# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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 
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data_C30H56N12O10Dy3Cr
_database_code_depnum_ccdc_archive 'CCDC 1561413'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H56 Cr Dy3 N12 O10'
_chemical_formula_sum            'C30 H56 Cr Dy3 N12 O10'
_chemical_formula_weight         1284.36
_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'
Cr Cr 0.3209 0.6236 '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      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   14.335(13)
_cell_length_b                   13.289(13)
_cell_length_c                   13.888(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2646(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.4939
_cell_measurement_theta_min      2.5546
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.439
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.4525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.6058.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1244
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.712
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.028
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            139241
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.340
_diffrn_reflns_theta_min         2.042
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5157
_reflns_number_total             6322
_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       'SAINT V8.27A (Bruker,2012)'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'SAINT V8.27A (Bruker,2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         6322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.035
_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)+(0.0250P)²+2.8050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0580
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H0Aa(0.5) H0Ab(0.5) H10a(0.5) H10b(0.5)
3.a Rotating group:
 O0AA(H0Aa,H0Ab), O10(H10a,H10b)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C14(H14)
3.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C3AA(H3Aa,H3Ab,H3Ac), C4AA(H4Aa,H4Ab,H4Ac)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.7500 0.61352(2) 0.27787(2) 0.01683(3) Uani 1 2 d S T P . .
Dy2 Dy 0.7500 0.7500 0.04630(2) 0.02807(5) Uani 1 4 d S T P . .
O2 O 0.66213(13) 0.7500 0.31883(12) 0.0190(3) Uani 1 2 d S T P . .
O3 O 0.66243(10) 0.86033(10) 0.13816(9) 0.0231(2) Uani 1 1 d . . . . .
N2 N 0.92680(12) 0.56471(12) 0.30001(13) 0.0263(3) Uani 1 1 d . . . . .
C5 C 0.56416(19) 0.7500 0.3051(2) 0.0235(5) Uani 1 2 d S T P . .
H5 H 0.5337 0.7500 0.3699 0.028 Uiso 1 2 calc RS T P . .
C6 C 0.53326(14) 0.84500(15) 0.25149(16) 0.0269(4) Uani 1 1 d . . . . .
H6 H 0.4637 0.8494 0.2537 0.032 Uiso 1 1 calc R . . . .
C7 C 0.56466(14) 0.84596(16) 0.14582(14) 0.0272(4) Uani 1 1 d . . . . .
H7 H 0.5334 0.9041 0.1134 0.033 Uiso 1 1 calc R . . . .
N8 N 0.9276(2) 0.7500 -0.00580(19) 0.0404(7) Uani 1 2 d S T P . .
C14 C 0.5339(2) 0.7500 0.0943(2) 0.0330(6) Uani 1 2 d S T P . .
H14 H 0.4642 0.7500 0.0902 0.040 Uiso 1 2 calc RS T P . .
Cr1 Cr 0.7500 0.2500 0.45460(6) 0.03092(14) Uani 1 4 d S T P . .
C0AA C 0.7500 0.3621(2) 0.3507(2) 0.0298(6) Uani 1 2 d S T P . .
N10 N 0.7500 0.42941(19) 0.2983(2) 0.0315(5) Uani 1 2 d S T P . .
O0AA O 0.7500 0.59497(16) 0.45198(14) 0.0340(5) Uani 1 2 d S T P . .
H0AA H 0.7926 0.6365 0.4803 0.051 Uiso 0.5 1 d GR . . . .
H0AB H 0.7702 0.5327 0.4702 0.051 Uiso 0.5 1 d GR . . . .
O10 O 0.7500 0.8722(3) -0.0810(2) 0.0728(11) Uani 1 2 d S T P . .
H10A H 0.7652 0.9497 -0.0766 0.109 Uiso 0.5 1 d GR . . . .
H10B H 0.7348 0.8613 -0.1545 0.109 Uiso 0.5 1 d GR . . . .
N5 N 0.9741(2) 0.2500 0.4361(2) 0.0415(7) Uani 1 2 d S T P . .
C1AA C 0.8947(3) 0.2500 0.4470(2) 0.0351(7) Uani 1 2 d S T P . .
C2AA C 0.7500 0.3635(2) 0.5577(3) 0.0366(7) Uani 1 2 d S T P . .
N7 N 0.7500 0.4297(2) 0.6113(2) 0.0443(7) Uani 1 2 d S T P . .
C4 C 0.96027(19) 0.55707(17) 0.40064(17) 0.0377(5) Uani 1 1 d . . . . .
H4A H 0.9382 0.6153 0.4374 0.057 Uiso 1 1 calc GR . . . .
H4B H 1.0286 0.5557 0.4013 0.057 Uiso 1 1 calc GR . . . .
H4C H 0.9362 0.4952 0.4298 0.057 Uiso 1 1 calc GR . . . .
C3AA C 0.95718(17) 0.47198(16) 0.25006(19) 0.0352(5) Uani 1 1 d . . . . .
H3AA H 0.9411 0.4132 0.2893 0.053 Uiso 1 1 calc GR . . . .
H3AB H 1.0248 0.4741 0.2402 0.053 Uiso 1 1 calc GR . . . .
H3AC H 0.9257 0.4672 0.1876 0.053 Uiso 1 1 calc GR . . . .
C4AA C 0.9600(3) 0.8401(3) -0.0594(2) 0.0614(9) Uani 1 1 d . . . . .
H4AA H 0.9387 0.8359 -0.1264 0.092 Uiso 1 1 calc GR . . . .
H4AB H 1.0283 0.8430 -0.0579 0.092 Uiso 1 1 calc GR . . . .
H4AC H 0.9343 0.9008 -0.0294 0.092 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy1 3.627(4) 2_665 ?
Dy1 Dy2 3.692(3) . ?
Dy1 O2 2.2803(19) 2_665 ?
Dy1 O2 2.2803(19) . ?
Dy1 O3 2.337(2) 8_575 ?
Dy1 O3 2.337(2) 2_665 ?
Dy1 N2 2.634(3) 7_755 ?
Dy1 N2 2.634(3) . ?
Dy1 N10 2.463(3) . ?
Dy1 O0AA 2.431(3) . ?
Dy2 Dy1 3.692(3) 2_665 ?
Dy2 O3 2.3137(19) . ?
Dy2 O3 2.3137(19) 7_755 ?
Dy2 O3 2.3137(19) 2_665 ?
Dy2 O3 2.3137(19) 8_575 ?
Dy2 N8 2.647(4) 2_665 ?
Dy2 N8 2.647(4) . ?
Dy2 O10 2.400(3) . ?
Dy2 O10 2.400(3) 2_665 ?
O2 Dy1 2.2803(19) 2_665 ?
O2 C5 1.417(4) . ?
O3 Dy1 2.337(2) 2_665 ?
O3 C7 1.418(3) . ?
N2 C6 1.491(3) 2_665 ?
N2 C4 1.481(3) . ?
N2 C3AA 1.480(3) . ?
C5 C6 1.531(3) . ?
C5 C6 1.531(3) 8_575 ?
C6 N2 1.491(3) 2_665 ?
C6 C7 1.535(3) . ?
C7 C14 1.527(3) . ?
N8 C14 1.496(5) 2_665 ?
N8 C4AA 1.485(3) . ?
N8 C4AA 1.485(3) 8_575 ?
C14 C7 1.527(3) 8_575 ?
C14 N8 1.496(5) 2_665 ?
Cr1 C0AA 2.073(3) . ?
Cr1 C0AA 2.073(3) 2_655 ?
Cr1 C1AA 2.077(4) 2_655 ?
Cr1 C1AA 2.077(4) . ?
Cr1 C2AA 2.080(4) . ?
Cr1 C2AA 2.080(4) 2_655 ?
C0AA N10 1.154(4) . ?
N5 C1AA 1.149(5) . ?
C2AA N7 1.153(5) . ?

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
Dy1 Dy1 Dy2 60.58(3) 2_665 . ?
O2 Dy1 Dy1 37.31(5) . 2_665 ?
O2 Dy1 Dy1 37.31(5) 2_665 2_665 ?
O2 Dy1 Dy2 80.01(6) 2_665 . ?
O2 Dy1 Dy2 80.01(6) . . ?
O2 Dy1 O2 67.06(10) 2_665 . ?
O2 Dy1 O3 112.68(6) 2_665 8_575 ?
O2 Dy1 O3 112.68(6) . 2_665 ?
O2 Dy1 O3 78.00(7) 2_665 2_665 ?
O2 Dy1 O3 78.00(7) . 8_575 ?
O2 Dy1 N2 68.61(7) 2_665 . ?
O2 Dy1 N2 68.61(7) . 7_755 ?
O2 Dy1 N2 134.29(6) . . ?
O2 Dy1 N2 134.28(6) 2_665 7_755 ?
O2 Dy1 N10 139.59(6) . . ?
O2 Dy1 N10 139.59(6) 2_665 . ?
O2 Dy1 O0AA 80.36(6) . . ?
O2 Dy1 O0AA 80.36(6) 2_665 . ?
O3 Dy1 Dy1 81.45(3) 8_575 2_665 ?
O3 Dy1 Dy1 81.45(4) 2_665 2_665 ?
O3 Dy1 Dy2 37.23(5) 8_575 . ?
O3 Dy1 Dy2 37.23(5) 2_665 . ?
O3 Dy1 O3 64.98(9) 8_575 2_665 ?
O3 Dy1 N2 67.46(7) 8_575 7_755 ?
O3 Dy1 N2 67.46(7) 2_665 . ?
O3 Dy1 N2 130.57(6) 8_575 . ?
O3 Dy1 N2 130.57(6) 2_665 7_755 ?
O3 Dy1 N10 104.08(7) 8_575 . ?
O3 Dy1 N10 104.08(7) 2_665 . ?
O3 Dy1 O0AA 147.25(5) 8_575 . ?
O3 Dy1 O0AA 147.25(5) 2_665 . ?
N2 Dy1 Dy1 104.26(4) 7_755 2_665 ?
N2 Dy1 Dy1 104.26(4) . 2_665 ?
N2 Dy1 Dy2 102.87(4) 7_755 . ?
N2 Dy1 Dy2 102.87(4) . . ?
N2 Dy1 N2 148.37(8) . 7_755 ?
N10 Dy1 Dy1 173.39(7) . 2_665 ?
N10 Dy1 Dy2 126.03(7) . . ?
N10 Dy1 N2 75.04(4) . . ?
N10 Dy1 N2 75.04(4) . 7_755 ?
O0AA Dy1 Dy1 95.82(5) . 2_665 ?
O0AA Dy1 Dy2 156.40(6) . . ?
O0AA Dy1 N2 81.89(4) . . ?
O0AA Dy1 N2 81.89(4) . 7_755 ?
O0AA Dy1 N10 77.57(8) . . ?
Dy1 Dy2 Dy1 58.84(7) . 2_665 ?
O3 Dy2 Dy1 37.67(4) 7_755 2_665 ?
O3 Dy2 Dy1 80.27(7) 8_575 2_665 ?
O3 Dy2 Dy1 37.67(4) 2_665 . ?
O3 Dy2 Dy1 37.67(4) . 2_665 ?
O3 Dy2 Dy1 80.27(7) 2_665 2_665 ?
O3 Dy2 Dy1 80.27(7) . . ?
O3 Dy2 Dy1 37.67(4) 8_575 . ?
O3 Dy2 Dy1 80.27(7) 7_755 . ?
O3 Dy2 O3 78.65(9) 7_755 2_665 ?
O3 Dy2 O3 65.72(9) 8_575 2_665 ?
O3 Dy2 O3 65.72(9) 7_755 . ?
O3 Dy2 O3 78.65(9) 8_575 . ?
O3 Dy2 O3 113.07(9) 2_665 . ?
O3 Dy2 O3 113.07(9) 7_755 8_575 ?
O3 Dy2 N8 132.27(5) 8_575 . ?
O3 Dy2 N8 132.27(5) 7_755 2_665 ?
O3 Dy2 N8 68.21(7) . 2_665 ?
O3 Dy2 N8 68.21(7) 8_575 2_665 ?
O3 Dy2 N8 68.21(7) 2_665 . ?
O3 Dy2 N8 132.27(5) 2_665 2_665 ?
O3 Dy2 N8 68.21(7) 7_755 . ?
O3 Dy2 N8 132.27(5) . . ?
O3 Dy2 O10 88.71(11) 2_665 2_665 ?
O3 Dy2 O10 146.59(5) 7_755 2_665 ?
O3 Dy2 O10 146.59(5) . 2_665 ?
O3 Dy2 O10 88.71(11) 7_755 . ?
O3 Dy2 O10 88.71(11) . . ?
O3 Dy2 O10 146.59(5) 2_665 . ?
O3 Dy2 O10 146.59(5) 8_575 . ?
O3 Dy2 O10 88.71(11) 8_575 2_665 ?
N8 Dy2 Dy1 103.78(6) 2_665 2_665 ?
N8 Dy2 Dy1 103.78(6) . 2_665 ?
N8 Dy2 Dy1 103.78(6) . . ?
N8 Dy2 Dy1 103.78(6) 2_665 . ?
N8 Dy2 N8 148.27(13) 2_665 . ?
O10 Dy2 Dy1 166.86(10) . . ?
O10 Dy2 Dy1 108.01(13) . 2_665 ?
O10 Dy2 Dy1 108.01(13) 2_665 . ?
O10 Dy2 Dy1 166.86(10) 2_665 2_665 ?
O10 Dy2 N8 78.38(5) . . ?
O10 Dy2 N8 78.38(5) . 2_665 ?
O10 Dy2 N8 78.38(5) 2_665 . ?
O10 Dy2 N8 78.38(5) 2_665 2_665 ?
O10 Dy2 O10 85.1(2) . 2_665 ?
Dy1 O2 Dy1 105.38(10) . 2_665 ?
C5 O2 Dy1 120.91(8) . 2_665 ?
C5 O2 Dy1 120.91(8) . . ?
Dy2 O3 Dy1 105.11(8) . 2_665 ?
C7 O3 Dy1 119.24(12) . 2_665 ?
C7 O3 Dy2 119.48(12) . . ?
C6 N2 Dy1 96.81(12) 2_665 . ?
C4 N2 Dy1 116.02(15) . . ?
C4 N2 C6 110.93(17) . 2_665 ?
C3AA N2 Dy1 115.70(13) . . ?
C3AA N2 C6 110.21(18) . 2_665 ?
C3AA N2 C4 106.85(17) . . ?
O2 C5 C6 110.62(14) . . ?
O2 C5 C6 110.63(14) . 8_575 ?
C6 C5 C6 111.1(2) . 8_575 ?
N2 C6 C5 109.45(18) 2_665 . ?
N2 C6 C7 108.23(17) 2_665 . ?
C5 C6 C7 112.74(18) . . ?
O3 C7 C6 111.26(15) . . ?
O3 C7 C14 111.3(2) . . ?
C14 C7 C6 110.9(2) . . ?
C14 N8 Dy2 95.80(17) 2_665 . ?
C4AA N8 Dy2 116.0(2) . . ?
C4AA N8 Dy2 116.0(2) 8_575 . ?
C4AA N8 C14 110.5(2) 8_575 2_665 ?
C4AA N8 C14 110.5(2) . 2_665 ?
C4AA N8 C4AA 107.5(3) 8_575 . ?
C7 C14 C7 113.2(2) . 8_575 ?
N8 C14 C7 109.20(18) 2_665 8_575 ?
N8 C14 C7 109.20(18) 2_665 . ?
C0AA Cr1 C0AA 91.83(18) 2_655 . ?
C0AA Cr1 C1AA 87.98(7) . . ?
C0AA Cr1 C1AA 87.98(7) . 2_655 ?
C0AA Cr1 C1AA 87.98(7) 2_655 2_655 ?
C0AA Cr1 C1AA 87.98(7) 2_655 . ?
C0AA Cr1 C2AA 179.43(12) 2_655 . ?
C0AA Cr1 C2AA 87.60(14) 2_655 2_655 ?
C0AA Cr1 C2AA 87.60(14) . . ?
C0AA Cr1 C2AA 179.43(12) . 2_655 ?
C1AA Cr1 C1AA 174.19(19) . 2_655 ?
C1AA Cr1 C2AA 92.00(7) . . ?
C1AA Cr1 C2AA 92.00(7) 2_655 . ?
C1AA Cr1 C2AA 92.00(7) . 2_655 ?
C1AA Cr1 C2AA 92.00(7) 2_655 2_655 ?
C2AA Cr1 C2AA 93.0(2) . 2_655 ?
N10 C0AA Cr1 175.1(3) . . ?
C0AA N10 Dy1 147.5(2) . . ?
N5 C1AA Cr1 175.3(3) . . ?
N7 C2AA Cr1 176.7(3) . . ?

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
O0AA H0AB N7 0.91 2.41 3.118(4) 134.7 .

_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 -0.755 0.240 0.000 783.5 176.1 18.H2O

_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_C30H54N12O9Ho3Fe
_database_code_depnum_ccdc_archive 'CCDC 1561419'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C60 H108 Fe2 Ho6 N24 O18)'
_chemical_formula_sum            'C30 H54 Fe Ho3 N12 O9'
_chemical_formula_weight         1277.49
_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   16.276(3)
_cell_length_b                   18.779(3)
_cell_length_c                   14.043(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4292.2(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7628
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.735
_shelx_estimated_absorpt_T_min   0.512
_exptl_absorpt_coefficient_mu    5.862
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.7454.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2468
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.056
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.619
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29300
_diffrn_reflns_point_group_measured_fraction_full 0.619
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.255
_diffrn_reflns_theta_min         1.811
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.619
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2246
_reflns_number_total             2477
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0234
_refine_ls_restrained_S_all      1.077
_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)+(0.0193P)²+19.7941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0545
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H3a(0.5) H3b(0.5) H2a(0.5) H2b(0.5) H1a(0.5) H1b(0.5)
3.a Rotating group:
 O3(H3a,H3b), O2(H2a,H2b), O1(H1a,H1b)
3.b Ternary CH refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C10(H10), C16(H16)
3.c Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C19(H19a,H19b,H19c), C9(H9a,H9b,H9c), C17(H17a,H17b,
 H17c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho2 Ho 0.67285(2) 0.2500 0.17384(3) 0.01807(13) Uani 1 2 d S T P . .
Ho1 Ho 0.61885(2) 0.2500 -0.07872(3) 0.01854(13) Uani 1 2 d S T P . .
Ho3 Ho 0.83476(2) 0.2500 -0.00906(3) 0.01542(13) Uani 1 2 d S T P . .
Fe4 Fe 1.15863(7) 0.2500 -0.05248(9) 0.0218(3) Uani 1 2 d S T P . .
O4 O 0.7370(2) 0.3159(2) -0.0842(3) 0.0177(9) Uani 1 1 d . . . . .
O6 O 0.7819(2) 0.1836(2) 0.1168(3) 0.0165(9) Uani 1 1 d . . . . .
O5 O 0.6099(2) 0.1827(2) 0.0583(3) 0.0209(10) Uani 1 1 d . . . . .
N8 N 0.5915(3) 0.3866(3) -0.1180(3) 0.0252(13) Uani 1 1 d . . . . .
C12 C 0.7965(4) 0.4137(3) 0.0051(4) 0.0216(15) Uani 1 1 d . . . . .
H12 H 0.8007 0.4669 0.0040 0.026 Uiso 1 1 calc R . . . .
C13 C 0.7354(4) 0.3902(3) -0.0703(4) 0.0195(15) Uani 1 1 d . . . . .
H13 H 0.7516 0.4132 -0.1317 0.023 Uiso 1 1 calc R . . . .
C14 C 0.6490(4) 0.4154(4) -0.0456(4) 0.0236(16) Uani 1 1 d . . . . .
H14 H 0.6476 0.4686 -0.0483 0.028 Uiso 1 1 calc R . . . .
C20 C 0.6164(4) 0.4099(4) -0.2145(4) 0.0337(18) Uani 1 1 d . . . . .
H20A H 0.6679 0.3862 -0.2323 0.051 Uiso 1 1 calc GR . . . .
H20B H 0.6246 0.4616 -0.2149 0.051 Uiso 1 1 calc GR . . . .
H20C H 0.5734 0.3972 -0.2603 0.051 Uiso 1 1 calc GR . . . .
C19 C 0.5074(4) 0.4140(4) -0.1018(5) 0.040(2) Uani 1 1 d . . . . .
H19A H 0.4712 0.3975 -0.1530 0.060 Uiso 1 1 calc GR . . . .
H19B H 0.5084 0.4662 -0.1012 0.060 Uiso 1 1 calc GR . . . .
H19C H 0.4868 0.3965 -0.0406 0.060 Uiso 1 1 calc GR . . . .
N6 N 0.6620(3) 0.1140(3) 0.2229(3) 0.0222(13) Uani 1 1 d . . . . .
C15 C 0.6855(4) 0.0851(3) 0.1278(4) 0.0231(16) Uani 1 1 d . . . . .
H15 H 0.6851 0.0319 0.1312 0.028 Uiso 1 1 calc R . . . .
C10 C 0.6225(4) 0.1088(3) 0.0539(4) 0.0227(16) Uani 1 1 d . . . . .
H10 H 0.5692 0.0849 0.0692 0.027 Uiso 1 1 calc R . . . .
C16 C 0.7728(4) 0.1099(3) 0.1053(4) 0.0195(15) Uani 1 1 d . . . . .
H16 H 0.8108 0.0859 0.1511 0.023 Uiso 1 1 calc R . . . .
N3 N 0.9814(5) 0.2500 0.0270(5) 0.0239(18) Uani 1 2 d S T P . .
C1 C 1.1111(5) 0.2500 -0.1791(7) 0.022(2) Uani 1 2 d S T P . .
C2 C 1.1987(5) 0.2500 0.0764(8) 0.027(2) Uani 1 2 d S T P . .
C3 C 1.0491(6) 0.2500 -0.0009(6) 0.021(2) Uani 1 2 d S T P . .
N7 N 0.8797(3) 0.3827(3) -0.0164(3) 0.0224(13) Uani 1 1 d . . . . .
N1 N 1.0828(4) 0.2500 -0.2533(6) 0.0237(18) Uani 1 2 d S T P . .
N2 N 1.2154(4) 0.2500 0.1574(6) 0.0271(19) Uani 1 2 d S T P . .
C9 C 0.9401(4) 0.4062(4) 0.0563(5) 0.0292(17) Uani 1 1 d . . . . .
H9A H 0.9294 0.3813 0.1164 0.044 Uiso 1 1 calc GR . . . .
H9B H 0.9349 0.4577 0.0661 0.044 Uiso 1 1 calc GR . . . .
H9C H 0.9958 0.3951 0.0343 0.044 Uiso 1 1 calc GR . . . .
C17 C 0.9100(4) 0.4089(4) -0.1103(5) 0.0321(17) Uani 1 1 d . . . . .
H17A H 0.9658 0.3910 -0.1214 0.048 Uiso 1 1 calc GR . . . .
H17B H 0.9107 0.4611 -0.1104 0.048 Uiso 1 1 calc GR . . . .
H17C H 0.8735 0.3918 -0.1609 0.048 Uiso 1 1 calc GR . . . .
C5 C 1.1603(5) 0.1479(5) -0.0520(5) 0.051(2) Uani 1 1 d . . . . .
C4 C 1.2648(8) 0.2500 -0.1129(8) 0.067(4) Uani 1 2 d S T P . .
N4 N 1.3244(7) 0.2500 -0.1541(8) 0.131(7) Uani 1 2 d S T P . .
O3 O 0.8985(4) 0.2500 -0.1643(4) 0.0284(16) Uani 1 2 d S T P . .
H3A H 0.9449 0.2768 -0.1648 0.043 Uiso 0.5 1 d GR . . . .
H3B H 0.8664 0.2722 -0.2081 0.043 Uiso 0.5 1 d GR . . . .
N5 N 1.1609(7) 0.0872(5) -0.0502(6) 0.114(4) Uani 1 1 d . . . . .
O2 O 0.5479(4) 0.2500 0.2626(4) 0.0311(16) Uani 1 2 d S T P . .
H2A H 0.5091 0.2723 0.2305 0.047 Uiso 0.5 1 d GR . . . .
H2B H 0.5536 0.2757 0.3148 0.047 Uiso 0.5 1 d GR . . . .
O1 O 0.4727(4) 0.2500 -0.0629(5) 0.045(2) Uani 1 2 d S T P . .
H1A H 0.4595 0.2572 -0.0033 0.067 Uiso 0.5 1 d GR . . . .
H1B H 0.4533 0.2076 -0.0756 0.067 Uiso 0.5 1 d GR . . . .
C6 C 0.7199(4) 0.0881(4) 0.2968(4) 0.0265(16) Uani 1 1 d . . . . .
H6A H 0.7739 0.1100 0.2869 0.040 Uiso 1 1 calc GR . . . .
H6B H 0.7250 0.0362 0.2922 0.040 Uiso 1 1 calc GR . . . .
H6C H 0.6992 0.1009 0.3600 0.040 Uiso 1 1 calc GR . . . .
C7 C 0.5784(4) 0.0896(4) 0.2503(5) 0.0367(18) Uani 1 1 d . . . . .
H7A H 0.5665 0.1049 0.3156 0.055 Uiso 1 1 calc GR . . . .
H7B H 0.5758 0.0376 0.2466 0.055 Uiso 1 1 calc GR . . . .
H7C H 0.5378 0.1104 0.2068 0.055 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho2 Ho1 3.6541(8) . ?
Ho2 Ho3 3.6799(7) . ?
Ho2 O6 2.312(4) . ?
Ho2 O6 2.312(4) 8_565 ?
Ho2 O5 2.298(4) . ?
Ho2 O5 2.298(4) 8_565 ?
Ho2 N6 2.651(5) . ?
Ho2 N6 2.651(5) 8_565 ?
Ho2 N2 2.469(8) 6_556 ?
Ho2 O2 2.386(6) . ?
Ho1 Ho3 3.6478(8) . ?
Ho1 O4 2.288(4) 8_565 ?
Ho1 O4 2.288(4) . ?
Ho1 O5 2.307(4) . ?
Ho1 O5 2.307(4) 8_565 ?
Ho1 N8 2.662(5) . ?
Ho1 N8 2.662(5) 8_565 ?
Ho1 N1 2.431(8) 6 ?
Ho1 O1 2.389(6) . ?
Ho3 O4 2.275(4) 8_565 ?
Ho3 O4 2.275(4) . ?
Ho3 O6 2.328(4) . ?
Ho3 O6 2.328(4) 8_565 ?
Ho3 N3 2.439(7) . ?
Ho3 N7 2.600(5) 8_565 ?
Ho3 N7 2.600(5) . ?
Ho3 O3 2.414(6) . ?
Fe4 C1 1.939(11) . ?
Fe4 C2 1.924(11) . ?
Fe4 C3 1.925(10) . ?
Fe4 C5 1.917(9) 8_565 ?
Fe4 C5 1.917(9) . ?
Fe4 C4 1.925(13) . ?
O4 C13 1.409(7) . ?
O6 C16 1.402(7) . ?
O5 C10 1.404(7) . ?
N8 C14 1.484(8) . ?
N8 C20 1.481(8) . ?
N8 C19 1.480(8) . ?
C12 C13 1.519(8) . ?
C12 C16 1.525(8) 8_565 ?
C12 N7 1.505(8) . ?
C13 C14 1.524(8) . ?
C14 C10 1.532(9) 8_565 ?
N6 C15 1.492(8) . ?
N6 C6 1.484(7) . ?
N6 C7 1.486(8) . ?
C15 C10 1.524(8) . ?
C15 C16 1.528(8) . ?
C10 C14 1.532(9) 8_565 ?
C16 C12 1.525(8) 8_565 ?
N3 C3 1.170(11) . ?
C1 N1 1.139(11) . ?
C2 N2 1.169(11) . ?
N7 C9 1.483(8) . ?
N7 C17 1.492(8) . ?
N1 Ho1 2.431(8) 6_655 ?
N2 Ho2 2.469(8) 6_656 ?
C5 N5 1.141(11) . ?
C4 N4 1.130(14) . ?

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
Ho1 Ho2 Ho3 59.653(15) . . ?
O6 Ho2 Ho1 81.28(9) . . ?
O6 Ho2 Ho1 81.28(9) 8_565 . ?
O6 Ho2 Ho3 37.66(9) . . ?
O6 Ho2 Ho3 37.66(9) 8_565 . ?
O6 Ho2 O6 65.24(19) . 8_565 ?
O6 Ho2 N6 67.80(14) 8_565 8_565 ?
O6 Ho2 N6 131.35(14) 8_565 . ?
O6 Ho2 N6 131.35(14) . 8_565 ?
O6 Ho2 N6 67.80(14) . . ?
O6 Ho2 N2 96.74(17) . 6_556 ?
O6 Ho2 N2 96.74(17) 8_565 6_556 ?
O6 Ho2 O2 146.68(10) . . ?
O6 Ho2 O2 146.68(10) 8_565 . ?
O5 Ho2 Ho1 37.57(10) . . ?
O5 Ho2 Ho1 37.57(10) 8_565 . ?
O5 Ho2 Ho3 80.01(10) . . ?
O5 Ho2 Ho3 80.01(10) 8_565 . ?
O5 Ho2 O6 78.53(13) . . ?
O5 Ho2 O6 78.53(13) 8_565 8_565 ?
O5 Ho2 O6 113.22(13) . 8_565 ?
O5 Ho2 O6 113.22(13) 8_565 . ?
O5 Ho2 O5 66.7(2) 8_565 . ?
O5 Ho2 N6 67.91(14) . . ?
O5 Ho2 N6 133.13(15) . 8_565 ?
O5 Ho2 N6 133.13(15) 8_565 . ?
O5 Ho2 N6 67.91(14) 8_565 8_565 ?
O5 Ho2 N2 143.40(12) . 6_556 ?
O5 Ho2 N2 143.40(12) 8_565 6_556 ?
O5 Ho2 O2 89.36(16) 8_565 . ?
O5 Ho2 O2 89.36(16) . . ?
N6 Ho2 Ho1 103.67(11) 8_565 . ?
N6 Ho2 Ho1 103.67(11) . . ?
N6 Ho2 Ho3 103.26(10) 8_565 . ?
N6 Ho2 Ho3 103.26(10) . . ?
N6 Ho2 N6 148.8(2) 8_565 . ?
N2 Ho2 Ho1 177.64(18) 6_556 . ?
N2 Ho2 Ho3 117.98(18) 6_556 . ?
N2 Ho2 N6 76.65(11) 6_556 8_565 ?
N2 Ho2 N6 76.65(11) 6_556 . ?
O2 Ho2 Ho1 107.59(15) . . ?
O2 Ho2 Ho3 167.24(15) . . ?
O2 Ho2 N6 78.88(11) . . ?
O2 Ho2 N6 78.88(11) . 8_565 ?
O2 Ho2 N2 74.8(2) . 6_556 ?
Ho3 Ho1 Ho2 60.525(10) . . ?
O4 Ho1 Ho2 80.24(9) . . ?
O4 Ho1 Ho2 80.24(9) 8_565 . ?
O4 Ho1 Ho3 36.80(9) . . ?
O4 Ho1 Ho3 36.80(9) 8_565 . ?
O4 Ho1 O4 65.45(19) . 8_565 ?
O4 Ho1 O5 77.59(13) . 8_565 ?
O4 Ho1 O5 112.19(13) . . ?
O4 Ho1 O5 77.59(13) 8_565 . ?
O4 Ho1 O5 112.19(13) 8_565 8_565 ?
O4 Ho1 N8 130.91(14) 8_565 . ?
O4 Ho1 N8 67.21(14) 8_565 8_565 ?
O4 Ho1 N8 130.91(14) . 8_565 ?
O4 Ho1 N8 67.21(14) . . ?
O4 Ho1 N1 99.79(18) . 6 ?
O4 Ho1 N1 99.79(18) 8_565 6 ?
O4 Ho1 O1 147.15(9) . . ?
O4 Ho1 O1 147.15(9) 8_565 . ?
O5 Ho1 Ho2 37.41(10) 8_565 . ?
O5 Ho1 Ho2 37.41(10) . . ?
O5 Ho1 Ho3 80.64(9) 8_565 . ?
O5 Ho1 Ho3 80.64(9) . . ?
O5 Ho1 O5 66.5(2) . 8_565 ?
O5 Ho1 N8 133.67(15) . . ?
O5 Ho1 N8 133.67(15) 8_565 8_565 ?
O5 Ho1 N8 68.53(15) . 8_565 ?
O5 Ho1 N8 68.53(15) 8_565 . ?
O5 Ho1 N1 142.57(13) 8_565 6 ?
O5 Ho1 N1 142.57(13) . 6 ?
O5 Ho1 O1 81.93(16) . . ?
O5 Ho1 O1 81.93(16) 8_565 . ?
N8 Ho1 Ho2 103.97(11) 8_565 . ?
N8 Ho1 Ho2 103.97(11) . . ?
N8 Ho1 Ho3 102.52(11) . . ?
N8 Ho1 Ho3 102.52(11) 8_565 . ?
N8 Ho1 N8 149.1(2) . 8_565 ?
N1 Ho1 Ho2 179.96(18) 6 . ?
N1 Ho1 Ho3 119.52(18) 6 . ?
N1 Ho1 N8 76.02(11) 6 8_565 ?
N1 Ho1 N8 76.02(11) 6 . ?
O1 Ho1 Ho2 98.60(16) . . ?
O1 Ho1 Ho3 159.13(16) . . ?
O1 Ho1 N8 81.52(11) . 8_565 ?
O1 Ho1 N8 81.52(11) . . ?
O1 Ho1 N1 81.4(2) . 6 ?
Ho1 Ho3 Ho2 59.822(15) . . ?
O4 Ho3 Ho2 79.81(9) . . ?
O4 Ho3 Ho2 79.81(9) 8_565 . ?
O4 Ho3 Ho1 37.05(10) . . ?
O4 Ho3 Ho1 37.05(10) 8_565 . ?
O4 Ho3 O4 65.89(19) 8_565 . ?
O4 Ho3 O6 112.64(13) 8_565 8_565 ?
O4 Ho3 O6 78.61(13) . 8_565 ?
O4 Ho3 O6 112.64(13) . . ?
O4 Ho3 O6 78.61(13) 8_565 . ?
O4 Ho3 N3 141.29(13) 8_565 . ?
O4 Ho3 N3 141.29(13) . . ?
O4 Ho3 N7 134.43(14) 8_565 . ?
O4 Ho3 N7 134.43(14) . 8_565 ?
O4 Ho3 N7 69.95(14) . . ?
O4 Ho3 N7 69.95(14) 8_565 8_565 ?
O4 Ho3 O3 83.21(15) . . ?
O4 Ho3 O3 83.21(15) 8_565 . ?
O6 Ho3 Ho2 37.37(9) . . ?
O6 Ho3 Ho2 37.37(9) 8_565 . ?
O6 Ho3 Ho1 81.23(9) . . ?
O6 Ho3 Ho1 81.23(9) 8_565 . ?
O6 Ho3 O6 64.75(19) 8_565 . ?
O6 Ho3 N3 101.78(17) . . ?
O6 Ho3 N3 101.78(17) 8_565 . ?
O6 Ho3 N7 130.35(14) . . ?
O6 Ho3 N7 67.72(14) . 8_565 ?
O6 Ho3 N7 67.72(14) 8_565 . ?
O6 Ho3 N7 130.35(14) 8_565 8_565 ?
O6 Ho3 O3 147.62(9) 8_565 . ?
O6 Ho3 O3 147.62(9) . . ?
N3 Ho3 Ho2 123.76(18) . . ?
N3 Ho3 Ho1 176.42(18) . . ?
N3 Ho3 N7 74.50(11) . . ?
N3 Ho3 N7 74.50(11) . 8_565 ?
N7 Ho3 Ho2 103.26(11) . . ?
N7 Ho3 Ho2 103.26(11) 8_565 . ?
N7 Ho3 Ho1 105.11(11) . . ?
N7 Ho3 Ho1 105.11(11) 8_565 . ?
N7 Ho3 N7 147.0(2) . 8_565 ?
O3 Ho3 Ho2 159.73(14) . . ?
O3 Ho3 Ho1 99.91(14) . . ?
O3 Ho3 N3 76.5(2) . . ?
O3 Ho3 N7 80.98(11) . 8_565 ?
O3 Ho3 N7 80.98(11) . . ?
C2 Fe4 C1 176.3(4) . . ?
C2 Fe4 C4 96.3(4) . . ?
C3 Fe4 C1 88.6(3) . . ?
C3 Fe4 C2 87.7(4) . . ?
C3 Fe4 C4 176.0(4) . . ?
C5 Fe4 C1 90.5(2) . . ?
C5 Fe4 C1 90.5(2) 8_565 . ?
C5 Fe4 C2 89.5(2) . . ?
C5 Fe4 C2 89.5(2) 8_565 . ?
C5 Fe4 C3 90.7(3) . . ?
C5 Fe4 C3 90.7(3) 8_565 . ?
C5 Fe4 C5 178.3(5) 8_565 . ?
C5 Fe4 C4 89.4(3) . . ?
C5 Fe4 C4 89.4(3) 8_565 . ?
C4 Fe4 C1 87.3(4) . . ?
Ho3 O4 Ho1 106.15(15) . . ?
C13 O4 Ho1 121.0(3) . . ?
C13 O4 Ho3 119.1(3) . . ?
Ho2 O6 Ho3 104.97(15) . . ?
C16 O6 Ho2 119.4(3) . . ?
C16 O6 Ho3 118.7(3) . . ?
Ho2 O5 Ho1 105.02(16) . . ?
C10 O5 Ho2 120.6(3) . . ?
C10 O5 Ho1 119.7(3) . . ?
C14 N8 Ho1 95.9(3) . . ?
C20 N8 Ho1 115.3(4) . . ?
C20 N8 C14 110.3(5) . . ?
C19 N8 Ho1 117.3(4) . . ?
C19 N8 C14 110.6(5) . . ?
C19 N8 C20 107.0(5) . . ?
C13 C12 C16 113.1(5) . 8_565 ?
N7 C12 C13 109.7(5) . . ?
N7 C12 C16 107.5(5) . 8_565 ?
O4 C13 C12 111.9(5) . . ?
O4 C13 C14 110.9(5) . . ?
C12 C13 C14 110.8(5) . . ?
N8 C14 C13 108.3(5) . . ?
N8 C14 C10 109.8(5) . 8_565 ?
C13 C14 C10 112.1(5) . 8_565 ?
C15 N6 Ho2 95.7(3) . . ?
C6 N6 Ho2 117.1(4) . . ?
C6 N6 C15 110.1(5) . . ?
C6 N6 C7 107.5(5) . . ?
C7 N6 Ho2 115.2(4) . . ?
C7 N6 C15 110.8(5) . . ?
N6 C15 C10 109.3(5) . . ?
N6 C15 C16 108.2(5) . . ?
C10 C15 C16 113.3(5) . . ?
O5 C10 C14 112.0(5) . 8_565 ?
O5 C10 C15 110.9(5) . . ?
C15 C10 C14 110.2(5) . 8_565 ?
O6 C16 C12 111.5(5) . 8_565 ?
O6 C16 C15 112.0(5) . . ?
C12 C16 C15 109.8(5) 8_565 . ?
C3 N3 Ho3 148.5(7) . . ?
N1 C1 Fe4 179.6(7) . . ?
N2 C2 Fe4 173.6(8) . . ?
N3 C3 Fe4 177.4(7) . . ?
C12 N7 Ho3 96.3(3) . . ?
C9 N7 Ho3 116.4(4) . . ?
C9 N7 C12 110.0(5) . . ?
C9 N7 C17 107.0(5) . . ?
C17 N7 Ho3 116.4(4) . . ?
C17 N7 C12 110.3(5) . . ?
C1 N1 Ho1 142.2(7) . 6_655 ?
C2 N2 Ho2 150.3(7) . 6_656 ?
N5 C5 Fe4 178.9(8) . . ?
N4 C4 Fe4 175.4(10) . . ?

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
O3 H3B N4 0.91 2.09 2.821(13) 136.3 3_454
O2 H2B N3 0.88 2.56 3.147(9) 124.7 3_455

_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 0.141 0.750 0.527 119.4 28.1 3H2O
2 0.359 0.250 0.027 119.4 27.7 3H2O
3 0.641 0.750 0.973 119.4 28.7 3H2O
4 0.859 0.250 0.473 119.4 28.3 3H2O

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT213_hofe2               
;
PROBLEM: Atom N4 has ADP max/min Ratio ..... 6.1 prolat 
RESPONSE: Disorder caused by vibration of -CN due to hydrogen bonding to water
molecules coordinated to the trinuclear complex. Attempts to model the -CN
group as split atoms were unfruitful. All of the compounds in this
family share the same characteristics.
;
_vrf_PLAT220_hofe2               
;
PROBLEM: Non-Solvent Resd 1 N Ueq(max)/Ueq(min) Range 8.3 Ratio
RESPONSE: Originated by vibration of the "free" (non covalently bonded
to the lanthanide ions) -CN group
;
_vrf_THETM01_hofe2               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The low value of sine(theta_max)/wavelength results from the exclusion
of low quality reflections in the refinement process.
;
####################################################################### 
# 
# 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_C30H56N12O10Er3Co
_database_code_depnum_ccdc_archive 'CCDC 1561416'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H56 Co Er3 N12 O10'
_chemical_formula_sum            'C30 H56 Co Er3 N12 O10'
_chemical_formula_weight         1305.57
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   24.591(9)
_cell_length_b                   12.863(5)
_cell_length_c                   16.091(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5090(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6561
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.871
_shelx_estimated_absorpt_T_min   0.195
_exptl_absorpt_coefficient_mu    5.269
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1334 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.7302.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.027
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48261
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.841
_diffrn_reflns_theta_min         2.027
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3652
_reflns_number_total             4591
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.146
_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     266
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.061
_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)+(0.0272P)²+1.7834P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C1BA)
Uanis(C8) = Uanis(C2AA)
Uanis(C4) = Uanis(N2)
3.a Rotating group:
 O4(H4a,H4b), O1AA(H1Aa,H1Ab)
3.b Ternary CH refined with riding coordinates:
 C0AA(H0AA), C3AA(H3AA), C2AA(H2AA), C8(H8), C4AA(H4AA), C6(H6), C0BA(H0BA),
 C1BA(H1BA)
3.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6AA(H6Aa,H6Ab,H6Ac), C7AA(H7Aa,H7Ab,H7Ac), C8AA(H8Aa,H8Ab,
 H8Ac), C10(H10a,H10b,H10c), C1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.14673(2) 0.11073(2) 0.79719(2) 0.01136(8) Uani 1 1 d . . . . .
Er2 Er 0.03383(2) 0.2500 0.69759(2) 0.01321(10) Uani 1 2 d S T P . .
O0AA O 0.05386(14) 0.1361(3) 0.80378(19) 0.0148(8) Uani 1 1 d . . . . .
O5 O 0.10383(14) 0.1371(3) 0.67082(19) 0.0131(8) Uani 1 1 d . . . . .
O3 O 0.19447(18) 0.2500 0.7490(3) 0.0127(11) Uani 1 2 d S T P . .
O1 O 0.14126(18) 0.2500 0.8827(3) 0.0136(11) Uani 1 2 d S T P . .
O4 O 0.22773(14) 0.0909(3) 0.8799(2) 0.0173(8) Uani 1 1 d . . . . .
H4A H 0.2259 0.1324 0.9228 0.026 Uiso 1 1 d GR . . . .
H4B H 0.2559 0.1132 0.8520 0.026 Uiso 1 1 d GR . . . .
N7 N 0.0591(2) 0.2500 0.5381(3) 0.0146(14) Uani 1 2 d S T P . .
N9 N -0.0443(2) 0.2500 0.8111(4) 0.0186(15) Uani 1 2 d S T P . .
N0AA N 0.10561(16) 0.0584(3) 0.9431(2) 0.0143(10) Uani 1 1 d . . . . .
C0AA C 0.1201(3) 0.2500 0.5517(4) 0.0137(16) Uani 1 2 d S T P . .
H0AA H 0.1386 0.2500 0.4964 0.016 Uiso 1 2 calc RS T P . .
C3AA C 0.1361(2) 0.1511(4) 0.5986(3) 0.0148(12) Uani 1 1 d . . . . .
H3AA H 0.1292 0.0907 0.5609 0.018 Uiso 1 1 calc R . . . .
C2AA C 0.1967(2) 0.1525(4) 0.6189(3) 0.0123(9) Uani 1 1 d . . . . .
H2AA H 0.2178 0.1479 0.5658 0.015 Uiso 1 1 calc R . . . .
O1AA O -0.02435(15) 0.3794(3) 0.6442(2) 0.0244(9) Uani 1 1 d . . . . .
H1AA H -0.0150 0.4485 0.6276 0.037 Uiso 1 1 d GR . . . .
H1AB H -0.0626 0.3747 0.6341 0.037 Uiso 1 1 d GR . . . .
N8 N 0.20918(16) 0.0583(3) 0.6708(2) 0.0135(9) Uani 1 1 d . . . . .
C8 C 0.2147(3) 0.2500 0.6661(4) 0.0123(9) Uani 1 2 d S T P . .
H8 H 0.2553 0.2500 0.6688 0.015 Uiso 1 2 calc RS T P . .
C5 C 0.1427(2) 0.0476(4) 1.0152(3) 0.0179(12) Uani 1 1 d . . . . .
H5A H 0.1647 -0.0154 1.0086 0.027 Uiso 1 1 calc GR . . . .
H5B H 0.1212 0.0426 1.0664 0.027 Uiso 1 1 calc GR . . . .
H5C H 0.1666 0.1084 1.0182 0.027 Uiso 1 1 calc GR . . . .
C4AA C -0.0065(3) 0.2500 0.8838(4) 0.0164(17) Uani 1 2 d S T P . .
H4AA H -0.0287 0.2500 0.9358 0.020 Uiso 1 2 calc RS T P . .
C6AA C 0.0725(2) -0.0381(4) 0.9408(3) 0.0191(12) Uani 1 1 d . . . . .
H6AA H 0.0535 -0.0427 0.8874 0.029 Uiso 1 1 calc GR . . . .
H6AB H 0.0459 -0.0368 0.9861 0.029 Uiso 1 1 calc GR . . . .
H6AC H 0.0964 -0.0986 0.9474 0.029 Uiso 1 1 calc GR . . . .
C7AA C 0.1938(2) -0.0357(4) 0.6234(3) 0.0223(13) Uani 1 1 d . . . . .
H7AA H 0.2085 -0.0974 0.6511 0.033 Uiso 1 1 calc GR . . . .
H7AB H 0.2085 -0.0311 0.5670 0.033 Uiso 1 1 calc GR . . . .
H7AC H 0.1541 -0.0409 0.6208 0.033 Uiso 1 1 calc GR . . . .
C8AA C 0.2681(2) 0.0510(4) 0.6889(3) 0.0199(13) Uani 1 1 d . . . . .
H8AA H 0.2786 0.1077 0.7263 0.030 Uiso 1 1 calc GR . . . .
H8AB H 0.2887 0.0563 0.6370 0.030 Uiso 1 1 calc GR . . . .
H8AC H 0.2758 -0.0159 0.7156 0.030 Uiso 1 1 calc GR . . . .
C6 C 0.1050(3) 0.2500 0.9522(4) 0.0142(10) Uani 1 2 d S T P . .
H6 H 0.1275 0.2500 1.0040 0.017 Uiso 1 2 calc RS T P . .
C0BA C 0.0282(2) 0.1514(4) 0.8826(3) 0.0147(12) Uani 1 1 d . . . . .
H0BA H 0.0032 0.0911 0.8920 0.018 Uiso 1 1 calc R . . . .
C1BA C 0.0698(2) 0.1511(4) 0.9528(3) 0.0142(10) Uani 1 1 d . . . . .
H1BA H 0.0503 0.1463 1.0072 0.017 Uiso 1 1 calc R . . . .
Co1 Co 0.23310(4) -0.2500 0.84710(6) 0.0143(2) Uani 1 2 d S T P . .
N2 N 0.15405(17) -0.0772(3) 0.8004(2) 0.0157(8) Uani 1 1 d . . . . .
C4 C 0.1838(2) -0.1441(4) 0.8176(3) 0.0157(8) Uani 1 1 d . . . . .
C7 C 0.2829(2) -0.1455(4) 0.8795(3) 0.0160(12) Uani 1 1 d . . . . .
C9 C 0.2648(3) -0.2500 0.7374(5) 0.0193(18) Uani 1 2 d S T P . .
N10 N 0.2828(3) -0.2500 0.6718(4) 0.0263(17) Uani 1 2 d S T P . .
N6 N 0.1786(3) -0.2500 1.0188(4) 0.0283(17) Uani 1 2 d S T P . .
N1AA N 0.31168(19) -0.0783(4) 0.8991(3) 0.0226(11) Uani 1 1 d . . . . .
C1AA C 0.2002(3) -0.2500 0.9552(5) 0.0177(17) Uani 1 2 d S T P . .
C10 C 0.0433(2) 0.3425(4) 0.4893(3) 0.0252(14) Uani 1 1 d . . . . .
H10A H 0.0045 0.3385 0.4757 0.038 Uiso 1 1 calc GR . . . .
H10B H 0.0646 0.3447 0.4378 0.038 Uiso 1 1 calc GR . . . .
H10C H 0.0503 0.4054 0.5219 0.038 Uiso 1 1 calc GR . . . .
C1 C -0.0807(2) 0.3425(4) 0.8137(3) 0.0234(13) Uani 1 1 d . . . . .
H1A H -0.0589 0.4059 0.8085 0.035 Uiso 1 1 calc GR . . . .
H1B H -0.1005 0.3436 0.8666 0.035 Uiso 1 1 calc GR . . . .
H1C H -0.1068 0.3389 0.7676 0.035 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 Er1 3.5826(14) 8_565 ?
Er1 Er2 3.6722(10) . ?
Er1 O0AA 2.309(4) . ?
Er1 O5 2.316(3) . ?
Er1 O3 2.278(3) . ?
Er1 O1 2.263(3) . ?
Er1 O4 2.409(3) . ?
Er1 N0AA 2.643(4) . ?
Er1 N8 2.637(4) . ?
Er1 N2 2.425(5) . ?
Er2 Er1 3.6722(10) 8_565 ?
Er2 O0AA 2.304(3) . ?
Er2 O0AA 2.304(3) 8_565 ?
Er2 O5 2.293(3) . ?
Er2 O5 2.293(3) 8_565 ?
Er2 N7 2.640(6) . ?
Er2 N9 2.651(6) . ?
Er2 O1AA 2.356(4) 8_565 ?
Er2 O1AA 2.356(4) . ?
O0AA C0BA 1.431(5) . ?
O5 C3AA 1.418(6) . ?
O3 Er1 2.278(3) 8_565 ?
O3 C8 1.423(8) . ?
O1 Er1 2.263(3) 8_565 ?
O1 C6 1.431(8) . ?
N7 C0AA 1.514(9) . ?
N7 C10 1.478(6) . ?
N7 C10 1.478(6) 8_565 ?
N9 C4AA 1.495(9) . ?
N9 C1 1.490(6) . ?
N9 C1 1.489(6) 8_565 ?
N0AA C5 1.482(6) . ?
N0AA C6AA 1.485(6) . ?
N0AA C1BA 1.490(6) . ?
C0AA C3AA 1.530(6) 8_565 ?
C0AA C3AA 1.530(6) . ?
C3AA C2AA 1.527(7) . ?
C2AA N8 1.502(6) . ?
C2AA C8 1.532(6) . ?
N8 C7AA 1.479(6) . ?
N8 C8AA 1.480(6) . ?
C8 C2AA 1.532(6) 8_565 ?
C4AA C0BA 1.529(6) 8_565 ?
C4AA C0BA 1.529(6) . ?
C6 C1BA 1.538(6) . ?
C6 C1BA 1.538(6) 8_565 ?
C0BA C1BA 1.525(7) . ?
Co1 C4 1.884(5) . ?
Co1 C4 1.884(6) 8 ?
Co1 C7 1.892(6) . ?
Co1 C7 1.892(6) 8 ?
Co1 C9 1.929(8) . ?
Co1 C1AA 1.918(8) . ?
N2 C4 1.163(7) . ?
C7 N1AA 1.161(7) . ?
C9 N10 1.145(9) . ?
N6 C1AA 1.154(9) . ?

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
Er1 Er1 Er2 60.803(13) 8_565 . ?
O0AA Er1 Er1 81.88(8) . 8_565 ?
O0AA Er1 Er2 37.21(8) . . ?
O0AA Er1 O5 64.48(11) . . ?
O0AA Er1 O4 143.84(11) . . ?
O0AA Er1 N0AA 67.47(12) . . ?
O0AA Er1 N8 130.36(12) . . ?
O0AA Er1 N2 102.31(13) . . ?
O5 Er1 Er1 81.58(8) . 8_565 ?
O5 Er1 Er2 36.96(8) . . ?
O5 Er1 O4 151.29(12) . . ?
O5 Er1 N0AA 130.01(12) . . ?
O5 Er1 N8 67.99(12) . . ?
O5 Er1 N2 101.44(13) . . ?
O3 Er1 Er1 38.16(9) . 8_565 ?
O3 Er1 Er2 81.80(11) . . ?
O3 Er1 O0AA 114.47(13) . . ?
O3 Er1 O5 79.65(14) . . ?
O3 Er1 O4 81.09(14) . . ?
O3 Er1 N0AA 134.42(14) . . ?
O3 Er1 N8 68.78(13) . . ?
O3 Er1 N2 138.84(13) . . ?
O1 Er1 Er1 37.67(9) . 8_565 ?
O1 Er1 Er2 80.46(11) . . ?
O1 Er1 O0AA 78.55(14) . . ?
O1 Er1 O5 113.02(13) . . ?
O1 Er1 O3 67.38(14) . . ?
O1 Er1 O4 78.29(14) . . ?
O1 Er1 N0AA 68.81(13) . . ?
O1 Er1 N8 134.93(14) . . ?
O1 Er1 N2 141.34(13) . . ?
O4 Er1 Er1 96.07(8) . 8_565 ?
O4 Er1 Er2 156.61(8) . . ?
O4 Er1 N0AA 78.40(12) . . ?
O4 Er1 N8 85.26(12) . . ?
O4 Er1 N2 79.72(13) . . ?
N0AA Er1 Er1 104.74(9) . 8_565 ?
N0AA Er1 Er2 102.86(9) . . ?
N8 Er1 Er1 104.81(9) . 8_565 ?
N8 Er1 Er2 103.20(9) . . ?
N8 Er1 N0AA 147.47(13) . . ?
N2 Er1 Er1 175.57(10) . 8_565 ?
N2 Er1 Er2 123.48(10) . . ?
N2 Er1 N0AA 75.88(13) . . ?
N2 Er1 N8 73.62(13) . . ?
Er1 Er2 Er1 58.39(3) 8_565 . ?
O0AA Er2 Er1 37.30(9) 8_565 8_565 ?
O0AA Er2 Er1 79.91(9) 8_565 . ?
O0AA Er2 Er1 79.92(9) . 8_565 ?
O0AA Er2 Er1 37.30(9) . . ?
O0AA Er2 O0AA 78.97(17) . 8_565 ?
O0AA Er2 N7 132.09(10) . . ?
O0AA Er2 N7 132.09(11) 8_565 . ?
O0AA Er2 N9 69.16(13) . . ?
O0AA Er2 N9 69.16(13) 8_565 . ?
O0AA Er2 O1AA 148.12(12) 8_565 8_565 ?
O0AA Er2 O1AA 87.20(12) 8_565 . ?
O0AA Er2 O1AA 148.12(12) . . ?
O0AA Er2 O1AA 87.20(13) . 8_565 ?
O5 Er2 Er1 37.39(8) 8_565 8_565 ?
O5 Er2 Er1 79.82(9) 8_565 . ?
O5 Er2 Er1 37.39(8) . . ?
O5 Er2 Er1 79.82(9) . 8_565 ?
O5 Er2 O0AA 64.92(12) . . ?
O5 Er2 O0AA 112.43(12) . 8_565 ?
O5 Er2 O0AA 112.43(12) 8_565 . ?
O5 Er2 O0AA 64.91(12) 8_565 8_565 ?
O5 Er2 O5 78.59(17) 8_565 . ?
O5 Er2 N7 68.93(12) 8_565 . ?
O5 Er2 N7 68.93(12) . . ?
O5 Er2 N9 132.35(10) 8_565 . ?
O5 Er2 N9 132.35(10) . . ?
O5 Er2 O1AA 146.56(12) 8_565 8_565 ?
O5 Er2 O1AA 86.57(13) 8_565 . ?
O5 Er2 O1AA 146.56(12) . . ?
O5 Er2 O1AA 86.57(13) . 8_565 ?
N7 Er2 Er1 104.24(11) . . ?
N7 Er2 Er1 104.24(11) . 8_565 ?
N7 Er2 N9 147.16(17) . . ?
N9 Er2 Er1 104.33(11) . . ?
N9 Er2 Er1 104.33(11) . 8_565 ?
O1AA Er2 Er1 164.26(9) . . ?
O1AA Er2 Er1 164.26(9) 8_565 8_565 ?
O1AA Er2 Er1 105.88(9) . 8_565 ?
O1AA Er2 Er1 105.88(9) 8_565 . ?
O1AA Er2 N7 77.81(12) . . ?
O1AA Er2 N7 77.81(12) 8_565 . ?
O1AA Er2 N9 79.10(13) . . ?
O1AA Er2 N9 79.10(13) 8_565 . ?
O1AA Er2 O1AA 89.83(18) . 8_565 ?
Er2 O0AA Er1 105.50(13) . . ?
C0BA O0AA Er1 119.8(3) . . ?
C0BA O0AA Er2 118.4(3) . . ?
Er2 O5 Er1 105.65(13) . . ?
C3AA O5 Er1 118.9(3) . . ?
C3AA O5 Er2 119.5(3) . . ?
Er1 O3 Er1 103.69(18) 8_565 . ?
C8 O3 Er1 119.97(19) . 8_565 ?
C8 O3 Er1 119.97(19) . . ?
Er1 O1 Er1 104.67(19) 8_565 . ?
C6 O1 Er1 120.83(17) . 8_565 ?
C6 O1 Er1 120.83(17) . . ?
C0AA N7 Er2 95.3(4) . . ?
C10 N7 Er2 117.1(3) . . ?
C10 N7 Er2 117.1(3) 8_565 . ?
C10 N7 C0AA 109.7(4) . . ?
C10 N7 C0AA 109.7(4) 8_565 . ?
C10 N7 C10 107.2(6) . 8_565 ?
C4AA N9 Er2 95.0(4) . . ?
C1 N9 Er2 117.0(3) . . ?
C1 N9 Er2 117.0(3) 8_565 . ?
C1 N9 C4AA 110.6(4) . . ?
C1 N9 C4AA 110.6(4) 8_565 . ?
C1 N9 C1 106.1(6) 8_565 . ?
C5 N0AA Er1 119.0(3) . . ?
C5 N0AA C6AA 106.1(4) . . ?
C5 N0AA C1BA 110.9(4) . . ?
C6AA N0AA Er1 113.6(3) . . ?
C6AA N0AA C1BA 110.4(4) . . ?
C1BA N0AA Er1 96.6(3) . . ?
N7 C0AA C3AA 109.0(4) . . ?
N7 C0AA C3AA 109.0(4) . 8_565 ?
C3AA C0AA C3AA 112.5(6) 8_565 . ?
O5 C3AA C0AA 111.5(4) . . ?
O5 C3AA C2AA 111.8(4) . . ?
C2AA C3AA C0AA 110.3(4) . . ?
C3AA C2AA C8 113.4(5) . . ?
N8 C2AA C3AA 108.0(4) . . ?
N8 C2AA C8 109.0(4) . . ?
C2AA N8 Er1 96.0(3) . . ?
C7AA N8 Er1 117.2(3) . . ?
C7AA N8 C2AA 108.7(4) . . ?
C7AA N8 C8AA 107.5(4) . . ?
C8AA N8 Er1 115.7(3) . . ?
C8AA N8 C2AA 111.1(4) . . ?
O3 C8 C2AA 111.3(4) . . ?
O3 C8 C2AA 111.3(4) . 8_565 ?
C2AA C8 C2AA 109.9(6) 8_565 . ?
N9 C4AA C0BA 109.7(4) . 8_565 ?
N9 C4AA C0BA 109.7(4) . . ?
C0BA C4AA C0BA 112.2(6) 8_565 . ?
O1 C6 C1BA 110.8(4) . 8_565 ?
O1 C6 C1BA 110.8(4) . . ?
C1BA C6 C1BA 111.6(6) . 8_565 ?
O0AA C0BA C4AA 111.8(4) . . ?
O0AA C0BA C1BA 111.1(4) . . ?
C1BA C0BA C4AA 111.6(4) . . ?
N0AA C1BA C6 109.2(4) . . ?
N0AA C1BA C0BA 108.7(4) . . ?
C0BA C1BA C6 111.8(4) . . ?
C4 Co1 C4 92.5(3) . 8 ?
C4 Co1 C7 88.4(2) 8 8 ?
C4 Co1 C7 178.5(2) . 8 ?
C4 Co1 C7 88.4(2) . . ?
C4 Co1 C7 178.5(2) 8 . ?
C4 Co1 C9 91.7(2) 8 . ?
C4 Co1 C9 91.7(2) . . ?
C4 Co1 C1AA 87.6(2) 8 . ?
C4 Co1 C1AA 87.6(2) . . ?
C7 Co1 C7 90.6(3) . 8 ?
C7 Co1 C9 89.4(2) 8 . ?
C7 Co1 C9 89.4(2) . . ?
C7 Co1 C1AA 91.3(2) 8 . ?
C7 Co1 C1AA 91.3(2) . . ?
C1AA Co1 C9 178.9(3) . . ?
C4 N2 Er1 142.2(4) . . ?
N2 C4 Co1 178.5(5) . . ?
N1AA C7 Co1 177.1(5) . . ?
N10 C9 Co1 178.8(7) . . ?
N6 C1AA Co1 177.5(7) . . ?

_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 -0.035 0.250 0.349 345.1 101.4 10H2O
2 0.035 -0.250 0.651 345.1 103.2 10H2O
3 0.465 0.250 0.151 345.1 100.4 10H2O
4 0.535 0.750 0.849 345.1 104.2 10H2O

_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_C30H54N12O9Er3Fe
_database_code_depnum_ccdc_archive 'CCDC 1561423'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H108 Er6 Fe2 N24 O18)'
_chemical_formula_sum            'C30 H54 Er3 Fe N12 O9'
_chemical_formula_weight         1284.48
_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'
Er Er -0.2586 4.9576 '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'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   16.239(4)
_cell_length_b                   18.833(4)
_cell_length_c                   14.043(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4294.8(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7784
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.768
_shelx_estimated_absorpt_T_min   0.549
_exptl_absorpt_coefficient_mu    6.193
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1066 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.7504.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.045
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39578
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.406
_diffrn_reflns_theta_min         2.163
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3123
_reflns_number_total             3633
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0261
_refine_ls_restrained_S_all      1.031
_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)+(0.0190P)²+19.3517P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0575
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1a(0.5) H1b(0.5) H3a(0.5) H3b(0.5) H2a(0.5) H2b(0.5)
3.a Rotating group:
 O1(H1a,H1b), O3(H3a,H3b), O2(H2a,H2b)
3.b Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C17(H17)
3.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C14(H14a,H14b,
 H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.12000(2) 0.7500 0.42212(2) 0.01589(9) Uani 1 2 d S T P . .
Er2 Er 0.17365(2) 0.7500 0.67286(2) 0.01601(10) Uani 1 2 d S T P . .
Er3 Er 0.33500(2) 0.7500 0.49086(2) 0.01243(9) Uani 1 2 d S T P . .
Fe1 Fe 0.16029(6) 0.7500 0.05225(7) 0.0168(2) Uani 1 2 d S T P . .
O5 O 0.1108(2) 0.68322(19) 0.5582(2) 0.0166(8) Uani 1 1 d . . . . .
O6 O 0.28250(19) 0.68400(18) 0.6168(2) 0.0141(7) Uani 1 1 d . . . . .
N8 N 0.0917(3) 0.6139(3) 0.3815(3) 0.0209(10) Uani 1 1 d . . . . .
C6 C 0.1228(3) 0.6090(3) 0.5539(3) 0.0208(12) Uani 1 1 d . . . . .
H6 H 0.0693 0.5854 0.5691 0.025 Uiso 1 1 calc R . . . .
C7 C 0.1860(3) 0.5856(3) 0.6281(4) 0.0202(12) Uani 1 1 d . . . . .
H7 H 0.1852 0.5326 0.6321 0.024 Uiso 1 1 calc R . . . .
C8 C 0.1497(3) 0.5847(3) 0.4541(4) 0.0201(12) Uani 1 1 d . . . . .
H8 H 0.1483 0.5317 0.4514 0.024 Uiso 1 1 calc R . . . .
C9 C 0.2982(3) 0.5862(3) 0.5047(4) 0.0170(11) Uani 1 1 d . . . . .
H9 H 0.3026 0.5332 0.5032 0.020 Uiso 1 1 calc R . . . .
N7 N 0.3810(2) 0.6178(2) 0.4830(3) 0.0185(10) Uani 1 1 d . . . . .
C10 C 0.2742(3) 0.6096(3) 0.6045(3) 0.0149(11) Uani 1 1 d . . . . .
H10 H 0.3123 0.5858 0.6504 0.018 Uiso 1 1 calc R . . . .
N6 N 0.1628(3) 0.6151(2) 0.7232(3) 0.0207(10) Uani 1 1 d . . . . .
C11 C 0.4409(3) 0.5941(3) 0.5558(4) 0.0233(13) Uani 1 1 d . . . . .
H11A H 0.4968 0.6057 0.5348 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.4360 0.5427 0.5648 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.4294 0.6183 0.6162 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.4112(3) 0.5911(3) 0.3905(4) 0.0259(13) Uani 1 1 d . . . . .
H12A H 0.3751 0.6081 0.3394 0.039 Uiso 1 1 calc GR . . . .
H12B H 0.4113 0.5391 0.3910 0.039 Uiso 1 1 calc GR . . . .
H12C H 0.4673 0.6085 0.3795 0.039 Uiso 1 1 calc GR . . . .
C13 C 0.2203(3) 0.5887(3) 0.7970(4) 0.0227(13) Uani 1 1 d . . . . .
H13A H 0.2748 0.6098 0.7870 0.034 Uiso 1 1 calc GR . . . .
H13B H 0.2244 0.5369 0.7926 0.034 Uiso 1 1 calc GR . . . .
H13C H 0.1998 0.6020 0.8601 0.034 Uiso 1 1 calc GR . . . .
C14 C 0.1163(4) 0.5909(3) 0.2847(4) 0.0285(14) Uani 1 1 d . . . . .
H14A H 0.0757 0.6078 0.2383 0.043 Uiso 1 1 calc GR . . . .
H14B H 0.1191 0.5389 0.2824 0.043 Uiso 1 1 calc GR . . . .
H14C H 0.1705 0.6107 0.2693 0.043 Uiso 1 1 calc GR . . . .
C15 C 0.0790(3) 0.5902(4) 0.7507(4) 0.0317(15) Uani 1 1 d . . . . .
H15A H 0.0683 0.6027 0.8173 0.048 Uiso 1 1 calc GR . . . .
H15B H 0.0757 0.5385 0.7432 0.048 Uiso 1 1 calc GR . . . .
H15C H 0.0378 0.6129 0.7098 0.048 Uiso 1 1 calc GR . . . .
C16 C 0.0078(3) 0.5869(4) 0.3979(4) 0.0381(17) Uani 1 1 d . . . . .
H16A H -0.0123 0.6040 0.4596 0.057 Uiso 1 1 calc GR . . . .
H16B H 0.0085 0.5349 0.3979 0.057 Uiso 1 1 calc GR . . . .
H16C H -0.0286 0.6039 0.3472 0.057 Uiso 1 1 calc GR . . . .
O4 O 0.23803(19) 0.81559(18) 0.4158(2) 0.0146(8) Uani 1 1 d . . . . .
C17 C 0.2369(3) 0.8898(3) 0.4289(3) 0.0170(11) Uani 1 1 d . . . . .
H17 H 0.2529 0.9124 0.3672 0.020 Uiso 1 1 calc R . . . .
N1 N 0.0855(4) 0.7500 0.2537(4) 0.0215(15) Uani 1 2 d S T P . .
C1 C 0.1140(4) 0.7500 0.1781(5) 0.0151(16) Uani 1 2 d S T P . .
C2 C 0.2007(4) 0.7500 -0.0774(5) 0.0194(17) Uani 1 2 d S T P . .
C3 C 0.0508(4) 0.7500 0.0013(5) 0.0173(16) Uani 1 2 d S T P . .
C5 C 0.1612(5) 0.8527(4) 0.0509(4) 0.0428(18) Uani 1 1 d . . . . .
O1 O -0.0255(3) 0.7500 0.4374(4) 0.0438(18) Uani 1 2 d S T P . .
H1A H -0.0400 0.7339 0.4944 0.066 Uiso 0.5 1 d GR . . . .
H1B H -0.0477 0.7190 0.3975 0.066 Uiso 0.5 1 d GR . . . .
N3 N -0.0166(4) 0.7500 -0.0249(4) 0.0188(14) Uani 1 2 d S T P . .
N2 N 0.2153(4) 0.7500 -0.1581(4) 0.0200(14) Uani 1 2 d S T P . .
C4 C 0.2663(6) 0.7500 0.1130(6) 0.061(4) Uani 1 2 d S T P . .
O3 O 0.3988(3) 0.7500 0.3359(3) 0.0234(13) Uani 1 2 d S T P . .
H3A H 0.4465 0.7750 0.3362 0.035 Uiso 0.5 1 d GR . . . .
H3B H 0.3678 0.7738 0.2927 0.035 Uiso 0.5 1 d GR . . . .
N5 N 0.1622(7) 0.9131(4) 0.0498(5) 0.110(4) Uani 1 1 d . . . . .
N4 N 0.3270(5) 0.7500 0.1545(6) 0.134(7) Uani 1 2 d S T P . .
O2 O 0.0488(3) 0.7500 0.7616(4) 0.0274(13) Uani 1 2 d S T P . .
H2A H 0.0103 0.7733 0.7303 0.041 Uiso 0.5 1 d GR . . . .
H2B H 0.0550 0.7746 0.8145 0.041 Uiso 0.5 1 d GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 Er2 3.6273(9) . ?
Er1 Er3 3.6225(9) . ?
Er1 O5 2.293(3) 8_575 ?
Er1 O5 2.293(3) . ?
Er1 N8 2.666(5) . ?
Er1 N8 2.666(5) 8_575 ?
Er1 O4 2.282(3) . ?
Er1 O4 2.282(3) 8_575 ?
Er1 N1 2.431(6) . ?
Er1 O1 2.372(6) . ?
Er2 Er3 3.6603(7) . ?
Er2 O5 2.284(3) 8_575 ?
Er2 O5 2.284(3) . ?
Er2 O6 2.300(3) 8_575 ?
Er2 O6 2.300(3) . ?
Er2 N6 2.643(5) 8_575 ?
Er2 N6 2.643(5) . ?
Er2 N2 2.468(6) 1_556 ?
Er2 O2 2.381(5) . ?
Er3 O6 2.323(3) 8_575 ?
Er3 O6 2.323(3) . ?
Er3 N7 2.602(5) 8_575 ?
Er3 N7 2.602(5) . ?
Er3 O4 2.262(3) 8_575 ?
Er3 O4 2.262(3) . ?
Er3 N3 2.456(6) 6_656 ?
Er3 O3 2.410(5) . ?
Fe1 C1 1.920(7) . ?
Fe1 C2 1.936(8) . ?
Fe1 C3 1.916(8) . ?
Fe1 C5 1.934(8) 8_575 ?
Fe1 C5 1.933(8) . ?
Fe1 C4 1.921(10) . ?
O5 C6 1.413(7) . ?
O6 C10 1.418(6) . ?
N8 C8 1.493(6) . ?
N8 C14 1.482(7) . ?
N8 C16 1.472(7) . ?
C6 C7 1.528(7) . ?
C6 C8 1.536(7) . ?
C7 C10 1.537(7) . ?
C7 N6 1.495(7) . ?
C8 C17 1.536(7) 8_575 ?
C9 N7 1.503(6) . ?
C9 C10 1.519(7) . ?
C9 C17 1.527(7) 8_575 ?
N7 C11 1.480(6) . ?
N7 C12 1.477(6) . ?
N6 C13 1.481(6) . ?
N6 C15 1.491(7) . ?
O4 C17 1.409(6) . ?
C17 C8 1.536(7) 8_575 ?
C17 C9 1.527(7) 8_575 ?
N1 C1 1.158(9) . ?
C2 N2 1.158(9) . ?
C3 N3 1.155(9) . ?
C5 N5 1.138(10) . ?
N3 Er3 2.456(6) 6_556 ?
N2 Er2 2.468(6) 1_554 ?
C4 N4 1.146(12) . ?

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
Er3 Er1 Er2 60.647(8) . . ?
O5 Er1 Er2 37.48(9) 8_575 . ?
O5 Er1 Er2 37.48(9) . . ?
O5 Er1 Er3 80.83(8) 8_575 . ?
O5 Er1 Er3 80.83(8) . . ?
O5 Er1 O5 66.53(18) 8_575 . ?
O5 Er1 N8 133.98(13) 8_575 . ?
O5 Er1 N8 133.98(13) . 8_575 ?
O5 Er1 N8 68.87(13) . . ?
O5 Er1 N8 68.87(13) 8_575 8_575 ?
O5 Er1 N1 142.76(11) . . ?
O5 Er1 N1 142.76(11) 8_575 . ?
O5 Er1 O1 81.92(14) . . ?
O5 Er1 O1 81.92(14) 8_575 . ?
N8 Er1 Er2 104.41(9) . . ?
N8 Er1 Er2 104.41(9) 8_575 . ?
N8 Er1 Er3 102.88(9) 8_575 . ?
N8 Er1 Er3 102.88(9) . . ?
N8 Er1 N8 148.15(18) 8_575 . ?
O4 Er1 Er2 80.56(8) . . ?
O4 Er1 Er2 80.56(8) 8_575 . ?
O4 Er1 Er3 36.95(8) . . ?
O4 Er1 Er3 36.95(8) 8_575 . ?
O4 Er1 O5 112.58(12) 8_575 8_575 ?
O4 Er1 O5 77.89(12) 8_575 . ?
O4 Er1 O5 77.89(12) . 8_575 ?
O4 Er1 O5 112.58(12) . . ?
O4 Er1 N8 67.40(12) 8_575 . ?
O4 Er1 N8 67.40(12) . 8_575 ?
O4 Er1 N8 131.06(12) . . ?
O4 Er1 N8 131.06(12) 8_575 8_575 ?
O4 Er1 O4 65.55(16) 8_575 . ?
O4 Er1 N1 98.97(15) 8_575 . ?
O4 Er1 N1 98.97(15) . . ?
O4 Er1 O1 147.14(8) . . ?
O4 Er1 O1 147.14(8) 8_575 . ?
N1 Er1 Er2 179.44(15) . . ?
N1 Er1 Er3 118.79(15) . . ?
N1 Er1 N8 75.66(9) . . ?
N1 Er1 N8 75.66(9) . 8_575 ?
O1 Er1 Er2 98.69(14) . . ?
O1 Er1 Er3 159.34(14) . . ?
O1 Er1 N8 81.26(10) . 8_575 ?
O1 Er1 N8 81.26(10) . . ?
O1 Er1 N1 81.9(2) . . ?
Er1 Er2 Er3 59.612(16) . . ?
O5 Er2 Er1 37.66(8) 8_575 . ?
O5 Er2 Er1 37.66(8) . . ?
O5 Er2 Er3 80.08(8) 8_575 . ?
O5 Er2 Er3 80.08(8) . . ?
O5 Er2 O5 66.83(17) . 8_575 ?
O5 Er2 O6 113.56(12) . 8_575 ?
O5 Er2 O6 78.72(12) . . ?
O5 Er2 O6 113.56(12) 8_575 . ?
O5 Er2 O6 78.72(12) 8_575 8_575 ?
O5 Er2 N6 68.24(12) 8_575 8_575 ?
O5 Er2 N6 133.48(13) . 8_575 ?
O5 Er2 N6 68.24(12) . . ?
O5 Er2 N6 133.48(13) 8_575 . ?
O5 Er2 N2 143.17(10) 8_575 1_556 ?
O5 Er2 N2 143.17(10) . 1_556 ?
O5 Er2 O2 89.33(14) . . ?
O5 Er2 O2 89.33(14) 8_575 . ?
O6 Er2 Er1 81.50(8) 8_575 . ?
O6 Er2 Er1 81.50(8) . . ?
O6 Er2 Er3 37.88(8) . . ?
O6 Er2 Er3 37.88(8) 8_575 . ?
O6 Er2 O6 65.42(17) . 8_575 ?
O6 Er2 N6 131.48(12) 8_575 . ?
O6 Er2 N6 67.88(12) 8_575 8_575 ?
O6 Er2 N6 131.48(12) . 8_575 ?
O6 Er2 N6 67.88(12) . . ?
O6 Er2 N2 96.83(14) . 1_556 ?
O6 Er2 N2 96.83(14) 8_575 1_556 ?
O6 Er2 O2 146.52(9) . . ?
O6 Er2 O2 146.52(9) 8_575 . ?
N6 Er2 Er1 104.10(9) . . ?
N6 Er2 Er1 104.10(9) 8_575 . ?
N6 Er2 Er3 103.57(9) 8_575 . ?
N6 Er2 Er3 103.57(9) . . ?
N6 Er2 N6 147.99(19) . 8_575 ?
N2 Er2 Er1 178.00(14) 1_556 . ?
N2 Er2 Er3 118.39(14) 1_556 . ?
N2 Er2 N6 76.18(9) 1_556 8_575 ?
N2 Er2 N6 76.17(9) 1_556 . ?
O2 Er2 Er1 107.68(13) . . ?
O2 Er2 Er3 167.29(13) . . ?
O2 Er2 N6 78.64(10) . 8_575 ?
O2 Er2 N6 78.64(10) . . ?
O2 Er2 N2 74.32(19) . 1_556 ?
Er1 Er3 Er2 59.741(16) . . ?
O6 Er3 Er1 81.32(8) 8_575 . ?
O6 Er3 Er1 81.32(8) . . ?
O6 Er3 Er2 37.43(8) . . ?
O6 Er3 Er2 37.43(8) 8_575 . ?
O6 Er3 O6 64.68(17) . 8_575 ?
O6 Er3 N7 68.03(12) 8_575 8_575 ?
O6 Er3 N7 68.03(12) . . ?
O6 Er3 N7 130.52(12) 8_575 . ?
O6 Er3 N7 130.52(12) . 8_575 ?
O6 Er3 N3 102.24(14) 8_575 6_656 ?
O6 Er3 N3 102.24(14) . 6_656 ?
O6 Er3 O3 147.66(8) . . ?
O6 Er3 O3 147.66(8) 8_575 . ?
N7 Er3 Er1 105.41(9) 8_575 . ?
N7 Er3 Er1 105.41(9) . . ?
N7 Er3 Er2 103.62(9) . . ?
N7 Er3 Er2 103.62(9) 8_575 . ?
N7 Er3 N7 146.22(18) . 8_575 ?
O4 Er3 Er1 37.33(8) . . ?
O4 Er3 Er1 37.33(8) 8_575 . ?
O4 Er3 Er2 80.03(8) 8_575 . ?
O4 Er3 Er2 80.03(8) . . ?
O4 Er3 O6 113.03(12) . . ?
O4 Er3 O6 78.87(11) . 8_575 ?
O4 Er3 O6 78.87(11) 8_575 . ?
O4 Er3 O6 113.03(12) 8_575 8_575 ?
O4 Er3 N7 134.65(12) 8_575 8_575 ?
O4 Er3 N7 134.65(12) . . ?
O4 Er3 N7 69.98(12) . 8_575 ?
O4 Er3 N7 69.98(12) 8_575 . ?
O4 Er3 O4 66.20(17) . 8_575 ?
O4 Er3 N3 140.67(11) . 6_656 ?
O4 Er3 N3 140.67(11) 8_575 6_656 ?
O4 Er3 O3 83.03(13) . . ?
O4 Er3 O3 83.03(13) 8_575 . ?
N3 Er3 Er1 175.75(14) 6_656 . ?
N3 Er3 Er2 124.50(14) 6_656 . ?
N3 Er3 N7 74.12(9) 6_656 . ?
N3 Er3 N7 74.12(9) 6_656 8_575 ?
O3 Er3 Er1 100.01(12) . . ?
O3 Er3 Er2 159.75(12) . . ?
O3 Er3 N7 80.68(10) . . ?
O3 Er3 N7 80.68(10) . 8_575 ?
O3 Er3 N3 75.75(18) . 6_656 ?
C1 Fe1 C2 176.8(3) . . ?
C1 Fe1 C5 90.71(17) . . ?
C1 Fe1 C5 90.71(17) . 8_575 ?
C1 Fe1 C4 86.7(3) . . ?
C3 Fe1 C1 88.9(3) . . ?
C3 Fe1 C2 87.9(3) . . ?
C3 Fe1 C5 90.2(2) . . ?
C3 Fe1 C5 90.2(2) . 8_575 ?
C3 Fe1 C4 175.6(3) . . ?
C5 Fe1 C2 89.30(17) . . ?
C5 Fe1 C2 89.30(17) 8_575 . ?
C5 Fe1 C5 178.5(4) . 8_575 ?
C4 Fe1 C2 96.5(3) . . ?
C4 Fe1 C5 89.8(2) . 8_575 ?
C4 Fe1 C5 89.8(2) . . ?
Er2 O5 Er1 104.86(14) . . ?
C6 O5 Er1 119.8(3) . . ?
C6 O5 Er2 120.9(3) . . ?
Er2 O6 Er3 104.69(13) . . ?
C10 O6 Er2 120.1(3) . . ?
C10 O6 Er3 118.1(3) . . ?
C8 N8 Er1 95.7(3) . . ?
C14 N8 Er1 115.5(3) . . ?
C14 N8 C8 110.5(4) . . ?
C16 N8 Er1 117.2(4) . . ?
C16 N8 C8 110.5(4) . . ?
C16 N8 C14 107.0(4) . . ?
O5 C6 C7 110.4(4) . . ?
O5 C6 C8 111.9(4) . . ?
C7 C6 C8 110.2(4) . . ?
C6 C7 C10 113.1(4) . . ?
N6 C7 C6 109.4(4) . . ?
N6 C7 C10 108.6(4) . . ?
N8 C8 C6 109.5(4) . . ?
N8 C8 C17 108.0(4) . 8_575 ?
C17 C8 C6 112.3(4) 8_575 . ?
N7 C9 C10 107.6(4) . . ?
N7 C9 C17 109.0(4) . 8_575 ?
C10 C9 C17 112.9(4) . 8_575 ?
C9 N7 Er3 96.5(3) . . ?
C11 N7 Er3 116.6(3) . . ?
C11 N7 C9 109.2(4) . . ?
C12 N7 Er3 117.3(3) . . ?
C12 N7 C9 110.0(4) . . ?
C12 N7 C11 106.7(4) . . ?
O6 C10 C7 110.7(4) . . ?
O6 C10 C9 112.0(4) . . ?
C9 C10 C7 110.7(4) . . ?
C7 N6 Er2 95.8(3) . . ?
C13 N6 Er2 117.9(3) . . ?
C13 N6 C7 109.9(4) . . ?
C13 N6 C15 106.8(4) . . ?
C15 N6 Er2 115.7(3) . . ?
C15 N6 C7 110.2(4) . . ?
Er3 O4 Er1 105.73(13) . . ?
C17 O4 Er1 121.3(3) . . ?
C17 O4 Er3 119.3(3) . . ?
C9 C17 C8 110.3(4) 8_575 8_575 ?
O4 C17 C8 110.7(4) . 8_575 ?
O4 C17 C9 112.1(4) . 8_575 ?
C1 N1 Er1 143.1(6) . . ?
N1 C1 Fe1 179.4(6) . . ?
N2 C2 Fe1 171.9(6) . . ?
N3 C3 Fe1 176.6(6) . . ?
N5 C5 Fe1 179.6(9) . . ?
C3 N3 Er3 150.2(5) . 6_556 ?
C2 N2 Er2 152.3(6) . 1_554 ?
N4 C4 Fe1 175.7(8) . . ?

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
O3 H3B N4 0.91 2.10 2.801(10) 133.4 .
O2 H2B N3 0.88 2.58 3.181(7) 126.2 1_556

_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 0.134 0.250 0.451 131.7 30.3 3H2O
2 -0.134 0.750 0.549 131.7 29.5 3H2O
3 0.366 0.750 -0.049 131.7 30.1 3H2O
4 0.634 0.250 0.049 131.7 29.7 3H2O

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT213_erfe                
;
PROBLEM: Atom N4 has ADP max/min Ratio ..... 6.1 prolat 
RESPONSE: Disorder caused by vibration of -CN due to hydrogen bonding to water
molecules coordinated to the trinuclear complex. Attempts to model the -CN
group as split atoms were unfruitful. All of the compounds in this
family share the same characteristics.
;
_vrf_PLAT220_erfe                
;
PROBLEM: Non-Solvent Resd 1 N Ueq(max)/Ueq(min) Range 8.3 Ratio
RESPONSE: Originated by vibration of the "free" (non covalently bonded
to the lanthanide ions) -CN group
;
####################################################################### 
# 
# 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_C30H56N12O10Y3Co
_database_code_depnum_ccdc_archive 'CCDC 1561422'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H56 Co N12 O10 Y3'
_chemical_formula_sum            'C30 H56 Co N12 O10 Y3'
_chemical_formula_weight         1070.52
_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'
Co Co 0.3494 0.9721 '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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   24.568(14)
_cell_length_b                   12.893(7)
_cell_length_c                   16.127(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5109(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1436 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.5723.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.024
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57895
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.084
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4922
_reflns_number_total             5815
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.051
_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)+(0.0384P)²+6.2447P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0808
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O1(H1a,H1b), O2(H2a,H2b)
2.b Ternary CH refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15)
2.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C7(H7a,H7b,H7c), C14(H14a,H14b,H14c), C16(H16a,H16b,H16c),
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.35293(2) 0.11061(2) 0.29736(2) 0.01006(7) Uani 1 1 d . . . . .
Y2 Y 0.46636(2) 0.2500 0.19740(2) 0.01258(8) Uani 1 2 d S T P . .
Co1 Co 0.26664(2) -0.2500 0.34679(3) 0.01248(11) Uani 1 2 d S T P . .
O4 O 0.44651(7) 0.36356(14) 0.30402(10) 0.0139(3) Uani 1 1 d . . . . .
O5 O 0.30503(10) 0.2500 0.24892(13) 0.0113(5) Uani 1 2 d S T P . .
O6 O 0.35877(9) 0.2500 0.38314(14) 0.0117(5) Uani 1 2 d S T P . .
O3 O 0.39569(7) 0.36315(13) 0.17096(10) 0.0135(3) Uani 1 1 d . . . . .
N5 N 0.39439(8) 0.05881(16) 0.44341(12) 0.0143(4) Uani 1 1 d . . . . .
N1 N 0.34563(9) -0.07832(17) 0.30023(13) 0.0170(4) Uani 1 1 d . . . . .
C1 C 0.31618(10) -0.35470(18) 0.31641(14) 0.0130(5) Uani 1 1 d . . . . .
O1 O 0.27167(7) 0.09144(13) 0.37975(11) 0.0165(4) Uani 1 1 d . . . . .
H1A H 0.2744 0.1291 0.4247 0.025 Uiso 1 1 d GR . . . .
H1B H 0.2694 0.0277 0.3982 0.025 Uiso 1 1 d GR . . . .
C5 C 0.42720(11) -0.0380(2) 0.44106(16) 0.0199(5) Uani 1 1 d . . . . .
H5A H 0.4029 -0.0982 0.4431 0.030 Uiso 1 1 calc GR . . . .
H5B H 0.4518 -0.0397 0.4888 0.030 Uiso 1 1 calc GR . . . .
H5C H 0.4485 -0.0400 0.3897 0.030 Uiso 1 1 calc GR . . . .
C4 C 0.21707(10) -0.35472(19) 0.37935(15) 0.0152(5) Uani 1 1 d . . . . .
N4 N 0.18796(9) -0.07913(17) 0.39846(14) 0.0225(5) Uani 1 1 d . . . . .
N8 N 0.44024(13) 0.2500 0.03769(18) 0.0178(6) Uani 1 2 d S T P . .
C6 C 0.37956(14) 0.2500 0.0517(2) 0.0140(7) Uani 1 2 d S T P . .
H6 H 0.3610 0.2500 -0.0034 0.017 Uiso 1 2 calc RS T P . .
N2 N 0.32099(14) -0.2500 0.5179(2) 0.0260(7) Uani 1 2 d S T P . .
C3 C 0.23557(16) -0.2500 0.2378(2) 0.0184(7) Uani 1 2 d S T P . .
C7 C 0.35709(10) 0.0482(2) 0.51509(15) 0.0186(5) Uani 1 1 d . . . . .
H7A H 0.3337 0.1096 0.5186 0.028 Uiso 1 1 calc GR . . . .
H7B H 0.3784 0.0417 0.5662 0.028 Uiso 1 1 calc GR . . . .
H7C H 0.3345 -0.0138 0.5079 0.028 Uiso 1 1 calc GR . . . .
C8 C 0.50671(14) -0.7500 0.3840(2) 0.0141(7) Uani 1 2 d S T P . .
H8 H 0.5289 -0.7500 0.4360 0.017 Uiso 1 2 calc RS T P . .
C9 C 0.36345(10) 0.34884(19) 0.09812(14) 0.0134(5) Uani 1 1 d . . . . .
H9 H 0.3703 0.4090 0.0604 0.016 Uiso 1 1 calc R . . . .
C10 C 0.30261(10) 0.15226(18) 0.11917(14) 0.0127(5) Uani 1 1 d . . . . .
H10 H 0.2813 0.1477 0.0664 0.015 Uiso 1 1 calc R . . . .
N6 N 0.29044(8) 0.05894(15) 0.17051(12) 0.0140(4) Uani 1 1 d . . . . .
N3 N 0.21699(15) -0.2500 0.1721(2) 0.0265(8) Uani 1 2 d S T P . .
C2 C 0.29940(15) -0.2500 0.4546(2) 0.0168(7) Uani 1 2 d S T P . .
C11 C 0.28491(14) 0.2500 0.1662(2) 0.0122(7) Uani 1 2 d S T P . .
H11 H 0.2443 0.2500 0.1689 0.015 Uiso 1 2 calc RS T P . .
N7 N 0.54437(12) -0.7500 0.31096(18) 0.0169(6) Uani 1 2 d S T P . .
C12 C 0.39464(14) 0.2500 0.4521(2) 0.0120(6) Uani 1 2 d S T P . .
H12 H 0.3721 0.2500 0.5038 0.014 Uiso 1 2 calc RS T P . .
C13 C 0.47215(10) 0.34884(19) 0.38189(14) 0.0138(5) Uani 1 1 d . . . . .
H13 H 0.4971 0.4090 0.3913 0.017 Uiso 1 1 calc R . . . .
C14 C 0.58075(11) -0.8421(2) 0.31402(17) 0.0217(6) Uani 1 1 d . . . . .
H14A H 0.5591 -0.9052 0.3063 0.033 Uiso 1 1 calc GR . . . .
H14B H 0.5991 -0.8447 0.3679 0.033 Uiso 1 1 calc GR . . . .
H14C H 0.6080 -0.8371 0.2698 0.033 Uiso 1 1 calc GR . . . .
C15 C 0.43014(10) 0.15175(19) 0.45251(14) 0.0139(5) Uani 1 1 d . . . . .
H15 H 0.4498 0.1473 0.5067 0.017 Uiso 1 1 calc R . . . .
O2 O 0.52472(8) 0.12053(15) 0.14413(12) 0.0253(4) Uani 1 1 d . . . . .
H2A H 0.5171 0.0503 0.1365 0.038 Uiso 1 1 d GR . . . .
H2B H 0.5606 0.1279 0.1260 0.038 Uiso 1 1 d GR . . . .
C16 C 0.30533(12) -0.03593(19) 0.12359(16) 0.0206(6) Uani 1 1 d . . . . .
H16A H 0.3451 -0.0414 0.1202 0.031 Uiso 1 1 calc GR . . . .
H16B H 0.2900 -0.0320 0.0676 0.031 Uiso 1 1 calc GR . . . .
H16C H 0.2907 -0.0970 0.1521 0.031 Uiso 1 1 calc GR . . . .
C17 C 0.45664(12) 0.3421(2) -0.01094(17) 0.0270(6) Uani 1 1 d . . . . .
H17A H 0.4501 0.4049 0.0218 0.040 Uiso 1 1 calc GR . . . .
H17B H 0.4353 0.3451 -0.0622 0.040 Uiso 1 1 calc GR . . . .
H17C H 0.4954 0.3373 -0.0246 0.040 Uiso 1 1 calc GR . . . .
C18 C 0.23137(11) 0.0520(2) 0.18890(16) 0.0188(5) Uani 1 1 d . . . . .
H18A H 0.2237 -0.0138 0.2170 0.028 Uiso 1 1 calc GR . . . .
H18B H 0.2107 0.0554 0.1370 0.028 Uiso 1 1 calc GR . . . .
H18C H 0.2207 0.1098 0.2249 0.028 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 Y1 3.594(2) 8_565 ?
Y1 Y2 3.6870(14) . ?
Y1 O4 2.326(2) 8_565 ?
Y1 O5 2.2859(17) . ?
Y1 O6 2.2725(17) . ?
Y1 O3 2.318(2) 8_565 ?
Y1 N5 2.652(2) . ?
Y1 N1 2.443(3) . ?
Y1 O1 2.411(2) . ?
Y1 N6 2.643(2) . ?
Y2 Y1 3.6871(14) 8_565 ?
Y2 O4 2.3105(19) 8_565 ?
Y2 O4 2.3105(19) . ?
Y2 O3 2.3075(19) 8_565 ?
Y2 O3 2.3075(19) . ?
Y2 N8 2.654(3) . ?
Y2 N7 2.651(3) 1_565 ?
Y2 O2 2.362(2) . ?
Y2 O2 2.362(2) 8_565 ?
Co1 C1 1.882(3) 8 ?
Co1 C1 1.883(3) . ?
Co1 C4 1.893(3) 8 ?
Co1 C4 1.893(3) . ?
Co1 C3 1.916(4) . ?
Co1 C2 1.915(4) . ?
O4 Y1 2.326(2) 8_565 ?
O4 C13 1.418(3) . ?
O5 Y1 2.2859(17) 8_565 ?
O5 C11 1.423(4) . ?
O6 Y1 2.2725(17) 8_565 ?
O6 C12 1.419(4) . ?
O3 Y1 2.318(2) 8_565 ?
O3 C9 1.429(3) . ?
N5 C5 1.486(3) . ?
N5 C7 1.482(3) . ?
N5 C15 1.493(3) . ?
N1 C1 1.156(3) 8 ?
C1 N1 1.156(3) 8 ?
C4 N4 1.155(3) 8 ?
N4 C4 1.155(3) 8 ?
N8 C6 1.508(5) . ?
N8 C17 1.479(3) 8_565 ?
N8 C17 1.479(3) . ?
C6 C9 1.530(3) 8_565 ?
C6 C9 1.530(3) . ?
N2 C2 1.152(5) . ?
C3 N3 1.154(5) . ?
C8 N7 1.498(4) . ?
C8 C13 1.532(3) 1_545 ?
C8 C13 1.532(3) 8 ?
C9 C10 1.533(3) 8_565 ?
C10 C9 1.533(3) 8_565 ?
C10 N6 1.491(3) . ?
C10 C11 1.533(3) . ?
N6 C16 1.484(3) . ?
N6 C18 1.484(3) . ?
C11 C10 1.533(3) 8_565 ?
N7 Y2 2.651(3) 1_545 ?
N7 C14 1.487(3) . ?
N7 C14 1.487(3) 8_545 ?
C12 C15 1.538(3) 8_565 ?
C12 C15 1.538(3) . ?
C13 C8 1.532(3) 1_565 ?
C13 C15 1.537(3) 8_565 ?
C15 C13 1.537(3) 8_565 ?

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
Y1 Y1 Y2 60.829(18) 8_565 . ?
O4 Y1 Y1 81.77(4) 8_565 8_565 ?
O4 Y1 Y2 37.18(4) 8_565 . ?
O4 Y1 N5 67.38(6) 8_565 . ?
O4 Y1 N1 102.39(7) 8_565 . ?
O4 Y1 O1 143.89(6) 8_565 . ?
O4 Y1 N6 130.25(6) 8_565 . ?
O5 Y1 Y1 38.17(5) . 8_565 ?
O5 Y1 Y2 81.75(7) . . ?
O5 Y1 O4 114.35(7) . 8_565 ?
O5 Y1 O3 79.52(7) . 8_565 ?
O5 Y1 N5 134.38(7) . . ?
O5 Y1 N1 138.81(7) . . ?
O5 Y1 O1 80.95(8) . . ?
O5 Y1 N6 68.57(7) . . ?
O6 Y1 Y1 37.74(5) . 8_565 ?
O6 Y1 Y2 80.39(6) . . ?
O6 Y1 O4 78.25(7) . 8_565 ?
O6 Y1 O5 67.59(7) . . ?
O6 Y1 O3 113.04(7) . 8_565 ?
O6 Y1 N5 68.54(7) . . ?
O6 Y1 N1 141.41(7) . . ?
O6 Y1 O1 78.33(7) . . ?
O6 Y1 N6 135.00(7) . . ?
O3 Y1 Y1 81.61(4) 8_565 8_565 ?
O3 Y1 Y2 37.05(4) 8_565 . ?
O3 Y1 O4 64.64(6) 8_565 8_565 ?
O3 Y1 N5 130.08(7) 8_565 . ?
O3 Y1 N1 101.27(7) 8_565 . ?
O3 Y1 O1 151.03(6) 8_565 . ?
O3 Y1 N6 67.63(7) 8_565 . ?
N5 Y1 Y1 104.59(5) . 8_565 ?
N5 Y1 Y2 102.76(5) . . ?
N1 Y1 Y1 175.65(5) . 8_565 ?
N1 Y1 Y2 123.36(5) . . ?
N1 Y1 N5 76.13(7) . . ?
N1 Y1 N6 73.78(7) . . ?
O1 Y1 Y1 95.88(4) . 8_565 ?
O1 Y1 Y2 156.47(4) . . ?
O1 Y1 N5 78.62(7) . . ?
O1 Y1 N1 80.01(7) . . ?
O1 Y1 N6 85.39(7) . . ?
N6 Y1 Y1 104.60(4) . 8_565 ?
N6 Y1 Y2 102.92(6) . . ?
N6 Y1 N5 147.90(7) . . ?
Y1 Y2 Y1 58.34(4) . 8_565 ?
O4 Y2 Y1 79.86(5) 8_565 8_565 ?
O4 Y2 Y1 37.46(4) . 8_565 ?
O4 Y2 Y1 37.46(4) 8_565 . ?
O4 Y2 Y1 79.86(5) . . ?
O4 Y2 O4 78.65(10) 8_565 . ?
O4 Y2 N8 132.15(6) . . ?
O4 Y2 N8 132.15(6) 8_565 . ?
O4 Y2 N7 68.80(7) . 1_565 ?
O4 Y2 N7 68.80(7) 8_565 1_565 ?
O4 Y2 O2 87.19(7) 8_565 . ?
O4 Y2 O2 87.19(7) . 8_565 ?
O4 Y2 O2 147.84(7) . . ?
O4 Y2 O2 147.84(7) 8_565 8_565 ?
O3 Y2 Y1 79.65(6) . . ?
O3 Y2 Y1 79.65(6) 8_565 8_565 ?
O3 Y2 Y1 37.24(5) . 8_565 ?
O3 Y2 Y1 37.24(5) 8_565 . ?
O3 Y2 O4 112.29(7) . 8_565 ?
O3 Y2 O4 112.30(7) 8_565 . ?
O3 Y2 O4 65.04(6) . . ?
O3 Y2 O4 65.04(6) 8_565 8_565 ?
O3 Y2 O3 78.43(9) . 8_565 ?
O3 Y2 N8 68.83(6) . . ?
O3 Y2 N8 68.83(6) 8_565 . ?
O3 Y2 N7 132.19(6) . 1_565 ?
O3 Y2 N7 132.19(6) 8_565 1_565 ?
O3 Y2 O2 146.75(7) 8_565 8_565 ?
O3 Y2 O2 86.72(8) 8_565 . ?
O3 Y2 O2 146.75(7) . . ?
O3 Y2 O2 86.72(8) . 8_565 ?
N8 Y2 Y1 103.98(6) . 8_565 ?
N8 Y2 Y1 103.98(6) . . ?
N7 Y2 Y1 104.15(7) 1_565 8_565 ?
N7 Y2 Y1 104.15(7) 1_565 . ?
N7 Y2 N8 147.69(9) 1_565 . ?
O2 Y2 Y1 105.86(6) . . ?
O2 Y2 Y1 164.19(5) 8_565 . ?
O2 Y2 Y1 105.86(6) 8_565 8_565 ?
O2 Y2 Y1 164.19(5) . 8_565 ?
O2 Y2 N8 78.10(7) 8_565 . ?
O2 Y2 N8 78.10(7) . . ?
O2 Y2 N7 79.19(7) . 1_565 ?
O2 Y2 N7 79.19(7) 8_565 1_565 ?
O2 Y2 O2 89.92(11) . 8_565 ?
C1 Co1 C1 91.63(15) 8 . ?
C1 Co1 C4 178.98(10) . 8 ?
C1 Co1 C4 88.66(11) 8 8 ?
C1 Co1 C4 88.66(11) . . ?
C1 Co1 C4 178.98(10) 8 . ?
C1 Co1 C3 91.08(11) . . ?
C1 Co1 C3 91.07(11) 8 . ?
C1 Co1 C2 87.97(11) . . ?
C1 Co1 C2 87.97(11) 8 . ?
C4 Co1 C4 91.03(15) 8 . ?
C4 Co1 C3 89.89(11) . . ?
C4 Co1 C3 89.89(11) 8 . ?
C4 Co1 C2 91.07(11) 8 . ?
C4 Co1 C2 91.07(11) . . ?
C2 Co1 C3 178.62(16) . . ?
Y2 O4 Y1 105.37(7) . 8_565 ?
C13 O4 Y1 119.95(14) . 8_565 ?
C13 O4 Y2 118.73(14) . . ?
Y1 O5 Y1 103.66(10) 8_565 . ?
C11 O5 Y1 119.95(9) . 8_565 ?
C11 O5 Y1 119.95(9) . . ?
Y1 O6 Y1 104.53(10) 8_565 . ?
C12 O6 Y1 121.08(9) . 8_565 ?
C12 O6 Y1 121.08(9) . . ?
Y2 O3 Y1 105.71(7) . 8_565 ?
C9 O3 Y1 119.38(14) . 8_565 ?
C9 O3 Y2 119.17(14) . . ?
C5 N5 Y1 113.41(15) . . ?
C5 N5 C15 110.95(19) . . ?
C7 N5 Y1 118.62(15) . . ?
C7 N5 C5 106.10(19) . . ?
C7 N5 C15 111.19(19) . . ?
C15 N5 Y1 96.38(13) . . ?
C1 N1 Y1 142.64(19) 8 . ?
N1 C1 Co1 177.1(2) 8 . ?
N4 C4 Co1 177.9(2) 8 . ?
C6 N8 Y2 95.35(18) . . ?
C17 N8 Y2 116.66(17) . . ?
C17 N8 Y2 116.66(17) 8_565 . ?
C17 N8 C6 110.43(19) . . ?
C17 N8 C6 110.43(19) 8_565 . ?
C17 N8 C17 106.8(3) 8_565 . ?
N8 C6 C9 109.23(18) . 8_565 ?
N8 C6 C9 109.23(18) . . ?
C9 C6 C9 112.8(3) . 8_565 ?
N3 C3 Co1 179.8(4) . . ?
N7 C8 C13 108.94(18) . 1_545 ?
N7 C8 C13 108.94(18) . 8 ?
C13 C8 C13 112.6(3) 8 1_545 ?
O3 C9 C6 111.5(2) . . ?
O3 C9 C10 111.08(19) . 8_565 ?
C6 C9 C10 110.7(2) . 8_565 ?
C9 C10 C11 113.2(2) 8_565 . ?
N6 C10 C9 108.13(19) . 8_565 ?
N6 C10 C11 109.39(19) . . ?
C10 N6 Y1 96.31(13) . . ?
C16 N6 Y1 117.33(15) . . ?
C16 N6 C10 109.42(19) . . ?
C18 N6 Y1 115.38(15) . . ?
C18 N6 C10 110.84(19) . . ?
C18 N6 C16 107.1(2) . . ?
N2 C2 Co1 177.4(3) . . ?
O5 C11 C10 111.41(17) . 8_565 ?
O5 C11 C10 111.41(17) . . ?
C10 C11 C10 110.5(3) . 8_565 ?
C8 N7 Y2 95.56(19) . 1_545 ?
C14 N7 Y2 117.22(16) 8_545 1_545 ?
C14 N7 Y2 117.22(16) . 1_545 ?
C14 N7 C8 110.18(18) 8_545 . ?
C14 N7 C8 110.18(18) . . ?
C14 N7 C14 106.0(3) 8_545 . ?
O6 C12 C15 110.83(17) . 8_565 ?
O6 C12 C15 110.83(17) . . ?
C15 C12 C15 110.9(3) 8_565 . ?
O4 C13 C8 112.2(2) . 1_565 ?
O4 C13 C15 111.02(19) . 8_565 ?
C8 C13 C15 110.6(2) 1_565 8_565 ?
N5 C15 C12 109.1(2) . . ?
N5 C15 C13 108.56(19) . 8_565 ?
C13 C15 C12 112.4(2) 8_565 . ?

_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 -0.036 -0.250 0.351 356.2 107.3 10H2O
2 0.036 0.250 0.649 356.2 108.6 10H2O
3 0.464 0.750 0.149 356.2 106.4 10H2O
4 0.536 0.250 0.851 356.2 109.5 10H2O

_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_C30H54N12O9Dy3Fe
_database_code_depnum_ccdc_archive 'CCDC 1561414'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C60 H108 Dy6 Fe2 N24 O18)'
_chemical_formula_sum            'C30 H54 Dy3 Fe N12 O9'
_chemical_formula_weight         1270.20
_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'
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'

_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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   16.325(2)
_cell_length_b                   18.887(3)
_cell_length_c                   14.075(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4339.6(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.16
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.556
_exptl_absorpt_coefficient_mu    5.493
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.7295.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2456
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.048
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.877
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38945
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.106
_diffrn_reflns_theta_min         2.157
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3166
_reflns_number_total             3554
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0226
_refine_ls_restrained_S_all      1.034
_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)+(0.0122P)²+15.7663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0467
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5) H1A(0.5) H1B(0.5)
3.a Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.11956(2) 0.2500 0.92163(2) 0.01542(8) Uani 1 2 d S T P . .
Dy2 Dy 0.17356(2) 0.2500 1.17411(2) 0.01555(8) Uani 1 2 d S T P . .
Dy3 Dy 0.33611(2) 0.2500 0.99119(2) 0.01133(8) Uani 1 2 d S T P . .
Fe1 Fe 0.16077(5) 0.2500 1.55302(6) 0.0158(2) Uani 1 2 d S T P . .
O4 O 0.23819(16) 0.31602(14) 0.91620(18) 0.0135(6) Uani 1 1 d . . . . .
O5 O 0.11033(16) 0.31707(16) 1.05832(19) 0.0187(7) Uani 1 1 d . . . . .
C6 C 0.2982(2) 0.4139(2) 1.0053(3) 0.0162(9) Uani 1 1 d . . . . .
H6 H 0.3023 0.4667 1.0040 0.019 Uiso 1 1 calc R . . . .
C7 C 0.1233(3) 0.3913(2) 1.0540(3) 0.0196(10) Uani 1 1 d . . . . .
H7 H 0.0702 0.4152 1.0691 0.024 Uiso 1 1 calc R . . . .
C8 C 0.1865(3) 0.4147(2) 1.1282(3) 0.0189(10) Uani 1 1 d . . . . .
H8 H 0.1860 0.4675 1.1317 0.023 Uiso 1 1 calc R . . . .
C9 C 0.2370(2) 0.3905(2) 0.9303(3) 0.0173(10) Uani 1 1 d . . . . .
H9 H 0.2530 0.4134 0.8690 0.021 Uiso 1 1 calc R . . . .
C10 C 0.1505(3) 0.4157(2) 0.9552(3) 0.0184(10) Uani 1 1 d . . . . .
H10 H 0.1488 0.4686 0.9525 0.022 Uiso 1 1 calc R . . . .
C11 C 0.2736(3) 0.3906(2) 1.1051(3) 0.0165(9) Uani 1 1 d . . . . .
H11 H 0.3114 0.4145 1.1509 0.020 Uiso 1 1 calc R . . . .
O6 O 0.28259(16) 0.31652(14) 1.11735(19) 0.0129(6) Uani 1 1 d . . . . .
N7 N 0.3807(2) 0.38323(19) 0.9837(2) 0.0174(8) Uani 1 1 d . . . . .
N6 N 0.1630(2) 0.3861(2) 1.2228(2) 0.0205(8) Uani 1 1 d . . . . .
N8 N 0.0925(2) 0.3861(2) 0.8820(2) 0.0221(9) Uani 1 1 d . . . . .
N2 N 0.2171(3) 0.2500 1.3441(4) 0.0225(12) Uani 1 2 d S T P . .
C2 C 0.2012(4) 0.2500 1.4242(5) 0.0189(14) Uani 1 2 d S T P . .
C12 C 0.4408(3) 0.4063(3) 1.0562(3) 0.0235(11) Uani 1 1 d . . . . .
H12A H 0.4292 0.3824 1.1165 0.035 Uiso 1 1 calc GR . . . .
H12B H 0.4367 0.4576 1.0650 0.035 Uiso 1 1 calc GR . . . .
H12C H 0.4962 0.3941 1.0350 0.035 Uiso 1 1 calc GR . . . .
C13 C 0.1172(3) 0.4099(3) 0.7862(3) 0.0286(11) Uani 1 1 d . . . . .
H13A H 0.1688 0.3870 0.7685 0.043 Uiso 1 1 calc GR . . . .
H13B H 0.1245 0.4614 0.7863 0.043 Uiso 1 1 calc GR . . . .
H13C H 0.0745 0.3970 0.7403 0.043 Uiso 1 1 calc GR . . . .
C14 C 0.2198(3) 0.4122(3) 1.2964(3) 0.0249(11) Uani 1 1 d . . . . .
H14A H 0.1983 0.4002 1.3594 0.037 Uiso 1 1 calc GR . . . .
H14B H 0.2253 0.4637 1.2909 0.037 Uiso 1 1 calc GR . . . .
H14C H 0.2736 0.3900 1.2878 0.037 Uiso 1 1 calc GR . . . .
C15 C 0.0796(3) 0.4104(3) 1.2500(3) 0.0311(12) Uani 1 1 d . . . . .
H15A H 0.0390 0.3885 1.2080 0.047 Uiso 1 1 calc GR . . . .
H15B H 0.0765 0.4620 1.2441 0.047 Uiso 1 1 calc GR . . . .
H15C H 0.0684 0.3967 1.3159 0.047 Uiso 1 1 calc GR . . . .
C16 C 0.4108(3) 0.4094(3) 0.8910(3) 0.0262(11) Uani 1 1 d . . . . .
H16A H 0.4673 0.3935 0.8813 0.039 Uiso 1 1 calc GR . . . .
H16B H 0.4089 0.4612 0.8902 0.039 Uiso 1 1 calc GR . . . .
H16C H 0.3761 0.3907 0.8401 0.039 Uiso 1 1 calc GR . . . .
C17 C 0.0085(3) 0.4140(3) 0.8986(3) 0.0370(14) Uani 1 1 d . . . . .
H17A H -0.0285 0.3957 0.8496 0.056 Uiso 1 1 calc GR . . . .
H17B H 0.0094 0.4658 0.8958 0.056 Uiso 1 1 calc GR . . . .
H17C H -0.0108 0.3988 0.9613 0.056 Uiso 1 1 calc GR . . . .
O2 O 0.0482(3) 0.2500 1.2635(3) 0.0281(11) Uani 1 2 d S T P . .
H2A H 0.0094 0.2736 1.2325 0.042 Uiso 0.5 1 d GR . . . .
H2B H 0.0542 0.2744 1.3170 0.042 Uiso 0.5 1 d GR . . . .
C1 C 0.1131(3) 0.2500 1.6780(4) 0.0149(13) Uani 1 2 d S T P . .
C3 C 0.0520(4) 0.2500 1.5013(4) 0.0154(13) Uani 1 2 d S T P . .
C5 C 0.1621(4) 0.3520(3) 1.5519(3) 0.0455(16) Uani 1 1 d . . . . .
C4 C 0.2659(5) 0.2500 1.6137(5) 0.061(3) Uani 1 2 d S T P . .
N1 N 0.0830(3) 0.2500 1.7521(4) 0.0198(12) Uani 1 2 d S T P . .
N3 N -0.0152(3) 0.2500 1.4740(3) 0.0177(12) Uani 1 2 d S T P . .
N5 N 0.1625(6) 0.4127(3) 1.5507(4) 0.112(3) Uani 1 1 d . . . . .
O3 O 0.4001(2) 0.2500 0.8348(3) 0.0211(10) Uani 1 2 d S T P . .
H3A H 0.4458 0.2763 0.8349 0.032 Uiso 0.5 1 d GR . . . .
H3B H 0.3682 0.2720 0.7921 0.032 Uiso 0.5 1 d GR . . . .
O1 O -0.0269(3) 0.2500 0.9383(3) 0.0470(16) Uani 1 2 d S T P . .
H1A H -0.0410 0.2329 0.9945 0.070 Uiso 0.5 1 d GR . . . .
H1B H -0.0493 0.2200 0.8976 0.070 Uiso 0.5 1 d GR . . . .
N4 N 0.3267(4) 0.2500 1.6553(5) 0.131(6) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy2 3.6614(6) . ?
Dy1 Dy3 3.6683(6) . ?
Dy1 O4 2.305(3) . ?
Dy1 O4 2.305(3) 8_565 ?
Dy1 O5 2.308(3) 8_565 ?
Dy1 O5 2.308(3) . ?
Dy1 N8 2.668(4) . ?
Dy1 N8 2.668(4) 8_565 ?
Dy1 N1 2.459(5) 1_554 ?
Dy1 O1 2.403(4) . ?
Dy2 Dy3 3.6974(5) . ?
Dy2 O5 2.308(3) 8_565 ?
Dy2 O5 2.308(3) . ?
Dy2 O6 2.321(3) 8_565 ?
Dy2 O6 2.321(3) . ?
Dy2 N6 2.667(4) 8_565 ?
Dy2 N6 2.667(4) . ?
Dy2 N2 2.496(5) . ?
Dy2 O2 2.403(4) . ?
Dy3 O4 2.286(3) 8_565 ?
Dy3 O4 2.286(3) . ?
Dy3 O6 2.344(3) . ?
Dy3 O6 2.344(3) 8_565 ?
Dy3 N7 2.622(4) 8_565 ?
Dy3 N7 2.622(4) . ?
Dy3 N3 2.476(5) 6_658 ?
Dy3 O3 2.436(4) . ?
Fe1 C2 1.929(7) . ?
Fe1 C1 1.924(6) . ?
Fe1 C3 1.919(6) . ?
Fe1 C5 1.926(6) 8_565 ?
Fe1 C5 1.926(6) . ?
Fe1 C4 1.918(8) . ?
O4 C9 1.421(5) . ?
O5 C7 1.419(5) . ?
C6 C9 1.518(6) . ?
C6 C11 1.525(6) . ?
C6 N7 1.497(5) . ?
C7 C8 1.534(6) . ?
C7 C10 1.531(6) . ?
C8 C11 1.528(6) . ?
C8 N6 1.487(5) . ?
C9 C10 1.531(6) . ?
C10 N8 1.506(5) . ?
C11 O6 1.418(5) . ?
N7 C12 1.480(5) . ?
N7 C16 1.479(5) . ?
N6 C14 1.476(5) . ?
N6 C15 1.486(5) . ?
N8 C13 1.477(6) . ?
N8 C17 1.488(6) . ?
N2 C2 1.158(8) . ?
C1 N1 1.153(7) . ?
C3 N3 1.163(7) . ?
C5 N5 1.147(8) . ?
C4 N4 1.152(10) . ?
N1 Dy1 2.459(5) 1_556 ?
N3 Dy3 2.476(5) 6_558 ?

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
Dy2 Dy1 Dy3 60.588(7) . . ?
O4 Dy1 Dy2 80.20(6) . . ?
O4 Dy1 Dy2 80.20(6) 8_565 . ?
O4 Dy1 Dy3 36.77(7) 8_565 . ?
O4 Dy1 Dy3 36.77(7) . . ?
O4 Dy1 O4 65.51(13) 8_565 . ?
O4 Dy1 O5 77.62(10) . . ?
O4 Dy1 O5 112.29(9) 8_565 . ?
O4 Dy1 O5 77.62(10) 8_565 8_565 ?
O4 Dy1 O5 112.29(9) . 8_565 ?
O4 Dy1 N8 67.09(10) . . ?
O4 Dy1 N8 67.09(10) 8_565 8_565 ?
O4 Dy1 N8 130.81(10) 8_565 . ?
O4 Dy1 N8 130.81(10) . 8_565 ?
O4 Dy1 N1 99.90(12) . 1_554 ?
O4 Dy1 N1 99.90(12) 8_565 1_554 ?
O4 Dy1 O1 147.09(7) . . ?
O4 Dy1 O1 147.09(7) 8_565 . ?
O5 Dy1 Dy2 37.51(7) . . ?
O5 Dy1 Dy2 37.51(7) 8_565 . ?
O5 Dy1 Dy3 80.82(7) . . ?
O5 Dy1 Dy3 80.82(7) 8_565 . ?
O5 Dy1 O5 66.56(15) 8_565 . ?
O5 Dy1 N8 68.56(11) . . ?
O5 Dy1 N8 68.56(11) 8_565 8_565 ?
O5 Dy1 N8 133.81(11) . 8_565 ?
O5 Dy1 N8 133.81(11) 8_565 . ?
O5 Dy1 N1 142.43(9) 8_565 1_554 ?
O5 Dy1 N1 142.43(9) . 1_554 ?
O5 Dy1 O1 81.58(12) 8_565 . ?
O5 Dy1 O1 81.58(12) . . ?
N8 Dy1 Dy2 104.04(8) . . ?
N8 Dy1 Dy2 104.04(8) 8_565 . ?
N8 Dy1 Dy3 102.43(8) . . ?
N8 Dy1 Dy3 102.43(8) 8_565 . ?
N8 Dy1 N8 149.08(15) 8_565 . ?
N1 Dy1 Dy2 179.87(12) 1_554 . ?
N1 Dy1 Dy3 119.54(12) 1_554 . ?
N1 Dy1 N8 75.94(8) 1_554 . ?
N1 Dy1 N8 75.94(8) 1_554 8_565 ?
O1 Dy1 Dy2 98.33(11) . . ?
O1 Dy1 Dy3 158.91(11) . . ?
O1 Dy1 N8 81.71(8) . 8_565 ?
O1 Dy1 N8 81.71(8) . . ?
O1 Dy1 N1 81.55(16) . 1_554 ?
Dy1 Dy2 Dy3 59.799(11) . . ?
O5 Dy2 Dy1 37.53(7) . . ?
O5 Dy2 Dy1 37.53(7) 8_565 . ?
O5 Dy2 Dy3 80.17(7) 8_565 . ?
O5 Dy2 Dy3 80.17(7) . . ?
O5 Dy2 O5 66.58(14) . 8_565 ?
O5 Dy2 O6 78.63(10) . . ?
O5 Dy2 O6 78.63(10) 8_565 8_565 ?
O5 Dy2 O6 113.40(9) . 8_565 ?
O5 Dy2 O6 113.40(10) 8_565 . ?
O5 Dy2 N6 67.87(10) 8_565 8_565 ?
O5 Dy2 N6 132.98(10) . 8_565 ?
O5 Dy2 N6 67.87(10) . . ?
O5 Dy2 N6 132.98(10) 8_565 . ?
O5 Dy2 N2 143.55(8) . . ?
O5 Dy2 N2 143.55(8) 8_565 . ?
O5 Dy2 O2 89.35(11) . . ?
O5 Dy2 O2 89.35(11) 8_565 . ?
O6 Dy2 Dy1 81.40(6) 8_565 . ?
O6 Dy2 Dy1 81.40(6) . . ?
O6 Dy2 Dy3 37.79(7) 8_565 . ?
O6 Dy2 Dy3 37.79(6) . . ?
O6 Dy2 O6 65.56(13) . 8_565 ?
O6 Dy2 N6 131.32(10) 8_565 . ?
O6 Dy2 N6 131.32(10) . 8_565 ?
O6 Dy2 N6 67.43(10) 8_565 8_565 ?
O6 Dy2 N6 67.43(10) . . ?
O6 Dy2 N2 96.40(12) 8_565 . ?
O6 Dy2 N2 96.40(12) . . ?
O6 Dy2 O2 146.49(7) 8_565 . ?
O6 Dy2 O2 146.49(7) . . ?
N6 Dy2 Dy1 103.53(7) . . ?
N6 Dy2 Dy1 103.53(8) 8_565 . ?
N6 Dy2 Dy3 103.04(8) 8_565 . ?
N6 Dy2 Dy3 103.04(8) . . ?
N6 Dy2 N6 149.25(15) 8_565 . ?
N2 Dy2 Dy1 177.38(12) . . ?
N2 Dy2 Dy3 117.58(12) . . ?
N2 Dy2 N6 76.82(8) . . ?
N2 Dy2 N6 76.82(8) . 8_565 ?
O2 Dy2 Dy1 107.64(11) . . ?
O2 Dy2 Dy3 167.44(10) . . ?
O2 Dy2 N6 79.05(8) . . ?
O2 Dy2 N6 79.06(8) . 8_565 ?
O2 Dy2 N2 74.98(16) . . ?
Dy1 Dy3 Dy2 59.613(12) . . ?
O4 Dy3 Dy1 37.13(7) . . ?
O4 Dy3 Dy1 37.13(7) 8_565 . ?
O4 Dy3 Dy2 79.60(7) 8_565 . ?
O4 Dy3 Dy2 79.60(7) . . ?
O4 Dy3 O4 66.12(13) 8_565 . ?
O4 Dy3 O6 112.42(9) 8_565 . ?
O4 Dy3 O6 78.27(9) . . ?
O4 Dy3 O6 112.43(9) . 8_565 ?
O4 Dy3 O6 78.27(9) 8_565 8_565 ?
O4 Dy3 N7 134.37(10) 8_565 . ?
O4 Dy3 N7 69.64(10) . . ?
O4 Dy3 N7 134.37(10) . 8_565 ?
O4 Dy3 N7 69.64(10) 8_565 8_565 ?
O4 Dy3 N3 140.99(9) 8_565 6_658 ?
O4 Dy3 N3 140.98(9) . 6_658 ?
O4 Dy3 O3 83.27(10) 8_565 . ?
O4 Dy3 O3 83.27(10) . . ?
O6 Dy3 Dy1 80.97(6) 8_565 . ?
O6 Dy3 Dy1 80.96(6) . . ?
O6 Dy3 Dy2 37.34(6) . . ?
O6 Dy3 Dy2 37.35(6) 8_565 . ?
O6 Dy3 O6 64.82(13) 8_565 . ?
O6 Dy3 N7 130.40(10) 8_565 . ?
O6 Dy3 N7 130.40(10) . 8_565 ?
O6 Dy3 N7 67.62(10) 8_565 8_565 ?
O6 Dy3 N7 67.62(10) . . ?
O6 Dy3 N3 102.44(11) 8_565 6_658 ?
O6 Dy3 N3 102.44(11) . 6_658 ?
O6 Dy3 O3 147.58(7) 8_565 . ?
O6 Dy3 O3 147.58(7) . . ?
N7 Dy3 Dy1 104.88(7) 8_565 . ?
N7 Dy3 Dy1 104.88(7) . . ?
N7 Dy3 Dy2 103.12(7) . . ?
N7 Dy3 Dy2 103.12(7) 8_565 . ?
N7 Dy3 N7 147.43(15) . 8_565 ?
N3 Dy3 Dy1 175.94(11) 6_658 . ?
N3 Dy3 Dy2 124.45(11) 6_658 . ?
N3 Dy3 N7 74.68(7) 6_658 8_565 ?
N3 Dy3 N7 74.68(7) 6_658 . ?
O3 Dy3 Dy1 99.91(10) . . ?
O3 Dy3 Dy2 159.52(10) . . ?
O3 Dy3 N7 81.08(8) . . ?
O3 Dy3 N7 81.08(8) . 8_565 ?
O3 Dy3 N3 76.03(15) . 6_658 ?
C1 Fe1 C2 176.1(2) . . ?
C1 Fe1 C5 90.69(15) . 8_565 ?
C1 Fe1 C5 90.69(15) . . ?
C3 Fe1 C2 87.7(2) . . ?
C3 Fe1 C1 88.4(2) . . ?
C3 Fe1 C5 90.43(19) . . ?
C3 Fe1 C5 90.4(2) . 8_565 ?
C5 Fe1 C2 89.34(14) . . ?
C5 Fe1 C2 89.34(14) 8_565 . ?
C5 Fe1 C5 178.4(4) 8_565 . ?
C4 Fe1 C2 96.5(3) . . ?
C4 Fe1 C1 87.4(3) . . ?
C4 Fe1 C3 175.9(3) . . ?
C4 Fe1 C5 89.62(19) . 8_565 ?
C4 Fe1 C5 89.62(19) . . ?
Dy3 O4 Dy1 106.10(11) . . ?
C9 O4 Dy1 121.3(2) . . ?
C9 O4 Dy3 119.0(2) . . ?
Dy2 O5 Dy1 104.96(12) . . ?
C7 O5 Dy1 119.8(2) . . ?
C7 O5 Dy2 120.4(2) . . ?
C9 C6 C11 112.5(3) . . ?
N7 C6 C9 109.8(3) . . ?
N7 C6 C11 108.2(3) . . ?
O5 C7 C8 110.8(3) . . ?
O5 C7 C10 112.3(3) . . ?
C10 C7 C8 109.7(3) . . ?
C11 C8 C7 113.3(3) . . ?
N6 C8 C7 109.4(4) . . ?
N6 C8 C11 108.9(3) . . ?
O4 C9 C6 112.1(3) . . ?
O4 C9 C10 110.6(3) . . ?
C6 C9 C10 111.0(3) . . ?
C7 C10 C9 112.4(3) . . ?
N8 C10 C7 109.1(3) . . ?
N8 C10 C9 108.0(3) . . ?
C6 C11 C8 110.8(3) . . ?
O6 C11 C6 111.7(3) . . ?
O6 C11 C8 111.3(3) . . ?
Dy2 O6 Dy3 104.87(10) . . ?
C11 O6 Dy2 119.8(2) . . ?
C11 O6 Dy3 118.4(2) . . ?
C6 N7 Dy3 96.5(2) . . ?
C12 N7 Dy3 116.0(3) . . ?
C12 N7 C6 110.1(3) . . ?
C16 N7 Dy3 116.6(3) . . ?
C16 N7 C6 110.4(3) . . ?
C16 N7 C12 106.8(3) . . ?
C8 N6 Dy2 95.9(2) . . ?
C14 N6 Dy2 117.5(3) . . ?
C14 N6 C8 110.2(3) . . ?
C14 N6 C15 107.0(3) . . ?
C15 N6 Dy2 115.0(3) . . ?
C15 N6 C8 110.9(3) . . ?
C10 N8 Dy1 96.3(2) . . ?
C13 N8 Dy1 116.0(3) . . ?
C13 N8 C10 109.9(3) . . ?
C13 N8 C17 106.7(4) . . ?
C17 N8 Dy1 117.4(3) . . ?
C17 N8 C10 109.9(3) . . ?
C2 N2 Dy2 150.5(5) . . ?
N2 C2 Fe1 173.0(5) . . ?
N1 C1 Fe1 178.7(5) . . ?
N3 C3 Fe1 177.0(5) . . ?
N5 C5 Fe1 179.5(7) . . ?
N4 C4 Fe1 175.9(7) . . ?
C1 N1 Dy1 140.7(4) . 1_556 ?
C3 N3 Dy3 149.3(4) . 6_558 ?

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
O2 H2B N3 0.89 2.53 3.138(6) 126.7 .
O3 H3B N4 0.90 2.08 2.796(8) 135.7 1_554

_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 0.140 0.750 0.972 127.8 30.4 H2O
2 0.360 0.250 0.472 127.8 30.5 H2O
3 0.640 0.750 0.528 127.8 29.8 H2O
4 0.860 0.250 0.028 127.8 29.9 H2O

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT213_dyfe                
;
PROBLEM: Atom N4 has ADP max/min Ratio ..... 6.1 prolat 
RESPONSE: Disorder caused by vibration of -CN due to hydrogen bonding to water
molecules coordinated to the trinuclear complex. Attempts to model the -CN
group as split atoms were unfruitful. All of the compounds in this
family share the same characteristics.
;
_vrf_PLAT220_dyfe                
;
PROBLEM: Non-Solvent Resd 1 N Ueq(max)/Ueq(min) Range 8.3 Ratio
RESPONSE: Originated by vibration of the "free" (non covalently bonded
to the lanthanide ions) -CN group
;
_vrf_THETM01_dyfe                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The low value of sine(theta_max)/wavelength results from the exclusion
of low quality reflections in the refinement process.
;
####################################################################### 
# 
# 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_C30H54N12O9Gd3Fe
_database_code_depnum_ccdc_archive 'CCDC 1561415'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C60 H108 Fe2 Gd6 N24 O18)'
_chemical_formula_sum            'C30 H54 Fe Gd3 N12 O9'
_chemical_formula_weight         1254.45
_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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   16.401(4)
_cell_length_b                   18.919(4)
_cell_length_c                   14.122(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4381.9(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5225
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.89
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   0.796
_shelx_estimated_absorpt_T_min   0.598
_exptl_absorpt_coefficient_mu    4.865
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1150 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.7560.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.049
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.791
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36000
_diffrn_reflns_point_group_measured_fraction_full 0.791
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.250
_diffrn_reflns_theta_min         2.153
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.791
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2723
_reflns_number_total             3240
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      1.051
_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)+(0.0250P)²+5.2007P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0615
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5) H1A(0.5) H1B(0.5)
3.a Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.11917(2) 0.7500 0.57910(3) 0.01751(12) Uani 1 2 d S T P . .
Gd2 Gd 0.17328(2) 0.7500 0.32436(3) 0.01830(12) Uani 1 2 d S T P . .
Gd3 Gd 0.33734(2) 0.7500 0.50851(3) 0.01352(12) Uani 1 2 d S T P . .
Fe1 Fe 0.16112(6) 0.7500 -0.05392(7) 0.0183(3) Uani 1 2 d S T P . .
O4 O 0.2389(2) 0.81673(18) 0.5839(2) 0.0143(8) Uani 1 1 d . . . . .
O6 O 0.2831(2) 0.81671(19) 0.3824(2) 0.0163(8) Uani 1 1 d . . . . .
O5 O 0.1108(2) 0.8177(2) 0.4412(2) 0.0198(9) Uani 1 1 d . . . . .
C6 C 0.1241(3) 0.8915(3) 0.4450(4) 0.0231(15) Uani 1 1 d . . . . .
H6 H 0.0714 0.9155 0.4300 0.028 Uiso 1 1 calc R . . . .
C7 C 0.2976(3) 0.9150(3) 0.4936(4) 0.0195(13) Uani 1 1 d . . . . .
H7 H 0.3012 0.9677 0.4944 0.023 Uiso 1 1 calc R . . . .
C8 C 0.2369(3) 0.8910(3) 0.5689(4) 0.0184(13) Uani 1 1 d . . . . .
H8 H 0.2528 0.9142 0.6298 0.022 Uiso 1 1 calc R . . . .
C9 C 0.1868(3) 0.9151(3) 0.3719(4) 0.0253(15) Uani 1 1 d . . . . .
H9 H 0.1863 0.9679 0.3686 0.030 Uiso 1 1 calc R . . . .
C10 C 0.1509(3) 0.9157(3) 0.5445(4) 0.0218(14) Uani 1 1 d . . . . .
H10 H 0.1493 0.9685 0.5471 0.026 Uiso 1 1 calc R . . . .
C11 C 0.2734(3) 0.8908(3) 0.3948(4) 0.0194(14) Uani 1 1 d . . . . .
H11 H 0.3108 0.9147 0.3489 0.023 Uiso 1 1 calc R . . . .
N7 N 0.3805(3) 0.8845(2) 0.5157(3) 0.0170(11) Uani 1 1 d . . . . .
N6 N 0.1628(3) 0.8865(3) 0.2773(3) 0.0222(12) Uani 1 1 d . . . . .
N8 N 0.0936(3) 0.8868(3) 0.6178(3) 0.0215(11) Uani 1 1 d . . . . .
C12 C 0.4403(3) 0.9072(3) 0.4431(4) 0.0245(14) Uani 1 1 d . . . . .
H12A H 0.4956 0.8974 0.4657 0.037 Uiso 1 1 calc GR . . . .
H12B H 0.4343 0.9580 0.4315 0.037 Uiso 1 1 calc GR . . . .
H12C H 0.4305 0.8813 0.3842 0.037 Uiso 1 1 calc GR . . . .
C13 C 0.2196(4) 0.9131(3) 0.2035(4) 0.0256(15) Uani 1 1 d . . . . .
H13A H 0.2735 0.8920 0.2128 0.038 Uiso 1 1 calc GR . . . .
H13B H 0.2238 0.9647 0.2082 0.038 Uiso 1 1 calc GR . . . .
H13C H 0.1988 0.9003 0.1407 0.038 Uiso 1 1 calc GR . . . .
C14 C 0.0797(3) 0.9105(4) 0.2508(4) 0.0378(18) Uani 1 1 d . . . . .
H14A H 0.0695 0.8992 0.1842 0.057 Uiso 1 1 calc GR . . . .
H14B H 0.0755 0.9617 0.2602 0.057 Uiso 1 1 calc GR . . . .
H14C H 0.0394 0.8865 0.2906 0.057 Uiso 1 1 calc GR . . . .
C15 C 0.4109(3) 0.9103(4) 0.6077(4) 0.0289(15) Uani 1 1 d . . . . .
H15A H 0.3766 0.8915 0.6587 0.043 Uiso 1 1 calc GR . . . .
H15B H 0.4089 0.9621 0.6088 0.043 Uiso 1 1 calc GR . . . .
H15C H 0.4672 0.8946 0.6168 0.043 Uiso 1 1 calc GR . . . .
C16 C 0.1177(4) 0.9104(3) 0.7139(4) 0.0307(16) Uani 1 1 d . . . . .
H16A H 0.0750 0.8975 0.7593 0.046 Uiso 1 1 calc GR . . . .
H16B H 0.1251 0.9618 0.7141 0.046 Uiso 1 1 calc GR . . . .
H16C H 0.1690 0.8874 0.7319 0.046 Uiso 1 1 calc GR . . . .
N2 N 0.2184(4) 0.7500 0.1533(5) 0.0258(18) Uani 1 2 d S T P . .
C2 C 0.2032(5) 0.7500 0.0749(6) 0.022(2) Uani 1 2 d S T P . .
O2 O 0.0467(3) 0.7500 0.2344(4) 0.0336(16) Uani 1 2 d S T P . .
H2A H 0.0095 0.7237 0.2633 0.050 Uiso 0.5 1 d GR . . . .
H2B H 0.0538 0.7285 0.1793 0.050 Uiso 0.5 1 d GR . . . .
N1 N 0.0807(4) 0.7500 0.7486(4) 0.0209(16) Uani 1 2 d S T P . .
C1 C 0.1122(5) 0.7500 -0.1782(6) 0.021(2) Uani 1 2 d S T P . .
O3 O 0.4020(3) 0.7500 0.6663(4) 0.0238(14) Uani 1 2 d S T P . .
H3A H 0.4448 0.7195 0.6686 0.036 Uiso 0.5 1 d GR . . . .
H3B H 0.3678 0.7324 0.7112 0.036 Uiso 0.5 1 d GR . . . .
N3 N 0.4869(4) 0.7500 0.4734(4) 0.0196(16) Uani 1 2 d S T P . .
C17 C 0.0098(4) 0.9141(4) 0.6010(5) 0.0405(19) Uani 1 1 d . . . . .
H17A H -0.0090 0.8991 0.5382 0.061 Uiso 1 1 calc GR . . . .
H17B H 0.0101 0.9658 0.6042 0.061 Uiso 1 1 calc GR . . . .
H17C H -0.0271 0.8953 0.6495 0.061 Uiso 1 1 calc GR . . . .
C5 C 0.1609(5) 0.8518(4) -0.0528(4) 0.047(2) Uani 1 1 d . . . . .
N5 N 0.1626(7) 0.9120(4) -0.0503(5) 0.123(4) Uani 1 1 d . . . . .
C3 C 0.5542(5) 0.7500 0.5012(5) 0.0154(18) Uani 1 2 d S T P . .
O1 O -0.0294(3) 0.7500 0.5611(4) 0.047(2) Uani 1 2 d S T P . .
H1A H -0.0442 0.7730 0.5082 0.070 Uiso 0.5 1 d GR . . . .
H1B H -0.0532 0.7753 0.6073 0.070 Uiso 0.5 1 d GR . . . .
C4 C 0.2640(6) 0.7500 -0.1154(6) 0.062(4) Uani 1 2 d S T P . .
N4 N 0.3259(5) 0.7500 -0.1569(7) 0.147(8) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Gd2 3.7052(9) . ?
Gd1 Gd3 3.7146(9) . ?
Gd1 O4 2.336(3) 8_575 ?
Gd1 O4 2.336(3) . ?
Gd1 O5 2.335(4) 8_575 ?
Gd1 O5 2.335(4) . ?
Gd1 N8 2.679(5) . ?
Gd1 N8 2.679(5) 8_575 ?
Gd1 N1 2.475(6) . ?
Gd1 O1 2.450(5) . ?
Gd2 Gd3 3.7420(8) . ?
Gd2 O6 2.346(3) . ?
Gd2 O6 2.346(3) 8_575 ?
Gd2 O5 2.326(4) 8_575 ?
Gd2 O5 2.326(4) . ?
Gd2 N6 2.673(5) 8_575 ?
Gd2 N6 2.673(5) . ?
Gd2 N2 2.526(7) . ?
Gd2 O2 2.433(5) . ?
Gd3 O4 2.309(3) . ?
Gd3 O4 2.309(3) 8_575 ?
Gd3 O6 2.357(3) 8_575 ?
Gd3 O6 2.357(3) . ?
Gd3 N7 2.644(5) 8_575 ?
Gd3 N7 2.644(5) . ?
Gd3 O3 2.468(5) . ?
Gd3 N3 2.503(6) . ?
Fe1 C2 1.946(9) . ?
Fe1 C1 1.930(8) . ?
Fe1 C5 1.927(8) 8_575 ?
Fe1 C5 1.927(8) . ?
Fe1 C3 1.905(8) 6_556 ?
Fe1 C4 1.898(10) . ?
O4 C8 1.422(6) . ?
O6 C11 1.421(6) . ?
O5 C6 1.414(7) . ?
C6 C9 1.524(7) . ?
C6 C10 1.542(8) . ?
C7 C8 1.526(7) . ?
C7 C11 1.521(7) . ?
C7 N7 1.509(7) . ?
C8 C10 1.525(7) . ?
C9 C11 1.528(7) . ?
C9 N6 1.493(7) . ?
C10 N8 1.500(7) . ?
N7 C12 1.482(7) . ?
N7 C15 1.474(7) . ?
N6 C13 1.485(7) . ?
N6 C14 1.484(7) . ?
N8 C16 1.482(7) . ?
N8 C17 1.488(7) . ?
N2 C2 1.135(9) . ?
N1 C1 1.156(9) 1_556 ?
C1 N1 1.156(9) 1_554 ?
N3 C3 1.172(9) . ?
C5 N5 1.138(10) . ?
C3 Fe1 1.905(8) 6_656 ?
C4 N4 1.172(12) . ?

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
Gd2 Gd1 Gd3 60.574(10) . . ?
O4 Gd1 Gd2 80.04(8) . . ?
O4 Gd1 Gd2 80.04(8) 8_575 . ?
O4 Gd1 Gd3 36.66(8) . . ?
O4 Gd1 Gd3 36.66(8) 8_575 . ?
O4 Gd1 O4 65.43(16) 8_575 . ?
O4 Gd1 N8 130.38(13) . 8_575 ?
O4 Gd1 N8 66.63(12) 8_575 8_575 ?
O4 Gd1 N8 66.63(12) . . ?
O4 Gd1 N8 130.38(13) 8_575 . ?
O4 Gd1 N1 100.71(15) . . ?
O4 Gd1 N1 100.71(14) 8_575 . ?
O4 Gd1 O1 147.07(8) 8_575 . ?
O4 Gd1 O1 147.07(8) . . ?
O5 Gd1 Gd2 37.28(9) 8_575 . ?
O5 Gd1 Gd2 37.28(9) . . ?
O5 Gd1 Gd3 80.36(8) 8_575 . ?
O5 Gd1 Gd3 80.36(8) . . ?
O5 Gd1 O4 77.13(12) . . ?
O5 Gd1 O4 77.13(12) 8_575 8_575 ?
O5 Gd1 O4 111.72(12) . 8_575 ?
O5 Gd1 O4 111.72(12) 8_575 . ?
O5 Gd1 O5 66.54(19) . 8_575 ?
O5 Gd1 N8 68.32(13) . . ?
O5 Gd1 N8 68.32(13) 8_575 8_575 ?
O5 Gd1 N8 133.71(13) 8_575 . ?
O5 Gd1 N8 133.71(13) . 8_575 ?
O5 Gd1 N1 142.34(11) . . ?
O5 Gd1 N1 142.34(11) 8_575 . ?
O5 Gd1 O1 81.67(14) . . ?
O5 Gd1 O1 81.67(14) 8_575 . ?
N8 Gd1 Gd2 103.61(9) 8_575 . ?
N8 Gd1 Gd2 103.61(9) . . ?
N8 Gd1 Gd3 101.85(9) . . ?
N8 Gd1 Gd3 101.85(9) 8_575 . ?
N8 Gd1 N8 150.23(18) . 8_575 ?
N1 Gd1 Gd2 179.10(14) . . ?
N1 Gd1 Gd3 120.32(14) . . ?
N1 Gd1 N8 76.29(9) . . ?
N1 Gd1 N8 76.30(9) . 8_575 ?
O1 Gd1 Gd2 97.90(14) . . ?
O1 Gd1 Gd3 158.47(14) . . ?
O1 Gd1 N8 82.28(10) . 8_575 ?
O1 Gd1 N8 82.27(10) . . ?
O1 Gd1 N1 81.2(2) . . ?
Gd1 Gd2 Gd3 59.837(16) . . ?
O6 Gd2 Gd1 81.07(8) 8_575 . ?
O6 Gd2 Gd1 81.07(8) . . ?
O6 Gd2 Gd3 37.40(8) 8_575 . ?
O6 Gd2 Gd3 37.40(8) . . ?
O6 Gd2 O6 65.08(17) . 8_575 ?
O6 Gd2 N6 130.99(13) . 8_575 ?
O6 Gd2 N6 130.99(13) 8_575 . ?
O6 Gd2 N6 67.44(13) 8_575 8_575 ?
O6 Gd2 N6 67.44(13) . . ?
O6 Gd2 N2 96.27(15) . . ?
O6 Gd2 N2 96.27(15) 8_575 . ?
O6 Gd2 O2 146.80(9) . . ?
O6 Gd2 O2 146.80(9) 8_575 . ?
O5 Gd2 Gd1 37.43(9) . . ?
O5 Gd2 Gd1 37.43(9) 8_575 . ?
O5 Gd2 Gd3 79.85(9) . . ?
O5 Gd2 Gd3 79.85(9) 8_575 . ?
O5 Gd2 O6 112.72(12) . 8_575 ?
O5 Gd2 O6 78.11(12) 8_575 8_575 ?
O5 Gd2 O6 112.72(12) 8_575 . ?
O5 Gd2 O6 78.11(12) . . ?
O5 Gd2 O5 66.81(18) . 8_575 ?
O5 Gd2 N6 132.85(13) 8_575 . ?
O5 Gd2 N6 132.85(13) . 8_575 ?
O5 Gd2 N6 67.41(13) . . ?
O5 Gd2 N6 67.41(13) 8_575 8_575 ?
O5 Gd2 N2 143.81(10) 8_575 . ?
O5 Gd2 N2 143.81(10) . . ?
O5 Gd2 O2 89.69(14) 8_575 . ?
O5 Gd2 O2 89.69(14) . . ?
N6 Gd2 Gd1 103.05(10) 8_575 . ?
N6 Gd2 Gd1 103.05(10) . . ?
N6 Gd2 Gd3 102.65(10) 8_575 . ?
N6 Gd2 Gd3 102.65(10) . . ?
N6 Gd2 N6 150.3(2) . 8_575 ?
N2 Gd2 Gd1 176.83(14) . . ?
N2 Gd2 Gd3 116.99(14) . . ?
N2 Gd2 N6 77.36(10) . . ?
N2 Gd2 N6 77.36(10) . 8_575 ?
O2 Gd2 Gd1 107.60(13) . . ?
O2 Gd2 Gd3 167.43(13) . . ?
O2 Gd2 N6 79.37(10) . . ?
O2 Gd2 N6 79.36(10) . 8_575 ?
O2 Gd2 N2 75.57(19) . . ?
Gd1 Gd3 Gd2 59.589(16) . . ?
O4 Gd3 Gd1 37.15(8) 8_575 . ?
O4 Gd3 Gd1 37.15(8) . . ?
O4 Gd3 Gd2 79.51(9) 8_575 . ?
O4 Gd3 Gd2 79.51(9) . . ?
O4 Gd3 O4 66.27(17) 8_575 . ?
O4 Gd3 O6 77.99(12) . . ?
O4 Gd3 O6 77.99(12) 8_575 8_575 ?
O4 Gd3 O6 112.16(12) . 8_575 ?
O4 Gd3 O6 112.16(12) 8_575 . ?
O4 Gd3 N7 69.10(12) . . ?
O4 Gd3 N7 134.09(12) . 8_575 ?
O4 Gd3 N7 69.10(12) 8_575 8_575 ?
O4 Gd3 N7 134.09(12) 8_575 . ?
O4 Gd3 O3 83.33(13) 8_575 . ?
O4 Gd3 O3 83.33(13) . . ?
O4 Gd3 N3 140.93(11) . . ?
O4 Gd3 N3 140.93(11) 8_575 . ?
O6 Gd3 Gd1 80.73(8) 8_575 . ?
O6 Gd3 Gd1 80.73(8) . . ?
O6 Gd3 Gd2 37.19(8) 8_575 . ?
O6 Gd3 Gd2 37.19(8) . . ?
O6 Gd3 O6 64.73(17) 8_575 . ?
O6 Gd3 N7 130.21(13) 8_575 . ?
O6 Gd3 N7 67.34(12) . . ?
O6 Gd3 N7 130.20(13) . 8_575 ?
O6 Gd3 N7 67.34(12) 8_575 8_575 ?
O6 Gd3 O3 147.62(9) 8_575 . ?
O6 Gd3 O3 147.62(9) . . ?
O6 Gd3 N3 102.74(15) . . ?
O6 Gd3 N3 102.74(15) 8_575 . ?
N7 Gd3 Gd1 104.35(9) 8_575 . ?
N7 Gd3 Gd1 104.34(9) . . ?
N7 Gd3 Gd2 102.67(9) . . ?
N7 Gd3 Gd2 102.67(9) 8_575 . ?
N7 Gd3 N7 148.60(18) . 8_575 ?
O3 Gd3 Gd1 99.89(12) . . ?
O3 Gd3 Gd2 159.48(12) . . ?
O3 Gd3 N7 81.39(10) . . ?
O3 Gd3 N7 81.39(10) . 8_575 ?
O3 Gd3 N3 75.97(19) . . ?
N3 Gd3 Gd1 175.86(14) . . ?
N3 Gd3 Gd2 124.55(14) . . ?
N3 Gd3 N7 75.23(9) . 8_575 ?
N3 Gd3 N7 75.23(9) . . ?
C1 Fe1 C2 176.2(3) . . ?
C5 Fe1 C2 89.58(18) 8_575 . ?
C5 Fe1 C2 89.58(18) . . ?
C5 Fe1 C1 90.40(19) 8_575 . ?
C5 Fe1 C1 90.40(19) . . ?
C5 Fe1 C5 179.0(4) 8_575 . ?
C3 Fe1 C2 87.8(3) 6_556 . ?
C3 Fe1 C1 88.4(3) 6_556 . ?
C3 Fe1 C5 89.7(2) 6_556 . ?
C3 Fe1 C5 89.7(2) 6_556 8_575 ?
C4 Fe1 C2 96.4(3) . . ?
C4 Fe1 C1 87.4(3) . . ?
C4 Fe1 C5 90.3(2) . 8_575 ?
C4 Fe1 C5 90.3(2) . . ?
C4 Fe1 C3 175.8(3) . 6_556 ?
Gd3 O4 Gd1 106.19(13) . . ?
C8 O4 Gd1 120.7(3) . . ?
C8 O4 Gd3 119.2(3) . . ?
Gd2 O6 Gd3 105.41(14) . . ?
C11 O6 Gd2 119.2(3) . . ?
C11 O6 Gd3 118.5(3) . . ?
Gd2 O5 Gd1 105.29(15) . . ?
C6 O5 Gd1 120.0(3) . . ?
C6 O5 Gd2 120.2(3) . . ?
O5 C6 C9 111.6(5) . . ?
O5 C6 C10 111.8(4) . . ?
C9 C6 C10 109.8(5) . . ?
C11 C7 C8 112.3(4) . . ?
N7 C7 C8 109.3(4) . . ?
N7 C7 C11 108.1(4) . . ?
O4 C8 C7 112.5(4) . . ?
O4 C8 C10 110.9(4) . . ?
C10 C8 C7 110.8(4) . . ?
C6 C9 C11 113.3(5) . . ?
N6 C9 C6 108.8(5) . . ?
N6 C9 C11 108.9(5) . . ?
C8 C10 C6 112.3(4) . . ?
N8 C10 C6 110.0(5) . . ?
N8 C10 C8 108.2(4) . . ?
O6 C11 C7 112.3(4) . . ?
O6 C11 C9 112.0(5) . . ?
C7 C11 C9 110.3(5) . . ?
C7 N7 Gd3 96.8(3) . . ?
C12 N7 Gd3 115.4(3) . . ?
C12 N7 C7 110.0(4) . . ?
C15 N7 Gd3 116.3(3) . . ?
C15 N7 C7 111.1(4) . . ?
C15 N7 C12 106.9(4) . . ?
C9 N6 Gd2 96.4(3) . . ?
C13 N6 Gd2 117.5(3) . . ?
C13 N6 C9 109.9(4) . . ?
C14 N6 Gd2 114.6(4) . . ?
C14 N6 C9 110.9(5) . . ?
C14 N6 C13 107.2(4) . . ?
C10 N8 Gd1 96.5(3) . . ?
C16 N8 Gd1 115.8(3) . . ?
C16 N8 C10 110.8(4) . . ?
C16 N8 C17 106.8(5) . . ?
C17 N8 Gd1 116.5(4) . . ?
C17 N8 C10 110.1(4) . . ?
C2 N2 Gd2 150.3(6) . . ?
N2 C2 Fe1 171.9(7) . . ?
C1 N1 Gd1 138.7(6) 1_556 . ?
N1 C1 Fe1 178.0(7) 1_554 . ?
C3 N3 Gd3 149.0(5) . . ?
N5 C5 Fe1 178.0(8) . . ?
N3 C3 Fe1 176.6(6) . 6_656 ?
N4 C4 Fe1 177.2(8) . . ?

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
O2 H2B N3 0.89 2.45 3.095(8) 129.6 3_465
O3 H3A N1 0.91 2.58 3.168(8) 122.8 3_566
O3 H3B N4 0.91 2.01 2.791(11) 142.7 1_556
O1 H1B N4 0.90 2.16 2.732(10) 121.1 3_465

_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 0.139 0.250 0.527 128.0 31.4 3H2O
2 0.361 0.750 0.027 128.0 31.3 3H2O
3 0.639 0.250 0.973 128.0 31.9 3H2O
4 0.861 0.750 0.473 128.0 31.8 3H2O

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT213_gdfe                
;
PROBLEM: Atom N4 has ADP max/min Ratio ..... 6.1 prolat 
RESPONSE: Disorder caused by vibration of -CN due to hydrogen bonding to water
molecules coordinated to the trinuclear complex. Attempts to model the -CN
group as split atoms were unfruitful.
;
_vrf_PLAT220_gdfe                
;
PROBLEM: Non-Solvent Resd 1 N Ueq(max)/Ueq(min) Range 8.3 Ratio
RESPONSE: Originated by vibration of the "free" (non covalently bonded
to the lanthanide ions) -CN group
;
_vrf_THETM01_gdfe                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The low value of sine(theta_max)/wavelength results from the exclusion
of low quality reflections in the refinement process. 
;
####################################################################### 
# 
# 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_C30H56N12O10Ho3Co
_database_code_depnum_ccdc_archive 'CCDC 1561418'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H56 Co Ho3 N12 O10'
_chemical_formula_sum            'C30 H56 Co Ho3 N12 O10'
_chemical_formula_weight         1298.58
_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'
Co Co 0.3494 0.9721 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   24.606(5)
_cell_length_b                   12.873(2)
_cell_length_c                   16.083(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5094.3(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.857
_shelx_estimated_absorpt_T_min   0.181
_exptl_absorpt_coefficient_mu    4.982
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1430 before and 0.0681 after correction.
The Ratio of minimum to maximum transmission is 0.7676.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.521
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.032
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.850
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44924
_diffrn_reflns_point_group_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.817
_diffrn_reflns_theta_min         2.026
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3541
_reflns_number_total             4109
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.045
_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)+(0.0195P)²+7.0227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0511
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O1AA(H1Aa,H1Ab), O6(H6a,H6b)
2.b Ternary CH refined with riding coordinates:
 C7(H7), C13(H13), C15(H15), C20(H20), C11(H11), C1AA(H1Ac), C17(H17), C19(H19)
2.c Idealised Me refined as rotating group:
 C0AA(H0Aa,H0Ab,H0Ac), C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C2AA(H2Aa,
 H2Ab,H2Ac), C3AA(H3Aa,H3Ab,H3Ac), C4AA(H4Aa,H4Ab,H4Ac)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.35319(2) 0.11022(2) 0.20280(2) 0.01029(7) Uani 1 1 d . . . . .
Ho2 Ho 0.46642(2) 0.2500 0.30297(2) 0.01255(8) Uani 1 2 d S T P . .
Co1 Co 0.26655(3) -0.2500 0.15288(4) 0.01293(17) Uani 1 2 d S T P . .
O1 O 0.35898(13) 0.2500 0.1171(2) 0.0117(8) Uani 1 2 d S T P . .
O2 O 0.44661(10) 0.3640(2) 0.19595(14) 0.0150(6) Uani 1 1 d . . . . .
O0AA O 0.30578(13) 0.2500 0.2513(2) 0.0101(8) Uani 1 2 d S T P . .
O1AA O 0.52483(11) 0.1197(2) 0.35622(17) 0.0242(7) Uani 1 1 d . . . . .
H1AA H 0.5622 0.1258 0.3698 0.036 Uiso 1 1 d GR . . . .
H1AB H 0.5161 0.0498 0.3689 0.036 Uiso 1 1 d GR . . . .
O3 O 0.39593(10) 0.36325(19) 0.32908(15) 0.0145(6) Uani 1 1 d . . . . .
O6 O 0.27231(10) 0.0906(2) 0.11952(15) 0.0165(6) Uani 1 1 d . . . . .
H6A H 0.2670 0.1471 0.0910 0.025 Uiso 1 1 d GR . . . .
H6B H 0.2441 0.0863 0.1520 0.025 Uiso 1 1 d GR . . . .
N1 N 0.34570(14) -0.0786(3) 0.19993(19) 0.0178(8) Uani 1 1 d . . . . .
N7 N 0.39444(12) 0.0582(2) 0.05671(19) 0.0150(7) Uani 1 1 d . . . . .
N8 N 0.54434(18) 0.2500 0.1896(3) 0.0169(11) Uani 1 2 d S T P . .
N6 N 0.44022(18) 0.2500 0.4625(3) 0.0173(11) Uani 1 2 d S T P . .
C7 C 0.3801(2) 0.2500 0.4486(3) 0.0140(12) Uani 1 2 d S T P . .
H7 H 0.3616 0.2500 0.5039 0.017 Uiso 1 2 calc RS T P . .
C0AA C 0.35756(16) 0.0479(3) -0.0152(2) 0.0196(9) Uani 1 1 d . . . . .
H0AA H 0.3342 -0.0130 -0.0074 0.029 Uiso 1 1 calc GR . . . .
H0AB H 0.3790 0.0395 -0.0661 0.029 Uiso 1 1 calc GR . . . .
H0AC H 0.3350 0.1103 -0.0197 0.029 Uiso 1 1 calc GR . . . .
C12 C 0.58066(16) 0.3421(3) 0.1864(3) 0.0236(10) Uani 1 1 d . . . . .
H12A H 0.5589 0.4055 0.1913 0.035 Uiso 1 1 calc GR . . . .
H12B H 0.6003 0.3427 0.1333 0.035 Uiso 1 1 calc GR . . . .
H12C H 0.6068 0.3388 0.2323 0.035 Uiso 1 1 calc GR . . . .
C13 C 0.36398(15) 0.3482(3) 0.4025(2) 0.0131(8) Uani 1 1 d . . . . .
H13 H 0.3708 0.4084 0.4403 0.016 Uiso 1 1 calc R . . . .
C14 C 0.42747(16) -0.0381(3) 0.0588(3) 0.0210(9) Uani 1 1 d . . . . .
H14A H 0.4484 -0.0404 0.1106 0.031 Uiso 1 1 calc GR . . . .
H14B H 0.4524 -0.0388 0.0113 0.031 Uiso 1 1 calc GR . . . .
H14C H 0.4034 -0.0987 0.0560 0.031 Uiso 1 1 calc GR . . . .
C15 C 0.5064(2) 0.2500 0.1159(3) 0.0162(12) Uani 1 2 d S T P . .
H15 H 0.5287 0.2500 0.0639 0.019 Uiso 1 2 calc RS T P . .
C20 C 0.47195(15) 0.3488(3) 0.1176(2) 0.0130(8) Uani 1 1 d . . . . .
H20 H 0.4969 0.4090 0.1079 0.016 Uiso 1 1 calc R . . . .
N10 N 0.29077(13) 0.4418(2) 0.32969(19) 0.0142(7) Uani 1 1 d . . . . .
C11 C 0.30314(15) 0.3472(3) 0.3812(2) 0.0132(8) Uani 1 1 d . . . . .
H11 H 0.2820 0.3516 0.4341 0.016 Uiso 1 1 calc R . . . .
C2AA C 0.30617(17) 0.5362(3) 0.3767(2) 0.0204(9) Uani 1 1 d . . . . .
H2AA H 0.3458 0.5399 0.3813 0.031 Uiso 1 1 calc GR . . . .
H2AB H 0.2902 0.5334 0.4324 0.031 Uiso 1 1 calc GR . . . .
H2AC H 0.2927 0.5979 0.3475 0.031 Uiso 1 1 calc GR . . . .
C1AA C 0.2854(2) 0.2500 0.3344(3) 0.0125(12) Uani 1 2 d S T P . .
H1AC H 0.2448 0.2500 0.3315 0.015 Uiso 1 2 calc RS T P . .
C17 C 0.3951(2) 0.2500 0.0479(3) 0.0128(12) Uani 1 2 d S T P . .
H17 H 0.3728 0.2500 -0.0041 0.015 Uiso 1 2 calc RS T P . .
C19 C 0.43023(15) 0.3482(3) 0.0478(2) 0.0143(8) Uani 1 1 d . . . . .
H19 H 0.4498 0.3527 -0.0065 0.017 Uiso 1 1 calc R . . . .
C3AA C 0.45694(17) 0.1579(3) 0.5110(3) 0.0263(10) Uani 1 1 d . . . . .
H3AA H 0.4496 0.0949 0.4788 0.039 Uiso 1 1 calc GR . . . .
H3AB H 0.4364 0.1556 0.5632 0.039 Uiso 1 1 calc GR . . . .
H3AC H 0.4959 0.1622 0.5233 0.039 Uiso 1 1 calc GR . . . .
C4AA C 0.23197(15) 0.4489(3) 0.3113(2) 0.0185(9) Uani 1 1 d . . . . .
H4AA H 0.2245 0.5140 0.2818 0.028 Uiso 1 1 calc GR . . . .
H4AB H 0.2114 0.4474 0.3634 0.028 Uiso 1 1 calc GR . . . .
H4AC H 0.2211 0.3900 0.2764 0.028 Uiso 1 1 calc GR . . . .
N0AA N 0.3207(2) -0.2500 -0.0180(3) 0.0263(12) Uani 1 2 d S T P . .
N1AA N 0.2173(2) -0.2500 0.3282(3) 0.0260(12) Uani 1 2 d S T P . .
C6AA C 0.21688(16) -0.3547(3) 0.1202(2) 0.0155(9) Uani 1 1 d . . . . .
C10 C 0.2353(2) -0.2500 0.2621(4) 0.0183(13) Uani 1 2 d S T P . .
C5AA C 0.2991(2) -0.2500 0.0455(4) 0.0175(13) Uani 1 2 d S T P . .
N2AA N 0.18781(14) -0.4213(3) 0.1016(2) 0.0222(8) Uani 1 1 d . . . . .
C2 C 0.31599(17) -0.1453(3) 0.1830(2) 0.0150(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
Ho1 Ho1 3.5989(8) 8_565 ?
Ho1 Ho2 3.6871(5) . ?
Ho1 O1 2.271(2) . ?
Ho1 O2 2.325(3) 8_565 ?
Ho1 O0AA 2.282(2) . ?
Ho1 O3 2.312(2) 8_565 ?
Ho1 O6 2.412(2) . ?
Ho1 N1 2.438(3) . ?
Ho1 N7 2.645(3) . ?
Ho1 N10 2.641(3) 8_565 ?
Ho2 Ho1 3.6872(5) 8_565 ?
Ho2 O2 2.314(2) 8_565 ?
Ho2 O2 2.314(2) . ?
Ho2 O1AA 2.369(3) . ?
Ho2 O1AA 2.369(3) 8_565 ?
Ho2 O3 2.304(3) . ?
Ho2 O3 2.304(3) 8_565 ?
Ho2 N8 2.646(4) . ?
Ho2 N6 2.645(4) . ?
Co1 C6AA 1.894(4) . ?
Co1 C6AA 1.894(4) 8 ?
Co1 C10 1.917(6) . ?
Co1 C5AA 1.904(6) . ?
Co1 C2 1.879(4) 8 ?
Co1 C2 1.879(4) . ?
O1 Ho1 2.271(2) 8_565 ?
O1 C17 1.424(6) . ?
O2 Ho1 2.325(3) 8_565 ?
O2 C20 1.419(4) . ?
O0AA Ho1 2.282(2) 8_565 ?
O0AA C1AA 1.427(6) . ?
O3 Ho1 2.312(2) 8_565 ?
O3 C13 1.432(4) . ?
N1 C2 1.160(5) . ?
N7 C0AA 1.475(5) . ?
N7 C14 1.483(5) . ?
N7 C19 1.499(5) 8_565 ?
N8 C12 1.485(5) 8_565 ?
N8 C12 1.486(5) . ?
N8 C15 1.507(7) . ?
N6 C7 1.496(7) . ?
N6 C3AA 1.478(5) . ?
N6 C3AA 1.478(5) 8_565 ?
C7 C13 1.518(5) . ?
C7 C13 1.518(5) 8_565 ?
C13 C11 1.536(5) . ?
C15 C20 1.529(5) . ?
C15 C20 1.529(5) 8_565 ?
C20 C19 1.521(5) . ?
N10 Ho1 2.641(3) 8_565 ?
N10 C11 1.504(5) . ?
N10 C2AA 1.480(5) . ?
N10 C4AA 1.480(5) . ?
C11 C1AA 1.525(5) . ?
C1AA C11 1.525(5) 8_565 ?
C17 C19 1.531(5) 8_565 ?
C17 C19 1.531(5) . ?
C19 N7 1.499(5) 8_565 ?
N0AA C5AA 1.150(7) . ?
N1AA C10 1.152(7) . ?
C6AA N2AA 1.156(5) . ?

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
Ho1 Ho1 Ho2 60.790(7) 8_565 . ?
O1 Ho1 Ho1 37.61(7) . 8_565 ?
O1 Ho1 Ho2 80.28(8) . . ?
O1 Ho1 O2 78.24(10) . 8_565 ?
O1 Ho1 O0AA 67.35(10) . . ?
O1 Ho1 O3 112.81(10) . 8_565 ?
O1 Ho1 O6 78.33(10) . . ?
O1 Ho1 N1 141.54(10) . . ?
O1 Ho1 N7 68.74(10) . . ?
O1 Ho1 N10 134.97(10) . 8_565 ?
O2 Ho1 Ho1 81.80(6) 8_565 8_565 ?
O2 Ho1 Ho2 37.26(6) 8_565 . ?
O2 Ho1 O6 143.55(8) 8_565 . ?
O2 Ho1 N1 102.47(10) 8_565 . ?
O2 Ho1 N7 67.35(9) 8_565 . ?
O2 Ho1 N10 130.37(9) 8_565 8_565 ?
O0AA Ho1 Ho1 37.95(6) . 8_565 ?
O0AA Ho1 Ho2 81.50(8) . . ?
O0AA Ho1 O2 114.15(10) . 8_565 ?
O0AA Ho1 O3 79.39(10) . 8_565 ?
O0AA Ho1 O6 81.40(10) . . ?
O0AA Ho1 N1 138.94(10) . . ?
O0AA Ho1 N7 134.37(10) . . ?
O0AA Ho1 N10 68.82(9) . 8_565 ?
O3 Ho1 Ho1 81.51(6) 8_565 8_565 ?
O3 Ho1 Ho2 36.92(6) 8_565 . ?
O3 Ho1 O2 64.59(9) 8_565 8_565 ?
O3 Ho1 O6 151.44(9) 8_565 . ?
O3 Ho1 N1 101.43(10) 8_565 . ?
O3 Ho1 N7 130.01(9) 8_565 . ?
O3 Ho1 N10 67.86(9) 8_565 8_565 ?
O6 Ho1 Ho1 96.01(6) . 8_565 ?
O6 Ho1 Ho2 156.51(6) . . ?
O6 Ho1 N1 79.79(10) . . ?
O6 Ho1 N7 78.28(9) . . ?
O6 Ho1 N10 85.56(9) . 8_565 ?
N1 Ho1 Ho1 175.53(8) . 8_565 ?
N1 Ho1 Ho2 123.50(8) . . ?
N1 Ho1 N7 76.10(10) . . ?
N1 Ho1 N10 73.60(10) . 8_565 ?
N7 Ho1 Ho1 104.67(7) . 8_565 ?
N7 Ho1 Ho2 102.81(7) . . ?
N10 Ho1 Ho1 104.70(7) 8_565 8_565 ?
N10 Ho1 Ho2 103.04(7) 8_565 . ?
N10 Ho1 N7 147.69(10) 8_565 . ?
Ho1 Ho2 Ho1 58.422(13) . 8_565 ?
O2 Ho2 Ho1 79.95(6) 8_565 8_565 ?
O2 Ho2 Ho1 37.47(6) 8_565 . ?
O2 Ho2 Ho1 79.95(7) . . ?
O2 Ho2 Ho1 37.47(6) . 8_565 ?
O2 Ho2 O2 78.75(13) 8_565 . ?
O2 Ho2 O1AA 87.00(9) . 8_565 ?
O2 Ho2 O1AA 147.76(9) . . ?
O2 Ho2 O1AA 147.76(9) 8_565 8_565 ?
O2 Ho2 O1AA 87.00(9) 8_565 . ?
O2 Ho2 N8 68.90(9) . . ?
O2 Ho2 N8 68.90(9) 8_565 . ?
O2 Ho2 N6 132.07(8) 8_565 . ?
O2 Ho2 N6 132.07(8) . . ?
O1AA Ho2 Ho1 164.14(7) 8_565 . ?
O1AA Ho2 Ho1 105.72(7) 8_565 8_565 ?
O1AA Ho2 Ho1 164.14(7) . 8_565 ?
O1AA Ho2 Ho1 105.72(7) . . ?
O1AA Ho2 O1AA 90.12(14) 8_565 . ?
O1AA Ho2 N8 79.02(9) 8_565 . ?
O1AA Ho2 N8 79.02(9) . . ?
O1AA Ho2 N6 78.30(9) 8_565 . ?
O1AA Ho2 N6 78.30(9) . . ?
O3 Ho2 Ho1 79.61(6) 8_565 8_565 ?
O3 Ho2 Ho1 37.07(6) 8_565 . ?
O3 Ho2 Ho1 79.61(6) . . ?
O3 Ho2 Ho1 37.07(6) . 8_565 ?
O3 Ho2 O2 112.23(9) 8_565 . ?
O3 Ho2 O2 64.89(9) . . ?
O3 Ho2 O2 64.89(9) 8_565 8_565 ?
O3 Ho2 O2 112.23(9) . 8_565 ?
O3 Ho2 O1AA 86.73(9) . 8_565 ?
O3 Ho2 O1AA 147.00(9) . . ?
O3 Ho2 O1AA 86.73(9) 8_565 . ?
O3 Ho2 O1AA 147.00(9) 8_565 8_565 ?
O3 Ho2 O3 78.50(13) . 8_565 ?
O3 Ho2 N8 132.14(8) . . ?
O3 Ho2 N8 132.14(8) 8_565 . ?
O3 Ho2 N6 68.89(9) . . ?
O3 Ho2 N6 68.89(9) 8_565 . ?
N8 Ho2 Ho1 104.26(8) . 8_565 ?
N8 Ho2 Ho1 104.26(8) . . ?
N6 Ho2 Ho1 103.86(8) . 8_565 ?
N6 Ho2 Ho1 103.86(8) . . ?
N6 Ho2 N8 147.67(13) . . ?
C6AA Co1 C6AA 90.7(2) 8 . ?
C6AA Co1 C10 89.76(16) 8 . ?
C6AA Co1 C10 89.76(16) . . ?
C6AA Co1 C5AA 91.13(16) 8 . ?
C6AA Co1 C5AA 91.13(16) . . ?
C5AA Co1 C10 178.7(2) . . ?
C2 Co1 C6AA 178.82(16) . . ?
C2 Co1 C6AA 88.80(16) 8 . ?
C2 Co1 C6AA 178.82(16) 8 8 ?
C2 Co1 C6AA 88.80(16) . 8 ?
C2 Co1 C10 91.32(16) . . ?
C2 Co1 C10 91.32(16) 8 . ?
C2 Co1 C5AA 87.79(16) 8 . ?
C2 Co1 C5AA 87.79(16) . . ?
C2 Co1 C2 91.6(2) 8 . ?
Ho1 O1 Ho1 104.78(13) 8_565 . ?
C17 O1 Ho1 120.90(13) . . ?
C17 O1 Ho1 120.90(13) . 8_565 ?
Ho2 O2 Ho1 105.28(10) . 8_565 ?
C20 O2 Ho1 119.7(2) . 8_565 ?
C20 O2 Ho2 118.7(2) . . ?
Ho1 O0AA Ho1 104.10(13) 8_565 . ?
C1AA O0AA Ho1 119.96(13) . . ?
C1AA O0AA Ho1 119.96(13) . 8_565 ?
Ho2 O3 Ho1 106.00(10) . 8_565 ?
C13 O3 Ho1 119.6(2) . 8_565 ?
C13 O3 Ho2 118.5(2) . . ?
C2 N1 Ho1 142.2(3) . . ?
C0AA N7 Ho1 118.9(2) . . ?
C0AA N7 C14 106.3(3) . . ?
C0AA N7 C19 111.0(3) . 8_565 ?
C14 N7 Ho1 113.7(2) . . ?
C14 N7 C19 110.6(3) . 8_565 ?
C19 N7 Ho1 96.1(2) 8_565 . ?
C12 N8 Ho2 117.4(2) 8_565 . ?
C12 N8 Ho2 117.4(2) . . ?
C12 N8 C12 105.9(4) 8_565 . ?
C12 N8 C15 110.2(3) 8_565 . ?
C12 N8 C15 110.2(3) . . ?
C15 N8 Ho2 95.3(3) . . ?
C7 N6 Ho2 95.5(3) . . ?
C3AA N6 Ho2 116.4(2) 8_565 . ?
C3AA N6 Ho2 116.4(2) . . ?
C3AA N6 C7 110.8(3) . . ?
C3AA N6 C7 110.8(3) 8_565 . ?
C3AA N6 C3AA 106.7(4) . 8_565 ?
N6 C7 C13 109.3(3) . . ?
N6 C7 C13 109.3(3) . 8_565 ?
C13 C7 C13 112.8(4) 8_565 . ?
O3 C13 C7 111.8(3) . . ?
O3 C13 C11 110.6(3) . . ?
C7 C13 C11 110.9(3) . . ?
N8 C15 C20 109.2(3) . . ?
N8 C15 C20 109.2(3) . 8_565 ?
C20 C15 C20 112.6(4) . 8_565 ?
O2 C20 C15 112.0(3) . . ?
O2 C20 C19 111.1(3) . . ?
C19 C20 C15 110.9(3) . . ?
C11 N10 Ho1 95.9(2) . 8_565 ?
C2AA N10 Ho1 117.0(2) . 8_565 ?
C2AA N10 C11 109.4(3) . . ?
C4AA N10 Ho1 115.4(2) . 8_565 ?
C4AA N10 C11 111.0(3) . . ?
C4AA N10 C2AA 107.6(3) . . ?
N10 C11 C13 108.3(3) . . ?
N10 C11 C1AA 109.6(3) . . ?
C1AA C11 C13 113.3(3) . . ?
O0AA C1AA C11 111.2(3) . 8_565 ?
O0AA C1AA C11 111.2(3) . . ?
C11 C1AA C11 110.4(4) 8_565 . ?
O1 C17 C19 110.6(3) . 8_565 ?
O1 C17 C19 110.6(3) . . ?
C19 C17 C19 111.3(4) . 8_565 ?
N7 C19 C20 108.8(3) 8_565 . ?
N7 C19 C17 109.4(3) 8_565 . ?
C20 C19 C17 112.6(3) . . ?
N2AA C6AA Co1 177.4(4) . . ?
N1AA C10 Co1 179.0(5) . . ?
N0AA C5AA Co1 177.4(5) . . ?
N1 C2 Co1 177.9(3) . . ?

_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 -0.035 -0.250 0.152 341.5 96.6 10H2O
2 0.035 0.250 0.848 341.5 100.5 10H2O
3 0.465 0.750 0.348 341.5 97.7 10H20
4 0.535 0.250 0.652 341.5 99.4 10H2O

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_THETM01_hoco                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The low value of sine(theta_max)/wavelength results from the exclusion
of low quality reflections in the refinement process. 
;
####################################################################### 
# 
# 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_C30H56N12O10Tb3Cr
_database_code_depnum_ccdc_archive 'CCDC 1561420'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H56 Cr N12 O10 Tb3'
_chemical_formula_sum            'C30 H56 Cr N12 O10 Tb3'
_chemical_formula_weight         1273.62
_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'
Cr Cr 0.3209 0.6236 '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      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   14.280(5)
_cell_length_b                   13.311(4)
_cell_length_c                   13.873(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2637.0(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.898
_shelx_estimated_absorpt_T_min   0.173
_exptl_absorpt_coefficient_mu    4.226
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1265 before and 0.0447 after correction.
The Ratio of minimum to maximum transmission is 0.5212.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1238
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.026
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29281
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         2.047
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2887
_reflns_number_total             3033
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.991
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3033
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.062
_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)+(0.0258P)²+3.1829P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0488
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H0AA(0.5) H0AB(0.5) H9A(0.5) H9B(0.5)
3.a Rotating group:
 O0AA(H0AA,H0AB), O9(H9A,H9B)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C9(H9), C10(H10), C0AA(H0AC)
3.c Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC), C1AA(H1AA,H1AB,H1AC), C3AA(H3AA,H3AB,H3AC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.7500 0.11319(2) 0.22214(2) 0.01680(5) Uani 1 2 d S T P . .
Tb2 Tb 0.7500 0.2500 0.45453(2) 0.02829(7) Uani 1 4 d S T P . .
O2 O 0.83882(15) 0.2500 0.18096(15) 0.0195(4) Uani 1 2 d S T P . .
O3 O 0.83838(11) 0.13969(12) 0.36213(11) 0.0234(3) Uani 1 1 d . . . . .
C5 C 0.9367(2) 0.2500 0.1954(2) 0.0245(7) Uani 1 2 d S T P . .
H5 H 0.9675 0.2500 0.1306 0.029 Uiso 1 2 calc RS T P . .
C9 C 0.93644(17) 0.15439(18) 0.35438(18) 0.0283(5) Uani 1 1 d . . . . .
H9 H 0.9680 0.0964 0.3868 0.034 Uiso 1 1 calc R . . . .
C10 C 0.96777(17) 0.15528(18) 0.24892(19) 0.0273(5) Uani 1 1 d . . . . .
H10 H 1.0377 0.1511 0.2467 0.033 Uiso 1 1 calc R . . . .
N4 N 0.92805(14) 0.06524(14) 0.20005(15) 0.0256(4) Uani 1 1 d . . . . .
N5 N 0.9287(3) 0.2500 0.5057(2) 0.0408(8) Uani 1 2 d S T P . .
Cr1 Cr 0.7500 -0.2500 0.04577(6) 0.02990(18) Uani 1 4 d S T P . .
O0AA O 0.7500 0.09391(19) 0.04691(17) 0.0350(6) Uani 1 2 d S T P . .
H0AA H 0.7064 0.1332 0.0200 0.052 Uiso 0.5 1 d GR . . . .
H0AB H 0.7320 0.0319 0.0303 0.052 Uiso 0.5 1 d GR . . . .
C4 C 0.7500 -0.1387(2) 0.1499(3) 0.0289(7) Uani 1 2 d S T P . .
N0AA N 0.7500 -0.0717(2) 0.2027(2) 0.0322(7) Uani 1 2 d S T P . .
C0AA C 0.9673(3) 0.2500 0.4057(3) 0.0330(8) Uani 1 2 d S T P . .
H0AC H 1.0373 0.2500 0.4098 0.040 Uiso 1 2 calc RS T P . .
C2AA C 0.9614(2) 0.0579(2) 0.0996(2) 0.0373(6) Uani 1 1 d . . . . .
H2AA H 0.9374 -0.0041 0.0704 0.056 Uiso 1 1 calc GR . . . .
H2AB H 1.0300 0.0569 0.0988 0.056 Uiso 1 1 calc GR . . . .
H2AC H 0.9388 0.1159 0.0628 0.056 Uiso 1 1 calc GR . . . .
C6 C 0.7500 -0.3627(3) -0.0577(3) 0.0356(8) Uani 1 2 d S T P . .
C8 C 0.6053(3) -0.2500 0.0535(3) 0.0340(8) Uani 1 2 d S T P . .
O9 O 0.7500 0.1261(4) 0.5821(3) 0.0777(13) Uani 1 2 d S T P . .
H9A H 0.7260 0.1344 0.6610 0.117 Uiso 0.5 1 d GR . . . .
H9B H 0.7739 0.0436 0.5797 0.117 Uiso 0.5 1 d GR . . . .
C1AA C 0.9584(2) -0.02762(19) 0.2498(2) 0.0347(6) Uani 1 1 d . . . . .
H1AA H 0.9285 -0.0313 0.3133 0.052 Uiso 1 1 calc GR . . . .
H1AB H 1.0266 -0.0268 0.2576 0.052 Uiso 1 1 calc GR . . . .
H1AC H 0.9401 -0.0862 0.2114 0.052 Uiso 1 1 calc GR . . . .
N2AA N 0.5255(3) -0.2500 0.0646(3) 0.0407(8) Uani 1 2 d S T P . .
N1AA N 0.7500 -0.4293(2) -0.1113(3) 0.0429(8) Uani 1 2 d S T P . .
C3AA C 0.9611(3) 0.1605(3) 0.5593(2) 0.0615(10) Uani 1 1 d . . . . .
H3AA H 0.9404 0.1651 0.6265 0.092 Uiso 1 1 calc GR . . . .
H3AB H 1.0296 0.1571 0.5571 0.092 Uiso 1 1 calc GR . . . .
H3AC H 0.9347 0.0998 0.5298 0.092 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 Tb1 3.6422(12) 2_655 ?
Tb1 Tb2 3.7028(10) . ?
Tb1 O2 2.2916(14) 2_655 ?
Tb1 O2 2.2916(14) . ?
Tb1 O3 2.3429(16) 7_755 ?
Tb1 O3 2.3429(16) . ?
Tb1 N4 2.639(2) 7_755 ?
Tb1 N4 2.639(2) . ?
Tb1 O0AA 2.444(2) . ?
Tb1 N0AA 2.476(3) . ?
Tb2 Tb1 3.7028(10) 2_655 ?
Tb2 O3 2.3221(17) 7_755 ?
Tb2 O3 2.3221(17) 8_565 ?
Tb2 O3 2.3221(17) 2_655 ?
Tb2 O3 2.3221(17) . ?
Tb2 N5 2.649(4) 2_655 ?
Tb2 N5 2.649(4) . ?
Tb2 O9 2.420(3) . ?
Tb2 O9 2.420(3) 2_655 ?
O2 Tb1 2.2916(14) 2_655 ?
O2 C5 1.411(4) . ?
O3 C9 1.418(3) . ?
C5 C10 1.529(3) 8_565 ?
C5 C10 1.529(3) . ?
C9 C10 1.530(4) . ?
C9 C0AA 1.523(3) . ?
C10 N4 1.489(3) . ?
N4 C2AA 1.476(3) . ?
N4 C1AA 1.480(3) . ?
N5 C0AA 1.494(5) . ?
N5 C3AA 1.479(4) . ?
N5 C3AA 1.479(4) 8_565 ?
Cr1 C4 2.069(4) . ?
Cr1 C4 2.069(4) 2_645 ?
Cr1 C6 2.076(4) . ?
Cr1 C6 2.076(4) 2_645 ?
Cr1 C8 2.070(4) . ?
Cr1 C8 2.070(4) 2_645 ?
C4 N0AA 1.154(5) . ?
C0AA C9 1.523(3) 8_565 ?
C6 N1AA 1.158(5) . ?
C8 N2AA 1.149(5) . ?

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
Tb1 Tb1 Tb2 60.540(11) 2_655 . ?
O2 Tb1 Tb1 37.37(4) . 2_655 ?
O2 Tb1 Tb1 37.37(4) 2_655 2_655 ?
O2 Tb1 Tb2 79.99(5) 2_655 . ?
O2 Tb1 Tb2 79.99(5) . . ?
O2 Tb1 O2 67.21(10) . 2_655 ?
O2 Tb1 O3 112.65(6) 2_655 . ?
O2 Tb1 O3 112.65(6) . 7_755 ?
O2 Tb1 O3 77.81(7) . . ?
O2 Tb1 O3 77.81(7) 2_655 7_755 ?
O2 Tb1 N4 134.14(6) . 7_755 ?
O2 Tb1 N4 68.29(6) 2_655 7_755 ?
O2 Tb1 N4 68.29(6) . . ?
O2 Tb1 N4 134.14(6) 2_655 . ?
O2 Tb1 O0AA 80.53(7) . . ?
O2 Tb1 O0AA 80.53(7) 2_655 . ?
O2 Tb1 N0AA 139.70(6) 2_655 . ?
O2 Tb1 N0AA 139.70(6) . . ?
O3 Tb1 Tb1 81.34(4) 7_755 2_655 ?
O3 Tb1 Tb1 81.34(4) . 2_655 ?
O3 Tb1 Tb2 37.27(4) . . ?
O3 Tb1 Tb2 37.27(4) 7_755 . ?
O3 Tb1 O3 65.19(8) 7_755 . ?
O3 Tb1 N4 130.66(6) . 7_755 ?
O3 Tb1 N4 67.28(6) 7_755 7_755 ?
O3 Tb1 N4 67.27(6) . . ?
O3 Tb1 N4 130.66(6) 7_755 . ?
O3 Tb1 O0AA 147.16(4) 7_755 . ?
O3 Tb1 O0AA 147.16(4) . . ?
O3 Tb1 N0AA 103.90(7) . . ?
O3 Tb1 N0AA 103.89(7) 7_755 . ?
N4 Tb1 Tb1 103.99(4) . 2_655 ?
N4 Tb1 Tb1 103.99(4) 7_755 2_655 ?
N4 Tb1 Tb2 102.71(4) . . ?
N4 Tb1 Tb2 102.71(4) 7_755 . ?
N4 Tb1 N4 148.88(9) 7_755 . ?
O0AA Tb1 Tb1 96.02(6) . 2_655 ?
O0AA Tb1 Tb2 156.56(6) . . ?
O0AA Tb1 N4 81.90(5) . 7_755 ?
O0AA Tb1 N4 81.90(5) . . ?
O0AA Tb1 N0AA 77.71(10) . . ?
N0AA Tb1 Tb1 173.73(8) . 2_655 ?
N0AA Tb1 Tb2 125.73(8) . . ?
N0AA Tb1 N4 75.34(4) . . ?
N0AA Tb1 N4 75.34(4) . 7_755 ?
Tb1 Tb2 Tb1 58.92(2) . 2_655 ?
O3 Tb2 Tb1 37.66(4) 8_565 2_655 ?
O3 Tb2 Tb1 80.23(4) . 2_655 ?
O3 Tb2 Tb1 80.23(4) 2_655 . ?
O3 Tb2 Tb1 37.66(4) 2_655 2_655 ?
O3 Tb2 Tb1 80.23(4) 7_755 2_655 ?
O3 Tb2 Tb1 80.23(4) 8_565 . ?
O3 Tb2 Tb1 37.66(4) 7_755 . ?
O3 Tb2 Tb1 37.66(4) . . ?
O3 Tb2 O3 65.85(8) . 7_755 ?
O3 Tb2 O3 78.45(8) 7_755 2_655 ?
O3 Tb2 O3 78.45(8) . 8_565 ?
O3 Tb2 O3 112.99(8) 7_755 8_565 ?
O3 Tb2 O3 65.85(8) 8_565 2_655 ?
O3 Tb2 O3 112.99(8) . 2_655 ?
O3 Tb2 N5 67.94(7) 7_755 2_655 ?
O3 Tb2 N5 132.19(6) . 2_655 ?
O3 Tb2 N5 132.19(6) 8_565 2_655 ?
O3 Tb2 N5 67.94(7) 8_565 . ?
O3 Tb2 N5 67.94(7) . . ?
O3 Tb2 N5 132.19(6) 2_655 . ?
O3 Tb2 N5 132.19(6) 7_755 . ?
O3 Tb2 N5 67.94(7) 2_655 2_655 ?
O3 Tb2 O9 146.61(4) 8_565 . ?
O3 Tb2 O9 146.61(4) 2_655 . ?
O3 Tb2 O9 88.43(11) . . ?
O3 Tb2 O9 88.43(11) 7_755 . ?
O3 Tb2 O9 88.43(11) 8_565 2_655 ?
O3 Tb2 O9 88.43(11) 2_655 2_655 ?
O3 Tb2 O9 146.61(4) 7_755 2_655 ?
O3 Tb2 O9 146.61(4) . 2_655 ?
N5 Tb2 Tb1 103.50(6) . 2_655 ?
N5 Tb2 Tb1 103.50(6) 2_655 2_655 ?
N5 Tb2 Tb1 103.50(6) 2_655 . ?
N5 Tb2 Tb1 103.50(6) . . ?
N5 Tb2 N5 148.90(15) . 2_655 ?
O9 Tb2 Tb1 166.47(12) . 2_655 ?
O9 Tb2 Tb1 107.55(12) . . ?
O9 Tb2 Tb1 107.56(12) 2_655 2_655 ?
O9 Tb2 Tb1 166.48(12) 2_655 . ?
O9 Tb2 N5 78.69(6) 2_655 2_655 ?
O9 Tb2 N5 78.69(6) 2_655 . ?
O9 Tb2 N5 78.69(6) . 2_655 ?
O9 Tb2 N5 78.69(6) . . ?
O9 Tb2 O9 86.0(2) 2_655 . ?
Tb1 O2 Tb1 105.25(9) 2_655 . ?
C5 O2 Tb1 120.83(8) . . ?
C5 O2 Tb1 120.83(8) . 2_655 ?
Tb2 O3 Tb1 105.07(7) . . ?
C9 O3 Tb1 119.33(14) . . ?
C9 O3 Tb2 119.43(14) . . ?
O2 C5 C10 110.88(17) . 8_565 ?
O2 C5 C10 110.88(17) . . ?
C10 C5 C10 111.1(3) 8_565 . ?
O3 C9 C10 111.25(19) . . ?
O3 C9 C0AA 111.5(2) . . ?
C0AA C9 C10 110.8(2) . . ?
C5 C10 C9 112.7(2) . . ?
N4 C10 C5 109.4(2) . . ?
N4 C10 C9 108.52(19) . . ?
C10 N4 Tb1 96.86(13) . . ?
C2AA N4 Tb1 115.85(16) . . ?
C2AA N4 C10 111.14(19) . . ?
C2AA N4 C1AA 106.9(2) . . ?
C1AA N4 Tb1 115.44(15) . . ?
C1AA N4 C10 110.4(2) . . ?
C0AA N5 Tb2 96.1(2) . . ?
C3AA N5 Tb2 115.8(2) 8_565 . ?
C3AA N5 Tb2 115.8(2) . . ?
C3AA N5 C0AA 110.6(3) 8_565 . ?
C3AA N5 C0AA 110.6(3) . . ?
C3AA N5 C3AA 107.4(4) . 8_565 ?
C4 Cr1 C4 91.49(19) . 2_645 ?
C4 Cr1 C6 179.48(14) . . ?
C4 Cr1 C6 87.99(14) 2_645 . ?
C4 Cr1 C6 87.99(14) . 2_645 ?
C4 Cr1 C6 179.49(14) 2_645 2_645 ?
C4 Cr1 C8 87.91(8) . 2_645 ?
C4 Cr1 C8 87.92(8) . . ?
C4 Cr1 C8 87.92(8) 2_645 . ?
C4 Cr1 C8 87.91(8) 2_645 2_645 ?
C6 Cr1 C6 92.5(2) 2_645 . ?
C8 Cr1 C6 92.07(8) 2_645 . ?
C8 Cr1 C6 92.07(8) 2_645 2_645 ?
C8 Cr1 C6 92.07(8) . 2_645 ?
C8 Cr1 C6 92.06(8) . . ?
C8 Cr1 C8 174.0(2) . 2_645 ?
N0AA C4 Cr1 175.2(3) . . ?
C4 N0AA Tb1 146.8(3) . . ?
C9 C0AA C9 113.3(3) . 8_565 ?
N5 C0AA C9 109.1(2) . . ?
N5 C0AA C9 109.1(2) . 8_565 ?
N1AA C6 Cr1 176.3(3) . . ?
N2AA C8 Cr1 175.3(4) . . ?

_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 -0.556 0.250 0.594 354.1 82.9 8H2O
2 -0.093 0.750 0.406 354.1 83.7 8H2O

_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_C30H56N12O10Gd3Cr
_database_code_depnum_ccdc_archive 'CCDC 1561417'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H56 Cr Gd3 N12 O10'
_chemical_formula_sum            'C30 H56 Cr Gd3 N12 O10'
_chemical_formula_weight         1268.61
_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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   14.419(6)
_cell_length_b                   13.366(6)
_cell_length_c                   13.772(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2654.2(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.950
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1396 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.6079.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.989
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.034
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25425
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.054
_diffrn_reflns_theta_min         2.045
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2365
_reflns_number_total             2533
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.050
_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)+(0.0202P)²+1.3095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0426
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H4d(0.5) H4e(0.5) H1a(0.5) H1b(0.5)
3.a Rotating group:
 O4(H4d,H4e), O1(H1a,H1b)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9)
3.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C7(H7a,H7b,H7c), C10(H10a,H10b,H10c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd2 Gd 0.2500 0.2500 0.95622(2) 0.02464(7) Uani 1 4 d S T P . .
Gd1 Gd 0.2500 0.11416(2) 0.72205(2) 0.01837(6) Uani 1 2 d S T P . .
Cr1 Cr 0.2500 -0.2500 0.54971(6) 0.0337(2) Uani 1 4 d S T P . .
O3 O 0.16323(11) 0.13981(12) 0.86315(12) 0.0265(4) Uani 1 1 d . . . . .
O2 O 0.33785(16) 0.2500 0.68124(16) 0.0246(5) Uani 1 2 d S T P . .
N1 N 0.2500 -0.0695(2) 0.7054(2) 0.0357(7) Uani 1 2 d S T P . .
C1 C 0.2500 -0.1378(3) 0.6532(3) 0.0330(8) Uani 1 2 d S T P . .
N4 N 0.07420(15) 0.06567(15) 0.70014(15) 0.0309(5) Uani 1 1 d . . . . .
N5 N 0.0738(2) 0.2500 1.0077(2) 0.0424(8) Uani 1 2 d S T P . .
C5 C 0.4345(2) 0.2500 0.6958(3) 0.0286(8) Uani 1 2 d S T P . .
H5 H 0.4643 0.2500 0.6318 0.034 Uiso 1 2 calc RS T P . .
C6 C 0.46504(17) 0.15536(19) 0.7492(2) 0.0315(6) Uani 1 1 d . . . . .
H6 H 0.5329 0.1512 0.7471 0.038 Uiso 1 1 calc R . . . .
C8 C 0.06607(17) 0.15470(19) 0.85537(18) 0.0303(6) Uani 1 1 d . . . . .
H8 H 0.0354 0.0982 0.8874 0.036 Uiso 1 1 calc R . . . .
C9 C 0.0357(3) 0.2500 0.9074(3) 0.0354(9) Uani 1 2 d S T P . .
H9 H -0.0321 0.2500 0.9116 0.042 Uiso 1 2 calc RS T P . .
C2 C 0.1064(3) -0.2500 0.5559(3) 0.0403(10) Uani 1 2 d S T P . .
N2 N 0.0278(3) -0.2500 0.5649(3) 0.0475(9) Uani 1 2 d S T P . .
C4 C 0.0415(2) 0.0586(2) 0.5988(2) 0.0453(7) Uani 1 1 d . . . . .
H4A H 0.0623 0.1161 0.5631 0.068 Uiso 1 1 calc GR . . . .
H4B H -0.0250 0.0562 0.5979 0.068 Uiso 1 1 calc GR . . . .
H4C H 0.0660 -0.0010 0.5695 0.068 Uiso 1 1 calc GR . . . .
C7 C 0.0432(2) -0.0268(2) 0.7495(2) 0.0400(7) Uani 1 1 d . . . . .
H7A H 0.0585 -0.0837 0.7101 0.060 Uiso 1 1 calc GR . . . .
H7B H -0.0227 -0.0243 0.7591 0.060 Uiso 1 1 calc GR . . . .
H7C H 0.0737 -0.0323 0.8112 0.060 Uiso 1 1 calc GR . . . .
C10 C 0.0420(2) 0.3393(3) 1.0620(2) 0.0636(10) Uani 1 1 d . . . . .
H10A H 0.0604 0.3336 1.1288 0.095 Uiso 1 1 calc GR . . . .
H10B H -0.0244 0.3440 1.0582 0.095 Uiso 1 1 calc GR . . . .
H10C H 0.0692 0.3983 1.0343 0.095 Uiso 1 1 calc GR . . . .
O4 O 0.2500 0.1304(3) 1.0851(2) 0.0616(9) Uani 1 2 d S T P . .
H4D H 0.2713 0.1399 1.1533 0.092 Uiso 0.5 1 d GR . . . .
H4E H 0.2284 0.0595 1.0831 0.092 Uiso 0.5 1 d GR . . . .
O1 O 0.2500 0.09463(19) 0.54725(17) 0.0417(7) Uani 1 2 d S T P . .
H1A H 0.2049 0.1325 0.5172 0.063 Uiso 0.5 1 d GR . . . .
H1B H 0.2337 0.0310 0.5278 0.063 Uiso 0.5 1 d GR . . . .
C3 C 0.2500 -0.1372(3) 0.4451(3) 0.0411(10) Uani 1 2 d S T P . .
N3 N 0.2500 -0.0704(3) 0.3924(3) 0.0529(10) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd2 Gd1 3.7010(13) . ?
Gd2 Gd1 3.7010(13) 2 ?
Gd2 O3 2.3189(17) 8_565 ?
Gd2 O3 2.3189(17) 2 ?
Gd2 O3 2.3189(17) . ?
Gd2 O3 2.3189(17) 7_655 ?
Gd2 N5 2.637(4) 2 ?
Gd2 N5 2.637(4) . ?
Gd2 O4 2.389(3) . ?
Gd2 O4 2.389(3) 2 ?
Gd1 Gd1 3.6314(15) 2 ?
Gd1 O3 2.3366(17) 7_655 ?
Gd1 O3 2.3366(17) . ?
Gd1 O2 2.2842(15) . ?
Gd1 O2 2.2841(15) 2 ?
Gd1 N1 2.465(3) . ?
Gd1 N4 2.634(2) . ?
Gd1 N4 2.634(2) 7_655 ?
Gd1 O1 2.421(3) . ?
Cr1 C1 2.069(4) 2_545 ?
Cr1 C1 2.069(4) . ?
Cr1 C2 2.072(5) 2_545 ?
Cr1 C2 2.072(5) . ?
Cr1 C3 2.086(4) . ?
Cr1 C3 2.086(4) 2_545 ?
O3 C8 1.419(3) . ?
O2 Gd1 2.2842(15) 2 ?
O2 C5 1.408(4) . ?
N1 C1 1.162(5) . ?
N4 C6 1.488(4) 7_655 ?
N4 C4 1.476(3) . ?
N4 C7 1.479(3) . ?
N5 C9 1.487(5) . ?
N5 C10 1.482(4) 8_565 ?
N5 C10 1.482(4) . ?
C5 C6 1.528(3) . ?
C5 C6 1.528(3) 8_565 ?
C6 N4 1.488(4) 7_655 ?
C6 C8 1.530(4) 7_655 ?
C8 C6 1.530(4) 7_655 ?
C8 C9 1.525(3) . ?
C9 C8 1.525(3) 8_565 ?
C2 N2 1.141(5) . ?
C3 N3 1.151(5) . ?

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
Gd1 Gd2 Gd1 58.76(3) . 2 ?
O3 Gd2 Gd1 37.51(4) 7_655 . ?
O3 Gd2 Gd1 37.51(4) 8_565 2 ?
O3 Gd2 Gd1 37.51(4) . . ?
O3 Gd2 Gd1 80.21(5) 7_655 2 ?
O3 Gd2 Gd1 80.21(5) 2 . ?
O3 Gd2 Gd1 37.51(4) 2 2 ?
O3 Gd2 Gd1 80.21(5) 8_565 . ?
O3 Gd2 Gd1 80.21(5) . 2 ?
O3 Gd2 O3 78.86(9) 7_655 2 ?
O3 Gd2 O3 78.86(9) 8_565 . ?
O3 Gd2 O3 112.90(8) 7_655 8_565 ?
O3 Gd2 O3 65.31(8) 7_655 . ?
O3 Gd2 O3 112.90(8) 2 . ?
O3 Gd2 O3 65.31(8) 2 8_565 ?
O3 Gd2 N5 68.21(7) 2 2 ?
O3 Gd2 N5 131.93(6) 8_565 2 ?
O3 Gd2 N5 131.93(6) 2 . ?
O3 Gd2 N5 68.21(7) . . ?
O3 Gd2 N5 68.21(7) 8_565 . ?
O3 Gd2 N5 131.93(6) 7_655 . ?
O3 Gd2 N5 68.21(7) 7_655 2 ?
O3 Gd2 N5 131.93(6) . 2 ?
O3 Gd2 O4 89.18(9) 2 2 ?
O3 Gd2 O4 146.69(4) 7_655 2 ?
O3 Gd2 O4 146.69(4) . 2 ?
O3 Gd2 O4 146.69(4) 8_565 . ?
O3 Gd2 O4 89.18(9) 8_565 2 ?
O3 Gd2 O4 89.18(9) 7_655 . ?
O3 Gd2 O4 146.69(4) 2 . ?
O3 Gd2 O4 89.18(9) . . ?
N5 Gd2 Gd1 103.54(6) 2 . ?
N5 Gd2 Gd1 103.54(6) 2 2 ?
N5 Gd2 Gd1 103.54(6) . . ?
N5 Gd2 Gd1 103.54(6) . 2 ?
N5 Gd2 N5 148.82(14) . 2 ?
O4 Gd2 Gd1 167.38(8) 2 . ?
O4 Gd2 Gd1 167.38(8) . 2 ?
O4 Gd2 Gd1 108.62(9) . . ?
O4 Gd2 Gd1 108.62(9) 2 2 ?
O4 Gd2 N5 78.48(6) 2 . ?
O4 Gd2 N5 78.48(6) 2 2 ?
O4 Gd2 N5 78.48(6) . . ?
O4 Gd2 N5 78.48(6) . 2 ?
O4 Gd2 O4 84.01(17) 2 . ?
Gd1 Gd1 Gd2 60.621(15) 2 . ?
O3 Gd1 Gd2 37.18(4) 7_655 . ?
O3 Gd1 Gd2 37.18(4) . . ?
O3 Gd1 Gd1 81.56(4) 7_655 2 ?
O3 Gd1 Gd1 81.56(4) . 2 ?
O3 Gd1 O3 64.75(8) . 7_655 ?
O3 Gd1 N1 102.92(7) . . ?
O3 Gd1 N1 102.92(7) 7_655 . ?
O3 Gd1 N4 130.30(6) . 7_655 ?
O3 Gd1 N4 130.30(6) 7_655 . ?
O3 Gd1 N4 67.42(6) . . ?
O3 Gd1 N4 67.42(6) 7_655 7_655 ?
O3 Gd1 O1 147.42(4) . . ?
O3 Gd1 O1 147.42(4) 7_655 . ?
O2 Gd1 Gd2 79.88(6) 2 . ?
O2 Gd1 Gd2 79.89(6) . . ?
O2 Gd1 Gd1 37.35(5) . 2 ?
O2 Gd1 Gd1 37.35(5) 2 2 ?
O2 Gd1 O3 77.94(7) . 7_655 ?
O2 Gd1 O3 112.64(7) . . ?
O2 Gd1 O3 77.93(7) 2 . ?
O2 Gd1 O3 112.64(7) 2 7_655 ?
O2 Gd1 O2 67.37(10) 2 . ?
O2 Gd1 N1 140.22(6) . . ?
O2 Gd1 N1 140.22(6) 2 . ?
O2 Gd1 N4 68.51(7) . 7_655 ?
O2 Gd1 N4 134.52(7) . . ?
O2 Gd1 N4 134.52(7) 2 7_655 ?
O2 Gd1 N4 68.51(7) 2 . ?
O2 Gd1 O1 80.86(7) 2 . ?
O2 Gd1 O1 80.86(7) . . ?
N1 Gd1 Gd2 124.73(8) . . ?
N1 Gd1 Gd1 174.65(7) . 2 ?
N1 Gd1 N4 75.19(5) . 7_655 ?
N1 Gd1 N4 75.19(5) . . ?
N4 Gd1 Gd2 102.74(5) . . ?
N4 Gd1 Gd2 102.74(5) 7_655 . ?
N4 Gd1 Gd1 104.24(5) . 2 ?
N4 Gd1 Gd1 104.24(5) 7_655 2 ?
N4 Gd1 N4 148.50(9) . 7_655 ?
O1 Gd1 Gd2 156.81(6) . . ?
O1 Gd1 Gd1 96.19(6) . 2 ?
O1 Gd1 N1 78.47(9) . . ?
O1 Gd1 N4 81.93(5) . . ?
O1 Gd1 N4 81.93(5) . 7_655 ?
C1 Cr1 C1 92.9(2) . 2_545 ?
C1 Cr1 C2 88.38(8) 2_545 . ?
C1 Cr1 C2 88.38(8) . . ?
C1 Cr1 C2 88.38(8) . 2_545 ?
C1 Cr1 C2 88.38(8) 2_545 2_545 ?
C1 Cr1 C3 179.84(15) 2_545 . ?
C1 Cr1 C3 87.23(15) 2_545 2_545 ?
C1 Cr1 C3 87.23(15) . . ?
C1 Cr1 C3 179.84(15) . 2_545 ?
C2 Cr1 C2 175.3(2) . 2_545 ?
C2 Cr1 C3 91.63(8) 2_545 . ?
C2 Cr1 C3 91.63(8) . . ?
C2 Cr1 C3 91.63(8) 2_545 2_545 ?
C2 Cr1 C3 91.63(8) . 2_545 ?
C3 Cr1 C3 92.6(2) . 2_545 ?
Gd2 O3 Gd1 105.30(7) . . ?
C8 O3 Gd2 119.04(14) . . ?
C8 O3 Gd1 119.10(14) . . ?
Gd1 O2 Gd1 105.30(9) . 2 ?
C5 O2 Gd1 120.93(9) . . ?
C5 O2 Gd1 120.93(9) . 2 ?
C1 N1 Gd1 147.1(3) . . ?
N1 C1 Cr1 174.7(3) . . ?
C6 N4 Gd1 96.65(14) 7_655 . ?
C4 N4 Gd1 115.55(17) . . ?
C4 N4 C6 111.1(2) . 7_655 ?
C4 N4 C7 106.5(2) . . ?
C7 N4 Gd1 116.33(16) . . ?
C7 N4 C6 110.5(2) . 7_655 ?
C9 N5 Gd2 96.1(2) . . ?
C10 N5 Gd2 115.7(2) . . ?
C10 N5 Gd2 115.7(2) 8_565 . ?
C10 N5 C9 110.8(2) . . ?
C10 N5 C9 110.8(2) 8_565 . ?
C10 N5 C10 107.3(4) 8_565 . ?
O2 C5 C6 110.72(18) . . ?
O2 C5 C6 110.72(18) . 8_565 ?
C6 C5 C6 111.7(3) . 8_565 ?
N4 C6 C5 109.8(2) 7_655 . ?
N4 C6 C8 108.5(2) 7_655 7_655 ?
C5 C6 C8 112.4(2) . 7_655 ?
O3 C8 C6 111.3(2) . 7_655 ?
O3 C8 C9 111.4(2) . . ?
C9 C8 C6 111.1(2) . 7_655 ?
N5 C9 C8 109.3(2) . 8_565 ?
N5 C9 C8 109.3(2) . . ?
C8 C9 C8 113.2(3) 8_565 . ?
N2 C2 Cr1 176.1(4) . . ?
N3 C3 Cr1 175.4(4) . . ?

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
O1 H1B N3 0.92 2.32 3.068(5) 138.4 .

_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 -0.002 -0.041 0.000 754.5 194.3 '20 H2O'

_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_C30H54N12O9Tb3Fe
_database_code_depnum_ccdc_archive 'CCDC 1561421'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-04-13 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C60 H108 Fe2 N24 O18 Tb6)'
_chemical_formula_sum            'C30 H54 Fe N12 O9 Tb3'
_chemical_formula_weight         1259.46
_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'
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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   16.359(3)
_cell_length_b                   18.917(3)
_cell_length_c                   14.106(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4365.1(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6546
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.186
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7996.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2444
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.042
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.822
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37251
_diffrn_reflns_point_group_measured_fraction_full 0.822
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.558
_diffrn_reflns_theta_min         2.153
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.822
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2864
_reflns_number_total             3353
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker-Axs ApexII'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.048
_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)+(0.0187P)²+11.9238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0558
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1a(0.5) H1b(0.5) H2a(0.5) H2b(0.5) H3a(0.5) H3b(0.5)
3.a Rotating group:
 O1(H1a,H1b), O2(H2a,H2b), O3(H3a,H3b)
3.b Ternary CH refined with riding coordinates:
 C8AA(H8AA), C12(H12), C0AA(H0AA), C1AA(H1AA), C9AA(H9AA), C4AA(H4AA)
3.c Idealised Me refined as rotating group:
 C2AA(H2Aa,H2Ab,H2Ac), C3AA(H3Aa,H3Ab,H3Ac), C14(H14a,H14b,H14c), C5AA(H5Aa,
 H5Ab,H5Ac), C13(H13a,H13b,H13c), C6AA(H6Aa,H6Ab,H6Ac)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb3 Tb 0.83602(2) 0.7500 0.50862(2) 0.01314(10) Uani 1 2 d S T P . .
Tb2 Tb 0.67311(2) 0.7500 0.32480(2) 0.01730(11) Uani 1 2 d S T P . .
Tb1 Tb 0.61881(2) 0.7500 0.57899(2) 0.01740(10) Uani 1 2 d S T P . .
O4 O 0.73774(19) 0.81636(17) 0.5835(2) 0.0156(8) Uani 1 1 d . . . . .
O6 O 0.78218(19) 0.81663(17) 0.3828(2) 0.0153(8) Uani 1 1 d . . . . .
O5 O 0.6096(2) 0.81733(19) 0.4414(2) 0.0199(8) Uani 1 1 d . . . . .
N8 N 0.5925(3) 0.8869(2) 0.6180(3) 0.0244(11) Uani 1 1 d . . . . .
C8AA C 0.6235(3) 0.8918(3) 0.4458(4) 0.0231(13) Uani 1 1 d . . . . .
H8AA H 0.5706 0.9159 0.4309 0.028 Uiso 1 1 calc R . . . .
C12 C 0.7970(3) 0.9142(3) 0.4943(3) 0.0186(12) Uani 1 1 d . . . . .
H12 H 0.8012 0.9669 0.4956 0.022 Uiso 1 1 calc R . . . .
C0AA C 0.7366(3) 0.8909(3) 0.5698(4) 0.0192(12) Uani 1 1 d . . . . .
H0AA H 0.7527 0.9137 0.6310 0.023 Uiso 1 1 calc R . . . .
C1AA C 0.6858(3) 0.9152(3) 0.3720(3) 0.0210(12) Uani 1 1 d . . . . .
H1AA H 0.6852 0.9680 0.3685 0.025 Uiso 1 1 calc R . . . .
N7 N 0.8797(2) 0.8833(2) 0.5162(3) 0.0187(10) Uani 1 1 d . . . . .
N6 N 0.6619(3) 0.8864(2) 0.2770(3) 0.0225(10) Uani 1 1 d . . . . .
C2AA C 0.5796(3) 0.9112(3) 0.2500(4) 0.0320(14) Uani 1 1 d . . . . .
H2AA H 0.5672 0.8956 0.1853 0.048 Uiso 1 1 calc GR . . . .
H2AB H 0.5779 0.9630 0.2529 0.048 Uiso 1 1 calc GR . . . .
H2AC H 0.5391 0.8916 0.2939 0.048 Uiso 1 1 calc GR . . . .
C3AA C 0.9101(3) 0.9095(3) 0.6084(4) 0.0277(14) Uani 1 1 d . . . . .
H3AA H 0.8719 0.8958 0.6587 0.041 Uiso 1 1 calc GR . . . .
H3AB H 0.9146 0.9611 0.6063 0.041 Uiso 1 1 calc GR . . . .
H3AC H 0.9640 0.8890 0.6213 0.041 Uiso 1 1 calc GR . . . .
C14 C 0.9395(3) 0.9066(3) 0.4436(4) 0.0263(13) Uani 1 1 d . . . . .
H14A H 0.9947 0.8930 0.4634 0.039 Uiso 1 1 calc GR . . . .
H14B H 0.9366 0.9581 0.4367 0.039 Uiso 1 1 calc GR . . . .
H14C H 0.9266 0.8841 0.3828 0.039 Uiso 1 1 calc GR . . . .
C5AA C 0.7195(3) 0.9125(3) 0.2033(3) 0.0257(13) Uani 1 1 d . . . . .
H5AA H 0.7729 0.8897 0.2117 0.039 Uiso 1 1 calc GR . . . .
H5AB H 0.7257 0.9638 0.2093 0.039 Uiso 1 1 calc GR . . . .
H5AC H 0.6980 0.9010 0.1403 0.039 Uiso 1 1 calc GR . . . .
C9AA C 0.6502(3) 0.9156(3) 0.5449(3) 0.0213(13) Uani 1 1 d . . . . .
H9AA H 0.6486 0.9684 0.5475 0.026 Uiso 1 1 calc R . . . .
C4AA C 0.7730(3) 0.8910(3) 0.3946(3) 0.0174(12) Uani 1 1 d . . . . .
H4AA H 0.8107 0.9149 0.3489 0.021 Uiso 1 1 calc R . . . .
C13 C 0.5090(3) 0.9141(4) 0.6013(4) 0.0401(17) Uani 1 1 d . . . . .
H13A H 0.4892 0.8972 0.5398 0.060 Uiso 1 1 calc GR . . . .
H13B H 0.5099 0.9659 0.6015 0.060 Uiso 1 1 calc GR . . . .
H13C H 0.4726 0.8972 0.6516 0.060 Uiso 1 1 calc GR . . . .
C6AA C 0.6172(4) 0.9101(3) 0.7142(4) 0.0316(14) Uani 1 1 d . . . . .
H6AA H 0.5743 0.8975 0.7597 0.047 Uiso 1 1 calc GR . . . .
H6AB H 0.6250 0.9615 0.7145 0.047 Uiso 1 1 calc GR . . . .
H6AC H 0.6684 0.8868 0.7319 0.047 Uiso 1 1 calc GR . . . .
Fe1 Fe 0.65939(6) 0.7500 0.94661(7) 0.0177(2) Uani 1 2 d S T P . .
O1 O 0.4712(3) 0.7500 0.5613(4) 0.0449(18) Uani 1 2 d S T P . .
H1A H 0.4584 0.7593 0.5024 0.067 Uiso 0.5 1 d GR . . . .
H1B H 0.4501 0.7850 0.5935 0.067 Uiso 0.5 1 d GR . . . .
O2 O 0.5466(3) 0.7500 0.2359(4) 0.0330(14) Uani 1 2 d S T P . .
H2A H 0.5091 0.7231 0.2646 0.049 Uiso 0.5 1 d GR . . . .
H2B H 0.5534 0.7289 0.1798 0.049 Uiso 0.5 1 d GR . . . .
N1 N 0.5810(4) 0.7500 0.7482(4) 0.0217(14) Uani 1 2 d S T P . .
C1 C 0.6113(4) 0.7500 0.8216(5) 0.0183(17) Uani 1 2 d S T P . .
C5 C 0.6596(4) 0.8522(4) 0.9475(4) 0.0426(18) Uani 1 1 d . . . . .
N5 N 0.6599(6) 0.9131(4) 0.9500(5) 0.105(3) Uani 1 1 d . . . . .
N2 N 0.7176(4) 0.7500 0.1548(4) 0.0245(15) Uani 1 2 d S T P . .
C2 C 0.7003(5) 0.7500 0.0745(6) 0.0236(18) Uani 1 2 d S T P . .
O3 O 0.8996(3) 0.7500 0.6654(3) 0.0256(13) Uani 1 2 d S T P . .
H3A H 0.9468 0.7251 0.6653 0.038 Uiso 0.5 1 d GR . . . .
H3B H 0.8686 0.7263 0.7080 0.038 Uiso 0.5 1 d GR . . . .
C4 C 0.7641(6) 0.7500 0.8848(6) 0.061(4) Uani 1 2 d S T P . .
N4 N 0.8249(5) 0.7500 0.8452(6) 0.133(7) Uani 1 2 d S T P . .
N3 N 0.9847(4) 0.7500 0.4725(4) 0.0195(14) Uani 1 2 d S T P . .
C3 C 1.0512(5) 0.7500 0.5009(5) 0.0174(16) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb3 Tb2 3.7183(6) . ?
Tb3 Tb1 3.6893(7) . ?
Tb3 O4 2.297(3) . ?
Tb3 O4 2.297(3) 8_575 ?
Tb3 O6 2.348(3) 8_575 ?
Tb3 O6 2.348(3) . ?
Tb3 N7 2.623(4) . ?
Tb3 N7 2.623(4) 8_575 ?
Tb3 O3 2.445(5) . ?
Tb3 N3 2.485(6) . ?
Tb2 Tb1 3.6939(8) . ?
Tb2 O6 2.333(3) . ?
Tb2 O6 2.333(3) 8_575 ?
Tb2 O5 2.325(3) . ?
Tb2 O5 2.325(3) 8_575 ?
Tb2 N6 2.673(4) . ?
Tb2 N6 2.673(4) 8_575 ?
Tb2 O2 2.420(5) . ?
Tb2 N2 2.507(6) . ?
Tb1 O4 2.316(3) . ?
Tb1 O4 2.316(3) 8_575 ?
Tb1 O5 2.326(3) 8_575 ?
Tb1 O5 2.326(3) . ?
Tb1 N8 2.683(5) . ?
Tb1 N8 2.683(5) 8_575 ?
Tb1 O1 2.428(5) . ?
Tb1 N1 2.465(6) . ?
O4 C0AA 1.423(6) . ?
O6 C4AA 1.425(6) . ?
O5 C8AA 1.428(6) . ?
N8 C9AA 1.499(6) . ?
N8 C13 1.479(7) . ?
N8 C6AA 1.482(7) . ?
C8AA C1AA 1.523(7) . ?
C8AA C9AA 1.533(7) . ?
C12 C0AA 1.519(7) . ?
C12 N7 1.505(6) . ?
C12 C4AA 1.524(7) . ?
C0AA C9AA 1.531(7) . ?
C1AA N6 1.499(6) . ?
C1AA C4AA 1.531(7) . ?
N7 C3AA 1.478(6) . ?
N7 C14 1.483(6) . ?
N6 C2AA 1.476(6) . ?
N6 C5AA 1.487(6) . ?
Fe1 C1 1.930(8) . ?
Fe1 C5 1.934(7) . ?
Fe1 C5 1.934(7) 8_575 ?
Fe1 C2 1.924(8) 1_556 ?
Fe1 C4 1.922(10) . ?
Fe1 C3 1.919(8) 6_557 ?
N1 C1 1.149(9) . ?
C5 N5 1.152(9) . ?
N2 C2 1.167(9) . ?
C2 Fe1 1.924(8) 1_554 ?
C4 N4 1.142(12) . ?
N3 C3 1.159(9) . ?
C3 Fe1 1.919(8) 6_657 ?

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
Tb1 Tb3 Tb2 59.821(14) . . ?
O4 Tb3 Tb2 79.58(8) . . ?
O4 Tb3 Tb2 79.58(8) 8_575 . ?
O4 Tb3 Tb1 37.08(8) 8_575 . ?
O4 Tb3 Tb1 37.08(8) . . ?
O4 Tb3 O4 66.24(16) . 8_575 ?
O4 Tb3 O6 112.24(11) . 8_575 ?
O4 Tb3 O6 77.99(11) 8_575 8_575 ?
O4 Tb3 O6 77.99(11) . . ?
O4 Tb3 O6 112.24(11) 8_575 . ?
O4 Tb3 N7 134.19(12) . 8_575 ?
O4 Tb3 N7 69.30(12) . . ?
O4 Tb3 N7 134.19(12) 8_575 . ?
O4 Tb3 N7 69.30(12) 8_575 8_575 ?
O4 Tb3 O3 83.20(13) . . ?
O4 Tb3 O3 83.20(13) 8_575 . ?
O4 Tb3 N3 141.20(10) 8_575 . ?
O4 Tb3 N3 141.20(10) . . ?
O6 Tb3 Tb2 37.26(8) 8_575 . ?
O6 Tb3 Tb2 37.26(8) . . ?
O6 Tb3 Tb1 80.91(8) . . ?
O6 Tb3 Tb1 80.91(8) 8_575 . ?
O6 Tb3 O6 64.93(16) 8_575 . ?
O6 Tb3 N7 67.48(12) . . ?
O6 Tb3 N7 130.47(12) 8_575 . ?
O6 Tb3 N7 67.48(12) 8_575 8_575 ?
O6 Tb3 N7 130.47(12) . 8_575 ?
O6 Tb3 O3 147.52(8) 8_575 . ?
O6 Tb3 O3 147.52(8) . . ?
O6 Tb3 N3 102.24(14) . . ?
O6 Tb3 N3 102.24(14) 8_575 . ?
N7 Tb3 Tb2 102.92(9) . . ?
N7 Tb3 Tb2 102.92(9) 8_575 . ?
N7 Tb3 Tb1 104.55(9) . . ?
N7 Tb3 Tb1 104.55(9) 8_575 . ?
N7 Tb3 N7 148.03(18) 8_575 . ?
O3 Tb3 Tb2 159.41(12) . . ?
O3 Tb3 Tb1 99.59(12) . . ?
O3 Tb3 N7 81.21(9) . 8_575 ?
O3 Tb3 N7 81.21(9) . . ?
O3 Tb3 N3 76.65(18) . . ?
N3 Tb3 Tb2 123.95(14) . . ?
N3 Tb3 Tb1 176.23(14) . . ?
N3 Tb3 N7 75.04(9) . 8_575 ?
N3 Tb3 N7 75.04(9) . . ?
Tb1 Tb2 Tb3 59.700(13) . . ?
O6 Tb2 Tb3 37.55(8) 8_575 . ?
O6 Tb2 Tb3 37.55(8) . . ?
O6 Tb2 Tb1 80.99(8) 8_575 . ?
O6 Tb2 Tb1 80.99(8) . . ?
O6 Tb2 O6 65.41(15) . 8_575 ?
O6 Tb2 N6 131.49(12) . 8_575 ?
O6 Tb2 N6 131.49(12) 8_575 . ?
O6 Tb2 N6 67.63(12) 8_575 8_575 ?
O6 Tb2 N6 67.63(12) . . ?
O6 Tb2 O2 146.71(8) 8_575 . ?
O6 Tb2 O2 146.71(8) . . ?
O6 Tb2 N2 96.53(14) . . ?
O6 Tb2 N2 96.53(14) 8_575 . ?
O5 Tb2 Tb3 80.04(8) . . ?
O5 Tb2 Tb3 80.04(8) 8_575 . ?
O5 Tb2 Tb1 37.44(8) . . ?
O5 Tb2 Tb1 37.44(8) 8_575 . ?
O5 Tb2 O6 78.33(11) . . ?
O5 Tb2 O6 78.33(11) 8_575 8_575 ?
O5 Tb2 O6 112.94(11) 8_575 . ?
O5 Tb2 O6 112.94(11) . 8_575 ?
O5 Tb2 O5 66.43(17) 8_575 . ?
O5 Tb2 N6 67.61(12) . . ?
O5 Tb2 N6 132.58(12) 8_575 . ?
O5 Tb2 N6 67.61(12) 8_575 8_575 ?
O5 Tb2 N6 132.58(12) . 8_575 ?
O5 Tb2 O2 89.09(14) . . ?
O5 Tb2 O2 89.09(14) 8_575 . ?
O5 Tb2 N2 143.76(10) 8_575 . ?
O5 Tb2 N2 143.76(10) . . ?
N6 Tb2 Tb3 103.01(9) 8_575 . ?
N6 Tb2 Tb3 103.01(9) . . ?
N6 Tb2 Tb1 103.21(9) . . ?
N6 Tb2 Tb1 103.21(9) 8_575 . ?
N6 Tb2 N6 149.67(18) . 8_575 ?
O2 Tb2 Tb3 166.99(13) . . ?
O2 Tb2 Tb1 107.29(13) . . ?
O2 Tb2 N6 79.08(9) . 8_575 ?
O2 Tb2 N6 79.08(9) . . ?
O2 Tb2 N2 75.67(19) . . ?
N2 Tb2 Tb3 117.34(14) . . ?
N2 Tb2 Tb1 177.04(14) . . ?
N2 Tb2 N6 77.19(9) . . ?
N2 Tb2 N6 77.19(9) . 8_575 ?
Tb3 Tb1 Tb2 60.479(9) . . ?
O4 Tb1 Tb3 36.72(8) . . ?
O4 Tb1 Tb3 36.73(8) 8_575 . ?
O4 Tb1 Tb2 79.92(8) . . ?
O4 Tb1 Tb2 79.92(8) 8_575 . ?
O4 Tb1 O4 65.63(15) . 8_575 ?
O4 Tb1 O5 77.34(11) 8_575 8_575 ?
O4 Tb1 O5 111.98(11) 8_575 . ?
O4 Tb1 O5 111.98(11) . 8_575 ?
O4 Tb1 O5 77.34(11) . . ?
O4 Tb1 N8 66.78(12) . . ?
O4 Tb1 N8 130.71(12) 8_575 . ?
O4 Tb1 N8 66.78(12) 8_575 8_575 ?
O4 Tb1 N8 130.71(12) . 8_575 ?
O4 Tb1 O1 146.97(8) . . ?
O4 Tb1 O1 146.97(8) 8_575 . ?
O4 Tb1 N1 100.59(14) . . ?
O4 Tb1 N1 100.59(14) 8_575 . ?
O5 Tb1 Tb3 80.68(8) 8_575 . ?
O5 Tb1 Tb3 80.68(8) . . ?
O5 Tb1 Tb2 37.42(8) 8_575 . ?
O5 Tb1 Tb2 37.42(8) . . ?
O5 Tb1 O5 66.39(17) 8_575 . ?
O5 Tb1 N8 68.41(12) 8_575 8_575 ?
O5 Tb1 N8 68.41(12) . . ?
O5 Tb1 N8 133.57(13) . 8_575 ?
O5 Tb1 N8 133.57(13) 8_575 . ?
O5 Tb1 O1 81.35(14) 8_575 . ?
O5 Tb1 O1 81.35(14) . . ?
O5 Tb1 N1 142.31(11) 8_575 . ?
O5 Tb1 N1 142.31(11) . . ?
N8 Tb1 Tb3 102.10(9) . . ?
N8 Tb1 Tb3 102.10(9) 8_575 . ?
N8 Tb1 Tb2 103.74(9) 8_575 . ?
N8 Tb1 Tb2 103.74(9) . . ?
N8 Tb1 N8 149.83(18) 8_575 . ?
O1 Tb1 Tb3 158.48(13) . . ?
O1 Tb1 Tb2 98.00(13) . . ?
O1 Tb1 N8 82.05(10) . . ?
O1 Tb1 N8 82.05(10) . 8_575 ?
O1 Tb1 N1 81.4(2) . . ?
N1 Tb1 Tb3 120.13(14) . . ?
N1 Tb1 Tb2 179.39(14) . . ?
N1 Tb1 N8 76.19(9) . . ?
N1 Tb1 N8 76.19(9) . 8_575 ?
Tb3 O4 Tb1 106.20(13) . . ?
C0AA O4 Tb3 119.2(3) . . ?
C0AA O4 Tb1 121.5(3) . . ?
Tb2 O6 Tb3 105.19(12) . . ?
C4AA O6 Tb3 118.8(3) . . ?
C4AA O6 Tb2 119.6(3) . . ?
Tb2 O5 Tb1 105.14(14) . . ?
C8AA O5 Tb2 120.0(3) . . ?
C8AA O5 Tb1 119.6(3) . . ?
C9AA N8 Tb1 96.2(3) . . ?
C13 N8 Tb1 116.8(4) . . ?
C13 N8 C9AA 110.3(4) . . ?
C13 N8 C6AA 107.1(4) . . ?
C6AA N8 Tb1 115.5(3) . . ?
C6AA N8 C9AA 110.6(4) . . ?
O5 C8AA C1AA 111.4(4) . . ?
O5 C8AA C9AA 112.0(4) . . ?
C1AA C8AA C9AA 110.3(4) . . ?
C0AA C12 C4AA 113.3(4) . . ?
N7 C12 C0AA 109.1(4) . . ?
N7 C12 C4AA 108.0(4) . . ?
O4 C0AA C12 112.0(4) . . ?
O4 C0AA C9AA 110.3(4) . . ?
C12 C0AA C9AA 110.5(4) . . ?
C8AA C1AA C4AA 113.2(4) . . ?
N6 C1AA C8AA 109.3(4) . . ?
N6 C1AA C4AA 108.7(4) . . ?
C12 N7 Tb3 96.9(3) . . ?
C3AA N7 Tb3 116.8(3) . . ?
C3AA N7 C12 110.7(4) . . ?
C3AA N7 C14 106.6(4) . . ?
C14 N7 Tb3 115.9(3) . . ?
C14 N7 C12 109.6(4) . . ?
C1AA N6 Tb2 96.2(3) . . ?
C2AA N6 Tb2 115.8(3) . . ?
C2AA N6 C1AA 110.7(4) . . ?
C2AA N6 C5AA 107.0(4) . . ?
C5AA N6 Tb2 116.9(3) . . ?
C5AA N6 C1AA 109.8(4) . . ?
N8 C9AA C8AA 110.0(4) . . ?
N8 C9AA C0AA 108.2(4) . . ?
C0AA C9AA C8AA 112.5(4) . . ?
O6 C4AA C12 111.4(4) . . ?
O6 C4AA C1AA 111.7(4) . . ?
C12 C4AA C1AA 110.3(4) . . ?
C1 Fe1 C5 90.37(17) . . ?
C1 Fe1 C5 90.38(17) . 8_575 ?
C5 Fe1 C5 179.2(3) . 8_575 ?
C2 Fe1 C1 176.3(3) 1_556 . ?
C2 Fe1 C5 89.62(17) 1_556 8_575 ?
C2 Fe1 C5 89.62(17) 1_556 . ?
C4 Fe1 C1 87.1(3) . . ?
C4 Fe1 C5 90.1(2) . 8_575 ?
C4 Fe1 C5 90.1(2) . . ?
C4 Fe1 C2 96.6(3) . 1_556 ?
C3 Fe1 C1 88.6(3) 6_557 . ?
C3 Fe1 C5 89.9(2) 6_557 . ?
C3 Fe1 C5 89.9(2) 6_557 8_575 ?
C3 Fe1 C2 87.7(3) 6_557 1_556 ?
C3 Fe1 C4 175.7(3) 6_557 . ?
C1 N1 Tb1 139.9(6) . . ?
N1 C1 Fe1 178.5(6) . . ?
N5 C5 Fe1 178.6(6) . . ?
C2 N2 Tb2 149.1(6) . . ?
N2 C2 Fe1 173.7(7) . 1_554 ?
N4 C4 Fe1 177.6(8) . . ?
C3 N3 Tb3 147.9(5) . . ?
N3 C3 Fe1 177.6(6) . 6_657 ?

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
O3 H3B N4 0.90 2.11 2.814(10) 133.9 .

_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 0.134 0.250 0.950 133.7 31.1 3H2O
2 -0.134 0.750 0.050 133.7 30.5 3H2O
3 0.366 0.750 0.450 133.7 31.0 3H2O
4 0.634 0.250 0.550 133.7 30.7 3H2O

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT213_tbfe2               
;
PROBLEM: Atom N4 has ADP max/min Ratio ..... 6.1 prolat 
RESPONSE: Disorder caused by vibration of -CN due to hydrogen bonding to water
molecules coordinated to the trinuclear complex. Attempts to model the -CN
group as split atoms were unfruitful. All of the compounds in this
family share the same characteristics.
;
_vrf_PLAT220_tbfe2               
;
PROBLEM: Non-Solvent Resd 1 N Ueq(max)/Ueq(min) Range 8.3 Ratio
RESPONSE: Originated by vibration of the "free" (non covalently bonded
to the lanthanide ions) -CN group
;
_vrf_THETM01_tbfe2               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The low value of sine(theta_max)/wavelength results from the exclusion
of low quality reflections in the refinement process.
;
