# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

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

data_1_Sam
_database_code_depnum_ccdc_archive 'CCDC 1054136'
_audit_update_record             
;
2019-03-14 deposited with the CCDC.	2019-03-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H26 Fe La N12 O, 7[H2O]'
_chemical_formula_sum            'C42 H26 Fe La N12 O'
_chemical_formula_weight         909.51
_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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.1602(7)
_cell_length_b                   13.2764(10)
_cell_length_c                   18.3804(10)
_cell_angle_alpha                69.305(6)
_cell_angle_beta                 86.823(5)
_cell_angle_gamma                73.400(6)
_cell_volume                     2438.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3503
_cell_measurement_temperature    293
_cell_measurement_theta_max      70.6867
_cell_measurement_theta_min      3.2731
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.132
_diffrn_reflns_theta_min         2.372
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8864
_reflns_number_total             11499
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.044
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         11499
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0525
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0679P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1465
_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:
 C4(C5,C6)
2.b Rotating group:
 O1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36)
;
_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 0.7575(5) 0.9244(4) 0.1116(3) 0.0469(12) Uani 1 1 d . . . . .
H1 H 0.724708 0.917392 0.160147 0.056 Uiso 1 1 calc R . . . .
C2 C 0.6809(5) 0.9975(4) 0.0464(4) 0.0589(16) Uani 1 1 d . . . . .
H2 H 0.599013 1.036171 0.051521 0.071 Uiso 1 1 calc R . . . .
C3 C 0.7282(6) 1.0115(5) -0.0252(4) 0.0607(17) Uani 1 1 d . . . . .
H3 H 0.678452 1.060102 -0.069677 0.073 Uiso 1 1 calc R . . . .
C4 C 0.8514(3) 0.9530(3) -0.0319(2) 0.0470(13) Uani 1 1 d . . . . .
C5 C 0.9221(4) 0.8779(3) 0.03787(19) 0.0387(11) Uani 1 1 d G . . . .
C6 C 0.9084(5) 0.9678(4) -0.10570(18) 0.0590(16) Uani 1 1 d G . . . .
H6 H 0.861633 1.017331 -0.151049 0.071 Uiso 1 1 calc R . . . .
C7 C 1.0270(6) 0.9119(5) -0.1105(3) 0.0583(15) Uani 1 1 d . . . . .
H7 H 1.062076 0.923359 -0.158838 0.070 Uiso 1 1 calc R . . . .
C8 C 1.1008(5) 0.8342(4) -0.0411(3) 0.0464(12) Uani 1 1 d . . . . .
C9 C 1.0488(5) 0.8162(4) 0.0315(3) 0.0380(11) Uani 1 1 d . . . . .
C10 C 1.2231(6) 0.7747(5) -0.0447(3) 0.0578(15) Uani 1 1 d . . . . .
H10 H 1.259744 0.784419 -0.092501 0.069 Uiso 1 1 calc R . . . .
C11 C 1.2897(5) 0.7014(5) 0.0222(3) 0.0545(14) Uani 1 1 d . . . . .
H11 H 1.372101 0.660241 0.020893 0.065 Uiso 1 1 calc R . . . .
C12 C 1.2329(5) 0.6896(4) 0.0918(3) 0.0467(12) Uani 1 1 d . . . . .
H12 H 1.280469 0.640965 0.137073 0.056 Uiso 1 1 calc R . . . .
C13 C 0.8421(5) 0.6292(4) 0.1064(3) 0.0439(12) Uani 1 1 d . . . . .
H13 H 0.789113 0.698719 0.103990 0.053 Uiso 1 1 calc R . . . .
C14 C 0.8069(6) 0.5737(5) 0.0634(4) 0.0639(17) Uani 1 1 d . . . . .
H14 H 0.732917 0.606238 0.032475 0.077 Uiso 1 1 calc R . . . .
C15 C 0.8812(6) 0.4723(5) 0.0671(4) 0.0693(18) Uani 1 1 d . . . . .
H15 H 0.858993 0.434529 0.038322 0.083 Uiso 1 1 calc R . . . .
C16 C 0.9916(5) 0.4235(5) 0.1139(4) 0.0556(15) Uani 1 1 d . . . . .
C17 C 1.0230(4) 0.4854(4) 0.1542(3) 0.0412(11) Uani 1 1 d . . . . .
C18 C 1.0737(6) 0.3138(5) 0.1224(4) 0.073(2) Uani 1 1 d . . . . .
H18 H 1.053851 0.273489 0.094766 0.088 Uiso 1 1 calc R . . . .
C19 C 1.1771(6) 0.2687(5) 0.1688(5) 0.074(2) Uani 1 1 d . . . . .
H19 H 1.226407 0.196663 0.174238 0.089 Uiso 1 1 calc R . . . .
C20 C 1.2141(5) 0.3289(4) 0.2106(4) 0.0562(15) Uani 1 1 d . . . . .
C21 C 1.1393(4) 0.4377(4) 0.2025(3) 0.0399(11) Uani 1 1 d . . . . .
C22 C 1.3196(6) 0.2841(5) 0.2606(4) 0.073(2) Uani 1 1 d . . . . .
H22 H 1.369352 0.211319 0.268728 0.087 Uiso 1 1 calc R . . . .
C23 C 1.3511(5) 0.3460(5) 0.2978(4) 0.0717(19) Uani 1 1 d . . . . .
H23 H 1.421847 0.316013 0.331413 0.086 Uiso 1 1 calc R . . . .
C24 C 1.2754(4) 0.4548(5) 0.2847(3) 0.0508(13) Uani 1 1 d . . . . .
H24 H 1.299148 0.497692 0.308653 0.061 Uiso 1 1 calc R . . . .
C25 C 0.8750(5) 0.4572(4) 0.3168(3) 0.0459(12) Uani 1 1 d . . . . .
H25 H 0.817627 0.502653 0.275240 0.055 Uiso 1 1 calc R . . . .
C26 C 0.8741(5) 0.3455(5) 0.3535(4) 0.0559(14) Uani 1 1 d . . . . .
H26 H 0.818219 0.317943 0.335815 0.067 Uiso 1 1 calc R . . . .
C27 C 0.9548(6) 0.2782(5) 0.4147(4) 0.0644(17) Uani 1 1 d . . . . .
H27 H 0.954730 0.203874 0.439706 0.077 Uiso 1 1 calc R . . . .
C28 C 1.0392(5) 0.3210(4) 0.4406(3) 0.0494(13) Uani 1 1 d . . . . .
C29 C 1.0332(4) 0.4349(4) 0.4012(3) 0.0393(11) Uani 1 1 d . . . . .
C30 C 1.1275(6) 0.2554(5) 0.5053(4) 0.0679(18) Uani 1 1 d . . . . .
H30 H 1.133348 0.179675 0.530369 0.081 Uiso 1 1 calc R . . . .
C31 C 1.2015(6) 0.3012(5) 0.5302(3) 0.0640(17) Uani 1 1 d . . . . .
H31 H 1.257394 0.257015 0.572708 0.077 Uiso 1 1 calc R . . . .
C32 C 1.1964(5) 0.4146(5) 0.4932(3) 0.0498(13) Uani 1 1 d . . . . .
C33 C 1.1132(4) 0.4835(4) 0.4279(3) 0.0365(10) Uani 1 1 d . . . . .
C34 C 1.2714(5) 0.4669(5) 0.5185(3) 0.0606(16) Uani 1 1 d . . . . .
H34 H 1.328768 0.424937 0.560549 0.073 Uiso 1 1 calc R . . . .
C35 C 1.2603(6) 0.5773(5) 0.4819(3) 0.0590(15) Uani 1 1 d . . . . .
H35 H 1.307021 0.612520 0.499779 0.071 Uiso 1 1 calc R . . . .
C36 C 1.1777(5) 0.6373(5) 0.4172(3) 0.0499(13) Uani 1 1 d . . . . .
H36 H 1.171963 0.712926 0.391967 0.060 Uiso 1 1 calc R . . . .
C37 C 1.3117(4) 0.7564(4) 0.2472(3) 0.0337(10) Uani 1 1 d . . . . .
C38 C 1.5233(4) 0.5881(4) 0.3027(3) 0.0436(12) Uani 1 1 d . . . . .
C39 C 1.4584(4) 0.7636(4) 0.3581(3) 0.0412(11) Uani 1 1 d . . . . .
C40 C 0.6608(4) 0.7356(4) 0.2641(3) 0.0332(10) Uani 1 1 d . . . . .
C41 C 1.4499(4) 0.9142(4) 0.2136(3) 0.0400(11) Uani 1 1 d . . . . .
C42 C 1.5111(4) 0.7480(4) 0.1511(3) 0.0396(11) Uani 1 1 d . . . . .
N1 N 0.8743(3) 0.8637(3) 0.1096(2) 0.0385(9) Uani 1 1 d . . . . .
N2 N 1.1152(3) 0.7425(3) 0.0988(2) 0.0387(9) Uani 1 1 d . . . . .
N3 N 0.9475(3) 0.5885(3) 0.1508(2) 0.0372(9) Uani 1 1 d . . . . .
N4 N 1.1711(3) 0.5001(3) 0.2396(2) 0.0393(9) Uani 1 1 d . . . . .
N5 N 0.9527(3) 0.5016(3) 0.3377(2) 0.0378(9) Uani 1 1 d . . . . .
N6 N 1.1067(4) 0.5932(3) 0.3890(2) 0.0432(10) Uani 1 1 d . . . . .
N7 N 1.2105(4) 0.7526(4) 0.2441(2) 0.0427(10) Uani 1 1 d . . . . .
N8 N 1.5296(4) 0.7487(4) 0.0894(3) 0.0597(13) Uani 1 1 d . . . . .
N9 N 1.5489(5) 0.4926(4) 0.3309(3) 0.0663(15) Uani 1 1 d . . . . .
N10 N 1.4433(5) 0.7733(5) 0.4169(3) 0.0702(15) Uani 1 1 d . . . . .
N11 N 0.7667(3) 0.7253(3) 0.2648(2) 0.0415(10) Uani 1 1 d . . . . .
N12 N 1.4322(5) 1.0091(4) 0.1883(3) 0.0685(15) Uani 1 1 d . . . . .
O1 O 0.9328(4) 0.8572(3) 0.2863(2) 0.0530(9) Uani 1 1 d . . . . .
H1A H 0.852486 0.883168 0.281223 0.079 Uiso 1 1 d GR . . . .
H1B H 0.958744 0.912138 0.256202 0.079 Uiso 1 1 d GR . . . .
Fe1 Fe 1.48471(5) 0.75093(5) 0.25589(4) 0.03081(15) Uani 1 1 d . . . . .
La1 La 1.00433(2) 0.69431(2) 0.23939(2) 0.03037(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.388(7) . ?
C1 N1 1.328(6) . ?
C2 C3 1.360(9) . ?
C3 C4 1.396(7) . ?
C4 C5 1.4211 . ?
C4 C6 1.4396 . ?
C5 C9 1.440(6) . ?
C5 N1 1.365(5) . ?
C6 C7 1.335(8) . ?
C7 C8 1.439(7) . ?
C8 C9 1.394(7) . ?
C8 C10 1.379(7) . ?
C9 N2 1.368(6) . ?
C10 C11 1.363(8) . ?
C11 C12 1.372(7) . ?
C12 N2 1.325(6) . ?
C13 C14 1.392(7) . ?
C13 N3 1.332(6) . ?
C14 C15 1.345(8) . ?
C15 C16 1.395(7) . ?
C16 C17 1.403(7) . ?
C16 C18 1.442(8) . ?
C17 C21 1.461(6) . ?
C17 N3 1.369(6) . ?
C18 C19 1.331(9) . ?
C19 C20 1.435(9) . ?
C20 C21 1.406(6) . ?
C20 C22 1.385(8) . ?
C21 N4 1.368(6) . ?
C22 C23 1.362(9) . ?
C23 C24 1.392(7) . ?
C24 N4 1.326(6) . ?
C25 C26 1.398(7) . ?
C25 N5 1.318(6) . ?
C26 C27 1.349(8) . ?
C27 C28 1.408(8) . ?
C28 C29 1.410(7) . ?
C28 C30 1.432(8) . ?
C29 C33 1.434(7) . ?
C29 N5 1.373(6) . ?
C30 C31 1.337(9) . ?
C31 C32 1.401(8) . ?
C32 C33 1.415(6) . ?
C32 C34 1.415(8) . ?
C33 N6 1.359(6) . ?
C34 C35 1.351(9) . ?
C35 C36 1.390(7) . ?
C36 N6 1.328(6) . ?
C37 N7 1.151(6) . ?
C37 Fe1 1.924(4) . ?
C38 N9 1.142(6) . ?
C38 Fe1 1.947(5) . ?
C39 N10 1.131(6) . ?
C39 Fe1 1.943(5) . ?
C40 N11 1.151(5) . ?
C40 Fe1 1.926(4) 1_455 ?
C41 N12 1.139(6) . ?
C41 Fe1 1.953(5) . ?
C42 N8 1.139(6) . ?
C42 Fe1 1.944(5) . ?
N1 La1 2.753(4) . ?
N2 La1 2.747(4) . ?
N3 La1 2.696(4) . ?
N4 La1 2.714(4) . ?
N5 La1 2.757(4) . ?
N6 La1 2.745(4) . ?
N7 La1 2.643(4) . ?
N11 La1 2.607(4) . ?
O1 La1 2.513(3) . ?

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
N1 C1 C2 124.8(5) . . ?
C3 C2 C1 118.6(5) . . ?
C2 C3 C4 119.9(5) . . ?
C3 C4 C5 117.6(4) . . ?
C3 C4 C6 122.6(4) . . ?
C5 C4 C6 119.8 . . ?
C4 C5 C9 118.0(3) . . ?
N1 C5 C4 122.3(3) . . ?
N1 C5 C9 119.7(3) . . ?
C7 C6 C4 121.5(3) . . ?
C6 C7 C8 120.2(5) . . ?
C9 C8 C7 120.2(5) . . ?
C10 C8 C7 121.2(5) . . ?
C10 C8 C9 118.5(5) . . ?
C8 C9 C5 120.3(4) . . ?
N2 C9 C5 117.5(4) . . ?
N2 C9 C8 122.2(5) . . ?
C11 C10 C8 119.4(5) . . ?
C10 C11 C12 118.8(5) . . ?
N2 C12 C11 124.6(5) . . ?
N3 C13 C14 123.7(5) . . ?
C15 C14 C13 119.1(5) . . ?
C14 C15 C16 120.2(5) . . ?
C15 C16 C17 117.7(5) . . ?
C15 C16 C18 123.1(5) . . ?
C17 C16 C18 119.2(5) . . ?
C16 C17 C21 119.0(4) . . ?
N3 C17 C16 122.3(4) . . ?
N3 C17 C21 118.6(4) . . ?
C19 C18 C16 121.6(6) . . ?
C18 C19 C20 121.4(5) . . ?
C21 C20 C19 119.3(5) . . ?
C22 C20 C19 123.1(5) . . ?
C22 C20 C21 117.6(5) . . ?
C20 C21 C17 119.4(4) . . ?
N4 C21 C17 118.7(4) . . ?
N4 C21 C20 121.9(4) . . ?
C23 C22 C20 120.4(5) . . ?
C22 C23 C24 118.9(5) . . ?
N4 C24 C23 123.0(5) . . ?
N5 C25 C26 123.7(5) . . ?
C27 C26 C25 119.4(5) . . ?
C26 C27 C28 119.7(5) . . ?
C27 C28 C29 117.5(5) . . ?
C27 C28 C30 123.2(5) . . ?
C29 C28 C30 119.3(5) . . ?
C28 C29 C33 119.4(4) . . ?
N5 C29 C28 122.1(5) . . ?
N5 C29 C33 118.5(4) . . ?
C31 C30 C28 121.0(5) . . ?
C30 C31 C32 121.1(5) . . ?
C31 C32 C33 120.7(5) . . ?
C31 C32 C34 123.0(5) . . ?
C34 C32 C33 116.3(5) . . ?
C32 C33 C29 118.4(4) . . ?
N6 C33 C29 118.6(4) . . ?
N6 C33 C32 123.0(5) . . ?
C35 C34 C32 120.5(5) . . ?
C34 C35 C36 118.8(5) . . ?
N6 C36 C35 124.1(5) . . ?
N7 C37 Fe1 175.8(4) . . ?
N9 C38 Fe1 178.2(5) . . ?
N10 C39 Fe1 178.5(5) . . ?
N11 C40 Fe1 175.8(4) . 1_455 ?
N12 C41 Fe1 178.5(5) . . ?
N8 C42 Fe1 177.4(5) . . ?
C1 N1 C5 116.7(4) . . ?
C1 N1 La1 122.5(3) . . ?
C5 N1 La1 120.2(3) . . ?
C9 N2 La1 121.5(3) . . ?
C12 N2 C9 116.4(4) . . ?
C12 N2 La1 121.8(3) . . ?
C13 N3 C17 117.0(4) . . ?
C13 N3 La1 122.3(3) . . ?
C17 N3 La1 120.6(3) . . ?
C21 N4 La1 119.8(3) . . ?
C24 N4 C21 118.0(4) . . ?
C24 N4 La1 121.4(3) . . ?
C25 N5 C29 117.5(4) . . ?
C25 N5 La1 122.3(3) . . ?
C29 N5 La1 118.0(3) . . ?
C33 N6 La1 118.9(3) . . ?
C36 N6 C33 117.3(4) . . ?
C36 N6 La1 121.6(3) . . ?
C37 N7 La1 166.4(4) . . ?
C40 N11 La1 168.1(4) . . ?
C37 Fe1 C38 88.14(19) . . ?
C37 Fe1 C39 89.7(2) . . ?
C37 Fe1 C40 176.19(18) . 1_655 ?
C37 Fe1 C41 93.47(19) . . ?
C37 Fe1 C42 91.23(19) . . ?
C38 Fe1 C41 177.1(2) . . ?
C39 Fe1 C38 90.4(2) . . ?
C39 Fe1 C41 87.2(2) . . ?
C39 Fe1 C42 176.4(2) . . ?
C40 Fe1 C38 88.51(18) 1_655 . ?
C40 Fe1 C39 92.2(2) 1_655 . ?
C40 Fe1 C41 89.96(19) 1_655 . ?
C40 Fe1 C42 87.14(19) 1_655 . ?
C42 Fe1 C38 93.1(2) . . ?
C42 Fe1 C41 89.3(2) . . ?
N1 La1 N5 131.32(11) . . ?
N2 La1 N1 59.97(11) . . ?
N2 La1 N5 132.08(12) . . ?
N3 La1 N1 74.97(11) . . ?
N3 La1 N2 67.76(12) . . ?
N3 La1 N4 61.69(11) . . ?
N3 La1 N5 72.15(12) . . ?
N3 La1 N6 125.77(12) . . ?
N4 La1 N1 125.26(12) . . ?
N4 La1 N2 73.13(12) . . ?
N4 La1 N5 65.26(12) . . ?
N4 La1 N6 75.88(12) . . ?
N6 La1 N1 157.88(12) . . ?
N6 La1 N2 130.97(12) . . ?
N6 La1 N5 59.74(11) . . ?
N7 La1 N1 102.24(12) . . ?
N7 La1 N2 67.29(12) . . ?
N7 La1 N3 128.65(12) . . ?
N7 La1 N4 82.49(12) . . ?
N7 La1 N5 126.30(12) . . ?
N7 La1 N6 71.81(13) . . ?
N11 La1 N1 72.78(12) . . ?
N11 La1 N2 128.14(12) . . ?
N11 La1 N3 81.07(12) . . ?
N11 La1 N4 126.42(12) . . ?
N11 La1 N5 67.51(11) . . ?
N11 La1 N6 100.82(13) . . ?
N11 La1 N7 148.47(13) . . ?
O1 La1 N1 77.88(12) . . ?
O1 La1 N2 114.13(12) . . ?
O1 La1 N3 146.35(11) . . ?
O1 La1 N4 151.90(12) . . ?
O1 La1 N5 113.78(12) . . ?
O1 La1 N6 80.01(12) . . ?
O1 La1 N7 76.39(13) . . ?
O1 La1 N11 72.12(13) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.083 0.393 -0.893 772.2 134.5 '7 H2O'

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT420_1_Sam               
;
PROBLEM: D-H Without Acceptor O1 --H1A . Please Check
RESPONSE: This is due to the fact that a mask has been used to determine
how many disordered water molecules we have.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_sam_2
_database_code_depnum_ccdc_archive 'CCDC 1054137'
_audit_update_record             
;
2019-03-14 deposited with the CCDC.	2019-03-18 downloaded from the CCDC.
;
_audit_creation_date             2019-02-28
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.02.04 svn.r3569 for OlexSys, GUI svn.r5585)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H40 Dy2 Fe2 N20 O4), 8(H2 O)'
_chemical_formula_sum            'C30 H36 Dy Fe N10 O10'
_chemical_formula_weight         915.04
_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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.7750(13)
_cell_length_b                   12.0537(7)
_cell_length_c                   14.8403(11)
_cell_angle_alpha                90
_cell_angle_beta                 116.610(8)
_cell_angle_gamma                90
_cell_volume                     3802.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2642
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6351
_cell_measurement_theta_min      3.3292
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7723
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.439
_diffrn_reflns_theta_min         4.160
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2942
_reflns_number_total             3578
_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
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_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-2013 (Sheldrick, 2013)'
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0587
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0398P)²+30.3102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1501
_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:
 Fe1(Dy1,O1W,H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
2.b Rotating group:
 O1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)
;
_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
C1 C 0.3917(4) 0.3665(7) 0.3398(6) 0.0488(19) Uani 1 1 d . . . . .
H1 H 0.381921 0.292983 0.319876 0.059 Uiso 1 1 calc R . . . .
C2 C 0.3518(4) 0.4258(8) 0.3686(7) 0.056(2) Uani 1 1 d . . . . .
H2 H 0.317091 0.391045 0.369430 0.067 Uiso 1 1 calc R . . . .
C3 C 0.3637(4) 0.5337(8) 0.3952(6) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.336628 0.574027 0.412652 0.064 Uiso 1 1 calc R . . . .
C4 C 0.4178(4) 0.5851(7) 0.3963(6) 0.0478(19) Uani 1 1 d . . . . .
C5 C 0.4568(3) 0.5182(7) 0.3708(5) 0.0413(17) Uani 1 1 d . . . . .
C6 C 0.4331(4) 0.6987(8) 0.4216(6) 0.057(2) Uani 1 1 d . . . . .
H6 H 0.407010 0.742245 0.438688 0.068 Uiso 1 1 calc R . . . .
C7 C 0.4843(4) 0.7439(7) 0.4210(7) 0.059(2) Uani 1 1 d . . . . .
H7 H 0.492513 0.818972 0.435312 0.071 Uiso 1 1 calc R . . . .
C8 C 0.5271(4) 0.6778(7) 0.3986(6) 0.0508(19) Uani 1 1 d . . . . .
C9 C 0.5133(3) 0.5656(6) 0.3741(5) 0.0405(17) Uani 1 1 d . . . . .
C10 C 0.5828(4) 0.7203(8) 0.4019(7) 0.061(2) Uani 1 1 d . . . . .
H10 H 0.592736 0.794942 0.415897 0.074 Uiso 1 1 calc R . . . .
C11 C 0.6225(4) 0.6512(8) 0.3842(7) 0.058(2) Uani 1 1 d . . . . .
H11 H 0.660196 0.677391 0.387786 0.070 Uiso 1 1 calc R . . . .
C12 C 0.6050(3) 0.5414(7) 0.3611(6) 0.0462(18) Uani 1 1 d . . . . .
H12 H 0.632630 0.494809 0.350360 0.055 Uiso 1 1 calc R . . . .
C13 C 0.6603(3) 0.2643(6) 0.4154(5) 0.0386(16) Uani 1 1 d . . . . .
C14 C 0.7621(4) 0.2591(7) 0.3786(6) 0.050(2) Uani 1 1 d . . . . .
C15 C 0.7597(3) 0.4102(7) 0.5112(5) 0.0429(18) Uani 1 1 d . . . . .
N1 N 0.4433(3) 0.4106(6) 0.3396(5) 0.0435(15) Uani 1 1 d . . . . .
N2 N 0.5520(3) 0.4980(5) 0.3530(4) 0.0403(14) Uani 1 1 d . . . . .
N3 N 0.6078(3) 0.2726(5) 0.3625(5) 0.0467(16) Uani 1 1 d . . . . .
N4 N 0.7699(4) 0.2649(8) 0.3080(6) 0.072(2) Uani 1 1 d . . . . .
N5 N 0.7672(4) 0.5045(7) 0.5165(7) 0.072(2) Uani 1 1 d . . . . .
O1 O 0.5111(3) 0.1749(5) 0.1579(4) 0.0532(14) Uani 1 1 d . . . . .
H1A H 0.491251 0.115146 0.163322 0.080 Uiso 1 1 d GR . . . .
H1B H 0.550660 0.152639 0.183915 0.080 Uiso 1 1 d GR . . . .
Fe1 Fe 0.750000 0.250000 0.500000 0.0387(4) Uani 1 2 d S T P . .
Dy1 Dy 0.50000(6) 0.32387(5) 0.2500(4) 0.0378(2) Uani 1 2 d GS T P . .
O1W O 0.5823(3) -0.0329(7) -0.0445(3) 0.107(3) Uani 1 1 d G . . . .
H1WA H 0.577846 0.003298 -0.096403 0.161 Uiso 1 1 d G . . . .
H1WB H 0.585617 0.016476 -0.001562 0.161 Uiso 1 1 d G . . . .
O2W O 0.7022(4) 0.1569(9) 0.1151(7) 0.110(3) Uani 1 1 d . . . . .
H2WA H 0.727952 0.143087 0.175915 0.166 Uiso 1 1 d G . . . .
H2WB H 0.713890 0.114855 0.080563 0.166 Uiso 1 1 d G . . . .
O3W O 0.6064(4) 0.0605(9) 0.1451(7) 0.102(3) Uani 1 1 d . . . . .
H3WA H 0.640510 0.072059 0.141209 0.152 Uiso 1 1 d G . . . .
H3WB H 0.617053 0.019794 0.196988 0.152 Uiso 1 1 d G . . . .
O4W O 0.6611(4) -0.1095(10) 0.2838(8) 0.114(3) Uani 1 1 d . . . . .
H4WA H 0.686319 -0.075154 0.336525 0.172 Uiso 1 1 d G . . . .
H4WB H 0.681750 -0.139754 0.256082 0.172 Uiso 1 1 d G . . . .


_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 H1 0.9300 . ?
C1 C2 1.400(11) . ?
C1 N1 1.338(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.352(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.422(11) . ?
C4 C5 1.404(10) . ?
C4 C6 1.423(12) . ?
C5 C9 1.441(10) . ?
C5 N1 1.366(10) . ?
C6 H6 0.9300 . ?
C6 C7 1.338(12) . ?
C7 H7 0.9300 . ?
C7 C8 1.443(11) . ?
C8 C9 1.401(11) . ?
C8 C10 1.399(12) . ?
C9 N2 1.365(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.368(12) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(11) . ?
C12 H12 0.9300 . ?
C12 N2 1.320(9) . ?
C13 N3 1.142(9) . ?
C13 Fe1 1.939(7) . ?
C14 N4 1.144(10) . ?
C14 Fe1 1.951(8) . ?
C15 N5 1.149(10) . ?
C15 Fe1 1.943(9) . ?
N1 Dy1 2.506(8) . ?
N2 Dy1 2.565(6) . ?
N3 Dy1 2.430(6) . ?
O1 H1A 0.8851 . ?
O1 H1B 0.8831 . ?
O1 Dy1 2.342(7) . ?
O1W H1WA 0.8497 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8496 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.8502 . ?
O4W H4WB 0.8500 . ?

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 H1 118.5 . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(8) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.5(8) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C6 123.0(8) . . ?
C5 C4 C3 116.8(8) . . ?
C5 C4 C6 120.2(8) . . ?
C4 C5 C9 118.8(7) . . ?
N1 C5 C4 123.6(7) . . ?
N1 C5 C9 117.5(6) . . ?
C4 C6 H6 119.5 . . ?
C7 C6 C4 121.0(8) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.0(8) . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 119.1(7) . . ?
C10 C8 C7 122.9(8) . . ?
C10 C8 C9 118.0(8) . . ?
C8 C9 C5 119.9(7) . . ?
N2 C9 C5 118.0(7) . . ?
N2 C9 C8 122.2(7) . . ?
C8 C10 H10 120.2 . . ?
C11 C10 C8 119.5(8) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.9 . . ?
C10 C11 C12 118.3(8) . . ?
C12 C11 H11 120.9 . . ?
C11 C12 H12 117.6 . . ?
N2 C12 C11 124.7(8) . . ?
N2 C12 H12 117.6 . . ?
N3 C13 Fe1 177.5(7) . . ?
N4 C14 Fe1 179.2(9) . . ?
N5 C15 Fe1 177.4(8) . . ?
C1 N1 C5 116.9(7) . . ?
C1 N1 Dy1 123.2(5) . . ?
C5 N1 Dy1 118.4(4) . . ?
C9 N2 Dy1 115.5(4) . . ?
C12 N2 C9 117.2(7) . . ?
C12 N2 Dy1 124.3(5) . . ?
C13 N3 Dy1 170.2(6) . . ?
H1A O1 H1B 102.7 . . ?
Dy1 O1 H1A 111.5 . . ?
Dy1 O1 H1B 110.7 . . ?
C13 Fe1 C13 180.0 . 7_656 ?
C13 Fe1 C14 91.6(3) 7_656 . ?
C13 Fe1 C14 91.7(3) . 7_656 ?
C13 Fe1 C14 88.4(3) . . ?
C13 Fe1 C14 88.4(3) 7_656 7_656 ?
C13 Fe1 C15 88.8(3) . 7_656 ?
C13 Fe1 C15 91.2(3) . . ?
C13 Fe1 C15 88.8(3) 7_656 . ?
C13 Fe1 C15 91.2(3) 7_656 7_656 ?
C14 Fe1 C14 180.0 . 7_656 ?
C15 Fe1 C14 87.9(3) 7_656 7_656 ?
C15 Fe1 C14 92.1(3) 7_656 . ?
C15 Fe1 C14 92.1(3) . 7_656 ?
C15 Fe1 C14 87.9(3) . . ?
C15 Fe1 C15 180.0 7_656 . ?
N1 Dy1 N1 130.7(3) . 2_655 ?
N1 Dy1 N2 64.7(2) 2_655 2_655 ?
N1 Dy1 N2 75.2(2) . 2_655 ?
N1 Dy1 N2 75.2(2) 2_655 . ?
N1 Dy1 N2 64.7(2) . . ?
N2 Dy1 N2 70.2(3) . 2_655 ?
N3 Dy1 N1 79.5(2) 2_655 . ?
N3 Dy1 N1 113.2(3) 2_655 2_655 ?
N3 Dy1 N1 79.5(2) . 2_655 ?
N3 Dy1 N1 113.2(3) . . ?
N3 Dy1 N2 73.7(2) . . ?
N3 Dy1 N2 134.1(2) . 2_655 ?
N3 Dy1 N2 73.7(2) 2_655 2_655 ?
N3 Dy1 N2 134.1(2) 2_655 . ?
N3 Dy1 N3 150.5(3) . 2_655 ?
O1 Dy1 N1 149.0(2) 2_655 2_655 ?
O1 Dy1 N1 149.0(2) . . ?
O1 Dy1 N1 77.4(3) 2_655 . ?
O1 Dy1 N1 77.4(3) . 2_655 ?
O1 Dy1 N2 115.4(3) 2_655 . ?
O1 Dy1 N2 145.6(3) . . ?
O1 Dy1 N2 115.4(3) . 2_655 ?
O1 Dy1 N2 145.6(2) 2_655 2_655 ?
O1 Dy1 N3 81.1(2) . . ?
O1 Dy1 N3 81.1(2) 2_655 2_655 ?
O1 Dy1 N3 76.4(2) . 2_655 ?
O1 Dy1 N3 76.4(2) 2_655 . ?
O1 Dy1 O1 79.9(3) 2_655 . ?
H1WA O1W H1WB 104.6 . . ?
H2WA O2W H2WB 104.5 . . ?
H3WA O3W H3WB 104.5 . . ?
H4WA O4W H4WB 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O1W 0.89 2.09 2.711(6) 125.9 5_655 yes
O1 H1B O3W 0.88 2.00 2.731(9) 139.1 . yes
O1W H1WB O3W 0.85 2.07 2.841(10) 149.9 . yes
O2W H2WA N4 0.85 2.29 2.890(13) 127.9 . yes
O3W H3WA O2W 0.85 1.96 2.766(15) 156.7 . yes
O3W H3WB O4W 0.85 1.99 2.780(16) 153.3 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.7(13) . . . . ?
C2 C1 N1 C5 1.0(11) . . . . ?
C2 C1 N1 Dy1 -164.5(6) . . . . ?
C2 C3 C4 C5 -1.1(11) . . . . ?
C2 C3 C4 C6 178.8(8) . . . . ?
C3 C4 C5 C9 -178.0(7) . . . . ?
C3 C4 C5 N1 4.2(11) . . . . ?
C3 C4 C6 C7 -179.6(8) . . . . ?
C4 C5 C9 C8 -2.5(11) . . . . ?
C4 C5 C9 N2 177.3(6) . . . . ?
C4 C5 N1 C1 -4.1(11) . . . . ?
C4 C5 N1 Dy1 162.1(6) . . . . ?
C4 C6 C7 C8 -2.4(14) . . . . ?
C5 C4 C6 C7 0.3(13) . . . . ?
C5 C9 N2 C12 -176.9(6) . . . . ?
C5 C9 N2 Dy1 21.8(8) . . . . ?
C6 C4 C5 C9 2.1(11) . . . . ?
C6 C4 C5 N1 -175.7(7) . . . . ?
C6 C7 C8 C9 2.0(13) . . . . ?
C6 C7 C8 C10 -176.9(9) . . . . ?
C7 C8 C9 C5 0.5(11) . . . . ?
C7 C8 C9 N2 -179.3(7) . . . . ?
C7 C8 C10 C11 176.9(8) . . . . ?
C8 C9 N2 C12 3.0(10) . . . . ?
C8 C9 N2 Dy1 -158.3(6) . . . . ?
C8 C10 C11 C12 1.7(13) . . . . ?
C9 C5 N1 C1 178.0(7) . . . . ?
C9 C5 N1 Dy1 -15.7(8) . . . . ?
C9 C8 C10 C11 -1.9(13) . . . . ?
C10 C8 C9 C5 179.4(7) . . . . ?
C10 C8 C9 N2 -0.4(12) . . . . ?
C10 C11 C12 N2 1.1(13) . . . . ?
C11 C12 N2 C9 -3.4(11) . . . . ?
C11 C12 N2 Dy1 156.1(7) . . . . ?
N1 C1 C2 C3 1.9(13) . . . . ?
N1 C5 C9 C8 175.5(7) . . . . ?
N1 C5 C9 N2 -4.7(10) . . . . ?

_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_4
_database_code_depnum_ccdc_archive 'CCDC 1054139'
_audit_update_record             
;
2019-03-14 deposited with the CCDC.	2019-03-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C60 H32 Fe2 N20 O4 Yb2), 6(H2 O), 1[(H2O)]'
_chemical_formula_sum            'C30 H28 Fe N10 O8 Yb'
_chemical_formula_weight         885.51
_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'
Fe Fe 0.3463 0.8444 '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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.4860(6)
_cell_length_b                   12.2600(4)
_cell_length_c                   15.1580(7)
_cell_angle_alpha                90
_cell_angle_beta                 117.168(7)
_cell_angle_gamma                90
_cell_volume                     3883.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2498
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2333
_cell_measurement_theta_min      2.7031
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_unetI/netI     0.1379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16512
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.298
_diffrn_reflns_theta_min         2.709
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2667
_reflns_number_total             4740
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.586
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0748
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0971P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.2110
_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. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(O1W) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(O3W) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
3. Rigid body (RIGU) restrains
 O2W, H2WB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 O1W(H1WA,H1WB,O2W,H2WA,H2WB,O3W,H3WA,H3WB)
4.b Rotating group:
 O1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C10(H10), C11(H11), C12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1115(5) 0.3629(9) -0.1709(8) 0.062(3) Uani 1 1 d . . . . .
H1 H -0.120484 0.290826 -0.191777 0.074 Uiso 1 1 calc R . . . .
C2 C -0.1540(5) 0.4197(9) -0.1430(8) 0.064(3) Uani 1 1 d . . . . .
H2 H -0.190450 0.385690 -0.146862 0.077 Uiso 1 1 calc R . . . .
C3 C -0.1401(5) 0.5243(10) -0.1107(8) 0.066(3) Uani 1 1 d . . . . .
H3 H -0.167286 0.563139 -0.092826 0.079 Uiso 1 1 calc R . . . .
C4 C -0.0836(5) 0.5741(9) -0.1046(7) 0.056(3) Uani 1 1 d . . . . .
C5 C -0.0448(4) 0.5100(8) -0.1336(7) 0.048(2) Uani 1 1 d . . . . .
C6 C -0.0664(6) 0.6837(9) -0.0713(8) 0.064(3) Uani 1 1 d . . . . .
C7 C -0.0128(5) 0.7301(10) -0.0652(8) 0.067(3) Uani 1 1 d . . . . .
C8 C 0.0289(5) 0.6676(7) -0.0906(8) 0.051(2) Uani 1 1 d . . . . .
C9 C 0.0138(4) 0.5587(8) -0.1256(6) 0.047(2) Uani 1 1 d . . . . .
C10 C 0.0863(5) 0.7090(10) -0.0842(8) 0.065(3) Uani 1 1 d . . . . .
H10 H 0.097509 0.781209 -0.065655 0.078 Uiso 1 1 calc R . . . .
C11 C 0.1256(6) 0.6446(9) -0.1049(9) 0.066(3) Uani 1 1 d . . . . .
H11 H 0.164309 0.671074 -0.098900 0.079 Uiso 1 1 calc R . . . .
C12 C 0.1063(4) 0.5370(8) -0.1356(7) 0.051(2) Uani 1 1 d . . . . .
H12 H 0.134552 0.492916 -0.146916 0.061 Uiso 1 1 calc R . . . .
C14 C 0.2409(4) 0.0953(8) -0.0036(7) 0.046(2) Uani 1 1 d . . . . .
C15 C 0.2389(5) 0.2511(10) 0.1176(9) 0.068(3) Uani 1 1 d . . . . .
C13 C 0.1592(4) 0.2658(7) -0.0851(6) 0.041(2) Uani 1 1 d . . . . .
N1 N -0.0600(3) 0.4092(6) -0.1680(5) 0.0461(18) Uani 1 1 d . . . . .
N2 N 0.0515(3) 0.4932(6) -0.1497(5) 0.0444(18) Uani 1 1 d . . . . .
N5 N 0.2318(5) 0.2514(11) 0.1883(8) 0.101(4) Uani 1 1 d . . . . .
N3 N 0.1060(3) 0.2757(7) -0.1370(6) 0.0514(19) Uani 1 1 d . . . . .
N4 N 0.2297(5) 0.0009(10) -0.0049(10) 0.099(4) Uani 1 1 d . . . . .
Fe1 Fe 0.250000 0.250000 0.000000 0.0451(5) Uani 1 2 d S T P . .
Yb1 Yb 0.000000 0.32661(4) -0.250000 0.0439(2) Uani 1 2 d S T P . .
O1 O -0.0106(3) 0.1799(4) -0.1623(6) 0.0569(18) Uani 1 1 d . . . . .
H1A H -0.048520 0.178608 -0.168722 0.085 Uiso 1 1 d GR . . . .
H1B H 0.012928 0.190216 -0.100627 0.085 Uiso 1 1 d GR . . . .
O1W O 0.2002(4) -0.1582(7) 0.1122(8) 0.123(4) Uani 1 1 d . U . . .
H1WA H 0.209474 -0.091029 0.124379 0.184 Uiso 1 1 d G . . . .
H1WB H 0.232724 -0.196809 0.147971 0.184 Uiso 1 1 d G . . . .
O2W O 0.0790(3) 0.0366(6) -0.0386(7) 0.135(4) Uani 1 1 d G U . . .
H2WA H 0.099567 0.024020 -0.071404 0.202 Uiso 1 1 d G . . . .
H2WB H 0.086606 0.103191 -0.021927 0.202 Uiso 1 1 d G U . . .
O3W O -0.1081(3) 0.0643(8) -0.1515(7) 0.122(3) Uani 1 1 d G U . A 1
H3WA H -0.104264 -0.003328 -0.160324 0.184 Uiso 1 1 d G . . B 1
H3WB H -0.103396 0.068402 -0.092636 0.184 Uiso 1 1 d G . . C 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 H1 0.9300 . ?
C1 C2 1.430(14) . ?
C1 N1 1.318(12) . ?
C2 H2 0.9300 . ?
C2 C3 1.358(15) . ?
C3 H3 0.9300 . ?
C3 C4 1.426(14) . ?
C4 C5 1.415(13) . ?
C4 C6 1.428(14) . ?
C5 C9 1.455(12) . ?
C5 N1 1.325(11) . ?
C6 C7 1.345(15) . ?
C7 C8 1.428(14) . ?
C8 C9 1.422(13) . ?
C8 C10 1.401(14) . ?
C9 N2 1.361(11) . ?
C10 H10 0.9300 . ?
C10 C11 1.355(15) . ?
C11 H11 0.9300 . ?
C11 C12 1.403(14) . ?
C12 H12 0.9300 . ?
C12 N2 1.320(10) . ?
C14 N4 1.185(13) . ?
C14 Fe1 1.907(10) . ?
C15 N5 1.157(14) . ?
C15 Fe1 1.916(13) . ?
C13 N3 1.140(10) . ?
C13 Fe1 1.933(8) . ?
N1 Yb1 2.482(7) . ?
N2 Yb1 2.503(7) . ?
N3 Yb1 2.371(7) . ?
Yb1 O1 2.317(6) 2_554 ?
Yb1 O1 2.317(6) . ?
Yb1 H1A 2.7186 . ?
Yb1 H1B 2.7180 . ?
O1 H1A 0.8504 . ?
O1 H1B 0.8502 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8508 . ?
O2W H2WA 0.8515 . ?
O2W H2WB 0.8496 . ?
O3W H3WA 0.8506 . ?
O3W H3WB 0.8496 . ?

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 H1 118.9 . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.2(10) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.8(9) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(9) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C6 122.0(9) . . ?
C5 C4 C3 117.0(10) . . ?
C5 C4 C6 121.0(10) . . ?
C4 C5 C9 117.7(9) . . ?
N1 C5 C4 123.0(9) . . ?
N1 C5 C9 119.3(8) . . ?
C7 C6 C4 121.8(9) . . ?
C6 C7 C8 119.3(10) . . ?
C9 C8 C7 121.3(9) . . ?
C10 C8 C7 123.0(9) . . ?
C10 C8 C9 115.7(9) . . ?
C8 C9 C5 118.8(8) . . ?
N2 C9 C5 116.2(8) . . ?
N2 C9 C8 124.9(8) . . ?
C8 C10 H10 119.7 . . ?
C11 C10 C8 120.6(10) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.9 . . ?
C10 C11 C12 118.3(10) . . ?
C12 C11 H11 120.9 . . ?
C11 C12 H12 117.3 . . ?
N2 C12 C11 125.4(9) . . ?
N2 C12 H12 117.3 . . ?
N4 C14 Fe1 173.3(9) . . ?
N5 C15 Fe1 179.6(13) . . ?
N3 C13 Fe1 178.4(8) . . ?
C1 N1 C5 119.5(8) . . ?
C1 N1 Yb1 122.0(7) . . ?
C5 N1 Yb1 117.7(6) . . ?
C9 N2 Yb1 116.8(5) . . ?
C12 N2 C9 115.0(8) . . ?
C12 N2 Yb1 126.5(6) . . ?
C13 N3 Yb1 170.2(8) . . ?
C14 Fe1 C14 180.0 . 7 ?
C14 Fe1 C15 91.6(5) . 7 ?
C14 Fe1 C15 88.4(5) 7 7 ?
C14 Fe1 C15 91.6(5) 7 . ?
C14 Fe1 C15 88.4(5) . . ?
C14 Fe1 C13 89.7(4) . 7 ?
C14 Fe1 C13 90.3(4) . . ?
C14 Fe1 C13 90.3(4) 7 7 ?
C14 Fe1 C13 89.7(4) 7 . ?
C15 Fe1 C15 180.0 . 7 ?
C15 Fe1 C13 87.5(4) 7 . ?
C15 Fe1 C13 92.5(4) 7 7 ?
C15 Fe1 C13 87.5(4) . 7 ?
C15 Fe1 C13 92.5(4) . . ?
C13 Fe1 C13 180.0 7 . ?
N1 Yb1 N1 131.8(3) 2_554 . ?
N1 Yb1 N2 65.8(2) 2_554 2_554 ?
N1 Yb1 N2 65.8(2) . . ?
N1 Yb1 N2 75.2(2) . 2_554 ?
N1 Yb1 N2 75.2(2) 2_554 . ?
N1 Yb1 H1A 162.0 2_554 . ?
N1 Yb1 H1A 66.0 . . ?
N1 Yb1 H1B 72.9 . . ?
N1 Yb1 H1B 142.7 2_554 . ?
N2 Yb1 N2 70.6(3) . 2_554 ?
N2 Yb1 H1A 129.3 2_554 . ?
N2 Yb1 H1A 117.1 . . ?
N2 Yb1 H1B 99.0 . . ?
N2 Yb1 H1B 147.9 2_554 . ?
N3 Yb1 N1 79.6(3) . 2_554 ?
N3 Yb1 N1 79.6(3) 2_554 . ?
N3 Yb1 N1 113.2(3) 2_554 2_554 ?
N3 Yb1 N1 113.2(3) . . ?
N3 Yb1 N2 73.7(3) 2_554 2_554 ?
N3 Yb1 N2 135.2(2) . 2_554 ?
N3 Yb1 N2 135.2(2) 2_554 . ?
N3 Yb1 N2 73.7(3) . . ?
N3 Yb1 N3 149.5(4) . 2_554 ?
N3 Yb1 H1A 68.5 2_554 . ?
N3 Yb1 H1A 90.9 . . ?
N3 Yb1 H1B 63.6 . . ?
N3 Yb1 H1B 96.9 2_554 . ?
O1 Yb1 N1 78.2(2) 2_554 2_554 ?
O1 Yb1 N1 147.0(3) 2_554 . ?
O1 Yb1 N1 147.0(3) . 2_554 ?
O1 Yb1 N1 78.2(2) . . ?
O1 Yb1 N2 115.7(2) . . ?
O1 Yb1 N2 146.5(2) . 2_554 ?
O1 Yb1 N2 146.5(2) 2_554 . ?
O1 Yb1 N2 115.7(2) 2_554 2_554 ?
O1 Yb1 N3 81.8(3) . 2_554 ?
O1 Yb1 N3 81.8(3) 2_554 . ?
O1 Yb1 N3 74.6(3) . . ?
O1 Yb1 N3 74.6(3) 2_554 2_554 ?
O1 Yb1 O1 78.1(3) . 2_554 ?
O1 Yb1 H1A 85.4 2_554 . ?
O1 Yb1 H1A 17.2 . . ?
O1 Yb1 H1B 17.2 . . ?
O1 Yb1 H1B 90.0 2_554 . ?
H1A Yb1 H1B 28.6 . . ?
Yb1 O1 H1A 109.2 . . ?
Yb1 O1 H1B 109.2 . . ?
H1A O1 H1B 104.5 . . ?
H1WA O1W H1WB 109.5 . . ?
H2WA O2W H2WB 104.4 . . ?
H3WA O3W H3WB 104.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.110 0.250 107.3 18.3 '1/2 (H2O)'
2 0.000 -0.110 0.750 107.3 19.7 '1/2 (H2O)'
3 0.500 0.390 0.750 107.3 19.7 '1/2 (H2O)'
4 0.500 0.610 0.250 107.3 18.3 '1/2 (H2O)'

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT417_4                   
;
PROBLEM: Short Inter D-H..H-D H1B ..H2WB . 1.92 Ang.
RESPONSE: These alerts are all related to the hydrogen atoms of
lattice water. Water molecules for which the hydrogen atoms could not
be located were placed geometrically only to satisfy the stoichiometry
and induces short H - H interactions.
;
_vrf_PLAT420_4                   
;
PROBLEM: D-H Without Acceptor O2W --H2WA . Please Check
RESPONSE: Because the acceptor atoms were disordered atoms.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3_Sam
_database_code_depnum_ccdc_archive 'CCDC 1054138'
_audit_update_record             
;
2019-03-14 deposited with the CCDC.	2019-03-18 downloaded from the CCDC.
;
_audit_creation_date             2019-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H40 Fe2 Ho2 N20 O4), 6(O), 1[(H2O)]'
_chemical_formula_sum            'C30 H20 Fe Ho N10 O8'
_chemical_formula_weight         869.34
_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'
Fe Fe 0.3463 0.8444 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.6159(9)
_cell_length_b                   12.3991(5)
_cell_length_c                   15.1656(8)
_cell_angle_alpha                90
_cell_angle_beta                 116.836(6)
_cell_angle_gamma                90
_cell_volume                     3962.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4604
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7797
_cell_measurement_theta_min      2.9319
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21951
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.843
_diffrn_reflns_theta_min         3.173
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3507
_reflns_number_total             4818
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.223
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4818
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0573
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0731P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1414
_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. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
3. Rigid body (RIGU) restrains
 H7, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6054(3) 0.5319(6) 0.3643(5) 0.0411(15) Uani 1 1 d . . . . .
H1 H 0.632535 0.488968 0.350067 0.049 Uiso 1 1 calc R . . . .
C2 C 0.6248(3) 0.6381(6) 0.3976(6) 0.0523(18) Uani 1 1 d . . . . .
H2 H 0.663811 0.663460 0.405167 0.063 Uiso 1 1 calc R . . . .
C3 C 0.5862(4) 0.7026(6) 0.4183(6) 0.055(2) Uani 1 1 d . . . . .
H3 H 0.597735 0.773530 0.438382 0.066 Uiso 1 1 calc R . . . .
C4 C 0.5280(3) 0.6604(5) 0.4088(5) 0.0422(16) Uani 1 1 d . . . . .
C5 C 0.5121(3) 0.5536(5) 0.3759(4) 0.0352(14) Uani 1 1 d . . . . .
C6 C 0.4855(4) 0.7203(7) 0.4346(6) 0.056(2) Uani 1 1 d . . . . .
H6 H 0.495780 0.790940 0.456824 0.068 Uiso 1 1 calc R . . . .
C7 C 0.4316(4) 0.6777(6) 0.4278(6) 0.0526(18) Uani 1 1 d . U . . .
H7 H 0.405099 0.718895 0.444792 0.063 Uiso 1 1 calc R U . . .
C8 C 0.4144(3) 0.5687(6) 0.3943(5) 0.0416(16) Uani 1 1 d . . . . .
C9 C 0.4539(3) 0.5075(5) 0.3671(4) 0.0343(14) Uani 1 1 d . . . . .
C10 C 0.3589(3) 0.5196(7) 0.3886(6) 0.0511(18) Uani 1 1 d . . . . .
H10 H 0.332255 0.557080 0.407908 0.061 Uiso 1 1 calc R . . . .
C11 C 0.3450(3) 0.4173(6) 0.3547(6) 0.0499(18) Uani 1 1 d . . . . .
H11 H 0.308413 0.383642 0.349387 0.060 Uiso 1 1 calc R . . . .
C12 C 0.3868(3) 0.3631(6) 0.3278(5) 0.0454(16) Uani 1 1 d . . . . .
H12 H 0.376970 0.292356 0.305665 0.054 Uiso 1 1 calc R . . . .
C13 C 0.3401(3) 0.2636(5) 0.0835(5) 0.0360(14) Uani 1 1 d . . . . .
C14 C 0.2406(3) 0.4031(6) 0.0019(5) 0.0415(15) Uani 1 1 d . . . . .
C15 C 0.2399(3) 0.2431(6) 0.1207(5) 0.0464(17) Uani 1 1 d . . . . .
N1 N 0.5512(2) 0.4899(4) 0.3523(4) 0.0340(11) Uani 1 1 d . . . . .
N2 N 0.4393(2) 0.4052(4) 0.3315(4) 0.0347(11) Uani 1 1 d . . . . .
N3 N 0.3928(2) 0.2710(4) 0.1353(4) 0.0413(13) Uani 1 1 d . . . . .
N4 N 0.2313(3) 0.4945(6) 0.0062(7) 0.077(2) Uani 1 1 d . . . . .
N5 N 0.2343(3) 0.2401(7) 0.1914(6) 0.075(2) Uani 1 1 d . . . . .
O1 O 0.5111(2) 0.1774(4) 0.1589(4) 0.0462(11) Uani 1 1 d . . . . .
H1A H 0.476314 0.169510 0.087296 0.069 Uiso 1 1 d GR . . . .
H1B H 0.548905 0.181001 0.141465 0.069 Uiso 1 1 d GR . . . .
Fe1 Fe 0.250000 0.250000 0.000000 0.0365(3) Uani 1 2 d S T P . .
Ho1 Ho 0.500000 0.32195(3) 0.250000 0.03082(15) Uani 1 2 d S T P . .
O1W O 0.2004(3) 0.6598(5) 0.1122(5) 0.089(2) Uani 1 1 d . U . . .
O2W O 0.5813(3) 0.0425(7) 0.4666(6) 0.107(2) Uani 1 1 d . U . . .
O3W O 0.3902(3) 0.0640(6) 0.3478(5) 0.090(2) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.410(10) . ?
C1 N1 1.318(7) . ?
C2 C3 1.352(10) . ?
C3 C4 1.418(10) . ?
C4 C5 1.405(9) . ?
C4 C6 1.438(10) . ?
C5 C9 1.438(8) . ?
C5 N1 1.380(7) . ?
C6 C7 1.338(11) . ?
C7 C8 1.436(10) . ?
C8 C9 1.401(8) . ?
C8 C10 1.412(10) . ?
C9 N2 1.361(8) . ?
C10 C11 1.352(10) . ?
C11 C12 1.398(9) . ?
C12 N2 1.322(8) . ?
C13 N3 1.137(7) . ?
C13 Fe1 1.931(6) . ?
C14 N4 1.161(9) . ?
C14 Fe1 1.913(7) . ?
C15 N5 1.137(9) . ?
C15 Fe1 1.953(8) . ?
N1 Ho1 2.552(5) . ?
N2 Ho1 2.500(5) . ?
N3 Ho1 2.420(5) . ?
O1 Ho1 2.349(4) . ?

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
N1 C1 C2 123.8(6) . . ?
C3 C2 C1 119.5(7) . . ?
C2 C3 C4 118.9(6) . . ?
C3 C4 C6 123.1(6) . . ?
C5 C4 C3 118.4(6) . . ?
C5 C4 C6 118.4(6) . . ?
C4 C5 C9 119.9(6) . . ?
N1 C5 C4 121.9(6) . . ?
N1 C5 C9 118.1(5) . . ?
C7 C6 C4 122.1(7) . . ?
C6 C7 C8 120.4(7) . . ?
C9 C8 C7 119.6(6) . . ?
C9 C8 C10 118.1(6) . . ?
C10 C8 C7 122.3(6) . . ?
C8 C9 C5 119.5(6) . . ?
N2 C9 C5 117.9(5) . . ?
N2 C9 C8 122.6(6) . . ?
C11 C10 C8 119.2(6) . . ?
C10 C11 C12 118.7(7) . . ?
N2 C12 C11 124.7(7) . . ?
N3 C13 Fe1 177.7(6) . . ?
N4 C14 Fe1 174.2(7) . . ?
N5 C15 Fe1 179.3(8) . . ?
C1 N1 C5 117.5(5) . . ?
C1 N1 Ho1 124.8(4) . . ?
C5 N1 Ho1 115.9(3) . . ?
C9 N2 Ho1 118.8(4) . . ?
C12 N2 C9 116.7(5) . . ?
C12 N2 Ho1 123.5(5) . . ?
C13 N3 Ho1 169.0(5) . . ?
C13 Fe1 C13 180.0(2) . 7 ?
C13 Fe1 C15 92.6(3) . 7 ?
C13 Fe1 C15 87.4(3) . . ?
C13 Fe1 C15 87.4(3) 7 7 ?
C13 Fe1 C15 92.6(3) 7 . ?
C14 Fe1 C13 89.8(3) 7 . ?
C14 Fe1 C13 90.2(3) . . ?
C14 Fe1 C13 89.8(3) . 7 ?
C14 Fe1 C13 90.2(3) 7 7 ?
C14 Fe1 C14 180.0 7 . ?
C14 Fe1 C15 88.0(3) . . ?
C14 Fe1 C15 92.0(3) . 7 ?
C14 Fe1 C15 88.0(3) 7 7 ?
C14 Fe1 C15 92.0(3) 7 . ?
C15 Fe1 C15 180.0(3) . 7 ?
N1 Ho1 N1 70.6(2) . 2_655 ?
N2 Ho1 N1 75.17(16) . 2_655 ?
N2 Ho1 N1 65.30(15) . . ?
N2 Ho1 N1 75.17(16) 2_655 . ?
N2 Ho1 N1 65.30(15) 2_655 2_655 ?
N2 Ho1 N2 131.2(2) . 2_655 ?
N3 Ho1 N1 73.83(17) . 2_655 ?
N3 Ho1 N1 134.81(16) . . ?
N3 Ho1 N1 134.81(16) 2_655 2_655 ?
N3 Ho1 N1 73.83(17) 2_655 . ?
N3 Ho1 N2 79.40(17) . . ?
N3 Ho1 N2 79.40(17) 2_655 2_655 ?
N3 Ho1 N2 113.56(18) . 2_655 ?
N3 Ho1 N2 113.56(18) 2_655 . ?
N3 Ho1 N3 149.7(3) . 2_655 ?
O1 Ho1 N1 146.37(15) 2_655 2_655 ?
O1 Ho1 N1 114.38(17) . 2_655 ?
O1 Ho1 N1 114.38(17) 2_655 . ?
O1 Ho1 N1 146.38(15) . . ?
O1 Ho1 N2 147.88(16) . . ?
O1 Ho1 N2 77.48(17) . 2_655 ?
O1 Ho1 N2 147.89(16) 2_655 2_655 ?
O1 Ho1 N2 77.48(17) 2_655 . ?
O1 Ho1 N3 82.27(18) 2_655 . ?
O1 Ho1 N3 74.67(17) 2_655 2_655 ?
O1 Ho1 N3 74.67(17) . . ?
O1 Ho1 N3 82.28(18) . 2_655 ?
O1 Ho1 O1 80.5(2) 2_655 . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.393 0.250 141.8 16.7 '1/2 (H2O)'
2 0.000 0.607 0.750 141.8 15.4 '1/2 (H2O)'
3 0.500 0.107 0.750 141.8 15.4 '1/2 (H2O)'
4 0.500 0.893 0.250 141.8 16.7 '1/2 (H2O)'

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT306_3_Sam               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: H atoms of water molecules were not located due to disorder and high thermal parameters of oxygen atoms.
;
_vrf_PLAT430_3_Sam               
;
PROBLEM: Short Inter D...A Contact O1W ..O3W . 2.74 Ang.
RESPONSE: H-atoms from the crystallisation water molecules are missing.
Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.
;
