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

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

data_adi-y-hexa-h2o
_audit_block_doi                 10.5517/ccdc.csd.cc2j8544
_database_code_depnum_ccdc_archive 'CCDC 2331545'
loop_
_audit_author_name
_audit_author_address
'ADITYA BORAH'
;jengraimukh college 
India
;
_audit_update_record             
;
2024-03-19 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-03-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H108 O24 P6 Y, 3(H5 O2)'
_chemical_formula_sum            'C72 H123 O30 P6 Y'
_chemical_formula_weight         1743.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Y C O P H'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
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                   23.5867(4)
_cell_length_b                   23.5867(4)
_cell_length_c                   13.2999(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6407.9(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    10739
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.4520
_cell_measurement_theta_min      2.9720
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.695
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2772
_exptl_crystal_preparation       .
_exptl_crystal_recrystallization_method .
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22325
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.992
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  75.00   1.00    6.00    --  -14.30  58.00 173.00  125
  2  ω    -48.00  75.00   1.00    6.00    --  -14.30  38.00 -60.00  123
  3  ω   -104.00  24.00   1.00    6.00    --  -14.30 -72.00   0.00  128
  4  ω    -53.00  39.00   1.00    6.00    --  -14.30  72.00  30.00   92
  5  ω   -104.00 -79.00   1.00    6.00    --  -14.30 -38.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0210958000
_diffrn_orient_matrix_UB_12      0.0158788000
_diffrn_orient_matrix_UB_13      -0.0413176000
_diffrn_orient_matrix_UB_21      0.0079538000
_diffrn_orient_matrix_UB_22      0.0308534000
_diffrn_orient_matrix_UB_23      0.0204493000
_diffrn_orient_matrix_UB_31      0.0264114000
_diffrn_orient_matrix_UB_32      0.0008355000
_diffrn_orient_matrix_UB_33      0.0267905000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ESI
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2408
_reflns_number_total             2499
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2499
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.050
_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)+(0.0428P)²+9.4432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0791
_refine_special_details          ESI
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H3,H5B)
2.b Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Y1 Y 0.333333 0.666667 0.166667 0.01245(13) Uani 1 6 d S T P . .
P1 P 0.48062(2) 0.79932(2) 0.27675(3) 0.01771(14) Uani 1 1 d . . . . .
O1 O 0.41277(6) 0.74450(6) 0.25917(9) 0.0202(3) Uani 1 1 d . . . . .
O2 O 0.49002(7) 0.86487(6) 0.23386(11) 0.0308(3) Uani 1 1 d . . . . .
H2 H 0.461699 0.856898 0.189402 0.046 Uiso 1 1 calc R U . . .
O3 O 0.53409(6) 0.78701(7) 0.24043(10) 0.0275(3) Uani 1 1 d . . . . .
O4 O 0.48986(6) 0.81441(6) 0.39376(9) 0.0183(3) Uani 1 1 d . . . . .
C1 C 0.53594(8) 0.81323(9) 0.45965(13) 0.0167(4) Uani 1 1 d . . . . .
C2 C 0.58930(9) 0.87385(9) 0.48643(13) 0.0185(4) Uani 1 1 d . . . . .
C3 C 0.63207(9) 0.87367(9) 0.55844(14) 0.0236(4) Uani 1 1 d . . . . .
H3A H 0.669019 0.913874 0.578375 0.028 Uiso 1 1 calc R U . . .
C4 C 0.62148(10) 0.81563(10) 0.60142(15) 0.0280(5) Uani 1 1 d . . . . .
H4 H 0.650781 0.816412 0.651127 0.034 Uiso 1 1 calc R U . . .
C5 C 0.56842(10) 0.75657(10) 0.57226(14) 0.0256(4) Uani 1 1 d . . . . .
H5 H 0.561855 0.717172 0.602216 0.031 Uiso 1 1 calc R U . . .
C6 C 0.52417(9) 0.75376(9) 0.49936(13) 0.0200(4) Uani 1 1 d . . . . .
C7 C 0.59888(9) 0.93698(9) 0.43995(14) 0.0211(4) Uani 1 1 d . . . . .
H7 H 0.583346 0.927326 0.368722 0.025 Uiso 1 1 calc R U . . .
C8 C 0.55633(11) 0.95908(10) 0.49514(16) 0.0319(5) Uani 1 1 d . . . . .
H8A H 0.510554 0.923763 0.493826 0.048 Uiso 1 1 calc R U . . .
H8B H 0.560118 0.997916 0.461928 0.048 Uiso 1 1 calc R U . . .
H8C H 0.571050 0.969710 0.565033 0.048 Uiso 1 1 calc R U . . .
C9 C 0.67015(10) 0.99183(10) 0.43848(17) 0.0337(5) Uani 1 1 d . . . . .
H9A H 0.685224 1.005712 0.507523 0.051 Uiso 1 1 calc R U . . .
H9B H 0.673871 1.029017 0.400132 0.051 Uiso 1 1 calc R U . . .
H9C H 0.697171 0.975998 0.406843 0.051 Uiso 1 1 calc R U . . .
C10 C 0.46815(9) 0.68783(9) 0.46590(14) 0.0227(4) Uani 1 1 d . . . . .
H10 H 0.439543 0.696090 0.419836 0.027 Uiso 1 1 calc R U . . .
C11 C 0.42624(11) 0.64734(10) 0.55466(17) 0.0380(5) Uani 1 1 d . . . . .
H11A H 0.452760 0.637081 0.599734 0.057 Uiso 1 1 calc R U . . .
H11B H 0.389061 0.606569 0.529723 0.057 Uiso 1 1 calc R U . . .
H11C H 0.410048 0.672410 0.591409 0.057 Uiso 1 1 calc R U . . .
C12 C 0.49431(11) 0.65017(10) 0.40684(18) 0.0358(5) Uani 1 1 d . . . . .
H12A H 0.518907 0.675977 0.348283 0.054 Uiso 1 1 calc R U . . .
H12B H 0.457599 0.608281 0.384296 0.054 Uiso 1 1 calc R U . . .
H12C H 0.523200 0.642114 0.450052 0.054 Uiso 1 1 calc R U . . .
O5 O 0.65364(7) 0.86482(8) 0.27405(12) 0.0392(4) Uani 1 1 d G . . . .
H3 H 0.613481 0.839608 0.259454 0.059 Uiso 1 1 d G U . . .
H5B H 0.676860 0.872436 0.221432 0.059 Uiso 1 1 d G U . . .
H5A H 0.666667 0.833333 0.333333 0.070(13) Uiso 1 2 d S . 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
Y1 O1 2.2259(12) 2_665 ?
Y1 O1 2.2260(12) 3_565 ?
Y1 O1 2.2259(12) 13_565 ?
Y1 O1 2.2258(12) 14_455 ?
Y1 O1 2.2259(12) . ?
Y1 O1 2.2261(12) 15 ?
P1 O1 1.4894(13) . ?
P1 O2 1.5563(14) . ?
P1 O3 1.5080(14) . ?
P1 O4 1.5870(13) . ?
O2 H2 0.8400 . ?
O4 C1 1.407(2) . ?
C1 C2 1.398(3) . ?
C1 C6 1.391(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.521(2) . ?
C3 H3A 0.9500 . ?
C3 C4 1.386(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.402(3) . ?
C6 C10 1.519(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.530(3) . ?
C7 C9 1.525(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.529(3) . ?
C10 C12 1.528(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O5 H3 0.8517 . ?
O5 H5B 0.8506 . ?
O5 H5A 1.2231(17) . ?

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 Y1 O1 180.0 2_665 14_455 ?
O1 Y1 O1 87.60(4) . 15 ?
O1 Y1 O1 87.61(4) 13_565 3_565 ?
O1 Y1 O1 92.39(4) 2_665 . ?
O1 Y1 O1 87.61(4) 14_455 3_565 ?
O1 Y1 O1 87.61(4) 14_455 . ?
O1 Y1 O1 92.40(4) 14_455 15 ?
O1 Y1 O1 87.60(4) 2_665 13_565 ?
O1 Y1 O1 92.39(4) 2_665 3_565 ?
O1 Y1 O1 92.40(4) 14_455 13_565 ?
O1 Y1 O1 92.39(4) . 3_565 ?
O1 Y1 O1 180.0 . 13_565 ?
O1 Y1 O1 180.0 15 3_565 ?
O1 Y1 O1 87.60(4) 2_665 15 ?
O1 Y1 O1 92.39(4) 13_565 15 ?
O1 P1 O2 111.24(7) . . ?
O1 P1 O3 114.94(8) . . ?
O1 P1 O4 108.43(7) . . ?
O2 P1 O4 101.61(7) . . ?
O3 P1 O2 110.87(9) . . ?
O3 P1 O4 108.84(7) . . ?
P1 O1 Y1 153.99(8) . . ?
P1 O2 H2 109.5 . . ?
C1 O4 P1 128.84(11) . . ?
C2 C1 O4 116.59(15) . . ?
C6 C1 O4 119.33(15) . . ?
C6 C1 C2 123.93(16) . . ?
C1 C2 C7 120.96(16) . . ?
C3 C2 C1 117.07(17) . . ?
C3 C2 C7 121.95(16) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 C2 120.89(17) . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.31(17) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.26(18) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 116.53(17) . . ?
C1 C6 C10 123.64(16) . . ?
C5 C6 C10 119.81(17) . . ?
C2 C7 H7 107.7 . . ?
C2 C7 C8 109.68(15) . . ?
C2 C7 C9 113.38(16) . . ?
C8 C7 H7 107.7 . . ?
C9 C7 H7 107.7 . . ?
C9 C7 C8 110.48(16) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.8 . . ?
C6 C10 C11 111.89(16) . . ?
C6 C10 C12 110.38(16) . . ?
C11 C10 H10 107.8 . . ?
C12 C10 H10 107.8 . . ?
C12 C10 C11 110.89(17) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
H3 O5 H5B 109.5 . . ?
H3 O5 H5A 104.6 . . ?
H5B O5 H5A 109.1 . . ?

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
P1 O4 C1 C2 102.52(17) . . . . ?
P1 O4 C1 C6 -81.8(2) . . . . ?
O1 P1 O4 C1 121.63(14) . . . . ?
O2 P1 O1 Y1 80.74(19) . . . . ?
O2 P1 O4 C1 -121.08(15) . . . . ?
O3 P1 O1 Y1 -46.3(2) . . . . ?
O3 P1 O4 C1 -4.05(16) . . . . ?
O4 P1 O1 Y1 -168.34(16) . . . . ?
O4 C1 C2 C3 174.43(16) . . . . ?
O4 C1 C2 C7 -4.4(2) . . . . ?
O4 C1 C6 C5 -173.68(16) . . . . ?
O4 C1 C6 C10 8.0(3) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C7 C8 82.1(2) . . . . ?
C1 C2 C7 C9 -153.90(17) . . . . ?
C1 C6 C10 C11 -126.3(2) . . . . ?
C1 C6 C10 C12 109.7(2) . . . . ?
C2 C1 C6 C5 1.7(3) . . . . ?
C2 C1 C6 C10 -176.63(17) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C3 C2 C7 C8 -96.6(2) . . . . ?
C3 C2 C7 C9 27.4(2) . . . . ?
C3 C4 C5 C6 -0.2(3) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?
C4 C5 C6 C10 177.35(18) . . . . ?
C5 C6 C10 C11 55.5(2) . . . . ?
C5 C6 C10 C12 -68.5(2) . . . . ?
C6 C1 C2 C3 -1.0(3) . . . . ?
C6 C1 C2 C7 -179.83(17) . . . . ?
C7 C2 C3 C4 178.49(18) . . . . ?

_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.761

# start Validation Reply Form
_vrf_PLAT420_adi-y-hexa-h2o      
;
PROBLEM: D-H Bond Without Acceptor O5 --H5B . Please Check
RESPONSE: H5B is a part of (H5O2)+ species and doesn't involved in H-bonding
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dyhexa
_database_code_depnum_ccdc_archive 'CCDC 2069003'
loop_
_audit_author_name
_audit_author_address
'R Murugavel'
;IIT Bombay
India
;
_audit_update_record             
;
2024-03-21 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT355_dyhexa              
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O5       - H3       .       1.18 Ang.
RESPONSE: There is a symmetric hydrogen bond between O5 and O5? at the centre; the variation in the distances involving H3 is due to dynamic motion of H3 between O5 and O3, depending on the lanthanide metal.
;
_vrf_PLAT420_dyhexa              
;
PROBLEM: D-H Bond Without Acceptor  O5       --H5B      .     Please Check
RESPONSE: H5B does not have any acceptor in the vicinity
;
# Added during the CSD deposition process: Thursday 21 March 2024 11:38 AM
# end Validation Reply Form

_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Dy
_chemical_formula_moiety         'C72 H123 Dy O30 P6'
_chemical_formula_sum            'C72 H123 Dy O30 P6'
_chemical_formula_weight         1817.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
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                   23.764(4)
_cell_length_b                   23.764(4)
_cell_length_c                   13.421(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6564(3)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    3020
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.8010
_cell_measurement_theta_min      2.4980
_shelx_estimated_absorpt_T_max   0.835
_shelx_estimated_absorpt_T_min   0.712
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2853
_exptl_crystal_preparation       ESI
_exptl_crystal_recrystallization_method ESI
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11886
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.988
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         2.494
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 724+ ccd diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ESI
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2561
_reflns_number_total             2568
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004  (Burla et al.,  2007)'
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2568
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0186
_refine_ls_restrained_S_all      1.056
_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)+(0.0277P)²+8.0021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0496
_refine_special_details          ESI
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Uiso: H2(0.08) H3(0.08) H5A(0.08) H5B(0.08)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.666667 0.333333 0.833333 0.01742(7) Uani 1 6 d S T P . .
P1 P 0.51938(2) 0.31799(2) 0.72382(3) 0.02728(11) Uani 1 1 d . . . . .
O1 O 0.58660(6) 0.33065(6) 0.74124(9) 0.0324(3) Uani 1 1 d . . . . .
O2 O 0.51044(8) 0.37387(8) 0.76592(12) 0.0497(4) Uani 1 1 d . . . . .
H2 H 0.5370(15) 0.3964(15) 0.808(2) 0.080 Uiso 1 1 d . U . . .
O3 O 0.46652(7) 0.25295(7) 0.76043(10) 0.0439(3) Uani 1 1 d . . . . .
H3 H 0.4021(16) 0.2287(14) 0.746(2) 0.080 Uiso 1 1 d . U . . .
O4 O 0.51012(6) 0.32353(6) 0.60803(9) 0.0288(3) Uani 1 1 d . . . . .
O5 O 0.34750(9) 0.21123(10) 0.72692(16) 0.0687(5) Uani 1 1 d . . . . .
H5A H 0.333333 0.166667 0.666667 0.080 Uiso 1 2 d S U P . .
H5B H 0.3275(16) 0.1982(17) 0.777(2) 0.080 Uiso 1 1 d . U . . .
C1 C 0.46438(8) 0.27713(8) 0.54215(12) 0.0262(4) Uani 1 1 d . . . . .
C2 C 0.41192(9) 0.28517(9) 0.51491(13) 0.0295(4) Uani 1 1 d . . . . .
C3 C 0.37003(10) 0.24311(11) 0.44264(15) 0.0414(5) Uani 1 1 d . . . . .
H3A H 0.333683 0.246760 0.422397 0.050 Uiso 1 1 calc R U . . .
C4 C 0.38025(11) 0.19617(12) 0.39978(16) 0.0491(6) Uani 1 1 d . . . . .
H4 H 0.351449 0.168426 0.349772 0.059 Uiso 1 1 calc R U . . .
C5 C 0.43227(11) 0.18942(11) 0.42941(16) 0.0445(5) Uani 1 1 d . . . . .
H5 H 0.438602 0.156749 0.399601 0.053 Uiso 1 1 calc R U . . .
C6 C 0.47566(9) 0.22964(9) 0.50223(13) 0.0333(4) Uani 1 1 d . . . . .
C7 C 0.40284(9) 0.33863(10) 0.56016(14) 0.0355(4) Uani 1 1 d . . . . .
H7 H 0.418708 0.344861 0.630521 0.043 Uiso 1 1 calc R U . . .
C8 C 0.44444(13) 0.40224(12) 0.5052(2) 0.0588(6) Uani 1 1 d . . . . .
H8A H 0.440175 0.436934 0.537425 0.088 Uiso 1 1 calc R U . . .
H8B H 0.429958 0.397694 0.435834 0.088 Uiso 1 1 calc R U . . .
H8C H 0.490007 0.413086 0.507026 0.088 Uiso 1 1 calc R U . . .
C9 C 0.33193(12) 0.32216(14) 0.5629(2) 0.0606(7) Uani 1 1 d . . . . .
H9A H 0.315875 0.318880 0.494693 0.091 Uiso 1 1 calc R U . . .
H9B H 0.328707 0.356423 0.598585 0.091 Uiso 1 1 calc R U . . .
H9C H 0.305721 0.280601 0.597260 0.091 Uiso 1 1 calc R U . . .
C10 C 0.53148(10) 0.21948(10) 0.53548(16) 0.0408(5) Uani 1 1 d . . . . .
H10 H 0.559685 0.255862 0.581581 0.049 Uiso 1 1 calc R U . . .
C11 C 0.57348(15) 0.22164(17) 0.4478(2) 0.0721(8) Uani 1 1 d . . . . .
H11A H 0.589366 0.262717 0.411763 0.108 Uiso 1 1 calc R U . . .
H11B H 0.547512 0.185265 0.402708 0.108 Uiso 1 1 calc R U . . .
H11C H 0.610500 0.218325 0.472576 0.108 Uiso 1 1 calc R U . . .
C12 C 0.50557(14) 0.15653(14) 0.5931(2) 0.0687(8) Uani 1 1 d . . . . .
H12A H 0.541908 0.151051 0.614897 0.103 Uiso 1 1 calc R U . . .
H12B H 0.476583 0.120014 0.550277 0.103 Uiso 1 1 calc R U . . .
H12C H 0.481452 0.157784 0.651510 0.103 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.2428(12) 2_655 ?
Dy1 O1 2.2427(12) 17_556 ?
Dy1 O1 2.2428(12) 18_546 ?
Dy1 O1 2.2428(12) 3_665 ?
Dy1 O1 2.2428(12) 16_656 ?
Dy1 O1 2.2428(12) . ?
P1 O1 1.4889(12) . ?
P1 O2 1.5524(15) . ?
P1 O3 1.5056(15) . ?
P1 O4 1.5842(13) . ?
O2 H2 0.81(3) . ?
O3 H3 1.35(3) . ?
O4 C1 1.407(2) . ?
O5 H3 1.18(3) . ?
O5 H5A 1.238(2) . ?
O5 H5B 0.79(3) . ?
C1 C2 1.401(2) . ?
C1 C6 1.391(3) . ?
C2 C3 1.391(3) . ?
C2 C7 1.518(3) . ?
C3 H3A 0.9500 . ?
C3 C4 1.380(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.395(3) . ?
C6 C10 1.529(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.520(3) . ?
C7 C9 1.528(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.527(3) . ?
C10 C12 1.515(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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 O1 92.55(5) 2_655 3_665 ?
O1 Dy1 O1 92.55(5) 18_546 17_556 ?
O1 Dy1 O1 87.45(5) 18_546 . ?
O1 Dy1 O1 87.45(5) 2_655 16_656 ?
O1 Dy1 O1 92.55(5) 3_665 . ?
O1 Dy1 O1 87.45(5) 3_665 16_656 ?
O1 Dy1 O1 87.45(5) 3_665 17_556 ?
O1 Dy1 O1 87.45(5) 2_655 18_546 ?
O1 Dy1 O1 92.55(5) 2_655 . ?
O1 Dy1 O1 180.0 3_665 18_546 ?
O1 Dy1 O1 180.0 16_656 . ?
O1 Dy1 O1 92.55(5) 16_656 18_546 ?
O1 Dy1 O1 87.45(5) 17_556 . ?
O1 Dy1 O1 180.0 2_655 17_556 ?
O1 Dy1 O1 92.55(5) 16_656 17_556 ?
O1 P1 O2 111.22(8) . . ?
O1 P1 O3 114.60(8) . . ?
O1 P1 O4 108.47(7) . . ?
O2 P1 O4 101.64(8) . . ?
O3 P1 O2 111.02(10) . . ?
O3 P1 O4 109.04(7) . . ?
P1 O1 Dy1 154.36(8) . . ?
P1 O2 H2 115(2) . . ?
P1 O3 H3 125.2(12) . . ?
C1 O4 P1 129.49(11) . . ?
H3 O5 H5A 102.9(14) . . ?
H3 O5 H5B 107(3) . . ?
H5A O5 H5B 111(3) . . ?
C2 C1 O4 116.64(15) . . ?
C6 C1 O4 119.41(15) . . ?
C6 C1 C2 123.77(16) . . ?
C1 C2 C7 121.23(16) . . ?
C3 C2 C1 116.72(17) . . ?
C3 C2 C7 122.03(16) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 C2 121.29(18) . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.19(19) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.31(19) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 116.70(17) . . ?
C1 C6 C10 123.37(17) . . ?
C5 C6 C10 119.92(18) . . ?
C2 C7 H7 107.5 . . ?
C2 C7 C8 110.13(17) . . ?
C2 C7 C9 113.29(18) . . ?
C8 C7 H7 107.5 . . ?
C8 C7 C9 110.61(19) . . ?
C9 C7 H7 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.7 . . ?
C11 C10 C6 111.94(18) . . ?
C11 C10 H10 107.7 . . ?
C12 C10 C6 110.41(18) . . ?
C12 C10 H10 107.7 . . ?
C12 C10 C11 111.3(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 O4 C1 C2 102.75(17) . . . . ?
P1 O4 C1 C6 -82.1(2) . . . . ?
O1 P1 O4 C1 121.81(14) . . . . ?
O2 P1 O1 Dy1 79.4(2) . . . . ?
O2 P1 O4 C1 -120.90(15) . . . . ?
O3 P1 O1 Dy1 -47.6(2) . . . . ?
O3 P1 O4 C1 -3.61(17) . . . . ?
O4 P1 O1 Dy1 -169.64(17) . . . . ?
O4 C1 C2 C3 174.08(16) . . . . ?
O4 C1 C2 C7 -4.1(2) . . . . ?
O4 C1 C6 C5 -173.33(17) . . . . ?
O4 C1 C6 C10 7.7(3) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C1 C2 C7 C8 83.1(2) . . . . ?
C1 C2 C7 C9 -152.45(19) . . . . ?
C1 C6 C10 C11 -125.7(2) . . . . ?
C1 C6 C10 C12 109.8(2) . . . . ?
C2 C1 C6 C5 1.5(3) . . . . ?
C2 C1 C6 C10 -177.44(18) . . . . ?
C2 C3 C4 C5 1.0(4) . . . . ?
C3 C2 C7 C8 -95.0(2) . . . . ?
C3 C2 C7 C9 29.5(3) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C5 C6 C1 -0.8(3) . . . . ?
C4 C5 C6 C10 178.1(2) . . . . ?
C5 C6 C10 C11 55.4(3) . . . . ?
C5 C6 C10 C12 -69.2(3) . . . . ?
C6 C1 C2 C3 -0.9(3) . . . . ?
C6 C1 C2 C7 -179.09(17) . . . . ?
C7 C2 C3 C4 177.8(2) . . . . ?

_olex2_exptl_crystal_mounting_method ESI
_olex2_submission_original_sample_id 1
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_adi-yb-hexa
_database_code_depnum_ccdc_archive 'CCDC 2069009'
loop_
_audit_author_name
_audit_author_address
'R Murugavel'
;IIT Bombay
India
;
_audit_update_record             
;
2024-03-21 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT355_adi-yb-hexa         
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O5       - H5B      .       1.08 Ang.
RESPONSE: Yes, this distance is marginally longer and is a consequence of partial protonation of the central water dimer
;
_vrf_PLAT420_adi-yb-hexa         
;
PROBLEM: D-H Bond Without Acceptor  O5       --H5B      .     Please Check
RESPONSE: H5B does not have any acceptor in the vicinity
;
# Added during the CSD deposition process: Thursday 21 March 2024 11:38 AM
# end Validation Reply Form

_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        2
_chemical_formula_moiety         'C72 H114 O24 P6 Yb, 3(H3 O2)'
_chemical_formula_sum            'C72 H123 O30 P6 Yb'
_chemical_formula_weight         1827.56
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
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                   23.5532(3)
_cell_length_b                   23.5532(3)
_cell_length_c                   13.4632(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6468.13(19)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    6976
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.1090
_cell_measurement_theta_min      2.4910
_shelx_estimated_absorpt_T_max   0.803
_shelx_estimated_absorpt_T_min   0.664
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2865
_exptl_crystal_preparation       esi
_exptl_crystal_recrystallization_method esi
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14642
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.505
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn 724+ ccd diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          esi
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2467
_reflns_number_total             2523
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0306
_refine_ls_restrained_S_all      1.080
_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)+(0.0251P)²+14.8839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0686
_refine_special_details          esi
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Uiso: H3(0.08) H2(0.08) H5A(0.08) H5B(0.08)
 Fixed X: H5B(0.805901)
 Fixed Y: H5B(0.6906)
 Fixed Z: H5B(0.7818)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.666667 0.333333 0.833333 0.02493(11) Uani 1 6 d S T P . .
P1 P 0.68418(4) 0.48056(4) 0.72413(6) 0.03237(19) Uani 1 1 d . . . . .
H3 H 0.758(2) 0.565(2) 0.750(3) 0.080 Uiso 1 1 d . U . . .
O1 O 0.67145(10) 0.41335(9) 0.74254(15) 0.0366(5) Uani 1 1 d . . . . .
O2 O 0.62943(15) 0.49092(13) 0.7676(2) 0.0596(8) Uani 1 1 d . . . . .
H2 H 0.608(2) 0.470(2) 0.809(3) 0.080 Uiso 1 1 d . U . . .
O3 O 0.75042(14) 0.53317(11) 0.75901(18) 0.0518(7) Uani 1 1 d . . . . .
O4 O 0.67793(9) 0.48918(9) 0.60892(14) 0.0314(4) Uani 1 1 d . . . . .
O5 O 0.78917(16) 0.65266(14) 0.7259(3) 0.0903(10) Uani 1 1 d . . . . .
H5A H 0.833333 0.666667 0.666667 0.080 Uiso 1 2 d S U P . .
H5B H 0.805901 0.690600 0.781800 0.080 Uiso 1 1 d . U . . .
C1 C 0.72422(13) 0.53532(13) 0.5428(2) 0.0289(6) Uani 1 1 d . . . . .
C2 C 0.71566(14) 0.58774(14) 0.5164(2) 0.0327(7) Uani 1 1 d . . . . .
C3 C 0.75796(16) 0.63038(16) 0.4446(2) 0.0449(8) Uani 1 1 d . . . . .
H3A H 0.754170 0.667082 0.424959 0.054 Uiso 1 1 calc R U . . .
C4 C 0.80505(18) 0.62034(18) 0.4017(3) 0.0558(10) Uani 1 1 d . . . . .
H4 H 0.832938 0.649579 0.351948 0.067 Uiso 1 1 calc R U . . .
C5 C 0.81207(17) 0.56839(17) 0.4303(3) 0.0491(9) Uani 1 1 d . . . . .
H5 H 0.845210 0.562412 0.400222 0.059 Uiso 1 1 calc R U . . .
C6 C 0.77176(15) 0.52408(15) 0.5024(2) 0.0367(7) Uani 1 1 d . . . . .
C7 C 0.66157(16) 0.59671(15) 0.5619(2) 0.0390(7) Uani 1 1 d . . . . .
H7 H 0.654863 0.580176 0.631735 0.047 Uiso 1 1 calc R U . . .
C8 C 0.59779(18) 0.5551(2) 0.5056(3) 0.0619(10) Uani 1 1 d . . . . .
H8A H 0.603281 0.569692 0.436307 0.093 Uiso 1 1 calc R U . . .
H8B H 0.562702 0.559915 0.536363 0.093 Uiso 1 1 calc R U . . .
H8C H 0.586335 0.509014 0.507926 0.093 Uiso 1 1 calc R U . . .
C9 C 0.6776(2) 0.66778(18) 0.5652(3) 0.0662(11) Uani 1 1 d . . . . .
H9A H 0.719575 0.694405 0.599148 0.099 Uiso 1 1 calc R U . . .
H9B H 0.642949 0.670635 0.601294 0.099 Uiso 1 1 calc R U . . .
H9C H 0.680495 0.684066 0.497341 0.099 Uiso 1 1 calc R U . . .
C10 C 0.78224(16) 0.46817(16) 0.5342(2) 0.0412(7) Uani 1 1 d . . . . .
H10 H 0.745435 0.439522 0.579899 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7798(2) 0.4259(2) 0.4469(3) 0.0736(12) Uani 1 1 d . . . . .
H11A H 0.738161 0.409598 0.411542 0.110 Uiso 1 1 calc R U . . .
H11B H 0.783544 0.388700 0.471430 0.110 Uiso 1 1 calc R U . . .
H11C H 0.816234 0.452150 0.401535 0.110 Uiso 1 1 calc R U . . .
C12 C 0.8457(2) 0.4933(2) 0.5925(3) 0.0677(11) Uani 1 1 d . . . . .
H12A H 0.882857 0.522448 0.550217 0.102 Uiso 1 1 calc R U . . .
H12B H 0.850492 0.456200 0.613885 0.102 Uiso 1 1 calc R U . . .
H12C H 0.844546 0.517592 0.650887 0.102 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.2015(18) 3_665 ?
Yb1 O1 2.2015(18) 17_556 ?
Yb1 O1 2.2014(18) . ?
Yb1 O1 2.2015(18) 2_655 ?
Yb1 O1 2.2016(18) 16_656 ?
Yb1 O1 2.2014(18) 18_546 ?
P1 H3 1.90(5) . ?
P1 O1 1.477(2) . ?
P1 O2 1.542(2) . ?
P1 O3 1.502(3) . ?
P1 O4 1.581(2) . ?
O2 H2 0.75(4) . ?
O3 H3 0.69(4) . ?
O4 C1 1.406(3) . ?
O5 H5A 1.218(4) . ?
O5 H5B 1.081(3) . ?
C1 C2 1.393(4) . ?
C1 C6 1.385(4) . ?
C2 C3 1.391(4) . ?
C2 C7 1.520(4) . ?
C3 H3A 0.9500 . ?
C3 C4 1.372(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(4) . ?
C6 C10 1.518(4) . ?
C7 H7 1.0000 . ?
C7 C8 1.523(5) . ?
C7 C9 1.522(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.524(5) . ?
C10 C12 1.521(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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 O1 92.15(7) 3_665 2_655 ?
O1 Yb1 O1 92.15(7) 16_656 17_556 ?
O1 Yb1 O1 87.85(7) . 18_546 ?
O1 Yb1 O1 87.85(7) 3_665 16_656 ?
O1 Yb1 O1 180.0 3_665 18_546 ?
O1 Yb1 O1 87.85(7) 2_655 16_656 ?
O1 Yb1 O1 180.0 2_655 17_556 ?
O1 Yb1 O1 92.15(7) 3_665 . ?
O1 Yb1 O1 87.85(7) . 17_556 ?
O1 Yb1 O1 92.15(7) 2_655 . ?
O1 Yb1 O1 92.15(7) 16_656 18_546 ?
O1 Yb1 O1 180.0 16_656 . ?
O1 Yb1 O1 92.15(7) 17_556 18_546 ?
O1 Yb1 O1 87.85(7) 3_665 17_556 ?
O1 Yb1 O1 87.85(7) 2_655 18_546 ?
O1 P1 H3 132.7(14) . . ?
O1 P1 O2 111.60(13) . . ?
O1 P1 O3 113.70(13) . . ?
O1 P1 O4 108.67(11) . . ?
O2 P1 H3 99.3(14) . . ?
O2 P1 O4 102.30(13) . . ?
O3 P1 H3 19.0(14) . . ?
O3 P1 O2 110.89(17) . . ?
O3 P1 O4 109.01(12) . . ?
O4 P1 H3 98.1(14) . . ?
P1 O1 Yb1 155.03(13) . . ?
P1 O2 H2 122(3) . . ?
P1 O3 H3 115(4) . . ?
C1 O4 P1 129.36(17) . . ?
H5A O5 H5B 108.9(2) . . ?
C2 C1 O4 116.5(2) . . ?
C6 C1 O4 119.3(2) . . ?
C6 C1 C2 123.9(3) . . ?
C1 C2 C7 121.6(3) . . ?
C3 C2 C1 116.6(3) . . ?
C3 C2 C7 121.8(3) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3A 119.4 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C5 116.4(3) . . ?
C1 C6 C10 123.5(3) . . ?
C5 C6 C10 120.1(3) . . ?
C2 C7 H7 107.7 . . ?
C2 C7 C8 109.7(3) . . ?
C2 C7 C9 113.6(3) . . ?
C8 C7 H7 107.7 . . ?
C9 C7 H7 107.7 . . ?
C9 C7 C8 110.1(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10 107.3 . . ?
C6 C10 C11 112.3(3) . . ?
C6 C10 C12 111.2(3) . . ?
C11 C10 H10 107.3 . . ?
C12 C10 H10 107.3 . . ?
C12 C10 C11 111.2(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 O4 C1 C2 -102.1(3) . . . . ?
P1 O4 C1 C6 82.7(3) . . . . ?
O1 P1 O4 C1 -122.6(2) . . . . ?
O2 P1 O1 Yb1 -75.6(3) . . . . ?
O2 P1 O4 C1 119.3(2) . . . . ?
O3 P1 O1 Yb1 50.8(3) . . . . ?
O3 P1 O4 C1 1.8(3) . . . . ?
O4 P1 O1 Yb1 172.4(3) . . . . ?
O4 C1 C2 C3 -174.6(3) . . . . ?
O4 C1 C2 C7 3.7(4) . . . . ?
O4 C1 C6 C5 174.0(3) . . . . ?
O4 C1 C6 C10 -7.4(4) . . . . ?
C1 C2 C3 C4 0.7(5) . . . . ?
C1 C2 C7 C8 -83.9(3) . . . . ?
C1 C2 C7 C9 152.4(3) . . . . ?
C1 C6 C10 C11 125.7(4) . . . . ?
C1 C6 C10 C12 -109.0(4) . . . . ?
C2 C1 C6 C5 -0.8(5) . . . . ?
C2 C1 C6 C10 177.8(3) . . . . ?
C2 C3 C4 C5 -1.1(6) . . . . ?
C3 C2 C7 C8 94.4(4) . . . . ?
C3 C2 C7 C9 -29.3(4) . . . . ?
C3 C4 C5 C6 0.6(6) . . . . ?
C4 C5 C6 C1 0.4(5) . . . . ?
C4 C5 C6 C10 -178.3(3) . . . . ?
C5 C6 C10 C11 -55.8(4) . . . . ?
C5 C6 C10 C12 69.5(4) . . . . ?
C6 C1 C2 C3 0.3(4) . . . . ?
C6 C1 C2 C7 178.6(3) . . . . ?
C7 C2 C3 C4 -177.6(3) . . . . ?

_olex2_exptl_crystal_mounting_method esi
_olex2_submission_original_sample_id 2
_olex2_submission_special_instructions 'No special instructions were received'
