# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_e
_database_code_depnum_ccdc_archive 'CCDC 2179111'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT415_e                   
;
PROBLEM: Short Inter D-H..H-X       H5B      ..H15      .       1.72 Ang.
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT417_e                   
;
PROBLEM: Short Inter D-H..H-D       H6A      ..H7A      .       1.10 Ang.
RESPONSE: Author Response: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT972_e                   
;
PROBLEM: Check Calcd Resid. Dens.  0.82Ang From Am1            -4.70 eA-3
RESPONSE: Author Response: This negative residual density (-4.70 eA-3 0.82Ang from Am1 and -4.29 eA-3 0.82Ang from Am1) is located near a very heavy atom so there are absorption issues. The Level B Alert (-2.96 eA-3 1.26Ang from O6) is located In the region of the unit cell between two non coordinated water molecules on the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT972_e_2                 
;
PROBLEM: Check Calcd Resid. Dens.  0.82Ang From Am1            -4.29 eA-3
RESPONSE: Author Response: This negative residual density (-4.70 eA-3 0.82Ang from Am1 and -4.29 eA-3 0.82Ang from Am1) is located near a very heavy atom so there are absorption issues. The Level B Alert (-2.96 eA-3 1.26Ang from O6) is located In the region of the unit cell between two non coordinated water molecules on the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT420_e                   
;
PROBLEM: D-H Bond Without Acceptor  O5       --H5B      .     Please Check
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT971_e                   
;
PROBLEM: Check Calcd Resid. Dens.  1.59Ang From C5              2.81 eA-3
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT972_e_3                 
;
PROBLEM: Check Calcd Resid. Dens.  1.23Ang From O6             -2.96 eA-3
RESPONSE: This negative residual density (-4.70 eA-3 0.82Ang from Am1 and -4.29 eA-3 0.82Ang from Am1) is located near a very heavy atom so there are absorption issues. The Level B Alert (-2.96 eA-3 1.26Ang from O6) is located In the region of the unit cell between two non coordinated water molecules on the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT042_e                   
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ     Please Check
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT043_e                   
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       3.88 Check
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT342_e                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01017 Ang.
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT911_e                   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          8 Report
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT913_e                   
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          4 Note
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT971_e_2                 
;
PROBLEM: Check Calcd Resid. Dens.  1.70Ang From S3              2.36 eA-3
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT972_e_4                 
;
PROBLEM: Check Calcd Resid. Dens.  0.93Ang From Am1            -1.93 eA-3
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT975_e                   
;
PROBLEM: Check Calcd Resid. Dens.  0.84Ang From O4      .       1.15 eA-3
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT976_e                   
;
PROBLEM: Check Calcd Resid. Dens.  0.74Ang From O4      .      -1.39 eA-3
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT977_e                   
;
PROBLEM: Check Negative Difference Density on H3        .      -0.33 eA-3
RESPONSE: This positive residual density (2.81 eA-3 1.59Ang From C5) is located within a channel within the packing of the crystal structure and could possibly be a partially occupied water molecule, but it does not refine well. Please ignore automatically generated responses to Level C alerts
;
# Added during the CSD deposition process: Tuesday 14 June 2022 07:47 PM
# end Validation Reply Form

_audit_creation_date             2022-02-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[Am(mpo)2(u-O-mpo)(H2O)]2?3H2O'
_chemical_formula_moiety         'C15 H14 Am N3 O4 S3, 3(H2O)'
_chemical_formula_sum            'C15 H20 Am N3 O7 S3'
_chemical_formula_weight         693.52
_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'
Am Am -7.8990 4.5130 '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'
S S 0.1246 0.1234 '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                   8.3942(10)
_cell_length_b                   9.6982(10)
_cell_length_c                   13.6896(18)
_cell_angle_alpha                92.332(5)
_cell_angle_beta                 107.744(4)
_cell_angle_gamma                92.932(3)
_cell_volume                     1058.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   0.520
_shelx_estimated_absorpt_T_min   0.225
_exptl_absorpt_coefficient_mu    3.963
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1681 before and 0.1088 after correction.
The Ratio of minimum to maximum transmission is 0.5773.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.536
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54347
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.353
_diffrn_reflns_theta_min         2.552
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_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                5084
_reflns_number_total             5265
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.870
_refine_diff_density_min         -4.895
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0392
_refine_ls_restrained_S_all      1.178
_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)+(0.0198P)²+19.3672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0973
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Am1-H4A \\sim Am1-H4B
 with sigma of 0.02
3.a Free rotating group:
 O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C15(H15), C8(H8), C4(H4), C9(H9), C10(H10), C14(H14),
 C12(H12), C13(H13), C2(H2), C3(H3)
;
_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
Am1 Am 0.36198(2) 0.58923(2) 0.59074(2) 0.00988(7) Uani 1 1 d D . . . .
S2 S 0.39953(18) 0.88669(16) 0.58798(12) 0.0143(3) Uani 1 1 d . . . . .
S3 S 0.2513(2) 0.68643(18) 0.75873(13) 0.0200(3) Uani 1 1 d . . . . .
S1 S 0.71668(19) 0.64083(17) 0.71380(12) 0.0165(3) Uani 1 1 d . . . . .
O1 O 0.5515(5) 0.4117(4) 0.5700(3) 0.0123(8) Uani 1 1 d . . . . .
O3 O 0.3498(6) 0.4199(5) 0.7073(3) 0.0159(9) Uani 1 1 d . . . . .
O2 O 0.1221(5) 0.6857(4) 0.4831(3) 0.0135(8) Uani 1 1 d . . . . .
N1 N 0.6506(6) 0.3698(6) 0.6598(4) 0.0127(10) Uani 1 1 d . . . . .
O4 O 0.1694(6) 0.4020(5) 0.4897(4) 0.0191(9) Uani 1 1 d G . . . .
H4A H 0.070474 0.379801 0.494571 0.029 Uiso 1 1 d DG U . . .
H4B H 0.162539 0.375721 0.426898 0.029 Uiso 1 1 d DG U . . .
N2 N 0.1034(6) 0.8145(5) 0.4476(4) 0.0131(10) Uani 1 1 d . . . . .
N3 N 0.3334(7) 0.4302(6) 0.8014(4) 0.0141(10) Uani 1 1 d . . . . .
C5 C 0.6479(8) 0.2332(7) 0.6759(5) 0.0168(12) Uani 1 1 d . . . . .
H5 H 0.573624 0.170498 0.625224 0.020 Uiso 1 1 calc R U . . .
C6 C 0.2235(7) 0.9172(6) 0.4890(5) 0.0128(11) Uani 1 1 d . . . . .
C7 C 0.1945(8) 1.0475(7) 0.4476(5) 0.0164(12) Uani 1 1 d . . . . .
H7 H 0.273353 1.123592 0.475862 0.020 Uiso 1 1 calc R U . . .
C15 C 0.3649(9) 0.3165(7) 0.8570(5) 0.0192(13) Uani 1 1 d . . . . .
H15 H 0.397975 0.235873 0.828594 0.023 Uiso 1 1 calc R U . . .
C11 C 0.2850(8) 0.5494(7) 0.8359(5) 0.0151(11) Uani 1 1 d . . . . .
C8 C 0.0534(8) 1.0664(7) 0.3666(5) 0.0175(12) Uani 1 1 d . . . . .
H8 H 0.036915 1.154041 0.337837 0.021 Uiso 1 1 calc R U . . .
C4 C 0.7495(10) 0.1839(8) 0.7632(6) 0.0253(15) Uani 1 1 d . . . . .
H4 H 0.745819 0.087930 0.774353 0.030 Uiso 1 1 calc R U . . .
C9 C -0.0652(8) 0.9555(7) 0.3271(5) 0.0194(13) Uani 1 1 d . . . . .
H9 H -0.163605 0.967218 0.271933 0.023 Uiso 1 1 calc R U . . .
C10 C -0.0378(8) 0.8308(7) 0.3687(5) 0.0150(11) Uani 1 1 d . . . . .
H10 H -0.117474 0.754750 0.342538 0.018 Uiso 1 1 calc R U . . .
C14 C 0.3493(10) 0.3173(8) 0.9544(5) 0.0230(14) Uani 1 1 d . . . . .
H14 H 0.371187 0.237769 0.993442 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2691(9) 0.5502(8) 0.9359(5) 0.0208(13) Uani 1 1 d . . . . .
H12 H 0.235545 0.631309 0.963362 0.025 Uiso 1 1 calc R U . . .
C13 C 0.3008(9) 0.4368(8) 0.9944(5) 0.0224(14) Uani 1 1 d . . . . .
H13 H 0.289829 0.439997 1.061469 0.027 Uiso 1 1 calc R U . . .
C1 C 0.7446(8) 0.4673(7) 0.7327(5) 0.0142(11) Uani 1 1 d . . . . .
C2 C 0.8559(9) 0.4157(9) 0.8213(5) 0.0243(15) Uani 1 1 d . . . . .
H2 H 0.930085 0.478763 0.871665 0.029 Uiso 1 1 calc R U . . .
O5 O 0.4395(7) -0.0056(6) 0.8625(5) 0.0314(12) Uani 1 1 d G . . . .
H5A H 0.539953 -0.024081 0.898701 0.047 Uiso 1 1 d G U . . .
H5B H 0.454625 0.067441 0.830702 0.047 Uiso 1 1 d G U . . .
O6 O 0.2414(8) -0.0229(7) 0.9918(5) 0.0349(13) Uani 1 1 d G . . . .
H6A H 0.159543 -0.086521 0.978676 0.052 Uiso 1 1 d G U . . .
H6B H 0.282067 -0.032500 0.940781 0.052 Uiso 1 1 d G U . . .
O7 O 0.0642(8) 0.1724(7) 1.0729(5) 0.0369(14) Uani 1 1 d G . . . .
H7A H -0.025344 0.116648 1.058874 0.055 Uiso 1 1 d G U . . .
H7B H 0.135285 0.125781 1.052562 0.055 Uiso 1 1 d G U . . .
C3 C 0.8592(10) 0.2777(9) 0.8360(5) 0.0267(16) Uani 1 1 d . . . . .
H3 H 0.936032 0.245277 0.895644 0.032 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Am1 S2 2.8890(16) . ?
Am1 S3 2.8734(16) . ?
Am1 S1 2.9453(16) . ?
Am1 O1 2.519(4) 2_666 ?
Am1 O1 2.468(4) . ?
Am1 O3 2.355(5) . ?
Am1 O2 2.366(4) . ?
Am1 N1 3.254(5) . ?
Am1 N1 3.439(5) 2_666 ?
Am1 O4 2.441(5) . ?
Am1 H4A 3.0260 . ?
Am1 H4B 3.0166 . ?
Am1 N2 3.401(5) . ?
Am1 N3 3.391(5) . ?
S2 C6 1.721(6) . ?
S3 C11 1.713(7) . ?
S1 C1 1.730(7) . ?
O1 N1 1.349(6) . ?
O3 N3 1.337(6) . ?
O2 N2 1.358(7) . ?
N1 C5 1.352(8) . ?
N1 C1 1.371(8) . ?
O4 H4A 0.8703 . ?
O4 H4B 0.8702 . ?
N2 C6 1.353(8) . ?
N2 C10 1.360(8) . ?
N3 C15 1.357(9) . ?
N3 C11 1.358(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.361(9) . ?
C6 C7 1.409(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.380(9) . ?
C15 H15 0.9500 . ?
C15 C14 1.379(9) . ?
C11 C12 1.414(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.398(10) . ?
C4 H4 0.9500 . ?
C4 C3 1.396(12) . ?
C9 H9 0.9500 . ?
C9 C10 1.357(10) . ?
C10 H10 0.9500 . ?
C14 H14 0.9500 . ?
C14 C13 1.394(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.376(10) . ?
C13 H13 0.9500 . ?
C1 C2 1.414(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.362(12) . ?
O5 H5A 0.8699 . ?
O5 H5B 0.8704 . ?
O6 H6A 0.8703 . ?
O6 H6B 0.8701 . ?
O7 H7A 0.8702 . ?
O7 H7B 0.8697 . ?
C3 H3 0.9500 . ?

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
S2 Am1 S1 79.53(4) . . ?
S2 Am1 N1 78.49(10) . 2_666 ?
S2 Am1 N1 128.97(10) . . ?
S2 Am1 H4A 132.8 . . ?
S2 Am1 H4B 130.7 . . ?
S2 Am1 N2 49.54(9) . . ?
S2 Am1 N3 122.02(10) . . ?
S3 Am1 S2 76.33(5) . . ?
S3 Am1 S1 91.77(5) . . ?
S3 Am1 N1 112.43(10) . . ?
S3 Am1 N1 146.02(9) . 2_666 ?
S3 Am1 H4A 97.0 . . ?
S3 Am1 H4B 123.3 . . ?
S3 Am1 N2 86.39(9) . . ?
S3 Am1 N3 49.27(10) . . ?
S1 Am1 N1 51.02(10) . . ?
S1 Am1 N1 105.71(9) . 2_666 ?
S1 Am1 H4A 147.7 . . ?
S1 Am1 H4B 135.7 . . ?
S1 Am1 N2 127.98(10) . . ?
S1 Am1 N3 83.29(9) . . ?
O1 Am1 S2 130.03(11) . . ?
O1 Am1 S2 84.81(10) 2_666 . ?
O1 Am1 S3 160.60(10) 2_666 . ?
O1 Am1 S3 134.11(11) . . ?
O1 Am1 S1 89.20(10) 2_666 . ?
O1 Am1 S1 64.04(10) . . ?
O1 Am1 O1 62.87(17) . 2_666 ?
O1 Am1 N1 22.32(13) . . ?
O1 Am1 N1 82.98(13) 2_666 . ?
O1 Am1 N1 79.83(13) . 2_666 ?
O1 Am1 N1 19.29(12) 2_666 2_666 ?
O1 Am1 H4A 88.2 . . ?
O1 Am1 H4A 92.4 2_666 . ?
O1 Am1 H4B 66.7 2_666 . ?
O1 Am1 H4B 71.8 . . ?
O1 Am1 N2 139.43(13) . . ?
O1 Am1 N2 77.81(13) 2_666 . ?
O1 Am1 N3 149.87(13) 2_666 . ?
O1 Am1 N3 87.78(14) . . ?
O3 Am1 S2 138.96(11) . . ?
O3 Am1 S3 65.95(11) . . ?
O3 Am1 S1 85.87(12) . . ?
O3 Am1 O1 73.54(15) . . ?
O3 Am1 O1 133.43(15) . 2_666 ?
O3 Am1 O2 123.46(16) . . ?
O3 Am1 N1 142.55(14) . 2_666 ?
O3 Am1 N1 58.53(15) . . ?
O3 Am1 O4 74.23(16) . . ?
O3 Am1 H4A 69.8 . . ?
O3 Am1 H4B 85.4 . . ?
O3 Am1 N2 137.89(15) . . ?
O3 Am1 N3 17.22(14) . . ?
O2 Am1 S2 66.77(11) . . ?
O2 Am1 S3 86.04(12) . . ?
O2 Am1 S1 145.79(11) . . ?
O2 Am1 O1 82.33(14) . 2_666 ?
O2 Am1 O1 136.02(15) . . ?
O2 Am1 N1 63.06(14) . 2_666 ?
O2 Am1 N1 157.15(14) . . ?
O2 Am1 O4 71.29(16) . . ?
O2 Am1 H4A 66.1 . . ?
O2 Am1 H4B 70.0 . . ?
O2 Am1 N2 17.83(14) . . ?
O2 Am1 N3 119.07(14) . . ?
N1 Am1 N1 101.10(11) . 2_666 ?
N1 Am1 H4A 97.1 . . ?
N1 Am1 H4A 83.7 2_666 . ?
N1 Am1 H4B 61.2 2_666 . ?
N1 Am1 H4B 88.1 . . ?
N1 Am1 N2 160.78(12) . . ?
N1 Am1 N3 69.62(13) . . ?
O4 Am1 S2 136.97(12) . . ?
O4 Am1 S3 110.32(12) . . ?
O4 Am1 S1 139.87(12) . . ?
O4 Am1 O1 76.88(15) . . ?
O4 Am1 O1 80.52(15) . 2_666 ?
O4 Am1 N1 89.09(15) . . ?
O4 Am1 N1 74.43(15) . 2_666 ?
O4 Am1 H4A 13.6 . . ?
O4 Am1 H4B 13.8 . . ?
O4 Am1 N2 87.74(15) . . ?
O4 Am1 N3 86.58(15) . . ?
H4A Am1 H4B 26.3 . . ?
N2 Am1 N1 59.82(12) . 2_666 ?
N2 Am1 H4A 83.7 . . ?
N2 Am1 H4B 84.3 . . ?
N3 Am1 N1 159.20(13) . 2_666 ?
N3 Am1 H4A 79.2 . . ?
N3 Am1 H4B 99.1 . . ?
N3 Am1 N2 129.02(13) . . ?
C6 S2 Am1 100.7(2) . . ?
C11 S3 Am1 102.0(2) . . ?
Am1 S1 Am1 65.98(3) . 2_666 ?
C1 S1 Am1 70.6(2) . 2_666 ?
C1 S1 Am1 93.3(2) . . ?
Am1 O1 Am1 117.14(17) . 2_666 ?
N1 O1 Am1 113.7(3) . . ?
N1 O1 Am1 122.6(3) . 2_666 ?
N3 O3 Am1 131.4(4) . . ?
N2 O2 Am1 129.9(3) . . ?
Am1 N1 Am1 78.90(11) . 2_666 ?
O1 N1 Am1 38.1(2) . 2_666 ?
O1 N1 Am1 44.0(2) . . ?
O1 N1 C5 118.4(5) . . ?
O1 N1 C1 119.0(5) . . ?
C5 N1 Am1 108.7(4) . 2_666 ?
C5 N1 Am1 133.9(4) . . ?
C5 N1 C1 122.6(5) . . ?
C1 N1 Am1 88.7(4) . . ?
C1 N1 Am1 117.4(4) . 2_666 ?
Am1 O4 H4A 125.1 . . ?
Am1 O4 H4B 124.2 . . ?
H4A O4 H4B 104.5 . . ?
O2 N2 Am1 32.2(2) . . ?
O2 N2 C10 116.2(5) . . ?
C6 N2 Am1 88.5(3) . . ?
C6 N2 O2 120.0(5) . . ?
C6 N2 C10 123.7(6) . . ?
C10 N2 Am1 146.8(4) . . ?
O3 N3 Am1 31.4(3) . . ?
O3 N3 C15 116.4(5) . . ?
O3 N3 C11 120.0(5) . . ?
C15 N3 Am1 146.6(4) . . ?
C15 N3 C11 123.6(6) . . ?
C11 N3 Am1 89.4(4) . . ?
Am1 C5 H5 77.6 2_666 . ?
N1 C5 Am1 53.0(3) . 2_666 ?
N1 C5 H5 119.4 . . ?
N1 C5 C4 121.2(7) . . ?
C4 C5 Am1 144.3(5) . 2_666 ?
C4 C5 H5 119.4 . . ?
S2 C6 Am1 51.50(17) . . ?
N2 C6 Am1 69.6(3) . . ?
N2 C6 S2 120.6(5) . . ?
N2 C6 C7 116.4(6) . . ?
C7 C6 Am1 171.1(4) . . ?
C7 C6 S2 123.0(5) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.0(6) . . ?
C8 C7 H7 119.5 . . ?
N3 C15 H15 119.8 . . ?
N3 C15 C14 120.4(7) . . ?
C14 C15 H15 119.8 . . ?
S3 C11 Am1 50.59(17) . . ?
N3 C11 Am1 68.7(3) . . ?
N3 C11 S3 119.0(5) . . ?
N3 C11 C12 116.0(6) . . ?
C12 C11 Am1 172.3(5) . . ?
C12 C11 S3 124.9(5) . . ?
C7 C8 H8 120.3 . . ?
C7 C8 C9 119.5(6) . . ?
C9 C8 H8 120.3 . . ?
C5 C4 H4 120.8 . . ?
C5 C4 C3 118.5(7) . . ?
C3 C4 H4 120.8 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.1(6) . . ?
C10 C9 H9 120.4 . . ?
N2 C10 H10 119.9 . . ?
C9 C10 N2 120.2(6) . . ?
C9 C10 H10 119.9 . . ?
C15 C14 H14 120.6 . . ?
C15 C14 C13 118.8(7) . . ?
C13 C14 H14 120.6 . . ?
C11 C12 H12 119.1 . . ?
C13 C12 C11 121.8(6) . . ?
C13 C12 H12 119.1 . . ?
C14 C13 H13 120.3 . . ?
C12 C13 C14 119.4(6) . . ?
C12 C13 H13 120.3 . . ?
Am1 C1 Am1 65.79(10) . 2_666 ?
S1 C1 Am1 86.8(2) . 2_666 ?
S1 C1 Am1 57.11(18) . . ?
N1 C1 Am1 46.0(3) . 2_666 ?
N1 C1 Am1 68.3(3) . . ?
N1 C1 S1 119.5(5) . . ?
N1 C1 C2 115.9(6) . . ?
C2 C1 Am1 137.1(4) . 2_666 ?
C2 C1 Am1 153.8(5) . . ?
C2 C1 S1 124.6(5) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.5(7) . . ?
C3 C2 H2 119.2 . . ?
H5A O5 H5B 104.5 . . ?
H6A O6 H6B 104.5 . . ?
H7A O7 H7B 104.5 . . ?
C4 C3 H3 120.1 . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.1 . . ?

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
Am1 S2 C6 N2 9.3(5) . . . . ?
Am1 S2 C6 C7 -171.4(5) . . . . ?
Am1 S3 C11 N3 -6.6(5) . . . . ?
Am1 S3 C11 C12 172.2(5) . . . . ?
Am1 S1 C1 Am1 63.08(8) . . . 2_666 ?
Am1 S1 C1 Am1 -63.08(9) 2_666 . . . ?
Am1 S1 C1 N1 -33.8(4) 2_666 . . . ?
Am1 S1 C1 N1 29.3(5) . . . . ?
Am1 S1 C1 C2 -148.5(6) . . . . ?
Am1 S1 C1 C2 148.4(6) 2_666 . . . ?
Am1 O1 N1 Am1 -150.7(5) . . . 2_666 ?
Am1 O1 N1 Am1 150.7(5) 2_666 . . . ?
Am1 O1 N1 C5 -84.3(6) 2_666 . . . ?
Am1 O1 N1 C5 125.0(5) . . . . ?
Am1 O1 N1 C1 -52.4(6) . . . . ?
Am1 O1 N1 C1 98.3(5) 2_666 . . . ?
Am1 O3 N3 C15 -166.9(4) . . . . ?
Am1 O3 N3 C11 14.1(8) . . . . ?
Am1 O2 N2 C6 -13.2(7) . . . . ?
Am1 O2 N2 C10 165.4(4) . . . . ?
Am1 N1 C5 Am1 92.5(5) . . . 2_666 ?
Am1 N1 C5 C4 137.1(6) 2_666 . . . ?
Am1 N1 C5 C4 -130.4(6) . . . . ?
Am1 N1 C1 Am1 -76.8(2) . . . 2_666 ?
Am1 N1 C1 Am1 76.8(2) 2_666 . . . ?
Am1 N1 C1 S1 -26.3(4) . . . . ?
Am1 N1 C1 S1 50.5(6) 2_666 . . . ?
Am1 N1 C1 C2 151.7(5) . . . . ?
Am1 N1 C1 C2 -131.5(5) 2_666 . . . ?
Am1 N2 C6 S2 -7.8(4) . . . . ?
Am1 N2 C6 C7 172.9(5) . . . . ?
Am1 N2 C10 C9 -164.6(5) . . . . ?
Am1 N3 C15 C14 168.4(5) . . . . ?
Am1 N3 C11 S3 5.5(4) . . . . ?
Am1 N3 C11 C12 -173.4(5) . . . . ?
Am1 C5 C4 C3 68.0(11) 2_666 . . . ?
Am1 C1 C2 C3 88.3(12) . . . . ?
Am1 C1 C2 C3 -57.0(10) 2_666 . . . ?
S2 C6 C7 C8 178.4(5) . . . . ?
S3 C11 C12 C13 -178.9(6) . . . . ?
S1 C1 C2 C3 173.1(6) . . . . ?
O1 N1 C5 Am1 40.4(3) . . . 2_666 ?
O1 N1 C5 C4 177.5(6) . . . . ?
O1 N1 C1 Am1 -43.4(4) . . . 2_666 ?
O1 N1 C1 Am1 33.4(4) . . . . ?
O1 N1 C1 S1 7.1(7) . . . . ?
O1 N1 C1 C2 -174.9(5) . . . . ?
O3 N3 C15 C14 -179.3(6) . . . . ?
O3 N3 C11 Am1 -7.3(4) . . . . ?
O3 N3 C11 S3 -1.8(8) . . . . ?
O3 N3 C11 C12 179.3(6) . . . . ?
O2 N2 C6 Am1 7.0(4) . . . . ?
O2 N2 C6 S2 -0.8(8) . . . . ?
O2 N2 C6 C7 179.9(5) . . . . ?
O2 N2 C10 C9 -178.8(6) . . . . ?
N1 C5 C4 C3 -0.8(10) . . . . ?
N1 C1 C2 C3 -4.8(10) . . . . ?
N2 C6 C7 C8 -2.2(9) . . . . ?
N3 C15 C14 C13 -0.1(11) . . . . ?
N3 C11 C12 C13 0.0(10) . . . . ?
C5 N1 C1 Am1 139.3(7) . . . 2_666 ?
C5 N1 C1 Am1 -143.9(6) . . . . ?
C5 N1 C1 S1 -170.2(5) . . . . ?
C5 N1 C1 C2 7.8(9) . . . . ?
C5 C4 C3 C2 3.7(11) . . . . ?
C6 N2 C10 C9 -0.3(9) . . . . ?
C6 C7 C8 C9 2.0(10) . . . . ?
C7 C8 C9 C10 -0.8(10) . . . . ?
C15 N3 C11 Am1 173.8(6) . . . . ?
C15 N3 C11 S3 179.3(5) . . . . ?
C15 N3 C11 C12 0.4(9) . . . . ?
C15 C14 C13 C12 0.4(11) . . . . ?
C11 N3 C15 C14 -0.3(10) . . . . ?
C11 C12 C13 C14 -0.3(11) . . . . ?
C8 C9 C10 N2 -0.1(10) . . . . ?
C10 N2 C6 Am1 -171.5(6) . . . . ?
C10 N2 C6 S2 -179.3(5) . . . . ?
C10 N2 C6 C7 1.4(9) . . . . ?
C1 N1 C5 Am1 -142.4(7) . . . 2_666 ?
C1 N1 C5 C4 -5.2(10) . . . . ?
C1 C2 C3 C4 -0.8(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 2179113'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H16 Ho N3 O5 S3, H2 O'
_chemical_formula_sum            'C15 H18 Ho N3 O6 S3'
_chemical_formula_weight         597.43
_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'
Ho Ho -0.2175 4.6783 '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'
S S 0.1246 0.1234 '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                   7.4507(8)
_cell_length_b                   11.1249(13)
_cell_length_c                   13.1555(16)
_cell_angle_alpha                111.452(3)
_cell_angle_beta                 93.982(3)
_cell_angle_gamma                91.030(3)
_cell_volume                     1011.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.01
_shelx_estimated_absorpt_T_max   0.640
_shelx_estimated_absorpt_T_min   0.265
_exptl_absorpt_coefficient_mu    4.258
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1409 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.7846.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 -1.00 -1.00 0.1610
-1.00 1.00 1.00 0.1630
1.00 0.00 0.00 0.1860
0.00 0.00 1.00 0.0070
0.00 0.00 -1.00 0.0760
0.00 1.00 0.00 0.0950
0.00 -1.00 0.00 0.0150
1.00 1.00 1.00 0.1660
-1.00 -1.00 -1.00 0.1220
0.00 1.00 -1.00 0.1170
0.00 -1.00 1.00 0.0190

_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.115
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.232
_diffrn_reflns_theta_min         2.743
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                3834
_reflns_number_total             4439
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.131
_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)+(0.0122P)²+0.5442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0486
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Ho01-H5A \\sim Ho01-H5B
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C5(H5), C14(H14), C12(H12), C7(H7), C9(H9), C13(H13),
 C8(H8), C2(H2), C4(H4), C3(H3)
;
_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
Ho01 Ho 0.72477(2) 0.28362(2) 0.37057(2) 0.02249(6) Uani 1 1 d D . . . .
S3 S 0.53222(12) 0.05630(8) 0.22213(8) 0.0389(2) Uani 1 1 d . . . . .
S1 S 0.68462(13) 0.30952(8) 0.16764(7) 0.0395(2) Uani 1 1 d . . . . .
S2 S 0.73054(15) 0.13532(8) 0.50376(8) 0.0432(2) Uani 1 1 d . . . . .
O1 O 0.7009(3) 0.50037(19) 0.38914(16) 0.0290(5) Uani 1 1 d . . . . .
O2 O 0.7638(3) 0.4118(2) 0.55633(17) 0.0313(5) Uani 1 1 d . . . . .
O4 O 0.4215(3) 0.3105(2) 0.41382(19) 0.0347(5) Uani 1 1 d . . . . .
H4A H 0.377966 0.240506 0.416384 0.052 Uiso 1 1 d R U . . .
H4B H 0.418126 0.365337 0.478643 0.052 Uiso 1 1 d R U . . .
O5 O 1.0252(3) 0.3650(2) 0.3842(2) 0.0386(6) Uani 1 1 d G . . . .
H5A H 1.064961 0.443095 0.405390 0.058 Uiso 1 1 d DG U . . .
H5B H 1.112525 0.320883 0.354649 0.058 Uiso 1 1 d DG U . . .
O3 O 0.9132(3) 0.1192(2) 0.28537(18) 0.0349(5) Uani 1 1 d . . . . .
O6 O 0.2219(3) 0.1051(2) 0.4086(2) 0.0425(6) Uani 1 1 d G . . . .
H6A H 0.242961 0.050247 0.438450 0.064 Uiso 1 1 d G U . . .
H6B H 0.117853 0.088432 0.374433 0.064 Uiso 1 1 d G U . . .
N3 N 0.8799(4) 0.0227(2) 0.1876(2) 0.0283(6) Uani 1 1 d . . . . .
N2 N 0.7203(3) 0.3796(2) 0.6412(2) 0.0277(6) Uani 1 1 d . . . . .
N1 N 0.7571(3) 0.5474(2) 0.3151(2) 0.0275(6) Uani 1 1 d . . . . .
C11 C 0.7052(5) -0.0149(3) 0.1467(3) 0.0318(8) Uani 1 1 d . . . . .
C6 C 0.7002(4) 0.2519(3) 0.6281(3) 0.0327(8) Uani 1 1 d . . . . .
C10 C 0.6964(5) 0.4767(3) 0.7371(3) 0.0358(8) Uani 1 1 d . . . . .
H10 H 0.708752 0.561917 0.741766 0.043 Uiso 1 1 calc R U . . .
C15 C 1.0226(5) -0.0347(3) 0.1346(3) 0.0380(8) Uani 1 1 d . . . . .
H15 H 1.138800 -0.007675 0.166675 0.046 Uiso 1 1 calc R U . . .
C1 C 0.7587(4) 0.4675(3) 0.2077(3) 0.0324(8) Uani 1 1 d . . . . .
C5 C 0.8089(5) 0.6744(3) 0.3514(3) 0.0398(9) Uani 1 1 d . . . . .
H5 H 0.806537 0.725157 0.425270 0.048 Uiso 1 1 calc R U . . .
C14 C 0.9972(6) -0.1319(4) 0.0345(3) 0.0499(11) Uani 1 1 d . . . . .
H14 H 1.095290 -0.172397 -0.001432 0.060 Uiso 1 1 calc R U . . .
C12 C 0.6822(6) -0.1128(3) 0.0425(3) 0.0454(10) Uani 1 1 d . . . . .
H12 H 0.566059 -0.139786 0.010265 0.054 Uiso 1 1 calc R U . . .
C7 C 0.6541(5) 0.2275(4) 0.7208(3) 0.0442(9) Uani 1 1 d . . . . .
H7 H 0.637317 0.142286 0.715484 0.053 Uiso 1 1 calc R U . . .
C9 C 0.6547(5) 0.4522(4) 0.8267(3) 0.0431(9) Uani 1 1 d . . . . .
H9 H 0.640628 0.519554 0.892648 0.052 Uiso 1 1 calc R U . . .
C13 C 0.8242(7) -0.1694(4) -0.0128(3) 0.0541(11) Uani 1 1 d . . . . .
H13 H 0.804963 -0.233288 -0.082299 0.065 Uiso 1 1 calc R U . . .
C8 C 0.6334(5) 0.3247(4) 0.8180(3) 0.0488(10) Uani 1 1 d . . . . .
H8 H 0.605113 0.305636 0.878364 0.059 Uiso 1 1 calc R U . . .
C2 C 0.8194(5) 0.5244(4) 0.1362(3) 0.0485(10) Uani 1 1 d . . . . .
H2 H 0.825124 0.473431 0.062698 0.058 Uiso 1 1 calc R U . . .
C4 C 0.8643(5) 0.7281(4) 0.2804(4) 0.0521(11) Uani 1 1 d . . . . .
H4 H 0.897903 0.815606 0.305351 0.063 Uiso 1 1 calc R U . . .
C3 C 0.8702(6) 0.6522(5) 0.1717(4) 0.0585(12) Uani 1 1 d . . . . .
H3 H 0.908657 0.687858 0.122696 0.070 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho01 S3 2.8522(9) . ?
Ho01 S1 2.7847(9) . ?
Ho01 S2 2.8108(9) . ?
Ho01 O1 2.344(2) . ?
Ho01 O2 2.330(2) . ?
Ho01 O4 2.366(2) . ?
Ho01 O5 2.370(2) . ?
Ho01 O3 2.321(2) . ?
S3 C11 1.707(4) . ?
S1 C1 1.709(4) . ?
S2 C6 1.708(4) . ?
O1 N1 1.349(3) . ?
O2 N2 1.349(3) . ?
O4 H4A 0.8506 . ?
O4 H4B 0.8505 . ?
O5 H5A 0.8498 . ?
O5 H5B 0.8500 . ?
O3 N3 1.344(3) . ?
O6 H6A 0.8498 . ?
O6 H6B 0.8498 . ?
N3 C11 1.370(4) . ?
N3 C15 1.351(4) . ?
N2 C6 1.371(4) . ?
N2 C10 1.353(4) . ?
N1 C1 1.367(4) . ?
N1 C5 1.354(4) . ?
C11 C12 1.401(5) . ?
C6 C7 1.406(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.358(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.362(5) . ?
C1 C2 1.405(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.361(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.379(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.357(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.360(5) . ?
C9 H9 0.9300 . ?
C9 C8 1.385(5) . ?
C13 H13 0.9300 . ?
C8 H8 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.360(6) . ?
C4 H4 0.9300 . ?
C4 C3 1.374(6) . ?
C3 H3 0.9300 . ?

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
S1 Ho01 S3 72.88(3) . . ?
S1 Ho01 S2 152.24(3) . . ?
S2 Ho01 S3 80.88(3) . . ?
O1 Ho01 S3 130.22(6) . . ?
O1 Ho01 S1 68.34(5) . . ?
O1 Ho01 S2 138.59(5) . . ?
O1 Ho01 O4 80.92(8) . . ?
O1 Ho01 O5 74.76(8) . . ?
O2 Ho01 S3 141.28(5) . . ?
O2 Ho01 S1 139.78(5) . . ?
O2 Ho01 S2 67.88(5) . . ?
O2 Ho01 O1 71.65(7) . . ?
O2 Ho01 O4 79.29(8) . . ?
O2 Ho01 O5 79.21(8) . . ?
O4 Ho01 S3 74.79(6) . . ?
O4 Ho01 S1 98.02(6) . . ?
O4 Ho01 S2 83.39(6) . . ?
O4 Ho01 O5 151.55(8) . . ?
O5 Ho01 S3 132.81(6) . . ?
O5 Ho01 S1 86.63(7) . . ?
O5 Ho01 S2 105.33(7) . . ?
O3 Ho01 S3 67.31(6) . . ?
O3 Ho01 S1 84.70(6) . . ?
O3 Ho01 S2 76.83(6) . . ?
O3 Ho01 O1 135.59(8) . . ?
O3 Ho01 O2 123.23(8) . . ?
O3 Ho01 O4 139.37(8) . . ?
O3 Ho01 O5 68.85(8) . . ?
C11 S3 Ho01 98.54(11) . . ?
C1 S1 Ho01 98.65(11) . . ?
C6 S2 Ho01 100.63(11) . . ?
N1 O1 Ho01 123.07(16) . . ?
N2 O2 Ho01 127.29(16) . . ?
Ho01 O4 H4A 109.3 . . ?
Ho01 O4 H4B 109.3 . . ?
H4A O4 H4B 104.5 . . ?
Ho01 O5 H5A 128.9 . . ?
Ho01 O5 H5B 125.3 . . ?
H5A O5 H5B 104.5 . . ?
N3 O3 Ho01 127.12(17) . . ?
H6A O6 H6B 109.5 . . ?
O3 N3 C11 119.4(3) . . ?
O3 N3 C15 117.7(3) . . ?
C15 N3 C11 122.9(3) . . ?
O2 N2 C6 119.8(3) . . ?
O2 N2 C10 117.8(3) . . ?
C10 N2 C6 122.3(3) . . ?
O1 N1 C1 119.9(2) . . ?
O1 N1 C5 117.5(3) . . ?
C5 N1 C1 122.6(3) . . ?
N3 C11 S3 120.0(2) . . ?
N3 C11 C12 115.8(3) . . ?
C12 C11 S3 124.2(3) . . ?
N2 C6 S2 119.4(2) . . ?
N2 C6 C7 115.9(3) . . ?
C7 C6 S2 124.7(3) . . ?
N2 C10 H10 119.3 . . ?
N2 C10 C9 121.3(3) . . ?
C9 C10 H10 119.3 . . ?
N3 C15 H15 119.8 . . ?
N3 C15 C14 120.4(4) . . ?
C14 C15 H15 119.8 . . ?
N1 C1 S1 119.7(2) . . ?
N1 C1 C2 116.1(3) . . ?
C2 C1 S1 124.2(3) . . ?
N1 C5 H5 119.8 . . ?
N1 C5 C4 120.4(4) . . ?
C4 C5 H5 119.8 . . ?
C15 C14 H14 120.4 . . ?
C15 C14 C13 119.1(4) . . ?
C13 C14 H14 120.4 . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.0(4) . . ?
C13 C12 H12 119.0 . . ?
C6 C7 H7 119.0 . . ?
C8 C7 C6 122.0(3) . . ?
C8 C7 H7 119.0 . . ?
C10 C9 H9 120.7 . . ?
C10 C9 C8 118.7(3) . . ?
C8 C9 H9 120.7 . . ?
C14 C13 H13 120.1 . . ?
C12 C13 C14 119.8(4) . . ?
C12 C13 H13 120.1 . . ?
C7 C8 C9 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(4) . . ?
C3 C2 H2 119.1 . . ?
C5 C4 H4 120.2 . . ?
C5 C4 C3 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?

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
Ho01 S3 C11 N3 18.7(3) . . . . ?
Ho01 S3 C11 C12 -161.6(3) . . . . ?
Ho01 S1 C1 N1 -21.3(3) . . . . ?
Ho01 S1 C1 C2 160.1(3) . . . . ?
Ho01 S2 C6 N2 -13.9(3) . . . . ?
Ho01 S2 C6 C7 165.8(3) . . . . ?
Ho01 O1 N1 C1 28.0(3) . . . . ?
Ho01 O1 N1 C5 -152.6(2) . . . . ?
Ho01 O2 N2 C6 21.1(4) . . . . ?
Ho01 O2 N2 C10 -158.3(2) . . . . ?
Ho01 O3 N3 C11 -24.2(4) . . . . ?
Ho01 O3 N3 C15 156.9(2) . . . . ?
S3 C11 C12 C13 -177.7(3) . . . . ?
S1 C1 C2 C3 177.3(3) . . . . ?
S2 C6 C7 C8 179.4(3) . . . . ?
O1 N1 C1 S1 1.4(4) . . . . ?
O1 N1 C1 C2 -179.9(3) . . . . ?
O1 N1 C5 C4 -179.0(3) . . . . ?
O2 N2 C6 S2 -0.1(4) . . . . ?
O2 N2 C6 C7 -179.8(3) . . . . ?
O2 N2 C10 C9 -179.2(3) . . . . ?
O3 N3 C11 S3 -2.6(4) . . . . ?
O3 N3 C11 C12 177.7(3) . . . . ?
O3 N3 C15 C14 -179.1(3) . . . . ?
N3 C11 C12 C13 1.9(5) . . . . ?
N3 C15 C14 C13 1.1(5) . . . . ?
N2 C6 C7 C8 -0.9(5) . . . . ?
N2 C10 C9 C8 -1.2(5) . . . . ?
N1 C1 C2 C3 -1.3(5) . . . . ?
N1 C5 C4 C3 -1.0(6) . . . . ?
C11 N3 C15 C14 2.0(5) . . . . ?
C11 C12 C13 C14 1.0(6) . . . . ?
C6 N2 C10 C9 1.5(5) . . . . ?
C6 C7 C8 C9 1.2(6) . . . . ?
C10 N2 C6 S2 179.3(3) . . . . ?
C10 N2 C6 C7 -0.4(5) . . . . ?
C10 C9 C8 C7 -0.1(6) . . . . ?
C15 N3 C11 S3 176.2(2) . . . . ?
C15 N3 C11 C12 -3.4(4) . . . . ?
C15 C14 C13 C12 -2.5(6) . . . . ?
C1 N1 C5 C4 0.4(5) . . . . ?
C1 C2 C3 C4 0.7(6) . . . . ?
C5 N1 C1 S1 -178.0(3) . . . . ?
C5 N1 C1 C2 0.7(5) . . . . ?
C5 C4 C3 C2 0.5(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_b_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2179112'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[Eu(mpo)2(mu-O-mpo)(H2O)]2'
_chemical_formula_moiety         'C15 H14 Eu N3 O4 S3'
_chemical_formula_sum            'C15 H14 Eu N3 O4 S3'
_chemical_formula_weight         548.43
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.0543(13)
_cell_length_b                   9.9635(13)
_cell_length_c                   19.422(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.902(4)
_cell_angle_gamma                90
_cell_volume                     1938.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.88
_shelx_estimated_absorpt_T_max   0.619
_shelx_estimated_absorpt_T_min   0.359
_exptl_absorpt_coefficient_mu    3.583
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1235 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.8710.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.148
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83814
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.299
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                4218
_reflns_number_total             4822
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4822
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0253
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0059P)²+4.2713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0511
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C5(H5), C12(H12), C2(H2), C13(H13), C10(H10), C4(H4),
 C3(H3), C9(H9), C7(H7), C8(H8)
;
_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
Eu01 Eu 0.34497(2) 0.58588(2) 0.55142(2) 0.02544(4) Uani 1 1 d . . . . .
S1 S 0.07733(8) 0.59562(9) 0.59786(4) 0.03831(19) Uani 1 1 d . . . . .
S3 S 0.58641(9) 0.61012(10) 0.64761(4) 0.0421(2) Uani 1 1 d . . . . .
S2 S 0.37537(11) 0.86527(10) 0.57733(6) 0.0567(3) Uani 1 1 d . . . . .
O3 O 0.51196(19) 0.4065(2) 0.54531(9) 0.0271(4) Uani 1 1 d . . . . .
O2 O 0.2181(2) 0.7129(2) 0.47202(12) 0.0398(5) Uani 1 1 d . . . . .
O4 O 0.2303(2) 0.4239(2) 0.47612(12) 0.0414(5) Uani 1 1 d . . . . .
H4A H 0.273835 0.411479 0.441025 0.062 Uiso 1 1 d R U . . .
H4B H 0.156206 0.456773 0.459699 0.062 Uiso 1 1 d R U . . .
N3 N 0.5559(2) 0.3539(3) 0.60770(12) 0.0288(5) Uani 1 1 d . . . . .
O1 O 0.3119(2) 0.4535(3) 0.64582(14) 0.0609(9) Uani 1 1 d . . . . .
N1 N 0.2059(2) 0.4133(3) 0.67615(14) 0.0391(6) Uani 1 1 d . . . . .
N2 N 0.1929(3) 0.8438(3) 0.47008(17) 0.0468(8) Uani 1 1 d . . . . .
C15 C 0.5534(3) 0.2196(4) 0.6137(2) 0.0435(8) Uani 1 1 d . . . . .
H15 H 0.524450 0.166840 0.575875 0.052 Uiso 1 1 calc R U . . .
C14 C 0.5937(4) 0.1603(5) 0.6759(2) 0.0598(12) Uani 1 1 d . . . . .
H14 H 0.591936 0.067480 0.680700 0.072 Uiso 1 1 calc R U . . .
C1 C 0.0859(3) 0.4713(3) 0.65832(16) 0.0316(6) Uani 1 1 d . . . . .
C5 C 0.2237(4) 0.3166(5) 0.7250(2) 0.0566(11) Uani 1 1 d . . . . .
H5 H 0.308370 0.280659 0.735617 0.068 Uiso 1 1 calc R U . . .
C11 C 0.5945(3) 0.4392(4) 0.66041(15) 0.0357(7) Uani 1 1 d . . . . .
C12 C 0.6362(3) 0.3769(5) 0.72347(18) 0.0524(11) Uani 1 1 d . . . . .
H12 H 0.664416 0.430054 0.761295 0.063 Uiso 1 1 calc R U . . .
C2 C -0.0218(3) 0.4222(4) 0.6925(2) 0.0478(9) Uani 1 1 d . . . . .
H2 H -0.106675 0.456945 0.681006 0.057 Uiso 1 1 calc R U . . .
C13 C 0.6367(4) 0.2404(5) 0.7309(2) 0.0636(13) Uani 1 1 d . . . . .
H13 H 0.666033 0.201898 0.773106 0.076 Uiso 1 1 calc R U . . .
C6 C 0.2597(4) 0.9281(4) 0.5158(3) 0.0579(11) Uani 1 1 d . . . . .
C10 C 0.0997(5) 0.8858(5) 0.4202(3) 0.0745(14) Uani 1 1 d . . . . .
H10 H 0.056781 0.823963 0.390109 0.089 Uiso 1 1 calc R U . . .
C4 C 0.1203(4) 0.2716(5) 0.7587(2) 0.0619(12) Uani 1 1 d . . . . .
H4 H 0.133534 0.205716 0.792486 0.074 Uiso 1 1 calc R U . . .
C3 C -0.0053(4) 0.3246(4) 0.7421(2) 0.0570(11) Uani 1 1 d . . . . .
H3 H -0.077830 0.294475 0.764500 0.068 Uiso 1 1 calc R U . . .
C9 C 0.0692(6) 1.0180(6) 0.4142(4) 0.121(3) Uani 1 1 d . . . . .
H9 H 0.005058 1.047480 0.380195 0.145 Uiso 1 1 calc R U . . .
C7 C 0.2275(5) 1.0642(5) 0.5083(4) 0.108(2) Uani 1 1 d . . . . .
H7 H 0.270816 1.126684 0.537940 0.129 Uiso 1 1 calc R U . . .
C8 C 0.1332(6) 1.1066(6) 0.4582(5) 0.140(4) Uani 1 1 d . . . . .
H8 H 0.112841 1.197513 0.454349 0.168 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu01 Eu01 4.2072(5) 3_666 ?
Eu01 S1 2.9118(8) . ?
Eu01 S3 2.9438(9) . ?
Eu01 S2 2.8407(11) . ?
Eu01 O3 2.4631(19) 3_666 ?
Eu01 O3 2.4623(19) . ?
Eu01 O2 2.296(2) . ?
Eu01 O4 2.405(2) . ?
Eu01 H4A 2.8047 . ?
Eu01 H4B 2.8022 . ?
Eu01 O1 2.306(2) . ?
S1 C1 1.704(3) . ?
S3 C11 1.722(4) . ?
S2 C6 1.714(5) . ?
O3 N3 1.359(3) . ?
O2 N2 1.328(4) . ?
O4 H4A 0.8500 . ?
O4 H4B 0.8503 . ?
N3 C15 1.344(4) . ?
N3 C11 1.361(4) . ?
O1 N1 1.322(3) . ?
N1 C1 1.356(4) . ?
N1 C5 1.354(4) . ?
N2 C6 1.357(5) . ?
N2 C10 1.355(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.374(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.373(7) . ?
C1 C2 1.405(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.351(5) . ?
C11 C12 1.405(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.368(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.370(5) . ?
C13 H13 0.9300 . ?
C6 C7 1.399(6) . ?
C10 H10 0.9300 . ?
C10 C9 1.355(7) . ?
C4 H4 0.9300 . ?
C4 C3 1.382(5) . ?
C3 H3 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.354(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.366(9) . ?
C8 H8 0.9300 . ?

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
Eu01 Eu01 H4A 62.4 3_666 . ?
Eu01 Eu01 H4B 90.0 3_666 . ?
S1 Eu01 Eu01 154.49(2) . 3_666 ?
S1 Eu01 S3 122.31(3) . . ?
S1 Eu01 H4A 94.3 . . ?
S1 Eu01 H4B 67.6 . . ?
S3 Eu01 Eu01 74.36(2) . 3_666 ?
S3 Eu01 H4A 132.7 . . ?
S3 Eu01 H4B 156.6 . . ?
S2 Eu01 Eu01 114.19(3) . 3_666 ?
S2 Eu01 S1 90.04(3) . . ?
S2 Eu01 S3 74.74(3) . . ?
S2 Eu01 H4A 139.4 . . ?
S2 Eu01 H4B 128.3 . . ?
O3 Eu01 Eu01 31.34(4) . 3_666 ?
O3 Eu01 Eu01 31.32(4) 3_666 3_666 ?
O3 Eu01 S1 133.72(5) . . ?
O3 Eu01 S1 148.28(5) 3_666 . ?
O3 Eu01 S3 63.99(5) . . ?
O3 Eu01 S3 88.73(5) 3_666 . ?
O3 Eu01 S2 131.04(5) . . ?
O3 Eu01 S2 92.50(6) 3_666 . ?
O3 Eu01 O3 62.66(8) . 3_666 ?
O3 Eu01 H4A 69.1 . . ?
O3 Eu01 H4A 64.1 3_666 . ?
O3 Eu01 H4B 86.4 3_666 . ?
O3 Eu01 H4B 93.6 . . ?
O2 Eu01 Eu01 107.29(6) . 3_666 ?
O2 Eu01 S1 73.41(6) . . ?
O2 Eu01 S3 139.62(7) . . ?
O2 Eu01 S2 67.91(7) . . ?
O2 Eu01 O3 78.34(7) . 3_666 ?
O2 Eu01 O3 135.23(7) . . ?
O2 Eu01 O4 75.61(8) . . ?
O2 Eu01 H4A 74.8 . . ?
O2 Eu01 H4B 61.2 . . ?
O2 Eu01 O1 137.71(8) . . ?
O4 Eu01 Eu01 76.97(6) . 3_666 ?
O4 Eu01 S1 78.64(6) . . ?
O4 Eu01 S3 140.13(6) . . ?
O4 Eu01 S2 143.51(6) . . ?
O4 Eu01 O3 77.12(7) . . ?
O4 Eu01 O3 80.67(7) . 3_666 ?
O4 Eu01 H4A 16.6 . . ?
O4 Eu01 H4B 16.7 . . ?
H4A Eu01 H4B 27.7 . . ?
O1 Eu01 Eu01 107.94(7) . 3_666 ?
O1 Eu01 S1 64.70(6) . . ?
O1 Eu01 S3 73.12(7) . . ?
O1 Eu01 S2 116.13(9) . . ?
O1 Eu01 O3 139.26(8) . 3_666 ?
O1 Eu01 O3 76.61(8) . . ?
O1 Eu01 O4 90.31(11) . . ?
O1 Eu01 H4A 102.0 . . ?
O1 Eu01 H4B 96.1 . . ?
C1 S1 Eu01 101.28(10) . . ?
C11 S3 Eu01 92.10(11) . . ?
C6 S2 Eu01 100.26(15) . . ?
Eu01 O3 Eu01 117.34(8) . 3_666 ?
N3 O3 Eu01 121.71(15) . 3_666 ?
N3 O3 Eu01 114.08(15) . . ?
N2 O2 Eu01 130.8(2) . . ?
Eu01 O4 H4A 109.4 . . ?
Eu01 O4 H4B 109.2 . . ?
H4A O4 H4B 104.5 . . ?
O3 N3 C11 118.7(3) . . ?
C15 N3 O3 117.0(3) . . ?
C15 N3 C11 124.3(3) . . ?
N1 O1 Eu01 134.75(19) . . ?
O1 N1 C1 119.4(3) . . ?
O1 N1 C5 117.7(3) . . ?
C5 N1 C1 122.9(3) . . ?
O2 N2 C6 120.4(3) . . ?
O2 N2 C10 116.3(4) . . ?
C10 N2 C6 123.3(4) . . ?
N3 C15 H15 120.1 . . ?
N3 C15 C14 119.9(4) . . ?
C14 C15 H15 120.1 . . ?
C15 C14 H14 120.5 . . ?
C13 C14 C15 118.9(4) . . ?
C13 C14 H14 120.5 . . ?
N1 C1 S1 118.5(2) . . ?
N1 C1 C2 115.9(3) . . ?
C2 C1 S1 125.6(3) . . ?
N1 C5 H5 119.5 . . ?
C4 C5 N1 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
N3 C11 S3 120.2(2) . . ?
N3 C11 C12 115.1(3) . . ?
C12 C11 S3 124.7(3) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.0(4) . . ?
C13 C12 H12 119.0 . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(3) . . ?
C3 C2 H2 119.1 . . ?
C14 C13 H13 120.1 . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 H13 120.1 . . ?
N2 C6 S2 119.9(3) . . ?
N2 C6 C7 115.8(4) . . ?
C7 C6 S2 124.3(4) . . ?
N2 C10 H10 120.0 . . ?
N2 C10 C9 120.0(6) . . ?
C9 C10 H10 120.0 . . ?
C5 C4 H4 120.4 . . ?
C5 C4 C3 119.1(4) . . ?
C3 C4 H4 120.4 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C10 C9 H9 120.4 . . ?
C8 C9 C10 119.2(6) . . ?
C8 C9 H9 120.4 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 120.9(6) . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 120.8(5) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?

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
Eu01 S1 C1 N1 7.6(3) . . . . ?
Eu01 S1 C1 C2 -172.7(3) . . . . ?
Eu01 S3 C11 N3 34.4(2) . . . . ?
Eu01 S3 C11 C12 -144.1(3) . . . . ?
Eu01 S2 C6 N2 -4.1(4) . . . . ?
Eu01 S2 C6 C7 176.0(5) . . . . ?
Eu01 O3 N3 C15 129.3(2) . . . . ?
Eu01 O3 N3 C15 -80.5(3) 3_666 . . . ?
Eu01 O3 N3 C11 -48.2(3) . . . . ?
Eu01 O3 N3 C11 102.0(2) 3_666 . . . ?
Eu01 O2 N2 C6 8.8(5) . . . . ?
Eu01 O2 N2 C10 -172.0(3) . . . . ?
Eu01 O1 N1 C1 -11.7(5) . . . . ?
Eu01 O1 N1 C5 169.4(3) . . . . ?
S1 C1 C2 C3 -177.9(3) . . . . ?
S3 C11 C12 C13 178.0(3) . . . . ?
S2 C6 C7 C8 -179.5(6) . . . . ?
O3 N3 C15 C14 -178.6(3) . . . . ?
O3 N3 C11 S3 0.3(3) . . . . ?
O3 N3 C11 C12 178.9(2) . . . . ?
O2 N2 C6 S2 -1.1(5) . . . . ?
O2 N2 C6 C7 178.8(4) . . . . ?
O2 N2 C10 C9 -179.3(5) . . . . ?
N3 C15 C14 C13 -0.3(6) . . . . ?
N3 C11 C12 C13 -0.5(5) . . . . ?
O1 N1 C1 S1 -0.7(4) . . . . ?
O1 N1 C1 C2 179.5(3) . . . . ?
O1 N1 C5 C4 179.3(4) . . . . ?
N1 C1 C2 C3 1.9(6) . . . . ?
N1 C5 C4 C3 0.6(8) . . . . ?
N2 C6 C7 C8 0.6(9) . . . . ?
N2 C10 C9 C8 0.3(11) . . . . ?
C15 N3 C11 S3 -177.0(2) . . . . ?
C15 N3 C11 C12 1.5(4) . . . . ?
C15 C14 C13 C12 1.3(6) . . . . ?
C1 N1 C5 C4 0.6(7) . . . . ?
C1 C2 C3 C4 -0.8(7) . . . . ?
C5 N1 C1 S1 178.0(3) . . . . ?
C5 N1 C1 C2 -1.8(5) . . . . ?
C5 C4 C3 C2 -0.5(8) . . . . ?
C11 N3 C15 C14 -1.2(5) . . . . ?
C11 C12 C13 C14 -0.9(6) . . . . ?
C6 N2 C10 C9 -0.1(8) . . . . ?
C6 C7 C8 C9 -0.4(12) . . . . ?
C10 N2 C6 S2 179.7(4) . . . . ?
C10 N2 C6 C7 -0.4(7) . . . . ?
C10 C9 C8 C7 -0.1(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2179117'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT350_a                   
;
PROBLEM: Short  C-H (X0.96,N1.08A)  C8       - H9B      .       0.45 Ang.
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT722_a                   
;
PROBLEM: Angle   Calc       63.00, Rep      59(10) Dev...       4.00 Degree
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT770_a                   
;
PROBLEM: Suspect C-H Bond in CIF:  C9       --H9B       .       1.50 Ang.
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT351_a                   
;
PROBLEM: Long   C-H (X0.96,N1.08A)  C7       - H9B      .       1.20 Ang.
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
_vrf_PLAT722_a_2                 
;
PROBLEM: Angle   Calc       89.00, Rep      92(10) Dev...       3.00 Degree
RESPONSE: Hydrogen atoms on non coordinated water molecules are refined on calculated positions not actual positions. The electron density of the hydrogen atoms on the non coordinated water molecules are not observed in the differences map. Please ignore automatically generated responses to Level C alerts
;
# Added during the CSD deposition process: Tuesday 14 June 2022 07:47 PM
# end Validation Reply Form

_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H17 Lu N3 O5 S3, H2 O'
_chemical_formula_sum            'C15 H19 Lu N3 O6 S3'
_chemical_formula_weight         608.48
_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'
Lu Lu -0.4720 5.8584 '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'
S S 0.1246 0.1234 '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                   7.4092(3)
_cell_length_b                   11.0676(5)
_cell_length_c                   13.0778(6)
_cell_angle_alpha                111.325(2)
_cell_angle_beta                 94.072(2)
_cell_angle_gamma                91.141(2)
_cell_volume                     995.25(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.760
_shelx_estimated_absorpt_T_max   0.473
_shelx_estimated_absorpt_T_min   0.191
_exptl_absorpt_coefficient_mu    5.312
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.0712 after correction. The Ratio of minimum to maximum transmission is 0.6033. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             594
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.166
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            72598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.562
_diffrn_reflns_theta_min         2.759
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                4314
_reflns_number_total             4577
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4577
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.087
_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)+(0.0173P)²+0.9843P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0408
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Lu1-H5A \\sim Lu1-H5B
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C5(H5), C14(H14), C12(H12), C9(H9A), C7(H7), C13(H13),
 C8(H8), C2(H2), C4(H4), C3(H3)
;
_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
Lu1 Lu 0.72465(2) 0.28436(2) 0.37186(2) 0.02002(4) Uani 1 1 d D . . . .
S3 S 0.52929(9) 0.05861(7) 0.22635(6) 0.03529(15) Uani 1 1 d . . . . .
S1 S 0.68764(11) 0.30537(7) 0.16907(5) 0.03664(15) Uani 1 1 d . . . . .
S2 S 0.73172(12) 0.13721(6) 0.50308(6) 0.03896(16) Uani 1 1 d . . . . .
O2 O 0.7638(3) 0.41360(17) 0.55487(14) 0.0295(4) Uani 1 1 d . . . . .
O1 O 0.7002(2) 0.49798(16) 0.38938(14) 0.0266(4) Uani 1 1 d . . . . .
O4 O 0.4255(2) 0.31183(18) 0.41376(17) 0.0323(4) Uani 1 1 d . . . . .
H4A H 0.381319 0.242449 0.418057 0.048 Uiso 1 1 d R U . . .
H4B H 0.422267 0.368565 0.478229 0.048 Uiso 1 1 d R U . . .
O3 O 0.9122(2) 0.12190(17) 0.28876(15) 0.0323(4) Uani 1 1 d . . . . .
O5 O 1.0220(2) 0.36383(18) 0.38660(18) 0.0345(4) Uani 1 1 d G . . . .
H5A H 1.065348 0.441713 0.412509 0.052 Uiso 1 1 d DG U . . .
H5B H 1.108510 0.319421 0.355509 0.052 Uiso 1 1 d DG U . . .
O6 O 0.2237(3) 0.1065(2) 0.4110(2) 0.0396(5) Uani 1 1 d G . . . .
H6A H 0.112751 0.096848 0.386864 0.059 Uiso 1 1 d G U . . .
H6B H 0.237481 0.049821 0.440390 0.059 Uiso 1 1 d G U . . .
N3 N 0.8772(3) 0.02533(19) 0.19084(17) 0.0270(4) Uani 1 1 d . . . . .
N2 N 0.7201(3) 0.3819(2) 0.64050(17) 0.0253(4) Uani 1 1 d . . . . .
N1 N 0.7568(3) 0.5446(2) 0.31485(17) 0.0253(4) Uani 1 1 d . . . . .
C11 C 0.7014(4) -0.0124(2) 0.1498(2) 0.0293(5) Uani 1 1 d . . . . .
C10 C 0.6956(4) 0.4796(3) 0.7355(2) 0.0336(6) Uani 1 1 d . . . . .
H10 H 0.706794 0.565089 0.739499 0.040 Uiso 1 1 calc R U . . .
C15 C 1.0211(4) -0.0315(3) 0.1375(2) 0.0358(6) Uani 1 1 d . . . . .
H15 H 1.137954 -0.003911 0.169753 0.043 Uiso 1 1 calc R U . . .
C1 C 0.7605(4) 0.4640(3) 0.2075(2) 0.0300(5) Uani 1 1 d . . . . .
C6 C 0.7011(3) 0.2538(3) 0.6276(2) 0.0286(5) Uani 1 1 d . . . . .
C5 C 0.8077(4) 0.6723(3) 0.3507(3) 0.0377(6) Uani 1 1 d . . . . .
H5 H 0.804507 0.723690 0.424702 0.045 Uiso 1 1 calc R U . . .
C14 C 0.9957(5) -0.1290(3) 0.0368(3) 0.0463(8) Uani 1 1 d . . . . .
H14 H 1.094233 -0.169203 0.000511 0.056 Uiso 1 1 calc R U . . .
C12 C 0.6780(5) -0.1109(3) 0.0449(2) 0.0429(7) Uani 1 1 d . . . . .
H12 H 0.561193 -0.138401 0.012505 0.052 Uiso 1 1 calc R U . . .
C9 C 0.6542(4) 0.4544(3) 0.8265(2) 0.0405(7) Uani 1 1 d . . . . .
H9A H 0.640199 0.522139 0.892636 0.049 Uiso 1 1 calc R U . . .
C7 C 0.6553(4) 0.2282(3) 0.7206(3) 0.0417(7) Uani 1 1 d . . . . .
H7 H 0.639303 0.142565 0.715448 0.050 Uiso 1 1 calc R U . . .
C13 C 0.8209(6) -0.1672(3) -0.0104(3) 0.0516(9) Uani 1 1 d . . . . .
H13 H 0.801281 -0.231410 -0.080246 0.062 Uiso 1 1 calc R U . . .
C8 C 0.6336(5) 0.3267(4) 0.8183(3) 0.0447(7) Uani 1 1 d . . . . .
H8 H 0.605190 0.307761 0.879214 0.054 Uiso 1 1 calc R U . . .
C2 C 0.8216(4) 0.5207(4) 0.1352(3) 0.0454(7) Uani 1 1 d . . . . .
H2 H 0.828235 0.468897 0.061570 0.054 Uiso 1 1 calc R U . . .
C4 C 0.8637(5) 0.7261(3) 0.2790(3) 0.0505(8) Uani 1 1 d . . . . .
H4 H 0.896752 0.814203 0.303636 0.061 Uiso 1 1 calc R U . . .
C3 C 0.8711(5) 0.6489(4) 0.1698(3) 0.0541(9) Uani 1 1 d . . . . .
H3 H 0.909639 0.684416 0.120167 0.065 Uiso 1 1 calc R U . . .
H9B H 0.59(3) 0.32(2) 0.791(17) 0.53(13) 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
Lu1 S3 2.8224(7) . ?
Lu1 S1 2.7405(7) . ?
Lu1 S2 2.7611(7) . ?
Lu1 O2 2.2920(18) . ?
Lu1 O1 2.3029(16) . ?
Lu1 O4 2.3206(17) . ?
Lu1 O3 2.2888(17) . ?
Lu1 O5 2.3243(18) . ?
S3 C11 1.702(3) . ?
S1 C1 1.706(3) . ?
S2 C6 1.704(3) . ?
O2 N2 1.347(3) . ?
O1 N1 1.344(2) . ?
O4 H4A 0.8508 . ?
O4 H4B 0.8509 . ?
O3 N3 1.340(3) . ?
O5 H5A 0.8499 . ?
O5 H5B 0.8499 . ?
O6 H6A 0.8498 . ?
O6 H6B 0.8503 . ?
N3 C11 1.369(3) . ?
N3 C15 1.354(3) . ?
N2 C10 1.345(3) . ?
N2 C6 1.369(3) . ?
N1 C1 1.365(3) . ?
N1 C5 1.354(3) . ?
C11 C12 1.404(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.370(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.363(4) . ?
C1 C2 1.405(4) . ?
C6 C7 1.406(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.362(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.383(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.356(5) . ?
C9 H9A 0.9300 . ?
C9 C8 1.384(5) . ?
C9 H9B 1.5(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.368(5) . ?
C7 H9B 1.2(2) . ?
C13 H13 0.9300 . ?
C8 H8 0.9300 . ?
C8 H9B 0.4(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.357(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.378(6) . ?
C3 H3 0.9300 . ?

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
S1 Lu1 S3 72.72(2) . . ?
S1 Lu1 S2 151.12(2) . . ?
S2 Lu1 S3 80.40(2) . . ?
O2 Lu1 S3 141.21(4) . . ?
O2 Lu1 S1 139.97(4) . . ?
O2 Lu1 S2 68.86(4) . . ?
O2 Lu1 O1 71.01(6) . . ?
O2 Lu1 O4 79.37(7) . . ?
O2 Lu1 O5 78.68(7) . . ?
O1 Lu1 S3 130.01(5) . . ?
O1 Lu1 S1 69.25(4) . . ?
O1 Lu1 S2 138.92(4) . . ?
O1 Lu1 O4 80.33(6) . . ?
O1 Lu1 O5 75.37(7) . . ?
O4 Lu1 S3 74.32(5) . . ?
O4 Lu1 S1 98.34(5) . . ?
O4 Lu1 S2 84.09(5) . . ?
O4 Lu1 O5 151.43(7) . . ?
O3 Lu1 S3 68.09(5) . . ?
O3 Lu1 S1 83.91(5) . . ?
O3 Lu1 S2 76.30(5) . . ?
O3 Lu1 O2 123.33(7) . . ?
O3 Lu1 O1 135.76(7) . . ?
O3 Lu1 O4 139.82(7) . . ?
O3 Lu1 O5 68.50(6) . . ?
O5 Lu1 S3 133.51(5) . . ?
O5 Lu1 S1 86.99(6) . . ?
O5 Lu1 S2 104.62(6) . . ?
C11 S3 Lu1 98.14(9) . . ?
C1 S1 Lu1 98.56(9) . . ?
C6 S2 Lu1 100.47(9) . . ?
N2 O2 Lu1 126.81(14) . . ?
N1 O1 Lu1 122.82(13) . . ?
Lu1 O4 H4A 109.5 . . ?
Lu1 O4 H4B 109.2 . . ?
H4A O4 H4B 104.5 . . ?
N3 O3 Lu1 126.39(14) . . ?
Lu1 O5 H5A 129.7 . . ?
Lu1 O5 H5B 125.0 . . ?
H5A O5 H5B 104.5 . . ?
H6A O6 H6B 104.5 . . ?
O3 N3 C11 119.7(2) . . ?
O3 N3 C15 117.2(2) . . ?
C15 N3 C11 123.1(2) . . ?
O2 N2 C6 119.5(2) . . ?
C10 N2 O2 117.5(2) . . ?
C10 N2 C6 123.0(2) . . ?
O1 N1 C1 120.0(2) . . ?
O1 N1 C5 117.5(2) . . ?
C5 N1 C1 122.5(2) . . ?
N3 C11 S3 119.71(19) . . ?
N3 C11 C12 115.7(3) . . ?
C12 C11 S3 124.6(2) . . ?
N2 C10 H10 119.7 . . ?
N2 C10 C9 120.6(3) . . ?
C9 C10 H10 119.7 . . ?
N3 C15 H15 119.8 . . ?
N3 C15 C14 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
N1 C1 S1 119.20(19) . . ?
N1 C1 C2 116.3(3) . . ?
C2 C1 S1 124.5(2) . . ?
N2 C6 S2 119.31(19) . . ?
N2 C6 C7 116.2(2) . . ?
C7 C6 S2 124.4(2) . . ?
N1 C5 H5 119.8 . . ?
N1 C5 C4 120.5(3) . . ?
C4 C5 H5 119.8 . . ?
C15 C14 H14 120.6 . . ?
C15 C14 C13 118.9(3) . . ?
C13 C14 H14 120.6 . . ?
C11 C12 H12 119.1 . . ?
C13 C12 C11 121.9(3) . . ?
C13 C12 H12 119.1 . . ?
C10 C9 H9A 120.5 . . ?
C10 C9 C8 118.9(3) . . ?
C10 C9 H9B 108(8) . . ?
H9A C9 H9B 129.1 . . ?
C8 C9 H9A 120.5 . . ?
C8 C9 H9B 17(8) . . ?
C6 C7 H7 119.3 . . ?
C6 C7 H9B 115(10) . . ?
H7 C7 H9B 122.7 . . ?
C8 C7 C6 121.4(3) . . ?
C8 C7 H7 119.3 . . ?
C8 C7 H9B 18(10) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C9 C8 H8 120.1 . . ?
C9 C8 H9B 92(10) . . ?
C7 C8 C9 119.8(3) . . ?
C7 C8 H8 120.1 . . ?
C7 C8 H9B 59(10) . . ?
H8 C8 H9B 118.5 . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(3) . . ?
C3 C2 H2 119.1 . . ?
C5 C4 H4 120.3 . . ?
C5 C4 C3 119.4(3) . . ?
C3 C4 H4 120.3 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?

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
Lu1 S3 C11 N3 19.3(2) . . . . ?
Lu1 S3 C11 C12 -161.5(2) . . . . ?
Lu1 S1 C1 N1 -21.1(2) . . . . ?
Lu1 S1 C1 C2 160.5(2) . . . . ?
Lu1 S2 C6 N2 -13.7(2) . . . . ?
Lu1 S2 C6 C7 165.8(2) . . . . ?
Lu1 O2 N2 C10 -158.13(18) . . . . ?
Lu1 O2 N2 C6 21.4(3) . . . . ?
Lu1 O1 N1 C1 27.4(3) . . . . ?
Lu1 O1 N1 C5 -152.83(19) . . . . ?
Lu1 O3 N3 C11 -24.3(3) . . . . ?
Lu1 O3 N3 C15 156.44(18) . . . . ?
S3 C11 C12 C13 -177.5(2) . . . . ?
S1 C1 C2 C3 177.3(3) . . . . ?
S2 C6 C7 C8 179.7(3) . . . . ?
O2 N2 C10 C9 -178.8(3) . . . . ?
O2 N2 C6 S2 -0.5(3) . . . . ?
O2 N2 C6 C7 -180.0(2) . . . . ?
O1 N1 C1 S1 1.6(3) . . . . ?
O1 N1 C1 C2 -180.0(2) . . . . ?
O1 N1 C5 C4 -179.0(3) . . . . ?
O3 N3 C11 S3 -3.0(3) . . . . ?
O3 N3 C11 C12 177.7(2) . . . . ?
O3 N3 C15 C14 -179.0(2) . . . . ?
N3 C11 C12 C13 1.7(4) . . . . ?
N3 C15 C14 C13 1.0(4) . . . . ?
N2 C10 C9 C8 -1.6(5) . . . . ?
N2 C6 C7 C8 -0.9(4) . . . . ?
N1 C1 C2 C3 -1.1(4) . . . . ?
N1 C5 C4 C3 -1.1(5) . . . . ?
C11 N3 C15 C14 1.7(4) . . . . ?
C11 C12 C13 C14 0.9(5) . . . . ?
C10 N2 C6 S2 179.0(2) . . . . ?
C10 N2 C6 C7 -0.5(4) . . . . ?
C10 C9 C8 C7 0.2(5) . . . . ?
C15 N3 C11 S3 176.3(2) . . . . ?
C15 N3 C11 C12 -3.0(4) . . . . ?
C15 C14 C13 C12 -2.3(5) . . . . ?
C1 N1 C5 C4 0.7(4) . . . . ?
C1 C2 C3 C4 0.8(5) . . . . ?
C6 N2 C10 C9 1.8(4) . . . . ?
C6 C7 C8 C9 1.0(5) . . . . ?
C5 N1 C1 S1 -178.1(2) . . . . ?
C5 N1 C1 C2 0.3(4) . . . . ?
C5 C4 C3 C2 0.3(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_b_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2179114'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[Gd(mpo)2(mu-O-mpo)(H2O)]2'
_chemical_formula_moiety         'C15 H14 Gd N3 O4 S3'
_chemical_formula_sum            'C15 H14 Gd N3 O4 S3'
_chemical_formula_weight         553.72
_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'
Gd Gd -0.1653 3.9035 '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'
S S 0.1246 0.1234 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.0345(7)
_cell_length_b                   9.9366(7)
_cell_length_c                   19.3797(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.848(2)
_cell_angle_gamma                90
_cell_volume                     1925.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      32.66
_cell_measurement_theta_min      2.81
_shelx_estimated_absorpt_T_max   0.492
_shelx_estimated_absorpt_T_min   0.129
_exptl_absorpt_coefficient_mu    3.795
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1207 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.6876.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.915
_exptl_crystal_size_mid          0.371
_exptl_crystal_size_min          0.218
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            96150
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.760
_diffrn_reflns_theta_min         2.806
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                5587
_reflns_number_total             6892
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         6892
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0145P)²+4.1983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0628
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C7 \\sim C6 \\sim C10: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Rotating group:
 O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C12(H12), C5(H5), C10(H10), C2(H2), C13(H13), C4(H4),
 C3(H3), C9(H9), C7(H7), C8(H8)
;
_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
Gd1 Gd 0.34521(2) 0.58545(2) 0.55133(2) 0.02409(4) Uani 1 1 d . . . . .
S1 S 0.07746(7) 0.59550(8) 0.59738(4) 0.03692(17) Uani 1 1 d . . . . .
S3 S 0.58597(8) 0.61000(9) 0.64728(4) 0.04089(19) Uani 1 1 d . . . . .
S2 S 0.37499(11) 0.86378(10) 0.57781(6) 0.0552(2) Uani 1 1 d . . . . .
O3 O 0.51174(18) 0.40643(19) 0.54487(9) 0.0253(4) Uani 1 1 d . . . . .
O2 O 0.2182(2) 0.7120(2) 0.47162(11) 0.0383(5) Uani 1 1 d . . . . .
O4 O 0.2312(2) 0.4244(2) 0.47649(12) 0.0391(5) Uani 1 1 d . . . . .
H4A H 0.273692 0.413637 0.440749 0.059 Uiso 1 1 d R U . . .
H4B H 0.155972 0.456351 0.460967 0.059 Uiso 1 1 d R U . . .
N3 N 0.5559(2) 0.3532(3) 0.60731(12) 0.0281(5) Uani 1 1 d . . . . .
O1 O 0.3125(2) 0.4536(3) 0.64571(14) 0.0600(8) Uani 1 1 d . . . . .
N2 N 0.1927(3) 0.8430(3) 0.47013(17) 0.0450(7) Uani 1 1 d . . . . .
N1 N 0.2061(2) 0.4137(3) 0.67600(13) 0.0365(6) Uani 1 1 d . . . . .
C15 C 0.5535(3) 0.2182(3) 0.61353(19) 0.0408(7) Uani 1 1 d . . . . .
H15 H 0.524141 0.165171 0.575729 0.049 Uiso 1 1 calc R U . . .
C14 C 0.5942(4) 0.1595(5) 0.6754(2) 0.0585(11) Uani 1 1 d . . . . .
H14 H 0.593670 0.066337 0.680006 0.070 Uiso 1 1 calc R U . . .
C12 C 0.6362(3) 0.3763(5) 0.72319(17) 0.0510(10) Uani 1 1 d . . . . .
H12 H 0.664733 0.429538 0.761056 0.061 Uiso 1 1 calc R U . . .
C11 C 0.5944(3) 0.4388(4) 0.65989(14) 0.0340(7) Uani 1 1 d . . . . .
C1 C 0.0854(3) 0.4705(3) 0.65811(15) 0.0302(6) Uani 1 1 d . . . . .
C5 C 0.2243(4) 0.3171(5) 0.7251(2) 0.0566(11) Uani 1 1 d . . . . .
H5 H 0.309094 0.281048 0.735643 0.068 Uiso 1 1 calc R U . . .
C10 C 0.1003(5) 0.8856(5) 0.4200(3) 0.0716(14) Uani 1 1 d . U . . .
H10 H 0.057763 0.823965 0.389476 0.086 Uiso 1 1 calc R U . . .
C6 C 0.2593(4) 0.9267(4) 0.5162(3) 0.0571(11) Uani 1 1 d . U . . .
C2 C -0.0218(3) 0.4226(4) 0.6926(2) 0.0464(8) Uani 1 1 d . . . . .
H2 H -0.106682 0.457898 0.681375 0.056 Uiso 1 1 calc R U . . .
C13 C 0.6361(4) 0.2398(5) 0.7306(2) 0.0620(13) Uani 1 1 d . . . . .
H13 H 0.664305 0.201129 0.773017 0.074 Uiso 1 1 calc R U . . .
C4 C 0.1203(4) 0.2724(5) 0.7590(2) 0.0594(11) Uani 1 1 d . . . . .
H4 H 0.133391 0.206734 0.793069 0.071 Uiso 1 1 calc R U . . .
C3 C -0.0052(4) 0.3255(4) 0.7424(2) 0.0559(10) Uani 1 1 d . . . . .
H3 H -0.077869 0.295449 0.764825 0.067 Uiso 1 1 calc R U . . .
C9 C 0.0699(6) 1.0177(7) 0.4145(4) 0.118(3) Uani 1 1 d . U . . .
H9 H 0.005871 1.047539 0.380433 0.142 Uiso 1 1 calc R U . . .
C7 C 0.2271(5) 1.0636(5) 0.5087(4) 0.105(2) Uani 1 1 d . U . . .
H7 H 0.270579 1.126187 0.538311 0.126 Uiso 1 1 calc R U . . .
C8 C 0.1335(6) 1.1062(5) 0.4588(5) 0.131(3) Uani 1 1 d . U . . .
H8 H 0.112886 1.197312 0.455141 0.158 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 S1 2.9034(8) . ?
Gd1 S3 2.9316(8) . ?
Gd1 S2 2.8241(10) . ?
Gd1 O3 2.4484(18) 3_666 ?
Gd1 O3 2.4511(18) . ?
Gd1 O2 2.293(2) . ?
Gd1 O4 2.386(2) . ?
Gd1 O1 2.296(2) . ?
S1 C1 1.708(3) . ?
S3 C11 1.720(4) . ?
S2 C6 1.711(5) . ?
O3 N3 1.360(3) . ?
O2 N2 1.327(4) . ?
O4 H4A 0.8501 . ?
O4 H4B 0.8502 . ?
N3 C15 1.347(4) . ?
N3 C11 1.358(4) . ?
O1 N1 1.321(3) . ?
N2 C10 1.352(5) . ?
N2 C6 1.355(6) . ?
N1 C1 1.355(4) . ?
N1 C5 1.353(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.364(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.372(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.407(4) . ?
C12 C13 1.364(6) . ?
C1 C2 1.397(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.354(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.350(7) . ?
C6 C7 1.403(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.364(5) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.378(5) . ?
C3 H3 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.352(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.357(9) . ?
C8 H8 0.9300 . ?

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
S1 Gd1 S3 122.45(2) . . ?
S2 Gd1 S1 89.82(3) . . ?
S2 Gd1 S3 74.60(3) . . ?
O3 Gd1 S1 133.89(5) . . ?
O3 Gd1 S1 148.23(4) 3_666 . ?
O3 Gd1 S3 64.15(5) . . ?
O3 Gd1 S3 88.60(5) 3_666 . ?
O3 Gd1 S2 131.14(5) . . ?
O3 Gd1 S2 92.65(5) 3_666 . ?
O3 Gd1 O3 62.55(7) 3_666 . ?
O2 Gd1 S1 73.28(6) . . ?
O2 Gd1 S3 139.72(6) . . ?
O2 Gd1 S2 68.27(6) . . ?
O2 Gd1 O3 134.91(7) . . ?
O2 Gd1 O3 78.29(7) . 3_666 ?
O2 Gd1 O4 75.38(8) . . ?
O2 Gd1 O1 137.80(8) . . ?
O4 Gd1 S1 78.54(6) . . ?
O4 Gd1 S3 140.22(6) . . ?
O4 Gd1 S2 143.63(6) . . ?
O4 Gd1 O3 77.07(7) . . ?
O4 Gd1 O3 80.85(7) . 3_666 ?
O1 Gd1 S1 64.93(6) . . ?
O1 Gd1 S3 73.02(7) . . ?
O1 Gd1 S2 115.73(9) . . ?
O1 Gd1 O3 139.29(8) . 3_666 ?
O1 Gd1 O3 76.74(8) . . ?
O1 Gd1 O4 90.46(11) . . ?
C1 S1 Gd1 101.33(10) . . ?
C11 S3 Gd1 92.06(10) . . ?
C6 S2 Gd1 100.13(14) . . ?
Gd1 O3 Gd1 117.45(7) 3_666 . ?
N3 O3 Gd1 121.49(14) . 3_666 ?
N3 O3 Gd1 114.14(14) . . ?
N2 O2 Gd1 130.4(2) . . ?
Gd1 O4 H4A 109.4 . . ?
Gd1 O4 H4B 109.3 . . ?
H4A O4 H4B 104.5 . . ?
C15 N3 O3 117.4(3) . . ?
C15 N3 C11 124.2(3) . . ?
C11 N3 O3 118.4(2) . . ?
N1 O1 Gd1 134.44(18) . . ?
O2 N2 C10 116.2(4) . . ?
O2 N2 C6 120.3(3) . . ?
C10 N2 C6 123.5(4) . . ?
O1 N1 C1 120.0(2) . . ?
O1 N1 C5 117.3(3) . . ?
C5 N1 C1 122.7(3) . . ?
N3 C15 H15 120.1 . . ?
N3 C15 C14 119.9(4) . . ?
C14 C15 H15 120.1 . . ?
C15 C14 H14 120.5 . . ?
C15 C14 C13 119.1(4) . . ?
C13 C14 H14 120.5 . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C13 C12 C11 121.8(4) . . ?
N3 C11 S3 120.3(2) . . ?
N3 C11 C12 115.0(3) . . ?
C12 C11 S3 124.6(3) . . ?
N1 C1 S1 117.9(2) . . ?
N1 C1 C2 116.3(3) . . ?
C2 C1 S1 125.8(2) . . ?
N1 C5 H5 119.7 . . ?
N1 C5 C4 120.7(3) . . ?
C4 C5 H5 119.7 . . ?
N2 C10 H10 120.1 . . ?
C9 C10 N2 119.8(6) . . ?
C9 C10 H10 120.1 . . ?
N2 C6 S2 120.2(3) . . ?
N2 C6 C7 115.4(4) . . ?
C7 C6 S2 124.3(4) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(3) . . ?
C3 C2 H2 119.1 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C5 C4 H4 120.4 . . ?
C5 C4 C3 119.2(3) . . ?
C3 C4 H4 120.4 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C10 C9 H9 120.3 . . ?
C10 C9 C8 119.4(6) . . ?
C8 C9 H9 120.3 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.1(6) . . ?
C8 C7 H7 119.4 . . ?
C9 C8 C7 120.7(5) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?

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
Gd1 S1 C1 N1 8.0(3) . . . . ?
Gd1 S1 C1 C2 -173.4(3) . . . . ?
Gd1 S3 C11 N3 34.2(2) . . . . ?
Gd1 S3 C11 C12 -143.9(3) . . . . ?
Gd1 S2 C6 N2 -4.3(4) . . . . ?
Gd1 S2 C6 C7 176.4(5) . . . . ?
Gd1 O3 N3 C15 129.2(2) . . . . ?
Gd1 O3 N3 C15 -80.6(3) 3_666 . . . ?
Gd1 O3 N3 C11 -48.2(3) . . . . ?
Gd1 O3 N3 C11 101.9(2) 3_666 . . . ?
Gd1 O2 N2 C10 -172.2(3) . . . . ?
Gd1 O2 N2 C6 9.0(5) . . . . ?
Gd1 O1 N1 C1 -11.3(5) . . . . ?
Gd1 O1 N1 C5 169.5(3) . . . . ?
S1 C1 C2 C3 -177.6(3) . . . . ?
S2 C6 C7 C8 -179.6(6) . . . . ?
O3 N3 C15 C14 -178.8(3) . . . . ?
O3 N3 C11 S3 0.4(3) . . . . ?
O3 N3 C11 C12 178.7(2) . . . . ?
O2 N2 C10 C9 -179.1(5) . . . . ?
O2 N2 C6 S2 -1.1(5) . . . . ?
O2 N2 C6 C7 178.3(4) . . . . ?
N3 C15 C14 C13 0.6(5) . . . . ?
O1 N1 C1 S1 -1.3(4) . . . . ?
O1 N1 C1 C2 -180.0(3) . . . . ?
O1 N1 C5 C4 179.1(4) . . . . ?
N2 C10 C9 C8 0.6(10) . . . . ?
N2 C6 C7 C8 1.0(9) . . . . ?
N1 C1 C2 C3 1.0(6) . . . . ?
N1 C5 C4 C3 0.7(8) . . . . ?
C15 N3 C11 S3 -176.9(2) . . . . ?
C15 N3 C11 C12 1.5(4) . . . . ?
C15 C14 C13 C12 0.1(6) . . . . ?
C11 N3 C15 C14 -1.4(5) . . . . ?
C11 C12 C13 C14 -0.1(6) . . . . ?
C1 N1 C5 C4 0.0(7) . . . . ?
C1 C2 C3 C4 -0.3(7) . . . . ?
C5 N1 C1 S1 177.8(3) . . . . ?
C5 N1 C1 C2 -0.9(5) . . . . ?
C5 C4 C3 C2 -0.6(7) . . . . ?
C10 N2 C6 S2 -179.9(4) . . . . ?
C10 N2 C6 C7 -0.4(7) . . . . ?
C10 C9 C8 C7 0.0(13) . . . . ?
C6 N2 C10 C9 -0.4(8) . . . . ?
C6 C7 C8 C9 -0.8(12) . . . . ?
C13 C12 C11 S3 177.5(3) . . . . ?
C13 C12 C11 N3 -0.7(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_c
_database_code_depnum_ccdc_archive 'CCDC 2179115'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H16 Dy N3 O5 S3, H2 O'
_chemical_formula_sum            'C15 H18 Dy N3 O6 S3'
_chemical_formula_weight         595.00
_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'
Dy Dy -0.1892 4.4098 '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'
S S 0.1246 0.1234 '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                   7.4805(9)
_cell_length_b                   11.1541(15)
_cell_length_c                   13.1843(17)
_cell_angle_alpha                111.472(3)
_cell_angle_beta                 93.931(3)
_cell_angle_gamma                91.055(3)
_cell_volume                     1020.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9638
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      3.01
_shelx_estimated_absorpt_T_max   0.529
_shelx_estimated_absorpt_T_min   0.175
_exptl_absorpt_coefficient_mu    4.006
_exptl_absorpt_correction_T_max  0.5661
_exptl_absorpt_correction_T_min  0.3690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1307 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.6679.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             582
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 1.00 0.2740
-1.00 0.00 -1.00 0.1280
0.00 0.00 1.00 0.0890
0.00 0.00 -1.00 0.0200
1.00 0.00 -1.00 0.2870
1.00 1.00 1.00 0.2520
-1.00 -1.00 -1.00 0.1210
0.00 1.00 1.00 0.1150
0.00 -1.00 -1.00 0.0640
-1.00 1.00 1.00 0.1240
1.00 -1.00 -1.00 0.2530
1.00 1.00 0.00 0.2950
-1.00 -1.00 0.00 0.1420
0.00 1.00 0.00 0.1550
-1.00 1.00 0.00 0.1290
1.00 -1.00 0.00 0.2930
1.00 1.00 -1.00 0.2960
-1.00 -1.00 1.00 0.1710
0.00 1.00 -1.00 0.1320
0.00 -1.00 1.00 0.0790

_exptl_crystal_size_max          0.668
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.182
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58168
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.576
_diffrn_reflns_theta_min         2.732
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                6779
_reflns_number_total             7556
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0312
_refine_ls_restrained_S_all      1.121
_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)+(0.0242P)²+2.1686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0771
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Dy01-H5A \\sim Dy01-H5B
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C2(H2), C14(H14), C12(H12), C4(H4), C10(H10), C13(H13),
 C3(H3), C7(H7), C8(H8), C9(H9)
;
_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
Dy01 Dy 0.27506(2) 0.71661(2) 0.62987(2) 0.02112(4) Uani 1 1 d D . . . .
S2 S 0.31691(14) 0.68949(8) 0.83293(7) 0.03752(18) Uani 1 1 d . . . . .
S3 S 0.46668(11) 0.94438(8) 0.77927(8) 0.03684(17) Uani 1 1 d . . . . .
S1 S 0.26982(16) 0.86550(8) 0.49656(8) 0.0419(2) Uani 1 1 d . . . . .
O1 O 0.2361(3) 0.5890(2) 0.44317(18) 0.0308(4) Uani 1 1 d . . . . .
O2 O 0.2993(3) 0.4990(2) 0.61122(17) 0.0277(4) Uani 1 1 d . . . . .
O5 O -0.0266(3) 0.6342(2) 0.6169(2) 0.0367(5) Uani 1 1 d G . . . .
H5A H -0.067169 0.556299 0.589647 0.055 Uiso 1 1 d DG U . . .
H5B H -0.115798 0.676940 0.644383 0.055 Uiso 1 1 d DG U . . .
O4 O 0.5800(3) 0.6895(2) 0.5859(2) 0.0339(5) Uani 1 1 d . . . . .
H4A H 0.619830 0.756058 0.575728 0.051 Uiso 1 1 d R U . . .
H4B H 0.584592 0.628187 0.524222 0.051 Uiso 1 1 d R U . . .
O3 O 0.0857(3) 0.8812(2) 0.7157(2) 0.0344(5) Uani 1 1 d . . . . .
O6 O 0.7786(4) 0.8953(3) 0.5919(3) 0.0417(6) Uani 1 1 d G . . . .
H6A H 0.884386 0.907807 0.622852 0.063 Uiso 1 1 d G U . . .
H6B H 0.764890 0.957977 0.570439 0.063 Uiso 1 1 d G U . . .
N3 N 0.1195(4) 0.9781(2) 0.8133(2) 0.0279(5) Uani 1 1 d . . . . .
N1 N 0.2803(3) 0.6214(2) 0.3588(2) 0.0263(5) Uani 1 1 d . . . . .
N2 N 0.2427(3) 0.4521(2) 0.6847(2) 0.0264(5) Uani 1 1 d . . . . .
C1 C 0.2999(4) 0.7490(3) 0.3720(3) 0.0301(6) Uani 1 1 d . . . . .
C11 C 0.2938(5) 1.0149(3) 0.8540(3) 0.0302(6) Uani 1 1 d . . . . .
C15 C -0.0245(5) 1.0348(3) 0.8658(3) 0.0371(7) Uani 1 1 d . . . . .
H15 H -0.139824 1.007034 0.833338 0.045 Uiso 1 1 calc R U . . .
C6 C 0.2415(4) 0.5318(3) 0.7930(3) 0.0310(6) Uani 1 1 d . . . . .
C5 C 0.3047(5) 0.5234(3) 0.2627(3) 0.0347(6) Uani 1 1 d . . . . .
H5 H 0.293061 0.438383 0.258008 0.042 Uiso 1 1 calc R U . . .
C2 C 0.3467(6) 0.7743(4) 0.2796(3) 0.0431(8) Uani 1 1 d . . . . .
H2 H 0.363726 0.859402 0.285308 0.052 Uiso 1 1 calc R U . . .
C14 C -0.0008(7) 1.1325(4) 0.9662(3) 0.0503(10) Uani 1 1 d . . . . .
H14 H -0.098891 1.172430 1.001961 0.060 Uiso 1 1 calc R U . . .
C12 C 0.3162(7) 1.1142(4) 0.9590(3) 0.0457(9) Uani 1 1 d . . . . .
H12 H 0.431464 1.141500 0.991628 0.055 Uiso 1 1 calc R U . . .
C4 C 0.3463(6) 0.5492(4) 0.1731(3) 0.0428(8) Uani 1 1 d . . . . .
H4 H 0.360024 0.482188 0.107171 0.051 Uiso 1 1 calc R U . . .
C10 C 0.1896(5) 0.3253(3) 0.6482(3) 0.0387(7) Uani 1 1 d . . . . .
H10 H 0.190920 0.275163 0.574297 0.046 Uiso 1 1 calc R U . . .
C13 C 0.1720(8) 1.1707(4) 1.0134(3) 0.0561(12) Uani 1 1 d . . . . .
H13 H 0.190388 1.235131 1.082517 0.067 Uiso 1 1 calc R U . . .
C3 C 0.3678(6) 0.6766(5) 0.1817(3) 0.0488(10) Uani 1 1 d . . . . .
H3 H 0.396235 0.695621 0.121452 0.059 Uiso 1 1 calc R U . . .
C7 C 0.1809(6) 0.4750(5) 0.8640(3) 0.0490(10) Uani 1 1 d . . . . .
H7 H 0.176105 0.525770 0.937492 0.059 Uiso 1 1 calc R U . . .
C8 C 0.1288(6) 0.3472(5) 0.8284(4) 0.0569(12) Uani 1 1 d . . . . .
H8 H 0.089975 0.311881 0.877371 0.068 Uiso 1 1 calc R U . . .
C9 C 0.1339(6) 0.2705(5) 0.7189(4) 0.0533(11) Uani 1 1 d . . . . .
H9 H 0.100192 0.183195 0.693807 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy01 S2 2.7998(9) . ?
Dy01 S3 2.8642(9) . ?
Dy01 S1 2.8246(9) . ?
Dy01 O1 2.343(2) . ?
Dy01 O2 2.360(2) . ?
Dy01 O5 2.392(2) . ?
Dy01 O4 2.389(2) . ?
Dy01 O3 2.335(2) . ?
S2 C6 1.712(4) . ?
S3 C11 1.705(4) . ?
S1 C1 1.714(3) . ?
O1 N1 1.349(3) . ?
O2 N2 1.347(3) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8502 . ?
O4 H4A 0.8535 . ?
O4 H4B 0.8533 . ?
O3 N3 1.348(3) . ?
O6 H6A 0.8499 . ?
O6 H6B 0.8500 . ?
N3 C11 1.370(4) . ?
N3 C15 1.359(4) . ?
N1 C1 1.372(4) . ?
N1 C5 1.363(4) . ?
N2 C6 1.379(4) . ?
N2 C10 1.357(4) . ?
C1 C2 1.411(4) . ?
C11 C12 1.418(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.370(6) . ?
C6 C7 1.401(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.367(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.373(6) . ?
C14 H14 0.9300 . ?
C14 C13 1.384(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.370(7) . ?
C4 H4 0.9300 . ?
C4 C3 1.389(6) . ?
C10 H10 0.9300 . ?
C10 C9 1.370(5) . ?
C13 H13 0.9300 . ?
C3 H3 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.367(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.386(7) . ?
C9 H9 0.9300 . ?

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
S2 Dy01 S3 72.81(3) . . ?
S2 Dy01 S1 152.38(3) . . ?
S1 Dy01 S3 80.94(3) . . ?
O1 Dy01 S2 139.86(6) . . ?
O1 Dy01 S3 141.25(6) . . ?
O1 Dy01 S1 67.61(6) . . ?
O1 Dy01 O2 72.00(7) . . ?
O1 Dy01 O5 79.50(9) . . ?
O1 Dy01 O4 79.21(9) . . ?
O2 Dy01 S2 68.04(5) . . ?
O2 Dy01 S3 130.12(6) . . ?
O2 Dy01 S1 138.64(5) . . ?
O2 Dy01 O5 74.63(8) . . ?
O2 Dy01 O4 80.84(8) . . ?
O5 Dy01 S2 86.51(7) . . ?
O5 Dy01 S3 132.56(6) . . ?
O5 Dy01 S1 105.72(7) . . ?
O4 Dy01 S2 97.77(7) . . ?
O4 Dy01 S3 75.03(6) . . ?
O4 Dy01 S1 83.30(7) . . ?
O4 Dy01 O5 151.46(8) . . ?
O3 Dy01 S2 84.98(7) . . ?
O3 Dy01 S3 67.27(6) . . ?
O3 Dy01 S1 76.97(7) . . ?
O3 Dy01 O1 123.05(9) . . ?
O3 Dy01 O2 135.48(9) . . ?
O3 Dy01 O5 68.79(8) . . ?
O3 Dy01 O4 139.55(8) . . ?
C6 S2 Dy01 98.79(11) . . ?
C11 S3 Dy01 98.46(11) . . ?
C1 S1 Dy01 100.69(10) . . ?
N1 O1 Dy01 127.37(17) . . ?
N2 O2 Dy01 123.05(17) . . ?
Dy01 O5 H5A 128.7 . . ?
Dy01 O5 H5B 126.6 . . ?
H5A O5 H5B 104.5 . . ?
Dy01 O4 H4A 109.4 . . ?
Dy01 O4 H4B 109.4 . . ?
H4A O4 H4B 104.3 . . ?
N3 O3 Dy01 127.02(18) . . ?
H6A O6 H6B 104.5 . . ?
O3 N3 C11 119.4(3) . . ?
O3 N3 C15 117.0(3) . . ?
C15 N3 C11 123.6(3) . . ?
O1 N1 C1 119.9(2) . . ?
O1 N1 C5 117.4(3) . . ?
C5 N1 C1 122.7(3) . . ?
O2 N2 C6 120.0(2) . . ?
O2 N2 C10 117.7(3) . . ?
C10 N2 C6 122.3(3) . . ?
N1 C1 S1 119.3(2) . . ?
N1 C1 C2 116.2(3) . . ?
C2 C1 S1 124.4(3) . . ?
N3 C11 S3 120.5(2) . . ?
N3 C11 C12 115.4(3) . . ?
C12 C11 S3 124.1(3) . . ?
N3 C15 H15 119.8 . . ?
N3 C15 C14 120.3(4) . . ?
C14 C15 H15 119.8 . . ?
N2 C6 S2 119.3(2) . . ?
N2 C6 C7 116.2(3) . . ?
C7 C6 S2 124.4(3) . . ?
N1 C5 H5 119.8 . . ?
N1 C5 C4 120.5(3) . . ?
C4 C5 H5 119.8 . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.7(3) . . ?
C3 C2 H2 119.1 . . ?
C15 C14 H14 120.6 . . ?
C15 C14 C13 118.7(4) . . ?
C13 C14 H14 120.6 . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.5(4) . . ?
C13 C12 H12 119.2 . . ?
C5 C4 H4 120.3 . . ?
C5 C4 C3 119.3(4) . . ?
C3 C4 H4 120.3 . . ?
N2 C10 H10 119.6 . . ?
N2 C10 C9 120.8(4) . . ?
C9 C10 H10 119.6 . . ?
C14 C13 H13 119.8 . . ?
C12 C13 C14 120.4(4) . . ?
C12 C13 H13 119.8 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C6 C7 H7 119.0 . . ?
C8 C7 C6 122.0(4) . . ?
C8 C7 H7 119.0 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.7(3) . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 118.9(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy01 S2 C6 N2 21.7(3) . . . . ?
Dy01 S2 C6 C7 -159.9(3) . . . . ?
Dy01 S3 C11 N3 -18.9(3) . . . . ?
Dy01 S3 C11 C12 162.0(3) . . . . ?
Dy01 S1 C1 N1 13.6(3) . . . . ?
Dy01 S1 C1 C2 -165.5(3) . . . . ?
Dy01 O1 N1 C1 -21.7(4) . . . . ?
Dy01 O1 N1 C5 157.9(2) . . . . ?
Dy01 O2 N2 C6 -28.7(3) . . . . ?
Dy01 O2 N2 C10 151.9(2) . . . . ?
Dy01 O3 N3 C11 23.3(4) . . . . ?
Dy01 O3 N3 C15 -157.1(2) . . . . ?
S2 C6 C7 C8 -177.4(4) . . . . ?
S3 C11 C12 C13 177.4(3) . . . . ?
S1 C1 C2 C3 -179.6(3) . . . . ?
O1 N1 C1 S1 0.6(4) . . . . ?
O1 N1 C1 C2 179.8(3) . . . . ?
O1 N1 C5 C4 178.7(3) . . . . ?
O2 N2 C6 S2 -1.3(4) . . . . ?
O2 N2 C6 C7 -179.8(3) . . . . ?
O2 N2 C10 C9 178.6(4) . . . . ?
O3 N3 C11 S3 3.2(4) . . . . ?
O3 N3 C11 C12 -177.7(3) . . . . ?
O3 N3 C15 C14 178.9(3) . . . . ?
N3 C11 C12 C13 -1.7(5) . . . . ?
N3 C15 C14 C13 -1.0(6) . . . . ?
N1 C1 C2 C3 1.3(6) . . . . ?
N1 C5 C4 C3 1.6(6) . . . . ?
N2 C6 C7 C8 1.1(6) . . . . ?
N2 C10 C9 C8 1.5(7) . . . . ?
C1 N1 C5 C4 -1.7(5) . . . . ?
C1 C2 C3 C4 -1.3(7) . . . . ?
C11 N3 C15 C14 -1.5(5) . . . . ?
C11 C12 C13 C14 -0.6(6) . . . . ?
C15 N3 C11 S3 -176.4(2) . . . . ?
C15 N3 C11 C12 2.8(4) . . . . ?
C15 C14 C13 C12 1.9(6) . . . . ?
C6 N2 C10 C9 -0.9(6) . . . . ?
C6 C7 C8 C9 -0.5(7) . . . . ?
C5 N1 C1 S1 -179.0(3) . . . . ?
C5 N1 C1 C2 0.3(5) . . . . ?
C5 C4 C3 C2 -0.1(6) . . . . ?
C10 N2 C6 S2 178.1(3) . . . . ?
C10 N2 C6 C7 -0.4(5) . . . . ?
C7 C8 C9 C10 -0.8(7) . . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2179120'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H14 N3 O4 S3 Sm'
_chemical_formula_sum            'C15 H14 N3 O4 S3 Sm'
_chemical_formula_weight         546.82
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.0701(15)
_cell_length_b                   9.9650(14)
_cell_length_c                   19.421(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.919(4)
_cell_angle_gamma                90
_cell_volume                     1941.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.635
_shelx_estimated_absorpt_T_min   0.291
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.8466.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dull gray'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.148
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            88915
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.004
_diffrn_reflns_theta_min         2.299
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                4446
_reflns_number_total             5167
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.106
_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)+(0.0300P)²+3.5211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0719
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C12(H12), C2(H2), C5(H5), C13(H13), C10(H10), C3(H3),
 C4(H4), C7(H7), C9(H9), C8(H8)
;
_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 0.65541(2) 0.58615(2) 0.44846(2) 0.02500(6) Uani 1 1 d . . . . .
S1 S 0.92336(9) 0.59445(9) 0.40172(5) 0.0378(2) Uani 1 1 d . . . . .
S3 S 0.41366(10) 0.60920(11) 0.35181(5) 0.0423(2) Uani 1 1 d . . . . .
S2 S 0.62529(13) 0.86646(11) 0.42245(7) 0.0583(3) Uani 1 1 d . . . . .
O3 O 0.4877(2) 0.4063(2) 0.45446(11) 0.0268(4) Uani 1 1 d . . . . .
O4 O 0.7701(3) 0.4249(3) 0.52502(14) 0.0418(6) Uani 1 1 d . . . . .
H4A H 0.725588 0.411954 0.559676 0.063 Uiso 1 1 d R U . . .
H4B H 0.843358 0.458364 0.542064 0.063 Uiso 1 1 d R U . . .
O2 O 0.7824(3) 0.7152(3) 0.52764(13) 0.0399(6) Uani 1 1 d . . . . .
N3 N 0.4440(2) 0.3536(3) 0.39209(13) 0.0292(6) Uani 1 1 d . . . . .
N1 N 0.7944(3) 0.4118(3) 0.32391(16) 0.0397(7) Uani 1 1 d . . . . .
O1 O 0.6888(3) 0.4522(4) 0.35421(16) 0.0621(10) Uani 1 1 d . . . . .
N2 N 0.8068(3) 0.8457(3) 0.5295(2) 0.0482(8) Uani 1 1 d . . . . .
C15 C 0.4458(4) 0.2190(4) 0.3863(2) 0.0433(9) Uani 1 1 d . . . . .
H15 H 0.474256 0.166253 0.424203 0.052 Uiso 1 1 calc R U . . .
C14 C 0.4055(5) 0.1601(5) 0.3242(3) 0.0617(14) Uani 1 1 d . . . . .
H14 H 0.406442 0.067233 0.319560 0.074 Uiso 1 1 calc R U . . .
C11 C 0.4061(3) 0.4387(4) 0.33960(17) 0.0364(8) Uani 1 1 d . . . . .
C1 C 0.9144(3) 0.4694(4) 0.34156(17) 0.0318(7) Uani 1 1 d . . . . .
C12 C 0.3635(4) 0.3764(6) 0.2763(2) 0.0526(11) Uani 1 1 d . . . . .
H12 H 0.334443 0.429388 0.238600 0.063 Uiso 1 1 calc R U . . .
C6 C 0.7402(5) 0.9292(4) 0.4837(3) 0.0605(13) Uani 1 1 d . . . . .
C2 C 1.0223(4) 0.4201(4) 0.3074(2) 0.0470(10) Uani 1 1 d . . . . .
H2 H 1.107255 0.454290 0.318945 0.056 Uiso 1 1 calc R U . . .
C5 C 0.7765(4) 0.3153(5) 0.2749(2) 0.0584(13) Uani 1 1 d . . . . .
H5 H 0.691838 0.280093 0.263853 0.070 Uiso 1 1 calc R U . . .
C13 C 0.3638(4) 0.2398(6) 0.2691(2) 0.0638(14) Uani 1 1 d . . . . .
H13 H 0.335620 0.201036 0.226805 0.077 Uiso 1 1 calc R U . . .
C10 C 0.8995(6) 0.8884(6) 0.5791(3) 0.0763(17) Uani 1 1 d . . . . .
H10 H 0.942075 0.827095 0.609637 0.092 Uiso 1 1 calc R U . . .
C3 C 1.0050(4) 0.3235(5) 0.2579(3) 0.0583(12) Uani 1 1 d . . . . .
H3 H 1.077108 0.293918 0.235171 0.070 Uiso 1 1 calc R U . . .
C4 C 0.8802(4) 0.2697(5) 0.2417(3) 0.0640(14) Uani 1 1 d . . . . .
H4 H 0.867530 0.202816 0.208348 0.077 Uiso 1 1 calc R U . . .
C7 C 0.7729(7) 1.0661(5) 0.4904(5) 0.112(3) Uani 1 1 d . . . . .
H7 H 0.730765 1.128411 0.460292 0.134 Uiso 1 1 calc R U . . .
C9 C 0.9302(8) 1.0198(8) 0.5843(5) 0.130(4) Uani 1 1 d . . . . .
H9 H 0.995393 1.049075 0.617816 0.156 Uiso 1 1 calc R U . . .
C8 C 0.8668(8) 1.1081(7) 0.5413(6) 0.145(5) Uani 1 1 d . . . . .
H8 H 0.886609 1.199010 0.545873 0.174 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 S1 2.9209(9) . ?
Sm1 S3 2.9527(10) . ?
Sm1 S2 2.8502(12) . ?
Sm1 O3 2.470(2) 3_666 ?
Sm1 O3 2.472(2) . ?
Sm1 O4 2.415(2) . ?
Sm1 O2 2.306(2) . ?
Sm1 O1 2.313(3) . ?
S1 C1 1.705(4) . ?
S3 C11 1.717(4) . ?
S2 C6 1.706(6) . ?
O3 N3 1.359(3) . ?
O4 H4A 0.8501 . ?
O4 H4B 0.8501 . ?
O2 N2 1.324(4) . ?
N3 C15 1.346(5) . ?
N3 C11 1.355(5) . ?
N1 O1 1.322(4) . ?
N1 C1 1.355(4) . ?
N1 C5 1.355(5) . ?
N2 C6 1.353(7) . ?
N2 C10 1.351(6) . ?
C15 H15 0.9300 . ?
C15 C14 1.371(6) . ?
C14 H14 0.9300 . ?
C14 C13 1.369(8) . ?
C11 C12 1.410(5) . ?
C1 C2 1.409(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.368(7) . ?
C6 C7 1.407(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.361(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.352(6) . ?
C13 H13 0.9300 . ?
C10 H10 0.9300 . ?
C10 C9 1.347(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(6) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.373(11) . ?
C9 H9 0.9300 . ?
C9 C8 1.338(13) . ?
C8 H8 0.9300 . ?

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
S1 Sm1 S3 122.24(3) . . ?
S2 Sm1 S1 90.25(3) . . ?
S2 Sm1 S3 75.03(3) . . ?
O3 Sm1 S1 148.33(5) 3_666 . ?
O3 Sm1 S1 133.50(5) . . ?
O3 Sm1 S3 88.84(5) 3_666 . ?
O3 Sm1 S3 63.70(5) . . ?
O3 Sm1 S2 92.60(6) 3_666 . ?
O3 Sm1 S2 130.99(6) . . ?
O3 Sm1 O3 62.64(8) 3_666 . ?
O4 Sm1 S1 78.71(7) . . ?
O4 Sm1 S3 140.16(7) . . ?
O4 Sm1 S2 143.06(7) . . ?
O4 Sm1 O3 80.21(8) . 3_666 ?
O4 Sm1 O3 77.37(8) . . ?
O2 Sm1 S1 73.57(7) . . ?
O2 Sm1 S3 139.50(7) . . ?
O2 Sm1 S2 67.42(7) . . ?
O2 Sm1 O3 135.64(8) . . ?
O2 Sm1 O3 78.49(8) . 3_666 ?
O2 Sm1 O4 75.64(9) . . ?
O2 Sm1 O1 137.72(9) . . ?
O1 Sm1 S1 64.52(7) . . ?
O1 Sm1 S3 73.12(8) . . ?
O1 Sm1 S2 116.48(11) . . ?
O1 Sm1 O3 139.04(9) . 3_666 ?
O1 Sm1 O3 76.41(9) . . ?
O1 Sm1 O4 90.50(12) . . ?
C1 S1 Sm1 101.32(11) . . ?
C11 S3 Sm1 92.01(11) . . ?
C6 S2 Sm1 100.37(16) . . ?
Sm1 O3 Sm1 117.36(8) 3_666 . ?
N3 O3 Sm1 121.79(16) . 3_666 ?
N3 O3 Sm1 114.12(17) . . ?
Sm1 O4 H4A 109.3 . . ?
Sm1 O4 H4B 109.3 . . ?
H4A O4 H4B 104.5 . . ?
N2 O2 Sm1 131.1(2) . . ?
C15 N3 O3 117.0(3) . . ?
C15 N3 C11 124.4(3) . . ?
C11 N3 O3 118.5(3) . . ?
O1 N1 C1 119.5(3) . . ?
O1 N1 C5 117.7(3) . . ?
C5 N1 C1 122.7(3) . . ?
N1 O1 Sm1 134.8(2) . . ?
O2 N2 C6 120.4(3) . . ?
O2 N2 C10 116.4(4) . . ?
C10 N2 C6 123.3(4) . . ?
N3 C15 H15 120.2 . . ?
N3 C15 C14 119.7(4) . . ?
C14 C15 H15 120.2 . . ?
C15 C14 H14 120.4 . . ?
C13 C14 C15 119.1(5) . . ?
C13 C14 H14 120.4 . . ?
N3 C11 S3 120.6(2) . . ?
N3 C11 C12 115.1(4) . . ?
C12 C11 S3 124.2(3) . . ?
N1 C1 S1 118.4(3) . . ?
N1 C1 C2 116.1(3) . . ?
C2 C1 S1 125.4(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.6(4) . . ?
C13 C12 H12 119.2 . . ?
N2 C6 S2 120.1(3) . . ?
N2 C6 C7 115.9(5) . . ?
C7 C6 S2 124.0(5) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.4(4) . . ?
C3 C2 H2 119.3 . . ?
N1 C5 H5 119.6 . . ?
C4 C5 N1 120.8(4) . . ?
C4 C5 H5 119.6 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(4) . . ?
C12 C13 H13 120.0 . . ?
N2 C10 H10 120.0 . . ?
C9 C10 N2 120.0(7) . . ?
C9 C10 H10 120.0 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.2(7) . . ?
C8 C7 H7 119.9 . . ?
C10 C9 H9 120.1 . . ?
C8 C9 C10 119.9(7) . . ?
C8 C9 H9 120.1 . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.8(6) . . ?
C9 C8 H8 119.6 . . ?

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 S1 C1 N1 7.7(3) . . . . ?
Sm1 S1 C1 C2 -172.9(3) . . . . ?
Sm1 S3 C11 N3 34.6(3) . . . . ?
Sm1 S3 C11 C12 -144.5(3) . . . . ?
Sm1 S2 C6 N2 -4.3(4) . . . . ?
Sm1 S2 C6 C7 175.4(5) . . . . ?
Sm1 O3 N3 C15 129.6(3) . . . . ?
Sm1 O3 N3 C15 -79.9(3) 3_666 . . . ?
Sm1 O3 N3 C11 102.3(3) 3_666 . . . ?
Sm1 O3 N3 C11 -48.2(3) . . . . ?
Sm1 O2 N2 C6 8.2(5) . . . . ?
Sm1 O2 N2 C10 -172.1(3) . . . . ?
S1 C1 C2 C3 -177.3(4) . . . . ?
S3 C11 C12 C13 177.8(3) . . . . ?
S2 C6 C7 C8 -180.0(7) . . . . ?
O3 N3 C15 C14 -178.7(3) . . . . ?
O3 N3 C11 S3 0.1(4) . . . . ?
O3 N3 C11 C12 179.3(3) . . . . ?
O2 N2 C6 S2 -0.6(6) . . . . ?
O2 N2 C6 C7 179.6(5) . . . . ?
O2 N2 C10 C9 179.8(6) . . . . ?
N3 C15 C14 C13 -0.1(6) . . . . ?
N3 C11 C12 C13 -1.4(5) . . . . ?
N1 C1 C2 C3 2.2(6) . . . . ?
N1 C5 C4 C3 -0.6(9) . . . . ?
O1 N1 C1 S1 -1.0(5) . . . . ?
O1 N1 C1 C2 179.5(4) . . . . ?
O1 N1 C5 C4 179.8(5) . . . . ?
N2 C6 C7 C8 -0.2(11) . . . . ?
N2 C10 C9 C8 1.4(13) . . . . ?
C15 N3 C11 S3 -177.5(3) . . . . ?
C15 N3 C11 C12 1.7(5) . . . . ?
C15 C14 C13 C12 0.4(7) . . . . ?
C11 N3 C15 C14 -1.0(5) . . . . ?
C11 C12 C13 C14 0.4(7) . . . . ?
C1 N1 O1 Sm1 -11.3(6) . . . . ?
C1 N1 C5 C4 1.3(8) . . . . ?
C1 C2 C3 C4 -1.6(8) . . . . ?
C6 N2 C10 C9 -0.5(9) . . . . ?
C6 C7 C8 C9 1.2(15) . . . . ?
C2 C3 C4 C5 0.8(9) . . . . ?
C5 N1 O1 Sm1 170.1(4) . . . . ?
C5 N1 C1 S1 177.5(4) . . . . ?
C5 N1 C1 C2 -2.0(6) . . . . ?
C10 N2 C6 S2 179.6(4) . . . . ?
C10 N2 C6 C7 -0.1(8) . . . . ?
C10 C9 C8 C7 -1.7(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_c_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2179119'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H16 N3 O5 S3 Tm, H2 O'
_chemical_formula_sum            'C15 H18 N3 O6 S3 Tm'
_chemical_formula_weight         601.43
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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                   7.4398(9)
_cell_length_b                   11.1083(14)
_cell_length_c                   13.1269(16)
_cell_angle_alpha                111.312(3)
_cell_angle_beta                 94.019(3)
_cell_angle_gamma                91.182(3)
_cell_volume                     1006.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.77
_cell_measurement_theta_min      2.75
_shelx_estimated_absorpt_T_max   0.497
_shelx_estimated_absorpt_T_min   0.184
_exptl_absorpt_coefficient_mu    4.754
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1129 before and 0.0475 after correction. The Ratio of minimum to maximum transmission is 0.6751. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             588
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -1.00 -1.00 0.1940
1.00 1.00 0.00 0.0850
-1.00 0.00 -1.00 0.1250
0.00 1.00 -1.00 0.0360
1.00 0.00 -1.00 0.1010
0.00 0.00 -1.00 0.0910
0.00 0.00 1.00 0.0210
0.00 1.00 0.00 0.0330
0.00 -1.00 -1.00 0.1270
1.00 -1.00 1.00 0.0760
1.00 0.00 0.00 0.1000
-1.00 1.00 0.00 0.1290
1.00 -1.00 -1.00 0.1050

_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.171
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15505
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.769
_diffrn_reflns_theta_min         2.748
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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                4846
_reflns_number_total             5179
_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 V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.183
_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)+(0.0134P)²+1.2826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0586
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B)
2.b Rotating group:
 O5(H5A,H5B), O4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C10(H10), C14(H14), C7(H7), C2(H2), C12(H12), C13(H13),
 C9(H9), C8(H8), C4(H4), C3(H3)
;
_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
Tm1 Tm 0.72464(2) 0.28392(2) 0.37115(2) 0.01958(5) Uani 1 1 d . . . . .
S3 S 0.53073(11) 0.05776(8) 0.22431(8) 0.03493(18) Uani 1 1 d . . . . .
S1 S 0.68619(13) 0.30720(9) 0.16808(7) 0.03599(19) Uani 1 1 d . . . . .
S2 S 0.73073(15) 0.13619(8) 0.50318(8) 0.0392(2) Uani 1 1 d . . . . .
O1 O 0.7007(3) 0.4989(2) 0.38919(17) 0.0263(4) Uani 1 1 d . . . . .
O2 O 0.7632(3) 0.4126(2) 0.55539(18) 0.0293(5) Uani 1 1 d . . . . .
O5 O 0.4231(3) 0.3112(2) 0.4137(2) 0.0310(5) Uani 1 1 d . . . . .
H5A H 0.414745 0.372338 0.479042 0.047 Uiso 1 1 d R U . . .
H5B H 0.376225 0.241598 0.421773 0.047 Uiso 1 1 d R U . . .
O3 O 0.9126(3) 0.1210(2) 0.28710(19) 0.0328(5) Uani 1 1 d . . . . .
O4 O 1.0235(3) 0.3652(2) 0.3845(2) 0.0349(5) Uani 1 1 d . . . . .
H4A H 1.093139 0.302290 0.360471 0.052 Uiso 1 1 d R U . . .
H4B H 1.061666 0.403123 0.452057 0.052 Uiso 1 1 d R U . . .
N3 N 0.8783(4) 0.0242(2) 0.1895(2) 0.0271(5) Uani 1 1 d . . . . .
N1 N 0.7574(3) 0.5457(2) 0.3150(2) 0.0241(5) Uani 1 1 d . . . . .
N2 N 0.7195(3) 0.3803(2) 0.6406(2) 0.0241(5) Uani 1 1 d . . . . .
O6 O 0.2232(3) 0.1058(2) 0.4099(3) 0.0396(6) Uani 1 1 d G . . . .
H6A H 0.248307 0.049141 0.437351 0.059 Uiso 1 1 d G U . . .
H6B H 0.117449 0.089238 0.377577 0.059 Uiso 1 1 d G U . . .
C1 C 0.7604(4) 0.4654(3) 0.2073(3) 0.0298(7) Uani 1 1 d . . . . .
C11 C 0.7030(5) -0.0133(3) 0.1485(3) 0.0291(7) Uani 1 1 d . . . . .
C6 C 0.6999(4) 0.2527(3) 0.6278(3) 0.0285(6) Uani 1 1 d . . . . .
C15 C 1.0220(5) -0.0328(3) 0.1366(3) 0.0343(7) Uani 1 1 d . . . . .
H15 H 1.138112 -0.005428 0.169114 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8090(5) 0.6733(3) 0.3510(3) 0.0361(8) Uani 1 1 d . . . . .
H5 H 0.806574 0.724120 0.424924 0.043 Uiso 1 1 calc R U . . .
C10 C 0.6952(5) 0.4784(3) 0.7364(3) 0.0328(7) Uani 1 1 d . . . . .
H10 H 0.707473 0.563638 0.740702 0.039 Uiso 1 1 calc R U . . .
C14 C 0.9979(7) -0.1302(4) 0.0358(3) 0.0472(10) Uani 1 1 d . . . . .
H14 H 1.096395 -0.169812 -0.000146 0.057 Uiso 1 1 calc R U . . .
C7 C 0.6539(5) 0.2277(4) 0.7206(3) 0.0413(8) Uani 1 1 d . . . . .
H7 H 0.637341 0.142414 0.715428 0.050 Uiso 1 1 calc R U . . .
C2 C 0.8207(6) 0.5220(5) 0.1358(3) 0.0464(9) Uani 1 1 d . . . . .
H2 H 0.826242 0.470574 0.062294 0.056 Uiso 1 1 calc R U . . .
C12 C 0.6803(6) -0.1120(4) 0.0435(3) 0.0432(9) Uani 1 1 d . . . . .
H12 H 0.564217 -0.139419 0.010821 0.052 Uiso 1 1 calc R U . . .
C13 C 0.8238(7) -0.1685(4) -0.0116(3) 0.0504(11) Uani 1 1 d . . . . .
H13 H 0.804747 -0.232739 -0.080958 0.060 Uiso 1 1 calc R U . . .
C9 C 0.6530(5) 0.4532(4) 0.8265(3) 0.0393(8) Uani 1 1 d . . . . .
H9 H 0.638006 0.520589 0.892261 0.047 Uiso 1 1 calc R U . . .
C8 C 0.6328(6) 0.3256(4) 0.8185(3) 0.0442(9) Uani 1 1 d . . . . .
H8 H 0.605050 0.306605 0.879151 0.053 Uiso 1 1 calc R U . . .
C4 C 0.8643(6) 0.7276(4) 0.2801(4) 0.0500(10) Uani 1 1 d . . . . .
H4 H 0.896645 0.815460 0.304675 0.060 Uiso 1 1 calc R U . . .
C3 C 0.8718(6) 0.6500(5) 0.1703(4) 0.0543(12) Uani 1 1 d . . . . .
H3 H 0.911225 0.685151 0.120902 0.065 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 S3 2.8371(9) . ?
Tm1 S1 2.7662(9) . ?
Tm1 S2 2.7854(9) . ?
Tm1 O1 2.325(2) . ?
Tm1 O2 2.312(2) . ?
Tm1 O5 2.349(2) . ?
Tm1 O3 2.306(2) . ?
Tm1 O4 2.353(2) . ?
S3 C11 1.704(4) . ?
S1 C1 1.709(4) . ?
S2 C6 1.711(4) . ?
O1 N1 1.346(3) . ?
O2 N2 1.350(3) . ?
O5 H5A 0.8870 . ?
O5 H5B 0.8861 . ?
O3 N3 1.343(3) . ?
O4 H4A 0.8563 . ?
O4 H4B 0.8563 . ?
N3 C11 1.371(4) . ?
N3 C15 1.356(4) . ?
N1 C1 1.373(4) . ?
N1 C5 1.359(4) . ?
N2 C6 1.369(4) . ?
N2 C10 1.358(4) . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8500 . ?
C1 C2 1.398(5) . ?
C11 C12 1.412(5) . ?
C6 C7 1.407(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.367(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.361(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.366(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.384(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.370(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.363(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.364(6) . ?
C13 H13 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.387(6) . ?
C8 H8 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.390(7) . ?
C3 H3 0.9300 . ?

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
S1 Tm1 S3 72.70(3) . . ?
S1 Tm1 S2 151.59(3) . . ?
S2 Tm1 S3 80.65(3) . . ?
O1 Tm1 S3 130.10(6) . . ?
O1 Tm1 S1 68.89(6) . . ?
O1 Tm1 S2 138.74(6) . . ?
O1 Tm1 O5 80.49(8) . . ?
O1 Tm1 O4 74.84(8) . . ?
O2 Tm1 S3 141.25(6) . . ?
O2 Tm1 S1 139.90(6) . . ?
O2 Tm1 S2 68.44(6) . . ?
O2 Tm1 O1 71.24(8) . . ?
O2 Tm1 O5 79.22(9) . . ?
O2 Tm1 O4 79.24(9) . . ?
O5 Tm1 S3 74.62(6) . . ?
O5 Tm1 S1 98.14(7) . . ?
O5 Tm1 S2 83.83(6) . . ?
O5 Tm1 O4 151.36(8) . . ?
O3 Tm1 S3 67.76(6) . . ?
O3 Tm1 S1 84.19(7) . . ?
O3 Tm1 S2 76.64(7) . . ?
O3 Tm1 O1 135.61(8) . . ?
O3 Tm1 O2 123.40(8) . . ?
O3 Tm1 O5 139.76(8) . . ?
O3 Tm1 O4 68.68(8) . . ?
O4 Tm1 S3 133.08(6) . . ?
O4 Tm1 S1 86.46(7) . . ?
O4 Tm1 S2 105.38(7) . . ?
C11 S3 Tm1 98.39(11) . . ?
C1 S1 Tm1 98.50(12) . . ?
C6 S2 Tm1 100.57(11) . . ?
N1 O1 Tm1 122.84(17) . . ?
N2 O2 Tm1 126.97(17) . . ?
Tm1 O5 H5A 111.4 . . ?
Tm1 O5 H5B 111.1 . . ?
H5A O5 H5B 102.6 . . ?
N3 O3 Tm1 126.81(18) . . ?
Tm1 O4 H4A 109.7 . . ?
Tm1 O4 H4B 109.8 . . ?
H4A O4 H4B 104.2 . . ?
O3 N3 C11 119.6(3) . . ?
O3 N3 C15 117.3(3) . . ?
C15 N3 C11 123.1(3) . . ?
O1 N1 C1 120.1(2) . . ?
O1 N1 C5 117.6(3) . . ?
C5 N1 C1 122.4(3) . . ?
O2 N2 C6 119.8(3) . . ?
O2 N2 C10 117.4(3) . . ?
C10 N2 C6 122.8(3) . . ?
H6A O6 H6B 109.5 . . ?
N1 C1 S1 119.3(2) . . ?
N1 C1 C2 116.3(3) . . ?
C2 C1 S1 124.3(3) . . ?
N3 C11 S3 119.9(2) . . ?
N3 C11 C12 115.5(3) . . ?
C12 C11 S3 124.6(3) . . ?
N2 C6 S2 119.2(2) . . ?
N2 C6 C7 116.1(3) . . ?
C7 C6 S2 124.7(3) . . ?
N3 C15 H15 119.6 . . ?
N3 C15 C14 120.7(4) . . ?
C14 C15 H15 119.6 . . ?
N1 C5 H5 119.7 . . ?
N1 C5 C4 120.7(4) . . ?
C4 C5 H5 119.7 . . ?
N2 C10 H10 119.6 . . ?
N2 C10 C9 120.7(3) . . ?
C9 C10 H10 119.6 . . ?
C15 C14 H14 120.7 . . ?
C15 C14 C13 118.6(4) . . ?
C13 C14 H14 120.7 . . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.8(3) . . ?
C8 C7 H7 119.1 . . ?
C1 C2 H2 118.9 . . ?
C3 C2 C1 122.1(4) . . ?
C3 C2 H2 118.9 . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 121.9(4) . . ?
C13 C12 H12 119.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.1(4) . . ?
C12 C13 H13 120.0 . . ?
C10 C9 H9 120.5 . . ?
C10 C9 C8 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C7 C8 C9 119.6(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C5 C4 H4 120.4 . . ?
C5 C4 C3 119.1(4) . . ?
C3 C4 H4 120.4 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tm1 S3 C11 N3 19.0(3) . . . . ?
Tm1 S3 C11 C12 -161.6(3) . . . . ?
Tm1 S1 C1 N1 -21.4(3) . . . . ?
Tm1 S1 C1 C2 160.5(3) . . . . ?
Tm1 S2 C6 N2 -13.8(3) . . . . ?
Tm1 S2 C6 C7 165.8(3) . . . . ?
Tm1 O1 N1 C1 27.8(3) . . . . ?
Tm1 O1 N1 C5 -152.7(2) . . . . ?
Tm1 O2 N2 C6 21.1(4) . . . . ?
Tm1 O2 N2 C10 -158.3(2) . . . . ?
Tm1 O3 N3 C11 -23.7(4) . . . . ?
Tm1 O3 N3 C15 156.9(2) . . . . ?
S3 C11 C12 C13 -177.6(3) . . . . ?
S1 C1 C2 C3 177.3(3) . . . . ?
S2 C6 C7 C8 179.4(3) . . . . ?
O1 N1 C1 S1 1.6(4) . . . . ?
O1 N1 C1 C2 179.8(3) . . . . ?
O1 N1 C5 C4 -178.6(3) . . . . ?
O2 N2 C6 S2 -0.2(4) . . . . ?
O2 N2 C6 C7 -179.9(3) . . . . ?
O2 N2 C10 C9 -179.2(3) . . . . ?
O3 N3 C11 S3 -3.1(4) . . . . ?
O3 N3 C11 C12 177.4(3) . . . . ?
O3 N3 C15 C14 -178.6(3) . . . . ?
N3 C11 C12 C13 1.9(5) . . . . ?
N3 C15 C14 C13 0.6(6) . . . . ?
N1 C1 C2 C3 -0.8(6) . . . . ?
N1 C5 C4 C3 -1.6(6) . . . . ?
N2 C6 C7 C8 -1.0(5) . . . . ?
N2 C10 C9 C8 -0.8(6) . . . . ?
C1 N1 C5 C4 0.9(5) . . . . ?
C1 C2 C3 C4 0.1(7) . . . . ?
C11 N3 C15 C14 2.0(5) . . . . ?
C11 C12 C13 C14 0.6(6) . . . . ?
C6 N2 C10 C9 1.4(5) . . . . ?
C6 C7 C8 C9 1.5(6) . . . . ?
C15 N3 C11 S3 176.3(3) . . . . ?
C15 N3 C11 C12 -3.2(5) . . . . ?
C15 C14 C13 C12 -1.9(6) . . . . ?
C5 N1 C1 S1 -177.9(3) . . . . ?
C5 N1 C1 C2 0.3(5) . . . . ?
C5 C4 C3 C2 1.1(7) . . . . ?
C10 N2 C6 S2 179.2(3) . . . . ?
C10 N2 C6 C7 -0.4(5) . . . . ?
C10 C9 C8 C7 -0.6(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2179116'
loop_
_audit_author_name
_audit_author_address
'Zachary K. Huffman'
;Florida State University
United States of America
;
_audit_update_record             
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_audit_creation_date             2021-10-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[Nd(mpo)2(mu-O-mpo)(H2O)]2'
_chemical_formula_moiety         'C15 H14 N3 Nd O4 S3'
_chemical_formula_sum            'C15 H14 N3 Nd O4 S3'
_chemical_formula_weight         540.71
_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'
Nd Nd -0.1943 3.0179 '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'
S S 0.1246 0.1234 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1252(2)
_cell_length_b                   9.9839(2)
_cell_length_c                   19.5248(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.0050(10)
_cell_angle_gamma                90
_cell_volume                     1966.22(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      40.35
_cell_measurement_theta_min      2.78
_shelx_estimated_absorpt_T_max   0.650
_shelx_estimated_absorpt_T_min   0.492
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0852 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.7868.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.158
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            112293
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.127
_diffrn_reflns_theta_min         2.019
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_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                11293
_reflns_number_total             13041
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.453
_refine_diff_density_min         -2.036
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         13041
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.176
_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)+(0.0225P)²+2.0145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C12(H12), C2(H2), C5(H5), C3(H3), C13(H13), C4(H4),
 C10(H10), C9(H9), C7(H7), C8(H8)
;
_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
Nd1 Nd 0.34362(2) 0.58683(2) 0.55187(2) 0.02561(3) Uani 1 1 d . . . . .
S1 S 0.07521(5) 0.59163(6) 0.59902(3) 0.03981(12) Uani 1 1 d . . . . .
S3 S 0.58607(6) 0.60762(7) 0.64940(3) 0.04415(13) Uani 1 1 d . . . . .
S2 S 0.37359(10) 0.86898(8) 0.57941(6) 0.0643(2) Uani 1 1 d . . . . .
O3 O 0.51279(14) 0.40538(14) 0.54601(7) 0.0279(2) Uani 1 1 d . . . . .
O4 O 0.22893(17) 0.42795(19) 0.47185(11) 0.0452(4) Uani 1 1 d . . . . .
H4A H 0.274132 0.416329 0.437502 0.068 Uiso 1 1 d R U . . .
H4B H 0.156502 0.462542 0.454678 0.068 Uiso 1 1 d R U . . .
O2 O 0.21693(19) 0.72074(19) 0.47326(9) 0.0452(4) Uani 1 1 d . . . . .
N3 N 0.55652(15) 0.35269(19) 0.60776(8) 0.0303(3) Uani 1 1 d . . . . .
O1 O 0.30934(17) 0.4494(3) 0.64602(12) 0.0674(8) Uani 1 1 d . . . . .
N1 N 0.20427(18) 0.4089(2) 0.67608(11) 0.0417(5) Uani 1 1 d . . . . .
N2 N 0.1932(2) 0.8511(3) 0.47195(15) 0.0549(6) Uani 1 1 d . . . . .
C15 C 0.5547(3) 0.2179(3) 0.61308(15) 0.0449(5) Uani 1 1 d . . . . .
H15 H 0.525850 0.165631 0.575258 0.054 Uiso 1 1 calc R U . . .
C1 C 0.08435(18) 0.4662(2) 0.65877(11) 0.0326(4) Uani 1 1 d . . . . .
C11 C 0.59408(19) 0.4371(3) 0.66090(10) 0.0367(4) Uani 1 1 d . . . . .
C14 C 0.5958(3) 0.1582(4) 0.67506(19) 0.0633(10) Uani 1 1 d . . . . .
H14 H 0.595565 0.065450 0.679386 0.076 Uiso 1 1 calc R U . . .
C12 C 0.6362(3) 0.3735(4) 0.72345(12) 0.0557(8) Uani 1 1 d . . . . .
H12 H 0.664391 0.425923 0.761315 0.067 Uiso 1 1 calc R U . . .
C2 C -0.0219(2) 0.4173(3) 0.69278(17) 0.0510(7) Uani 1 1 d . . . . .
H2 H -0.106151 0.452427 0.681868 0.061 Uiso 1 1 calc R U . . .
C5 C 0.2227(3) 0.3123(4) 0.72459(17) 0.0613(9) Uani 1 1 d . . . . .
H5 H 0.306896 0.276502 0.734924 0.074 Uiso 1 1 calc R U . . .
C3 C -0.0047(3) 0.3191(4) 0.74173(19) 0.0633(9) Uani 1 1 d . . . . .
H3 H -0.076664 0.287893 0.763612 0.076 Uiso 1 1 calc R U . . .
C13 C 0.6371(3) 0.2375(4) 0.73022(16) 0.0672(11) Uani 1 1 d . . . . .
H13 H 0.665617 0.198601 0.772193 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1201(3) 0.2669(4) 0.75831(19) 0.0670(10) Uani 1 1 d . . . . .
H4 H 0.133657 0.201578 0.792135 0.080 Uiso 1 1 calc R U . . .
C6 C 0.2594(3) 0.9331(3) 0.5187(3) 0.0676(11) Uani 1 1 d . . . . .
C10 C 0.1022(5) 0.8947(5) 0.4217(3) 0.0920(16) Uani 1 1 d . . . . .
H10 H 0.061164 0.834941 0.390117 0.110 Uiso 1 1 calc R U . . .
C9 C 0.0719(6) 1.0279(7) 0.4184(5) 0.155(4) Uani 1 1 d . . . . .
H9 H 0.007805 1.059042 0.385205 0.186 Uiso 1 1 calc R U . . .
C7 C 0.2271(5) 1.0697(4) 0.5126(5) 0.132(3) Uani 1 1 d . . . . .
H7 H 0.269482 1.130978 0.542942 0.159 Uiso 1 1 calc R U . . .
C8 C 0.1342(6) 1.1137(5) 0.4628(6) 0.172(5) Uani 1 1 d . . . . .
H8 H 0.114108 1.204449 0.459614 0.206 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 S1 2.9450(5) . ?
Nd1 S3 2.9800(6) . ?
Nd1 S2 2.8790(8) . ?
Nd1 O3 2.5013(13) 3_666 ?
Nd1 O3 2.5026(13) . ?
Nd1 O4 2.4472(18) . ?
Nd1 O2 2.3335(16) . ?
Nd1 O1 2.3441(18) . ?
S1 C1 1.708(2) . ?
S3 C11 1.718(3) . ?
S2 C6 1.707(4) . ?
O3 N3 1.3540(19) . ?
O4 H4A 0.8522 . ?
O4 H4B 0.8525 . ?
O2 N2 1.323(3) . ?
N3 C15 1.350(3) . ?
N3 C11 1.365(3) . ?
O1 N1 1.322(2) . ?
N1 C1 1.358(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.359(5) . ?
N2 C10 1.358(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.380(4) . ?
C1 C2 1.400(3) . ?
C11 C12 1.409(3) . ?
C14 H14 0.9300 . ?
C14 C13 1.372(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.364(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.370(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.355(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(4) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C6 C7 1.405(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.365(7) . ?
C9 H9 0.9300 . ?
C9 C8 1.336(12) . ?
C7 H7 0.9300 . ?
C7 C8 1.365(10) . ?
C8 H8 0.9300 . ?

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
S1 Nd1 S3 122.025(19) . . ?
S2 Nd1 S1 90.62(2) . . ?
S2 Nd1 S3 75.22(2) . . ?
O3 Nd1 S1 148.44(3) 3_666 . ?
O3 Nd1 S1 132.85(4) . . ?
O3 Nd1 S3 89.13(3) 3_666 . ?
O3 Nd1 S3 63.30(3) . . ?
O3 Nd1 S2 93.06(4) 3_666 . ?
O3 Nd1 S2 130.95(4) . . ?
O3 Nd1 O3 62.73(5) 3_666 . ?
O4 Nd1 S1 79.09(5) . . ?
O4 Nd1 S3 140.51(5) . . ?
O4 Nd1 S2 142.18(5) . . ?
O4 Nd1 O3 78.90(6) . 3_666 ?
O4 Nd1 O3 77.89(5) . . ?
O2 Nd1 S1 74.15(5) . . ?
O2 Nd1 S3 139.06(6) . . ?
O2 Nd1 S2 66.74(6) . . ?
O2 Nd1 O3 136.38(5) . . ?
O2 Nd1 O3 78.61(6) . 3_666 ?
O2 Nd1 O4 75.43(7) . . ?
O2 Nd1 O1 137.79(7) . . ?
O1 Nd1 S1 63.93(4) . . ?
O1 Nd1 S3 73.13(6) . . ?
O1 Nd1 S2 116.54(8) . . ?
O1 Nd1 O3 138.86(6) . 3_666 ?
O1 Nd1 O3 76.16(6) . . ?
O1 Nd1 O4 91.53(9) . . ?
C1 S1 Nd1 101.83(7) . . ?
C11 S3 Nd1 92.37(7) . . ?
C6 S2 Nd1 100.58(12) . . ?
Nd1 O3 Nd1 117.27(5) 3_666 . ?
N3 O3 Nd1 121.72(10) . 3_666 ?
N3 O3 Nd1 114.36(10) . . ?
Nd1 O4 H4A 109.5 . . ?
Nd1 O4 H4B 109.4 . . ?
H4A O4 H4B 104.4 . . ?
N2 O2 Nd1 131.65(19) . . ?
O3 N3 C11 119.00(18) . . ?
C15 N3 O3 116.7(2) . . ?
C15 N3 C11 124.2(2) . . ?
N1 O1 Nd1 134.99(14) . . ?
O1 N1 C1 119.81(18) . . ?
O1 N1 C5 117.47(19) . . ?
C5 N1 C1 122.7(2) . . ?
O2 N2 C6 120.1(2) . . ?
O2 N2 C10 116.1(4) . . ?
C10 N2 C6 123.7(3) . . ?
N3 C15 H15 120.2 . . ?
N3 C15 C14 119.5(3) . . ?
C14 C15 H15 120.2 . . ?
N1 C1 S1 118.22(15) . . ?
N1 C1 C2 116.2(2) . . ?
C2 C1 S1 125.54(17) . . ?
N3 C11 S3 120.38(15) . . ?
N3 C11 C12 115.1(3) . . ?
C12 C11 S3 124.5(2) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14 120.4 . . ?
C11 C12 H12 118.9 . . ?
C13 C12 C11 122.1(3) . . ?
C13 C12 H12 118.9 . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.6(2) . . ?
C3 C2 H2 119.2 . . ?
N1 C5 H5 119.6 . . ?
N1 C5 C4 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(2) . . ?
C12 C13 H13 120.0 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N2 C6 S2 120.3(2) . . ?
N2 C6 C7 115.5(4) . . ?
C7 C6 S2 124.2(4) . . ?
N2 C10 H10 120.6 . . ?
N2 C10 C9 118.9(6) . . ?
C9 C10 H10 120.6 . . ?
C10 C9 H9 119.9 . . ?
C8 C9 C10 120.1(6) . . ?
C8 C9 H9 119.9 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.9(6) . . ?
C8 C7 H7 119.6 . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?

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
Nd1 S1 C1 N1 7.3(2) . . . . ?
Nd1 S1 C1 C2 -173.6(2) . . . . ?
Nd1 S3 C11 N3 34.64(16) . . . . ?
Nd1 S3 C11 C12 -144.42(19) . . . . ?
Nd1 S2 C6 N2 -4.7(3) . . . . ?
Nd1 S2 C6 C7 175.6(5) . . . . ?
Nd1 O3 N3 C15 129.57(16) . . . . ?
Nd1 O3 N3 C15 -79.9(2) 3_666 . . . ?
Nd1 O3 N3 C11 102.79(16) 3_666 . . . ?
Nd1 O3 N3 C11 -47.79(19) . . . . ?
Nd1 O2 N2 C6 7.6(4) . . . . ?
Nd1 O2 N2 C10 -173.1(3) . . . . ?
Nd1 O1 N1 C1 -10.7(5) . . . . ?
Nd1 O1 N1 C5 170.7(3) . . . . ?
S1 C1 C2 C3 -177.8(3) . . . . ?
S3 C11 C12 C13 178.1(2) . . . . ?
S2 C6 C7 C8 -179.8(6) . . . . ?
O3 N3 C15 C14 -178.9(2) . . . . ?
O3 N3 C11 S3 -0.1(2) . . . . ?
O3 N3 C11 C12 179.07(17) . . . . ?
O2 N2 C6 S2 0.1(4) . . . . ?
O2 N2 C6 C7 179.8(4) . . . . ?
O2 N2 C10 C9 179.0(5) . . . . ?
N3 C15 C14 C13 0.4(4) . . . . ?
N3 C11 C12 C13 -1.0(4) . . . . ?
O1 N1 C1 S1 -1.0(4) . . . . ?
O1 N1 C1 C2 179.8(3) . . . . ?
O1 N1 C5 C4 179.1(4) . . . . ?
N1 C1 C2 C3 1.3(5) . . . . ?
N1 C5 C4 C3 1.1(7) . . . . ?
N2 C6 C7 C8 0.5(9) . . . . ?
N2 C10 C9 C8 2.0(11) . . . . ?
C15 N3 C11 S3 -177.23(17) . . . . ?
C15 N3 C11 C12 1.9(3) . . . . ?
C15 C14 C13 C12 0.4(5) . . . . ?
C1 N1 C5 C4 0.5(6) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
C11 N3 C15 C14 -1.7(4) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C2 C3 C4 C5 -1.4(7) . . . . ?
C5 N1 C1 S1 177.6(3) . . . . ?
C5 N1 C1 C2 -1.6(4) . . . . ?
C6 N2 C10 C9 -1.7(7) . . . . ?
C6 C7 C8 C9 -0.1(13) . . . . ?
C10 N2 C6 S2 -179.2(3) . . . . ?
C10 N2 C6 C7 0.5(6) . . . . ?
C10 C9 C8 C7 -1.1(13) . . . . ?

