# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

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

data_nm240a77small
_database_code_depnum_ccdc_archive 'CCDC 2320542'
loop_
_audit_author_name
_audit_author_address
'Miguel Clemente-Leon' 'Universidad de Valencia'
_audit_update_record             
;
2023-12-22 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_audit_creation_date             2023-12-22
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H20 Dy2 N18 O16, 9(H2 O)'
_chemical_formula_sum            'C30 H38 Dy2 N18 O25'
_chemical_formula_weight         1375.78
_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                   8.9737(4)
_cell_length_b                   9.4011(4)
_cell_length_c                   15.5290(6)
_cell_angle_alpha                75.273(4)
_cell_angle_beta                 77.475(4)
_cell_angle_gamma                68.042(4)
_cell_volume                     1164.23(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    14175
_cell_measurement_temperature    120.4(9)
_cell_measurement_theta_max      27.4180
_cell_measurement_theta_min      3.9170
_shelx_estimated_absorpt_T_max   0.674
_shelx_estimated_absorpt_T_min   0.531
_exptl_absorpt_coefficient_mu    3.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17487
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.267
_diffrn_ambient_temperature      120.4(9)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -82.00    8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442  -64.0000  -38.0272 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -83.00    9.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442  -67.0000 -143.9906 92

#__ type_ start__ end____ width___ exp.time_
  3 omega  -83.00    9.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0442  -69.0000   65.3698 92

#__ type_ start__ end____ width___ exp.time_
  4 omega  -52.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -64.0000   13.6391 91

#__ type_ start__ end____ width___ exp.time_
  5 omega  -52.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -66.0000  103.0586 91

#__ type_ start__ end____ width___ exp.time_
  6 omega   -6.00   85.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255   57.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
  7 omega  -52.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -64.0000  -78.2193 91

#__ type_ start__ end____ width___ exp.time_
  8 omega  -52.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -68.0000 -173.7221 92

#__ type_ start__ end____ width___ exp.time_
  9 omega  -52.00  -23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8255  -67.0000 -125.2935 29
;
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0072278000
_diffrn_orient_matrix_UB_12      -0.0450205000
_diffrn_orient_matrix_UB_13      0.0440676000
_diffrn_orient_matrix_UB_21      0.0471034000
_diffrn_orient_matrix_UB_22      0.0411339000
_diffrn_orient_matrix_UB_23      0.0069503000
_diffrn_orient_matrix_UB_31      -0.0716152000
_diffrn_orient_matrix_UB_32      0.0561261000
_diffrn_orient_matrix_UB_33      0.0167945000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4714
_reflns_number_total             4931
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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         0.899
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4931
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.071
_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)+(0.0164P)²+1.5579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0460
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5) O12(0.5) H12A(0.5) H12B(0.5) O13(0.5)
 H13A(0.5) H13B(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.5) H15A(0.5) H15B(0.5)
3.a Free rotating group:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B),
 O14(H14A,H14B), O15(H15A,H15B)
3.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C14(H14), C15(H15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.66455(2) 0.60899(2) 0.21429(2) 0.01114(4) Uani 1 1 d . . . . .
O1 O 0.4456(2) 0.6187(2) 0.32960(11) 0.0139(4) Uani 1 1 d . . . . .
O2 O 0.2573(2) 0.5079(2) 0.63680(11) 0.0137(4) Uani 1 1 d . . . . .
O3 O 0.4630(2) 0.5384(2) 0.16863(11) 0.0162(4) Uani 1 1 d . . . . .
O4 O 0.2654(2) 0.4596(2) -0.06503(11) 0.0171(4) Uani 1 1 d . . . . .
O5 O 0.4428(2) 0.8371(2) 0.16577(12) 0.0191(4) Uani 1 1 d . . . . .
O6 O 0.2592(2) 1.1961(2) -0.09269(12) 0.0196(4) Uani 1 1 d . . . . .
O7 O 0.7336(2) 0.3304(2) 0.24494(12) 0.0169(4) Uani 1 1 d . . . . .
H7A H 0.781970 0.292478 0.196195 0.025 Uiso 1 1 d GR . . . .
H7B H 0.646145 0.304388 0.258978 0.025 Uiso 1 1 d GR . . . .
O8 O 0.7036(2) 0.7941(2) 0.28034(12) 0.0213(4) Uani 1 1 d . . . . .
H8A H 0.778637 0.747860 0.315479 0.032 Uiso 1 1 d GR . . . .
H8B H 0.617167 0.833860 0.316668 0.032 Uiso 1 1 d GR . . . .
O9 O 0.8877(2) 0.1283(2) 0.37913(14) 0.0230(4) Uani 1 1 d . . . . .
H9A H 0.908314 0.169605 0.415849 0.034 Uiso 1 1 d G . . . .
H9B H 0.975354 0.065208 0.357317 0.034 Uiso 1 1 d G . . . .
N1 N -0.0425(3) 0.6951(3) 0.38985(15) 0.0197(5) Uani 1 1 d . . . . .
N2 N 0.0454(3) 0.7197(3) 0.50838(15) 0.0208(5) Uani 1 1 d . . . . .
N3 N 0.1706(2) 0.6277(2) 0.45768(13) 0.0103(4) Uani 1 1 d . . . . .
N4 N -0.0337(3) 0.5226(3) 0.18871(14) 0.0144(4) Uani 1 1 d . . . . .
N5 N 0.2242(3) 0.3666(3) 0.19823(16) 0.0285(6) Uani 1 1 d . . . . .
N6 N 0.2145(2) 0.4788(2) 0.12116(13) 0.0128(4) Uani 1 1 d . . . . .
N7 N -0.0839(3) 1.1424(3) 0.12784(15) 0.0227(5) Uani 1 1 d . . . . .
N8 N 0.1075(3) 0.9155(3) 0.09985(16) 0.0212(5) Uani 1 1 d . . . . .
N9 N 0.1699(3) 1.0344(2) 0.07690(14) 0.0144(4) Uani 1 1 d . . . . .
C1 C 0.4616(3) 0.5637(3) 0.41106(15) 0.0091(5) Uani 1 1 d . . . . .
C2 C 0.3326(3) 0.5639(3) 0.47978(15) 0.0096(5) Uani 1 1 d . . . . .
C3 C 0.3625(3) 0.5069(3) 0.56890(15) 0.0093(5) Uani 1 1 d . . . . .
C4 C 0.1146(3) 0.6165(3) 0.38755(18) 0.0189(6) Uani 1 1 d . . . . .
H4 H 0.177779 0.560852 0.343030 0.023 Uiso 1 1 calc R . . . .
C5 C -0.0780(3) 0.7553(3) 0.46472(19) 0.0215(6) Uani 1 1 d . . . . .
H5 H -0.182126 0.817482 0.484166 0.026 Uiso 1 1 calc R . . . .
C6 C 0.4747(3) 0.5167(3) 0.09157(16) 0.0125(5) Uani 1 1 d . . . . .
C7 C 0.3557(3) 0.4879(3) 0.05987(16) 0.0125(5) Uani 1 1 d . . . . .
C8 C 0.3696(3) 0.4762(3) -0.02926(16) 0.0134(5) Uani 1 1 d . . . . .
C9 C 0.0608(3) 0.5697(3) 0.11738(16) 0.0122(5) Uani 1 1 d . . . . .
H9 H 0.024551 0.654086 0.071410 0.015 Uiso 1 1 calc R . . . .
C10 C 0.0728(3) 0.3994(4) 0.23572(18) 0.0252(7) Uani 1 1 d . . . . .
H10 H 0.040929 0.342615 0.290323 0.030 Uiso 1 1 calc R . . . .
C11 C 0.4590(3) 0.9161(3) 0.08796(17) 0.0145(5) Uani 1 1 d . . . . .
C12 C 0.3337(3) 1.0142(3) 0.03900(16) 0.0138(5) Uani 1 1 d . . . . .
C13 C 0.3653(3) 1.1012(3) -0.04613(17) 0.0151(5) Uani 1 1 d . . . . .
C14 C 0.0543(3) 1.1664(3) 0.09429(17) 0.0204(6) Uani 1 1 d . . . . .
H14 H 0.069257 1.262310 0.084096 0.024 Uiso 1 1 calc R . . . .
C15 C -0.0451(3) 0.9868(3) 0.13065(19) 0.0228(6) Uani 1 1 d . . . . .
H15 H -0.119888 0.935043 0.152498 0.027 Uiso 1 1 calc R . . . .
O10 O 0.1946(3) 0.9664(3) 0.31403(19) 0.0509(7) Uani 1 1 d . . . A 1
H10A H 0.247541 0.908296 0.275916 0.076 Uiso 1 1 d G . . A 1
H10B H 0.266147 0.965541 0.342346 0.076 Uiso 1 1 d G . . A 1
O11 O 0.4543(5) 0.9604(5) 0.3755(3) 0.0253(9) Uiso 0.5 1 d . . P B 1
H11A H 0.458672 1.052316 0.362956 0.038 Uiso 0.5 1 d G . P B 1
H11B H 0.468567 0.928241 0.430389 0.038 Uiso 0.5 1 d G . P B 1
O12 O 0.3594(7) 0.9071(6) 0.4754(4) 0.0476(13) Uiso 0.5 1 d . . P C 2
H12A H 0.407574 0.867317 0.521787 0.071 Uiso 0.5 1 d G . P C 2
H12B H 0.314676 1.003553 0.477731 0.071 Uiso 0.5 1 d G . P C 2
O13 O 0.4081(7) 0.9173(6) 0.5601(4) 0.0468(13) Uiso 0.5 1 d . . P D 1
H13A H 0.469138 0.824154 0.556597 0.070 Uiso 0.5 1 d G . P D 1
H13B H 0.312387 0.914398 0.568346 0.070 Uiso 0.5 1 d G . P D 1
O14 O 0.5294(6) 1.1356(5) 0.2623(3) 0.0316(10) Uiso 0.5 1 d . . P E 2
H14A H 0.561757 1.096267 0.215199 0.047 Uiso 0.5 1 d G . P E 2
H14B H 0.459501 1.094741 0.292501 0.047 Uiso 0.5 1 d G . P E 2
O15 O 0.4443(5) 1.2607(5) 0.3309(3) 0.0241(9) Uiso 0.5 1 d . . P F 1
H15A H 0.394223 1.286154 0.285713 0.036 Uiso 0.5 1 d G . P F 1
H15B H 0.386718 1.326771 0.363955 0.036 Uiso 0.5 1 d G . P F 1


_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 2.3449(16) . ?
Dy1 O2 2.4253(16) 2_666 ?
Dy1 O3 2.4303(17) . ?
Dy1 O4 2.4511(17) 2_665 ?
Dy1 O5 2.4007(18) . ?
Dy1 O6 2.4516(17) 2_675 ?
Dy1 O7 2.3976(18) . ?
Dy1 O8 2.3924(19) . ?
Dy1 N4 2.491(2) 1_655 ?
O1 C1 1.256(3) . ?
O2 C3 1.253(3) . ?
O3 C6 1.240(3) . ?
O4 C8 1.259(3) . ?
O5 C11 1.257(3) . ?
O6 C13 1.249(3) . ?
O7 H7A 0.8762 . ?
O7 H7B 0.8752 . ?
O8 H8A 0.8717 . ?
O8 H8B 0.8719 . ?
O9 H9A 0.8496 . ?
O9 H9B 0.8501 . ?
N1 C4 1.322(3) . ?
N1 C5 1.346(4) . ?
N2 N3 1.366(3) . ?
N2 C5 1.316(4) . ?
N3 C2 1.431(3) . ?
N3 C4 1.336(3) . ?
N4 C9 1.329(3) . ?
N4 C10 1.353(3) . ?
N5 N6 1.374(3) . ?
N5 C10 1.310(4) . ?
N6 C7 1.427(3) . ?
N6 C9 1.328(3) . ?
N7 C14 1.315(4) . ?
N7 C15 1.362(4) . ?
N8 N9 1.367(3) . ?
N8 C15 1.321(4) . ?
N9 C12 1.419(3) . ?
N9 C14 1.332(3) . ?
C1 C2 1.394(3) . ?
C1 C3 1.534(3) 2_666 ?
C2 C3 1.397(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.403(3) . ?
C6 C8 1.531(3) 2_665 ?
C7 C8 1.391(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.390(3) . ?
C11 C13 1.533(4) 2_675 ?
C12 C13 1.400(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O10 H10A 0.8502 . ?
O10 H10B 0.8495 . ?
O11 H11A 0.8498 . ?
O11 H11B 0.8501 . ?
O12 H12A 0.8496 . ?
O12 H12B 0.8501 . ?
O13 H13A 0.8499 . ?
O13 H13B 0.8502 . ?
O14 H14A 0.8499 . ?
O14 H14B 0.8501 . ?
O15 H15A 0.8498 . ?
O15 H15B 0.8504 . ?

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 O2 65.77(6) . 2_666 ?
O1 Dy1 O3 70.20(6) . . ?
O1 Dy1 O4 135.01(6) . 2_665 ?
O1 Dy1 O5 73.27(6) . . ?
O1 Dy1 O6 134.38(6) . 2_675 ?
O1 Dy1 O7 87.99(6) . . ?
O1 Dy1 O8 84.32(6) . . ?
O1 Dy1 N4 141.57(6) . 1_655 ?
O2 Dy1 O3 118.56(6) 2_666 . ?
O2 Dy1 O4 137.86(6) 2_666 2_665 ?
O2 Dy1 O6 132.79(6) 2_666 2_675 ?
O2 Dy1 N4 75.82(6) 2_666 1_655 ?
O3 Dy1 O4 64.82(6) . 2_665 ?
O3 Dy1 O6 108.60(6) . 2_675 ?
O3 Dy1 N4 134.56(6) . 1_655 ?
O4 Dy1 O6 65.21(6) 2_665 2_675 ?
O4 Dy1 N4 76.46(6) 2_665 1_655 ?
O5 Dy1 O2 130.16(6) . 2_666 ?
O5 Dy1 O3 68.95(6) . . ?
O5 Dy1 O4 91.41(6) . 2_665 ?
O5 Dy1 O6 64.88(6) . 2_675 ?
O5 Dy1 N4 137.20(7) . 1_655 ?
O6 Dy1 N4 72.86(6) 2_675 1_655 ?
O7 Dy1 O2 67.97(6) . 2_666 ?
O7 Dy1 O3 69.86(6) . . ?
O7 Dy1 O4 75.94(6) . 2_665 ?
O7 Dy1 O5 138.45(6) . . ?
O7 Dy1 O6 135.93(6) . 2_675 ?
O7 Dy1 N4 78.72(6) . 1_655 ?
O8 Dy1 O2 68.92(6) . 2_666 ?
O8 Dy1 O3 144.32(6) . . ?
O8 Dy1 O4 135.53(6) . 2_665 ?
O8 Dy1 O5 80.24(6) . . ?
O8 Dy1 O6 71.83(6) . 2_675 ?
O8 Dy1 O7 135.48(6) . . ?
O8 Dy1 N4 80.64(7) . 1_655 ?
C1 O1 Dy1 123.64(15) . . ?
C3 O2 Dy1 120.74(15) . 2_666 ?
C6 O3 Dy1 122.02(15) . . ?
C8 O4 Dy1 120.52(16) . 2_665 ?
C11 O5 Dy1 119.23(17) . . ?
C13 O6 Dy1 118.06(16) . 2_675 ?
Dy1 O7 H7A 110.6 . . ?
Dy1 O7 H7B 110.8 . . ?
H7A O7 H7B 103.3 . . ?
Dy1 O8 H8A 110.8 . . ?
Dy1 O8 H8B 110.2 . . ?
H8A O8 H8B 103.4 . . ?
H9A O9 H9B 109.5 . . ?
C4 N1 C5 102.6(2) . . ?
C5 N2 N3 102.7(2) . . ?
N2 N3 C2 122.10(19) . . ?
C4 N3 N2 108.6(2) . . ?
C4 N3 C2 129.2(2) . . ?
C9 N4 Dy1 127.78(17) . 1_455 ?
C9 N4 C10 103.1(2) . . ?
C10 N4 Dy1 128.26(17) . 1_455 ?
C10 N5 N6 102.7(2) . . ?
N5 N6 C7 121.5(2) . . ?
C9 N6 N5 109.3(2) . . ?
C9 N6 C7 129.2(2) . . ?
C14 N7 C15 102.9(2) . . ?
C15 N8 N9 102.1(2) . . ?
N8 N9 C12 123.1(2) . . ?
C14 N9 N8 109.7(2) . . ?
C14 N9 C12 127.2(2) . . ?
O1 C1 C2 124.2(2) . . ?
O1 C1 C3 114.9(2) . 2_666 ?
C2 C1 C3 121.0(2) . 2_666 ?
C1 C2 N3 119.0(2) . . ?
C1 C2 C3 119.8(2) . . ?
C3 C2 N3 121.1(2) . . ?
O2 C3 C1 114.9(2) . 2_666 ?
O2 C3 C2 126.0(2) . . ?
C2 C3 C1 119.1(2) . 2_666 ?
N1 C4 N3 111.0(2) . . ?
N1 C4 H4 124.5 . . ?
N3 C4 H4 124.5 . . ?
N1 C5 H5 122.4 . . ?
N2 C5 N1 115.1(2) . . ?
N2 C5 H5 122.4 . . ?
O3 C6 C7 124.2(2) . . ?
O3 C6 C8 116.0(2) . 2_665 ?
C7 C6 C8 119.8(2) . 2_665 ?
C6 C7 N6 117.7(2) . . ?
C8 C7 N6 120.5(2) . . ?
C8 C7 C6 121.7(2) . . ?
O4 C8 C6 115.4(2) . 2_665 ?
O4 C8 C7 126.3(2) . . ?
C7 C8 C6 118.3(2) . 2_665 ?
N4 C9 H9 124.9 . . ?
N6 C9 N4 110.2(2) . . ?
N6 C9 H9 124.9 . . ?
N4 C10 H10 122.7 . . ?
N5 C10 N4 114.7(2) . . ?
N5 C10 H10 122.7 . . ?
O5 C11 C12 125.8(2) . . ?
O5 C11 C13 115.0(2) . 2_675 ?
C12 C11 C13 119.2(2) . 2_675 ?
C11 C12 N9 120.2(2) . . ?
C11 C12 C13 121.0(2) . . ?
C13 C12 N9 118.7(2) . . ?
O6 C13 C11 115.5(2) . 2_675 ?
O6 C13 C12 124.7(2) . . ?
C12 C13 C11 119.8(2) . 2_675 ?
N7 C14 N9 110.7(2) . . ?
N7 C14 H14 124.7 . . ?
N9 C14 H14 124.7 . . ?
N7 C15 H15 122.7 . . ?
N8 C15 N7 114.6(2) . . ?
N8 C15 H15 122.7 . . ?
H10A O10 H10B 104.5 . . ?
H11A O11 H11B 104.5 . . ?
H12A O12 H12B 104.5 . . ?
H13A O13 H13B 104.5 . . ?
H14A O14 H14B 104.5 . . ?
H15A O15 H15B 104.5 . . ?

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

data_nm274a
_database_code_depnum_ccdc_archive 'CCDC 2320544'
loop_
_audit_author_name
_audit_author_address
'Miguel Clemente-Leon'
;Universidad de Valencia
Spain
;
_audit_update_record             
;
2023-12-19 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_audit_creation_date             2020-07-22
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H10 N9 O8 Tb, 4.5(H2 O)'
_chemical_formula_sum            'C15 H19 N9 O12.50 Tb'
_chemical_formula_weight         684.31
_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'
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                   8.9903(4)
_cell_length_b                   9.4164(4)
_cell_length_c                   15.5861(6)
_cell_angle_alpha                75.214(3)
_cell_angle_beta                 77.435(4)
_cell_angle_gamma                68.017(4)
_cell_volume                     1172.01(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7932
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.2170
_cell_measurement_theta_min      3.9090
_shelx_estimated_absorpt_T_max   0.727
_shelx_estimated_absorpt_T_min   0.621
_exptl_absorpt_coefficient_mu    3.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15479
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.934
_diffrn_reflns_theta_min         3.257
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00   0.00   1.00    2.00    --  -14.89 -63.00-179.02   74
  2  ω    -67.00   2.00   1.00    2.00    --  -14.89 -65.00  83.59   69
  3  ω    -53.00  37.00   1.00    2.00    --   15.83 -57.00-120.00   90
  4  ω      3.00  84.00   1.00    2.00    --   15.83  57.00 -60.00   81
  5  ω     11.00  37.00   1.00    2.00    --   15.83 -57.00  90.00   26
  6  ω    -35.00  39.00   1.00    2.00    --   15.83 -65.00  48.00   74
  7  ω     -6.00  62.00   1.00    2.00    --   15.83  57.00  60.00   68
  8  ω    -50.00  37.00   1.00    2.00    --   15.83 -57.00 -30.00   87
  9  ω    -51.00  37.00   1.00    2.00    --   15.83 -58.00 147.19   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0218406000
_diffrn_orient_matrix_UB_12      0.0450124000
_diffrn_orient_matrix_UB_13      -0.0414619000
_diffrn_orient_matrix_UB_21      0.0520593000
_diffrn_orient_matrix_UB_22      0.0182924000
_diffrn_orient_matrix_UB_23      0.0204162000
_diffrn_orient_matrix_UB_31      0.0647182000
_diffrn_orient_matrix_UB_32      -0.0670119000
_diffrn_orient_matrix_UB_33      -0.0110098000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4392
_reflns_number_total             4908
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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         1.006
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         4908
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0199P)²+0.7534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0602
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5) O13(0.5) H13A(0.5) H13B(0.5) O12(0.5)
 H12A(0.5) H12B(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.5) H15A(0.5) H15B(0.5)
3.a Free rotating group:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O13(H13A,H13B), O12(H12A,H12B),
 O14(H14A,H14B), O15(H15A,H15B)
3.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C14(H14), C15(H15)
;
_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
C1 C 0.4593(4) 0.9165(4) 0.0878(2) 0.0143(8) Uani 1 1 d . . . . .
C2 C 0.3339(4) 1.0143(4) 0.0385(2) 0.0137(8) Uani 1 1 d . . . . .
C3 C 0.3652(4) 1.1007(4) -0.0462(2) 0.0159(8) Uani 1 1 d . . . . .
C4 C 0.0556(5) 1.1667(4) 0.0938(2) 0.0204(9) Uani 1 1 d . . . . .
H4 H 0.070847 1.262382 0.083317 0.024 Uiso 1 1 calc R . . . .
C5 C -0.0434(5) 0.9875(5) 0.1299(3) 0.0238(9) Uani 1 1 d . . . . .
H5 H -0.118337 0.936059 0.151536 0.029 Uiso 1 1 calc R . . . .
C6 C 0.4750(4) 0.5169(4) 0.0914(2) 0.0135(8) Uani 1 1 d . . . . .
C7 C 0.3563(4) 0.4884(4) 0.0595(2) 0.0135(8) Uani 1 1 d . . . . .
C8 C 0.3697(4) 0.4761(4) -0.0288(2) 0.0134(8) Uani 1 1 d . . . . .
C9 C 0.0616(4) 0.5697(4) 0.1175(2) 0.0132(7) Uani 1 1 d . . . . .
H9 H 0.025275 0.654116 0.071733 0.016 Uiso 1 1 calc R . . . .
C10 C 0.0740(4) 0.3992(5) 0.2351(3) 0.0270(10) Uani 1 1 d . . . . .
H10 H 0.042281 0.341862 0.289365 0.032 Uiso 1 1 calc R . . . .
C11 C 0.4613(4) 0.5634(4) 0.4110(2) 0.0096(7) Uani 1 1 d . . . . .
C12 C 0.3332(4) 0.5634(4) 0.4799(2) 0.0094(7) Uani 1 1 d . . . . .
C13 C 0.3620(4) 0.5072(4) 0.5686(2) 0.0107(7) Uani 1 1 d . . . . .
C14 C 0.1152(4) 0.6157(5) 0.3885(3) 0.0201(9) Uani 1 1 d . . . . .
H14 H 0.178323 0.559669 0.344331 0.024 Uiso 1 1 calc R . . . .
C15 C -0.0773(4) 0.7552(5) 0.4649(3) 0.0217(9) Uani 1 1 d . . . . .
H15 H -0.181360 0.816917 0.484457 0.026 Uiso 1 1 calc R . . . .
N1 N -0.0826(4) 1.1427(4) 0.1276(2) 0.0227(7) Uani 1 1 d . . . . .
N2 N 0.1700(3) 1.0349(3) 0.07680(19) 0.0145(7) Uani 1 1 d . . . . .
N3 N 0.1076(4) 0.9158(4) 0.0993(2) 0.0221(7) Uani 1 1 d . . . . .
N4 N -0.0324(3) 0.5227(4) 0.18842(19) 0.0152(7) Uani 1 1 d . . . . .
N5 N 0.2153(3) 0.4787(3) 0.12117(18) 0.0137(6) Uani 1 1 d . . . . .
N6 N 0.2250(4) 0.3670(4) 0.1976(2) 0.0295(9) Uani 1 1 d . . . . .
N7 N -0.0422(3) 0.6946(4) 0.3902(2) 0.0195(7) Uani 1 1 d . . . . .
N8 N 0.1712(3) 0.6272(3) 0.45780(18) 0.0098(6) Uani 1 1 d . . . . .
N9 N 0.0459(3) 0.7208(4) 0.5080(2) 0.0206(7) Uani 1 1 d . . . . .
O1 O 0.4426(3) 0.8386(3) 0.16535(16) 0.0191(6) Uani 1 1 d . . . . .
O2 O 0.2599(3) 1.1944(3) -0.09303(17) 0.0213(6) Uani 1 1 d . . . . .
O3 O 0.4635(3) 0.5387(3) 0.16830(16) 0.0167(6) Uani 1 1 d . . . . .
O4 O 0.2656(3) 0.4594(3) -0.06462(16) 0.0182(6) Uani 1 1 d . . . . .
O5 O 0.4459(3) 0.6177(3) 0.32993(15) 0.0140(5) Uani 1 1 d . . . . .
O6 O 0.2574(3) 0.5084(3) 0.63632(15) 0.0148(5) Uani 1 1 d . . . . .
O7 O 0.7356(3) 0.3291(3) 0.24496(16) 0.0178(6) Uani 1 1 d . . . . .
H7A H 0.784792 0.292388 0.196637 0.027 Uiso 1 1 d GR . . . .
H7B H 0.648879 0.303157 0.257972 0.027 Uiso 1 1 d GR . . . .
O8 O 0.7058(3) 0.7929(3) 0.28153(17) 0.0210(6) Uani 1 1 d . . . . .
H8A H 0.632921 0.812919 0.328579 0.032 Uiso 1 1 d GR . . . .
H8B H 0.687357 0.884635 0.245677 0.032 Uiso 1 1 d GR . . . .
O9 O 0.8878(3) 0.1290(3) 0.37870(19) 0.0236(6) Uani 1 1 d . . . . .
H9A H 0.911783 0.176973 0.410168 0.035 Uiso 1 1 d G . . . .
H9B H 0.973541 0.062318 0.358368 0.035 Uiso 1 1 d G . . . .
Tb1 Tb 0.66472(2) 0.60937(2) 0.21435(2) 0.01250(6) Uani 1 1 d . . . . .
O10 O 0.1949(4) 0.9669(4) 0.3139(3) 0.0519(10) Uani 1 1 d . . . . .
H10A H 0.266230 0.957819 0.344718 0.078 Uiso 1 1 d G . . . .
H10B H 0.242878 0.900514 0.280023 0.078 Uiso 1 1 d G . . . .
O11 O 0.5307(7) 1.1333(7) 0.2620(5) 0.0334(15) Uani 0.5 1 d . . P A 1
H11A H 0.439054 1.153666 0.246201 0.050 Uiso 0.5 1 d G . P A 1
H11B H 0.542692 1.221638 0.252544 0.050 Uiso 0.5 1 d G . P A 1
O13 O 0.4433(6) 1.2637(6) 0.3304(4) 0.0229(12) Uani 0.5 1 d . . P B 2
H13A H 0.381515 1.287486 0.290917 0.034 Uiso 0.5 1 d G . P B 2
H13B H 0.469635 1.165157 0.346308 0.034 Uiso 0.5 1 d G . P B 2
O12 O 0.3605(9) 0.9077(9) 0.4755(5) 0.0478(18) Uani 0.5 1 d . . P C 2
H12A H 0.309638 0.880253 0.525958 0.072 Uiso 0.5 1 d G . P C 2
H12B H 0.393201 0.980015 0.478389 0.072 Uiso 0.5 1 d G . P C 2
O14 O 0.4536(7) 0.9602(6) 0.3746(4) 0.0255(13) Uani 0.5 1 d . . P D 1
H14A H 0.460455 0.931678 0.430345 0.038 Uiso 0.5 1 d G . P D 1
H14B H 0.471138 1.046471 0.360006 0.038 Uiso 0.5 1 d G . P D 1
O15 O 0.4079(8) 0.9180(9) 0.5596(5) 0.0477(19) Uani 0.5 1 d . . P E 1
H15A H 0.316305 0.916594 0.588197 0.072 Uiso 0.5 1 d G . P E 1
H15B H 0.452584 0.838950 0.534690 0.072 Uiso 0.5 1 d G . P E 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.395(5) . ?
C1 C3 1.534(5) 2_675 ?
C1 O1 1.254(4) . ?
C2 C3 1.394(5) . ?
C2 N2 1.424(4) . ?
C3 O2 1.247(4) . ?
C4 H4 0.9300 . ?
C4 N1 1.318(5) . ?
C4 N2 1.327(4) . ?
C5 H5 0.9300 . ?
C5 N1 1.362(5) . ?
C5 N3 1.312(5) . ?
C6 C7 1.404(5) . ?
C6 C8 1.533(5) 2_665 ?
C6 O3 1.242(4) . ?
C7 C8 1.387(5) . ?
C7 N5 1.432(4) . ?
C8 O4 1.262(4) . ?
C9 H9 0.9300 . ?
C9 N4 1.325(4) . ?
C9 N5 1.330(4) . ?
C10 H10 0.9300 . ?
C10 N4 1.355(5) . ?
C10 N6 1.309(5) . ?
C11 C12 1.393(4) . ?
C11 C13 1.545(4) 2_666 ?
C11 O5 1.253(4) . ?
C12 C13 1.392(5) . ?
C12 N8 1.434(4) . ?
C13 O6 1.251(4) . ?
C14 H14 0.9300 . ?
C14 N7 1.327(4) . ?
C14 N8 1.330(4) . ?
C15 H15 0.9300 . ?
C15 N7 1.351(5) . ?
C15 N9 1.315(5) . ?
N2 N3 1.371(4) . ?
N4 Tb1 2.504(3) 1_455 ?
N5 N6 1.368(4) . ?
N8 N9 1.373(4) . ?
O1 Tb1 2.413(2) . ?
O2 Tb1 2.459(2) 2_675 ?
O3 Tb1 2.438(2) . ?
O4 Tb1 2.468(2) 2_665 ?
O5 Tb1 2.353(2) . ?
O6 Tb1 2.439(2) 2_666 ?
O7 H7A 0.8693 . ?
O7 H7B 0.8699 . ?
O7 Tb1 2.415(2) . ?
O8 H8A 0.8785 . ?
O8 H8B 0.8790 . ?
O8 Tb1 2.406(3) . ?
O9 H9A 0.8501 . ?
O9 H9B 0.8498 . ?
O10 H10A 0.8498 . ?
O10 H10B 0.8502 . ?
O11 H11A 0.8501 . ?
O11 H11B 0.8500 . ?
O13 H13A 0.8498 . ?
O13 H13B 0.8497 . ?
O12 H12A 0.8499 . ?
O12 H12B 0.8500 . ?
O14 H14A 0.8500 . ?
O14 H14B 0.8499 . ?
O15 H15A 0.8501 . ?
O15 H15B 0.8497 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C3 119.1(3) . 2_675 ?
O1 C1 C2 125.7(3) . . ?
O1 C1 C3 115.1(3) . 2_675 ?
C1 C2 N2 120.0(3) . . ?
C3 C2 C1 121.2(3) . . ?
C3 C2 N2 118.8(3) . . ?
C2 C3 C1 119.7(3) . 2_675 ?
O2 C3 C1 115.3(3) . 2_675 ?
O2 C3 C2 125.0(3) . . ?
N1 C4 H4 124.8 . . ?
N1 C4 N2 110.4(3) . . ?
N2 C4 H4 124.8 . . ?
N1 C5 H5 122.4 . . ?
N3 C5 H5 122.4 . . ?
N3 C5 N1 115.3(3) . . ?
C7 C6 C8 119.3(3) . 2_665 ?
O3 C6 C7 124.5(3) . . ?
O3 C6 C8 116.2(3) . 2_665 ?
C6 C7 N5 117.4(3) . . ?
C8 C7 C6 122.2(3) . . ?
C8 C7 N5 120.4(3) . . ?
C7 C8 C6 118.3(3) . 2_665 ?
O4 C8 C6 115.0(3) . 2_665 ?
O4 C8 C7 126.7(3) . . ?
N4 C9 H9 124.9 . . ?
N4 C9 N5 110.2(3) . . ?
N5 C9 H9 124.9 . . ?
N4 C10 H10 122.7 . . ?
N6 C10 H10 122.7 . . ?
N6 C10 N4 114.5(3) . . ?
C12 C11 C13 120.5(3) . 2_666 ?
O5 C11 C12 124.7(3) . . ?
O5 C11 C13 114.9(3) . 2_666 ?
C11 C12 N8 118.7(3) . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 N8 120.8(3) . . ?
C12 C13 C11 119.0(3) . 2_666 ?
O6 C13 C11 114.6(3) . 2_666 ?
O6 C13 C12 126.4(3) . . ?
N7 C14 H14 124.3 . . ?
N7 C14 N8 111.4(3) . . ?
N8 C14 H14 124.3 . . ?
N7 C15 H15 122.3 . . ?
N9 C15 H15 122.3 . . ?
N9 C15 N7 115.3(3) . . ?
C4 N1 C5 102.6(3) . . ?
C4 N2 C2 127.0(3) . . ?
C4 N2 N3 110.1(3) . . ?
N3 N2 C2 122.8(3) . . ?
C5 N3 N2 101.6(3) . . ?
C9 N4 C10 103.1(3) . . ?
C9 N4 Tb1 127.8(2) . 1_455 ?
C10 N4 Tb1 128.2(2) . 1_455 ?
C9 N5 C7 129.0(3) . . ?
C9 N5 N6 109.3(3) . . ?
N6 N5 C7 121.7(3) . . ?
C10 N6 N5 102.8(3) . . ?
C14 N7 C15 102.1(3) . . ?
C14 N8 C12 129.3(3) . . ?
C14 N8 N9 108.5(3) . . ?
N9 N8 C12 122.1(3) . . ?
C15 N9 N8 102.6(3) . . ?
C1 O1 Tb1 119.1(2) . . ?
C3 O2 Tb1 118.2(2) . 2_675 ?
C6 O3 Tb1 122.3(2) . . ?
C8 O4 Tb1 120.7(2) . 2_665 ?
C11 O5 Tb1 124.0(2) . . ?
C13 O6 Tb1 121.0(2) . 2_666 ?
H7A O7 H7B 103.5 . . ?
Tb1 O7 H7A 110.1 . . ?
Tb1 O7 H7B 110.5 . . ?
H8A O8 H8B 103.0 . . ?
Tb1 O8 H8A 110.4 . . ?
Tb1 O8 H8B 111.1 . . ?
H9A O9 H9B 109.5 . . ?
O1 Tb1 N4 137.00(9) . 1_655 ?
O1 Tb1 O2 64.53(8) . 2_675 ?
O1 Tb1 O3 69.02(8) . . ?
O1 Tb1 O4 91.21(8) . 2_665 ?
O1 Tb1 O6 130.27(8) . 2_666 ?
O1 Tb1 O7 138.75(8) . . ?
O2 Tb1 N4 72.97(9) 2_675 1_655 ?
O2 Tb1 O4 65.47(9) 2_675 2_665 ?
O3 Tb1 N4 134.35(9) . 1_655 ?
O3 Tb1 O2 108.47(8) . 2_675 ?
O3 Tb1 O4 64.48(8) . 2_665 ?
O3 Tb1 O6 118.54(8) . 2_666 ?
O4 Tb1 N4 76.51(8) 2_665 1_655 ?
O5 Tb1 N4 141.50(8) . 1_655 ?
O5 Tb1 O1 73.69(8) . . ?
O5 Tb1 O2 134.42(8) . 2_675 ?
O5 Tb1 O3 70.36(8) . . ?
O5 Tb1 O4 134.82(8) . 2_665 ?
O5 Tb1 O6 65.49(7) . 2_666 ?
O5 Tb1 O7 87.96(8) . . ?
O5 Tb1 O8 84.47(9) . . ?
O6 Tb1 N4 76.03(8) 2_666 1_655 ?
O6 Tb1 O2 132.93(8) 2_666 2_675 ?
O6 Tb1 O4 137.91(8) 2_666 2_665 ?
O7 Tb1 N4 78.46(9) . 1_655 ?
O7 Tb1 O2 135.98(8) . 2_675 ?
O7 Tb1 O3 70.07(8) . . ?
O7 Tb1 O4 75.85(8) . 2_665 ?
O7 Tb1 O6 67.85(8) . 2_666 ?
O8 Tb1 N4 80.31(9) . 1_655 ?
O8 Tb1 O1 80.86(8) . . ?
O8 Tb1 O2 72.08(9) . 2_675 ?
O8 Tb1 O3 144.88(8) . . ?
O8 Tb1 O4 135.89(8) . 2_665 ?
O8 Tb1 O6 68.45(8) . 2_666 ?
O8 Tb1 O7 134.76(8) . . ?
H10A O10 H10B 104.5 . . ?
H11A O11 H11B 104.5 . . ?
H13A O13 H13B 104.5 . . ?
H12A O12 H12B 109.5 . . ?
H14A O14 H14B 104.5 . . ?
H15A O15 H15B 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 1.433
_oxdiff_exptl_absorpt_empirical_full_min 0.816
####################################################################### 
# 
# 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_nm240prisma
_database_code_depnum_ccdc_archive 'CCDC 2320543'
loop_
_audit_author_name
_audit_author_address
'Miguel Clemente-Leon'
;Universidad de Valencia
Spain
;
_audit_update_record             
;
2023-12-19 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_audit_creation_date             2021-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H10 Dy N9 O8, 2(H2 O)'
_chemical_formula_sum            'C15 H14 Dy N9 O10'
_chemical_formula_weight         642.85
_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                   8.6480(4)
_cell_length_b                   10.4211(5)
_cell_length_c                   12.0603(6)
_cell_angle_alpha                80.197(4)
_cell_angle_beta                 79.454(4)
_cell_angle_gamma                82.476(4)
_cell_volume                     1047.33(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7656
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.4640
_cell_measurement_theta_min      3.6620
_shelx_estimated_absorpt_T_max   0.759
_shelx_estimated_absorpt_T_min   0.629
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.038
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17270
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.441
_diffrn_reflns_theta_min         3.282
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00   2.00   1.00    5.00    --  -19.95 -69.00 -64.12   88
  2  ω    -85.00   1.00   1.00    5.00    --  -19.95 -57.00  90.00   86
  3  ω    -88.00  -5.00   1.00    5.00    --  -19.95 -69.00-151.38   83
  4  ω    -79.00  -1.00   1.00    5.00    --  -19.95 -57.00   0.00   78
  5  ω    -46.00  42.00   1.00    5.00    --   20.73 -68.00  -0.60   88
  6  ω    -45.00  42.00   1.00    5.00    --   20.73 -65.00 163.93   87
  7  ω    -41.00  45.00   1.00    5.00    --   20.73 -67.00  78.83   86
  8  ω    -38.00  47.00   1.00    5.00    --   22.00 -69.00-117.78   85
  9  ω     -8.00  45.00   1.00    5.00    --   22.00 -66.00 -73.27   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0131820000
_diffrn_orient_matrix_UB_12      -0.0479856000
_diffrn_orient_matrix_UB_13      -0.0315215000
_diffrn_orient_matrix_UB_21      0.0156735000
_diffrn_orient_matrix_UB_22      0.0442575000
_diffrn_orient_matrix_UB_23      -0.0513588000
_diffrn_orient_matrix_UB_31      0.0813357000
_diffrn_orient_matrix_UB_32      -0.0236809000
_diffrn_orient_matrix_UB_33      -0.0054775000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4953
_reflns_number_total             5565
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.904
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0094P)²+0.7704P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0583
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O00(H00E,H00F), O1(H1A,H1B)
2.b Rotating group:
 O004(H00A,H00B), O009(H00C,H00D)
2.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00S(H00S), C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy01 Dy 0.78043(2) 0.25811(2) 0.25018(2) 0.00714(5) Uani 1 1 d . . . . .
O002 O 1.2514(3) -0.0717(2) -0.15288(19) 0.0102(5) Uani 1 1 d . . . . .
O003 O 0.7095(3) 0.2996(2) 0.44302(19) 0.0115(5) Uani 1 1 d . . . . .
O004 O 0.7011(3) 0.3379(2) 0.07201(19) 0.0142(5) Uani 1 1 d . . . . .
H00A H 0.674831 0.420719 0.066341 0.021 Uiso 1 1 d GR . . . .
H00B H 0.615445 0.306247 0.069078 0.021 Uiso 1 1 d GR . . . .
O005 O 0.2158(3) -0.0520(2) 0.62259(19) 0.0098(5) Uani 1 1 d . . . . .
O006 O 0.4156(3) 0.5453(2) 0.71801(19) 0.0120(5) Uani 1 1 d . . . . .
O007 O 1.0091(3) 0.1841(2) 0.1292(2) 0.0109(5) Uani 1 1 d . . . . .
O008 O 0.5237(3) 0.1894(2) 0.31683(19) 0.0104(5) Uani 1 1 d . . . . .
O009 O 0.9121(3) 0.4491(2) 0.1852(2) 0.0143(5) Uani 1 1 d . . . . .
H00C H 1.014897 0.429910 0.176710 0.021 Uiso 1 1 d GR . . . .
H00D H 0.893371 0.500629 0.237485 0.021 Uiso 1 1 d GR . . . .
N00A N 0.0178(3) 0.2331(3) 0.3531(2) 0.0103(6) Uani 1 1 d . . . . .
O00 O 0.2433(3) 0.4624(3) 0.1261(2) 0.0232(6) Uani 1 1 d . . . . .
H00E H 0.302818 0.391347 0.137256 0.035 Uiso 1 1 d G . . . .
H00F H 0.252792 0.504130 0.178743 0.035 Uiso 1 1 d G . . . .
N00C N 1.2771(3) 0.1341(3) -0.0281(2) 0.0082(6) Uani 1 1 d . . . . .
N00D N 0.2208(3) 0.1544(3) 0.4369(2) 0.0081(6) Uani 1 1 d . . . . .
N00E N 1.4596(3) 0.2357(3) 0.0122(3) 0.0152(7) Uani 1 1 d . . . . .
O1 O 0.8329(4) 0.6469(3) 0.3084(3) 0.0381(8) Uani 1 1 d . . . . .
H1A H 0.828002 0.676326 0.370643 0.057 Uiso 1 1 d G . . . .
H1B H 0.793364 0.705900 0.260633 0.057 Uiso 1 1 d G . . . .
C00G C 1.1395(4) -0.0332(3) -0.0812(3) 0.0091(7) Uani 1 1 d . . . . .
N00H N 0.6389(3) 0.3203(3) 0.6714(2) 0.0101(6) Uani 1 1 d . . . . .
N00I N 1.2967(3) 0.2382(3) -0.1132(2) 0.0150(6) Uani 1 1 d . . . . .
C00J C 1.0124(4) 0.0996(3) 0.0661(3) 0.0075(6) Uani 1 1 d . . . . .
C00K C 1.1422(4) 0.0633(3) -0.0132(3) 0.0092(7) Uani 1 1 d . . . . .
N00L N 0.1686(4) 0.2714(3) 0.4751(3) 0.0190(7) Uani 1 1 d . . . . .
C00M C 0.4603(4) 0.5174(3) 0.6198(3) 0.0103(7) Uani 1 1 d . . . . .
C00N C 0.5051(4) 0.1032(3) 0.4032(3) 0.0090(7) Uani 1 1 d . . . . .
C00O C 0.1303(4) 0.1359(3) 0.3641(3) 0.0110(7) Uani 1 1 d . . . . .
H00O H 0.144556 0.063759 0.325930 0.013 Uiso 1 1 calc R . . . .
C00P C 0.3584(4) 0.0772(3) 0.4684(3) 0.0093(7) Uani 1 1 d . . . . .
C00Q C 0.6116(4) 0.3917(3) 0.4754(3) 0.0102(7) Uani 1 1 d . . . . .
C00R C 0.3435(4) -0.0228(3) 0.5629(3) 0.0082(7) Uani 1 1 d . . . . .
C00S C 1.3745(4) 0.1350(3) 0.0458(3) 0.0128(7) Uani 1 1 d . . . . .
H00S H 1.381479 0.074005 0.111092 0.015 Uiso 1 1 calc R . . . .
C00T C 0.5691(4) 0.4123(3) 0.5882(3) 0.0105(7) Uani 1 1 d . . . . .
N00U N 0.7471(3) 0.3505(3) 0.7303(3) 0.0164(7) Uani 1 1 d . . . . .
C00V C 0.0481(4) 0.3134(4) 0.4223(3) 0.0187(8) Uani 1 1 d . . . . .
H00V H -0.012396 0.392635 0.431448 0.022 Uiso 1 1 calc R . . . .
C00W C 1.4066(4) 0.2953(3) -0.0847(3) 0.0137(7) Uani 1 1 d . . . . .
H00W H 1.445284 0.370755 -0.127603 0.016 Uiso 1 1 calc R . . . .
N00X N 0.7256(4) 0.1327(3) 0.7645(3) 0.0214(7) Uani 1 1 d . . . . .
C00Y C 0.6304(4) 0.1912(3) 0.6930(3) 0.0167(8) Uani 1 1 d . . . . .
H00Y H 0.565548 0.147825 0.661545 0.020 Uiso 1 1 calc R . . . .
C00Z C 0.7924(4) 0.2351(4) 0.7837(3) 0.0206(9) Uani 1 1 d . . . . .
H00Z H 0.866550 0.224350 0.832380 0.025 Uiso 1 1 calc R . . . .


_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
Dy01 O002 2.502(2) 2_755 ?
Dy01 O003 2.392(2) . ?
Dy01 O004 2.358(2) . ?
Dy01 O005 2.418(2) 2_656 ?
Dy01 O006 2.518(2) 2_666 ?
Dy01 O007 2.358(2) . ?
Dy01 O008 2.378(2) . ?
Dy01 O009 2.368(2) . ?
Dy01 N00A 2.550(3) 1_655 ?
O002 C00G 1.247(4) . ?
O003 C00Q 1.258(4) . ?
O004 H00A 0.8580 . ?
O004 H00B 0.8576 . ?
O005 C00R 1.246(4) . ?
O006 C00M 1.248(4) . ?
O007 C00J 1.252(4) . ?
O008 C00N 1.255(4) . ?
O009 H00C 0.8764 . ?
O009 H00D 0.8756 . ?
N00A C00O 1.316(4) . ?
N00A C00V 1.356(4) . ?
O00 H00E 0.8501 . ?
O00 H00F 0.8498 . ?
N00C N00I 1.366(4) . ?
N00C C00K 1.429(4) . ?
N00C C00S 1.334(4) . ?
N00D N00L 1.369(4) . ?
N00D C00O 1.330(4) . ?
N00D C00P 1.421(4) . ?
N00E C00S 1.326(4) . ?
N00E C00W 1.355(4) . ?
O1 H1A 0.8502 . ?
O1 H1B 0.8501 . ?
C00G C00J 1.531(4) 2_755 ?
C00G C00K 1.408(4) . ?
N00H C00T 1.426(4) . ?
N00H N00U 1.369(4) . ?
N00H C00Y 1.336(4) . ?
N00I C00W 1.309(4) . ?
C00J C00K 1.391(4) . ?
N00L C00V 1.309(4) . ?
C00M C00Q 1.530(5) 2_666 ?
C00M C00T 1.404(4) . ?
C00N C00P 1.398(5) . ?
C00N C00R 1.541(4) 2_656 ?
C00O H00O 0.9300 . ?
C00P C00R 1.407(4) . ?
C00Q C00T 1.388(4) . ?
C00S H00S 0.9300 . ?
N00U C00Z 1.312(4) . ?
C00V H00V 0.9300 . ?
C00W H00W 0.9300 . ?
N00X C00Y 1.320(4) . ?
N00X C00Z 1.349(5) . ?
C00Y H00Y 0.9300 . ?
C00Z H00Z 0.9300 . ?

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
O002 Dy01 O006 127.07(7) 2_755 2_666 ?
O002 Dy01 N00A 116.93(8) 2_755 1_655 ?
O003 Dy01 O002 133.25(8) . 2_755 ?
O003 Dy01 O005 70.85(8) . 2_656 ?
O003 Dy01 O006 64.08(7) . 2_666 ?
O003 Dy01 N00A 67.10(8) . 1_655 ?
O004 Dy01 O002 69.76(8) . 2_755 ?
O004 Dy01 O003 138.15(8) . . ?
O004 Dy01 O005 136.13(8) . 2_656 ?
O004 Dy01 O006 74.40(8) . 2_666 ?
O004 Dy01 O007 80.66(8) . . ?
O004 Dy01 O008 88.24(8) . . ?
O004 Dy01 O009 76.41(8) . . ?
O004 Dy01 N00A 141.97(9) . 1_655 ?
O005 Dy01 O002 67.98(7) 2_656 2_755 ?
O005 Dy01 O006 124.64(7) 2_656 2_666 ?
O005 Dy01 N00A 70.93(8) 2_656 1_655 ?
O006 Dy01 N00A 115.40(8) 2_666 1_655 ?
O007 Dy01 O002 65.18(7) . 2_755 ?
O007 Dy01 O003 137.71(8) . . ?
O007 Dy01 O005 91.99(8) . 2_656 ?
O007 Dy01 O006 143.27(8) . 2_666 ?
O007 Dy01 O008 135.72(8) . . ?
O007 Dy01 O009 76.75(8) . . ?
O007 Dy01 N00A 70.80(8) . 1_655 ?
O008 Dy01 O002 70.73(7) . 2_755 ?
O008 Dy01 O003 73.74(8) . . ?
O008 Dy01 O005 67.29(7) . 2_656 ?
O008 Dy01 O006 70.52(8) . 2_666 ?
O008 Dy01 N00A 129.77(8) . 1_655 ?
O009 Dy01 O002 132.01(8) . 2_755 ?
O009 Dy01 O003 94.56(8) . . ?
O009 Dy01 O005 143.95(8) . 2_656 ?
O009 Dy01 O006 71.51(8) . 2_666 ?
O009 Dy01 O008 141.62(8) . . ?
O009 Dy01 N00A 73.03(8) . 1_655 ?
C00G O002 Dy01 118.7(2) . 2_755 ?
C00Q O003 Dy01 124.9(2) . . ?
Dy01 O004 H00A 109.9 . . ?
Dy01 O004 H00B 109.4 . . ?
H00A O004 H00B 104.0 . . ?
C00R O005 Dy01 117.3(2) . 2_656 ?
C00M O006 Dy01 120.1(2) . 2_666 ?
C00J O007 Dy01 124.0(2) . . ?
C00N O008 Dy01 118.3(2) . . ?
Dy01 O009 H00C 110.9 . . ?
Dy01 O009 H00D 110.5 . . ?
H00C O009 H00D 103.2 . . ?
C00O N00A Dy01 130.3(2) . 1_455 ?
C00O N00A C00V 102.3(3) . . ?
C00V N00A Dy01 127.0(2) . 1_455 ?
H00E O00 H00F 104.5 . . ?
N00I N00C C00K 120.0(3) . . ?
C00S N00C N00I 109.6(3) . . ?
C00S N00C C00K 128.5(3) . . ?
N00L N00D C00P 121.6(3) . . ?
C00O N00D N00L 109.0(3) . . ?
C00O N00D C00P 129.3(3) . . ?
C00S N00E C00W 103.2(3) . . ?
H1A O1 H1B 109.5 . . ?
O002 C00G C00J 116.1(3) . 2_755 ?
O002 C00G C00K 125.8(3) . . ?
C00K C00G C00J 118.1(3) . 2_755 ?
N00U N00H C00T 123.3(3) . . ?
C00Y N00H C00T 127.2(3) . . ?
C00Y N00H N00U 108.8(3) . . ?
C00W N00I N00C 102.7(3) . . ?
O007 C00J C00G 115.6(3) . 2_755 ?
O007 C00J C00K 124.7(3) . . ?
C00K C00J C00G 119.7(3) . 2_755 ?
C00G C00K N00C 120.6(3) . . ?
C00J C00K N00C 117.1(3) . . ?
C00J C00K C00G 122.2(3) . . ?
C00V N00L N00D 102.3(3) . . ?
O006 C00M C00Q 115.9(3) . 2_666 ?
O006 C00M C00T 126.9(3) . . ?
C00T C00M C00Q 117.1(3) . 2_666 ?
O008 C00N C00P 124.3(3) . . ?
O008 C00N C00R 116.3(3) . 2_656 ?
C00P C00N C00R 119.4(3) . 2_656 ?
N00A C00O N00D 111.1(3) . . ?
N00A C00O H00O 124.4 . . ?
N00D C00O H00O 124.4 . . ?
C00N C00P N00D 118.4(3) . . ?
C00N C00P C00R 122.1(3) . . ?
C00R C00P N00D 119.5(3) . . ?
O003 C00Q C00M 115.0(3) . 2_666 ?
O003 C00Q C00T 124.1(3) . . ?
C00T C00Q C00M 121.0(3) . 2_666 ?
O005 C00R C00N 116.6(3) . 2_656 ?
O005 C00R C00P 124.9(3) . . ?
C00P C00R C00N 118.5(3) . 2_656 ?
N00C C00S H00S 125.1 . . ?
N00E C00S N00C 109.9(3) . . ?
N00E C00S H00S 125.1 . . ?
C00M C00T N00H 121.1(3) . . ?
C00Q C00T N00H 117.0(3) . . ?
C00Q C00T C00M 121.9(3) . . ?
C00Z N00U N00H 101.7(3) . . ?
N00A C00V H00V 122.4 . . ?
N00L C00V N00A 115.2(3) . . ?
N00L C00V H00V 122.4 . . ?
N00E C00W H00W 122.7 . . ?
N00I C00W N00E 114.7(3) . . ?
N00I C00W H00W 122.7 . . ?
C00Y N00X C00Z 101.5(3) . . ?
N00H C00Y H00Y 124.2 . . ?
N00X C00Y N00H 111.5(3) . . ?
N00X C00Y H00Y 124.2 . . ?
N00U C00Z N00X 116.5(3) . . ?
N00U C00Z H00Z 121.7 . . ?
N00X C00Z H00Z 121.7 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.182
_oxdiff_exptl_absorpt_empirical_full_min 0.834
####################################################################### 
# 
# 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_nm274ba
_database_code_depnum_ccdc_archive 'CCDC 2320545'
loop_
_audit_author_name
_audit_author_address
'Miguel Clemente-Leon'
;Universidad de Valencia
Spain
;
_audit_update_record             
;
2023-12-19 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_audit_creation_date             2021-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H10 N9 O8 Tb, 2(H2 O)'
_chemical_formula_sum            'C15 H14 N9 O10 Tb'
_chemical_formula_weight         639.27
_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'
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                   8.6577(2)
_cell_length_b                   10.4166(3)
_cell_length_c                   12.0856(4)
_cell_angle_alpha                80.206(2)
_cell_angle_beta                 79.607(2)
_cell_angle_gamma                82.473(2)
_cell_volume                     1050.75(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14605
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      30.4240
_cell_measurement_theta_min      3.7370
_shelx_estimated_absorpt_T_max   0.795
_shelx_estimated_absorpt_T_min   0.609
_exptl_absorpt_coefficient_mu    3.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20971
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.539
_diffrn_reflns_theta_min         3.280
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00   1.00   1.00   10.00    --  -19.95 -60.00   5.67   89
  2  ω    -88.00   4.00   1.00   10.00    --  -19.95 -68.00-174.88   92
  3  ω    -89.00   1.00   1.00   10.00    --  -19.95 -57.00  90.00   90
  4  ω    -88.00   5.00   1.00   10.00    --  -19.95 -69.00 -91.18   93
  5  ω    -48.00  45.00   1.00   10.00    --   20.73 -69.00 -22.49   93
  6  ω    -46.00  46.00   1.00   10.00    --   22.00 -67.00 150.97   92
  7  ω    -46.00  46.00   1.00   10.00    --   22.00 -67.00  61.42   92
  8  ω    -45.00  45.00   1.00   10.00    --   22.00 -64.00-111.99   90
  9  ω    -47.00  45.00   1.00   10.00    --   20.73 -67.00-139.91   92
 10  ω    -45.00  11.00   1.00   10.00    --   22.00 -64.00 108.22   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341760000
_diffrn_orient_matrix_UB_12      0.0656804000
_diffrn_orient_matrix_UB_13      0.0003265000
_diffrn_orient_matrix_UB_21      0.0355142000
_diffrn_orient_matrix_UB_22      0.0036540000
_diffrn_orient_matrix_UB_23      0.0477197000
_diffrn_orient_matrix_UB_31      0.0677030000
_diffrn_orient_matrix_UB_32      0.0223453000
_diffrn_orient_matrix_UB_33      -0.0369499000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5394
_reflns_number_total             5718
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.916
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5718
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0201
_refine_ls_restrained_S_all      1.064
_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)+(0.0159P)²+0.8377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0453
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O00B(H00E,H00F), O00G(H00G,H00H)
2.b Rotating group:
 O005(H00A,H00B), O008(H00C,H00D)
2.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00Q(H00Q), C00T(H00T), C00W(H00W), C00Y(H00Y), C00Z(H00Z)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb01 Tb 0.78009(2) 0.25875(2) 0.24972(2) 0.00625(3) Uani 1 1 d . . . . .
O002 O 0.70944(18) 0.29987(15) 0.44294(12) 0.0114(3) Uani 1 1 d . . . . .
O003 O 0.41633(18) 0.54424(15) 0.71736(12) 0.0115(3) Uani 1 1 d . . . . .
O004 O 1.25120(17) -0.07191(15) -0.15196(13) 0.0106(3) Uani 1 1 d . . . . .
O005 O 0.70054(19) 0.33961(16) 0.07122(13) 0.0139(3) Uani 1 1 d . . . . .
H00A H 0.678672 0.422748 0.064705 0.021 Uiso 1 1 d GR . . . .
H00B H 0.613132 0.310967 0.069064 0.021 Uiso 1 1 d GR . . . .
O006 O 1.00963(18) 0.18521(15) 0.12834(13) 0.0110(3) Uani 1 1 d . . . . .
O007 O 0.21655(17) -0.05206(15) 0.62231(12) 0.0099(3) Uani 1 1 d . . . . .
O008 O 0.91322(19) 0.45039(16) 0.18486(14) 0.0153(3) Uani 1 1 d . . . . .
H00C H 1.015328 0.430629 0.177163 0.023 Uiso 1 1 d GR . . . .
H00D H 0.894076 0.502280 0.236450 0.023 Uiso 1 1 d GR . . . .
O009 O 0.52299(18) 0.18904(15) 0.31696(12) 0.0103(3) Uani 1 1 d . . . . .
N00A N 0.0190(2) 0.23356(19) 0.35311(15) 0.0107(4) Uani 1 1 d . . . . .
O00B O 0.2444(2) 0.46211(18) 0.12680(15) 0.0214(4) Uani 1 1 d . . . . .
H00E H 0.258028 0.501882 0.179597 0.032 Uiso 1 1 d G . . . .
H00F H 0.304079 0.390723 0.134836 0.032 Uiso 1 1 d G . . . .
N00C N 1.4592(2) 0.2359(2) 0.01221(16) 0.0149(4) Uani 1 1 d . . . . .
N00D N 1.2767(2) 0.13409(18) -0.02760(15) 0.0092(4) Uani 1 1 d . . . . .
C00E C 1.1397(2) -0.0336(2) -0.08062(17) 0.0084(4) Uani 1 1 d . . . . .
N00F N 0.2210(2) 0.15450(18) 0.43684(15) 0.0084(3) Uani 1 1 d . . . . .
O00G O 0.8333(3) 0.6471(2) 0.30772(19) 0.0386(6) Uani 1 1 d . . . . .
H00G H 0.822829 0.682735 0.367334 0.058 Uiso 1 1 d G . . . .
H00H H 0.790893 0.704773 0.260545 0.058 Uiso 1 1 d G . . . .
C00H C 1.1418(2) 0.0631(2) -0.01292(18) 0.0096(4) Uani 1 1 d . . . . .
N00I N 0.6388(2) 0.32014(18) 0.67138(15) 0.0105(4) Uani 1 1 d . . . . .
C00J C 0.4608(3) 0.5170(2) 0.61941(17) 0.0094(4) Uani 1 1 d . . . . .
N00K N 1.2963(2) 0.2378(2) -0.11311(16) 0.0145(4) Uani 1 1 d . . . . .
C00L C 1.0121(2) 0.0997(2) 0.06572(17) 0.0087(4) Uani 1 1 d . . . . .
C00M C 0.6122(2) 0.3917(2) 0.47522(17) 0.0090(4) Uani 1 1 d . . . . .
N00N N 0.1689(2) 0.2707(2) 0.47593(18) 0.0188(5) Uani 1 1 d . . . . .
C00O C 0.1307(3) 0.1353(2) 0.36417(18) 0.0109(4) Uani 1 1 d . . . . .
H00O H 0.144357 0.062818 0.326499 0.013 Uiso 1 1 calc R . . . .
C00P C 0.5051(2) 0.1031(2) 0.40326(17) 0.0086(4) Uani 1 1 d . . . . .
C00Q C 1.3741(3) 0.1356(2) 0.04583(19) 0.0132(4) Uani 1 1 d . . . . .
H00Q H 1.381179 0.074905 0.111192 0.016 Uiso 1 1 calc R . . . .
N00R N 0.7463(2) 0.3500(2) 0.72993(17) 0.0167(4) Uani 1 1 d . . . . .
C00S C 0.3590(2) 0.0771(2) 0.46869(18) 0.0091(4) Uani 1 1 d . . . . .
C00T C 1.4063(3) 0.2950(2) -0.08491(19) 0.0139(4) Uani 1 1 d . . . . .
H00T H 1.445071 0.370169 -0.128034 0.017 Uiso 1 1 calc R . . . .
C00U C 0.3439(2) -0.0226(2) 0.56333(17) 0.0078(4) Uani 1 1 d . . . . .
C00V C 0.5692(3) 0.4119(2) 0.58825(17) 0.0097(4) Uani 1 1 d . . . . .
C00W C 0.0484(3) 0.3138(2) 0.4224(2) 0.0190(5) Uani 1 1 d . . . . .
H00W H -0.011836 0.393220 0.431358 0.023 Uiso 1 1 calc R . . . .
N00X N 0.7246(3) 0.1322(2) 0.76412(17) 0.0207(5) Uani 1 1 d . . . . .
C00Y C 0.6296(3) 0.1909(2) 0.6927(2) 0.0174(5) Uani 1 1 d . . . . .
H00Y H 0.564525 0.147917 0.661112 0.021 Uiso 1 1 calc R . . . .
C00Z C 0.7922(3) 0.2341(3) 0.7842(2) 0.0209(5) Uani 1 1 d . . . . .
H00Z H 0.866215 0.223328 0.832928 0.025 Uiso 1 1 calc R . . . .


_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
Tb01 O002 2.4014(14) . ?
Tb01 O003 2.5260(15) 2_666 ?
Tb01 O004 2.5086(15) 2_755 ?
Tb01 O005 2.3672(15) . ?
Tb01 O006 2.3707(15) . ?
Tb01 O007 2.4279(15) 2_656 ?
Tb01 O008 2.3817(17) . ?
Tb01 O009 2.3900(15) . ?
Tb01 N00A 2.5664(18) 1_655 ?
O002 C00M 1.255(2) . ?
O003 C00J 1.246(2) . ?
O004 C00E 1.245(2) . ?
O005 H00A 0.8552 . ?
O005 H00B 0.8552 . ?
O006 C00L 1.259(2) . ?
O007 C00U 1.245(3) . ?
O008 H00C 0.8728 . ?
O008 H00D 0.8731 . ?
O009 C00P 1.254(3) . ?
N00A C00O 1.320(3) . ?
N00A C00W 1.355(3) . ?
O00B H00E 0.8500 . ?
O00B H00F 0.8498 . ?
N00C C00Q 1.323(3) . ?
N00C C00T 1.357(3) . ?
N00D C00H 1.431(3) . ?
N00D N00K 1.367(3) . ?
N00D C00Q 1.333(3) . ?
C00E C00H 1.406(3) . ?
C00E C00L 1.531(3) 2_755 ?
N00F N00N 1.367(2) . ?
N00F C00O 1.331(3) . ?
N00F C00S 1.426(3) . ?
O00G H00G 0.8505 . ?
O00G H00H 0.8498 . ?
C00H C00L 1.391(3) . ?
N00I N00R 1.361(3) . ?
N00I C00V 1.424(3) . ?
N00I C00Y 1.337(3) . ?
C00J C00M 1.531(3) 2_666 ?
C00J C00V 1.402(3) . ?
N00K C00T 1.308(3) . ?
C00M C00V 1.394(3) . ?
N00N C00W 1.315(3) . ?
C00O H00O 0.9300 . ?
C00P C00S 1.398(3) . ?
C00P C00U 1.537(3) 2_656 ?
C00Q H00Q 0.9300 . ?
N00R C00Z 1.320(3) . ?
C00S C00U 1.408(3) . ?
C00T H00T 0.9300 . ?
C00W H00W 0.9300 . ?
N00X C00Y 1.320(3) . ?
N00X C00Z 1.353(3) . ?
C00Y H00Y 0.9300 . ?
C00Z H00Z 0.9300 . ?

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
O002 Tb01 O003 63.86(5) . 2_666 ?
O002 Tb01 O004 133.27(5) . 2_755 ?
O002 Tb01 O007 70.52(5) . 2_656 ?
O002 Tb01 N00A 67.11(5) . 1_655 ?
O003 Tb01 N00A 115.20(5) 2_666 1_655 ?
O004 Tb01 O003 127.34(5) 2_755 2_666 ?
O004 Tb01 N00A 116.84(5) 2_755 1_655 ?
O005 Tb01 O002 138.18(5) . . ?
O005 Tb01 O003 74.63(5) . 2_666 ?
O005 Tb01 O004 69.92(5) . 2_755 ?
O005 Tb01 O006 80.57(5) . . ?
O005 Tb01 O007 136.43(5) . 2_656 ?
O005 Tb01 O008 76.36(6) . . ?
O005 Tb01 O009 88.62(5) . . ?
O005 Tb01 N00A 141.80(6) . 1_655 ?
O006 Tb01 O002 137.67(5) . . ?
O006 Tb01 O003 143.30(5) . 2_666 ?
O006 Tb01 O004 65.20(5) . 2_755 ?
O006 Tb01 O007 92.42(5) . 2_656 ?
O006 Tb01 O008 76.34(5) . . ?
O006 Tb01 O009 135.91(5) . . ?
O006 Tb01 N00A 70.75(5) . 1_655 ?
O007 Tb01 O003 124.15(5) 2_656 2_666 ?
O007 Tb01 O004 68.19(5) 2_656 2_755 ?
O007 Tb01 N00A 70.98(6) 2_656 1_655 ?
O008 Tb01 O002 94.69(6) . . ?
O008 Tb01 O003 71.85(5) . 2_666 ?
O008 Tb01 O004 131.83(5) . 2_755 ?
O008 Tb01 O007 143.77(5) . 2_656 ?
O008 Tb01 O009 142.03(5) . . ?
O008 Tb01 N00A 72.79(6) . 1_655 ?
O009 Tb01 O002 73.56(5) . . ?
O009 Tb01 O003 70.58(5) . 2_666 ?
O009 Tb01 O004 70.91(5) . 2_755 ?
O009 Tb01 O007 66.92(5) . 2_656 ?
O009 Tb01 N00A 129.57(5) . 1_655 ?
C00M O002 Tb01 124.87(13) . . ?
C00J O003 Tb01 120.21(13) . 2_666 ?
C00E O004 Tb01 118.78(14) . 2_755 ?
Tb01 O005 H00A 109.8 . . ?
Tb01 O005 H00B 109.4 . . ?
H00A O005 H00B 104.2 . . ?
C00L O006 Tb01 123.45(14) . . ?
C00U O007 Tb01 117.48(13) . 2_656 ?
Tb01 O008 H00C 110.6 . . ?
Tb01 O008 H00D 110.6 . . ?
H00C O008 H00D 103.4 . . ?
C00P O009 Tb01 118.37(13) . . ?
C00O N00A Tb01 129.83(15) . 1_455 ?
C00O N00A C00W 102.94(18) . . ?
C00W N00A Tb01 126.77(14) . 1_455 ?
H00E O00B H00F 104.5 . . ?
C00Q N00C C00T 103.05(19) . . ?
N00K N00D C00H 119.94(18) . . ?
C00Q N00D C00H 128.75(19) . . ?
C00Q N00D N00K 109.44(18) . . ?
O004 C00E C00H 125.9(2) . . ?
O004 C00E C00L 116.26(18) . 2_755 ?
C00H C00E C00L 117.79(18) . 2_755 ?
N00N N00F C00S 121.25(17) . . ?
C00O N00F N00N 109.57(17) . . ?
C00O N00F C00S 129.05(18) . . ?
H00G O00G H00H 104.4 . . ?
C00E C00H N00D 120.49(18) . . ?
C00L C00H N00D 117.00(18) . . ?
C00L C00H C00E 122.4(2) . . ?
N00R N00I C00V 123.38(19) . . ?
C00Y N00I N00R 109.04(19) . . ?
C00Y N00I C00V 126.89(19) . . ?
O003 C00J C00M 115.85(18) . 2_666 ?
O003 C00J C00V 126.6(2) . . ?
C00V C00J C00M 117.60(17) . 2_666 ?
C00T N00K N00D 102.66(18) . . ?
O006 C00L C00E 115.89(18) . 2_755 ?
O006 C00L C00H 124.3(2) . . ?
C00H C00L C00E 119.80(18) . 2_755 ?
O002 C00M C00J 115.19(18) . 2_666 ?
O002 C00M C00V 124.09(19) . . ?
C00V C00M C00J 120.72(18) . 2_666 ?
C00W N00N N00F 102.30(18) . . ?
N00A C00O N00F 110.41(19) . . ?
N00A C00O H00O 124.8 . . ?
N00F C00O H00O 124.8 . . ?
O009 C00P C00S 124.34(19) . . ?
O009 C00P C00U 116.39(19) . 2_656 ?
C00S C00P C00U 119.27(18) . 2_656 ?
N00C C00Q N00D 110.1(2) . . ?
N00C C00Q H00Q 124.9 . . ?
N00D C00Q H00Q 124.9 . . ?
C00Z N00R N00I 102.2(2) . . ?
C00P C00S N00F 118.15(19) . . ?
C00P C00S C00U 122.47(19) . . ?
C00U C00S N00F 119.38(19) . . ?
N00C C00T H00T 122.6 . . ?
N00K C00T N00C 114.7(2) . . ?
N00K C00T H00T 122.6 . . ?
O007 C00U C00P 116.82(19) . 2_656 ?
O007 C00U C00S 124.93(19) . . ?
C00S C00U C00P 118.25(18) . 2_656 ?
C00J C00V N00I 121.17(18) . . ?
C00M C00V N00I 117.16(18) . . ?
C00M C00V C00J 121.67(19) . . ?
N00A C00W H00W 122.6 . . ?
N00N C00W N00A 114.8(2) . . ?
N00N C00W H00W 122.6 . . ?
C00Y N00X C00Z 101.9(2) . . ?
N00I C00Y H00Y 124.3 . . ?
N00X C00Y N00I 111.4(2) . . ?
N00X C00Y H00Y 124.3 . . ?
N00R C00Z N00X 115.6(2) . . ?
N00R C00Z H00Z 122.2 . . ?
N00X C00Z H00Z 122.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.605
_oxdiff_exptl_absorpt_empirical_full_min 0.677
####################################################################### 
# 
# 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_nm275ba
_database_code_depnum_ccdc_archive 'CCDC 2320547'
loop_
_audit_author_name
_audit_author_address
'Miguel Clemente-Leon'
;Universidad de Valencia
Spain
;
_audit_update_record             
;
2023-12-19 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_audit_creation_date             2021-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H10 Ho N9 O8, 2(H2 O)'
_chemical_formula_sum            'C15 H14 Ho N9 O10'
_chemical_formula_weight         645.28
_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'
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                   8.6344(2)
_cell_length_b                   10.4202(2)
_cell_length_c                   12.0281(3)
_cell_angle_alpha                80.171(2)
_cell_angle_beta                 79.315(2)
_cell_angle_gamma                82.353(2)
_cell_volume                     1042.06(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16223
_cell_measurement_temperature    120.2(3)
_cell_measurement_theta_max      30.3500
_cell_measurement_theta_min      3.7600
_shelx_estimated_absorpt_T_max   0.722
_shelx_estimated_absorpt_T_min   0.400
_exptl_absorpt_coefficient_mu    3.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.057
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.29
_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  0.0255
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20633
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.430
_diffrn_reflns_theta_min         3.487
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00   4.00   1.00   10.00    --  -19.95 -67.00-130.14   92
  2  ω    -88.00   4.00   1.00   10.00    --  -19.95 -67.00  26.48   92
  3  ω    -88.00   1.00   1.00   10.00    --  -19.95 -60.00 -63.58   89
  4  ω    -88.00   2.00   1.00   10.00    --  -19.95 -63.00 122.64   90
  5  ω    -48.00  42.00   1.00   10.00    --   20.73 -57.00 -90.00   90
  6  ω    -47.00  44.00   1.00   10.00    --   20.73 -66.00 103.21   91
  7  ω    -46.00  47.00   1.00   10.00    --   22.00 -69.00 152.86   93
  8  ω    -46.00  47.00   1.00   10.00    --   22.00 -69.00-155.12   93
  9  ω    -46.00  47.00   1.00   10.00    --   22.00 -69.00   4.14   93
 10  ω    -47.00   9.00   1.00   10.00    --   20.73 -65.00-108.54   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0773182000
_diffrn_orient_matrix_UB_12      0.0173691000
_diffrn_orient_matrix_UB_13      -0.0022028000
_diffrn_orient_matrix_UB_21      -0.0224797000
_diffrn_orient_matrix_UB_22      0.0171038000
_diffrn_orient_matrix_UB_23      0.0557920000
_diffrn_orient_matrix_UB_31      0.0241369000
_diffrn_orient_matrix_UB_32      -0.0650486000
_diffrn_orient_matrix_UB_33      0.0238017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5504
_reflns_number_total             5678
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.742
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0166
_refine_ls_restrained_S_all      1.061
_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)+(0.0099P)²+1.0402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0370
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O00B(H00E,H00F), O00G(H00G,H00H)
2.b Rotating group:
 O003(H00A,H00B), O007(H00C,H00D)
2.c Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00U(H00U), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho01 Ho 0.78039(2) 0.25771(2) 0.25049(2) 0.00664(3) Uani 1 1 d . . . . .
O002 O 0.70992(16) 0.29969(13) 0.44273(11) 0.0122(3) Uani 1 1 d . . . . .
O003 O 0.70111(17) 0.33730(14) 0.07344(11) 0.0145(3) Uani 1 1 d . . . . .
H00A H 0.682224 0.421986 0.064682 0.022 Uiso 1 1 d GR . . . .
H00B H 0.610353 0.311287 0.071693 0.022 Uiso 1 1 d GR . . . .
O004 O 1.25193(15) -0.07175(13) -0.15356(11) 0.0114(3) Uani 1 1 d . . . . .
O005 O 0.41544(16) 0.54593(13) 0.71850(11) 0.0124(3) Uani 1 1 d . . . . .
O006 O 0.21501(15) -0.05273(12) 0.62245(11) 0.0103(2) Uani 1 1 d . . . . .
O007 O 0.91130(17) 0.44763(13) 0.18554(12) 0.0154(3) Uani 1 1 d . . . . .
H00C H 1.013192 0.428235 0.179065 0.023 Uiso 1 1 d GR . . . .
H00D H 0.889814 0.499654 0.236797 0.023 Uiso 1 1 d GR . . . .
O008 O 1.00928(15) 0.18434(13) 0.12962(11) 0.0121(3) Uani 1 1 d . . . . .
O009 O 0.52436(15) 0.18993(13) 0.31689(11) 0.0107(3) Uani 1 1 d . . . . .
N00A N 0.01783(19) 0.23321(15) 0.35222(13) 0.0112(3) Uani 1 1 d . . . . .
O00B O 0.24264(19) 0.46169(15) 0.12566(13) 0.0226(3) Uani 1 1 d . . . . .
H00E H 0.301795 0.389892 0.133922 0.034 Uiso 1 1 d G . . . .
H00F H 0.257270 0.501743 0.178129 0.034 Uiso 1 1 d G . . . .
N00C N 1.4599(2) 0.23573(17) 0.01279(14) 0.0157(3) Uani 1 1 d . . . . .
C00D C 1.1404(2) -0.03356(17) -0.08157(15) 0.0092(3) Uani 1 1 d . . . . .
N00E N 1.27705(18) 0.13368(15) -0.02787(13) 0.0101(3) Uani 1 1 d . . . . .
N00F N 0.22070(18) 0.15420(15) 0.43636(13) 0.0095(3) Uani 1 1 d . . . . .
O00G O 0.8322(3) 0.64547(17) 0.30874(16) 0.0365(5) Uani 1 1 d . . . . .
H00G H 0.827277 0.676040 0.370601 0.055 Uiso 1 1 d G . . . .
H00H H 0.796588 0.704809 0.259261 0.055 Uiso 1 1 d G . . . .
N00H N 0.63941(19) 0.32088(15) 0.67191(13) 0.0117(3) Uani 1 1 d . . . . .
C00I C 1.1426(2) 0.06319(18) -0.01345(15) 0.0102(3) Uani 1 1 d . . . . .
C00J C 0.5056(2) 0.10372(17) 0.40324(15) 0.0087(3) Uani 1 1 d . . . . .
C00K C 0.3431(2) -0.02311(17) 0.56306(15) 0.0087(3) Uani 1 1 d . . . . .
N00L N 0.1690(2) 0.27173(17) 0.47417(15) 0.0184(4) Uani 1 1 d . . . . .
C00M C 0.1295(2) 0.13457(18) 0.36406(16) 0.0112(3) Uani 1 1 d . . . . .
H00M H 0.142682 0.061490 0.327055 0.013 Uiso 1 1 calc R . . . .
C00N C 0.6123(2) 0.39153(17) 0.47496(15) 0.0097(3) Uani 1 1 d . . . . .
C00O C 0.4605(2) 0.51776(18) 0.62018(15) 0.0102(3) Uani 1 1 d . . . . .
N00P N 1.2964(2) 0.23842(17) -0.11333(14) 0.0156(3) Uani 1 1 d . . . . .
N00Q N 0.7474(2) 0.35051(17) 0.73067(15) 0.0181(4) Uani 1 1 d . . . . .
C00R C 0.3586(2) 0.07711(18) 0.46849(15) 0.0097(3) Uani 1 1 d . . . . .
C00S C 1.0119(2) 0.09936(17) 0.06646(15) 0.0092(3) Uani 1 1 d . . . . .
N00T N 0.7259(2) 0.13264(18) 0.76450(15) 0.0225(4) Uani 1 1 d . . . . .
C00U C 1.3744(2) 0.13502(19) 0.04598(17) 0.0139(4) Uani 1 1 d . . . . .
H00U H 1.381417 0.073972 0.111458 0.017 Uiso 1 1 calc R . . . .
C00V C 0.5700(2) 0.41254(18) 0.58888(15) 0.0115(3) Uani 1 1 d . . . . .
C00W C 0.0479(2) 0.3142(2) 0.42133(18) 0.0189(4) Uani 1 1 d . . . . .
H00W H -0.012783 0.393561 0.430453 0.023 Uiso 1 1 calc R . . . .
C00X C 1.4066(2) 0.2957(2) -0.08458(16) 0.0149(4) Uani 1 1 d . . . . .
H00X H 1.445044 0.371321 -0.127447 0.018 Uiso 1 1 calc R . . . .
C00Y C 0.6303(3) 0.19177(19) 0.69336(17) 0.0180(4) Uani 1 1 d . . . . .
H00Y H 0.564785 0.148944 0.662049 0.022 Uiso 1 1 calc R . . . .
C00Z C 0.7941(3) 0.2346(2) 0.78457(19) 0.0225(4) Uani 1 1 d . . . . .
H00Z H 0.868655 0.223553 0.833055 0.027 Uiso 1 1 calc R . . . .


_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
Ho01 O002 2.3793(13) . ?
Ho01 O003 2.3405(13) . ?
Ho01 O004 2.4956(13) 2_755 ?
Ho01 O005 2.5081(13) 2_666 ?
Ho01 O006 2.4052(13) 2_656 ?
Ho01 O007 2.3547(13) . ?
Ho01 O008 2.3487(13) . ?
Ho01 O009 2.3647(13) . ?
Ho01 N00A 2.5396(16) 1_655 ?
O002 C00N 1.252(2) . ?
O003 H00A 0.8676 . ?
O003 H00B 0.8675 . ?
O004 C00D 1.242(2) . ?
O005 C00O 1.246(2) . ?
O006 C00K 1.245(2) . ?
O007 H00C 0.8681 . ?
O007 H00D 0.8680 . ?
O008 C00S 1.257(2) . ?
O009 C00J 1.253(2) . ?
N00A C00M 1.320(2) . ?
N00A C00W 1.359(2) . ?
O00B H00E 0.8498 . ?
O00B H00F 0.8497 . ?
N00C C00U 1.326(2) . ?
N00C C00X 1.359(3) . ?
C00D C00I 1.408(2) . ?
C00D C00S 1.530(2) 2_755 ?
N00E C00I 1.423(2) . ?
N00E N00P 1.370(2) . ?
N00E C00U 1.334(2) . ?
N00F N00L 1.369(2) . ?
N00F C00M 1.333(2) . ?
N00F C00R 1.422(2) . ?
O00G H00G 0.8500 . ?
O00G H00H 0.8500 . ?
N00H N00Q 1.364(2) . ?
N00H C00V 1.419(2) . ?
N00H C00Y 1.336(2) . ?
C00I C00S 1.396(2) . ?
C00J C00K 1.538(3) 2_656 ?
C00J C00R 1.397(2) . ?
C00K C00R 1.406(3) . ?
N00L C00W 1.312(3) . ?
C00M H00M 0.9300 . ?
C00N C00O 1.529(3) 2_666 ?
C00N C00V 1.398(2) . ?
C00O C00V 1.404(2) . ?
N00P C00X 1.313(3) . ?
N00Q C00Z 1.320(3) . ?
N00T C00Y 1.319(3) . ?
N00T C00Z 1.356(3) . ?
C00U H00U 0.9300 . ?
C00W H00W 0.9300 . ?
C00X H00X 0.9300 . ?
C00Y H00Y 0.9300 . ?
C00Z H00Z 0.9300 . ?

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
O002 Ho01 O004 133.31(4) . 2_755 ?
O002 Ho01 O005 64.27(4) . 2_666 ?
O002 Ho01 O006 70.97(4) . 2_656 ?
O002 Ho01 N00A 67.20(5) . 1_655 ?
O003 Ho01 O002 137.98(5) . . ?
O003 Ho01 O004 69.87(5) . 2_755 ?
O003 Ho01 O005 74.02(5) . 2_666 ?
O003 Ho01 O006 136.32(5) . 2_656 ?
O003 Ho01 O007 76.37(5) . . ?
O003 Ho01 O008 80.86(5) . . ?
O003 Ho01 O009 88.05(5) . . ?
O003 Ho01 N00A 141.78(5) . 1_655 ?
O004 Ho01 O005 126.83(4) 2_755 2_666 ?
O004 Ho01 N00A 117.06(5) 2_755 1_655 ?
O005 Ho01 N00A 115.55(5) 2_666 1_655 ?
O006 Ho01 O004 68.01(4) 2_656 2_755 ?
O006 Ho01 O005 124.94(4) 2_656 2_666 ?
O006 Ho01 N00A 70.99(5) 2_656 1_655 ?
O007 Ho01 O002 94.38(5) . . ?
O007 Ho01 O004 132.15(5) . 2_755 ?
O007 Ho01 O005 71.39(5) . 2_666 ?
O007 Ho01 O006 143.82(5) . 2_656 ?
O007 Ho01 O009 141.50(5) . . ?
O007 Ho01 N00A 72.84(5) . 1_655 ?
O008 Ho01 O002 137.51(5) . . ?
O008 Ho01 O004 65.56(4) . 2_755 ?
O008 Ho01 O005 142.96(4) . 2_666 ?
O008 Ho01 O006 91.99(4) . 2_656 ?
O008 Ho01 O007 76.59(5) . . ?
O008 Ho01 O009 135.94(4) . . ?
O008 Ho01 N00A 70.49(5) . 1_655 ?
O009 Ho01 O002 73.96(5) . . ?
O009 Ho01 O004 70.57(4) . 2_755 ?
O009 Ho01 O005 70.51(4) . 2_666 ?
O009 Ho01 O006 67.57(4) . 2_656 ?
O009 Ho01 N00A 130.15(5) . 1_655 ?
C00N O002 Ho01 124.87(12) . . ?
Ho01 O003 H00A 110.5 . . ?
Ho01 O003 H00B 110.2 . . ?
H00A O003 H00B 103.7 . . ?
C00D O004 Ho01 118.54(11) . 2_755 ?
C00O O005 Ho01 119.97(12) . 2_666 ?
C00K O006 Ho01 117.23(12) . 2_656 ?
Ho01 O007 H00C 110.4 . . ?
Ho01 O007 H00D 110.2 . . ?
H00C O007 H00D 103.6 . . ?
C00S O008 Ho01 123.40(11) . . ?
C00J O009 Ho01 118.30(11) . . ?
C00M N00A Ho01 129.93(12) . 1_455 ?
C00M N00A C00W 102.74(16) . . ?
C00W N00A Ho01 126.84(13) . 1_455 ?
H00E O00B H00F 104.5 . . ?
C00U N00C C00X 102.88(16) . . ?
O004 C00D C00I 125.91(17) . . ?
O004 C00D C00S 116.12(15) . 2_755 ?
C00I C00D C00S 117.96(15) . 2_755 ?
N00P N00E C00I 119.88(16) . . ?
C00U N00E C00I 128.87(16) . . ?
C00U N00E N00P 109.29(15) . . ?
N00L N00F C00R 121.28(15) . . ?
C00M N00F N00L 109.28(15) . . ?
C00M N00F C00R 129.30(16) . . ?
H00G O00G H00H 109.5 . . ?
N00Q N00H C00V 123.39(16) . . ?
C00Y N00H N00Q 108.92(16) . . ?
C00Y N00H C00V 127.01(17) . . ?
C00D C00I N00E 120.85(15) . . ?
C00S C00I C00D 122.13(16) . . ?
C00S C00I N00E 116.94(15) . . ?
O009 C00J C00K 116.31(15) . 2_656 ?
O009 C00J C00R 124.44(17) . . ?
C00R C00J C00K 119.25(16) . 2_656 ?
O006 C00K C00J 116.68(16) . 2_656 ?
O006 C00K C00R 124.99(17) . . ?
C00R C00K C00J 118.33(15) . 2_656 ?
C00W N00L N00F 102.51(16) . . ?
N00A C00M N00F 110.64(16) . . ?
N00A C00M H00M 124.7 . . ?
N00F C00M H00M 124.7 . . ?
O002 C00N C00O 115.17(15) . 2_666 ?
O002 C00N C00V 123.86(17) . . ?
C00V C00N C00O 120.97(16) . 2_666 ?
O005 C00O C00N 115.71(16) . 2_666 ?
O005 C00O C00V 126.75(17) . . ?
C00V C00O C00N 117.54(15) . 2_666 ?
C00X N00P N00E 102.71(16) . . ?
C00Z N00Q N00H 102.22(17) . . ?
C00J C00R N00F 118.12(16) . . ?
C00J C00R C00K 122.40(17) . . ?
C00K C00R N00F 119.47(16) . . ?
O008 C00S C00D 115.90(15) . 2_755 ?
O008 C00S C00I 124.19(16) . . ?
C00I C00S C00D 119.91(15) . 2_755 ?
C00Y N00T C00Z 101.81(18) . . ?
N00C C00U N00E 110.40(17) . . ?
N00C C00U H00U 124.8 . . ?
N00E C00U H00U 124.8 . . ?
C00N C00V N00H 117.08(16) . . ?
C00N C00V C00O 121.49(17) . . ?
C00O C00V N00H 121.41(16) . . ?
N00A C00W H00W 122.6 . . ?
N00L C00W N00A 114.84(18) . . ?
N00L C00W H00W 122.6 . . ?
N00C C00X H00X 122.6 . . ?
N00P C00X N00C 114.72(17) . . ?
N00P C00X H00X 122.6 . . ?
N00H C00Y H00Y 124.2 . . ?
N00T C00Y N00H 111.55(19) . . ?
N00T C00Y H00Y 124.2 . . ?
N00Q C00Z N00T 115.5(2) . . ?
N00Q C00Z H00Z 122.2 . . ?
N00T C00Z H00Z 122.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.618
####################################################################### 
# 
# 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_nm275a77small
_database_code_depnum_ccdc_archive 'CCDC 2320546'
loop_
_audit_author_name
_audit_author_address
'Miguel Clemente-Leon'
;Universidad de Valencia
Spain
;
_audit_update_record             
;
2023-12-19 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;
_audit_creation_date             2020-05-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H10 Ho N9 O8, 4.5(H2 O)'
_chemical_formula_sum            'C15 H19 Ho N9 O12.50'
_chemical_formula_weight         690.32
_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'
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                   8.9571(3)
_cell_length_b                   9.4084(3)
_cell_length_c                   15.4980(4)
_cell_angle_alpha                75.173(2)
_cell_angle_beta                 77.349(2)
_cell_angle_gamma                67.977(3)
_cell_volume                     1159.35(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14068
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.4330
_cell_measurement_theta_min      3.9310
_shelx_estimated_absorpt_T_max   0.700
_shelx_estimated_absorpt_T_min   0.541
_exptl_absorpt_coefficient_mu    3.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16014
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.313
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details      ?
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0622309000
_diffrn_orient_matrix_UB_12      -0.0266410000
_diffrn_orient_matrix_UB_13      0.0277512000
_diffrn_orient_matrix_UB_21      -0.0511640000
_diffrn_orient_matrix_UB_22      0.0784432000
_diffrn_orient_matrix_UB_23      0.0007056000
_diffrn_orient_matrix_UB_31      -0.0307680000
_diffrn_orient_matrix_UB_32      0.0019777000
_diffrn_orient_matrix_UB_33      -0.0389081000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4666
_reflns_number_total             4772
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         0.800
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4772
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0184
_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)+(0.0221P)²+1.6658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0461
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5) O12(0.5) H12A(0.5) H12B(0.5) O13(0.5)
 H13A(0.5) H13B(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.5) H15A(0.5) H15B(0.5)
3.a Free rotating group:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B),
 O14(H14A,H14B), O15(H15A,H15B)
3.b Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C14(H14), C15(H15)
;
_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 0.66402(2) 0.60887(2) 0.21414(2) 0.01099(4) Uani 1 1 d . . . . .
O1 O 0.4625(2) 0.5391(2) 0.16896(11) 0.0160(3) Uani 1 1 d . . . . .
O2 O 0.2652(2) 0.4601(2) -0.06512(11) 0.0179(4) Uani 1 1 d . . . . .
O3 O 0.44574(19) 0.61893(19) 0.32916(10) 0.0136(3) Uani 1 1 d . . . . .
O4 O 0.25693(19) 0.50795(19) 0.63706(11) 0.0139(3) Uani 1 1 d . . . . .
O5 O 0.4429(2) 0.8358(2) 0.16569(11) 0.0184(4) Uani 1 1 d . . . . .
O6 O 0.2591(2) 1.1970(2) -0.09264(12) 0.0195(4) Uani 1 1 d . . . . .
O7 O 0.7327(2) 0.3315(2) 0.24467(12) 0.0171(4) Uani 1 1 d . . . . .
H7A H 0.778291 0.294145 0.195341 0.026 Uiso 1 1 d GR . . . .
H7B H 0.644965 0.305346 0.260416 0.026 Uiso 1 1 d GR . . . .
O8 O 0.7009(2) 0.7932(2) 0.28085(12) 0.0208(4) Uani 1 1 d . . . . .
H8A H 0.714816 0.870979 0.239813 0.031 Uiso 1 1 d GR . . . .
H8B H 0.791114 0.752322 0.303815 0.031 Uiso 1 1 d GR . . . .
N1 N -0.0358(2) 0.5232(2) 0.18892(13) 0.0144(4) Uani 1 1 d . . . . .
N2 N 0.2233(3) 0.3675(3) 0.19875(15) 0.0280(6) Uani 1 1 d . . . . .
N3 N 0.2131(2) 0.4791(2) 0.12157(13) 0.0130(4) Uani 1 1 d . . . . .
N4 N -0.0439(3) 0.6955(3) 0.38990(15) 0.0206(5) Uani 1 1 d . . . . .
N5 N 0.0450(3) 0.7209(3) 0.50833(15) 0.0213(5) Uani 1 1 d . . . . .
N6 N 0.1697(2) 0.6282(2) 0.45773(13) 0.0106(4) Uani 1 1 d . . . . .
N7 N -0.0848(3) 1.1425(3) 0.12812(15) 0.0226(5) Uani 1 1 d . . . . .
N8 N 0.1068(3) 0.9155(2) 0.09979(15) 0.0210(5) Uani 1 1 d . . . . .
N9 N 0.1691(2) 1.0345(2) 0.07727(13) 0.0147(4) Uani 1 1 d . . . . .
C1 C 0.4743(3) 0.5170(3) 0.09202(15) 0.0122(4) Uani 1 1 d . . . . .
C2 C 0.3549(3) 0.4883(3) 0.05981(16) 0.0130(5) Uani 1 1 d . . . . .
C3 C 0.3692(3) 0.4763(3) -0.02909(16) 0.0126(4) Uani 1 1 d . . . . .
C4 C 0.0710(3) 0.4000(3) 0.23649(17) 0.0238(6) Uani 1 1 d . . . . .
H4 H 0.039008 0.343152 0.291283 0.029 Uiso 1 1 calc R . . . .
C5 C 0.0595(3) 0.5698(3) 0.11738(16) 0.0126(4) Uani 1 1 d . . . . .
H5 H 0.023583 0.653901 0.071050 0.015 Uiso 1 1 calc R . . . .
C6 C 0.4614(3) 0.5642(2) 0.41062(15) 0.0097(4) Uani 1 1 d . . . . .
C7 C 0.3323(3) 0.5641(3) 0.47990(15) 0.0101(4) Uani 1 1 d . . . . .
C8 C 0.3618(3) 0.5070(2) 0.56919(15) 0.0100(4) Uani 1 1 d . . . . .
C9 C -0.0789(3) 0.7558(3) 0.46462(19) 0.0212(5) Uani 1 1 d . . . . .
H9 H -0.183349 0.818015 0.484170 0.025 Uiso 1 1 calc R . . . .
C10 C 0.1138(3) 0.6164(3) 0.38749(17) 0.0192(5) Uani 1 1 d . . . . .
H10 H 0.177061 0.560362 0.343031 0.023 Uiso 1 1 calc R . . . .
C11 C 0.4592(3) 0.9150(3) 0.08818(16) 0.0149(5) Uani 1 1 d . . . . .
C12 C 0.3337(3) 1.0139(3) 0.03935(16) 0.0147(5) Uani 1 1 d . . . . .
C13 C 0.3649(3) 1.1021(3) -0.04616(16) 0.0147(5) Uani 1 1 d . . . . .
C14 C -0.0457(3) 0.9867(3) 0.13070(18) 0.0227(5) Uani 1 1 d . . . . .
H14 H -0.120709 0.935003 0.152556 0.027 Uiso 1 1 calc R . . . .
C15 C 0.0538(3) 1.1665(3) 0.09459(17) 0.0205(5) Uani 1 1 d . . . . .
H15 H 0.069107 1.262239 0.084434 0.025 Uiso 1 1 calc R . . . .
O9 O 0.8877(2) 0.1281(2) 0.37883(13) 0.0224(4) Uani 1 1 d . . . . .
H9A H 0.905248 0.175684 0.413266 0.034 Uiso 1 1 d G . . . .
H9B H 0.977962 0.071396 0.354762 0.034 Uiso 1 1 d G . . . .
O10 O 0.1943(3) 0.9650(3) 0.31331(18) 0.0507(7) Uani 1 1 d . . . . .
H10A H 0.246327 0.908853 0.274060 0.076 Uiso 1 1 d G . . . .
H10B H 0.266559 0.959938 0.342682 0.076 Uiso 1 1 d G . . . .
O11 O 0.4540(5) 0.9606(4) 0.3755(3) 0.0249(8) Uiso 0.5 1 d . . P A 1
H11A H 0.480318 0.931150 0.428333 0.037 Uiso 0.5 1 d G . P A 1
H11B H 0.458051 1.052619 0.358532 0.037 Uiso 0.5 1 d G . P A 1
O12 O 0.5293(5) 1.1343(5) 0.2621(3) 0.0324(9) Uiso 0.5 1 d . . P B 2
H12A H 0.549285 1.116132 0.209019 0.049 Uiso 0.5 1 d G . P B 2
H12B H 0.457841 1.092958 0.289037 0.049 Uiso 0.5 1 d G . P B 2
O13 O 0.4432(5) 1.2610(4) 0.3314(3) 0.0240(8) Uiso 0.5 1 d . . P C 1
H13A H 0.379439 1.294918 0.291734 0.036 Uiso 0.5 1 d G . P C 1
H13B H 0.389952 1.308751 0.374205 0.036 Uiso 0.5 1 d G . P C 1
O14 O 0.3608(7) 0.9059(7) 0.4758(4) 0.0509(13) Uiso 0.5 1 d . . P D 2
H14A H 0.330618 1.003774 0.473449 0.076 Uiso 0.5 1 d G . P D 2
H14B H 0.406098 0.865086 0.523241 0.076 Uiso 0.5 1 d G . P D 2
O15 O 0.4095(7) 0.9156(6) 0.5603(4) 0.0489(13) Uiso 0.5 1 d . . P E 1
H15A H 0.308208 0.930137 0.572125 0.073 Uiso 0.5 1 d G . P E 1
H15B H 0.461393 0.820590 0.556287 0.073 Uiso 0.5 1 d G . P E 1


_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 O1 2.4205(16) . ?
Ho1 O2 2.4440(17) 2_665 ?
Ho1 O3 2.3303(16) . ?
Ho1 O4 2.4211(16) 2_666 ?
Ho1 O5 2.3882(17) . ?
Ho1 O6 2.4434(17) 2_675 ?
Ho1 O7 2.3887(17) . ?
Ho1 O8 2.3838(18) . ?
Ho1 N1 2.471(2) 1_655 ?
O1 C1 1.237(3) . ?
O2 C3 1.257(3) . ?
O3 C6 1.253(3) . ?
O4 C8 1.247(3) . ?
O5 C11 1.251(3) . ?
O6 C13 1.245(3) . ?
O7 H7A 0.8761 . ?
O7 H7B 0.8762 . ?
O8 H8A 0.8668 . ?
O8 H8B 0.8660 . ?
N1 C4 1.358(3) . ?
N1 C5 1.330(3) . ?
N2 N3 1.369(3) . ?
N2 C4 1.313(3) . ?
N3 C2 1.430(3) . ?
N3 C5 1.325(3) . ?
N4 C9 1.344(4) . ?
N4 C10 1.324(3) . ?
N5 N6 1.364(3) . ?
N5 C9 1.319(3) . ?
N6 C7 1.434(3) . ?
N6 C10 1.338(3) . ?
N7 C14 1.365(4) . ?
N7 C15 1.316(4) . ?
N8 N9 1.367(3) . ?
N8 C14 1.317(3) . ?
N9 C12 1.421(3) . ?
N9 C15 1.330(3) . ?
C1 C2 1.409(3) . ?
C1 C3 1.535(3) 2_665 ?
C2 C3 1.385(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.395(3) . ?
C6 C8 1.539(3) 2_666 ?
C7 C8 1.395(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.390(3) . ?
C11 C13 1.532(3) 2_675 ?
C12 C13 1.404(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O9 H9A 0.8497 . ?
O9 H9B 0.8503 . ?
O10 H10A 0.8499 . ?
O10 H10B 0.8499 . ?
O11 H11A 0.8501 . ?
O11 H11B 0.8500 . ?
O12 H12A 0.8500 . ?
O12 H12B 0.8500 . ?
O13 H13A 0.8498 . ?
O13 H13B 0.8502 . ?
O14 H14A 0.8499 . ?
O14 H14B 0.8500 . ?
O15 H15A 0.8500 . ?
O15 H15B 0.8501 . ?

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 Ho1 O2 64.99(5) . 2_665 ?
O1 Ho1 O4 118.68(5) . 2_666 ?
O1 Ho1 O6 108.76(6) . 2_675 ?
O1 Ho1 N1 134.80(6) . 1_655 ?
O2 Ho1 N1 76.48(6) 2_665 1_655 ?
O3 Ho1 O1 70.15(6) . . ?
O3 Ho1 O2 135.11(6) . 2_665 ?
O3 Ho1 O4 65.98(5) . 2_666 ?
O3 Ho1 O5 73.24(6) . . ?
O3 Ho1 O6 134.38(6) . 2_675 ?
O3 Ho1 O7 88.07(6) . . ?
O3 Ho1 O8 83.76(6) . . ?
O3 Ho1 N1 141.45(6) . 1_655 ?
O4 Ho1 O2 137.59(6) 2_666 2_665 ?
O4 Ho1 O6 132.51(6) 2_666 2_675 ?
O4 Ho1 N1 75.50(6) 2_666 1_655 ?
O5 Ho1 O1 68.85(6) . . ?
O5 Ho1 O2 91.54(6) . 2_665 ?
O5 Ho1 O4 130.34(6) . 2_666 ?
O5 Ho1 O6 64.99(6) . 2_675 ?
O5 Ho1 O7 138.33(6) . . ?
O5 Ho1 N1 137.23(6) . 1_655 ?
O6 Ho1 O2 65.34(6) 2_675 2_665 ?
O6 Ho1 N1 72.78(6) 2_675 1_655 ?
O7 Ho1 O1 69.82(6) . . ?
O7 Ho1 O2 75.74(6) . 2_665 ?
O7 Ho1 O4 68.07(6) . 2_666 ?
O7 Ho1 O6 135.88(6) . 2_675 ?
O7 Ho1 N1 78.81(6) . 1_655 ?
O8 Ho1 O1 143.85(6) . . ?
O8 Ho1 O2 136.00(6) . 2_665 ?
O8 Ho1 O4 68.70(6) . 2_666 ?
O8 Ho1 O5 80.12(6) . . ?
O8 Ho1 O6 72.12(6) . 2_675 ?
O8 Ho1 O7 135.53(6) . . ?
O8 Ho1 N1 80.92(6) . 1_655 ?
C1 O1 Ho1 122.00(14) . . ?
C3 O2 Ho1 120.61(15) . 2_665 ?
C6 O3 Ho1 123.71(14) . . ?
C8 O4 Ho1 120.63(14) . 2_666 ?
C11 O5 Ho1 119.34(16) . . ?
C13 O6 Ho1 118.06(15) . 2_675 ?
Ho1 O7 H7A 110.5 . . ?
Ho1 O7 H7B 110.8 . . ?
H7A O7 H7B 103.2 . . ?
Ho1 O8 H8A 110.3 . . ?
Ho1 O8 H8B 110.1 . . ?
H8A O8 H8B 103.6 . . ?
C4 N1 Ho1 128.25(16) . 1_455 ?
C5 N1 Ho1 127.91(16) . 1_455 ?
C5 N1 C4 103.0(2) . . ?
C4 N2 N3 102.6(2) . . ?
N2 N3 C2 121.38(19) . . ?
C5 N3 N2 109.69(19) . . ?
C5 N3 C2 128.9(2) . . ?
C10 N4 C9 102.5(2) . . ?
C9 N5 N6 102.4(2) . . ?
N5 N6 C7 121.88(19) . . ?
C10 N6 N5 108.96(19) . . ?
C10 N6 C7 129.1(2) . . ?
C15 N7 C14 102.9(2) . . ?
C14 N8 N9 101.9(2) . . ?
N8 N9 C12 122.8(2) . . ?
C15 N9 N8 110.1(2) . . ?
C15 N9 C12 127.0(2) . . ?
O1 C1 C2 124.5(2) . . ?
O1 C1 C3 116.1(2) . 2_665 ?
C2 C1 C3 119.4(2) . 2_665 ?
C1 C2 N3 117.4(2) . . ?
C3 C2 N3 120.6(2) . . ?
C3 C2 C1 121.9(2) . . ?
O2 C3 C1 115.0(2) . 2_665 ?
O2 C3 C2 126.5(2) . . ?
C2 C3 C1 118.5(2) . 2_665 ?
N1 C4 H4 122.8 . . ?
N2 C4 N1 114.5(2) . . ?
N2 C4 H4 122.8 . . ?
N1 C5 H5 124.9 . . ?
N3 C5 N1 110.2(2) . . ?
N3 C5 H5 124.9 . . ?
O3 C6 C7 124.4(2) . . ?
O3 C6 C8 114.86(19) . 2_666 ?
C7 C6 C8 120.69(19) . 2_666 ?
C6 C7 N6 118.80(19) . . ?
C6 C7 C8 120.1(2) . . ?
C8 C7 N6 121.06(19) . . ?
O4 C8 C6 114.73(19) . 2_666 ?
O4 C8 C7 126.2(2) . . ?
C7 C8 C6 119.10(19) . 2_666 ?
N4 C9 H9 122.3 . . ?
N5 C9 N4 115.4(2) . . ?
N5 C9 H9 122.3 . . ?
N4 C10 N6 110.8(2) . . ?
N4 C10 H10 124.6 . . ?
N6 C10 H10 124.6 . . ?
O5 C11 C12 125.8(2) . . ?
O5 C11 C13 115.1(2) . 2_675 ?
C12 C11 C13 119.1(2) . 2_675 ?
C11 C12 N9 120.4(2) . . ?
C11 C12 C13 121.2(2) . . ?
C13 C12 N9 118.3(2) . . ?
O6 C13 C11 115.3(2) . 2_675 ?
O6 C13 C12 125.1(2) . . ?
C12 C13 C11 119.6(2) . 2_675 ?
N7 C14 H14 122.6 . . ?
N8 C14 N7 114.7(2) . . ?
N8 C14 H14 122.6 . . ?
N7 C15 N9 110.4(2) . . ?
N7 C15 H15 124.8 . . ?
N9 C15 H15 124.8 . . ?
H9A O9 H9B 109.5 . . ?
H10A O10 H10B 104.5 . . ?
H11A O11 H11B 104.5 . . ?
H12A O12 H12B 104.5 . . ?
H13A O13 H13B 104.5 . . ?
H14A O14 H14B 104.5 . . ?
H15A O15 H15B 109.5 . . ?


_olex2_submission_special_instructions 'No special instructions were received'
