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

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

data_eu_sq_210810
_database_code_depnum_ccdc_archive 'CCDC 2218673'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-11-09
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Eu2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'europium(III) squarate'
_chemical_formula_moiety         'C12 H16 Eu2 O20'
_chemical_formula_sum            'C12 H16 Eu2 O20'
_chemical_formula_weight         784.17
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C7H6EuO9
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9363(9)
_cell_length_b                   8.2215(5)
_cell_length_c                   10.1229(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.017(7)
_cell_angle_gamma                90
_cell_volume                     987.93(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2856
_cell_measurement_temperature    296.3(3)
_cell_measurement_theta_max      30.0130
_cell_measurement_theta_min      2.9500
_shelx_estimated_absorpt_T_max   0.745
_shelx_estimated_absorpt_T_min   0.195
_exptl_absorpt_coefficient_mu    6.397
_exptl_absorpt_correction_T_max  0.06682
_exptl_absorpt_correction_T_min  0.04018
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.049
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7654
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.664
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.077
_diffrn_reflns_theta_min         2.477
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.3(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     49.00  84.00   0.50    5.42    --   -5.40  45.00 150.00   70
  2  ω    -94.00  83.00   0.50    5.42    --   -5.40  45.00  90.00  354
  3  ω    -46.00  26.00   0.50    5.42    --   -5.40  45.00 150.00  144
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0153061000
_diffrn_orient_matrix_UB_12      -0.0790105000
_diffrn_orient_matrix_UB_13      0.0198603000
_diffrn_orient_matrix_UB_21      0.0575420000
_diffrn_orient_matrix_UB_22      -0.0233886000
_diffrn_orient_matrix_UB_23      0.0065992000
_diffrn_orient_matrix_UB_31      0.0054219000
_diffrn_orient_matrix_UB_32      0.0252249000
_diffrn_orient_matrix_UB_33      0.0673162000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.576
_reflns_Friedel_fraction_full    0.743
_reflns_Friedel_fraction_max     0.486
_reflns_number_gt                3114
_reflns_number_total             3858
_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       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3858
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0689P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1112
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Eu1-H16A \\sim Eu1-H16B
 with sigma of 0.02
 Eu2-H18A \\sim Eu2-H18B
 with sigma of 0.02
 Eu1-H15A \\sim Eu1-H15B
 with sigma of 0.02
 Eu2-H19A \\sim Eu2-H19B
 with sigma of 0.02
3.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
3.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_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
C1 C 0.1471(15) 0.3667(16) 0.6174(16) 0.025(3) Uani 1 1 d . . . . .
C2 C 0.1180(15) 0.2038(18) 0.6636(17) 0.029(3) Uani 1 1 d . . . . .
C3 C 0.1736(15) 0.1323(17) 0.5586(17) 0.024(4) Uani 1 1 d . . . . .
C4 C 0.1967(14) 0.2917(19) 0.5067(18) 0.029(4) Uani 1 1 d . . . . .
C5 C 0.4728(10) 0.9898(12) 0.5827(12) 0.029(2) Uani 1 1 d . . . . .
C6 C 0.4531(17) 1.1609(15) 0.618(2) 0.043(4) Uani 1 1 d . . . . .
C7 C 0.5265(11) 1.2083(15) 0.5108(13) 0.031(2) Uani 1 1 d . . . . .
C8 C 0.5528(10) 1.0388(12) 0.4898(12) 0.028(2) Uani 1 1 d . . . . .
C9 C 0.8227(15) 0.3685(16) 0.5616(18) 0.024(4) Uani 1 1 d . . . . .
C10 C 0.7997(13) 0.2114(17) 0.6180(13) 0.021(3) Uani 1 1 d . . . . .
C11 C 0.8496(16) 0.1276(15) 0.5114(16) 0.023(4) Uani 1 1 d . . . . .
C12 C 0.8803(14) 0.2836(17) 0.4584(17) 0.022(3) Uani 1 1 d . . . . .
Eu1 Eu 0.25443(4) 0.75489(5) 0.67850(4) 0.0208(3) Uani 1 1 d D . . . .
Eu2 Eu 0.74636(4) 0.74840(5) 0.44366(4) 0.0214(3) Uani 1 1 d D . . . .
O1 O 0.1436(11) 0.5117(10) 0.6568(12) 0.034(3) Uani 1 1 d . . . . .
O2 O 0.0656(12) 0.1604(11) 0.7581(13) 0.036(3) Uani 1 1 d . . . . .
O3 O 0.2001(11) -0.0134(10) 0.5369(12) 0.029(3) Uani 1 1 d . . . . .
O4 O 0.2447(12) 0.3378(10) 0.4078(12) 0.030(3) Uani 1 1 d . . . . .
O5 O 0.4312(12) 0.8563(10) 0.6195(14) 0.036(3) Uani 1 1 d . . . . .
O6 O 0.4043(10) 1.2343(8) 0.6957(11) 0.033(2) Uani 1 1 d . . . . .
O7 O 0.5513(13) 1.3370(11) 0.4592(14) 0.049(4) Uani 1 1 d . . . . .
O8 O 0.6168(11) 0.9645(11) 0.4180(12) 0.034(2) Uani 1 1 d . . . . .
O9 O 0.7961(12) 0.5112(10) 0.5893(11) 0.027(3) Uani 1 1 d . . . . .
O10 O 0.7520(12) 0.1572(9) 0.7165(12) 0.030(3) Uani 1 1 d . . . . .
O11 O 0.8616(11) -0.0104(10) 0.4681(12) 0.032(2) Uani 1 1 d . . . . .
O12 O 0.9278(11) 0.3378(10) 0.3641(13) 0.031(3) Uani 1 1 d . . . . .
O13 O 0.3986(10) 0.5531(10) 0.7258(13) 0.040(3) Uani 1 1 d . . . . .
H13A H 0.4205 0.5116 0.6512 0.059 Uiso 1 1 d R U . . .
H13B H 0.3725 0.4657 0.7651 0.059 Uiso 1 1 d R U . . .
O14 O 0.2507(16) 0.6674(12) 0.4490(14) 0.059(4) Uani 1 1 d . . . . .
H14A H 0.3016 0.7217 0.4070 0.089 Uiso 1 1 d R U . . .
H14B H 0.2736 0.5643 0.4431 0.089 Uiso 1 1 d R U . . .
O15 O 0.0736(11) 0.8353(11) 0.7367(14) 0.033(3) Uani 1 1 d G . . . .
H15A H 0.0201 0.7731 0.7536 0.049 Uiso 1 1 d DG U . . .
H15B H 0.0434 0.9287 0.7262 0.049 Uiso 1 1 d DG U . . .
O16 O 0.3063(11) 0.9837(10) 0.8165(12) 0.028(2) Uani 1 1 d G . . . .
H16A H 0.2676 1.0227 0.8749 0.041 Uiso 1 1 d DG U . . .
H16B H 0.3478 1.0622 0.7967 0.041 Uiso 1 1 d DG U . . .
O17 O 0.7529(15) 0.8249(9) 0.6781(15) 0.046(3) Uani 1 1 d . . . . .
H17A H 0.7713 0.9255 0.6873 0.068 Uiso 1 1 d R U . . .
H17B H 0.8064 0.7739 0.7239 0.068 Uiso 1 1 d R U . . .
O18 O 0.5715(11) 0.6460(10) 0.5137(14) 0.035(3) Uani 1 1 d G . . . .
H18A H 0.5482 0.5483 0.5110 0.052 Uiso 1 1 d DG U . . .
H18B H 0.5256 0.6964 0.5577 0.052 Uiso 1 1 d DG U . . .
O19 O 0.6864(12) 0.5192(10) 0.3101(12) 0.033(3) Uani 1 1 d G . . . .
H19A H 0.7021 0.4974 0.2320 0.050 Uiso 1 1 d DG U . . .
H19B H 0.6499 0.4367 0.3326 0.050 Uiso 1 1 d DG U . . .
O20 O 0.9243(12) 0.6633(11) 0.3941(14) 0.040(3) Uani 1 1 d . . . . .
H20A H 0.9199 0.5668 0.3616 0.059 Uiso 1 1 d R U . . .
H20B H 0.9458 0.7217 0.3310 0.059 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
C1 C2 1.472(19) . ?
C1 C4 1.46(2) . ?
C1 O1 1.259(16) . ?
C2 C3 1.44(2) . ?
C2 O2 1.248(19) . ?
C3 C4 1.450(18) . ?
C3 O3 1.264(17) . ?
C4 O4 1.262(19) . ?
C5 C6 1.476(16) . ?
C5 C8 1.464(15) . ?
C5 O5 1.277(14) . ?
C6 C7 1.51(2) . ?
C6 O6 1.19(2) . ?
C7 C8 1.449(16) . ?
C7 O7 1.230(15) . ?
C8 O8 1.266(14) . ?
C9 C10 1.450(18) . ?
C9 C12 1.483(18) . ?
C9 O9 1.255(15) . ?
C10 C11 1.459(19) . ?
C10 O10 1.279(17) . ?
C11 C12 1.452(18) . ?
C11 O11 1.230(16) . ?
C12 O12 1.243(18) . ?
Eu1 O1 2.395(10) . ?
Eu1 O3 2.431(10) 1_565 ?
Eu1 O4 2.457(11) 2_565 ?
Eu1 O5 2.401(13) . ?
Eu1 O13 2.402(11) . ?
Eu1 O14 2.428(14) . ?
Eu1 O15 2.389(12) . ?
Eu1 O16 2.386(10) . ?
Eu2 O8 2.352(10) . ?
Eu2 O9 2.479(10) . ?
Eu2 O10 2.435(11) 2_564 ?
Eu2 O11 2.412(10) 1_565 ?
Eu2 O17 2.449(15) . ?
Eu2 O18 2.424(11) . ?
Eu2 O19 2.385(10) . ?
Eu2 O20 2.340(14) . ?
Eu2 H20A 2.7511 . ?
Eu2 H20B 2.7535 . ?
O3 Eu1 2.431(10) 1_545 ?
O4 Eu1 2.457(11) 2_564 ?
O10 Eu2 2.435(11) 2_565 ?
O11 Eu2 2.412(10) 1_545 ?
O13 H13A 0.8925 . ?
O13 H13B 0.8929 . ?
O14 H14A 0.8965 . ?
O14 H14B 0.8952 . ?
O15 H15A 0.8502 . ?
O15 H15B 0.8501 . ?
O16 H16A 0.8501 . ?
O16 H16B 0.8501 . ?
O17 H17A 0.8580 . ?
O17 H17B 0.8582 . ?
O18 H18A 0.8498 . ?
O18 H18B 0.8492 . ?
O19 H19A 0.8499 . ?
O19 H19B 0.8500 . ?
O20 H20A 0.8584 . ?
O20 H20B 0.8585 . ?

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
C4 C1 C2 89.3(10) . . ?
O1 C1 C2 138.0(16) . . ?
O1 C1 C4 132.3(15) . . ?
C3 C2 C1 89.7(12) . . ?
O2 C2 C1 131.1(15) . . ?
O2 C2 C3 139.2(15) . . ?
C2 C3 C4 91.1(11) . . ?
O3 C3 C2 131.3(15) . . ?
O3 C3 C4 137.2(16) . . ?
C3 C4 C1 89.7(11) . . ?
O4 C4 C1 137.5(15) . . ?
O4 C4 C3 132.7(17) . . ?
C8 C5 C6 91.4(10) . . ?
O5 C5 C6 132.3(12) . . ?
O5 C5 C8 136.3(10) . . ?
C5 C6 C7 87.4(12) . . ?
O6 C6 C5 138.0(15) . . ?
O6 C6 C7 134.6(11) . . ?
C8 C7 C6 90.5(10) . . ?
O7 C7 C6 135.1(14) . . ?
O7 C7 C8 134.4(13) . . ?
C7 C8 C5 90.2(8) . . ?
O8 C8 C5 135.2(10) . . ?
O8 C8 C7 134.5(11) . . ?
C10 C9 C12 88.8(10) . . ?
O9 C9 C10 133.0(14) . . ?
O9 C9 C12 138.1(14) . . ?
C9 C10 C11 91.2(11) . . ?
O10 C10 C9 137.4(14) . . ?
O10 C10 C11 131.4(12) . . ?
C12 C11 C10 89.7(10) . . ?
O11 C11 C10 140.5(14) . . ?
O11 C11 C12 129.8(14) . . ?
C11 C12 C9 90.1(11) . . ?
O12 C12 C9 130.9(13) . . ?
O12 C12 C11 138.9(14) . . ?
O1 Eu1 O3 119.3(5) . 1_565 ?
O1 Eu1 O4 75.4(4) . 2_565 ?
O1 Eu1 O5 139.3(4) . . ?
O1 Eu1 O13 79.6(4) . . ?
O1 Eu1 O14 73.2(4) . . ?
O3 Eu1 O4 139.8(4) 1_565 2_565 ?
O5 Eu1 O3 76.6(4) . 1_565 ?
O5 Eu1 O4 118.2(5) . 2_565 ?
O5 Eu1 O13 70.1(4) . . ?
O5 Eu1 O14 78.1(5) . . ?
O13 Eu1 O3 143.1(5) . 1_565 ?
O13 Eu1 O4 72.6(4) . 2_565 ?
O13 Eu1 O14 85.8(5) . . ?
O14 Eu1 O3 72.0(4) . 1_565 ?
O14 Eu1 O4 144.5(2) . 2_565 ?
O15 Eu1 O1 75.5(4) . . ?
O15 Eu1 O3 74.7(4) . 1_565 ?
O15 Eu1 O4 73.7(5) . 2_565 ?
O15 Eu1 O5 143.6(3) . . ?
O15 Eu1 O13 142.1(4) . . ?
O15 Eu1 O14 113.0(6) . . ?
O16 Eu1 O1 145.0(5) . . ?
O16 Eu1 O3 76.4(3) . 1_565 ?
O16 Eu1 O4 74.1(4) . 2_565 ?
O16 Eu1 O5 72.0(4) . . ?
O16 Eu1 O13 106.9(5) . . ?
O16 Eu1 O14 140.5(4) . . ?
O16 Eu1 O15 79.8(4) . . ?
O8 Eu2 O9 140.7(4) . . ?
O8 Eu2 O10 74.8(4) . 2_564 ?
O8 Eu2 O11 75.6(3) . 1_565 ?
O8 Eu2 O17 82.3(4) . . ?
O8 Eu2 O18 73.7(4) . . ?
O8 Eu2 O19 112.3(5) . . ?
O8 Eu2 H20A 152.1 . . ?
O8 Eu2 H20B 127.0 . . ?
O9 Eu2 H20A 67.2 . . ?
O9 Eu2 H20B 91.1 . . ?
O10 Eu2 O9 141.6(3) 2_564 . ?
O10 Eu2 O17 146.3(3) 2_564 . ?
O10 Eu2 H20A 78.0 2_564 . ?
O10 Eu2 H20B 61.6 2_564 . ?
O11 Eu2 O9 119.2(5) 1_565 . ?
O11 Eu2 O10 76.3(4) 1_565 2_564 ?
O11 Eu2 O17 74.3(4) 1_565 . ?
O11 Eu2 O18 139.0(4) 1_565 . ?
O11 Eu2 H20A 92.2 1_565 . ?
O11 Eu2 H20B 66.4 1_565 . ?
O17 Eu2 O9 69.2(3) . . ?
O17 Eu2 H20A 118.9 . . ?
O17 Eu2 H20B 118.7 . . ?
O18 Eu2 O9 73.3(4) . . ?
O18 Eu2 O10 119.8(5) . 2_564 ?
O18 Eu2 O17 75.3(5) . . ?
O18 Eu2 H20A 126.8 . . ?
O18 Eu2 H20B 154.3 . . ?
O19 Eu2 O9 75.8(3) . . ?
O19 Eu2 O10 75.7(4) . 2_564 ?
O19 Eu2 O11 147.4(5) . 1_565 ?
O19 Eu2 O17 136.9(4) . . ?
O19 Eu2 O18 71.0(4) . . ?
O19 Eu2 H20A 65.8 . . ?
O19 Eu2 H20B 85.6 . . ?
O20 Eu2 O8 143.4(4) . . ?
O20 Eu2 O9 74.1(4) . . ?
O20 Eu2 O10 77.1(4) . 2_564 ?
O20 Eu2 O11 75.3(4) . 1_565 ?
O20 Eu2 O17 110.3(6) . . ?
O20 Eu2 O18 142.0(3) . . ?
O20 Eu2 O19 82.4(4) . . ?
O20 Eu2 H20A 17.1 . . ?
O20 Eu2 H20B 17.0 . . ?
H20A Eu2 H20B 28.5 . . ?
C1 O1 Eu1 141.6(11) . . ?
C3 O3 Eu1 134.1(10) . 1_545 ?
C4 O4 Eu1 136.6(11) . 2_564 ?
C5 O5 Eu1 138.6(8) . . ?
C8 O8 Eu2 136.9(8) . . ?
C9 O9 Eu2 130.7(10) . . ?
C10 O10 Eu2 133.1(9) . 2_565 ?
C11 O11 Eu2 135.1(11) . 1_545 ?
Eu1 O13 H13A 111.2 . . ?
Eu1 O13 H13B 111.6 . . ?
H13A O13 H13B 102.5 . . ?
Eu1 O14 H14A 111.1 . . ?
Eu1 O14 H14B 111.7 . . ?
H14A O14 H14B 102.2 . . ?
Eu1 O15 H15A 126.9 . . ?
Eu1 O15 H15B 127.0 . . ?
H15A O15 H15B 104.5 . . ?
Eu1 O16 H16A 125.3 . . ?
Eu1 O16 H16B 125.6 . . ?
H16A O16 H16B 104.5 . . ?
Eu2 O17 H17A 109.5 . . ?
Eu2 O17 H17B 110.1 . . ?
H17A O17 H17B 104.2 . . ?
Eu2 O18 H18A 127.4 . . ?
Eu2 O18 H18B 127.3 . . ?
H18A O18 H18B 104.6 . . ?
Eu2 O19 H19A 127.7 . . ?
Eu2 O19 H19B 127.6 . . ?
H19A O19 H19B 104.5 . . ?
Eu2 O20 H20A 109.7 . . ?
Eu2 O20 H20B 109.9 . . ?
H20A O20 H20B 104.1 . . ?

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
C1 C2 C3 C4 -3.4(14) . . . . ?
C1 C2 C3 O3 169.6(18) . . . . ?
C1 C4 O4 Eu1 -146.0(16) . . . 2_564 ?
C2 C1 C4 C3 -3.3(14) . . . . ?
C2 C1 C4 O4 179.2(19) . . . . ?
C2 C1 O1 Eu1 135.1(18) . . . . ?
C2 C3 C4 C1 3.4(14) . . . . ?
C2 C3 C4 O4 -178.9(18) . . . . ?
C2 C3 O3 Eu1 -32(3) . . . 1_545 ?
C3 C4 O4 Eu1 37(3) . . . 2_564 ?
C4 C1 C2 C3 3.4(14) . . . . ?
C4 C1 C2 O2 -176.7(18) . . . . ?
C4 C1 O1 Eu1 -37(3) . . . . ?
C4 C3 O3 Eu1 138.0(17) . . . 1_545 ?
C5 C6 C7 C8 -5.6(11) . . . . ?
C5 C6 C7 O7 172.4(16) . . . . ?
C5 C8 O8 Eu2 -46(2) . . . . ?
C6 C5 C8 C7 -5.8(11) . . . . ?
C6 C5 C8 O8 175.7(17) . . . . ?
C6 C5 O5 Eu1 35(3) . . . . ?
C6 C7 C8 C5 5.6(11) . . . . ?
C6 C7 C8 O8 -175.8(16) . . . . ?
C7 C8 O8 Eu2 135.7(13) . . . . ?
C8 C5 C6 C7 5.5(11) . . . . ?
C8 C5 C6 O6 -173(2) . . . . ?
C8 C5 O5 Eu1 -142.3(12) . . . . ?
C9 C10 C11 C12 3.7(15) . . . . ?
C9 C10 C11 O11 -173(2) . . . . ?
C9 C10 O10 Eu2 -38(3) . . . 2_565 ?
C10 C9 C12 C11 3.6(15) . . . . ?
C10 C9 C12 O12 -179.8(19) . . . . ?
C10 C9 O9 Eu2 -143.6(15) . . . . ?
C10 C11 C12 C9 -3.6(15) . . . . ?
C10 C11 C12 O12 -180(2) . . . . ?
C10 C11 O11 Eu2 38(3) . . . 1_545 ?
C11 C10 O10 Eu2 145.5(13) . . . 2_565 ?
C12 C9 C10 C11 -3.6(15) . . . . ?
C12 C9 C10 O10 179.0(19) . . . . ?
C12 C9 O9 Eu2 31(3) . . . . ?
C12 C11 O11 Eu2 -137.3(16) . . . 1_545 ?
O1 C1 C2 C3 -170(2) . . . . ?
O1 C1 C2 O2 9(4) . . . . ?
O1 C1 C4 C3 171.0(17) . . . . ?
O1 C1 C4 O4 -6(3) . . . . ?
O2 C2 C3 C4 177(2) . . . . ?
O2 C2 C3 O3 -10(4) . . . . ?
O3 C3 C4 C1 -169(2) . . . . ?
O3 C3 C4 O4 9(4) . . . . ?
O5 C5 C6 C7 -172.6(15) . . . . ?
O5 C5 C6 O6 9(4) . . . . ?
O5 C5 C8 C7 172.2(16) . . . . ?
O5 C5 C8 O8 -6(3) . . . . ?
O6 C6 C7 C8 173(2) . . . . ?
O6 C6 C7 O7 -9(4) . . . . ?
O7 C7 C8 C5 -172.4(16) . . . . ?
O7 C7 C8 O8 6(3) . . . . ?
O9 C9 C10 C11 172.7(18) . . . . ?
O9 C9 C10 O10 -5(3) . . . . ?
O9 C9 C12 C11 -172(2) . . . . ?
O9 C9 C12 O12 4(4) . . . . ?
O10 C10 C11 C12 -178.6(17) . . . . ?
O10 C10 C11 O11 5(4) . . . . ?
O11 C11 C12 C9 173.4(17) . . . . ?
O11 C11 C12 O12 -3(4) . . . . ?

_olex2_submission_original_sample_id Eu_squarate
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.821
####################################################################### 
# 
# 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_yb_sq
_database_code_depnum_ccdc_archive 'CCDC 2218679'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Yb2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'ytterbium(III) squarate'
_chemical_formula_moiety         'C12 H16 O20 Yb2'
_chemical_formula_sum            'C12 H16 O20 Yb2'
_chemical_formula_weight         826.33
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16O20Yb2
_chemical_oxdiff_usercomment     'willow-leaf type'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9168(4)
_cell_length_b                   8.1217(2)
_cell_length_c                   9.9844(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.823(3)
_cell_angle_gamma                90
_cell_volume                     961.35(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7938
_cell_measurement_temperature    297.95(10)
_cell_measurement_theta_max      31.8180
_cell_measurement_theta_min      3.5540
_shelx_estimated_absorpt_T_max   0.596
_shelx_estimated_absorpt_T_min   0.184
_exptl_absorpt_coefficient_mu    9.777
_exptl_absorpt_correction_T_max  0.617
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.855
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 0 1 0.0715
-17 -1 0 0.0730
13 -6 -6 0.0397
-6 -5 -11 0.1183
-16 3 -1 0.0671
16 -3 1 0.0367
0 -11 -1 0.0556
0 11 -2 0.0102
0 -11 1 0.0541
-9 -4 -10 0.1125
17 -1 0 0.0252
0 6 12 0.1107
-14 4 7 0.0864
-17 0 -1 0.0730
-1 -11 -2 0.0629
3 -2 13 0.1179
0 11 -1 0.0042
-5 -6 -10 0.1131
-15 -5 1 0.0854
-13 -1 9 0.1016
15 5 0 0.0195

_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.059
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-16.7816 -0.2616 0.7269 0.9010 0.3738 0.2203
-16.6636 -0.7066 -0.1925 0.8830 0.3660 0.2938
12.9354 -6.1137 -5.9955 -0.6846 -0.5840 0.4363
-6.3610 -4.6054 -11.1321 0.1738 0.1546 0.9726
-15.9664 3.0674 -0.8846 0.7491 0.6428 0.1600
15.9637 -2.8288 1.3249 -0.7439 -0.6386 -0.1971
-0.2879 -11.3908 -1.3592 0.2290 -0.7777 0.5855
-0.4584 11.3435 -1.8114 -0.2625 0.8870 -0.3799
0.2948 -11.4084 1.1160 0.2563 -0.8670 0.4274
-9.3435 -4.4194 -9.5144 0.3634 0.1936 0.9113
16.6690 -0.6530 0.1839 -0.8542 -0.4644 -0.2338
0.3819 6.0199 11.8730 0.1259 0.0735 -0.9893
-14.1116 4.1309 6.8812 0.8094 0.4430 -0.3854
-16.5674 0.2725 -0.9233 0.8399 0.4563 0.2938
-0.6561 -11.2478 -2.4970 0.2188 -0.7244 0.6538
3.2355 -2.0846 13.2255 0.1826 -0.6243 -0.7595
-0.1904 11.4199 -0.9574 -0.2584 0.8605 -0.4390
-5.4621 -6.1473 -10.4369 0.1761 -0.0000 0.9844
-15.0030 -5.1357 0.6392 0.9109 -0.0206 0.4122
-13.4417 -1.0423 9.4497 0.9455 -0.0247 -0.3248
14.6940 5.4092 0.3199 -0.8783 0.0195 -0.4777

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11611
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.853
_diffrn_reflns_theta_min         3.437
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.95(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  33.00   0.50    0.50    --    3.74 -99.00-150.00  102
  2  ω    -17.00  34.00   0.50    0.50    --    3.74 -99.00 -90.00  102
  3  ω    -15.00  11.00   0.50    0.50    --    3.74 -99.00   0.00   52
  4  ω    -37.00  20.00   0.50    0.50    --    3.74 -81.00  45.00  114
  5  ω    -16.00  21.00   0.50    0.50    --    3.74  81.00 167.00   74
  6  ω     13.00  50.00   0.50    0.50    --    3.74  77.00  30.00   74
  7  ω    -52.00  -1.00   0.50    0.50    --   -4.52   0.00 -30.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0523454000
_diffrn_orient_matrix_UB_12      -0.0215499000
_diffrn_orient_matrix_UB_13      0.0232162000
_diffrn_orient_matrix_UB_21      -0.0246938000
_diffrn_orient_matrix_UB_22      0.0724472000
_diffrn_orient_matrix_UB_23      -0.0297461000
_diffrn_orient_matrix_UB_31      -0.0150730000
_diffrn_orient_matrix_UB_32      -0.0437808000
_diffrn_orient_matrix_UB_33      -0.0606417000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.841
_reflns_number_gt                4091
_reflns_number_total             4622
_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       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0296P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0607
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.56(2)
 0.44(2)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Yb1-H14A \\sim Yb1-H14B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_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
Yb1 Yb 0.74432(2) 0.24442(3) 0.32090(2) 0.01400(13) Uani 1 1 d D . . . .
Yb2 Yb 0.25512(2) 0.25172(3) 0.55687(2) 0.01252(12) Uani 1 1 d . . . . .
O1 O 0.8519(6) 0.4853(6) 0.3368(7) 0.0239(12) Uani 1 1 d . . . . .
O2 O 0.9319(6) 0.8399(7) 0.2374(7) 0.0267(14) Uani 1 1 d . . . . .
O3 O 0.7963(6) 1.0164(7) 0.4637(6) 0.0189(12) Uani 1 1 d . . . . .
O4 O 0.7516(6) 0.6594(7) 0.5951(7) 0.0249(14) Uani 1 1 d . . . . .
O5 O 0.5687(6) 0.1493(7) 0.3834(7) 0.0244(14) Uani 1 1 d . . . . .
O6 O 0.5977(5) -0.2337(6) 0.3046(6) 0.0249(12) Uani 1 1 d . . . . .
O7 O 0.4484(5) -0.3351(7) 0.5504(6) 0.0312(13) Uani 1 1 d . . . . .
O8 O 0.3777(5) 0.0391(6) 0.5802(6) 0.0217(11) Uani 1 1 d . . . . .
O9 O 0.2065(6) 0.4871(6) 0.4140(6) 0.0179(12) Uani 1 1 d . . . . .
O10 O 0.2468(6) 0.8453(6) 0.2822(6) 0.0185(12) Uani 1 1 d . . . . .
O11 O 0.1382(5) 1.0184(6) 0.5358(7) 0.0219(11) Uani 1 1 d . . . . .
O12 O 0.0712(6) 0.6617(7) 0.6416(7) 0.0232(13) Uani 1 1 d . . . . .
O13 O 0.6049(5) 0.4447(6) 0.2799(6) 0.0259(12) Uani 1 1 d . . . . .
H13A H 0.6315 0.5293 0.2421 0.039 Uiso 1 1 d R U . . .
H13B H 0.5529 0.4092 0.2210 0.039 Uiso 1 1 d R U . . .
O14 O 0.7494(8) 0.3273(8) 0.5453(8) 0.0401(18) Uani 1 1 d . . . . .
H14A H 0.6908 0.2864 0.5847 0.060 Uiso 1 1 d DR U . . .
H14B H 0.7392 0.4367 0.5536 0.060 Uiso 1 1 d DR U . . .
O15 O 0.9194(6) 0.1683(8) 0.2707(8) 0.0274(14) Uani 1 1 d G . . . .
H15A H 0.9736 0.2318 0.2593 0.041 Uiso 1 1 d G U . . .
H15B H 0.9502 0.0764 0.2874 0.041 Uiso 1 1 d G U . . .
O16 O 0.6933(6) 0.0228(7) 0.1871(7) 0.0238(13) Uani 1 1 d G . . . .
H16A H 0.7217 -0.0078 0.1177 0.036 Uiso 1 1 d G U . . .
H16B H 0.6654 -0.0632 0.2170 0.036 Uiso 1 1 d G U . . .
O17 O 0.2425(7) 0.1798(6) 0.3270(8) 0.0298(12) Uani 1 1 d . . . . .
H17A H 0.2239 0.0777 0.3169 0.045 Uiso 1 1 d R U . . .
H17B H 0.1882 0.2311 0.2796 0.045 Uiso 1 1 d R U . . .
O18 O 0.4227(6) 0.3529(8) 0.4879(8) 0.0292(15) Uani 1 1 d G . . . .
H18A H 0.4455 0.4503 0.4986 0.044 Uiso 1 1 d G U . . .
H18B H 0.4809 0.2995 0.4737 0.044 Uiso 1 1 d G U . . .
O19 O 0.3114(6) 0.4741(7) 0.6925(7) 0.0212(12) Uani 1 1 d G . . . .
H19A H 0.2952 0.5082 0.7674 0.032 Uiso 1 1 d G U . . .
H19B H 0.3513 0.5496 0.6639 0.032 Uiso 1 1 d G U . . .
O20 O 0.0803(6) 0.3348(7) 0.6058(7) 0.0254(14) Uani 1 1 d . . . . .
H20A H 0.0845 0.4304 0.6428 0.038 Uiso 1 1 d R U . . .
H20B H 0.0565 0.2728 0.6668 0.038 Uiso 1 1 d R U . . .
C1 C 0.8481(7) 0.6279(9) 0.3843(9) 0.0168(16) Uani 1 1 d . U . . .
C2 C 0.8813(8) 0.7895(10) 0.3333(9) 0.0143(14) Uani 1 1 d . U . . .
C3 C 0.8257(7) 0.8705(9) 0.4383(9) 0.0151(15) Uani 1 1 d . U . . .
C4 C 0.8008(7) 0.7111(10) 0.4940(8) 0.0151(13) Uani 1 1 d . U . . .
C5 C 0.5270(5) 0.0133(7) 0.4182(6) 0.0174(11) Uani 1 1 d . . . . .
C6 C 0.5451(6) -0.1591(8) 0.3882(8) 0.0199(14) Uani 1 1 d . . . . .
C7 C 0.4725(6) -0.2060(9) 0.4930(7) 0.0203(12) Uani 1 1 d . . . . .
C8 C 0.4446(5) -0.0322(7) 0.5113(6) 0.0173(11) Uani 1 1 d . . . . .
C9 C 0.1803(7) 0.6324(9) 0.4388(9) 0.0133(14) Uani 1 1 d . U . . .
C10 C 0.2009(7) 0.7951(11) 0.3815(8) 0.0156(13) Uani 1 1 d . U . . .
C11 C 0.1491(7) 0.8757(9) 0.4945(8) 0.0142(15) Uani 1 1 d . U . . .
C12 C 0.1193(7) 0.7119(11) 0.5437(9) 0.0166(14) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.336(6) . ?
Yb1 O3 2.381(6) 1_545 ?
Yb1 O4 2.396(7) 2_564 ?
Yb1 O5 2.373(7) . ?
Yb1 O13 2.331(6) . ?
Yb1 H13A 2.7505 . ?
Yb1 H13B 2.7431 . ?
Yb1 O14 2.335(8) . ?
Yb1 O15 2.280(7) . ?
Yb1 O16 2.286(6) . ?
Yb2 O8 2.259(5) . ?
Yb2 O9 2.420(6) . ?
Yb2 O10 2.395(6) 2_565 ?
Yb2 O11 2.349(5) 1_545 ?
Yb2 O17 2.358(8) . ?
Yb2 O18 2.327(7) . ?
Yb2 O19 2.316(6) . ?
Yb2 O20 2.290(7) . ?
Yb2 H20A 2.7069 . ?
Yb2 H20B 2.7131 . ?
O1 C1 1.254(9) . ?
O2 C2 1.251(10) . ?
O3 Yb1 2.381(6) 1_565 ?
O3 C3 1.269(9) . ?
O4 Yb1 2.396(7) 2_565 ?
O4 C4 1.288(10) . ?
O5 C5 1.274(8) . ?
O6 C6 1.250(9) . ?
O7 C7 1.242(8) . ?
O8 C8 1.247(7) . ?
O9 C9 1.252(8) . ?
O10 Yb2 2.395(6) 2_564 ?
O10 C10 1.248(9) . ?
O11 Yb2 2.349(5) 1_565 ?
O11 C11 1.241(9) . ?
O12 C12 1.251(11) . ?
O13 H13A 0.8600 . ?
O13 H13B 0.8600 . ?
O14 H14A 0.8997 . ?
O14 H14B 0.9019 . ?
O15 H15A 0.8436 . ?
O15 H15B 0.8408 . ?
O16 H16A 0.8395 . ?
O16 H16B 0.8416 . ?
O17 H17A 0.8618 . ?
O17 H17B 0.8687 . ?
O18 H18A 0.8403 . ?
O18 H18B 0.8423 . ?
O19 H19A 0.8385 . ?
O19 H19B 0.8426 . ?
O20 H20A 0.8585 . ?
O20 H20B 0.8596 . ?
C1 C2 1.476(11) . ?
C1 C4 1.449(11) . ?
C2 C3 1.453(11) . ?
C3 C4 1.452(11) . ?
C5 C6 1.452(8) . ?
C5 C8 1.466(8) . ?
C6 C7 1.474(10) . ?
C7 C8 1.466(9) . ?
C9 C10 1.471(10) . ?
C9 C12 1.482(11) . ?
C10 C11 1.492(11) . ?
C11 C12 1.474(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Yb1 O3 120.2(2) . 1_545 ?
O1 Yb1 O4 73.7(2) . 2_564 ?
O1 Yb1 O5 138.4(2) . . ?
O1 Yb1 H13A 64.1 . . ?
O1 Yb1 H13B 92.7 . . ?
O3 Yb1 O4 141.7(2) 1_545 2_564 ?
O3 Yb1 H13A 156.3 1_545 . ?
O3 Yb1 H13B 138.9 1_545 . ?
O4 Yb1 H13A 61.3 2_564 . ?
O4 Yb1 H13B 66.8 2_564 . ?
O5 Yb1 O3 76.8(2) . 1_545 ?
O5 Yb1 O4 118.1(3) . 2_564 ?
O5 Yb1 H13A 86.0 . . ?
O5 Yb1 H13B 62.1 . . ?
O13 Yb1 O1 78.7(2) . . ?
O13 Yb1 O3 141.8(3) . 1_545 ?
O13 Yb1 O4 72.6(2) . 2_564 ?
O13 Yb1 O5 69.0(2) . . ?
O13 Yb1 H13A 17.1 . . ?
O13 Yb1 H13B 17.2 . . ?
O13 Yb1 O14 85.2(2) . . ?
H13A Yb1 H13B 28.5 . . ?
O14 Yb1 O1 74.5(2) . . ?
O14 Yb1 O3 70.7(2) . 1_545 ?
O14 Yb1 O4 144.03(16) . 2_564 ?
O14 Yb1 O5 77.3(3) . . ?
O14 Yb1 H13A 89.8 . . ?
O14 Yb1 H13B 98.5 . . ?
O15 Yb1 O1 74.6(2) . . ?
O15 Yb1 O3 74.5(2) . 1_545 ?
O15 Yb1 O4 76.1(3) . 2_564 ?
O15 Yb1 O5 145.13(17) . . ?
O15 Yb1 O13 143.4(2) . . ?
O15 Yb1 H13A 126.6 . . ?
O15 Yb1 H13B 142.9 . . ?
O15 Yb1 O14 110.7(3) . . ?
O15 Yb1 O16 81.5(3) . . ?
O16 Yb1 O1 144.1(3) . . ?
O16 Yb1 O3 77.01(15) . 1_545 ?
O16 Yb1 O4 74.9(2) . 2_564 ?
O16 Yb1 O5 73.0(2) . . ?
O16 Yb1 O13 107.7(3) . . ?
O16 Yb1 H13A 113.7 . . ?
O16 Yb1 H13B 90.6 . . ?
O16 Yb1 O14 140.1(3) . . ?
O8 Yb2 O9 141.1(3) . . ?
O8 Yb2 O10 74.9(2) . 2_565 ?
O8 Yb2 O11 76.35(18) . 1_545 ?
O8 Yb2 O17 83.6(2) . . ?
O8 Yb2 O18 74.6(2) . . ?
O8 Yb2 O19 113.0(3) . . ?
O8 Yb2 O20 142.8(2) . . ?
O8 Yb2 H20A 151.2 . . ?
O8 Yb2 H20B 126.0 . . ?
O9 Yb2 H20A 67.7 . . ?
O9 Yb2 H20B 91.2 . . ?
O10 Yb2 O9 141.5(2) 2_565 . ?
O10 Yb2 H20A 77.0 2_565 . ?
O10 Yb2 H20B 61.3 2_565 . ?
O11 Yb2 O9 118.7(2) 1_545 . ?
O11 Yb2 O10 74.8(2) 1_545 2_565 ?
O11 Yb2 O17 74.6(2) 1_545 . ?
O11 Yb2 H20A 90.2 1_545 . ?
O11 Yb2 H20B 63.5 1_545 . ?
O17 Yb2 O9 68.5(2) . . ?
O17 Yb2 O10 145.91(17) . 2_565 ?
O17 Yb2 H20A 117.7 . . ?
O17 Yb2 H20B 115.9 . . ?
O18 Yb2 O9 73.0(2) . . ?
O18 Yb2 O10 120.8(3) . 2_565 ?
O18 Yb2 O11 141.0(3) . 1_545 ?
O18 Yb2 O17 76.8(3) . . ?
O18 Yb2 H20A 126.8 . . ?
O18 Yb2 H20B 155.1 . . ?
O19 Yb2 O9 76.49(17) . . ?
O19 Yb2 O10 75.2(2) . 2_565 ?
O19 Yb2 O11 144.7(3) . 1_545 ?
O19 Yb2 O17 138.4(2) . . ?
O19 Yb2 O18 72.0(2) . . ?
O19 Yb2 H20A 65.1 . . ?
O19 Yb2 H20B 85.8 . . ?
O20 Yb2 O9 74.0(2) . . ?
O20 Yb2 O10 76.8(2) . 2_565 ?
O20 Yb2 O11 73.3(2) . 1_545 ?
O20 Yb2 O17 108.1(3) . . ?
O20 Yb2 O18 141.8(2) . . ?
O20 Yb2 O19 82.0(2) . . ?
O20 Yb2 H20A 17.3 . . ?
O20 Yb2 H20B 17.3 . . ?
H20A Yb2 H20B 28.8 . . ?
C1 O1 Yb1 139.3(6) . . ?
C3 O3 Yb1 131.8(5) . 1_565 ?
C4 O4 Yb1 134.0(5) . 2_565 ?
C5 O5 Yb1 137.2(4) . . ?
C8 O8 Yb2 137.8(5) . . ?
C9 O9 Yb2 132.7(5) . . ?
C10 O10 Yb2 134.6(5) . 2_564 ?
C11 O11 Yb2 134.6(5) . 1_565 ?
Yb1 O13 H13A 110.3 . . ?
Yb1 O13 H13B 109.7 . . ?
H13A O13 H13B 103.9 . . ?
Yb1 O14 H14A 111.5 . . ?
Yb1 O14 H14B 112.4 . . ?
H14A O14 H14B 101.9 . . ?
Yb1 O15 H15A 126.5 . . ?
Yb1 O15 H15B 126.0 . . ?
H15A O15 H15B 104.1 . . ?
Yb1 O16 H16A 127.6 . . ?
Yb1 O16 H16B 122.5 . . ?
H16A O16 H16B 104.7 . . ?
Yb2 O17 H17A 110.0 . . ?
Yb2 O17 H17B 112.5 . . ?
H17A O17 H17B 103.2 . . ?
Yb2 O18 H18A 124.8 . . ?
Yb2 O18 H18B 127.9 . . ?
H18A O18 H18B 104.2 . . ?
Yb2 O19 H19A 134.4 . . ?
Yb2 O19 H19B 120.6 . . ?
H19A O19 H19B 104.6 . . ?
Yb2 O20 H20A 110.1 . . ?
Yb2 O20 H20B 110.5 . . ?
H20A O20 H20B 103.6 . . ?
O1 C1 C2 132.0(8) . . ?
O1 C1 C4 138.4(8) . . ?
C4 C1 C2 89.1(6) . . ?
O2 C2 C1 136.2(8) . . ?
O2 C2 C3 134.0(8) . . ?
C3 C2 C1 89.8(6) . . ?
O3 C3 C2 136.3(8) . . ?
O3 C3 C4 133.3(8) . . ?
C4 C3 C2 89.9(6) . . ?
O4 C4 C1 133.2(8) . . ?
O4 C4 C3 135.8(8) . . ?
C1 C4 C3 90.9(6) . . ?
O5 C5 C6 135.1(6) . . ?
O5 C5 C8 134.1(5) . . ?
C6 C5 C8 90.6(5) . . ?
O6 C6 C5 134.4(7) . . ?
O6 C6 C7 136.0(6) . . ?
C5 C6 C7 89.6(5) . . ?
O7 C7 C6 136.5(7) . . ?
O7 C7 C8 133.6(6) . . ?
C8 C7 C6 89.8(5) . . ?
O8 C8 C5 137.7(6) . . ?
O8 C8 C7 133.0(6) . . ?
C7 C8 C5 89.4(4) . . ?
O9 C9 C10 135.7(8) . . ?
O9 C9 C12 134.4(8) . . ?
C10 C9 C12 89.8(6) . . ?
O10 C10 C9 134.9(8) . . ?
O10 C10 C11 134.9(8) . . ?
C9 C10 C11 90.1(6) . . ?
O11 C11 C10 136.6(8) . . ?
O11 C11 C12 134.1(8) . . ?
C12 C11 C10 89.3(6) . . ?
O12 C12 C9 135.0(8) . . ?
O12 C12 C11 134.3(8) . . ?
C11 C12 C9 90.4(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
Yb1 O1 C1 C2 -141.4(8) . . . . ?
Yb1 O1 C1 C4 28.8(16) . . . . ?
Yb1 O3 C3 C2 28.6(15) 1_565 . . . ?
Yb1 O3 C3 C4 -139.9(7) 1_565 . . . ?
Yb1 O4 C4 C1 147.4(7) 2_565 . . . ?
Yb1 O4 C4 C3 -37.1(14) 2_565 . . . ?
Yb1 O5 C5 C6 -30.3(13) . . . . ?
Yb1 O5 C5 C8 145.7(6) . . . . ?
Yb2 O8 C8 C5 41.6(12) . . . . ?
Yb2 O8 C8 C7 -139.0(6) . . . . ?
Yb2 O9 C9 C10 143.8(7) . . . . ?
Yb2 O9 C9 C12 -32.6(13) . . . . ?
Yb2 O10 C10 C9 37.3(12) 2_564 . . . ?
Yb2 O10 C10 C11 -146.2(7) 2_564 . . . ?
Yb2 O11 C11 C10 -39.9(13) 1_565 . . . ?
Yb2 O11 C11 C12 136.4(8) 1_565 . . . ?
O1 C1 C2 O2 -8.0(18) . . . . ?
O1 C1 C2 C3 169.4(8) . . . . ?
O1 C1 C4 O4 8.2(17) . . . . ?
O1 C1 C4 C3 -168.6(10) . . . . ?
O2 C2 C3 O3 9.9(18) . . . . ?
O2 C2 C3 C4 -178.4(10) . . . . ?
O3 C3 C4 O4 -8.7(16) . . . . ?
O3 C3 C4 C1 168.0(9) . . . . ?
O5 C5 C6 O6 -11.0(14) . . . . ?
O5 C5 C6 C7 171.1(8) . . . . ?
O5 C5 C8 O8 8.5(13) . . . . ?
O5 C5 C8 C7 -171.1(8) . . . . ?
O6 C6 C7 O7 12.3(15) . . . . ?
O6 C6 C7 C8 -171.8(9) . . . . ?
O7 C7 C8 O8 -9.5(12) . . . . ?
O7 C7 C8 C5 170.1(7) . . . . ?
O9 C9 C10 O10 5.0(15) . . . . ?
O9 C9 C10 C11 -172.5(9) . . . . ?
O9 C9 C12 O12 -1.8(17) . . . . ?
O9 C9 C12 C11 172.5(8) . . . . ?
O10 C10 C11 O11 -5.1(15) . . . . ?
O10 C10 C11 C12 177.5(8) . . . . ?
O11 C11 C12 O12 1.8(17) . . . . ?
O11 C11 C12 C9 -172.5(8) . . . . ?
C1 C2 C3 O3 -167.7(9) . . . . ?
C1 C2 C3 C4 4.0(7) . . . . ?
C2 C1 C4 O4 -179.1(9) . . . . ?
C2 C1 C4 C3 4.1(7) . . . . ?
C2 C3 C4 O4 179.2(9) . . . . ?
C2 C3 C4 C1 -4.1(7) . . . . ?
C4 C1 C2 O2 178.5(10) . . . . ?
C4 C1 C2 C3 -4.1(7) . . . . ?
C5 C6 C7 O7 -169.9(8) . . . . ?
C5 C6 C7 C8 6.1(5) . . . . ?
C6 C5 C8 O8 -174.3(8) . . . . ?
C6 C5 C8 C7 6.1(5) . . . . ?
C6 C7 C8 O8 174.3(7) . . . . ?
C6 C7 C8 C5 -6.0(5) . . . . ?
C8 C5 C6 O6 171.8(8) . . . . ?
C8 C5 C6 C7 -6.1(5) . . . . ?
C9 C10 C11 O11 172.4(9) . . . . ?
C9 C10 C11 C12 -5.0(6) . . . . ?
C10 C9 C12 O12 -179.3(10) . . . . ?
C10 C9 C12 C11 -5.0(6) . . . . ?
C10 C11 C12 O12 179.3(10) . . . . ?
C10 C11 C12 C9 5.0(6) . . . . ?
C12 C9 C10 O10 -177.5(8) . . . . ?
C12 C9 C10 C11 5.0(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.737
_oxdiff_exptl_absorpt_empirical_full_min 0.442
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.56(2)
2 0.44(2)

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_er_sq_block_no1_20211118_a_autored
_database_code_depnum_ccdc_archive 'CCDC 2218677'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Er2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'erbium(III) squarate'
_chemical_formula_moiety         'C12 H16 Er2 O20'
_chemical_formula_sum            'C12 H16 Er2 O20'
_chemical_formula_weight         814.77
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16Er2O20
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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9232(4)
_cell_length_b                   8.1407(2)
_cell_length_c                   10.0025(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.988(3)
_cell_angle_gamma                90
_cell_volume                     965.59(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4374
_cell_measurement_temperature    297.8(4)
_cell_measurement_theta_max      29.6900
_cell_measurement_theta_min      3.0430
_shelx_estimated_absorpt_T_max   0.396
_shelx_estimated_absorpt_T_min   0.318
_exptl_absorpt_coefficient_mu    8.740
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.368
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale pink'
_exptl_crystal_density_diffrn    2.802
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 2 13 0.0671
6 0 13 0.0656
0 -11 0 0.0601
0 11 1 0.0652
-6 0 -13 0.0665
17 1 0 0.0643
-16 -1 -1 0.0635
5 -2 -14 0.0771
-13 -2 -8 0.0694
-13 1 10 0.0885
17 0 -1 0.0576
-16 0 -1 0.0603
-12 -1 -9 0.0634
10 4 -11 0.0965
0 0 14 0.0745
1 6 -12 0.0818

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.1803 2.4363 13.1728 0.0415 -0.1545 0.9871
5.8596 0.2238 12.6342 0.1858 0.0509 0.9813
0.1085 -11.4735 -0.0406 0.9365 0.2800 -0.2113
0.3144 11.4440 0.9514 -0.9194 -0.2752 0.2812
-5.8627 0.4154 -12.6257 -0.2379 -0.0665 -0.9690
16.5771 1.2016 0.3538 -0.2487 0.8421 0.4786
-16.4650 -1.2834 -0.9116 0.2429 -0.8230 -0.5136
4.7217 -1.8710 -13.6822 -0.1734 0.5697 -0.8033
-12.6506 -2.1200 -7.7619 0.1341 -0.4633 -0.8760
-12.9034 0.7269 10.0759 0.2706 -0.9032 0.3332
16.7900 -0.0611 -0.8025 -0.1713 0.9067 0.3855
-16.4656 -0.3639 -1.3473 0.1587 -0.8361 -0.5250
-12.1574 -0.6581 -8.5919 -0.0072 -0.4553 -0.8903
9.5734 4.2056 -11.1597 -0.6646 0.6311 -0.4000
-0.2288 0.4312 14.0385 0.2557 -0.3047 0.9175
1.3321 5.7684 -12.1920 -0.7352 0.1782 -0.6540

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.149
_diffrn_reflns_theta_min         3.035
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.8(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     11.00  36.00   0.50    0.05    --   12.56-110.00 -31.00   50
  2  ω     45.00  73.00   0.50    0.05    --   12.56-178.00 120.00   56
  3  ω     47.00  95.00   0.50    0.05    --   12.56 178.00  60.00   96
  4  ω     57.00  94.00   0.50    0.05    --   12.56 178.00-120.00   74
  5  ω     47.00  77.00   0.50    0.05    --   12.56 178.00 -30.00   60
  6  ω    -25.00  61.00   0.50    0.05    --  -13.50  19.00   0.00  172
  7  ω    -53.00 -27.00   0.50    0.05    --  -13.50 110.00  63.00   52
  8  ω     -9.00  32.00   0.50    0.05    --  -13.50 -99.00 150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0095157000
_diffrn_orient_matrix_UB_12      -0.0817832000
_diffrn_orient_matrix_UB_13      0.0205700000
_diffrn_orient_matrix_UB_21      0.0529532000
_diffrn_orient_matrix_UB_22      -0.0238300000
_diffrn_orient_matrix_UB_23      -0.0201078000
_diffrn_orient_matrix_UB_31      0.0261436000
_diffrn_orient_matrix_UB_32      0.0184298000
_diffrn_orient_matrix_UB_33      0.0652156000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.826
_reflns_number_gt                3103
_reflns_number_total             3455
_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       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    
'olex2.solve 1.5-ac5-018 (Bourhis et al., 2015)'
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.0098(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3455
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0215
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0247P)²+0.1224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0537
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.03(3)
 -0.03(3)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Er1-H16A \\sim Er1-H16B
 with sigma of 0.02
 Er2-H18A \\sim Er2-H18B
 with sigma of 0.02
 Er1-H15A \\sim Er1-H15B
 with sigma of 0.02
 Er2-H19A \\sim Er2-H19B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8486(9) 0.6297(11) 0.3851(10) 0.016(2) Uani 1 1 d . U . . .
C2 C 0.8822(9) 0.7882(13) 0.3349(10) 0.0135(18) Uani 1 1 d . U . . .
C3 C 0.8253(9) 0.8694(10) 0.4403(10) 0.0142(19) Uani 1 1 d . U . . .
C4 C 0.8016(9) 0.7118(12) 0.4965(10) 0.0146(18) Uani 1 1 d . U . . .
C5 C 0.5266(6) 0.0121(8) 0.4192(7) 0.0155(14) Uani 1 1 d . . . . .
C6 C 0.5441(7) -0.1598(9) 0.3881(8) 0.0174(17) Uani 1 1 d . . . . .
C7 C 0.4727(7) -0.2042(9) 0.4926(8) 0.0171(14) Uani 1 1 d . . . . .
C8 C 0.4457(6) -0.0332(8) 0.5115(6) 0.0160(14) Uani 1 1 d . . . . .
C9 C 0.1781(8) 0.6322(11) 0.4398(10) 0.0130(18) Uani 1 1 d . U . . .
C10 C 0.2017(9) 0.7933(13) 0.3829(10) 0.0159(18) Uani 1 1 d . U . . .
C11 C 0.1484(8) 0.8745(10) 0.4937(10) 0.0122(18) Uani 1 1 d . U . . .
C12 C 0.1202(10) 0.7109(13) 0.5435(11) 0.0164(19) Uani 1 1 d . U . . .
O1 O 0.8512(6) 0.4866(7) 0.3390(7) 0.0235(14) Uani 1 1 d . . . . .
O2 O 0.9316(6) 0.8398(7) 0.2393(7) 0.0238(16) Uani 1 1 d . . . . .
O3 O 0.7968(6) 1.0160(7) 0.4653(6) 0.0180(14) Uani 1 1 d . . . . .
O4 O 0.7521(7) 0.6596(7) 0.5943(7) 0.0219(15) Uani 1 1 d . . . . .
O5 O 0.5680(6) 0.1477(7) 0.3842(7) 0.0213(15) Uani 1 1 d . . . . .
O6 O 0.5971(5) -0.2331(6) 0.3051(6) 0.0207(12) Uani 1 1 d . . . . .
O7 O 0.4488(6) -0.3359(7) 0.5508(6) 0.0260(15) Uani 1 1 d . . . . .
O8 O 0.3790(6) 0.0381(7) 0.5817(6) 0.0208(13) Uani 1 1 d . . . . .
O9 O 0.2058(6) 0.4865(7) 0.4149(6) 0.0173(14) Uani 1 1 d . . . . .
O10 O 0.2477(7) 0.8444(6) 0.2840(6) 0.0181(14) Uani 1 1 d . . . . .
O11 O 0.1379(6) 1.0160(7) 0.5363(7) 0.0193(12) Uani 1 1 d . . . . .
O12 O 0.0720(6) 0.6619(7) 0.6426(7) 0.0214(15) Uani 1 1 d . . . . .
O13 O 0.6042(6) 0.4441(7) 0.2799(7) 0.0242(14) Uani 1 1 d . . . . .
H13A H 0.6343 0.5359 0.2639 0.036 Uiso 1 1 d R U . . .
H13B H 0.5636 0.4208 0.2073 0.036 Uiso 1 1 d R U . . .
O14 O 0.7485(9) 0.3278(8) 0.5475(8) 0.042(2) Uani 1 1 d G . . . .
H14A H 0.7444 0.4173 0.5896 0.063 Uiso 1 1 d G U . . .
H14B H 0.7902 0.2672 0.6007 0.063 Uiso 1 1 d G U . . .
O15 O 0.9203(6) 0.1679(8) 0.2710(8) 0.0244(15) Uani 1 1 d G . . . .
H15A H 0.9677 0.2289 0.2379 0.037 Uiso 1 1 d DG U . . .
H15B H 0.9413 0.0718 0.2542 0.037 Uiso 1 1 d DG U . . .
O16 O 0.6933(7) 0.0195(7) 0.1875(7) 0.0190(14) Uani 1 1 d G . . . .
H16A H 0.7313 -0.0102 0.1252 0.029 Uiso 1 1 d DG U . . .
H16B H 0.6730 -0.0690 0.2217 0.029 Uiso 1 1 d DG U . . .
O17 O 0.2427(7) 0.1795(7) 0.3267(8) 0.0264(13) Uani 1 1 d . . . . .
H17A H 0.2379 0.0750 0.3186 0.040 Uiso 1 1 d R U . . .
H17B H 0.1814 0.2145 0.2832 0.040 Uiso 1 1 d R U . . .
O18 O 0.4237(6) 0.3533(8) 0.4882(8) 0.0294(17) Uani 1 1 d G . . . .
H18A H 0.4454 0.4518 0.4867 0.044 Uiso 1 1 d DG U . . .
H18B H 0.4782 0.2991 0.4634 0.044 Uiso 1 1 d DG U . . .
O19 O 0.3132(7) 0.4749(8) 0.6942(7) 0.0235(15) Uani 1 1 d G . . . .
H19A H 0.2885 0.5049 0.7660 0.035 Uiso 1 1 d DG U . . .
H19B H 0.3589 0.5495 0.6774 0.035 Uiso 1 1 d DG U . . .
O20 O 0.0779(6) 0.3365(7) 0.6074(7) 0.0235(15) Uani 1 1 d . . . . .
H20A H 0.0823 0.4325 0.6416 0.035 Uiso 1 1 d R U . . .
H20B H 0.0556 0.2765 0.6695 0.035 Uiso 1 1 d R U . . .
Er1 Er 0.74445(2) 0.24452(3) 0.32068(2) 0.01247(16) Uani 1 1 d D . . . .
Er2 Er 0.25496(2) 0.25172(3) 0.55670(2) 0.01146(15) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.456(13) . ?
C1 C4 1.461(12) . ?
C1 O1 1.254(10) . ?
C2 C3 1.469(13) . ?
C2 O2 1.247(12) . ?
C3 C4 1.441(12) . ?
C3 O3 1.273(10) . ?
C4 O4 1.267(11) . ?
C5 C6 1.453(10) . ?
C5 C7 2.037(10) . ?
C5 C8 1.451(9) . ?
C5 O5 1.273(8) . ?
C6 C7 1.461(10) . ?
C6 O6 1.247(10) . ?
C7 C8 1.445(10) . ?
C7 O7 1.267(9) . ?
C8 O8 1.256(8) . ?
C9 C10 1.468(12) . ?
C9 C12 1.453(13) . ?
C9 O9 1.263(10) . ?
C10 C11 1.489(13) . ?
C10 O10 1.252(11) . ?
C11 C12 1.473(12) . ?
C11 O11 1.239(10) . ?
C12 O12 1.262(13) . ?
O1 Er1 2.343(6) . ?
O3 Er1 2.399(6) 1_565 ?
O4 Er1 2.406(7) 2_565 ?
O5 Er1 2.393(7) . ?
O8 Er2 2.280(6) . ?
O9 Er2 2.416(6) . ?
O10 Er2 2.414(6) 2_564 ?
O11 Er2 2.369(6) 1_565 ?
O13 H13A 0.8510 . ?
O13 H13B 0.8512 . ?
O13 Er1 2.336(6) . ?
O14 H14A 0.8457 . ?
O14 H14B 0.8472 . ?
O14 Er1 2.364(8) . ?
O15 H15A 0.8455 . ?
O15 H15B 0.8429 . ?
O15 Er1 2.292(7) . ?
O16 H16A 0.8433 . ?
O16 H16B 0.8434 . ?
O16 Er1 2.310(6) . ?
O17 H17A 0.8556 . ?
O17 H17B 0.8603 . ?
O17 Er2 2.364(8) . ?
O18 H18A 0.8427 . ?
O18 H18B 0.8438 . ?
O18 Er2 2.343(7) . ?
O19 H19A 0.8402 . ?
O19 H19B 0.8438 . ?
O19 Er2 2.340(6) . ?
O20 H20A 0.8530 . ?
O20 H20B 0.8540 . ?
O20 Er2 2.327(7) . ?
Er1 O3 2.399(6) 1_545 ?
Er1 O4 2.406(7) 2_564 ?
Er2 O10 2.414(6) 2_565 ?
Er2 O11 2.369(6) 1_545 ?

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
C2 C1 C4 89.9(7) . . ?
O1 C1 C2 132.7(10) . . ?
O1 C1 C4 137.0(10) . . ?
C1 C2 C3 89.2(8) . . ?
O2 C2 C1 137.0(10) . . ?
O2 C2 C3 133.6(10) . . ?
C4 C3 C2 90.2(7) . . ?
O3 C3 C2 135.7(9) . . ?
O3 C3 C4 133.7(10) . . ?
C3 C4 C1 90.2(7) . . ?
O4 C4 C1 133.0(9) . . ?
O4 C4 C3 136.6(10) . . ?
C6 C5 C7 45.8(4) . . ?
C8 C5 C6 90.6(5) . . ?
C8 C5 C7 45.2(4) . . ?
O5 C5 C6 135.0(7) . . ?
O5 C5 C7 173.9(6) . . ?
O5 C5 C8 134.3(6) . . ?
C5 C6 C7 88.7(6) . . ?
O6 C6 C5 134.2(7) . . ?
O6 C6 C7 137.0(7) . . ?
C6 C7 C5 45.5(4) . . ?
C8 C7 C5 45.4(4) . . ?
C8 C7 C6 90.6(6) . . ?
O7 C7 C5 172.6(6) . . ?
O7 C7 C6 135.6(8) . . ?
O7 C7 C8 133.7(7) . . ?
C7 C8 C5 89.4(5) . . ?
O8 C8 C5 137.7(6) . . ?
O8 C8 C7 132.9(7) . . ?
C12 C9 C10 90.4(7) . . ?
O9 C9 C10 134.2(9) . . ?
O9 C9 C12 135.1(9) . . ?
C9 C10 C11 89.6(7) . . ?
O10 C10 C9 136.1(10) . . ?
O10 C10 C11 134.2(9) . . ?
C12 C11 C10 88.9(7) . . ?
O11 C11 C10 137.3(9) . . ?
O11 C11 C12 133.6(10) . . ?
C9 C12 C11 90.9(8) . . ?
O12 C12 C9 135.3(10) . . ?
O12 C12 C11 133.7(10) . . ?
C1 O1 Er1 140.9(7) . . ?
C3 O3 Er1 131.8(5) . 1_565 ?
C4 O4 Er1 133.2(6) . 2_565 ?
C5 O5 Er1 137.3(5) . . ?
C8 O8 Er2 137.1(5) . . ?
C9 O9 Er2 132.8(5) . . ?
C10 O10 Er2 134.3(6) . 2_564 ?
C11 O11 Er2 134.6(6) . 1_565 ?
H13A O13 H13B 104.4 . . ?
Er1 O13 H13A 109.6 . . ?
Er1 O13 H13B 109.1 . . ?
H14A O14 H14B 104.5 . . ?
Er1 O14 H14A 136.8 . . ?
Er1 O14 H14B 112.8 . . ?
H15A O15 H15B 104.1 . . ?
Er1 O15 H15A 126.1 . . ?
Er1 O15 H15B 126.3 . . ?
H16A O16 H16B 104.7 . . ?
Er1 O16 H16A 121.6 . . ?
Er1 O16 H16B 120.8 . . ?
H17A O17 H17B 103.6 . . ?
Er2 O17 H17A 109.6 . . ?
Er2 O17 H17B 111.9 . . ?
H18A O18 H18B 104.2 . . ?
Er2 O18 H18A 128.0 . . ?
Er2 O18 H18B 127.7 . . ?
H19A O19 H19B 104.6 . . ?
Er2 O19 H19A 128.2 . . ?
Er2 O19 H19B 126.8 . . ?
H20A O20 H20B 104.0 . . ?
Er2 O20 H20A 109.9 . . ?
Er2 O20 H20B 110.4 . . ?
O1 Er1 O3 120.0(3) . 1_545 ?
O1 Er1 O4 74.1(2) . 2_564 ?
O1 Er1 O5 137.9(3) . . ?
O1 Er1 O14 74.2(2) . . ?
O3 Er1 O4 141.8(2) 1_545 2_564 ?
O5 Er1 O3 76.4(2) . 1_545 ?
O5 Er1 O4 118.5(3) . 2_564 ?
O13 Er1 O1 78.6(2) . . ?
O13 Er1 O3 141.4(3) . 1_545 ?
O13 Er1 O4 73.0(2) . 2_564 ?
O13 Er1 O5 69.1(2) . . ?
O13 Er1 O14 84.9(3) . . ?
O14 Er1 O3 70.5(2) . 1_545 ?
O14 Er1 O4 144.23(18) . 2_564 ?
O14 Er1 O5 76.7(3) . . ?
O15 Er1 O1 75.2(2) . . ?
O15 Er1 O3 74.5(2) . 1_545 ?
O15 Er1 O4 76.0(3) . 2_564 ?
O15 Er1 O5 144.82(19) . . ?
O15 Er1 O13 143.7(3) . . ?
O15 Er1 O14 111.0(3) . . ?
O15 Er1 O16 81.5(3) . . ?
O16 Er1 O1 145.2(3) . . ?
O16 Er1 O3 76.65(15) . 1_545 ?
O16 Er1 O4 75.4(2) . 2_564 ?
O16 Er1 O5 72.9(2) . . ?
O16 Er1 O13 108.0(3) . . ?
O16 Er1 O14 139.4(3) . . ?
O8 Er2 O9 141.5(3) . . ?
O8 Er2 O10 74.7(2) . 2_565 ?
O8 Er2 O11 76.18(19) . 1_545 ?
O8 Er2 O17 83.7(2) . . ?
O8 Er2 O18 74.6(2) . . ?
O8 Er2 O19 112.2(3) . . ?
O8 Er2 O20 142.7(2) . . ?
O10 Er2 O9 141.2(2) 2_565 . ?
O11 Er2 O9 119.1(3) 1_545 . ?
O11 Er2 O10 74.9(2) 1_545 2_565 ?
O17 Er2 O9 68.8(2) . . ?
O17 Er2 O10 146.21(18) . 2_565 ?
O17 Er2 O11 74.9(2) . 1_545 ?
O18 Er2 O9 73.3(2) . . ?
O18 Er2 O10 120.4(3) . 2_565 ?
O18 Er2 O11 141.0(3) . 1_545 ?
O18 Er2 O17 76.8(3) . . ?
O19 Er2 O9 76.69(19) . . ?
O19 Er2 O10 74.7(2) . 2_565 ?
O19 Er2 O11 144.6(3) . 1_545 ?
O19 Er2 O17 138.5(3) . . ?
O19 Er2 O18 71.7(2) . . ?
O20 Er2 O9 73.9(2) . . ?
O20 Er2 O10 76.6(3) . 2_565 ?
O20 Er2 O11 73.7(2) . 1_545 ?
O20 Er2 O17 108.7(3) . . ?
O20 Er2 O18 141.8(2) . . ?
O20 Er2 O19 82.1(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
C1 C2 C3 C4 4.9(8) . . . . ?
C1 C2 C3 O3 -168.4(11) . . . . ?
C1 C4 O4 Er1 148.6(8) . . . 2_565 ?
C2 C1 C4 C3 4.9(8) . . . . ?
C2 C1 C4 O4 179.8(11) . . . . ?
C2 C1 O1 Er1 -140.8(9) . . . . ?
C2 C3 C4 C1 -4.9(8) . . . . ?
C2 C3 C4 O4 -179.4(12) . . . . ?
C2 C3 O3 Er1 30.1(17) . . . 1_565 ?
C3 C4 O4 Er1 -38.9(17) . . . 2_565 ?
C4 C1 C2 C3 -4.8(8) . . . . ?
C4 C1 C2 O2 179.0(13) . . . . ?
C4 C1 O1 Er1 30.1(18) . . . . ?
C4 C3 O3 Er1 -140.5(9) . . . 1_565 ?
C5 C6 C7 C8 6.2(5) . . . . ?
C5 C6 C7 O7 -169.7(8) . . . . ?
C5 C7 C8 O8 -179.5(10) . . . . ?
C5 C8 O8 Er2 42.4(13) . . . . ?
C6 C5 C8 C7 6.3(5) . . . . ?
C6 C5 C8 O8 -174.2(9) . . . . ?
C6 C5 O5 Er1 -31.2(13) . . . . ?
C6 C7 C8 C5 -6.2(5) . . . . ?
C6 C7 C8 O8 174.2(8) . . . . ?
C7 C5 C6 O6 179.2(12) . . . . ?
C7 C5 C8 O8 179.5(11) . . . . ?
C7 C8 O8 Er2 -138.3(7) . . . . ?
C8 C5 C6 C7 -6.2(5) . . . . ?
C8 C5 C6 O6 173.0(9) . . . . ?
C8 C5 O5 Er1 145.7(7) . . . . ?
C9 C10 C11 C12 -3.0(8) . . . . ?
C9 C10 C11 O11 171.8(10) . . . . ?
C9 C10 O10 Er2 36.0(16) . . . 2_564 ?
C10 C9 C12 C11 -3.1(8) . . . . ?
C10 C9 C12 O12 -178.6(12) . . . . ?
C10 C9 O9 Er2 142.2(8) . . . . ?
C10 C11 C12 C9 3.1(8) . . . . ?
C10 C11 C12 O12 178.7(12) . . . . ?
C10 C11 O11 Er2 -36.7(15) . . . 1_565 ?
C11 C10 O10 Er2 -144.5(8) . . . 2_564 ?
C12 C9 C10 C11 3.1(8) . . . . ?
C12 C9 C10 O10 -177.3(11) . . . . ?
C12 C9 O9 Er2 -30.1(16) . . . . ?
C12 C11 O11 Er2 136.2(9) . . . 1_565 ?
O1 C1 C2 C3 168.9(10) . . . . ?
O1 C1 C2 O2 -7(2) . . . . ?
O1 C1 C4 C3 -168.3(11) . . . . ?
O1 C1 C4 O4 7(2) . . . . ?
O2 C2 C3 C4 -178.7(12) . . . . ?
O2 C2 C3 O3 8(2) . . . . ?
O3 C3 C4 C1 168.6(10) . . . . ?
O3 C3 C4 O4 -6(2) . . . . ?
O5 C5 C6 C7 171.6(8) . . . . ?
O5 C5 C6 O6 -9.3(15) . . . . ?
O5 C5 C8 C7 -171.5(8) . . . . ?
O5 C5 C8 O8 8.0(14) . . . . ?
O6 C6 C7 C5 -179.1(13) . . . . ?
O6 C6 C7 C8 -172.9(10) . . . . ?
O6 C6 C7 O7 11.2(16) . . . . ?
O7 C7 C8 C5 169.8(8) . . . . ?
O7 C7 C8 O8 -9.7(14) . . . . ?
O9 C9 C10 C11 -171.5(9) . . . . ?
O9 C9 C10 O10 8.1(18) . . . . ?
O9 C9 C12 C11 171.4(10) . . . . ?
O9 C9 C12 O12 -4(2) . . . . ?
O10 C10 C11 C12 177.3(10) . . . . ?
O10 C10 C11 O11 -7.8(19) . . . . ?
O11 C11 C12 C9 -172.1(9) . . . . ?
O11 C11 C12 O12 3(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.931
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.03(3)
2 -0.03(3)

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

data_dy_sq_syn20211020_autored
_database_code_depnum_ccdc_archive 'CCDC 2218675'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Dy2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'dysprosium(III) squarate'
_chemical_formula_moiety         'C12 H16 Dy2 O20'
_chemical_formula_sum            'C12 H16 Dy2 O20'
_chemical_formula_weight         805.25
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16O20Dy2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9063(8)
_cell_length_b                   8.1711(5)
_cell_length_c                   10.0452(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.934(6)
_cell_angle_gamma                90
_cell_volume                     972.04(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2517
_cell_measurement_temperature    295.5(2)
_cell_measurement_theta_max      30.7790
_cell_measurement_theta_min      2.4630
_shelx_estimated_absorpt_T_max   0.801
_shelx_estimated_absorpt_T_min   0.221
_exptl_absorpt_coefficient_mu    7.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.751
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
17 1 -1 0.0130
2 -5 13 0.1001
-3 4 -13 0.1148
0 -12 0 0.0468
-1 12 0 0.0308
-17 -1 1 0.0130

_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
16.7257 0.9583 -1.3106 -0.8300 -0.0580 -0.5547
1.5349 -4.5269 12.7658 -0.6100 -0.0427 0.7913
-2.5467 4.4407 -12.6077 0.6569 0.0459 -0.7526
0.4729 -11.5186 0.4163 -0.2544 0.8873 0.3846
-0.8297 11.5137 0.0245 0.2581 -0.9001 -0.3511
-16.7257 -0.9583 1.3106 0.8300 0.0580 0.5547

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7732
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.734
_diffrn_reflns_theta_min         2.493
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.5(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     46.00  72.00   0.50   22.53    --    5.00  45.00  90.00   52
  2  ω    -50.00  29.00   0.50   22.53    --  -11.00  45.00  60.00  158
  3  ω     35.00  65.00   0.50   22.53    --  -11.00  45.00  60.00   60
  4  ω     30.00  74.00   0.50   22.53    --  -11.00  45.00   0.00   88
  5  ω   -100.00   3.00   0.50   22.53    --  -11.00  45.00   0.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RINC): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534165000
_diffrn_orient_matrix_UB_12      0.0186403000
_diffrn_orient_matrix_UB_13      -0.0347477000
_diffrn_orient_matrix_UB_21      -0.0014111000
_diffrn_orient_matrix_UB_22      -0.0782086000
_diffrn_orient_matrix_UB_23      -0.0309051000
_diffrn_orient_matrix_UB_31      -0.0270915000
_diffrn_orient_matrix_UB_32      -0.0325623000
_diffrn_orient_matrix_UB_33      0.0536950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.857
_reflns_number_gt                3161
_reflns_number_total             3920
_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       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(4)
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0848
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.77(4)
 0.23(4)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Dy1-H14A \\sim Dy1-H14B
 with sigma of 0.02
 Dy1-H15A \\sim Dy1-H15B
 with sigma of 0.02
 Dy2-H18A \\sim Dy2-H18B
 with sigma of 0.02
 Dy2-H19A \\sim Dy2-H19B
 with sigma of 0.02
 Dy1-H16A \\sim Dy1-H16B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_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
Dy1 Dy 0.74492(3) 0.24459(4) 0.32131(3) 0.0144(2) Uani 1 1 d D . . . .
Dy2 Dy 0.25438(3) 0.25145(4) 0.55648(3) 0.0126(2) Uani 1 1 d D . . . .
O1 O 0.8541(9) 0.4856(8) 0.3400(10) 0.026(2) Uani 1 1 d . . . . .
O2 O 0.9321(9) 0.8379(9) 0.2390(11) 0.028(3) Uani 1 1 d . . . . .
O3 O 0.7983(10) 1.0159(9) 0.4647(10) 0.022(2) Uani 1 1 d . . . . .
O4 O 0.7523(10) 0.6596(9) 0.5930(10) 0.024(2) Uani 1 1 d . . . . .
O5 O 0.5674(9) 0.1458(8) 0.3814(11) 0.025(2) Uani 1 1 d . . . . .
O6 O 0.5967(7) -0.2340(7) 0.3050(9) 0.0231(17) Uani 1 1 d . . . . .
O7 O 0.4474(9) -0.3364(9) 0.5476(9) 0.031(2) Uani 1 1 d . . . . .
O8 O 0.3793(8) 0.0370(9) 0.5794(9) 0.0221(19) Uani 1 1 d . . . . .
O9 O 0.2047(10) 0.4881(8) 0.4124(10) 0.018(2) Uani 1 1 d . . . . .
O10 O 0.2460(10) 0.8438(7) 0.2824(9) 0.019(2) Uani 1 1 d . . . . .
O11 O 0.1379(9) 1.0138(9) 0.5326(10) 0.025(2) Uani 1 1 d . . . . .
O12 O 0.0721(9) 0.6610(9) 0.6390(11) 0.024(2) Uani 1 1 d . . . . .
O13 O 0.6031(9) 0.4453(8) 0.2775(10) 0.029(2) Uani 1 1 d . . . . .
H13A H 0.6333 0.5378 0.2628 0.044 Uiso 1 1 d R U . . .
H13B H 0.5629 0.4232 0.2038 0.044 Uiso 1 1 d R U . . .
O14 O 0.7469(13) 0.3294(9) 0.5489(12) 0.048(3) Uani 1 1 d . . . . .
H14A H 0.6927 0.2772 0.5910 0.072 Uiso 1 1 d DR U . . .
H14B H 0.7260 0.4363 0.5576 0.072 Uiso 1 1 d DR U . . .
O15 O 0.9234(9) 0.1662(10) 0.2684(12) 0.028(2) Uani 1 1 d G . . . .
H15A H 0.9716 0.2242 0.2337 0.042 Uiso 1 1 d DG U . . .
H15B H 0.9541 0.0730 0.2779 0.042 Uiso 1 1 d DG U . . .
O16 O 0.6954(10) 0.0181(9) 0.1867(10) 0.025(2) Uani 1 1 d G . . . .
H16A H 0.7214 -0.0037 0.1130 0.038 Uiso 1 1 d DG U . . .
H16B H 0.6735 -0.0738 0.2142 0.038 Uiso 1 1 d DG U . . .
O17 O 0.2428(11) 0.1778(8) 0.3246(12) 0.031(2) Uani 1 1 d . . . . .
H17A H 0.2335 0.0711 0.3141 0.047 Uiso 1 1 d R U . . .
H17B H 0.1818 0.2182 0.2770 0.047 Uiso 1 1 d R U . . .
O18 O 0.4257(10) 0.3524(9) 0.4858(12) 0.031(3) Uani 1 1 d G . . . .
H18A H 0.4458 0.4512 0.4805 0.047 Uiso 1 1 d DG U . . .
H18B H 0.4782 0.2986 0.4560 0.047 Uiso 1 1 d DG U . . .
O19 O 0.3130(10) 0.4767(10) 0.6917(10) 0.023(2) Uani 1 1 d G . . . .
H19A H 0.2876 0.5074 0.7629 0.035 Uiso 1 1 d DG U . . .
H19B H 0.3580 0.5520 0.6744 0.035 Uiso 1 1 d DG U . . .
O20 O 0.0772(10) 0.3348(9) 0.6064(11) 0.030(3) Uani 1 1 d . . . . .
H20A H 0.0820 0.4292 0.6441 0.045 Uiso 1 1 d R U . . .
H20B H 0.0532 0.2720 0.6660 0.045 Uiso 1 1 d R U . . .
C1 C 0.8490(13) 0.6309(14) 0.3845(15) 0.021(3) Uani 1 1 d . U . . .
C2 C 0.8829(12) 0.7924(15) 0.3368(15) 0.017(2) Uani 1 1 d . U . . .
C3 C 0.8268(12) 0.8717(13) 0.4410(14) 0.017(3) Uani 1 1 d . U . . .
C4 C 0.8013(11) 0.7136(15) 0.4945(14) 0.017(2) Uani 1 1 d . U . . .
C5 C 0.5254(8) 0.0113(9) 0.4181(10) 0.019(2) Uani 1 1 d . . . . .
C6 C 0.5451(10) -0.1604(11) 0.3859(12) 0.020(2) Uani 1 1 d . . . . .
C7 C 0.4727(10) -0.2064(12) 0.4907(11) 0.022(2) Uani 1 1 d . . . . .
C8 C 0.4441(8) -0.0360(9) 0.5095(9) 0.0169(19) Uani 1 1 d . . . . .
C9 C 0.1781(12) 0.6328(13) 0.4392(14) 0.016(3) Uani 1 1 d . U . . .
C10 C 0.2002(11) 0.7930(14) 0.3798(14) 0.016(2) Uani 1 1 d . U . . .
C11 C 0.1476(11) 0.8741(11) 0.4916(14) 0.013(2) Uani 1 1 d . U . . .
C12 C 0.1194(13) 0.7138(14) 0.5452(15) 0.017(3) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.356(8) . ?
Dy1 O3 2.405(9) 1_545 ?
Dy1 O4 2.433(10) 2_564 ?
Dy1 O5 2.397(10) . ?
Dy1 O13 2.363(9) . ?
Dy1 O14 2.387(12) . ?
Dy1 O15 2.333(11) . ?
Dy1 O16 2.332(9) . ?
Dy2 O8 2.295(8) . ?
Dy2 O9 2.451(8) . ?
Dy2 O10 2.411(9) 2_565 ?
Dy2 O11 2.384(9) 1_545 ?
Dy2 O17 2.396(12) . ?
Dy2 O18 2.375(10) . ?
Dy2 O19 2.351(9) . ?
Dy2 O20 2.321(11) . ?
O1 C1 1.272(13) . ?
O2 C2 1.252(16) . ?
O3 Dy1 2.405(9) 1_565 ?
O3 C3 1.256(14) . ?
O4 Dy1 2.433(10) 2_565 ?
O4 C4 1.278(15) . ?
O5 C5 1.278(10) . ?
O6 C6 1.226(13) . ?
O7 C7 1.258(12) . ?
O8 C8 1.247(11) . ?
O9 C9 1.260(12) . ?
O10 Dy2 2.411(9) 2_564 ?
O10 C10 1.239(15) . ?
O11 Dy2 2.384(9) 1_565 ?
O11 C11 1.223(12) . ?
O12 C12 1.225(16) . ?
O13 H13A 0.8560 . ?
O13 H13B 0.8577 . ?
O14 H14A 0.9127 . ?
O14 H14B 0.9149 . ?
O15 H15A 0.8464 . ?
O15 H15B 0.8461 . ?
O16 H16A 0.8503 . ?
O16 H16B 0.8499 . ?
O17 H17A 0.8845 . ?
O17 H17B 0.8901 . ?
O18 H18A 0.8451 . ?
O18 H18B 0.8447 . ?
O19 H19A 0.8423 . ?
O19 H19B 0.8455 . ?
O20 H20A 0.8583 . ?
O20 H20B 0.8595 . ?
C1 C2 1.475(16) . ?
C1 C4 1.459(17) . ?
C2 C3 1.451(16) . ?
C3 C4 1.444(15) . ?
C5 C6 1.464(12) . ?
C5 C8 1.453(12) . ?
C6 C7 1.477(15) . ?
C7 C8 1.450(12) . ?
C9 C10 1.473(15) . ?
C9 C12 1.489(18) . ?
C10 C11 1.497(17) . ?
C11 C12 1.468(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O3 119.5(4) . 1_545 ?
O1 Dy1 O4 74.5(3) . 2_564 ?
O1 Dy1 O5 139.0(3) . . ?
O1 Dy1 O13 79.2(3) . . ?
O1 Dy1 O14 74.3(3) . . ?
O3 Dy1 O4 141.4(3) 1_545 2_564 ?
O5 Dy1 O3 76.9(3) . 1_545 ?
O5 Dy1 O4 117.7(4) . 2_564 ?
O13 Dy1 O3 142.3(4) . 1_545 ?
O13 Dy1 O4 72.3(3) . 2_564 ?
O13 Dy1 O5 69.4(3) . . ?
O13 Dy1 O14 85.0(4) . . ?
O14 Dy1 O3 71.1(3) . 1_545 ?
O14 Dy1 O4 144.3(2) . 2_564 ?
O14 Dy1 O5 77.2(4) . . ?
O15 Dy1 O1 74.9(3) . . ?
O15 Dy1 O3 74.5(4) . 1_545 ?
O15 Dy1 O4 75.6(4) . 2_564 ?
O15 Dy1 O5 144.3(2) . . ?
O15 Dy1 O13 143.0(3) . . ?
O15 Dy1 O14 112.3(5) . . ?
O16 Dy1 O1 144.5(4) . . ?
O16 Dy1 O3 76.5(2) . 1_545 ?
O16 Dy1 O4 74.9(3) . 2_564 ?
O16 Dy1 O5 72.7(3) . . ?
O16 Dy1 O13 108.1(4) . . ?
O16 Dy1 O14 139.7(3) . . ?
O16 Dy1 O15 80.3(4) . . ?
O8 Dy2 O9 140.9(4) . . ?
O8 Dy2 O10 75.4(3) . 2_565 ?
O8 Dy2 O11 75.7(3) . 1_545 ?
O8 Dy2 O17 83.0(3) . . ?
O8 Dy2 O18 74.2(3) . . ?
O8 Dy2 O19 112.9(4) . . ?
O8 Dy2 O20 142.8(3) . . ?
O10 Dy2 O9 141.2(3) 2_565 . ?
O11 Dy2 O9 118.7(4) 1_545 . ?
O11 Dy2 O10 75.6(3) 1_545 2_565 ?
O11 Dy2 O17 73.9(3) 1_545 . ?
O17 Dy2 O9 68.8(3) . . ?
O17 Dy2 O10 146.1(2) . 2_565 ?
O18 Dy2 O9 73.2(3) . . ?
O18 Dy2 O10 120.9(5) . 2_565 ?
O18 Dy2 O11 139.6(3) . 1_545 ?
O18 Dy2 O17 76.2(4) . . ?
O19 Dy2 O9 76.3(2) . . ?
O19 Dy2 O10 75.4(3) . 2_565 ?
O19 Dy2 O11 146.2(4) . 1_545 ?
O19 Dy2 O17 137.9(3) . . ?
O19 Dy2 O18 71.8(3) . . ?
O20 Dy2 O9 74.1(3) . . ?
O20 Dy2 O10 76.4(4) . 2_565 ?
O20 Dy2 O11 74.2(3) . 1_545 ?
O20 Dy2 O17 108.7(4) . . ?
O20 Dy2 O18 142.2(3) . . ?
O20 Dy2 O19 82.4(3) . . ?
C1 O1 Dy1 139.6(9) . . ?
C3 O3 Dy1 132.5(8) . 1_565 ?
C4 O4 Dy1 133.0(8) . 2_565 ?
C5 O5 Dy1 138.1(7) . . ?
C8 O8 Dy2 137.8(7) . . ?
C9 O9 Dy2 131.6(8) . . ?
C10 O10 Dy2 134.3(7) . 2_564 ?
C11 O11 Dy2 136.1(9) . 1_565 ?
Dy1 O13 H13A 109.9 . . ?
Dy1 O13 H13B 109.8 . . ?
H13A O13 H13B 104.1 . . ?
Dy1 O14 H14A 111.7 . . ?
Dy1 O14 H14B 113.1 . . ?
H14A O14 H14B 101.0 . . ?
Dy1 O15 H15A 127.8 . . ?
Dy1 O15 H15B 128.0 . . ?
H15A O15 H15B 104.3 . . ?
Dy1 O16 H16A 125.3 . . ?
Dy1 O16 H16B 125.4 . . ?
H16A O16 H16B 104.5 . . ?
Dy2 O17 H17A 110.9 . . ?
Dy2 O17 H17B 113.0 . . ?
H17A O17 H17B 102.5 . . ?
Dy2 O18 H18A 127.5 . . ?
Dy2 O18 H18B 128.0 . . ?
H18A O18 H18B 104.4 . . ?
Dy2 O19 H19A 127.8 . . ?
Dy2 O19 H19B 127.3 . . ?
H19A O19 H19B 104.4 . . ?
Dy2 O20 H20A 109.8 . . ?
Dy2 O20 H20B 110.5 . . ?
H20A O20 H20B 103.9 . . ?
O1 C1 C2 134.1(14) . . ?
O1 C1 C4 137.3(13) . . ?
C4 C1 C2 88.4(9) . . ?
O2 C2 C1 133.4(13) . . ?
O2 C2 C3 136.2(12) . . ?
C3 C2 C1 90.2(10) . . ?
O3 C3 C2 135.2(12) . . ?
O3 C3 C4 134.2(13) . . ?
C4 C3 C2 90.0(9) . . ?
O4 C4 C1 132.1(11) . . ?
O4 C4 C3 136.7(12) . . ?
C3 C4 C1 91.1(10) . . ?
O5 C5 C6 133.2(9) . . ?
O5 C5 C8 135.8(8) . . ?
C8 C5 C6 91.0(7) . . ?
O6 C6 C5 136.0(10) . . ?
O6 C6 C7 135.8(8) . . ?
C5 C6 C7 88.1(8) . . ?
O7 C7 C6 136.4(10) . . ?
O7 C7 C8 133.0(9) . . ?
C8 C7 C6 90.6(8) . . ?
O8 C8 C5 136.0(7) . . ?
O8 C8 C7 134.3(8) . . ?
C7 C8 C5 89.6(7) . . ?
O9 C9 C10 133.4(13) . . ?
O9 C9 C12 135.8(12) . . ?
C10 C9 C12 90.7(9) . . ?
O10 C10 C9 136.8(12) . . ?
O10 C10 C11 134.1(10) . . ?
C9 C10 C11 89.0(9) . . ?
O11 C11 C10 136.6(12) . . ?
O11 C11 C12 132.6(13) . . ?
C12 C11 C10 90.5(9) . . ?
O12 C12 C9 132.9(11) . . ?
O12 C12 C11 137.4(13) . . ?
C11 C12 C9 89.6(10) . . ?

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
Dy1 O1 C1 C2 -140.5(13) . . . . ?
Dy1 O1 C1 C4 33(3) . . . . ?
Dy1 O3 C3 C2 30(2) 1_565 . . . ?
Dy1 O3 C3 C4 -138.4(13) 1_565 . . . ?
Dy1 O4 C4 C1 148.0(11) 2_565 . . . ?
Dy1 O4 C4 C3 -36(2) 2_565 . . . ?
Dy1 O5 C5 C6 -33(2) . . . . ?
Dy1 O5 C5 C8 144.1(10) . . . . ?
Dy2 O8 C8 C5 44.6(18) . . . . ?
Dy2 O8 C8 C7 -138.7(10) . . . . ?
Dy2 O9 C9 C10 144.3(12) . . . . ?
Dy2 O9 C9 C12 -31(2) . . . . ?
Dy2 O10 C10 C9 37(2) 2_564 . . . ?
Dy2 O10 C10 C11 -145.7(11) 2_564 . . . ?
Dy2 O11 C11 C10 -39(2) 1_565 . . . ?
Dy2 O11 C11 C12 134.1(13) 1_565 . . . ?
O1 C1 C2 O2 -3(3) . . . . ?
O1 C1 C2 C3 171.6(15) . . . . ?
O1 C1 C4 O4 6(3) . . . . ?
O1 C1 C4 C3 -171.4(16) . . . . ?
O2 C2 C3 O3 8(3) . . . . ?
O2 C2 C3 C4 179.1(17) . . . . ?
O3 C3 C4 O4 -10(3) . . . . ?
O3 C3 C4 C1 167.3(15) . . . . ?
O5 C5 C6 O6 -10(2) . . . . ?
O5 C5 C6 C7 171.9(13) . . . . ?
O5 C5 C8 O8 6(2) . . . . ?
O5 C5 C8 C7 -171.7(13) . . . . ?
O6 C6 C7 O7 11(2) . . . . ?
O6 C6 C7 C8 -172.1(14) . . . . ?
O7 C7 C8 O8 -7(2) . . . . ?
O7 C7 C8 C5 171.1(12) . . . . ?
O9 C9 C10 O10 4(3) . . . . ?
O9 C9 C10 C11 -173.5(14) . . . . ?
O9 C9 C12 O12 -4(3) . . . . ?
O9 C9 C12 C11 173.3(15) . . . . ?
O10 C10 C11 O11 -7(3) . . . . ?
O10 C10 C11 C12 178.8(14) . . . . ?
O11 C11 C12 O12 6(3) . . . . ?
O11 C11 C12 C9 -171.6(14) . . . . ?
C1 C2 C3 O3 -167.2(16) . . . . ?
C1 C2 C3 C4 4.3(12) . . . . ?
C2 C1 C4 O4 -178.6(14) . . . . ?
C2 C1 C4 C3 4.3(12) . . . . ?
C2 C3 C4 O4 178.8(15) . . . . ?
C2 C3 C4 C1 -4.3(12) . . . . ?
C4 C1 C2 O2 -179.3(16) . . . . ?
C4 C1 C2 C3 -4.3(12) . . . . ?
C5 C6 C7 O7 -171.0(13) . . . . ?
C5 C6 C7 C8 6.3(8) . . . . ?
C6 C5 C8 O8 -176.0(12) . . . . ?
C6 C5 C8 C7 6.4(8) . . . . ?
C6 C7 C8 O8 176.0(12) . . . . ?
C6 C7 C8 C5 -6.3(8) . . . . ?
C8 C5 C6 O6 172.1(14) . . . . ?
C8 C5 C6 C7 -6.3(8) . . . . ?
C9 C10 C11 O11 171.2(15) . . . . ?
C9 C10 C11 C12 -3.4(11) . . . . ?
C10 C9 C12 O12 178.9(16) . . . . ?
C10 C9 C12 C11 -3.4(11) . . . . ?
C10 C11 C12 O12 -179.1(18) . . . . ?
C10 C11 C12 C9 3.4(11) . . . . ?
C12 C9 C10 O10 -178.9(15) . . . . ?
C12 C9 C10 C11 3.4(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.671
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.77(4)
2 0.23(4)

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_ho_sq_syn20211020_a_auto
_database_code_depnum_ccdc_archive 'CCDC 2218676'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-11-10
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Ho2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'holmium(III) squarate'
_chemical_formula_moiety         'C12 H16 Ho2 O20'
_chemical_formula_sum            'C12 H16 Ho2 O20'
_chemical_formula_weight         810.11
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16O20Ho2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9195(7)
_cell_length_b                   8.1486(5)
_cell_length_c                   10.0126(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.907(6)
_cell_angle_gamma                90
_cell_volume                     967.33(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3339
_cell_measurement_temperature    295.3(3)
_cell_measurement_theta_max      30.6970
_cell_measurement_theta_min      3.1530
_shelx_estimated_absorpt_T_max   0.719
_shelx_estimated_absorpt_T_min   0.151
_exptl_absorpt_coefficient_mu    8.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    2.781
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.043
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8074
_diffrn_reflns_point_group_measured_fraction_full 0.770
_diffrn_reflns_point_group_measured_fraction_max 0.597
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.601
_diffrn_reflns_theta_min         2.499
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.3(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00 -17.00   0.50   15.74    --    5.00  45.00   0.00   72
  2  ω    -98.00  78.00   0.50   15.74    --  -10.80  45.00  90.00  352
  3  ω    -54.00  21.00   0.50   15.74    --  -10.80  45.00  30.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RINC): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0153713000
_diffrn_orient_matrix_UB_12      0.0357371000
_diffrn_orient_matrix_UB_13      0.0600793000
_diffrn_orient_matrix_UB_21      -0.0457561000
_diffrn_orient_matrix_UB_22      -0.0558479000
_diffrn_orient_matrix_UB_23      -0.0001971000
_diffrn_orient_matrix_UB_31      0.0353619000
_diffrn_orient_matrix_UB_32      -0.0562223000
_diffrn_orient_matrix_UB_33      0.0384093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage         0.387
_reflns_Friedel_fraction_full    0.540
_reflns_Friedel_fraction_max     0.333
_reflns_number_gt                3180
_reflns_number_total             3550
_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       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 
;
 Flack x determined using 856 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(19)
_refine_ls_extinction_coef       0.00166(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0195
_refine_ls_restrained_S_all      0.995
_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)+(0.0204P)²+0.0969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0496
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
4.b Rotating group:
 O13(H13A,H13B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_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
C1 C 0.1504(7) 0.3714(8) 0.6168(9) 0.0174(16) Uani 1 1 d . U . . .
C2 C 0.1166(8) 0.2087(9) 0.6646(9) 0.0144(15) Uani 1 1 d . U . . .
C3 C 0.1746(7) 0.1299(8) 0.5592(8) 0.0140(16) Uani 1 1 d . U . . .
C4 C 0.1992(7) 0.2882(9) 0.5032(8) 0.0148(15) Uani 1 1 d . U . . .
C5 C 0.4730(5) 0.9886(6) 0.5810(6) 0.0152(11) Uani 1 1 d . . . . .
C6 C 0.4544(6) 1.1602(7) 0.6124(7) 0.0164(13) Uani 1 1 d . . . . .
C7 C 0.5263(5) 1.2060(7) 0.5076(6) 0.0165(12) Uani 1 1 d . . . . .
C8 C 0.5548(5) 1.0335(6) 0.4880(6) 0.0160(12) Uani 1 1 d . . . . .
C9 C 0.8210(7) 0.3680(8) 0.5606(8) 0.0141(16) Uani 1 1 d . U . . .
C10 C 0.8003(7) 0.2070(9) 0.6174(8) 0.0143(15) Uani 1 1 d . U . . .
C11 C 0.8498(7) 0.1266(8) 0.5086(8) 0.0141(16) Uani 1 1 d . U . . .
C12 C 0.8781(8) 0.2875(9) 0.4571(8) 0.0139(15) Uani 1 1 d . U . . .
O1 O 0.1472(5) 0.5142(5) 0.6606(6) 0.0223(12) Uani 1 1 d . . . . .
O2 O 0.0671(6) 0.1607(6) 0.7602(6) 0.0274(16) Uani 1 1 d . . . . .
O3 O 0.2016(6) -0.0163(5) 0.5356(6) 0.0173(12) Uani 1 1 d . . . . .
O4 O 0.2475(6) 0.3390(5) 0.4058(6) 0.0226(14) Uani 1 1 d . . . . .
O5 O 0.4327(5) 0.8534(5) 0.6179(7) 0.0215(13) Uani 1 1 d . . . . .
O6 O 0.4026(5) 1.2338(5) 0.6949(5) 0.0225(11) Uani 1 1 d . . . . .
O7 O 0.5518(5) 1.3356(5) 0.4501(5) 0.0277(13) Uani 1 1 d . . . . .
O8 O 0.6205(5) 0.9631(5) 0.4184(6) 0.0222(11) Uani 1 1 d . . . . .
O9 O 0.7936(6) 0.5132(5) 0.5864(6) 0.0170(12) Uani 1 1 d . . . . .
O10 O 0.7530(5) 0.1554(4) 0.7177(5) 0.0173(12) Uani 1 1 d . . . . .
O11 O 0.8613(5) -0.0151(5) 0.4648(6) 0.0223(11) Uani 1 1 d . . . . .
O12 O 0.9272(6) 0.3377(5) 0.3589(7) 0.0215(13) Uani 1 1 d . . . . .
O13 O 0.3973(5) 0.5560(5) 0.7217(6) 0.0242(12) Uani 1 1 d . . . . .
H13A H 0.3680 0.4602 0.7149 0.036 Uiso 1 1 d R U . . .
H13B H 0.4255 0.5619 0.8037 0.036 Uiso 1 1 d R U . . .
O14 O 0.2512(8) 0.6724(6) 0.4518(7) 0.0427(19) Uani 1 1 d G . . . .
H14A H 0.2643 0.5789 0.4198 0.064 Uiso 1 1 d G U . . .
H14B H 0.3037 0.7330 0.4285 0.064 Uiso 1 1 d G U . . .
O15 O 0.0796(5) 0.8325(6) 0.7304(7) 0.0253(14) Uani 1 1 d G . . . .
H15A H 0.0234 0.7810 0.7543 0.038 Uiso 1 1 d G U . . .
H15B H 0.0616 0.9322 0.7363 0.038 Uiso 1 1 d G U . . .
O16 O 0.3062(6) 0.9799(6) 0.8134(6) 0.0195(12) Uani 1 1 d G . . . .
H16A H 0.2933 1.0100 0.8909 0.029 Uiso 1 1 d G U . . .
H16B H 0.3406 1.0597 0.7826 0.029 Uiso 1 1 d G U . . .
O17 O 0.7576(7) 0.8221(4) 0.6747(7) 0.0277(12) Uani 1 1 d . . . . .
H17A H 0.7787 0.9223 0.6846 0.042 Uiso 1 1 d R U . . .
H17B H 0.8097 0.7681 0.7218 0.042 Uiso 1 1 d R U . . .
O18 O 0.5764(6) 0.6471(5) 0.5139(7) 0.0297(15) Uani 1 1 d G . . . .
H18A H 0.5576 0.5474 0.5135 0.045 Uiso 1 1 d G U . . .
H18B H 0.5228 0.6960 0.5462 0.045 Uiso 1 1 d G U . . .
O19 O 0.6879(6) 0.5235(6) 0.3070(6) 0.0218(12) Uani 1 1 d G . . . .
H19A H 0.7168 0.4862 0.2402 0.033 Uiso 1 1 d G U . . .
H19B H 0.6512 0.4438 0.3345 0.033 Uiso 1 1 d G U . . .
O20 O 0.9227(5) 0.6643(6) 0.3925(6) 0.0239(14) Uani 1 1 d . . . . .
H20A H 0.9183 0.5681 0.3586 0.036 Uiso 1 1 d R U . . .
H20B H 0.9450 0.7239 0.3301 0.036 Uiso 1 1 d R U . . .
Ho1 Ho 0.25528(2) 0.75551(2) 0.67900(2) 0.01239(14) Uani 1 1 d . . . . .
Ho2 Ho 0.74534(2) 0.74843(3) 0.44334(2) 0.01179(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.479(9) . ?
C1 C4 1.493(10) . ?
C1 O1 1.245(8) . ?
C2 C3 1.468(10) . ?
C2 O2 1.238(9) . ?
C3 C4 1.449(9) . ?
C3 O3 1.262(8) . ?
C4 O4 1.252(9) . ?
C5 C6 1.455(7) . ?
C5 C8 1.463(7) . ?
C5 O5 1.272(6) . ?
C6 C7 1.470(9) . ?
C6 O6 1.236(8) . ?
C7 C8 1.464(8) . ?
C7 O7 1.255(7) . ?
C8 O8 1.241(7) . ?
C9 C10 1.461(9) . ?
C9 C12 1.453(10) . ?
C9 O9 1.262(8) . ?
C10 C11 1.447(10) . ?
C10 O10 1.273(9) . ?
C11 C12 1.461(9) . ?
C11 O11 1.248(8) . ?
C12 O12 1.263(9) . ?
O1 Ho1 2.348(5) . ?
O3 Ho1 2.396(5) 1_545 ?
O4 Ho1 2.409(6) 2_564 ?
O5 Ho1 2.398(6) . ?
O8 Ho2 2.294(5) . ?
O9 Ho2 2.427(5) . ?
O10 Ho2 2.402(5) 2_565 ?
O11 Ho2 2.368(5) 1_545 ?
O13 H13A 0.8552 . ?
O13 H13B 0.8564 . ?
O13 Ho1 2.354(5) . ?
O14 H14A 0.8465 . ?
O14 H14B 0.8486 . ?
O14 Ho1 2.369(7) . ?
O15 H15A 0.8458 . ?
O15 H15B 0.8439 . ?
O15 Ho1 2.295(6) . ?
O16 H16A 0.8434 . ?
O16 H16B 0.8440 . ?
O16 Ho1 2.314(5) . ?
O17 H17A 0.8567 . ?
O17 H17B 0.8613 . ?
O17 Ho2 2.383(7) . ?
O18 H18A 0.8430 . ?
O18 H18B 0.8442 . ?
O18 Ho2 2.352(6) . ?
O19 H19A 0.8402 . ?
O19 H19B 0.8441 . ?
O19 Ho2 2.345(5) . ?
O20 H20A 0.8541 . ?
O20 H20B 0.8546 . ?
O20 Ho2 2.328(6) . ?
Ho1 O3 2.396(5) 1_565 ?
Ho1 O4 2.409(6) 2_565 ?
Ho2 O10 2.402(5) 2_564 ?
Ho2 O11 2.368(5) 1_565 ?

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
C2 C1 C4 88.9(6) . . ?
O1 C1 C2 134.8(8) . . ?
O1 C1 C4 136.1(7) . . ?
C3 C2 C1 89.7(6) . . ?
O2 C2 C1 134.5(7) . . ?
O2 C2 C3 135.6(7) . . ?
C4 C3 C2 91.0(6) . . ?
O3 C3 C2 134.0(7) . . ?
O3 C3 C4 134.6(7) . . ?
C3 C4 C1 89.9(6) . . ?
O4 C4 C1 133.6(7) . . ?
O4 C4 C3 136.4(8) . . ?
C6 C5 C8 91.4(4) . . ?
O5 C5 C6 134.4(5) . . ?
O5 C5 C8 134.3(5) . . ?
C5 C6 C7 88.7(4) . . ?
O6 C6 C5 135.1(6) . . ?
O6 C6 C7 136.2(5) . . ?
C8 C7 C6 90.7(4) . . ?
O7 C7 C6 136.7(6) . . ?
O7 C7 C8 132.5(5) . . ?
C5 C8 C7 88.6(4) . . ?
O8 C8 C5 138.0(5) . . ?
O8 C8 C7 133.4(5) . . ?
C12 C9 C10 89.0(5) . . ?
O9 C9 C10 134.8(7) . . ?
O9 C9 C12 136.1(7) . . ?
C11 C10 C9 90.9(6) . . ?
O10 C10 C9 135.3(8) . . ?
O10 C10 C11 133.8(7) . . ?
C10 C11 C12 89.2(6) . . ?
O11 C11 C10 138.7(7) . . ?
O11 C11 C12 132.0(7) . . ?
C9 C12 C11 90.6(6) . . ?
O12 C12 C9 134.2(7) . . ?
O12 C12 C11 135.1(7) . . ?
C1 O1 Ho1 140.7(5) . . ?
C3 O3 Ho1 132.7(5) . 1_545 ?
C4 O4 Ho1 133.9(5) . 2_564 ?
C5 O5 Ho1 137.0(4) . . ?
C8 O8 Ho2 137.0(4) . . ?
C9 O9 Ho2 132.1(5) . . ?
C10 O10 Ho2 134.2(4) . 2_565 ?
C11 O11 Ho2 134.5(5) . 1_545 ?
H13A O13 H13B 104.1 . . ?
Ho1 O13 H13A 109.6 . . ?
Ho1 O13 H13B 109.9 . . ?
H14A O14 H14B 104.5 . . ?
Ho1 O14 H14A 129.3 . . ?
Ho1 O14 H14B 98.9 . . ?
H15A O15 H15B 104.1 . . ?
Ho1 O15 H15A 134.1 . . ?
Ho1 O15 H15B 121.5 . . ?
H16A O16 H16B 104.7 . . ?
Ho1 O16 H16A 134.7 . . ?
Ho1 O16 H16B 120.3 . . ?
H17A O17 H17B 103.7 . . ?
Ho2 O17 H17A 109.8 . . ?
Ho2 O17 H17B 111.8 . . ?
H18A O18 H18B 104.3 . . ?
Ho2 O18 H18A 124.9 . . ?
Ho2 O18 H18B 130.8 . . ?
H19A O19 H19B 104.5 . . ?
Ho2 O19 H19A 128.8 . . ?
Ho2 O19 H19B 122.7 . . ?
H20A O20 H20B 104.0 . . ?
Ho2 O20 H20A 109.7 . . ?
Ho2 O20 H20B 110.5 . . ?
O1 Ho1 O3 119.5(2) . 1_565 ?
O1 Ho1 O4 74.46(18) . 2_565 ?
O1 Ho1 O5 138.57(19) . . ?
O1 Ho1 O13 79.30(17) . . ?
O1 Ho1 O14 74.23(19) . . ?
O3 Ho1 O4 141.19(19) 1_565 2_565 ?
O3 Ho1 O5 77.13(19) 1_565 . ?
O5 Ho1 O4 117.9(2) . 2_565 ?
O13 Ho1 O3 142.0(2) . 1_565 ?
O13 Ho1 O4 72.84(19) . 2_565 ?
O13 Ho1 O5 68.86(17) . . ?
O13 Ho1 O14 85.4(2) . . ?
O14 Ho1 O3 70.66(19) . 1_565 ?
O14 Ho1 O4 144.56(13) . 2_565 ?
O14 Ho1 O5 77.4(3) . . ?
O15 Ho1 O1 74.96(19) . . ?
O15 Ho1 O3 74.2(2) . 1_565 ?
O15 Ho1 O4 75.6(2) . 2_565 ?
O15 Ho1 O5 144.65(13) . . ?
O15 Ho1 O13 143.5(2) . . ?
O15 Ho1 O14 111.4(3) . . ?
O15 Ho1 O16 81.1(2) . . ?
O16 Ho1 O1 144.8(2) . . ?
O16 Ho1 O3 76.87(14) . 1_565 ?
O16 Ho1 O4 74.81(19) . 2_565 ?
O16 Ho1 O5 72.5(2) . . ?
O16 Ho1 O13 107.4(2) . . ?
O16 Ho1 O14 139.7(2) . . ?
O8 Ho2 O9 141.1(2) . . ?
O8 Ho2 O10 74.68(17) . 2_564 ?
O8 Ho2 O11 75.84(17) . 1_565 ?
O8 Ho2 O17 83.6(2) . . ?
O8 Ho2 O18 74.60(19) . . ?
O8 Ho2 O19 112.7(3) . . ?
O8 Ho2 O20 142.59(19) . . ?
O10 Ho2 O9 141.58(17) 2_564 . ?
O11 Ho2 O9 119.2(2) 1_565 . ?
O11 Ho2 O10 75.03(18) 1_565 2_564 ?
O11 Ho2 O17 74.33(19) 1_565 . ?
O17 Ho2 O9 68.77(17) . . ?
O17 Ho2 O10 145.87(13) . 2_564 ?
O18 Ho2 O9 72.7(2) . . ?
O18 Ho2 O10 120.9(3) . 2_564 ?
O18 Ho2 O11 140.2(2) . 1_565 ?
O18 Ho2 O17 76.4(3) . . ?
O19 Ho2 O9 76.31(16) . . ?
O19 Ho2 O10 75.21(19) . 2_564 ?
O19 Ho2 O11 145.3(2) . 1_565 ?
O19 Ho2 O17 138.4(2) . . ?
O19 Ho2 O18 72.1(2) . . ?
O20 Ho2 O9 74.41(19) . . ?
O20 Ho2 O10 76.5(2) . 2_564 ?
O20 Ho2 O11 74.02(19) . 1_565 ?
O20 Ho2 O17 108.7(3) . . ?
O20 Ho2 O18 141.95(16) . . ?
O20 Ho2 O19 82.0(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
C1 C2 C3 C4 -5.1(7) . . . . ?
C1 C2 C3 O3 168.8(9) . . . . ?
C1 C4 O4 Ho1 -147.8(7) . . . 2_564 ?
C2 C1 C4 C3 -5.0(7) . . . . ?
C2 C1 C4 O4 178.9(9) . . . . ?
C2 C1 O1 Ho1 140.3(8) . . . . ?
C2 C3 C4 C1 5.0(7) . . . . ?
C2 C3 C4 O4 -179.1(10) . . . . ?
C2 C3 O3 Ho1 -32.4(14) . . . 1_545 ?
C3 C4 O4 Ho1 37.9(15) . . . 2_564 ?
C4 C1 C2 C3 4.9(7) . . . . ?
C4 C1 C2 O2 -179.7(10) . . . . ?
C4 C1 O1 Ho1 -32.2(16) . . . . ?
C4 C3 O3 Ho1 139.0(8) . . . 1_545 ?
C5 C6 C7 C8 -6.2(5) . . . . ?
C5 C6 C7 O7 170.8(8) . . . . ?
C5 C8 O8 Ho2 -42.8(12) . . . . ?
C6 C5 C8 C7 -6.3(5) . . . . ?
C6 C5 C8 O8 174.8(8) . . . . ?
C6 C5 O5 Ho1 33.9(12) . . . . ?
C6 C7 C8 C5 6.2(5) . . . . ?
C6 C7 C8 O8 -174.8(8) . . . . ?
C7 C8 O8 Ho2 138.7(6) . . . . ?
C8 C5 C6 C7 6.2(5) . . . . ?
C8 C5 C6 O6 -172.1(9) . . . . ?
C8 C5 O5 Ho1 -144.7(6) . . . . ?
C9 C10 C11 C12 3.9(7) . . . . ?
C9 C10 C11 O11 -172.1(10) . . . . ?
C9 C10 O10 Ho2 -38.0(13) . . . 2_565 ?
C10 C9 C12 C11 3.9(7) . . . . ?
C10 C9 C12 O12 -179.0(10) . . . . ?
C10 C9 O9 Ho2 -144.3(8) . . . . ?
C10 C11 C12 C9 -3.9(7) . . . . ?
C10 C11 C12 O12 179.0(10) . . . . ?
C10 C11 O11 Ho2 38.4(15) . . . 1_545 ?
C11 C10 O10 Ho2 146.3(7) . . . 2_565 ?
C12 C9 C10 C11 -3.9(7) . . . . ?
C12 C9 C10 O10 179.2(9) . . . . ?
C12 C9 O9 Ho2 29.6(14) . . . . ?
C12 C11 O11 Ho2 -136.2(8) . . . 1_545 ?
O1 C1 C2 C3 -169.8(9) . . . . ?
O1 C1 C2 O2 5.5(18) . . . . ?
O1 C1 C4 C3 169.6(10) . . . . ?
O1 C1 C4 O4 -6.5(17) . . . . ?
O2 C2 C3 C4 179.7(10) . . . . ?
O2 C2 C3 O3 -6.4(18) . . . . ?
O3 C3 C4 C1 -168.8(9) . . . . ?
O3 C3 C4 O4 7.1(18) . . . . ?
O5 C5 C6 C7 -172.8(7) . . . . ?
O5 C5 C6 O6 8.9(15) . . . . ?
O5 C5 C8 C7 172.8(7) . . . . ?
O5 C5 C8 O8 -6.2(13) . . . . ?
O6 C6 C7 C8 172.1(9) . . . . ?
O6 C6 C7 O7 -10.9(15) . . . . ?
O7 C7 C8 C5 -171.0(7) . . . . ?
O7 C7 C8 O8 8.0(12) . . . . ?
O9 C9 C10 C11 171.9(9) . . . . ?
O9 C9 C10 O10 -5.0(17) . . . . ?
O9 C9 C12 C11 -171.8(9) . . . . ?
O9 C9 C12 O12 5.3(17) . . . . ?
O10 C10 C11 C12 -179.2(9) . . . . ?
O10 C10 C11 O11 4.8(17) . . . . ?
O11 C11 C12 C9 172.5(8) . . . . ?
O11 C11 C12 O12 -4.6(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.627
_oxdiff_exptl_absorpt_empirical_full_min 0.785
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_tmoac_sq_20211213_autored
_database_code_depnum_ccdc_archive 'CCDC 2218678'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-11-09
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Tm2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'thulium(III) squarate'
_chemical_formula_moiety         'C12 H16 O20 Tm2'
_chemical_formula_sum            'C12 H16 O20 Tm2'
_chemical_formula_weight         818.11
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16O20Tm2
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'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9240(4)
_cell_length_b                   8.1318(2)
_cell_length_c                   9.9899(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.876(3)
_cell_angle_gamma                90
_cell_volume                     963.56(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5578
_cell_measurement_temperature    295.8(2)
_cell_measurement_theta_max      31.1030
_cell_measurement_theta_min      2.5040
_shelx_estimated_absorpt_T_max   0.607
_shelx_estimated_absorpt_T_min   0.181
_exptl_absorpt_coefficient_mu    9.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.820
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -11 0 0.0352
-4 11 0 0.0337
-17 -2 0 0.0326
2 -1 14 0.0937
1 -7 -11 0.1285
-4 9 -9 0.1115
17 1 0 0.0193
2 -9 8 0.0739
-3 11 2 0.0374

_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.6237 -11.1842 0.1193 -0.1744 0.5728 0.8009
-3.5798 11.1960 0.3408 0.1818 -0.5980 -0.7806
-16.5422 -1.6698 -0.0439 0.9104 0.3796 -0.1647
1.6005 -0.5287 13.7990 0.2085 -0.7102 0.6724
1.1404 -7.0811 -11.0693 -0.2856 0.9583 -0.0056
-3.5028 8.5898 -8.5107 -0.0067 0.0075 -0.9999
16.5687 1.2867 0.3744 -0.9040 -0.3752 0.2050
2.1968 -8.9115 8.4365 0.0775 0.0370 0.9963
-3.3899 11.1364 1.9882 0.2067 -0.6830 -0.7006

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.404
_diffrn_reflns_theta_min         2.505
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.8(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  28.00   0.50    1.00    --  -15.72 -99.00  30.00   90
  2  ω    -27.00  28.00   0.50    1.00    --   14.78 -55.00-163.00  110
  3  ω     47.00  76.00   0.50    1.00    --   14.78 178.00-180.00   58
  4  ω    -11.00  90.00   0.50    1.00    --   14.78  55.00 -20.00  202
  5  ω      7.00  67.00   0.50    1.00    --  -15.72  19.00  30.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0548924000
_diffrn_orient_matrix_UB_12      -0.0019653000
_diffrn_orient_matrix_UB_13      0.0213995000
_diffrn_orient_matrix_UB_21      -0.0170262000
_diffrn_orient_matrix_UB_22      -0.0572811000
_diffrn_orient_matrix_UB_23      -0.0516881000
_diffrn_orient_matrix_UB_31      0.0164815000
_diffrn_orient_matrix_UB_32      -0.0658014000
_diffrn_orient_matrix_UB_33      0.0442965000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                3297
_reflns_number_total             3610
_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       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    
'olex2.solve 1.5-ac5-018 (Bourhis et al., 2015)'
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.766(19)
_refine_ls_extinction_coef       0.00152(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0182
_refine_ls_restrained_S_all      1.049
_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)+(0.0337P)²+0.2347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0546
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.234(19)
 0.766(19)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Tm2-H18A \\sim Tm2-H18B
 with sigma of 0.02
 Tm1-H15A \\sim Tm1-H15B
 with sigma of 0.02
 Tm2-H19A \\sim Tm2-H19B
 with sigma of 0.02
 Tm1-H16A \\sim Tm1-H16B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1511(7) 0.3716(8) 0.6142(9) 0.0157(15) Uani 1 1 d . U . . .
C2 C 0.1172(7) 0.2098(8) 0.6656(9) 0.0151(14) Uani 1 1 d . U . . .
C3 C 0.1744(7) 0.1299(8) 0.5616(8) 0.0148(15) Uani 1 1 d . U . . .
C4 C 0.1983(7) 0.2881(9) 0.5044(8) 0.0155(13) Uani 1 1 d . U . . .
C5 C 0.4743(5) 0.9881(6) 0.5814(6) 0.0182(11) Uani 1 1 d . . . . .
C6 C 0.4553(6) 1.1593(6) 0.6134(8) 0.0187(13) Uani 1 1 d . . . . .
C7 C 0.5269(5) 1.2065(7) 0.5078(7) 0.0202(12) Uani 1 1 d . . . . .
C8 C 0.5554(5) 1.0326(5) 0.4883(6) 0.0162(11) Uani 1 1 d . . . . .
C9 C 0.8207(7) 0.3673(7) 0.5611(8) 0.0149(14) Uani 1 1 d . U . . .
C10 C 0.7983(6) 0.2053(8) 0.6181(8) 0.0148(13) Uani 1 1 d . U . . .
C11 C 0.8505(7) 0.1250(8) 0.5055(8) 0.0158(15) Uani 1 1 d . U . . .
C12 C 0.8797(7) 0.2872(9) 0.4561(9) 0.0150(13) Uani 1 1 d . U . . .
O1 O 0.1477(5) 0.5151(5) 0.6615(6) 0.0245(12) Uani 1 1 d . . . . .
O2 O 0.0681(5) 0.1610(5) 0.7625(6) 0.0263(14) Uani 1 1 d . . . . .
O3 O 0.2033(5) -0.0162(5) 0.5350(6) 0.0177(11) Uani 1 1 d . . . . .
O4 O 0.2478(6) 0.3399(5) 0.4053(6) 0.0230(13) Uani 1 1 d . . . . .
O5 O 0.4313(5) 0.8529(5) 0.6166(7) 0.0239(13) Uani 1 1 d . . . . .
O6 O 0.4026(5) 1.2338(4) 0.6947(6) 0.0226(11) Uani 1 1 d . . . . .
O7 O 0.5519(5) 1.3358(5) 0.4485(6) 0.0313(13) Uani 1 1 d . . . . .
O8 O 0.6221(5) 0.9621(5) 0.4181(6) 0.0213(11) Uani 1 1 d . . . . .
O9 O 0.7941(6) 0.5129(5) 0.5854(6) 0.0186(12) Uani 1 1 d . . . . .
O10 O 0.7524(5) 0.1551(4) 0.7176(6) 0.0185(12) Uani 1 1 d . . . . .
O11 O 0.8613(5) -0.0174(5) 0.4636(6) 0.0223(11) Uani 1 1 d . . . . .
O12 O 0.9283(5) 0.3386(5) 0.3584(7) 0.0236(13) Uani 1 1 d . . . . .
O13 O 0.3957(5) 0.5561(5) 0.7194(7) 0.0264(12) Uani 1 1 d . . . . .
H13A H 0.3666 0.4610 0.7081 0.040 Uiso 1 1 d R U . . .
H13B H 0.4209 0.5585 0.8021 0.040 Uiso 1 1 d R U . . .
O14 O 0.2511(7) 0.6732(6) 0.4542(7) 0.0418(17) Uani 1 1 d G . . . .
H14A H 0.2733 0.5763 0.4244 0.063 Uiso 1 1 d G U . . .
H14B H 0.2891 0.7359 0.4206 0.063 Uiso 1 1 d G U . . .
O15 O 0.0806(5) 0.8320(6) 0.7295(7) 0.0245(13) Uani 1 1 d G . . . .
H15A H 0.0298 0.7715 0.7562 0.037 Uiso 1 1 d DG U . . .
H15B H 0.0499 0.9251 0.7197 0.037 Uiso 1 1 d DG U . . .
O16 O 0.3062(6) 0.9779(5) 0.8130(6) 0.0211(12) Uani 1 1 d G . . . .
H16A H 0.2731 1.0091 0.8800 0.032 Uiso 1 1 d DG U . . .
H16B H 0.3344 1.0654 0.7840 0.032 Uiso 1 1 d DG U . . .
O17 O 0.7572(6) 0.8216(4) 0.6731(8) 0.0299(11) Uani 1 1 d . . . . .
H17A H 0.7715 0.9242 0.6820 0.045 Uiso 1 1 d R U . . .
H17B H 0.8137 0.7753 0.7186 0.045 Uiso 1 1 d R U . . .
O18 O 0.5765(5) 0.6480(5) 0.5124(8) 0.0295(15) Uani 1 1 d G . . . .
H18A H 0.5528 0.5505 0.5094 0.044 Uiso 1 1 d DG U . . .
H18B H 0.5247 0.7018 0.5435 0.044 Uiso 1 1 d DG U . . .
O19 O 0.6878(6) 0.5248(6) 0.3073(6) 0.0233(12) Uani 1 1 d G . . . .
H19A H 0.7076 0.4984 0.2321 0.035 Uiso 1 1 d DG U . . .
H19B H 0.6469 0.4463 0.3283 0.035 Uiso 1 1 d DG U . . .
O20 O 0.9205(5) 0.6655(5) 0.3929(7) 0.0268(13) Uani 1 1 d . . . . .
H20A H 0.9157 0.5706 0.3566 0.040 Uiso 1 1 d R U . . .
H20B H 0.9435 0.7271 0.3324 0.040 Uiso 1 1 d R U . . .
Tm1 Tm 0.25560(2) 0.75553(2) 0.67917(2) 0.01354(13) Uani 1 1 d D . . . .
Tm2 Tm 0.74497(2) 0.74824(2) 0.44325(2) 0.01204(13) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.484(9) . ?
C1 C4 1.452(10) . ?
C1 O1 1.262(8) . ?
C2 C3 1.454(10) . ?
C2 O2 1.246(9) . ?
C3 C4 1.448(9) . ?
C3 O3 1.273(8) . ?
C4 O4 1.275(9) . ?
C5 C6 1.451(7) . ?
C5 C8 1.455(7) . ?
C5 O5 1.278(6) . ?
C6 C7 1.475(9) . ?
C6 O6 1.235(8) . ?
C7 C8 1.472(7) . ?
C7 O7 1.258(7) . ?
C8 O8 1.252(7) . ?
C9 C10 1.471(8) . ?
C9 C12 1.473(10) . ?
C9 O9 1.256(7) . ?
C10 C11 1.490(10) . ?
C10 O10 1.251(8) . ?
C11 C12 1.462(9) . ?
C11 O11 1.243(7) . ?
C12 O12 1.257(9) . ?
O1 Tm1 2.337(5) . ?
O3 Tm1 2.392(5) 1_545 ?
O4 Tm1 2.399(6) 2_564 ?
O5 Tm1 2.382(6) . ?
O8 Tm2 2.271(5) . ?
O9 Tm2 2.419(5) . ?
O10 Tm2 2.398(6) 2_565 ?
O11 Tm2 2.354(5) 1_545 ?
O13 H13A 0.8495 . ?
O13 H13B 0.8505 . ?
O13 Tm1 2.333(5) . ?
O14 H14A 0.8915 . ?
O14 H14B 0.7802 . ?
O14 Tm1 2.340(7) . ?
O15 H15A 0.8450 . ?
O15 H15B 0.8423 . ?
O15 Tm1 2.282(6) . ?
O16 H16A 0.8499 . ?
O16 H16B 0.8502 . ?
O16 Tm1 2.292(5) . ?
O17 H17A 0.8541 . ?
O17 H17B 0.8599 . ?
O17 Tm2 2.362(7) . ?
O18 H18A 0.8414 . ?
O18 H18B 0.8428 . ?
O18 Tm2 2.337(6) . ?
O19 H19A 0.8388 . ?
O19 H19B 0.8431 . ?
O19 Tm2 2.328(5) . ?
O20 H20A 0.8519 . ?
O20 H20B 0.8520 . ?
O20 Tm2 2.303(6) . ?
Tm1 O3 2.392(5) 1_565 ?
Tm1 O4 2.399(6) 2_565 ?
Tm2 O10 2.398(6) 2_564 ?
Tm2 O11 2.354(5) 1_565 ?

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
C4 C1 C2 89.3(5) . . ?
O1 C1 C2 132.1(7) . . ?
O1 C1 C4 138.2(7) . . ?
C3 C2 C1 89.1(6) . . ?
O2 C2 C1 135.9(7) . . ?
O2 C2 C3 134.8(7) . . ?
C4 C3 C2 90.7(5) . . ?
O3 C3 C2 136.3(7) . . ?
O3 C3 C4 132.7(7) . . ?
C3 C4 C1 90.5(6) . . ?
O4 C4 C1 132.7(7) . . ?
O4 C4 C3 136.5(7) . . ?
C6 C5 C8 91.8(4) . . ?
O5 C5 C6 133.5(5) . . ?
O5 C5 C8 134.6(5) . . ?
C5 C6 C7 88.7(5) . . ?
O6 C6 C5 135.8(6) . . ?
O6 C6 C7 135.5(5) . . ?
C8 C7 C6 90.2(4) . . ?
O7 C7 C6 137.5(6) . . ?
O7 C7 C8 132.3(6) . . ?
C5 C8 C7 88.7(4) . . ?
O8 C8 C5 138.3(4) . . ?
O8 C8 C7 133.0(5) . . ?
C10 C9 C12 89.9(5) . . ?
O9 C9 C10 135.3(7) . . ?
O9 C9 C12 134.7(7) . . ?
C9 C10 C11 89.7(5) . . ?
O10 C10 C9 135.4(7) . . ?
O10 C10 C11 135.0(6) . . ?
C12 C11 C10 89.5(5) . . ?
O11 C11 C10 136.8(7) . . ?
O11 C11 C12 133.6(7) . . ?
C11 C12 C9 90.6(5) . . ?
O12 C12 C9 134.2(7) . . ?
O12 C12 C11 135.0(7) . . ?
C1 O1 Tm1 139.8(5) . . ?
C3 O3 Tm1 131.2(5) . 1_545 ?
C4 O4 Tm1 133.6(4) . 2_564 ?
C5 O5 Tm1 138.3(4) . . ?
C8 O8 Tm2 136.7(4) . . ?
C9 O9 Tm2 133.1(5) . . ?
C10 O10 Tm2 134.5(4) . 2_565 ?
C11 O11 Tm2 134.7(5) . 1_545 ?
H13A O13 H13B 104.5 . . ?
Tm1 O13 H13A 109.6 . . ?
Tm1 O13 H13B 109.1 . . ?
H14A O14 H14B 103.2 . . ?
Tm1 O14 H14A 126.5 . . ?
Tm1 O14 H14B 105.6 . . ?
H15A O15 H15B 104.1 . . ?
Tm1 O15 H15A 127.8 . . ?
Tm1 O15 H15B 128.0 . . ?
H16A O16 H16B 104.5 . . ?
Tm1 O16 H16A 125.4 . . ?
Tm1 O16 H16B 123.4 . . ?
H17A O17 H17B 103.6 . . ?
Tm2 O17 H17A 109.8 . . ?
Tm2 O17 H17B 111.8 . . ?
H18A O18 H18B 104.3 . . ?
Tm2 O18 H18A 127.9 . . ?
Tm2 O18 H18B 127.8 . . ?
H19A O19 H19B 104.6 . . ?
Tm2 O19 H19A 129.1 . . ?
Tm2 O19 H19B 126.0 . . ?
H20A O20 H20B 104.1 . . ?
Tm2 O20 H20A 109.6 . . ?
Tm2 O20 H20B 110.4 . . ?
O1 Tm1 O3 119.7(2) . 1_565 ?
O1 Tm1 O4 74.13(18) . 2_565 ?
O1 Tm1 O5 138.6(2) . . ?
O1 Tm1 O14 74.33(19) . . ?
O3 Tm1 O4 141.7(2) 1_565 2_565 ?
O5 Tm1 O3 76.48(19) . 1_565 ?
O5 Tm1 O4 118.3(2) . 2_565 ?
O13 Tm1 O1 79.05(18) . . ?
O13 Tm1 O3 141.3(2) . 1_565 ?
O13 Tm1 O4 73.1(2) . 2_565 ?
O13 Tm1 O5 69.09(18) . . ?
O13 Tm1 O14 84.9(2) . . ?
O14 Tm1 O3 70.4(2) . 1_565 ?
O14 Tm1 O4 144.32(13) . 2_565 ?
O14 Tm1 O5 77.1(3) . . ?
O15 Tm1 O1 74.7(2) . . ?
O15 Tm1 O3 74.5(2) . 1_565 ?
O15 Tm1 O4 75.9(2) . 2_565 ?
O15 Tm1 O5 144.66(13) . . ?
O15 Tm1 O13 143.7(2) . . ?
O15 Tm1 O14 111.0(3) . . ?
O15 Tm1 O16 81.3(2) . . ?
O16 Tm1 O1 144.5(3) . . ?
O16 Tm1 O3 77.05(13) . 1_565 ?
O16 Tm1 O4 74.88(19) . 2_565 ?
O16 Tm1 O5 72.8(2) . . ?
O16 Tm1 O13 107.9(2) . . ?
O16 Tm1 O14 139.9(2) . . ?
O8 Tm2 O9 141.8(2) . . ?
O8 Tm2 O10 74.35(18) . 2_564 ?
O8 Tm2 O11 75.96(16) . 1_565 ?
O8 Tm2 O17 83.65(19) . . ?
O8 Tm2 O18 74.67(19) . . ?
O8 Tm2 O19 112.7(2) . . ?
O8 Tm2 O20 142.2(2) . . ?
O10 Tm2 O9 141.38(19) 2_564 . ?
O11 Tm2 O9 119.0(2) 1_565 . ?
O11 Tm2 O10 74.80(18) 1_565 2_564 ?
O11 Tm2 O17 74.59(19) 1_565 . ?
O17 Tm2 O9 69.02(17) . . ?
O17 Tm2 O10 145.75(13) . 2_564 ?
O18 Tm2 O9 73.4(2) . . ?
O18 Tm2 O10 120.5(3) . 2_564 ?
O18 Tm2 O11 140.7(2) . 1_565 ?
O18 Tm2 O17 76.7(3) . . ?
O19 Tm2 O9 76.34(16) . . ?
O19 Tm2 O10 75.18(19) . 2_564 ?
O19 Tm2 O11 144.8(3) . 1_565 ?
O19 Tm2 O17 138.5(2) . . ?
O19 Tm2 O18 72.0(2) . . ?
O20 Tm2 O9 74.11(19) . . ?
O20 Tm2 O10 76.6(2) . 2_564 ?
O20 Tm2 O11 73.4(2) . 1_565 ?
O20 Tm2 O17 108.6(3) . . ?
O20 Tm2 O18 142.25(16) . . ?
O20 Tm2 O19 82.1(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
C1 C2 C3 C4 -4.9(6) . . . . ?
C1 C2 C3 O3 169.1(9) . . . . ?
C1 C4 O4 Tm1 -147.8(6) . . . 2_564 ?
C2 C1 C4 C3 -4.9(6) . . . . ?
C2 C1 C4 O4 179.7(8) . . . . ?
C2 C1 O1 Tm1 140.8(7) . . . . ?
C2 C3 C4 C1 5.0(6) . . . . ?
C2 C3 C4 O4 -179.9(9) . . . . ?
C2 C3 O3 Tm1 -30.6(14) . . . 1_545 ?
C3 C4 O4 Tm1 38.9(13) . . . 2_564 ?
C4 C1 C2 C3 4.9(6) . . . . ?
C4 C1 C2 O2 -179.8(10) . . . . ?
C4 C1 O1 Tm1 -29.5(15) . . . . ?
C4 C3 O3 Tm1 141.2(7) . . . 1_545 ?
C5 C6 C7 C8 -6.2(5) . . . . ?
C5 C6 C7 O7 170.0(8) . . . . ?
C5 C8 O8 Tm2 -41.6(11) . . . . ?
C6 C5 C8 C7 -6.3(5) . . . . ?
C6 C5 C8 O8 174.3(8) . . . . ?
C6 C5 O5 Tm1 30.7(12) . . . . ?
C6 C7 C8 C5 6.2(5) . . . . ?
C6 C7 C8 O8 -174.4(7) . . . . ?
C7 C8 O8 Tm2 139.2(6) . . . . ?
C8 C5 C6 C7 6.2(5) . . . . ?
C8 C5 C6 O6 -173.3(8) . . . . ?
C8 C5 O5 Tm1 -144.7(6) . . . . ?
C9 C10 C11 C12 4.0(6) . . . . ?
C9 C10 C11 O11 -172.7(9) . . . . ?
C9 C10 O10 Tm2 -36.5(12) . . . 2_565 ?
C10 C9 C12 C11 4.1(6) . . . . ?
C10 C9 C12 O12 179.7(9) . . . . ?
C10 C9 O9 Tm2 -142.6(7) . . . . ?
C10 C11 C12 C9 -4.0(6) . . . . ?
C10 C11 C12 O12 -179.6(9) . . . . ?
C10 C11 O11 Tm2 38.8(13) . . . 1_545 ?
C11 C10 O10 Tm2 145.6(6) . . . 2_565 ?
C12 C9 C10 C11 -4.0(6) . . . . ?
C12 C9 C10 O10 177.5(8) . . . . ?
C12 C9 O9 Tm2 31.3(13) . . . . ?
C12 C11 O11 Tm2 -136.7(8) . . . 1_545 ?
O1 C1 C2 C3 -168.7(8) . . . . ?
O1 C1 C2 O2 6.6(16) . . . . ?
O1 C1 C4 C3 167.9(9) . . . . ?
O1 C1 C4 O4 -7.5(16) . . . . ?
O2 C2 C3 C4 179.7(9) . . . . ?
O2 C2 C3 O3 -6.3(17) . . . . ?
O3 C3 C4 C1 -169.3(8) . . . . ?
O3 C3 C4 O4 5.8(16) . . . . ?
O5 C5 C6 C7 -170.5(7) . . . . ?
O5 C5 C6 O6 10.0(14) . . . . ?
O5 C5 C8 C7 170.4(7) . . . . ?
O5 C5 C8 O8 -9.0(12) . . . . ?
O6 C6 C7 C8 173.3(8) . . . . ?
O6 C6 C7 O7 -10.5(15) . . . . ?
O7 C7 C8 C5 -170.3(7) . . . . ?
O7 C7 C8 O8 9.1(12) . . . . ?
O9 C9 C10 C11 171.6(8) . . . . ?
O9 C9 C10 O10 -6.9(15) . . . . ?
O9 C9 C12 C11 -171.6(8) . . . . ?
O9 C9 C12 O12 4.1(16) . . . . ?
O10 C10 C11 C12 -177.5(8) . . . . ?
O10 C10 C11 O11 5.8(15) . . . . ?
O11 C11 C12 C9 172.9(8) . . . . ?
O11 C11 C12 O12 -2.7(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.220
_oxdiff_exptl_absorpt_empirical_full_min 0.730
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.234(19)
2 0.766(19)

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_lu_sq_willow
_database_code_depnum_ccdc_archive 'CCDC 2218680'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Lu2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'lutetium(III) squarate'
_chemical_formula_moiety         'C12 H16 Lu2 O20'
_chemical_formula_sum            'C12 H16 Lu2 O20'
_chemical_formula_weight         830.19
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16Lu2O20
_chemical_oxdiff_usercomment     'willow leaf'
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'
O O 0.0106 0.0060 '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'

_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           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9151(5)
_cell_length_b                   8.1066(3)
_cell_length_c                   9.9577(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.748(4)
_cell_angle_gamma                90
_cell_volume                     956.99(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6105
_cell_measurement_temperature    297.95(10)
_cell_measurement_theta_max      32.1730
_cell_measurement_theta_min      3.5710
_shelx_estimated_absorpt_T_max   0.561
_shelx_estimated_absorpt_T_min   0.139
_exptl_absorpt_coefficient_mu    10.365
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.881
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 10 -3 0.0491
8 -10 -4 0.0305
-6 10 -1 0.0382
5 -11 -1 0.0239
2 11 -1 0.0325
2 -11 2 0.0281
-15 4 4 0.0575
13 4 -8 0.0625
14 -6 -2 0.0409
8 -10 3 0.0435
-13 -4 8 0.0724
7 -10 -2 0.0263
15 4 3 0.0668
1 11 -1 0.0315
-17 1 0 0.0577
-7 -10 3 0.0443
17 -1 1 0.0488
5 11 -3 0.0374
7 -10 1 0.0289
-2 11 3 0.0409
-3 -11 -1 0.0308

_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.063
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-7.4307 9.8605 -2.7581 -0.0022 0.0099 0.9999
8.1103 -9.5144 -4.4385 -0.1131 -0.4912 -0.8637
-6.3895 10.4730 -1.1213 -0.0645 0.1436 0.9875
5.0991 -10.8739 -0.8759 0.1287 -0.2984 -0.9457
2.0112 11.3342 -0.6255 -0.5333 0.2494 0.8083
2.2789 -11.2048 1.7349 0.3134 -0.1443 -0.9386
-15.1611 4.4996 3.6772 0.6631 0.2726 0.6971
13.4604 3.7482 -8.1203 -0.9220 -0.3839 0.0513
13.8539 -6.4236 -1.9103 -0.5064 -0.2068 -0.8371
7.9609 -9.6801 2.6579 -0.0333 -0.0091 -0.9994
-12.8518 -4.4145 8.2772 0.9162 0.3818 -0.1213
6.6017 -10.4405 -1.9106 0.0240 -0.3496 -0.9366
14.5003 4.4248 3.3271 -0.8956 0.4248 -0.1324
0.9258 11.3892 -0.8026 -0.4800 0.2321 0.8460
-16.6477 0.5900 -0.3331 0.8495 -0.1082 0.5164
-6.5492 -10.3541 2.8295 0.7557 -0.1011 -0.6471
16.5187 -1.3509 0.5446 -0.8124 0.1031 -0.5738
5.1315 10.6832 -2.9358 -0.6944 0.0934 0.7135
6.5753 -10.4675 0.5646 0.0494 -0.1806 -0.9823
-2.3173 11.0316 3.2532 -0.2587 0.4821 0.8371
-3.3632 -11.1552 -0.8293 0.5842 -0.3529 -0.7309

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8950
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.727
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.95(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  52.00   0.50    0.20    --   -4.52  40.00  43.00  126
  2  ω    -38.00   0.00   0.50    0.20    --   -4.52   0.00-120.00   76
  3  ω    -75.00 -13.00   0.50    0.20    --   -4.52 -40.00-109.00  124
  4  ω    -42.00  -5.00   0.50    0.20    --   -4.52 -38.00-180.00   74
  5  ω     -1.00  34.00   0.50    0.20    --    3.74 -99.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525333000
_diffrn_orient_matrix_UB_12      -0.0372179000
_diffrn_orient_matrix_UB_13      0.0092787000
_diffrn_orient_matrix_UB_21      0.0060020000
_diffrn_orient_matrix_UB_22      0.0247245000
_diffrn_orient_matrix_UB_23      0.0686320000
_diffrn_orient_matrix_UB_31      -0.0279892000
_diffrn_orient_matrix_UB_32      0.0752942000
_diffrn_orient_matrix_UB_33      -0.0179583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                3441
_reflns_number_total             4006
_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       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(3)
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.005
_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)+(0.0573P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.59(3)
 0.41(3)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Lu1-H16A \\sim Lu1-H16B
 with sigma of 0.02
 Lu1-H14A \\sim Lu1-H14B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_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 0.74429(2) 0.24478(3) 0.32109(2) 0.0141(2) Uani 1 1 d D . . . .
Lu2 Lu 0.25515(3) 0.25175(3) 0.55672(3) 0.01324(19) Uani 1 1 d . . . . .
O1 O 0.8523(9) 0.4840(8) 0.3376(10) 0.0275(19) Uani 1 1 d . . . . .
O2 O 0.9316(9) 0.8396(8) 0.2354(10) 0.029(2) Uani 1 1 d . . . . .
O3 O 0.7961(9) 1.0160(8) 0.4631(9) 0.0178(18) Uani 1 1 d . . . . .
O4 O 0.7522(10) 0.6587(8) 0.5933(9) 0.025(2) Uani 1 1 d . . . . .
O5 O 0.5682(9) 0.1492(8) 0.3810(11) 0.027(2) Uani 1 1 d . . . . .
O6 O 0.5973(8) -0.2337(7) 0.3042(8) 0.0232(16) Uani 1 1 d . . . . .
O7 O 0.4489(8) -0.3368(8) 0.5515(9) 0.0329(19) Uani 1 1 d . . . . .
O8 O 0.3774(8) 0.0389(8) 0.5804(9) 0.0254(17) Uani 1 1 d . . . . .
O9 O 0.2069(9) 0.4859(8) 0.4140(9) 0.0216(19) Uani 1 1 d . . . . .
O10 O 0.2476(9) 0.8444(7) 0.2804(9) 0.0201(18) Uani 1 1 d . . . . .
O11 O 0.1388(8) 1.0167(7) 0.5369(10) 0.0241(17) Uani 1 1 d . . . . .
O12 O 0.0706(9) 0.6609(8) 0.6406(10) 0.023(2) Uani 1 1 d . . . . .
O13 O 0.6072(8) 0.4435(8) 0.2807(10) 0.0291(18) Uani 1 1 d . . . . .
H13A H 0.6300 0.5200 0.2306 0.044 Uiso 1 1 d R U . . .
H13B H 0.5500 0.4022 0.2331 0.044 Uiso 1 1 d R U . . .
O14 O 0.7516(12) 0.3243(9) 0.5436(10) 0.039(3) Uani 1 1 d . . . . .
H14A H 0.6896 0.3741 0.5578 0.059 Uiso 1 1 d DR U . . .
H14B H 0.8029 0.3989 0.5612 0.059 Uiso 1 1 d DR U . . .
O15 O 0.9187(9) 0.1684(9) 0.2708(11) 0.028(2) Uani 1 1 d G . . . .
H15A H 0.9686 0.2321 0.2461 0.042 Uiso 1 1 d G U . . .
H15B H 0.9540 0.0813 0.2929 0.042 Uiso 1 1 d G U . . .
O16 O 0.6925(9) 0.0253(9) 0.1864(9) 0.0225(19) Uani 1 1 d G . . . .
H16A H 0.7387 -0.0208 0.1404 0.034 Uiso 1 1 d DG U . . .
H16B H 0.6549 -0.0524 0.2153 0.034 Uiso 1 1 d DG U . . .
O17 O 0.2434(10) 0.1791(7) 0.3260(11) 0.0289(17) Uani 1 1 d . . . . .
H17A H 0.2398 0.0743 0.3178 0.043 Uiso 1 1 d R U . . .
H17B H 0.1813 0.2124 0.2828 0.043 Uiso 1 1 d R U . . .
O18 O 0.4213(9) 0.3524(8) 0.4848(11) 0.031(2) Uani 1 1 d G . . . .
H18A H 0.4458 0.4482 0.5006 0.046 Uiso 1 1 d G U . . .
H18B H 0.4725 0.3061 0.4464 0.046 Uiso 1 1 d G U . . .
O19 O 0.3112(10) 0.4733(8) 0.6908(10) 0.0252(19) Uani 1 1 d G . . . .
H19A H 0.2939 0.5049 0.7659 0.038 Uiso 1 1 d G U . . .
H19B H 0.3545 0.5472 0.6667 0.038 Uiso 1 1 d G U . . .
O20 O 0.0806(9) 0.3334(8) 0.6043(10) 0.027(2) Uani 1 1 d . . . . .
H20A H 0.0816 0.4364 0.6222 0.041 Uiso 1 1 d R U . . .
H20B H 0.0643 0.2886 0.6774 0.041 Uiso 1 1 d R U . . .
C1 C 0.8481(11) 0.6276(11) 0.3829(13) 0.019(2) Uani 1 1 d . U . . .
C2 C 0.8816(11) 0.7902(13) 0.3332(12) 0.018(2) Uani 1 1 d . U . . .
C3 C 0.8253(11) 0.8724(11) 0.4378(12) 0.018(2) Uani 1 1 d . U . . .
C4 C 0.8008(10) 0.7120(13) 0.4951(11) 0.0178(19) Uani 1 1 d . U . . .
C5 C 0.5257(8) 0.0128(9) 0.4186(9) 0.0190(16) Uani 1 1 d . . . . .
C6 C 0.5453(10) -0.1585(10) 0.3873(11) 0.0199(19) Uani 1 1 d . . . . .
C7 C 0.4732(9) -0.2049(11) 0.4918(10) 0.0223(17) Uani 1 1 d . . . . .
C8 C 0.4438(8) -0.0319(8) 0.5123(9) 0.0200(17) Uani 1 1 d . . . . .
C9 C 0.1796(10) 0.6327(10) 0.4387(12) 0.0136(19) Uani 1 1 d . U . . .
C10 C 0.2008(10) 0.7951(12) 0.3811(11) 0.0173(19) Uani 1 1 d . U . . .
C11 C 0.1490(11) 0.8748(11) 0.4931(12) 0.017(2) Uani 1 1 d . U . . .
C12 C 0.1196(11) 0.7125(14) 0.5441(12) 0.0169(19) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O1 2.324(8) . ?
Lu1 O3 2.376(7) 1_545 ?
Lu1 O4 2.410(9) 2_564 ?
Lu1 O5 2.368(10) . ?
Lu1 O13 2.301(8) . ?
Lu1 O14 2.301(10) . ?
Lu1 O15 2.272(10) . ?
Lu1 O16 2.276(8) . ?
Lu2 O8 2.255(8) . ?
Lu2 O9 2.406(8) . ?
Lu2 O10 2.370(8) 2_565 ?
Lu2 O11 2.353(8) 1_545 ?
Lu2 O17 2.362(11) . ?
Lu2 O18 2.319(10) . ?
Lu2 O19 2.297(8) . ?
Lu2 O20 2.277(10) . ?
O1 C1 1.252(11) . ?
O2 C2 1.257(14) . ?
O3 Lu1 2.376(7) 1_565 ?
O3 C3 1.248(11) . ?
O4 Lu1 2.410(9) 2_565 ?
O4 C4 1.261(13) . ?
O5 C5 1.288(10) . ?
O6 C6 1.242(12) . ?
O7 C7 1.271(10) . ?
O8 C8 1.234(10) . ?
O9 C9 1.264(11) . ?
O10 Lu2 2.370(8) 2_564 ?
O10 C10 1.261(11) . ?
O11 Lu2 2.353(8) 1_565 ?
O11 C11 1.240(11) . ?
O12 C12 1.246(13) . ?
O13 H13A 0.8565 . ?
O13 H13B 0.8576 . ?
O14 H14A 0.8655 . ?
O14 H14B 0.8652 . ?
O15 H15A 0.8430 . ?
O15 H15B 0.8395 . ?
O16 H16A 0.8382 . ?
O16 H16B 0.8401 . ?
O17 H17A 0.8540 . ?
O17 H17B 0.8615 . ?
O18 H18A 0.8389 . ?
O18 H18B 0.8407 . ?
O19 H19A 0.8357 . ?
O19 H19B 0.8414 . ?
O20 H20A 0.8529 . ?
O20 H20B 0.8534 . ?
C1 C2 1.476(14) . ?
C1 C4 1.470(14) . ?
C2 C3 1.456(15) . ?
C3 C4 1.461(13) . ?
C5 C6 1.447(11) . ?
C5 C8 1.461(11) . ?
C6 C7 1.463(13) . ?
C7 C8 1.465(11) . ?
C9 C10 1.468(12) . ?
C9 C12 1.477(14) . ?
C10 C11 1.476(15) . ?
C11 C12 1.466(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Lu1 O3 120.0(4) . 1_545 ?
O1 Lu1 O4 73.9(3) . 2_564 ?
O1 Lu1 O5 138.9(3) . . ?
O3 Lu1 O4 141.4(3) 1_545 2_564 ?
O5 Lu1 O3 77.2(3) . 1_545 ?
O5 Lu1 O4 117.5(4) . 2_564 ?
O13 Lu1 O1 78.9(3) . . ?
O13 Lu1 O3 142.0(4) . 1_545 ?
O13 Lu1 O4 72.7(3) . 2_564 ?
O13 Lu1 O5 69.0(3) . . ?
O13 Lu1 O14 86.0(4) . . ?
O14 Lu1 O1 74.4(3) . . ?
O14 Lu1 O3 70.3(3) . 1_545 ?
O14 Lu1 O4 144.5(2) . 2_564 ?
O14 Lu1 O5 78.4(4) . . ?
O15 Lu1 O1 74.4(3) . . ?
O15 Lu1 O3 74.3(3) . 1_545 ?
O15 Lu1 O4 76.0(4) . 2_564 ?
O15 Lu1 O5 145.0(2) . . ?
O15 Lu1 O13 143.3(3) . . ?
O15 Lu1 O14 110.0(5) . . ?
O15 Lu1 O16 81.8(4) . . ?
O16 Lu1 O1 144.0(4) . . ?
O16 Lu1 O3 77.2(2) . 1_545 ?
O16 Lu1 O4 74.5(3) . 2_564 ?
O16 Lu1 O5 72.4(3) . . ?
O16 Lu1 O13 107.4(4) . . ?
O16 Lu1 O14 140.2(3) . . ?
O8 Lu2 O9 141.2(4) . . ?
O8 Lu2 O10 74.6(3) . 2_565 ?
O8 Lu2 O11 76.0(3) . 1_545 ?
O8 Lu2 O17 83.4(3) . . ?
O8 Lu2 O18 74.9(3) . . ?
O8 Lu2 O19 113.0(4) . . ?
O8 Lu2 O20 142.6(3) . . ?
O10 Lu2 O9 141.8(3) 2_565 . ?
O11 Lu2 O9 119.0(4) 1_545 . ?
O11 Lu2 O10 74.6(3) 1_545 2_565 ?
O11 Lu2 O17 74.9(3) 1_545 . ?
O17 Lu2 O9 68.6(3) . . ?
O17 Lu2 O10 145.9(2) . 2_565 ?
O18 Lu2 O9 72.6(3) . . ?
O18 Lu2 O10 121.3(4) . 2_565 ?
O18 Lu2 O11 140.6(3) . 1_545 ?
O18 Lu2 O17 75.9(4) . . ?
O19 Lu2 O9 76.4(2) . . ?
O19 Lu2 O10 75.3(3) . 2_565 ?
O19 Lu2 O11 144.7(4) . 1_545 ?
O19 Lu2 O17 138.2(3) . . ?
O19 Lu2 O18 72.4(3) . . ?
O20 Lu2 O9 74.0(3) . . ?
O20 Lu2 O10 77.2(3) . 2_565 ?
O20 Lu2 O11 73.2(3) . 1_545 ?
O20 Lu2 O17 108.0(4) . . ?
O20 Lu2 O18 141.9(3) . . ?
O20 Lu2 O19 82.5(3) . . ?
C1 O1 Lu1 139.4(8) . . ?
C3 O3 Lu1 132.0(7) . 1_565 ?
C4 O4 Lu1 133.0(7) . 2_565 ?
C5 O5 Lu1 137.6(6) . . ?
C8 O8 Lu2 137.8(6) . . ?
C9 O9 Lu2 132.7(7) . . ?
C10 O10 Lu2 134.8(6) . 2_564 ?
C11 O11 Lu2 134.6(8) . 1_565 ?
Lu1 O13 H13A 110.3 . . ?
Lu1 O13 H13B 109.5 . . ?
H13A O13 H13B 104.0 . . ?
Lu1 O14 H14A 109.7 . . ?
Lu1 O14 H14B 110.4 . . ?
H14A O14 H14B 103.8 . . ?
Lu1 O15 H15A 125.8 . . ?
Lu1 O15 H15B 128.1 . . ?
H15A O15 H15B 104.0 . . ?
Lu1 O16 H16A 121.1 . . ?
Lu1 O16 H16B 120.5 . . ?
H16A O16 H16B 104.8 . . ?
Lu2 O17 H17A 109.8 . . ?
Lu2 O17 H17B 111.9 . . ?
H17A O17 H17B 103.3 . . ?
Lu2 O18 H18A 124.0 . . ?
Lu2 O18 H18B 131.6 . . ?
H18A O18 H18B 104.1 . . ?
Lu2 O19 H19A 132.5 . . ?
Lu2 O19 H19B 122.8 . . ?
H19A O19 H19B 104.6 . . ?
Lu2 O20 H20A 109.5 . . ?
Lu2 O20 H20B 110.2 . . ?
H20A O20 H20B 103.8 . . ?
O1 C1 C2 133.5(11) . . ?
O1 C1 C4 137.7(11) . . ?
C4 C1 C2 88.6(7) . . ?
O2 C2 C1 135.2(10) . . ?
O2 C2 C3 134.1(10) . . ?
C3 C2 C1 90.6(8) . . ?
O3 C3 C2 136.8(11) . . ?
O3 C3 C4 132.9(11) . . ?
C2 C3 C4 89.8(8) . . ?
O4 C4 C1 132.1(10) . . ?
O4 C4 C3 137.1(10) . . ?
C3 C4 C1 90.6(8) . . ?
O5 C5 C6 133.2(8) . . ?
O5 C5 C8 134.9(7) . . ?
C6 C5 C8 91.8(6) . . ?
O6 C6 C5 135.7(8) . . ?
O6 C6 C7 135.6(8) . . ?
C5 C6 C7 88.6(7) . . ?
O7 C7 C6 136.7(9) . . ?
O7 C7 C8 132.1(8) . . ?
C6 C7 C8 91.0(7) . . ?
O8 C8 C5 137.9(7) . . ?
O8 C8 C7 134.2(8) . . ?
C5 C8 C7 87.9(6) . . ?
O9 C9 C10 135.3(10) . . ?
O9 C9 C12 134.7(10) . . ?
C10 C9 C12 89.9(7) . . ?
O10 C10 C9 134.5(10) . . ?
O10 C10 C11 135.6(9) . . ?
C9 C10 C11 89.8(7) . . ?
O11 C11 C10 137.3(10) . . ?
O11 C11 C12 132.5(11) . . ?
C12 C11 C10 90.1(7) . . ?
O12 C12 C9 134.3(10) . . ?
O12 C12 C11 135.7(10) . . ?
C11 C12 C9 89.8(8) . . ?

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 O1 C1 C2 -140.6(12) . . . . ?
Lu1 O1 C1 C4 32(2) . . . . ?
Lu1 O3 C3 C2 29(2) 1_565 . . . ?
Lu1 O3 C3 C4 -140.7(11) 1_565 . . . ?
Lu1 O4 C4 C1 148.7(10) 2_565 . . . ?
Lu1 O4 C4 C3 -38(2) 2_565 . . . ?
Lu1 O5 C5 C6 -33.0(19) . . . . ?
Lu1 O5 C5 C8 143.8(9) . . . . ?
Lu2 O8 C8 C5 40.8(19) . . . . ?
Lu2 O8 C8 C7 -138.8(9) . . . . ?
Lu2 O9 C9 C10 143.6(10) . . . . ?
Lu2 O9 C9 C12 -31(2) . . . . ?
Lu2 O10 C10 C9 37.9(18) 2_564 . . . ?
Lu2 O10 C10 C11 -145.4(10) 2_564 . . . ?
Lu2 O11 C11 C10 -37(2) 1_565 . . . ?
Lu2 O11 C11 C12 136.9(11) 1_565 . . . ?
O1 C1 C2 O2 -6(3) . . . . ?
O1 C1 C2 C3 170.2(13) . . . . ?
O1 C1 C4 O4 6(2) . . . . ?
O1 C1 C4 C3 -169.8(14) . . . . ?
O2 C2 C3 O3 8(3) . . . . ?
O2 C2 C3 C4 -179.2(15) . . . . ?
O3 C3 C4 O4 -7(2) . . . . ?
O3 C3 C4 C1 167.9(13) . . . . ?
O5 C5 C6 O6 -11(2) . . . . ?
O5 C5 C6 C7 171.8(11) . . . . ?
O5 C5 C8 O8 9(2) . . . . ?
O5 C5 C8 C7 -171.7(12) . . . . ?
O6 C6 C7 O7 13(2) . . . . ?
O6 C6 C7 C8 -171.8(13) . . . . ?
O7 C7 C8 O8 -10.2(19) . . . . ?
O7 C7 C8 C5 170.0(10) . . . . ?
O9 C9 C10 O10 6(2) . . . . ?
O9 C9 C10 C11 -171.9(12) . . . . ?
O9 C9 C12 O12 -4(2) . . . . ?
O9 C9 C12 C11 172.0(12) . . . . ?
O10 C10 C11 O11 -7(2) . . . . ?
O10 C10 C11 C12 177.9(12) . . . . ?
O11 C11 C12 O12 5(2) . . . . ?
O11 C11 C12 C9 -171.5(12) . . . . ?
C1 C2 C3 O3 -167.5(14) . . . . ?
C1 C2 C3 C4 4.9(10) . . . . ?
C2 C1 C4 O4 -179.5(13) . . . . ?
C2 C1 C4 C3 4.8(10) . . . . ?
C2 C3 C4 O4 179.8(14) . . . . ?
C2 C3 C4 C1 -4.9(10) . . . . ?
C4 C1 C2 O2 179.3(15) . . . . ?
C4 C1 C2 C3 -4.8(10) . . . . ?
C5 C6 C7 O7 -169.6(11) . . . . ?
C5 C6 C7 C8 5.9(7) . . . . ?
C6 C5 C8 O8 -173.8(13) . . . . ?
C6 C5 C8 C7 5.9(7) . . . . ?
C6 C7 C8 O8 173.9(12) . . . . ?
C6 C7 C8 C5 -5.8(7) . . . . ?
C8 C5 C6 O6 171.7(13) . . . . ?
C8 C5 C6 C7 -5.9(7) . . . . ?
C9 C10 C11 O11 171.1(13) . . . . ?
C9 C10 C11 C12 -4.4(9) . . . . ?
C10 C9 C12 O12 179.3(14) . . . . ?
C10 C9 C12 C11 -4.4(9) . . . . ?
C10 C11 C12 O12 -179.4(14) . . . . ?
C10 C11 C12 C9 4.4(9) . . . . ?
C12 C9 C10 O10 -177.9(12) . . . . ?
C12 C9 C10 C11 4.4(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.769
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.59(3)
2 0.41(3)

####################################################################### 
# 
# 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_gd_sq_rtcl_syn20210906_a_autored
_database_code_depnum_ccdc_archive 'CCDC 2218674'
loop_
_audit_author_name
_audit_author_address
'Takayuki Ishida'
;The University of ElectroCommunications
Japan
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_audit_creation_date             2022-11-09
_audit_creation_method           
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            '[Gd2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'gadolinium(III) squarate'
_chemical_formula_moiety         'C12 H16 Gd2 O20'
_chemical_formula_sum            'C12 H16 Gd2 O20'
_chemical_formula_weight         794.75
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H16Gd2O20
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   11.9359(7)
_cell_length_b                   8.1994(4)
_cell_length_c                   10.0894(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.928(5)
_cell_angle_gamma                90
_cell_volume                     982.14(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3059
_cell_measurement_temperature    295.40(14)
_cell_measurement_theta_max      30.5170
_cell_measurement_theta_min      2.4530
_shelx_estimated_absorpt_T_max   0.759
_shelx_estimated_absorpt_T_min   0.188
_exptl_absorpt_coefficient_mu    6.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.687
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
17 1 0 0.0324
7 10 -4 0.0853
0 0 14 0.0524
0 0 -14 0.0717
-7 -10 4 0.0710
-16 0 -1 0.0398
16 0 3 0.0184

_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.043
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
16.6729 0.6982 0.2039 0.9976 0.0698 -0.0000
7.1050 10.1748 -3.8186 0.3883 0.7962 -0.4640
0.2856 0.1613 14.1171 0.1204 0.2469 0.9615
-0.4872 -0.4487 -14.0848 -0.1320 -0.2707 -0.9536
-7.0096 -10.0507 4.4842 -0.3778 -0.7747 0.5070
-16.4473 -0.4501 -1.4562 -0.9935 -0.0695 -0.0905
16.0088 0.1534 2.9145 0.9782 0.0684 0.1961

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9785
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.637
_diffrn_reflns_theta_min         2.484
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.40(14)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  -6.00   0.50    8.90    --    5.00  45.00 120.00   52
  2  ω    -45.00 -19.00   0.50    8.90    --    5.00  45.00   0.00   52
  3  ω     28.00  65.00   0.50    8.90    --  -11.00  45.00 120.00   74
  4  ω    -88.00  -8.00   0.50    8.90    --  -11.00  45.00 120.00  160
  5  ω   -100.00  78.00   0.50    8.90    --  -11.00  45.00 165.01  356
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0597765000
_diffrn_orient_matrix_UB_12      -0.0008249000
_diffrn_orient_matrix_UB_13      0.0073308000
_diffrn_orient_matrix_UB_21      0.0004588000
_diffrn_orient_matrix_UB_22      0.0841302000
_diffrn_orient_matrix_UB_23      0.0165203000
_diffrn_orient_matrix_UB_31      0.0000001000
_diffrn_orient_matrix_UB_32      -0.0199564000
_diffrn_orient_matrix_UB_33      0.0683387000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                3462
_reflns_number_total             3976
_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       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    
'olex2.solve 1.5-ac5-018 (Bourhis et al., 2015)'
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(3)
_refine_ls_extinction_coef       0.0030(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3976
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0234
_refine_ls_restrained_S_all      1.023
_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)+(0.0202P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0565
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.83(3)
 0.17(3)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Gd1-H16A \\sim Gd1-H16B
 with sigma of 0.02
 Gd2-H18A \\sim Gd2-H18B
 with sigma of 0.02
 Gd1-H15A \\sim Gd1-H15B
 with sigma of 0.02
 Gd2-H19A \\sim Gd2-H19B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O17(H17A,H17B), O20(H20A,H20B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8509(9) 0.6308(10) 0.3841(11) 0.019(2) Uani 1 1 d . U . . .
C2 C 0.8825(9) 0.7917(11) 0.3368(11) 0.0164(18) Uani 1 1 d . U . . .
C3 C 0.8262(9) 0.8698(9) 0.4408(10) 0.0138(19) Uani 1 1 d . U . . .
C4 C 0.8021(8) 0.7112(11) 0.4956(10) 0.0155(18) Uani 1 1 d . U . . .
C5 C 0.5262(6) 0.0101(7) 0.4179(7) 0.0211(14) Uani 1 1 d . . . . .
C6 C 0.5453(7) -0.1614(8) 0.3871(9) 0.0182(17) Uani 1 1 d . . . . .
C7 C 0.4735(6) -0.2057(8) 0.4906(8) 0.0196(14) Uani 1 1 d . . . . .
C8 C 0.4458(6) -0.0363(7) 0.5117(7) 0.0201(14) Uani 1 1 d . . . . .
C9 C 0.1779(9) 0.6327(9) 0.4380(10) 0.0158(19) Uani 1 1 d . U . . .
C10 C 0.2008(8) 0.7923(11) 0.3827(10) 0.0162(18) Uani 1 1 d . U . . .
C11 C 0.1490(8) 0.8724(9) 0.4896(10) 0.0131(19) Uani 1 1 d . U . . .
C12 C 0.1197(9) 0.7123(11) 0.5423(10) 0.0158(19) Uani 1 1 d . U . . .
O1 O 0.8538(6) 0.4887(6) 0.3421(7) 0.0240(15) Uani 1 1 d . . . . .
O2 O 0.9330(7) 0.8391(7) 0.2415(8) 0.0284(18) Uani 1 1 d . . . . .
O3 O 0.7986(7) 1.0145(6) 0.4649(7) 0.0186(15) Uani 1 1 d . . . . .
O4 O 0.7534(7) 0.6609(6) 0.5933(7) 0.0203(15) Uani 1 1 d . . . . .
O5 O 0.5667(6) 0.1448(6) 0.3821(8) 0.0246(16) Uani 1 1 d . . . . .
O6 O 0.5964(5) -0.2341(5) 0.3055(6) 0.0241(12) Uani 1 1 d . . . . .
O7 O 0.4479(6) -0.3364(6) 0.5470(7) 0.0309(16) Uani 1 1 d . . . . .
O8 O 0.3806(6) 0.0360(6) 0.5809(7) 0.0248(14) Uani 1 1 d . . . . .
O9 O 0.2040(7) 0.4875(6) 0.4120(7) 0.0191(15) Uani 1 1 d . . . . .
O10 O 0.2469(7) 0.8424(6) 0.2839(7) 0.0217(15) Uani 1 1 d . . . . .
O11 O 0.1366(6) 1.0133(6) 0.5329(7) 0.0231(13) Uani 1 1 d . . . . .
O12 O 0.0719(7) 0.6623(6) 0.6370(8) 0.0235(16) Uani 1 1 d . . . . .
O13 O 0.6017(6) 0.4467(6) 0.2769(7) 0.0260(14) Uani 1 1 d . . . . .
H13A H 0.6321 0.5392 0.2646 0.039 Uiso 1 1 d R U . . .
H13B H 0.5630 0.4260 0.2024 0.039 Uiso 1 1 d R U . . .
O14 O 0.7456(11) 0.3304(7) 0.5496(9) 0.057(3) Uani 1 1 d G . . . .
H14A H 0.7259 0.4230 0.5775 0.085 Uiso 1 1 d G U . . .
H14B H 0.7737 0.2809 0.6197 0.085 Uiso 1 1 d G U . . .
O15 O 0.9246(6) 0.1658(7) 0.2670(9) 0.0278(17) Uani 1 1 d G . . . .
H15A H 0.9726 0.2243 0.2326 0.042 Uiso 1 1 d DG U . . .
H15B H 0.9499 0.0693 0.2628 0.042 Uiso 1 1 d DG U . . .
O16 O 0.6929(7) 0.0162(7) 0.1857(8) 0.0236(16) Uani 1 1 d G . . . .
H16A H 0.7321 -0.0149 0.1249 0.035 Uiso 1 1 d DG U . . .
H16B H 0.6719 -0.0715 0.2204 0.035 Uiso 1 1 d DG U . . .
O17 O 0.2441(8) 0.1766(5) 0.3232(8) 0.0308(14) Uani 1 1 d . . . . .
H17A H 0.2450 0.0720 0.3156 0.046 Uiso 1 1 d R U . . .
H17B H 0.1803 0.2044 0.2812 0.046 Uiso 1 1 d R U . . .
O18 O 0.4253(7) 0.3542(6) 0.4860(9) 0.0300(18) Uani 1 1 d G . . . .
H18A H 0.4419 0.4528 0.4721 0.045 Uiso 1 1 d DG U . . .
H18B H 0.4767 0.2998 0.4542 0.045 Uiso 1 1 d DG U . . .
O19 O 0.3125(7) 0.4802(7) 0.6930(7) 0.0246(16) Uani 1 1 d G . . . .
H19A H 0.3010 0.4985 0.7730 0.037 Uiso 1 1 d DG U . . .
H19B H 0.3543 0.5582 0.6730 0.037 Uiso 1 1 d DG U . . .
O20 O 0.0751(7) 0.3372(7) 0.6081(8) 0.0279(17) Uani 1 1 d . . . . .
H20A H 0.0784 0.4364 0.6357 0.042 Uiso 1 1 d R U . . .
H20B H 0.0553 0.2831 0.6748 0.042 Uiso 1 1 d R U . . .
Gd1 Gd 0.74546(2) 0.24464(3) 0.32152(2) 0.01334(18) Uani 1 1 d D . . . .
Gd2 Gd 0.25399(2) 0.25141(3) 0.55636(3) 0.01282(18) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.465(11) . ?
C1 C4 1.475(12) . ?
C1 O1 1.242(10) . ?
C2 C3 1.452(12) . ?
C2 O2 1.249(11) . ?
C3 C4 1.453(10) . ?
C3 O3 1.262(9) . ?
C4 O4 1.264(11) . ?
C5 C6 1.463(9) . ?
C5 C8 1.466(8) . ?
C5 O5 1.273(8) . ?
C6 C7 1.464(10) . ?
C6 O6 1.228(9) . ?
C7 C8 1.449(9) . ?
C7 O7 1.265(8) . ?
C8 O8 1.248(8) . ?
C9 C10 1.459(11) . ?
C9 C12 1.472(12) . ?
C9 O9 1.265(9) . ?
C10 C11 1.454(12) . ?
C10 O10 1.257(11) . ?
C11 C12 1.472(11) . ?
C11 O11 1.249(9) . ?
C12 O12 1.233(11) . ?
O1 Gd1 2.380(6) . ?
O3 Gd1 2.422(6) 1_565 ?
O4 Gd1 2.441(7) 2_565 ?
O5 Gd1 2.422(7) . ?
O8 Gd2 2.321(6) . ?
O9 Gd2 2.459(6) . ?
O10 Gd2 2.431(6) 2_564 ?
O11 Gd2 2.400(6) 1_565 ?
O13 H13A 0.8556 . ?
O13 H13B 0.8574 . ?
O13 Gd1 2.394(6) . ?
O14 H14A 0.8519 . ?
O14 H14B 0.8527 . ?
O14 Gd1 2.406(9) . ?
O15 H15A 0.8487 . ?
O15 H15B 0.8488 . ?
O15 Gd1 2.353(7) . ?
O16 H16A 0.8484 . ?
O16 H16B 0.8486 . ?
O16 Gd1 2.367(7) . ?
O17 H17A 0.8614 . ?
O17 H17B 0.8630 . ?
O17 Gd2 2.422(8) . ?
O18 H18A 0.8480 . ?
O18 H18B 0.8477 . ?
O18 Gd2 2.387(7) . ?
O19 H19A 0.8458 . ?
O19 H19B 0.8484 . ?
O19 Gd2 2.389(6) . ?
O20 H20A 0.8593 . ?
O20 H20B 0.8598 . ?
O20 Gd2 2.357(7) . ?
Gd1 O3 2.422(6) 1_545 ?
Gd1 O4 2.441(7) 2_564 ?
Gd2 O10 2.430(6) 2_565 ?
Gd2 O11 2.400(6) 1_545 ?

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
C2 C1 C4 88.9(7) . . ?
O1 C1 C2 135.8(10) . . ?
O1 C1 C4 135.0(9) . . ?
C3 C2 C1 90.5(7) . . ?
O2 C2 C1 133.7(10) . . ?
O2 C2 C3 135.7(9) . . ?
C2 C3 C4 90.3(7) . . ?
O3 C3 C2 134.7(9) . . ?
O3 C3 C4 134.6(9) . . ?
C3 C4 C1 90.0(7) . . ?
O4 C4 C1 134.3(8) . . ?
O4 C4 C3 135.5(9) . . ?
C6 C5 C8 90.8(5) . . ?
O5 C5 C6 134.5(6) . . ?
O5 C5 C8 134.6(6) . . ?
C5 C6 C7 88.4(5) . . ?
O6 C6 C5 135.1(7) . . ?
O6 C6 C7 136.5(6) . . ?
C8 C7 C6 91.5(5) . . ?
O7 C7 C6 135.9(7) . . ?
O7 C7 C8 132.6(7) . . ?
C7 C8 C5 88.8(5) . . ?
O8 C8 C5 136.5(6) . . ?
O8 C8 C7 134.6(6) . . ?
C10 C9 C12 89.8(7) . . ?
O9 C9 C10 134.8(9) . . ?
O9 C9 C12 135.3(9) . . ?
C11 C10 C9 90.6(7) . . ?
O10 C10 C9 135.3(9) . . ?
O10 C10 C11 134.1(8) . . ?
C10 C11 C12 90.0(7) . . ?
O11 C11 C10 138.8(9) . . ?
O11 C11 C12 131.1(9) . . ?
C11 C12 C9 89.4(7) . . ?
O12 C12 C9 134.2(8) . . ?
O12 C12 C11 136.3(9) . . ?
C1 O1 Gd1 141.7(6) . . ?
C3 O3 Gd1 132.5(6) . 1_565 ?
C4 O4 Gd1 134.2(6) . 2_565 ?
C5 O5 Gd1 137.4(5) . . ?
C8 O8 Gd2 137.6(5) . . ?
C9 O9 Gd2 131.9(6) . . ?
C10 O10 Gd2 134.9(5) . 2_564 ?
C11 O11 Gd2 134.2(6) . 1_565 ?
H13A O13 H13B 104.3 . . ?
Gd1 O13 H13A 109.5 . . ?
Gd1 O13 H13B 109.8 . . ?
H14A O14 H14B 104.4 . . ?
Gd1 O14 H14A 127.2 . . ?
Gd1 O14 H14B 128.0 . . ?
H15A O15 H15B 104.3 . . ?
Gd1 O15 H15A 127.5 . . ?
Gd1 O15 H15B 127.2 . . ?
H16A O16 H16B 104.6 . . ?
Gd1 O16 H16A 121.5 . . ?
Gd1 O16 H16B 120.2 . . ?
H17A O17 H17B 103.8 . . ?
Gd2 O17 H17A 109.8 . . ?
Gd2 O17 H17B 111.2 . . ?
H18A O18 H18B 104.4 . . ?
Gd2 O18 H18A 127.4 . . ?
Gd2 O18 H18B 127.0 . . ?
H19A O19 H19B 104.5 . . ?
Gd2 O19 H19A 128.5 . . ?
Gd2 O19 H19B 126.8 . . ?
H20A O20 H20B 104.0 . . ?
Gd2 O20 H20A 110.0 . . ?
Gd2 O20 H20B 110.3 . . ?
O1 Gd1 O3 119.8(3) . 1_545 ?
O1 Gd1 O4 75.0(2) . 2_564 ?
O1 Gd1 O5 138.3(2) . . ?
O1 Gd1 O13 78.9(2) . . ?
O1 Gd1 O14 74.0(2) . . ?
O3 Gd1 O4 141.0(2) 1_545 2_564 ?
O3 Gd1 O5 76.6(2) 1_545 . ?
O5 Gd1 O4 117.8(3) . 2_564 ?
O13 Gd1 O3 142.2(3) . 1_545 ?
O13 Gd1 O4 72.5(2) . 2_564 ?
O13 Gd1 O5 69.4(2) . . ?
O13 Gd1 O14 84.7(3) . . ?
O14 Gd1 O3 71.5(2) . 1_545 ?
O14 Gd1 O4 144.42(15) . 2_564 ?
O14 Gd1 O5 76.8(3) . . ?
O15 Gd1 O1 75.7(2) . . ?
O15 Gd1 O3 74.8(2) . 1_545 ?
O15 Gd1 O4 75.1(3) . 2_564 ?
O15 Gd1 O5 144.25(16) . . ?
O15 Gd1 O13 142.9(2) . . ?
O15 Gd1 O14 113.1(4) . . ?
O15 Gd1 O16 80.8(3) . . ?
O16 Gd1 O1 145.6(3) . . ?
O16 Gd1 O3 76.51(16) . 1_545 ?
O16 Gd1 O4 74.9(2) . 2_564 ?
O16 Gd1 O5 72.0(2) . . ?
O16 Gd1 O13 107.3(3) . . ?
O16 Gd1 O14 139.4(3) . . ?
O8 Gd2 O9 141.1(3) . . ?
O8 Gd2 O10 75.2(2) . 2_565 ?
O8 Gd2 O11 76.0(2) . 1_545 ?
O8 Gd2 O17 82.9(2) . . ?
O8 Gd2 O18 74.5(2) . . ?
O8 Gd2 O19 112.8(3) . . ?
O8 Gd2 O20 142.9(2) . . ?
O10 Gd2 O9 141.1(2) 2_565 . ?
O11 Gd2 O9 118.6(3) 1_545 . ?
O11 Gd2 O10 76.1(2) 1_545 2_565 ?
O11 Gd2 O17 74.3(2) 1_545 . ?
O17 Gd2 O9 68.9(2) . . ?
O17 Gd2 O10 146.53(15) . 2_565 ?
O18 Gd2 O9 73.1(2) . . ?
O18 Gd2 O10 120.5(3) . 2_565 ?
O18 Gd2 O11 140.1(2) . 1_545 ?
O18 Gd2 O17 76.0(3) . . ?
O18 Gd2 O19 71.7(2) . . ?
O19 Gd2 O9 76.25(18) . . ?
O19 Gd2 O10 74.9(2) . 2_565 ?
O19 Gd2 O11 145.9(3) . 1_545 ?
O19 Gd2 O17 137.8(2) . . ?
O20 Gd2 O9 74.1(2) . . ?
O20 Gd2 O10 76.4(3) . 2_565 ?
O20 Gd2 O11 74.4(2) . 1_545 ?
O20 Gd2 O17 109.6(3) . . ?
O20 Gd2 O18 141.64(18) . . ?
O20 Gd2 O19 81.7(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
C1 C2 C3 C4 4.3(8) . . . . ?
C1 C2 C3 O3 -168.8(11) . . . . ?
C1 C4 O4 Gd1 147.2(9) . . . 2_565 ?
C2 C1 C4 C3 4.2(8) . . . . ?
C2 C1 C4 O4 -179.5(11) . . . . ?
C2 C1 O1 Gd1 -138.1(10) . . . . ?
C2 C3 C4 C1 -4.3(8) . . . . ?
C2 C3 C4 O4 179.6(11) . . . . ?
C2 C3 O3 Gd1 30.6(17) . . . 1_565 ?
C3 C4 O4 Gd1 -38.1(16) . . . 2_565 ?
C4 C1 C2 C3 -4.2(8) . . . . ?
C4 C1 C2 O2 178.5(12) . . . . ?
C4 C1 O1 Gd1 33.2(19) . . . . ?
C4 C3 O3 Gd1 -139.6(10) . . . 1_565 ?
C5 C6 C7 C8 5.3(6) . . . . ?
C5 C6 C7 O7 -171.5(9) . . . . ?
C5 C8 O8 Gd2 42.8(14) . . . . ?
C6 C5 C8 C7 5.3(6) . . . . ?
C6 C5 C8 O8 -174.6(9) . . . . ?
C6 C5 O5 Gd1 -32.9(15) . . . . ?
C6 C7 C8 C5 -5.3(6) . . . . ?
C6 C7 C8 O8 174.6(9) . . . . ?
C7 C8 O8 Gd2 -137.1(7) . . . . ?
C8 C5 C6 C7 -5.3(6) . . . . ?
C8 C5 C6 O6 172.4(10) . . . . ?
C8 C5 O5 Gd1 143.3(7) . . . . ?
C9 C10 C11 C12 -3.0(8) . . . . ?
C9 C10 C11 O11 172.6(11) . . . . ?
C9 C10 O10 Gd2 36.8(16) . . . 2_564 ?
C10 C9 C12 C11 -3.0(8) . . . . ?
C10 C9 C12 O12 -179.8(12) . . . . ?
C10 C9 O9 Gd2 142.4(9) . . . . ?
C10 C11 C12 C9 3.0(8) . . . . ?
C10 C11 C12 O12 179.7(12) . . . . ?
C10 C11 O11 Gd2 -38.0(17) . . . 1_565 ?
C11 C10 O10 Gd2 -143.9(9) . . . 2_564 ?
C12 C9 C10 C11 3.0(8) . . . . ?
C12 C9 C10 O10 -177.5(11) . . . . ?
C12 C9 O9 Gd2 -31.8(17) . . . . ?
C12 C11 O11 Gd2 136.2(9) . . . 1_565 ?
O1 C1 C2 C3 169.6(11) . . . . ?
O1 C1 C2 O2 -8(2) . . . . ?
O1 C1 C4 C3 -169.7(11) . . . . ?
O1 C1 C4 O4 7(2) . . . . ?
O2 C2 C3 C4 -178.6(12) . . . . ?
O2 C2 C3 O3 8(2) . . . . ?
O3 C3 C4 C1 168.8(11) . . . . ?
O3 C3 C4 O4 -7(2) . . . . ?
O5 C5 C6 C7 172.1(10) . . . . ?
O5 C5 C6 O6 -10.3(18) . . . . ?
O5 C5 C8 C7 -172.0(9) . . . . ?
O5 C5 C8 O8 8.1(16) . . . . ?
O6 C6 C7 C8 -172.2(10) . . . . ?
O6 C6 C7 O7 10.9(18) . . . . ?
O7 C7 C8 C5 171.7(8) . . . . ?
O7 C7 C8 O8 -8.4(15) . . . . ?
O9 C9 C10 C11 -172.9(11) . . . . ?
O9 C9 C10 O10 7(2) . . . . ?
O9 C9 C12 C11 172.9(11) . . . . ?
O9 C9 C12 O12 -4(2) . . . . ?
O10 C10 C11 C12 177.5(10) . . . . ?
O10 C10 C11 O11 -7(2) . . . . ?
O11 C11 C12 C9 -173.2(9) . . . . ?
O11 C11 C12 O12 4(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.511
_oxdiff_exptl_absorpt_empirical_full_min 0.605
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.83(3)
2 0.17(3)

_exptl_crystal_preparation       'Magnetic properties'
