
C24 C23 C31 O24 2.5(6) . . . . ?
C22 C23 C31 O24 179.6(4) . . . . ?
C24 C23 C31 C32 -175.7(4) . . . . ?
C22 C23 C31 C32 1.5(6) . . . . ?
C50 O41 C42 O42 -178.8(3) . . . . ?
C50 O41 C42 C43 0.6(5) . . . . ?
O42 C42 C43 C44 179.9(4) . . . . ?
O41 C42 C43 C44 0.5(5) . . . . ?
O42 C42 C43 C51 -2.2(6) . . . . ?
O41 C42 C43 C51 178.4(3) . . . . ?
Tb1 O43 C44 C43 38.3(4) . . . . ?
Tb1 O43 C44 C45 -142.4(2) . . . . ?
C51 C43 C44 O43 0.2(5) . . . . ?
C42 C43 C44 O43 178.1(3) . . . . ?
C51 C43 C44 C45 -179.0(3) . . . . ?
C42 C43 C44 C45 -1.2(5) . . . . ?
O43 C44 C45 C50 -178.6(3) . . . . ?
C43 C44 C45 C50 0.7(5) . . . . ?
O43 C44 C45 C46 2.8(5) . . . . ?
C43 C44 C45 C46 -177.9(3) . . . . ?
C50 C45 C46 C47 1.0(6) . . . . ?
C44 C45 C46 C47 179.6(4) . . . . ?
C45 C46 C47 C48 -0.3(7) . . . . ?
C46 C47 C48 C49 -0.2(8) . . . . ?
C47 C48 C49 C50 0.1(7) . . . . ?
C46 C45 C50 O41 179.2(3) . . . . ?
C44 C45 C50 O41 0.5(5) . . . . ?
C46 C45 C50 C49 -1.1(6) . . . . ?
C44 C45 C50 C49 -179.8(4) . . . . ?
C42 O41 C50 C45 -1.2(6) . . . . ?
C42 O41 C50 C49 179.1(4) . . . . ?
C48 C49 C50 C45 0.6(7) . . . . ?
C48 C49 C50 O41 -179.7(4) . . . . ?
Tb1 O44 C51 C43 -26.4(5) . . . . ?
Tb1 O44 C51 C52 152.6(2) . . . . ?
C44 C43 C51 O44 -6.1(5) . . . . ?
C42 C43 C51 O44 176.1(3) . . . . ?
C44 C43 C51 C52 175.1(3) . . . . ?
C42 C43 C51 C52 -2.7(5) . . . . ?
C74 N61 C62 C63 1.5(5) . . . . ?
Tb1 N61 C62 C63 -166.3(3) . . . . ?
N61 C62 C63 C64 1.2(6) . . . . ?
C62 C63 C64 C65 -1.9(6) . . . . ?
C63 C64 C65 C74 0.0(6) . . . . ?
C63 C64 C65 C66 -177.8(4) . . . . ?
C74 C65 C66 C67 -3.2(6) . . . . ?
C64 C65 C66 C67 174.6(4) . . . . ?
C65 C66 C67 C68 -0.5(6) . . . . ?
C66 C67 C68 C73 4.0(6) . . . . ?
C66 C67 C68 C69 -174.3(4) . . . . ?
C73 C68 C69 C70 -0.2(5) . . . . ?
C67 C68 C69 C70 178.1(4) . . . . ?
C68 C69 C70 C71 2.5(6) . . . . ?
C69 C70 C71 N72 -1.2(6) . . . . ?
C70 C71 N72 C73 -2.4(5) . . . . ?
C70 C71 N72 Tb1 167.4(3) . . . . ?
C71 N72 C73 C68 4.8(5) . . . . ?
Tb1 N72 C73 C68 -165.6(3) . . . . ?
C71 N72 C73 C74 -173.4(3) . . . . ?
Tb1 N72 C73 C74 16.1(4) . . . . ?
C69 C68 C73 N72 -3.6(5) . . . . ?
C67 C68 C73 N72 178.0(3) . . . . ?
C69 C68 C73 C74 174.6(3) . . . . ?
C67 C68 C73 C74 -3.7(5) . . . . ?
C62 N61 C74 C65 -3.6(5) . . . . ?
Tb1 N61 C74 C65 164.9(3) . . . . ?
C62 N61 C74 C73 173.9(3) . . . . ?
Tb1 N61 C74 C73 -17.6(4) . . . . ?
C64 C65 C74 N61 2.8(5) . . . . ?
C66 C65 C74 N61 -179.2(3) . . . . ?
C64 C65 C74 C73 -174.6(3) . . . . ?
C66 C65 C74 C73 3.3(5) . . . . ?
N72 C73 C74 N61 0.9(5) . . . . ?
C68 C73 C74 N61 -177.4(3) . . . . ?
N72 C73 C74 C65 178.5(3) . . . . ?
C68 C73 C74 C65 0.2(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C12 H12A O81 0.96 2.06 2.949(12) 153.1 . no
C12 H12C O2 0.96 2.59 3.518(7) 161.7 2_567 no
C52 H52C O43 0.96 2.62 3.419(4) 141.0 2_667 no
C71 H71A O2 0.93 2.55 3.233(5) 130.4 2_567 no
O81 H81A O22 0.88(2) 2.39(6) 3.127(10) 142(8) 2_556 no

_refine_diff_density_max         1.249
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.072

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_Tb-batho
_database_code_depnum_ccdc_archive 'CCDC 2013258'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  Tb(Cum)3Bato
# Clave IF-UAP:  TbCum3Bato
# Solicitud: 219
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM)
# Clave datos : ... \BUAP\Sylvain\TbCum3Bato\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_audit_creation_date             2018-12-06

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H37 N2 O12 Tb, 0.7(C2 H6 O)'
_chemical_formula_sum            'C58.40 H41.20 N2 O12.70 Tb'
_chemical_formula_weight         1133.05
_chemical_absolute_configuration .
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.3496 2.7654 '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       ?

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

_cell_length_a                   11.6630(4)
_cell_length_b                   13.2469(6)
_cell_length_c                   18.3330(8)
_cell_angle_alpha                78.553(3)
_cell_angle_beta                 76.079(3)
_cell_angle_gamma                68.680(3)
_cell_volume                     2541.72(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    35290
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      26.80

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.032
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 2 6 0.0170
-3 -2 -6 0.0150
-3 -5 0 0.1910
3 5 1 0.2080
0 1 7 0.0700
0 -1 -7 0.0650

_exptl_absorpt_coefficient_mu    0.786
_shelx_estimated_absorpt_T_min   0.745
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4071
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA 1.82 (Stoe & Cie, 2018)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.500
_diffrn_source_power             0.0325
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1206 frames, 60 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            73159
_diffrn_reflns_av_unetI/netI     0.1015
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.556
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13480
_reflns_number_gt                8056
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA 1.82 (Stoe & Cie, 2018)'
_computing_cell_refinement       'X-AREA 1.82'
_computing_data_reduction        'X-AREA 1.82'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'

_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)+(0.0298P)²] 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         13480
_refine_ls_number_parameters     681
_refine_ls_number_restraints     1
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0750
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_restrained_S_all      0.795
_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
Tb1 Tb 0.40788(2) 0.36250(2) 0.31644(2) 0.04281(6) Uani 1 1 d . . . . .
O1 O 0.3066(3) 0.0627(3) 0.59345(16) 0.0740(9) Uani 1 1 d . . . . .
O2 O 0.3848(3) 0.1534(3) 0.64364(18) 0.0905(11) Uani 1 1 d . . . . .
O3 O 0.4105(3) 0.1933(2) 0.37896(15) 0.0611(7) Uani 1 1 d . . . . .
O4 O 0.4659(2) 0.3342(2) 0.43645(15) 0.0549(7) Uani 1 1 d . . . . .
C2 C 0.3677(4) 0.1379(4) 0.5851(3) 0.0620(11) Uani 1 1 d . . . . .
C3 C 0.4021(3) 0.1887(3) 0.5092(2) 0.0478(9) Uani 1 1 d . . . . .
C4 C 0.3783(3) 0.1578(3) 0.4466(2) 0.0475(9) Uani 1 1 d . . . . .
C5 C 0.3124(3) 0.0792(3) 0.4605(2) 0.0521(10) Uani 1 1 d . . . . .
C6 C 0.2803(4) 0.0492(4) 0.4019(3) 0.0704(12) Uani 1 1 d . . . . .
H6A H 0.306060 0.075928 0.352104 0.084 Uiso 1 1 calc R U . . .
C7 C 0.2109(5) -0.0194(4) 0.4165(3) 0.0867(15) Uani 1 1 d . . . . .
H7A H 0.188521 -0.038753 0.377243 0.104 Uiso 1 1 calc R U . . .
C8 C 0.1752(5) -0.0592(4) 0.4908(4) 0.0949(17) Uani 1 1 d . . . . .
H8A H 0.127582 -0.105149 0.501080 0.114 Uiso 1 1 calc R U . . .
C9 C 0.2078(5) -0.0330(4) 0.5497(3) 0.0872(16) Uani 1 1 d . . . . .
H9A H 0.184433 -0.061837 0.599325 0.105 Uiso 1 1 calc R U . . .
C10 C 0.2764(4) 0.0376(3) 0.5336(3) 0.0615(11) Uani 1 1 d . . . . .
C11 C 0.4579(3) 0.2732(3) 0.4981(2) 0.0506(10) Uani 1 1 d . . . . .
C12 C 0.5097(4) 0.2923(4) 0.5598(2) 0.0734(13) Uani 1 1 d . . . . .
H12A H 0.568626 0.225043 0.577783 0.110 Uiso 1 1 calc R U . . .
H12B H 0.442621 0.318544 0.600820 0.110 Uiso 1 1 calc R U . . .
H12C H 0.551085 0.345523 0.540205 0.110 Uiso 1 1 calc R U . . .
O21 O -0.1481(2) 0.5798(3) 0.43226(17) 0.0685(8) Uani 1 1 d . . . . .
O22 O -0.0824(3) 0.7139(3) 0.4358(2) 0.0989(12) Uani 1 1 d . . . . .
O23 O 0.2009(2) 0.3837(2) 0.34536(18) 0.0714(9) Uani 1 1 d . . . . .
O24 O 0.2895(2) 0.5348(2) 0.35889(15) 0.0548(7) Uani 1 1 d . . . . .
C22 C -0.0513(4) 0.6231(4) 0.4202(3) 0.0628(12) Uani 1 1 d . . . . .
C23 C 0.0754(3) 0.5536(3) 0.3909(2) 0.0494(9) Uani 1 1 d . . . . .
C24 C 0.0962(3) 0.4493(4) 0.3727(2) 0.0531(10) Uani 1 1 d . . . . .
C25 C -0.0124(3) 0.4128(3) 0.3843(2) 0.0525(10) Uani 1 1 d . . . . .
C26 C 0.0006(4) 0.3115(4) 0.3660(2) 0.0618(11) Uani 1 1 d . . . . .
H26A H 0.079162 0.265835 0.345896 0.074 Uiso 1 1 calc R U . . .
C27 C -0.1029(4) 0.2788(4) 0.3778(2) 0.0666(12) Uani 1 1 d . . . . .
H27A H -0.094428 0.211549 0.365204 0.080 Uiso 1 1 calc R U . . .
C28 C -0.2184(4) 0.3465(4) 0.4084(3) 0.0702(13) Uani 1 1 d . . . . .
H28A H -0.287826 0.324096 0.416326 0.084 Uiso 1 1 calc R U . . .
C29 C -0.2335(4) 0.4455(4) 0.4274(3) 0.0685(13) Uani 1 1 d . . . . .
H29A H -0.312103 0.490042 0.448516 0.082 Uiso 1 1 calc R U . . .
C30 C -0.1288(3) 0.4790(4) 0.4145(2) 0.0568(11) Uani 1 1 d . . . . .
C31 C 0.1786(4) 0.5935(3) 0.3792(2) 0.0508(10) Uani 1 1 d . . . . .
C32 C 0.1602(4) 0.7086(4) 0.3899(3) 0.0753(14) Uani 1 1 d . . . . .
H32A H 0.118319 0.721476 0.440764 0.113 Uiso 1 1 calc R U . . .
H32B H 0.110347 0.759015 0.354943 0.113 Uiso 1 1 calc R U . . .
H32C H 0.240194 0.718538 0.380720 0.113 Uiso 1 1 calc R U . . .
O41 O 0.2420(3) 0.4909(3) 0.01359(17) 0.0823(10) Uani 1 1 d . . . . .
O42 O 0.1788(3) 0.3504(4) 0.0591(2) 0.1034(13) Uani 1 1 d . . . . .
O43 O 0.3909(2) 0.4654(2) 0.19910(15) 0.0607(7) Uani 1 1 d . . . . .
O44 O 0.3838(2) 0.2633(2) 0.23105(15) 0.0579(7) Uani 1 1 d . . . . .
C42 C 0.2378(4) 0.4038(5) 0.0686(3) 0.0748(14) Uani 1 1 d . . . . .
C43 C 0.3020(3) 0.3862(4) 0.1307(2) 0.0580(11) Uani 1 1 d . . . . .
C44 C 0.3505(3) 0.4660(3) 0.1407(2) 0.0524(10) Uani 1 1 d . . . . .
C45 C 0.3570(4) 0.5526(4) 0.0778(2) 0.0586(11) Uani 1 1 d . . . . .
C46 C 0.4202(4) 0.6233(4) 0.0763(3) 0.0715(13) Uani 1 1 d . . . . .
H46A H 0.456194 0.619493 0.117280 0.086 Uiso 1 1 calc R U . . .
C47 C 0.4302(5) 0.6994(4) 0.0142(3) 0.0838(15) Uani 1 1 d . . . . .
H47A H 0.474672 0.745767 0.012625 0.101 Uiso 1 1 calc R U . . .
C48 C 0.3738(5) 0.7068(5) -0.0459(3) 0.0909(17) Uani 1 1 d . . . . .
H48A H 0.378734 0.759391 -0.087407 0.109 Uiso 1 1 calc R U . . .
C49 C 0.3112(5) 0.6374(5) -0.0445(3) 0.0876(16) Uani 1 1 d . . . . .
H49A H 0.273263 0.642824 -0.084990 0.105 Uiso 1 1 calc R U . . .
C50 C 0.3037(4) 0.5598(4) 0.0162(2) 0.0674(12) Uani 1 1 d . . . . .
C51 C 0.3276(3) 0.2828(4) 0.1777(2) 0.0568(11) Uani 1 1 d . . . . .
C52 C 0.2982(5) 0.1879(4) 0.1630(3) 0.0954(17) Uani 1 1 d . . . . .
H52A H 0.315357 0.184540 0.109451 0.143 Uiso 1 1 calc R U . . .
H52B H 0.211378 0.197256 0.182639 0.143 Uiso 1 1 calc R U . . .
H52C H 0.349111 0.121394 0.187480 0.143 Uiso 1 1 calc R U . . .
N1 N 0.5759(3) 0.4556(3) 0.27998(16) 0.0442(7) Uani 1 1 d . . . . .
N2 N 0.6287(3) 0.2420(3) 0.26902(17) 0.0467(7) Uani 1 1 d . . . . .
C61 C 0.5496(3) 0.5595(3) 0.2848(2) 0.0544(10) Uani 1 1 d . . . . .
H61A H 0.470335 0.597524 0.309515 0.065 Uiso 1 1 calc R U . . .
C62 C 0.6340(3) 0.6159(3) 0.2548(2) 0.0544(10) Uani 1 1 d . . . . .
H62A H 0.610335 0.689267 0.260655 0.065 Uiso 1 1 calc R U . . .
C63 C 0.7506(3) 0.5650(3) 0.2171(2) 0.0480(9) Uani 1 1 d . . . . .
C64 C 0.7837(3) 0.4514(3) 0.2112(2) 0.0457(9) Uani 1 1 d . . . . .
C65 C 0.9038(3) 0.3860(3) 0.1766(2) 0.0533(10) Uani 1 1 d . . . . .
H65A H 0.964734 0.418507 0.155603 0.064 Uiso 1 1 calc R U . . .
C66 C 0.9325(3) 0.2792(3) 0.1730(2) 0.0545(10) Uani 1 1 d . . . . .
H66A H 1.012172 0.239651 0.149631 0.065 Uiso 1 1 calc R U . . .
C67 C 0.8415(3) 0.2254(3) 0.2048(2) 0.0467(9) Uani 1 1 d . . . . .
C68 C 0.8678(3) 0.1125(3) 0.2032(2) 0.0523(10) Uani 1 1 d . . . . .
C69 C 0.7747(4) 0.0691(3) 0.2349(2) 0.0573(10) Uani 1 1 d . . . . .
H69A H 0.789923 -0.005014 0.235476 0.069 Uiso 1 1 calc R U . . .
C70 C 0.6575(4) 0.1355(3) 0.2664(2) 0.0546(10) Uani 1 1 d . . . . .
H70A H 0.595492 0.104039 0.286807 0.066 Uiso 1 1 calc R U . . .
C71 C 0.7223(3) 0.2863(3) 0.23898(19) 0.0427(9) Uani 1 1 d . . . . .
C72 C 0.6919(3) 0.4016(3) 0.24341(19) 0.0423(8) Uani 1 1 d . . . . .
C73 C 0.8413(3) 0.6250(3) 0.1853(2) 0.0508(9) Uani 1 1 d . . . . .
C74 C 0.8707(4) 0.6777(4) 0.2317(3) 0.0671(12) Uani 1 1 d . . . . .
H74A H 0.834186 0.675841 0.282730 0.081 Uiso 1 1 calc R U . . .
C75 C 0.9554(5) 0.7340(4) 0.2023(3) 0.0871(16) Uani 1 1 d . . . . .
H75A H 0.976851 0.768260 0.234124 0.105 Uiso 1 1 calc R U . . .
C76 C 1.0067(5) 0.7390(5) 0.1276(4) 0.0963(18) Uani 1 1 d . . . . .
H76A H 1.063453 0.776476 0.108216 0.116 Uiso 1 1 calc R U . . .
C77 C 0.9756(4) 0.6897(4) 0.0811(3) 0.0857(16) Uani 1 1 d . . . . .
H77A H 1.009477 0.695123 0.029668 0.103 Uiso 1 1 calc R U . . .
C78 C 0.8938(4) 0.6312(4) 0.1091(2) 0.0647(12) Uani 1 1 d . . . . .
H78A H 0.874237 0.596318 0.076854 0.078 Uiso 1 1 calc R U . . .
C79 C 0.9942(4) 0.0444(4) 0.1697(3) 0.0753(14) Uani 1 1 d . . . . .
C80 C 1.0308(6) 0.0494(6) 0.0922(4) 0.135(3) Uani 1 1 d . . . . .
H80A H 0.974658 0.093273 0.061007 0.162 Uiso 1 1 calc R U . . .
C81 C 1.1509(10) -0.0108(10) 0.0606(8) 0.209(7) Uani 1 1 d . . . . .
H81A H 1.176702 -0.007863 0.008335 0.250 Uiso 1 1 calc R U . . .
C82 C 1.2307(9) -0.0747(10) 0.1081(11) 0.209(9) Uani 1 1 d . . . . .
H82A H 1.312198 -0.113589 0.086999 0.251 Uiso 1 1 calc R U . . .
C83 C 1.1975(8) -0.0838(8) 0.1828(8) 0.201(5) Uani 1 1 d . . . . .
H83A H 1.252932 -0.129467 0.213893 0.241 Uiso 1 1 calc R U . . .
C84 C 1.0749(6) -0.0215(6) 0.2132(5) 0.135(3) Uani 1 1 d . . . . .
H84A H 1.049229 -0.026551 0.265490 0.162 Uiso 1 1 calc R U . . .
C91 C 0.5915(9) -0.1053(11) 0.0899(6) 0.160(5) Uani 0.7 1 d . . P . .
H91A H 0.662159 -0.109176 0.049490 0.240 Uiso 0.7 1 calc R U P . .
H91B H 0.517957 -0.051110 0.074354 0.240 Uiso 0.7 1 calc R U P . .
H91C H 0.579380 -0.175014 0.102306 0.240 Uiso 0.7 1 calc R U P . .
C92 C 0.6126(9) -0.0780(8) 0.1511(6) 0.124(3) Uani 0.7 1 d D . P . .
H92A H 0.614650 -0.003878 0.139849 0.149 Uiso 0.7 1 calc R U P . .
H92B H 0.694425 -0.125657 0.160939 0.149 Uiso 0.7 1 calc R U P . .
O92 O 0.5208(8) -0.0849(6) 0.2185(4) 0.146(3) Uani 0.7 1 d D . P . .
H92 H 0.524580 -0.049339 0.249182 0.220 Uiso 0.7 1 calc R U P . .


_geom_special_details            ?

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 O23 2.266(2) . ?
Tb1 O3 2.299(3) . ?
Tb1 O43 2.317(3) . ?
Tb1 O44 2.357(3) . ?
Tb1 O24 2.370(3) . ?
Tb1 O4 2.376(3) . ?
Tb1 N2 2.534(3) . ?
Tb1 N1 2.570(3) . ?
O1 C10 1.360(5) . ?
O1 C2 1.390(5) . ?
O2 C2 1.205(5) . ?
O3 C4 1.255(4) . ?
O4 C11 1.257(4) . ?
C2 C3 1.452(5) . ?
C3 C4 1.408(5) . ?
C3 C11 1.447(5) . ?
C4 C5 1.457(5) . ?
C5 C10 1.372(5) . ?
C5 C6 1.386(6) . ?
C6 C7 1.374(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.381(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.369(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.388(6) . ?
C9 H9A 0.9300 . ?
C11 C12 1.505(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.364(5) . ?
O21 C22 1.398(5) . ?
O22 C22 1.195(5) . ?
O23 C24 1.267(4) . ?
O24 C31 1.252(4) . ?
C22 C23 1.464(5) . ?
C23 C24 1.407(5) . ?
C23 C31 1.438(5) . ?
C24 C25 1.469(5) . ?
C25 C30 1.372(5) . ?
C25 C26 1.392(5) . ?
C26 C27 1.382(5) . ?
C26 H26A 0.9300 . ?
C27 C28 1.375(6) . ?
C27 H27A 0.9300 . ?
C28 C29 1.362(6) . ?
C28 H28A 0.9300 . ?
C29 C30 1.399(5) . ?
C29 H29A 0.9300 . ?
C31 C32 1.506(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.365(5) . ?
O41 C42 1.382(6) . ?
O42 C42 1.211(5) . ?
O43 C44 1.267(4) . ?
O44 C51 1.241(4) . ?
C42 C43 1.444(6) . ?
C43 C44 1.425(5) . ?
C43 C51 1.438(6) . ?
C44 C45 1.466(6) . ?
C45 C46 1.379(6) . ?
C45 C50 1.387(6) . ?
C46 C47 1.375(6) . ?
C46 H46A 0.9300 . ?
C47 C48 1.385(7) . ?
C47 H47A 0.9300 . ?
C48 C49 1.359(7) . ?
C48 H48A 0.9300 . ?
C49 C50 1.367(6) . ?
C49 H49A 0.9300 . ?
C51 C52 1.503(6) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N1 C61 1.314(4) . ?
N1 C72 1.357(4) . ?
N2 C70 1.333(5) . ?
N2 C71 1.374(4) . ?
C61 C62 1.393(5) . ?
C61 H61A 0.9300 . ?
C62 C63 1.359(5) . ?
C62 H62A 0.9300 . ?
C63 C64 1.430(5) . ?
C63 C73 1.491(5) . ?
C64 C72 1.409(4) . ?
C64 C65 1.423(5) . ?
C65 C66 1.341(5) . ?
C65 H65A 0.9300 . ?
C66 C67 1.436(5) . ?
C66 H66A 0.9300 . ?
C67 C71 1.394(5) . ?
C67 C68 1.418(5) . ?
C68 C69 1.366(5) . ?
C68 C79 1.477(6) . ?
C69 C70 1.387(5) . ?
C69 H69A 0.9300 . ?
C70 H70A 0.9300 . ?
C71 C72 1.452(5) . ?
C73 C74 1.370(5) . ?
C73 C78 1.384(5) . ?
C74 C75 1.394(6) . ?
C74 H74A 0.9300 . ?
C75 C76 1.356(7) . ?
C75 H75A 0.9300 . ?
C76 C77 1.352(7) . ?
C76 H76A 0.9300 . ?
C77 C78 1.385(5) . ?
C77 H77A 0.9300 . ?
C78 H78A 0.9300 . ?
C79 C84 1.331(8) . ?
C79 C80 1.377(8) . ?
C80 C81 1.384(10) . ?
C80 H80A 0.9300 . ?
C81 C82 1.37(2) . ?
C81 H81A 0.9300 . ?
C82 C83 1.324(18) . ?
C82 H82A 0.9300 . ?
C83 C84 1.406(10) . ?
C83 H83A 0.9300 . ?
C84 H84A 0.9300 . ?
C91 C92 1.344(11) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C92 O92 1.439(7) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
O92 H92 0.8200 . ?

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
O23 Tb1 O3 78.48(11) . . ?
O23 Tb1 O43 92.70(11) . . ?
O3 Tb1 O43 141.22(9) . . ?
O23 Tb1 O44 76.45(9) . . ?
O3 Tb1 O44 72.09(9) . . ?
O43 Tb1 O44 69.13(9) . . ?
O23 Tb1 O24 69.30(9) . . ?
O3 Tb1 O24 127.50(9) . . ?
O43 Tb1 O24 81.90(10) . . ?
O44 Tb1 O24 133.54(9) . . ?
O23 Tb1 O4 103.77(10) . . ?
O3 Tb1 O4 68.91(9) . . ?
O43 Tb1 O4 148.95(9) . . ?
O44 Tb1 O4 139.98(9) . . ?
O24 Tb1 O4 79.70(9) . . ?
O23 Tb1 N2 147.51(9) . . ?
O3 Tb1 N2 77.38(10) . . ?
O43 Tb1 N2 92.64(10) . . ?
O44 Tb1 N2 75.64(9) . . ?
O24 Tb1 N2 143.19(8) . . ?
O4 Tb1 N2 87.40(9) . . ?
O23 Tb1 N1 147.07(10) . . ?
O3 Tb1 N1 131.81(10) . . ?
O43 Tb1 N1 71.18(9) . . ?
O44 Tb1 N1 120.66(9) . . ?
O24 Tb1 N1 79.87(9) . . ?
O4 Tb1 N1 81.09(9) . . ?
N2 Tb1 N1 64.05(9) . . ?
C10 O1 C2 122.3(3) . . ?
C4 O3 Tb1 134.3(2) . . ?
C11 O4 Tb1 138.5(2) . . ?
O2 C2 O1 114.3(4) . . ?
O2 C2 C3 127.9(4) . . ?
O1 C2 C3 117.7(4) . . ?
C4 C3 C11 120.1(3) . . ?
C4 C3 C2 120.1(3) . . ?
C11 C3 C2 119.8(4) . . ?
O3 C4 C3 124.3(3) . . ?
O3 C4 C5 117.2(3) . . ?
C3 C4 C5 118.5(3) . . ?
C10 C5 C6 119.3(4) . . ?
C10 C5 C4 119.0(4) . . ?
C6 C5 C4 121.6(4) . . ?
C7 C6 C5 120.7(4) . . ?
C7 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C6 C7 C8 118.6(5) . . ?
C6 C7 H7A 120.7 . . ?
C8 C7 H7A 120.7 . . ?
C9 C8 C7 122.0(5) . . ?
C9 C8 H8A 119.0 . . ?
C7 C8 H8A 119.0 . . ?
C8 C9 C10 118.3(5) . . ?
C8 C9 H9A 120.8 . . ?
C10 C9 H9A 120.8 . . ?
O1 C10 C5 122.1(4) . . ?
O1 C10 C9 116.9(4) . . ?
C5 C10 C9 121.0(4) . . ?
O4 C11 C3 121.8(3) . . ?
O4 C11 C12 116.6(4) . . ?
C3 C11 C12 121.6(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 122.4(3) . . ?
C24 O23 Tb1 141.4(2) . . ?
C31 O24 Tb1 141.1(2) . . ?
O22 C22 O21 115.2(4) . . ?
O22 C22 C23 127.4(4) . . ?
O21 C22 C23 117.4(4) . . ?
C24 C23 C31 120.0(3) . . ?
C24 C23 C22 120.5(3) . . ?
C31 C23 C22 119.5(4) . . ?
O23 C24 C23 125.7(3) . . ?
O23 C24 C25 116.2(4) . . ?
C23 C24 C25 118.0(3) . . ?
C30 C25 C26 119.2(3) . . ?
C30 C25 C24 119.6(4) . . ?
C26 C25 C24 121.2(4) . . ?
C27 C26 C25 120.1(4) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C28 C27 C26 119.5(4) . . ?
C28 C27 H27A 120.2 . . ?
C26 C27 H27A 120.2 . . ?
C29 C28 C27 121.5(4) . . ?
C29 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
C28 C29 C30 118.8(4) . . ?
C28 C29 H29A 120.6 . . ?
C30 C29 H29A 120.6 . . ?
O21 C30 C25 122.0(3) . . ?
O21 C30 C29 117.2(4) . . ?
C25 C30 C29 120.8(4) . . ?
O24 C31 C23 121.9(4) . . ?
O24 C31 C32 115.8(3) . . ?
C23 C31 C32 122.2(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.5(4) . . ?
C44 O43 Tb1 137.8(3) . . ?
C51 O44 Tb1 137.4(3) . . ?
O42 C42 O41 115.1(4) . . ?
O42 C42 C43 127.1(5) . . ?
O41 C42 C43 117.8(4) . . ?
C44 C43 C51 120.1(4) . . ?
C44 C43 C42 120.5(4) . . ?
C51 C43 C42 119.1(4) . . ?
O43 C44 C43 124.6(4) . . ?
O43 C44 C45 118.2(4) . . ?
C43 C44 C45 117.2(4) . . ?
C46 C45 C50 119.1(4) . . ?
C46 C45 C44 122.0(4) . . ?
C50 C45 C44 118.8(4) . . ?
C47 C46 C45 120.1(5) . . ?
C47 C46 H46A 119.9 . . ?
C45 C46 H46A 119.9 . . ?
C46 C47 C48 119.8(5) . . ?
C46 C47 H47A 120.1 . . ?
C48 C47 H47A 120.1 . . ?
C49 C48 C47 120.2(5) . . ?
C49 C48 H48A 119.9 . . ?
C47 C48 H48A 119.9 . . ?
C48 C49 C50 120.2(5) . . ?
C48 C49 H49A 119.9 . . ?
C50 C49 H49A 119.9 . . ?
O41 C50 C49 117.5(5) . . ?
O41 C50 C45 122.0(4) . . ?
C49 C50 C45 120.5(5) . . ?
O44 C51 C43 121.6(4) . . ?
O44 C51 C52 114.9(4) . . ?
C43 C51 C52 123.4(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 N1 C72 117.3(3) . . ?
C61 N1 Tb1 122.5(2) . . ?
C72 N1 Tb1 119.4(2) . . ?
C70 N2 C71 116.9(3) . . ?
C70 N2 Tb1 122.3(2) . . ?
C71 N2 Tb1 120.6(2) . . ?
N1 C61 C62 123.6(4) . . ?
N1 C61 H61A 118.2 . . ?
C62 C61 H61A 118.2 . . ?
C63 C62 C61 120.8(4) . . ?
C63 C62 H62A 119.6 . . ?
C61 C62 H62A 119.6 . . ?
C62 C63 C64 117.5(3) . . ?
C62 C63 C73 120.9(3) . . ?
C64 C63 C73 121.6(3) . . ?
C72 C64 C65 118.5(3) . . ?
C72 C64 C63 117.5(3) . . ?
C65 C64 C63 124.0(3) . . ?
C66 C65 C64 122.6(3) . . ?
C66 C65 H65A 118.7 . . ?
C64 C65 H65A 118.7 . . ?
C65 C66 C67 120.7(3) . . ?
C65 C66 H66A 119.7 . . ?
C67 C66 H66A 119.7 . . ?
C71 C67 C68 118.4(3) . . ?
C71 C67 C66 118.8(3) . . ?
C68 C67 C66 122.8(3) . . ?
C69 C68 C67 118.3(3) . . ?
C69 C68 C79 121.7(4) . . ?
C67 C68 C79 120.1(3) . . ?
C68 C69 C70 119.9(4) . . ?
C68 C69 H69A 120.0 . . ?
C70 C69 H69A 120.0 . . ?
N2 C70 C69 123.8(3) . . ?
N2 C70 H70A 118.1 . . ?
C69 C70 H70A 118.1 . . ?
N2 C71 C67 122.6(3) . . ?
N2 C71 C72 117.0(3) . . ?
C67 C71 C72 120.3(3) . . ?
N1 C72 C64 123.3(3) . . ?
N1 C72 C71 117.6(3) . . ?
C64 C72 C71 119.1(3) . . ?
C74 C73 C78 119.2(3) . . ?
C74 C73 C63 119.7(4) . . ?
C78 C73 C63 121.0(3) . . ?
C73 C74 C75 120.0(4) . . ?
C73 C74 H74A 120.0 . . ?
C75 C74 H74A 120.0 . . ?
C76 C75 C74 120.2(5) . . ?
C76 C75 H75A 119.9 . . ?
C74 C75 H75A 119.9 . . ?
C77 C76 C75 120.1(4) . . ?
C77 C76 H76A 120.0 . . ?
C75 C76 H76A 120.0 . . ?
C76 C77 C78 120.9(5) . . ?
C76 C77 H77A 119.6 . . ?
C78 C77 H77A 119.6 . . ?
C73 C78 C77 119.6(4) . . ?
C73 C78 H78A 120.2 . . ?
C77 C78 H78A 120.2 . . ?
C84 C79 C80 118.9(6) . . ?
C84 C79 C68 121.1(6) . . ?
C80 C79 C68 120.0(6) . . ?
C79 C80 C81 120.1(9) . . ?
C79 C80 H80A 119.9 . . ?
C81 C80 H80A 119.9 . . ?
C82 C81 C80 118.3(13) . . ?
C82 C81 H81A 120.8 . . ?
C80 C81 H81A 120.8 . . ?
C83 C82 C81 123.1(11) . . ?
C83 C82 H82A 118.4 . . ?
C81 C82 H82A 118.4 . . ?
C82 C83 C84 117.2(12) . . ?
C82 C83 H83A 121.4 . . ?
C84 C83 H83A 121.4 . . ?
C79 C84 C83 122.3(9) . . ?
C79 C84 H84A 118.8 . . ?
C83 C84 H84A 118.8 . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C91 C92 O92 114.2(8) . . ?
C91 C92 H92A 108.7 . . ?
O92 C92 H92A 108.7 . . ?
C91 C92 H92B 108.7 . . ?
O92 C92 H92B 108.7 . . ?
H92A C92 H92B 107.6 . . ?
C92 O92 H92 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 178.1(4) . . . . ?
C10 O1 C2 C3 -1.4(6) . . . . ?
O2 C2 C3 C4 177.8(4) . . . . ?
O1 C2 C3 C4 -2.7(6) . . . . ?
O2 C2 C3 C11 -3.8(7) . . . . ?
O1 C2 C3 C11 175.6(3) . . . . ?
Tb1 O3 C4 C3 -42.1(5) . . . . ?
Tb1 O3 C4 C5 138.1(3) . . . . ?
C11 C3 C4 O3 5.4(6) . . . . ?
C2 C3 C4 O3 -176.3(4) . . . . ?
C11 C3 C4 C5 -174.8(3) . . . . ?
C2 C3 C4 C5 3.5(5) . . . . ?
O3 C4 C5 C10 179.5(4) . . . . ?
C3 C4 C5 C10 -0.4(5) . . . . ?
O3 C4 C5 C6 -3.5(6) . . . . ?
C3 C4 C5 C6 176.7(4) . . . . ?
C10 C5 C6 C7 1.4(7) . . . . ?
C4 C5 C6 C7 -175.7(4) . . . . ?
C5 C6 C7 C8 -0.8(8) . . . . ?
C6 C7 C8 C9 -0.6(9) . . . . ?
C7 C8 C9 C10 1.4(9) . . . . ?
C2 O1 C10 C5 4.8(6) . . . . ?
C2 O1 C10 C9 -175.6(4) . . . . ?
C6 C5 C10 O1 179.0(4) . . . . ?
C4 C5 C10 O1 -3.8(6) . . . . ?
C6 C5 C10 C9 -0.5(7) . . . . ?
C4 C5 C10 C9 176.6(4) . . . . ?
C8 C9 C10 O1 179.6(5) . . . . ?
C8 C9 C10 C5 -0.9(8) . . . . ?
Tb1 O4 C11 C3 1.8(6) . . . . ?
Tb1 O4 C11 C12 -178.4(3) . . . . ?
C4 C3 C11 O4 13.0(6) . . . . ?
C2 C3 C11 O4 -165.4(4) . . . . ?
C4 C3 C11 C12 -166.8(4) . . . . ?
C2 C3 C11 C12 14.8(6) . . . . ?
C30 O21 C22 O22 177.4(4) . . . . ?
C30 O21 C22 C23 -3.1(6) . . . . ?
O22 C22 C23 C24 -177.8(5) . . . . ?
O21 C22 C23 C24 2.7(6) . . . . ?
O22 C22 C23 C31 0.9(7) . . . . ?
O21 C22 C23 C31 -178.5(4) . . . . ?
Tb1 O23 C24 C23 6.8(8) . . . . ?
Tb1 O23 C24 C25 -174.8(3) . . . . ?
C31 C23 C24 O23 -0.5(7) . . . . ?
C22 C23 C24 O23 178.2(4) . . . . ?
C31 C23 C24 C25 -178.9(4) . . . . ?
C22 C23 C24 C25 -0.2(6) . . . . ?
O23 C24 C25 C30 179.3(4) . . . . ?
C23 C24 C25 C30 -2.2(6) . . . . ?
O23 C24 C25 C26 0.1(6) . . . . ?
C23 C24 C25 C26 178.6(4) . . . . ?
C30 C25 C26 C27 0.5(6) . . . . ?
C24 C25 C26 C27 179.6(4) . . . . ?
C25 C26 C27 C28 -0.7(7) . . . . ?
C26 C27 C28 C29 0.1(7) . . . . ?
C27 C28 C29 C30 0.7(7) . . . . ?
C22 O21 C30 C25 0.8(6) . . . . ?
C22 O21 C30 C29 -178.4(4) . . . . ?
C26 C25 C30 O21 -178.8(4) . . . . ?
C24 C25 C30 O21 2.0(6) . . . . ?
C26 C25 C30 C29 0.3(6) . . . . ?
C24 C25 C30 C29 -178.8(4) . . . . ?
C28 C29 C30 O21 178.3(4) . . . . ?
C28 C29 C30 C25 -0.9(6) . . . . ?
Tb1 O24 C31 C23 8.3(6) . . . . ?
Tb1 O24 C31 C32 -171.1(3) . . . . ?
C24 C23 C31 O24 -5.9(6) . . . . ?
C22 C23 C31 O24 175.3(4) . . . . ?
C24 C23 C31 C32 173.5(4) . . . . ?
C22 C23 C31 C32 -5.3(6) . . . . ?
C50 O41 C42 O42 179.4(4) . . . . ?
C50 O41 C42 C43 -0.1(6) . . . . ?
O42 C42 C43 C44 -169.8(5) . . . . ?
O41 C42 C43 C44 9.7(6) . . . . ?
O42 C42 C43 C51 16.5(7) . . . . ?
O41 C42 C43 C51 -164.0(4) . . . . ?
Tb1 O43 C44 C43 -3.2(6) . . . . ?
Tb1 O43 C44 C45 178.5(3) . . . . ?
C51 C43 C44 O43 -17.5(6) . . . . ?
C42 C43 C44 O43 168.9(4) . . . . ?
C51 C43 C44 C45 160.8(4) . . . . ?
C42 C43 C44 C45 -12.9(5) . . . . ?
O43 C44 C45 C46 9.0(6) . . . . ?
C43 C44 C45 C46 -169.4(4) . . . . ?
O43 C44 C45 C50 -174.7(4) . . . . ?
C43 C44 C45 C50 7.0(5) . . . . ?
C50 C45 C46 C47 -0.1(7) . . . . ?
C44 C45 C46 C47 176.2(4) . . . . ?
C45 C46 C47 C48 1.7(7) . . . . ?
C46 C47 C48 C49 -1.5(8) . . . . ?
C47 C48 C49 C50 -0.1(8) . . . . ?
C42 O41 C50 C49 174.4(4) . . . . ?
C42 O41 C50 C45 -5.9(6) . . . . ?
C48 C49 C50 O41 -178.6(4) . . . . ?
C48 C49 C50 C45 1.7(7) . . . . ?
C46 C45 C50 O41 178.7(4) . . . . ?
C44 C45 C50 O41 2.3(6) . . . . ?
C46 C45 C50 C49 -1.6(7) . . . . ?
C44 C45 C50 C49 -178.0(4) . . . . ?
Tb1 O44 C51 C43 29.5(6) . . . . ?
Tb1 O44 C51 C52 -155.0(3) . . . . ?
C44 C43 C51 O44 5.3(6) . . . . ?
C42 C43 C51 O44 179.1(4) . . . . ?
C44 C43 C51 C52 -169.8(4) . . . . ?
C42 C43 C51 C52 4.0(6) . . . . ?
C72 N1 C61 C62 -0.2(6) . . . . ?
Tb1 N1 C61 C62 -169.8(3) . . . . ?
N1 C61 C62 C63 1.0(6) . . . . ?
C61 C62 C63 C64 -1.5(6) . . . . ?
C61 C62 C63 C73 -179.7(4) . . . . ?
C62 C63 C64 C72 1.4(5) . . . . ?
C73 C63 C64 C72 179.6(3) . . . . ?
C62 C63 C64 C65 -177.0(4) . . . . ?
C73 C63 C64 C65 1.1(6) . . . . ?
C72 C64 C65 C66 0.5(6) . . . . ?
C63 C64 C65 C66 179.0(4) . . . . ?
C64 C65 C66 C67 -0.2(6) . . . . ?
C65 C66 C67 C71 0.5(6) . . . . ?
C65 C66 C67 C68 -179.2(4) . . . . ?
C71 C67 C68 C69 0.3(6) . . . . ?
C66 C67 C68 C69 -179.9(4) . . . . ?
C71 C67 C68 C79 -178.0(4) . . . . ?
C66 C67 C68 C79 1.7(6) . . . . ?
C67 C68 C69 C70 1.2(6) . . . . ?
C79 C68 C69 C70 179.5(4) . . . . ?
C71 N2 C70 C69 -0.5(6) . . . . ?
Tb1 N2 C70 C69 174.4(3) . . . . ?
C68 C69 C70 N2 -1.1(6) . . . . ?
C70 N2 C71 C67 2.1(5) . . . . ?
Tb1 N2 C71 C67 -172.9(3) . . . . ?
C70 N2 C71 C72 -178.6(3) . . . . ?
Tb1 N2 C71 C72 6.5(4) . . . . ?
C68 C67 C71 N2 -2.0(5) . . . . ?
C66 C67 C71 N2 178.2(3) . . . . ?
C68 C67 C71 C72 178.7(3) . . . . ?
C66 C67 C71 C72 -1.1(5) . . . . ?
C61 N1 C72 C64 0.2(5) . . . . ?
Tb1 N1 C72 C64 170.1(3) . . . . ?
C61 N1 C72 C71 179.0(3) . . . . ?
Tb1 N1 C72 C71 -11.1(4) . . . . ?
C65 C64 C72 N1 177.7(3) . . . . ?
C63 C64 C72 N1 -0.8(5) . . . . ?
C65 C64 C72 C71 -1.1(5) . . . . ?
C63 C64 C72 C71 -179.6(3) . . . . ?
N2 C71 C72 N1 3.2(5) . . . . ?
C67 C71 C72 N1 -177.5(3) . . . . ?
N2 C71 C72 C64 -178.0(3) . . . . ?
C67 C71 C72 C64 1.4(5) . . . . ?
C62 C63 C73 C74 55.1(6) . . . . ?
C64 C63 C73 C74 -122.9(4) . . . . ?
C62 C63 C73 C78 -123.0(4) . . . . ?
C64 C63 C73 C78 58.9(5) . . . . ?
C78 C73 C74 C75 -1.8(7) . . . . ?
C63 C73 C74 C75 -180.0(4) . . . . ?
C73 C74 C75 C76 1.5(8) . . . . ?
C74 C75 C76 C77 0.2(9) . . . . ?
C75 C76 C77 C78 -1.7(9) . . . . ?
C74 C73 C78 C77 0.4(7) . . . . ?
C63 C73 C78 C77 178.6(4) . . . . ?
C76 C77 C78 C73 1.3(8) . . . . ?
C69 C68 C79 C84 -76.1(6) . . . . ?
C67 C68 C79 C84 102.2(6) . . . . ?
C69 C68 C79 C80 104.6(6) . . . . ?
C67 C68 C79 C80 -77.1(6) . . . . ?
C84 C79 C80 C81 -2.1(10) . . . . ?
C68 C79 C80 C81 177.3(6) . . . . ?
C79 C80 C81 C82 0.2(14) . . . . ?
C80 C81 C82 C83 2(2) . . . . ?
C81 C82 C83 C84 -1.9(19) . . . . ?
C80 C79 C84 C83 2.0(10) . . . . ?
C68 C79 C84 C83 -177.3(6) . . . . ?
C82 C83 C84 C79 -0.1(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C61 H61A O24 0.93 2.45 3.118(4) 128.5 . yes
C70 H70A O3 0.93 2.47 3.051(5) 120.8 . yes

_refine_diff_density_max         1.162
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.075

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_Eu-batho
_database_code_depnum_ccdc_archive 'CCDC 2013257'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  EuBF
# Clave IF-UAP:  EuBF
# Solicitud: 235
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM) 
# Clave datos : ... \BUAP\Sylvain\EuBF\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_audit_creation_date             2019-01-17

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H37 Eu N2 O12, 0.7(C2 H6 O)'
_chemical_formula_sum            'C58.40 H41.20 Eu N2 O12.70'
_chemical_formula_weight         1126.09
_chemical_absolute_configuration ?
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.3977 2.4351 '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       ?

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

_cell_length_a                   11.7006(4)
_cell_length_b                   13.2487(6)
_cell_length_c                   18.3375(8)
_cell_angle_alpha                78.623(3)
_cell_angle_beta                 76.024(3)
_cell_angle_gamma                68.680(3)
_cell_volume                     2550.80(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    73654
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      27.11

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             1140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.588
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.091
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 7 3 0.0370
-2 -8 -3 0.0540
-1 3 4 0.1070
1 -3 -4 0.0880
3 2 7 0.2450
4 -1 4 0.2760
-5 1 -6 0.3200
-3 -1 -6 0.3120

_exptl_absorpt_coefficient_mu    0.698
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4014
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA 1.82 (Stoe & Cie, 2018)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.500
_diffrn_source_power             0.025
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1195 frames, 65 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            66985
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.752
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             13494
_reflns_number_gt                10568
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA 1.82 (Stoe & Cie, 2018)'
_computing_cell_refinement       'X-AREA 1.82'
_computing_data_reduction        'X-AREA 1.82'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'

_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)+(0.0421P)²+0.2415P] 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         13494
_refine_ls_number_parameters     681
_refine_ls_number_restraints     37
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.056
_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
Eu1 Eu 0.40623(2) 0.36312(2) 0.31722(2) 0.03550(5) Uani 1 1 d . . . . .
O1 O 0.3062(2) 0.0602(2) 0.59397(14) 0.0655(6) Uani 1 1 d . . . . .
O2 O 0.3849(3) 0.1495(3) 0.64450(15) 0.0819(8) Uani 1 1 d . . . . .
O3 O 0.4096(2) 0.19242(18) 0.37967(12) 0.0533(5) Uani 1 1 d . . . . .
O4 O 0.46563(18) 0.33179(17) 0.43878(12) 0.0477(5) Uani 1 1 d . . . . .
C2 C 0.3678(3) 0.1345(3) 0.58563(19) 0.0549(8) Uani 1 1 d . . . . .
C3 C 0.4018(2) 0.1861(2) 0.51042(16) 0.0405(6) Uani 1 1 d . . . . .
C4 C 0.3775(2) 0.1564(2) 0.44726(17) 0.0415(6) Uani 1 1 d . . . . .
C5 C 0.3107(3) 0.0781(2) 0.46079(19) 0.0464(7) Uani 1 1 d . . . . .
C6 C 0.2772(4) 0.0497(3) 0.4018(2) 0.0631(9) Uani 1 1 d . . . . .
H6 H 0.301992 0.077184 0.352088 0.076 Uiso 1 1 calc R U . . .
C7 C 0.2074(4) -0.0190(3) 0.4168(3) 0.0800(12) Uani 1 1 d . . . . .
H7 H 0.184907 -0.038166 0.377462 0.096 Uiso 1 1 calc R U . . .
C8 C 0.1712(4) -0.0591(4) 0.4912(3) 0.0865(14) Uani 1 1 d . . . . .
H8 H 0.122728 -0.104213 0.501442 0.104 Uiso 1 1 calc R U . . .
C9 C 0.2053(4) -0.0336(3) 0.5504(3) 0.0809(12) Uani 1 1 d . . . . .
H9 H 0.181803 -0.062261 0.599930 0.097 Uiso 1 1 calc R U . . .
C10 C 0.2753(3) 0.0359(3) 0.5345(2) 0.0558(8) Uani 1 1 d . . . . .
C11 C 0.4588(2) 0.2693(2) 0.49917(17) 0.0425(6) Uani 1 1 d . . . . .
C12 C 0.5118(4) 0.2867(3) 0.5609(2) 0.0667(10) Uani 1 1 d . . . . .
H12A H 0.570267 0.218949 0.578313 0.100 Uiso 1 1 calc R U . . .
H12B H 0.445381 0.312745 0.602288 0.100 Uiso 1 1 calc R U . . .
H12C H 0.553535 0.339574 0.541577 0.100 Uiso 1 1 calc R U . . .
O21 O -0.15017(18) 0.58243(19) 0.43368(15) 0.0605(6) Uani 1 1 d . . . . .
O22 O -0.0848(2) 0.7157(2) 0.4370(2) 0.0931(11) Uani 1 1 d . . . . .
O23 O 0.19690(19) 0.3858(2) 0.34682(17) 0.0699(8) Uani 1 1 d . . . . .
O24 O 0.28634(18) 0.53703(17) 0.36036(13) 0.0491(5) Uani 1 1 d . . . . .
C22 C -0.0528(3) 0.6243(3) 0.4215(2) 0.0542(8) Uani 1 1 d . . . . .
C23 C 0.0728(2) 0.5556(2) 0.39202(18) 0.0420(6) Uani 1 1 d . . . . .
C24 C 0.0927(2) 0.4516(2) 0.37360(18) 0.0449(7) Uani 1 1 d . . . . .
C25 C -0.0154(2) 0.4149(2) 0.38548(18) 0.0452(7) Uani 1 1 d . . . . .
C26 C -0.0029(3) 0.3141(3) 0.3668(2) 0.0534(8) Uani 1 1 d . . . . .
H26 H 0.075337 0.268329 0.346470 0.064 Uiso 1 1 calc R U . . .
C27 C -0.1063(3) 0.2818(3) 0.3784(2) 0.0599(9) Uani 1 1 d . . . . .
H27 H -0.097816 0.214476 0.365720 0.072 Uiso 1 1 calc R U . . .
C28 C -0.2226(3) 0.3499(3) 0.4090(2) 0.0635(10) Uani 1 1 d . . . . .
H28 H -0.292136 0.328095 0.416429 0.076 Uiso 1 1 calc R U . . .
C29 C -0.2365(3) 0.4488(3) 0.4284(2) 0.0626(9) Uani 1 1 d . . . . .
H29 H -0.314603 0.493387 0.449855 0.075 Uiso 1 1 calc R U . . .
C30 C -0.1318(2) 0.4822(3) 0.41547(19) 0.0490(7) Uani 1 1 d . . . . .
C31 C 0.1760(3) 0.5956(2) 0.38040(18) 0.0431(6) Uani 1 1 d . . . . .
C32 C 0.1573(3) 0.7101(3) 0.3915(3) 0.0699(11) Uani 1 1 d . . . . .
H32A H 0.116227 0.722429 0.442651 0.105 Uiso 1 1 calc R U . . .
H32B H 0.106779 0.760689 0.357136 0.105 Uiso 1 1 calc R U . . .
H32C H 0.236871 0.720480 0.381970 0.105 Uiso 1 1 calc R U . . .
O41 O 0.2417(2) 0.4901(3) 0.01338(15) 0.0736(7) Uani 1 1 d . . . . .
O42 O 0.1779(3) 0.3513(3) 0.05905(17) 0.0946(10) Uani 1 1 d . . . . .
O43 O 0.3907(2) 0.46551(19) 0.19833(13) 0.0558(5) Uani 1 1 d . . . . .
O44 O 0.3824(2) 0.26354(18) 0.23103(13) 0.0524(5) Uani 1 1 d . . . . .
C42 C 0.2372(3) 0.4033(4) 0.0686(2) 0.0652(10) Uani 1 1 d . . . . .
C43 C 0.3017(3) 0.3852(3) 0.13066(18) 0.0498(7) Uani 1 1 d . . . . .
C44 C 0.3494(3) 0.4654(3) 0.14029(17) 0.0475(7) Uani 1 1 d . . . . .
C45 C 0.3564(3) 0.5518(3) 0.07761(18) 0.0522(7) Uani 1 1 d . . . . .
C46 C 0.4195(4) 0.6235(3) 0.0757(2) 0.0624(9) Uani 1 1 d . . . . .
H46 H 0.455167 0.619919 0.116665 0.075 Uiso 1 1 calc R U . . .
C47 C 0.4297(4) 0.7003(3) 0.0134(2) 0.0731(11) Uani 1 1 d . . . . .
H47 H 0.473167 0.747193 0.012106 0.088 Uiso 1 1 calc R U . . .
C48 C 0.3750(4) 0.7066(3) -0.0465(2) 0.0788(12) Uani 1 1 d . . . . .
H48 H 0.381058 0.758506 -0.088223 0.095 Uiso 1 1 calc R U . . .
C49 C 0.3115(4) 0.6371(4) -0.0456(2) 0.0793(12) Uani 1 1 d . . . . .
H49 H 0.274032 0.642605 -0.086222 0.095 Uiso 1 1 calc R U . . .
C50 C 0.3033(3) 0.5589(3) 0.01593(19) 0.0619(9) Uani 1 1 d . . . . .
C51 C 0.3272(3) 0.2825(3) 0.17777(18) 0.0500(7) Uani 1 1 d . . . . .
C52 C 0.2950(5) 0.1896(4) 0.1630(3) 0.0909(15) Uani 1 1 d . . . . .
H52A H 0.319580 0.181755 0.110029 0.136 Uiso 1 1 calc R U . . .
H52B H 0.206604 0.204148 0.178104 0.136 Uiso 1 1 calc R U . . .
H52C H 0.338241 0.123485 0.191539 0.136 Uiso 1 1 calc R U . . .
N1 N 0.5759(2) 0.45589(18) 0.27986(13) 0.0383(5) Uani 1 1 d . . . . .
N2 N 0.6299(2) 0.24178(18) 0.26923(14) 0.0402(5) Uani 1 1 d . . . . .
C61 C 0.5493(3) 0.5610(2) 0.28428(18) 0.0461(7) Uani 1 1 d . . . . .
H61 H 0.470027 0.599200 0.308699 0.055 Uiso 1 1 calc R U . . .
C62 C 0.6337(3) 0.6176(2) 0.25433(19) 0.0487(7) Uani 1 1 d . . . . .
H62 H 0.610176 0.691147 0.259669 0.058 Uiso 1 1 calc R U . . .
C63 C 0.7511(3) 0.5649(2) 0.21710(17) 0.0419(6) Uani 1 1 d . . . . .
C64 C 0.7834(2) 0.4520(2) 0.21141(16) 0.0390(6) Uani 1 1 d . . . . .
C65 C 0.9043(2) 0.3867(2) 0.17621(18) 0.0471(7) Uani 1 1 d . . . . .
H65 H 0.964961 0.419216 0.154867 0.056 Uiso 1 1 calc R U . . .
C66 C 0.9320(2) 0.2801(3) 0.17329(19) 0.0483(7) Uani 1 1 d . . . . .
H66 H 1.011805 0.240262 0.150511 0.058 Uiso 1 1 calc R U . . .
C67 C 0.8419(2) 0.2258(2) 0.20439(17) 0.0407(6) Uani 1 1 d . . . . .
C68 C 0.8681(2) 0.1129(2) 0.20373(18) 0.0452(7) Uani 1 1 d . . . . .
C69 C 0.7749(3) 0.0690(2) 0.2353(2) 0.0510(7) Uani 1 1 d . . . . .
H69 H 0.790099 -0.005041 0.235530 0.061 Uiso 1 1 calc R U . . .
C70 C 0.6572(3) 0.1361(2) 0.26697(19) 0.0487(7) Uani 1 1 d . . . . .
H70 H 0.594929 0.105073 0.287472 0.058 Uiso 1 1 calc R U . . .
C71 C 0.7219(2) 0.2867(2) 0.23928(15) 0.0359(5) Uani 1 1 d . . . . .
C72 C 0.6927(2) 0.4013(2) 0.24334(15) 0.0355(5) Uani 1 1 d . . . . .
C73 C 0.8416(3) 0.6249(2) 0.18550(18) 0.0441(6) Uani 1 1 d . . . . .
C74 C 0.8705(3) 0.6781(3) 0.2323(2) 0.0598(9) Uani 1 1 d . . . . .
H74 H 0.833381 0.676487 0.283288 0.072 Uiso 1 1 calc R U . . .
C75 C 0.9550(4) 0.7341(4) 0.2037(3) 0.0806(13) Uani 1 1 d . . . . .
H75 H 0.976063 0.768169 0.235798 0.097 Uiso 1 1 calc R U . . .
C76 C 1.0072(4) 0.7392(4) 0.1285(3) 0.0861(14) Uani 1 1 d . . . . .
H76 H 1.063586 0.776810 0.109367 0.103 Uiso 1 1 calc R U . . .
C77 C 0.9765(4) 0.6890(4) 0.0812(3) 0.0783(12) Uani 1 1 d . . . . .
H77 H 1.010758 0.694284 0.029849 0.094 Uiso 1 1 calc R U . . .
C78 C 0.8948(3) 0.6305(3) 0.1090(2) 0.0602(8) Uani 1 1 d . . . . .
H78 H 0.875752 0.595256 0.076766 0.072 Uiso 1 1 calc R U . . .
C79 C 0.9948(3) 0.0445(3) 0.1695(3) 0.0676(10) Uani 1 1 d . . . . .
C80 C 1.0318(6) 0.0492(6) 0.0923(4) 0.130(2) Uani 1 1 d . . . . .
H80 H 0.976326 0.093025 0.060916 0.155 Uiso 1 1 calc R U . . .
C81 C 1.1503(8) -0.0105(8) 0.0617(6) 0.197(4) Uani 1 1 d . . . . .
H81 H 1.175929 -0.007136 0.009452 0.236 Uiso 1 1 calc R U . . .
C82 C 1.2311(6) -0.0751(7) 0.1083(8) 0.199(5) Uani 1 1 d . . . . .
H82 H 1.312085 -0.114689 0.087117 0.239 Uiso 1 1 calc R U . . .
C83 C 1.1960(6) -0.0827(7) 0.1835(7) 0.210(4) Uani 1 1 d . . . . .
H83 H 1.251715 -0.126997 0.214650 0.252 Uiso 1 1 calc R U . . .
C84 C 1.0741(5) -0.0227(5) 0.2145(4) 0.128(2) Uani 1 1 d . . . . .
H84 H 1.047375 -0.029233 0.266695 0.153 Uiso 1 1 calc R U . . .
C91 C 0.5913(9) -0.1048(10) 0.0908(6) 0.152(4) Uani 0.7 1 d . . P . .
H91A H 0.658220 -0.102060 0.049009 0.229 Uiso 0.7 1 calc R U P . .
H91B H 0.513945 -0.054016 0.078157 0.229 Uiso 0.7 1 calc R U P . .
H91C H 0.586460 -0.177225 0.101257 0.229 Uiso 0.7 1 calc R U P . .
C92 C 0.6124(8) -0.0785(7) 0.1520(5) 0.113(3) Uani 0.7 1 d D . P . .
H92A H 0.615186 -0.004668 0.141323 0.136 Uiso 0.7 1 calc R U P . .
H92B H 0.693337 -0.126974 0.162225 0.136 Uiso 0.7 1 calc R U P . .
O92 O 0.5183(7) -0.0854(6) 0.2189(4) 0.145(3) Uani 0.7 1 d D . P . .
H92 H 0.515015 -0.044121 0.247883 0.218 Uiso 0.7 1 calc R U P . .


_geom_special_details            ?

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 O23 2.2959(19) . ?
Eu1 O3 2.316(2) . ?
Eu1 O43 2.339(2) . ?
Eu1 O44 2.370(2) . ?
Eu1 O24 2.395(2) . ?
Eu1 O4 2.408(2) . ?
Eu1 N2 2.568(2) . ?
Eu1 N1 2.590(2) . ?
O1 C10 1.356(4) . ?
O1 C2 1.383(4) . ?
O2 C2 1.210(4) . ?
O3 C4 1.256(3) . ?
O4 C11 1.250(4) . ?
C2 C3 1.445(4) . ?
C3 C4 1.413(4) . ?
C3 C11 1.443(4) . ?
C4 C5 1.465(4) . ?
C5 C10 1.382(5) . ?
C5 C6 1.392(5) . ?
C6 C7 1.381(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.386(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.380(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(5) . ?
C9 H9 0.9300 . ?
C11 C12 1.505(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.361(4) . ?
O21 C22 1.394(4) . ?
O22 C22 1.201(4) . ?
O23 C24 1.263(3) . ?
O24 C31 1.249(3) . ?
C22 C23 1.455(4) . ?
C23 C24 1.408(4) . ?
C23 C31 1.441(4) . ?
C24 C25 1.469(4) . ?
C25 C30 1.379(4) . ?
C25 C26 1.391(4) . ?
C26 C27 1.382(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.386(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.367(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.403(4) . ?
C29 H29 0.9300 . ?
C31 C32 1.501(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.364(5) . ?
O41 C42 1.382(5) . ?
O42 C42 1.201(4) . ?
O43 C44 1.271(4) . ?
O44 C51 1.235(4) . ?
C42 C43 1.448(4) . ?
C43 C44 1.422(4) . ?
C43 C51 1.432(5) . ?
C44 C45 1.463(4) . ?
C45 C50 1.389(5) . ?
C45 C46 1.390(5) . ?
C46 C47 1.385(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.374(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.373(7) . ?
C48 H48 0.9300 . ?
C49 C50 1.384(5) . ?
C49 H49 0.9300 . ?
C51 C52 1.499(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N1 C61 1.327(4) . ?
N1 C72 1.367(3) . ?
N2 C70 1.325(4) . ?
N2 C71 1.366(3) . ?
C61 C62 1.397(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.370(4) . ?
C62 H62 0.9300 . ?
C63 C64 1.423(4) . ?
C63 C73 1.491(3) . ?
C64 C72 1.408(3) . ?
C64 C65 1.434(4) . ?
C65 C66 1.338(4) . ?
C65 H65 0.9300 . ?
C66 C67 1.434(4) . ?
C66 H66 0.9300 . ?
C67 C71 1.406(4) . ?
C67 C68 1.415(4) . ?
C68 C69 1.374(4) . ?
C68 C79 1.488(4) . ?
C69 C70 1.397(4) . ?
C69 H69 0.9300 . ?
C70 H70 0.9300 . ?
C71 C72 1.442(4) . ?
C73 C74 1.379(4) . ?
C73 C78 1.389(5) . ?
C74 C75 1.390(5) . ?
C74 H74 0.9300 . ?
C75 C76 1.366(7) . ?
C75 H75 0.9300 . ?
C76 C77 1.369(6) . ?
C76 H76 0.9300 . ?
C77 C78 1.387(5) . ?
C77 H77 0.9300 . ?
C78 H78 0.9300 . ?
C79 C84 1.346(7) . ?
C79 C80 1.372(8) . ?
C80 C81 1.365(9) . ?
C80 H80 0.9300 . ?
C81 C82 1.367(15) . ?
C81 H81 0.9300 . ?
C82 C83 1.335(16) . ?
C82 H82 0.9300 . ?
C83 C84 1.397(8) . ?
C83 H83 0.9300 . ?
C84 H84 0.9300 . ?
C91 C92 1.340(11) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C92 O92 1.450(7) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
O92 H92 0.8200 . ?

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
O23 Eu1 O3 78.96(9) . . ?
O23 Eu1 O43 92.95(10) . . ?
O3 Eu1 O43 140.75(8) . . ?
O23 Eu1 O44 76.87(8) . . ?
O3 Eu1 O44 72.10(8) . . ?
O43 Eu1 O44 68.67(8) . . ?
O23 Eu1 O24 68.74(7) . . ?
O3 Eu1 O24 127.63(8) . . ?
O43 Eu1 O24 82.44(8) . . ?
O44 Eu1 O24 133.42(7) . . ?
O23 Eu1 O4 103.72(9) . . ?
O3 Eu1 O4 68.25(7) . . ?
O43 Eu1 O4 149.80(7) . . ?
O44 Eu1 O4 139.29(7) . . ?
O24 Eu1 O4 80.49(7) . . ?
O23 Eu1 N2 148.26(7) . . ?
O3 Eu1 N2 77.37(8) . . ?
O43 Eu1 N2 92.14(8) . . ?
O44 Eu1 N2 75.93(7) . . ?
O24 Eu1 N2 143.00(6) . . ?
O4 Eu1 N2 86.76(7) . . ?
O23 Eu1 N1 147.01(8) . . ?
O3 Eu1 N1 131.51(8) . . ?
O43 Eu1 N1 71.02(7) . . ?
O44 Eu1 N1 120.17(8) . . ?
O24 Eu1 N1 80.41(7) . . ?
O4 Eu1 N1 81.66(7) . . ?
N2 Eu1 N1 63.37(7) . . ?
C10 O1 C2 122.3(3) . . ?
C4 O3 Eu1 134.33(19) . . ?
C11 O4 Eu1 138.34(18) . . ?
O2 C2 O1 114.1(3) . . ?
O2 C2 C3 127.6(3) . . ?
O1 C2 C3 118.3(3) . . ?
C4 C3 C11 119.4(3) . . ?
C4 C3 C2 120.0(3) . . ?
C11 C3 C2 120.5(3) . . ?
O3 C4 C3 124.5(3) . . ?
O3 C4 C5 117.2(3) . . ?
C3 C4 C5 118.3(3) . . ?
C10 C5 C6 119.8(3) . . ?
C10 C5 C4 118.6(3) . . ?
C6 C5 C4 121.5(3) . . ?
C7 C6 C5 120.2(4) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 119.1(4) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C9 C8 C7 121.6(4) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 118.7(4) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
O1 C10 C5 122.1(3) . . ?
O1 C10 C9 117.2(3) . . ?
C5 C10 C9 120.6(4) . . ?
O4 C11 C3 122.5(3) . . ?
O4 C11 C12 116.2(3) . . ?
C3 C11 C12 121.3(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 122.0(2) . . ?
C24 O23 Eu1 141.75(18) . . ?
C31 O24 Eu1 141.15(17) . . ?
O22 C22 O21 114.1(3) . . ?
O22 C22 C23 127.5(3) . . ?
O21 C22 C23 118.4(3) . . ?
C24 C23 C31 120.3(2) . . ?
C24 C23 C22 119.9(2) . . ?
C31 C23 C22 119.7(3) . . ?
O23 C24 C23 125.5(2) . . ?
O23 C24 C25 116.1(3) . . ?
C23 C24 C25 118.4(2) . . ?
C30 C25 C26 119.5(3) . . ?
C30 C25 C24 119.1(3) . . ?
C26 C25 C24 121.4(3) . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 119.8(3) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C29 C28 C27 120.8(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 119.3(3) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
O21 C30 C25 122.1(3) . . ?
O21 C30 C29 117.5(3) . . ?
C25 C30 C29 120.4(3) . . ?
O24 C31 C23 122.1(3) . . ?
O24 C31 C32 115.9(3) . . ?
C23 C31 C32 122.0(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.4(3) . . ?
C44 O43 Eu1 137.3(2) . . ?
C51 O44 Eu1 137.7(2) . . ?
O42 C42 O41 114.5(3) . . ?
O42 C42 C43 127.4(4) . . ?
O41 C42 C43 118.1(3) . . ?
C44 C43 C51 120.2(3) . . ?
C44 C43 C42 119.8(3) . . ?
C51 C43 C42 119.7(3) . . ?
O43 C44 C43 124.9(3) . . ?
O43 C44 C45 117.3(3) . . ?
C43 C44 C45 117.8(3) . . ?
C50 C45 C46 118.7(3) . . ?
C50 C45 C44 118.6(3) . . ?
C46 C45 C44 122.6(3) . . ?
C47 C46 C45 120.7(4) . . ?
C47 C46 H46 119.6 . . ?
C45 C46 H46 119.6 . . ?
C48 C47 C46 119.5(4) . . ?
C48 C47 H47 120.3 . . ?
C46 C47 H47 120.3 . . ?
C49 C48 C47 120.8(4) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C48 C49 C50 119.8(4) . . ?
C48 C49 H49 120.1 . . ?
C50 C49 H49 120.1 . . ?
O41 C50 C49 117.6(4) . . ?
O41 C50 C45 121.9(3) . . ?
C49 C50 C45 120.5(4) . . ?
O44 C51 C43 121.8(3) . . ?
O44 C51 C52 115.9(3) . . ?
C43 C51 C52 122.3(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 N1 C72 117.3(2) . . ?
C61 N1 Eu1 122.11(17) . . ?
C72 N1 Eu1 119.76(16) . . ?
C70 N2 C71 118.1(2) . . ?
C70 N2 Eu1 121.25(17) . . ?
C71 N2 Eu1 120.40(17) . . ?
N1 C61 C62 123.7(3) . . ?
N1 C61 H61 118.1 . . ?
C62 C61 H61 118.1 . . ?
C63 C62 C61 120.1(3) . . ?
C63 C62 H62 119.9 . . ?
C61 C62 H62 119.9 . . ?
C62 C63 C64 117.8(2) . . ?
C62 C63 C73 120.2(3) . . ?
C64 C63 C73 121.9(3) . . ?
C72 C64 C63 118.3(2) . . ?
C72 C64 C65 118.3(2) . . ?
C63 C64 C65 123.4(2) . . ?
C66 C65 C64 121.7(2) . . ?
C66 C65 H65 119.2 . . ?
C64 C65 H65 119.2 . . ?
C65 C66 C67 121.7(3) . . ?
C65 C66 H66 119.2 . . ?
C67 C66 H66 119.2 . . ?
C71 C67 C68 117.9(2) . . ?
C71 C67 C66 118.6(2) . . ?
C68 C67 C66 123.4(3) . . ?
C69 C68 C67 118.7(3) . . ?
C69 C68 C79 121.4(3) . . ?
C67 C68 C79 119.9(3) . . ?
C68 C69 C70 119.6(3) . . ?
C68 C69 H69 120.2 . . ?
C70 C69 H69 120.2 . . ?
N2 C70 C69 123.2(3) . . ?
N2 C70 H70 118.4 . . ?
C69 C70 H70 118.4 . . ?
N2 C71 C67 122.4(2) . . ?
N2 C71 C72 118.0(2) . . ?
C67 C71 C72 119.6(2) . . ?
N1 C72 C64 122.7(2) . . ?
N1 C72 C71 117.2(2) . . ?
C64 C72 C71 120.1(2) . . ?
C74 C73 C78 119.4(3) . . ?
C74 C73 C63 119.6(3) . . ?
C78 C73 C63 120.9(3) . . ?
C73 C74 C75 120.3(4) . . ?
C73 C74 H74 119.9 . . ?
C75 C74 H74 119.9 . . ?
C76 C75 C74 120.0(4) . . ?
C76 C75 H75 120.0 . . ?
C74 C75 H75 120.0 . . ?
C75 C76 C77 120.1(3) . . ?
C75 C76 H76 120.0 . . ?
C77 C76 H76 120.0 . . ?
C76 C77 C78 120.8(4) . . ?
C76 C77 H77 119.6 . . ?
C78 C77 H77 119.6 . . ?
C77 C78 C73 119.4(4) . . ?
C77 C78 H78 120.3 . . ?
C73 C78 H78 120.3 . . ?
C84 C79 C80 119.6(5) . . ?
C84 C79 C68 119.8(4) . . ?
C80 C79 C68 120.6(5) . . ?
C81 C80 C79 119.9(8) . . ?
C81 C80 H80 120.1 . . ?
C79 C80 H80 120.1 . . ?
C80 C81 C82 119.7(9) . . ?
C80 C81 H81 120.1 . . ?
C82 C81 H81 120.1 . . ?
C83 C82 C81 121.3(6) . . ?
C83 C82 H82 119.3 . . ?
C81 C82 H82 119.3 . . ?
C82 C83 C84 118.7(9) . . ?
C82 C83 H83 120.7 . . ?
C84 C83 H83 120.7 . . ?
C79 C84 C83 120.7(8) . . ?
C79 C84 H84 119.7 . . ?
C83 C84 H84 119.7 . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C91 C92 O92 113.2(8) . . ?
C91 C92 H92A 108.9 . . ?
O92 C92 H92A 108.9 . . ?
C91 C92 H92B 108.9 . . ?
O92 C92 H92B 108.9 . . ?
H92A C92 H92B 107.8 . . ?
C92 O92 H92 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 177.8(3) . . . . ?
C10 O1 C2 C3 -1.1(5) . . . . ?
O2 C2 C3 C4 178.3(3) . . . . ?
O1 C2 C3 C4 -3.0(4) . . . . ?
O2 C2 C3 C11 -2.8(5) . . . . ?
O1 C2 C3 C11 175.9(3) . . . . ?
Eu1 O3 C4 C3 -42.9(4) . . . . ?
Eu1 O3 C4 C5 137.4(2) . . . . ?
C11 C3 C4 O3 5.0(4) . . . . ?
C2 C3 C4 O3 -176.0(3) . . . . ?
C11 C3 C4 C5 -175.2(2) . . . . ?
C2 C3 C4 C5 3.7(4) . . . . ?
O3 C4 C5 C10 179.2(3) . . . . ?
C3 C4 C5 C10 -0.6(4) . . . . ?
O3 C4 C5 C6 -3.9(4) . . . . ?
C3 C4 C5 C6 176.3(3) . . . . ?
C10 C5 C6 C7 1.0(5) . . . . ?
C4 C5 C6 C7 -175.9(3) . . . . ?
C5 C6 C7 C8 0.1(6) . . . . ?
C6 C7 C8 C9 -1.3(7) . . . . ?
C7 C8 C9 C10 1.4(7) . . . . ?
C2 O1 C10 C5 4.5(5) . . . . ?
C2 O1 C10 C9 -175.2(3) . . . . ?
C6 C5 C10 O1 179.5(3) . . . . ?
C4 C5 C10 O1 -3.6(5) . . . . ?
C6 C5 C10 C9 -0.8(5) . . . . ?
C4 C5 C10 C9 176.1(3) . . . . ?
C8 C9 C10 O1 179.3(4) . . . . ?
C8 C9 C10 C5 -0.3(6) . . . . ?
Eu1 O4 C11 C3 -0.1(4) . . . . ?
Eu1 O4 C11 C12 -179.1(2) . . . . ?
C4 C3 C11 O4 14.5(4) . . . . ?
C2 C3 C11 O4 -164.5(3) . . . . ?
C4 C3 C11 C12 -166.6(3) . . . . ?
C2 C3 C11 C12 14.5(4) . . . . ?
C30 O21 C22 O22 176.5(3) . . . . ?
C30 O21 C22 C23 -3.2(5) . . . . ?
O22 C22 C23 C24 -177.0(4) . . . . ?
O21 C22 C23 C24 2.7(5) . . . . ?
O22 C22 C23 C31 1.7(6) . . . . ?
O21 C22 C23 C31 -178.6(3) . . . . ?
Eu1 O23 C24 C23 5.6(6) . . . . ?
Eu1 O23 C24 C25 -174.9(3) . . . . ?
C31 C23 C24 O23 0.3(5) . . . . ?
C22 C23 C24 O23 179.0(3) . . . . ?
C31 C23 C24 C25 -179.2(3) . . . . ?
C22 C23 C24 C25 -0.5(5) . . . . ?
O23 C24 C25 C30 179.2(3) . . . . ?
C23 C24 C25 C30 -1.2(5) . . . . ?
O23 C24 C25 C26 -1.1(5) . . . . ?
C23 C24 C25 C26 178.5(3) . . . . ?
C30 C25 C26 C27 -0.1(5) . . . . ?
C24 C25 C26 C27 -179.8(3) . . . . ?
C25 C26 C27 C28 -0.2(5) . . . . ?
C26 C27 C28 C29 -0.4(6) . . . . ?
C27 C28 C29 C30 1.4(5) . . . . ?
C22 O21 C30 C25 1.5(5) . . . . ?
C22 O21 C30 C29 -178.5(3) . . . . ?
C26 C25 C30 O21 -178.9(3) . . . . ?
C24 C25 C30 O21 0.8(5) . . . . ?
C26 C25 C30 C29 1.1(5) . . . . ?
C24 C25 C30 C29 -179.2(3) . . . . ?
C28 C29 C30 O21 178.3(3) . . . . ?
C28 C29 C30 C25 -1.8(5) . . . . ?
Eu1 O24 C31 C23 8.8(5) . . . . ?
Eu1 O24 C31 C32 -171.2(3) . . . . ?
C24 C23 C31 O24 -6.4(5) . . . . ?
C22 C23 C31 O24 174.8(3) . . . . ?
C24 C23 C31 C32 173.5(3) . . . . ?
C22 C23 C31 C32 -5.2(5) . . . . ?
C50 O41 C42 O42 178.9(3) . . . . ?
C50 O41 C42 C43 -0.6(5) . . . . ?
O42 C42 C43 C44 -169.1(4) . . . . ?
O41 C42 C43 C44 10.4(5) . . . . ?
O42 C42 C43 C51 16.6(6) . . . . ?
O41 C42 C43 C51 -163.9(3) . . . . ?
Eu1 O43 C44 C43 -4.9(5) . . . . ?
Eu1 O43 C44 C45 177.8(2) . . . . ?
C51 C43 C44 O43 -16.6(5) . . . . ?
C42 C43 C44 O43 169.1(3) . . . . ?
C51 C43 C44 C45 160.7(3) . . . . ?
C42 C43 C44 C45 -13.6(4) . . . . ?
O43 C44 C45 C50 -175.1(3) . . . . ?
C43 C44 C45 C50 7.4(4) . . . . ?
O43 C44 C45 C46 8.2(5) . . . . ?
C43 C44 C45 C46 -169.3(3) . . . . ?
C50 C45 C46 C47 -0.3(5) . . . . ?
C44 C45 C46 C47 176.5(3) . . . . ?
C45 C46 C47 C48 1.1(6) . . . . ?
C46 C47 C48 C49 -0.6(6) . . . . ?
C47 C48 C49 C50 -0.7(6) . . . . ?
C42 O41 C50 C49 174.3(3) . . . . ?
C42 O41 C50 C45 -5.7(5) . . . . ?
C48 C49 C50 O41 -178.5(4) . . . . ?
C48 C49 C50 C45 1.5(6) . . . . ?
C46 C45 C50 O41 179.0(3) . . . . ?
C44 C45 C50 O41 2.1(5) . . . . ?
C46 C45 C50 C49 -1.0(5) . . . . ?
C44 C45 C50 C49 -177.9(3) . . . . ?
Eu1 O44 C51 C43 29.4(5) . . . . ?
Eu1 O44 C51 C52 -153.8(3) . . . . ?
C44 C43 C51 O44 5.4(5) . . . . ?
C42 C43 C51 O44 179.7(3) . . . . ?
C44 C43 C51 C52 -171.2(4) . . . . ?
C42 C43 C51 C52 3.1(5) . . . . ?
C72 N1 C61 C62 -0.4(5) . . . . ?
Eu1 N1 C61 C62 -170.1(2) . . . . ?
N1 C61 C62 C63 0.8(5) . . . . ?
C61 C62 C63 C64 -1.0(5) . . . . ?
C61 C62 C63 C73 -179.6(3) . . . . ?
C62 C63 C64 C72 0.9(4) . . . . ?
C73 C63 C64 C72 179.5(3) . . . . ?
C62 C63 C64 C65 -177.8(3) . . . . ?
C73 C63 C64 C65 0.8(5) . . . . ?
C72 C64 C65 C66 -0.1(5) . . . . ?
C63 C64 C65 C66 178.6(3) . . . . ?
C64 C65 C66 C67 0.8(5) . . . . ?
C65 C66 C67 C71 -0.5(5) . . . . ?
C65 C66 C67 C68 -178.8(3) . . . . ?
C71 C67 C68 C69 1.6(5) . . . . ?
C66 C67 C68 C69 179.8(3) . . . . ?
C71 C67 C68 C79 -178.2(3) . . . . ?
C66 C67 C68 C79 0.0(5) . . . . ?
C67 C68 C69 C70 0.1(5) . . . . ?
C79 C68 C69 C70 179.9(4) . . . . ?
C71 N2 C70 C69 -0.2(5) . . . . ?
Eu1 N2 C70 C69 174.3(3) . . . . ?
C68 C69 C70 N2 -0.8(5) . . . . ?
C70 N2 C71 C67 2.1(4) . . . . ?
Eu1 N2 C71 C67 -172.5(2) . . . . ?
C70 N2 C71 C72 -178.7(3) . . . . ?
Eu1 N2 C71 C72 6.8(3) . . . . ?
C68 C67 C71 N2 -2.8(4) . . . . ?
C66 C67 C71 N2 178.9(3) . . . . ?
C68 C67 C71 C72 178.0(3) . . . . ?
C66 C67 C71 C72 -0.3(4) . . . . ?
C61 N1 C72 C64 0.3(4) . . . . ?
Eu1 N1 C72 C64 170.2(2) . . . . ?
C61 N1 C72 C71 179.4(3) . . . . ?
Eu1 N1 C72 C71 -10.7(3) . . . . ?
C63 C64 C72 N1 -0.5(4) . . . . ?
C65 C64 C72 N1 178.2(3) . . . . ?
C63 C64 C72 C71 -179.6(3) . . . . ?
C65 C64 C72 C71 -0.8(4) . . . . ?
N2 C71 C72 N1 2.6(4) . . . . ?
C67 C71 C72 N1 -178.1(2) . . . . ?
N2 C71 C72 C64 -178.3(2) . . . . ?
C67 C71 C72 C64 1.0(4) . . . . ?
C62 C63 C73 C74 55.5(4) . . . . ?
C64 C63 C73 C74 -123.0(3) . . . . ?
C62 C63 C73 C78 -122.7(4) . . . . ?
C64 C63 C73 C78 58.7(4) . . . . ?
C78 C73 C74 C75 -1.9(5) . . . . ?
C63 C73 C74 C75 179.8(3) . . . . ?
C73 C74 C75 C76 1.8(6) . . . . ?
C74 C75 C76 C77 -0.1(7) . . . . ?
C75 C76 C77 C78 -1.5(7) . . . . ?
C76 C77 C78 C73 1.4(6) . . . . ?
C74 C73 C78 C77 0.3(5) . . . . ?
C63 C73 C78 C77 178.5(3) . . . . ?
C69 C68 C79 C84 -75.8(5) . . . . ?
C67 C68 C79 C84 104.0(5) . . . . ?
C69 C68 C79 C80 104.3(5) . . . . ?
C67 C68 C79 C80 -75.9(5) . . . . ?
C84 C79 C80 C81 -2.8(9) . . . . ?
C68 C79 C80 C81 177.1(6) . . . . ?
C79 C80 C81 C82 0.4(12) . . . . ?
C80 C81 C82 C83 1.0(15) . . . . ?
C81 C82 C83 C84 -0.1(15) . . . . ?
C80 C79 C84 C83 3.8(9) . . . . ?
C68 C79 C84 C83 -176.1(6) . . . . ?
C82 C83 C84 C79 -2.4(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C61 H61 O24 0.93 2.49 3.159(3) 129.2 . yes
C70 H70 O3 0.93 2.47 3.060(4) 121.9 . yes
C61 H61 O24 0.93 2.49 3.159(3) 129.2 . yes
C70 H70 O3 0.93 2.47 3.060(4) 121.9 . yes

_refine_diff_density_max         1.496
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.074

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_Dy-phen
_database_code_depnum_ccdc_archive 'CCDC 2013255'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  DyCum3Fen
# Clave IF-UAP:  DyCum3Fen
# Solicitud: 102
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM)
# Clave datos : ... \BUAP\Sylvain\DyCum3Fen\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_audit_creation_date             2018-04-27

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H29 Dy N2 O12, 0.50(H2 O)'
_chemical_formula_sum            'C45 H30 Dy N2 O12.50'
_chemical_formula_weight         961.21
_chemical_absolute_configuration .
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.3302 2.9404 '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       ?

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

_cell_length_a                   11.0739(7)
_cell_length_b                   13.0473(8)
_cell_length_c                   14.2413(8)
_cell_angle_alpha                104.471(4)
_cell_angle_beta                 92.631(5)
_cell_angle_gamma                98.450(5)
_cell_volume                     1963.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    22980
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      25.71

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 3 -2 0.0480
3 1 1 0.0600
-1 -2 7 0.0850
-2 -1 2 0.0730
-7 -3 -1 0.0680
-1 1 -6 0.0600
-3 5 -2 0.0480
3 -5 2 0.0420

_exptl_absorpt_coefficient_mu    1.065
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3626
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA (Stoe & Cie, 2015)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1378 frames, 45 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            67227
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.177
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10444
_reflns_number_gt                7315
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA (Stoe & Cie, 2015)'
_computing_cell_refinement       X-AREA
_computing_data_reduction        X-AREA
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'
_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)+(0.0344P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         10444
_refine_ls_number_parameters     559
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_restrained_S_all      0.875
_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 0.28845(2) 0.25263(2) 0.78553(2) 0.04710(6) Uani 1 1 d . . . . .
O1 O 0.0968(4) 0.6532(3) 0.7890(3) 0.1032(11) Uani 1 1 d . . . . .
O2 O -0.0164(5) 0.5869(4) 0.8891(3) 0.1468(19) Uani 1 1 d . . . . .
O3 O 0.2493(2) 0.38012(19) 0.70534(15) 0.0542(6) Uani 1 1 d . . . . .
O4 O 0.0907(2) 0.2904(2) 0.80739(18) 0.0646(6) Uani 1 1 d . . . . .
C2 C 0.0547(5) 0.5687(5) 0.8281(3) 0.0964(17) Uani 1 1 d . . . . .
C3 C 0.0983(4) 0.4669(3) 0.7925(3) 0.0668(11) Uani 1 1 d . . . . .
C4 C 0.1961(3) 0.4615(3) 0.7324(2) 0.0565(9) Uani 1 1 d . . . . .
C5 C 0.2381(4) 0.5556(3) 0.6964(3) 0.0643(10) Uani 1 1 d . . . . .
C6 C 0.3308(4) 0.5577(4) 0.6358(3) 0.0823(12) Uani 1 1 d . . . . .
H6A H 0.368462 0.497586 0.616051 0.099 Uiso 1 1 calc R U . . .
C7 C 0.3690(6) 0.6477(5) 0.6037(4) 0.1081(18) Uani 1 1 d . . . . .
H7A H 0.432488 0.648479 0.563191 0.130 Uiso 1 1 calc R U . . .
C8 C 0.3124(7) 0.7361(5) 0.6320(5) 0.121(2) Uani 1 1 d . . . . .
H8A H 0.337013 0.795978 0.609064 0.145 Uiso 1 1 calc R U . . .
C9 C 0.2213(6) 0.7379(4) 0.6927(4) 0.1085(19) Uani 1 1 d . . . . .
H9A H 0.184307 0.798456 0.712022 0.130 Uiso 1 1 calc R U . . .
C10 C 0.1844(5) 0.6469(4) 0.7253(3) 0.0818(13) Uani 1 1 d . . . . .
C11 C 0.0426(4) 0.3727(4) 0.8202(3) 0.0727(12) Uani 1 1 d . . . . .
C12 C -0.0780(5) 0.3662(6) 0.8626(4) 0.138(3) Uani 1 1 d . . . . .
H12A H -0.116150 0.292484 0.849149 0.207 Uiso 1 1 calc DR U . . .
H12B H -0.129824 0.405374 0.834164 0.207 Uiso 1 1 calc R U . . .
H12C H -0.065798 0.396615 0.931692 0.207 Uiso 1 1 calc R U . . .
O21 O 0.1309(3) -0.1406(2) 0.44347(18) 0.0724(7) Uani 1 1 d . . . . .
O22 O 0.2971(3) -0.0712(3) 0.3924(2) 0.1032(11) Uani 1 1 d . . . . .
O23 O 0.1668(2) 0.09461(18) 0.69883(16) 0.0582(6) Uani 1 1 d . . . . .
O24 O 0.3575(2) 0.19206(19) 0.63313(16) 0.0602(6) Uani 1 1 d . . . . .
C22 C 0.2316(4) -0.0597(3) 0.4579(3) 0.0681(10) Uani 1 1 d . . . . .
C23 C 0.2455(3) 0.0255(3) 0.5462(2) 0.0523(8) Uani 1 1 d . . . . .
C24 C 0.1612(3) 0.0246(2) 0.6185(2) 0.0483(7) Uani 1 1 d . . . . .
C25 C 0.0574(3) -0.0644(3) 0.5974(2) 0.0516(8) Uani 1 1 d . . . . .
C26 C -0.0311(4) -0.0718(3) 0.6624(3) 0.0628(9) Uani 1 1 d . . . . .
H26A H -0.024999 -0.020159 0.721484 0.075 Uiso 1 1 calc DR U . . .
C27 C -0.1281(4) -0.1557(3) 0.6393(3) 0.0804(12) Uani 1 1 d . . . . .
H27A H -0.187488 -0.160711 0.682718 0.097 Uiso 1 1 calc R U . . .
C28 C -0.1368(4) -0.2329(3) 0.5508(3) 0.0827(13) Uani 1 1 d . . . . .
H28A H -0.202502 -0.289236 0.535440 0.099 Uiso 1 1 calc R U . . .
C29 C -0.0500(4) -0.2271(3) 0.4860(3) 0.0737(11) Uani 1 1 d . . . . .
H29A H -0.056011 -0.278832 0.426998 0.088 Uiso 1 1 calc R U . . .
C30 C 0.0469(3) -0.1424(3) 0.5104(3) 0.0572(9) Uani 1 1 d . . . . .
C31 C 0.3422(3) 0.1159(3) 0.5595(2) 0.0565(8) Uani 1 1 d . . . . .
C32 C 0.4298(4) 0.1276(4) 0.4827(3) 0.0838(13) Uani 1 1 d . . . . .
H32A H 0.492831 0.188466 0.508777 0.126 Uiso 1 1 calc R U . . .
H32B H 0.385817 0.137709 0.426956 0.126 Uiso 1 1 calc R U . . .
H32C H 0.466312 0.063964 0.463824 0.126 Uiso 1 1 calc R U . . .
O41 O 0.6436(3) 0.6439(2) 0.8149(2) 0.0767(8) Uani 1 1 d . . . . .
O42 O 0.5181(3) 0.7119(2) 0.9171(2) 0.0880(9) Uani 1 1 d . . . . .
O43 O 0.4859(2) 0.33539(17) 0.79202(17) 0.0550(6) Uani 1 1 d . . . . .
O44 O 0.3252(2) 0.41070(18) 0.91153(15) 0.0523(5) Uani 1 1 d . . . . .
C42 C 0.5438(4) 0.6295(3) 0.8685(3) 0.0649(10) Uani 1 1 d . . . . .
C43 C 0.4850(3) 0.5207(3) 0.8624(2) 0.0505(8) Uani 1 1 d . . . . .
C44 C 0.5296(3) 0.4325(3) 0.8014(2) 0.0492(7) Uani 1 1 d . . . . .
C45 C 0.6335(3) 0.4547(3) 0.7458(3) 0.0566(8) Uani 1 1 d . . . . .
C46 C 0.6813(4) 0.3733(3) 0.6822(3) 0.0705(10) Uani 1 1 d . . . . .
H46A H 0.646648 0.302037 0.674828 0.085 Uiso 1 1 calc R U . . .
C47 C 0.7783(4) 0.3968(4) 0.6306(3) 0.0868(13) Uani 1 1 d . . . . .
H47A H 0.808990 0.342104 0.588169 0.104 Uiso 1 1 calc R U . . .
C48 C 0.8304(5) 0.5033(5) 0.6423(4) 0.0950(15) Uani 1 1 d . . . . .
H48A H 0.896931 0.519583 0.608064 0.114 Uiso 1 1 calc R U . . .
C49 C 0.7850(4) 0.5848(4) 0.7037(4) 0.0861(13) Uani 1 1 d . . . . .
H49A H 0.819944 0.655902 0.710814 0.103 Uiso 1 1 calc R U . . .
C50 C 0.6867(4) 0.5598(3) 0.7550(3) 0.0662(10) Uani 1 1 d . . . . .
C51 C 0.3837(3) 0.5028(3) 0.9192(2) 0.0507(8) Uani 1 1 d . . . . .
C52 C 0.3400(4) 0.5929(3) 0.9908(3) 0.0645(10) Uani 1 1 d . . . . .
H52A H 0.279952 0.563610 1.027705 0.097 Uiso 1 1 calc R U . . .
H52B H 0.304054 0.636905 0.956249 0.097 Uiso 1 1 calc R U . . .
H52C H 0.408160 0.635482 1.034091 0.097 Uiso 1 1 calc R U . . .
N61 N 0.4082(3) 0.1134(2) 0.82048(19) 0.0539(7) Uani 1 1 d . . . . .
C62 C 0.5030(4) 0.0842(3) 0.7736(3) 0.0629(9) Uani 1 1 d . . . . .
H62A H 0.538339 0.126364 0.735056 0.076 Uiso 1 1 calc R U . . .
C63 C 0.5530(4) -0.0069(3) 0.7790(3) 0.0705(11) Uani 1 1 d . . . . .
H63A H 0.621077 -0.023297 0.746001 0.085 Uiso 1 1 calc R U . . .
C64 C 0.5010(4) -0.0708(3) 0.8328(3) 0.0711(11) Uani 1 1 d . . . . .
H64A H 0.531648 -0.132806 0.835208 0.085 Uiso 1 1 calc R U . . .
C65 C 0.4007(4) -0.0433(3) 0.8850(3) 0.0606(9) Uani 1 1 d . . . . .
C66 C 0.3435(4) -0.1040(3) 0.9459(3) 0.0741(11) Uani 1 1 d . . . . .
H66A H 0.367949 -0.168626 0.947943 0.089 Uiso 1 1 calc R U . . .
C67 C 0.2548(4) -0.0691(3) 1.0003(3) 0.0740(11) Uani 1 1 d . . . . .
H67A H 0.218912 -0.110390 1.039377 0.089 Uiso 1 1 calc R U . . .
C68 C 0.2137(4) 0.0301(3) 1.0000(2) 0.0591(9) Uani 1 1 d . . . . .
C69 C 0.1294(4) 0.0743(3) 1.0616(3) 0.0685(11) Uani 1 1 d . . . . .
H69A H 0.094347 0.037766 1.104582 0.082 Uiso 1 1 calc R U . . .
C70 C 0.0988(4) 0.1707(3) 1.0588(3) 0.0691(11) Uani 1 1 d . . . . .
H70A H 0.044921 0.201877 1.100897 0.083 Uiso 1 1 calc R U . . .
C71 C 0.1500(3) 0.2220(3) 0.9912(2) 0.0600(9) Uani 1 1 d . . . . .
H71A H 0.127845 0.287425 0.989049 0.072 Uiso 1 1 calc R U . . .
N72 N 0.2283(3) 0.1824(2) 0.93006(19) 0.0526(7) Uani 1 1 d . . . . .
C73 C 0.2636(3) 0.0894(3) 0.9364(2) 0.0518(8) Uani 1 1 d . . . . .
C74 C 0.3597(3) 0.0518(3) 0.8782(2) 0.0519(8) Uani 1 1 d . . . . .
O81 O -0.1301(10) 0.1300(8) 0.8014(6) 0.149(3) Uani 0.5 1 d D . P . .
H81A H -0.064(7) 0.1483(19) 0.773(8) 0.179 Uiso 0.5 1 d D U P . .
H81B H -0.164(3) 0.072(4) 0.758(6) 0.179 Uiso 0.5 1 d D U P . .


_geom_special_details            ?

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 O43 2.279(2) . ?
Dy1 O23 2.313(2) . ?
Dy1 O3 2.318(2) . ?
Dy1 O24 2.322(2) . ?
Dy1 O4 2.333(3) . ?
Dy1 O44 2.340(2) . ?
Dy1 N61 2.531(3) . ?
Dy1 N72 2.532(3) . ?
O1 C10 1.356(6) . ?
O1 C2 1.385(6) . ?
O2 C2 1.202(5) . ?
O3 C4 1.274(4) . ?
O4 C11 1.244(5) . ?
C2 C3 1.459(6) . ?
C3 C4 1.410(5) . ?
C3 C11 1.445(6) . ?
C4 C5 1.468(5) . ?
C5 C6 1.373(6) . ?
C5 C10 1.389(6) . ?
C6 C7 1.381(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.374(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.357(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.394(7) . ?
C9 H9A 0.9300 . ?
C11 C12 1.491(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.364(4) . ?
O21 C22 1.386(5) . ?
O22 C22 1.202(4) . ?
O23 C24 1.266(4) . ?
O24 C31 1.237(4) . ?
C22 C23 1.440(5) . ?
C23 C24 1.423(4) . ?
C23 C31 1.439(5) . ?
C24 C25 1.470(5) . ?
C25 C30 1.381(5) . ?
C25 C26 1.388(5) . ?
C26 C27 1.379(5) . ?
C26 H26A 0.9300 . ?
C27 C28 1.392(6) . ?
C27 H27A 0.9300 . ?
C28 C29 1.369(6) . ?
C28 H28A 0.9300 . ?
C29 C30 1.385(5) . ?
C29 H29A 0.9300 . ?
C31 C32 1.515(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.372(5) . ?
O41 C42 1.389(5) . ?
O42 C42 1.204(4) . ?
O43 C44 1.259(4) . ?
O44 C51 1.254(4) . ?
C42 C43 1.452(5) . ?
C43 C44 1.425(5) . ?
C43 C51 1.439(5) . ?
C44 C45 1.461(5) . ?
C45 C50 1.383(5) . ?
C45 C46 1.399(5) . ?
C46 C47 1.370(5) . ?
C46 H46A 0.9300 . ?
C47 C48 1.390(7) . ?
C47 H47A 0.9300 . ?
C48 C49 1.371(7) . ?
C48 H48A 0.9300 . ?
C49 C50 1.382(6) . ?
C49 H49A 0.9300 . ?
C51 C52 1.506(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N61 C62 1.322(4) . ?
N61 C74 1.361(4) . ?
C62 C63 1.400(5) . ?
C62 H62A 0.9300 . ?
C63 C64 1.354(5) . ?
C63 H63A 0.9300 . ?
C64 C65 1.405(5) . ?
C64 H64A 0.9300 . ?
C65 C74 1.407(5) . ?
C65 C66 1.423(5) . ?
C66 C67 1.341(6) . ?
C66 H66A 0.9300 . ?
C67 C68 1.434(5) . ?
C67 H67A 0.9300 . ?
C68 C69 1.398(5) . ?
C68 C73 1.413(4) . ?
C69 C70 1.359(5) . ?
C69 H69A 0.9300 . ?
C70 C71 1.399(5) . ?
C70 H70A 0.9300 . ?
C71 N72 1.324(4) . ?
C71 H71A 0.9300 . ?
N72 C73 1.351(4) . ?
C73 C74 1.446(5) . ?
O81 H81A 0.88(2) . ?
O81 H81B 0.87(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O43 Dy1 O23 137.73(8) . . ?
O43 Dy1 O3 82.79(8) . . ?
O23 Dy1 O3 105.22(8) . . ?
O43 Dy1 O24 72.76(8) . . ?
O23 Dy1 O24 69.27(8) . . ?
O3 Dy1 O24 76.36(8) . . ?
O43 Dy1 O4 141.43(9) . . ?
O23 Dy1 O4 77.24(9) . . ?
O3 Dy1 O4 69.61(9) . . ?
O24 Dy1 O4 122.99(9) . . ?
O43 Dy1 O44 69.80(8) . . ?
O23 Dy1 O44 152.24(8) . . ?
O3 Dy1 O44 77.90(8) . . ?
O24 Dy1 O44 136.59(8) . . ?
O4 Dy1 O44 78.24(9) . . ?
O43 Dy1 N61 77.90(9) . . ?
O23 Dy1 N61 78.29(9) . . ?
O3 Dy1 N61 153.49(8) . . ?
O24 Dy1 N61 80.65(9) . . ?
O4 Dy1 N61 135.56(9) . . ?
O44 Dy1 N61 111.48(8) . . ?
O43 Dy1 N72 116.71(9) . . ?
O23 Dy1 N72 82.84(8) . . ?
O3 Dy1 N72 141.50(8) . . ?
O24 Dy1 N72 139.28(9) . . ?
O4 Dy1 N72 75.94(9) . . ?
O44 Dy1 N72 78.75(8) . . ?
N61 Dy1 N72 64.63(9) . . ?
C10 O1 C2 122.1(4) . . ?
C4 O3 Dy1 130.4(2) . . ?
C11 O4 Dy1 135.1(3) . . ?
O2 C2 O1 115.7(5) . . ?
O2 C2 C3 125.8(5) . . ?
O1 C2 C3 118.5(4) . . ?
C4 C3 C11 120.3(4) . . ?
C4 C3 C2 119.7(4) . . ?
C11 C3 C2 120.0(4) . . ?
O3 C4 C3 124.8(3) . . ?
O3 C4 C5 117.4(3) . . ?
C3 C4 C5 117.7(4) . . ?
C6 C5 C10 118.2(4) . . ?
C6 C5 C4 122.3(4) . . ?
C10 C5 C4 119.5(4) . . ?
C5 C6 C7 121.0(5) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C6 119.5(6) . . ?
C8 C7 H7A 120.3 . . ?
C6 C7 H7A 120.3 . . ?
C9 C8 C7 121.5(5) . . ?
C9 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C8 C9 C10 118.5(5) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
O1 C10 C5 121.7(4) . . ?
O1 C10 C9 116.9(5) . . ?
C5 C10 C9 121.3(5) . . ?
O4 C11 C3 122.0(3) . . ?
O4 C11 C12 115.6(5) . . ?
C3 C11 C12 122.3(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 122.2(3) . . ?
C24 O23 Dy1 139.7(2) . . ?
C31 O24 Dy1 143.2(2) . . ?
O22 C22 O21 113.6(3) . . ?
O22 C22 C23 128.2(4) . . ?
O21 C22 C23 118.2(3) . . ?
C24 C23 C31 119.3(3) . . ?
C24 C23 C22 120.9(3) . . ?
C31 C23 C22 119.7(3) . . ?
O23 C24 C23 125.7(3) . . ?
O23 C24 C25 117.1(3) . . ?
C23 C24 C25 117.2(3) . . ?
C30 C25 C26 119.0(3) . . ?
C30 C25 C24 119.3(3) . . ?
C26 C25 C24 121.8(3) . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C28 119.9(4) . . ?
C26 C27 H27A 120.1 . . ?
C28 C27 H27A 120.1 . . ?
C29 C28 C27 120.9(4) . . ?
C29 C28 H28A 119.5 . . ?
C27 C28 H28A 119.5 . . ?
C28 C29 C30 118.5(4) . . ?
C28 C29 H29A 120.7 . . ?
C30 C29 H29A 120.7 . . ?
O21 C30 C25 122.1(3) . . ?
O21 C30 C29 116.1(3) . . ?
C25 C30 C29 121.8(4) . . ?
O24 C31 C23 122.5(3) . . ?
O24 C31 C32 114.7(3) . . ?
C23 C31 C32 122.7(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 122.7(3) . . ?
C44 O43 Dy1 130.8(2) . . ?
C51 O44 Dy1 133.5(2) . . ?
O42 C42 O41 114.0(3) . . ?
O42 C42 C43 127.7(4) . . ?
O41 C42 C43 118.3(3) . . ?
C44 C43 C51 120.6(3) . . ?
C44 C43 C42 119.6(3) . . ?
C51 C43 C42 119.8(3) . . ?
O43 C44 C43 124.4(3) . . ?
O43 C44 C45 117.0(3) . . ?
C43 C44 C45 118.6(3) . . ?
C50 C45 C46 118.1(3) . . ?
C50 C45 C44 119.4(3) . . ?
C46 C45 C44 122.5(3) . . ?
C47 C46 C45 121.1(4) . . ?
C47 C46 H46A 119.5 . . ?
C45 C46 H46A 119.5 . . ?
C46 C47 C48 119.3(4) . . ?
C46 C47 H47A 120.3 . . ?
C48 C47 H47A 120.3 . . ?
C49 C48 C47 120.9(4) . . ?
C49 C48 H48A 119.5 . . ?
C47 C48 H48A 119.5 . . ?
C48 C49 C50 119.1(4) . . ?
C48 C49 H49A 120.4 . . ?
C50 C49 H49A 120.4 . . ?
O41 C50 C49 117.2(4) . . ?
O41 C50 C45 121.3(3) . . ?
C49 C50 C45 121.5(4) . . ?
O44 C51 C43 121.9(3) . . ?
O44 C51 C52 115.7(3) . . ?
C43 C51 C52 122.4(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C62 N61 C74 117.3(3) . . ?
C62 N61 Dy1 123.9(2) . . ?
C74 N61 Dy1 117.8(2) . . ?
N61 C62 C63 123.4(3) . . ?
N61 C62 H62A 118.3 . . ?
C63 C62 H62A 118.3 . . ?
C64 C63 C62 119.2(4) . . ?
C64 C63 H63A 120.4 . . ?
C62 C63 H63A 120.4 . . ?
C63 C64 C65 120.0(4) . . ?
C63 C64 H64A 120.0 . . ?
C65 C64 H64A 120.0 . . ?
C64 C65 C74 116.8(3) . . ?
C64 C65 C66 123.5(4) . . ?
C74 C65 C66 119.6(3) . . ?
C67 C66 C65 120.9(4) . . ?
C67 C66 H66A 119.6 . . ?
C65 C66 H66A 119.6 . . ?
C66 C67 C68 121.9(3) . . ?
C66 C67 H67A 119.1 . . ?
C68 C67 H67A 119.1 . . ?
C69 C68 C73 117.3(3) . . ?
C69 C68 C67 123.9(3) . . ?
C73 C68 C67 118.8(3) . . ?
C70 C69 C68 119.9(3) . . ?
C70 C69 H69A 120.0 . . ?
C68 C69 H69A 120.0 . . ?
C69 C70 C71 118.7(3) . . ?
C69 C70 H70A 120.6 . . ?
C71 C70 H70A 120.6 . . ?
N72 C71 C70 123.6(3) . . ?
N72 C71 H71A 118.2 . . ?
C70 C71 H71A 118.2 . . ?
C71 N72 C73 117.7(3) . . ?
C71 N72 Dy1 124.0(2) . . ?
C73 N72 Dy1 117.5(2) . . ?
N72 C73 C68 122.6(3) . . ?
N72 C73 C74 118.2(3) . . ?
C68 C73 C74 119.1(3) . . ?
N61 C74 C65 123.2(3) . . ?
N61 C74 C73 117.2(3) . . ?
C65 C74 C73 119.6(3) . . ?
H81A O81 H81B 100(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 174.7(5) . . . . ?
C10 O1 C2 C3 -5.7(7) . . . . ?
O2 C2 C3 C4 -170.0(5) . . . . ?
O1 C2 C3 C4 10.5(6) . . . . ?
O2 C2 C3 C11 9.1(8) . . . . ?
O1 C2 C3 C11 -170.4(4) . . . . ?
Dy1 O3 C4 C3 -33.3(5) . . . . ?
Dy1 O3 C4 C5 148.0(2) . . . . ?
C11 C3 C4 O3 -6.5(6) . . . . ?
C2 C3 C4 O3 172.6(4) . . . . ?
C11 C3 C4 C5 172.1(3) . . . . ?
C2 C3 C4 C5 -8.8(5) . . . . ?
O3 C4 C5 C6 0.1(5) . . . . ?
C3 C4 C5 C6 -178.6(4) . . . . ?
O3 C4 C5 C10 -178.8(3) . . . . ?
C3 C4 C5 C10 2.5(5) . . . . ?
C10 C5 C6 C7 -0.6(7) . . . . ?
C4 C5 C6 C7 -179.5(4) . . . . ?
C5 C6 C7 C8 -0.7(8) . . . . ?
C6 C7 C8 C9 1.4(10) . . . . ?
C7 C8 C9 C10 -0.8(9) . . . . ?
C2 O1 C10 C5 -0.7(7) . . . . ?
C2 O1 C10 C9 -178.6(4) . . . . ?
C6 C5 C10 O1 -176.5(4) . . . . ?
C4 C5 C10 O1 2.4(6) . . . . ?
C6 C5 C10 C9 1.2(6) . . . . ?
C4 C5 C10 C9 -179.8(4) . . . . ?
C8 C9 C10 O1 177.3(5) . . . . ?
C8 C9 C10 C5 -0.5(8) . . . . ?
Dy1 O4 C11 C3 21.3(6) . . . . ?
Dy1 O4 C11 C12 -160.7(3) . . . . ?
C4 C3 C11 O4 12.9(6) . . . . ?
C2 C3 C11 O4 -166.1(4) . . . . ?
C4 C3 C11 C12 -164.9(4) . . . . ?
C2 C3 C11 C12 16.1(6) . . . . ?
C30 O21 C22 O22 179.1(4) . . . . ?
C30 O21 C22 C23 -1.1(6) . . . . ?
O22 C22 C23 C24 -177.6(4) . . . . ?
O21 C22 C23 C24 2.6(6) . . . . ?
O22 C22 C23 C31 5.6(7) . . . . ?
O21 C22 C23 C31 -174.1(3) . . . . ?
Dy1 O23 C24 C23 -0.1(6) . . . . ?
Dy1 O23 C24 C25 -179.0(2) . . . . ?
C31 C23 C24 O23 -4.5(5) . . . . ?
C22 C23 C24 O23 178.7(4) . . . . ?
C31 C23 C24 C25 174.4(3) . . . . ?
C22 C23 C24 C25 -2.4(5) . . . . ?
O23 C24 C25 C30 179.6(3) . . . . ?
C23 C24 C25 C30 0.6(5) . . . . ?
O23 C24 C25 C26 0.1(5) . . . . ?
C23 C24 C25 C26 -178.9(3) . . . . ?
C30 C25 C26 C27 -0.4(6) . . . . ?
C24 C25 C26 C27 179.1(4) . . . . ?
C25 C26 C27 C28 0.1(7) . . . . ?
C26 C27 C28 C29 0.2(7) . . . . ?
C27 C28 C29 C30 -0.1(7) . . . . ?
C22 O21 C30 C25 -0.7(5) . . . . ?
C22 O21 C30 C29 179.2(4) . . . . ?
C26 C25 C30 O21 -179.5(3) . . . . ?
C24 C25 C30 O21 1.0(5) . . . . ?
C26 C25 C30 C29 0.5(5) . . . . ?
C24 C25 C30 C29 -179.0(3) . . . . ?
C28 C29 C30 O21 179.8(4) . . . . ?
C28 C29 C30 C25 -0.3(6) . . . . ?
Dy1 O24 C31 C23 5.6(7) . . . . ?
Dy1 O24 C31 C32 -176.9(3) . . . . ?
C24 C23 C31 O24 2.2(6) . . . . ?
C22 C23 C31 O24 179.0(4) . . . . ?
C24 C23 C31 C32 -175.1(4) . . . . ?
C22 C23 C31 C32 1.7(6) . . . . ?
C50 O41 C42 O42 -179.8(4) . . . . ?
C50 O41 C42 C43 1.6(5) . . . . ?
O42 C42 C43 C44 -179.2(4) . . . . ?
O41 C42 C43 C44 -0.7(5) . . . . ?
O42 C42 C43 C51 -0.3(6) . . . . ?
O41 C42 C43 C51 178.1(3) . . . . ?
Dy1 O43 C44 C43 38.2(5) . . . . ?
Dy1 O43 C44 C45 -142.2(2) . . . . ?
C51 C43 C44 O43 0.2(5) . . . . ?
C42 C43 C44 O43 179.1(3) . . . . ?
C51 C43 C44 C45 -179.4(3) . . . . ?
C42 C43 C44 C45 -0.5(5) . . . . ?
O43 C44 C45 C50 -178.6(3) . . . . ?
C43 C44 C45 C50 1.0(5) . . . . ?
O43 C44 C45 C46 2.1(5) . . . . ?
C43 C44 C45 C46 -178.3(3) . . . . ?
C50 C45 C46 C47 0.2(6) . . . . ?
C44 C45 C46 C47 179.5(4) . . . . ?
C45 C46 C47 C48 0.4(7) . . . . ?
C46 C47 C48 C49 -0.8(8) . . . . ?
C47 C48 C49 C50 0.5(8) . . . . ?
C42 O41 C50 C49 178.6(4) . . . . ?
C42 O41 C50 C45 -1.1(6) . . . . ?
C48 C49 C50 O41 -179.5(4) . . . . ?
C48 C49 C50 C45 0.2(7) . . . . ?
C46 C45 C50 O41 179.1(4) . . . . ?
C44 C45 C50 O41 -0.2(5) . . . . ?
C46 C45 C50 C49 -0.6(6) . . . . ?
C44 C45 C50 C49 -179.9(4) . . . . ?
Dy1 O44 C51 C43 -26.5(5) . . . . ?
Dy1 O44 C51 C52 152.9(2) . . . . ?
C44 C43 C51 O44 -5.8(5) . . . . ?
C42 C43 C51 O44 175.3(3) . . . . ?
C44 C43 C51 C52 174.9(3) . . . . ?
C42 C43 C51 C52 -4.0(5) . . . . ?
C74 N61 C62 C63 1.4(6) . . . . ?
Dy1 N61 C62 C63 -166.6(3) . . . . ?
N61 C62 C63 C64 1.6(6) . . . . ?
C62 C63 C64 C65 -2.2(6) . . . . ?
C63 C64 C65 C74 -0.2(6) . . . . ?
C63 C64 C65 C66 -177.8(4) . . . . ?
C64 C65 C66 C67 174.4(4) . . . . ?
C74 C65 C66 C67 -3.1(6) . . . . ?
C65 C66 C67 C68 -0.1(7) . . . . ?
C66 C67 C68 C69 -174.2(4) . . . . ?
C66 C67 C68 C73 3.6(6) . . . . ?
C73 C68 C69 C70 -0.1(6) . . . . ?
C67 C68 C69 C70 177.7(4) . . . . ?
C68 C69 C70 C71 2.1(6) . . . . ?
C69 C70 C71 N72 -0.8(6) . . . . ?
C70 C71 N72 C73 -2.6(6) . . . . ?
C70 C71 N72 Dy1 167.0(3) . . . . ?
C71 N72 C73 C68 4.7(5) . . . . ?
Dy1 N72 C73 C68 -165.5(3) . . . . ?
C71 N72 C73 C74 -172.8(3) . . . . ?
Dy1 N72 C73 C74 17.0(4) . . . . ?
C69 C68 C73 N72 -3.4(5) . . . . ?
C67 C68 C73 N72 178.6(3) . . . . ?
C69 C68 C73 C74 174.1(3) . . . . ?
C67 C68 C73 C74 -3.8(5) . . . . ?
C62 N61 C74 C65 -4.0(5) . . . . ?
Dy1 N61 C74 C65 164.8(3) . . . . ?
C62 N61 C74 C73 174.4(3) . . . . ?
Dy1 N61 C74 C73 -16.9(4) . . . . ?
C64 C65 C74 N61 3.4(5) . . . . ?
C66 C65 C74 N61 -178.9(4) . . . . ?
C64 C65 C74 C73 -174.9(3) . . . . ?
C66 C65 C74 C73 2.8(5) . . . . ?
N72 C73 C74 N61 -0.1(5) . . . . ?
C68 C73 C74 N61 -177.7(3) . . . . ?
N72 C73 C74 C65 178.3(3) . . . . ?
C68 C73 C74 C65 0.7(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C12 H12A O81 0.96 2.04 2.946(12) 157.1 . no
C12 H12C O2 0.96 2.62 3.517(7) 156.4 2_567 no
C52 H52C O43 0.96 2.60 3.411(5) 141.7 2_667 no
C71 H71A O2 0.93 2.57 3.241(5) 129.7 2_567 no
O81 H81A O4 0.88(2) 2.27(5) 2.959(10) 135(6) . no
O81 H81B O22 0.87(2) 2.53(7) 3.111(11) 125(7) 2_556 no

_refine_diff_density_max         1.295
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.073

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_Tm-batho
_database_code_depnum_ccdc_archive 'CCDC 2013260'
loop_
_audit_author_name
_audit_author_address
'Sylvain Bernes'
;Instituto de Fisica, BUAP, Puebla
Mexico
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-09-22 downloaded from the CCDC.
;

# Clave Lab.  :  TmBF
# Clave IF-UAP:  TmBF
# Solicitud: 234
# Firma en la Solicitud: Dra. Laura Gasque (FQ-UNAM)
# Clave datos : ... \BUAP\Sylvain\TmBF\40mm_1\

_database_code_CAS               ?
_database_code_CSD               ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_audit_creation_date             2019-01-17

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H37 N2 O12 Tm, 0.7(C2 H6 O)'
_chemical_formula_sum            'C58.40 H41.20 N2 O12.70 Tm'
_chemical_formula_weight         1143.06
_chemical_absolute_configuration ?
_chemical_optical_rotation       ?

_chemical_properties_physical    ?
_chemical_properties_biological  ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3084 3.5155 '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       ?

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

_cell_length_a                   11.5992(5)
_cell_length_b                   13.3015(6)
_cell_length_c                   18.3354(8)
_cell_angle_alpha                78.343(4)
_cell_angle_beta                 76.447(3)
_cell_angle_gamma                68.722(3)
_cell_volume                     2541.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    31185
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      24.98

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.032
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 3 -8 0.0370
-2 -2 7 0.0470
-2 -5 -6 0.1390
2 5 4 0.1610
-4 4 -1 0.0110
4 -4 1 0.0200

_exptl_absorpt_coefficient_mu    0.977
_shelx_estimated_absorpt_T_min   0.757
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4837
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'X-AREA 1.82 (Stoe & Cie, 2018)'

_diffrn_ambient_temperature      295(1)
_diffrn_ambient_environment      air
_diffrn_measurement_specimen_support Mitegen
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Axo Astix-f Microfocus source'
_diffrn_source_voltage           65
_diffrn_source_current           0.600
_diffrn_source_power             0.039
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  -90
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_type            'Dectris Pilatus 100K R'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_details      
;
1151 frames, 65 s/frame, 1 deg./frame, detector distance = 40 mm
;
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            69885
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.615
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        19.664
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13501
_reflns_number_gt                7615
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          ?

_computing_data_collection       'X-AREA 1.82 (Stoe & Cie, 2018)'
_computing_cell_refinement       'X-AREA 1.82'
_computing_data_reduction        'X-AREA 1.82'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'PublCif (Westrip, 2010)'
_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)+(0.0143P)²] 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         13501
_refine_ls_number_parameters     681
_refine_ls_number_restraints     13
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0567
_refine_ls_goodness_of_fit_ref   0.768
_refine_ls_restrained_S_all      0.768
_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
Tm1 Tm 0.41157(2) 0.36102(2) 0.31503(2) 0.04353(6) Uani 1 1 d . . . . .
O1 O 0.3067(3) 0.0690(2) 0.59307(15) 0.0734(8) Uani 1 1 d . . . . .
O2 O 0.3818(3) 0.1624(3) 0.64269(16) 0.0876(10) Uani 1 1 d . . . . .
O3 O 0.4145(2) 0.1956(2) 0.37737(14) 0.0609(8) Uani 1 1 d . . . . .
O4 O 0.4667(2) 0.3381(2) 0.43339(14) 0.0521(7) Uani 1 1 d . . . . .
C2 C 0.3667(4) 0.1454(3) 0.5839(2) 0.0594(11) Uani 1 1 d . . . . .
C3 C 0.4017(3) 0.1947(3) 0.50831(19) 0.0438(9) Uani 1 1 d . . . . .
C4 C 0.3812(3) 0.1618(3) 0.4453(2) 0.0476(9) Uani 1 1 d . . . . .
C5 C 0.3177(4) 0.0803(3) 0.4594(2) 0.0527(10) Uani 1 1 d . . . . .
C6 C 0.2884(4) 0.0480(3) 0.4007(2) 0.0705(13) Uani 1 1 d . . . . .
H6 H 0.314519 0.074058 0.350891 0.085 Uiso 1 1 calc R U . . .
C7 C 0.2205(5) -0.0228(4) 0.4160(3) 0.0865(15) Uani 1 1 d . . . . .
H7 H 0.200863 -0.044732 0.376758 0.104 Uiso 1 1 calc R U . . .
C8 C 0.1820(5) -0.0607(4) 0.4906(3) 0.0964(18) Uani 1 1 d . . . . .
H8 H 0.135129 -0.107285 0.500939 0.116 Uiso 1 1 calc R U . . .
C9 C 0.2113(5) -0.0312(4) 0.5490(3) 0.0908(17) Uani 1 1 d . . . . .
H9 H 0.186448 -0.058475 0.598783 0.109 Uiso 1 1 calc R U . . .
C10 C 0.2794(4) 0.0409(3) 0.5328(3) 0.0627(11) Uani 1 1 d . . . . .
C11 C 0.4567(3) 0.2796(3) 0.4958(2) 0.0470(10) Uani 1 1 d . . . . .
C12 C 0.5059(4) 0.3018(4) 0.5575(2) 0.0722(13) Uani 1 1 d . . . . .
H12A H 0.563748 0.235457 0.577777 0.108 Uiso 1 1 calc R U . . .
H12B H 0.437139 0.329992 0.596926 0.108 Uiso 1 1 calc R U . . .
H12C H 0.548237 0.354104 0.537265 0.108 Uiso 1 1 calc R U . . .
O21 O -0.1425(2) 0.5738(2) 0.43043(16) 0.0687(8) Uani 1 1 d . . . . .
O22 O -0.0767(3) 0.7074(3) 0.4336(2) 0.0950(11) Uani 1 1 d . . . . .
O23 O 0.2081(2) 0.3791(2) 0.34423(17) 0.0732(9) Uani 1 1 d . . . . .
O24 O 0.2970(2) 0.5293(2) 0.35554(14) 0.0543(7) Uani 1 1 d . . . . .
C22 C -0.0451(4) 0.6170(4) 0.4179(2) 0.0619(12) Uani 1 1 d . . . . .
C23 C 0.0808(3) 0.5494(3) 0.3882(2) 0.0485(9) Uani 1 1 d . . . . .
C24 C 0.1023(4) 0.4443(4) 0.3713(2) 0.0523(11) Uani 1 1 d . . . . .
C25 C -0.0062(3) 0.4070(3) 0.3829(2) 0.0515(10) Uani 1 1 d . . . . .
C26 C 0.0071(4) 0.3057(4) 0.3652(2) 0.0627(12) Uani 1 1 d . . . . .
H26 H 0.085808 0.260470 0.345053 0.075 Uiso 1 1 calc R U . . .
C27 C -0.0968(4) 0.2727(4) 0.3776(2) 0.0676(13) Uani 1 1 d . . . . .
H27 H -0.088195 0.205597 0.365232 0.081 Uiso 1 1 calc R U . . .
C28 C -0.2125(4) 0.3391(4) 0.4081(2) 0.0721(14) Uani 1 1 d . . . . .
H28 H -0.281889 0.316171 0.416550 0.087 Uiso 1 1 calc R U . . .
C29 C -0.2277(4) 0.4389(4) 0.4263(2) 0.0717(13) Uani 1 1 d . . . . .
H29 H -0.306491 0.483418 0.446853 0.086 Uiso 1 1 calc R U . . .
C30 C -0.1225(4) 0.4723(4) 0.4133(2) 0.0549(10) Uani 1 1 d . . . . .
C31 C 0.1860(4) 0.5881(3) 0.3760(2) 0.0499(10) Uani 1 1 d . . . . .
C32 C 0.1661(4) 0.7039(3) 0.3856(3) 0.0757(13) Uani 1 1 d . . . . .
H32A H 0.134346 0.714287 0.437760 0.113 Uiso 1 1 calc R U . . .
H32B H 0.106703 0.753276 0.355112 0.113 Uiso 1 1 calc R U . . .
H32C H 0.244590 0.717611 0.369922 0.113 Uiso 1 1 calc R U . . .
O41 O 0.2421(3) 0.4899(3) 0.01421(16) 0.0801(9) Uani 1 1 d . . . . .
O42 O 0.1794(3) 0.3510(3) 0.05939(17) 0.0986(12) Uani 1 1 d . . . . .
O43 O 0.3937(2) 0.4630(2) 0.20035(14) 0.0608(7) Uani 1 1 d . . . . .
O44 O 0.3869(2) 0.2626(2) 0.23264(14) 0.0577(7) Uani 1 1 d . . . . .
C42 C 0.2398(4) 0.4023(4) 0.0693(2) 0.0705(13) Uani 1 1 d . . . . .
C43 C 0.3032(3) 0.3850(3) 0.1317(2) 0.0528(10) Uani 1 1 d . . . . .
C44 C 0.3516(3) 0.4642(3) 0.1421(2) 0.0515(10) Uani 1 1 d . . . . .
C45 C 0.3574(4) 0.5512(3) 0.0790(2) 0.0561(10) Uani 1 1 d . . . . .
C46 C 0.4219(4) 0.6222(3) 0.0778(2) 0.0639(11) Uani 1 1 d . . . . .
H46 H 0.459416 0.617296 0.118627 0.077 Uiso 1 1 calc R U . . .
C47 C 0.4299(5) 0.7001(4) 0.0157(3) 0.0784(14) Uani 1 1 d . . . . .
H47 H 0.472644 0.747670 0.014716 0.094 Uiso 1 1 calc R U . . .
C48 C 0.3744(5) 0.7066(4) -0.0444(3) 0.0838(15) Uani 1 1 d . . . . .
H48 H 0.379600 0.758854 -0.086077 0.101 Uiso 1 1 calc R U . . .
C49 C 0.3111(5) 0.6361(4) -0.0434(3) 0.0824(14) Uani 1 1 d . . . . .
H49 H 0.273243 0.641550 -0.084160 0.099 Uiso 1 1 calc R U . . .
C50 C 0.3037(4) 0.5584(4) 0.0172(2) 0.0640(12) Uani 1 1 d . . . . .
C51 C 0.3307(4) 0.2825(4) 0.1785(2) 0.0556(11) Uani 1 1 d . . . . .
C52 C 0.3018(5) 0.1871(4) 0.1627(3) 0.0923(17) Uani 1 1 d . . . . .
H52A H 0.315664 0.186527 0.109003 0.138 Uiso 1 1 calc R U . . .
H52B H 0.215728 0.194030 0.183723 0.138 Uiso 1 1 calc R U . . .
H52C H 0.355861 0.120334 0.185258 0.138 Uiso 1 1 calc R U . . .
N1 N 0.5764(3) 0.4534(2) 0.28074(15) 0.0418(7) Uani 1 1 d . . . . .
N2 N 0.6280(3) 0.2421(2) 0.26942(16) 0.0447(7) Uani 1 1 d . . . . .
C61 C 0.5508(3) 0.5564(3) 0.2860(2) 0.0525(10) Uani 1 1 d . . . . .
H61 H 0.471851 0.594047 0.311194 0.063 Uiso 1 1 calc R U . . .
C62 C 0.6363(4) 0.6125(3) 0.2558(2) 0.0531(10) Uani 1 1 d . . . . .
H62 H 0.613124 0.685389 0.261894 0.064 Uiso 1 1 calc R U . . .
C63 C 0.7520(3) 0.5624(3) 0.21785(19) 0.0444(9) Uani 1 1 d . . . . .
C64 C 0.7847(3) 0.4498(3) 0.21166(19) 0.0422(9) Uani 1 1 d . . . . .
C65 C 0.9046(3) 0.3843(3) 0.1770(2) 0.0521(10) Uani 1 1 d . . . . .
H65 H 0.965928 0.416574 0.156080 0.063 Uiso 1 1 calc R U . . .
C66 C 0.9328(3) 0.2789(3) 0.1731(2) 0.0516(10) Uani 1 1 d . . . . .
H66 H 1.012477 0.239918 0.149615 0.062 Uiso 1 1 calc R U . . .
C67 C 0.8418(3) 0.2245(3) 0.2047(2) 0.0445(9) Uani 1 1 d . . . . .
C68 C 0.8676(4) 0.1123(3) 0.2030(2) 0.0519(11) Uani 1 1 d . . . . .
C69 C 0.7734(4) 0.0698(3) 0.2350(2) 0.0562(11) Uani 1 1 d . . . . .
H69 H 0.787527 -0.003825 0.235794 0.067 Uiso 1 1 calc R U . . .
C70 C 0.6570(4) 0.1367(3) 0.2663(2) 0.0551(11) Uani 1 1 d . . . . .
H70 H 0.594490 0.105533 0.286661 0.066 Uiso 1 1 calc R U . . .
C71 C 0.7217(3) 0.2861(3) 0.23940(18) 0.0391(9) Uani 1 1 d . . . . .
C72 C 0.6925(3) 0.3990(3) 0.24387(18) 0.0386(8) Uani 1 1 d . . . . .
C73 C 0.8431(3) 0.6225(3) 0.1852(2) 0.0479(9) Uani 1 1 d D . . . .
C74 C 0.8730(4) 0.6757(3) 0.2319(2) 0.0619(12) Uani 1 1 d D . . . .
H74 H 0.837228 0.673875 0.282908 0.074 Uiso 1 1 calc R U . . .
C75 C 0.9575(5) 0.7319(4) 0.2013(3) 0.0841(15) Uani 1 1 d D . . . .
H75 H 0.979370 0.766501 0.232614 0.101 Uiso 1 1 calc R U . . .
C76 C 1.0080(4) 0.7371(4) 0.1271(3) 0.0907(17) Uani 1 1 d D . . . .
H76 H 1.064175 0.775083 0.107805 0.109 Uiso 1 1 calc R U . . .
C77 C 0.9771(4) 0.6866(4) 0.0798(3) 0.0796(14) Uani 1 1 d D . . . .
H77 H 1.011190 0.690908 0.028481 0.096 Uiso 1 1 calc R U . . .
C78 C 0.8946(4) 0.6294(3) 0.1096(2) 0.0640(12) Uani 1 1 d D . . . .
H78 H 0.873528 0.594882 0.077856 0.077 Uiso 1 1 calc R U . . .
C79 C 0.9945(4) 0.0436(4) 0.1690(3) 0.0697(13) Uani 1 1 d D . . . .
C80 C 1.0280(6) 0.0506(5) 0.0926(4) 0.131(2) Uani 1 1 d D . . . .
H80 H 0.970727 0.095207 0.061818 0.158 Uiso 1 1 calc R U . . .
C81 C 1.1482(8) -0.0094(8) 0.0607(6) 0.202(6) Uani 1 1 d D . . . .
H81 H 1.171660 -0.004512 0.008335 0.243 Uiso 1 1 calc R U . . .
C82 C 1.2331(8) -0.0759(8) 0.1056(7) 0.214(8) Uani 1 1 d D . . . .
H82 H 1.314042 -0.115506 0.084311 0.256 Uiso 1 1 calc R U . . .
C83 C 1.1970(7) -0.0825(7) 0.1805(6) 0.197(5) Uani 1 1 d D . . . .
H83 H 1.253457 -0.127565 0.211525 0.237 Uiso 1 1 calc R U . . .
C84 C 1.0772(6) -0.0236(5) 0.2127(4) 0.131(2) Uani 1 1 d D . . . .
H84 H 1.053561 -0.030372 0.265034 0.157 Uiso 1 1 calc R U . . .
C91 C 0.5894(8) -0.1080(9) 0.0916(5) 0.155(4) Uani 0.7 1 d . . P . .
H91A H 0.661238 -0.116895 0.051723 0.233 Uiso 0.7 1 calc R U P . .
H91B H 0.518146 -0.051650 0.074381 0.233 Uiso 0.7 1 calc R U P . .
H91C H 0.571499 -0.175024 0.105918 0.233 Uiso 0.7 1 calc R U P . .
C92 C 0.6135(8) -0.0805(7) 0.1516(6) 0.119(3) Uani 0.7 1 d D . P . .
H92A H 0.618809 -0.007707 0.138604 0.143 Uiso 0.7 1 calc R U P . .
H92B H 0.695083 -0.129625 0.161704 0.143 Uiso 0.7 1 calc R U P . .
O92 O 0.5234(7) -0.0830(6) 0.2187(4) 0.151(3) Uani 0.7 1 d D . P . .
H92 H 0.545937 -0.068254 0.253267 0.226 Uiso 0.7 1 calc R U P . .


_geom_special_details            ?

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
Tm1 O23 2.228(2) . ?
Tm1 O3 2.258(2) . ?
Tm1 O43 2.270(3) . ?
Tm1 O44 2.313(2) . ?
Tm1 O24 2.319(3) . ?
Tm1 O4 2.335(2) . ?
Tm1 N2 2.485(3) . ?
Tm1 N1 2.528(2) . ?
O1 C10 1.371(5) . ?
O1 C2 1.390(4) . ?
O2 C2 1.209(4) . ?
O3 C4 1.256(4) . ?
O4 C11 1.254(4) . ?
C2 C3 1.441(5) . ?
C3 C4 1.410(5) . ?
C3 C11 1.444(5) . ?
C4 C5 1.470(5) . ?
C5 C10 1.374(5) . ?
C5 C6 1.385(5) . ?
C6 C7 1.385(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.386(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.362(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.399(5) . ?
C9 H9 0.9300 . ?
C11 C12 1.501(5) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
O21 C30 1.373(4) . ?
O21 C22 1.398(4) . ?
O22 C22 1.197(4) . ?
O23 C24 1.273(4) . ?
O24 C31 1.253(4) . ?
C22 C23 1.453(5) . ?
C23 C24 1.413(5) . ?
C23 C31 1.444(5) . ?
C24 C25 1.471(4) . ?
C25 C30 1.370(5) . ?
C25 C26 1.394(5) . ?
C26 C27 1.383(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.372(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.373(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.399(5) . ?
C29 H29 0.9300 . ?
C31 C32 1.513(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C50 1.363(5) . ?
O41 C42 1.384(5) . ?
O42 C42 1.203(4) . ?
O43 C44 1.270(4) . ?
O44 C51 1.247(4) . ?
C42 C43 1.438(5) . ?
C43 C44 1.421(5) . ?
C43 C51 1.427(5) . ?
C44 C45 1.469(5) . ?
C45 C50 1.387(5) . ?
C45 C46 1.397(5) . ?
C46 C47 1.387(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.375(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.380(6) . ?
C48 H48 0.9300 . ?
C49 C50 1.366(6) . ?
C49 H49 0.9300 . ?
C51 C52 1.520(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N1 C61 1.311(4) . ?
N1 C72 1.363(4) . ?
N2 C70 1.328(4) . ?
N2 C71 1.370(4) . ?
C61 C62 1.400(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.353(5) . ?
C62 H62 0.9300 . ?
C63 C64 1.427(5) . ?
C63 C73 1.496(4) . ?
C64 C72 1.420(4) . ?
C64 C65 1.424(5) . ?
C65 C66 1.332(5) . ?
C65 H65 0.9300 . ?
C66 C67 1.440(4) . ?
C66 H66 0.9300 . ?
C67 C71 1.408(5) . ?
C67 C68 1.418(5) . ?
C68 C69 1.368(5) . ?
C68 C79 1.488(5) . ?
C69 C70 1.384(5) . ?
C69 H69 0.9300 . ?
C70 H70 0.9300 . ?
C71 C72 1.431(4) . ?
C73 C78 1.374(5) . ?
C73 C74 1.384(4) . ?
C74 C75 1.392(5) . ?
C74 H74 0.9300 . ?
C75 C76 1.348(6) . ?
C75 H75 0.9300 . ?
C76 C77 1.374(6) . ?
C76 H76 0.9300 . ?
C77 C78 1.382(5) . ?
C77 H77 0.9300 . ?
C78 H78 0.9300 . ?
C79 C84 1.345(7) . ?
C79 C80 1.357(6) . ?
C80 C81 1.387(8) . ?
C80 H80 0.9300 . ?
C81 C82 1.373(12) . ?
C81 H81 0.9300 . ?
C82 C83 1.332(12) . ?
C82 H82 0.9300 . ?
C83 C84 1.380(8) . ?
C83 H83 0.9300 . ?
C84 H84 0.9300 . ?
C91 C92 1.342(9) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C92 O92 1.420(7) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
O92 H92 0.8200 . ?

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
O23 Tm1 O3 77.60(10) . . ?
O23 Tm1 O43 93.50(10) . . ?
O3 Tm1 O43 141.97(8) . . ?
O23 Tm1 O44 76.15(9) . . ?
O3 Tm1 O44 71.73(9) . . ?
O43 Tm1 O44 70.24(9) . . ?
O23 Tm1 O24 70.33(9) . . ?
O3 Tm1 O24 127.63(9) . . ?
O43 Tm1 O24 81.28(9) . . ?
O44 Tm1 O24 134.08(9) . . ?
O23 Tm1 O4 102.80(10) . . ?
O3 Tm1 O4 69.90(8) . . ?
O43 Tm1 O4 147.46(8) . . ?
O44 Tm1 O4 140.82(9) . . ?
O24 Tm1 O4 78.10(9) . . ?
O23 Tm1 N2 146.46(9) . . ?
O3 Tm1 N2 77.04(9) . . ?
O43 Tm1 N2 93.11(9) . . ?
O44 Tm1 N2 75.30(9) . . ?
O24 Tm1 N2 143.20(8) . . ?
O4 Tm1 N2 88.63(9) . . ?
O23 Tm1 N1 147.51(10) . . ?
O3 Tm1 N1 131.72(10) . . ?
O43 Tm1 N1 71.35(9) . . ?
O44 Tm1 N1 121.84(9) . . ?
O24 Tm1 N1 78.87(9) . . ?
O4 Tm1 N1 80.11(8) . . ?
N2 Tm1 N1 65.00(9) . . ?
C10 O1 C2 121.9(3) . . ?
C4 O3 Tm1 133.5(2) . . ?
C11 O4 Tm1 138.1(2) . . ?
O2 C2 O1 113.6(4) . . ?
O2 C2 C3 128.1(4) . . ?
O1 C2 C3 118.3(4) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 C11 118.8(3) . . ?
C2 C3 C11 120.7(3) . . ?
O3 C4 C3 125.2(3) . . ?
O3 C4 C5 116.7(3) . . ?
C3 C4 C5 118.1(3) . . ?
C10 C5 C6 119.4(4) . . ?
C10 C5 C4 118.9(4) . . ?
C6 C5 C4 121.6(3) . . ?
C7 C6 C5 120.3(4) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 119.2(4) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C9 C8 C7 121.5(4) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 118.6(4) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
O1 C10 C5 122.1(3) . . ?
O1 C10 C9 117.0(4) . . ?
C5 C10 C9 121.0(4) . . ?
O4 C11 C3 122.4(3) . . ?
O4 C11 C12 116.4(3) . . ?
C3 C11 C12 121.2(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 O21 C22 122.0(3) . . ?
C24 O23 Tm1 141.1(2) . . ?
C31 O24 Tm1 141.1(2) . . ?
O22 C22 O21 114.7(4) . . ?
O22 C22 C23 127.4(4) . . ?
O21 C22 C23 117.8(4) . . ?
C24 C23 C31 118.9(3) . . ?
C24 C23 C22 120.5(3) . . ?
C31 C23 C22 120.6(4) . . ?
O23 C24 C23 125.7(3) . . ?
O23 C24 C25 116.1(4) . . ?
C23 C24 C25 118.2(4) . . ?
C30 C25 C26 119.4(3) . . ?
C30 C25 C24 119.1(4) . . ?
C26 C25 C24 121.5(4) . . ?
C27 C26 C25 119.9(4) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 119.9(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 121.1(4) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C28 C29 C30 118.9(4) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C25 C30 O21 122.3(3) . . ?
C25 C30 C29 120.8(4) . . ?
O21 C30 C29 116.9(4) . . ?
O24 C31 C23 122.4(4) . . ?
O24 C31 C32 116.7(3) . . ?
C23 C31 C32 120.9(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C50 O41 C42 121.8(3) . . ?
C44 O43 Tm1 137.4(2) . . ?
C51 O44 Tm1 136.8(3) . . ?
O42 C42 O41 113.8(4) . . ?
O42 C42 C43 127.8(5) . . ?
O41 C42 C43 118.4(4) . . ?
C44 C43 C51 119.3(3) . . ?
C44 C43 C42 120.6(4) . . ?
C51 C43 C42 119.6(4) . . ?
O43 C44 C43 124.9(4) . . ?
O43 C44 C45 118.1(3) . . ?
C43 C44 C45 117.0(4) . . ?
C50 C45 C46 119.3(4) . . ?
C50 C45 C44 118.9(4) . . ?
C46 C45 C44 121.7(4) . . ?
C47 C46 C45 119.9(4) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C48 C47 C46 119.6(4) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
C47 C48 C49 120.5(5) . . ?
C47 C48 H48 119.7 . . ?
C49 C48 H48 119.7 . . ?
C50 C49 C48 120.2(5) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
O41 C50 C49 117.5(4) . . ?
O41 C50 C45 122.2(4) . . ?
C49 C50 C45 120.4(5) . . ?
O44 C51 C43 122.3(3) . . ?
O44 C51 C52 115.0(4) . . ?
C43 C51 C52 122.5(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C61 N1 C72 117.7(3) . . ?
C61 N1 Tm1 123.1(2) . . ?
C72 N1 Tm1 118.3(2) . . ?
C70 N2 C71 116.6(3) . . ?
C70 N2 Tm1 122.9(2) . . ?
C71 N2 Tm1 120.2(2) . . ?
N1 C61 C62 123.4(4) . . ?
N1 C61 H61 118.3 . . ?
C62 C61 H61 118.3 . . ?
C63 C62 C61 121.0(4) . . ?
C63 C62 H62 119.5 . . ?
C61 C62 H62 119.5 . . ?
C62 C63 C64 117.6(3) . . ?
C62 C63 C73 121.0(3) . . ?
C64 C63 C73 121.4(3) . . ?
C72 C64 C65 117.8(3) . . ?
C72 C64 C63 117.8(3) . . ?
C65 C64 C63 124.4(3) . . ?
C66 C65 C64 123.0(3) . . ?
C66 C65 H65 118.5 . . ?
C64 C65 H65 118.5 . . ?
C65 C66 C67 121.0(3) . . ?
C65 C66 H66 119.5 . . ?
C67 C66 H66 119.5 . . ?
C71 C67 C68 118.7(3) . . ?
C71 C67 C66 118.1(3) . . ?
C68 C67 C66 123.2(3) . . ?
C69 C68 C67 117.8(4) . . ?
C69 C68 C79 121.8(4) . . ?
C67 C68 C79 120.4(3) . . ?
C68 C69 C70 119.8(4) . . ?
C68 C69 H69 120.1 . . ?
C70 C69 H69 120.1 . . ?
N2 C70 C69 124.8(3) . . ?
N2 C70 H70 117.6 . . ?
C69 C70 H70 117.6 . . ?
N2 C71 C67 122.4(3) . . ?
N2 C71 C72 117.1(3) . . ?
C67 C71 C72 120.5(3) . . ?
N1 C72 C64 122.5(3) . . ?
N1 C72 C71 117.9(3) . . ?
C64 C72 C71 119.6(3) . . ?
C78 C73 C74 119.1(3) . . ?
C78 C73 C63 121.7(3) . . ?
C74 C73 C63 119.2(3) . . ?
C73 C74 C75 119.1(4) . . ?
C73 C74 H74 120.5 . . ?
C75 C74 H74 120.5 . . ?
C76 C75 C74 121.0(4) . . ?
C76 C75 H75 119.5 . . ?
C74 C75 H75 119.5 . . ?
C75 C76 C77 120.5(4) . . ?
C75 C76 H76 119.7 . . ?
C77 C76 H76 119.7 . . ?
C76 C77 C78 119.0(4) . . ?
C76 C77 H77 120.5 . . ?
C78 C77 H77 120.5 . . ?
C73 C78 C77 121.3(4) . . ?
C73 C78 H78 119.4 . . ?
C77 C78 H78 119.4 . . ?
C84 C79 C80 119.6(5) . . ?
C84 C79 C68 121.2(5) . . ?
C80 C79 C68 119.3(5) . . ?
C79 C80 C81 119.4(7) . . ?
C79 C80 H80 120.3 . . ?
C81 C80 H80 120.3 . . ?
C80 C81 C82 120.7(9) . . ?
C80 C81 H81 119.7 . . ?
C82 C81 H81 119.7 . . ?
C83 C82 C81 118.6(8) . . ?
C83 C82 H82 120.7 . . ?
C81 C82 H82 120.7 . . ?
C82 C83 C84 121.1(9) . . ?
C82 C83 H83 119.4 . . ?
C84 C83 H83 119.4 . . ?
C79 C84 C83 120.6(7) . . ?
C79 C84 H84 119.7 . . ?
C83 C84 H84 119.7 . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C91 C92 O92 114.9(8) . . ?
C91 C92 H92A 108.5 . . ?
O92 C92 H92A 108.5 . . ?
C91 C92 H92B 108.5 . . ?
O92 C92 H92B 108.5 . . ?
H92A C92 H92B 107.5 . . ?
C92 O92 H92 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C2 O2 178.7(4) . . . . ?
C10 O1 C2 C3 -0.6(6) . . . . ?
O2 C2 C3 C4 177.5(4) . . . . ?
O1 C2 C3 C4 -3.3(6) . . . . ?
O2 C2 C3 C11 -3.3(7) . . . . ?
O1 C2 C3 C11 175.9(3) . . . . ?
Tm1 O3 C4 C3 -41.2(6) . . . . ?
Tm1 O3 C4 C5 139.8(3) . . . . ?
C2 C3 C4 O3 -175.9(4) . . . . ?
C11 C3 C4 O3 4.9(6) . . . . ?
C2 C3 C4 C5 3.1(6) . . . . ?
C11 C3 C4 C5 -176.2(3) . . . . ?
O3 C4 C5 C10 -180.0(4) . . . . ?
C3 C4 C5 C10 1.0(6) . . . . ?
O3 C4 C5 C6 -4.3(6) . . . . ?
C3 C4 C5 C6 176.6(4) . . . . ?
C10 C5 C6 C7 0.4(7) . . . . ?
C4 C5 C6 C7 -175.2(4) . . . . ?
C5 C6 C7 C8 0.2(8) . . . . ?
C6 C7 C8 C9 -1.1(9) . . . . ?
C7 C8 C9 C10 1.4(9) . . . . ?
C2 O1 C10 C5 4.9(6) . . . . ?
C2 O1 C10 C9 -175.7(4) . . . . ?
C6 C5 C10 O1 179.3(4) . . . . ?
C4 C5 C10 O1 -4.9(6) . . . . ?
C6 C5 C10 C9 -0.1(7) . . . . ?
C4 C5 C10 C9 175.7(4) . . . . ?
C8 C9 C10 O1 179.8(5) . . . . ?
C8 C9 C10 C5 -0.8(8) . . . . ?
Tm1 O4 C11 C3 2.9(6) . . . . ?
Tm1 O4 C11 C12 -177.4(2) . . . . ?
C4 C3 C11 O4 12.8(6) . . . . ?
C2 C3 C11 O4 -166.4(4) . . . . ?
C4 C3 C11 C12 -166.9(3) . . . . ?
C2 C3 C11 C12 13.9(6) . . . . ?
C30 O21 C22 O22 178.0(4) . . . . ?
C30 O21 C22 C23 -2.1(6) . . . . ?
O22 C22 C23 C24 -178.8(5) . . . . ?
O21 C22 C23 C24 1.3(6) . . . . ?
O22 C22 C23 C31 1.6(7) . . . . ?
O21 C22 C23 C31 -178.3(3) . . . . ?
Tm1 O23 C24 C23 6.6(7) . . . . ?
Tm1 O23 C24 C25 -175.8(3) . . . . ?
C31 C23 C24 O23 -1.4(6) . . . . ?
C22 C23 C24 O23 179.0(4) . . . . ?
C31 C23 C24 C25 -179.0(3) . . . . ?
C22 C23 C24 C25 1.4(6) . . . . ?
O23 C24 C25 C30 178.7(4) . . . . ?
C23 C24 C25 C30 -3.5(6) . . . . ?
O23 C24 C25 C26 0.1(6) . . . . ?
C23 C24 C25 C26 177.9(4) . . . . ?
C30 C25 C26 C27 0.7(6) . . . . ?
C24 C25 C26 C27 179.3(4) . . . . ?
C25 C26 C27 C28 -0.7(6) . . . . ?
C26 C27 C28 C29 0.4(7) . . . . ?
C27 C28 C29 C30 -0.1(7) . . . . ?
C26 C25 C30 O21 -178.6(4) . . . . ?
C24 C25 C30 O21 2.8(6) . . . . ?
C26 C25 C30 C29 -0.3(6) . . . . ?
C24 C25 C30 C29 -179.0(4) . . . . ?
C22 O21 C30 C25 0.0(6) . . . . ?
C22 O21 C30 C29 -178.3(4) . . . . ?
C28 C29 C30 C25 0.0(6) . . . . ?
C28 C29 C30 O21 178.3(4) . . . . ?
Tm1 O24 C31 C23 7.7(6) . . . . ?
Tm1 O24 C31 C32 -170.7(3) . . . . ?
C24 C23 C31 O24 -4.7(6) . . . . ?
C22 C23 C31 O24 174.9(4) . . . . ?
C24 C23 C31 C32 173.7(4) . . . . ?
C22 C23 C31 C32 -6.7(6) . . . . ?
C50 O41 C42 O42 178.5(4) . . . . ?
C50 O41 C42 C43 0.9(6) . . . . ?
O42 C42 C43 C44 -168.7(5) . . . . ?
O41 C42 C43 C44 8.6(6) . . . . ?
O42 C42 C43 C51 18.7(7) . . . . ?
O41 C42 C43 C51 -164.0(4) . . . . ?
Tm1 O43 C44 C43 -4.0(6) . . . . ?
Tm1 O43 C44 C45 178.5(2) . . . . ?
C51 C43 C44 O43 -17.2(6) . . . . ?
C42 C43 C44 O43 170.2(4) . . . . ?
C51 C43 C44 C45 160.4(3) . . . . ?
C42 C43 C44 C45 -12.2(6) . . . . ?
O43 C44 C45 C50 -175.4(4) . . . . ?
C43 C44 C45 C50 6.9(6) . . . . ?
O43 C44 C45 C46 8.5(6) . . . . ?
C43 C44 C45 C46 -169.2(4) . . . . ?
C50 C45 C46 C47 1.0(6) . . . . ?
C44 C45 C46 C47 177.1(4) . . . . ?
C45 C46 C47 C48 -0.1(7) . . . . ?
C46 C47 C48 C49 -0.1(7) . . . . ?
C47 C48 C49 C50 -0.5(8) . . . . ?
C42 O41 C50 C49 173.8(4) . . . . ?
C42 O41 C50 C45 -6.4(6) . . . . ?
C48 C49 C50 O41 -178.7(4) . . . . ?
C48 C49 C50 C45 1.4(7) . . . . ?
C46 C45 C50 O41 178.5(4) . . . . ?
C44 C45 C50 O41 2.3(6) . . . . ?
C46 C45 C50 C49 -1.7(6) . . . . ?
C44 C45 C50 C49 -177.8(4) . . . . ?
Tm1 O44 C51 C43 27.2(6) . . . . ?
Tm1 O44 C51 C52 -156.9(3) . . . . ?
C44 C43 C51 O44 6.3(6) . . . . ?
C42 C43 C51 O44 179.0(4) . . . . ?
C44 C43 C51 C52 -169.3(4) . . . . ?
C42 C43 C51 C52 3.3(6) . . . . ?
C72 N1 C61 C62 0.1(5) . . . . ?
Tm1 N1 C61 C62 -169.1(3) . . . . ?
N1 C61 C62 C63 0.8(6) . . . . ?
C61 C62 C63 C64 -1.7(5) . . . . ?
C61 C62 C63 C73 179.7(3) . . . . ?
C62 C63 C64 C72 1.7(5) . . . . ?
C73 C63 C64 C72 -179.7(3) . . . . ?
C62 C63 C64 C65 -176.7(4) . . . . ?
C73 C63 C64 C65 1.9(5) . . . . ?
C72 C64 C65 C66 0.6(5) . . . . ?
C63 C64 C65 C66 179.0(4) . . . . ?
C64 C65 C66 C67 -0.2(6) . . . . ?
C65 C66 C67 C71 0.4(5) . . . . ?
C65 C66 C67 C68 -179.1(4) . . . . ?
C71 C67 C68 C69 0.4(5) . . . . ?
C66 C67 C68 C69 179.9(4) . . . . ?
C71 C67 C68 C79 -178.1(4) . . . . ?
C66 C67 C68 C79 1.4(6) . . . . ?
C67 C68 C69 C70 1.2(6) . . . . ?
C79 C68 C69 C70 179.7(4) . . . . ?
C71 N2 C70 C69 -0.3(6) . . . . ?
Tm1 N2 C70 C69 173.8(3) . . . . ?
C68 C69 C70 N2 -1.4(6) . . . . ?
C70 N2 C71 C67 2.0(5) . . . . ?
Tm1 N2 C71 C67 -172.3(2) . . . . ?
C70 N2 C71 C72 -178.7(3) . . . . ?
Tm1 N2 C71 C72 7.0(4) . . . . ?
C68 C67 C71 N2 -2.1(5) . . . . ?
C66 C67 C71 N2 178.4(3) . . . . ?
C68 C67 C71 C72 178.6(3) . . . . ?
C66 C67 C71 C72 -0.9(5) . . . . ?
C61 N1 C72 C64 0.0(5) . . . . ?
Tm1 N1 C72 C64 169.7(2) . . . . ?
C61 N1 C72 C71 178.7(3) . . . . ?
Tm1 N1 C72 C71 -11.6(4) . . . . ?
C65 C64 C72 N1 177.6(3) . . . . ?
C63 C64 C72 N1 -0.9(5) . . . . ?
C65 C64 C72 C71 -1.1(5) . . . . ?
C63 C64 C72 C71 -179.6(3) . . . . ?
N2 C71 C72 N1 3.2(5) . . . . ?
C67 C71 C72 N1 -177.5(3) . . . . ?
N2 C71 C72 C64 -178.1(3) . . . . ?
C67 C71 C72 C64 1.3(5) . . . . ?
C62 C63 C73 C78 -123.2(4) . . . . ?
C64 C63 C73 C78 58.2(5) . . . . ?
C62 C63 C73 C74 54.5(5) . . . . ?
C64 C63 C73 C74 -124.0(4) . . . . ?
C78 C73 C74 C75 -1.9(6) . . . . ?
C63 C73 C74 C75 -179.8(4) . . . . ?
C73 C74 C75 C76 1.4(8) . . . . ?
C74 C75 C76 C77 0.0(8) . . . . ?
C75 C76 C77 C78 -0.8(8) . . . . ?
C74 C73 C78 C77 1.2(7) . . . . ?
C63 C73 C78 C77 178.9(4) . . . . ?
C76 C77 C78 C73 0.2(7) . . . . ?
C69 C68 C79 C84 -76.4(6) . . . . ?
C67 C68 C79 C84 102.0(5) . . . . ?
C69 C68 C79 C80 105.0(5) . . . . ?
C67 C68 C79 C80 -76.6(5) . . . . ?
C84 C79 C80 C81 -1.8(9) . . . . ?
C68 C79 C80 C81 176.9(6) . . . . ?
C79 C80 C81 C82 0.3(13) . . . . ?
C80 C81 C82 C83 0.7(17) . . . . ?
C81 C82 C83 C84 -0.3(17) . . . . ?
C80 C79 C84 C83 2.2(9) . . . . ?
C68 C79 C84 C83 -176.5(6) . . . . ?
C82 C83 C84 C79 -1.1(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C61 H61 O24 0.93 2.39 3.041(4) 126.6 . yes
C70 H70 O3 0.93 2.43 3.005(5) 119.7 . yes

_refine_diff_density_max         1.227
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.074





_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
