# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_aj0023r
_database_code_depnum_ccdc_archive 'CCDC 1891541'
loop_
_audit_author_name
_audit_author_address
'PANKAJ KALITA'
;National Institute of Science Education and Research
India
;
_audit_update_record             
;
2019-03-04 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H22 Dy N9 O10, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 Dy N9 O13'
_chemical_formula_weight         867.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3165(3)
_cell_length_b                   11.6740(4)
_cell_length_c                   13.7042(2)
_cell_angle_alpha                94.491(2)
_cell_angle_beta                 105.765(2)
_cell_angle_gamma                105.073(3)
_cell_volume                     1660.64(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13019
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.9910
_cell_measurement_theta_min      2.9240
_shelx_estimated_absorpt_T_max   0.873
_shelx_estimated_absorpt_T_min   0.542
_exptl_absorpt_coefficient_mu    2.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63614
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31915
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.566
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00   0.00   1.00   21.88    --    3.50 -55.00 122.00   53
  2  ω    -23.00  92.00   1.00   21.88    --    3.50  55.00 -94.00  115
  3  ω    -84.00  33.00   1.00   21.88    --    3.50 -38.00 -30.00  117
  4  ω      6.00  70.00   1.00   21.88    --   -3.80  38.00-150.00   64
  5  ω    -42.00 -10.00   1.00   21.88    --   -3.80 -82.00-180.00   32
  6  ω    -26.00   1.00   1.00   21.88    --   -3.80 -82.00  60.00   27
  7  ω    -62.00  31.00   1.00   21.88    --   -3.80 -82.00  90.00   93
  8  ω    -63.00  35.00   1.00   21.88    --   -3.80 -82.00 -30.00   98
;
_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                6103
_reflns_number_total             6862
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.737
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+5.6669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0874
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O10-H10
 0.85 with sigma of 0.01
 O13-C28
 1.42 with sigma of 0.002
 C25-H10
 1.907547 with sigma of 0.02
 Dy1-H10
 2.893164 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N2(H2), C24(H24), C19(H19), C15(H15), C12(H12), C5(H5), C6(H6A),
 C3(H3), C7(H7), C17(H17), C9(H9), C21(H21), C18(H18), C22(H22), C23(H23),
 C11(H11), C10(H10A)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C)
4.c Idealised tetrahedral OH refined as rotating group:
 O11(H11A), O13(H13), O12(H12A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.63777(2) 0.66428(2) 0.77663(2) 0.01564(7) Uani 1 1 d D . . . .
O1 O 0.7584(3) 0.6465(3) 0.6728(2) 0.0197(6) Uani 1 1 d . . . . .
O4 O 0.5224(3) 0.7998(3) 0.7790(2) 0.0172(6) Uani 1 1 d . . . . .
O10 O 0.7636(3) 0.8665(3) 0.7785(2) 0.0203(6) Uani 1 1 d D . . . .
H10 H 0.737(3) 0.9207(14) 0.803(3) 0.031 Uiso 1 1 d DR . . . .
O9 O 0.6109(3) 0.5003(3) 0.8883(2) 0.0247(7) Uani 1 1 d . . . . .
O7 O 0.6233(3) 0.4520(3) 0.7371(2) 0.0271(7) Uani 1 1 d . . . . .
O6 O 0.2796(3) 0.9479(3) 1.1066(2) 0.0238(7) Uani 1 1 d . . . . .
N5 N 0.8519(3) 0.6743(3) 0.9030(3) 0.0188(7) Uani 1 1 d . . . . .
O5 O 0.1541(3) 0.9877(3) 0.9712(3) 0.0317(8) Uani 1 1 d . . . . .
N7 N 0.6698(3) 0.7492(3) 0.9607(2) 0.0168(7) Uani 1 1 d . . . . .
N6 N 0.7741(3) 0.7345(4) 1.0331(2) 0.0207(8) Uani 1 1 d . . . . .
H6 H 0.777515 0.740886 1.098297 0.025 Uiso 1 1 calc R . . . .
N3 N 0.5032(3) 0.6400(3) 0.5915(3) 0.0188(7) Uani 1 1 d . . . . .
O11 O 0.4963(4) 0.9179(3) 0.6080(3) 0.0381(9) Uani 1 1 d . . . . .
H11A H 0.508295 0.877542 0.655977 0.057 Uiso 1 1 calc GR . . . .
N1 N 0.3979(3) 0.5581(3) 0.7380(3) 0.0191(7) Uani 1 1 d . . . . .
O3 O 0.9443(3) 0.8097(3) 0.3041(3) 0.0340(8) Uani 1 1 d . . . . .
O2 O 0.7442(4) 0.8021(4) 0.2462(2) 0.0369(9) Uani 1 1 d . . . . .
O8 O 0.5884(4) 0.3136(3) 0.8323(3) 0.0417(9) Uani 1 1 d . . . . .
N9 N 0.6067(4) 0.4182(4) 0.8202(3) 0.0253(8) Uani 1 1 d . . . . .
O13 O 0.2002(4) 0.5916(5) 0.3794(3) 0.0515(12) Uani 1 1 d D . . . .
H13 H 0.245602 0.551559 0.362803 0.077 Uiso 1 1 calc GR . . . .
N2 N 0.3737(3) 0.6175(4) 0.5766(3) 0.0231(8) Uani 1 1 d . . . . .
H2 H 0.324413 0.630646 0.519464 0.028 Uiso 1 1 calc R . . . .
C1 C 0.7746(4) 0.6813(4) 0.5884(3) 0.0169(8) Uani 1 1 d . . . . .
N8 N 0.2427(3) 0.9480(3) 1.0122(3) 0.0224(8) Uani 1 1 d . . . . .
C24 C 0.9492(4) 0.6471(4) 0.8763(3) 0.0216(9) Uani 1 1 d . . . . .
H24 H 0.936932 0.623200 0.805490 0.026 Uiso 1 1 calc R . . . .
C19 C 0.5913(4) 0.7874(4) 0.9986(3) 0.0187(8) Uani 1 1 d . . . . .
H19 H 0.607661 0.795074 1.070942 0.022 Uiso 1 1 calc R . . . .
C15 C 0.4093(4) 0.8587(4) 0.9970(3) 0.0179(8) Uani 1 1 d . . . . .
H15 H 0.430028 0.856507 1.068648 0.021 Uiso 1 1 calc R . . . .
C14 C 0.4811(4) 0.8193(4) 0.9403(3) 0.0159(8) Uani 1 1 d . . . . .
N4 N 0.8349(4) 0.7910(4) 0.3137(3) 0.0254(8) Uani 1 1 d . . . . .
C20 C 0.8726(4) 0.7099(4) 1.0035(3) 0.0176(8) Uani 1 1 d . . . . .
C2 C 0.6700(4) 0.6912(4) 0.5068(3) 0.0178(8) Uani 1 1 d . . . . .
C13 C 0.4521(4) 0.8265(4) 0.8328(3) 0.0165(8) Uani 1 1 d . . . . .
C12 C 0.3418(4) 0.5169(4) 0.8090(3) 0.0225(9) Uani 1 1 d . . . . .
H12 H 0.395068 0.506065 0.872154 0.027 Uiso 1 1 calc R . . . .
C5 C 0.9182(4) 0.7427(4) 0.4850(3) 0.0229(9) Uani 1 1 d . . . . .
H5 H 1.001504 0.760326 0.476881 0.028 Uiso 1 1 calc R . . . .
C6 C 0.8980(4) 0.7069(4) 0.5737(3) 0.0212(9) Uani 1 1 d . . . . .
H6A H 0.968241 0.698902 0.626645 0.025 Uiso 1 1 calc R . . . .
C3 C 0.6912(4) 0.7262(4) 0.4163(3) 0.0207(9) Uani 1 1 d . . . . .
H3 H 0.621725 0.731728 0.361262 0.025 Uiso 1 1 calc R . . . .
C7 C 0.5393(4) 0.6642(4) 0.5116(3) 0.0187(8) Uani 1 1 d . . . . .
H7 H 0.474460 0.664222 0.450727 0.022 Uiso 1 1 calc R . . . .
C16 C 0.3084(4) 0.9008(4) 0.9494(3) 0.0182(8) Uani 1 1 d . . . . .
C17 C 0.2740(4) 0.9035(4) 0.8438(3) 0.0233(9) Uani 1 1 d . . . . .
H17 H 0.203243 0.931032 0.811837 0.028 Uiso 1 1 calc R . . . .
C9 C 0.1872(4) 0.5520(4) 0.6303(3) 0.0240(9) Uani 1 1 d . . . . .
H9 H 0.135926 0.566404 0.567783 0.029 Uiso 1 1 calc R . . . .
C4 C 0.8145(4) 0.7529(4) 0.4071(3) 0.0217(9) Uani 1 1 d . . . . .
C8 C 0.3208(4) 0.5748(4) 0.6502(3) 0.0192(9) Uani 1 1 d . . . . .
C21 C 0.9879(4) 0.7176(4) 1.0791(3) 0.0209(9) Uani 1 1 d . . . . .
H21 H 0.998858 0.742328 1.149513 0.025 Uiso 1 1 calc R . . . .
C18 C 0.3436(4) 0.8659(4) 0.7870(3) 0.0218(9) Uani 1 1 d . . . . .
H18 H 0.318905 0.866217 0.715042 0.026 Uiso 1 1 calc R . . . .
C22 C 1.0841(4) 0.6889(4) 1.0494(3) 0.0241(9) Uani 1 1 d . . . . .
H22 H 1.163257 0.693985 1.098859 0.029 Uiso 1 1 calc R . . . .
C25 C 0.8950(4) 0.9217(5) 0.7831(4) 0.0310(11) Uani 1 1 d D . . . .
H25A H 0.897578 0.976806 0.732810 0.046 Uiso 1 1 calc GR . . . .
H25B H 0.933783 0.859405 0.767544 0.046 Uiso 1 1 calc GR . . . .
H25C H 0.943073 0.966602 0.852203 0.046 Uiso 1 1 calc GR . . . .
C23 C 1.0643(4) 0.6521(4) 0.9452(3) 0.0235(9) Uani 1 1 d . . . . .
H23 H 1.129204 0.630864 0.922694 0.028 Uiso 1 1 calc R . . . .
O12 O 0.2383(5) 0.8569(4) 0.5086(5) 0.0797(18) Uani 1 1 d . . . . .
H12A H 0.316873 0.864319 0.533829 0.120 Uiso 1 1 calc GR . . . .
C11 C 0.2112(5) 0.4898(4) 0.7946(4) 0.0256(10) Uani 1 1 d . . . . .
H11 H 0.175591 0.459095 0.845868 0.031 Uiso 1 1 calc R . . . .
C10 C 0.1329(4) 0.5085(4) 0.7031(4) 0.0265(10) Uani 1 1 d . . . . .
H10A H 0.042904 0.491288 0.691324 0.032 Uiso 1 1 calc R . . . .
C26 C 0.5532(7) 1.0424(6) 0.6482(5) 0.0588(19) Uani 1 1 d . . . . .
H26A H 0.530002 1.089922 0.594049 0.088 Uiso 1 1 calc GR . . . .
H26B H 0.646785 1.059923 0.672909 0.088 Uiso 1 1 calc GR . . . .
H26C H 0.521860 1.063211 0.705186 0.088 Uiso 1 1 calc GR . . . .
C28 C 0.1911(9) 0.6811(9) 0.3164(8) 0.104(4) Uani 1 1 d D . . . .
H28A H 0.117120 0.648610 0.254667 0.156 Uiso 1 1 calc GR . . . .
H28B H 0.269684 0.706521 0.296607 0.156 Uiso 1 1 calc GR . . . .
H28C H 0.179998 0.750312 0.354369 0.156 Uiso 1 1 calc GR . . . .
C27 C 0.2189(9) 0.9732(8) 0.5110(7) 0.085(3) Uani 1 1 d . U . . .
H27A H 0.265025 1.019440 0.468995 0.128 Uiso 1 1 calc GR . . . .
H27B H 0.251372 1.015331 0.581972 0.128 Uiso 1 1 calc GR . . . .
H27C H 0.126962 0.964484 0.483580 0.128 Uiso 1 1 calc GR . . . .


_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 2.256(3) . ?
Dy1 O4 2.302(3) . ?
Dy1 O10 2.413(3) . ?
Dy1 O9 2.551(3) . ?
Dy1 O7 2.448(3) . ?
Dy1 N5 2.535(3) . ?
Dy1 N7 2.530(3) . ?
Dy1 N3 2.530(3) . ?
Dy1 N1 2.560(4) . ?
O1 C1 1.299(5) . ?
O4 C13 1.298(5) . ?
O10 H10 0.854(9) . ?
O10 C25 1.441(5) . ?
O9 N9 1.267(5) . ?
O7 N9 1.279(5) . ?
O6 N8 1.247(5) . ?
N5 C24 1.352(5) . ?
N5 C20 1.345(5) . ?
O5 N8 1.229(5) . ?
N7 N6 1.379(5) . ?
N7 C19 1.297(5) . ?
N6 H6 0.8800 . ?
N6 C20 1.372(5) . ?
N3 N2 1.374(5) . ?
N3 C7 1.295(5) . ?
O11 H11A 0.8400 . ?
O11 C26 1.423(7) . ?
N1 C12 1.352(5) . ?
N1 C8 1.342(6) . ?
O3 N4 1.245(5) . ?
O2 N4 1.224(5) . ?
O8 N9 1.217(5) . ?
O13 H13 0.8400 . ?
O13 C28 1.414(2) . ?
N2 H2 0.8800 . ?
N2 C8 1.369(5) . ?
C1 C2 1.427(6) . ?
C1 C6 1.423(6) . ?
N8 C16 1.443(5) . ?
C24 H24 0.9500 . ?
C24 C23 1.370(6) . ?
C19 H19 0.9500 . ?
C19 C14 1.441(6) . ?
C15 H15 0.9500 . ?
C15 C14 1.399(6) . ?
C15 C16 1.381(6) . ?
C14 C13 1.434(6) . ?
N4 C4 1.444(5) . ?
C20 C21 1.405(6) . ?
C2 C3 1.398(6) . ?
C2 C7 1.451(6) . ?
C13 C18 1.426(6) . ?
C12 H12 0.9500 . ?
C12 C11 1.383(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.373(6) . ?
C5 C4 1.394(6) . ?
C6 H6A 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.391(6) . ?
C7 H7 0.9500 . ?
C16 C17 1.398(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.371(6) . ?
C9 H9 0.9500 . ?
C9 C8 1.409(6) . ?
C9 C10 1.372(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.369(6) . ?
C18 H18 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.397(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C23 H23 0.9500 . ?
O12 H12A 0.8400 . ?
O12 C27 1.429(10) . ?
C11 H11 0.9500 . ?
C11 C10 1.394(7) . ?
C10 H10A 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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 O4 127.06(10) . . ?
O1 Dy1 O10 74.45(10) . . ?
O1 Dy1 O9 114.72(10) . . ?
O1 Dy1 O7 71.13(11) . . ?
O1 Dy1 N5 77.43(11) . . ?
O1 Dy1 N7 138.53(11) . . ?
O1 Dy1 N3 70.67(11) . . ?
O1 Dy1 N1 126.09(11) . . ?
O4 Dy1 O10 68.01(10) . . ?
O4 Dy1 O9 117.87(10) . . ?
O4 Dy1 O7 144.99(11) . . ?
O4 Dy1 N5 126.89(11) . . ?
O4 Dy1 N7 70.55(10) . . ?
O4 Dy1 N3 75.91(10) . . ?
O4 Dy1 N1 68.42(11) . . ?
O10 Dy1 O9 142.53(10) . . ?
O10 Dy1 O7 143.75(10) . . ?
O10 Dy1 N5 78.37(11) . . ?
O10 Dy1 N7 81.67(11) . . ?
O10 Dy1 N3 93.76(11) . . ?
O10 Dy1 N1 134.85(11) . . ?
O9 Dy1 N1 71.29(11) . . ?
O7 Dy1 O9 51.05(10) . . ?
O7 Dy1 N5 83.38(11) . . ?
O7 Dy1 N7 118.02(10) . . ?
O7 Dy1 N3 85.45(11) . . ?
O7 Dy1 N1 76.87(11) . . ?
N5 Dy1 O9 69.30(11) . . ?
N5 Dy1 N1 140.09(11) . . ?
N7 Dy1 O9 67.89(11) . . ?
N7 Dy1 N5 64.72(11) . . ?
N7 Dy1 N1 94.72(11) . . ?
N3 Dy1 O9 123.70(11) . . ?
N3 Dy1 N5 148.09(11) . . ?
N3 Dy1 N7 145.39(11) . . ?
N3 Dy1 N1 64.50(11) . . ?
C1 O1 Dy1 138.7(3) . . ?
C13 O4 Dy1 136.4(3) . . ?
Dy1 O10 H10 113.8(14) . . ?
C25 O10 Dy1 134.6(3) . . ?
C25 O10 H10 107.3(14) . . ?
N9 O9 Dy1 94.2(2) . . ?
N9 O7 Dy1 98.8(2) . . ?
C24 N5 Dy1 124.3(3) . . ?
C20 N5 Dy1 118.9(3) . . ?
C20 N5 C24 116.8(4) . . ?
N6 N7 Dy1 115.9(2) . . ?
C19 N7 Dy1 128.6(3) . . ?
C19 N7 N6 114.5(3) . . ?
N7 N6 H6 120.0 . . ?
C20 N6 N7 120.0(3) . . ?
C20 N6 H6 120.0 . . ?
N2 N3 Dy1 114.8(2) . . ?
C7 N3 Dy1 129.4(3) . . ?
C7 N3 N2 114.8(3) . . ?
C26 O11 H11A 109.5 . . ?
C12 N1 Dy1 124.5(3) . . ?
C8 N1 Dy1 115.8(3) . . ?
C8 N1 C12 117.0(4) . . ?
O9 N9 O7 115.7(4) . . ?
O8 N9 O9 122.6(4) . . ?
O8 N9 O7 121.6(4) . . ?
C28 O13 H13 109.5 . . ?
N3 N2 H2 119.8 . . ?
C8 N2 N3 120.4(4) . . ?
C8 N2 H2 119.8 . . ?
O1 C1 C2 121.7(4) . . ?
O1 C1 C6 120.2(4) . . ?
C6 C1 C2 118.1(4) . . ?
O6 N8 C16 118.1(3) . . ?
O5 N8 O6 122.6(4) . . ?
O5 N8 C16 119.2(4) . . ?
N5 C24 H24 118.1 . . ?
N5 C24 C23 123.9(4) . . ?
C23 C24 H24 118.1 . . ?
N7 C19 H19 117.2 . . ?
N7 C19 C14 125.5(4) . . ?
C14 C19 H19 117.2 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C16 C15 C14 120.5(4) . . ?
C15 C14 C19 116.0(4) . . ?
C15 C14 C13 119.6(4) . . ?
C13 C14 C19 123.9(4) . . ?
O3 N4 C4 118.6(4) . . ?
O2 N4 O3 122.2(4) . . ?
O2 N4 C4 119.2(4) . . ?
N5 C20 N6 118.0(4) . . ?
N5 C20 C21 122.9(4) . . ?
N6 C20 C21 119.0(4) . . ?
C1 C2 C7 123.1(4) . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 C7 117.1(4) . . ?
O4 C13 C14 121.7(4) . . ?
O4 C13 C18 120.9(4) . . ?
C18 C13 C14 117.4(4) . . ?
N1 C12 H12 118.2 . . ?
N1 C12 C11 123.6(4) . . ?
C11 C12 H12 118.2 . . ?
C6 C5 H5 120.6 . . ?
C6 C5 C4 118.9(4) . . ?
C4 C5 H5 120.6 . . ?
C1 C6 H6A 119.1 . . ?
C5 C6 C1 121.7(4) . . ?
C5 C6 H6A 119.1 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 H3 120.2 . . ?
N3 C7 C2 125.8(4) . . ?
N3 C7 H7 117.1 . . ?
C2 C7 H7 117.1 . . ?
C15 C16 N8 118.4(4) . . ?
C15 C16 C17 121.2(4) . . ?
C17 C16 N8 120.3(4) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.2(4) . . ?
C18 C17 H17 120.4 . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C10 C9 C8 118.6(4) . . ?
C5 C4 N4 119.3(4) . . ?
C3 C4 N4 118.9(4) . . ?
C3 C4 C5 121.8(4) . . ?
N1 C8 N2 119.0(4) . . ?
N1 C8 C9 123.0(4) . . ?
N2 C8 C9 118.0(4) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 C20 118.7(4) . . ?
C22 C21 H21 120.6 . . ?
C13 C18 H18 119.0 . . ?
C17 C18 C13 121.9(4) . . ?
C17 C18 H18 119.0 . . ?
C21 C22 H22 120.4 . . ?
C21 C22 C23 119.1(4) . . ?
C23 C22 H22 120.4 . . ?
O10 C25 H25A 109.5 . . ?
O10 C25 H25B 109.5 . . ?
O10 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C23 C22 118.6(4) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C27 O12 H12A 109.5 . . ?
C12 C11 H11 120.8 . . ?
C12 C11 C10 118.5(4) . . ?
C10 C11 H11 120.8 . . ?
C9 C10 C11 119.3(4) . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
O11 C26 H26A 109.5 . . ?
O11 C26 H26B 109.5 . . ?
O11 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O13 C28 H28A 109.5 . . ?
O13 C28 H28B 109.5 . . ?
O13 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O12 C27 H27A 109.5 . . ?
O12 C27 H27B 109.5 . . ?
O12 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
O10 H10 O6 0.854(9) 1.972(17) 2.801(4) 164(4) 2_677 yes
O11 H11A O4 0.84 1.96 2.796(4) 170.4 . yes
N2 H2 O13 0.88 1.98 2.816(5) 157.6 . yes
O12 H12A O11 0.84 1.92 2.738(6) 165.9 . yes

_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
;
# start Validation Reply Form
_vrf_PLAT971_aj0023r             
;
RESPONSE: The large residual density is around the heavy metal atom, which 
          might be caused by the improper absorption correction or the highly
          polarized electron densities.
;
# end Validation Reply Form 
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aj0805
_database_code_depnum_ccdc_archive 'CCDC 1891560'
loop_
_audit_author_name
_audit_author_address
'PANKAJ KALITA'
;National Institute of Science Education and Research
India
;
_audit_update_record             
;
2019-03-04 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H22 N9 O10 Tb, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 N9 O13 Tb'
_chemical_formula_weight         863.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOTb
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'
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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3219(3)
_cell_length_b                   11.7730(3)
_cell_length_c                   13.7532(4)
_cell_angle_alpha                93.856(2)
_cell_angle_beta                 105.196(3)
_cell_angle_gamma                105.168(3)
_cell_volume                     1689.22(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18921
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      29.1300
_cell_measurement_theta_min      2.8920
_shelx_estimated_absorpt_T_max   0.829
_shelx_estimated_absorpt_T_min   0.683
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42732
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.994
_diffrn_reflns_theta_min         2.821
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.874
_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  -9.00   0.50    1.85    --    7.20 -66.00 157.00   52
  2  ω     33.00  59.00   0.50    1.85    --    7.20  66.00 -67.00   52
  3  ω    -42.00   3.00   0.50    1.85    --   -7.60 -66.00 157.00   90
  4  ω     -4.00  21.00   0.50    1.85    --   -7.60  66.00 -67.00   50
  5  ω    -80.00  13.00   0.50    1.85    --    7.20 -57.00   0.00  186
  6  ω    -23.00  45.00   0.50    1.85    --    7.20  57.00 -30.00  136
  7  ω    -22.00  82.00   0.50    1.85    --    7.20  57.00 120.00  208
  8  ω     50.00  97.00   0.50    1.85    --    7.20  77.00-150.00   94
  9  ω     63.00  94.00   0.50    1.85    --    7.20  77.00 -90.00   62
 10  ω    -58.00 -23.00   0.50    1.85    --   -7.60 -82.00 -90.00   70
 11  ω    -43.00 -18.00   0.50    1.85    --   -7.60 -82.00  90.00   50
 12  ω    -16.00   9.00   0.50    1.85    --   -7.60 -82.00 -90.00   50
 13  ω    -57.00  29.00   0.50    1.85    --   -7.60 -82.00   0.00  172
;
_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      0.0074087000
_diffrn_orient_matrix_UB_12      -0.0464768000
_diffrn_orient_matrix_UB_13      0.0291549000
_diffrn_orient_matrix_UB_21      0.0622087000
_diffrn_orient_matrix_UB_22      0.0354356000
_diffrn_orient_matrix_UB_23      0.0284682000
_diffrn_orient_matrix_UB_31      -0.0260142000
_diffrn_orient_matrix_UB_32      0.0237800000
_diffrn_orient_matrix_UB_33      0.0354638000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7199
_reflns_number_total             7845
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7845
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.033
_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)+(0.0195P)²+1.2759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0594
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C25-H3
 1.893253 with sigma of 0.02
 Tb1-H3
 2.932969 with sigma of 0.02
 O0AA-C0AA \\sim O1A-C0AA
 with sigma of 0.02
 C0AA-O0AA \\sim O0AA-O1A
 with sigma of 0.02
3. Others
 Sof(H0AE)=Sof(H0AF)=Sof(H0AG)=Sof(O1A)=Sof(H1A)=1-FVAR(1)
 Sof(O0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C19(H19), N5(H5), C3(H3A), C12(H12), C24(H24), C5(H5A), C17(H17),
 C7(H7), C23(H23), C15(H15), C11(H11), C10(H10), C22(H22), C2(H2A), C9(H9),
 C21(H21), C14(H14)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C01E(H01A,H01B,H01C), C01G(H01D,H01E,H01F), C0AA(H0AB,
 H0AC,H0AD), C0AA(H0AE,H0AF,H0AG)
4.c Idealised tetrahedral OH refined as rotating group:
 O00I(H00I), O00O(H00O), O0AA(H0AA), O1A(H1A)
;
_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 0.63335(2) 0.66607(2) 0.77611(2) 0.01676(4) Uani 1 1 d D . . . .
O3 O 0.76151(17) 0.86789(16) 0.77633(14) 0.0254(4) Uani 1 1 d D . . . .
H3 H 0.7368(19) 0.9217(12) 0.803(2) 0.038 Uiso 1 1 d DR . . . .
N6 N 0.49976(18) 0.64151(19) 0.59183(15) 0.0195(4) Uani 1 1 d . . . . .
N2 N 0.7711(2) 0.7365(2) 1.03020(15) 0.0240(5) Uani 1 1 d . . . . .
H2 H 0.774926 0.743387 1.093689 0.029 Uiso 1 1 calc R . . . .
O1 O 0.51902(16) 0.80233(16) 0.77943(12) 0.0203(4) Uani 1 1 d . . . . .
N1 N 0.66668(19) 0.75137(19) 0.95905(15) 0.0194(4) Uani 1 1 d . . . . .
C19 C 0.5347(2) 0.6624(2) 0.51096(19) 0.0232(5) Uani 1 1 d . . . . .
H19 H 0.471095 0.661000 0.451867 0.028 Uiso 1 1 calc R . . . .
O4 O 0.60780(18) 0.50471(18) 0.89028(14) 0.0311(4) Uani 1 1 d . . . . .
O5 O 0.61616(19) 0.45403(18) 0.73939(15) 0.0318(4) Uani 1 1 d . . . . .
O2 O 0.75291(16) 0.64735(16) 0.67075(12) 0.0216(4) Uani 1 1 d . . . . .
N9 N 0.8293(2) 0.7835(2) 0.30964(18) 0.0317(6) Uani 1 1 d . . . . .
N7 N 0.6042(2) 0.4228(2) 0.82403(19) 0.0313(6) Uani 1 1 d . . . . .
N3 N 0.84781(19) 0.6772(2) 0.90028(15) 0.0212(5) Uani 1 1 d . . . . .
O9 O 0.15373(18) 0.9879(2) 0.97448(16) 0.0365(5) Uani 1 1 d . . . . .
O7 O 0.7384(2) 0.7930(2) 0.24157(16) 0.0468(6) Uani 1 1 d . . . . .
O8 O 0.9381(2) 0.8042(2) 0.29964(16) 0.0442(6) Uani 1 1 d . . . . .
O00I O 0.4907(2) 0.9191(2) 0.60809(16) 0.0401(5) Uani 1 1 d . . . . .
H00I H 0.502540 0.879440 0.654524 0.060 Uiso 1 1 calc GR . . . .
O10 O 0.27877(18) 0.94804(18) 1.10790(14) 0.0306(4) Uani 1 1 d . . . . .
N5 N 0.3708(2) 0.6195(2) 0.57854(17) 0.0274(5) Uani 1 1 d . . . . .
H5 H 0.322847 0.632204 0.523075 0.033 Uiso 1 1 calc R . . . .
O6 O 0.5900(3) 0.3202(2) 0.8393(2) 0.0574(7) Uani 1 1 d . . . . .
N4 N 0.3943(2) 0.56189(19) 0.73948(16) 0.0225(5) Uani 1 1 d . . . . .
O00O O 0.2308(3) 0.8645(2) 0.5195(2) 0.0585(7) Uani 1 1 d . . . . .
H00O H 0.308165 0.874056 0.537983 0.088 Uiso 1 1 calc GR . . . .
C3 C 0.2721(2) 0.9044(3) 0.8469(2) 0.0271(6) Uani 1 1 d . . . . .
H3A H 0.202422 0.930637 0.816367 0.033 Uiso 1 1 calc R . . . .
C12 C 0.9450(2) 0.6499(2) 0.8730(2) 0.0239(6) Uani 1 1 d . . . . .
H12 H 0.933199 0.626987 0.804255 0.029 Uiso 1 1 calc R . . . .
C24 C 0.3375(3) 0.5200(2) 0.8101(2) 0.0278(6) Uani 1 1 d . . . . .
H24 H 0.388884 0.508469 0.871304 0.033 Uiso 1 1 calc R . . . .
C8 C 0.8683(2) 0.7108(2) 0.99998(19) 0.0194(5) Uani 1 1 d . . . . .
C5 C 0.4083(2) 0.8606(2) 0.99778(19) 0.0193(5) Uani 1 1 d . . . . .
H5A H 0.428837 0.857960 1.067479 0.023 Uiso 1 1 calc R . . . .
C4 C 0.3075(2) 0.9019(2) 0.95153(19) 0.0212(5) Uani 1 1 d . . . . .
C16 C 0.8081(3) 0.7461(2) 0.40288(19) 0.0243(6) Uani 1 1 d . . . . .
C6 C 0.4797(2) 0.8227(2) 0.94088(18) 0.0188(5) Uani 1 1 d . . . . .
C1 C 0.4493(2) 0.8288(2) 0.83398(19) 0.0192(5) Uani 1 1 d . . . . .
N8 N 0.2420(2) 0.9483(2) 1.01477(18) 0.0259(5) Uani 1 1 d . . . . .
C17 C 0.6867(3) 0.7210(2) 0.41369(19) 0.0236(6) Uani 1 1 d . . . . .
H17 H 0.619102 0.725970 0.360236 0.028 Uiso 1 1 calc R . . . .
C20 C 0.3180(2) 0.5778(2) 0.6520(2) 0.0230(6) Uani 1 1 d . . . . .
C7 C 0.5893(2) 0.7896(2) 0.99753(19) 0.0213(5) Uani 1 1 d . . . . .
H7 H 0.605635 0.796422 1.067884 0.026 Uiso 1 1 calc R . . . .
C23 C 0.2082(3) 0.4934(3) 0.7967(2) 0.0331(7) Uani 1 1 d . . . . .
H23 H 0.173138 0.463589 0.847042 0.040 Uiso 1 1 calc R . . . .
C25 C 0.8921(3) 0.9207(3) 0.7804(3) 0.0369(7) Uani 1 1 d D . . . .
H25A H 0.896943 0.981690 0.737424 0.055 Uiso 1 1 calc GR . . . .
H25B H 0.926161 0.860892 0.757283 0.055 Uiso 1 1 calc GR . . . .
H25C H 0.940855 0.954924 0.849236 0.055 Uiso 1 1 calc GR . . . .
C15 C 0.9116(3) 0.7373(3) 0.4805(2) 0.0267(6) Uani 1 1 d . . . . .
H15 H 0.992907 0.753844 0.471993 0.032 Uiso 1 1 calc R . . . .
C11 C 1.0590(3) 0.6539(3) 0.9404(2) 0.0274(6) Uani 1 1 d . . . . .
H11 H 1.122388 0.633415 0.918013 0.033 Uiso 1 1 calc R . . . .
C10 C 1.0783(2) 0.6894(2) 1.0432(2) 0.0260(6) Uani 1 1 d . . . . .
H10 H 1.155230 0.693265 1.090733 0.031 Uiso 1 1 calc R . . . .
C22 C 0.1309(3) 0.5120(3) 0.7062(2) 0.0353(7) Uani 1 1 d . . . . .
H22 H 0.043144 0.495459 0.695469 0.042 Uiso 1 1 calc R . . . .
C2 C 0.3416(3) 0.8676(2) 0.7894(2) 0.0257(6) Uani 1 1 d . . . . .
H2A H 0.317311 0.868134 0.719440 0.031 Uiso 1 1 calc R . . . .
C9 C 0.9828(2) 0.7187(2) 1.07398(19) 0.0229(5) Uani 1 1 d . . . . .
H9 H 0.993915 0.743228 1.142318 0.027 Uiso 1 1 calc R . . . .
C13 C 0.7688(2) 0.6792(2) 0.58547(18) 0.0196(5) Uani 1 1 d . . . . .
C21 C 0.1850(3) 0.5550(3) 0.6329(2) 0.0306(6) Uani 1 1 d . . . . .
H21 H 0.135029 0.568664 0.571969 0.037 Uiso 1 1 calc R . . . .
C18 C 0.6648(2) 0.6880(2) 0.50441(18) 0.0206(5) Uani 1 1 d . . . . .
C14 C 0.8912(2) 0.7039(2) 0.5693(2) 0.0254(6) Uani 1 1 d . . . . .
H14 H 0.959803 0.697029 0.620864 0.030 Uiso 1 1 calc R . . . .
C01E C 0.5526(4) 1.0401(3) 0.6459(3) 0.0584(11) Uani 1 1 d . . . . .
H01A H 0.535481 1.086936 0.592250 0.088 Uiso 1 1 calc GR . . . .
H01B H 0.643082 1.052096 0.671123 0.088 Uiso 1 1 calc GR . . . .
H01C H 0.521428 1.063918 0.700182 0.088 Uiso 1 1 calc GR . . . .
C01G C 0.2074(5) 0.9746(4) 0.5159(5) 0.0961(19) Uani 1 1 d . . . . .
H01D H 0.252790 1.018646 0.473901 0.144 Uiso 1 1 calc GR . . . .
H01E H 0.236000 1.017982 0.583461 0.144 Uiso 1 1 calc GR . . . .
H01F H 0.117402 0.963270 0.487741 0.144 Uiso 1 1 calc GR . . . .
O0AA O 0.2023(3) 0.5822(3) 0.3773(2) 0.0290(10) Uani 0.711(7) 1 d D . P A 1
H0AA H 0.230071 0.533731 0.351786 0.044 Uiso 0.711(7) 1 calc GR . P A 1
C0AA C 0.1916(3) 0.6699(3) 0.3152(3) 0.0461(8) Uani 1 1 d D . . . .
H0AB H 0.130744 0.634704 0.250329 0.069 Uiso 0.711(7) 1 calc GR . P A 1
H0AC H 0.273363 0.706622 0.305733 0.069 Uiso 0.711(7) 1 calc GR . P A 1
H0AD H 0.163396 0.728938 0.346784 0.069 Uiso 0.711(7) 1 calc GR . P A 1
H0AE H 0.123454 0.701006 0.282257 0.069 Uiso 0.289(7) 1 calc GR . P A 2
H0AF H 0.180836 0.593714 0.278753 0.069 Uiso 0.289(7) 1 calc GR . P A 2
H0AG H 0.272080 0.723571 0.315985 0.069 Uiso 0.289(7) 1 calc GR . P A 2
O1A O 0.1895(8) 0.6580(8) 0.4116(6) 0.042(3) Uani 0.289(7) 1 d D . P A 2
H1A H 0.196579 0.722770 0.442236 0.063 Uiso 0.289(7) 1 calc GR . P A 2


_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 O3 2.4379(18) . ?
Tb1 N6 2.541(2) . ?
Tb1 O1 2.3150(17) . ?
Tb1 N1 2.539(2) . ?
Tb1 O4 2.5515(19) . ?
Tb1 O5 2.460(2) . ?
Tb1 O2 2.2632(16) . ?
Tb1 N3 2.541(2) . ?
Tb1 N4 2.559(2) . ?
O3 H3 0.853(9) . ?
O3 C25 1.431(3) . ?
N6 C19 1.293(3) . ?
N6 N5 1.374(3) . ?
N2 H2 0.8600 . ?
N2 N1 1.382(3) . ?
N2 C8 1.368(3) . ?
O1 C1 1.300(3) . ?
N1 C7 1.291(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.452(3) . ?
O4 N7 1.266(3) . ?
O5 N7 1.274(3) . ?
O2 C13 1.297(3) . ?
N9 O7 1.232(3) . ?
N9 O8 1.237(3) . ?
N9 C16 1.442(3) . ?
N7 O6 1.216(3) . ?
N3 C12 1.357(3) . ?
N3 C8 1.343(3) . ?
O9 N8 1.230(3) . ?
O00I H00I 0.8200 . ?
O00I C01E 1.406(4) . ?
O10 N8 1.239(3) . ?
N5 H5 0.8600 . ?
N5 C20 1.360(3) . ?
N4 C24 1.352(3) . ?
N4 C20 1.341(3) . ?
O00O H00O 0.8200 . ?
O00O C01G 1.391(5) . ?
C3 H3A 0.9300 . ?
C3 C4 1.394(4) . ?
C3 C2 1.375(4) . ?
C12 H12 0.9300 . ?
C12 C11 1.364(4) . ?
C24 H24 0.9300 . ?
C24 C23 1.373(4) . ?
C8 C9 1.399(3) . ?
C5 H5A 0.9300 . ?
C5 C4 1.377(4) . ?
C5 C6 1.392(3) . ?
C4 N8 1.446(3) . ?
C16 C17 1.377(4) . ?
C16 C15 1.396(4) . ?
C6 C1 1.431(4) . ?
C6 C7 1.445(3) . ?
C1 C2 1.417(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.395(3) . ?
C20 C21 1.407(4) . ?
C7 H7 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.388(5) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C15 H15 0.9300 . ?
C15 C14 1.365(4) . ?
C11 H11 0.9300 . ?
C11 C10 1.391(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.372(4) . ?
C22 H22 0.9300 . ?
C22 C21 1.371(4) . ?
C2 H2A 0.9300 . ?
C9 H9 0.9300 . ?
C13 C18 1.425(3) . ?
C13 C14 1.419(3) . ?
C21 H21 0.9300 . ?
C14 H14 0.9300 . ?
C01E H01A 0.9600 . ?
C01E H01B 0.9600 . ?
C01E H01C 0.9600 . ?
C01G H01D 0.9600 . ?
C01G H01E 0.9600 . ?
C01G H01F 0.9600 . ?
O0AA H0AA 0.8200 . ?
O0AA C0AA 1.393(4) . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 0.9600 . ?
C0AA H0AD 0.9600 . ?
C0AA H0AE 0.9600 . ?
C0AA H0AF 0.9600 . ?
C0AA H0AG 0.9600 . ?
C0AA O1A 1.348(8) . ?
O1A H1A 0.8200 . ?

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
O3 Tb1 N6 94.34(7) . . ?
O3 Tb1 N1 81.02(7) . . ?
O3 Tb1 O4 141.61(6) . . ?
O3 Tb1 O5 144.36(6) . . ?
O3 Tb1 N3 77.36(7) . . ?
O3 Tb1 N4 135.12(7) . . ?
N6 Tb1 O4 124.04(7) . . ?
N6 Tb1 N3 147.67(6) . . ?
N6 Tb1 N4 64.32(7) . . ?
O1 Tb1 O3 68.10(6) . . ?
O1 Tb1 N6 76.76(6) . . ?
O1 Tb1 N1 70.17(6) . . ?
O1 Tb1 O4 117.75(6) . . ?
O1 Tb1 O5 144.69(6) . . ?
O1 Tb1 N3 126.07(6) . . ?
O1 Tb1 N4 68.69(6) . . ?
N1 Tb1 N6 145.92(6) . . ?
N1 Tb1 O4 67.79(7) . . ?
N1 Tb1 N3 64.42(6) . . ?
N1 Tb1 N4 95.40(7) . . ?
O4 Tb1 N4 71.93(7) . . ?
O5 Tb1 N6 85.15(7) . . ?
O5 Tb1 N1 117.86(7) . . ?
O5 Tb1 O4 50.86(6) . . ?
O5 Tb1 N3 84.21(7) . . ?
O5 Tb1 N4 76.19(7) . . ?
O2 Tb1 O3 74.66(6) . . ?
O2 Tb1 N6 70.04(6) . . ?
O2 Tb1 O1 127.18(6) . . ?
O2 Tb1 N1 138.52(6) . . ?
O2 Tb1 O4 114.78(6) . . ?
O2 Tb1 O5 71.72(7) . . ?
O2 Tb1 N3 77.64(6) . . ?
O2 Tb1 N4 125.48(6) . . ?
N3 Tb1 O4 69.40(7) . . ?
N3 Tb1 N4 140.85(7) . . ?
Tb1 O3 H3 113.7(12) . . ?
C25 O3 Tb1 134.30(17) . . ?
C25 O3 H3 106.9(12) . . ?
C19 N6 Tb1 130.16(16) . . ?
C19 N6 N5 114.7(2) . . ?
N5 N6 Tb1 114.41(15) . . ?
N1 N2 H2 119.9 . . ?
C8 N2 H2 119.9 . . ?
C8 N2 N1 120.2(2) . . ?
C1 O1 Tb1 136.25(16) . . ?
N2 N1 Tb1 115.79(14) . . ?
C7 N1 Tb1 128.77(16) . . ?
C7 N1 N2 114.4(2) . . ?
N6 C19 H19 117.2 . . ?
N6 C19 C18 125.7(2) . . ?
C18 C19 H19 117.2 . . ?
N7 O4 Tb1 94.49(15) . . ?
N7 O5 Tb1 98.69(16) . . ?
C13 O2 Tb1 139.77(15) . . ?
O7 N9 O8 121.7(2) . . ?
O7 N9 C16 119.1(2) . . ?
O8 N9 C16 119.2(2) . . ?
O4 N7 O5 116.0(2) . . ?
O6 N7 O4 122.6(3) . . ?
O6 N7 O5 121.4(3) . . ?
C12 N3 Tb1 124.28(16) . . ?
C8 N3 Tb1 119.15(16) . . ?
C8 N3 C12 116.6(2) . . ?
C01E O00I H00I 109.5 . . ?
N6 N5 H5 119.6 . . ?
C20 N5 N6 120.8(2) . . ?
C20 N5 H5 119.6 . . ?
C24 N4 Tb1 124.68(18) . . ?
C20 N4 Tb1 116.08(16) . . ?
C20 N4 C24 116.9(2) . . ?
C01G O00O H00O 109.5 . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C2 C3 C4 119.1(2) . . ?
N3 C12 H12 118.0 . . ?
N3 C12 C11 123.9(2) . . ?
C11 C12 H12 118.0 . . ?
N4 C24 H24 118.1 . . ?
N4 C24 C23 123.7(3) . . ?
C23 C24 H24 118.1 . . ?
N2 C8 C9 118.8(2) . . ?
N3 C8 N2 118.0(2) . . ?
N3 C8 C9 123.2(2) . . ?
C4 C5 H5A 119.8 . . ?
C4 C5 C6 120.4(2) . . ?
C6 C5 H5A 119.8 . . ?
C3 C4 N8 120.2(2) . . ?
C5 C4 C3 121.4(2) . . ?
C5 C4 N8 118.4(2) . . ?
C17 C16 N9 119.5(2) . . ?
C17 C16 C15 121.6(2) . . ?
C15 C16 N9 119.0(2) . . ?
C5 C6 C1 119.7(2) . . ?
C5 C6 C7 116.2(2) . . ?
C1 C6 C7 123.9(2) . . ?
O1 C1 C6 121.6(2) . . ?
O1 C1 C2 120.7(2) . . ?
C2 C1 C6 117.6(2) . . ?
O9 N8 O10 122.7(2) . . ?
O9 N8 C4 119.0(2) . . ?
O10 N8 C4 118.4(2) . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
N5 C20 C21 118.0(2) . . ?
N4 C20 N5 119.0(2) . . ?
N4 C20 C21 123.0(2) . . ?
N1 C7 C6 125.7(2) . . ?
N1 C7 H7 117.1 . . ?
C6 C7 H7 117.1 . . ?
C24 C23 H23 120.7 . . ?
C24 C23 C22 118.6(3) . . ?
C22 C23 H23 120.7 . . ?
O3 C25 H25A 109.5 . . ?
O3 C25 H25B 109.5 . . ?
O3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C16 C15 H15 120.7 . . ?
C14 C15 C16 118.7(2) . . ?
C14 C15 H15 120.7 . . ?
C12 C11 H11 120.7 . . ?
C12 C11 C10 118.6(2) . . ?
C10 C11 H11 120.7 . . ?
C11 C10 H10 120.3 . . ?
C9 C10 C11 119.4(2) . . ?
C9 C10 H10 120.3 . . ?
C23 C22 H22 120.3 . . ?
C21 C22 C23 119.5(3) . . ?
C21 C22 H22 120.3 . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
C8 C9 H9 120.8 . . ?
C10 C9 C8 118.4(2) . . ?
C10 C9 H9 120.8 . . ?
O2 C13 C18 121.7(2) . . ?
O2 C13 C14 120.5(2) . . ?
C14 C13 C18 117.8(2) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 C20 118.3(3) . . ?
C22 C21 H21 120.8 . . ?
C17 C18 C19 117.7(2) . . ?
C17 C18 C13 119.4(2) . . ?
C13 C18 C19 122.9(2) . . ?
C15 C14 C13 122.2(2) . . ?
C15 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
O00I C01E H01A 109.5 . . ?
O00I C01E H01B 109.5 . . ?
O00I C01E H01C 109.5 . . ?
H01A C01E H01B 109.5 . . ?
H01A C01E H01C 109.5 . . ?
H01B C01E H01C 109.5 . . ?
O00O C01G H01D 109.5 . . ?
O00O C01G H01E 109.5 . . ?
O00O C01G H01F 109.5 . . ?
H01D C01G H01E 109.5 . . ?
H01D C01G H01F 109.5 . . ?
H01E C01G H01F 109.5 . . ?
C0AA O0AA H0AA 109.5 . . ?
O0AA C0AA H0AB 109.5 . . ?
O0AA C0AA H0AC 109.5 . . ?
O0AA C0AA H0AD 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
H0AB C0AA H0AD 109.5 . . ?
H0AC C0AA H0AD 109.5 . . ?
H0AE C0AA H0AF 109.5 . . ?
H0AE C0AA H0AG 109.5 . . ?
H0AF C0AA H0AG 109.5 . . ?
O1A C0AA H0AE 109.5 . . ?
O1A C0AA H0AF 109.5 . . ?
O1A C0AA H0AG 109.5 . . ?
C0AA O1A H1A 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.093
_oxdiff_exptl_absorpt_empirical_full_min 0.628
# start Validation Reply Form
_vrf_PLAT417_aj0805              
;
Problem: ALERT_2_B Short Inter D-H..H-D H00O ..H1A . 2.03 Ang.
 	x,y,z = 1_555 Check
RESPONSE: The H1A atom belongs to a disordered MeOH solvent molecule 
	which is involved in short interactions.        
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
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# Please retain this information to preserve the provenance of 
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data_aj0806
_database_code_depnum_ccdc_archive 'CCDC 1891553'
loop_
_audit_author_name
_audit_author_address
'PANKAJ KALITA'
;National Institute of Science Education and Research
India
;
_audit_update_record             
;
2019-03-04 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H22 Ho N9 O10, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 Ho N9 O13'
_chemical_formula_weight         869.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNOHo
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3398(4)
_cell_length_b                   11.7893(4)
_cell_length_c                   13.7166(3)
_cell_angle_alpha                93.941(2)
_cell_angle_beta                 105.350(3)
_cell_angle_gamma                105.348(3)
_cell_volume                     1686.16(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20977
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      28.9200
_cell_measurement_theta_min      2.8860
_shelx_estimated_absorpt_T_max   0.830
_shelx_estimated_absorpt_T_min   0.712
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80098
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.952
_diffrn_reflns_theta_min         2.830
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00 -49.00   0.50    2.50    --    7.10 -30.00-170.00   52
  2  ω      1.00  39.00   0.50    2.50    --    7.10  30.00 -10.00   76
  3  ω    -12.00  13.00   0.50    2.50    --   -7.50  30.00 -10.00   50
  4  ω    -52.00 -27.00   0.50    2.50    --   -7.50 -30.00-170.00   50
  5  ω     50.00  96.00   0.50    2.50    --    7.10  77.00 150.00   92
  6  ω    -62.00  23.00   0.50    2.50    --   -7.50 -82.00-150.00  170
  7  ω    -55.00   5.00   0.50    2.50    --   -7.50 -77.00 120.00  120
  8  ω    -13.00  13.00   0.50    2.50    --   -7.50 -82.00   0.00   52
  9  ω    -48.00  -2.00   0.50    2.50    --   -7.50  38.00 -90.00   92
 10  ω      3.00  80.00   0.50    2.50    --   -7.50  38.00 -90.00  154
 11  ω    -63.00 -17.00   0.50    2.50    --   -7.50 -82.00   0.00   92
 12  ω    -81.00  76.00   0.50    2.50    --   -7.50  19.00  30.00  314
 13  ω    -51.00  21.00   0.50    2.50    --   -7.50 -82.00  60.00  144
;
_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      -0.0641838000
_diffrn_orient_matrix_UB_12      -0.0250868000
_diffrn_orient_matrix_UB_13      -0.0000254000
_diffrn_orient_matrix_UB_21      0.0164314000
_diffrn_orient_matrix_UB_22      -0.0489768000
_diffrn_orient_matrix_UB_23      0.0210808000
_diffrn_orient_matrix_UB_31      0.0146953000
_diffrn_orient_matrix_UB_32      0.0308722000
_diffrn_orient_matrix_UB_33      0.0499666000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7314
_reflns_number_total             7858
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7858
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.047
_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)+(0.0145P)²+1.0635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0479
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C25-H3
 1.897634 with sigma of 0.02
 Ho1-H3
 2.897801 with sigma of 0.02
 O019-C01E \\sim O0-C01E
 with sigma of 0.02
 O0-O019 \\sim O019-C01E
 with sigma of 0.02
3. Others
 Sof(H01D)=Sof(H01E)=Sof(H01F)=Sof(O0)=Sof(H0)=1-FVAR(1)
 Sof(O019)=Sof(H019)=Sof(H01A)=Sof(H01B)=Sof(H01C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C24(H24), C7(H7), C17(H17), C5(H5A), C19(H19), C2(H2A),
 C3(H3A), C22(H22), C23(H23), C12(H12), C21(H21), C15(H15), C14(H14), C9(H9),
 C11(H11), C10(H10)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C01D(H01G,H01H,H01I), C01E(H01A,H01B,H01C), C01E(H01D,
 H01E,H01F), C01F(H01J,H01K,H01L)
4.c Idealised tetrahedral OH refined as rotating group:
 O00C(H00C), O00S(H00S), O019(H019), O0(H0)
;
_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
Ho1 Ho 0.36544(2) 0.33351(2) 0.22240(2) 0.01830(4) Uani 1 1 d D . . . .
O2 O 0.24610(15) 0.35013(14) 0.32678(11) 0.0245(3) Uani 1 1 d . . . . .
O1 O 0.48004(14) 0.19825(13) 0.22152(11) 0.0214(3) Uani 1 1 d . . . . .
O3 O 0.23926(15) 0.13339(14) 0.22173(12) 0.0266(3) Uani 1 1 d D . . . .
H3 H 0.2624(18) 0.0811(12) 0.1921(19) 0.040 Uiso 1 1 d DR . . . .
O4 O 0.38903(16) 0.49356(15) 0.10886(12) 0.0320(4) Uani 1 1 d . . . . .
O7 O 0.72068(16) 0.05222(15) -0.10662(13) 0.0316(4) Uani 1 1 d . . . . .
O5 O 0.38351(17) 0.54360(15) 0.26094(13) 0.0328(4) Uani 1 1 d . . . . .
N3 N 0.15211(17) 0.32246(16) 0.09947(13) 0.0219(4) Uani 1 1 d . . . . .
O8 O 0.84618(17) 0.01349(17) 0.02808(14) 0.0393(4) Uani 1 1 d . . . . .
N4 N 0.49881(17) 0.35902(16) 0.40557(13) 0.0217(4) Uani 1 1 d . . . . .
N6 N 0.60207(18) 0.43790(16) 0.25658(14) 0.0245(4) Uani 1 1 d . . . . .
O00C O 0.5075(2) 0.08052(17) 0.39245(14) 0.0445(5) Uani 1 1 d . . . . .
H00C H 0.494455 0.120787 0.346566 0.067 Uiso 1 1 calc GR . . . .
N2 N 0.22807(18) 0.26272(18) -0.03064(13) 0.0258(4) Uani 1 1 d . . . . .
H2 H 0.223525 0.254736 -0.094438 0.031 Uiso 1 1 calc R . . . .
N1 N 0.33292(17) 0.24879(16) 0.04070(13) 0.0213(4) Uani 1 1 d . . . . .
N5 N 0.62842(18) 0.38279(19) 0.41921(15) 0.0302(5) Uani 1 1 d . . . . .
H5 H 0.677098 0.371783 0.475261 0.036 Uiso 1 1 calc R . . . .
N8 N 0.75720(18) 0.05253(17) -0.01282(15) 0.0276(4) Uani 1 1 d . . . . .
O10 O 0.2628(2) 0.2063(2) 0.75749(14) 0.0524(5) Uani 1 1 d . . . . .
O9 O 0.0636(2) 0.19604(19) 0.69978(15) 0.0496(5) Uani 1 1 d . . . . .
N7 N 0.3938(2) 0.57515(18) 0.17600(17) 0.0317(5) Uani 1 1 d . . . . .
C24 C 0.0558(2) 0.3500(2) 0.12646(18) 0.0261(5) Uani 1 1 d . . . . .
H24 H 0.067919 0.373007 0.195484 0.031 Uiso 1 1 calc R . . . .
C1 C 0.2308(2) 0.31914(19) 0.41237(16) 0.0219(5) Uani 1 1 d . . . . .
N9 N 0.1720(2) 0.21626(19) 0.68983(16) 0.0367(5) Uani 1 1 d . . . . .
O6 O 0.4077(2) 0.67800(17) 0.16129(18) 0.0580(6) Uani 1 1 d . . . . .
C20 C 0.1316(2) 0.28908(19) -0.00063(16) 0.0212(4) Uani 1 1 d . . . . .
C6 C 0.3358(2) 0.31151(19) 0.49371(16) 0.0215(5) Uani 1 1 d . . . . .
C18 C 0.5200(2) 0.17807(19) 0.05963(16) 0.0208(4) Uani 1 1 d . . . . .
C13 C 0.5499(2) 0.17219(18) 0.16696(16) 0.0199(4) Uani 1 1 d . . . . .
O00S O 0.7672(2) 0.1346(2) 0.4816(2) 0.0649(6) Uani 1 1 d . . . . .
H00S H 0.689752 0.124510 0.464250 0.097 Uiso 1 1 calc GR . . . .
C7 C 0.4649(2) 0.3378(2) 0.48745(17) 0.0252(5) Uani 1 1 d . . . . .
H7 H 0.528952 0.339819 0.546698 0.030 Uiso 1 1 calc R . . . .
C8 C 0.6798(2) 0.42352(19) 0.34462(18) 0.0254(5) Uani 1 1 d . . . . .
C17 C 0.5913(2) 0.14026(19) 0.00288(17) 0.0215(4) Uani 1 1 d . . . . .
H17 H 0.570937 0.142651 -0.067079 0.026 Uiso 1 1 calc R . . . .
C5 C 0.3143(2) 0.2787(2) 0.58494(17) 0.0259(5) Uani 1 1 d . . . . .
H5A H 0.382131 0.273936 0.638583 0.031 Uiso 1 1 calc R . . . .
C19 C 0.4097(2) 0.21055(19) 0.00237(16) 0.0221(5) Uani 1 1 d . . . . .
H19 H 0.392936 0.203066 -0.068277 0.027 Uiso 1 1 calc R . . . .
C2 C 0.1085(2) 0.2946(2) 0.42868(18) 0.0290(5) Uani 1 1 d . . . . .
H2A H 0.039794 0.301360 0.376921 0.035 Uiso 1 1 calc R . . . .
C3 C 0.0885(2) 0.2616(2) 0.51769(18) 0.0303(5) Uani 1 1 d . . . . .
H3A H 0.007327 0.244893 0.526365 0.036 Uiso 1 1 calc R . . . .
C22 C -0.0783(2) 0.3105(2) -0.04427(18) 0.0282(5) Uani 1 1 d . . . . .
H22 H -0.155278 0.306572 -0.092042 0.034 Uiso 1 1 calc R . . . .
C23 C -0.0587(2) 0.3463(2) 0.05875(18) 0.0285(5) Uani 1 1 d . . . . .
H23 H -0.121622 0.367222 0.081232 0.034 Uiso 1 1 calc R . . . .
C12 C 0.6572(2) 0.4785(2) 0.1848(2) 0.0319(6) Uani 1 1 d . . . . .
H12 H 0.604979 0.488315 0.123038 0.038 Uiso 1 1 calc R . . . .
C21 C 0.0168(2) 0.2811(2) -0.07495(17) 0.0246(5) Uani 1 1 d . . . . .
H21 H 0.005332 0.256326 -0.143552 0.030 Uiso 1 1 calc R . . . .
C4 C 0.1929(2) 0.2532(2) 0.59578(17) 0.0278(5) Uani 1 1 d . . . . .
C15 C 0.7270(2) 0.0970(2) 0.15510(18) 0.0275(5) Uani 1 1 d . . . . .
H15 H 0.796457 0.070918 0.186159 0.033 Uiso 1 1 calc R . . . .
C16 C 0.6922(2) 0.09922(19) 0.04997(17) 0.0234(5) Uani 1 1 d . . . . .
C14 C 0.6575(2) 0.1337(2) 0.21201(17) 0.0269(5) Uani 1 1 d . . . . .
H14 H 0.681732 0.133398 0.282261 0.032 Uiso 1 1 calc R . . . .
C9 C 0.8125(2) 0.4474(2) 0.3633(2) 0.0345(6) Uani 1 1 d . . . . .
H9 H 0.863450 0.434798 0.424449 0.041 Uiso 1 1 calc R . . . .
O019 O 0.7984(3) 0.4203(3) 0.62186(19) 0.0298(9) Uani 0.646(6) 1 d D . P A 1
H019 H 0.772375 0.469376 0.648355 0.045 Uiso 0.646(6) 1 calc GR . P A 1
C25 C 0.1086(2) 0.0796(2) 0.2167(2) 0.0387(6) Uani 1 1 d D . . . .
H25A H 0.060862 0.043031 0.147795 0.058 Uiso 1 1 calc GR . . . .
H25B H 0.073265 0.139264 0.237653 0.058 Uiso 1 1 calc GR . . . .
H25C H 0.104065 0.020246 0.261253 0.058 Uiso 1 1 calc GR . . . .
C11 C 0.7864(3) 0.5061(2) 0.1983(2) 0.0388(6) Uani 1 1 d . . . . .
H11 H 0.820702 0.535405 0.147302 0.047 Uiso 1 1 calc R . . . .
C10 C 0.8649(3) 0.4897(2) 0.2890(2) 0.0405(7) Uani 1 1 d . . . . .
H10 H 0.952678 0.507276 0.299395 0.049 Uiso 1 1 calc R . . . .
C01D C 0.4464(4) -0.0414(3) 0.3528(3) 0.0636(10) Uani 1 1 d . . . . .
H01G H 0.479027 -0.063816 0.298914 0.095 Uiso 1 1 calc GR . . . .
H01H H 0.355882 -0.054262 0.326231 0.095 Uiso 1 1 calc GR . . . .
H01I H 0.462951 -0.088602 0.406210 0.095 Uiso 1 1 calc GR . . . .
C01E C 0.8079(3) 0.3321(3) 0.6829(3) 0.0524(8) Uani 1 1 d D . . . .
H01A H 0.836658 0.273703 0.651201 0.079 Uiso 0.646(6) 1 calc GR . P A 1
H01B H 0.725694 0.294758 0.691178 0.079 Uiso 0.646(6) 1 calc GR . P A 1
H01C H 0.868073 0.366740 0.748695 0.079 Uiso 0.646(6) 1 calc GR . P A 1
H01D H 0.730181 0.273480 0.681507 0.079 Uiso 0.354(6) 1 calc GR . P A 2
H01E H 0.812118 0.406767 0.718444 0.079 Uiso 0.354(6) 1 calc GR . P A 2
H01F H 0.879927 0.306965 0.717587 0.079 Uiso 0.354(6) 1 calc GR . P A 2
C01F C 0.7912(4) 0.0246(4) 0.4868(4) 0.1075(18) Uani 1 1 d . . . . .
H01J H 0.771522 -0.016278 0.418883 0.161 Uiso 1 1 calc GR . . . .
H01K H 0.738857 -0.022152 0.522903 0.161 Uiso 1 1 calc GR . . . .
H01L H 0.879799 0.036686 0.522219 0.161 Uiso 1 1 calc GR . . . .
O0 O 0.8102(6) 0.3448(6) 0.5855(5) 0.050(2) Uani 0.354(6) 1 d D . P A 2
H0 H 0.788282 0.279020 0.551046 0.074 Uiso 0.354(6) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O2 2.2466(14) . ?
Ho1 O1 2.3097(14) . ?
Ho1 O3 2.4118(15) . ?
Ho1 O4 2.5327(16) . ?
Ho1 O5 2.4393(16) . ?
Ho1 N3 2.5210(18) . ?
Ho1 N4 2.5167(18) . ?
Ho1 N6 2.5379(19) . ?
Ho1 N1 2.5143(18) . ?
O2 C1 1.294(3) . ?
O1 C13 1.301(3) . ?
O3 H3 0.849(9) . ?
O3 C25 1.430(3) . ?
O4 N7 1.265(3) . ?
O7 N8 1.242(3) . ?
O5 N7 1.272(3) . ?
N3 C24 1.349(3) . ?
N3 C20 1.343(3) . ?
O8 N8 1.235(2) . ?
N4 N5 1.379(3) . ?
N4 C7 1.299(3) . ?
N6 C8 1.345(3) . ?
N6 C12 1.350(3) . ?
O00C H00C 0.8200 . ?
O00C C01D 1.417(4) . ?
N2 H2 0.8600 . ?
N2 N1 1.381(2) . ?
N2 C20 1.365(3) . ?
N1 C19 1.286(3) . ?
N5 H5 0.8600 . ?
N5 C8 1.361(3) . ?
N8 C16 1.440(3) . ?
O10 N9 1.228(3) . ?
O9 N9 1.235(3) . ?
N7 O6 1.219(3) . ?
C24 H24 0.9300 . ?
C24 C23 1.369(3) . ?
C1 C6 1.428(3) . ?
C1 C2 1.420(3) . ?
N9 C4 1.447(3) . ?
C20 C21 1.401(3) . ?
C6 C7 1.441(3) . ?
C6 C5 1.398(3) . ?
C18 C13 1.432(3) . ?
C18 C17 1.391(3) . ?
C18 C19 1.450(3) . ?
C13 C14 1.418(3) . ?
O00S H00S 0.8200 . ?
O00S C01F 1.396(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.404(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.380(3) . ?
C5 H5A 0.9300 . ?
C5 C4 1.380(3) . ?
C19 H19 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C3 1.364(3) . ?
C3 H3A 0.9300 . ?
C3 C4 1.401(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.388(3) . ?
C22 C21 1.371(3) . ?
C23 H23 0.9300 . ?
C12 H12 0.9300 . ?
C12 C11 1.372(4) . ?
C21 H21 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.395(3) . ?
C15 C14 1.370(3) . ?
C14 H14 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.369(4) . ?
O019 H019 0.8200 . ?
O019 C01E 1.388(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C11 H11 0.9300 . ?
C11 C10 1.385(4) . ?
C10 H10 0.9300 . ?
C01D H01G 0.9600 . ?
C01D H01H 0.9600 . ?
C01D H01I 0.9600 . ?
C01E H01A 0.9600 . ?
C01E H01B 0.9600 . ?
C01E H01C 0.9600 . ?
C01E H01D 0.9600 . ?
C01E H01E 0.9600 . ?
C01E H01F 0.9600 . ?
C01E O0 1.362(6) . ?
C01F H01J 0.9600 . ?
C01F H01K 0.9600 . ?
C01F H01L 0.9600 . ?
O0 H0 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ho1 O1 126.23(5) . . ?
O2 Ho1 O3 74.35(5) . . ?
O2 Ho1 O4 114.77(5) . . ?
O2 Ho1 O5 71.91(6) . . ?
O2 Ho1 N3 77.13(5) . . ?
O2 Ho1 N4 70.34(6) . . ?
O2 Ho1 N6 126.53(6) . . ?
O2 Ho1 N1 138.41(6) . . ?
O1 Ho1 O3 67.78(5) . . ?
O1 Ho1 O4 118.72(5) . . ?
O1 Ho1 O5 144.32(6) . . ?
O1 Ho1 N3 127.00(5) . . ?
O1 Ho1 N4 76.00(5) . . ?
O1 Ho1 N6 68.72(6) . . ?
O1 Ho1 N1 70.76(5) . . ?
O3 Ho1 O4 141.48(6) . . ?
O3 Ho1 O5 144.47(5) . . ?
O3 Ho1 N3 77.59(6) . . ?
O3 Ho1 N4 94.49(6) . . ?
O3 Ho1 N6 135.22(6) . . ?
O3 Ho1 N1 81.00(6) . . ?
O4 Ho1 N6 71.62(6) . . ?
O5 Ho1 O4 51.20(5) . . ?
O5 Ho1 N3 84.35(6) . . ?
O5 Ho1 N4 84.50(6) . . ?
O5 Ho1 N6 76.03(6) . . ?
O5 Ho1 N1 118.47(6) . . ?
N3 Ho1 O4 69.10(6) . . ?
N3 Ho1 N6 140.22(6) . . ?
N4 Ho1 O4 124.02(6) . . ?
N4 Ho1 N3 147.45(6) . . ?
N4 Ho1 N6 64.94(6) . . ?
N1 Ho1 O4 67.92(6) . . ?
N1 Ho1 N3 65.05(6) . . ?
N1 Ho1 N4 145.64(6) . . ?
N1 Ho1 N6 94.48(6) . . ?
C1 O2 Ho1 140.06(14) . . ?
C13 O1 Ho1 135.57(13) . . ?
Ho1 O3 H3 112.8(11) . . ?
C25 O3 Ho1 134.36(15) . . ?
C25 O3 H3 106.3(12) . . ?
N7 O4 Ho1 94.31(12) . . ?
N7 O5 Ho1 98.60(13) . . ?
C24 N3 Ho1 124.70(14) . . ?
C20 N3 Ho1 118.77(14) . . ?
C20 N3 C24 116.52(19) . . ?
N5 N4 Ho1 114.56(13) . . ?
C7 N4 Ho1 130.44(15) . . ?
C7 N4 N5 114.25(18) . . ?
C8 N6 Ho1 115.94(14) . . ?
C8 N6 C12 117.0(2) . . ?
C12 N6 Ho1 124.71(16) . . ?
C01D O00C H00C 109.5 . . ?
N1 N2 H2 119.8 . . ?
C20 N2 H2 119.7 . . ?
C20 N2 N1 120.50(17) . . ?
N2 N1 Ho1 115.51(12) . . ?
C19 N1 Ho1 129.00(15) . . ?
C19 N1 N2 114.57(18) . . ?
N4 N5 H5 119.8 . . ?
C8 N5 N4 120.49(19) . . ?
C8 N5 H5 119.8 . . ?
O7 N8 C16 118.47(19) . . ?
O8 N8 O7 122.42(19) . . ?
O8 N8 C16 119.1(2) . . ?
O4 N7 O5 115.88(18) . . ?
O6 N7 O4 122.7(2) . . ?
O6 N7 O5 121.4(2) . . ?
N3 C24 H24 117.9 . . ?
N3 C24 C23 124.2(2) . . ?
C23 C24 H24 117.9 . . ?
O2 C1 C6 121.4(2) . . ?
O2 C1 C2 120.5(2) . . ?
C2 C1 C6 118.11(19) . . ?
O10 N9 O9 122.0(2) . . ?
O10 N9 C4 119.0(2) . . ?
O9 N9 C4 119.1(2) . . ?
N3 C20 N2 117.96(19) . . ?
N3 C20 C21 123.1(2) . . ?
N2 C20 C21 118.97(19) . . ?
C1 C6 C7 123.23(19) . . ?
C5 C6 C1 119.1(2) . . ?
C5 C6 C7 117.6(2) . . ?
C13 C18 C19 123.57(19) . . ?
C17 C18 C13 119.8(2) . . ?
C17 C18 C19 116.30(19) . . ?
O1 C13 C18 121.90(19) . . ?
O1 C13 C14 120.65(19) . . ?
C14 C13 C18 117.43(19) . . ?
C01F O00S H00S 109.5 . . ?
N4 C7 C6 125.2(2) . . ?
N4 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
N6 C8 N5 119.0(2) . . ?
N6 C8 C9 123.0(2) . . ?
N5 C8 C9 117.9(2) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5A 119.9 . . ?
N1 C19 C18 125.7(2) . . ?
N1 C19 H19 117.1 . . ?
C18 C19 H19 117.1 . . ?
C1 C2 H2A 118.9 . . ?
C3 C2 C1 122.2(2) . . ?
C3 C2 H2A 118.9 . . ?
C2 C3 H3A 120.7 . . ?
C2 C3 C4 118.5(2) . . ?
C4 C3 H3A 120.7 . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C21 C22 C23 119.4(2) . . ?
C24 C23 C22 118.3(2) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
N6 C12 H12 118.4 . . ?
N6 C12 C11 123.3(2) . . ?
C11 C12 H12 118.4 . . ?
C20 C21 H21 120.8 . . ?
C22 C21 C20 118.5(2) . . ?
C22 C21 H21 120.8 . . ?
C5 C4 N9 119.4(2) . . ?
C5 C4 C3 121.7(2) . . ?
C3 C4 N9 118.8(2) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.1(2) . . ?
C17 C16 N8 118.4(2) . . ?
C17 C16 C15 121.3(2) . . ?
C15 C16 N8 120.2(2) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 C13 121.9(2) . . ?
C15 C14 H14 119.0 . . ?
C8 C9 H9 120.9 . . ?
C10 C9 C8 118.2(3) . . ?
C10 C9 H9 120.9 . . ?
C01E O019 H019 109.5 . . ?
O3 C25 H25A 109.5 . . ?
O3 C25 H25B 109.5 . . ?
O3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C12 C11 H11 120.5 . . ?
C12 C11 C10 118.9(2) . . ?
C10 C11 H11 120.5 . . ?
C9 C10 C11 119.6(2) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
O00C C01D H01G 109.5 . . ?
O00C C01D H01H 109.5 . . ?
O00C C01D H01I 109.5 . . ?
H01G C01D H01H 109.5 . . ?
H01G C01D H01I 109.5 . . ?
H01H C01D H01I 109.5 . . ?
O019 C01E H01A 109.5 . . ?
O019 C01E H01B 109.5 . . ?
O019 C01E H01C 109.5 . . ?
H01A C01E H01B 109.5 . . ?
H01A C01E H01C 109.5 . . ?
H01B C01E H01C 109.5 . . ?
H01D C01E H01E 109.5 . . ?
H01D C01E H01F 109.5 . . ?
H01E C01E H01F 109.5 . . ?
O0 C01E H01D 109.5 . . ?
O0 C01E H01E 109.5 . . ?
O0 C01E H01F 109.5 . . ?
O00S C01F H01J 109.5 . . ?
O00S C01F H01K 109.5 . . ?
O00S C01F H01L 109.5 . . ?
H01J C01F H01K 109.5 . . ?
H01J C01F H01L 109.5 . . ?
H01K C01F H01L 109.5 . . ?
C01E O0 H0 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.168
_oxdiff_exptl_absorpt_empirical_full_min 0.856
# start Validation Reply Form
_vrf_PLAT417_aj0806              
;
Problem: ALERT_2_B Short Inter H5 ..H0 . 2.01 Ang.
 	x,y,z = 1_555 Check
	ALERT_2_B Short Inter D-H..H-D H00S ..H0 . 1.98 Ang.
 	x,y,z = 1_555 Check 

RESPONSE: The H0 atom belongs to a disordered MeOH solvent molecule 
	which is involved in short interactions.        
;
# End Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mono_gd
_database_code_depnum_ccdc_archive 'CCDC 1891542'
loop_
_audit_author_name
_audit_author_address
'PANKAJ KALITA'
;National Institute of Science Education and Research
India
;
_audit_update_record             
;
2019-03-04 deposited with the CCDC.	2019-03-07 downloaded from the CCDC.
;
_audit_creation_date             2019-03-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H22 Gd N9 O10, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 Gd N9 O13'
_chemical_formula_weight         861.89
_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'
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2570(4)
_cell_length_b                   11.7166(4)
_cell_length_c                   13.7355(5)
_cell_angle_alpha                94.1350(10)
_cell_angle_beta                 104.9910(10)
_cell_angle_gamma                105.1770(10)
_cell_volume                     1669.83(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.065
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0755 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.8340.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25878
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.406
_diffrn_reflns_theta_min         2.566
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6970
_reflns_number_total             8366
_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       
;
'SAINT V8.35A (?, 2016)'
;
_computing_data_collection       
;
'SAINT V8.35A (?, 2016)'
;
_computing_data_reduction        
;
'SAINT V8.35A (?, 2016)'
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8366
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.023
_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)+(0.0353P)²+0.5821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0778
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 C01C-H3
 1.913106 with sigma of 0.02
 Gd1-H3
 2.929969 with sigma of 0.02
 O0AA-C0AA \\sim O0AB-C0AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O0AA) = Uanis(O0AB)
4. Others
 Sof(H0AE)=Sof(H0AF)=Sof(H0AG)=Sof(O0AB)=Sof(H0AH)=1-FVAR(1)
 Sof(O0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=FVAR(1)
5.a Riding coordinates:
 C0AA(H0AB,H0AC,H0AD), C0AA(H0AE,H0AF,H0AG)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C7(H7), C5(H5A), C24(H24), C12(H12), C17(H17), C19(H19),
 C3(H3A), C14(H14), C15(H15), C2(H2A), C21(H21), C10(H10), C11(H11), C23(H23),
 C9(H9), C22(H22)
5.c Idealised Me refined as rotating group:
 C01C(H01A,H01B,H01C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
5.d Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O8(H8), O0AA(H0AA), O0AB(H0AH)
;
_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 0.63364(2) 0.66413(2) 0.77552(2) 0.01268(6) Uani 1 1 d D . . . .
O1 O 0.5190(2) 0.8028(2) 0.77943(16) 0.0164(5) Uani 1 1 d . . . . .
O2 O 0.7546(2) 0.6429(2) 0.66876(16) 0.0164(5) Uani 1 1 d . . . . .
O5 O 0.6056(2) 0.5024(2) 0.88812(18) 0.0218(5) Uani 1 1 d . . . . .
O3 O 0.7625(2) 0.8666(2) 0.77505(18) 0.0190(5) Uani 1 1 d D . . . .
H3 H 0.739(2) 0.9224(13) 0.804(3) 0.029 Uiso 1 1 d DR . . . .
O4 O 0.6144(2) 0.4494(2) 0.73711(18) 0.0232(6) Uani 1 1 d . . . . .
O12 O 0.2783(2) 0.9491(2) 1.10954(17) 0.0204(5) Uani 1 1 d . . . . .
O13 O 0.1523(2) 0.9898(2) 0.97628(19) 0.0268(6) Uani 1 1 d . . . . .
O11 O 0.7444(3) 0.7965(2) 0.24272(18) 0.0288(6) Uani 1 1 d . . . . .
N1 N 0.6672(3) 0.7506(2) 0.96004(19) 0.0148(6) Uani 1 1 d . . . . .
N3 N 0.8497(3) 0.6761(2) 0.9009(2) 0.0151(6) Uani 1 1 d . . . . .
N2 N 0.7713(3) 0.7359(2) 1.0307(2) 0.0171(6) Uani 1 1 d . . . . .
H2 H 0.775068 0.742878 1.095696 0.021 Uiso 1 1 calc R . . . .
O10 O 0.9455(3) 0.8075(2) 0.30194(19) 0.0295(6) Uani 1 1 d . . . . .
O7 O 0.4939(3) 0.9171(2) 0.6083(2) 0.0337(7) Uani 1 1 d . . . . .
H7A H 0.502423 0.877843 0.657196 0.051 Uiso 1 1 calc GR . . . .
N4 N 0.5006(3) 0.6420(2) 0.59017(19) 0.0147(6) Uani 1 1 d . . . . .
N6 N 0.3924(3) 0.5603(2) 0.7366(2) 0.0156(6) Uani 1 1 d . . . . .
N5 N 0.3710(3) 0.6213(3) 0.5772(2) 0.0194(6) Uani 1 1 d . . . . .
H5 H 0.322540 0.636027 0.520997 0.023 Uiso 1 1 calc R . . . .
N7 N 0.6009(3) 0.4187(3) 0.8225(2) 0.0223(7) Uani 1 1 d . . . . .
N8 N 0.2414(3) 0.9494(2) 1.0161(2) 0.0198(6) Uani 1 1 d . . . . .
N9 N 0.8359(3) 0.7864(3) 0.3107(2) 0.0213(7) Uani 1 1 d . . . . .
O6 O 0.5845(3) 0.3161(2) 0.8378(2) 0.0387(7) Uani 1 1 d . . . . .
C6 C 0.4796(3) 0.8224(3) 0.9413(2) 0.0136(7) Uani 1 1 d . . . . .
C7 C 0.5893(3) 0.7897(3) 0.9980(2) 0.0153(7) Uani 1 1 d . . . . .
H7 H 0.605878 0.797703 1.069945 0.018 Uiso 1 1 calc R . . . .
C5 C 0.4079(3) 0.8612(3) 0.9988(2) 0.0150(7) Uani 1 1 d . . . . .
H5A H 0.428699 0.858239 1.069988 0.018 Uiso 1 1 calc R . . . .
C24 C 0.3333(3) 0.5168(3) 0.8061(3) 0.0188(7) Uani 1 1 d . . . . .
H24 H 0.384835 0.504062 0.868637 0.023 Uiso 1 1 calc R . . . .
C13 C 0.7713(3) 0.6775(3) 0.5842(2) 0.0151(7) Uani 1 1 d . . . . .
C1 C 0.4493(3) 0.8292(3) 0.8349(2) 0.0145(7) Uani 1 1 d . . . . .
C8 C 0.8693(3) 0.7103(3) 1.0002(2) 0.0144(7) Uani 1 1 d . . . . .
O8 O 0.2331(3) 0.8615(3) 0.5195(3) 0.0499(9) Uani 1 1 d . . . . .
H8 H 0.312264 0.869451 0.533223 0.075 Uiso 1 1 calc GR . . . .
C12 C 0.9470(3) 0.6494(3) 0.8734(3) 0.0192(7) Uani 1 1 d . . . . .
H12 H 0.934944 0.625868 0.803035 0.023 Uiso 1 1 calc R . . . .
C18 C 0.6673(3) 0.6888(3) 0.5043(2) 0.0152(7) Uani 1 1 d . . . . .
C17 C 0.6905(3) 0.7229(3) 0.4139(2) 0.0172(7) Uani 1 1 d . . . . .
H17 H 0.621597 0.728645 0.359273 0.021 Uiso 1 1 calc R . . . .
C4 C 0.3070(3) 0.9037(3) 0.9529(3) 0.0162(7) Uani 1 1 d . . . . .
C16 C 0.8131(3) 0.7482(3) 0.4036(2) 0.0169(7) Uani 1 1 d . . . . .
C20 C 0.3168(3) 0.5787(3) 0.6494(2) 0.0163(7) Uani 1 1 d . . . . .
C19 C 0.5366(3) 0.6636(3) 0.5100(2) 0.0163(7) Uani 1 1 d . . . . .
H19 H 0.471972 0.662927 0.449557 0.020 Uiso 1 1 calc R . . . .
C3 C 0.2724(3) 0.9062(3) 0.8484(3) 0.0203(7) Uani 1 1 d . . . . .
H3A H 0.200869 0.932919 0.817271 0.024 Uiso 1 1 calc R . . . .
C14 C 0.8942(3) 0.7021(3) 0.5689(3) 0.0185(7) Uani 1 1 d . . . . .
H14 H 0.963631 0.693270 0.621297 0.022 Uiso 1 1 calc R . . . .
C15 C 0.9168(3) 0.7382(3) 0.4813(3) 0.0213(8) Uani 1 1 d . . . . .
H15 H 1.000769 0.756022 0.473292 0.026 Uiso 1 1 calc R . . . .
C2 C 0.3420(3) 0.8700(3) 0.7911(3) 0.0202(7) Uani 1 1 d . . . . .
H2A H 0.318062 0.872079 0.719790 0.024 Uiso 1 1 calc R . . . .
C21 C 0.1834(3) 0.5557(3) 0.6296(3) 0.0214(8) Uani 1 1 d . . . . .
H21 H 0.133066 0.570960 0.567668 0.026 Uiso 1 1 calc R . . . .
C10 C 1.0811(3) 0.6908(3) 1.0436(3) 0.0184(7) Uani 1 1 d . . . . .
H10 H 1.160155 0.695820 1.092325 0.022 Uiso 1 1 calc R . . . .
C11 C 1.0621(3) 0.6543(3) 0.9409(3) 0.0193(7) Uani 1 1 d . . . . .
H11 H 1.127429 0.633327 0.918062 0.023 Uiso 1 1 calc R . . . .
C23 C 0.2039(3) 0.4903(3) 0.7916(3) 0.0228(8) Uani 1 1 d . . . . .
H23 H 0.166766 0.458333 0.842101 0.027 Uiso 1 1 calc R . . . .
C9 C 0.9850(3) 0.7192(3) 1.0736(2) 0.0169(7) Uani 1 1 d . . . . .
H9 H 0.996231 0.744840 1.143434 0.020 Uiso 1 1 calc R . . . .
C22 C 0.1273(3) 0.5109(3) 0.7017(3) 0.0237(8) Uani 1 1 d . . . . .
H22 H 0.037079 0.494128 0.690214 0.028 Uiso 1 1 calc R . . . .
C01C C 0.8945(3) 0.9193(3) 0.7787(3) 0.0280(9) Uani 1 1 d D . . . .
H01A H 0.899694 0.981807 0.734891 0.042 Uiso 1 1 calc GR . . . .
H01B H 0.928869 0.857592 0.754686 0.042 Uiso 1 1 calc GR . . . .
H01C H 0.944788 0.954540 0.848980 0.042 Uiso 1 1 calc GR . . . .
C25 C 0.5566(4) 1.0403(4) 0.6450(3) 0.0450(12) Uani 1 1 d . . . . .
H25A H 0.537934 1.087072 0.589590 0.068 Uiso 1 1 calc GR . . . .
H25B H 0.649548 1.053132 0.669882 0.068 Uiso 1 1 calc GR . . . .
H25C H 0.525424 1.065858 0.700763 0.068 Uiso 1 1 calc GR . . . .
C26 C 0.2126(5) 0.9757(4) 0.5216(5) 0.0649(17) Uani 1 1 d . . . . .
H26A H 0.263143 1.024169 0.482828 0.097 Uiso 1 1 calc GR . . . .
H26B H 0.239352 1.015267 0.592326 0.097 Uiso 1 1 calc GR . . . .
H26C H 0.121163 0.966741 0.491042 0.097 Uiso 1 1 calc GR . . . .
O0AA O 0.2024(3) 0.5859(3) 0.3775(2) 0.0250(8) Uani 0.814(5) 1 d D . P A 1
H0AA H 0.231319 0.535384 0.352333 0.038 Uiso 0.814(5) 1 calc GR . P A 1
C0AA C 0.1914(4) 0.6722(4) 0.3138(3) 0.0389(10) Uani 1 1 d D . . . .
H0AB H 0.162285 0.634090 0.242463 0.058 Uiso 0.814(5) 1 d R . P A 1
H0AC H 0.129045 0.711450 0.327023 0.058 Uiso 0.814(5) 1 d R . P A 1
H0AD H 0.275295 0.731910 0.327023 0.058 Uiso 0.814(5) 1 d R . P A 1
H0AE H 0.118295 0.609390 0.268283 0.058 Uiso 0.186(5) 1 d R . P A 2
H0AF H 0.181065 0.750790 0.300983 0.058 Uiso 0.186(5) 1 d R . P A 2
H0AG H 0.271195 0.665420 0.300983 0.058 Uiso 0.186(5) 1 d R . P A 2
O0AB O 0.1962(13) 0.6605(14) 0.4098(9) 0.0250(8) Uani 0.186(5) 1 d D . P A 2
H0AH H 0.208814 0.727683 0.443118 0.038 Uiso 0.186(5) 1 calc GR . P A 2


_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 O1 2.330(2) . ?
Gd1 O2 2.285(2) . ?
Gd1 O5 2.538(2) . ?
Gd1 O3 2.437(2) . ?
Gd1 O4 2.473(2) . ?
Gd1 N1 2.555(3) . ?
Gd1 N3 2.554(3) . ?
Gd1 N4 2.554(3) . ?
Gd1 N6 2.562(3) . ?
O1 C1 1.301(4) . ?
O2 C13 1.299(4) . ?
O5 N7 1.264(4) . ?
O3 H3 0.875(9) . ?
O3 C01C 1.438(4) . ?
O4 N7 1.285(4) . ?
O12 N8 1.243(4) . ?
O13 N8 1.238(3) . ?
O11 N9 1.236(4) . ?
N1 N2 1.373(4) . ?
N1 C7 1.290(4) . ?
N3 C8 1.337(4) . ?
N3 C12 1.347(4) . ?
N2 H2 0.8800 . ?
N2 C8 1.370(4) . ?
O10 N9 1.233(4) . ?
O7 H7A 0.8400 . ?
O7 C25 1.419(5) . ?
N4 N5 1.376(4) . ?
N4 C19 1.288(4) . ?
N6 C24 1.355(4) . ?
N6 C20 1.346(4) . ?
N5 H5 0.8800 . ?
N5 C20 1.352(4) . ?
N7 O6 1.210(4) . ?
N8 C4 1.434(4) . ?
N9 C16 1.444(4) . ?
C6 C7 1.439(4) . ?
C6 C5 1.397(4) . ?
C6 C1 1.425(4) . ?
C7 H7 0.9500 . ?
C5 H5A 0.9500 . ?
C5 C4 1.382(4) . ?
C24 H24 0.9500 . ?
C24 C23 1.364(5) . ?
C13 C18 1.425(5) . ?
C13 C14 1.412(5) . ?
C1 C2 1.420(5) . ?
C8 C9 1.399(4) . ?
O8 H8 0.8400 . ?
O8 C26 1.415(5) . ?
C12 H12 0.9500 . ?
C12 C11 1.370(5) . ?
C18 C17 1.398(4) . ?
C18 C19 1.447(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.380(5) . ?
C4 C3 1.390(5) . ?
C16 C15 1.400(5) . ?
C20 C21 1.403(5) . ?
C19 H19 0.9500 . ?
C3 H3A 0.9500 . ?
C3 C2 1.364(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.366(4) . ?
C15 H15 0.9500 . ?
C2 H2A 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.371(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(5) . ?
C10 C9 1.360(5) . ?
C11 H11 0.9500 . ?
C23 H23 0.9500 . ?
C23 C22 1.388(5) . ?
C9 H9 0.9500 . ?
C22 H22 0.9500 . ?
C01C H01A 0.9800 . ?
C01C H01B 0.9800 . ?
C01C H01C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O0AA H0AA 0.8400 . ?
O0AA C0AA 1.394(5) . ?
C0AA H0AB 0.9801 . ?
C0AA H0AC 0.9799 . ?
C0AA H0AD 0.9800 . ?
C0AA H0AE 0.9801 . ?
C0AA H0AF 0.9800 . ?
C0AA H0AG 0.9802 . ?
C0AA O0AB 1.325(11) . ?
O0AB H0AH 0.8400 . ?

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 Gd1 O5 117.68(8) . . ?
O1 Gd1 O3 67.89(8) . . ?
O1 Gd1 O4 144.56(8) . . ?
O1 Gd1 N1 70.21(8) . . ?
O1 Gd1 N3 125.64(8) . . ?
O1 Gd1 N4 76.43(8) . . ?
O1 Gd1 N6 68.70(8) . . ?
O2 Gd1 O1 127.45(8) . . ?
O2 Gd1 O5 114.53(8) . . ?
O2 Gd1 O3 74.95(8) . . ?
O2 Gd1 O4 71.27(8) . . ?
O2 Gd1 N1 138.71(8) . . ?
O2 Gd1 N3 77.93(8) . . ?
O2 Gd1 N4 69.86(8) . . ?
O2 Gd1 N6 124.70(8) . . ?
O5 Gd1 N1 67.89(8) . . ?
O5 Gd1 N3 69.82(8) . . ?
O5 Gd1 N4 124.45(8) . . ?
O5 Gd1 N6 72.15(8) . . ?
O3 Gd1 O5 142.29(8) . . ?
O3 Gd1 O4 144.44(8) . . ?
O3 Gd1 N1 81.38(8) . . ?
O3 Gd1 N3 77.49(8) . . ?
O3 Gd1 N4 93.25(8) . . ?
O3 Gd1 N6 134.63(8) . . ?
O4 Gd1 O5 50.95(8) . . ?
O4 Gd1 N1 118.04(8) . . ?
O4 Gd1 N3 84.85(8) . . ?
O4 Gd1 N4 85.47(8) . . ?
O4 Gd1 N6 76.03(8) . . ?
N1 Gd1 N6 95.96(9) . . ?
N3 Gd1 N1 64.06(8) . . ?
N3 Gd1 N6 141.47(8) . . ?
N4 Gd1 N1 145.77(9) . . ?
N4 Gd1 N3 147.79(8) . . ?
N4 Gd1 N6 64.15(9) . . ?
C1 O1 Gd1 135.6(2) . . ?
C13 O2 Gd1 138.6(2) . . ?
N7 O5 Gd1 95.50(18) . . ?
Gd1 O3 H3 113.8(13) . . ?
C01C O3 Gd1 134.1(2) . . ?
C01C O3 H3 106.3(13) . . ?
N7 O4 Gd1 98.02(19) . . ?
N2 N1 Gd1 115.87(18) . . ?
C7 N1 Gd1 128.3(2) . . ?
C7 N1 N2 114.9(3) . . ?
C8 N3 Gd1 119.0(2) . . ?
C8 N3 C12 117.1(3) . . ?
C12 N3 Gd1 123.9(2) . . ?
N1 N2 H2 119.9 . . ?
C8 N2 N1 120.2(3) . . ?
C8 N2 H2 119.9 . . ?
C25 O7 H7A 109.5 . . ?
N5 N4 Gd1 114.00(18) . . ?
C19 N4 Gd1 130.2(2) . . ?
C19 N4 N5 115.0(3) . . ?
C24 N6 Gd1 124.9(2) . . ?
C20 N6 Gd1 116.1(2) . . ?
C20 N6 C24 116.6(3) . . ?
N4 N5 H5 119.4 . . ?
C20 N5 N4 121.1(3) . . ?
C20 N5 H5 119.4 . . ?
O5 N7 O4 115.5(3) . . ?
O6 N7 O5 122.9(3) . . ?
O6 N7 O4 121.5(3) . . ?
O12 N8 C4 118.5(3) . . ?
O13 N8 O12 122.4(3) . . ?
O13 N8 C4 119.1(3) . . ?
O11 N9 C16 118.6(3) . . ?
O10 N9 O11 122.4(3) . . ?
O10 N9 C16 118.9(3) . . ?
C5 C6 C7 115.8(3) . . ?
C5 C6 C1 119.4(3) . . ?
C1 C6 C7 124.4(3) . . ?
N1 C7 C6 126.0(3) . . ?
N1 C7 H7 117.0 . . ?
C6 C7 H7 117.0 . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5A 119.8 . . ?
N6 C24 H24 118.1 . . ?
N6 C24 C23 123.8(3) . . ?
C23 C24 H24 118.1 . . ?
O2 C13 C18 121.7(3) . . ?
O2 C13 C14 120.0(3) . . ?
C14 C13 C18 118.3(3) . . ?
O1 C1 C6 121.8(3) . . ?
O1 C1 C2 120.4(3) . . ?
C2 C1 C6 117.7(3) . . ?
N3 C8 N2 118.4(3) . . ?
N3 C8 C9 122.5(3) . . ?
N2 C8 C9 119.1(3) . . ?
C26 O8 H8 109.5 . . ?
N3 C12 H12 118.1 . . ?
N3 C12 C11 123.8(3) . . ?
C11 C12 H12 118.1 . . ?
C13 C18 C19 123.5(3) . . ?
C17 C18 C13 119.0(3) . . ?
C17 C18 C19 117.4(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 C18 120.3(3) . . ?
C16 C17 H17 119.9 . . ?
C5 C4 N8 118.3(3) . . ?
C5 C4 C3 121.0(3) . . ?
C3 C4 N8 120.6(3) . . ?
C17 C16 N9 119.5(3) . . ?
C17 C16 C15 121.6(3) . . ?
C15 C16 N9 118.8(3) . . ?
N6 C20 N5 119.0(3) . . ?
N6 C20 C21 122.9(3) . . ?
N5 C20 C21 118.1(3) . . ?
N4 C19 C18 125.5(3) . . ?
N4 C19 H19 117.3 . . ?
C18 C19 H19 117.3 . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3A 120.3 . . ?
C13 C14 H14 118.8 . . ?
C15 C14 C13 122.3(3) . . ?
C15 C14 H14 118.8 . . ?
C16 C15 H15 120.8 . . ?
C14 C15 C16 118.3(3) . . ?
C14 C15 H15 120.8 . . ?
C1 C2 H2A 119.1 . . ?
C3 C2 C1 121.9(3) . . ?
C3 C2 H2A 119.1 . . ?
C20 C21 H21 120.7 . . ?
C22 C21 C20 118.6(3) . . ?
C22 C21 H21 120.7 . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C9 C10 C11 119.2(3) . . ?
C12 C11 C10 118.3(3) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C24 C23 H23 120.5 . . ?
C24 C23 C22 118.9(3) . . ?
C22 C23 H23 120.5 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C21 C22 C23 119.2(3) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
O3 C01C H01A 109.5 . . ?
O3 C01C H01B 109.5 . . ?
O3 C01C H01C 109.5 . . ?
H01A C01C H01B 109.5 . . ?
H01A C01C H01C 109.5 . . ?
H01B C01C H01C 109.5 . . ?
O7 C25 H25A 109.5 . . ?
O7 C25 H25B 109.5 . . ?
O7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O8 C26 H26A 109.5 . . ?
O8 C26 H26B 109.5 . . ?
O8 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C0AA O0AA H0AA 109.5 . . ?
O0AA C0AA H0AB 109.5 . . ?
O0AA C0AA H0AC 109.5 . . ?
O0AA C0AA H0AD 109.4 . . ?
H0AB C0AA H0AC 109.5 . . ?
H0AB C0AA H0AD 109.5 . . ?
H0AC C0AA H0AD 109.5 . . ?
H0AE C0AA H0AF 109.5 . . ?
H0AE C0AA H0AG 109.5 . . ?
H0AF C0AA H0AG 109.5 . . ?
O0AB C0AA H0AE 109.5 . . ?
O0AB C0AA H0AF 109.3 . . ?
O0AB C0AA H0AG 109.6 . . ?
C0AA O0AB H0AH 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
Gd1 O1 C1 C6 35.6(5) . . . . ?
Gd1 O1 C1 C2 -146.6(3) . . . . ?
Gd1 O2 C13 C18 -36.0(5) . . . . ?
Gd1 O2 C13 C14 145.6(3) . . . . ?
Gd1 O5 N7 O4 1.7(3) . . . . ?
Gd1 O5 N7 O6 -178.2(3) . . . . ?
Gd1 O4 N7 O5 -1.7(3) . . . . ?
Gd1 O4 N7 O6 178.2(3) . . . . ?
Gd1 N1 N2 C8 18.9(4) . . . . ?
Gd1 N1 C7 C6 -17.3(5) . . . . ?
Gd1 N3 C8 N2 0.9(4) . . . . ?
Gd1 N3 C8 C9 -179.9(2) . . . . ?
Gd1 N3 C12 C11 -179.1(3) . . . . ?
Gd1 N4 N5 C20 -20.1(4) . . . . ?
Gd1 N4 C19 C18 10.7(5) . . . . ?
Gd1 N6 C24 C23 162.4(3) . . . . ?
Gd1 N6 C20 N5 17.1(4) . . . . ?
Gd1 N6 C20 C21 -162.8(3) . . . . ?
O1 C1 C2 C3 -175.4(3) . . . . ?
O2 C13 C18 C17 -178.1(3) . . . . ?
O2 C13 C18 C19 0.2(5) . . . . ?
O2 C13 C14 C15 179.7(3) . . . . ?
O12 N8 C4 C5 0.3(4) . . . . ?
O12 N8 C4 C3 -177.6(3) . . . . ?
O13 N8 C4 C5 178.7(3) . . . . ?
O13 N8 C4 C3 0.9(5) . . . . ?
O11 N9 C16 C17 0.7(5) . . . . ?
O11 N9 C16 C15 -179.2(3) . . . . ?
N1 N2 C8 N3 -13.5(4) . . . . ?
N1 N2 C8 C9 167.3(3) . . . . ?
N3 C8 C9 C10 -0.9(5) . . . . ?
N3 C12 C11 C10 -1.1(5) . . . . ?
N2 N1 C7 C6 174.4(3) . . . . ?
N2 C8 C9 C10 178.3(3) . . . . ?
O10 N9 C16 C17 -179.2(3) . . . . ?
O10 N9 C16 C15 0.9(5) . . . . ?
N4 N5 C20 N6 2.3(5) . . . . ?
N4 N5 C20 C21 -177.9(3) . . . . ?
N6 C24 C23 C22 -1.4(5) . . . . ?
N6 C20 C21 C22 -1.0(5) . . . . ?
N5 N4 C19 C18 179.6(3) . . . . ?
N5 C20 C21 C22 179.1(3) . . . . ?
N8 C4 C3 C2 175.5(3) . . . . ?
N9 C16 C15 C14 180.0(3) . . . . ?
C6 C5 C4 N8 -176.2(3) . . . . ?
C6 C5 C4 C3 1.6(5) . . . . ?
C6 C1 C2 C3 2.5(5) . . . . ?
C7 N1 N2 C8 -171.3(3) . . . . ?
C7 C6 C5 C4 174.8(3) . . . . ?
C7 C6 C1 O1 1.7(5) . . . . ?
C7 C6 C1 C2 -176.2(3) . . . . ?
C5 C6 C7 N1 179.2(3) . . . . ?
C5 C6 C1 O1 174.7(3) . . . . ?
C5 C6 C1 C2 -3.1(5) . . . . ?
C5 C4 C3 C2 -2.3(5) . . . . ?
C24 N6 C20 N5 -179.6(3) . . . . ?
C24 N6 C20 C21 0.5(5) . . . . ?
C24 C23 C22 C21 0.8(5) . . . . ?
C13 C18 C17 C16 -1.7(5) . . . . ?
C13 C18 C19 N4 8.5(5) . . . . ?
C13 C14 C15 C16 -1.5(5) . . . . ?
C1 C6 C7 N1 -7.5(5) . . . . ?
C1 C6 C5 C4 1.2(5) . . . . ?
C8 N3 C12 C11 0.7(5) . . . . ?
C12 N3 C8 N2 -178.8(3) . . . . ?
C12 N3 C8 C9 0.3(5) . . . . ?
C18 C13 C14 C15 1.2(5) . . . . ?
C18 C17 C16 N9 -178.4(3) . . . . ?
C18 C17 C16 C15 1.5(5) . . . . ?
C17 C18 C19 N4 -173.2(3) . . . . ?
C17 C16 C15 C14 0.1(5) . . . . ?
C4 C3 C2 C1 0.2(5) . . . . ?
C20 N6 C24 C23 0.8(5) . . . . ?
C20 C21 C22 C23 0.3(5) . . . . ?
C19 N4 N5 C20 169.1(3) . . . . ?
C19 C18 C17 C16 179.9(3) . . . . ?
C14 C13 C18 C17 0.4(5) . . . . ?
C14 C13 C18 C19 178.6(3) . . . . ?
C11 C10 C9 C8 0.4(5) . . . . ?
C9 C10 C11 C12 0.5(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT417_mono_gd             
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Problem: ALERT_2_B Short Inter D-H..H-D       H5       ..H0AH     .       2.03 Ang.  
                                                      x,y,z  =      1_555 Check 
Short Inter D-H..H-D       H8       ..H0AH     .       1.90 Ang.  
                                                      x,y,z  =      1_555 Check 

RESPONSE: The H0AH atom belongs to a disordered MeOH solvent molecule 
	which is involved in short interactions.        
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# start Validation Reply Form
