# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

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

data_mo_d8v5281_0m
_database_code_depnum_ccdc_archive 'CCDC 2291807'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_mo_d8v5281_0m       
;
PROBLEM: D-H Bond Without Acceptor  O11      --H11B     .     Please Check
RESPONSE: A result of disordered water molecules. A hydrogen bond could not be generated without creating more serious alert
;
# Added during the CSD deposition process: Tuesday 23 April 2024 08:51 AM
# end Validation Reply Form

_audit_creation_date             2024-04-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H28 Eu N4 Na O10, 3(H2 O)'
_chemical_formula_sum            'C16 H34 Eu N4 Na O13'
_chemical_formula_weight         665.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.6270(5)
_cell_length_b                   9.1258(6)
_cell_length_c                   15.6209(9)
_cell_angle_alpha                82.982(2)
_cell_angle_beta                 85.085(2)
_cell_angle_gamma                81.209(3)
_cell_volume                     1203.44(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   0.855
_shelx_estimated_absorpt_T_min   0.608
_exptl_absorpt_coefficient_mu    2.696
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1158 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.8610.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0530
0.00 0.00 -1.00 0.0670
0.00 -1.00 0.00 0.0890
0.00 1.00 0.00 0.0880
-1.00 0.00 0.00 0.0280
1.00 0.00 0.00 0.0300

_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.272
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6502
_reflns_number_total             7345
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7345
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0250
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+0.6940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0488
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9D
 0.85 with sigma of 0.02
 O11-H11B
 0.85 with sigma of 0.0002
3.a Free rotating group:
 O9(H9C), O5(H5A), O3(H3C,H3D)
3.b Rotating group:
 O10(H10A,H10B)
3.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10C,H10D), C12(H12A,H12B), C2(H2A,
 H2B), C9(H9A,H9B), C11(H11C,H11D), C3(H3A,H3B), C13(H13A,H13B), C7(H7A,H7B),
 C15(H15A,H15B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.40872(2) 0.74956(2) 0.19292(2) 0.00596(3) Uani 1 1 d . . . . .
Na1 Na 0.63079(10) 0.17571(10) 0.10004(5) 0.01333(18) Uani 1 1 d . . . . .
O1 O 0.19468(17) 1.01768(17) -0.03671(9) 0.0106(3) Uani 1 1 d . . . . .
O4 O 0.39645(18) 0.33027(17) 0.07363(10) 0.0124(3) Uani 1 1 d . . . . .
O6 O 0.75955(18) 0.53018(18) 0.37941(10) 0.0141(3) Uani 1 1 d . . . . .
O8 O 0.46410(17) 0.51619(16) 0.13552(9) 0.0098(3) Uani 1 1 d . . . . .
O10 O 0.64081(17) 0.74427(17) 0.08958(9) 0.0109(3) Uani 1 1 d . . . . .
H10A H 0.617205 0.721361 0.041653 0.016 Uiso 1 1 d R U . . .
H10B H 0.664505 0.831966 0.077817 0.016 Uiso 1 1 d R U . . .
O12 O 0.31315(17) 0.83853(17) 0.05453(9) 0.0102(3) Uani 1 1 d . . . . .
O13 O 0.63196(17) 0.67148(17) 0.27403(9) 0.0109(3) Uani 1 1 d . . . . .
O7 O 0.49273(17) 0.98548(17) 0.19055(9) 0.0102(3) Uani 1 1 d . . . . .
O2 O 0.61515(19) 1.13353(18) 0.25579(10) 0.0146(3) Uani 1 1 d . . . . .
O9 O 1.0249(2) 0.7183(2) 0.57791(11) 0.0192(4) Uani 1 1 d DG . . . .
H9C H 1.096502 0.644222 0.587208 0.029 Uiso 1 1 d G U . . .
O5 O 1.2063(2) 0.9282(2) 0.59861(12) 0.0213(4) Uani 1 1 d G . . . .
H5A H 1.181838 1.022351 0.589543 0.032 Uiso 1 1 d G U . . .
O11 O 0.7747(2) 0.3737(2) 0.11682(14) 0.0274(4) Uani 1 1 d D . . . .
N1 N 0.1553(2) 0.62199(19) 0.17900(11) 0.0079(3) Uani 1 1 d . . . . .
N4 N 0.1489(2) 0.94599(19) 0.19757(11) 0.0084(3) Uani 1 1 d . . . . .
N2 N 0.3543(2) 0.8657(2) 0.34443(11) 0.0086(3) Uani 1 1 d . . . . .
N3 N 0.3632(2) 0.5446(2) 0.32438(11) 0.0083(3) Uani 1 1 d . . . . .
O3 O 0.8735(3) 0.7692(2) 0.42958(13) 0.0292(4) Uani 1 1 d G . . . .
H3C H 0.899909 0.739987 0.480711 0.044 Uiso 1 1 d G U . . .
H3D H 0.823806 0.701856 0.417012 0.044 Uiso 1 1 d G U . . .
C1 C 0.3643(2) 0.4509(2) 0.10511(13) 0.0089(4) Uani 1 1 d . . . . .
C4 C 0.1486(3) 1.0433(2) 0.26737(13) 0.0105(4) Uani 1 1 d . . . . .
H4A H 0.042147 1.100047 0.276114 0.013 Uiso 1 1 calc R U . . .
H4B H 0.222663 1.115932 0.249415 0.013 Uiso 1 1 calc R U . . .
C6 C 0.2597(2) 0.4414(2) 0.30217(14) 0.0099(4) Uani 1 1 d . . . . .
H6A H 0.225753 0.380647 0.355403 0.012 Uiso 1 1 calc R U . . .
H6B H 0.319225 0.372870 0.262569 0.012 Uiso 1 1 calc R U . . .
C8 C 0.0180(2) 0.7376(2) 0.15899(14) 0.0100(4) Uani 1 1 d . . . . .
H8A H -0.079823 0.692026 0.170527 0.012 Uiso 1 1 calc R U . . .
H8B H 0.026597 0.775433 0.096871 0.012 Uiso 1 1 calc R U . . .
C10 C 0.1447(2) 1.0404(2) 0.11352(13) 0.0097(4) Uani 1 1 d . . . . .
H10C H 0.198944 1.127262 0.117222 0.012 Uiso 1 1 calc R U . . .
H10D H 0.033858 1.078639 0.102192 0.012 Uiso 1 1 calc R U . . .
C12 C 0.1956(2) 0.5293(2) 0.10674(13) 0.0106(4) Uani 1 1 d . . . . .
H12A H 0.179263 0.593350 0.051453 0.013 Uiso 1 1 calc R U . . .
H12B H 0.123676 0.453470 0.111604 0.013 Uiso 1 1 calc R U . . .
C14 C 0.6474(2) 0.5614(2) 0.33193(13) 0.0091(4) Uani 1 1 d . . . . .
C16 C 0.2210(2) 0.9591(2) 0.03825(13) 0.0084(4) Uani 1 1 d . . . . .
C2 C 0.1156(2) 0.5261(2) 0.25930(13) 0.0109(4) Uani 1 1 d . . . . .
H2A H 0.049806 0.453576 0.245314 0.013 Uiso 1 1 calc R U . . .
H2B H 0.052774 0.589247 0.300717 0.013 Uiso 1 1 calc R U . . .
C9 C 0.2927(3) 0.6143(2) 0.40260(13) 0.0109(4) Uani 1 1 d . . . . .
H9A H 0.302720 0.538370 0.453571 0.013 Uiso 1 1 calc R U . . .
H9B H 0.179238 0.647532 0.395953 0.013 Uiso 1 1 calc R U . . .
C5 C 0.5311(2) 1.0339(2) 0.25778(13) 0.0098(4) Uani 1 1 d . . . . .
C11 C 0.1953(2) 0.9540(2) 0.35199(13) 0.0109(4) Uani 1 1 d . . . . .
H11C H 0.192787 1.023040 0.396437 0.013 Uiso 1 1 calc R U . . .
H11D H 0.117509 0.885498 0.371535 0.013 Uiso 1 1 calc R U . . .
C3 C 0.3687(3) 0.7460(2) 0.41885(13) 0.0103(4) Uani 1 1 d . . . . .
H3A H 0.317899 0.786741 0.471912 0.012 Uiso 1 1 calc R U . . .
H3B H 0.481259 0.712667 0.428199 0.012 Uiso 1 1 calc R U . . .
C13 C 0.5202(2) 0.4601(2) 0.34244(14) 0.0110(4) Uani 1 1 d . . . . .
H13A H 0.547634 0.382374 0.302483 0.013 Uiso 1 1 calc R U . . .
H13B H 0.516167 0.409528 0.402213 0.013 Uiso 1 1 calc R U . . .
C7 C 0.4762(3) 0.9616(2) 0.34603(13) 0.0113(4) Uani 1 1 d . . . . .
H7A H 0.568264 0.901065 0.373060 0.014 Uiso 1 1 calc R U . . .
H7B H 0.435147 1.041332 0.383124 0.014 Uiso 1 1 calc R U . . .
C15 C 0.0087(2) 0.8667(2) 0.21269(14) 0.0105(4) Uani 1 1 d . . . . .
H15A H -0.086351 0.938744 0.199117 0.013 Uiso 1 1 calc R U . . .
H15B H -0.002861 0.828554 0.274674 0.013 Uiso 1 1 calc R U . . .
H9D H 1.069(4) 0.790(3) 0.583(2) 0.045(11) Uiso 1 1 d D . . . .
H5B H 1.250(4) 0.908(4) 0.637(2) 0.044(11) Uiso 1 1 d . . . . .
H11A H 0.698(5) 0.437(5) 0.122(2) 0.060(12) Uiso 1 1 d . . . . .
H11B H 0.8133(15) 0.350(4) 0.1657(4) 0.094(18) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O8 2.3770(14) . ?
Eu1 O10 2.4603(14) . ?
Eu1 O12 2.3843(14) . ?
Eu1 O13 2.3664(15) . ?
Eu1 O7 2.3696(15) . ?
Eu1 N1 2.6653(17) . ?
Eu1 N4 2.6491(17) . ?
Eu1 N2 2.6863(17) . ?
Eu1 N3 2.6491(17) . ?
Na1 O1 2.3916(17) 2_665 ?
Na1 O4 2.3186(17) . ?
Na1 O12 2.4368(16) 2_665 ?
Na1 O7 2.4849(17) 1_545 ?
Na1 O2 2.4116(17) 1_545 ?
Na1 O11 2.394(2) . ?
Na1 C16 2.740(2) 2_665 ?
Na1 C5 2.772(2) 1_545 ?
Na1 H11A 2.61(4) . ?
O1 C16 1.251(2) . ?
O4 C1 1.244(3) . ?
O6 C14 1.247(3) . ?
O8 C1 1.272(2) . ?
O10 H10A 0.8503 . ?
O10 H10B 0.8507 . ?
O12 C16 1.267(3) . ?
O13 C14 1.266(3) . ?
O7 C5 1.275(2) . ?
O2 C5 1.243(3) . ?
O9 H9C 0.8505 . ?
O9 H9D 0.820(18) . ?
O5 H5A 0.8499 . ?
O5 H5B 0.72(4) . ?
O11 H11A 0.82(4) . ?
O11 H11B 0.8500(2) . ?
N1 C8 1.488(3) . ?
N1 C12 1.479(3) . ?
N1 C2 1.485(3) . ?
N4 C4 1.487(3) . ?
N4 C10 1.480(3) . ?
N4 C15 1.490(3) . ?
N2 C11 1.484(3) . ?
N2 C3 1.494(3) . ?
N2 C7 1.471(3) . ?
N3 C6 1.481(3) . ?
N3 C9 1.487(3) . ?
N3 C13 1.484(3) . ?
O3 H3C 0.8495 . ?
O3 H3D 0.8511 . ?
C1 C12 1.519(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C11 1.517(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C2 1.521(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C15 1.516(3) . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 C16 1.516(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C13 1.526(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C3 1.511(3) . ?
C5 C7 1.524(3) . ?
C11 H11C 0.9900 . ?
C11 H11D 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?

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
O8 Eu1 O10 69.41(5) . . ?
O8 Eu1 O12 84.01(5) . . ?
O8 Eu1 N1 65.77(5) . . ?
O8 Eu1 N4 131.02(5) . . ?
O8 Eu1 N2 141.16(5) . . ?
O8 Eu1 N3 74.05(5) . . ?
O10 Eu1 N1 125.57(5) . . ?
O10 Eu1 N4 129.64(5) . . ?
O10 Eu1 N2 129.87(5) . . ?
O10 Eu1 N3 125.85(5) . . ?
O12 Eu1 O10 73.66(5) . . ?
O12 Eu1 N1 72.52(5) . . ?
O12 Eu1 N4 65.83(5) . . ?
O12 Eu1 N2 130.81(5) . . ?
O12 Eu1 N3 139.77(5) . . ?
O13 Eu1 O8 87.20(5) . . ?
O13 Eu1 O10 73.06(5) . . ?
O13 Eu1 O12 146.58(5) . . ?
O13 Eu1 O7 82.02(5) . . ?
O13 Eu1 N1 131.70(5) . . ?
O13 Eu1 N4 138.43(5) . . ?
O13 Eu1 N2 71.67(5) . . ?
O13 Eu1 N3 66.51(5) . . ?
O7 Eu1 O8 144.19(5) . . ?
O7 Eu1 O10 74.79(5) . . ?
O7 Eu1 O12 86.49(5) . . ?
O7 Eu1 N1 142.19(5) . . ?
O7 Eu1 N4 74.13(5) . . ?
O7 Eu1 N2 66.06(5) . . ?
O7 Eu1 N3 130.14(5) . . ?
N1 Eu1 N2 104.49(5) . . ?
N4 Eu1 N1 68.68(5) . . ?
N4 Eu1 N2 67.67(5) . . ?
N4 Eu1 N3 104.48(5) . . ?
N3 Eu1 N1 67.83(5) . . ?
N3 Eu1 N2 67.75(5) . . ?
O1 Na1 O12 54.67(5) 2_665 2_665 ?
O1 Na1 O7 90.18(6) 2_665 1_545 ?
O1 Na1 O2 111.73(6) 2_665 1_545 ?
O1 Na1 O11 108.79(7) 2_665 . ?
O1 Na1 C16 27.13(6) 2_665 2_665 ?
O1 Na1 C5 103.06(6) 2_665 1_545 ?
O1 Na1 H11A 125.8(9) 2_665 . ?
O4 Na1 O1 139.53(6) . 2_665 ?
O4 Na1 O12 90.29(6) . 2_665 ?
O4 Na1 O7 92.15(6) . 1_545 ?
O4 Na1 O2 102.00(6) . 1_545 ?
O4 Na1 O11 95.12(7) . . ?
O4 Na1 C16 115.68(7) . 2_665 ?
O4 Na1 C5 97.11(6) . 1_545 ?
O4 Na1 H11A 77.6(9) . . ?
O12 Na1 O7 120.51(6) 2_665 1_545 ?
O12 Na1 C16 27.54(6) 2_665 2_665 ?
O12 Na1 C5 146.81(7) 2_665 1_545 ?
O12 Na1 H11A 103.7(8) 2_665 . ?
O7 Na1 C16 106.51(6) 1_545 2_665 ?
O7 Na1 C5 27.38(5) 1_545 1_545 ?
O7 Na1 H11A 134.8(8) 1_545 . ?
O2 Na1 O12 166.38(7) 1_545 2_665 ?
O2 Na1 O7 53.94(5) 1_545 1_545 ?
O2 Na1 C16 138.86(7) 1_545 2_665 ?
O2 Na1 C5 26.59(6) 1_545 1_545 ?
O2 Na1 H11A 84.9(8) 1_545 . ?
O11 Na1 O12 99.29(7) . 2_665 ?
O11 Na1 O7 139.49(7) . 1_545 ?
O11 Na1 O2 85.58(7) . 1_545 ?
O11 Na1 C16 105.92(7) . 2_665 ?
O11 Na1 C5 112.11(7) . 1_545 ?
O11 Na1 H11A 18.1(9) . . ?
C16 Na1 C5 126.52(7) 2_665 1_545 ?
C16 Na1 H11A 117.7(8) 2_665 . ?
C5 Na1 H11A 109.5(8) 1_545 . ?
C16 O1 Na1 92.16(12) . 2_665 ?
C1 O4 Na1 120.54(14) . . ?
C1 O8 Eu1 125.49(13) . . ?
Eu1 O10 H10A 109.4 . . ?
Eu1 O10 H10B 109.4 . . ?
H10A O10 H10B 104.5 . . ?
Eu1 O12 Na1 143.45(7) . 2_665 ?
C16 O12 Eu1 124.48(13) . . ?
C16 O12 Na1 89.68(12) . 2_665 ?
C14 O13 Eu1 125.46(13) . . ?
Eu1 O7 Na1 144.04(7) . 1_565 ?
C5 O7 Eu1 123.07(13) . . ?
C5 O7 Na1 88.95(12) . 1_565 ?
C5 O2 Na1 93.09(13) . 1_565 ?
H9C O9 H9D 103.4 . . ?
H5A O5 H5B 110.8 . . ?
Na1 O11 H11A 96(3) . . ?
Na1 O11 H11B 105(3) . . ?
H11A O11 H11B 109(3) . . ?
C8 N1 Eu1 110.44(12) . . ?
C12 N1 Eu1 105.88(12) . . ?
C12 N1 C8 109.94(16) . . ?
C12 N1 C2 109.56(16) . . ?
C2 N1 Eu1 111.70(12) . . ?
C2 N1 C8 109.27(16) . . ?
C4 N4 Eu1 110.97(12) . . ?
C4 N4 C15 109.20(16) . . ?
C10 N4 Eu1 107.77(12) . . ?
C10 N4 C4 108.62(16) . . ?
C10 N4 C15 110.40(16) . . ?
C15 N4 Eu1 109.86(12) . . ?
C11 N2 Eu1 111.54(12) . . ?
C11 N2 C3 108.55(16) . . ?
C3 N2 Eu1 111.13(12) . . ?
C7 N2 Eu1 105.69(12) . . ?
C7 N2 C11 110.57(17) . . ?
C7 N2 C3 109.34(16) . . ?
C6 N3 Eu1 111.03(12) . . ?
C6 N3 C9 109.12(16) . . ?
C6 N3 C13 109.49(16) . . ?
C9 N3 Eu1 111.22(12) . . ?
C13 N3 Eu1 106.55(12) . . ?
C13 N3 C9 109.38(16) . . ?
H3C O3 H3D 104.5 . . ?
O4 C1 O8 124.44(19) . . ?
O4 C1 C12 118.90(18) . . ?
O8 C1 C12 116.65(18) . . ?
N4 C4 H4A 109.2 . . ?
N4 C4 H4B 109.2 . . ?
N4 C4 C11 111.94(17) . . ?
H4A C4 H4B 107.9 . . ?
C11 C4 H4A 109.2 . . ?
C11 C4 H4B 109.2 . . ?
N3 C6 H6A 109.4 . . ?
N3 C6 H6B 109.4 . . ?
N3 C6 C2 111.37(17) . . ?
H6A C6 H6B 108.0 . . ?
C2 C6 H6A 109.4 . . ?
C2 C6 H6B 109.4 . . ?
N1 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
N1 C8 C15 111.57(17) . . ?
H8A C8 H8B 108.0 . . ?
C15 C8 H8A 109.3 . . ?
C15 C8 H8B 109.3 . . ?
N4 C10 H10C 108.9 . . ?
N4 C10 H10D 108.9 . . ?
N4 C10 C16 113.57(17) . . ?
H10C C10 H10D 107.7 . . ?
C16 C10 H10C 108.9 . . ?
C16 C10 H10D 108.9 . . ?
N1 C12 C1 112.88(17) . . ?
N1 C12 H12A 109.0 . . ?
N1 C12 H12B 109.0 . . ?
C1 C12 H12A 109.0 . . ?
C1 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O6 C14 Eu1 160.00(16) . . ?
O6 C14 O13 124.5(2) . . ?
O6 C14 C13 118.60(19) . . ?
O13 C14 Eu1 36.14(10) . . ?
O13 C14 C13 116.93(18) . . ?
C13 C14 Eu1 81.07(11) . . ?
O1 C16 Na1 60.71(11) . 2_665 ?
O1 C16 O12 123.48(19) . . ?
O1 C16 C10 118.21(18) . . ?
O12 C16 Na1 62.78(10) . 2_665 ?
O12 C16 C10 118.24(18) . . ?
C10 C16 Na1 176.84(15) . 2_665 ?
N1 C2 C6 113.18(16) . . ?
N1 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
C6 C2 H2A 108.9 . . ?
C6 C2 H2B 108.9 . . ?
H2A C2 H2B 107.8 . . ?
N3 C9 H9A 109.0 . . ?
N3 C9 H9B 109.0 . . ?
N3 C9 C3 113.13(17) . . ?
H9A C9 H9B 107.8 . . ?
C3 C9 H9A 109.0 . . ?
C3 C9 H9B 109.0 . . ?
Na1 C5 Eu1 99.92(6) 1_565 . ?
O7 C5 Eu1 37.72(10) . . ?
O7 C5 Na1 63.67(11) . 1_565 ?
O7 C5 C7 118.29(19) . . ?
O2 C5 Eu1 156.19(15) . . ?
O2 C5 Na1 60.31(11) . 1_565 ?
O2 C5 O7 123.89(19) . . ?
O2 C5 C7 117.78(18) . . ?
C7 C5 Eu1 82.21(12) . . ?
C7 C5 Na1 177.76(15) . 1_565 ?
N2 C11 C4 112.61(16) . . ?
N2 C11 H11C 109.1 . . ?
N2 C11 H11D 109.1 . . ?
C4 C11 H11C 109.1 . . ?
C4 C11 H11D 109.1 . . ?
H11C C11 H11D 107.8 . . ?
N2 C3 C9 111.24(17) . . ?
N2 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
C9 C3 H3A 109.4 . . ?
C9 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N3 C13 C14 111.89(17) . . ?
N3 C13 H13A 109.2 . . ?
N3 C13 H13B 109.2 . . ?
C14 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
N2 C7 C5 114.84(17) . . ?
N2 C7 H7A 108.6 . . ?
N2 C7 H7B 108.6 . . ?
C5 C7 H7A 108.6 . . ?
C5 C7 H7B 108.6 . . ?
H7A C7 H7B 107.5 . . ?
N4 C15 C8 113.33(16) . . ?
N4 C15 H15A 108.9 . . ?
N4 C15 H15B 108.9 . . ?
C8 C15 H15A 108.9 . . ?
C8 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?

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
Eu1 O8 C1 O4 178.35(15) . . . . ?
Eu1 O8 C1 C12 -0.6(3) . . . . ?
Eu1 O12 C16 Na1 166.13(14) . . . 2_665 ?
Eu1 O12 C16 O1 166.50(15) . . . . ?
Eu1 O12 C16 C10 -10.5(3) . . . . ?
Eu1 O13 C14 O6 -173.09(15) . . . . ?
Eu1 O13 C14 C13 7.8(2) . . . . ?
Eu1 O7 C5 Na1 162.57(14) . . . 1_565 ?
Eu1 O7 C5 O2 158.92(16) . . . . ?
Eu1 O7 C5 C7 -18.7(3) . . . . ?
Eu1 N1 C8 C15 -42.83(19) . . . . ?
Eu1 N1 C12 C1 38.90(19) . . . . ?
Eu1 N1 C2 C6 -37.7(2) . . . . ?
Eu1 N4 C4 C11 -46.74(19) . . . . ?
Eu1 N4 C10 C16 31.75(19) . . . . ?
Eu1 N4 C15 C8 -43.88(19) . . . . ?
Eu1 N2 C11 C4 -38.5(2) . . . . ?
Eu1 N2 C3 C9 -42.05(19) . . . . ?
Eu1 N2 C7 C5 31.2(2) . . . . ?
Eu1 N3 C6 C2 -46.73(18) . . . . ?
Eu1 N3 C9 C3 -44.1(2) . . . . ?
Eu1 N3 C13 C14 38.14(18) . . . . ?
Eu1 C14 C13 N3 -29.06(14) . . . . ?
Eu1 C5 C7 N2 -24.65(16) . . . . ?
Na1 O1 C16 O12 -0.4(2) 2_665 . . . ?
Na1 O1 C16 C10 176.61(16) 2_665 . . . ?
Na1 O4 C1 O8 17.0(3) . . . . ?
Na1 O4 C1 C12 -164.12(14) . . . . ?
Na1 O12 C16 O1 0.4(2) 2_665 . . . ?
Na1 O12 C16 C10 -176.61(17) 2_665 . . . ?
Na1 O7 C5 Eu1 -162.57(13) 1_565 . . . ?
Na1 O7 C5 O2 -3.7(2) 1_565 . . . ?
Na1 O7 C5 C7 178.78(17) 1_565 . . . ?
Na1 O2 C5 Eu1 36.8(4) 1_565 . . . ?
Na1 O2 C5 O7 3.8(2) 1_565 . . . ?
Na1 O2 C5 C7 -178.66(16) 1_565 . . . ?
O4 C1 C12 N1 151.55(19) . . . . ?
O6 C14 C13 N3 147.14(18) . . . . ?
O8 C1 C12 N1 -29.5(3) . . . . ?
O13 C14 C13 N3 -33.7(2) . . . . ?
O7 C5 C7 N2 -13.3(3) . . . . ?
O2 C5 C7 N2 169.03(18) . . . . ?
N1 C8 C15 N4 60.9(2) . . . . ?
N4 C4 C11 N2 59.1(2) . . . . ?
N4 C10 C16 O1 165.01(18) . . . . ?
N4 C10 C16 O12 -17.9(3) . . . . ?
N3 C6 C2 N1 58.5(2) . . . . ?
N3 C9 C3 N2 59.8(2) . . . . ?
C4 N4 C10 C16 152.06(17) . . . . ?
C4 N4 C15 C8 -165.80(17) . . . . ?
C6 N3 C9 C3 -166.95(17) . . . . ?
C6 N3 C13 C14 158.30(16) . . . . ?
C8 N1 C12 C1 158.20(17) . . . . ?
C8 N1 C2 C6 -160.20(17) . . . . ?
C10 N4 C4 C11 -165.04(17) . . . . ?
C10 N4 C15 C8 74.8(2) . . . . ?
C12 N1 C8 C15 -159.30(17) . . . . ?
C12 N1 C2 C6 79.3(2) . . . . ?
C2 N1 C8 C15 80.4(2) . . . . ?
C2 N1 C12 C1 -81.7(2) . . . . ?
C9 N3 C6 C2 76.2(2) . . . . ?
C9 N3 C13 C14 -82.2(2) . . . . ?
C11 N2 C3 C9 81.0(2) . . . . ?
C11 N2 C7 C5 -89.6(2) . . . . ?
C3 N2 C11 C4 -161.29(17) . . . . ?
C3 N2 C7 C5 150.93(17) . . . . ?
C13 N3 C6 C2 -164.11(17) . . . . ?
C13 N3 C9 C3 73.3(2) . . . . ?
C7 N2 C11 C4 78.8(2) . . . . ?
C7 N2 C3 C9 -158.34(17) . . . . ?
C15 N4 C4 C11 74.5(2) . . . . ?
C15 N4 C10 C16 -88.2(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_mo_d8v5508_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2291817'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_mo_d8v5508_0m_a     
;
PROBLEM: Check Calcd Resid. Dens.  1.71Ang From O1             -3.60 eA-3
RESPONSE: Different atom types have been considered, however this was the only resonable solution creating a neutrally charged compound with the known ligand - and charge of the ligand. The structure contains a lot of solvent molecules, which behave disordered.
;
_vrf_PLAT975_mo_d8v5508_0m_a     
;
PROBLEM: Check Calcd Resid. Dens.  0.59Ang From O6      .       2.49 eA-3
RESPONSE: Different atom types have been considered, however this was the only resonable solution creating a neutrally charged compound with the known ligand - and charge of the ligand. The structure contains a lot of solvent molecules, which behave disordered.
;
_vrf_PLAT934_mo_d8v5508_0m_a     
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          6 Check
RESPONSE: Disordered solvent
;
# Added during the CSD deposition process: Tuesday 23 April 2024 09:06 AM
# end Validation Reply Form

_audit_creation_date             2024-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H27 Eu Na3 O23'
_chemical_formula_sum            'C12 H27 Eu Na3 O23'
_chemical_formula_weight         760.26
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   17.520(3)
_cell_length_b                   8.3804(13)
_cell_length_c                   19.059(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.350(4)
_cell_angle_gamma                90
_cell_volume                     2606.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.687
_cell_measurement_theta_min      2.497
_shelx_estimated_absorpt_T_max   0.766
_shelx_estimated_absorpt_T_min   0.656
_exptl_absorpt_coefficient_mu    2.556
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1266 before and 0.0762 after correction.
The Ratio of minimum to maximum transmission is 0.7864.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1516
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 0.00 0.0610
-1.00 0.00 0.00 0.0550
0.00 0.00 1.00 0.0520
0.00 0.00 -1.00 0.0550
0.00 -1.00 0.00 0.0580
0.00 1.00 0.00 0.0900

_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29301
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.506
_diffrn_reflns_theta_min         2.295
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4239
_reflns_number_total             4349
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.579
_refine_diff_density_min         -3.369
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.00117(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.363
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4349
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+41.3327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1088
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(O3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(O3B)=Sof(H3BA)=Sof(H3BB)=FVAR(1)
 Fixed Sof: H9B(0.5) Na2(0.5)
4.a Rotating group:
 O14(H14A,H14B), O2(H2A), O9(H9A,H9B), O3B(H3BA,H3BB), O3A(H3AA,H3AB)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.500000 0.44560(3) 0.750000 0.00822(9) Uani 1 2 d S T P . .
Na1 Na 0.72001(11) 0.4494(3) 0.53139(10) 0.0208(4) Uani 1 1 d . . . . .
O1 O 0.5615(2) 0.6411(4) 0.8455(2) 0.0219(7) Uani 1 1 d . . . . .
O4 O 0.54518(19) 0.3618(4) 0.65200(17) 0.0178(6) Uani 1 1 d . . . . .
O6 O 1.000000 0.6496(6) 0.750000 0.0217(9) Uani 1 2 d S T P . .
O8 O 0.62000(19) 0.5953(4) 0.74117(19) 0.0179(6) Uani 1 1 d . . . . .
O10 O 0.6766(3) 0.7425(4) 0.9276(2) 0.0311(9) Uani 1 1 d . . . . .
O12 O 0.8772(2) 0.8181(5) 0.6691(2) 0.0231(7) Uani 1 1 d . . . . .
O14 O 0.6110(2) 0.6515(5) 0.4869(2) 0.0250(7) Uani 1 1 d . . . . .
H14A H 0.577181 0.642225 0.510647 0.038 Uiso 1 1 d R U . . .
H14B H 0.580295 0.633624 0.440195 0.038 Uiso 1 1 d R U . . .
O7 O 0.7958(3) 0.6092(7) 0.6277(3) 0.0422(11) Uani 1 1 d . U . . .
O2 O 0.7805(3) 0.5895(6) 0.4546(3) 0.0408(12) Uani 1 1 d . . . . .
H2A H 0.811274 0.673662 0.479426 0.061 Uiso 1 1 d R U . . .
O9 O 0.4986(3) 0.2351(6) 0.4472(2) 0.0343(9) Uani 1 1 d . . . . .
H9A H 0.498041 0.287576 0.407495 0.051 Uiso 1 1 d R U . . .
H9B H 0.471532 0.148729 0.429620 0.051 Uiso 0.5 1 d R U P . .
O5 O 0.6361(3) 0.3532(6) 0.5950(2) 0.0350(10) Uani 1 1 d . . . . .
C1 C 0.6744(3) 0.6730(6) 0.8066(3) 0.0240(9) Uani 1 1 d . . . . .
H1A H 0.688118 0.780421 0.793076 0.029 Uiso 1 1 calc R U . . .
H1B H 0.725797 0.611000 0.827758 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6353(3) 0.6879(5) 0.8646(3) 0.0210(9) Uani 1 1 d . . . . .
C6 C 0.8620(3) 0.6723(7) 0.6648(3) 0.0266(11) Uani 1 1 d . . . . .
C3 C 0.6586(3) 0.5388(7) 0.6914(3) 0.0253(10) Uani 1 1 d . . . . .
H3A H 0.713982 0.498297 0.721332 0.030 Uiso 1 1 calc R U . . .
H3B H 0.664602 0.628165 0.659870 0.030 Uiso 1 1 calc R U . . .
C2 C 0.6092(3) 0.4082(6) 0.6417(2) 0.0201(9) Uani 1 1 d . . . . .
C5 C 0.9303(5) 0.5605(7) 0.7077(3) 0.0378(15) Uani 1 1 d . . . . .
H5A H 0.912884 0.492875 0.741749 0.045 Uiso 1 1 calc R U . . .
H5B H 0.943603 0.489896 0.672081 0.045 Uiso 1 1 calc R U . . .
O3B O 0.9226(7) 0.4710(10) 0.3804(5) 0.035(3) Uani 0.52(2) 1 d . . P A 2
H3BA H 0.935339 0.433391 0.340248 0.053 Uiso 0.52(2) 1 d R U P A 2
H3BB H 0.871020 0.431190 0.365037 0.053 Uiso 0.52(2) 1 d R U P A 2
O3A O 0.6274(6) -0.0035(10) 0.6293(5) 0.025(2) Uani 0.48(2) 1 d . . P A 1
H3AA H 0.667832 -0.008746 0.674031 0.037 Uiso 0.48(2) 1 d R U P A 1
H3AB H 0.589117 -0.068585 0.633312 0.037 Uiso 0.48(2) 1 d R U P A 1
Na2 Na 0.6233(2) 0.1409(5) 0.5301(2) 0.0185(7) Uani 0.5 1 d . . P . .
H2B H 0.805(7) 0.606(14) 0.415(6) 0.09(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.393(3) 2_656 ?
Eu1 O1 2.393(3) . ?
Eu1 O4 2.384(3) 2_656 ?
Eu1 O4 2.384(3) . ?
Eu1 O6 2.481(5) 3_445 ?
Eu1 O8 2.506(3) . ?
Eu1 O8 2.506(3) 2_656 ?
Eu1 O12 2.394(3) 3_445 ?
Eu1 O12 2.394(3) 4_646 ?
Na1 Na1 3.824(4) 7_656 ?
Na1 O10 2.446(4) 6_565 ?
Na1 O10 2.423(4) 4_646 ?
Na1 O14 2.461(4) . ?
Na1 O7 2.269(5) . ?
Na1 O2 2.403(5) . ?
Na1 O5 2.363(4) . ?
Na1 Na2 3.438(4) 7_656 ?
Na1 Na2 3.086(4) . ?
O1 C4 1.271(6) . ?
O4 C2 1.268(5) . ?
O6 C5 1.408(6) 2_756 ?
O6 C5 1.408(6) . ?
O8 C1 1.422(6) . ?
O8 C3 1.430(6) . ?
O10 C4 1.242(6) . ?
O10 Na2 2.641(6) 6_566 ?
O12 C6 1.247(7) . ?
O14 H14A 0.8703 . ?
O14 H14B 0.8685 . ?
O7 C6 1.236(6) . ?
O2 H2A 0.9093 . ?
O2 Na2 2.509(6) 7_656 ?
O2 H2B 1.00(12) . ?
O9 H9A 0.8718 . ?
O9 H9B 0.8629 . ?
O9 Na2 2.320(6) . ?
O5 C2 1.237(5) . ?
O5 Na2 2.132(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.501(8) . ?
C6 C5 1.505(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.500(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
O3B H3BA 0.9271 . ?
O3B H3BB 0.9064 . ?
O3B Na2 2.331(9) 7_656 ?
O3A H3AA 0.8888 . ?
O3A H3AB 0.8894 . ?
O3A Na2 2.224(9) . ?
Na2 H9B 2.6526 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O1 93.60(18) 2_656 . ?
O1 Eu1 O6 133.20(9) . 3_445 ?
O1 Eu1 O6 133.20(9) 2_656 3_445 ?
O1 Eu1 O8 63.38(12) 2_656 2_656 ?
O1 Eu1 O8 63.39(12) . . ?
O1 Eu1 O8 76.26(11) 2_656 . ?
O1 Eu1 O8 76.26(11) . 2_656 ?
O1 Eu1 O12 76.46(13) 2_656 3_445 ?
O1 Eu1 O12 147.71(12) 2_656 4_646 ?
O1 Eu1 O12 147.71(12) . 3_445 ?
O1 Eu1 O12 76.46(13) . 4_646 ?
O4 Eu1 O1 77.99(13) 2_656 . ?
O4 Eu1 O1 127.69(12) . . ?
O4 Eu1 O1 77.99(13) . 2_656 ?
O4 Eu1 O1 127.69(12) 2_656 2_656 ?
O4 Eu1 O4 145.73(17) 2_656 . ?
O4 Eu1 O6 72.86(9) 2_656 3_445 ?
O4 Eu1 O6 72.87(9) . 3_445 ?
O4 Eu1 O8 136.55(11) 2_656 . ?
O4 Eu1 O8 136.55(11) . 2_656 ?
O4 Eu1 O8 64.47(11) 2_656 2_656 ?
O4 Eu1 O8 64.47(11) . . ?
O4 Eu1 O12 84.05(12) 2_656 3_445 ?
O4 Eu1 O12 80.83(12) 2_656 4_646 ?
O4 Eu1 O12 84.05(12) . 4_646 ?
O4 Eu1 O12 80.83(12) . 3_445 ?
O6 Eu1 O8 120.05(8) 3_445 2_656 ?
O6 Eu1 O8 120.05(8) 3_445 . ?
O8 Eu1 O8 119.90(16) . 2_656 ?
O12 Eu1 O6 63.48(10) 4_646 3_445 ?
O12 Eu1 O6 63.48(10) 3_445 3_445 ?
O12 Eu1 O8 139.40(12) 4_646 2_656 ?
O12 Eu1 O8 71.81(12) 3_445 2_656 ?
O12 Eu1 O8 71.81(12) 4_646 . ?
O12 Eu1 O8 139.40(12) 3_445 . ?
O12 Eu1 O12 126.97(19) 3_445 4_646 ?
O10 Na1 Na1 38.03(9) 6_565 7_656 ?
O10 Na1 Na1 38.47(10) 4_646 7_656 ?
O10 Na1 O10 76.50(14) 4_646 6_565 ?
O10 Na1 O14 101.52(14) 6_565 . ?
O10 Na1 O14 177.71(16) 4_646 . ?
O10 Na1 Na2 49.96(14) 4_646 7_656 ?
O10 Na1 Na2 68.37(13) 6_565 7_656 ?
O10 Na1 Na2 55.57(14) 6_565 . ?
O10 Na1 Na2 75.32(14) 4_646 . ?
O14 Na1 Na1 139.53(13) . 7_656 ?
O14 Na1 Na2 102.64(13) . . ?
O14 Na1 Na2 130.52(13) . 7_656 ?
O7 Na1 Na1 128.49(18) . 7_656 ?
O7 Na1 O10 90.73(19) . 4_646 ?
O7 Na1 O10 163.79(19) . 6_565 ?
O7 Na1 O14 91.42(19) . . ?
O7 Na1 O2 86.95(18) . . ?
O7 Na1 O5 94.36(17) . . ?
O7 Na1 Na2 95.81(15) . 7_656 ?
O7 Na1 Na2 131.18(16) . . ?
O2 Na1 Na1 90.23(13) . 7_656 ?
O2 Na1 O10 95.90(18) . 4_646 ?
O2 Na1 O10 84.52(16) . 6_565 ?
O2 Na1 O14 85.00(17) . . ?
O2 Na1 Na2 46.84(14) . 7_656 ?
O2 Na1 Na2 140.08(14) . . ?
O5 Na1 Na1 98.95(15) . 7_656 ?
O5 Na1 O10 97.04(18) . 6_565 ?
O5 Na1 O10 96.99(17) . 4_646 ?
O5 Na1 O14 82.06(15) . . ?
O5 Na1 O2 167.02(19) . . ?
O5 Na1 Na2 43.60(14) . . ?
O5 Na1 Na2 145.40(16) . 7_656 ?
Na2 Na1 Na1 49.96(8) 7_656 7_656 ?
Na2 Na1 Na1 58.51(9) . 7_656 ?
Na2 Na1 Na2 108.47(10) . 7_656 ?
C4 O1 Eu1 123.9(3) . . ?
C2 O4 Eu1 126.6(3) . . ?
C5 O6 Eu1 122.0(3) 2_756 3 ?
C5 O6 Eu1 122.0(3) . 3 ?
C5 O6 C5 115.9(6) . 2_756 ?
C1 O8 Eu1 118.7(3) . . ?
C1 O8 C3 114.0(4) . . ?
C3 O8 Eu1 119.3(3) . . ?
Na1 O10 Na1 103.50(14) 4_656 6_566 ?
Na1 O10 Na2 85.41(15) 4_656 6_566 ?
Na1 O10 Na2 74.59(16) 6_566 6_566 ?
C4 O10 Na1 132.9(4) . 4_656 ?
C4 O10 Na1 116.1(3) . 6_566 ?
C4 O10 Na2 127.8(4) . 6_566 ?
C6 O12 Eu1 126.9(3) . 3 ?
Na1 O14 H14A 110.4 . . ?
Na1 O14 H14B 110.4 . . ?
H14A O14 H14B 103.5 . . ?
C6 O7 Na1 149.9(4) . . ?
Na1 O2 H2A 111.8 . . ?
Na1 O2 Na2 88.8(2) . 7_656 ?
Na1 O2 H2B 158(7) . . ?
H2A O2 H2B 87.0 . . ?
Na2 O2 H2A 106.9 7_656 . ?
Na2 O2 H2B 75(7) 7_656 . ?
H9A O9 H9B 104.8 . . ?
Na2 O9 H9A 118.2 . . ?
Na2 O9 H9B 103.1 . . ?
C2 O5 Na1 135.5(4) . . ?
C2 O5 Na2 137.8(4) . . ?
Na2 O5 Na1 86.56(17) . . ?
O8 C1 H1A 109.6 . . ?
O8 C1 H1B 109.6 . . ?
O8 C1 C4 110.1(4) . . ?
H1A C1 H1B 108.2 . . ?
C4 C1 H1A 109.6 . . ?
C4 C1 H1B 109.6 . . ?
O1 C4 C1 116.9(4) . . ?
O10 C4 O1 124.4(5) . . ?
O10 C4 C1 118.7(5) . . ?
O12 C6 C5 117.7(4) . . ?
O7 C6 O12 126.2(6) . . ?
O7 C6 C5 116.1(6) . . ?
O8 C3 H3A 109.4 . . ?
O8 C3 H3B 109.4 . . ?
O8 C3 C2 111.0(4) . . ?
H3A C3 H3B 108.0 . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
O4 C2 C3 117.7(4) . . ?
O5 C2 O4 126.0(5) . . ?
O5 C2 C3 116.3(5) . . ?
O6 C5 C6 109.5(4) . . ?
O6 C5 H5A 109.8 . . ?
O6 C5 H5B 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
H3BA O3B H3BB 96.8 . . ?
Na2 O3B H3BA 135.9 7_656 . ?
Na2 O3B H3BB 61.3 7_656 . ?
H3AA O3A H3BB 84.9 . 7_656 ?
H3AA O3A H3AB 104.5 . . ?
H3AB O3A H3BB 125.2 . 7_656 ?
Na2 O3A H3BB 66(3) . 7_656 ?
Na2 O3A H3AA 127.6 . . ?
Na2 O3A H3AB 127.9 . . ?
Na1 Na2 Na1 71.53(10) . 7_656 ?
Na1 Na2 H9B 118.3 7_656 . ?
Na1 Na2 H9B 112.8 . . ?
Na1 Na2 H3BB 120(2) 7_656 7_656 ?
Na1 Na2 H3BB 114(3) . 7_656 ?
O10 Na2 Na1 44.62(11) 6_565 7_656 ?
O10 Na2 Na1 49.83(11) 6_565 . ?
O10 Na2 H9B 89.3 6_565 . ?
O10 Na2 H3BB 157.4(8) 6_565 7_656 ?
O2 Na2 Na1 107.48(17) 7_656 . ?
O2 Na2 Na1 44.33(13) 7_656 7_656 ?
O2 Na2 O10 88.16(18) 7_656 6_565 ?
O2 Na2 H9B 123.9 7_656 . ?
O2 Na2 H3BB 82(3) 7_656 7_656 ?
O9 Na2 Na1 120.91(17) . 7_656 ?
O9 Na2 Na1 95.65(18) . . ?
O9 Na2 O10 82.46(17) . 6_565 ?
O9 Na2 O2 140.1(2) . 7_656 ?
O9 Na2 H9B 18.5 . . ?
O9 Na2 O3B 98.3(4) . 7_656 ?
O9 Na2 H3BB 117.5(14) . 7_656 ?
H9B Na2 H3BB 113.0 . 7_656 ?
O5 Na2 Na1 116.97(19) . 7_656 ?
O5 Na2 Na1 49.84(14) . . ?
O5 Na2 O10 97.5(2) . 6_565 ?
O5 Na2 O2 130.6(2) . 7_656 ?
O5 Na2 O9 89.1(2) . . ?
O5 Na2 H9B 105.3 . . ?
O5 Na2 O3B 84.4(3) . 7_656 ?
O5 Na2 H3BB 74(4) . 7_656 ?
O5 Na2 O3A 89.8(3) . . ?
O3B Na2 Na1 131.7(3) 7_656 . ?
O3B Na2 H9B 90.9 7_656 . ?
O3A Na2 Na1 127.0(3) . . ?
O3A Na2 Na1 112.8(3) . 7_656 ?
O3A Na2 O10 156.9(3) . 6_565 ?
O3A Na2 O2 70.7(3) . 7_656 ?
O3A Na2 O9 119.7(3) . . ?
O3A Na2 H9B 109.9 . . ?
O3A Na2 O3B 21.9(3) . 7_656 ?
O3A Na2 H3BB 16(4) . 7_656 ?

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
Eu1 O1 C4 O10 -153.8(4) . . . . ?
Eu1 O1 C4 C1 25.2(6) . . . . ?
Eu1 O4 C2 O5 172.8(4) . . . . ?
Eu1 O4 C2 C3 -5.6(6) . . . . ?
Eu1 O6 C5 C6 1.1(6) 3 . . . ?
Eu1 O8 C1 C4 -16.0(5) . . . . ?
Eu1 O8 C3 C2 9.7(5) . . . . ?
Eu1 O12 C6 O7 173.2(4) 3 . . . ?
Eu1 O12 C6 C5 -7.6(6) 3 . . . ?
Na1 O10 C4 O1 71.5(5) 6_566 . . . ?
Na1 O10 C4 O1 -144.5(4) 4_656 . . . ?
Na1 O10 C4 C1 -107.6(4) 6_566 . . . ?
Na1 O10 C4 C1 36.4(7) 4_656 . . . ?
Na1 O7 C6 O12 114.7(10) . . . . ?
Na1 O7 C6 C5 -64.5(11) . . . . ?
Na1 O5 C2 O4 155.5(4) . . . . ?
Na1 O5 C2 C3 -26.1(7) . . . . ?
O8 C1 C4 O1 -4.4(6) . . . . ?
O8 C1 C4 O10 174.8(4) . . . . ?
O8 C3 C2 O4 -3.2(6) . . . . ?
O8 C3 C2 O5 178.3(4) . . . . ?
O12 C6 C5 O6 3.8(7) . . . . ?
O7 C6 C5 O6 -176.9(4) . . . . ?
C1 O8 C3 C2 158.1(4) . . . . ?
C3 O8 C1 C4 -164.6(4) . . . . ?
C5 O6 C5 C6 -179.0(6) 2_756 . . . ?
Na2 O10 C4 O1 -18.9(7) 6_566 . . . ?
Na2 O10 C4 C1 162.1(3) 6_566 . . . ?
Na2 O5 C2 O4 -19.3(8) . . . . ?
Na2 O5 C2 C3 159.1(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_mo_d8v5243_0ma
_database_code_depnum_ccdc_archive 'CCDC 2291811'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_mo_d8v5243_0ma      
;
PROBLEM: NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        8.8 Ratio
RESPONSE: The structure contains a lot of solvent molecules, which behave disordered. The position of the hydrogen atoms has been atempted to be optimised, such that the minimum ammount of alerts were created.
;
_vrf_PLAT417_mo_d8v5243_0ma      
;
PROBLEM: Short Inter D-H..H-D       H10B     ..H17B     .       2.04 Ang.
RESPONSE: Again, disordered solvent. The position of the hydrogen atoms has been attempted to be optimised to create an acceptor, however this resulted in the generation of more serious alerts
;
# Added during the CSD deposition process: Tuesday 23 April 2024 08:56 AM
# end Validation Reply Form

_audit_creation_date             2024-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H22.983 Eu N2 Na O13.491, 2.509(H2 O)'
_chemical_formula_sum            'C10 H28 Eu N2 Na O16'
_chemical_formula_weight         607.29
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   19.3808(9)
_cell_length_b                   35.2814(17)
_cell_length_c                   12.0315(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8226.9(7)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    9146
_cell_measurement_temperature    100
_cell_measurement_theta_max      55.86
_cell_measurement_theta_min      3.12
_shelx_estimated_absorpt_T_max   0.342
_shelx_estimated_absorpt_T_min   0.251
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.5128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1185 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.6828.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             4864
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 0.00 0.2610
0.00 1.00 0.00 0.1410
-1.00 0.00 0.00 0.2350
1.00 0.00 0.00 0.3030
0.00 0.00 1.00 0.1780
0.00 0.00 -1.00 0.2170
0.00 -1.00 1.00 0.2000
0.00 1.00 -1.00 0.1800

_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.606
_exptl_crystal_size_mid          0.522
_exptl_crystal_size_min          0.434
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35327
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         2.074
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                6407
_reflns_number_total             6527
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(10)
_refine_ls_extinction_coef       0.00039(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0193
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+23.3911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0464
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.982(10)
 0.018(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All H(H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 Na1-H7C \\sim Na1-H7D
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O3 \\sim H3A \\sim H3B: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
Uanis(O6) \\sim Ueq, : with sigma of 0.001 and sigma for terminal atoms of 0.002
Uiso(H6A) = Uiso(H10A)
5. Others
 Sof(O2)=Sof(H2A)=Sof(H2B)=Sof(O13)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(O18)=Sof(H18A)=Sof(H18B)=Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(1)
6.a Free rotating group:
 O17(H17A), O18(H18A,H18B), O7(H7C,H7D), O15(H15A,H15B), O2(H2A,H2B)
6.b Rotating group:
 O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B)
6.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C10(H10C,H10D), C5(H5A,H5B), C3(H3C,H3D), C7(H7A,H7B)
6.d Tetrahedral OH refined with riding coordinates:
 O3(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.41609(2) 0.65515(2) 0.47158(2) 0.00639(5) Uani 1 1 d . . . . .
O1 O 0.48824(13) 0.67080(8) 0.8233(2) 0.0136(5) Uani 1 1 d . . . . .
O4 O 0.18644(13) 0.67683(9) 0.4993(2) 0.0189(6) Uani 1 1 d . . . . .
O6 O 0.36261(14) 0.61027(8) 0.5968(2) 0.0118(4) Uani 1 1 d . U . . .
O8 O 0.29469(12) 0.66945(7) 0.4397(2) 0.0117(4) Uani 1 1 d . . . . .
O10 O 0.36609(13) 0.60628(7) 0.3493(2) 0.0099(4) Uani 1 1 d . . . . .
H10A H 0.321834 0.599568 0.369723 0.015 Uiso 1 1 d R U . . .
H10B H 0.388565 0.583128 0.354342 0.015 Uiso 1 1 d R U . . .
O12 O 0.49593(13) 0.59821(6) 0.4841(2) 0.0109(4) Uani 1 1 d . . . . .
H12A H 0.467527 0.578200 0.458589 0.016 Uiso 1 1 d R U . . .
H12B H 0.509578 0.591028 0.549499 0.016 Uiso 1 1 d R U . . .
O14 O 0.48142(13) 0.66454(7) 0.6385(2) 0.0101(4) Uani 1 1 d . . . . .
O16 O 0.39586(16) 0.73249(8) 0.1757(2) 0.0173(5) Uani 1 1 d . . . . .
O17 O 0.43642(15) 0.54126(8) 0.3667(2) 0.0157(5) Uani 1 1 d G . . . .
H17A H 0.450023 0.534248 0.303054 0.024 Uiso 1 1 d G U . . .
O9 O 0.52808(12) 0.66868(7) 0.3988(2) 0.0121(4) Uani 1 1 d . . . . .
O5 O 0.40262(13) 0.68273(7) 0.2888(2) 0.0108(4) Uani 1 1 d . . . . .
O11 O 0.59616(16) 0.71050(9) 0.3138(3) 0.0244(6) Uani 1 1 d . . . . .
N1 N 0.44241(14) 0.72863(7) 0.4653(3) 0.0117(4) Uani 1 1 d . . . . .
C1 C 0.45658(15) 0.67280(8) 0.7339(3) 0.0087(5) Uani 1 1 d . . . . .
N2 N 0.34955(15) 0.69331(8) 0.6315(3) 0.0110(5) Uani 1 1 d . . . . .
O3 O 0.6306(3) 0.57052(12) 0.2671(3) 0.0449(10) Uani 1 1 d . U . . .
H3A H 0.630358 0.548779 0.295499 0.067 Uiso 1 1 calc R U . . .
C4 C 0.38182(16) 0.68566(10) 0.7401(3) 0.0127(6) Uani 1 1 d . . . . .
H4A H 0.354657 0.665864 0.778653 0.015 Uiso 1 1 calc R U . . .
H4B H 0.379450 0.708980 0.785671 0.015 Uiso 1 1 calc R U . . .
C6 C 0.24984(18) 0.67555(10) 0.5148(3) 0.0134(6) Uani 1 1 d . . . . .
C8 C 0.4053(2) 0.74455(11) 0.3681(4) 0.0179(7) Uani 1 1 d . . . . .
H8A H 0.428687 0.768184 0.344579 0.021 Uiso 1 1 calc R U . . .
H8B H 0.357793 0.751250 0.390930 0.021 Uiso 1 1 calc R U . . .
C10 C 0.35061(19) 0.73438(10) 0.6056(3) 0.0149(6) Uani 1 1 d . . . . .
H10C H 0.336418 0.748764 0.672461 0.018 Uiso 1 1 calc R U . . .
H10D H 0.316627 0.739658 0.546147 0.018 Uiso 1 1 calc R U . . .
C5 C 0.42057(19) 0.74797(11) 0.5687(3) 0.0126(7) Uani 1 1 d . . . . .
H5A H 0.419011 0.775673 0.555953 0.015 Uiso 1 1 calc R U . . .
H5B H 0.454731 0.742936 0.628112 0.015 Uiso 1 1 calc R U . . .
C3 C 0.27677(17) 0.68088(10) 0.6323(3) 0.0135(6) Uani 1 1 d . . . . .
H3C H 0.248295 0.700033 0.671141 0.016 Uiso 1 1 calc R U . . .
H3D H 0.272851 0.656680 0.673445 0.016 Uiso 1 1 calc R U . . .
C7 C 0.51782(19) 0.73354(10) 0.4494(3) 0.0162(7) Uani 1 1 d . . . . .
H7A H 0.540603 0.734239 0.522988 0.019 Uiso 1 1 calc R U . . .
H7B H 0.526459 0.758134 0.412267 0.019 Uiso 1 1 calc R U . . .
C2 C 0.40172(17) 0.71773(9) 0.2695(3) 0.0115(6) Uani 1 1 d . . . . .
C9 C 0.54952(18) 0.70206(10) 0.3804(3) 0.0137(6) Uani 1 1 d . . . . .
Na1 Na 0.61063(9) 0.61702(5) 0.40909(14) 0.0193(3) Uani 1 1 d D . . . .
O18 O 0.5881(6) 0.6505(3) 0.1543(12) 0.038(3) Uani 0.509(15) 1 d G . P A 1
H18A H 0.623587 0.653507 0.110766 0.058 Uiso 0.509(15) 1 d G U P A 1
H18B H 0.599434 0.662323 0.215139 0.058 Uiso 0.509(15) 1 d G U P A 1
O7 O 0.7258(3) 0.63815(14) 0.3847(7) 0.087(3) Uani 1 1 d G . . . .
H7C H 0.761776 0.623443 0.389886 0.130 Uiso 1 1 d DG U . . .
H7D H 0.740463 0.660193 0.406688 0.130 Uiso 1 1 d DG U . . .
O15 O 0.7608(4) 0.7069(3) 0.4323(6) 0.041(3) Uani 0.509(15) 1 d G . P A 1
H15A H 0.733092 0.688074 0.418137 0.061 Uiso 0.509(15) 1 d G U P A 1
H15B H 0.796390 0.696360 0.463758 0.061 Uiso 0.509(15) 1 d G U P A 1
O2 O 0.7262(4) 0.7192(3) 0.3947(6) 0.038(3) Uani 0.491(15) 1 d G . P A 2
H2A H 0.762869 0.730999 0.371536 0.057 Uiso 0.491(15) 1 d G U P A 2
H2B H 0.692680 0.728810 0.355714 0.057 Uiso 0.491(15) 1 d G U P A 2
H3B H 0.683(4) 0.579(2) 0.278(8) 0.051(4) Uiso 1 1 d . U . . .
H6A H 0.323(6) 0.599(3) 0.584(11) 0.076 Uiso 1 1 d . U . . .
O13 O 0.6149(8) 0.6500(3) 0.1840(10) 0.040(3) Uani 0.491(15) 1 d . . P A 2
H13A H 0.600378 0.673840 0.162762 0.061 Uiso 0.491(15) 1 d R U P A 2
H13B H 0.631368 0.638720 0.119872 0.061 Uiso 0.491(15) 1 d R U P A 2
H17B H 0.415(3) 0.528(2) 0.383(6) 0.025(16) Uiso 1 1 d . . . . .
H6B H 0.385(5) 0.596(2) 0.635(8) 0.05(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O6 2.419(3) . ?
Eu1 O8 2.437(2) . ?
Eu1 O10 2.465(3) . ?
Eu1 O12 2.540(2) . ?
Eu1 O14 2.397(2) . ?
Eu1 O9 2.389(2) . ?
Eu1 O5 2.419(2) . ?
Eu1 N1 2.643(3) . ?
Eu1 N2 2.679(3) . ?
O1 C1 1.240(4) . ?
O4 C6 1.244(4) . ?
O6 H6A 0.87(11) . ?
O6 H6B 0.81(9) . ?
O8 C6 1.273(4) . ?
O10 H10A 0.9231 . ?
O10 H10B 0.9276 . ?
O10 Na1 2.477(3) 11_464 ?
O12 H12A 0.9462 . ?
O12 H12B 0.8683 . ?
O12 Na1 2.489(3) . ?
O14 C1 1.279(4) . ?
O16 C2 1.249(4) . ?
O17 H17A 0.8467 . ?
O17 H17B 0.67(7) . ?
O9 C9 1.268(4) . ?
O9 Na1 2.428(3) . ?
O5 C2 1.257(4) . ?
O5 Na1 2.485(3) 11_464 ?
O11 C9 1.244(4) . ?
N1 C8 1.483(5) . ?
N1 C5 1.481(5) . ?
N1 C7 1.484(4) . ?
C1 C4 1.520(4) . ?
N2 C4 1.473(4) . ?
N2 C10 1.482(5) . ?
N2 C3 1.477(4) . ?
O3 H3A 0.8400 . ?
O3 Na1 2.400(4) . ?
O3 H3B 1.07(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C3 1.518(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C2 1.519(5) . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 C5 1.505(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C9 1.516(5) . ?
Na1 O7 2.372(6) . ?
Na1 H3B 2.51(8) . ?
Na1 O13 2.948(12) . ?
O18 H18A 0.8705 . ?
O18 H18B 0.8702 . ?
O7 H7C 0.8707 . ?
O7 H7D 0.8690 . ?
O15 H15A 0.8712 . ?
O15 H15B 0.8696 . ?
O2 H2A 0.8700 . ?
O2 H2B 0.8706 . ?
O13 H13A 0.9246 . ?
O13 H13B 0.9238 . ?

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
O6 Eu1 O8 79.63(9) . . ?
O6 Eu1 O10 75.25(8) . . ?
O6 Eu1 O12 72.93(9) . . ?
O6 Eu1 N1 137.95(10) . . ?
O6 Eu1 N2 71.06(9) . . ?
O8 Eu1 O10 70.81(8) . . ?
O8 Eu1 O12 139.58(8) . . ?
O8 Eu1 N1 88.78(8) . . ?
O8 Eu1 N2 62.89(8) . . ?
O10 Eu1 O12 73.83(8) . . ?
O10 Eu1 N1 138.14(9) . . ?
O10 Eu1 N2 126.22(9) . . ?
O12 Eu1 N1 131.29(8) . . ?
O12 Eu1 N2 130.41(9) . . ?
O14 Eu1 O6 78.17(9) . . ?
O14 Eu1 O8 127.83(8) . . ?
O14 Eu1 O10 143.55(8) . . ?
O14 Eu1 O12 74.81(8) . . ?
O14 Eu1 O5 139.74(8) . . ?
O14 Eu1 N1 77.68(9) . . ?
O14 Eu1 N2 65.36(8) . . ?
O9 Eu1 O6 138.46(9) . . ?
O9 Eu1 O8 141.10(9) . . ?
O9 Eu1 O10 106.16(9) . . ?
O9 Eu1 O12 68.05(8) . . ?
O9 Eu1 O14 78.43(9) . . ?
O9 Eu1 O5 71.61(8) . . ?
O9 Eu1 N1 67.55(9) . . ?
O9 Eu1 N2 126.88(9) . . ?
O5 Eu1 O6 141.57(9) . . ?
O5 Eu1 O8 70.68(8) . . ?
O5 Eu1 O10 72.32(8) . . ?
O5 Eu1 O12 115.95(8) . . ?
O5 Eu1 N1 66.43(9) . . ?
O5 Eu1 N2 113.50(9) . . ?
N1 Eu1 N2 67.71(10) . . ?
Eu1 O6 H6A 124(8) . . ?
Eu1 O6 H6B 123(6) . . ?
H6A O6 H6B 106(10) . . ?
C6 O8 Eu1 125.6(2) . . ?
Eu1 O10 H10A 112.7 . . ?
Eu1 O10 H10B 113.1 . . ?
Eu1 O10 Na1 107.58(10) . 11_464 ?
H10A O10 H10B 101.1 . . ?
Na1 O10 H10A 107.7 11_464 . ?
Na1 O10 H10B 114.5 11_464 . ?
Eu1 O12 H12A 102.5 . . ?
Eu1 O12 H12B 118.0 . . ?
H12A O12 H12B 104.7 . . ?
Na1 O12 Eu1 108.16(9) . . ?
Na1 O12 H12A 126.9 . . ?
Na1 O12 H12B 97.7 . . ?
C1 O14 Eu1 125.8(2) . . ?
H17A O17 H17B 104.4 . . ?
Eu1 O9 Na1 115.47(11) . . ?
C9 O9 Eu1 123.2(2) . . ?
C9 O9 Na1 119.3(2) . . ?
Eu1 O5 Na1 108.79(10) . 11_464 ?
C2 O5 Eu1 124.4(2) . . ?
C2 O5 Na1 125.0(2) . 11_464 ?
C8 N1 Eu1 107.5(2) . . ?
C8 N1 C7 109.4(3) . . ?
C5 N1 Eu1 111.9(2) . . ?
C5 N1 C8 110.5(3) . . ?
C5 N1 C7 109.6(3) . . ?
C7 N1 Eu1 107.95(18) . . ?
O1 C1 O14 125.4(3) . . ?
O1 C1 C4 116.5(3) . . ?
O14 C1 C4 118.1(3) . . ?
C4 N2 Eu1 109.89(19) . . ?
C4 N2 C10 111.1(3) . . ?
C4 N2 C3 110.2(3) . . ?
C10 N2 Eu1 109.5(2) . . ?
C3 N2 Eu1 108.36(19) . . ?
C3 N2 C10 107.8(3) . . ?
H3A O3 H3B 101.6 . . ?
Na1 O3 H3A 109.5 . . ?
Na1 O3 H3B 83(5) . . ?
C1 C4 H4A 108.6 . . ?
C1 C4 H4B 108.6 . . ?
N2 C4 C1 114.6(3) . . ?
N2 C4 H4A 108.6 . . ?
N2 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
O4 C6 O8 125.0(3) . . ?
O4 C6 C3 118.4(3) . . ?
O8 C6 C3 116.6(3) . . ?
N1 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
N1 C8 C2 113.7(3) . . ?
H8A C8 H8B 107.7 . . ?
C2 C8 H8A 108.8 . . ?
C2 C8 H8B 108.8 . . ?
N2 C10 H10C 109.1 . . ?
N2 C10 H10D 109.1 . . ?
N2 C10 C5 112.7(3) . . ?
H10C C10 H10D 107.8 . . ?
C5 C10 H10C 109.1 . . ?
C5 C10 H10D 109.1 . . ?
N1 C5 C10 111.0(3) . . ?
N1 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
C10 C5 H5A 109.4 . . ?
C10 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N2 C3 C6 111.1(3) . . ?
N2 C3 H3C 109.4 . . ?
N2 C3 H3D 109.4 . . ?
C6 C3 H3C 109.4 . . ?
C6 C3 H3D 109.4 . . ?
H3C C3 H3D 108.0 . . ?
N1 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
N1 C7 C9 112.6(3) . . ?
H7A C7 H7B 107.8 . . ?
C9 C7 H7A 109.1 . . ?
C9 C7 H7B 109.1 . . ?
O16 C2 O5 125.3(3) . . ?
O16 C2 C8 116.8(3) . . ?
O5 C2 C8 117.9(3) . . ?
O9 C9 Eu1 37.82(16) . . ?
O9 C9 C7 116.9(3) . . ?
O11 C9 Eu1 156.1(3) . . ?
O11 C9 O9 124.9(4) . . ?
O11 C9 C7 118.1(3) . . ?
C7 C9 Eu1 82.33(19) . . ?
Eu1 Na1 Eu1 98.06(4) 3_565 . ?
Eu1 Na1 H3B 110(2) 3_565 . ?
Eu1 Na1 H3B 144(2) . . ?
O10 Na1 Eu1 36.10(6) 3_565 3_565 ?
O10 Na1 Eu1 75.13(7) 3_565 . ?
O10 Na1 O12 78.74(10) 3_565 . ?
O10 Na1 O5 71.01(9) 3_565 3_565 ?
O10 Na1 H3B 140(2) 3_565 . ?
O10 Na1 O13 134.2(2) 3_565 . ?
O12 Na1 Eu1 36.34(5) . . ?
O12 Na1 Eu1 81.18(7) . 3_565 ?
O12 Na1 H3B 125.8(19) . . ?
O12 Na1 O13 117.6(3) . . ?
O9 Na1 Eu1 111.88(8) . 3_565 ?
O9 Na1 Eu1 31.97(6) . . ?
O9 Na1 O10 77.86(10) . 3_565 ?
O9 Na1 O12 68.29(9) . . ?
O9 Na1 O5 141.04(11) . 3_565 ?
O9 Na1 H3B 138(2) . . ?
O9 Na1 O13 71.1(3) . . ?
O5 Na1 Eu1 114.86(8) 3_565 . ?
O5 Na1 Eu1 35.05(6) 3_565 3_565 ?
O5 Na1 O12 82.91(10) 3_565 . ?
O5 Na1 H3B 80(2) 3_565 . ?
O5 Na1 O13 147.8(3) 3_565 . ?
O3 Na1 Eu1 119.58(11) . 3_565 ?
O3 Na1 Eu1 120.43(14) . . ?
O3 Na1 O10 155.61(14) . 3_565 ?
O3 Na1 O12 102.70(15) . . ?
O3 Na1 O9 125.67(14) . . ?
O3 Na1 O5 84.93(12) . 3_565 ?
O3 Na1 H3B 25.0(19) . . ?
O3 Na1 O13 67.1(3) . . ?
O7 Na1 Eu1 142.21(14) . . ?
O7 Na1 Eu1 85.7(2) . 3_565 ?
O7 Na1 O10 87.4(2) . 3_565 ?
O7 Na1 O12 165.7(2) . . ?
O7 Na1 O9 112.20(15) . . ?
O7 Na1 O5 89.51(19) . 3_565 ?
O7 Na1 O3 88.6(2) . . ?
O7 Na1 H3B 64.1(19) . . ?
O7 Na1 O13 74.7(4) . . ?
O13 Na1 Eu1 93.8(3) . . ?
O13 Na1 H3B 68(2) . . ?
H18A O18 H18B 104.4 . . ?
Na1 O7 H7C 123.8 . . ?
Na1 O7 H7D 123.4 . . ?
H7C O7 H7D 104.5 . . ?
H15A O15 H15B 104.4 . . ?
H2A O2 H2B 104.4 . . ?
Na1 O13 H13A 127.2 . . ?
Na1 O13 H13B 127.4 . . ?
H13A O13 H13B 105.4 . . ?

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
Eu1 O8 C6 O4 -167.9(3) . . . . ?
Eu1 O8 C6 C3 10.9(4) . . . . ?
Eu1 O14 C1 O1 165.9(3) . . . . ?
Eu1 O14 C1 C4 -13.2(4) . . . . ?
Eu1 O9 C9 O11 -156.8(3) . . . . ?
Eu1 O9 C9 C7 26.2(4) . . . . ?
Eu1 O5 C2 O16 178.9(3) . . . . ?
Eu1 O5 C2 C8 -3.6(4) . . . . ?
Eu1 N1 C8 C2 -34.7(4) . . . . ?
Eu1 N1 C5 C10 -43.5(3) . . . . ?
Eu1 N1 C7 C9 32.2(3) . . . . ?
Eu1 N2 C4 C1 23.3(3) . . . . ?
Eu1 N2 C10 C5 -45.1(3) . . . . ?
Eu1 N2 C3 C6 -40.0(3) . . . . ?
O1 C1 C4 N2 171.0(3) . . . . ?
O4 C6 C3 N2 -157.9(3) . . . . ?
O8 C6 C3 N2 23.2(4) . . . . ?
O14 C1 C4 N2 -9.9(4) . . . . ?
N1 C8 C2 O16 -153.9(4) . . . . ?
N1 C8 C2 O5 28.3(5) . . . . ?
N1 C7 C9 Eu1 -24.5(2) . . . . ?
N1 C7 C9 O9 -40.4(4) . . . . ?
N1 C7 C9 O11 142.4(3) . . . . ?
N2 C10 C5 N1 61.7(4) . . . . ?
C4 N2 C10 C5 76.5(4) . . . . ?
C4 N2 C3 C6 -160.3(3) . . . . ?
C8 N1 C5 C10 76.2(4) . . . . ?
C8 N1 C7 C9 -84.4(3) . . . . ?
C10 N2 C4 C1 -98.0(3) . . . . ?
C10 N2 C3 C6 78.4(3) . . . . ?
C5 N1 C8 C2 -157.0(3) . . . . ?
C5 N1 C7 C9 154.3(3) . . . . ?
C3 N2 C4 C1 142.6(3) . . . . ?
C3 N2 C10 C5 -162.7(3) . . . . ?
C7 N1 C8 C2 82.3(4) . . . . ?
C7 N1 C5 C10 -163.2(3) . . . . ?
Na1 O9 C9 Eu1 -163.1(3) . . . . ?
Na1 O9 C9 O11 40.1(5) . . . . ?
Na1 O9 C9 C7 -136.9(3) . . . . ?
Na1 O5 C2 O16 -18.3(5) 11_464 . . . ?
Na1 O5 C2 C8 159.2(3) 11_464 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.982(10)
2 0.018(10)

####################################################################### 
# 
# 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_mo_d8v5332_0ma
_database_code_depnum_ccdc_archive 'CCDC 2291820'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_mo_d8v5332_0ma      
;
PROBLEM: NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        8.3 Ratio
RESPONSE: Different atom types have been considered, however this was the only resonable solution creating a neutrally charged compound with the known ligand - and charge of the ligand
;
# Added during the CSD deposition process: Tuesday 23 April 2024 09:12 AM
# end Validation Reply Form

_audit_creation_date             2024-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H23.113 N2 Na O13.557 Sm, 2.443(H2 O)'
_chemical_formula_sum            'C10 H28 N2 Na O16 Sm'
_chemical_formula_weight         605.68
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   19.459(3)
_cell_length_b                   35.397(6)
_cell_length_c                   12.032(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8288(2)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.23
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   0.716
_shelx_estimated_absorpt_T_min   0.283
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.6962.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             4848
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.2960
1.00 0.00 0.00 0.2910
-1.00 0.00 1.00 0.1490
1.00 0.00 -1.00 0.1540
1.00 1.00 1.00 0.1970
-1.00 -1.00 -1.00 0.1890
0.00 -1.00 0.00 0.0160
0.00 1.00 0.00 0.0610

_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.122
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42482
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         2.071
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                8445
_reflns_number_total             8972
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.024(10)
_refine_ls_extinction_coef       0.000101(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         8972
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0236
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²+12.5418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0516
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.976(10)
 0.024(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O16-H16B
 0.85 with sigma of 0.0002
 O13-H13C \\sim O13A-H13A
 with sigma of 0.02
 O13-H13D \\sim O13A-H13B
 with sigma of 0.02
 H13C-H13D \\sim H13A-H13B
 with sigma of 0.04
4. Others
 Sof(O2)=Sof(H2A)=Sof(H2B)=1-FVAR(1)
 Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Sof(O13A)=Sof(H13A)=Sof(H13B)=1-FVAR(2)
 Sof(O13)=Sof(H13C)=Sof(H13D)=FVAR(2)
5.a Free rotating group:
 O6(H6A,H6B), O12(H12A,H12B), O13(H13C,H13D), O7(H7C,H7D), O15(H15A,H15B),
 O2(H2A,H2B), O13A(H13A,H13B)
5.b Rotating group:
 O3(H3A,H3B)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C6(H6C,H6D), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.58435(2) 0.65509(2) 0.52930(2) 0.00557(4) Uani 1 1 d . . . . .
Na1 Na 0.38992(8) 0.61722(4) 0.59246(13) 0.0184(3) Uani 1 1 d . . . . .
O1 O 0.51225(13) 0.67107(7) 0.1765(2) 0.0133(4) Uani 1 1 d . . . . .
O4 O 0.81394(12) 0.67634(8) 0.4994(2) 0.0192(5) Uani 1 1 d . . . . .
O6 O 0.63771(13) 0.60986(7) 0.4036(2) 0.0118(4) Uani 1 1 d G . . . .
H6A H 0.613907 0.596395 0.359606 0.018 Uiso 1 1 d G U . . .
H6B H 0.674754 0.597445 0.412724 0.018 Uiso 1 1 d G U . . .
O8 O 0.70642(11) 0.66944(7) 0.56030(19) 0.0114(4) Uani 1 1 d . . . . .
O10 O 0.60418(15) 0.73273(7) 0.8254(2) 0.0169(5) Uani 1 1 d . . . . .
O12 O 0.56392(14) 0.54131(7) 0.6341(2) 0.0149(4) Uani 1 1 d G . . . .
H12A H 0.581299 0.520758 0.610724 0.022 Uiso 1 1 d G U . . .
H12B H 0.549454 0.536065 0.699014 0.022 Uiso 1 1 d G U . . .
O14 O 0.50379(12) 0.59801(6) 0.5168(2) 0.0102(4) Uani 1 1 d . . . . .
O16 O 0.63478(12) 0.60606(6) 0.6519(2) 0.0093(4) Uani 1 1 d D . . . .
O17 O 0.51919(12) 0.66468(6) 0.36119(19) 0.0092(4) Uani 1 1 d . . . . .
O9 O 0.40461(15) 0.71111(8) 0.6859(2) 0.0234(6) Uani 1 1 d . . . . .
O5 O 0.59799(12) 0.68302(6) 0.71215(19) 0.0104(4) Uani 1 1 d . . . . .
O11 O 0.47213(12) 0.66920(6) 0.6015(2) 0.0118(4) Uani 1 1 d . . . . .
N1 N 0.55825(13) 0.72875(6) 0.5347(3) 0.0110(4) Uani 1 1 d . . . . .
C1 C 0.61841(15) 0.68566(9) 0.2599(2) 0.0121(5) Uani 1 1 d . . . . .
H1A H 0.645229 0.665916 0.220976 0.015 Uiso 1 1 calc R U . . .
H1B H 0.620811 0.708938 0.214414 0.015 Uiso 1 1 calc R U . . .
C8 C 0.58071(18) 0.74796(10) 0.4311(3) 0.0129(6) Uani 1 1 d . . . . .
H8A H 0.582652 0.775562 0.443877 0.016 Uiso 1 1 calc R U . . .
H8B H 0.546762 0.743110 0.371465 0.016 Uiso 1 1 calc R U . . .
N2 N 0.65097(13) 0.69316(8) 0.3680(2) 0.0096(4) Uani 1 1 d . . . . .
C5 C 0.54384(14) 0.67298(7) 0.2662(2) 0.0086(5) Uani 1 1 d . . . . .
O3 O 0.3689(3) 0.57033(11) 0.7331(3) 0.0489(11) Uani 1 1 d . . . . .
H3A H 0.368036 0.545322 0.713871 0.073 Uiso 1 1 d R U . . .
H3B H 0.323281 0.574415 0.744981 0.073 Uiso 1 1 d R U . . .
C7 C 0.65031(17) 0.73412(9) 0.3945(3) 0.0134(5) Uani 1 1 d . . . . .
H7A H 0.664850 0.748499 0.327975 0.016 Uiso 1 1 calc R U . . .
H7B H 0.684058 0.739140 0.454285 0.016 Uiso 1 1 calc R U . . .
C9 C 0.48333(17) 0.73390(9) 0.5505(3) 0.0155(6) Uani 1 1 d . . . . .
H9A H 0.460686 0.734690 0.476879 0.019 Uiso 1 1 calc R U . . .
H9B H 0.475047 0.758452 0.587569 0.019 Uiso 1 1 calc R U . . .
C10 C 0.75046(16) 0.67521(9) 0.4841(3) 0.0119(5) Uani 1 1 d . . . . .
C6 C 0.5954(2) 0.74474(10) 0.6317(3) 0.0166(7) Uani 1 1 d . . . . .
H6C H 0.572424 0.768429 0.654756 0.020 Uiso 1 1 calc R U . . .
H6D H 0.642848 0.751191 0.608797 0.020 Uiso 1 1 calc R U . . .
C3 C 0.59862(16) 0.71807(8) 0.7311(3) 0.0100(5) Uani 1 1 d . . . . .
C4 C 0.72333(16) 0.68048(10) 0.3667(3) 0.0127(5) Uani 1 1 d . . . . .
H4A H 0.751813 0.699417 0.327423 0.015 Uiso 1 1 calc R U . . .
H4B H 0.726807 0.656296 0.325777 0.015 Uiso 1 1 calc R U . . .
C2 C 0.45091(16) 0.70249(9) 0.6199(3) 0.0130(5) Uani 1 1 d . . . . .
O13 O 0.4131(11) 0.6510(3) 0.844(2) 0.033(5) Uani 0.44(5) 1 d DG . P A 1
H13C H 0.401430 0.666918 0.795405 0.050 Uiso 0.44(5) 1 d DG U P A 1
H13D H 0.375785 0.644535 0.875711 0.050 Uiso 0.44(5) 1 d DG U P A 1
H14A H 0.520(3) 0.5773(15) 0.545(5) 0.032(14) Uiso 1 1 d . . . . .
H14B H 0.490(2) 0.5917(12) 0.447(5) 0.011(11) Uiso 1 1 d . . . . .
O7 O 0.2736(3) 0.63812(12) 0.6138(6) 0.076(2) Uani 1 1 d G . . . .
H7C H 0.264154 0.661503 0.609263 0.115 Uiso 1 1 d G U . . .
H7D H 0.234787 0.627168 0.612078 0.115 Uiso 1 1 d G U . . .
O15 O 0.2390(4) 0.7076(2) 0.5679(6) 0.037(2) Uani 0.490(12) 1 d G . P B 1
H15A H 0.201136 0.703590 0.534606 0.056 Uiso 0.490(12) 1 d G U P B 1
H15B H 0.231662 0.727341 0.606408 0.056 Uiso 0.490(12) 1 d G U P B 1
O2 O 0.2748(4) 0.7176(2) 0.6055(6) 0.036(2) Uani 0.510(12) 1 d G . P B 2
H2A H 0.269244 0.740856 0.589920 0.054 Uiso 0.510(12) 1 d G U P B 2
H2B H 0.315969 0.716215 0.628774 0.054 Uiso 0.510(12) 1 d G U P B 2
H16A H 0.669(3) 0.6013(16) 0.637(6) 0.024(15) Uiso 1 1 d . . . . .
H16B H 0.6157(9) 0.5845(2) 0.649(6) 0.06(2) Uiso 1 1 d D . . . .
O13A O 0.3872(16) 0.6494(3) 0.8142(9) 0.046(4) Uani 0.56(5) 1 d DG . P A 2
H13A H 0.406180 0.667786 0.781806 0.02(2) Uiso 0.56(5) 1 d DG . P A 2
H13B H 0.379427 0.656949 0.879828 0.01(2) Uiso 0.56(5) 1 d DG . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O6 2.434(2) . ?
Sm1 O8 2.458(2) . ?
Sm1 O14 2.562(2) . ?
Sm1 O16 2.480(2) . ?
Sm1 O17 2.411(2) . ?
Sm1 O5 2.427(2) . ?
Sm1 O11 2.402(2) . ?
Sm1 N1 2.657(2) . ?
Sm1 N2 2.695(3) . ?
Na1 O14 2.490(3) . ?
Na1 O16 2.483(3) 11_464 ?
Na1 O5 2.507(3) 11_464 ?
Na1 O11 2.441(3) . ?
Na1 O3 2.406(4) . ?
Na1 O7 2.395(5) . ?
Na1 O13A 2.901(11) . ?
O1 C5 1.244(4) . ?
O4 C10 1.250(4) . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8513 . ?
O8 C10 1.272(4) . ?
O10 C3 1.252(4) . ?
O12 H12A 0.8501 . ?
O12 H12B 0.8504 . ?
O14 H14A 0.87(6) . ?
O14 H14B 0.91(5) . ?
O16 H16A 0.71(5) . ?
O16 H16B 0.8500(5) . ?
O17 C5 1.274(4) . ?
O9 C2 1.240(4) . ?
O5 C3 1.262(4) . ?
O11 C2 1.268(4) . ?
N1 C8 1.486(5) . ?
N1 C9 1.482(4) . ?
N1 C6 1.486(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 N2 1.471(4) . ?
C1 C5 1.521(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.506(5) . ?
N2 C7 1.485(4) . ?
N2 C4 1.478(4) . ?
O3 H3A 0.9152 . ?
O3 H3B 0.9100 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C2 1.526(5) . ?
C10 C4 1.519(4) . ?
C6 H6C 0.9900 . ?
C6 H6D 0.9900 . ?
C6 C3 1.525(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O13 H13C 0.8438 . ?
O13 H13D 0.8503 . ?
O7 H7C 0.8497 . ?
O7 H7D 0.8489 . ?
O15 H15A 0.8499 . ?
O15 H15B 0.8495 . ?
O2 H2A 0.8498 . ?
O2 H2B 0.8502 . ?
O13A H13A 0.8434 . ?
O13A H13B 0.8476 . ?

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
O6 Sm1 O8 79.51(8) . . ?
O6 Sm1 O14 72.90(8) . . ?
O6 Sm1 O16 74.95(7) . . ?
O6 Sm1 N1 137.89(9) . . ?
O6 Sm1 N2 71.12(9) . . ?
O8 Sm1 O14 139.77(7) . . ?
O8 Sm1 O16 70.85(8) . . ?
O8 Sm1 N1 88.75(8) . . ?
O8 Sm1 N2 62.68(8) . . ?
O14 Sm1 N1 131.18(7) . . ?
O14 Sm1 N2 130.28(8) . . ?
O16 Sm1 O14 74.04(8) . . ?
O16 Sm1 N1 138.41(9) . . ?
O16 Sm1 N2 126.00(8) . . ?
O17 Sm1 O6 78.22(8) . . ?
O17 Sm1 O8 127.33(7) . . ?
O17 Sm1 O14 74.93(7) . . ?
O17 Sm1 O16 143.66(8) . . ?
O17 Sm1 O5 139.52(8) . . ?
O17 Sm1 N1 77.39(8) . . ?
O17 Sm1 N2 65.07(8) . . ?
O5 Sm1 O6 141.66(8) . . ?
O5 Sm1 O8 70.88(8) . . ?
O5 Sm1 O14 116.20(8) . . ?
O5 Sm1 O16 72.71(8) . . ?
O5 Sm1 N1 66.36(9) . . ?
O5 Sm1 N2 113.37(8) . . ?
O11 Sm1 O6 138.50(8) . . ?
O11 Sm1 O8 141.32(8) . . ?
O11 Sm1 O14 68.23(7) . . ?
O11 Sm1 O16 106.88(8) . . ?
O11 Sm1 O17 78.23(8) . . ?
O11 Sm1 O5 71.76(8) . . ?
O11 Sm1 N1 67.26(8) . . ?
O11 Sm1 N2 126.40(8) . . ?
N1 Sm1 N2 67.59(9) . . ?
Sm1 Na1 Sm1 98.04(3) 11_464 . ?
O14 Na1 Sm1 36.63(5) . . ?
O14 Na1 Sm1 80.93(7) . 11_464 ?
O14 Na1 O5 82.38(9) . 11_464 ?
O14 Na1 O13A 117.4(6) . . ?
O16 Na1 Sm1 74.96(7) 11_464 . ?
O16 Na1 Sm1 36.28(6) 11_464 11_464 ?
O16 Na1 O14 78.59(9) 11_464 . ?
O16 Na1 O5 71.30(8) 11_464 11_464 ?
O16 Na1 O13A 134.3(2) 11_464 . ?
O5 Na1 Sm1 114.70(7) 11_464 . ?
O5 Na1 Sm1 35.19(5) 11_464 11_464 ?
O5 Na1 O13A 147.9(4) 11_464 . ?
O11 Na1 Sm1 32.20(6) . . ?
O11 Na1 Sm1 111.59(7) . 11_464 ?
O11 Na1 O14 68.83(8) . . ?
O11 Na1 O16 77.30(9) . 11_464 ?
O11 Na1 O5 140.88(10) . 11_464 ?
O11 Na1 O13A 71.0(4) . . ?
O3 Na1 Sm1 120.99(14) . . ?
O3 Na1 Sm1 118.73(10) . 11_464 ?
O3 Na1 O14 102.72(14) . . ?
O3 Na1 O16 154.94(13) . 11_464 ?
O3 Na1 O5 83.98(11) . 11_464 ?
O3 Na1 O11 126.91(13) . . ?
O3 Na1 O13A 67.7(2) . . ?
O7 Na1 Sm1 142.55(12) . . ?
O7 Na1 Sm1 84.63(18) . 11_464 ?
O7 Na1 O14 164.7(2) . . ?
O7 Na1 O16 86.76(19) . 11_464 ?
O7 Na1 O5 88.77(16) . 11_464 ?
O7 Na1 O11 112.45(13) . . ?
O7 Na1 O3 88.7(2) . . ?
O7 Na1 O13A 76.3(6) . . ?
O13A Na1 Sm1 93.4(6) . . ?
Sm1 O6 H6A 121.6 . . ?
Sm1 O6 H6B 128.4 . . ?
H6A O6 H6B 104.6 . . ?
C10 O8 Sm1 125.1(2) . . ?
H12A O12 H12B 104.4 . . ?
Sm1 O14 H14A 115(4) . . ?
Sm1 O14 H14B 115(3) . . ?
Na1 O14 Sm1 107.92(8) . . ?
Na1 O14 H14A 114(4) . . ?
Na1 O14 H14B 98(3) . . ?
H14A O14 H14B 105(5) . . ?
Sm1 O16 Na1 107.37(9) . 3_565 ?
Sm1 O16 H16A 113(5) . . ?
Sm1 O16 H16B 116(4) . . ?
Na1 O16 H16A 106(5) 3_565 . ?
Na1 O16 H16B 113(5) 3_565 . ?
H16A O16 H16B 101(5) . . ?
C5 O17 Sm1 125.95(19) . . ?
Sm1 O5 Na1 108.27(9) . 3_565 ?
C3 O5 Sm1 124.5(2) . . ?
C3 O5 Na1 125.5(2) . 3_565 ?
Sm1 O11 Na1 115.02(10) . . ?
C2 O11 Sm1 123.5(2) . . ?
C2 O11 Na1 119.7(2) . . ?
C8 N1 Sm1 111.9(2) . . ?
C9 N1 Sm1 108.17(17) . . ?
C9 N1 C8 110.0(2) . . ?
C9 N1 C6 109.3(3) . . ?
C6 N1 Sm1 107.45(19) . . ?
C6 N1 C8 110.0(2) . . ?
H1A C1 H1B 107.5 . . ?
N2 C1 H1A 108.6 . . ?
N2 C1 H1B 108.6 . . ?
N2 C1 C5 114.8(2) . . ?
C5 C1 H1A 108.6 . . ?
C5 C1 H1B 108.6 . . ?
N1 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
N1 C8 C7 111.2(3) . . ?
H8A C8 H8B 108.0 . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C1 N2 Sm1 109.85(17) . . ?
C1 N2 C7 111.2(2) . . ?
C1 N2 C4 110.3(3) . . ?
C7 N2 Sm1 109.23(19) . . ?
C4 N2 Sm1 108.29(18) . . ?
C4 N2 C7 107.9(2) . . ?
O1 C5 O17 125.4(3) . . ?
O1 C5 C1 116.4(3) . . ?
O17 C5 C1 118.2(2) . . ?
Na1 O3 H3A 119.5 . . ?
Na1 O3 H3B 99.6 . . ?
H3A O3 H3B 100.1 . . ?
C8 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
N2 C7 C8 112.8(3) . . ?
N2 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
N1 C9 H9A 109.0 . . ?
N1 C9 H9B 109.0 . . ?
N1 C9 C2 112.8(2) . . ?
H9A C9 H9B 107.8 . . ?
C2 C9 H9A 109.0 . . ?
C2 C9 H9B 109.0 . . ?
O4 C10 O8 124.4(3) . . ?
O4 C10 C4 118.5(3) . . ?
O8 C10 C4 117.1(3) . . ?
N1 C6 H6C 108.8 . . ?
N1 C6 H6D 108.8 . . ?
N1 C6 C3 113.6(3) . . ?
H6C C6 H6D 107.7 . . ?
C3 C6 H6C 108.8 . . ?
C3 C6 H6D 108.8 . . ?
O10 C3 O5 124.9(3) . . ?
O10 C3 C6 117.2(3) . . ?
O5 C3 C6 117.8(3) . . ?
N2 C4 C10 111.0(3) . . ?
N2 C4 H4A 109.4 . . ?
N2 C4 H4B 109.4 . . ?
C10 C4 H4A 109.4 . . ?
C10 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O9 C2 O11 125.3(3) . . ?
O9 C2 C9 118.1(3) . . ?
O11 C2 C9 116.5(3) . . ?
H13C O13 H13D 105.2 . . ?
Na1 O7 H7C 119.9 . . ?
Na1 O7 H7D 134.2 . . ?
H7C O7 H7D 104.5 . . ?
H15A O15 H15B 104.5 . . ?
H2A O2 H2B 104.5 . . ?
Na1 O13A H13A 82.6 . . ?
Na1 O13A H13B 169.8 . . ?
H13A O13A H13B 105.4 . . ?

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
Sm1 O8 C10 O4 -167.7(3) . . . . ?
Sm1 O8 C10 C4 11.4(4) . . . . ?
Sm1 O17 C5 O1 165.9(2) . . . . ?
Sm1 O17 C5 C1 -12.9(4) . . . . ?
Sm1 O5 C3 O10 178.4(3) . . . . ?
Sm1 O5 C3 C6 -4.3(4) . . . . ?
Sm1 O11 C2 O9 -156.6(3) . . . . ?
Sm1 O11 C2 C9 26.3(4) . . . . ?
Sm1 N1 C8 C7 -43.0(3) . . . . ?
Sm1 N1 C9 C2 31.9(3) . . . . ?
Sm1 N1 C6 C3 -35.0(4) . . . . ?
Sm1 N2 C7 C8 -45.7(3) . . . . ?
Sm1 N2 C4 C10 -40.3(3) . . . . ?
Na1 O5 C3 O10 -18.4(5) 3_565 . . . ?
Na1 O5 C3 C6 158.9(2) 3_565 . . . ?
Na1 O11 C2 O9 39.4(4) . . . . ?
Na1 O11 C2 C9 -137.7(2) . . . . ?
O4 C10 C4 N2 -157.8(3) . . . . ?
O8 C10 C4 N2 23.1(4) . . . . ?
N1 C8 C7 N2 62.0(3) . . . . ?
N1 C9 C2 O9 142.5(3) . . . . ?
N1 C9 C2 O11 -40.2(4) . . . . ?
N1 C6 C3 O10 -153.4(3) . . . . ?
N1 C6 C3 O5 29.0(5) . . . . ?
C1 N2 C7 C8 75.8(3) . . . . ?
C1 N2 C4 C10 -160.5(3) . . . . ?
C8 N1 C9 C2 154.4(3) . . . . ?
C8 N1 C6 C3 -157.0(3) . . . . ?
N2 C1 C5 O1 171.1(3) . . . . ?
N2 C1 C5 O17 -10.0(4) . . . . ?
C5 C1 N2 Sm1 23.1(3) . . . . ?
C5 C1 N2 C7 -98.0(3) . . . . ?
C5 C1 N2 C4 142.4(3) . . . . ?
C7 N2 C4 C10 77.8(3) . . . . ?
C9 N1 C8 C7 -163.3(3) . . . . ?
C9 N1 C6 C3 82.2(3) . . . . ?
C6 N1 C8 C7 76.3(3) . . . . ?
C6 N1 C9 C2 -84.8(3) . . . . ?
C4 N2 C7 C8 -163.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.976(10)
2 0.024(10)

####################################################################### 
# 
# 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_mo_d8v5763_0ma
_database_code_depnum_ccdc_archive 'CCDC 2291822'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT355_mo_d8v5763_0ma      
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O12      - H12B     .       1.08 Ang.
RESPONSE: The structure contains a lot of solvent molecules, which behave disordered. The position of the hydrogen atoms has been atempted to be optimised, such that the minimum ammount of alerts were created.
;
_vrf_PLAT420_mo_d8v5763_0ma      
;
PROBLEM: D-H Bond Without Acceptor  O6       --H6B      .     Please Check
RESPONSE: Disordered solvent. The position of the hydrogen atoms has been attempted to be optimised to create an acceptor, however this 
;
_vrf_PLAT976_mo_d8v5763_0ma      
;
PROBLEM: Check Calcd Resid. Dens.  0.59Ang From O11     .      -1.63 eA-3
RESPONSE: Disordered solvent
;
# Added during the CSD deposition process: Tuesday 23 April 2024 09:17 AM
# end Validation Reply Form

_audit_creation_date             2024-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C21 H17 Cs3 N3 O18 Sm, 3(H2 O)'
_chemical_formula_sum            'C21 H23 Cs3 N3 O21 Sm'
_chemical_formula_weight         1202.50
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'

_cell_length_a                   10.0017(13)
_cell_length_b                   18.033(3)
_cell_length_c                   18.530(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3342.1(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    100
_cell_measurement_theta_max      45.28
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.715
_shelx_estimated_absorpt_T_min   0.494
_exptl_absorpt_coefficient_mu    5.067
_exptl_absorpt_correction_T_max  0.7492
_exptl_absorpt_correction_T_min  0.5940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1034 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.7928.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 2.00 0.00 0.0810
0.00 -2.00 0.00 0.0750
1.00 1.00 0.00 0.0340
-1.00 -1.00 0.00 0.0630
0.00 0.00 1.00 0.0190
0.00 0.00 -1.00 0.0350

_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.071
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64847
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.330
_diffrn_reflns_theta_min         2.198
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7616
_reflns_number_total             8116
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.347
_refine_diff_density_min         -2.019
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.132(16)
_refine_ls_extinction_coef       0.00019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         8116
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.711
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+10.9945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0637
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.868(16)
 0.132(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C6-H6 = C6-C2 = C6-C9
 0.4 with sigma of 0.02
 C2-C4 = C2-C6 = C2-H2
 0.4 with sigma of 0.02
 C9-C3
 0.4 with sigma of 0.02
 Cs1-O8 \\sim Cs1A-O8
 with sigma of 0.02
 Cs1-O12 \\sim Cs1A-O12
 with sigma of 0.02
4. Rigid bond restraints
 C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
6. Others
 Sof(Cs1A)=Sof(O1)=1-FVAR(1)
 Sof(Cs1)=Sof(O2)=FVAR(1)
 Fixed Sof: H11A(0.5) H11B(0.5)
7.a Free rotating group:
 O3(H3A,H3B), O11(H11A,H11B)
7.b Rotating group:
 O6(H6A,H6B), O12(H12A,H12B)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C2(H2), C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.74803(3) 0.500000 0.500000 0.00621(5) Uani 1 2 d S T P . .
Cs1 Cs 0.24206(13) 0.47367(5) 0.24329(6) 0.0080(3) Uani 0.614(13) 1 d D . P . .
Cs2 Cs 0.500000 0.25917(2) 0.250000 0.01908(10) Uani 1 2 d S T P . .
O4 O 1.0342(4) 0.6081(2) 0.6572(2) 0.0287(9) Uani 1 1 d . . . . .
O6 O 0.5400(4) 0.0868(2) 0.3211(2) 0.0216(7) Uani 1 1 d . . . . .
H6A H 0.456182 0.070624 0.334639 0.032 Uiso 1 1 d R U . . .
H6B H 0.599793 0.068956 0.291229 0.032 Uiso 1 1 d R U . . .
N1 N 1.0006(5) 0.500000 0.500000 0.0137(7) Uani 1 2 d S T P . .
O8 O 0.4577(3) 0.4012(2) 0.33916(18) 0.0140(5) Uani 1 1 d D . . . .
O10 O 0.8071(3) 0.41344(16) 0.59856(15) 0.0120(5) Uani 1 1 d . . . . .
O12 O 0.4533(5) 0.5842(3) 0.3198(3) 0.0329(10) Uani 1 1 d D . . . .
H12A H 0.407981 0.614344 0.358870 0.049 Uiso 1 1 d R U . . .
H12B H 0.532812 0.558826 0.350920 0.049 Uiso 1 1 d R U . . .
O3 O 0.7499(6) 0.1636(3) 0.3820(3) 0.0491(12) Uani 1 1 d G . . . .
H3A H 0.678215 0.157197 0.358161 0.074 Uiso 1 1 d G U . . .
H3B H 0.778775 0.205592 0.368027 0.074 Uiso 1 1 d G U . . .
N2 N 0.6228(3) 0.37660(16) 0.50477(17) 0.0088(4) Uani 1 1 d . . . . .
O7 O 0.7647(4) 0.3139(2) 0.66741(17) 0.0248(7) Uani 1 1 d . . . . .
O2 O 0.7773(6) 0.6969(4) 0.6722(4) 0.0291(18) Uani 0.614(13) 1 d . . P A 1
C1 C 0.9816(5) 0.5787(3) 0.6036(2) 0.0187(9) Uani 1 1 d . . . . .
O9 O 0.5776(3) 0.47929(16) 0.40672(15) 0.0111(4) Uani 1 1 d . . . . .
C4 C 0.6420(4) 0.3278(2) 0.55860(19) 0.0110(6) Uani 1 1 d D . . . .
C6 C 0.4905(7) 0.2456(2) 0.5082(3) 0.0240(11) Uani 1 1 d D . . . .
H6 H 0.447631 0.198591 0.508221 0.029 Uiso 1 1 calc DR U . . .
C8 C 1.2062(4) 0.5398(5) 0.5508(3) 0.0378(17) Uani 1 1 d . . . . .
H8 H 1.253085 0.567556 0.586281 0.045 Uiso 1 1 calc R U . . .
C10 C 0.5212(3) 0.4172(2) 0.3941(2) 0.0089(6) Uani 1 1 d . . . . .
C11 C 1.0682(4) 0.5385(3) 0.5492(2) 0.0199(9) Uani 1 1 d . . . . .
C3 C 0.5345(4) 0.3587(2) 0.45276(19) 0.0114(6) Uani 1 1 d D . . . .
C7 C 0.7458(5) 0.35291(19) 0.61322(18) 0.0125(5) Uani 1 1 d . . . . .
O5 O 0.8566(3) 0.57914(17) 0.58919(16) 0.0144(5) Uani 1 1 d . . . . .
C2 C 0.5749(5) 0.2623(3) 0.5615(2) 0.0185(7) Uani 1 1 d D . . . .
H2 H 0.587878 0.229145 0.600679 0.022 Uiso 1 1 calc DR U . . .
C9 C 0.4642(4) 0.2939(2) 0.4540(2) 0.0172(7) Uani 1 1 d D . . . .
C5 C 1.2725(5) 0.500000 0.500000 0.0297(18) Uani 1 2 d S T P . .
H5 H 1.367443 0.500001 0.499998 0.036 Uiso 1 2 calc R U P . .
O11 O 1.000000 0.7535(2) 0.750000 0.0115(8) Uani 1 2 d GS TU P . .
H11A H 1.065381 0.728847 0.766903 0.017 Uiso 0.5 1 d G U P . .
H11B H 1.028734 0.797778 0.747676 0.017 Uiso 0.5 1 d G U P . .
Cs1A Cs 0.2414(3) 0.47533(15) 0.24322(17) 0.0303(9) Uani 0.386(13) 1 d D . P .
.
H9 H 0.415(6) 0.283(4) 0.419(3) 0.017(15) Uiso 1 1 d . . . . .
O1 O 0.8027(10) 0.7055(6) 0.7200(6) 0.027(3) Uani 0.386(13) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 N1 2.526(5) . ?
Sm1 O10 2.474(3) 2_566 ?
Sm1 O10 2.474(3) . ?
Sm1 N2 2.555(3) . ?
Sm1 N2 2.555(3) 2_566 ?
Sm1 O9 2.456(3) 2_566 ?
Sm1 O9 2.456(3) . ?
Sm1 O5 2.438(3) . ?
Sm1 O5 2.438(3) 2_566 ?
Cs1 O4 3.146(4) 2_466 ?
Cs1 O6 3.213(4) 5_455 ?
Cs1 H6B 2.401(4) 5_455 ?
Cs1 O8 3.085(3) . ?
Cs1 O10 3.403(3) 4_664 ?
Cs1 O12 3.232(5) . ?
Cs1 O2 3.352(7) 4_664 ?
Cs1 O9 3.315(3) 3_655 ?
Cs1 O5 3.168(3) 4_664 ?
Cs1 O1 3.290(11) 4_664 ?
Cs2 O6 3.400(4) 3_655 ?
Cs2 O8 3.077(3) . ?
Cs2 O8 3.077(3) 3_655 ?
Cs2 H3A 3.2520 . ?
Cs2 O7 3.101(4) 8_654 ?
Cs2 O7 3.101(4) 6_456 ?
Cs2 O2 3.224(6) 4_664 ?
Cs2 O2 3.224(6) 2_566 ?
Cs2 H9 3.27(6) . ?
Cs2 O1 3.143(10) 2_566 ?
Cs2 O1 3.143(10) 4_664 ?
O4 C1 1.242(6) . ?
O6 H6A 0.9227 . ?
O6 H6B 0.8761 . ?
N1 C11 1.330(5) 2_566 ?
N1 C11 1.330(5) . ?
O8 C10 1.234(5) . ?
O8 Cs1A 3.103(4) . ?
O10 C7 1.281(5) . ?
O12 H12A 1.0132 . ?
O12 H12B 1.0832 . ?
O12 Cs1A 3.218(5) . ?
O3 H3A 0.8502 . ?
O3 H3B 0.8504 . ?
N2 C4 1.345(5) . ?
N2 C3 1.347(4) . ?
O7 C7 1.240(4) . ?
C1 C11 1.513(7) . ?
C1 O5 1.279(5) . ?
O9 C10 1.275(5) . ?
C4 C7 1.520(6) . ?
C4 C2 1.358(6) . ?
C6 H6 0.9500 . ?
C6 C2 1.334(7) . ?
C6 C9 1.355(6) . ?
C8 H8 0.9500 . ?
C8 C11 1.381(6) . ?
C8 C5 1.357(7) . ?
C10 C3 1.521(5) . ?
C3 C9 1.365(5) . ?
C2 H2 0.9500 . ?
C9 H9 0.84(6) . ?
C5 H5 0.9500 . ?
O11 H11A 0.85(8) 3_756 ?
O11 H11A 0.8505 . ?
O11 H11B 0.8497 . ?
O11 H11B 0.85(6) 3_756 ?
Cs1A O1 3.318(11) 4_664 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sm1 N2 119.36(6) . . ?
N1 Sm1 N2 119.36(6) . 2_566 ?
O10 Sm1 N1 76.18(7) 2_566 . ?
O10 Sm1 N1 76.18(7) . . ?
O10 Sm1 O10 152.37(13) 2_566 . ?
O10 Sm1 N2 62.75(9) . . ?
O10 Sm1 N2 133.80(10) 2_566 . ?
O10 Sm1 N2 133.79(10) . 2_566 ?
O10 Sm1 N2 62.75(9) 2_566 2_566 ?
N2 Sm1 N2 121.29(13) 2_566 . ?
O9 Sm1 N1 133.95(7) . . ?
O9 Sm1 N1 133.95(7) 2_566 . ?
O9 Sm1 O10 126.11(9) . . ?
O9 Sm1 O10 75.06(9) . 2_566 ?
O9 Sm1 O10 126.11(9) 2_566 2_566 ?
O9 Sm1 O10 75.06(9) 2_566 . ?
O9 Sm1 N2 63.37(9) 2_566 2_566 ?
O9 Sm1 N2 76.58(10) . 2_566 ?
O9 Sm1 N2 76.58(10) 2_566 . ?
O9 Sm1 N2 63.37(9) . . ?
O9 Sm1 O9 92.11(13) 2_566 . ?
O5 Sm1 N1 63.57(7) 2_566 . ?
O5 Sm1 N1 63.57(7) . . ?
O5 Sm1 O10 91.42(10) 2_566 . ?
O5 Sm1 O10 91.42(10) . 2_566 ?
O5 Sm1 O10 76.27(10) 2_566 2_566 ?
O5 Sm1 O10 76.27(10) . . ?
O5 Sm1 N2 74.45(10) 2_566 . ?
O5 Sm1 N2 74.45(10) . 2_566 ?
O5 Sm1 N2 134.79(10) . . ?
O5 Sm1 N2 134.79(10) 2_566 2_566 ?
O5 Sm1 O9 75.11(10) 2_566 . ?
O5 Sm1 O9 151.03(10) 2_566 2_566 ?
O5 Sm1 O9 75.11(10) . 2_566 ?
O5 Sm1 O9 151.03(10) . . ?
O5 Sm1 O5 127.13(15) 2_566 . ?
O4 Cs1 O6 67.60(10) 2_466 5_455 ?
O4 Cs1 H6B 74.2(6) 2_466 5_455 ?
O4 Cs1 O10 130.32(10) 2_466 4_664 ?
O4 Cs1 O12 117.63(14) 2_466 . ?
O4 Cs1 O2 76.24(15) 2_466 4_664 ?
O4 Cs1 O9 149.93(10) 2_466 3_655 ?
O4 Cs1 O5 100.48(11) 2_466 4_664 ?
O4 Cs1 O1 61.77(19) 2_466 4_664 ?
O6 Cs1 H6B 6.8(3) 5_455 5_455 ?
O6 Cs1 O10 83.28(9) 5_455 4_664 ?
O6 Cs1 O12 79.80(10) 5_455 . ?
O6 Cs1 O2 136.29(14) 5_455 4_664 ?
O6 Cs1 O9 134.35(9) 5_455 3_655 ?
O6 Cs1 O1 126.65(19) 5_455 4_664 ?
O8 Cs1 O4 85.75(9) . 2_466 ?
O8 Cs1 O6 116.76(10) . 5_455 ?
O8 Cs1 H6B 120.3(10) . 5_455 ?
O8 Cs1 O10 143.93(9) . 4_664 ?
O8 Cs1 O12 63.34(10) . . ?
O8 Cs1 O2 82.98(13) . 4_664 ?
O8 Cs1 O9 96.63(9) . 3_655 ?
O8 Cs1 O5 127.55(9) . 4_664 ?
O8 Cs1 O1 75.8(2) . 4_664 ?
O10 Cs1 H6B 77.2(3) 4_664 5_455 ?
O12 Cs1 H6B 77.5(13) . 5_455 ?
O12 Cs1 O10 94.09(10) . 4_664 ?
O12 Cs1 O2 140.88(14) . 4_664 ?
O12 Cs1 O9 89.61(11) . 3_655 ?
O12 Cs1 O1 138.8(2) . 4_664 ?
O2 Cs1 H6B 140.2(12) 4_664 5_455 ?
O2 Cs1 O10 103.36(13) 4_664 4_664 ?
O9 Cs1 H6B 127.64(13) 3_655 5_455 ?
O9 Cs1 O10 53.09(7) 3_655 4_664 ?
O9 Cs1 O2 74.33(14) 3_655 4_664 ?
O5 Cs1 O6 113.56(10) 4_664 5_455 ?
O5 Cs1 H6B 111.4(11) 4_664 5_455 ?
O5 Cs1 O10 54.86(8) 4_664 4_664 ?
O5 Cs1 O12 141.66(11) 4_664 . ?
O5 Cs1 O2 49.60(13) 4_664 4_664 ?
O5 Cs1 O9 54.74(7) 4_664 3_655 ?
O5 Cs1 O1 62.87(19) 4_664 4_664 ?
O6 Cs2 H3A 77.7 3_655 . ?
O6 Cs2 H9 117.3(12) 3_655 . ?
O8 Cs2 O6 162.36(9) . 3_655 ?
O8 Cs2 O6 124.69(9) 3_655 3_655 ?
O8 Cs2 O8 67.31(13) 3_655 . ?
O8 Cs2 H3A 136.6 3_655 . ?
O8 Cs2 H3A 102.4 . . ?
O8 Cs2 O7 89.11(10) . 6_456 ?
O8 Cs2 O7 89.11(10) 3_655 8_654 ?
O8 Cs2 O7 136.30(9) 3_655 6_456 ?
O8 Cs2 O7 136.30(9) . 8_654 ?
O8 Cs2 O2 70.96(13) 3_655 4_664 ?
O8 Cs2 O2 85.27(14) . 4_664 ?
O8 Cs2 O2 70.96(13) . 2_566 ?
O8 Cs2 O2 85.27(14) 3_655 2_566 ?
O8 Cs2 H9 116.2(12) 3_655 . ?
O8 Cs2 H9 48.9(12) . . ?
O8 Cs2 O1 82.44(19) . 2_566 ?
O8 Cs2 O1 78.1(2) 3_655 2_566 ?
O8 Cs2 O1 82.44(19) 3_655 4_664 ?
O8 Cs2 O1 78.1(2) . 4_664 ?
H3A Cs2 H9 68.1 . . ?
O7 Cs2 O6 73.34(9) 6_456 3_655 ?
O7 Cs2 O6 60.63(9) 8_654 3_655 ?
O7 Cs2 H3A 82.6 6_456 . ?
O7 Cs2 H3A 69.4 8_654 . ?
O7 Cs2 O7 129.70(14) 6_456 8_654 ?
O7 Cs2 O2 122.44(16) 6_456 2_566 ?
O7 Cs2 O2 70.87(15) 8_654 2_566 ?
O7 Cs2 O2 70.87(15) 6_456 4_664 ?
O7 Cs2 O2 122.44(16) 8_654 4_664 ?
O7 Cs2 H9 52.1(11) 6_456 . ?
O7 Cs2 H9 136.5(11) 8_654 . ?
O7 Cs2 O1 136.9(2) 6_456 2_566 ?
O7 Cs2 O1 136.9(2) 8_654 4_664 ?
O7 Cs2 O1 56.13(19) 6_456 4_664 ?
O7 Cs2 O1 56.13(19) 8_654 2_566 ?
O2 Cs2 O6 87.12(14) 4_664 3_655 ?
O2 Cs2 O6 119.94(13) 2_566 3_655 ?
O2 Cs2 H3A 52.5 2_566 . ?
O2 Cs2 H3A 152.4 4_664 . ?
O2 Cs2 O2 151.6(2) 2_566 4_664 ?
O2 Cs2 H9 99.8(11) 4_664 . ?
O2 Cs2 H9 76.4(11) 2_566 . ?
O1 Cs2 H3A 58.5 2_566 . ?
O1 Cs2 H3A 138.7 4_664 . ?
O1 Cs2 H9 93.2(11) 2_566 . ?
O1 Cs2 H9 83.8(11) 4_664 . ?
O1 Cs2 O1 156.6(4) 2_566 4_664 ?
Cs1 O4 Cs1 93.25(11) 2_666 4_665 ?
C1 O4 Cs1 123.3(4) . 2_666 ?
C1 O4 Cs1 81.5(3) . 4_665 ?
Cs1 O6 Cs1 89.12(10) 5_545 7_545 ?
Cs1 O6 Cs2 118.72(11) 5_545 . ?
Cs1 O6 H6A 38.4 7_545 . ?
Cs1 O6 H6A 119.5 5_545 . ?
Cs1 O6 H6B 96.6 7_545 . ?
Cs1 O6 H6B 18.9 5_545 . ?
Cs2 O6 Cs1 106.90(10) . 7_545 ?
Cs2 O6 H6A 106.7 . . ?
Cs2 O6 H6B 99.8 . . ?
H6A O6 H6B 132.5 . . ?
C11 N1 Sm1 120.5(3) . . ?
C11 N1 Sm1 120.5(3) 2_566 . ?
C11 N1 C11 118.9(5) . 2_566 ?
Cs1 O8 Cs1 100.63(10) . 3_655 ?
Cs1 O8 Cs1A 0.46(7) . . ?
Cs2 O8 Cs1 87.70(8) . 3_655 ?
Cs2 O8 Cs1 98.02(9) . . ?
Cs2 O8 Cs1A 98.44(10) . . ?
C10 O8 Cs1 137.3(3) . . ?
C10 O8 Cs1 80.6(2) . 3_655 ?
C10 O8 Cs2 124.6(3) . . ?
C10 O8 Cs1A 136.9(3) . . ?
Cs1A O8 Cs1 100.45(11) . 3_655 ?
Sm1 O10 Cs1 99.78(9) . 4_665 ?
C7 O10 Sm1 125.5(2) . . ?
C7 O10 Cs1 105.9(2) . 4_665 ?
Cs1 O12 H12A 110.6 . . ?
Cs1 O12 H12B 117.0 . . ?
H12A O12 H12B 100.0 . . ?
Cs1A O12 Cs1 0.49(7) . . ?
Cs1A O12 H12A 110.4 . . ?
Cs1A O12 H12B 117.5 . . ?
H3A O3 H3B 104.4 . . ?
C4 N2 Sm1 121.8(2) . . ?
C4 N2 C3 117.9(3) . . ?
C3 N2 Sm1 120.4(2) . . ?
C7 O7 Cs2 139.1(4) . 6_556 ?
Cs2 O2 Cs1 90.01(16) 2_566 4_665 ?
O4 C1 Cs1 78.3(3) . 4_665 ?
O4 C1 C11 119.6(4) . . ?
O4 C1 O5 125.3(5) . . ?
C11 C1 Cs1 135.9(3) . 4_665 ?
O5 C1 Cs1 62.4(2) . 4_665 ?
O5 C1 C11 115.0(4) . . ?
Sm1 O9 Cs1 102.54(9) . 3_655 ?
C10 O9 Sm1 124.7(2) . . ?
C10 O9 Cs1 93.4(2) . 3_655 ?
N2 C4 C7 113.3(3) . . ?
N2 C4 C2 121.9(3) . . ?
C2 C4 C7 124.8(3) . . ?
C2 C6 H6 119.1 . . ?
C2 C6 C9 121.8(4) . . ?
C9 C6 H6 119.1 . . ?
Cs1 C8 H8 45.6 2_666 . ?
C11 C8 Cs1 96.5(3) . 2_666 ?
C11 C8 H8 121.2 . . ?
C5 C8 Cs1 127.6(3) . 2_666 ?
C5 C8 H8 121.2 . . ?
C5 C8 C11 117.7(5) . . ?
Cs1 C10 Cs2 76.14(7) 3_655 . ?
O8 C10 Cs1 79.8(2) . 3_655 ?
O8 C10 Cs2 40.4(2) . . ?
O8 C10 O9 125.8(4) . . ?
O8 C10 C3 118.2(4) . . ?
O9 C10 Cs1 65.99(19) . 3_655 ?
O9 C10 Cs2 142.1(2) . . ?
O9 C10 C3 116.0(3) . . ?
C3 C10 Cs1 129.8(2) . 3_655 ?
C3 C10 Cs2 89.3(2) . . ?
N1 C11 C1 114.6(3) . . ?
N1 C11 C8 122.1(5) . . ?
C8 C11 C1 123.3(5) . . ?
N2 C3 C10 113.8(3) . . ?
N2 C3 C9 122.1(4) . . ?
C9 C3 C10 124.1(3) . . ?
O10 C7 C4 116.1(3) . . ?
O7 C7 O10 125.6(4) . . ?
O7 C7 C4 118.3(4) . . ?
Sm1 O5 Cs1 107.24(10) . 4_665 ?
C1 O5 Sm1 125.0(3) . . ?
C1 O5 Cs1 96.6(2) . 4_665 ?
C4 C2 H2 120.7 . . ?
C6 C2 C4 118.7(4) . . ?
C6 C2 H2 120.7 . . ?
Cs2 C9 H9 42(4) . . ?
C6 C9 Cs2 127.3(3) . . ?
C6 C9 C3 117.6(4) . . ?
C6 C9 H9 122(5) . . ?
C3 C9 Cs2 94.3(3) . . ?
C3 C9 H9 120(5) . . ?
C8 C5 C8 121.5(6) 2_566 . ?
C8 C5 H5 119.2 2_566 . ?
C8 C5 H5 119.2 . . ?
H11A O11 H11A 117.0 . 3_756 ?
H11A O11 H11B 104.5 3_756 3_756 ?
H11A O11 H11B 137.1 . 3_756 ?
H11A O11 H11B 104.5 . . ?
H11B O11 H11A 137.1 . 3_756 ?
H11B O11 H11B 40.0 . 3_756 ?
O4 Cs1A O6 67.75(12) 2_466 5_455 ?
O4 Cs1A H6B 74.2(6) 2_466 5_455 ?
O4 Cs1A O10 130.67(13) 2_466 4_664 ?
O4 Cs1A O12 117.72(17) 2_466 . ?
O4 Cs1A O2 75.72(17) 2_466 4_664 ?
O4 Cs1A O9 149.13(14) 2_466 3_655 ?
O4 Cs1A O5 100.12(13) 2_466 4_664 ?
O4 Cs1A O1 61.3(2) 2_466 4_664 ?
O6 Cs1A H6B 6.7(3) 5_455 5_455 ?
O6 Cs1A O10 83.94(10) 5_455 4_664 ?
O6 Cs1A O12 80.33(12) 5_455 . ?
O6 Cs1A O2 136.10(17) 5_455 4_664 ?
O6 Cs1A O9 135.23(12) 5_455 3_655 ?
O6 Cs1A O1 126.4(2) 5_455 4_664 ?
O8 Cs1A O4 85.26(11) . 2_466 ?
O8 Cs1A O6 116.89(14) . 5_455 ?
O8 Cs1A H6B 120.5(10) . 5_455 ?
O8 Cs1A O10 144.04(13) . 4_664 ?
O8 Cs1A O12 63.31(11) . . ?
O8 Cs1A O2 82.27(14) . 4_664 ?
O8 Cs1A O9 96.24(11) . 3_655 ?
O8 Cs1A O5 126.67(12) . 4_664 ?
O8 Cs1A O1 75.2(2) . 4_664 ?
O10 Cs1A H6B 77.9(4) 4_664 5_455 ?
O12 Cs1A H6B 78.1(13) . 5_455 ?
O12 Cs1A O10 94.72(12) . 4_664 ?
O12 Cs1A O2 140.24(17) . 4_664 ?
O12 Cs1A O9 89.82(13) . 3_655 ?
O12 Cs1A O1 138.1(2) . 4_664 ?
O2 Cs1A H6B 140.0(12) 4_664 5_455 ?
O2 Cs1A O10 103.22(15) 4_664 4_664 ?
O9 Cs1A H6B 128.57(16) 3_655 5_455 ?
O9 Cs1A O10 53.25(8) 3_655 4_664 ?
O9 Cs1A O2 73.96(14) 3_655 4_664 ?
O9 Cs1A O1 89.14(19) 3_655 4_664 ?
O5 Cs1A O6 114.02(13) 4_664 5_455 ?
O5 Cs1A H6B 111.9(11) 4_664 5_455 ?
O5 Cs1A O10 55.01(9) 4_664 4_664 ?
O5 Cs1A O12 142.06(15) 4_664 . ?
O5 Cs1A O2 49.32(13) 4_664 4_664 ?
O5 Cs1A O9 54.67(9) 4_664 3_655 ?
O5 Cs1A O1 62.49(19) 4_664 4_664 ?
Cs1 O1 H11A 114(2) 4_665 3_756 ?
Cs2 O1 Cs1 92.6(3) 2_566 4_665 ?
Cs2 O1 H11A 144(5) 2_566 3_756 ?

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
Sm1 N1 C11 C1 1.3(4) . . . . ?
Sm1 N1 C11 C8 -180.0(4) . . . . ?
Sm1 O10 C7 O7 -170.9(4) . . . . ?
Sm1 O10 C7 C4 9.3(5) . . . . ?
Sm1 N2 C4 C7 -1.4(4) . . . . ?
Sm1 N2 C4 C2 179.6(3) . . . . ?
Sm1 N2 C3 C10 0.7(4) . . . . ?
Sm1 N2 C3 C9 -179.0(3) . . . . ?
Sm1 O9 C10 Cs1 -107.9(2) . . . 3_655 ?
Sm1 O9 C10 Cs2 -110.8(3) . . . . ?
Sm1 O9 C10 O8 -163.7(3) . . . . ?
Sm1 O9 C10 C3 16.4(4) . . . . ?
Cs1 O4 C1 Cs1 88.3(3) 2_666 . . 4_665 ?
Cs1 O4 C1 C11 -48.2(5) 2_666 . . . ?
Cs1 O4 C1 C11 -136.5(4) 4_665 . . . ?
Cs1 O4 C1 O5 43.4(4) 4_665 . . . ?
Cs1 O4 C1 O5 131.7(4) 2_666 . . . ?
Cs1 O8 C10 Cs1 -95.5(3) . . . 3_655 ?
Cs1 O8 C10 Cs2 -176.1(6) . . . . ?
Cs1 O8 C10 Cs2 -80.6(2) 3_655 . . . ?
Cs1 O8 C10 O9 -45.3(6) . . . . ?
Cs1 O8 C10 O9 50.2(4) 3_655 . . . ?
Cs1 O8 C10 C3 134.6(3) . . . . ?
Cs1 O8 C10 C3 -129.9(3) 3_655 . . . ?
Cs1 O10 C7 O7 -56.1(5) 4_665 . . . ?
Cs1 O10 C7 C4 124.1(3) 4_665 . . . ?
Cs1 C1 C11 N1 66.0(5) 4_665 . . . ?
Cs1 C1 C11 C8 -112.7(5) 4_665 . . . ?
Cs1 C1 O5 Sm1 -116.4(3) 4_665 . . . ?
Cs1 O9 C10 Cs2 -2.9(4) 3_655 . . . ?
Cs1 O9 C10 O8 -55.9(4) 3_655 . . . ?
Cs1 O9 C10 C3 124.2(3) 3_655 . . . ?
Cs1 C8 C11 N1 -139.0(3) 2_666 . . . ?
Cs1 C8 C11 C1 39.6(5) 2_666 . . . ?
Cs1 C8 C5 C8 124.5(5) 2_666 . . 2_566 ?
Cs1 C10 C3 N2 69.1(4) 3_655 . . . ?
Cs1 C10 C3 C9 -111.2(4) 3_655 . . . ?
Cs2 O8 C10 Cs1 80.6(2) . . . 3_655 ?
Cs2 O8 C10 O9 130.8(3) . . . . ?
Cs2 O8 C10 C3 -49.3(4) . . . . ?
Cs2 O7 C7 O10 -50.8(7) 6_556 . . . ?
Cs2 O7 C7 C4 129.0(4) 6_556 . . . ?
Cs2 C10 C3 N2 140.3(3) . . . . ?
Cs2 C10 C3 C9 -40.0(4) . . . . ?
O4 C1 C11 N1 170.6(4) . . . . ?
O4 C1 C11 C8 -8.2(7) . . . . ?
O4 C1 O5 Sm1 -165.8(4) . . . . ?
O4 C1 O5 Cs1 -49.4(5) . . . 4_665 ?
O8 C10 C3 N2 169.7(3) . . . . ?
O8 C10 C3 C9 -10.6(6) . . . . ?
N2 C4 C7 O10 -4.7(5) . . . . ?
N2 C4 C7 O7 175.5(4) . . . . ?
N2 C4 C2 C6 1.8(7) . . . . ?
N2 C3 C9 Cs2 -139.3(3) . . . . ?
N2 C3 C9 C6 -2.9(7) . . . . ?
O9 C10 C3 N2 -10.4(5) . . . . ?
O9 C10 C3 C9 169.3(4) . . . . ?
C4 N2 C3 C10 -179.4(3) . . . . ?
C4 N2 C3 C9 0.8(6) . . . . ?
C10 C3 C9 Cs2 40.9(4) . . . . ?
C10 C3 C9 C6 177.4(5) . . . . ?
C11 N1 C11 C1 -178.7(4) 2_566 . . . ?
C11 N1 C11 C8 0.0(4) 2_566 . . . ?
C11 C1 O5 Sm1 14.1(5) . . . . ?
C11 C1 O5 Cs1 130.5(3) . . . 4_665 ?
C11 C8 C5 C8 0.0(4) . . . 2_566 ?
C3 N2 C4 C7 178.7(3) . . . . ?
C3 N2 C4 C2 -0.3(6) . . . . ?
C7 C4 C2 C6 -177.0(5) . . . . ?
O5 C1 C11 N1 -9.4(5) . . . . ?
O5 C1 C11 C8 171.9(5) . . . . ?
C2 C4 C7 O10 174.3(4) . . . . ?
C2 C4 C7 O7 -5.5(7) . . . . ?
C2 C6 C9 Cs2 124.8(5) . . . . ?
C2 C6 C9 C3 4.5(9) . . . . ?
C9 C6 C2 C4 -4.0(9) . . . . ?
C5 C8 C11 N1 -0.1(8) . . . . ?
C5 C8 C11 C1 178.5(4) . . . . ?
Cs1A O8 C10 Cs1 -95.3(3) . . . 3_655 ?
Cs1A O8 C10 Cs2 -175.9(6) . . . . ?
Cs1A O8 C10 O9 -45.1(6) . . . . ?
Cs1A O8 C10 C3 134.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.868(16)
2 0.132(16)

_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_mo_d8v5335_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2291819'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_mo_d8v5335_0m_a     
;
PROBLEM: D-H Bond Without Acceptor  O3       --H3D      .     Please Check
RESPONSE: The structure contains a lot of solvent molecules, which behave disordered. The position of the hydrogen atoms has been atempted to be optimised, such that the minimum ammount of alerts were created.
;
# Added during the CSD deposition process: Tuesday 23 April 2024 09:08 AM
# end Validation Reply Form

_audit_creation_date             2024-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H28 N4 Na O10 Sm, 3(H2 O)'
_chemical_formula_sum            'C16 H34 N4 Na O13 Sm'
_chemical_formula_weight         663.81
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.6233(8)
_cell_length_b                   9.1615(8)
_cell_length_c                   15.6526(14)
_cell_angle_alpha                82.938(3)
_cell_angle_beta                 84.975(3)
_cell_angle_gamma                80.994(3)
_cell_volume                     1209.13(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9647
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   0.818
_shelx_estimated_absorpt_T_min   0.528
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1064 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.8397.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             670
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.0400
1.00 0.00 0.00 0.0640
0.00 1.00 0.00 0.1280
0.00 -1.00 0.00 0.0580
0.00 0.00 1.00 0.0410
0.00 0.00 -1.00 0.0240

_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.083
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59699
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.030
_diffrn_reflns_theta_min         2.265
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Ventue'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7737
_reflns_number_total             8427
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0200
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)²+0.6614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0450
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9C,H9D), O5(H5C,H5D), O11(H11C,H11D)
2.b Rotating group:
 O12(H12A,H12B), O3(H3C)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C10(H10A,H10B), C12(H12C,H12D), C16(H16A,H16B),
 C2(H2A,H2B), C9(H9A,H9B), C5(H5A,H5B), C11(H11A,H11B), C3(H3A,H3B), C13(H13A,
 H13B), C7(H7A,H7B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.58961(2) 0.25049(2) 0.80734(2) 0.00535(2) Uani 1 1 d . . . . .
O1 O 0.80611(14) -0.01792(12) 1.03635(7) 0.0100(2) Uani 1 1 d . . . . .
O4 O 0.60353(14) 0.66996(12) 0.92554(8) 0.0118(2) Uani 1 1 d . . . . .
O6 O 0.53476(13) 0.48449(12) 0.86462(7) 0.0096(2) Uani 1 1 d . . . . .
O8 O 0.23928(14) 0.46991(13) 0.61954(8) 0.0137(2) Uani 1 1 d . . . . .
O10 O 0.68709(13) 0.16121(12) 0.94559(7) 0.0095(2) Uani 1 1 d . . . . .
O12 O 0.35599(13) 0.25657(12) 0.91185(7) 0.0101(2) Uani 1 1 d . . . . .
H12A H 0.381080 0.273896 0.961005 0.015 Uiso 1 1 d R U . . .
H12B H 0.327916 0.169938 0.921489 0.015 Uiso 1 1 d R U . . .
O13 O 0.50595(14) 0.01409(12) 0.80941(7) 0.0092(2) Uani 1 1 d . . . . .
O7 O 0.36540(14) 0.32954(12) 0.72573(7) 0.0105(2) Uani 1 1 d . . . . .
O2 O 0.38521(15) -0.13362(13) 0.74399(8) 0.0145(2) Uani 1 1 d . . . . .
O9 O 0.02394(15) 0.71941(14) 0.57794(9) 0.0186(3) Uani 1 1 d G . . . .
H9C H 0.073138 0.790603 0.583675 0.028 Uiso 1 1 d G U . . .
H9D H 0.090229 0.641552 0.588419 0.028 Uiso 1 1 d G U . . .
O5 O -0.20646(17) 1.07270(15) 0.40142(9) 0.0203(3) Uani 1 1 d G . . . .
H5C H -0.187776 0.978280 0.407790 0.031 Uiso 1 1 d G U . . .
H5D H -0.259545 1.093801 0.357080 0.031 Uiso 1 1 d G U . . .
N1 N 0.63509(15) 0.45522(14) 0.67504(8) 0.0075(2) Uani 1 1 d . . . . .
N4 N 0.85114(16) 0.05387(14) 0.80236(8) 0.0078(2) Uani 1 1 d . . . . .
N2 N 0.84393(15) 0.37809(14) 0.82056(8) 0.0077(2) Uani 1 1 d . . . . .
O11 O -0.1266(2) 0.76980(16) 0.42950(10) 0.0273(3) Uani 1 1 d G . . . .
H11C H -0.099215 0.742165 0.480418 0.041 Uiso 1 1 d G U . . .
H11D H -0.165251 0.696925 0.415460 0.041 Uiso 1 1 d G U . . .
N3 N 0.64496(16) 0.13405(14) 0.65569(8) 0.0080(2) Uani 1 1 d . . . . .
C1 C 0.85552(19) -0.04062(16) 0.88639(10) 0.0092(3) Uani 1 1 d . . . . .
H1A H 0.966541 -0.079466 0.897419 0.011 Uiso 1 1 calc R U . . .
H1B H 0.800888 -0.126774 0.882793 0.011 Uiso 1 1 calc R U . . .
C4 C 0.85161(19) -0.04308(17) 0.73270(10) 0.0103(3) Uani 1 1 d . . . . .
H4A H 0.777745 -0.115466 0.750776 0.012 Uiso 1 1 calc R U . . .
H4B H 0.958269 -0.099669 0.723791 0.012 Uiso 1 1 calc R U . . .
C6 C 0.63537(18) 0.54948(16) 0.89415(10) 0.0085(3) Uani 1 1 d . . . . .
C8 C 0.77968(18) 0.04071(16) 0.96186(10) 0.0080(3) Uani 1 1 d . . . . .
C10 C 0.73946(19) 0.55773(17) 0.69712(10) 0.0097(3) Uani 1 1 d . . . . .
H10A H 0.679937 0.626449 0.736577 0.012 Uiso 1 1 calc R U . . .
H10B H 0.773600 0.617997 0.643911 0.012 Uiso 1 1 calc R U . . .
C12 C 0.80412(19) 0.47022(17) 0.89255(10) 0.0100(3) Uani 1 1 d . . . . .
H12C H 0.876529 0.545159 0.887689 0.012 Uiso 1 1 calc R U . . .
H12D H 0.820181 0.406184 0.947718 0.012 Uiso 1 1 calc R U . . .
C14 C 0.35062(18) 0.43847(17) 0.66750(10) 0.0089(3) Uani 1 1 d . . . . .
C16 C 0.80435(19) 0.04595(18) 0.64834(10) 0.0107(3) Uani 1 1 d . . . . .
H16A H 0.881944 0.114149 0.628727 0.013 Uiso 1 1 calc R U . . .
H16B H 0.807215 -0.022961 0.604023 0.013 Uiso 1 1 calc R U . . .
C2 C 0.88360(19) 0.47288(18) 0.73996(10) 0.0107(3) Uani 1 1 d . . . . .
H2A H 0.946287 0.409294 0.698761 0.013 Uiso 1 1 calc R U . . .
H2B H 0.949799 0.544923 0.753513 0.013 Uiso 1 1 calc R U . . .
C9 C 0.98147(18) 0.26225(17) 0.84057(10) 0.0094(3) Uani 1 1 d . . . . .
H9A H 0.972712 0.224783 0.902619 0.011 Uiso 1 1 calc R U . . .
H9B H 1.079375 0.307320 0.828988 0.011 Uiso 1 1 calc R U . . .
C5 C 0.47837(18) 0.53913(17) 0.65714(10) 0.0098(3) Uani 1 1 d . . . . .
H5A H 0.482551 0.589690 0.597504 0.012 Uiso 1 1 calc R U . . .
H5B H 0.450666 0.616533 0.697058 0.012 Uiso 1 1 calc R U . . .
C11 C 0.63077(19) 0.25294(17) 0.58136(10) 0.0101(3) Uani 1 1 d . . . . .
H11A H 0.518123 0.286446 0.571940 0.012 Uiso 1 1 calc R U . . .
H11B H 0.681905 0.212078 0.528485 0.012 Uiso 1 1 calc R U . . .
C3 C 0.5231(2) 0.03846(17) 0.65402(10) 0.0106(3) Uani 1 1 d . . . . .
H3A H 0.564513 -0.040909 0.616893 0.013 Uiso 1 1 calc R U . . .
H3B H 0.430756 0.098856 0.627217 0.013 Uiso 1 1 calc R U . . .
C13 C 0.7069(2) 0.38468(17) 0.59746(10) 0.0105(3) Uani 1 1 d . . . . .
H13A H 0.820292 0.351183 0.604599 0.013 Uiso 1 1 calc R U . . .
H13B H 0.697649 0.459871 0.546316 0.013 Uiso 1 1 calc R U . . .
C7 C 0.99124(18) 0.13303(17) 0.78713(10) 0.0099(3) Uani 1 1 d . . . . .
H7A H 1.002784 0.170787 0.725221 0.012 Uiso 1 1 calc R U . . .
H7B H 1.086536 0.061256 0.800738 0.012 Uiso 1 1 calc R U . . .
C15 C 0.46879(19) -0.03380(17) 0.74232(10) 0.0094(3) Uani 1 1 d . . . . .
Na1 Na 0.36843(8) 0.82516(7) 0.89975(4) 0.01246(13) Uani 1 1 d . . . . .
O3 O 0.22504(19) 0.62718(18) 0.88496(13) 0.0268(3) Uani 1 1 d . . . . .
H3C H 0.308014 0.556786 0.879382 0.040 Uiso 1 1 d R U . . .
H3D H 0.192(5) 0.644(4) 0.846(2) 0.077(15) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O6 2.3884(11) . ?
Sm1 O10 2.3930(11) . ?
Sm1 O12 2.4794(11) . ?
Sm1 O13 2.3832(11) . ?
Sm1 O7 2.3793(12) . ?
Sm1 N1 2.6632(13) . ?
Sm1 N4 2.6587(13) . ?
Sm1 N2 2.6759(13) . ?
Sm1 N3 2.6953(13) . ?
O1 C8 1.2467(18) . ?
O1 Na1 2.3923(13) 2_667 ?
O4 C6 1.2450(18) . ?
O4 Na1 2.3226(14) . ?
O6 C6 1.2730(19) . ?
O8 C14 1.2469(19) . ?
O10 C8 1.2696(18) . ?
O10 Na1 2.4409(13) 2_667 ?
O12 H12A 0.8568 . ?
O12 H12B 0.8577 . ?
O13 C15 1.2705(19) . ?
O13 Na1 2.4797(13) 1_545 ?
O7 C14 1.2648(18) . ?
O2 C15 1.2464(19) . ?
O2 Na1 2.4159(14) 1_545 ?
O9 H9C 0.8493 . ?
O9 H9D 0.8500 . ?
O5 H5C 0.8498 . ?
O5 H5D 0.8506 . ?
N1 C10 1.487(2) . ?
N1 C5 1.478(2) . ?
N1 C13 1.4871(19) . ?
N4 C1 1.4830(19) . ?
N4 C4 1.4880(19) . ?
N4 C7 1.491(2) . ?
N2 C12 1.475(2) . ?
N2 C2 1.487(2) . ?
N2 C9 1.490(2) . ?
O11 H11C 0.8483 . ?
O11 H11D 0.8508 . ?
N3 C16 1.484(2) . ?
N3 C11 1.492(2) . ?
N3 C3 1.473(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C8 1.519(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C16 1.517(2) . ?
C6 C12 1.521(2) . ?
C8 Na1 2.7409(17) 2_667 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C2 1.521(2) . ?
C12 H12C 0.9900 . ?
C12 H12D 0.9900 . ?
C14 C5 1.530(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C7 1.519(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C13 1.517(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C15 1.525(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C15 Na1 2.7721(17) 1_545 ?
Na1 O3 2.3933(17) . ?
Na1 H3C 2.6535 . ?
Na1 H3D 2.67(4) . ?
O3 H3C 0.8910 . ?
O3 H3D 0.69(4) . ?

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
O6 Sm1 O10 84.09(4) . . ?
O6 Sm1 O12 69.54(4) . . ?
O6 Sm1 N1 74.04(4) . . ?
O6 Sm1 N4 130.77(4) . . ?
O6 Sm1 N2 65.50(4) . . ?
O6 Sm1 N3 141.09(4) . . ?
O10 Sm1 O12 73.80(4) . . ?
O10 Sm1 N1 139.69(4) . . ?
O10 Sm1 N4 65.63(4) . . ?
O10 Sm1 N2 72.46(4) . . ?
O10 Sm1 N3 130.56(4) . . ?
O12 Sm1 N1 125.95(4) . . ?
O12 Sm1 N4 129.68(4) . . ?
O12 Sm1 N2 125.47(4) . . ?
O12 Sm1 N3 130.13(4) . . ?
O13 Sm1 O6 144.65(4) . . ?
O13 Sm1 O10 86.69(4) . . ?
O13 Sm1 O12 75.11(4) . . ?
O13 Sm1 N1 129.84(4) . . ?
O13 Sm1 N4 74.10(4) . . ?
O13 Sm1 N2 142.21(4) . . ?
O13 Sm1 N3 65.86(4) . . ?
O7 Sm1 O6 87.34(4) . . ?
O7 Sm1 O10 147.06(4) . . ?
O7 Sm1 O12 73.39(4) . . ?
O7 Sm1 O13 82.13(4) . . ?
O7 Sm1 N1 66.27(4) . . ?
O7 Sm1 N4 138.36(4) . . ?
O7 Sm1 N2 131.38(4) . . ?
O7 Sm1 N3 71.66(4) . . ?
N1 Sm1 N2 67.75(4) . . ?
N1 Sm1 N3 67.63(4) . . ?
N4 Sm1 N1 104.33(4) . . ?
N4 Sm1 N2 68.68(4) . . ?
N4 Sm1 N3 67.56(4) . . ?
N2 Sm1 N3 104.34(4) . . ?
C8 O1 Na1 92.26(9) . 2_667 ?
C6 O4 Na1 120.55(10) . . ?
C6 O6 Sm1 125.46(10) . . ?
Sm1 O10 Na1 143.40(5) . 2_667 ?
C8 O10 Sm1 124.68(10) . . ?
C8 O10 Na1 89.47(9) . 2_667 ?
Sm1 O12 H12A 109.7 . . ?
Sm1 O12 H12B 109.8 . . ?
H12A O12 H12B 104.2 . . ?
Sm1 O13 Na1 143.84(5) . 1_545 ?
C15 O13 Sm1 122.99(10) . . ?
C15 O13 Na1 89.28(9) . 1_545 ?
C14 O7 Sm1 125.50(10) . . ?
C15 O2 Na1 92.80(10) . 1_545 ?
H9C O9 H9D 104.5 . . ?
H5C O5 H5D 104.5 . . ?
C10 N1 Sm1 110.86(9) . . ?
C10 N1 C13 108.85(12) . . ?
C5 N1 Sm1 106.50(9) . . ?
C5 N1 C10 109.80(12) . . ?
C5 N1 C13 109.84(12) . . ?
C13 N1 Sm1 110.98(9) . . ?
C1 N4 Sm1 107.76(9) . . ?
C1 N4 C4 108.54(12) . . ?
C1 N4 C7 110.49(12) . . ?
C4 N4 Sm1 110.94(9) . . ?
C4 N4 C7 109.30(12) . . ?
C7 N4 Sm1 109.79(9) . . ?
C12 N2 Sm1 106.00(9) . . ?
C12 N2 C2 109.90(12) . . ?
C12 N2 C9 109.76(12) . . ?
C2 N2 Sm1 111.68(9) . . ?
C2 N2 C9 109.24(12) . . ?
C9 N2 Sm1 110.21(9) . . ?
H11C O11 H11D 104.7 . . ?
C16 N3 Sm1 111.42(9) . . ?
C16 N3 C11 108.50(12) . . ?
C11 N3 Sm1 111.21(9) . . ?
C3 N3 Sm1 105.80(9) . . ?
C3 N3 C16 110.55(12) . . ?
C3 N3 C11 109.34(12) . . ?
N4 C1 H1A 108.9 . . ?
N4 C1 H1B 108.9 . . ?
N4 C1 C8 113.56(12) . . ?
H1A C1 H1B 107.7 . . ?
C8 C1 H1A 108.9 . . ?
C8 C1 H1B 108.9 . . ?
N4 C4 H4A 109.2 . . ?
N4 C4 H4B 109.2 . . ?
N4 C4 C16 111.96(12) . . ?
H4A C4 H4B 107.9 . . ?
C16 C4 H4A 109.2 . . ?
C16 C4 H4B 109.2 . . ?
O4 C6 O6 124.40(15) . . ?
O4 C6 C12 118.89(14) . . ?
O6 C6 C12 116.69(13) . . ?
O1 C8 O10 123.65(14) . . ?
O1 C8 C1 118.22(13) . . ?
O1 C8 Na1 60.71(8) . 2_667 ?
O10 C8 C1 118.05(13) . . ?
O10 C8 Na1 62.94(8) . 2_667 ?
C1 C8 Na1 176.63(10) . 2_667 ?
N1 C10 H10A 109.3 . . ?
N1 C10 H10B 109.3 . . ?
N1 C10 C2 111.49(12) . . ?
H10A C10 H10B 108.0 . . ?
C2 C10 H10A 109.3 . . ?
C2 C10 H10B 109.3 . . ?
N2 C12 C6 112.77(13) . . ?
N2 C12 H12C 109.0 . . ?
N2 C12 H12D 109.0 . . ?
C6 C12 H12C 109.0 . . ?
C6 C12 H12D 109.0 . . ?
H12C C12 H12D 107.8 . . ?
O8 C14 O7 124.75(15) . . ?
O8 C14 C5 118.46(14) . . ?
O7 C14 C5 116.79(14) . . ?
N3 C16 C4 112.88(13) . . ?
N3 C16 H16A 109.0 . . ?
N3 C16 H16B 109.0 . . ?
C4 C16 H16A 109.0 . . ?
C4 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
N2 C2 C10 113.27(13) . . ?
N2 C2 H2A 108.9 . . ?
N2 C2 H2B 108.9 . . ?
C10 C2 H2A 108.9 . . ?
C10 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N2 C9 H9A 109.3 . . ?
N2 C9 H9B 109.3 . . ?
N2 C9 C7 111.77(13) . . ?
H9A C9 H9B 107.9 . . ?
C7 C9 H9A 109.3 . . ?
C7 C9 H9B 109.3 . . ?
N1 C5 C14 112.13(12) . . ?
N1 C5 H5A 109.2 . . ?
N1 C5 H5B 109.2 . . ?
C14 C5 H5A 109.2 . . ?
C14 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N3 C11 H11A 109.4 . . ?
N3 C11 H11B 109.4 . . ?
N3 C11 C13 111.27(12) . . ?
H11A C11 H11B 108.0 . . ?
C13 C11 H11A 109.4 . . ?
C13 C11 H11B 109.4 . . ?
N3 C3 H3A 108.6 . . ?
N3 C3 H3B 108.6 . . ?
N3 C3 C15 114.62(13) . . ?
H3A C3 H3B 107.6 . . ?
C15 C3 H3A 108.6 . . ?
C15 C3 H3B 108.6 . . ?
N1 C13 C11 113.11(13) . . ?
N1 C13 H13A 109.0 . . ?
N1 C13 H13B 109.0 . . ?
C11 C13 H13A 109.0 . . ?
C11 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N4 C7 C9 113.46(12) . . ?
N4 C7 H7A 108.9 . . ?
N4 C7 H7B 108.9 . . ?
C9 C7 H7A 108.9 . . ?
C9 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
O13 C15 C3 118.68(13) . . ?
O13 C15 Na1 63.44(8) . 1_545 ?
O2 C15 O13 123.86(15) . . ?
O2 C15 C3 117.40(14) . . ?
O2 C15 Na1 60.51(8) . 1_545 ?
C3 C15 Na1 177.74(11) . 1_545 ?
O1 Na1 O10 54.62(4) 2_667 2_667 ?
O1 Na1 O13 90.25(4) 2_667 1_565 ?
O1 Na1 O2 112.24(5) 2_667 1_565 ?
O1 Na1 C8 27.03(4) 2_667 2_667 ?
O1 Na1 C15 103.30(5) 2_667 1_565 ?
O1 Na1 O3 108.74(5) 2_667 . ?
O1 Na1 H3C 127.0 2_667 . ?
O1 Na1 H3D 107.4(9) 2_667 . ?
O4 Na1 O1 139.51(5) . 2_667 ?
O4 Na1 O10 90.29(5) . 2_667 ?
O4 Na1 O13 92.17(5) . 1_565 ?
O4 Na1 O2 101.55(5) . 1_565 ?
O4 Na1 C8 115.75(5) . 2_667 ?
O4 Na1 C15 96.89(5) . 1_565 ?
O4 Na1 O3 94.71(6) . . ?
O4 Na1 H3C 75.9 . . ?
O4 Na1 H3D 103.0(9) . . ?
O10 Na1 O13 120.56(5) 2_667 1_565 ?
O10 Na1 C8 27.59(4) 2_667 2_667 ?
O10 Na1 C15 146.84(5) 2_667 1_565 ?
O10 Na1 H3C 103.3 2_667 . ?
O10 Na1 H3D 109.8(9) 2_667 . ?
O13 Na1 C8 106.57(5) 1_565 2_667 ?
O13 Na1 C15 27.28(4) 1_565 1_565 ?
O13 Na1 H3C 134.7 1_565 . ?
O13 Na1 H3D 127.1(8) 1_565 . ?
O2 Na1 O10 166.83(5) 1_565 2_667 ?
O2 Na1 O13 53.94(4) 1_565 1_565 ?
O2 Na1 C8 139.26(5) 1_565 2_667 ?
O2 Na1 C15 26.69(4) 1_565 1_565 ?
O2 Na1 H3C 85.4 1_565 . ?
O2 Na1 H3D 73.4(9) 1_565 . ?
C8 Na1 C15 126.65(5) 2_667 1_565 ?
C8 Na1 H3C 118.1 2_667 . ?
C8 Na1 H3D 111.1(9) 2_667 . ?
C15 Na1 H3C 109.9 1_565 . ?
C15 Na1 H3D 100.0(8) 1_565 . ?
O3 Na1 O10 98.66(6) . 2_667 ?
O3 Na1 O13 140.13(6) . 1_565 ?
O3 Na1 O2 86.23(6) . 1_565 ?
O3 Na1 C8 105.50(5) . 2_667 ?
O3 Na1 C15 112.86(6) . 1_565 ?
O3 Na1 H3C 19.5 . . ?
O3 Na1 H3D 14.3(8) . . ?
H3C Na1 H3D 28.0 . . ?
Na1 O3 H3C 97.0 . . ?
Na1 O3 H3D 107(3) . . ?
H3C O3 H3D 108.7 . . ?

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
Sm1 O6 C6 O4 -178.28(11) . . . . ?
Sm1 O6 C6 C12 -0.09(19) . . . . ?
Sm1 O10 C8 O1 -166.11(11) . . . . ?
Sm1 O10 C8 C1 10.48(19) . . . . ?
Sm1 O10 C8 Na1 -165.89(11) . . . 2_667 ?
Sm1 O13 C15 O2 -159.15(12) . . . . ?
Sm1 O13 C15 C3 18.20(19) . . . . ?
Sm1 O13 C15 Na1 -162.67(10) . . . 1_545 ?
Sm1 O7 C14 O8 172.66(12) . . . . ?
Sm1 O7 C14 C5 -8.41(19) . . . . ?
Sm1 N1 C10 C2 46.61(14) . . . . ?
Sm1 N1 C5 C14 -38.40(14) . . . . ?
Sm1 N1 C13 C11 44.53(15) . . . . ?
Sm1 N4 C1 C8 -32.14(14) . . . . ?
Sm1 N4 C4 C16 46.70(15) . . . . ?
Sm1 N4 C7 C9 43.69(14) . . . . ?
Sm1 N2 C12 C6 -39.38(14) . . . . ?
Sm1 N2 C2 C10 38.00(15) . . . . ?
Sm1 N2 C9 C7 42.94(14) . . . . ?
Sm1 N3 C16 C4 38.51(15) . . . . ?
Sm1 N3 C11 C13 42.02(14) . . . . ?
Sm1 N3 C3 C15 -31.43(15) . . . . ?
O4 C6 C12 N2 -151.50(14) . . . . ?
O6 C6 C12 N2 30.21(19) . . . . ?
O8 C14 C5 N1 -146.65(14) . . . . ?
O7 C14 C5 N1 34.34(19) . . . . ?
N1 C10 C2 N2 -58.69(17) . . . . ?
N4 C1 C8 O1 -165.07(13) . . . . ?
N4 C1 C8 O10 18.2(2) . . . . ?
N4 C4 C16 N3 -59.16(18) . . . . ?
N2 C9 C7 N4 -61.00(17) . . . . ?
N3 C11 C13 N1 -60.15(17) . . . . ?
N3 C3 C15 O13 13.6(2) . . . . ?
N3 C3 C15 O2 -168.85(14) . . . . ?
C1 N4 C4 C16 164.92(13) . . . . ?
C1 N4 C7 C9 -75.04(16) . . . . ?
C4 N4 C1 C8 -152.36(13) . . . . ?
C4 N4 C7 C9 165.59(13) . . . . ?
C10 N1 C5 C14 -158.48(12) . . . . ?
C10 N1 C13 C11 166.79(13) . . . . ?
C12 N2 C2 C10 -79.34(16) . . . . ?
C12 N2 C9 C7 159.33(13) . . . . ?
C16 N3 C11 C13 -80.86(15) . . . . ?
C16 N3 C3 C15 89.34(16) . . . . ?
C2 N2 C12 C6 81.44(15) . . . . ?
C2 N2 C9 C7 -80.11(15) . . . . ?
C9 N2 C12 C6 -158.39(12) . . . . ?
C9 N2 C2 C10 160.18(13) . . . . ?
C5 N1 C10 C2 164.01(13) . . . . ?
C5 N1 C13 C11 -72.97(16) . . . . ?
C11 N3 C16 C4 161.26(13) . . . . ?
C11 N3 C3 C15 -151.28(13) . . . . ?
C3 N3 C16 C4 -78.85(16) . . . . ?
C3 N3 C11 C13 158.50(13) . . . . ?
C13 N1 C10 C2 -75.73(15) . . . . ?
C13 N1 C5 C14 81.85(15) . . . . ?
C7 N4 C1 C8 87.81(15) . . . . ?
C7 N4 C4 C16 -74.51(16) . . . . ?
Na1 O1 C8 O10 0.22(16) 2_667 . . . ?
Na1 O1 C8 C1 -176.36(12) 2_667 . . . ?
Na1 O4 C6 O6 -17.4(2) . . . . ?
Na1 O4 C6 C12 164.48(11) . . . . ?
Na1 O10 C8 O1 -0.22(15) 2_667 . . . ?
Na1 O10 C8 C1 176.37(12) 2_667 . . . ?
Na1 O13 C15 O2 3.52(16) 1_545 . . . ?
Na1 O13 C15 C3 -179.13(13) 1_545 . . . ?
Na1 O2 C15 O13 -3.62(17) 1_545 . . . ?
Na1 O2 C15 C3 179.00(12) 1_545 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_mo_d8v5829_0m
_database_code_depnum_ccdc_archive 'CCDC 2291821'
loop_
_audit_author_name
_audit_author_address
'Sabina Svava Mortensen'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_audit_creation_date             2024-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H24 Na3 O21 Sm, 2(H2 O)'
_chemical_formula_sum            'C12 H28 Na3 O23 Sm'
_chemical_formula_weight         759.66
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   17.5900(13)
_cell_length_b                   8.3808(6)
_cell_length_c                   19.0418(16)
_cell_angle_alpha                90
_cell_angle_beta                 111.266(3)
_cell_angle_gamma                90
_cell_volume                     2616.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9607
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.44
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.644
_shelx_estimated_absorpt_T_min   0.436
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0982 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.8010.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1516
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.202
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46133
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.337
_diffrn_reflns_theta_min         2.295
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                9872
_reflns_number_total             10559
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.031(7)
_refine_ls_extinction_coef       0.00087(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         10559
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0226
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0130P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0437
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.969(7)
 0.031(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Na3-H7A \\sim Na3-H7B
 with sigma of 0.02
4.a Free rotating group:
 O7(H7A,H7B), O19(H19A,H19B), O5(H5C,H5D), O21(H21A,H21B), O11(H11A,H11B)
4.b Rotating group:
 O22(H22A,H22B), O23(H23A,H23B), O15(H15A,H15B)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C12(H12A,H12B), C3(H3A,H3B), C7(H7C,H7D), C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.00635(2) 0.44477(2) 0.50299(2) 0.00440(3) Uani 1 1 d . . . . .
Na1 Na 0.22809(13) 0.46241(17) 0.28323(12) 0.0084(3) Uani 1 1 d . . . . .
Na3 Na 0.78783(13) 0.43307(16) 0.72030(13) 0.0083(4) Uani 1 1 d D . . . .
O1 O 0.12578(17) 0.6007(4) 0.49945(15) 0.0076(5) Uani 1 1 d . . . . .
O4 O 0.70174(15) 0.5818(3) 0.61994(15) 0.0144(5) Uani 1 1 d . . . . .
O6 O 0.94049(16) 0.6483(3) 0.41145(16) 0.0089(5) Uani 1 1 d . . . . .
O8 O 0.62697(17) 0.8024(3) 0.58044(16) 0.0104(5) Uani 1 1 d . . . . .
O10 O 0.87484(15) 0.3290(3) 0.66130(15) 0.0096(5) Uani 1 1 d . . . . .
O12 O 0.17691(14) 0.7443(3) 0.68666(14) 0.0077(5) Uani 1 1 d . . . . .
O14 O 0.05468(17) 0.3725(3) 0.40497(17) 0.0094(5) Uani 1 1 d . . . . .
O16 O 0.50091(19) 0.64719(19) 0.49518(17) 0.0083(5) Uani 1 1 d . . . . .
O18 O 0.38249(17) 0.8298(3) 0.41748(16) 0.0100(5) Uani 1 1 d . . . . .
O20 O 0.96309(17) 0.3507(3) 0.60224(17) 0.0094(5) Uani 1 1 d . . . . .
O22 O 0.11586(18) 0.6615(3) 0.23826(18) 0.0134(6) Uani 1 1 d . . . . .
H22A H 0.080617 0.645041 0.260200 0.020 Uiso 1 1 d R U . . .
H22B H 0.087912 0.645540 0.190348 0.020 Uiso 1 1 d R U . . .
O23 O 0.21815(17) -0.0753(3) 0.28944(16) 0.0147(6) Uani 1 1 d . . . . .
H23A H 0.212335 -0.170947 0.269958 0.022 Uiso 1 1 d R U . . .
H23B H 0.236555 -0.082747 0.338568 0.022 Uiso 1 1 d R U . . .
O3 O 0.06485(16) 0.6339(3) 0.60308(16) 0.0092(5) Uani 1 1 d . . . . .
C1 C 0.8287(2) 0.6661(4) 0.4531(2) 0.0082(7) Uani 1 1 d . . . . .
H1A H 0.814405 0.771949 0.467863 0.010 Uiso 1 1 calc R U . . .
H1B H 0.778090 0.602258 0.432456 0.010 Uiso 1 1 calc R U . . .
O13 O 0.82196(15) 0.7402(3) 0.33114(15) 0.0115(5) Uani 1 1 d . . . . .
O7 O 0.89139(18) 0.6430(4) 0.76325(18) 0.0152(6) Uani 1 1 d G . . . .
H7A H 0.916995 0.680267 0.735336 0.023 Uiso 1 1 d DG U . . .
H7B H 0.928507 0.637630 0.808268 0.023 Uiso 1 1 d DG U . . .
O15 O 0.27877(16) 0.6052(3) 0.19897(15) 0.0141(5) Uani 1 1 d . . . . .
H15A H 0.315096 0.674586 0.224669 0.021 Uiso 1 1 d R U . . .
H15B H 0.239727 0.662664 0.167898 0.021 Uiso 1 1 d R U . . .
O2 O 0.14904(15) 0.3723(3) 0.35178(15) 0.0118(5) Uani 1 1 d . . . . .
C4 C 0.6370(2) 0.6516(4) 0.5846(2) 0.0089(7) Uani 1 1 d . . . . .
C6 C 0.8666(2) 0.6864(4) 0.3932(2) 0.0086(7) Uani 1 1 d . . . . .
C8 C 0.8478(3) 0.5248(5) 0.5662(3) 0.0117(7) Uani 1 1 d . . . . .
H8A H 0.793135 0.482385 0.536006 0.014 Uiso 1 1 calc R U . . .
H8B H 0.840827 0.610655 0.599037 0.014 Uiso 1 1 calc R U . . .
O17 O 0.88504(17) 0.5880(3) 0.51732(16) 0.0076(5) Uani 1 1 d . . . . .
C10 C 0.1196(2) 0.4235(4) 0.3976(2) 0.0067(7) Uani 1 1 d . . . . .
C12 C 0.5637(2) 0.5502(4) 0.5444(2) 0.0111(7) Uani 1 1 d . . . . .
H12A H 0.578437 0.465740 0.515293 0.013 Uiso 1 1 calc R U . . .
H12B H 0.544417 0.498171 0.581597 0.013 Uiso 1 1 calc R U . . .
C3 C 0.4249(2) 0.5663(4) 0.4602(3) 0.0116(7) Uani 1 1 d . . . . .
H3A H 0.407358 0.517470 0.499220 0.014 Uiso 1 1 calc R U . . .
H3B H 0.431193 0.480236 0.427135 0.014 Uiso 1 1 calc R U . . .
C7 C 0.1649(3) 0.5569(4) 0.4485(3) 0.0098(8) Uani 1 1 d . . . . .
H7C H 0.221578 0.522550 0.477333 0.012 Uiso 1 1 calc R U . . .
H7D H 0.167281 0.650531 0.417610 0.012 Uiso 1 1 calc R U . . .
C2 C 0.8999(2) 0.3922(4) 0.6145(2) 0.0086(6) Uani 1 1 d . . . . .
C9 C 0.1378(2) 0.6869(4) 0.6233(2) 0.0077(7) Uani 1 1 d . . . . .
C5 C 0.1785(2) 0.6788(4) 0.5664(2) 0.0074(6) Uani 1 1 d . . . . .
H5A H 0.191021 0.787943 0.553912 0.009 Uiso 1 1 calc R U . . .
H5B H 0.230390 0.619129 0.587714 0.009 Uiso 1 1 calc R U . . .
C11 C 0.3618(2) 0.6835(4) 0.4146(2) 0.0091(7) Uani 1 1 d . . . . .
O9 O 0.29339(14) 0.6320(3) 0.37671(14) 0.0135(5) Uani 1 1 d . . . . .
O19 O -0.00157(18) 0.2203(3) 0.19789(17) 0.0161(6) Uani 1 1 d G . . . .
H19A H 0.013159 0.288978 0.170966 0.024 Uiso 1 1 d G U . . .
H19B H -0.040920 0.161256 0.168398 0.024 Uiso 1 1 d G U . . .
O5 O 0.37846(15) 0.5045(3) 0.12332(14) 0.0176(5) Uani 1 1 d G . . . .
H5C H 0.344402 0.530661 0.145019 0.026 Uiso 1 1 d G U . . .
H5D H 0.391412 0.405958 0.136843 0.026 Uiso 1 1 d G U . . .
O21 O 0.08403(17) 0.0292(3) 0.37311(15) 0.0197(5) Uani 1 1 d G . . . .
H21A H 0.057631 0.111407 0.380388 0.030 Uiso 1 1 d G U . . .
H21B H 0.049924 -0.048084 0.353309 0.030 Uiso 1 1 d G U . . .
O11 O 1.00137(17) 0.7496(4) 0.30380(17) 0.0152(6) Uani 1 1 d G . . . .
H11A H 0.977050 0.724142 0.334738 0.023 Uiso 1 1 d G U . . .
H11B H 0.965552 0.728894 0.259341 0.023 Uiso 1 1 d G U . . .
Na2 Na 0.12963(7) 0.14110(13) 0.28283(7) 0.0110(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.496(3) . ?
Sm1 O6 2.414(3) 1_455 ?
Sm1 O8 2.415(3) 3_445 ?
Sm1 O14 2.392(3) . ?
Sm1 O16 2.4982(16) 3_445 ?
Sm1 O18 2.398(3) 3_445 ?
Sm1 O20 2.412(3) 1_455 ?
Sm1 O3 2.404(3) . ?
Sm1 O17 2.548(3) 1_455 ?
Na1 Na3 3.7998(16) 4_454 ?
Na1 O12 2.448(3) 2_564 ?
Na1 O22 2.488(4) . ?
Na1 O13 2.436(3) 3_445 ?
Na1 O15 2.416(3) . ?
Na1 O2 2.350(3) . ?
Na1 O9 2.241(3) . ?
Na1 Na2 3.200(2) . ?
Na3 O4 2.324(3) . ?
Na3 O10 2.369(3) . ?
Na3 O12 2.411(3) 3_545 ?
Na3 O23 2.414(3) 4 ?
Na3 O13 2.450(3) 2_565 ?
Na3 O7 2.450(4) . ?
Na3 Na2 3.457(3) 4 ?
O1 C7 1.427(5) . ?
O1 C5 1.433(5) . ?
O4 C4 1.239(5) . ?
O6 C6 1.259(5) . ?
O8 C4 1.275(4) . ?
O10 C2 1.247(5) . ?
O12 C9 1.249(5) . ?
O12 Na2 2.464(3) 2_565 ?
O14 C10 1.273(5) . ?
O16 C12 1.417(4) . ?
O16 C3 1.431(4) . ?
O18 C11 1.274(4) . ?
O20 C2 1.264(5) . ?
O22 H22A 0.8752 . ?
O22 H22B 0.8755 . ?
O23 H23A 0.8736 . ?
O23 H23B 0.8742 . ?
O23 Na2 2.364(3) . ?
O3 C9 1.278(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C6 1.524(5) . ?
C1 O17 1.424(5) . ?
O13 C6 1.243(5) . ?
O7 H7A 0.8698 . ?
O7 H7B 0.8702 . ?
O15 H15A 0.8714 . ?
O15 H15B 0.8712 . ?
O2 C10 1.242(4) . ?
O2 Na2 2.295(2) . ?
C4 C12 1.502(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 O17 1.421(5) . ?
C8 C2 1.520(6) . ?
C10 C7 1.504(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C11 1.500(5) . ?
C7 H7C 0.9900 . ?
C7 H7D 0.9900 . ?
C9 C5 1.501(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C11 O9 1.236(5) . ?
O19 H19A 0.8702 . ?
O19 H19B 0.8704 . ?
O19 Na2 2.382(3) . ?
O5 H5C 0.8701 . ?
O5 H5D 0.8705 . ?
O21 H21A 0.8694 . ?
O21 H21B 0.8705 . ?
O21 Na2 2.341(3) . ?
O11 H11A 0.8708 . ?
O11 H11B 0.8700 . ?
Na2 H23B 2.5953 . ?
Na2 H19A 2.6654 . ?
Na2 H21A 2.6122 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O16 122.39(10) . 3_445 ?
O1 Sm1 O17 120.14(6) . 1_455 ?
O6 Sm1 O1 78.38(9) 1_455 . ?
O6 Sm1 O8 151.11(9) 1_455 3_445 ?
O6 Sm1 O16 131.65(10) 1_455 3_445 ?
O6 Sm1 O17 62.82(9) 1_455 1_455 ?
O8 Sm1 O1 73.35(10) 3_445 . ?
O8 Sm1 O16 63.21(9) 3_445 3_445 ?
O8 Sm1 O17 138.76(10) 3_445 1_455 ?
O14 Sm1 O1 64.57(9) . . ?
O14 Sm1 O6 80.14(10) . 1_455 ?
O14 Sm1 O8 82.49(10) . 3_445 ?
O14 Sm1 O16 73.60(11) . 3_445 ?
O14 Sm1 O18 82.02(10) . 3_445 ?
O14 Sm1 O20 146.21(7) . 1_455 ?
O14 Sm1 O3 127.90(9) . . ?
O14 Sm1 O17 138.69(10) . 1_455 ?
O16 Sm1 O17 117.46(10) 3_445 1_455 ?
O18 Sm1 O1 139.31(9) 3_445 . ?
O18 Sm1 O6 73.37(9) 3_445 1_455 ?
O18 Sm1 O8 126.64(7) 3_445 3_445 ?
O18 Sm1 O16 63.44(9) 3_445 3_445 ?
O18 Sm1 O20 86.19(10) 3_445 1_455 ?
O18 Sm1 O3 145.60(9) 3_445 . ?
O18 Sm1 O17 70.85(10) 3_445 1_455 ?
O20 Sm1 O1 134.46(10) 1_455 . ?
O20 Sm1 O6 126.28(9) 1_455 1_455 ?
O20 Sm1 O8 79.46(10) 1_455 3_445 ?
O20 Sm1 O16 72.79(10) 1_455 3_445 ?
O20 Sm1 O17 63.60(9) 1_455 1_455 ?
O3 Sm1 O1 63.50(9) . . ?
O3 Sm1 O6 93.55(6) . 1_455 ?
O3 Sm1 O8 79.22(9) . 3_445 ?
O3 Sm1 O16 134.54(10) . 3_445 ?
O3 Sm1 O20 76.13(9) . 1_455 ?
O3 Sm1 O17 74.86(9) . 1_455 ?
O12 Na1 Na3 38.20(7) 2_564 4_454 ?
O12 Na1 O22 100.74(12) 2_564 . ?
O12 Na1 Na2 49.56(7) 2_564 . ?
O22 Na1 Na3 138.78(9) . 4_454 ?
O22 Na1 Na2 101.67(10) . . ?
O13 Na1 Na3 39.09(8) 3_445 4_454 ?
O13 Na1 O12 75.81(9) 3_445 2_564 ?
O13 Na1 O22 170.81(13) 3_445 . ?
O13 Na1 Na2 69.53(7) 3_445 . ?
O15 Na1 Na3 90.68(8) . 4_454 ?
O15 Na1 O12 88.59(12) . 2_564 ?
O15 Na1 O22 82.94(11) . . ?
O15 Na1 O13 105.32(12) . 3_445 ?
O15 Na1 Na2 138.14(11) . . ?
O2 Na1 Na3 100.47(8) . 4_454 ?
O2 Na1 O12 93.39(10) . 2_564 ?
O2 Na1 O22 81.45(12) . . ?
O2 Na1 O13 90.20(11) . 3_445 ?
O2 Na1 O15 164.36(13) . . ?
O2 Na1 Na2 45.75(7) . . ?
O9 Na1 Na3 133.06(8) . 4_454 ?
O9 Na1 O12 171.17(13) . 2_564 ?
O9 Na1 O22 87.84(11) . . ?
O9 Na1 O13 96.01(12) . 3_445 ?
O9 Na1 O15 90.41(11) . . ?
O9 Na1 O2 89.93(12) . . ?
O9 Na1 Na2 131.02(11) . . ?
Na2 Na1 Na3 58.44(5) . 4_454 ?
O4 Na3 Na1 123.71(8) . 4 ?
O4 Na3 O10 98.50(13) . . ?
O4 Na3 O12 84.85(12) . 3_545 ?
O4 Na3 O23 82.85(12) . 4 ?
O4 Na3 O13 155.40(13) . 2_565 ?
O4 Na3 O7 94.20(11) . . ?
O4 Na3 Na2 90.79(10) . 4 ?
O10 Na3 Na1 97.38(7) . 4 ?
O10 Na3 O12 103.42(10) . 3_545 ?
O10 Na3 O23 169.61(13) . 4 ?
O10 Na3 O13 101.05(11) . 2_565 ?
O10 Na3 O7 83.84(12) . . ?
O10 Na3 Na2 146.75(8) . 4 ?
O12 Na3 Na1 38.91(8) 3_545 4 ?
O12 Na3 O23 86.95(11) 3_545 4 ?
O12 Na3 O13 76.23(9) 3_545 2_565 ?
O12 Na3 O7 172.74(14) 3_545 . ?
O12 Na3 Na2 45.46(7) 3_545 4 ?
O23 Na3 Na1 90.32(8) 4 4 ?
O23 Na3 O13 80.62(12) 4 2_565 ?
O23 Na3 O7 85.79(11) 4 . ?
O23 Na3 Na2 43.08(7) 4 4 ?
O13 Na3 Na1 38.82(8) 2_565 4 ?
O13 Na3 Na2 64.73(8) 2_565 4 ?
O7 Na3 Na1 141.11(10) . 4 ?
O7 Na3 O13 102.58(13) . 2_565 ?
O7 Na3 Na2 127.46(11) . 4 ?
Na2 Na3 Na1 52.07(3) 4 4 ?
C7 O1 Sm1 120.1(2) . . ?
C7 O1 C5 114.0(3) . . ?
C5 O1 Sm1 119.6(2) . . ?
C4 O4 Na3 153.7(3) . . ?
C6 O6 Sm1 123.7(2) . 1_655 ?
C4 O8 Sm1 126.8(3) . 3 ?
C2 O10 Na3 129.8(2) . . ?
Na1 O12 Na2 81.31(9) 2_565 2_565 ?
Na3 O12 Na1 102.89(13) 3_455 2_565 ?
Na3 O12 Na2 90.32(10) 3_455 2_565 ?
C9 O12 Na1 112.1(2) . 2_565 ?
C9 O12 Na3 128.2(2) . 3_455 ?
C9 O12 Na2 130.7(2) . 2_565 ?
C10 O14 Sm1 126.0(2) . . ?
C12 O16 Sm1 122.0(2) . 3 ?
C12 O16 C3 114.1(2) . . ?
C3 O16 Sm1 120.7(2) . 3 ?
C11 O18 Sm1 126.2(2) . 3 ?
C2 O20 Sm1 127.1(2) . 1_655 ?
Na1 O22 H22A 109.9 . . ?
Na1 O22 H22B 109.4 . . ?
H22A O22 H22B 104.2 . . ?
Na3 O23 H23A 103.1 4_454 . ?
Na3 O23 H23B 123.7 4_454 . ?
H23A O23 H23B 109.2 . . ?
Na2 O23 Na3 92.70(10) . 4_454 ?
Na2 O23 H23A 135.1 . . ?
Na2 O23 H23B 95.3 . . ?
C9 O3 Sm1 124.2(2) . . ?
H1A C1 H1B 108.2 . . ?
C6 C1 H1A 109.7 . . ?
C6 C1 H1B 109.7 . . ?
O17 C1 H1A 109.7 . . ?
O17 C1 H1B 109.7 . . ?
O17 C1 C6 109.7(3) . . ?
Na1 O13 Na3 102.09(13) 3 2_564 ?
C6 O13 Na1 137.9(2) . 3 ?
C6 O13 Na3 118.5(2) . 2_564 ?
Na3 O7 H7A 122.8 . . ?
Na3 O7 H7B 119.5 . . ?
H7A O7 H7B 104.5 . . ?
Na1 O15 H15A 109.2 . . ?
Na1 O15 H15B 109.6 . . ?
H15A O15 H15B 104.4 . . ?
C10 O2 Na1 139.5(2) . . ?
C10 O2 Na2 132.9(2) . . ?
Na2 O2 Na1 87.07(10) . . ?
O4 C4 O8 125.5(4) . . ?
O4 C4 C12 117.3(3) . . ?
O8 C4 C12 117.1(3) . . ?
O6 C6 C1 117.0(3) . . ?
O13 C6 O6 125.9(4) . . ?
O13 C6 C1 117.1(3) . . ?
H8A C8 H8B 108.1 . . ?
O17 C8 H8A 109.6 . . ?
O17 C8 H8B 109.6 . . ?
O17 C8 C2 110.4(4) . . ?
C2 C8 H8A 109.6 . . ?
C2 C8 H8B 109.6 . . ?
C1 O17 Sm1 118.3(2) . 1_655 ?
C8 O17 Sm1 119.8(2) . 1_655 ?
C8 O17 C1 113.1(3) . . ?
O14 C10 C7 117.8(3) . . ?
O2 C10 O14 125.5(3) . . ?
O2 C10 C7 116.7(3) . . ?
O16 C12 C4 109.4(3) . . ?
O16 C12 H12A 109.8 . . ?
O16 C12 H12B 109.8 . . ?
C4 C12 H12A 109.8 . . ?
C4 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
O16 C3 H3A 109.8 . . ?
O16 C3 H3B 109.8 . . ?
O16 C3 C11 109.2(3) . . ?
H3A C3 H3B 108.3 . . ?
C11 C3 H3A 109.8 . . ?
C11 C3 H3B 109.8 . . ?
O1 C7 C10 110.8(3) . . ?
O1 C7 H7C 109.5 . . ?
O1 C7 H7D 109.5 . . ?
C10 C7 H7C 109.5 . . ?
C10 C7 H7D 109.5 . . ?
H7C C7 H7D 108.1 . . ?
O10 C2 O20 125.3(3) . . ?
O10 C2 C8 116.8(3) . . ?
O20 C2 C8 117.8(4) . . ?
O12 C9 O3 124.5(4) . . ?
O12 C9 C5 118.4(3) . . ?
O3 C9 C5 117.2(3) . . ?
O1 C5 C9 109.8(3) . . ?
O1 C5 H5A 109.7 . . ?
O1 C5 H5B 109.7 . . ?
C9 C5 H5A 109.7 . . ?
C9 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O18 C11 C3 117.8(3) . . ?
O9 C11 O18 124.3(3) . . ?
O9 C11 C3 117.9(3) . . ?
C11 O9 Na1 142.7(2) . . ?
H19A O19 H19B 109.5 . . ?
Na2 O19 H19A 99.3 . . ?
Na2 O19 H19B 128.9 . . ?
H5C O5 H5D 104.5 . . ?
H21A O21 H21B 109.5 . . ?
Na2 O21 H21A 98.3 . . ?
Na2 O21 H21B 110.2 . . ?
H11A O11 H11B 104.4 . . ?
Na1 Na2 Na3 69.49(5) . 4_454 ?
Na1 Na2 H23B 107.2 . . ?
Na1 Na2 H19A 82.5 . . ?
Na1 Na2 H21A 118.7 . . ?
Na3 Na2 H23B 57.1 4_454 . ?
Na3 Na2 H19A 106.8 4_454 . ?
Na3 Na2 H21A 152.4 4_454 . ?
O12 Na2 Na1 49.13(8) 2_564 . ?
O12 Na2 Na3 44.22(7) 2_564 4_454 ?
O12 Na2 H23B 101.3 2_564 . ?
O12 Na2 H19A 66.0 2_564 . ?
O12 Na2 H21A 161.3 2_564 . ?
O23 Na2 Na1 107.45(9) . . ?
O23 Na2 Na3 44.22(7) . 4_454 ?
O23 Na2 O12 86.85(9) . 2_564 ?
O23 Na2 H23B 19.6 . . ?
O23 Na2 O19 135.01(12) . . ?
O23 Na2 H19A 134.4 . . ?
O23 Na2 H21A 111.7 . . ?
H23B Na2 H19A 153.6 . . ?
H23B Na2 H21A 96.1 . . ?
O2 Na2 Na1 47.18(8) . . ?
O2 Na2 Na3 112.17(8) . 4_454 ?
O2 Na2 O12 94.35(9) . 2_564 ?
O2 Na2 O23 131.20(11) . . ?
O2 Na2 H23B 116.2 . . ?
O2 Na2 O19 93.42(11) . . ?
O2 Na2 H19A 88.6 . . ?
O2 Na2 O21 86.42(9) . . ?
O2 Na2 H21A 71.6 . . ?
O19 Na2 Na1 99.05(8) . . ?
O19 Na2 Na3 121.25(9) . 4_454 ?
O19 Na2 O12 83.79(10) . 2_564 ?
O19 Na2 H23B 149.2 . . ?
O19 Na2 H19A 18.8 . . ?
O19 Na2 H21A 84.8 . . ?
H19A Na2 H21A 100.5 . . ?
O21 Na2 Na1 131.66(8) . . ?
O21 Na2 Na3 135.56(8) . 4_454 ?
O21 Na2 O12 179.21(10) . 2_564 ?
O21 Na2 O23 92.76(10) . . ?
O21 Na2 H23B 78.5 . . ?
O21 Na2 O19 96.01(10) . . ?
O21 Na2 H19A 113.9 . . ?
O21 Na2 H21A 19.2 . . ?

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
Sm1 O1 C7 C10 5.2(5) . . . . ?
Sm1 O1 C5 C9 -15.2(4) . . . . ?
Sm1 O6 C6 C1 29.5(4) 1_655 . . . ?
Sm1 O6 C6 O13 -151.1(3) 1_655 . . . ?
Sm1 O8 C4 O4 173.6(3) 3 . . . ?
Sm1 O8 C4 C12 -7.7(5) 3 . . . ?
Sm1 O14 C10 O2 171.4(3) . . . . ?
Sm1 O14 C10 C7 -8.5(5) . . . . ?
Sm1 O16 C12 C4 -13.6(4) 3 . . . ?
Sm1 O16 C3 C11 15.4(4) 3 . . . ?
Sm1 O18 C11 C3 -9.9(5) 3 . . . ?
Sm1 O18 C11 O9 170.2(3) 3 . . . ?
Sm1 O20 C2 O10 171.9(3) 1_655 . . . ?
Sm1 O20 C2 C8 -5.1(5) 1_655 . . . ?
Sm1 O3 C9 O12 -157.4(3) . . . . ?
Sm1 O3 C9 C5 22.5(4) . . . . ?
Na1 O12 C9 O3 76.5(4) 2_565 . . . ?
Na1 O12 C9 C5 -103.4(3) 2_565 . . . ?
Na1 O13 C6 O6 -130.6(3) 3 . . . ?
Na1 O13 C6 C1 48.8(5) 3 . . . ?
Na1 O2 C10 O14 150.9(3) . . . . ?
Na1 O2 C10 C7 -29.2(6) . . . . ?
Na3 O4 C4 O8 105.4(6) . . . . ?
Na3 O4 C4 C12 -73.3(7) . . . . ?
Na3 O10 C2 O20 158.0(3) . . . . ?
Na3 O10 C2 C8 -24.9(5) . . . . ?
Na3 O12 C9 O3 -154.7(3) 3_455 . . . ?
Na3 O12 C9 C5 25.4(5) 3_455 . . . ?
Na3 O13 C6 O6 66.2(4) 2_564 . . . ?
Na3 O13 C6 C1 -114.4(3) 2_564 . . . ?
O4 C4 C12 O16 -168.1(3) . . . . ?
O8 C4 C12 O16 13.1(5) . . . . ?
O12 C9 C5 O1 176.5(3) . . . . ?
O14 C10 C7 O1 1.6(5) . . . . ?
O16 C3 C11 O18 -4.2(5) . . . . ?
O16 C3 C11 O9 175.7(3) . . . . ?
O18 C11 O9 Na1 120.2(4) . . . . ?
O3 C9 C5 O1 -3.5(5) . . . . ?
O2 C10 C7 O1 -178.3(3) . . . . ?
C6 C1 O17 Sm1 -15.9(4) . . . 1_655 ?
C6 C1 O17 C8 -163.4(3) . . . . ?
O17 C1 C6 O6 -6.8(4) . . . . ?
O17 C1 C6 O13 173.8(3) . . . . ?
O17 C8 C2 O10 178.4(4) . . . . ?
O17 C8 C2 O20 -4.3(6) . . . . ?
C12 O16 C3 C11 175.5(3) . . . . ?
C3 O16 C12 C4 -173.3(3) . . . . ?
C3 C11 O9 Na1 -59.7(6) . . . . ?
C7 O1 C5 C9 -167.4(3) . . . . ?
C2 C8 O17 Sm1 11.0(5) . . . 1_655 ?
C2 C8 O17 C1 157.9(3) . . . . ?
C5 O1 C7 C10 157.3(3) . . . . ?
Na2 O12 C9 O3 -21.2(5) 2_565 . . . ?
Na2 O12 C9 C5 158.8(2) 2_565 . . . ?
Na2 O2 C10 O14 -17.7(6) . . . . ?
Na2 O2 C10 C7 162.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.969(7)
2 0.031(7)

_exptl_crystal_preparation       Luminescent
