# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_sl243
_database_code_depnum_ccdc_archive 'CCDC 1495740'
_audit_update_record             
;
2016-07-23 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            
'[CrIII2TbIII2(OMe)2-x(OH)x(2-Cl-4,5-F-benz)4(mdea)2(NO3)2]?xMeOH'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H38.40 Cl4 Cr2 F8 N4 O21.20 Tb2'
_chemical_formula_weight         1629.98

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'
Tb Tb -0.1723 4.1537 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6481(6)
_cell_length_b                   11.3861(7)
_cell_length_c                   13.3598(8)
_cell_angle_alpha                67.617(5)
_cell_angle_beta                 78.339(5)
_cell_angle_gamma                87.410(5)
_cell_volume                     1328.23(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9851
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      27.43

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             793
_exptl_absorpt_coefficient_mu    3.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18565
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6101
_reflns_number_gt                5374
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The structure was solved by direct methods. The asymmetric unit contains half the cluster, with a disordered methoxide/hydroxide group and a disordered solvent MeOH molecule.
It is found that the methoxide group is present 40 % of the time and the hydroxide and the solvent MeOH ligands are present 60 % of the time.
All non-H atoms are refined anisotropically. The H-atoms are placed in calculated positions except for the H atom found on the disordered OH ligands, which were omitted. These atoms were later added to the formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0239P)²+0.2590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6101
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.614621(16) 0.607271(14) 0.549211(12) 0.01449(6) Uani 1 1 d . . .
Cr2 Cr 0.56964(5) 0.29524(5) 0.64789(4) 0.01367(11) Uani 1 1 d . . .
Cl1 Cl 0.11518(9) 0.00579(8) 0.61122(7) 0.02604(19) Uani 1 1 d . . .
Cl2 Cl 0.35197(10) 0.23762(10) 1.01338(8) 0.0346(2) Uani 1 1 d . . .
F1 F -0.0313(2) -0.2675(2) 1.0131(2) 0.0467(7) Uani 1 1 d . . .
F2 F 0.1295(3) -0.1323(3) 1.07562(19) 0.0587(8) Uani 1 1 d . A .
F3 F 0.6753(2) 0.3119(2) 1.23745(17) 0.0358(5) Uani 1 1 d . . .
F4 F 0.8473(2) 0.4727(2) 1.0571(2) 0.0437(6) Uani 1 1 d . A .
O1 O 0.4397(2) 0.43568(19) 0.60521(18) 0.0154(5) Uani 1 1 d . . .
O1S O 0.2197(4) 0.4040(5) 0.7707(4) 0.0330(14) Uani 0.599(6) 1 d P A 2
H1S H 0.2157 0.3906 0.8375 0.040 Uiso 0.599(6) 1 calc PR A 2
O2 O 0.2592(2) 0.2307(2) 0.61395(18) 0.0190(5) Uani 1 1 d . . .
O3 O 0.4145(2) 0.1649(2) 0.72792(18) 0.0188(5) Uani 1 1 d . . .
O4 O 0.5656(2) 0.2700(2) 0.51196(18) 0.0173(5) Uani 1 1 d . . .
O5 O 0.7257(2) 0.42175(19) 0.57702(18) 0.0148(5) Uani 1 1 d . . .
O6 O 0.5719(2) 0.3045(2) 0.79358(18) 0.0171(5) Uani 1 1 d . . .
O7 O 0.5762(2) 0.5164(2) 0.74651(18) 0.0181(5) Uani 1 1 d . . .
O8 O 0.8286(2) 0.6549(2) 0.6024(2) 0.0229(5) Uani 1 1 d . . .
O9 O 0.6521(2) 0.7784(2) 0.61202(19) 0.0214(5) Uani 1 1 d . . .
O10 O 0.8361(3) 0.7958(3) 0.6760(3) 0.0450(8) Uani 1 1 d . . .
N1 N 0.7301(3) 0.1658(2) 0.6629(2) 0.0182(6) Uani 1 1 d . . .
N2 N 0.7737(3) 0.7445(3) 0.6321(2) 0.0251(7) Uani 1 1 d . A .
C1 C 0.3125(9) 0.4453(7) 0.6832(7) 0.018(2) Uani 0.401(6) 1 d P A 1
H1A H 0.2283 0.4221 0.6633 0.028 Uiso 0.401(6) 1 calc PR A 1
H1B H 0.3056 0.5328 0.6800 0.028 Uiso 0.401(6) 1 calc PR A 1
H1C H 0.3187 0.3875 0.7583 0.028 Uiso 0.401(6) 1 calc PR A 1
C1S C 0.0986(8) 0.4703(8) 0.7364(6) 0.050(2) Uani 0.599(6) 1 d P A 2
H1S1 H 0.0138 0.4148 0.7744 0.075 Uiso 0.599(6) 1 calc PR A 2
H1S2 H 0.1090 0.4955 0.6564 0.075 Uiso 0.599(6) 1 calc PR A 2
H1S3 H 0.0894 0.5462 0.7547 0.075 Uiso 0.599(6) 1 calc PR A 2
C2 C 0.2993(4) 0.1559(3) 0.6988(3) 0.0192(7) Uani 1 1 d . A .
C3 C 0.2063(4) 0.0429(3) 0.7780(3) 0.0202(7) Uani 1 1 d . . .
C4 C 0.1211(3) -0.0283(3) 0.7479(3) 0.0196(7) Uani 1 1 d . A .
C5 C 0.0412(4) -0.1344(3) 0.8266(3) 0.0244(8) Uani 1 1 d . . .
H5 H -0.0148 -0.1835 0.8048 0.029 Uiso 1 1 calc R A .
C6 C 0.0451(4) -0.1661(3) 0.9348(3) 0.0301(9) Uani 1 1 d . A .
C7 C 0.1294(4) -0.0971(4) 0.9668(3) 0.0362(10) Uani 1 1 d . . .
C8 C 0.2100(4) 0.0049(4) 0.8900(3) 0.0305(9) Uani 1 1 d . A .
H8 H 0.2691 0.0504 0.9127 0.037 Uiso 1 1 calc R . .
C9 C 0.6175(4) 0.1486(3) 0.5192(3) 0.0232(8) Uani 1 1 d . A .
H9A H 0.6357 0.1433 0.4454 0.028 Uiso 1 1 calc R . .
H9B H 0.5467 0.0810 0.5697 0.028 Uiso 1 1 calc R . .
C10 C 0.7539(4) 0.1313(4) 0.5627(3) 0.0283(8) Uani 1 1 d . A .
H10A H 0.7825 0.0420 0.5826 0.034 Uiso 1 1 calc R . .
H10B H 0.8307 0.1866 0.5050 0.034 Uiso 1 1 calc R . .
C11 C 0.8556(4) 0.2388(3) 0.6635(3) 0.0241(8) Uani 1 1 d . A .
H11A H 0.8468 0.2440 0.7368 0.029 Uiso 1 1 calc R . .
H11B H 0.9436 0.1946 0.6491 0.029 Uiso 1 1 calc R . .
C12 C 0.8624(4) 0.3700(3) 0.5760(3) 0.0276(8) Uani 1 1 d . A .
H12A H 0.9269 0.4254 0.5892 0.033 Uiso 1 1 calc R . .
H12B H 0.9009 0.3667 0.5027 0.033 Uiso 1 1 calc R . .
C13 C 0.7007(4) 0.0503(3) 0.7650(3) 0.0249(8) Uani 1 1 d . A .
H13A H 0.6196 0.0023 0.7639 0.037 Uiso 1 1 calc R . .
H13B H 0.6791 0.0746 0.8293 0.037 Uiso 1 1 calc R . .
H13C H 0.7840 -0.0026 0.7695 0.037 Uiso 1 1 calc R . .
C14 C 0.5789(3) 0.4041(3) 0.8132(3) 0.0179(7) Uani 1 1 d . A .
C15 C 0.5956(4) 0.3829(3) 0.9290(3) 0.0184(7) Uani 1 1 d . . .
C16 C 0.5056(4) 0.3025(3) 1.0238(3) 0.0203(7) Uani 1 1 d . A .
C17 C 0.5296(4) 0.2787(3) 1.1285(3) 0.0241(8) Uani 1 1 d . . .
H17 H 0.4666 0.2245 1.1924 0.029 Uiso 1 1 calc R A .
C18 C 0.6467(4) 0.3353(3) 1.1373(3) 0.0260(8) Uani 1 1 d . A .
C19 C 0.7346(4) 0.4172(3) 1.0447(3) 0.0262(8) Uani 1 1 d . . .
C20 C 0.7103(4) 0.4429(3) 0.9408(3) 0.0229(8) Uani 1 1 d . A .
H20 H 0.7710 0.5010 0.8776 0.028 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O5 2.260(2) . ?
Tb1 O4 2.265(2) 2_666 ?
Tb1 O2 2.388(2) 2_666 ?
Tb1 O7 2.391(2) . ?
Tb1 O1 2.429(2) . ?
Tb1 O1 2.449(2) 2_666 ?
Tb1 O8 2.460(2) . ?
Tb1 O9 2.463(2) . ?
Tb1 N2 2.871(3) . ?
Tb1 Cr2 3.2885(5) 2_666 ?
Cr2 O4 1.952(2) . ?
Cr2 O5 1.954(2) . ?
Cr2 O1 1.967(2) . ?
Cr2 O3 1.983(2) . ?
Cr2 O6 1.993(2) . ?
Cr2 N1 2.074(3) . ?
Cr2 Tb1 3.2886(5) 2_666 ?
Cl1 C4 1.729(3) . ?
Cl2 C16 1.738(3) . ?
F1 C6 1.347(4) . ?
F2 C7 1.353(4) . ?
F3 C18 1.344(4) . ?
F4 C19 1.351(4) . ?
O1 C1 1.470(9) . ?
O1 Tb1 2.449(2) 2_666 ?
O1S C1S 1.420(8) . ?
O2 C2 1.253(4) . ?
O2 Tb1 2.388(2) 2_666 ?
O3 C2 1.270(4) . ?
O4 C9 1.423(4) . ?
O4 Tb1 2.265(2) 2_666 ?
O5 C12 1.420(4) . ?
O6 C14 1.265(4) . ?
O7 C14 1.252(4) . ?
O8 N2 1.285(4) . ?
O9 N2 1.267(4) . ?
O10 N2 1.219(3) . ?
N1 C13 1.477(4) . ?
N1 C11 1.503(4) . ?
N1 C10 1.506(4) . ?
C2 C3 1.505(5) . ?
C3 C4 1.392(4) . ?
C3 C8 1.398(5) . ?
C4 C5 1.396(5) . ?
C5 C6 1.359(5) . ?
C6 C7 1.384(5) . ?
C7 C8 1.363(5) . ?
C9 C10 1.519(5) . ?
C11 C12 1.500(5) . ?
C14 C15 1.514(4) . ?
C15 C20 1.391(4) . ?
C15 C16 1.393(5) . ?
C16 C17 1.385(5) . ?
C17 C18 1.373(5) . ?
C18 C19 1.374(5) . ?
C19 C20 1.373(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
O5 Tb1 O4 147.95(7) . 2_666 ?
O5 Tb1 O2 109.43(8) . 2_666 ?
O4 Tb1 O2 79.28(8) 2_666 2_666 ?
O5 Tb1 O7 79.01(8) . . ?
O4 Tb1 O7 112.11(8) 2_666 . ?
O2 Tb1 O7 144.88(7) 2_666 . ?
O5 Tb1 O1 70.64(7) . . ?
O4 Tb1 O1 83.09(7) 2_666 . ?
O2 Tb1 O1 140.28(7) 2_666 . ?
O7 Tb1 O1 74.83(7) . . ?
O5 Tb1 O1 81.31(7) . 2_666 ?
O4 Tb1 O1 71.24(7) 2_666 2_666 ?
O2 Tb1 O1 74.46(7) 2_666 2_666 ?
O7 Tb1 O1 140.32(7) . 2_666 ?
O1 Tb1 O1 66.21(9) . 2_666 ?
O5 Tb1 O8 79.92(7) . . ?
O4 Tb1 O8 131.70(7) 2_666 . ?
O2 Tb1 O8 75.41(7) 2_666 . ?
O7 Tb1 O8 72.66(8) . . ?
O1 Tb1 O8 139.48(7) . . ?
O1 Tb1 O8 136.45(8) 2_666 . ?
O5 Tb1 O9 129.61(7) . . ?
O4 Tb1 O9 82.11(7) 2_666 . ?
O2 Tb1 O9 76.61(8) 2_666 . ?
O7 Tb1 O9 72.55(7) . . ?
O1 Tb1 O9 135.56(8) . . ?
O1 Tb1 O9 143.60(7) 2_666 . ?
O8 Tb1 O9 52.43(8) . . ?
O5 Tb1 N2 104.55(8) . . ?
O4 Tb1 N2 107.50(8) 2_666 . ?
O2 Tb1 N2 76.27(8) 2_666 . ?
O7 Tb1 N2 68.63(8) . . ?
O1 Tb1 N2 143.33(8) . . ?
O1 Tb1 N2 150.40(8) 2_666 . ?
O8 Tb1 N2 26.48(8) . . ?
O9 Tb1 N2 26.07(8) . . ?
O5 Tb1 Cr2 117.51(5) . 2_666 ?
O4 Tb1 Cr2 35.45(5) 2_666 2_666 ?
O2 Tb1 Cr2 68.32(5) 2_666 2_666 ?
O7 Tb1 Cr2 139.33(5) . 2_666 ?
O1 Tb1 Cr2 76.69(5) . 2_666 ?
O1 Tb1 Cr2 36.52(5) 2_666 2_666 ?
O8 Tb1 Cr2 143.21(6) . 2_666 ?
O9 Tb1 Cr2 111.14(5) . 2_666 ?
N2 Tb1 Cr2 131.63(6) . 2_666 ?
O4 Cr2 O5 93.20(9) . . ?
O4 Cr2 O1 89.12(9) . . ?
O5 Cr2 O1 87.63(9) . . ?
O4 Cr2 O3 89.76(9) . . ?
O5 Cr2 O3 176.75(9) . . ?
O1 Cr2 O3 93.76(9) . . ?
O4 Cr2 O6 174.95(9) . . ?
O5 Cr2 O6 90.47(9) . . ?
O1 Cr2 O6 94.50(9) . . ?
O3 Cr2 O6 86.50(9) . . ?
O4 Cr2 N1 84.17(10) . . ?
O5 Cr2 N1 83.99(10) . . ?
O1 Cr2 N1 168.94(11) . . ?
O3 Cr2 N1 94.99(10) . . ?
O6 Cr2 N1 92.77(10) . . ?
O4 Cr2 Tb1 42.31(6) . 2_666 ?
O5 Cr2 Tb1 98.32(6) . 2_666 ?
O1 Cr2 Tb1 47.82(6) . 2_666 ?
O3 Cr2 Tb1 84.77(6) . 2_666 ?
O6 Cr2 Tb1 140.38(7) . 2_666 ?
N1 Cr2 Tb1 126.44(8) . 2_666 ?
C1 O1 Cr2 121.6(3) . . ?
C1 O1 Tb1 114.0(3) . . ?
Cr2 O1 Tb1 96.73(8) . . ?
C1 O1 Tb1 113.1(3) . 2_666 ?
Cr2 O1 Tb1 95.65(9) . 2_666 ?
Tb1 O1 Tb1 113.79(9) . 2_666 ?
C2 O2 Tb1 131.3(2) . 2_666 ?
C2 O3 Cr2 127.6(2) . . ?
C9 O4 Cr2 110.22(18) . . ?
C9 O4 Tb1 137.48(18) . 2_666 ?
Cr2 O4 Tb1 102.23(9) . 2_666 ?
C12 O5 Cr2 114.36(19) . . ?
C12 O5 Tb1 141.82(19) . . ?
Cr2 O5 Tb1 102.84(9) . . ?
C14 O6 Cr2 126.8(2) . . ?
C14 O7 Tb1 131.8(2) . . ?
N2 O8 Tb1 94.89(18) . . ?
N2 O9 Tb1 95.25(18) . . ?
C13 N1 C11 109.6(2) . . ?
C13 N1 C10 110.5(3) . . ?
C11 N1 C10 111.3(3) . . ?
C13 N1 Cr2 114.1(2) . . ?
C11 N1 Cr2 103.73(19) . . ?
C10 N1 Cr2 107.45(19) . . ?
O10 N2 O9 121.4(3) . . ?
O10 N2 O8 121.7(3) . . ?
O9 N2 O8 116.9(3) . . ?
O10 N2 Tb1 174.6(3) . . ?
O9 N2 Tb1 58.68(15) . . ?
O8 N2 Tb1 58.63(15) . . ?
O2 C2 O3 126.5(3) . . ?
O2 C2 C3 119.9(3) . . ?
O3 C2 C3 113.7(3) . . ?
C4 C3 C8 118.0(3) . . ?
C4 C3 C2 125.0(3) . . ?
C8 C3 C2 116.9(3) . . ?
C3 C4 C5 121.4(3) . . ?
C3 C4 Cl1 121.8(3) . . ?
C5 C4 Cl1 116.8(3) . . ?
C6 C5 C4 118.7(3) . . ?
F1 C6 C5 120.3(3) . . ?
F1 C6 C7 118.7(3) . . ?
C5 C6 C7 121.0(3) . . ?
F2 C7 C8 120.7(3) . . ?
F2 C7 C6 118.8(3) . . ?
C8 C7 C6 120.5(4) . . ?
C7 C8 C3 120.4(3) . . ?
O4 C9 C10 108.1(3) . . ?
N1 C10 C9 108.8(3) . . ?
C12 C11 N1 109.3(3) . . ?
O5 C12 C11 110.5(3) . . ?
O7 C14 O6 126.7(3) . . ?
O7 C14 C15 117.8(3) . . ?
O6 C14 C15 115.5(3) . . ?
C20 C15 C16 118.7(3) . . ?
C20 C15 C14 118.0(3) . . ?
C16 C15 C14 123.2(3) . . ?
C17 C16 C15 121.7(3) . . ?
C17 C16 Cl2 118.0(3) . . ?
C15 C16 Cl2 120.1(2) . . ?
C18 C17 C16 118.3(3) . . ?
F3 C18 C17 119.9(3) . . ?
F3 C18 C19 119.5(3) . . ?
C17 C18 C19 120.6(3) . . ?
F4 C19 C20 119.8(3) . . ?
F4 C19 C18 118.8(3) . . ?
C20 C19 C18 121.4(3) . . ?
C19 C20 C15 119.2(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.142
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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_p-1
_database_code_depnum_ccdc_archive 'CCDC 1495741'
_audit_update_record             
;
2016-07-23 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H37.20 Cl4 Cr2 Dy2 F8 N4 O20.60'
_chemical_formula_weight         1626.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5430(19)
_cell_length_b                   11.414(2)
_cell_length_c                   13.306(3)
_cell_angle_alpha                67.56(3)
_cell_angle_beta                 77.95(3)
_cell_angle_gamma                87.25(3)
_cell_volume                     1309.2(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16519
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Plate
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             789
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_T_max  0.592
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71079
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16519
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4234
_reflns_number_gt                4040
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The collection was performed at the Australian synchrotron. We
were restricted to one 360 degree phi scan.
The structure was solved by direct methods. The asymmetric unit contains half the cluster, with a disordered methoxide/hydroxide group and a disordered solvent MeOH molecule.
It is found that the methoxide group is present 70 % of the time and the hydroxide and the solvent MeOH ligands are present 30 % of the time.
All non-H atoms are refined anisotropically. The H-atoms are placed in calculated positions except for the H atom found on the disordered OH ligands, which were omitted. These atoms were later added to the formula.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0545P)²+2.5434P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4234
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.615106(19) 0.607356(16) 0.549353(15) 0.01778(9) Uani 1 1 d . . .
Cr1 Cr 0.56853(7) 0.29776(6) 0.64809(6) 0.01776(16) Uani 1 1 d . . .
Cl1 Cl 0.11439(12) 0.00399(11) 0.61237(10) 0.0299(2) Uani 1 1 d . . .
Cl2 Cl 0.35232(14) 0.23487(14) 1.01474(11) 0.0402(3) Uani 1 1 d . . .
F1 F -0.0329(4) -0.2685(3) 1.0165(3) 0.0495(8) Uani 1 1 d . . .
F2 F 0.1277(4) -0.1326(4) 1.0778(3) 0.0597(10) Uani 1 1 d . A .
F3 F 0.6776(3) 0.3089(3) 1.2389(2) 0.0386(7) Uani 1 1 d . . .
F4 F 0.8476(4) 0.4742(4) 1.0588(3) 0.0509(9) Uani 1 1 d . A .
O1 O 0.4361(3) 0.4374(3) 0.6056(2) 0.0208(6) Uani 1 1 d . . .
O1S O 0.2152(13) 0.4036(13) 0.7727(10) 0.041(4) Uani 0.299(10) 1 d P A 2
H9 H 0.2774 0.4018 0.7179 0.049 Uiso 0.30 1 d P A 2
O2 O 0.2576(3) 0.2291(3) 0.6138(3) 0.0242(6) Uani 1 1 d . . .
O3 O 0.4139(3) 0.1667(3) 0.7285(3) 0.0219(6) Uani 1 1 d . . .
O4 O 0.5661(3) 0.2727(3) 0.5112(2) 0.0212(6) Uani 1 1 d . . .
O5 O 0.7267(3) 0.4238(3) 0.5767(2) 0.0204(6) Uani 1 1 d . . .
O6 O 0.5711(3) 0.3061(3) 0.7943(2) 0.0211(6) Uani 1 1 d . . .
O7 O 0.5760(3) 0.5175(3) 0.7472(3) 0.0233(6) Uani 1 1 d . . .
O8 O 0.8291(3) 0.6573(3) 0.6009(3) 0.0270(7) Uani 1 1 d . . .
O9 O 0.6477(3) 0.7783(3) 0.6107(3) 0.0249(7) Uani 1 1 d . . .
O10 O 0.8333(5) 0.7965(4) 0.6762(4) 0.0519(11) Uani 1 1 d . . .
N1 N 0.7319(4) 0.1684(3) 0.6624(3) 0.0224(8) Uani 1 1 d . . .
N2 N 0.7728(4) 0.7468(4) 0.6292(3) 0.0289(9) Uani 1 1 d . A .
C1 C 0.3065(6) 0.4473(6) 0.6831(5) 0.0228(16) Uani 0.701(10) 1 d P A 1
H2A H 0.2220 0.4238 0.6629 0.034 Uiso 0.701(10) 1 calc PR A 1
H2B H 0.2990 0.5348 0.6794 0.034 Uiso 0.701(10) 1 calc PR A 1
H2C H 0.3118 0.3901 0.7588 0.034 Uiso 0.701(10) 1 calc PR A 1
C1S C 0.096(2) 0.474(3) 0.7339(17) 0.055(6) Uani 0.299(10) 1 d P A 2
H22A H 0.0063 0.4296 0.7813 0.082 Uiso 0.299(10) 1 calc PR A 2
H22B H 0.0997 0.4832 0.6572 0.082 Uiso 0.299(10) 1 calc PR A 2
H22C H 0.1002 0.5586 0.7368 0.082 Uiso 0.299(10) 1 calc PR A 2
C2 C 0.2983(5) 0.1557(4) 0.6984(4) 0.0220(9) Uani 1 1 d . A .
C3 C 0.2058(5) 0.0417(4) 0.7789(4) 0.0245(9) Uani 1 1 d . . .
C4 C 0.1202(5) -0.0308(4) 0.7503(4) 0.0245(9) Uani 1 1 d . A .
C5 C 0.0400(5) -0.1353(4) 0.8276(4) 0.0298(10) Uani 1 1 d . . .
H21 H -0.0169 -0.1838 0.8058 0.036 Uiso 1 1 calc R A .
C6 C 0.0445(5) -0.1677(5) 0.9375(5) 0.0348(11) Uani 1 1 d . A .
C7 C 0.1277(6) -0.0979(5) 0.9690(5) 0.0385(12) Uani 1 1 d . . .
C8 C 0.2098(5) 0.0056(5) 0.8911(4) 0.0328(11) Uani 1 1 d . A .
H4 H 0.2687 0.0520 0.9134 0.039 Uiso 1 1 calc R . .
C9 C 0.6187(5) 0.1516(5) 0.5188(4) 0.0272(10) Uani 1 1 d . A .
H8A H 0.6375 0.1460 0.4447 0.033 Uiso 1 1 calc R . .
H8B H 0.5470 0.0841 0.5700 0.033 Uiso 1 1 calc R . .
C10 C 0.7551(5) 0.1351(5) 0.5616(4) 0.0304(10) Uani 1 1 d . A .
H20A H 0.7846 0.0462 0.5810 0.037 Uiso 1 1 calc R . .
H20B H 0.8325 0.1907 0.5033 0.037 Uiso 1 1 calc R . .
C11 C 0.8584(5) 0.2419(4) 0.6627(4) 0.0284(10) Uani 1 1 d . A .
H17A H 0.8489 0.2469 0.7364 0.034 Uiso 1 1 calc R . .
H17B H 0.9478 0.1982 0.6479 0.034 Uiso 1 1 calc R . .
C12 C 0.8651(5) 0.3732(5) 0.5748(4) 0.0304(10) Uani 1 1 d . A .
H9A H 0.9299 0.4286 0.5879 0.036 Uiso 1 1 calc R . .
H9B H 0.9043 0.3702 0.5008 0.036 Uiso 1 1 calc R . .
C13 C 0.7008(5) 0.0532(4) 0.7637(4) 0.0271(9) Uani 1 1 d . A .
H12A H 0.7872 0.0032 0.7712 0.041 Uiso 1 1 calc R . .
H12B H 0.6238 0.0028 0.7592 0.041 Uiso 1 1 calc R . .
H12C H 0.6708 0.0766 0.8284 0.041 Uiso 1 1 calc R . .
C14 C 0.5774(5) 0.4062(4) 0.8144(4) 0.0227(9) Uani 1 1 d . A .
C15 C 0.5959(5) 0.3830(4) 0.9299(4) 0.0228(9) Uani 1 1 d . . .
C16 C 0.5069(5) 0.3013(4) 1.0248(4) 0.0250(9) Uani 1 1 d . A .
C17 C 0.5309(5) 0.2756(4) 1.1300(4) 0.0296(10) Uani 1 1 d . . .
H19 H 0.4684 0.2197 1.1943 0.036 Uiso 1 1 calc R A .
C18 C 0.6484(5) 0.3339(5) 1.1381(4) 0.0300(10) Uani 1 1 d . A .
C19 C 0.7355(5) 0.4184(5) 1.0460(4) 0.0327(11) Uani 1 1 d . . .
C20 C 0.7101(5) 0.4451(5) 0.9414(4) 0.0293(10) Uani 1 1 d . A .
H16 H 0.7699 0.5050 0.8779 0.035 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O5 2.241(3) . ?
Dy1 O4 2.242(3) 2_666 ?
Dy1 O7 2.384(3) . ?
Dy1 O2 2.387(3) 2_666 ?
Dy1 O1 2.432(3) . ?
Dy1 O9 2.439(3) . ?
Dy1 O8 2.442(3) . ?
Dy1 O1 2.449(3) 2_666 ?
Dy1 N2 2.849(4) . ?
Dy1 Cr1 3.2732(12) 2_666 ?
Dy1 Cr1 3.2823(12) . ?
Cr1 O4 1.953(3) . ?
Cr1 O5 1.954(3) . ?
Cr1 O1 1.968(3) . ?
Cr1 O3 1.972(3) . ?
Cr1 O6 1.989(3) . ?
Cr1 N1 2.082(4) . ?
Cr1 Dy1 3.2731(12) 2_666 ?
Cl1 C4 1.736(5) . ?
Cl2 C16 1.742(4) . ?
F1 C6 1.345(6) . ?
F2 C7 1.347(6) . ?
F3 C18 1.347(5) . ?
F4 C19 1.343(6) . ?
O1 C1 1.466(7) . ?
O1 Dy1 2.449(3) 2_666 ?
O1S C1S 1.43(2) . ?
O2 C2 1.245(5) . ?
O2 Dy1 2.387(3) 2_666 ?
O3 C2 1.276(5) . ?
O4 C9 1.422(5) . ?
O4 Dy1 2.242(3) 2_666 ?
O5 C12 1.416(5) . ?
O6 C14 1.276(5) . ?
O7 C14 1.245(6) . ?
O8 N2 1.277(5) . ?
O9 N2 1.277(5) . ?
O10 N2 1.225(5) . ?
N1 C13 1.466(6) . ?
N1 C10 1.500(5) . ?
N1 C11 1.504(5) . ?
C2 C3 1.507(6) . ?
C3 C4 1.390(6) . ?
C3 C8 1.397(7) . ?
C4 C5 1.374(7) . ?
C5 C6 1.374(7) . ?
C6 C7 1.376(7) . ?
C7 C8 1.379(7) . ?
C9 C10 1.503(6) . ?
C11 C12 1.502(7) . ?
C14 C15 1.504(6) . ?
C15 C16 1.383(7) . ?
C15 C20 1.393(6) . ?
C16 C17 1.383(6) . ?
C17 C18 1.375(7) . ?
C18 C19 1.368(8) . ?
C19 C20 1.378(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Dy1 O4 147.46(10) . 2_666 ?
O5 Dy1 O7 79.17(11) . . ?
O4 Dy1 O7 112.16(11) 2_666 . ?
O5 Dy1 O2 110.00(11) . 2_666 ?
O4 Dy1 O2 79.22(11) 2_666 2_666 ?
O7 Dy1 O2 144.15(10) . 2_666 ?
O5 Dy1 O1 71.18(10) . . ?
O4 Dy1 O1 82.11(10) 2_666 . ?
O7 Dy1 O1 75.27(10) . . ?
O2 Dy1 O1 140.53(10) 2_666 . ?
O5 Dy1 O9 130.75(10) . . ?
O4 Dy1 O9 81.44(10) 2_666 . ?
O7 Dy1 O9 72.70(10) . . ?
O2 Dy1 O9 75.88(10) 2_666 . ?
O1 Dy1 O9 134.84(10) . . ?
O5 Dy1 O8 80.61(10) . . ?
O4 Dy1 O8 131.47(10) 2_666 . ?
O7 Dy1 O8 72.81(11) . . ?
O2 Dy1 O8 74.70(11) 2_666 . ?
O1 Dy1 O8 140.60(10) . . ?
O9 Dy1 O8 52.97(10) . . ?
O5 Dy1 O1 80.50(10) . 2_666 ?
O4 Dy1 O1 71.71(10) 2_666 2_666 ?
O7 Dy1 O1 140.42(10) . 2_666 ?
O2 Dy1 O1 75.06(10) 2_666 2_666 ?
O1 Dy1 O1 66.12(12) . 2_666 ?
O9 Dy1 O1 143.42(10) . 2_666 ?
O8 Dy1 O1 135.94(10) . 2_666 ?
O5 Dy1 N2 105.38(11) . . ?
O4 Dy1 N2 107.15(11) 2_666 . ?
O7 Dy1 N2 69.06(11) . . ?
O2 Dy1 N2 75.11(11) 2_666 . ?
O1 Dy1 N2 144.06(11) . . ?
O9 Dy1 N2 26.52(11) . . ?
O8 Dy1 N2 26.54(11) . . ?
O1 Dy1 N2 149.78(11) 2_666 . ?
O5 Dy1 Cr1 116.96(8) . 2_666 ?
O4 Dy1 Cr1 35.66(7) 2_666 2_666 ?
O7 Dy1 Cr1 139.65(8) . 2_666 ?
O2 Dy1 Cr1 68.52(8) 2_666 2_666 ?
O1 Dy1 Cr1 76.04(8) . 2_666 ?
O9 Dy1 Cr1 110.63(8) . 2_666 ?
O8 Dy1 Cr1 142.78(8) . 2_666 ?
O1 Dy1 Cr1 36.81(7) 2_666 2_666 ?
N2 Dy1 Cr1 131.11(8) . 2_666 ?
O5 Dy1 Cr1 35.48(8) . . ?
O4 Dy1 Cr1 118.32(8) 2_666 . ?
O7 Dy1 Cr1 68.08(7) . . ?
O2 Dy1 Cr1 138.15(8) 2_666 . ?
O1 Dy1 Cr1 36.62(7) . . ?
O9 Dy1 Cr1 140.39(8) . . ?
O8 Dy1 Cr1 108.34(8) . . ?
O1 Dy1 Cr1 75.66(7) 2_666 . ?
N2 Dy1 Cr1 126.09(9) . . ?
Cr1 Dy1 Cr1 102.77(3) 2_666 . ?
O4 Cr1 O5 93.09(13) . . ?
O4 Cr1 O1 89.16(12) . . ?
O5 Cr1 O1 87.98(12) . . ?
O4 Cr1 O3 89.76(13) . . ?
O5 Cr1 O3 176.47(13) . . ?
O1 Cr1 O3 94.15(13) . . ?
O4 Cr1 O6 174.74(12) . . ?
O5 Cr1 O6 90.35(12) . . ?
O1 Cr1 O6 94.94(12) . . ?
O3 Cr1 O6 86.66(12) . . ?
O4 Cr1 N1 83.93(13) . . ?
O5 Cr1 N1 83.80(13) . . ?
O1 Cr1 N1 168.94(14) . . ?
O3 Cr1 N1 94.44(14) . . ?
O6 Cr1 N1 92.50(13) . . ?
O4 Cr1 Dy1 42.00(8) . 2_666 ?
O5 Cr1 Dy1 98.54(9) . 2_666 ?
O1 Cr1 Dy1 48.19(8) . 2_666 ?
O3 Cr1 Dy1 84.97(9) . 2_666 ?
O6 Cr1 Dy1 141.20(9) . 2_666 ?
N1 Cr1 Dy1 125.87(10) . 2_666 ?
O4 Cr1 Dy1 100.02(9) . . ?
O5 Cr1 Dy1 41.74(9) . . ?
O1 Cr1 Dy1 47.49(9) . . ?
O3 Cr1 Dy1 139.63(9) . . ?
O6 Cr1 Dy1 85.19(9) . . ?
N1 Cr1 Dy1 125.35(11) . . ?
Dy1 Cr1 Dy1 77.23(3) 2_666 . ?
C1 O1 Cr1 122.1(3) . . ?
C1 O1 Dy1 114.5(3) . . ?
Cr1 O1 Dy1 95.88(11) . . ?
C1 O1 Dy1 113.2(3) . 2_666 ?
Cr1 O1 Dy1 95.00(11) . 2_666 ?
Dy1 O1 Dy1 113.88(12) . 2_666 ?
C2 O2 Dy1 130.8(3) . 2_666 ?
C2 O3 Cr1 127.4(3) . . ?
C9 O4 Cr1 110.1(3) . . ?
C9 O4 Dy1 137.2(2) . 2_666 ?
Cr1 O4 Dy1 102.34(12) . 2_666 ?
C12 O5 Cr1 114.8(3) . . ?
C12 O5 Dy1 141.5(3) . . ?
Cr1 O5 Dy1 102.78(12) . . ?
C14 O6 Cr1 126.7(3) . . ?
C14 O7 Dy1 132.0(3) . . ?
N2 O8 Dy1 94.8(2) . . ?
N2 O9 Dy1 94.9(2) . . ?
C13 N1 C10 110.2(3) . . ?
C13 N1 C11 110.6(3) . . ?
C10 N1 C11 111.8(4) . . ?
C13 N1 Cr1 113.8(3) . . ?
C10 N1 Cr1 106.9(3) . . ?
C11 N1 Cr1 103.5(3) . . ?
O10 N2 O9 121.4(4) . . ?
O10 N2 O8 121.6(4) . . ?
O9 N2 O8 116.9(3) . . ?
O10 N2 Dy1 172.2(4) . . ?
O9 N2 Dy1 58.56(18) . . ?
O8 N2 Dy1 58.67(19) . . ?
O2 C2 O3 126.7(4) . . ?
O2 C2 C3 120.1(4) . . ?
O3 C2 C3 113.2(4) . . ?
C4 C3 C8 118.1(4) . . ?
C4 C3 C2 125.5(4) . . ?
C8 C3 C2 116.5(4) . . ?
C5 C4 C3 122.7(4) . . ?
C5 C4 Cl1 116.3(3) . . ?
C3 C4 Cl1 120.9(4) . . ?
C6 C5 C4 118.1(4) . . ?
F1 C6 C5 120.4(4) . . ?
F1 C6 C7 118.7(5) . . ?
C5 C6 C7 120.9(5) . . ?
F2 C7 C6 118.8(5) . . ?
F2 C7 C8 120.3(4) . . ?
C6 C7 C8 120.9(5) . . ?
C7 C8 C3 119.4(4) . . ?
O4 C9 C10 107.9(3) . . ?
N1 C10 C9 109.6(4) . . ?
C12 C11 N1 109.5(4) . . ?
O5 C12 C11 110.3(4) . . ?
O7 C14 O6 126.4(4) . . ?
O7 C14 C15 118.9(4) . . ?
O6 C14 C15 114.7(4) . . ?
C16 C15 C20 118.7(4) . . ?
C16 C15 C14 123.2(4) . . ?
C20 C15 C14 118.1(4) . . ?
C15 C16 C17 122.2(4) . . ?
C15 C16 Cl2 120.0(3) . . ?
C17 C16 Cl2 117.6(4) . . ?
C18 C17 C16 117.6(4) . . ?
F3 C18 C19 119.1(4) . . ?
F3 C18 C17 119.4(5) . . ?
C19 C18 C17 121.5(4) . . ?
F4 C19 C18 119.0(4) . . ?
F4 C19 C20 120.2(5) . . ?
C18 C19 C20 120.7(4) . . ?
C19 C20 C15 119.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.916
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.916
_refine_diff_density_max         0.919
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.127
####################################################################### 
# 
# 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_merge
_database_code_depnum_ccdc_archive 'CCDC 1495742'
_audit_update_record             
;
2016-07-23 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H37.67 Cl4 Cr2 F8 Ho2 N4 O20.83'
_chemical_formula_weight         1635.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6670(19)
_cell_length_b                   11.331(2)
_cell_length_c                   13.316(3)
_cell_angle_alpha                67.54(3)
_cell_angle_beta                 78.27(3)
_cell_angle_gamma                87.69(3)
_cell_volume                     1318.7(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27401
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.50

_exptl_crystal_description       Plate
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             793
_exptl_absorpt_coefficient_mu    3.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71079
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27401
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5907
_reflns_number_gt                5734
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
The collection was performed at the Australian synchrotron. We
were restricted to one 360 degree phi scan.
The structure was solved by direct methods. The asymmetric unit contains half the cluster, with a disordered methoxide/hydroxide group and a disordered solvent MeOH molecule.
It is found that the methoxide group is present 59 % of the time and the hydroxide and the solvent MeOH ligands are present 41 % of the time.
All non-H atoms are refined anisotropically. The H-atoms are placed in calculated positions except for the H atom found on the disordered OH ligands, which were omitted. These atoms were later added to the formula.
 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0446P)²+3.3261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5907
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0819
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.614721(17) 0.607274(14) 0.548861(12) 0.02446(6) Uani 1 1 d . . .
Cr1 Cr 0.56819(6) 0.29626(5) 0.64739(4) 0.02440(12) Uani 1 1 d . . .
Cl1 Cl 0.11279(11) 0.00402(10) 0.61253(8) 0.0382(2) Uani 1 1 d . . .
Cl2 Cl 0.35193(13) 0.23955(12) 1.01319(9) 0.0473(3) Uani 1 1 d . . .
F1 F -0.0356(3) -0.2677(3) 1.0167(3) 0.0621(9) Uani 1 1 d . . .
F2 F 0.1275(4) -0.1319(4) 1.0776(2) 0.0748(12) Uani 1 1 d . A .
F3 F 0.6782(3) 0.3109(3) 1.2369(2) 0.0482(6) Uani 1 1 d . . .
F4 F 0.8499(3) 0.4733(4) 1.0555(3) 0.0618(8) Uani 1 1 d . A .
O1 O 0.4381(3) 0.4371(2) 0.6042(2) 0.0260(5) Uani 1 1 d . . .
O1S O 0.2174(9) 0.4011(10) 0.7728(7) 0.053(3) Uani 0.414(10) 1 d P A 2
H1S H 0.2919 0.4317 0.7255 0.063 Uiso 0.414(10) 1 calc PR A 2
O2 O 0.2596(3) 0.2302(3) 0.6129(2) 0.0311(6) Uani 1 1 d . . .
O3 O 0.4137(3) 0.1647(2) 0.7276(2) 0.0290(5) Uani 1 1 d . . .
O4 O 0.5638(3) 0.2723(2) 0.5104(2) 0.0279(5) Uani 1 1 d . . .
O5 O 0.7243(3) 0.4233(2) 0.5764(2) 0.0272(5) Uani 1 1 d . . .
O6 O 0.5716(3) 0.3049(2) 0.7936(2) 0.0280(5) Uani 1 1 d . . .
O7 O 0.5756(3) 0.5178(2) 0.7449(2) 0.0298(5) Uani 1 1 d . . .
O8 O 0.8266(3) 0.6554(3) 0.5999(2) 0.0374(6) Uani 1 1 d . . .
O9 O 0.6486(3) 0.7779(3) 0.6100(2) 0.0350(6) Uani 1 1 d . . .
O10 O 0.8309(5) 0.7931(4) 0.6781(4) 0.0725(12) Uani 1 1 d . . .
N1 N 0.7291(4) 0.1664(3) 0.6619(3) 0.0315(7) Uani 1 1 d . . .
N2 N 0.7726(4) 0.7458(3) 0.6291(3) 0.0402(8) Uani 1 1 d . A .
C1 C 0.3099(8) 0.4465(7) 0.6820(5) 0.0316(16) Uani 0.586(10) 1 d P A 1
H1A H 0.2261 0.4265 0.6596 0.047 Uiso 0.586(10) 1 calc PR A 1
H1B H 0.3052 0.5335 0.6810 0.047 Uiso 0.586(10) 1 calc PR A 1
H1C H 0.3131 0.3857 0.7571 0.047 Uiso 0.586(10) 1 calc PR A 1
C1S C 0.0991(16) 0.4695(19) 0.7328(12) 0.069(5) Uani 0.414(10) 1 d P A 2
H1S1 H 0.0114 0.4193 0.7754 0.104 Uiso 0.414(10) 1 calc PR A 2
H1S2 H 0.1085 0.4843 0.6542 0.104 Uiso 0.414(10) 1 calc PR A 2
H1S3 H 0.0964 0.5518 0.7413 0.104 Uiso 0.414(10) 1 calc PR A 2
C2 C 0.2996(4) 0.1553(3) 0.6979(3) 0.0277(7) Uani 1 1 d . A .
C3 C 0.2054(4) 0.0418(4) 0.7784(3) 0.0310(7) Uani 1 1 d . . .
C4 C 0.1194(4) -0.0300(4) 0.7499(3) 0.0322(8) Uani 1 1 d . A .
C5 C 0.0379(4) -0.1349(4) 0.8276(4) 0.0382(9) Uani 1 1 d . . .
H5 H -0.0194 -0.1834 0.8060 0.046 Uiso 1 1 calc R A .
C6 C 0.0425(5) -0.1665(4) 0.9371(4) 0.0439(10) Uani 1 1 d . A .
C7 C 0.1268(5) -0.0970(5) 0.9683(4) 0.0487(12) Uani 1 1 d . . .
C8 C 0.2097(5) 0.0057(4) 0.8909(4) 0.0423(10) Uani 1 1 d . A .
H8 H 0.2693 0.0517 0.9131 0.051 Uiso 1 1 calc R . .
C9 C 0.6167(5) 0.1504(4) 0.5175(4) 0.0389(9) Uani 1 1 d . A .
H9A H 0.6353 0.1456 0.4433 0.047 Uiso 1 1 calc R . .
H9B H 0.5460 0.0819 0.5681 0.047 Uiso 1 1 calc R . .
C10 C 0.7518(5) 0.1332(4) 0.5610(4) 0.0423(10) Uani 1 1 d . A .
H10A H 0.7801 0.0435 0.5804 0.051 Uiso 1 1 calc R . .
H10B H 0.8286 0.1892 0.5030 0.051 Uiso 1 1 calc R . .
C11 C 0.8544(5) 0.2404(4) 0.6617(4) 0.0388(9) Uani 1 1 d . A .
H11A H 0.9421 0.1969 0.6460 0.047 Uiso 1 1 calc R . .
H11B H 0.8466 0.2444 0.7356 0.047 Uiso 1 1 calc R . .
C12 C 0.8611(5) 0.3736(4) 0.5749(4) 0.0406(9) Uani 1 1 d . A .
H12A H 0.9243 0.4293 0.5893 0.049 Uiso 1 1 calc R . .
H12B H 0.9007 0.3721 0.5007 0.049 Uiso 1 1 calc R . .
C13 C 0.6994(5) 0.0511(4) 0.7644(4) 0.0385(9) Uani 1 1 d . A .
H13A H 0.6224 -0.0004 0.7615 0.058 Uiso 1 1 calc R . .
H13B H 0.6718 0.0759 0.8284 0.058 Uiso 1 1 calc R . .
H13C H 0.7844 0.0009 0.7716 0.058 Uiso 1 1 calc R . .
C14 C 0.5781(4) 0.4063(3) 0.8121(3) 0.0257(7) Uani 1 1 d . A .
C15 C 0.5970(4) 0.3840(4) 0.9276(3) 0.0289(7) Uani 1 1 d . . .
C16 C 0.5065(4) 0.3040(4) 1.0229(3) 0.0328(8) Uani 1 1 d . A .
C17 C 0.5301(5) 0.2790(4) 1.1287(3) 0.0366(9) Uani 1 1 d . . .
H17 H 0.4669 0.2247 1.1931 0.044 Uiso 1 1 calc R A .
C18 C 0.6479(5) 0.3359(4) 1.1364(3) 0.0366(9) Uani 1 1 d . A .
C19 C 0.7369(5) 0.4185(4) 1.0433(4) 0.0410(9) Uani 1 1 d . . .
C20 C 0.7121(5) 0.4442(4) 0.9391(4) 0.0376(9) Uani 1 1 d . A .
H20 H 0.7729 0.5026 0.8755 0.045 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O5 2.236(3) . ?
Ho1 O4 2.238(3) 2_666 ?
Ho1 O2 2.365(3) 2_666 ?
Ho1 O7 2.365(3) . ?
Ho1 O1 2.418(3) . ?
Ho1 O9 2.424(3) . ?
Ho1 O8 2.428(3) . ?
Ho1 O1 2.428(3) 2_666 ?
Cr1 O5 1.949(3) . ?
Cr1 O4 1.953(3) . ?
Cr1 O1 1.972(3) . ?
Cr1 O3 1.977(3) . ?
Cr1 O6 1.993(3) . ?
Cr1 N1 2.083(3) . ?
Cr1 Ho1 3.2699(12) 2_666 ?
Cl1 C4 1.734(4) . ?
Cl2 C16 1.739(4) . ?
F1 C6 1.350(5) . ?
F2 C7 1.355(5) . ?
F3 C18 1.349(5) . ?
F4 C19 1.345(5) . ?
O1 C1 1.474(7) . ?
O1 Ho1 2.428(3) 2_666 ?
O1S C1S 1.433(17) . ?
O2 C2 1.253(5) . ?
O2 Ho1 2.365(3) 2_666 ?
O3 C2 1.266(5) . ?
O4 C9 1.428(5) . ?
O4 Ho1 2.238(3) 2_666 ?
O5 C12 1.417(5) . ?
O6 C14 1.270(4) . ?
O7 C14 1.241(4) . ?
O8 N2 1.284(5) . ?
O9 N2 1.285(5) . ?
O10 N2 1.213(5) . ?
N1 C13 1.470(5) . ?
N1 C11 1.500(5) . ?
N1 C10 1.502(5) . ?
C2 C3 1.508(5) . ?
C3 C4 1.384(6) . ?
C3 C8 1.403(6) . ?
C4 C5 1.382(6) . ?
C5 C6 1.371(7) . ?
C6 C7 1.378(7) . ?
C7 C8 1.371(6) . ?
C9 C10 1.510(6) . ?
C11 C12 1.504(6) . ?
C14 C15 1.509(5) . ?
C15 C16 1.390(5) . ?
C15 C20 1.392(6) . ?
C16 C17 1.391(5) . ?
C17 C18 1.371(6) . ?
C18 C19 1.378(6) . ?
C19 C20 1.374(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ho1 O4 147.92(10) . 2_666 ?
O5 Ho1 O2 109.49(10) . 2_666 ?
O4 Ho1 O2 79.79(10) 2_666 2_666 ?
O5 Ho1 O7 79.42(10) . . ?
O4 Ho1 O7 111.40(10) 2_666 . ?
O2 Ho1 O7 144.37(9) 2_666 . ?
O5 Ho1 O1 71.46(9) . . ?
O4 Ho1 O1 81.99(9) 2_666 . ?
O2 Ho1 O1 140.30(9) 2_666 . ?
O7 Ho1 O1 75.29(9) . . ?
O5 Ho1 O9 130.36(10) . . ?
O4 Ho1 O9 81.33(10) 2_666 . ?
O2 Ho1 O9 76.26(10) 2_666 . ?
O7 Ho1 O9 72.49(9) . . ?
O1 Ho1 O9 134.91(9) . . ?
O5 Ho1 O8 79.75(10) . . ?
O4 Ho1 O8 131.93(10) 2_666 . ?
O2 Ho1 O8 74.79(10) 2_666 . ?
O7 Ho1 O8 73.06(10) . . ?
O1 Ho1 O8 140.36(9) . . ?
O9 Ho1 O8 53.45(11) . . ?
O5 Ho1 O1 80.92(9) . 2_666 ?
O4 Ho1 O1 71.78(9) 2_666 2_666 ?
O2 Ho1 O1 75.02(9) 2_666 2_666 ?
O7 Ho1 O1 140.29(9) . 2_666 ?
O1 Ho1 O1 65.83(10) . 2_666 ?
O9 Ho1 O1 143.47(9) . 2_666 ?
O8 Ho1 O1 135.92(10) . 2_666 ?
O5 Cr1 O4 93.09(12) . . ?
O5 Cr1 O1 87.91(11) . . ?
O4 Cr1 O1 88.55(11) . . ?
O5 Cr1 O3 176.66(11) . . ?
O4 Cr1 O3 89.85(12) . . ?
O1 Cr1 O3 93.76(11) . . ?
O5 Cr1 O6 90.25(11) . . ?
O4 Cr1 O6 175.20(11) . . ?
O1 Cr1 O6 95.02(11) . . ?
O3 Cr1 O6 86.73(11) . . ?
O5 Cr1 N1 83.71(13) . . ?
O4 Cr1 N1 84.44(12) . . ?
O1 Cr1 N1 168.76(12) . . ?
O3 Cr1 N1 95.00(13) . . ?
O6 Cr1 N1 92.51(12) . . ?
O5 Cr1 Ho1 98.60(8) . 2_666 ?
O4 Cr1 Ho1 41.95(8) . 2_666 ?
O1 Cr1 Ho1 47.66(8) . 2_666 ?
O3 Cr1 Ho1 84.65(8) . 2_666 ?
O6 Cr1 Ho1 140.75(8) . 2_666 ?
N1 Cr1 Ho1 126.34(9) . 2_666 ?
C1 O1 Cr1 121.9(3) . . ?
C1 O1 Ho1 114.6(3) . . ?
Cr1 O1 Ho1 95.81(11) . . ?
C1 O1 Ho1 112.7(3) . 2_666 ?
Cr1 O1 Ho1 95.44(10) . 2_666 ?
Ho1 O1 Ho1 114.17(10) . 2_666 ?
C2 O2 Ho1 130.9(3) . 2_666 ?
C2 O3 Cr1 127.3(2) . . ?
C9 O4 Cr1 109.7(2) . . ?
C9 O4 Ho1 137.8(2) . 2_666 ?
Cr1 O4 Ho1 102.36(11) . 2_666 ?
C12 O5 Cr1 115.3(2) . . ?
C12 O5 Ho1 141.1(2) . . ?
Cr1 O5 Ho1 102.61(11) . . ?
C14 O6 Cr1 125.9(2) . . ?
C14 O7 Ho1 131.9(2) . . ?
N2 O8 Ho1 94.8(2) . . ?
N2 O9 Ho1 95.0(2) . . ?
C13 N1 C11 109.8(3) . . ?
C13 N1 C10 111.2(3) . . ?
C11 N1 C10 111.3(4) . . ?
C13 N1 Cr1 113.7(3) . . ?
C11 N1 Cr1 103.7(2) . . ?
C10 N1 Cr1 106.9(2) . . ?
O10 N2 O8 122.2(4) . . ?
O10 N2 O9 121.4(4) . . ?
O8 N2 O9 116.2(3) . . ?
O2 C2 O3 126.8(3) . . ?
O2 C2 C3 119.6(3) . . ?
O3 C2 C3 113.5(3) . . ?
C4 C3 C8 118.3(4) . . ?
C4 C3 C2 125.5(3) . . ?
C8 C3 C2 116.2(4) . . ?
C5 C4 C3 122.7(4) . . ?
C5 C4 Cl1 115.9(3) . . ?
C3 C4 Cl1 121.4(3) . . ?
C6 C5 C4 117.7(4) . . ?
F1 C6 C5 120.3(4) . . ?
F1 C6 C7 118.6(4) . . ?
C5 C6 C7 121.1(4) . . ?
F2 C7 C8 120.0(4) . . ?
F2 C7 C6 118.9(4) . . ?
C8 C7 C6 121.1(4) . . ?
C7 C8 C3 119.2(4) . . ?
O4 C9 C10 108.6(3) . . ?
N1 C10 C9 109.4(4) . . ?
N1 C11 C12 109.9(3) . . ?
O5 C12 C11 110.2(4) . . ?
O7 C14 O6 126.9(3) . . ?
O7 C14 C15 118.8(3) . . ?
O6 C14 C15 114.3(3) . . ?
C16 C15 C20 118.5(4) . . ?
C16 C15 C14 123.0(3) . . ?
C20 C15 C14 118.5(3) . . ?
C15 C16 C17 122.2(4) . . ?
C15 C16 Cl2 120.1(3) . . ?
C17 C16 Cl2 117.5(3) . . ?
C18 C17 C16 117.5(4) . . ?
F3 C18 C17 119.7(4) . . ?
F3 C18 C19 118.9(4) . . ?
C17 C18 C19 121.4(4) . . ?
F4 C19 C20 120.1(4) . . ?
F4 C19 C18 119.0(4) . . ?
C20 C19 C18 120.9(4) . . ?
C19 C20 C15 119.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_p-1
_database_code_depnum_ccdc_archive 'CCDC 1495743'
_audit_update_record             
;
2016-07-23 deposited with the CCDC.
2016-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H114 Cr2 Dy2 N4 O23'
_chemical_formula_weight         1808.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.164(2)
_cell_length_b                   11.907(2)
_cell_length_c                   16.534(3)
_cell_angle_alpha                70.77(3)
_cell_angle_beta                 73.76(3)
_cell_angle_gamma                82.43(3)
_cell_volume                     1990.5(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    32265
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.50

_exptl_crystal_description       Plate
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             925
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_T_max  0.482
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71079
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32265
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8352
_reflns_number_gt                8051
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The collection was performed at the Australian synchrotron. We
were restricted to one 360 degree phi scan.
The structure was solved by direct methods. The asymmetric unit contains half the cluster, with a disordered methoxide/hydroxide group, a disordered solvent MeOH molecule and a diethyl ether solvent molecule. The tert-butyl group of one of the 4-tertbutylbenzoate ligands is disordered over two positions (45:55 occupancy). Bond (DFIX) and thermal (ISOR) restraints are placed on the disordered atoms.
It is found that the methoxide group is present 50 % of the time and the hydroxide and the solvent MeOH ligands are present 50 % of the time.
All non-H atoms are refined anisotropically. The H-atoms are placed in calculated positions except for the H atom found on the disordered OH ligands, which were omitted. These atoms were later added to the formula.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0664P)²+7.5417P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8352
_refine_ls_number_parameters     512
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1177
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 1.154353(14) 0.401365(16) 0.460673(12) 0.02198(8) Uani 1 1 d . . .
Cr1 Cr 0.86677(5) 0.31092(6) 0.56028(4) 0.02228(14) Uani 1 1 d . . .
O1 O 0.9720(3) 0.4166(3) 0.57811(19) 0.0240(6) Uani 1 1 d . . 1
O1S O 0.9979(17) 0.3886(18) 0.7385(9) 0.120(6) Uani 0.50 1 d P A 2
H10 H 1.0507 0.3376 0.7583 0.144 Uiso 0.50 1 calc PR A 2
O2 O 0.7384(3) 0.4831(3) 0.6818(2) 0.0297(7) Uani 1 1 d . . .
O2S O 1.1100(6) 0.2117(6) 0.8265(4) 0.0884(19) Uani 1 1 d . . .
O3 O 0.7467(3) 0.2963(3) 0.6764(2) 0.0282(6) Uani 1 1 d . . .
O4 O 0.7781(3) 0.4555(3) 0.5040(2) 0.0255(6) Uani 1 1 d . . .
O5 O 0.9920(3) 0.3200(3) 0.4493(2) 0.0255(6) Uani 1 1 d . . .
O6 O 0.9559(3) 0.1671(3) 0.6220(2) 0.0278(6) Uani 1 1 d . . .
O7 O 1.1557(3) 0.2210(3) 0.5758(2) 0.0301(7) Uani 1 1 d . . .
O8 O 1.2640(3) 0.2650(3) 0.3793(2) 0.0329(7) Uani 1 1 d . . .
O9 O 1.3738(3) 0.3328(3) 0.4410(2) 0.0350(7) Uani 1 1 d . . .
O10 O 1.4648(4) 0.2278(4) 0.3517(3) 0.0531(11) Uani 1 1 d . . .
N1 N 0.7584(3) 0.2256(3) 0.5079(3) 0.0281(8) Uani 1 1 d . . .
N2 N 1.3707(3) 0.2729(4) 0.3905(3) 0.0353(9) Uani 1 1 d . . .
C1 C 1.0047(7) 0.3958(7) 0.6606(5) 0.0207(14) Uani 0.50 1 d P B 1
H1D H 0.9675 0.4600 0.6858 0.031 Uiso 0.50 1 calc PR B 1
H1E H 1.0957 0.3939 0.6497 0.031 Uiso 0.50 1 calc PR B 1
H1F H 0.9731 0.3195 0.7021 0.031 Uiso 0.50 1 calc PR B 1
C1S C 0.945(3) 0.455(2) 0.7991(16) 0.113(8) Uani 0.50 1 d P A 2
H34A H 0.9040 0.5293 0.7688 0.170 Uiso 0.50 1 calc PR A 2
H34B H 1.0105 0.4745 0.8203 0.170 Uiso 0.50 1 calc PR A 2
H34C H 0.8826 0.4081 0.8494 0.170 Uiso 0.50 1 calc PR A 2
C2 C 0.7096(4) 0.3768(4) 0.7142(3) 0.0257(8) Uani 1 1 d . . .
C2S C 1.0418(12) 0.1149(11) 0.8889(7) 0.099(3) Uani 1 1 d . . .
H29A H 1.0493 0.1067 0.9488 0.119 Uiso 1 1 calc R . .
H29B H 1.0757 0.0404 0.8750 0.119 Uiso 1 1 calc R . .
C3 C 0.6245(4) 0.3378(4) 0.8053(3) 0.0284(9) Uani 1 1 d . . .
C3S C 0.9071(10) 0.1353(10) 0.8866(7) 0.096(3) Uani 1 1 d . . .
H28A H 0.8750 0.2108 0.8978 0.143 Uiso 1 1 calc R . .
H28B H 0.8587 0.0700 0.9321 0.143 Uiso 1 1 calc R . .
H28C H 0.8996 0.1383 0.8282 0.143 Uiso 1 1 calc R . .
C4 C 0.5741(5) 0.4204(5) 0.8499(3) 0.0376(11) Uani 1 1 d . . .
H16 H 0.5956 0.5013 0.8229 0.045 Uiso 1 1 calc R . .
C4S C 1.2406(12) 0.2048(13) 0.8190(10) 0.120(5) Uani 1 1 d . . .
H30A H 1.2788 0.1320 0.8039 0.144 Uiso 1 1 calc R . .
H30B H 1.2558 0.2008 0.8761 0.144 Uiso 1 1 calc R . .
C5 C 0.4926(6) 0.3859(6) 0.9336(4) 0.0482(14) Uani 1 1 d . . .
H2 H 0.4602 0.4436 0.9633 0.058 Uiso 1 1 calc R . .
C5S C 1.2970(10) 0.3117(13) 0.7487(11) 0.132(5) Uani 1 1 d . . .
H31A H 1.2943 0.3081 0.6909 0.198 Uiso 1 1 calc R . .
H31B H 1.3840 0.3145 0.7495 0.198 Uiso 1 1 calc R . .
H31C H 1.2501 0.3834 0.7592 0.198 Uiso 1 1 calc R . .
C6 C 0.4577(7) 0.2697(6) 0.9743(4) 0.0524(15) Uani 1 1 d . . .
C7 C 0.5087(7) 0.1878(6) 0.9289(4) 0.0559(17) Uani 1 1 d . . .
H7 H 0.4867 0.1070 0.9558 0.067 Uiso 1 1 calc R . .
C8 C 0.5908(5) 0.2209(5) 0.8453(4) 0.0441(13) Uani 1 1 d . . .
H18 H 0.6238 0.1631 0.8158 0.053 Uiso 1 1 calc R . .
C9 C 0.3693(11) 0.2355(8) 1.0675(6) 0.116(5) Uani 1 1 d D . .
C10 C 0.3126(10) 0.1218(8) 1.0942(7) 0.088(3) Uani 1 1 d DU . .
H10A H 0.2647 0.1028 1.1562 0.131 Uiso 1 1 calc R . .
H10B H 0.3781 0.0596 1.0877 0.131 Uiso 1 1 calc R . .
H10C H 0.2568 0.1261 1.0567 0.131 Uiso 1 1 calc R . .
C11 C 0.2832(13) 0.3344(11) 1.0905(10) 0.131(5) Uani 1 1 d DU . .
H11A H 0.2058 0.3365 1.0731 0.197 Uiso 1 1 calc R . .
H11B H 0.3236 0.4104 1.0591 0.197 Uiso 1 1 calc R . .
H11C H 0.2640 0.3208 1.1545 0.197 Uiso 1 1 calc R . .
C12 C 0.449(2) 0.219(2) 1.133(2) 0.325(16) Uani 1 1 d DU . .
H12A H 0.4005 0.1818 1.1931 0.487 Uiso 1 1 d . . .
H12B H 0.4716 0.2996 1.1291 0.487 Uiso 1 1 d . . .
H12C H 0.5244 0.1725 1.1178 0.487 Uiso 1 1 d . . .
C13 C 0.6687(5) 0.4310(5) 0.4872(5) 0.0481(15) Uani 1 1 d . . .
H15A H 0.6469 0.4987 0.4389 0.058 Uiso 1 1 calc R . .
H15B H 0.5990 0.4234 0.5409 0.058 Uiso 1 1 calc R . .
C14 C 0.6822(7) 0.3245(6) 0.4631(6) 0.063(2) Uani 1 1 d . . .
H3A H 0.7195 0.3448 0.3985 0.076 Uiso 1 1 calc R . .
H3B H 0.5979 0.2958 0.4749 0.076 Uiso 1 1 calc R . .
C15 C 0.8601(7) 0.1845(9) 0.4421(6) 0.083(3) Uani 1 1 d . . .
H5A H 0.8911 0.1043 0.4728 0.100 Uiso 1 1 calc R . .
H5B H 0.8235 0.1761 0.3965 0.100 Uiso 1 1 calc R . .
C16 C 0.9649(5) 0.2585(6) 0.3983(4) 0.0436(13) Uani 1 1 d . . .
H13A H 1.0392 0.2082 0.3806 0.052 Uiso 1 1 calc R . .
H13B H 0.9486 0.3169 0.3436 0.052 Uiso 1 1 calc R . .
C17 C 0.6796(6) 0.1184(6) 0.5670(4) 0.0534(16) Uani 1 1 d . . .
C18 C 0.6273(6) 0.0611(6) 0.5165(4) 0.0497(14) Uani 1 1 d . . .
H1A H 0.6929 0.0114 0.4896 0.075 Uiso 1 1 calc R . .
H1B H 0.5965 0.1230 0.4700 0.075 Uiso 1 1 calc R . .
H1C H 0.5583 0.0115 0.5569 0.075 Uiso 1 1 calc R . .
C19 C 0.5546(6) 0.1721(7) 0.6228(6) 0.068(2) Uani 1 1 d . . .
H22A H 0.5025 0.1067 0.6643 0.102 Uiso 1 1 calc R . .
H22B H 0.5076 0.2252 0.5819 0.102 Uiso 1 1 calc R . .
H22C H 0.5783 0.2169 0.6557 0.102 Uiso 1 1 calc R . .
C20 C 0.7322(8) 0.0380(7) 0.6386(5) 0.068(2) Uani 1 1 d . . .
H19A H 0.6749 -0.0261 0.6744 0.102 Uiso 1 1 calc R . .
H19B H 0.7438 0.0826 0.6759 0.102 Uiso 1 1 calc R . .
H19C H 0.8130 0.0037 0.6131 0.102 Uiso 1 1 calc R . .
C21 C 1.0716(4) 0.1493(4) 0.6218(3) 0.0270(9) Uani 1 1 d . . .
C22 C 1.1048(4) 0.0318(4) 0.6821(3) 0.0332(10) Uani 1 1 d . . .
C23 C 1.0125(5) -0.0489(5) 0.7333(4) 0.0464(14) Uani 1 1 d . . .
H17 H 0.9281 -0.0286 0.7308 0.056 Uiso 1 1 calc R . .
C24 C 1.0430(7) -0.1587(6) 0.7880(5) 0.068(2) Uani 1 1 d . . .
H21 H 0.9790 -0.2131 0.8217 0.082 Uiso 1 1 calc R . .
C25 C 1.1633(8) -0.1910(7) 0.7948(5) 0.076(3) Uani 1 1 d . . .
C26 C 1.2561(7) -0.1089(6) 0.7439(4) 0.0602(19) Uani 1 1 d . . .
H6 H 1.3400 -0.1286 0.7478 0.072 Uiso 1 1 calc R . .
C27 C 1.2267(5) 0.0001(5) 0.6883(3) 0.0390(11) Uani 1 1 d . . .
H14 H 1.2908 0.0541 0.6539 0.047 Uiso 1 1 calc R . .
C28 C 1.1979(10) -0.3132(8) 0.8558(6) 0.103(4) Uani 1 1 d D . .
C29 C 1.197(2) -0.3029(19) 0.9425(10) 0.077(6) Uani 0.46(2) 1 d PDU . 3
H35A H 1.1985 -0.3827 0.9852 0.115 Uiso 0.46(2) 1 calc PR . 3
H35B H 1.1216 -0.2578 0.9634 0.115 Uiso 0.46(2) 1 calc PR . 3
H35C H 1.2710 -0.2616 0.9364 0.115 Uiso 0.46(2) 1 calc PR . 3
C29' C 1.297(3) -0.294(3) 0.896(2) 0.178(14) Uani 0.54(2) 1 d PDU . 4
H1'1 H 1.3725 -0.2672 0.8497 0.267 Uiso 0.54(2) 1 calc PR . 4
H1'2 H 1.3155 -0.3693 0.9391 0.267 Uiso 0.54(2) 1 calc PR . 4
H1'3 H 1.2654 -0.2340 0.9267 0.267 Uiso 0.54(2) 1 calc PR . 4
C30 C 1.3121(18) -0.3709(19) 0.8091(13) 0.072(5) Uani 0.46(2) 1 d PDU . 3
H47A H 1.3382 -0.4426 0.8516 0.108 Uiso 0.46(2) 1 calc PR . 3
H47B H 1.3797 -0.3150 0.7831 0.108 Uiso 0.46(2) 1 calc PR . 3
H47C H 1.2927 -0.3928 0.7621 0.108 Uiso 0.46(2) 1 calc PR . 3
C30' C 1.2677(14) -0.3844(12) 0.8085(8) 0.050(3) Uani 0.54(2) 1 d PU . 4
H2'1 H 1.3470 -0.3475 0.7734 0.076 Uiso 0.54(2) 1 calc PR . 4
H2'2 H 1.2220 -0.3945 0.7688 0.076 Uiso 0.54(2) 1 calc PR . 4
H2'3 H 1.2842 -0.4623 0.8491 0.076 Uiso 0.54(2) 1 calc PR . 4
C31 C 1.097(3) -0.395(3) 0.866(3) 0.177(16) Uani 0.46(2) 1 d PDU . 3
H36A H 1.0135 -0.3524 0.8783 0.265 Uiso 0.46 1 d P . 3
H36B H 1.0965 -0.4657 0.9195 0.265 Uiso 0.46 1 d P . 3
H36C H 1.1087 -0.4195 0.8152 0.265 Uiso 0.46 1 d P . 3
C31' C 1.0967(17) -0.356(2) 0.9379(11) 0.105(7) Uani 0.54(2) 1 d PDU . 4
H3'1 H 1.1269 -0.4282 0.9780 0.157 Uiso 0.54 1 d P . 4
H3'2 H 1.0251 -0.3773 0.9218 0.157 Uiso 0.54 1 d P . 4
H3'3 H 1.0697 -0.2950 0.9664 0.157 Uiso 0.54 1 d P . 4


_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 O5 2.243(3) . ?
Dy1 O4 2.249(3) 2_766 ?
Dy1 O7 2.356(3) . ?
Dy1 O2 2.365(3) 2_766 ?
Dy1 O1 2.423(3) . ?
Dy1 O1 2.425(3) 2_766 ?
Dy1 O8 2.437(4) . ?
Dy1 O9 2.445(3) . ?
Dy1 N2 2.854(4) . ?
Cr1 O5 1.951(3) . ?
Cr1 O4 1.955(3) . ?
Cr1 O1 1.970(3) . ?
Cr1 O3 1.979(3) . ?
Cr1 O6 1.982(3) . ?
Cr1 N1 2.176(4) . ?
Cr1 Dy1 3.3111(10) 2_766 ?
O1 C1 1.444(8) . ?
O1 Dy1 2.425(3) 2_766 ?
O1S C1S 1.43(3) . ?
O1S H10 0.8400 . ?
O2 C2 1.248(5) . ?
O2 Dy1 2.365(3) 2_766 ?
O2S C2S 1.407(13) . ?
O2S C4S 1.422(13) . ?
O3 C2 1.274(6) . ?
O4 C13 1.411(5) . ?
O4 Dy1 2.249(3) 2_766 ?
O5 C16 1.396(6) . ?
O6 C21 1.280(5) . ?
O7 C21 1.254(5) . ?
O8 N2 1.275(5) . ?
O9 N2 1.274(6) . ?
O10 N2 1.227(6) . ?
N1 C14 1.474(7) . ?
N1 C15 1.492(8) . ?
N1 C17 1.534(6) . ?
C1 H1D 0.9800 . ?
C1 H1E 0.9800 . ?
C1 H1F 0.9800 . ?
C1S H34A 0.9800 . ?
C1S H34B 0.9800 . ?
C1S H34C 0.9800 . ?
C2 C3 1.497(6) . ?
C2S C3S 1.500(15) . ?
C2S H29A 0.9900 . ?
C2S H29B 0.9900 . ?
C3 C8 1.381(7) . ?
C3 C4 1.388(7) . ?
C3S H28A 0.9800 . ?
C3S H28B 0.9800 . ?
C3S H28C 0.9800 . ?
C4 C5 1.390(7) . ?
C4 H16 0.9500 . ?
C4S C5S 1.482(18) . ?
C4S H30A 0.9900 . ?
C4S H30B 0.9900 . ?
C5 C6 1.379(8) . ?
C5 H2 0.9500 . ?
C5S H31A 0.9800 . ?
C5S H31B 0.9800 . ?
C5S H31C 0.9800 . ?
C6 C7 1.391(9) . ?
C6 C9 1.535(9) . ?
C7 C8 1.391(7) . ?
C7 H7 0.9500 . ?
C8 H18 0.9500 . ?
C9 C10 1.451(8) . ?
C9 C11 1.499(9) . ?
C9 C12 1.534(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9782 . ?
C12 H12B 1.0007 . ?
C12 H12C 0.9606 . ?
C13 C14 1.428(10) . ?
C13 H15A 0.9900 . ?
C13 H15B 0.9900 . ?
C14 H3A 0.9900 . ?
C14 H3B 0.9900 . ?
C15 C16 1.430(8) . ?
C15 H5A 0.9900 . ?
C15 H5B 0.9900 . ?
C16 H13A 0.9900 . ?
C16 H13B 0.9900 . ?
C17 C20 1.468(9) . ?
C17 C18 1.503(8) . ?
C17 C19 1.626(11) . ?
C18 H1A 0.9800 . ?
C18 H1B 0.9800 . ?
C18 H1C 0.9800 . ?
C19 H22A 0.9800 . ?
C19 H22B 0.9800 . ?
C19 H22C 0.9800 . ?
C20 H19A 0.9800 . ?
C20 H19B 0.9800 . ?
C20 H19C 0.9800 . ?
C21 C22 1.496(6) . ?
C22 C27 1.386(7) . ?
C22 C23 1.394(7) . ?
C23 C24 1.385(8) . ?
C23 H17 0.9500 . ?
C24 C25 1.373(11) . ?
C24 H21 0.9500 . ?
C25 C26 1.405(11) . ?
C25 C28 1.545(9) . ?
C26 C27 1.382(7) . ?
C26 H6 0.9500 . ?
C27 H14 0.9500 . ?
C28 C30' 1.364(16) . ?
C28 C29 1.475(9) . ?
C28 C31' 1.490(10) . ?
C28 C30 1.504(10) . ?
C28 C29' 1.514(7) . ?
C28 C31 1.522(10) . ?
C29 H35A 0.9800 . ?
C29 H35B 0.9800 . ?
C29 H35C 0.9800 . ?
C29' H1'1 0.9800 . ?
C29' H1'2 0.9800 . ?
C29' H1'3 0.9800 . ?
C30 H47A 0.9800 . ?
C30 H47B 0.9800 . ?
C30 H47C 0.9800 . ?
C30' H2'1 0.9800 . ?
C30' H2'2 0.9800 . ?
C30' H2'3 0.9800 . ?
C31 H36A 0.9957 . ?
C31 H36B 0.9986 . ?
C31 H36C 0.9567 . ?
C31 H3'2 1.0908 . ?
C31' H3'1 0.9802 . ?
C31' H3'2 0.9939 . ?
C31' H3'3 0.9663 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Dy1 O4 147.60(11) . 2_766 ?
O5 Dy1 O7 81.66(11) . . ?
O4 Dy1 O7 108.55(12) 2_766 . ?
O5 Dy1 O2 109.21(12) . 2_766 ?
O4 Dy1 O2 80.05(12) 2_766 2_766 ?
O7 Dy1 O2 145.63(11) . 2_766 ?
O5 Dy1 O1 70.02(11) . . ?
O4 Dy1 O1 82.91(11) 2_766 . ?
O7 Dy1 O1 74.60(11) . . ?
O2 Dy1 O1 139.68(11) 2_766 . ?
O5 Dy1 O1 82.51(11) . 2_766 ?
O4 Dy1 O1 70.23(10) 2_766 2_766 ?
O7 Dy1 O1 140.89(10) . 2_766 ?
O2 Dy1 O1 73.47(11) 2_766 2_766 ?
O1 Dy1 O1 66.41(12) . 2_766 ?
O5 Dy1 O8 79.60(11) . . ?
O4 Dy1 O8 132.03(11) 2_766 . ?
O7 Dy1 O8 78.21(12) . . ?
O2 Dy1 O8 72.23(11) 2_766 . ?
O1 Dy1 O8 141.53(11) . . ?
O1 Dy1 O8 133.08(11) 2_766 . ?
O5 Dy1 O9 129.88(12) . . ?
O4 Dy1 O9 82.39(12) 2_766 . ?
O7 Dy1 O9 74.93(11) . . ?
O2 Dy1 O9 73.37(12) 2_766 . ?
O1 Dy1 O9 139.66(11) . . ?
O1 Dy1 O9 139.90(11) 2_766 . ?
O8 Dy1 O9 52.74(12) . . ?
O5 Dy1 N2 105.35(12) . . ?
O4 Dy1 N2 106.93(12) 2_766 . ?
O7 Dy1 N2 76.51(12) . . ?
O2 Dy1 N2 69.20(12) 2_766 . ?
O1 Dy1 N2 151.11(11) . . ?
O1 Dy1 N2 142.39(11) 2_766 . ?
O8 Dy1 N2 26.42(12) . . ?
O9 Dy1 N2 26.40(13) . . ?
O5 Cr1 O4 91.75(13) . . ?
O5 Cr1 O1 86.30(13) . . ?
O4 Cr1 O1 86.64(13) . . ?
O5 Cr1 O3 176.77(13) . . ?
O4 Cr1 O3 91.22(13) . . ?
O1 Cr1 O3 92.60(13) . . ?
O5 Cr1 O6 90.09(13) . . ?
O4 Cr1 O6 177.39(14) . . ?
O1 Cr1 O6 91.63(13) . . ?
O3 Cr1 O6 86.90(13) . . ?
O5 Cr1 N1 83.93(14) . . ?
O4 Cr1 N1 83.40(14) . . ?
O1 Cr1 N1 165.81(14) . . ?
O3 Cr1 N1 97.68(14) . . ?
O6 Cr1 N1 98.64(14) . . ?
O5 Cr1 Dy1 97.06(10) . 2_766 ?
O4 Cr1 Dy1 41.28(9) . 2_766 ?
O1 Cr1 Dy1 46.61(9) . 2_766 ?
O3 Cr1 Dy1 84.34(10) . 2_766 ?
O6 Cr1 Dy1 136.58(10) . 2_766 ?
N1 Cr1 Dy1 124.64(11) . 2_766 ?
C1 O1 Cr1 123.3(4) . . ?
C1 O1 Dy1 111.4(3) . . ?
Cr1 O1 Dy1 97.31(13) . . ?
C1 O1 Dy1 112.7(4) . 2_766 ?
Cr1 O1 Dy1 97.23(11) . 2_766 ?
Dy1 O1 Dy1 113.59(12) . 2_766 ?
C1S O1S H10 109.5 . . ?
C2 O2 Dy1 133.5(3) . 2_766 ?
C2S O2S C4S 116.4(9) . . ?
C2 O3 Cr1 127.7(3) . . ?
C13 O4 Cr1 112.4(3) . . ?
C13 O4 Dy1 137.9(3) . 2_766 ?
Cr1 O4 Dy1 103.72(13) . 2_766 ?
C16 O5 Cr1 114.9(3) . . ?
C16 O5 Dy1 139.7(3) . . ?
Cr1 O5 Dy1 104.06(14) . . ?
C21 O6 Cr1 129.8(3) . . ?
C21 O7 Dy1 131.5(3) . . ?
N2 O8 Dy1 95.4(3) . . ?
N2 O9 Dy1 95.0(2) . . ?
C14 N1 C15 110.9(6) . . ?
C14 N1 C17 111.6(4) . . ?
C15 N1 C17 107.6(5) . . ?
C14 N1 Cr1 103.9(3) . . ?
C15 N1 Cr1 100.4(3) . . ?
C17 N1 Cr1 121.7(3) . . ?
O10 N2 O9 122.7(5) . . ?
O10 N2 O8 120.7(5) . . ?
O9 N2 O8 116.5(4) . . ?
O10 N2 Dy1 172.9(4) . . ?
O9 N2 Dy1 58.6(2) . . ?
O8 N2 Dy1 58.2(2) . . ?
O1S C1S H34A 109.5 . . ?
O1S C1S H34B 109.5 . . ?
H34A C1S H34B 109.5 . . ?
O1S C1S H34C 109.5 . . ?
H34A C1S H34C 109.5 . . ?
H34B C1S H34C 109.5 . . ?
O2 C2 O3 125.6(4) . . ?
O2 C2 C3 118.5(4) . . ?
O3 C2 C3 115.9(4) . . ?
O2S C2S C3S 109.4(9) . . ?
O2S C2S H29A 109.8 . . ?
C3S C2S H29A 109.8 . . ?
O2S C2S H29B 109.8 . . ?
C3S C2S H29B 109.8 . . ?
H29A C2S H29B 108.2 . . ?
C8 C3 C4 118.7(4) . . ?
C8 C3 C2 121.2(4) . . ?
C4 C3 C2 120.1(4) . . ?
C2S C3S H28A 109.5 . . ?
C2S C3S H28B 109.5 . . ?
H28A C3S H28B 109.5 . . ?
C2S C3S H28C 109.5 . . ?
H28A C3S H28C 109.5 . . ?
H28B C3S H28C 109.5 . . ?
C3 C4 C5 120.7(5) . . ?
C3 C4 H16 119.7 . . ?
C5 C4 H16 119.7 . . ?
O2S C4S C5S 108.8(9) . . ?
O2S C4S H30A 109.9 . . ?
C5S C4S H30A 109.9 . . ?
O2S C4S H30B 109.9 . . ?
C5S C4S H30B 109.9 . . ?
H30A C4S H30B 108.3 . . ?
C6 C5 C4 121.4(5) . . ?
C6 C5 H2 119.3 . . ?
C4 C5 H2 119.3 . . ?
C4S C5S H31A 109.5 . . ?
C4S C5S H31B 109.5 . . ?
H31A C5S H31B 109.5 . . ?
C4S C5S H31C 109.5 . . ?
H31A C5S H31C 109.5 . . ?
H31B C5S H31C 109.5 . . ?
C5 C6 C7 117.4(5) . . ?
C5 C6 C9 119.4(6) . . ?
C7 C6 C9 123.1(6) . . ?
C8 C7 C6 121.9(5) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C3 C8 C7 120.0(5) . . ?
C3 C8 H18 120.0 . . ?
C7 C8 H18 120.0 . . ?
C10 C9 C11 115.3(9) . . ?
C10 C9 C12 104.5(11) . . ?
C11 C9 C12 97.9(10) . . ?
C10 C9 C6 114.5(8) . . ?
C11 C9 C6 115.2(9) . . ?
C12 C9 C6 106.8(16) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 108.3 . . ?
H12A C12 H12B 107.9 . . ?
C9 C12 H12C 110.5 . . ?
H12A C12 H12C 111.3 . . ?
H12B C12 H12C 109.4 . . ?
O4 C13 C14 112.5(4) . . ?
O4 C13 H15A 109.1 . . ?
C14 C13 H15A 109.1 . . ?
O4 C13 H15B 109.1 . . ?
C14 C13 H15B 109.1 . . ?
H15A C13 H15B 107.8 . . ?
C13 C14 N1 116.6(5) . . ?
C13 C14 H3A 108.1 . . ?
N1 C14 H3A 108.1 . . ?
C13 C14 H3B 108.1 . . ?
N1 C14 H3B 108.1 . . ?
H3A C14 H3B 107.3 . . ?
C16 C15 N1 116.7(6) . . ?
C16 C15 H5A 108.1 . . ?
N1 C15 H5A 108.1 . . ?
C16 C15 H5B 108.1 . . ?
N1 C15 H5B 108.1 . . ?
H5A C15 H5B 107.3 . . ?
O5 C16 C15 114.2(5) . . ?
O5 C16 H13A 108.7 . . ?
C15 C16 H13A 108.7 . . ?
O5 C16 H13B 108.7 . . ?
C15 C16 H13B 108.7 . . ?
H13A C16 H13B 107.6 . . ?
C20 C17 C18 116.7(6) . . ?
C20 C17 N1 114.6(5) . . ?
C18 C17 N1 113.6(5) . . ?
C20 C17 C19 101.3(6) . . ?
C18 C17 C19 102.4(5) . . ?
N1 C17 C19 105.9(5) . . ?
C17 C18 H1A 109.5 . . ?
C17 C18 H1B 109.5 . . ?
H1A C18 H1B 109.5 . . ?
C17 C18 H1C 109.5 . . ?
H1A C18 H1C 109.5 . . ?
H1B C18 H1C 109.5 . . ?
C17 C19 H22A 109.5 . . ?
C17 C19 H22B 109.5 . . ?
H22A C19 H22B 109.5 . . ?
C17 C19 H22C 109.5 . . ?
H22A C19 H22C 109.5 . . ?
H22B C19 H22C 109.5 . . ?
C17 C20 H19A 109.5 . . ?
C17 C20 H19B 109.5 . . ?
H19A C20 H19B 109.5 . . ?
C17 C20 H19C 109.5 . . ?
H19A C20 H19C 109.5 . . ?
H19B C20 H19C 109.5 . . ?
O7 C21 O6 125.4(4) . . ?
O7 C21 C22 119.4(4) . . ?
O6 C21 C22 115.2(4) . . ?
C27 C22 C23 118.4(5) . . ?
C27 C22 C21 121.5(4) . . ?
C23 C22 C21 120.1(4) . . ?
C24 C23 C22 120.3(6) . . ?
C24 C23 H17 119.8 . . ?
C22 C23 H17 119.8 . . ?
C25 C24 C23 121.8(7) . . ?
C25 C24 H21 119.1 . . ?
C23 C24 H21 119.1 . . ?
C24 C25 C26 117.8(6) . . ?
C24 C25 C28 122.0(8) . . ?
C26 C25 C28 120.1(7) . . ?
C27 C26 C25 120.7(6) . . ?
C27 C26 H6 119.6 . . ?
C25 C26 H6 119.6 . . ?
C26 C27 C22 120.9(5) . . ?
C26 C27 H14 119.5 . . ?
C22 C27 H14 119.5 . . ?
C30' C28 C29 131.6(12) . . ?
C30' C28 C31' 124.1(13) . . ?
C29 C28 C31' 56.0(12) . . ?
C30' C28 C30 21.2(9) . . ?
C29 C28 C30 117.5(14) . . ?
C31' C28 C30 134.4(14) . . ?
C30' C28 C29' 98.3(16) . . ?
C29 C28 C29' 45.3(16) . . ?
C31' C28 C29' 99.3(18) . . ?
C30 C28 C29' 78.4(17) . . ?
C30' C28 C31 81(2) . . ?
C29 C28 C31 110(2) . . ?
C31' C28 C31 55.4(18) . . ?
C30 C28 C31 102(2) . . ?
C29' C28 C31 145(2) . . ?
C30' C28 C25 111.7(9) . . ?
C29 C28 C25 110.0(12) . . ?
C31' C28 C25 112.4(11) . . ?
C30 C28 C25 111.5(10) . . ?
C29' C28 C25 107.7(17) . . ?
C31 C28 C25 105.1(19) . . ?
C28 C29 H35A 109.5 . . ?
C28 C29 H35B 109.5 . . ?
C28 C29 H35C 109.5 . . ?
C28 C29 H3'3 91.6 . . ?
H35A C29 H3'3 91.5 . . ?
H35B C29 H3'3 32.6 . . ?
H35C C29 H3'3 142.1 . . ?
C28 C29' H1'1 109.5 . . ?
C28 C29' H1'2 109.5 . . ?
C28 C29' H1'3 109.5 . . ?
C28 C30 H47A 109.5 . . ?
C28 C30 H47B 109.5 . . ?
C28 C30 H47C 109.5 . . ?
C28 C30' H2'1 109.5 . . ?
C28 C30' H2'2 109.5 . . ?
C28 C30' H2'3 109.5 . . ?
C28 C31 H36A 109.2 . . ?
C28 C31 H36B 109.0 . . ?
H36A C31 H36B 106.7 . . ?
C28 C31 H36C 111.8 . . ?
H36A C31 H36C 110.1 . . ?
H36B C31 H36C 109.9 . . ?
C28 C31 H3'2 101.3 . . ?
H36A C31 H3'2 40.2 . . ?
H36B C31 H3'2 72.6 . . ?
H36C C31 H3'2 143.0 . . ?
C28 C31' H36A 87.2 . . ?
C28 C31' H36B 90.4 . . ?
H36A C31' H36B 65.6 . . ?
C28 C31' H3'1 109.5 . . ?
H36A C31' H3'1 126.0 . . ?
H36B C31' H3'1 63.4 . . ?
C28 C31' H3'2 108.7 . . ?
H36A C31' H3'2 23.4 . . ?
H36B C31' H3'2 58.1 . . ?
H3'1 C31' H3'2 108.3 . . ?
C28 C31' H3'3 110.3 . . ?
H36A C31' H3'3 110.4 . . ?
H36B C31' H3'3 159.0 . . ?
H3'1 C31' H3'3 110.6 . . ?
H3'2 C31' H3'3 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.913
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.913
_refine_diff_density_max         2.369
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.137
