# 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_gd
_database_code_depnum_ccdc_archive 'CCDC 2296556'
loop_
_audit_author_name
_audit_author_address
'NAUSHAD AHMED'
;TIFR Hyderabad
India
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_audit_creation_date             2024-04-28
_audit_creation_method           
;
Olex2 1.5-alpha
(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         'C13 H34 Gd N12 O12 P2, Cl, 1[CH3OH], 1[H2O]'
_chemical_formula_sum            'C14 H40 Cl Gd N12 O14 P2'
_chemical_formula_weight         855.22
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9642(6)
_cell_length_b                   13.9446(8)
_cell_length_c                   18.4472(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.725(5)
_cell_angle_gamma                90
_cell_volume                     3312.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13861
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.9860
_cell_measurement_theta_min      2.5150
_shelx_estimated_absorpt_T_max   0.674
_shelx_estimated_absorpt_T_min   0.637
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (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    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33646
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.507
_diffrn_ambient_temperature      293.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00 -10.00   0.50   14.95    --    7.20 -28.00-121.00   50
  2  ω    -14.00  11.00   0.50   14.95    --   -7.60  28.00  41.00   50
  3  ω    -50.00 -25.00   0.50   14.95    --   -7.60 -28.00-121.00   50
  4  ω     51.00  96.00   0.50   14.95    --    7.20  77.00-150.00   90
  5  ω     50.00  90.00   0.50   14.95    --    7.20  77.00  90.00   80
  6  ω     68.00  97.00   0.50   14.95    --    7.20  77.00-120.00   58
  7  ω    -62.00   2.00   0.50   14.95    --   -7.60 -82.00 -90.00  128
  8  ω    -40.00 -14.00   0.50   14.95    --   -7.60 -82.00  60.00   52
  9  ω     10.00  35.00   0.50   14.95    --   -7.60 -82.00  60.00   50
 10  ω    -61.00   8.00   0.50   14.95    --   -7.60 -82.00 -30.00  138
 11  ω    -36.00  -9.00   0.50   14.95    --   -7.60 -82.00-150.00   54
 12  ω      8.00  36.00   0.50   14.95    --   -7.60 -82.00 -90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4932
_reflns_number_total             5770
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.922
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.099
_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)+(0.0328P)²+23.1763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1216
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1-H1A
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 C1-H1A
 1.90228 with sigma of 0.02
 Gd1-H1A
 3.010024 with sigma of 0.02
 P1-H4
 1.942171 with sigma of 0.02
 Gd1-H4
 2.60943 with sigma of 0.02
 P2-H2
 1.941209 with sigma of 0.02
 Gd1-H2
 2.763712 with sigma of 0.02
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N7(H7)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C10(H10A,H10B,H10C), C1(H1B,H1C,H1D), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.30851(2) 0.61999(2) 0.23458(2) 0.03198(12) Uani 1 1 d D . . . .
P1 P 0.21301(13) 0.85739(12) 0.30031(9) 0.0324(4) Uani 1 1 d D . . . .
P2 P 0.42280(13) 0.84041(13) 0.18454(10) 0.0359(4) Uani 1 1 d D . . . .
Cl1 Cl -0.0696(2) 0.8567(3) 0.2076(2) 0.1243(14) Uani 1 1 d . . . . .
O5 O 0.2015(3) 0.9456(3) 0.2542(2) 0.0368(10) Uani 1 1 d . . . . .
O4 O 0.2268(4) 0.7673(3) 0.2599(3) 0.0417(11) Uani 1 1 d D . . . .
H4 H 0.177(4) 0.761(3) 0.226(3) 0.063 Uiso 1 1 d D U . . .
O3 O 0.4419(3) 0.8946(3) 0.2529(3) 0.0395(11) Uani 1 1 d . . . . .
O2 O 0.4147(4) 0.7346(3) 0.1896(3) 0.0450(12) Uani 1 1 d D . . . .
H2 H 0.471(3) 0.7104(14) 0.178(4) 0.068 Uiso 1 1 d D U . . .
O7 O 0.3239(4) 0.5590(4) 0.1096(3) 0.0526(13) Uani 1 1 d . . . . .
O10 O 0.4188(4) 0.6777(4) 0.3492(3) 0.0588(14) Uani 1 1 d . . . . .
O1W O 0.1294(4) 0.5774(4) 0.2372(4) 0.0632(16) Uani 1 1 d . . . . .
H1WA H 0.077271 0.615624 0.213400 0.095 Uiso 1 1 d R U . . .
H1WB H 0.112191 0.522684 0.262030 0.095 Uiso 1 1 d R U . . .
O9 O 0.2884(4) 0.5888(4) 0.3650(3) 0.0556(14) Uani 1 1 d . . . . .
N1 N 0.3206(4) 0.8851(4) 0.1334(3) 0.0400(13) Uani 1 1 d . . . . .
H1 H 0.274539 0.915861 0.154140 0.048 Uiso 1 1 calc R U . . .
O6 O 0.2093(4) 0.6674(4) 0.1135(3) 0.0588(14) Uani 1 1 d . . . . .
N7 N 0.3112(4) 0.8709(4) 0.3662(3) 0.0427(14) Uani 1 1 d . . . . .
H7 H 0.371439 0.882514 0.352955 0.051 Uiso 1 1 calc R U . . .
N6 N 0.1154(4) 0.8475(4) 0.3513(3) 0.0401(13) Uani 1 1 d . . . . .
N12 N 0.3667(5) 0.6346(4) 0.3928(3) 0.0445(14) Uani 1 1 d . . . . .
O1 O 0.4830(4) 0.5479(4) 0.2438(4) 0.0663(17) Uani 1 1 d D . . . .
H1A H 0.4920(17) 0.491(2) 0.260(5) 0.099 Uiso 1 1 d D U . . .
N3 N 0.5133(4) 0.8674(4) 0.1287(3) 0.0425(14) Uani 1 1 d . . . . .
O11 O 0.3907(5) 0.6401(5) 0.4586(3) 0.0733(18) Uani 1 1 d . . . . .
N11 N 0.2582(5) 0.6127(5) 0.0758(3) 0.0479(15) Uani 1 1 d . . . . .
N8 N 0.2153(6) 0.8589(4) 0.4680(4) 0.0540(17) Uani 1 1 d . . . . .
N2 N 0.3907(5) 0.8648(5) 0.0213(3) 0.0490(16) Uani 1 1 d . . . . .
O8 O 0.2411(5) 0.6095(6) 0.0092(3) 0.081(2) Uani 1 1 d . . . . .
N4 N 0.2138(5) 0.8770(5) 0.0238(4) 0.0533(16) Uani 1 1 d . . . . .
N9 N 0.0373(6) 0.8625(5) 0.4575(4) 0.0587(19) Uani 1 1 d . . . . .
C8 C 0.3047(6) 0.8652(5) 0.4394(4) 0.0460(17) Uani 1 1 d . . . . .
N5 N 0.5640(5) 0.8784(4) 0.0128(4) 0.0552(18) Uani 1 1 d . . . . .
C2 C 0.3072(6) 0.8744(5) 0.0591(4) 0.0440(17) Uani 1 1 d . . . . .
N10 N 0.3939(6) 0.8684(5) 0.4838(4) 0.0610(18) Uani 1 1 d . . . . .
C3 C 0.4863(6) 0.8704(5) 0.0546(4) 0.0446(18) Uani 1 1 d . . . . .
C9 C 0.1256(6) 0.8572(5) 0.4253(4) 0.0444(18) Uani 1 1 d . . . . .
C6 C 0.5406(8) 0.8869(6) -0.0666(5) 0.071(3) Uani 1 1 d . . . . .
H6A H 0.507787 0.829085 -0.085929 0.106 Uiso 1 1 calc R U . . .
H6B H 0.603920 0.896833 -0.087891 0.106 Uiso 1 1 calc R U . . .
H6C H 0.494863 0.940256 -0.078134 0.106 Uiso 1 1 calc R U . . .
C13 C -0.0637(7) 0.8604(7) 0.4162(6) 0.073(3) Uani 1 1 d . . . . .
H13A H -0.070131 0.912862 0.382325 0.110 Uiso 1 1 calc R U . . .
H13B H -0.116041 0.865827 0.448769 0.110 Uiso 1 1 calc R U . . .
H13C H -0.072541 0.800939 0.389945 0.110 Uiso 1 1 calc R U . . .
C4 C 0.1197(6) 0.8782(7) 0.0612(5) 0.066(2) Uani 1 1 d . . . . .
H4A H 0.128254 0.834966 0.101913 0.098 Uiso 1 1 calc R U . . .
H4B H 0.061142 0.858529 0.027756 0.098 Uiso 1 1 calc R U . . .
H4C H 0.108186 0.941939 0.078194 0.098 Uiso 1 1 calc R U . . .
C12 C 0.0433(8) 0.8733(7) 0.5364(5) 0.073(3) Uani 1 1 d . . . . .
H12A H 0.090609 0.826645 0.559657 0.110 Uiso 1 1 calc R U . . .
H12B H -0.024327 0.863709 0.551595 0.110 Uiso 1 1 calc R U . . .
H12C H 0.067494 0.936547 0.550022 0.110 Uiso 1 1 calc R U . . .
C10 C 0.4946(7) 0.8727(7) 0.4581(6) 0.075(3) Uani 1 1 d . . . . .
H10A H 0.502627 0.819082 0.426563 0.113 Uiso 1 1 calc R U . . .
H10B H 0.547710 0.870573 0.498953 0.113 Uiso 1 1 calc R U . . .
H10C H 0.500607 0.931281 0.431554 0.113 Uiso 1 1 calc R U . . .
C1 C 0.5811(7) 0.5936(9) 0.2462(6) 0.087(3) Uani 1 1 d D . . . .
H1B H 0.587701 0.622334 0.199723 0.131 Uiso 1 1 calc R U . . .
H1C H 0.635188 0.547122 0.257399 0.131 Uiso 1 1 calc R U . . .
H1D H 0.586651 0.642362 0.283256 0.131 Uiso 1 1 calc R U . . .
C7 C 0.6732(7) 0.8800(7) 0.0436(6) 0.075(3) Uani 1 1 d . . . . .
H7A H 0.683822 0.929964 0.079512 0.113 Uiso 1 1 calc R U . . .
H7B H 0.715992 0.891668 0.005480 0.113 Uiso 1 1 calc R U . . .
H7C H 0.691440 0.819291 0.066188 0.113 Uiso 1 1 calc R U . . .
C11 C 0.3909(10) 0.8578(9) 0.5622(5) 0.098(4) Uani 1 1 d . . . . .
H11A H 0.328381 0.886320 0.575493 0.148 Uiso 1 1 calc R U . . .
H11B H 0.450050 0.889174 0.587992 0.148 Uiso 1 1 calc R U . . .
H11C H 0.392191 0.790922 0.574572 0.148 Uiso 1 1 calc R U . . .
C5 C 0.1967(9) 0.8724(9) -0.0552(5) 0.094(4) Uani 1 1 d . . . . .
H5A H 0.154061 0.925382 -0.073498 0.140 Uiso 1 1 calc R U . . .
H5B H 0.162496 0.813295 -0.069923 0.140 Uiso 1 1 calc R U . . .
H5C H 0.262246 0.875497 -0.074529 0.140 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O5 2.445(4) 2_545 ?
Gd1 O4 2.383(4) . ?
Gd1 H4 2.604(17) . ?
Gd1 O2 2.325(4) . ?
Gd1 O7 2.487(5) . ?
Gd1 O10 2.541(6) . ?
Gd1 O1W 2.403(5) . ?
Gd1 O9 2.488(5) . ?
Gd1 O6 2.532(5) . ?
Gd1 O1 2.463(5) . ?
P1 O5 1.493(5) . ?
P1 O4 1.482(5) . ?
P1 N7 1.665(6) . ?
P1 N6 1.669(5) . ?
P2 O3 1.466(5) . ?
P2 O2 1.482(5) . ?
P2 N1 1.655(6) . ?
P2 N3 1.691(5) . ?
O4 H4 0.849(10) . ?
O2 H2 0.849(9) . ?
O7 N11 1.246(8) . ?
O10 N12 1.261(8) . ?
O1W H1WA 0.9299 . ?
O1W H1WB 0.9302 . ?
O9 N12 1.257(8) . ?
N1 H1 0.8600 . ?
N1 C2 1.370(9) . ?
O6 N11 1.253(8) . ?
N7 H7 0.8600 . ?
N7 C8 1.364(9) . ?
N6 C9 1.363(9) . ?
N12 O11 1.220(8) . ?
O1 H1A 0.859(10) . ?
O1 C1 1.418(10) . ?
N3 C3 1.371(10) . ?
N11 O8 1.224(8) . ?
N8 C8 1.332(10) . ?
N8 C9 1.326(11) . ?
N2 C2 1.360(9) . ?
N2 C3 1.320(10) . ?
N4 C2 1.306(10) . ?
N4 C4 1.470(11) . ?
N4 C5 1.450(11) . ?
N9 C9 1.353(9) . ?
N9 C13 1.436(12) . ?
N9 C12 1.456(11) . ?
C8 N10 1.338(10) . ?
N5 C3 1.344(9) . ?
N5 C6 1.466(12) . ?
N5 C7 1.463(12) . ?
N10 C10 1.443(12) . ?
N10 C11 1.457(12) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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 Gd1 H4 135.8(15) 2_545 . ?
O5 Gd1 O7 75.45(16) 2_545 . ?
O5 Gd1 O10 105.97(17) 2_545 . ?
O5 Gd1 O9 74.45(17) 2_545 . ?
O5 Gd1 O6 107.92(18) 2_545 . ?
O5 Gd1 O1 69.26(17) 2_545 . ?
O4 Gd1 O5 144.27(15) . 2_545 ?
O4 Gd1 H4 19.0(2) . . ?
O4 Gd1 O7 124.22(18) . . ?
O4 Gd1 O10 77.49(18) . . ?
O4 Gd1 O1W 75.90(18) . . ?
O4 Gd1 O9 82.07(18) . . ?
O4 Gd1 O6 75.88(18) . . ?
O4 Gd1 O1 139.82(18) . . ?
O2 Gd1 O5 138.90(15) . 2_545 ?
O2 Gd1 O4 76.83(16) . . ?
O2 Gd1 H4 82.6(18) . . ?
O2 Gd1 O7 77.86(18) . . ?
O2 Gd1 O10 77.29(18) . . ?
O2 Gd1 O1W 142.29(18) . . ?
O2 Gd1 O9 126.75(18) . . ?
O2 Gd1 O6 76.51(19) . . ?
O2 Gd1 O1 74.22(18) . . ?
O7 Gd1 H4 109.2(11) . . ?
O7 Gd1 O10 141.39(18) . . ?
O7 Gd1 O9 149.90(19) . . ?
O7 Gd1 O6 50.15(18) . . ?
O10 Gd1 H4 96.4(3) . . ?
O1W Gd1 O5 72.02(17) . 2_545 ?
O1W Gd1 H4 63.8(15) . . ?
O1W Gd1 O7 96.7(2) . . ?
O1W Gd1 O10 120.8(2) . . ?
O1W Gd1 O9 74.1(2) . . ?
O1W Gd1 O6 71.9(2) . . ?
O1W Gd1 O1 141.23(19) . . ?
O9 Gd1 H4 92.7(15) . . ?
O9 Gd1 O10 50.44(17) . . ?
O9 Gd1 O6 143.01(18) . . ?
O6 Gd1 H4 59.2(10) . . ?
O6 Gd1 O10 146.1(2) . . ?
O1 Gd1 H4 154.8(14) . . ?
O1 Gd1 O7 75.6(2) . . ?
O1 Gd1 O10 69.4(2) . . ?
O1 Gd1 O9 93.5(2) . . ?
O1 Gd1 O6 122.4(2) . . ?
O5 P1 N7 109.8(3) . . ?
O5 P1 N6 110.9(3) . . ?
O4 P1 O5 114.9(3) . . ?
O4 P1 N7 109.6(3) . . ?
O4 P1 N6 111.0(3) . . ?
N7 P1 N6 99.4(3) . . ?
O3 P2 O2 117.7(3) . . ?
O3 P2 N1 109.8(3) . . ?
O3 P2 N3 110.5(3) . . ?
O2 P2 N1 110.6(3) . . ?
O2 P2 N3 108.6(3) . . ?
N1 P2 N3 97.8(3) . . ?
P1 O5 Gd1 140.7(3) . 2 ?
Gd1 O4 H4 95.4(12) . . ?
P1 O4 Gd1 155.8(3) . . ?
P1 O4 H4 108.8(13) . . ?
Gd1 O2 H2 111.9(14) . . ?
P2 O2 Gd1 139.1(3) . . ?
P2 O2 H2 108.1(14) . . ?
N11 O7 Gd1 97.7(4) . . ?
N12 O10 Gd1 95.0(4) . . ?
Gd1 O1W H1WA 120.0 . . ?
Gd1 O1W H1WB 120.1 . . ?
H1WA O1W H1WB 120.0 . . ?
N12 O9 Gd1 97.8(4) . . ?
P2 N1 H1 119.1 . . ?
C2 N1 P2 121.8(5) . . ?
C2 N1 H1 119.1 . . ?
N11 O6 Gd1 95.3(4) . . ?
P1 N7 H7 117.1 . . ?
C8 N7 P1 125.8(5) . . ?
C8 N7 H7 117.1 . . ?
C9 N6 P1 124.4(5) . . ?
O9 N12 O10 116.7(6) . . ?
O11 N12 O10 120.7(7) . . ?
O11 N12 O9 122.5(6) . . ?
Gd1 O1 H1A 119.3(17) . . ?
C1 O1 Gd1 129.2(6) . . ?
C1 O1 H1A 108.9(18) . . ?
C3 N3 P2 119.9(5) . . ?
O7 N11 O6 116.7(6) . . ?
O8 N11 O7 120.9(7) . . ?
O8 N11 O6 122.3(7) . . ?
C9 N8 C8 120.6(6) . . ?
C3 N2 C2 121.0(7) . . ?
C2 N4 C4 122.6(7) . . ?
C2 N4 C5 121.5(8) . . ?
C5 N4 C4 115.7(7) . . ?
C9 N9 C13 122.1(7) . . ?
C9 N9 C12 119.7(8) . . ?
C13 N9 C12 118.1(7) . . ?
N8 C8 N7 123.6(7) . . ?
N8 C8 N10 119.3(7) . . ?
N10 C8 N7 117.1(7) . . ?
C3 N5 C6 120.0(8) . . ?
C3 N5 C7 122.3(8) . . ?
C7 N5 C6 117.7(7) . . ?
N2 C2 N1 120.6(7) . . ?
N4 C2 N1 119.8(7) . . ?
N4 C2 N2 119.6(7) . . ?
C8 N10 C10 123.4(7) . . ?
C8 N10 C11 118.9(8) . . ?
C10 N10 C11 117.5(8) . . ?
N2 C3 N3 125.4(6) . . ?
N2 C3 N5 117.6(7) . . ?
N5 C3 N3 117.0(7) . . ?
N8 C9 N6 125.0(6) . . ?
N8 C9 N9 117.8(7) . . ?
N9 C9 N6 117.2(7) . . ?
N5 C6 H6A 109.5 . . ?
N5 C6 H6B 109.5 . . ?
N5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N9 C13 H13A 109.5 . . ?
N9 C13 H13B 109.5 . . ?
N9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C12 H12A 109.5 . . ?
N9 C12 H12B 109.5 . . ?
N9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N10 C10 H10A 109.5 . . ?
N10 C10 H10B 109.5 . . ?
N10 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N5 C7 H7A 109.5 . . ?
N5 C7 H7B 109.5 . . ?
N5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N10 C11 H11A 109.5 . . ?
N10 C11 H11B 109.5 . . ?
N10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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 H1WB O3 0.93 1.93 2.725(7) 142.6 2_545 yes
N1 H1 O5 0.86 2.21 2.977(7) 148.4 . yes
N7 H7 O3 0.86 2.16 2.859(7) 138.3 . yes
O1 H1A Cl1 0.859(10) 2.170(13) 2.990(7) 160(3) 2_545 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O7 N11 O6 -3.9(7) . . . . ?
Gd1 O7 N11 O8 178.0(6) . . . . ?
Gd1 O10 N12 O9 -2.2(6) . . . . ?
Gd1 O10 N12 O11 179.7(6) . . . . ?
Gd1 O9 N12 O10 2.3(7) . . . . ?
Gd1 O9 N12 O11 -179.7(6) . . . . ?
Gd1 O6 N11 O7 3.8(7) . . . . ?
Gd1 O6 N11 O8 -178.1(7) . . . . ?
P1 N7 C8 N8 -8.2(10) . . . . ?
P1 N7 C8 N10 173.4(5) . . . . ?
P1 N6 C9 N8 -12.5(10) . . . . ?
P1 N6 C9 N9 169.7(5) . . . . ?
P2 N1 C2 N2 -28.0(9) . . . . ?
P2 N1 C2 N4 154.6(6) . . . . ?
P2 N3 C3 N2 8.3(10) . . . . ?
P2 N3 C3 N5 -170.6(5) . . . . ?
O5 P1 O4 Gd1 128.5(7) . . . . ?
O5 P1 N7 C8 121.6(6) . . . . ?
O5 P1 N6 C9 -111.2(6) . . . . ?
O4 P1 O5 Gd1 -172.9(3) . . . 2 ?
O4 P1 N7 C8 -111.2(6) . . . . ?
O4 P1 N6 C9 119.7(6) . . . . ?
O3 P2 O2 Gd1 63.8(6) . . . . ?
O3 P2 N1 C2 155.5(5) . . . . ?
O3 P2 N3 C3 -144.9(5) . . . . ?
O2 P2 N1 C2 -73.0(6) . . . . ?
O2 P2 N3 C3 84.6(6) . . . . ?
N1 P2 O2 Gd1 -63.6(5) . . . . ?
N1 P2 N3 C3 -30.3(6) . . . . ?
N7 P1 O5 Gd1 -48.7(5) . . . 2 ?
N7 P1 O4 Gd1 4.2(8) . . . . ?
N7 P1 N6 C9 4.4(6) . . . . ?
N7 C8 N10 C10 -3.2(11) . . . . ?
N7 C8 N10 C11 -177.0(8) . . . . ?
N6 P1 O5 Gd1 60.2(5) . . . 2 ?
N6 P1 O4 Gd1 -104.7(7) . . . . ?
N6 P1 N7 C8 5.2(7) . . . . ?
N3 P2 O2 Gd1 -169.8(4) . . . . ?
N3 P2 N1 C2 40.3(6) . . . . ?
N8 C8 N10 C10 178.3(8) . . . . ?
N8 C8 N10 C11 4.5(12) . . . . ?
C8 N8 C9 N6 10.0(11) . . . . ?
C8 N8 C9 N9 -172.1(7) . . . . ?
C2 N2 C3 N3 13.3(11) . . . . ?
C2 N2 C3 N5 -167.8(7) . . . . ?
C3 N2 C2 N1 -3.5(10) . . . . ?
C3 N2 C2 N4 173.9(7) . . . . ?
C9 N8 C8 N7 0.4(11) . . . . ?
C9 N8 C8 N10 178.8(7) . . . . ?
C6 N5 C3 N3 -177.0(6) . . . . ?
C6 N5 C3 N2 4.0(10) . . . . ?
C13 N9 C9 N6 -1.4(11) . . . . ?
C13 N9 C9 N8 -179.4(7) . . . . ?
C4 N4 C2 N1 -8.4(11) . . . . ?
C4 N4 C2 N2 174.2(7) . . . . ?
C12 N9 C9 N6 -179.8(7) . . . . ?
C12 N9 C9 N8 2.2(11) . . . . ?
C7 N5 C3 N3 2.4(10) . . . . ?
C7 N5 C3 N2 -176.6(7) . . . . ?
C5 N4 C2 N1 175.8(8) . . . . ?
C5 N4 C2 N2 -1.6(12) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 92 electrons were 
found in a volume of 520Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH], 1[H2O] per formula unit 
which account for 112 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 -0.751 0.750 259.5 46.2 '2 CH3OH,2 H2O'
2 -0.250 -0.570 0.250 259.5 46.4 '2 CH3OH,2 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;
_vrf_PLAT420_gd                  
;
PROBLEM: D-H Bond Without Acceptor O1W --H1WA . Please Check
RESPONSE: The acceptor moiety of D-H belongs to lattice solvent
molecule which is involved in disorder and therefore squeezed.
;
####################################################################### 
# 
# 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_tb
_database_code_depnum_ccdc_archive 'CCDC 2296557'
loop_
_audit_author_name
_audit_author_address
'NAUSHAD AHMED'
;TIFR Hyderabad
India
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_audit_creation_date             2024-04-28
_audit_creation_method           
;
Olex2 1.5-alpha
(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         'C13 H34 N12 O12 P2 Tb, Cl, 2(C H4 O)'
_chemical_formula_sum            'C15 H42 Cl N12 O14 P2 Tb'
_chemical_formula_weight         870.91
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9417(3)
_cell_length_b                   13.8877(4)
_cell_length_c                   18.2069(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.507(2)
_cell_angle_gamma                90
_cell_volume                     3244.29(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21785
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.0310
_cell_measurement_theta_min      2.9290
_shelx_estimated_absorpt_T_max   0.726
_shelx_estimated_absorpt_T_min   0.592
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41550
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.613
_diffrn_reflns_theta_min         2.691
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00 -17.00   0.50   12.94    --    7.10 -40.00-141.00   50
  2  ω      7.00  32.00   0.50   12.94    --    7.10  40.00  12.00   50
  3  ω    -24.00   2.00   0.50   12.94    --   -7.50  40.00  12.00   52
  4  ω    -56.00 -31.00   0.50   12.94    --   -7.50 -40.00-141.00   50
  5  ω     51.00  89.00   0.50   12.94    --    7.10  77.00 120.00   76
  6  ω     57.00  82.00   0.50   12.94    --    7.10  77.00 -90.00   50
  7  ω     58.00  83.00   0.50   12.94    --    7.10  77.00  60.00   50
  8  ω     50.00  96.00   0.50   12.94    --    7.10  77.00-180.00   92
  9  ω     50.00  96.00   0.50   12.94    --    7.10  77.00-120.00   92
 10  ω     55.00  81.00   0.50   12.94    --    7.10  77.00  30.00   52
 11  ω     50.00  95.00   0.50   12.94    --    7.10  77.00 -60.00   90
 12  ω    -31.00  14.00   0.50   12.94    --   -7.50 -77.00  30.00   90
 13  ω    -60.00  25.00   0.50   12.94    --   -7.50 -82.00-180.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6751
_reflns_number_total             7738
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.879
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7738
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.054
_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)+(0.0370P)²+5.8675P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0867
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.02
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 O4-H4
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.34 with sigma of 0.04
 C1-H1
 1.923963 with sigma of 0.02
 Tb1-H1
 2.96708 with sigma of 0.02
 P2-H4
 1.945033 with sigma of 0.02
 Tb1-H4
 2.608988 with sigma of 0.02
 P1-H2
 1.948274 with sigma of 0.02
 Tb1-H2
 2.743654 with sigma of 0.02
3.a Riding coordinates:
 O14(H14)
3.b Free rotating group:
 O1W(H1WA,H1WB)
3.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N1(H1A)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C1(H1B,H1C,H1D), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
3.e Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.30407(2) 0.12058(2) 0.23087(2) 0.01038(6) Uani 1 1 d D . . . .
P2 P 0.20928(6) 0.35686(6) 0.29856(4) 0.01030(16) Uani 1 1 d D . . . .
P1 P 0.41790(6) 0.34052(6) 0.18330(5) 0.01166(16) Uani 1 1 d D . . . .
Cl1 Cl -0.07466(7) 0.36747(7) 0.19884(6) 0.0306(2) Uani 1 1 d . . . . .
O5 O 0.19924(16) 0.44691(16) 0.25262(12) 0.0123(4) Uani 1 1 d . . . . .
O3 O 0.43825(17) 0.39186(16) 0.25511(13) 0.0144(5) Uani 1 1 d . . . . .
O10 O 0.41544(18) 0.17754(18) 0.34605(13) 0.0203(5) Uani 1 1 d . . . . .
O1 O 0.48001(18) 0.05375(17) 0.23688(15) 0.0212(5) Uani 1 1 d D . . . .
H1 H 0.4891(15) -0.0025(14) 0.258(2) 0.032 Uiso 1 1 d D U . . .
O2 O 0.40824(17) 0.23359(16) 0.18511(13) 0.0150(5) Uani 1 1 d D . . . .
H2 H 0.4630(16) 0.2092(12) 0.172(2) 0.023 Uiso 1 1 d D U . . .
O4 O 0.22059(17) 0.26634(16) 0.25672(12) 0.0134(4) Uani 1 1 d D . . . .
H4 H 0.1655(15) 0.2557(17) 0.2274(17) 0.020 Uiso 1 1 d D U . . .
O7 O 0.31532(18) 0.05677(17) 0.10732(13) 0.0173(5) Uani 1 1 d . . . . .
O1W O 0.12781(18) 0.07248(17) 0.22659(15) 0.0208(5) Uani 1 1 d DG . . . .
H1WA H 0.103365 0.017981 0.237117 0.031 Uiso 1 1 d DG U . . .
H1WB H 0.067910 0.110189 0.232539 0.031 Uiso 1 1 d DG U . . .
O6 O 0.20580(18) 0.17400(18) 0.10713(13) 0.0199(5) Uani 1 1 d . . . . .
O9 O 0.27997(19) 0.09340(19) 0.36179(14) 0.0214(5) Uani 1 1 d . . . . .
N12 N 0.3594(2) 0.13901(19) 0.39017(15) 0.0126(5) Uani 1 1 d . . . . .
O11 O 0.3814(2) 0.1478(2) 0.45787(14) 0.0261(6) Uani 1 1 d . . . . .
O8 O 0.2340(2) 0.1095(2) 0.00223(15) 0.0283(6) Uani 1 1 d . . . . .
N8 N 0.3078(2) 0.36681(19) 0.36748(16) 0.0150(6) Uani 1 1 d . . . . .
H8 H 0.369252 0.374473 0.355185 0.018 Uiso 1 1 calc R U . . .
N7 N 0.2095(2) 0.3579(2) 0.46891(15) 0.0161(6) Uani 1 1 d . . . . .
N6 N 0.1109(2) 0.3493(2) 0.34914(15) 0.0145(5) Uani 1 1 d . . . . .
N3 N 0.5080(2) 0.36954(19) 0.12818(16) 0.0142(6) Uani 1 1 d . . . . .
N11 N 0.2508(2) 0.1135(2) 0.07036(17) 0.0169(6) Uani 1 1 d . . . . .
N1 N 0.3148(2) 0.38918(19) 0.13162(16) 0.0143(6) Uani 1 1 d . . . . .
H1A H 0.269159 0.420099 0.152705 0.017 Uiso 1 1 calc R U . . .
N2 N 0.3835(2) 0.3695(2) 0.01833(17) 0.0174(6) Uani 1 1 d . . . . .
N9 N 0.0318(2) 0.3640(2) 0.45520(17) 0.0184(6) Uani 1 1 d . . . . .
N10 N 0.3872(2) 0.3686(2) 0.48798(17) 0.0204(6) Uani 1 1 d . . . . .
N5 N 0.5593(2) 0.37995(19) 0.01167(18) 0.0196(6) Uani 1 1 d . . . . .
N4 N 0.2062(2) 0.3847(2) 0.02046(17) 0.0193(6) Uani 1 1 d . . . . .
C9 C 0.2996(3) 0.3639(2) 0.44119(19) 0.0148(6) Uani 1 1 d . . . . .
C2 C 0.3022(3) 0.3804(2) 0.05634(19) 0.0149(7) Uani 1 1 d . . . . .
C8 C 0.1200(3) 0.3581(2) 0.42447(18) 0.0147(6) Uani 1 1 d . . . . .
C3 C 0.4814(3) 0.3731(2) 0.0525(2) 0.0161(7) Uani 1 1 d . . . . .
C5 C 0.1139(3) 0.3859(3) 0.0594(2) 0.0218(8) Uani 1 1 d . . . . .
H5A H 0.123632 0.341507 0.100170 0.033 Uiso 1 1 calc R U . . .
H5B H 0.053703 0.367256 0.025857 0.033 Uiso 1 1 calc R U . . .
H5C H 0.103821 0.449557 0.077685 0.033 Uiso 1 1 calc R U . . .
C7 C 0.5380(3) 0.3872(3) -0.0689(2) 0.0231(8) Uani 1 1 d . . . . .
H7A H 0.540165 0.324240 -0.090306 0.035 Uiso 1 1 calc R U . . .
H7B H 0.589602 0.427459 -0.086797 0.035 Uiso 1 1 calc R U . . .
H7C H 0.470173 0.414837 -0.082477 0.035 Uiso 1 1 calc R U . . .
C1 C 0.5787(3) 0.1024(3) 0.2428(2) 0.0269(8) Uani 1 1 d D . . . .
H1B H 0.586534 0.132411 0.196340 0.040 Uiso 1 1 calc R U . . .
H1C H 0.633879 0.056657 0.255158 0.040 Uiso 1 1 calc R U . . .
H1D H 0.581702 0.150575 0.280804 0.040 Uiso 1 1 calc R U . . .
C11 C 0.0341(3) 0.3748(3) 0.5351(2) 0.0260(8) Uani 1 1 d . . . . .
H11A H 0.011610 0.315970 0.555632 0.039 Uiso 1 1 calc R U . . .
H11B H -0.011610 0.426245 0.545060 0.039 Uiso 1 1 calc R U . . .
H11C H 0.103861 0.389390 0.557053 0.039 Uiso 1 1 calc R U . . .
C12 C 0.3836(4) 0.3618(3) 0.5678(2) 0.0340(10) Uani 1 1 d . . . . .
H12A H 0.323059 0.395006 0.580013 0.051 Uiso 1 1 calc R U . . .
H12B H 0.445096 0.390675 0.593897 0.051 Uiso 1 1 calc R U . . .
H12C H 0.380230 0.295355 0.581727 0.051 Uiso 1 1 calc R U . . .
C4 C 0.1860(3) 0.3845(3) -0.0604(2) 0.0305(9) Uani 1 1 d . . . . .
H4A H 0.250949 0.385763 -0.080521 0.046 Uiso 1 1 calc R U . . .
H4B H 0.145646 0.440292 -0.077001 0.046 Uiso 1 1 calc R U . . .
H4C H 0.148018 0.327431 -0.076947 0.046 Uiso 1 1 calc R U . . .
C6 C 0.6684(3) 0.3788(3) 0.0450(2) 0.0250(8) Uani 1 1 d . . . . .
H6A H 0.680825 0.431053 0.079549 0.038 Uiso 1 1 calc R U . . .
H6B H 0.712651 0.385604 0.006947 0.038 Uiso 1 1 calc R U . . .
H6C H 0.683370 0.318850 0.070526 0.038 Uiso 1 1 calc R U . . .
C10 C -0.0695(3) 0.3630(3) 0.4103(2) 0.0264(8) Uani 1 1 d . . . . .
H10A H -0.073493 0.415018 0.375297 0.040 Uiso 1 1 calc R U . . .
H10B H -0.123093 0.370386 0.441635 0.040 Uiso 1 1 calc R U . . .
H10C H -0.078842 0.302914 0.384160 0.040 Uiso 1 1 calc R U . . .
C13 C 0.4900(3) 0.3698(3) 0.4620(2) 0.0270(8) Uani 1 1 d . . . . .
H13A H 0.496159 0.315211 0.430485 0.040 Uiso 1 1 calc R U . . .
H13B H 0.543434 0.366859 0.503809 0.040 Uiso 1 1 calc R U . . .
H13C H 0.497543 0.427954 0.434770 0.040 Uiso 1 1 calc R U . . .
O14 O 0.6958(3) 0.3656(3) 0.22575(19) 0.0518(10) Uani 1 1 d . . . . .
H14 H 0.636066 0.367433 0.204240 0.078 Uiso 1 1 d R U . . .
C15 C 0.6927(4) 0.3653(5) 0.3030(3) 0.0518(15) Uani 1 1 d . . . . .
H15A H 0.621696 0.360097 0.312560 0.078 Uiso 1 1 calc R U . . .
H15B H 0.722255 0.424152 0.324009 0.078 Uiso 1 1 calc R U . . .
H15C H 0.732001 0.311630 0.324908 0.078 Uiso 1 1 calc R U . . .
O12 O -0.0406(2) 0.1696(3) 0.2599(2) 0.0461(8) Uani 1 1 d . . . . .
H12 H -0.049530 0.219381 0.235701 0.069 Uiso 1 1 calc R U . . .
C14 C -0.1385(4) 0.1224(4) 0.2613(3) 0.0500(14) Uani 1 1 d . . . . .
H14A H -0.184244 0.137938 0.217001 0.075 Uiso 1 1 calc R U . . .
H14B H -0.169165 0.143650 0.303735 0.075 Uiso 1 1 calc R U . . .
H14C H -0.127922 0.054052 0.263995 0.075 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
Tb1 O5 2.432(2) 2_545 ?
Tb1 O10 2.512(2) . ?
Tb1 O1 2.448(2) . ?
Tb1 O2 2.295(2) . ?
Tb1 O4 2.370(2) . ?
Tb1 O7 2.440(2) . ?
Tb1 O1W 2.368(2) . ?
Tb1 O6 2.548(2) . ?
Tb1 O9 2.473(2) . ?
P2 O5 1.501(2) . ?
P2 O4 1.487(2) . ?
P2 N8 1.674(3) . ?
P2 N6 1.669(3) . ?
P1 O3 1.482(2) . ?
P1 O2 1.491(2) . ?
P1 N3 1.684(3) . ?
P1 N1 1.672(3) . ?
O10 N12 1.269(4) . ?
O1 H1 0.870(15) . ?
O1 C1 1.437(4) . ?
O2 H2 0.847(9) . ?
O4 H4 0.846(9) . ?
O7 N11 1.274(4) . ?
O1W H1WA 0.8518 . ?
O1W H1WB 0.9534 . ?
O6 N11 1.263(4) . ?
O9 N12 1.259(4) . ?
N12 O11 1.234(4) . ?
O8 N11 1.232(4) . ?
N8 H8 0.8600 . ?
N8 C9 1.361(5) . ?
N7 C9 1.331(5) . ?
N7 C8 1.324(4) . ?
N6 C8 1.367(4) . ?
N3 C3 1.377(5) . ?
N1 H1A 0.8600 . ?
N1 C2 1.364(5) . ?
N2 C2 1.341(5) . ?
N2 C3 1.338(5) . ?
N9 C8 1.337(4) . ?
N9 C11 1.458(5) . ?
N9 C10 1.452(5) . ?
N10 C9 1.328(4) . ?
N10 C12 1.463(5) . ?
N10 C13 1.468(5) . ?
N5 C3 1.332(5) . ?
N5 C7 1.460(5) . ?
N5 C6 1.463(5) . ?
N4 C2 1.328(5) . ?
N4 C5 1.467(5) . ?
N4 C4 1.462(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O14 H14 0.8199 . ?
O14 C15 1.412(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
O12 H12 0.8200 . ?
O12 C14 1.429(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?

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 Tb1 O10 103.10(8) 2_545 . ?
O5 Tb1 O1 69.49(7) 2_545 . ?
O5 Tb1 O7 75.99(8) 2_545 . ?
O5 Tb1 O6 112.53(7) 2_545 . ?
O5 Tb1 O9 73.92(8) 2_545 . ?
O10 Tb1 O6 144.28(8) . . ?
O1 Tb1 O10 69.71(8) . . ?
O1 Tb1 O6 120.25(8) . . ?
O1 Tb1 O9 97.63(9) . . ?
O2 Tb1 O5 138.05(8) . 2_545 ?
O2 Tb1 O10 77.73(8) . . ?
O2 Tb1 O1 71.85(8) . . ?
O2 Tb1 O4 78.04(8) . . ?
O2 Tb1 O7 78.76(8) . . ?
O2 Tb1 O1W 142.17(8) . . ?
O2 Tb1 O6 74.28(8) . . ?
O2 Tb1 O9 127.46(8) . . ?
O4 Tb1 O5 143.77(7) . 2_545 ?
O4 Tb1 O10 77.99(8) . . ?
O4 Tb1 O1 139.48(8) . . ?
O4 Tb1 O7 125.24(8) . . ?
O4 Tb1 O6 74.89(7) . . ?
O4 Tb1 O9 79.68(8) . . ?
O7 Tb1 O10 141.92(8) . . ?
O7 Tb1 O1 74.71(8) . . ?
O7 Tb1 O6 51.22(7) . . ?
O7 Tb1 O9 149.71(8) . . ?
O1W Tb1 O5 72.05(8) . 2_545 ?
O1W Tb1 O10 124.15(9) . . ?
O1W Tb1 O1 141.33(8) . . ?
O1W Tb1 O4 77.61(8) . . ?
O1W Tb1 O7 92.32(9) . . ?
O1W Tb1 O6 71.69(8) . . ?
O1W Tb1 O9 75.31(8) . . ?
O9 Tb1 O10 51.27(8) . . ?
O9 Tb1 O6 141.75(8) . . ?
O5 P2 N8 110.55(13) . . ?
O5 P2 N6 110.05(13) . . ?
O4 P2 O5 115.23(13) . . ?
O4 P2 N8 109.71(13) . . ?
O4 P2 N6 111.28(14) . . ?
N6 P2 N8 98.80(14) . . ?
O3 P1 O2 117.73(14) . . ?
O3 P1 N3 110.70(14) . . ?
O3 P1 N1 109.80(14) . . ?
O2 P1 N3 108.56(13) . . ?
O2 P1 N1 110.61(13) . . ?
N1 P1 N3 97.58(14) . . ?
P2 O5 Tb1 139.41(13) . 2 ?
N12 O10 Tb1 94.73(17) . . ?
Tb1 O1 H1 115.6(14) . . ?
C1 O1 Tb1 129.6(2) . . ?
C1 O1 H1 108.7(14) . . ?
Tb1 O2 H2 112.4(12) . . ?
P1 O2 Tb1 138.07(14) . . ?
P1 O2 H2 108.5(12) . . ?
Tb1 O4 H4 95.4(11) . . ?
P2 O4 Tb1 154.37(13) . . ?
P2 O4 H4 109.9(11) . . ?
N11 O7 Tb1 98.53(19) . . ?
Tb1 O1W H1WA 128.9 . . ?
Tb1 O1W H1WB 129.4 . . ?
H1WA O1W H1WB 97.5 . . ?
N11 O6 Tb1 93.64(18) . . ?
N12 O9 Tb1 96.88(18) . . ?
O9 N12 O10 117.1(3) . . ?
O11 N12 O10 120.9(3) . . ?
O11 N12 O9 122.0(3) . . ?
P2 N8 H8 117.0 . . ?
C9 N8 P2 125.9(2) . . ?
C9 N8 H8 117.0 . . ?
C8 N7 C9 120.5(3) . . ?
C8 N6 P2 125.2(2) . . ?
C3 N3 P1 120.2(2) . . ?
O6 N11 O7 116.6(3) . . ?
O8 N11 O7 121.4(3) . . ?
O8 N11 O6 122.0(3) . . ?
P1 N1 H1A 119.6 . . ?
C2 N1 P1 120.7(2) . . ?
C2 N1 H1A 119.6 . . ?
C3 N2 C2 121.0(3) . . ?
C8 N9 C11 121.1(3) . . ?
C8 N9 C10 121.4(3) . . ?
C10 N9 C11 117.5(3) . . ?
C9 N10 C12 119.9(3) . . ?
C9 N10 C13 121.8(3) . . ?
C12 N10 C13 117.9(3) . . ?
C3 N5 C7 120.5(3) . . ?
C3 N5 C6 121.8(3) . . ?
C7 N5 C6 117.6(3) . . ?
C2 N4 C5 122.1(3) . . ?
C2 N4 C4 121.9(3) . . ?
C4 N4 C5 115.9(3) . . ?
N7 C9 N8 124.1(3) . . ?
N10 C9 N8 117.4(3) . . ?
N10 C9 N7 118.5(3) . . ?
N2 C2 N1 122.0(3) . . ?
N4 C2 N1 118.1(3) . . ?
N4 C2 N2 119.9(3) . . ?
N7 C8 N6 124.5(3) . . ?
N7 C8 N9 118.1(3) . . ?
N9 C8 N6 117.3(3) . . ?
N2 C3 N3 124.2(3) . . ?
N5 C3 N3 116.9(3) . . ?
N5 C3 N2 118.9(3) . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 C7 H7A 109.5 . . ?
N5 C7 H7B 109.5 . . ?
N5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
O1 C1 H1D 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
N9 C11 H11A 109.5 . . ?
N9 C11 H11B 109.5 . . ?
N9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N10 C12 H12A 109.5 . . ?
N10 C12 H12B 109.5 . . ?
N10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N5 C6 H6A 109.5 . . ?
N5 C6 H6B 109.5 . . ?
N5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N9 C10 H10A 109.5 . . ?
N9 C10 H10B 109.5 . . ?
N9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N10 C13 H13A 109.5 . . ?
N10 C13 H13B 109.5 . . ?
N10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 O14 H14 109.2 . . ?
O14 C15 H15A 109.5 . . ?
O14 C15 H15B 109.5 . . ?
O14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 O12 H12 109.5 . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14B 109.5 . . ?
O12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
Tb1 O10 N12 O9 -0.1(3) . . . . ?
Tb1 O10 N12 O11 -178.8(3) . . . . ?
Tb1 O7 N11 O6 -2.3(3) . . . . ?
Tb1 O7 N11 O8 177.4(3) . . . . ?
Tb1 O6 N11 O7 2.2(3) . . . . ?
Tb1 O6 N11 O8 -177.6(3) . . . . ?
Tb1 O9 N12 O10 0.1(3) . . . . ?
Tb1 O9 N12 O11 178.8(3) . . . . ?
P2 N8 C9 N7 -4.0(5) . . . . ?
P2 N8 C9 N10 177.0(2) . . . . ?
P2 N6 C8 N7 -11.6(5) . . . . ?
P2 N6 C8 N9 170.7(2) . . . . ?
P1 N3 C3 N2 10.8(4) . . . . ?
P1 N3 C3 N5 -168.7(2) . . . . ?
P1 N1 C2 N2 -27.3(4) . . . . ?
P1 N1 C2 N4 154.0(2) . . . . ?
O5 P2 O4 Tb1 125.1(3) . . . . ?
O5 P2 N8 C9 118.0(3) . . . . ?
O5 P2 N6 C8 -111.2(3) . . . . ?
O3 P1 O2 Tb1 60.4(2) . . . . ?
O3 P1 N3 C3 -147.2(2) . . . . ?
O3 P1 N1 C2 156.2(2) . . . . ?
O2 P1 N3 C3 82.1(3) . . . . ?
O2 P1 N1 C2 -72.2(3) . . . . ?
O4 P2 O5 Tb1 -171.89(16) . . . 2 ?
O4 P2 N8 C9 -113.8(3) . . . . ?
O4 P2 N6 C8 119.8(3) . . . . ?
N8 P2 O5 Tb1 -46.8(2) . . . 2 ?
N8 P2 O4 Tb1 -0.4(4) . . . . ?
N8 P2 N6 C8 4.5(3) . . . . ?
N6 P2 O5 Tb1 61.3(2) . . . 2 ?
N6 P2 O4 Tb1 -108.7(3) . . . . ?
N6 P2 N8 C9 2.7(3) . . . . ?
N3 P1 O2 Tb1 -172.92(18) . . . . ?
N3 P1 N1 C2 41.0(3) . . . . ?
N1 P1 O2 Tb1 -67.0(2) . . . . ?
N1 P1 N3 C3 -32.7(3) . . . . ?
C9 N7 C8 N6 10.4(5) . . . . ?
C9 N7 C8 N9 -171.9(3) . . . . ?
C2 N2 C3 N3 12.8(5) . . . . ?
C2 N2 C3 N5 -167.7(3) . . . . ?
C8 N7 C9 N8 -2.6(5) . . . . ?
C8 N7 C9 N10 176.5(3) . . . . ?
C3 N2 C2 N1 -4.4(5) . . . . ?
C3 N2 C2 N4 174.3(3) . . . . ?
C5 N4 C2 N1 -8.1(5) . . . . ?
C5 N4 C2 N2 173.2(3) . . . . ?
C7 N5 C3 N3 -178.0(3) . . . . ?
C7 N5 C3 N2 2.4(5) . . . . ?
C11 N9 C8 N7 3.1(5) . . . . ?
C11 N9 C8 N6 -179.1(3) . . . . ?
C12 N10 C9 N8 -177.5(3) . . . . ?
C12 N10 C9 N7 3.4(5) . . . . ?
C4 N4 C2 N1 174.5(3) . . . . ?
C4 N4 C2 N2 -4.2(5) . . . . ?
C6 N5 C3 N3 3.0(4) . . . . ?
C6 N5 C3 N2 -176.5(3) . . . . ?
C10 N9 C8 N7 -179.0(3) . . . . ?
C10 N9 C8 N6 -1.1(5) . . . . ?
C13 N10 C9 N8 -4.4(5) . . . . ?
C13 N10 C9 N7 176.5(3) . . . . ?

_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
;
_vrf_PLAT974_tb                  
;
PROBLEM: Check Calcd Negative Resid. Density on Tb1 -1.84 eA-3 
RESPONSE: The residual density is around the heavy atom terbium, 
which might be caused by the improper absorption correction or the highly 
polarized electron densities. 
;
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 2296559'
loop_
_audit_author_name
_audit_author_address
'NAUSHAD AHMED'
;TIFR Hyderabad
India
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_audit_creation_date             2024-04-28
_audit_creation_method           
;
Olex2 1.5-alpha
(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         'C13 H34 Er N12 O12 P2, Cl, 2(C H4 O)'
_chemical_formula_sum            'C15 H42 Cl Er N12 O14 P2'
_chemical_formula_weight         879.25
_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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9252(3)
_cell_length_b                   13.7997(3)
_cell_length_c                   18.2660(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.052(2)
_cell_angle_gamma                90
_cell_volume                     3233.35(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14619
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.9270
_cell_measurement_theta_min      2.9530
_shelx_estimated_absorpt_T_max   0.642
_shelx_estimated_absorpt_T_min   0.524
_exptl_absorpt_coefficient_mu    2.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29965
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.919
_diffrn_reflns_theta_min         2.530
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     51.00  96.00   0.50    7.29    --    7.10  77.00  60.00   90
  2  ω     50.00  95.00   0.50    7.29    --    7.10  77.00  30.00   90
  3  ω     50.00  75.00   0.50    7.29    --    7.10  77.00 120.00   50
  4  ω    -28.00  -1.00   0.50    7.29    --   -7.50 -77.00-150.00   54
  5  ω    -76.00  31.00   0.50    7.29    --   -7.50 -77.00 150.00  214
  6  ω     -9.00  54.00   0.50    7.29    --   -7.50  57.00-120.00  126
  7  ω     -7.00  19.00   0.50    7.29    --   -7.50 -77.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6514
_reflns_number_total             7610
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_refine_diff_density_max         3.243
_refine_diff_density_min         -2.810
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7610
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0625P)²+4.7213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1103
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 P1-H2
 1.946318 with sigma of 0.02
 Er1-H2
 2.717119 with sigma of 0.02
 P2-H5
 1.950498 with sigma of 0.02
 Er1-H5
 2.840606 with sigma of 0.02
 Er1-H1WA \\sim Er1-H1WB
 with sigma of 0.02
3.a Riding coordinates:
 O2(H2), O1(H1), O3S(H3S)
3.b Free rotating group:
 O1W(H1WA,H1WB)
3.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N3(H3)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C), C1(H1A,H1B,H1C),
 C12(H12A,H12B,H12C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C),
 C11(H11A,H11B,H11C), C3S(H3SA,H3SB,H3SC), C15(H15A,H15B,H15C)
3.e Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.69535(2) 0.12193(2) 0.26900(2) 0.01170(8) Uani 1 1 d D . . . .
P1 P 0.58296(7) 0.34105(7) 0.31776(5) 0.01232(19) Uani 1 1 d D . . . .
P2 P 0.71013(7) -0.14209(7) 0.29870(5) 0.01186(19) Uani 1 1 d D . . . .
Cl1 Cl 0.42569(10) -0.13204(9) 0.19758(9) 0.0395(3) Uani 1 1 d . . . . .
O5 O 0.69983(19) -0.05184(19) 0.25315(14) 0.0136(5) Uani 1 1 d D . . . .
H5 H 0.689(4) -0.0679(13) 0.2081(6) 0.020 Uiso 1 1 d D U . . .
O3 O 0.5628(2) 0.39365(19) 0.24644(15) 0.0161(6) Uani 1 1 d . . . . .
O2 O 0.59240(19) 0.23363(18) 0.31526(14) 0.0145(5) Uani 1 1 d D . . . .
H2 H 0.541153 0.205480 0.327170 0.022 Uiso 1 1 d DR U . . .
O4 O 0.7221(2) -0.23337(19) 0.25676(15) 0.0160(5) Uani 1 1 d . . . . .
O10 O 0.7177(2) 0.0934(2) 0.14018(16) 0.0223(6) Uani 1 1 d . . . . .
O6 O 0.6857(2) 0.05790(19) 0.39022(15) 0.0182(6) Uani 1 1 d . . . . .
O7 O 0.7933(2) 0.1766(2) 0.38968(16) 0.0211(6) Uani 1 1 d . . . . .
O9 O 0.5846(2) 0.1810(2) 0.15731(15) 0.0212(6) Uani 1 1 d . . . . .
O1 O 0.5228(2) 0.0540(2) 0.26285(17) 0.0229(6) Uani 1 1 d . . . . .
H1 H 0.514998 -0.001536 0.247114 0.034 Uiso 1 1 d R U . . .
O1W O 0.8691(2) 0.0742(2) 0.27196(18) 0.0218(6) Uani 1 1 d G . . . .
H1WA H 0.889936 0.018554 0.260231 0.033 Uiso 1 1 d DG U . . .
H1WB H 0.921273 0.111065 0.269756 0.033 Uiso 1 1 d DG U . . .
O8 O 0.7666(3) 0.1117(2) 0.49424(19) 0.0300(8) Uani 1 1 d . . . . .
N1 N 0.6856(3) 0.3903(2) 0.36887(19) 0.0151(7) Uani 1 1 d . . . . .
N12 N 0.6388(3) 0.1411(2) 0.11209(19) 0.0163(7) Uani 1 1 d . . . . .
N8 N 0.6108(3) -0.1506(2) 0.34888(18) 0.0157(7) Uani 1 1 d . . . . .
O11 O 0.6163(3) 0.1488(2) 0.04493(16) 0.0269(7) Uani 1 1 d . . . . .
N6 N 0.8074(3) -0.1320(2) 0.36742(19) 0.0163(7) Uani 1 1 d . . . . .
H6 H 0.868969 -0.124259 0.355060 0.020 Uiso 1 1 calc R U . . .
N11 N 0.7490(3) 0.1154(2) 0.4264(2) 0.0171(7) Uani 1 1 d . . . . .
N3 N 0.4925(3) 0.3691(2) 0.37351(19) 0.0148(7) Uani 1 1 d . . . . .
H3 H 0.429596 0.381064 0.354529 0.018 Uiso 1 1 calc R U . . .
N2 N 0.6156(3) 0.3690(2) 0.4822(2) 0.0182(7) Uani 1 1 d . . . . .
N7 N 0.7079(3) -0.1402(2) 0.46839(19) 0.0181(7) Uani 1 1 d . . . . .
N5 N 0.7935(3) 0.3846(2) 0.4801(2) 0.0207(8) Uani 1 1 d . . . . .
N9 N 0.5300(3) -0.1355(3) 0.4547(2) 0.0204(8) Uani 1 1 d . . . . .
N10 N 0.8853(3) -0.1297(2) 0.4874(2) 0.0241(8) Uani 1 1 d . . . . .
N4 N 0.4406(3) 0.3796(2) 0.4895(2) 0.0215(8) Uani 1 1 d . . . . .
C2 C 0.6973(3) 0.3804(3) 0.4437(2) 0.0167(8) Uani 1 1 d . . . . .
C8 C 0.7993(3) -0.1348(3) 0.4407(2) 0.0173(8) Uani 1 1 d . . . . .
C3 C 0.5177(4) 0.3730(2) 0.4485(2) 0.0170(8) Uani 1 1 d . . . . .
O3S O 0.3059(3) 0.3647(4) 0.2753(2) 0.0596(14) Uani 1 1 d . . . . .
H3S H 0.244903 0.365529 0.283292 0.089 Uiso 1 1 d R U . . .
C9 C 0.6192(3) -0.1410(3) 0.4243(2) 0.0156(8) Uani 1 1 d . . . . .
C7 C 0.4610(4) 0.3865(3) 0.5699(2) 0.0241(10) Uani 1 1 d . . . . .
H7A H 0.441234 0.327009 0.591531 0.036 Uiso 1 1 calc R U . . .
H7B H 0.421257 0.439009 0.586719 0.036 Uiso 1 1 calc R U . . .
H7C H 0.533935 0.398168 0.584161 0.036 Uiso 1 1 calc R U . . .
C4 C 0.8856(3) 0.3868(3) 0.4410(3) 0.0228(9) Uani 1 1 d . . . . .
H4A H 0.879448 0.337873 0.403350 0.034 Uiso 1 1 calc R U . . .
H4B H 0.946775 0.374733 0.475191 0.034 Uiso 1 1 calc R U . . .
H4C H 0.891208 0.449340 0.418729 0.034 Uiso 1 1 calc R U . . .
C13 C 0.4289(4) -0.1368(3) 0.4101(3) 0.0279(10) Uani 1 1 d . . . . .
H13A H 0.425248 -0.084917 0.374888 0.042 Uiso 1 1 calc R U . . .
H13B H 0.375039 -0.128759 0.441417 0.042 Uiso 1 1 calc R U . . .
H13C H 0.419582 -0.197591 0.384597 0.042 Uiso 1 1 calc R U . . .
C1 C 0.4234(4) 0.1011(4) 0.2575(3) 0.0339(11) Uani 1 1 d . . . . .
H1A H 0.419041 0.148977 0.219087 0.051 Uiso 1 1 calc R U . . .
H1B H 0.415328 0.131902 0.303574 0.051 Uiso 1 1 calc R U . . .
H1C H 0.369073 0.054021 0.246181 0.051 Uiso 1 1 calc R U . . .
C12 C 0.5320(4) -0.1247(3) 0.5343(3) 0.0280(11) Uani 1 1 d . . . . .
H12A H 0.504319 -0.182183 0.554332 0.042 Uiso 1 1 calc R U . . .
H12B H 0.490429 -0.069882 0.544604 0.042 Uiso 1 1 calc R U . . .
H12C H 0.602511 -0.115082 0.556454 0.042 Uiso 1 1 calc R U . . .
C5 C 0.8129(4) 0.3828(3) 0.5604(3) 0.0321(11) Uani 1 1 d . . . . .
H5A H 0.747662 0.383252 0.580463 0.048 Uiso 1 1 calc R U . . .
H5B H 0.852838 0.438839 0.577483 0.048 Uiso 1 1 calc R U . . .
H5C H 0.851018 0.325261 0.576090 0.048 Uiso 1 1 calc R U . . .
C10 C 0.9889(4) -0.1281(3) 0.4615(3) 0.0286(10) Uani 1 1 d . . . . .
H10A H 0.996931 -0.184477 0.431873 0.043 Uiso 1 1 calc R U . . .
H10B H 1.041954 -0.127905 0.503160 0.043 Uiso 1 1 calc R U . . .
H10C H 0.995424 -0.070888 0.432465 0.043 Uiso 1 1 calc R U . . .
C6 C 0.3307(4) 0.3790(3) 0.4565(3) 0.0259(11) Uani 1 1 d . . . . .
H6A H 0.317922 0.433282 0.423797 0.039 Uiso 1 1 calc R U . . .
H6B H 0.286380 0.383204 0.494839 0.039 Uiso 1 1 calc R U . . .
H6C H 0.316273 0.319938 0.429314 0.039 Uiso 1 1 calc R U . . .
C11 C 0.8810(4) -0.1372(4) 0.5668(3) 0.0375(12) Uani 1 1 d . . . . .
H11A H 0.823793 -0.099229 0.579853 0.056 Uiso 1 1 calc R U . . .
H11B H 0.944989 -0.113479 0.592873 0.056 Uiso 1 1 calc R U . . .
H11C H 0.871375 -0.203711 0.579665 0.056 Uiso 1 1 calc R U . . .
C3S C 0.3092(5) 0.3655(6) 0.2002(4) 0.060(2) Uani 1 1 d . . . . .
H3SA H 0.274116 0.309209 0.178528 0.090 Uiso 1 1 calc R U . . .
H3SB H 0.380433 0.365128 0.190350 0.090 Uiso 1 1 calc R U . . .
H3SC H 0.275175 0.422802 0.179350 0.090 Uiso 1 1 calc R U . . .
O14 O 1.0407(3) 0.1708(4) 0.2400(3) 0.0601(12) Uani 1 1 d . . . . .
H14 H 1.050398 0.222195 0.262272 0.090 Uiso 1 1 calc R U . . .
C15 C 1.1380(7) 0.1219(5) 0.2389(4) 0.069(2) Uani 1 1 d . . . . .
H15A H 1.175909 0.151425 0.202703 0.103 Uiso 1 1 calc R U . . .
H15B H 1.125468 0.054939 0.226564 0.103 Uiso 1 1 calc R U . . .
H15C H 1.178096 0.126496 0.286612 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
Er1 O5 2.417(3) . ?
Er1 O2 2.266(2) . ?
Er1 O4 2.339(3) 2_655 ?
Er1 O10 2.438(3) . ?
Er1 O6 2.401(3) . ?
Er1 O7 2.519(3) . ?
Er1 O9 2.481(3) . ?
Er1 O1 2.409(3) . ?
Er1 O1W 2.335(3) . ?
P1 O3 1.486(3) . ?
P1 O2 1.489(3) . ?
P1 N1 1.670(3) . ?
P1 N3 1.687(3) . ?
P2 O5 1.495(3) . ?
P2 O4 1.492(3) . ?
P2 N8 1.671(3) . ?
P2 N6 1.670(4) . ?
O5 H5 0.846(9) . ?
O2 H2 0.8200 . ?
O10 N12 1.269(5) . ?
O6 N11 1.267(4) . ?
O7 N11 1.258(4) . ?
O9 N12 1.271(4) . ?
O1 H1 0.8202 . ?
O1 C1 1.434(5) . ?
O1W H1WA 0.8495 . ?
O1W H1WB 0.8498 . ?
O8 N11 1.233(5) . ?
N1 C2 1.364(5) . ?
N12 O11 1.230(4) . ?
N8 C9 1.375(5) . ?
N6 H6 0.8600 . ?
N6 C8 1.356(5) . ?
N3 H3 0.8600 . ?
N3 C3 1.370(6) . ?
N2 C2 1.348(6) . ?
N2 C3 1.339(6) . ?
N7 C8 1.343(5) . ?
N7 C9 1.317(6) . ?
N5 C2 1.336(6) . ?
N5 C4 1.463(6) . ?
N5 C5 1.458(6) . ?
N9 C9 1.342(5) . ?
N9 C13 1.452(6) . ?
N9 C12 1.460(6) . ?
N10 C8 1.317(6) . ?
N10 C10 1.474(6) . ?
N10 C11 1.462(6) . ?
N4 C3 1.319(5) . ?
N4 C7 1.463(6) . ?
N4 C6 1.473(6) . ?
O3S H3S 0.8199 . ?
O3S C3S 1.378(9) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C3S H3SA 0.9600 . ?
C3S H3SB 0.9600 . ?
C3S H3SC 0.9600 . ?
O14 H14 0.8200 . ?
O14 C15 1.430(8) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?

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 Er1 O10 73.56(9) . . ?
O5 Er1 O7 112.64(9) . . ?
O5 Er1 O9 104.32(9) . . ?
O2 Er1 O5 138.01(9) . . ?
O2 Er1 O4 78.33(9) . 2_655 ?
O2 Er1 O10 127.89(9) . . ?
O2 Er1 O6 78.88(9) . . ?
O2 Er1 O7 74.05(9) . . ?
O2 Er1 O9 77.14(9) . . ?
O2 Er1 O1 72.52(9) . . ?
O2 Er1 O1W 142.23(10) . . ?
O4 Er1 O5 143.58(8) 2_655 . ?
O4 Er1 O10 80.34(10) 2_655 . ?
O4 Er1 O6 125.19(9) 2_655 . ?
O4 Er1 O7 74.21(9) 2_655 . ?
O4 Er1 O9 77.61(9) 2_655 . ?
O4 Er1 O1 139.96(9) 2_655 . ?
O10 Er1 O7 141.86(9) . . ?
O10 Er1 O9 51.98(9) . . ?
O6 Er1 O5 75.53(9) . . ?
O6 Er1 O10 148.93(9) . . ?
O6 Er1 O7 51.74(9) . . ?
O6 Er1 O9 142.08(9) . . ?
O6 Er1 O1 75.35(10) . . ?
O9 Er1 O7 142.97(10) . . ?
O1 Er1 O5 69.14(9) . . ?
O1 Er1 O10 96.38(10) . . ?
O1 Er1 O7 121.35(10) . . ?
O1 Er1 O9 69.66(10) . . ?
O1W Er1 O5 71.68(9) . . ?
O1W Er1 O4 77.54(9) . 2_655 ?
O1W Er1 O10 75.47(10) . . ?
O1W Er1 O6 91.93(10) . . ?
O1W Er1 O7 71.67(10) . . ?
O1W Er1 O9 124.59(10) . . ?
O1W Er1 O1 140.67(10) . . ?
O3 P1 O2 117.76(16) . . ?
O3 P1 N1 109.45(17) . . ?
O3 P1 N3 110.91(16) . . ?
O2 P1 N1 111.10(16) . . ?
O2 P1 N3 108.20(15) . . ?
N1 P1 N3 97.54(17) . . ?
O5 P2 N8 110.00(16) . . ?
O5 P2 N6 110.88(16) . . ?
O4 P2 O5 115.18(16) . . ?
O4 P2 N8 110.92(16) . . ?
O4 P2 N6 109.90(16) . . ?
N6 P2 N8 98.74(17) . . ?
Er1 O5 H5 111.9(12) . . ?
P2 O5 Er1 139.63(16) . . ?
P2 O5 H5 108.4(12) . . ?
Er1 O2 H2 107.9 . . ?
P1 O2 Er1 137.97(15) . . ?
P1 O2 H2 113.1 . . ?
P2 O4 Er1 154.49(17) . 2_645 ?
N12 O10 Er1 97.0(2) . . ?
N11 O6 Er1 98.5(2) . . ?
N11 O7 Er1 93.0(2) . . ?
N12 O9 Er1 94.8(2) . . ?
Er1 O1 H1 117.0 . . ?
C1 O1 Er1 130.1(3) . . ?
C1 O1 H1 109.2 . . ?
Er1 O1W H1WA 125.7 . . ?
Er1 O1W H1WB 126.6 . . ?
H1WA O1W H1WB 104.6 . . ?
C2 N1 P1 120.1(3) . . ?
O10 N12 O9 116.2(3) . . ?
O11 N12 O10 121.9(3) . . ?
O11 N12 O9 122.0(3) . . ?
C9 N8 P2 124.8(3) . . ?
P2 N6 H6 116.6 . . ?
C8 N6 P2 126.7(3) . . ?
C8 N6 H6 116.6 . . ?
O7 N11 O6 116.7(3) . . ?
O8 N11 O6 121.7(3) . . ?
O8 N11 O7 121.6(3) . . ?
P1 N3 H3 119.5 . . ?
C3 N3 P1 121.1(3) . . ?
C3 N3 H3 119.5 . . ?
C3 N2 C2 120.8(4) . . ?
C9 N7 C8 120.7(4) . . ?
C2 N5 C4 121.5(4) . . ?
C2 N5 C5 122.3(4) . . ?
C5 N5 C4 116.2(4) . . ?
C9 N9 C13 121.9(4) . . ?
C9 N9 C12 120.4(4) . . ?
C13 N9 C12 117.7(4) . . ?
C8 N10 C10 121.4(4) . . ?
C8 N10 C11 120.4(4) . . ?
C11 N10 C10 117.8(4) . . ?
C3 N4 C7 121.2(4) . . ?
C3 N4 C6 121.6(4) . . ?
C7 N4 C6 117.2(4) . . ?
N2 C2 N1 122.5(4) . . ?
N5 C2 N1 118.4(4) . . ?
N5 C2 N2 119.1(4) . . ?
N7 C8 N6 123.4(4) . . ?
N10 C8 N6 118.4(4) . . ?
N10 C8 N7 118.1(4) . . ?
N2 C3 N3 123.6(4) . . ?
N4 C3 N3 117.8(4) . . ?
N4 C3 N2 118.6(4) . . ?
C3S O3S H3S 108.9 . . ?
N7 C9 N8 124.7(4) . . ?
N7 C9 N9 118.4(4) . . ?
N9 C9 N8 116.9(4) . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N9 C13 H13A 109.5 . . ?
N9 C13 H13B 109.5 . . ?
N9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N9 C12 H12A 109.5 . . ?
N9 C12 H12B 109.5 . . ?
N9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C5 H5A 109.5 . . ?
N5 C5 H5B 109.5 . . ?
N5 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N10 C10 H10A 109.5 . . ?
N10 C10 H10B 109.5 . . ?
N10 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C6 H6A 109.5 . . ?
N4 C6 H6B 109.5 . . ?
N4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N10 C11 H11A 109.5 . . ?
N10 C11 H11B 109.5 . . ?
N10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3S C3S H3SA 109.5 . . ?
O3S C3S H3SB 109.5 . . ?
O3S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
C15 O14 H14 109.5 . . ?
O14 C15 H15A 109.5 . . ?
O14 C15 H15B 109.5 . . ?
O14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
Er1 O10 N12 O9 0.1(3) . . . . ?
Er1 O10 N12 O11 179.6(3) . . . . ?
Er1 O6 N11 O7 -2.7(3) . . . . ?
Er1 O6 N11 O8 177.4(3) . . . . ?
Er1 O7 N11 O6 2.6(3) . . . . ?
Er1 O7 N11 O8 -177.6(3) . . . . ?
Er1 O9 N12 O10 -0.1(3) . . . . ?
Er1 O9 N12 O11 -179.6(3) . . . . ?
P1 N1 C2 N2 -27.9(5) . . . . ?
P1 N1 C2 N5 153.9(3) . . . . ?
P1 N3 C3 N2 9.7(5) . . . . ?
P1 N3 C3 N4 -169.2(3) . . . . ?
P2 N8 C9 N7 -12.1(6) . . . . ?
P2 N8 C9 N9 170.3(3) . . . . ?
P2 N6 C8 N7 -4.4(6) . . . . ?
P2 N6 C8 N10 177.2(3) . . . . ?
O5 P2 O4 Er1 125.6(3) . . . 2_645 ?
O5 P2 N8 C9 -110.7(3) . . . . ?
O5 P2 N6 C8 117.7(3) . . . . ?
O3 P1 O2 Er1 60.4(3) . . . . ?
O3 P1 N1 C2 156.3(3) . . . . ?
O3 P1 N3 C3 -146.6(3) . . . . ?
O2 P1 N1 C2 -72.0(3) . . . . ?
O2 P1 N3 C3 82.9(3) . . . . ?
O4 P2 O5 Er1 -171.99(18) . . . . ?
O4 P2 N8 C9 120.7(3) . . . . ?
O4 P2 N6 C8 -113.8(3) . . . . ?
N1 P1 O2 Er1 -66.9(3) . . . . ?
N1 P1 N3 C3 -32.3(3) . . . . ?
N8 P2 O5 Er1 61.8(3) . . . . ?
N8 P2 O4 Er1 -108.6(4) . . . 2_645 ?
N8 P2 N6 C8 2.3(4) . . . . ?
N6 P2 O5 Er1 -46.4(3) . . . . ?
N6 P2 O4 Er1 -0.5(4) . . . 2_645 ?
N6 P2 N8 C9 5.4(3) . . . . ?
N3 P1 O2 Er1 -172.9(2) . . . . ?
N3 P1 N1 C2 40.9(3) . . . . ?
C2 N2 C3 N3 13.5(6) . . . . ?
C2 N2 C3 N4 -167.6(3) . . . . ?
C8 N7 C9 N8 9.8(6) . . . . ?
C8 N7 C9 N9 -172.6(4) . . . . ?
C3 N2 C2 N1 -4.2(6) . . . . ?
C3 N2 C2 N5 174.0(3) . . . . ?
C9 N7 C8 N6 -1.5(6) . . . . ?
C9 N7 C8 N10 176.9(4) . . . . ?
C7 N4 C3 N3 -178.5(3) . . . . ?
C7 N4 C3 N2 2.5(5) . . . . ?
C4 N5 C2 N1 -8.1(5) . . . . ?
C4 N5 C2 N2 173.6(3) . . . . ?
C13 N9 C9 N8 -1.7(6) . . . . ?
C13 N9 C9 N7 -179.5(4) . . . . ?
C12 N9 C9 N8 -179.7(3) . . . . ?
C12 N9 C9 N7 2.6(6) . . . . ?
C5 N5 C2 N1 174.8(4) . . . . ?
C5 N5 C2 N2 -3.5(6) . . . . ?
C10 N10 C8 N6 -4.4(6) . . . . ?
C10 N10 C8 N7 177.1(4) . . . . ?
C6 N4 C3 N3 2.4(5) . . . . ?
C6 N4 C3 N2 -176.6(3) . . . . ?
C11 N10 C8 N6 -177.0(4) . . . . ?
C11 N10 C8 N7 4.6(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
;
_vrf_PLAT971_er                  
;
PROBLEM: Check Calcd Resid. Dens. 1.03Ang From Er1 3.19 eA-3 
PROBLEM: Check Calcd Resid. Dens. 0.93Ang From Er1 3.15 eA-3 
RESPONSE: The residual density is around the heavy atom erbium, 
which might be caused by the improper absorption correction or the highly 
polarized electron densities. 
;
_vrf_PLAT972_er                  
;
PROBLEM: Check Calcd Resid. Dens. 0.85Ang From Er1 -2.60 eA-3 
RESPONSE: The residual density is around the heavy atom erbium, 
which might be caused by the improper absorption correction or the highly 
polarized electron densities. 
;
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 2296558'
loop_
_audit_author_name
_audit_author_address
'NAUSHAD AHMED'
;TIFR Hyderabad
India
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_audit_creation_date             2024-04-28
_audit_creation_method           
;
Olex2 1.5-alpha
(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         'C13 H34 Dy N12 O12 P2, Cl, C H4 O, 1[CH3OH]'
_chemical_formula_sum            'C15 H42 Cl Dy N12 O14 P2'
_chemical_formula_weight         874.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O P Cl Dy '
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9512(3)
_cell_length_b                   13.8255(4)
_cell_length_c                   18.1765(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.668(3)
_cell_angle_gamma                90
_cell_volume                     3225.52(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21048
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.0180
_cell_measurement_theta_min      2.9550
_shelx_estimated_absorpt_T_max   0.640
_shelx_estimated_absorpt_T_min   0.565
_exptl_absorpt_coefficient_mu    2.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39612
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.036
_diffrn_reflns_theta_min         2.539
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.890
_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   8.00   0.50    6.59    --    7.20 -19.00 -61.00   50
  2  ω    -32.00  -7.00   0.50    6.59    --   -7.60 -19.00 -61.00   50
  3  ω    -32.00  -7.00   0.50    6.59    --   -7.60  19.00 106.00   50
  4  ω    -80.00  38.00   0.50    6.59    --    7.20 -57.00-120.00  236
  5  ω     51.00  83.00   0.50    6.59    --    7.20  77.00-120.00   64
  6  ω     71.00  97.00   0.50    6.59    --    7.20  77.00 -60.00   52
  7  ω    -62.00 -25.00   0.50    6.59    --    7.20 -82.00 150.00   74
  8  ω    -53.00  44.00   0.50    6.59    --    7.20 -82.00-150.00  194
  9  ω     -8.00  17.00   0.50    6.59    --    7.20 -82.00-120.00   50
 10  ω    -21.00   4.00   0.50    6.59    --   -7.60 -82.00  90.00   50
 11  ω    -62.00 -37.00   0.50    6.59    --   -7.60 -82.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180150000
_diffrn_orient_matrix_UB_12      0.0120773000
_diffrn_orient_matrix_UB_13      -0.0340216000
_diffrn_orient_matrix_UB_21      0.0513823000
_diffrn_orient_matrix_UB_22      0.0049829000
_diffrn_orient_matrix_UB_23      0.0187356000
_diffrn_orient_matrix_UB_31      0.0095389000
_diffrn_orient_matrix_UB_32      -0.0496083000
_diffrn_orient_matrix_UB_33      -0.0063948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6412
_reflns_number_total             7673
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.378
_refine_diff_density_min         -3.207
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0591
_refine_ls_restrained_S_all      1.159
_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)+(0.0322P)²+79.3250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1671
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 P1-H4
 1.956822 with sigma of 0.02
 Dy1-H4
 2.748928 with sigma of 0.02
 P2-H2
 1.959859 with sigma of 0.02
 Dy1-H2
 2.597923 with sigma of 0.02
3.a Riding coordinates:
 O1(H1), O1W(H1WA,H1WB), C1(H1A,H1B,H1C)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C1S(H1SA,H1SB,H1SC)
3.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.69550(3) 0.12168(3) 0.76936(2) 0.01405(11) Uani 1 1 d D . . . .
P1 P 0.58099(16) 0.34167(15) 0.81617(12) 0.0158(4) Uani 1 1 d D . . . .
P2 P 0.79001(15) 0.35797(14) 0.70115(11) 0.0139(4) Uani 1 1 d D . . . .
O1 O 0.5207(4) 0.0544(5) 0.7630(4) 0.0277(14) Uani 1 1 d . . . . .
H1 H 0.515458 0.004529 0.738373 0.042 Uiso 1 1 d R U . . .
O1W O 0.8711(5) 0.0748(5) 0.7728(4) 0.0260(14) Uani 1 1 d . . . . .
H1WA H 0.874894 0.013322 0.770852 0.039 Uiso 1 1 d R U . . .
H1WB H 0.904584 0.089432 0.814882 0.039 Uiso 1 1 d R U . . .
O2 O 0.7778(5) 0.2674(4) 0.7435(3) 0.0194(12) Uani 1 1 d D . . . .
H2 H 0.839(2) 0.251(3) 0.766(4) 0.029 Uiso 1 1 d D U . . .
O3 O 0.8003(4) 0.4481(4) 0.7475(3) 0.0166(11) Uani 1 1 d . . . . .
O4 O 0.5903(5) 0.2346(4) 0.8138(3) 0.0204(12) Uani 1 1 d D . . . .
H4 H 0.530(3) 0.2102(16) 0.820(5) 0.031 Uiso 1 1 d D U . . .
O5 O 0.5606(4) 0.3932(4) 0.7448(3) 0.0193(12) Uani 1 1 d . . . . .
O6 O 0.5853(5) 0.1786(5) 0.6544(3) 0.0229(13) Uani 1 1 d . . . . .
O7 O 0.7208(5) 0.0938(5) 0.6389(3) 0.0239(13) Uani 1 1 d . . . . .
O8 O 0.6184(5) 0.1477(5) 0.5424(3) 0.0268(14) Uani 1 1 d . . . . .
O9 O 0.7935(5) 0.1765(5) 0.8922(3) 0.0240(13) Uani 1 1 d . . . . .
O10 O 0.6842(5) 0.0580(4) 0.8925(3) 0.0219(12) Uani 1 1 d . . . . .
O11 O 0.7645(6) 0.1109(6) 0.9977(3) 0.0353(17) Uani 1 1 d . . . . .
N1 N 0.8879(5) 0.3498(5) 0.6503(4) 0.0161(13) Uani 1 1 d . . . . .
N2 N 0.7889(6) 0.3594(5) 0.5302(4) 0.0201(14) Uani 1 1 d . . . . .
N3 N 0.6913(6) 0.3684(5) 0.6321(4) 0.0210(14) Uani 1 1 d . . . . .
H3 H 0.628621 0.376708 0.644611 0.025 Uiso 1 1 calc R U . . .
N4 N 0.9675(6) 0.3646(6) 0.5448(4) 0.0255(16) Uani 1 1 d . . . . .
N5 N 0.6113(6) 0.3701(6) 0.5110(4) 0.0255(16) Uani 1 1 d . . . . .
N6 N 0.6846(5) 0.3900(5) 0.8681(4) 0.0180(14) Uani 1 1 d . . . . .
H6 H 0.730908 0.421965 0.846328 0.022 Uiso 1 1 calc R U . . .
N7 N 0.6158(6) 0.3692(5) 0.9814(4) 0.0241(16) Uani 1 1 d . . . . .
N8 N 0.4907(5) 0.3696(5) 0.8717(4) 0.0165(13) Uani 1 1 d . . . . .
N9 N 0.7934(6) 0.3847(6) 0.9793(4) 0.0240(15) Uani 1 1 d . . . . .
N10 N 0.4400(6) 0.3796(5) 0.9888(4) 0.0235(15) Uani 1 1 d . . . . .
N11 N 0.6393(5) 0.1402(5) 0.6093(4) 0.0180(14) Uani 1 1 d . . . . .
N12 N 0.7465(6) 0.1156(5) 0.9292(4) 0.0207(14) Uani 1 1 d . . . . .
C1 C 0.4213(8) 0.1010(9) 0.7565(6) 0.039(3) Uani 1 1 d . . . . .
H1A H 0.402140 0.112718 0.806155 0.058 Uiso 1 1 d R U . . .
H1B H 0.368550 0.059758 0.728335 0.058 Uiso 1 1 d R U . . .
H1C H 0.425180 0.162808 0.730645 0.058 Uiso 1 1 d R U . . .
C2 C 0.8779(7) 0.3588(6) 0.5743(5) 0.0209(17) Uani 1 1 d . . . . .
C3 C 0.6995(7) 0.3651(6) 0.5585(5) 0.0196(16) Uani 1 1 d . . . . .
C4 C 1.0694(7) 0.3647(8) 0.5897(6) 0.033(2) Uani 1 1 d . . . . .
H4A H 1.071478 0.415195 0.627744 0.049 Uiso 1 1 calc R U . . .
H4B H 1.123347 0.377392 0.557953 0.049 Uiso 1 1 calc R U . . .
H4C H 1.081949 0.301546 0.613757 0.049 Uiso 1 1 calc R U . . .
C5 C 0.9674(9) 0.3747(7) 0.4649(5) 0.032(2) Uani 1 1 d . . . . .
H5A H 0.999252 0.317361 0.445690 0.047 Uiso 1 1 calc R U . . .
H5B H 1.007237 0.432348 0.454839 0.047 Uiso 1 1 calc R U . . .
H5C H 0.895489 0.381230 0.440604 0.047 Uiso 1 1 calc R U . . .
C6 C 0.6149(10) 0.3608(9) 0.4311(6) 0.041(3) Uani 1 1 d . . . . .
H6A H 0.670941 0.401541 0.416838 0.061 Uiso 1 1 calc R U . . .
H6B H 0.548178 0.381398 0.403782 0.061 Uiso 1 1 calc R U . . .
H6C H 0.628117 0.293152 0.419115 0.061 Uiso 1 1 calc R U . . .
C7 C 0.5096(7) 0.3704(8) 0.5364(6) 0.032(2) Uani 1 1 d . . . . .
H7A H 0.506226 0.318252 0.572531 0.049 Uiso 1 1 calc R U . . .
H7B H 0.455409 0.360575 0.494027 0.049 Uiso 1 1 calc R U . . .
H7C H 0.498414 0.432716 0.559910 0.049 Uiso 1 1 calc R U . . .
C8 C 0.6985(7) 0.3809(6) 0.9437(5) 0.0197(16) Uani 1 1 d . . . . .
C9 C 0.5184(7) 0.3732(6) 0.9475(5) 0.0174(15) Uani 1 1 d . . . . .
C10 C 0.8859(7) 0.3864(7) 0.9407(5) 0.0256(19) Uani 1 1 d . . . . .
H10A H 0.869238 0.356447 0.891700 0.038 Uiso 1 1 calc R U . . .
H10B H 0.942467 0.350506 0.969777 0.038 Uiso 1 1 calc R U . . .
H10C H 0.907650 0.453575 0.934824 0.038 Uiso 1 1 calc R U . . .
C11 C 0.8135(8) 0.3844(8) 1.0607(5) 0.032(2) Uani 1 1 d . . . . .
H11A H 0.747279 0.389642 1.081012 0.048 Uiso 1 1 calc R U . . .
H11B H 0.858176 0.439318 1.077712 0.048 Uiso 1 1 calc R U . . .
H11C H 0.848299 0.323937 1.077758 0.048 Uiso 1 1 calc R U . . .
C12 C 0.4618(8) 0.3861(6) 1.0697(5) 0.0253(19) Uani 1 1 d . . . . .
H12A H 0.482729 0.322445 1.090229 0.038 Uiso 1 1 calc R U . . .
H12B H 0.399018 0.407669 1.089707 0.038 Uiso 1 1 calc R U . . .
H12C H 0.518190 0.432608 1.083428 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3317(7) 0.3775(8) 0.9559(6) 0.031(2) Uani 1 1 d . . . . .
H13A H 0.316989 0.433451 0.923097 0.046 Uiso 1 1 calc R U . . .
H13B H 0.286824 0.379698 0.995237 0.046 Uiso 1 1 calc R U . . .
H13C H 0.317956 0.317817 0.927112 0.046 Uiso 1 1 calc R U . . .
Cl1 Cl 1.07484(19) 0.3686(2) 0.80224(16) 0.0397(6) Uani 1 1 d . . . . .
O1S O 0.3034(7) 0.3601(11) 0.7753(5) 0.079(4) Uani 1 1 d . . . . .
H1S H 0.362596 0.374351 0.797345 0.119 Uiso 1 1 calc R U . . .
C1S C 0.3044(10) 0.3655(13) 0.6960(7) 0.063(4) Uani 1 1 d . . . . .
H1SA H 0.241980 0.334020 0.670424 0.094 Uiso 1 1 calc R U . . .
H1SB H 0.366649 0.332772 0.683080 0.094 Uiso 1 1 calc R U . . .
H1SC H 0.305426 0.433500 0.680807 0.094 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 2.436(6) . ?
Dy1 O1W 2.357(6) . ?
Dy1 O2 2.356(6) . ?
Dy1 O3 2.420(5) 2_646 ?
Dy1 O4 2.289(6) . ?
Dy1 O6 2.496(6) . ?
Dy1 O7 2.467(6) . ?
Dy1 O9 2.533(6) . ?
Dy1 O10 2.427(6) . ?
P1 O4 1.486(6) . ?
P1 O5 1.472(6) . ?
P1 N6 1.673(7) . ?
P1 N8 1.688(7) . ?
P2 O2 1.489(6) . ?
P2 O3 1.500(6) . ?
P2 N1 1.670(7) . ?
P2 N3 1.674(8) . ?
O1 H1 0.8198 . ?
O1 C1 1.431(12) . ?
O1W H1WA 0.8523 . ?
O1W H1WB 0.8521 . ?
O2 H2 0.874(10) . ?
O4 H4 0.874(10) . ?
O6 N11 1.263(9) . ?
O7 N11 1.290(9) . ?
O8 N11 1.214(9) . ?
O9 N12 1.280(9) . ?
O10 N12 1.260(10) . ?
O11 N12 1.238(10) . ?
N1 C2 1.375(11) . ?
N2 C2 1.313(12) . ?
N2 C3 1.330(11) . ?
N3 H3 0.8800 . ?
N3 C3 1.356(11) . ?
N4 C2 1.345(11) . ?
N4 C4 1.456(13) . ?
N4 C5 1.458(11) . ?
N5 C3 1.339(11) . ?
N5 C6 1.466(12) . ?
N5 C7 1.454(12) . ?
N6 H6 0.8800 . ?
N6 C8 1.369(11) . ?
N7 C8 1.356(11) . ?
N7 C9 1.328(12) . ?
N8 C9 1.377(11) . ?
N9 C8 1.311(12) . ?
N9 C10 1.467(11) . ?
N9 C11 1.468(11) . ?
N10 C9 1.344(10) . ?
N10 C12 1.463(12) . ?
N10 C13 1.450(12) . ?
C1 H1A 0.9801 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9803 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O1S H1S 0.8400 . ?
O1S C1S 1.445(16) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 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 O6 69.9(2) . . ?
O1 Dy1 O7 97.8(2) . . ?
O1 Dy1 O9 120.6(2) . . ?
O1W Dy1 O1 141.6(2) . . ?
O1W Dy1 O3 72.1(2) . 2_646 ?
O1W Dy1 O6 123.4(2) . . ?
O1W Dy1 O7 74.4(2) . . ?
O1W Dy1 O9 72.0(2) . . ?
O1W Dy1 O10 93.0(2) . . ?
O2 Dy1 O1 139.4(2) . . ?
O2 Dy1 O1W 77.3(2) . . ?
O2 Dy1 O3 143.55(19) . 2_646 ?
O2 Dy1 O6 77.7(2) . . ?
O2 Dy1 O7 79.7(2) . . ?
O2 Dy1 O9 74.5(2) . . ?
O2 Dy1 O10 125.3(2) . . ?
O3 Dy1 O1 69.6(2) 2_646 . ?
O3 Dy1 O6 103.1(2) 2_646 . ?
O3 Dy1 O7 73.5(2) 2_646 . ?
O3 Dy1 O9 113.0(2) 2_646 . ?
O3 Dy1 O10 76.24(19) 2_646 . ?
O4 Dy1 O1 71.6(2) . . ?
O4 Dy1 O1W 142.7(2) . . ?
O4 Dy1 O2 78.1(2) . . ?
O4 Dy1 O3 138.2(2) . 2_646 ?
O4 Dy1 O6 77.3(2) . . ?
O4 Dy1 O7 127.4(2) . . ?
O4 Dy1 O9 74.7(2) . . ?
O4 Dy1 O10 79.1(2) . . ?
O6 Dy1 O9 143.8(2) . . ?
O7 Dy1 O6 51.60(19) . . ?
O7 Dy1 O9 141.2(2) . . ?
O10 Dy1 O1 74.7(2) . . ?
O10 Dy1 O6 142.1(2) . . ?
O10 Dy1 O7 149.5(2) . . ?
O10 Dy1 O9 51.7(2) . . ?
O4 P1 N6 110.7(4) . . ?
O4 P1 N8 108.1(3) . . ?
O5 P1 O4 117.5(4) . . ?
O5 P1 N6 109.8(3) . . ?
O5 P1 N8 111.0(3) . . ?
N6 P1 N8 98.0(3) . . ?
O2 P2 O3 114.5(3) . . ?
O2 P2 N1 111.8(3) . . ?
O2 P2 N3 109.7(4) . . ?
O3 P2 N1 110.5(3) . . ?
O3 P2 N3 110.6(4) . . ?
N1 P2 N3 98.7(3) . . ?
Dy1 O1 H1 110.8 . . ?
C1 O1 Dy1 130.7(6) . . ?
C1 O1 H1 109.0 . . ?
Dy1 O1W H1WA 109.5 . . ?
Dy1 O1W H1WB 109.4 . . ?
H1WA O1W H1WB 104.4 . . ?
Dy1 O2 H2 95.3(13) . . ?
P2 O2 Dy1 154.7(4) . . ?
P2 O2 H2 107.9(14) . . ?
P2 O3 Dy1 139.0(3) . 2_656 ?
Dy1 O4 H4 111.6(15) . . ?
P1 O4 Dy1 138.1(3) . . ?
P1 O4 H4 107.6(16) . . ?
N11 O6 Dy1 96.1(5) . . ?
N11 O7 Dy1 96.7(4) . . ?
N12 O9 Dy1 92.8(5) . . ?
N12 O10 Dy1 98.4(5) . . ?
C2 N1 P2 125.0(6) . . ?
C2 N2 C3 120.2(7) . . ?
P2 N3 H3 117.1 . . ?
C3 N3 P2 125.8(6) . . ?
C3 N3 H3 117.1 . . ?
C2 N4 C4 122.8(8) . . ?
C2 N4 C5 121.1(9) . . ?
C4 N4 C5 116.1(8) . . ?
C3 N5 C6 119.9(8) . . ?
C3 N5 C7 121.8(8) . . ?
C7 N5 C6 117.7(8) . . ?
P1 N6 H6 119.4 . . ?
C8 N6 P1 121.2(6) . . ?
C8 N6 H6 119.4 . . ?
C9 N7 C8 121.7(8) . . ?
C9 N8 P1 119.8(6) . . ?
C8 N9 C10 122.4(7) . . ?
C8 N9 C11 121.7(8) . . ?
C10 N9 C11 115.9(8) . . ?
C9 N10 C12 120.5(8) . . ?
C9 N10 C13 122.0(8) . . ?
C13 N10 C12 117.5(7) . . ?
O6 N11 O7 115.6(7) . . ?
O8 N11 O6 123.0(7) . . ?
O8 N11 O7 121.4(7) . . ?
O10 N12 O9 116.9(7) . . ?
O11 N12 O9 121.6(8) . . ?
O11 N12 O10 121.4(7) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.7 . . ?
O1 C1 H1C 109.2 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 N1 124.8(7) . . ?
N2 C2 N4 119.4(8) . . ?
N4 C2 N1 115.8(8) . . ?
N2 C3 N3 124.7(8) . . ?
N2 C3 N5 117.7(8) . . ?
N5 C3 N3 117.5(8) . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 C6 H6A 109.5 . . ?
N5 C6 H6B 109.5 . . ?
N5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C7 H7A 109.5 . . ?
N5 C7 H7B 109.5 . . ?
N5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N7 C8 N6 120.7(8) . . ?
N9 C8 N6 118.8(7) . . ?
N9 C8 N7 120.5(8) . . ?
N7 C9 N8 124.6(7) . . ?
N7 C9 N10 119.0(8) . . ?
N10 C9 N8 116.4(8) . . ?
N9 C10 H10A 109.5 . . ?
N9 C10 H10B 109.5 . . ?
N9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N9 C11 H11A 109.5 . . ?
N9 C11 H11B 109.5 . . ?
N9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N10 C12 H12A 109.5 . . ?
N10 C12 H12B 109.5 . . ?
N10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N10 C13 H13A 109.5 . . ?
N10 C13 H13B 109.5 . . ?
N10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1SA 109.5 . . ?
O1S C1S H1SB 109.5 . . ?
O1S C1S H1SC 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?

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 O5 0.85 1.90 2.695(9) 155.2 2_646 yes
N3 H3 O5 0.88 2.14 2.848(9) 137.2 . yes
O1S H1S N8 0.84 2.00 2.800(12) 159.8 . yes

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 O6 N11 O7 -0.7(7) . . . . ?
Dy1 O6 N11 O8 -179.2(7) . . . . ?
Dy1 O7 N11 O6 0.7(7) . . . . ?
Dy1 O7 N11 O8 179.2(7) . . . . ?
Dy1 O9 N12 O10 3.7(7) . . . . ?
Dy1 O9 N12 O11 -179.1(7) . . . . ?
Dy1 O10 N12 O9 -3.9(7) . . . . ?
Dy1 O10 N12 O11 178.9(7) . . . . ?
P1 N6 C8 N7 -27.0(11) . . . . ?
P1 N6 C8 N9 153.9(7) . . . . ?
P1 N8 C9 N7 9.7(11) . . . . ?
P1 N8 C9 N10 -169.1(6) . . . . ?
P2 N1 C2 N2 -11.6(12) . . . . ?
P2 N1 C2 N4 170.2(6) . . . . ?
P2 N3 C3 N2 -4.7(12) . . . . ?
P2 N3 C3 N5 176.9(6) . . . . ?
O2 P2 O3 Dy1 -171.8(4) . . . 2_656 ?
O2 P2 N1 C2 120.0(7) . . . . ?
O2 P2 N3 C3 -114.2(7) . . . . ?
O3 P2 O2 Dy1 126.6(8) . . . . ?
O3 P2 N1 C2 -111.2(7) . . . . ?
O3 P2 N3 C3 118.6(7) . . . . ?
O4 P1 N6 C8 -72.1(7) . . . . ?
O4 P1 N8 C9 83.1(7) . . . . ?
O5 P1 O4 Dy1 62.0(6) . . . . ?
O5 P1 N6 C8 156.5(6) . . . . ?
O5 P1 N8 C9 -146.7(6) . . . . ?
N1 P2 O2 Dy1 -106.7(8) . . . . ?
N1 P2 O3 Dy1 61.0(6) . . . 2_656 ?
N1 P2 N3 C3 2.8(8) . . . . ?
N3 P2 O2 Dy1 1.6(10) . . . . ?
N3 P2 O3 Dy1 -47.2(6) . . . 2_656 ?
N3 P2 N1 C2 4.7(7) . . . . ?
N6 P1 O4 Dy1 -65.3(6) . . . . ?
N6 P1 N8 C9 -31.8(7) . . . . ?
N8 P1 O4 Dy1 -171.5(5) . . . . ?
N8 P1 N6 C8 40.7(7) . . . . ?
C2 N2 C3 N3 -1.6(13) . . . . ?
C2 N2 C3 N5 176.9(8) . . . . ?
C3 N2 C2 N1 9.8(12) . . . . ?
C3 N2 C2 N4 -172.1(8) . . . . ?
C4 N4 C2 N1 -1.9(12) . . . . ?
C4 N4 C2 N2 179.8(8) . . . . ?
C5 N4 C2 N1 -179.8(8) . . . . ?
C5 N4 C2 N2 1.9(12) . . . . ?
C6 N5 C3 N2 5.3(13) . . . . ?
C6 N5 C3 N3 -176.1(8) . . . . ?
C7 N5 C3 N2 176.1(8) . . . . ?
C7 N5 C3 N3 -5.4(13) . . . . ?
C8 N7 C9 N8 13.7(13) . . . . ?
C8 N7 C9 N10 -167.5(8) . . . . ?
C9 N7 C8 N6 -4.9(12) . . . . ?
C9 N7 C8 N9 174.3(8) . . . . ?
C10 N9 C8 N6 -7.7(13) . . . . ?
C10 N9 C8 N7 173.1(8) . . . . ?
C11 N9 C8 N6 174.3(8) . . . . ?
C11 N9 C8 N7 -4.9(13) . . . . ?
C12 N10 C9 N7 2.5(12) . . . . ?
C12 N10 C9 N8 -178.6(7) . . . . ?
C13 N10 C9 N7 -175.7(8) . . . . ?
C13 N10 C9 N8 3.2(12) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 68 electrons were 
found in a volume of 216Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH] per formula unit 
which account for 72 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.139 -0.123 0.264 53.5 16.8 '1 CH3OH'
2 0.139 0.123 0.736 53.5 16.7 '1 CH3OH'
3 0.361 0.623 0.764 53.5 16.9 '1 CH3OH'
4 0.639 0.377 0.236 53.5 16.6 '1 CH3OH'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.830
_vrf_PLAT971_dy                  
;
RESPONSE:Residual density resides near the heaviour Dy atoms
and is not likely from any unaccounted atom types. 
;
_vrf_PLAT972_dy                  
;
RESPONSE:Residual density resides near the heaviour Dy atoms
and is not likely from any unaccounted atom types. 
;
