# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_La-ONDI
_database_code_depnum_ccdc_archive 'CCDC 2181884'
loop_
_audit_author_name
_audit_author_address
'Harald Krautscheid'
;Universitaet Leipzig
Germany
;
_audit_update_record             
;
2022-09-15 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;

_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
SHELXL-2014/7
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C14 H8 La N2 O8, 2(H2 O), 1[Cl], 0.75[C4 H9 N O]'
_chemical_formula_sum            'C17 H18.75 Cl La N2.75 O10.75'
_chemical_formula_weight         607.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   19.2116(14)
_cell_length_b                   14.8074(11)
_cell_length_c                   8.5126(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.908(6)
_cell_angle_gamma                90
_cell_volume                     2385.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    14102
_cell_measurement_theta_min      3.75
_cell_measurement_theta_max      70.01

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    15.397
_shelx_estimated_absorpt_T_min   0.372
_shelx_estimated_absorpt_T_max   0.709
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9350
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.790
_diffrn_reflns_theta_max         70.631
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2257
_reflns_number_gt                2106
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_refine_special_details          SQUEEZE
_platon_squeeze_special_details  
;
A solvent mask was calculated and 246 electrons were 
found in a volume of 910Å³ in 1 void per unit cell. 
This is consistent with the presence of 1[Cl] per Formula Unit 
which account for 68 electrons per unit cell.
0.75[C4H9NO] per Formula Unit account for 144 electrons per unit cell.
;

_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 Riding coordinates:
 O2W(H2WA,H2WB)
2.b Rotating group:
 O1W(H1WA,H1WB)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0705P)²+1.9807P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2257
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0916
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.5000 0.46505(2) 0.2500 0.02644(13) Uani 1 2 d S T P . .
C1 C 0.6499(2) 0.6214(3) 0.6483(5) 0.0367(9) Uani 1 1 d . . . . .
C2 C 0.6209(2) 0.6318(3) 0.3555(5) 0.0358(9) Uani 1 1 d . . . . .
C3 C 0.6790(2) 0.6951(3) 0.3542(5) 0.0392(10) Uani 1 1 d . . . . .
C4 C 0.6925(3) 0.7307(4) 0.2114(5) 0.0489(12) Uani 1 1 d . . . . .
H4 H 0.6638 0.7137 0.1136 0.059 Uiso 1 1 calc R U . . .
C5 C 0.7482(3) 0.7914(4) 0.2111(5) 0.0499(13) Uani 1 1 d . . . . .
H5 H 0.7570 0.8157 0.1131 0.060 Uiso 1 1 calc R U . . .
C6 C 0.7907(2) 0.8164(3) 0.3530(5) 0.0394(9) Uani 1 1 d . . . . .
C7 C 0.7782(2) 0.7805(3) 0.4992(5) 0.0383(9) Uani 1 1 d . . . . .
N1 N 0.61282(17) 0.5968(3) 0.5012(4) 0.0345(7) Uani 1 1 d . . . . .
O1 O 0.63210(16) 0.5914(2) 0.7701(3) 0.0419(7) Uani 1 1 d . . . . .
O2 O 0.55906(16) 0.53678(18) 0.5014(4) 0.0329(6) Uani 1 1 d . . . . .
O3 O 0.57997(15) 0.6064(2) 0.2350(3) 0.0394(7) Uani 1 1 d . . . . .
O1W O 0.4775(2) 0.3182(3) 0.0810(4) 0.0576(9) Uani 1 1 d . . . . .
H1WA H 0.4415 0.3245 -0.0211 0.086 Uiso 1 1 d R U . . .
H1WB H 0.4542 0.2673 0.1332 0.086 Uiso 1 1 d R U . . .
O2W O 0.3953(4) 0.1693(5) 0.1492(11) 0.152(3) Uani 1 1 d . . . . .
H2WA H 0.3901 0.1490 0.2424 0.228 Uiso 1 1 d R U . . .
H2WB H 0.3689 0.1342 0.0817 0.228 Uiso 1 1 d 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
La1 O2 2.482(3) . ?
La1 O2 2.482(3) 2_655 ?
La1 O2 2.568(3) 6_565 ?
La1 O2 2.568(3) 5_666 ?
La1 O1W 2.602(4) 2_655 ?
La1 O1W 2.602(4) . ?
La1 O3 2.612(3) . ?
La1 O3 2.612(3) 2_655 ?
La1 O1 2.649(3) 5_666 ?
La1 O1 2.649(3) 6_565 ?
C1 O1 1.229(5) . ?
C1 N1 1.379(5) . ?
C1 C6 1.467(6) 7_666 ?
C2 O3 1.239(5) . ?
C2 N1 1.378(5) . ?
C2 C3 1.460(6) . ?
C3 C4 1.390(6) . ?
C3 C7 1.418(6) 7_666 ?
C4 C5 1.397(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.412(6) . ?
C6 C1 1.467(6) 7_666 ?
C7 C7 1.412(8) 7_666 ?
C7 C3 1.418(6) 7_666 ?
N1 O2 1.362(4) . ?
O1 La1 2.649(3) 5_666 ?
O2 La1 2.568(3) 5_666 ?
O1W H1WA 1.0174 . ?
O1W H1WB 1.0173 . ?
O2W H2WA 0.8701 . ?
O2W H2WB 0.8699 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 La1 O2 129.32(13) . 2_655 ?
O2 La1 O2 120.92(11) . 6_565 ?
O2 La1 O2 59.68(11) 2_655 6_565 ?
O2 La1 O2 59.68(11) . 5_666 ?
O2 La1 O2 120.92(11) 2_655 5_666 ?
O2 La1 O2 178.79(12) 6_565 5_666 ?
O2 La1 O1W 82.69(10) . 2_655 ?
O2 La1 O1W 147.38(11) 2_655 2_655 ?
O2 La1 O1W 113.08(10) 6_565 2_655 ?
O2 La1 O1W 65.82(11) 5_666 2_655 ?
O2 La1 O1W 147.39(11) . . ?
O2 La1 O1W 82.69(10) 2_655 . ?
O2 La1 O1W 65.82(11) 6_565 . ?
O2 La1 O1W 113.08(10) 5_666 . ?
O1W La1 O1W 66.66(17) 2_655 . ?
O2 La1 O3 60.91(8) . . ?
O2 La1 O3 78.49(9) 2_655 . ?
O2 La1 O3 67.73(9) 6_565 . ?
O2 La1 O3 113.32(8) 5_666 . ?
O1W La1 O3 130.78(11) 2_655 . ?
O1W La1 O3 133.28(11) . . ?
O2 La1 O3 78.49(9) . 2_655 ?
O2 La1 O3 60.91(8) 2_655 2_655 ?
O2 La1 O3 113.32(8) 6_565 2_655 ?
O2 La1 O3 67.73(9) 5_666 2_655 ?
O1W La1 O3 133.28(11) 2_655 2_655 ?
O1W La1 O3 130.78(11) . 2_655 ?
O3 La1 O3 73.53(15) . 2_655 ?
O2 La1 O1 118.78(9) . 5_666 ?
O2 La1 O1 77.80(9) 2_655 5_666 ?
O2 La1 O1 119.85(9) 6_565 5_666 ?
O2 La1 O1 59.71(9) 5_666 5_666 ?
O1W La1 O1 80.70(12) 2_655 5_666 ?
O1W La1 O1 68.55(11) . 5_666 ?
O3 La1 O1 144.55(11) . 5_666 ?
O3 La1 O1 72.00(11) 2_655 5_666 ?
O2 La1 O1 77.80(9) . 6_565 ?
O2 La1 O1 118.78(9) 2_655 6_565 ?
O2 La1 O1 59.71(9) 6_565 6_565 ?
O2 La1 O1 119.85(9) 5_666 6_565 ?
O1W La1 O1 68.56(11) 2_655 6_565 ?
O1W La1 O1 80.70(12) . 6_565 ?
O3 La1 O1 72.00(11) . 6_565 ?
O3 La1 O1 144.55(11) 2_655 6_565 ?
O1 La1 O1 143.21(16) 5_666 6_565 ?
O1 C1 N1 119.7(4) . . ?
O1 C1 C6 124.2(4) . 7_666 ?
N1 C1 C6 116.1(3) . 7_666 ?
O3 C2 N1 118.5(4) . . ?
O3 C2 C3 124.5(4) . . ?
N1 C2 C3 116.9(4) . . ?
C4 C3 C7 120.4(4) . 7_666 ?
C4 C3 C2 120.6(4) . . ?
C7 C3 C2 119.1(4) 7_666 . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 120.5(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.2(4) . . ?
C5 C6 C1 120.2(4) . 7_666 ?
C7 C6 C1 119.6(4) . 7_666 ?
C6 C7 C7 119.8(5) . 7_666 ?
C6 C7 C3 121.2(4) . 7_666 ?
C7 C7 C3 118.9(5) 7_666 7_666 ?
O2 N1 C2 116.7(3) . . ?
O2 N1 C1 116.4(3) . . ?
C2 N1 C1 126.7(4) . . ?
C1 O1 La1 117.5(3) . 5_666 ?
N1 O2 La1 120.8(2) . . ?
N1 O2 La1 116.8(2) . 5_666 ?
La1 O2 La1 120.32(11) . 5_666 ?
C2 O3 La1 119.8(3) . . ?
La1 O1W H1WA 114.8 . . ?
La1 O1W H1WB 114.9 . . ?
H1WA O1W H1WB 99.0 . . ?
H2WA O2W H2WB 104.5 . . ?

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
O3 C2 C3 C4 -0.8(8) . . . . ?
N1 C2 C3 C4 177.4(5) . . . . ?
O3 C2 C3 C7 179.5(4) . . . 7_666 ?
N1 C2 C3 C7 -2.3(7) . . . 7_666 ?
C7 C3 C4 C5 -0.4(8) 7_666 . . . ?
C2 C3 C4 C5 179.9(5) . . . . ?
C3 C4 C5 C6 0.3(9) . . . . ?
C4 C5 C6 C7 0.2(8) . . . . ?
C4 C5 C6 C1 178.6(5) . . . 7_666 ?
C5 C6 C7 C7 -0.5(9) . . . 7_666 ?
C1 C6 C7 C7 -178.9(5) 7_666 . . 7_666 ?
C5 C6 C7 C3 179.9(5) . . . 7_666 ?
C1 C6 C7 C3 1.5(7) 7_666 . . 7_666 ?
O3 C2 N1 O2 -0.8(6) . . . . ?
C3 C2 N1 O2 -179.2(4) . . . . ?
O3 C2 N1 C1 -175.2(4) . . . . ?
C3 C2 N1 C1 6.4(7) . . . . ?
O1 C1 N1 O2 -2.2(6) . . . . ?
C6 C1 N1 O2 177.9(4) 7_666 . . . ?
O1 C1 N1 C2 172.3(4) . . . . ?
C6 C1 N1 C2 -7.6(7) 7_666 . . . ?
N1 C1 O1 La1 -22.9(6) . . . 5_666 ?
C6 C1 O1 La1 157.0(4) 7_666 . . 5_666 ?
C2 N1 O2 La1 15.4(5) . . . . ?
C1 N1 O2 La1 -169.6(3) . . . . ?
C2 N1 O2 La1 -148.2(3) . . . 5_666 ?
C1 N1 O2 La1 26.8(4) . . . 5_666 ?
N1 C2 O3 La1 -13.3(5) . . . . ?
C3 C2 O3 La1 164.9(4) . . . . ?

_refine_diff_density_max         0.915
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.112

# start Validation Reply Form
_vrf_PLAT420_la-neu              
;
PROBLEM: D-H Bond Without Acceptor O2W --H2WA . Please Check
RESPONSE: The Platon SQUEEZE routine has been applied to take 
care of not assigned electron density in the voids of this 
crystal structure.
;
# end Validation Reply Form



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

data_Sm-ONDI
_database_code_depnum_ccdc_archive 'CCDC 2181885'
loop_
_audit_author_name
_audit_author_address
'Harald Krautscheid'
;Universitaet Leipzig
Germany
;
_audit_update_record             
;
2022-09-15 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;

_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
SHELXL-2014/7
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H6 N2 O7 Sm, 1[Cl], 1[C3 H7 N O]'
_chemical_formula_sum            'C17 H13 Cl N3 O8 Sm'
_chemical_formula_weight         573.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   20.5997(12)
_cell_length_b                   12.3311(9)
_cell_length_c                   8.2059(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.074(5)
_cell_angle_gamma                90
_cell_volume                     2076.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    13840
_cell_measurement_theta_min      4.19
_cell_measurement_theta_max      71.31

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_F_000             1116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    22.873
_shelx_estimated_absorpt_T_min   0.204
_shelx_estimated_absorpt_T_max   0.658
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6670
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         4.183
_diffrn_reflns_theta_max         70.969
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1953
_reflns_number_gt                1847
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_refine_special_details          SQUEEZE
_platon_squeeze_special_details  
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 834Å³ in 1 void per unit cell. 
This is consistent with the presence of 1[Cl] per Formula Unit 
which accounts for 68 electrons per unit cell.
1[C3H7NO] per Formula Unit accounts for 160 electrons per unit cell.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0865P)²+8.4712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1953
_refine_ls_number_parameters     111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.5000 0.48435(4) 0.7500 0.0351(2) Uani 1 2 d S T P . .
C1 C 0.6399(3) 0.3795(6) 0.6514(7) 0.0397(14) Uani 1 1 d . . . . .
C2 C 0.7029(3) 0.3229(6) 0.6499(8) 0.0441(15) Uani 1 1 d . . . . .
C3 C 0.7441(3) 0.3172(7) 0.7900(8) 0.0535(19) Uani 1 1 d . . . . .
H3 H 0.7324 0.3504 0.8877 0.064 Uiso 1 1 calc R U . . .
C4 C 0.7199(3) 0.2775(6) 0.5006(8) 0.0439(15) Uani 1 1 d . . . . .
C5 C 0.6791(3) 0.2832(6) 0.3546(7) 0.0432(15) Uani 1 1 d . . . . .
C6 C 0.6958(3) 0.2384(7) 0.2115(8) 0.0494(17) Uani 1 1 d . . . . .
H6 H 0.6674 0.2445 0.1143 0.059 Uiso 1 1 calc R U . . .
C7 C 0.6175(3) 0.3436(6) 0.3552(8) 0.0394(13) Uani 1 1 d . . . . .
N1 N 0.6033(2) 0.3863(5) 0.5015(6) 0.0399(12) Uani 1 1 d . . . . .
O1 O 0.6180(2) 0.4186(4) 0.7730(5) 0.0464(11) Uani 1 1 d . . . . .
O2 O 0.54620(19) 0.4429(4) 0.5011(5) 0.0397(9) Uani 1 1 d . . . . .
O3 O 0.5778(2) 0.3589(4) 0.2326(5) 0.0463(11) Uani 1 1 d . . . . .
O1W O 0.5000 0.2910(7) 0.7500 0.070(2) Uani 1 2 d S T P . .
H1WA H 0.5116 0.2442 0.8385 0.105 Uiso 0.5 1 d R U P . .
H1WB H 0.4884 0.2442 0.6615 0.105 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O2 2.368(4) 6_566 ?
Sm1 O2 2.368(4) 5_666 ?
Sm1 O1W 2.384(9) . ?
Sm1 O2 2.384(4) . ?
Sm1 O2 2.384(4) 2_656 ?
Sm1 O3 2.524(5) 6_566 ?
Sm1 O3 2.524(5) 5_666 ?
Sm1 O1 2.554(4) . ?
Sm1 O1 2.554(4) 2_656 ?
C1 O1 1.229(7) . ?
C1 N1 1.387(8) . ?
C1 C2 1.475(8) . ?
C2 C3 1.369(9) . ?
C2 C4 1.419(9) . ?
C3 C6 1.416(9) 7_656 ?
C3 H3 0.9500 . ?
C4 C5 1.403(9) . ?
C4 C4 1.413(12) 7_656 ?
C5 C6 1.370(9) . ?
C5 C7 1.471(8) . ?
C6 C3 1.416(9) 7_656 ?
C6 H6 0.9500 . ?
C7 O3 1.253(7) . ?
C7 N1 1.366(8) . ?
N1 O2 1.368(6) . ?
O2 Sm1 2.368(4) 5_666 ?
O3 Sm1 2.524(5) 5_666 ?
O1W H1WA 0.9416 . ?
O1W H1WB 0.9416 . ?

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
O2 Sm1 O2 135.5(3) 6_566 5_666 ?
O2 Sm1 O1W 112.26(12) 6_566 . ?
O2 Sm1 O1W 112.26(13) 5_666 . ?
O2 Sm1 O2 131.79(18) 6_566 . ?
O2 Sm1 O2 59.73(17) 5_666 . ?
O1W Sm1 O2 77.62(13) . . ?
O2 Sm1 O2 59.73(17) 6_566 2_656 ?
O2 Sm1 O2 131.79(18) 5_666 2_656 ?
O1W Sm1 O2 77.63(13) . 2_656 ?
O2 Sm1 O2 155.3(3) . 2_656 ?
O2 Sm1 O3 63.29(14) 6_566 6_566 ?
O2 Sm1 O3 82.48(15) 5_666 6_566 ?
O1W Sm1 O3 140.00(11) . 6_566 ?
O2 Sm1 O3 79.16(16) . 6_566 ?
O2 Sm1 O3 121.09(15) 2_656 6_566 ?
O2 Sm1 O3 82.48(15) 6_566 5_666 ?
O2 Sm1 O3 63.29(14) 5_666 5_666 ?
O1W Sm1 O3 140.00(11) . 5_666 ?
O2 Sm1 O3 121.09(15) . 5_666 ?
O2 Sm1 O3 79.16(16) 2_656 5_666 ?
O3 Sm1 O3 80.0(2) 6_566 5_666 ?
O2 Sm1 O1 75.48(14) 6_566 . ?
O2 Sm1 O1 119.42(14) 5_666 . ?
O1W Sm1 O1 71.49(12) . . ?
O2 Sm1 O1 62.98(13) . . ?
O2 Sm1 O1 108.56(15) 2_656 . ?
O3 Sm1 O1 69.02(16) 6_566 . ?
O3 Sm1 O1 147.61(17) 5_666 . ?
O2 Sm1 O1 119.42(14) 6_566 2_656 ?
O2 Sm1 O1 75.48(15) 5_666 2_656 ?
O1W Sm1 O1 71.49(12) . 2_656 ?
O2 Sm1 O1 108.56(15) . 2_656 ?
O2 Sm1 O1 62.98(13) 2_656 2_656 ?
O3 Sm1 O1 147.61(17) 6_566 2_656 ?
O3 Sm1 O1 69.02(16) 5_666 2_656 ?
O1 Sm1 O1 143.0(2) . 2_656 ?
O1 C1 N1 119.2(5) . . ?
O1 C1 C2 125.3(6) . . ?
N1 C1 C2 115.5(5) . . ?
C3 C2 C4 121.5(6) . . ?
C3 C2 C1 119.8(6) . . ?
C4 C2 C1 118.7(6) . . ?
C2 C3 C6 119.7(6) . 7_656 ?
C2 C3 H3 120.2 . . ?
C6 C3 H3 120.2 7_656 . ?
C5 C4 C4 118.6(7) . 7_656 ?
C5 C4 C2 122.8(6) . . ?
C4 C4 C2 118.6(7) 7_656 . ?
C6 C5 C4 122.3(6) . . ?
C6 C5 C7 119.3(5) . . ?
C4 C5 C7 118.4(6) . . ?
C5 C6 C3 119.3(6) . 7_656 ?
C5 C6 H6 120.3 . . ?
C3 C6 H6 120.3 7_656 . ?
O3 C7 N1 118.2(5) . . ?
O3 C7 C5 125.1(6) . . ?
N1 C7 C5 116.7(5) . . ?
C7 N1 O2 116.4(5) . . ?
C7 N1 C1 127.9(5) . . ?
O2 N1 C1 115.6(5) . . ?
C1 O1 Sm1 118.6(4) . . ?
N1 O2 Sm1 118.4(3) . 5_666 ?
N1 O2 Sm1 121.0(3) . . ?
Sm1 O2 Sm1 120.27(17) 5_666 . ?
C7 O3 Sm1 116.3(4) . 5_666 ?
Sm1 O1W H1WA 127.8 . . ?
Sm1 O1W H1WB 127.8 . . ?
H1WA O1W H1WB 104.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -4.4(12) . . . . ?
N1 C1 C2 C3 176.3(7) . . . . ?
O1 C1 C2 C4 177.0(7) . . . . ?
N1 C1 C2 C4 -2.2(10) . . . . ?
C4 C2 C3 C6 -2.3(13) . . . 7_656 ?
C1 C2 C3 C6 179.2(7) . . . 7_656 ?
C3 C2 C4 C5 -179.1(8) . . . . ?
C1 C2 C4 C5 -0.6(11) . . . . ?
C3 C2 C4 C4 2.0(14) . . . 7_656 ?
C1 C2 C4 C4 -179.5(8) . . . 7_656 ?
C4 C4 C5 C6 -0.6(14) 7_656 . . . ?
C2 C4 C5 C6 -179.5(7) . . . . ?
C4 C4 C5 C7 -178.0(8) 7_656 . . . ?
C2 C4 C5 C7 3.1(11) . . . . ?
C4 C5 C6 C3 0.9(12) . . . 7_656 ?
C7 C5 C6 C3 178.3(7) . . . 7_656 ?
C6 C5 C7 O3 -0.5(11) . . . . ?
C4 C5 C7 O3 177.0(7) . . . . ?
C6 C5 C7 N1 179.8(7) . . . . ?
C4 C5 C7 N1 -2.6(10) . . . . ?
O3 C7 N1 O2 -0.1(9) . . . . ?
C5 C7 N1 O2 179.6(6) . . . . ?
O3 C7 N1 C1 180.0(6) . . . . ?
C5 C7 N1 C1 -0.3(10) . . . . ?
O1 C1 N1 C7 -176.5(7) . . . . ?
C2 C1 N1 C7 2.7(10) . . . . ?
O1 C1 N1 O2 3.5(9) . . . . ?
C2 C1 N1 O2 -177.2(6) . . . . ?
N1 C1 O1 Sm1 9.1(8) . . . . ?
C2 C1 O1 Sm1 -170.1(5) . . . . ?
C7 N1 O2 Sm1 -22.2(7) . . . 5_666 ?
C1 N1 O2 Sm1 157.7(4) . . . 5_666 ?
C7 N1 O2 Sm1 164.3(4) . . . . ?
C1 N1 O2 Sm1 -15.7(7) . . . . ?
N1 C7 O3 Sm1 20.5(8) . . . 5_666 ?
C5 C7 O3 Sm1 -159.1(5) . . . 5_666 ?

_refine_diff_density_max         1.411
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.135



