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

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

data_olmio4
_database_code_depnum_ccdc_archive 'CCDC 2351940'
loop_
_audit_author_name
_audit_author_address
'Nadia Marino'
;University of Calabria
Italy
;
_audit_update_record             
;
2024-04-29 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;

_vrf_PLAT430_olmio4              
;
PROBLEM: Short Inter D...A Contact  O9W      ..O9W      .       1.95 Ang.  
RESPONSE: O9w is the oxygen of an extremely disordered water molecule 
          of crystallization, whose occupancy has been set  
          to 1 to comply whith the total crystallization water                 
          content evidenced by other experimental techniques. The same 
          disorder has been found in the crystal structures of litterature
          analogue 3D oxalate compounds with lanthanide ions.
          Concerning other short O---O contacts, they can be described
          as strongly hydrogen bonded oxygen atoms (perhaps as an effect
          of confinement of the water molecules of crystallization into
          the hexagonal channels of the 3D net). 
;
_vrf_PLAT043_olmio4              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      12.10 Check 
RESPONSE: No hydrogen atoms have been found, neither have them been set in 
          calculated positions, for the disordered water molecules of 
          crystallization. Thus, the calculated and reported mol. weight  
          differ by 12 if Z is set to 18 (as the check-cif software does), 
          and by 24 if Z is set to 9 (our choice, in agreement with the   
          literature: this allows to describe the compound as a 3D polymer  
          with an integer number of oxalate ions in its formula unit).
;
_vrf_PLAT260_olmio4              
;
PROBLEM: Large Average Ueq of Residue Including       O9W      0.602 Check 
RESPONSE: O9w is the oxygen of an extremely disordered water molecule 
          of crystallization
;
_vrf_PLAT306_olmio4              
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O4W Check 
RESPONSE: No hydrogen atoms have been found, neither have they been set in 
          calculated positions, for the disordered water molecules of 
          crystallization (named O4w, O5w, O6w, O7w, O8w and O9w).
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H12 Ho2 O18, 12(H2 O)'
_chemical_formula_sum            'C6 H36 Ho2 O30'
_chemical_formula_weight         918.21

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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   30.500(9)
_cell_length_b                   30.500(9)
_cell_length_c                   7.127(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5741(4)
_cell_formula_units_Z            9
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      28.74

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_F_000             4014
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.036
_exptl_absorpt_coefficient_mu    6.281
_shelx_estimated_absorpt_T_min   0.213
_shelx_estimated_absorpt_T_max   0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3987
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6873
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.961
_diffrn_reflns_theta_max         28.564
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3241
_reflns_number_gt                2215
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'CRYSTAL MAKER, DIAMOND'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0425P)²+255.0972P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Direct
_atom_sites_solution_secondary   Difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3241
_refine_ls_number_parameters     184
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1614
_refine_ls_wR_factor_gt          0.1393
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.44342(2) 0.55699(2) 0.84064(6) 0.02827(18) Uani 1 1 d . . . . .
C1 C 0.3411(4) 0.4870(4) 0.6136(15) 0.031(2) Uani 1 1 d . U . . .
C2 C 0.3241(4) 0.5164(4) 0.7386(15) 0.030(2) Uani 1 1 d . U . . .
O1 O 0.3854(3) 0.4961(3) 0.6303(11) 0.0351(18) Uani 1 1 d . U . . .
O2 O 0.3074(3) 0.4548(3) 0.5053(11) 0.0367(19) Uani 1 1 d . U . . .
O3 O 0.3576(3) 0.5483(3) 0.8470(11) 0.0372(19) Uani 1 1 d . U . . .
O4 O 0.2796(3) 0.5072(3) 0.7193(11) 0.0387(19) Uani 1 1 d . U . . .
C3 C 0.5156(4) 0.5239(4) 1.0590(14) 0.029(2) Uani 1 1 d . U . . .
O5 O 0.5088(3) 0.5602(3) 1.0416(11) 0.0339(17) Uani 1 1 d . U . . .
O6 O 0.5491(3) 0.5214(3) 1.1622(11) 0.0354(18) Uani 1 1 d . U . . .
O1W O 0.4924(3) 0.5565(3) 0.5838(12) 0.041(2) Uani 1 1 d D . . . .
H1WA H 0.510(5) 0.581(4) 0.487(15) 0.061 Uiso 1 1 d D U . . .
H1WB H 0.517(4) 0.547(5) 0.61(2) 0.061 Uiso 1 1 d D U . . .
O2W O 0.4431(3) 0.6097(3) 1.0795(12) 0.043(2) Uani 1 1 d D . . . .
H2WA H 0.429085 0.628803 1.024501 0.064 Uiso 1 1 d D U . . .
H2WB H 0.413247 0.584261 1.142778 0.064 Uiso 1 1 d D U . . .
O3W O 0.3945(3) 0.5050(3) 1.0916(11) 0.042(2) Uani 1 1 d D . . . .
H3WA H 0.409(5) 0.490(5) 1.169(18) 0.063 Uiso 1 1 d D U . . .
H3WB H 0.362(3) 0.478(4) 1.05(2) 0.063 Uiso 1 1 d D U . . .
O4W O 0.5424(4) 0.6330(3) 0.3282(12) 0.045(2) Uani 1 1 d . . . . .
O5W O 0.5717(4) 0.5397(4) 0.6473(12) 0.045(2) Uani 1 1 d . . . . .
O6W O 0.3316(4) 0.3817(4) 0.4275(16) 0.061(3) Uani 1 1 d . . . . .
O7W O 0.6396(4) 0.6097(4) 1.1754(15) 0.057(3) Uani 1 1 d . . . . .
O8W O 0.2508(5) 0.5511(6) 0.9882(16) 0.079(4) Uani 1 1 d . . . . .
O9W O 0.2918(17) 0.654(2) 0.895(12) 0.58(7) 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
Ho1 O2W 2.345(9) . ?
Ho1 O1 2.354(8) . ?
Ho1 O3W 2.361(8) . ?
Ho1 O1W 2.367(9) . ?
Ho1 O4 2.402(8) 15_556 ?
Ho1 O5 2.416(8) . ?
Ho1 O2 2.445(8) 15_556 ?
Ho1 O3 2.497(8) . ?
Ho1 O6 2.513(8) 10_667 ?
C1 O1 1.242(13) . ?
C1 O2 1.269(14) . ?
C1 C2 1.527(16) . ?
C2 O4 1.248(14) . ?
C2 O3 1.262(13) . ?
C3 O5 1.232(13) . ?
C3 O6 1.292(13) . ?
C3 C3 1.53(2) 10_667 ?
O1W H1WA 0.96(2) . ?
O1W H1WB 0.96(2) . ?
O2W H2WA 0.9617 . ?
O2W H2WB 0.9636 . ?
O3W H3WA 0.96(2) . ?
O3W H3WB 0.96(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2W Ho1 O1 138.1(3) . . ?
O2W Ho1 O3W 72.1(3) . . ?
O1 Ho1 O3W 88.8(3) . . ?
O2W Ho1 O1W 141.7(3) . . ?
O1 Ho1 O1W 74.3(3) . . ?
O3W Ho1 O1W 140.4(3) . . ?
O2W Ho1 O4 88.9(3) . 15_556 ?
O1 Ho1 O4 81.1(3) . 15_556 ?
O3W Ho1 O4 138.2(3) . 15_556 ?
O1W Ho1 O4 75.2(3) . 15_556 ?
O2W Ho1 O5 80.1(3) . . ?
O1 Ho1 O5 133.5(3) . . ?
O3W Ho1 O5 79.0(3) . . ?
O1W Ho1 O5 87.0(3) . . ?
O4 Ho1 O5 135.0(3) 15_556 . ?
O2W Ho1 O2 68.7(3) . 15_556 ?
O1 Ho1 O2 138.3(3) . 15_556 ?
O3W Ho1 O2 132.8(3) . 15_556 ?
O1W Ho1 O2 73.0(3) . 15_556 ?
O4 Ho1 O2 66.0(3) 15_556 15_556 ?
O5 Ho1 O2 69.4(3) . 15_556 ?
O2W Ho1 O3 72.3(3) . . ?
O1 Ho1 O3 66.0(3) . . ?
O3W Ho1 O3 68.8(3) . . ?
O1W Ho1 O3 130.2(3) . . ?
O4 Ho1 O3 70.1(3) 15_556 . ?
O5 Ho1 O3 142.5(3) . . ?
O2 Ho1 O3 120.4(3) 15_556 . ?
O2W Ho1 O6 133.8(3) . 10_667 ?
O1 Ho1 O6 68.5(3) . 10_667 ?
O3W Ho1 O6 72.2(3) . 10_667 ?
O1W Ho1 O6 68.3(3) . 10_667 ?
O4 Ho1 O6 137.3(3) 15_556 10_667 ?
O5 Ho1 O6 65.0(3) . 10_667 ?
O2 Ho1 O6 120.3(3) 15_556 10_667 ?
O3 Ho1 O6 119.2(3) . 10_667 ?
O1 C1 O2 126.9(10) . . ?
O1 C1 C2 117.7(10) . . ?
O2 C1 C2 115.3(10) . . ?
O4 C2 O3 127.6(11) . . ?
O4 C2 C1 117.1(10) . . ?
O3 C2 C1 115.4(10) . . ?
C1 O1 Ho1 122.7(7) . . ?
C1 O2 Ho1 120.1(7) . 14_456 ?
C2 O3 Ho1 118.1(7) . . ?
C2 O4 Ho1 121.5(7) . 14_456 ?
O5 C3 O6 127.2(10) . . ?
O5 C3 C3 119.8(12) . 10_667 ?
O6 C3 C3 112.9(12) . 10_667 ?
C3 O5 Ho1 122.0(7) . . ?
C3 O6 Ho1 120.1(7) . 10_667 ?
Ho1 O1W H1WA 131(9) . . ?
Ho1 O1W H1WB 115(9) . . ?
H1WA O1W H1WB 101(10) . . ?
Ho1 O2W H2WA 105.9 . . ?
Ho1 O2W H2WB 96.5 . . ?
H2WA O2W H2WB 98.7 . . ?
Ho1 O3W H3WA 118(9) . . ?
Ho1 O3W H3WB 113(9) . . ?
H3WA O3W H3WB 105(10) . . ?

_refine_diff_density_max         2.474
_refine_diff_density_min         -2.061
_refine_diff_density_rms         0.282



####################################################################### 
# 
# 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_olmio3
_database_code_depnum_ccdc_archive 'CCDC 2351941'
loop_
_audit_author_name
_audit_author_address
'Nadia Marino'
;University of Calabria
Italy
;
_audit_update_record             
;
2024-04-29 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;

_vrf_PLAT430_olmio3              
;
PROBLEM: Short Inter D...A Contact  O4W      ..O5W      .       1.63 Ang.  
RESPONSE: O4w, O5w, O6w and O7w are the oxygen atoms of disordered water  
          molecules of crystallization whose total occupancy has been set  
          to 2-per-Ho-atom, to comply whith the total crystallization water                 
          content evidenced by other experimental techniques. 
          Crystallographically, it appears clear that the single occupancies 
          of O4w, O5w, O6w and O7w must be equal to 0.5, because the four 
          oxygen atoms are lined up to form a 4 membered zig-zag motif,
          so that only O7w is compatible with the full occupancy of O4w,  
          while only O6w is compatible with the presence of O5w, and the two
          sets  (O4w + O7w and O5w + O6w) are mutually exclusive. In spite 
          of these considerations, O4w and O5w are fairly more disordered than
          O6w and O7w.
;
_vrf_PLAT043_olmio3              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.03 Check 
RESPONSE: No hydrogen atoms have been found, neither have them been set in 
          calculated positions, for the disordered water molecules of 
          crystallization. Thus, the calculated and reported mol. weight  
          differ by 4 if Z is set to 4 (as the check-cif software does), 
          and by 8 if Z is set to 2 (our choice, in agreement with the   
          literature: this allows to describe the compound as a 2D polymer  
          with an integer number of oxalate ions in its formula unit).  
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H12 Ho2 O18, 4(H2 O)'
_chemical_formula_sum            'C6 H20 Ho2 O22'
_chemical_formula_weight         774.08

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.9347(3)
_cell_length_b                   9.6040(3)
_cell_length_c                   9.9542(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.1430(10)
_cell_angle_gamma                90
_cell_volume                     953.92(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      28.74


_exptl_crystal_description       PLATE
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.695
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.049
_exptl_absorpt_coefficient_mu    8.344
_shelx_estimated_absorpt_T_min   0.460
_shelx_estimated_absorpt_T_max   0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6297
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14424
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.944
_diffrn_reflns_theta_max         28.744
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2469
_reflns_number_gt                2306
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'CRYSTAL MAKER, DIAMOND'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0134P)²+1.0920P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Direct
_atom_sites_solution_secondary   Difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00070(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2469
_refine_ls_number_parameters     173
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0146
_refine_ls_wR_factor_ref         0.0378
_refine_ls_wR_factor_gt          0.0364
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.69080(2) 0.45752(2) 0.33094(2) 0.01262(5) Uani 1 1 d . . . . .
C1 C 0.4449(3) 0.5261(3) 0.4274(3) 0.0181(4) Uani 1 1 d . U . . .
O1 O 0.4739(2) 0.5261(2) 0.3172(2) 0.0213(4) Uani 1 1 d . U . . .
O2 O 0.3371(2) 0.5629(2) 0.4306(2) 0.0265(4) Uani 1 1 d . U . . .
C2 C 0.9994(2) 0.4471(2) 0.5577(3) 0.0150(4) Uani 1 1 d . U . . .
O3 O 0.88933(18) 0.3916(2) 0.5351(2) 0.0212(4) Uani 1 1 d . U . . .
O4 O 1.10876(18) 0.4262(2) 0.6644(2) 0.0206(4) Uani 1 1 d . U . . .
C3 C 0.5330(2) 0.5714(2) 0.0024(3) 0.0160(4) Uani 1 1 d . U . . .
O5 O 0.6278(2) 0.6032(2) 0.1216(2) 0.0232(4) Uani 1 1 d . U . . .
O6 O 0.48729(18) 0.64298(19) -0.11252(19) 0.0188(3) Uani 1 1 d . U . . .
O1W O 0.7105(2) 0.6867(2) 0.4276(3) 0.0328(5) Uani 1 1 d D . . . .
H1WA H 0.779(3) 0.728(4) 0.505(4) 0.049 Uiso 1 1 d D U . . .
H1WB H 0.638(3) 0.744(4) 0.420(4) 0.049 Uiso 1 1 d D U . . .
O2W O 0.7953(2) 0.3202(2) 0.2016(3) 0.0313(5) Uani 1 1 d D . . . .
H2WA H 0.8852(19) 0.324(4) 0.229(5) 0.047 Uiso 1 1 d D U . . .
H2WB H 0.775(4) 0.228(2) 0.181(4) 0.047 Uiso 1 1 d D U . . .
O3W O 0.6644(3) 0.2209(2) 0.3812(2) 0.0348(5) Uani 1 1 d D . . . .
H3WA H 0.713(4) 0.176(4) 0.468(3) 0.052 Uiso 1 1 d D U . . .
H3WB H 0.614(4) 0.153(3) 0.319(3) 0.052 Uiso 1 1 d D U . . .
O4W O 1.1009(18) 0.988(2) 0.549(3) 0.248(13) Uani 0.5 1 d . . P . .
O5W O 0.8524(16) 0.8958(16) 0.320(2) 0.216(12) Uani 0.5 1 d . . P . .
O6W O 0.9415(8) 0.7862(18) 0.6267(14) 0.162(7) Uani 0.5 1 d . . P . .
O7W O 0.9222(6) 0.6750(8) 0.7189(9) 0.0565(18) Uani 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O5 2.3663(18) . ?
Ho1 O3W 2.369(2) . ?
Ho1 O3 2.3739(18) . ?
Ho1 O1W 2.376(2) . ?
Ho1 O1 2.4108(19) . ?
Ho1 O2W 2.430(2) . ?
Ho1 O4 2.4434(19) 3_766 ?
Ho1 O6 2.4469(18) 3_665 ?
Ho1 O2 2.522(2) 3_666 ?
C1 O2 1.243(3) . ?
C1 O1 1.260(3) . ?
C1 C1 1.539(5) 3_666 ?
C2 O4 1.249(3) . ?
C2 O3 1.250(3) . ?
C2 C2 1.537(5) 3_766 ?
C3 O6 1.251(3) . ?
C3 O5 1.253(3) . ?
C3 C3 1.541(5) 3_665 ?
O1W H1WA 0.914(18) . ?
O1W H1WB 0.940(18) . ?
O2W H2WA 0.907(18) . ?
O2W H2WB 0.920(18) . ?
O3W H3WA 0.918(18) . ?
O3W H3WB 0.916(18) . ?
O4W O5W 1.63(3) 3_776 ?
O5W O7W 1.63(3) 4_575 ?
O6W O7W 1.479(18) . ?

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
O5 Ho1 O3W 137.41(7) . . ?
O5 Ho1 O3 138.29(6) . . ?
O3W Ho1 O3 73.20(7) . . ?
O5 Ho1 O1W 75.79(8) . . ?
O3W Ho1 O1W 143.27(9) . . ?
O3 Ho1 O1W 90.03(8) . . ?
O5 Ho1 O1 82.12(7) . . ?
O3W Ho1 O1 94.15(8) . . ?
O3 Ho1 O1 130.96(7) . . ?
O1W Ho1 O1 72.19(7) . . ?
O5 Ho1 O2W 83.40(8) . . ?
O3W Ho1 O2W 73.47(9) . . ?
O3 Ho1 O2W 81.10(7) . . ?
O1W Ho1 O2W 137.11(8) . . ?
O1 Ho1 O2W 141.54(7) . . ?
O5 Ho1 O4 71.47(6) . 3_766 ?
O3W Ho1 O4 128.31(8) . 3_766 ?
O3 Ho1 O4 66.84(6) . 3_766 ?
O1W Ho1 O4 68.71(7) . 3_766 ?
O1 Ho1 O4 136.90(7) . 3_766 ?
O2W Ho1 O4 69.24(7) . 3_766 ?
O5 Ho1 O6 67.15(6) . 3_665 ?
O3W Ho1 O6 71.81(7) . 3_665 ?
O3 Ho1 O6 140.55(7) . 3_665 ?
O1W Ho1 O6 129.25(7) . 3_665 ?
O1 Ho1 O6 69.53(7) . 3_665 ?
O2W Ho1 O6 72.00(7) . 3_665 ?
O4 Ho1 O6 125.37(6) 3_766 3_665 ?
O5 Ho1 O2 140.44(7) . 3_666 ?
O3W Ho1 O2 69.81(8) . 3_666 ?
O3 Ho1 O2 66.03(7) . 3_666 ?
O1W Ho1 O2 73.53(8) . 3_666 ?
O1 Ho1 O2 65.15(6) . 3_666 ?
O2W Ho1 O2 136.12(8) . 3_666 ?
O4 Ho1 O2 118.08(7) 3_766 3_666 ?
O6 Ho1 O2 116.55(7) 3_665 3_666 ?
O2 C1 O1 126.9(2) . . ?
O2 C1 C1 117.0(3) . 3_666 ?
O1 C1 C1 116.0(3) . 3_666 ?
C1 O1 Ho1 122.84(16) . . ?
C1 O2 Ho1 118.88(17) . 3_666 ?
O4 C2 O3 126.9(2) . . ?
O4 C2 C2 116.4(3) . 3_766 ?
O3 C2 C2 116.7(3) . 3_766 ?
C2 O3 Ho1 121.07(16) . . ?
C2 O4 Ho1 118.81(16) . 3_766 ?
O6 C3 O5 126.7(2) . . ?
O6 C3 C3 117.0(3) . 3_665 ?
O5 C3 C3 116.3(3) . 3_665 ?
C3 O5 Ho1 121.30(16) . . ?
C3 O6 Ho1 118.10(15) . 3_665 ?
Ho1 O1W H1WA 130(2) . . ?
Ho1 O1W H1WB 125(2) . . ?
H1WA O1W H1WB 101(2) . . ?
Ho1 O2W H2WA 120(3) . . ?
Ho1 O2W H2WB 121(3) . . ?
H2WA O2W H2WB 104(2) . . ?
Ho1 O3W H3WA 125(2) . . ?
Ho1 O3W H3WB 129(2) . . ?
H3WA O3W H3WB 105(2) . . ?
O4W O5W O7W 134.7(14) 3_776 4_575 ?
O6W O7W O5W 154.4(8) . 4_576 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WA O6W 0.914(18) 1.79(2) 2.669(8) 162(4) . yes
O1W H1WB O6 0.940(18) 1.890(18) 2.828(3) 175(4) 4_576 yes
O2W H2WA O7W 0.907(18) 1.95(2) 2.859(7) 177(4) 3_766 yes
O2W H2WB O2 0.920(18) 2.03(2) 2.895(3) 156(4) 2_645 yes
O3W H3WA O2W 0.918(18) 2.12(3) 2.940(3) 148(4) 4_566 yes
O3W H3WB O1 0.916(18) 1.780(19) 2.691(3) 173(4) 2_645 yes

_refine_diff_density_max         0.616
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.110



