# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_complex5
_database_code_depnum_ccdc_archive 'CCDC 1550309'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C44 H52 N24 O14, Ho H16 O8, 2(N O3), Cl, 10(H2 O)'
_chemical_formula_sum            'C44 H88 Cl Ho N26 O38'
_chemical_formula_weight         1789.78

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'
Ho Ho -0.2175 4.6783 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.377(4)
_cell_length_b                   12.440(2)
_cell_length_c                   26.896(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.367(3)
_cell_angle_gamma                90.00
_cell_volume                     6973(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3688
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6983
_exptl_absorpt_correction_T_max  0.7558
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25745
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6785
_reflns_number_gt                6094
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.0819P)²+53.0214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6785
_refine_ls_number_parameters     502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1577
_refine_ls_wR_factor_gt          0.1528
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.3698(13) -0.4175(14) 0.0781(6) 0.381(17) Uani 0.50 1 d P . .
N13 N 0.4531(6) -0.3061(9) 0.4417(3) 0.104(3) Uani 1 1 d . . .
O9 O 0.5039(4) -0.2668(7) 0.4764(3) 0.110(3) Uani 1 1 d . . .
O10 O 0.4017(4) -0.2556(11) 0.4291(4) 0.134(4) Uani 1 1 d . . .
O11 O 0.4638(8) -0.3946(8) 0.4176(4) 0.175(6) Uani 1 1 d . . .
O1W O 0.5531(4) -0.2618(6) 0.2251(3) 0.0328(17) Uani 0.50 1 d P . .
O2W O 0.5211(9) -0.3410(10) 0.1763(6) 0.103(6) Uani 0.50 1 d P . .
O3W O 0.5287(4) -0.4707(6) 0.1796(3) 0.0343(18) Uani 0.50 1 d P . .
O4W O 0.5529(6) -0.5508(10) 0.2256(7) 0.085(4) Uani 0.50 1 d P . .
O5W O 0.4292(4) -0.5511(6) 0.2161(3) 0.0324(18) Uani 0.50 1 d P . .
O6W O 0.4188(7) -0.4815(10) 0.1754(6) 0.099(5) Uani 0.50 1 d P . .
O7W O 0.4208(4) -0.3344(6) 0.1724(3) 0.041(2) Uani 0.50 1 d P . .
O8W O 0.4275(6) -0.2671(9) 0.2219(7) 0.082(4) Uani 0.50 1 d P . .
Ho1 Ho 0.5000 -0.40641(2) 0.2500 0.02169(13) Uani 1 2 d S . .
C1 C 0.6874(3) -0.0634(4) 0.2546(3) 0.0376(14) Uani 1 1 d . . .
C2 C 0.7194(3) 0.0941(4) 0.2222(3) 0.0360(14) Uani 1 1 d . . .
C3 C 0.7507(3) 0.0920(4) 0.2863(3) 0.0340(13) Uani 1 1 d . . .
C4 C 0.6868(3) 0.2470(4) 0.2584(3) 0.0350(13) Uani 1 1 d . . .
C5 C 0.7398(3) -0.0512(5) 0.3525(3) 0.0426(15) Uani 1 1 d . . .
H5A H 0.7854 -0.0382 0.3727 0.051 Uiso 1 1 calc R . .
H5B H 0.7331 -0.1292 0.3500 0.051 Uiso 1 1 calc R . .
C6 C 0.7438(3) 0.2321(4) 0.3552(3) 0.0401(14) Uani 1 1 d . . .
H6A H 0.7389 0.3104 0.3530 0.048 Uiso 1 1 calc R . .
H6B H 0.7894 0.2163 0.3741 0.048 Uiso 1 1 calc R . .
C7 C 0.6520(3) -0.0593(5) 0.3869(3) 0.0386(14) Uani 1 1 d . . .
C8 C 0.7211(3) 0.0885(4) 0.4166(3) 0.0374(14) Uani 1 1 d . . .
C9 C 0.6690(3) 0.0904(4) 0.4443(2) 0.0376(14) Uani 1 1 d . . .
C10 C 0.6575(3) 0.2454(4) 0.3915(2) 0.0366(13) Uani 1 1 d . . .
C11 C 0.5831(3) -0.0517(5) 0.4392(3) 0.0420(15) Uani 1 1 d . . .
H11A H 0.5969 -0.0432 0.4780 0.050 Uiso 1 1 calc R . .
H11B H 0.5802 -0.1290 0.4316 0.050 Uiso 1 1 calc R . .
C12 C 0.5850(3) 0.2361(5) 0.4408(3) 0.0403(14) Uani 1 1 d . . .
H12A H 0.5977 0.2258 0.4794 0.048 Uiso 1 1 calc R . .
H12B H 0.5828 0.3137 0.4340 0.048 Uiso 1 1 calc R . .
C13 C 0.4699(3) -0.0617(5) 0.3798(3) 0.0381(14) Uani 1 1 d . A .
C14 C 0.4993(3) 0.0932(4) 0.4322(2) 0.0344(13) Uani 1 1 d . . .
C15 C 0.4251(3) 0.0957(4) 0.4003(3) 0.0365(13) Uani 1 1 d . A .
C16 C 0.4720(3) 0.2477(4) 0.3794(3) 0.0400(14) Uani 1 1 d . . .
C17 C 0.3504(3) -0.0486(5) 0.3424(3) 0.0464(16) Uani 1 1 d . . .
H17A H 0.3544 -0.1267 0.3400 0.056 Uiso 1 1 calc R . .
H17B H 0.3239 -0.0347 0.3638 0.056 Uiso 1 1 calc R . .
C18 C 0.3534(3) 0.2386(5) 0.3392(3) 0.0428(15) Uani 1 1 d . . .
H18A H 0.3266 0.2311 0.3608 0.051 Uiso 1 1 calc R A .
H18B H 0.3586 0.3156 0.3343 0.051 Uiso 1 1 calc R . .
C19 C 0.7677(4) 0.0979(6) 0.1943(4) 0.0540(19) Uani 1 1 d . . .
H19A H 0.7932 0.0326 0.2021 0.081 Uiso 1 1 calc R . .
H19B H 0.7956 0.1596 0.2070 0.081 Uiso 1 1 calc R . .
H19C H 0.7450 0.1038 0.1561 0.081 Uiso 1 1 calc R . .
C20 C 0.8237(3) 0.0888(5) 0.3090(4) 0.0507(18) Uani 1 1 d . . .
H20A H 0.8404 0.1551 0.3002 0.076 Uiso 1 1 calc R . .
H20B H 0.8386 0.0285 0.2938 0.076 Uiso 1 1 calc R . .
H20C H 0.8386 0.0809 0.3475 0.076 Uiso 1 1 calc R . .
C21 C 0.7900(4) 0.0834(6) 0.4554(4) 0.065(2) Uani 1 1 d . . .
H21A H 0.8000 0.1478 0.4773 0.097 Uiso 1 1 calc R . .
H21B H 0.8185 0.0782 0.4357 0.097 Uiso 1 1 calc R . .
H21C H 0.7956 0.0208 0.4782 0.097 Uiso 1 1 calc R . .
C22 C 0.6965(5) 0.0886(7) 0.5061(3) 0.067(2) Uani 1 1 d . . .
H22A H 0.7211 0.1535 0.5193 0.100 Uiso 1 1 calc R . .
H22B H 0.7240 0.0264 0.5184 0.100 Uiso 1 1 calc R . .
H22C H 0.6615 0.0849 0.5192 0.100 Uiso 1 1 calc R . .
N1 N 0.6824(2) -0.0067(4) 0.2108(2) 0.0385(12) Uani 1 1 d . . .
N2 N 0.7237(2) -0.0081(4) 0.2990(2) 0.0389(12) Uani 1 1 d . . .
N3 N 0.6799(2) 0.1909(3) 0.2123(2) 0.0366(11) Uani 1 1 d . . .
N4 N 0.7246(2) 0.1893(4) 0.3015(2) 0.0351(11) Uani 1 1 d . . .
N5 N 0.7021(2) -0.0049(4) 0.3819(2) 0.0389(12) Uani 1 1 d . . .
N6 N 0.6317(2) -0.0061(4) 0.4219(2) 0.0384(12) Uani 1 1 d . . .
N7 N 0.7077(2) 0.1901(4) 0.3864(2) 0.0387(12) Uani 1 1 d . . .
N8 N 0.6346(2) 0.1911(4) 0.4242(2) 0.0377(12) Uani 1 1 d . . .
N9 N 0.5199(2) -0.0047(4) 0.4145(2) 0.0352(11) Uani 1 1 d . A .
N10 N 0.4142(2) -0.0033(4) 0.3701(2) 0.0391(12) Uani 1 1 d . . .
N11 N 0.5217(2) 0.1909(4) 0.4147(2) 0.0355(11) Uani 1 1 d . A .
N12 N 0.4161(2) 0.1924(4) 0.3685(2) 0.0371(11) Uani 1 1 d . A .
O1 O 0.6656(2) -0.1546(3) 0.2546(2) 0.0529(13) Uani 1 1 d . . .
O2 O 0.6304(3) -0.1434(4) 0.3649(2) 0.0622(15) Uani 1 1 d . . .
O3 O 0.4735(3) -0.1499(4) 0.3616(2) 0.0576(14) Uani 1 1 d . . .
O4 O 0.6649(2) 0.3360(3) 0.2603(2) 0.0446(11) Uani 1 1 d . . .
O5 O 0.6404(3) 0.3354(4) 0.3729(2) 0.0535(12) Uani 1 1 d . . .
O6 O 0.4785(3) 0.3349(4) 0.3606(3) 0.0701(17) Uani 1 1 d . A .
O7 O 0.5182(5) 0.0892(7) 0.4881(3) 0.057(3) Uani 0.588(13) 1 d P A 1
O8 O 0.3847(5) 0.0914(9) 0.4293(4) 0.041(3) Uani 0.412(13) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N13 O10 1.245(14) . ?
N13 O9 1.276(12) . ?
N13 O11 1.343(14) . ?
O1W O8W 1.331(17) 2_655 ?
O1W O2W 1.588(18) . ?
O1W Ho1 2.382(7) . ?
O2W O3W 1.621(14) . ?
O2W Ho1 2.343(12) . ?
O3W O4W 1.525(18) . ?
O3W Ho1 2.349(7) . ?
O4W O5W 1.470(18) 2_655 ?
O4W Ho1 2.372(10) . ?
O5W O6W 1.349(17) . ?
O5W O4W 1.470(18) 2_655 ?
O5W Ho1 2.352(6) . ?
O6W Ho1 2.354(11) . ?
O7W O8W 1.533(18) . ?
O7W Ho1 2.368(7) . ?
O8W O1W 1.331(17) 2_655 ?
O8W Ho1 2.305(10) . ?
Ho1 O8W 2.305(10) 2_655 ?
Ho1 O2W 2.343(12) 2_655 ?
Ho1 O3W 2.349(7) 2_655 ?
Ho1 O5W 2.352(6) 2_655 ?
Ho1 O6W 2.354(11) 2_655 ?
Ho1 O7W 2.368(7) 2_655 ?
C1 O1 1.234(7) . ?
C1 N1 1.343(9) . ?
C1 N2 1.362(8) . ?
C2 N3 1.460(7) . ?
C2 N1 1.472(7) . ?
C2 C19 1.524(9) . ?
C2 C3 1.607(10) . ?
C3 N4 1.466(7) . ?
C3 N2 1.477(7) . ?
C3 C20 1.522(8) . ?
C4 O4 1.220(7) . ?
C4 N4 1.364(8) . ?
C4 N3 1.380(8) . ?
C5 N2 1.451(9) . ?
C5 N5 1.468(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.449(8) . ?
C6 N7 1.455(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.212(8) . ?
C7 N6 1.358(9) . ?
C7 N5 1.358(8) . ?
C8 N5 1.455(7) . ?
C8 N7 1.473(7) . ?
C8 C21 1.516(9) . ?
C8 C9 1.596(10) . ?
C9 N6 1.461(7) . ?
C9 N8 1.467(7) . ?
C9 C22 1.547(10) . ?
C10 O5 1.230(7) . ?
C10 N8 1.348(8) . ?
C10 N7 1.368(8) . ?
C11 N6 1.444(8) . ?
C11 N9 1.449(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.447(8) . ?
C12 N8 1.450(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.217(8) . ?
C13 N9 1.366(8) . ?
C13 N10 1.381(8) . ?
C14 O7 1.404(10) . ?
C14 N9 1.443(7) . ?
C14 N11 1.458(7) . ?
C14 C15 1.566(9) . ?
C15 O8 1.396(12) . ?
C15 N12 1.447(7) . ?
C15 N10 1.447(7) . ?
C16 O6 1.228(7) . ?
C16 N12 1.362(8) . ?
C16 N11 1.365(8) . ?
C17 N1 1.446(9) 2_655 ?
C17 N10 1.462(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N3 1.439(8) 2_655 ?
C18 N12 1.455(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N1 C17 1.446(9) 2_655 ?
N3 C18 1.439(8) 2_655 ?

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
O10 N13 O9 119.6(11) . . ?
O10 N13 O11 126.3(12) . . ?
O9 N13 O11 113.5(13) . . ?
O8W O1W O2W 136.6(8) 2_655 . ?
O8W O1W Ho1 70.3(5) 2_655 . ?
O2W O1W Ho1 69.0(5) . . ?
O1W O2W O3W 124.4(11) . . ?
O1W O2W Ho1 71.7(6) . . ?
O3W O2W Ho1 70.0(5) . . ?
O4W O3W O2W 133.9(9) . . ?
O4W O3W Ho1 72.0(5) . . ?
O2W O3W Ho1 69.6(5) . . ?
O5W O4W O3W 138.1(9) 2_655 . ?
O5W O4W Ho1 71.1(5) 2_655 . ?
O3W O4W Ho1 70.3(5) . . ?
O6W O5W O4W 139.8(9) . 2_655 ?
O6W O5W Ho1 73.4(5) . . ?
O4W O5W Ho1 72.6(5) 2_655 . ?
O5W O6W Ho1 73.2(6) . . ?
O8W O7W Ho1 68.6(5) . . ?
O1W O8W O7W 147.9(9) 2_655 . ?
O1W O8W Ho1 76.7(6) 2_655 . ?
O7W O8W Ho1 73.1(5) . . ?
O8W Ho1 O8W 82.5(7) 2_655 . ?
O8W Ho1 O2W 78.2(5) 2_655 2_655 ?
O8W Ho1 O2W 71.4(6) . 2_655 ?
O8W Ho1 O2W 71.4(6) 2_655 . ?
O8W Ho1 O2W 78.2(5) . . ?
O2W Ho1 O2W 139.4(6) 2_655 . ?
O8W Ho1 O3W 111.0(5) 2_655 2_655 ?
O8W Ho1 O3W 98.8(4) . 2_655 ?
O2W Ho1 O3W 40.4(4) 2_655 2_655 ?
O2W Ho1 O3W 176.1(5) . 2_655 ?
O8W Ho1 O3W 98.8(4) 2_655 . ?
O8W Ho1 O3W 111.0(5) . . ?
O2W Ho1 O3W 176.1(5) 2_655 . ?
O2W Ho1 O3W 40.4(4) . . ?
O3W Ho1 O3W 140.2(4) 2_655 . ?
O8W Ho1 O5W 175.6(4) 2_655 . ?
O8W Ho1 O5W 98.9(4) . . ?
O2W Ho1 O5W 106.2(4) 2_655 . ?
O2W Ho1 O5W 104.6(5) . . ?
O3W Ho1 O5W 73.0(3) 2_655 . ?
O3W Ho1 O5W 76.7(3) . . ?
O8W Ho1 O5W 98.9(4) 2_655 2_655 ?
O8W Ho1 O5W 175.6(4) . 2_655 ?
O2W Ho1 O5W 104.6(5) 2_655 2_655 ?
O2W Ho1 O5W 106.2(4) . 2_655 ?
O3W Ho1 O5W 76.7(3) 2_655 2_655 ?
O3W Ho1 O5W 73.0(3) . 2_655 ?
O5W Ho1 O5W 80.1(4) . 2_655 ?
O8W Ho1 O6W 144.1(6) 2_655 . ?
O8W Ho1 O6W 77.7(5) . . ?
O2W Ho1 O6W 121.8(6) 2_655 . ?
O2W Ho1 O6W 75.4(7) . . ?
O3W Ho1 O6W 101.5(5) 2_655 . ?
O3W Ho1 O6W 62.0(5) . . ?
O5W Ho1 O6W 33.3(4) . . ?
O5W Ho1 O6W 103.2(4) 2_655 . ?
O8W Ho1 O6W 77.7(5) 2_655 2_655 ?
O8W Ho1 O6W 144.1(6) . 2_655 ?
O2W Ho1 O6W 75.4(7) 2_655 2_655 ?
O2W Ho1 O6W 121.8(6) . 2_655 ?
O3W Ho1 O6W 62.0(5) 2_655 2_655 ?
O3W Ho1 O6W 101.5(5) . 2_655 ?
O5W Ho1 O6W 103.2(4) . 2_655 ?
O5W Ho1 O6W 33.3(4) 2_655 2_655 ?
O6W Ho1 O6W 133.3(6) . 2_655 ?
O8W Ho1 O7W 38.3(5) 2_655 2_655 ?
O8W Ho1 O7W 102.5(5) . 2_655 ?
O2W Ho1 O7W 55.9(5) 2_655 2_655 ?
O2W Ho1 O7W 107.3(5) . 2_655 ?
O3W Ho1 O7W 75.8(3) 2_655 2_655 ?
O3W Ho1 O7W 120.1(3) . 2_655 ?
O5W Ho1 O7W 144.5(3) . 2_655 ?
O5W Ho1 O7W 76.4(3) 2_655 2_655 ?
O6W Ho1 O7W 177.3(5) . 2_655 ?
O6W Ho1 O7W 45.7(4) 2_655 2_655 ?
O8W Ho1 O7W 102.5(5) 2_655 . ?
O8W Ho1 O7W 38.3(5) . . ?
O2W Ho1 O7W 107.3(5) 2_655 . ?
O2W Ho1 O7W 55.9(5) . . ?
O3W Ho1 O7W 120.1(3) 2_655 . ?
O3W Ho1 O7W 75.8(3) . . ?
O5W Ho1 O7W 76.4(3) . . ?
O5W Ho1 O7W 144.5(3) 2_655 . ?
O6W Ho1 O7W 45.7(4) . . ?
O6W Ho1 O7W 177.3(5) 2_655 . ?
O7W Ho1 O7W 135.5(4) 2_655 . ?
O1 C1 N1 125.1(6) . . ?
O1 C1 N2 125.1(6) . . ?
N1 C1 N2 109.7(5) . . ?
N3 C2 N1 114.0(5) . . ?
N3 C2 C19 112.0(5) . . ?
N1 C2 C19 111.7(5) . . ?
N3 C2 C3 102.0(5) . . ?
N1 C2 C3 101.7(5) . . ?
C19 C2 C3 114.8(5) . . ?
N4 C3 N2 113.1(5) . . ?
N4 C3 C20 112.8(5) . . ?
N2 C3 C20 110.8(5) . . ?
N4 C3 C2 102.9(4) . . ?
N2 C3 C2 102.0(4) . . ?
C20 C3 C2 114.5(6) . . ?
O4 C4 N4 125.1(6) . . ?
O4 C4 N3 125.6(6) . . ?
N4 C4 N3 109.3(5) . . ?
N2 C5 N5 113.9(5) . . ?
N2 C5 H5A 108.8 . . ?
N5 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
N5 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N4 C6 N7 114.6(5) . . ?
N4 C6 H6A 108.6 . . ?
N7 C6 H6A 108.6 . . ?
N4 C6 H6B 108.6 . . ?
N7 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
O2 C7 N6 125.9(6) . . ?
O2 C7 N5 125.2(6) . . ?
N6 C7 N5 108.9(5) . . ?
N5 C8 N7 112.1(5) . . ?
N5 C8 C21 113.2(6) . . ?
N7 C8 C21 111.5(5) . . ?
N5 C8 C9 102.7(5) . . ?
N7 C8 C9 102.1(5) . . ?
C21 C8 C9 114.3(6) . . ?
N6 C9 N8 114.0(5) . . ?
N6 C9 C22 112.0(6) . . ?
N8 C9 C22 111.0(6) . . ?
N6 C9 C8 101.6(5) . . ?
N8 C9 C8 102.3(5) . . ?
C22 C9 C8 115.4(6) . . ?
O5 C10 N8 125.9(6) . . ?
O5 C10 N7 124.2(6) . . ?
N8 C10 N7 109.6(5) . . ?
N6 C11 N9 114.6(5) . . ?
N6 C11 H11A 108.6 . . ?
N9 C11 H11A 108.6 . . ?
N6 C11 H11B 108.6 . . ?
N9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N11 C12 N8 115.2(5) . . ?
N11 C12 H12A 108.5 . . ?
N8 C12 H12A 108.5 . . ?
N11 C12 H12B 108.5 . . ?
N8 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
O3 C13 N9 125.8(6) . . ?
O3 C13 N10 125.9(6) . . ?
N9 C13 N10 108.3(5) . . ?
O7 C14 N9 108.3(6) . . ?
O7 C14 N11 111.8(6) . . ?
N9 C14 N11 114.1(5) . . ?
O7 C14 C15 115.7(6) . . ?
N9 C14 C15 103.8(5) . . ?
N11 C14 C15 103.0(4) . . ?
O8 C15 N12 112.6(6) . . ?
O8 C15 N10 105.7(6) . . ?
N12 C15 N10 114.6(5) . . ?
O8 C15 C14 117.8(7) . . ?
N12 C15 C14 103.5(5) . . ?
N10 C15 C14 102.7(5) . . ?
O6 C16 N12 126.4(6) . . ?
O6 C16 N11 123.7(6) . . ?
N12 C16 N11 109.9(5) . . ?
N1 C17 N10 114.4(5) 2_655 . ?
N1 C17 H17A 108.7 2_655 . ?
N10 C17 H17A 108.7 . . ?
N1 C17 H17B 108.7 2_655 . ?
N10 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N3 C18 N12 114.7(5) 2_655 . ?
N3 C18 H18A 108.6 2_655 . ?
N12 C18 H18A 108.6 . . ?
N3 C18 H18B 108.6 2_655 . ?
N12 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C17 121.9(5) . 2_655 ?
C1 N1 C2 113.8(5) . . ?
C17 N1 C2 123.9(6) 2_655 . ?
C1 N2 C5 122.3(5) . . ?
C1 N2 C3 112.7(5) . . ?
C5 N2 C3 124.5(5) . . ?
C4 N3 C18 120.3(5) . 2_655 ?
C4 N3 C2 113.0(5) . . ?
C18 N3 C2 125.6(6) 2_655 . ?
C4 N4 C6 121.5(5) . . ?
C4 N4 C3 112.5(5) . . ?
C6 N4 C3 125.3(5) . . ?
C7 N5 C8 113.1(5) . . ?
C7 N5 C5 121.0(5) . . ?
C8 N5 C5 124.7(5) . . ?
C7 N6 C11 120.8(5) . . ?
C7 N6 C9 113.7(5) . . ?
C11 N6 C9 125.0(6) . . ?
C10 N7 C6 121.7(5) . . ?
C10 N7 C8 112.6(5) . . ?
C6 N7 C8 125.7(5) . . ?
C10 N8 C12 121.4(5) . . ?
C10 N8 C9 113.4(5) . . ?
C12 N8 C9 124.9(5) . . ?
C13 N9 C14 112.5(5) . . ?
C13 N9 C11 121.6(5) . . ?
C14 N9 C11 124.4(5) . . ?
C13 N10 C15 112.7(5) . . ?
C13 N10 C17 122.6(5) . . ?
C15 N10 C17 123.3(5) . . ?
C16 N11 C12 122.8(5) . . ?
C16 N11 C14 111.6(5) . . ?
C12 N11 C14 123.9(5) . . ?
C16 N12 C15 111.9(5) . . ?
C16 N12 C18 123.1(5) . . ?
C15 N12 C18 123.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.959
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.142

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.250 0.000 158 59 ' '
2 0.750 0.250 0.000 158 59 ' '
3 0.500 0.093 0.250 118 39 ' '
4 0.750 -0.250 0.500 158 59 ' '
5 0.250 0.250 0.500 158 59 ' '
6 0.500 -0.093 0.750 118 39 ' '
7 0.000 0.407 0.750 118 39 ' '
8 1.000 0.593 0.250 118 39 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex3
_database_code_depnum_ccdc_archive 'CCDC 1550307'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O14, Tb H16 O8, Cl3, 10(H2 O)'
_chemical_formula_sum            'C44 H88 Cl3 N24 O32 Tb'
_chemical_formula_weight         1730.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.215(5)
_cell_length_b                   12.391(5)
_cell_length_c                   14.675(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.468(5)
_cell_angle_gamma                90.00
_cell_volume                     3831(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_T_max  0.7590
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17233
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.82
_reflns_number_total             4713
_reflns_number_gt                4604
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.1096P)²+1.2036P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4713
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1479
_refine_ls_wR_factor_gt          0.1460
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.133
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.4108(6) 0.0000 0.5622(8) 0.192(6) Uani 0.50 2 d SP . .
Cl2 Cl 0.2457(12) 0.2009(11) 0.5989(15) 0.55(2) Uani 0.50 1 d P . .
O1W O 0.0814(3) 0.4317(5) 0.1376(5) 0.0497(15) Uani 0.50 1 d P . .
O2W O 0.0711(3) 0.3524(5) 0.0537(5) 0.0434(13) Uani 0.50 1 d P . .
O3W O 0.0505(3) 0.3508(5) -0.0491(5) 0.0453(14) Uani 0.50 1 d P . .
O4W O 0.0274(4) 0.4343(5) -0.1321(5) 0.0505(16) Uani 0.50 1 d P . .
Tb1 Tb 0.0000 0.5000 0.0000 0.02573(14) Uani 1 4 d S . .
C1 C 0.1878(2) 0.1546(3) 0.0096(5) 0.0563(13) Uani 1 1 d . . .
C2 C 0.2267(3) 0.0000 -0.0435(8) 0.062(2) Uani 1 2 d S . .
C3 C 0.2483(3) 0.0000 0.0653(8) 0.064(2) Uani 1 2 d S . .
C4 C 0.2301(3) 0.1421(4) 0.1851(5) 0.0685(16) Uani 1 1 d . . .
H4A H 0.2745 0.1298 0.2232 0.082 Uiso 1 1 calc R . .
H4B H 0.2233 0.2203 0.1798 0.082 Uiso 1 1 calc R . .
C5 C 0.1394(3) 0.1515(4) 0.2443(4) 0.0603(14) Uani 1 1 d . . .
C6 C 0.2036(4) 0.0000 0.2944(6) 0.060(2) Uani 1 2 d S . .
C7 C 0.1516(4) 0.0000 0.3414(5) 0.062(2) Uani 1 2 d S . .
C8 C 0.0663(4) 0.1439(4) 0.3365(4) 0.0703(16) Uani 1 1 d . . .
H8A H 0.0781 0.1352 0.4063 0.084 Uiso 1 1 calc R . .
H8B H 0.0640 0.2215 0.3227 0.084 Uiso 1 1 calc R . .
C9 C -0.0438(3) 0.1547(4) 0.2350(4) 0.0619(14) Uani 1 1 d . A .
C10 C -0.0177(5) 0.0000 0.3264(5) 0.058(2) Uani 1 2 d S . .
C11 C -0.0866(5) 0.0000 0.2755(7) 0.068(3) Uani 1 2 d S . .
C12 C 0.1603(3) 0.1421(4) -0.1646(5) 0.0656(16) Uani 1 1 d . . .
H12A H 0.1891 0.1286 -0.2020 0.079 Uiso 1 1 calc R . .
H12B H 0.1563 0.2205 -0.1596 0.079 Uiso 1 1 calc R . .
C13 C 0.2821(5) 0.0000 -0.0859(11) 0.095(4) Uani 1 2 d S . .
H13A H 0.3062 0.0663 -0.0680 0.142 Uiso 0.50 1 calc PR . .
H13B H 0.2653 -0.0050 -0.1553 0.142 Uiso 0.50 1 calc PR . .
H13C H 0.3095 -0.0613 -0.0609 0.142 Uiso 0.50 1 calc PR . .
C14 C 0.3208(4) 0.0000 0.1140(12) 0.116(6) Uani 1 2 d S . .
H14A H 0.3386 -0.0660 0.0978 0.175 Uiso 0.50 1 calc PR . .
H14B H 0.3303 0.0043 0.1831 0.175 Uiso 0.50 1 calc PR . .
H14C H 0.3392 0.0617 0.0918 0.175 Uiso 0.50 1 calc PR . .
C15 C 0.2676(7) 0.0000 0.3687(11) 0.154(8) Uani 1 2 d S . .
H15A H 0.2730 0.0656 0.4064 0.230 Uiso 0.50 1 calc PR . .
H15B H 0.3000 -0.0036 0.3374 0.230 Uiso 1 2 calc SR . .
H15C H 0.2714 -0.0621 0.4104 0.230 Uiso 0.50 1 calc PR . .
C16 C 0.1764(8) 0.0000 0.4511(7) 0.129(6) Uani 1 2 d S . .
H16A H 0.2006 0.0653 0.4735 0.193 Uiso 0.50 1 calc PR . .
H16B H 0.2033 -0.0625 0.4734 0.193 Uiso 0.50 1 calc PR . .
H16C H 0.1408 -0.0028 0.4760 0.193 Uiso 1 2 calc SR . .
N1 N 0.1885(2) 0.0986(3) -0.0693(4) 0.0604(12) Uani 1 1 d . . .
N2 N 0.21961(19) 0.0981(3) 0.0884(4) 0.0598(12) Uani 1 1 d . . .
N3 N 0.1904(2) 0.0975(3) 0.2358(4) 0.0584(11) Uani 1 1 d . . .
N4 N 0.1156(2) 0.0975(3) 0.3043(3) 0.0568(11) Uani 1 1 d . . .
N5 N 0.0044(3) 0.0976(3) 0.2931(3) 0.0585(11) Uani 1 1 d . A .
N6 N -0.0988(3) 0.0981(3) 0.2161(4) 0.0637(13) Uani 1 1 d . . .
O1 O 0.16447(18) 0.2452(3) 0.0088(3) 0.0633(10) Uani 1 1 d . . .
O2 O 0.1196(3) 0.2378(3) 0.2041(4) 0.0878(15) Uani 1 1 d . . .
O3 O -0.0392(3) 0.2465(4) 0.2054(4) 0.0925(16) Uani 1 1 d . . .
O4 O -0.0025(8) 0.0000 0.4228(8) 0.095(5) Uani 0.622(16) 2 d SP A 1
O5 O -0.1225(11) 0.0000 0.3396(14) 0.088(8) Uani 0.378(16) 2 d SP . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W O2W 1.534(9) . ?
O1W O1W 1.693(12) 6_565 ?
O1W Tb1 2.397(6) . ?
O2W O3W 1.431(9) . ?
O2W Tb1 2.382(5) . ?
O3W O4W 1.556(9) . ?
O3W Tb1 2.388(5) . ?
O4W O4W 1.628(12) 6_565 ?
O4W Tb1 2.353(6) . ?
Tb1 O4W 2.353(6) 6_565 ?
Tb1 O4W 2.353(6) 5_565 ?
Tb1 O4W 2.353(6) 2 ?
Tb1 O2W 2.382(5) 2 ?
Tb1 O2W 2.382(5) 6_565 ?
Tb1 O2W 2.382(5) 5_565 ?
Tb1 O3W 2.388(5) 2 ?
Tb1 O3W 2.388(5) 5_565 ?
Tb1 O3W 2.388(5) 6_565 ?
C1 O1 1.235(5) . ?
C1 N2 1.345(8) . ?
C1 N1 1.353(8) . ?
C2 N1 1.468(6) 6 ?
C2 N1 1.468(6) . ?
C2 C3 1.516(14) . ?
C2 C13 1.543(9) . ?
C3 N2 1.462(6) . ?
C3 N2 1.462(6) 6 ?
C3 C14 1.541(10) . ?
C4 N3 1.434(8) . ?
C4 N2 1.467(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.233(6) . ?
C5 N4 1.342(8) . ?
C5 N3 1.354(8) . ?
C6 N3 1.457(6) 6 ?
C6 N3 1.457(6) . ?
C6 C15 1.492(11) . ?
C6 C7 1.521(14) . ?
C7 N4 1.456(6) 6 ?
C7 N4 1.456(6) . ?
C7 C16 1.527(11) . ?
C8 N5 1.440(8) . ?
C8 N4 1.443(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.234(6) . ?
C9 N5 1.339(8) . ?
C9 N6 1.359(8) . ?
C10 O4 1.345(12) . ?
C10 N5 1.447(6) 6 ?
C10 N5 1.447(6) . ?
C10 C11 1.476(14) . ?
C11 O5 1.413(13) . ?
C11 N6 1.469(6) 6 ?
C11 N6 1.469(6) . ?
C12 N1 1.443(8) . ?
C12 N6 1.444(8) 2 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
N6 C12 1.444(8) 2 ?

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
O2W O1W O1W 129.8(3) . 6_565 ?
O2W O1W Tb1 70.7(3) . . ?
O1W O1W Tb1 69.33(14) 6_565 . ?
O3W O2W O1W 140.4(5) . . ?
O3W O2W Tb1 72.8(3) . . ?
O1W O2W Tb1 71.8(3) . . ?
O2W O3W O4W 137.1(5) . . ?
O2W O3W Tb1 72.3(3) . . ?
O4W O3W Tb1 69.6(3) . . ?
O3W O4W O4W 131.7(3) . 6_565 ?
O3W O4W Tb1 72.1(3) . . ?
O4W O4W Tb1 69.76(14) 6_565 . ?
O4W Tb1 O4W 40.5(3) 6_565 . ?
O4W Tb1 O4W 139.5(3) 6_565 5_565 ?
O4W Tb1 O4W 180.0(3) . 5_565 ?
O4W Tb1 O4W 180.000(1) 6_565 2 ?
O4W Tb1 O4W 139.5(3) . 2 ?
O4W Tb1 O4W 40.5(3) 5_565 2 ?
O4W Tb1 O2W 108.1(2) 6_565 2 ?
O4W Tb1 O2W 77.2(2) . 2 ?
O4W Tb1 O2W 102.8(2) 5_565 2 ?
O4W Tb1 O2W 71.9(2) 2 2 ?
O4W Tb1 O2W 71.9(2) 6_565 6_565 ?
O4W Tb1 O2W 102.8(2) . 6_565 ?
O4W Tb1 O2W 77.2(2) 5_565 6_565 ?
O4W Tb1 O2W 108.1(2) 2 6_565 ?
O2W Tb1 O2W 180.0(3) 2 6_565 ?
O4W Tb1 O2W 77.2(2) 6_565 5_565 ?
O4W Tb1 O2W 108.1(2) . 5_565 ?
O4W Tb1 O2W 71.9(2) 5_565 5_565 ?
O4W Tb1 O2W 102.8(2) 2 5_565 ?
O2W Tb1 O2W 100.3(3) 2 5_565 ?
O2W Tb1 O2W 79.7(3) 6_565 5_565 ?
O4W Tb1 O2W 102.8(2) 6_565 . ?
O4W Tb1 O2W 71.9(2) . . ?
O4W Tb1 O2W 108.1(2) 5_565 . ?
O4W Tb1 O2W 77.2(2) 2 . ?
O2W Tb1 O2W 79.7(3) 2 . ?
O2W Tb1 O2W 100.3(3) 6_565 . ?
O2W Tb1 O2W 180.0(3) 5_565 . ?
O4W Tb1 O3W 141.7(2) 6_565 2 ?
O4W Tb1 O3W 104.4(2) . 2 ?
O4W Tb1 O3W 75.6(2) 5_565 2 ?
O4W Tb1 O3W 38.3(2) 2 2 ?
O2W Tb1 O3W 34.9(2) 2 2 ?
O2W Tb1 O3W 145.1(2) 6_565 2 ?
O2W Tb1 O3W 111.6(2) 5_565 2 ?
O2W Tb1 O3W 68.4(2) . 2 ?
O4W Tb1 O3W 104.4(2) 6_565 5_565 ?
O4W Tb1 O3W 141.7(2) . 5_565 ?
O4W Tb1 O3W 38.3(2) 5_565 5_565 ?
O4W Tb1 O3W 75.6(2) 2 5_565 ?
O2W Tb1 O3W 111.6(2) 2 5_565 ?
O2W Tb1 O3W 68.4(2) 6_565 5_565 ?
O2W Tb1 O3W 34.9(2) 5_565 5_565 ?
O2W Tb1 O3W 145.1(2) . 5_565 ?
O3W Tb1 O3W 101.4(3) 2 5_565 ?
O4W Tb1 O3W 75.6(2) 6_565 . ?
O4W Tb1 O3W 38.3(2) . . ?
O4W Tb1 O3W 141.7(2) 5_565 . ?
O4W Tb1 O3W 104.4(2) 2 . ?
O2W Tb1 O3W 68.4(2) 2 . ?
O2W Tb1 O3W 111.6(2) 6_565 . ?
O2W Tb1 O3W 145.1(2) 5_565 . ?
O2W Tb1 O3W 34.9(2) . . ?
O3W Tb1 O3W 78.6(3) 2 . ?
O3W Tb1 O3W 180.0(3) 5_565 . ?
O4W Tb1 O3W 38.3(2) 6_565 6_565 ?
O4W Tb1 O3W 75.6(2) . 6_565 ?
O4W Tb1 O3W 104.4(2) 5_565 6_565 ?
O4W Tb1 O3W 141.7(2) 2 6_565 ?
O2W Tb1 O3W 145.1(2) 2 6_565 ?
O2W Tb1 O3W 34.9(2) 6_565 6_565 ?
O2W Tb1 O3W 68.4(2) 5_565 6_565 ?
O2W Tb1 O3W 111.6(2) . 6_565 ?
O3W Tb1 O3W 180.0(3) 2 6_565 ?
O3W Tb1 O3W 78.6(3) 5_565 6_565 ?
O3W Tb1 O3W 101.4(3) . 6_565 ?
O1 C1 N2 125.9(6) . . ?
O1 C1 N1 125.2(6) . . ?
N2 C1 N1 108.9(4) . . ?
N1 C2 N1 112.7(6) 6 . ?
N1 C2 C3 103.6(5) 6 . ?
N1 C2 C3 103.6(5) . . ?
N1 C2 C13 111.5(5) 6 . ?
N1 C2 C13 111.5(5) . . ?
C3 C2 C13 113.5(8) . . ?
N2 C3 N2 112.5(6) . 6 ?
N2 C3 C2 103.2(5) . . ?
N2 C3 C2 103.2(5) 6 . ?
N2 C3 C14 111.2(5) . . ?
N2 C3 C14 111.2(5) 6 . ?
C2 C3 C14 115.1(9) . . ?
N3 C4 N2 115.0(4) . . ?
N3 C4 H4A 108.5 . . ?
N2 C4 H4A 108.5 . . ?
N3 C4 H4B 108.5 . . ?
N2 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N4 126.2(6) . . ?
O2 C5 N3 124.6(6) . . ?
N4 C5 N3 109.2(4) . . ?
N3 C6 N3 111.9(6) 6 . ?
N3 C6 C15 113.4(5) 6 . ?
N3 C6 C15 113.4(5) . . ?
N3 C6 C7 103.1(5) 6 . ?
N3 C6 C7 103.1(5) . . ?
C15 C6 C7 110.7(10) . . ?
N4 C7 N4 112.1(6) 6 . ?
N4 C7 C6 103.7(5) 6 . ?
N4 C7 C6 103.7(5) . . ?
N4 C7 C16 111.5(5) 6 . ?
N4 C7 C16 111.5(5) . . ?
C6 C7 C16 114.0(9) . . ?
N5 C8 N4 114.5(4) . . ?
N5 C8 H8A 108.6 . . ?
N4 C8 H8A 108.6 . . ?
N5 C8 H8B 108.6 . . ?
N4 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
O3 C9 N5 125.0(6) . . ?
O3 C9 N6 125.0(6) . . ?
N5 C9 N6 110.0(5) . . ?
O4 C10 N5 110.9(5) . 6 ?
O4 C10 N5 110.9(5) . . ?
N5 C10 N5 113.4(6) 6 . ?
O4 C10 C11 114.0(9) . . ?
N5 C10 C11 103.7(5) 6 . ?
N5 C10 C11 103.7(5) . . ?
O5 C11 N6 111.0(7) . 6 ?
O5 C11 N6 111.0(6) . . ?
N6 C11 N6 111.6(7) 6 . ?
O5 C11 C10 112.1(12) . . ?
N6 C11 C10 105.4(5) 6 . ?
N6 C11 C10 105.4(5) . . ?
N1 C12 N6 114.5(4) . 2 ?
N1 C12 H12A 108.6 . . ?
N6 C12 H12A 108.6 2 . ?
N1 C12 H12B 108.6 . . ?
N6 C12 H12B 108.6 2 . ?
H12A C12 H12B 107.6 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 H15A 109.5 . . ?
C6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C16 H16A 109.5 . . ?
C7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C12 121.2(4) . . ?
C1 N1 C2 111.7(6) . . ?
C12 N1 C2 126.7(6) . . ?
C1 N2 C3 112.5(6) . . ?
C1 N2 C4 121.2(4) . . ?
C3 N2 C4 125.8(6) . . ?
C5 N3 C4 121.8(4) . . ?
C5 N3 C6 112.0(6) . . ?
C4 N3 C6 125.7(6) . . ?
C5 N4 C8 120.9(4) . . ?
C5 N4 C7 112.0(6) . . ?
C8 N4 C7 126.3(6) . . ?
C9 N5 C8 122.0(5) . . ?
C9 N5 C10 111.7(6) . . ?
C8 N5 C10 124.2(6) . . ?
C9 N6 C12 123.6(4) . 2 ?
C9 N6 C11 108.8(6) . . ?
C12 N6 C11 126.0(6) 2 . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.82
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.624
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.149

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 117 26 ' '
2 0.500 0.000 0.500 241 63 ' '
3 0.685 0.000 0.299 9 5 ' '
4 0.315 0.000 0.701 9 5 ' '
5 1.000 0.500 0.500 241 63 ' '
6 0.500 0.500 0.000 117 26 ' '
7 0.185 0.500 0.299 9 5 ' '
8 0.815 0.500 0.701 9 5 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex4
_database_code_depnum_ccdc_archive 'CCDC 1550308'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O14, Dy H16 O8, Cl3, 11(H2 O)'
_chemical_formula_sum            'C44 H90 Cl3 Dy N24 O33'
_chemical_formula_weight         1752.25

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.190(2)
_cell_length_b                   12.2997(12)
_cell_length_c                   14.6385(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.175(3)
_cell_angle_gamma                90.00
_cell_volume                     3796.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1806
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_T_max  0.7321
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16630
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.69
_reflns_number_total             4636
_reflns_number_gt                4457
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.0982P)²+5.2313P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4636
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1391
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.6501(7) 0.5000 0.2984(8) 0.234(8) Uani 0.50 2 d SP . .
Cl2 Cl 0.7501(12) 0.1991(10) 0.6027(13) 0.54(2) Uani 0.50 1 d P . .
O1W O 0.5270(4) 0.5655(5) -0.1300(6) 0.0515(17) Uani 0.50 1 d P . .
O2W O 0.5493(3) 0.6474(5) -0.0488(5) 0.0437(14) Uani 0.50 1 d P . .
O3W O 0.5692(3) 0.6453(5) 0.0547(5) 0.0458(15) Uani 0.50 1 d P . .
O4W O 0.5781(3) 0.5683(5) 0.1332(5) 0.0497(17) Uani 0.50 1 d P . .
Dy1 Dy 0.5000 0.5000 0.0000 0.02331(13) Uani 1 4 d S . .
C1 C 0.6389(3) 0.1524(4) 0.2445(4) 0.0552(13) Uani 1 1 d . . .
C2 C 0.6511(4) 0.0000 0.3423(5) 0.058(2) Uani 1 2 d S . .
C3 C 0.7039(4) 0.0000 0.2933(6) 0.057(2) Uani 1 2 d S . .
C4 C 0.7297(3) 0.1434(4) 0.1850(5) 0.0659(17) Uani 1 1 d . . .
H4A H 0.7741 0.1313 0.2229 0.079 Uiso 1 1 calc R . .
H4B H 0.7227 0.2221 0.1798 0.079 Uiso 1 1 calc R . .
C5 C 0.6872(2) 0.1561(3) 0.0095(5) 0.0511(13) Uani 1 1 d . . .
C6 C 0.7488(3) 0.0000 0.0649(8) 0.060(2) Uani 1 2 d S . .
C7 C 0.7268(3) 0.0000 -0.0446(7) 0.056(2) Uani 1 2 d S . .
C8 C 0.6606(3) 0.1421(4) -0.1637(5) 0.0623(15) Uani 1 1 d . . .
H8A H 0.6895 0.1285 -0.2012 0.075 Uiso 1 1 calc R . .
H8B H 0.6567 0.2211 -0.1586 0.075 Uiso 1 1 calc R . .
C9 C 0.5441(3) 0.1565(4) -0.2344(4) 0.0586(13) Uani 1 1 d . . .
C10 C 0.5888(5) 0.0000 -0.2743(6) 0.059(2) Uani 1 2 d S . .
C11 C 0.5185(5) 0.0000 -0.3265(6) 0.057(2) Uani 1 2 d S . .
C12 C 0.4338(3) 0.1445(5) -0.3373(5) 0.0660(16) Uani 1 1 d . . .
H12A H 0.4357 0.2229 -0.3245 0.079 Uiso 1 1 calc R . .
H12B H 0.4223 0.1348 -0.4071 0.079 Uiso 1 1 calc R . .
C13 C 0.6714(8) 0.0000 0.4530(8) 0.122(6) Uani 1 2 d S . .
H13A H 0.6957 0.0653 0.4773 0.182 Uiso 0.50 1 calc PR . .
H13B H 0.6974 -0.0635 0.4774 0.182 Uiso 0.50 1 calc PR . .
H13C H 0.6341 -0.0018 0.4739 0.182 Uiso 1 2 calc SR . .
C14 C 0.7695(5) 0.0000 0.3650(9) 0.097(4) Uani 1 2 d S . .
H14A H 0.7760 0.0667 0.4021 0.146 Uiso 0.50 1 calc PR . .
H14B H 0.8007 -0.0049 0.3312 0.146 Uiso 0.50 1 calc PR . .
H14C H 0.7740 -0.0618 0.4078 0.146 Uiso 0.50 1 calc PR . .
C15 C 0.8204(4) 0.0000 0.1149(10) 0.094(4) Uani 1 2 d S . .
H15A H 0.8384 0.0673 0.1007 0.142 Uiso 0.50 1 calc PR . .
H15B H 0.8394 -0.0610 0.0920 0.142 Uiso 0.50 1 calc PR . .
H15C H 0.8289 -0.0064 0.1838 0.142 Uiso 0.50 1 calc PR . .
C16 C 0.7807(4) 0.0000 -0.0881(10) 0.083(3) Uani 1 2 d S . .
H16A H 0.8042 0.0675 -0.0721 0.124 Uiso 0.50 1 calc PR . .
H16B H 0.7634 -0.0067 -0.1575 0.124 Uiso 0.50 1 calc PR . .
H16C H 0.8087 -0.0608 -0.0627 0.124 Uiso 0.50 1 calc PR . .
N1 N 0.6151(2) 0.0983(3) 0.3049(3) 0.0553(11) Uani 1 1 d . . .
N2 N 0.6900(2) 0.0981(3) 0.2365(4) 0.0554(11) Uani 1 1 d . . .
N3 N 0.71952(19) 0.0994(3) 0.0883(4) 0.0577(12) Uani 1 1 d . . .
N4 N 0.6884(2) 0.0991(3) -0.0697(4) 0.0565(12) Uani 1 1 d . . .
N5 N 0.5988(3) 0.0984(3) -0.2160(4) 0.0611(12) Uani 1 1 d . . .
N6 N 0.4962(3) 0.0984(4) -0.2930(3) 0.0578(11) Uani 1 1 d . . .
O1 O 0.6178(3) 0.2382(4) 0.2042(4) 0.0863(15) Uani 1 1 d . . .
O2 O 0.66363(17) 0.2461(3) 0.0087(3) 0.0613(11) Uani 1 1 d . . .
O3 O 0.5396(3) 0.2479(4) -0.2055(4) 0.0889(16) Uani 1 1 d . . .
O4 O 0.5051(7) 0.0000 -0.4227(8) 0.071(5) Uani 0.501(16) 2 d SP . 1
O5 O 0.6198(9) 0.0000 -0.3426(12) 0.095(6) Uani 0.499(16) 2 d SP . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W O2W 1.518(10) . ?
O1W O1W 1.610(12) 6_565 ?
O1W Dy1 2.310(7) . ?
O2W O3W 1.440(10) . ?
O2W Dy1 2.341(6) . ?
O3W O4W 1.455(10) . ?
O3W Dy1 2.329(6) . ?
O4W O4W 1.679(13) 6_565 ?
O4W Dy1 2.325(6) . ?
Dy1 O1W 2.310(7) 2_655 ?
Dy1 O1W 2.310(7) 5_665 ?
Dy1 O1W 2.310(7) 6_565 ?
Dy1 O4W 2.325(6) 5_665 ?
Dy1 O4W 2.325(6) 2_655 ?
Dy1 O4W 2.325(6) 6_565 ?
Dy1 O3W 2.329(6) 5_665 ?
Dy1 O3W 2.329(6) 2_655 ?
Dy1 O3W 2.329(6) 6_565 ?
C1 O1 1.228(6) . ?
C1 N1 1.340(8) . ?
C1 N2 1.353(7) . ?
C2 N1 1.458(6) 6 ?
C2 N1 1.458(6) . ?
C2 C13 1.539(13) . ?
C2 C3 1.555(14) . ?
C3 N2 1.442(6) 6 ?
C3 N2 1.442(6) . ?
C3 C14 1.506(10) . ?
C4 N2 1.438(8) . ?
C4 N3 1.466(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.223(5) . ?
C5 N3 1.346(7) . ?
C5 N4 1.362(7) . ?
C6 N3 1.474(6) 6 ?
C6 N3 1.474(6) . ?
C6 C7 1.522(14) . ?
C6 C15 1.529(10) . ?
C7 N4 1.468(6) 6 ?
C7 N4 1.468(6) . ?
C7 C16 1.519(10) . ?
C8 N4 1.423(8) . ?
C8 N5 1.449(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.215(6) . ?
C9 N6 1.345(8) . ?
C9 N5 1.361(8) . ?
C10 O5 1.381(14) . ?
C10 N5 1.457(6) . ?
C10 N5 1.457(6) 6 ?
C10 C11 1.507(14) . ?
C11 O4 1.345(13) . ?
C11 N6 1.450(6) 6 ?
C11 N6 1.450(6) . ?
C12 N1 1.430(8) 2_655 ?
C12 N6 1.450(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
N1 C12 1.430(8) 2_655 ?

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
O2W O1W O1W 131.6(4) . 6_565 ?
O2W O1W Dy1 72.0(3) . . ?
O1W O1W Dy1 69.60(15) 6_565 . ?
O3W O2W O1W 136.9(6) . . ?
O3W O2W Dy1 71.6(3) . . ?
O1W O2W Dy1 69.9(3) . . ?
O2W O3W O4W 139.8(6) . . ?
O2W O3W Dy1 72.5(3) . . ?
O4W O3W Dy1 71.6(3) . . ?
O3W O4W O4W 130.7(4) . 6_565 ?
O3W O4W Dy1 72.0(3) . . ?
O4W O4W Dy1 68.83(16) 6_565 . ?
O1W Dy1 O1W 40.8(3) 2_655 5_665 ?
O1W Dy1 O1W 139.2(3) 2_655 . ?
O1W Dy1 O1W 180.0(3) 5_665 . ?
O1W Dy1 O1W 180.0 2_655 6_565 ?
O1W Dy1 O1W 139.2(3) 5_665 6_565 ?
O1W Dy1 O1W 40.8(3) . 6_565 ?
O1W Dy1 O4W 120.0(3) 2_655 5_665 ?
O1W Dy1 O4W 104.4(3) 5_665 5_665 ?
O1W Dy1 O4W 75.6(3) . 5_665 ?
O1W Dy1 O4W 60.0(3) 6_565 5_665 ?
O1W Dy1 O4W 60.0(3) 2_655 . ?
O1W Dy1 O4W 75.6(3) 5_665 . ?
O1W Dy1 O4W 104.4(3) . . ?
O1W Dy1 O4W 120.0(3) 6_565 . ?
O4W Dy1 O4W 180.0(3) 5_665 . ?
O1W Dy1 O4W 104.4(3) 2_655 2_655 ?
O1W Dy1 O4W 120.0(3) 5_665 2_655 ?
O1W Dy1 O4W 60.0(3) . 2_655 ?
O1W Dy1 O4W 75.6(3) 6_565 2_655 ?
O4W Dy1 O4W 42.3(3) 5_665 2_655 ?
O4W Dy1 O4W 137.7(3) . 2_655 ?
O1W Dy1 O4W 75.6(3) 2_655 6_565 ?
O1W Dy1 O4W 60.0(3) 5_665 6_565 ?
O1W Dy1 O4W 120.0(3) . 6_565 ?
O1W Dy1 O4W 104.4(3) 6_565 6_565 ?
O4W Dy1 O4W 137.7(3) 5_665 6_565 ?
O4W Dy1 O4W 42.3(3) . 6_565 ?
O4W Dy1 O4W 180.0(4) 2_655 6_565 ?
O1W Dy1 O3W 103.8(2) 2_655 5_665 ?
O1W Dy1 O3W 72.8(3) 5_665 5_665 ?
O1W Dy1 O3W 107.2(3) . 5_665 ?
O1W Dy1 O3W 76.2(2) 6_565 5_665 ?
O4W Dy1 O3W 36.4(2) 5_665 5_665 ?
O4W Dy1 O3W 143.6(2) . 5_665 ?
O4W Dy1 O3W 75.5(2) 2_655 5_665 ?
O4W Dy1 O3W 104.5(2) 6_565 5_665 ?
O1W Dy1 O3W 76.2(2) 2_655 . ?
O1W Dy1 O3W 107.2(3) 5_665 . ?
O1W Dy1 O3W 72.8(3) . . ?
O1W Dy1 O3W 103.8(2) 6_565 . ?
O4W Dy1 O3W 143.6(2) 5_665 . ?
O4W Dy1 O3W 36.4(2) . . ?
O4W Dy1 O3W 104.5(2) 2_655 . ?
O4W Dy1 O3W 75.5(2) 6_565 . ?
O3W Dy1 O3W 180.0(4) 5_665 . ?
O1W Dy1 O3W 72.8(3) 2_655 2_655 ?
O1W Dy1 O3W 103.8(2) 5_665 2_655 ?
O1W Dy1 O3W 76.2(2) . 2_655 ?
O1W Dy1 O3W 107.2(3) 6_565 2_655 ?
O4W Dy1 O3W 75.5(2) 5_665 2_655 ?
O4W Dy1 O3W 104.5(2) . 2_655 ?
O4W Dy1 O3W 36.4(2) 2_655 2_655 ?
O4W Dy1 O3W 143.6(2) 6_565 2_655 ?
O3W Dy1 O3W 100.2(3) 5_665 2_655 ?
O3W Dy1 O3W 79.8(3) . 2_655 ?
O1W Dy1 O3W 107.2(3) 2_655 6_565 ?
O1W Dy1 O3W 76.2(2) 5_665 6_565 ?
O1W Dy1 O3W 103.8(2) . 6_565 ?
O1W Dy1 O3W 72.8(3) 6_565 6_565 ?
O4W Dy1 O3W 104.5(2) 5_665 6_565 ?
O4W Dy1 O3W 75.5(2) . 6_565 ?
O4W Dy1 O3W 143.6(2) 2_655 6_565 ?
O4W Dy1 O3W 36.4(2) 6_565 6_565 ?
O3W Dy1 O3W 79.8(3) 5_665 6_565 ?
O3W Dy1 O3W 100.2(3) . 6_565 ?
O3W Dy1 O3W 180.0 2_655 6_565 ?
O1 C1 N1 125.1(6) . . ?
O1 C1 N2 125.9(6) . . ?
N1 C1 N2 109.0(5) . . ?
N1 C2 N1 112.0(6) 6 . ?
N1 C2 C13 110.0(6) 6 . ?
N1 C2 C13 110.0(6) . . ?
N1 C2 C3 103.3(5) 6 . ?
N1 C2 C3 103.3(5) . . ?
C13 C2 C3 118.0(9) . . ?
N2 C3 N2 113.5(6) 6 . ?
N2 C3 C14 112.8(5) 6 . ?
N2 C3 C14 112.8(5) . . ?
N2 C3 C2 102.1(5) 6 . ?
N2 C3 C2 102.1(5) . . ?
C14 C3 C2 112.5(8) . . ?
N2 C4 N3 115.4(4) . . ?
N2 C4 H4A 108.4 . . ?
N3 C4 H4A 108.4 . . ?
N2 C4 H4B 108.4 . . ?
N3 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N3 126.1(6) . . ?
O2 C5 N4 125.4(6) . . ?
N3 C5 N4 108.4(4) . . ?
N3 C6 N3 112.1(6) 6 . ?
N3 C6 C7 103.0(5) 6 . ?
N3 C6 C7 103.0(5) . . ?
N3 C6 C15 110.9(5) 6 . ?
N3 C6 C15 110.9(5) . . ?
C7 C6 C15 116.6(8) . . ?
N4 C7 N4 112.3(6) 6 . ?
N4 C7 C16 111.5(5) 6 . ?
N4 C7 C16 111.5(5) . . ?
N4 C7 C6 103.5(5) 6 . ?
N4 C7 C6 103.5(5) . . ?
C16 C7 C6 114.0(8) . . ?
N4 C8 N5 115.2(4) . . ?
N4 C8 H8A 108.5 . . ?
N5 C8 H8A 108.5 . . ?
N4 C8 H8B 108.5 . . ?
N5 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
O3 C9 N6 125.4(6) . . ?
O3 C9 N5 125.6(6) . . ?
N6 C9 N5 109.0(5) . . ?
O5 C10 N5 113.9(6) . . ?
O5 C10 N5 113.9(6) . 6 ?
N5 C10 N5 112.3(7) . 6 ?
O5 C10 C11 107.7(11) . . ?
N5 C10 C11 104.0(5) . . ?
N5 C10 C11 104.0(5) 6 . ?
O4 C11 N6 111.5(5) . 6 ?
O4 C11 N6 111.5(5) . . ?
N6 C11 N6 113.2(6) 6 . ?
O4 C11 C10 112.8(9) . . ?
N6 C11 C10 103.7(5) 6 . ?
N6 C11 C10 103.7(5) . . ?
N1 C12 N6 114.4(5) 2_655 . ?
N1 C12 H12A 108.7 2_655 . ?
N6 C12 H12A 108.7 . . ?
N1 C12 H12B 108.7 2_655 . ?
N6 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 H15A 109.5 . . ?
C6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C16 H16A 109.5 . . ?
C7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C12 121.1(5) . 2_655 ?
C1 N1 C2 112.2(6) . . ?
C12 N1 C2 126.0(6) 2_655 . ?
C1 N2 C4 121.4(4) . . ?
C1 N2 C3 113.4(6) . . ?
C4 N2 C3 124.8(6) . . ?
C5 N3 C4 121.1(4) . . ?
C5 N3 C6 112.7(6) . . ?
C4 N3 C6 125.7(6) . . ?
C5 N4 C8 121.0(4) . . ?
C5 N4 C7 112.2(6) . . ?
C8 N4 C7 126.4(6) . . ?
C9 N5 C8 123.2(5) . . ?
C9 N5 C10 110.9(6) . . ?
C8 N5 C10 124.3(6) . . ?
C9 N6 C11 112.0(6) . . ?
C9 N6 C12 122.2(5) . . ?
C11 N6 C12 123.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.69
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.137

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 117 37 ' '
2 1.000 0.000 0.500 342 77 ' '
3 0.500 0.500 0.500 342 77 ' '
4 0.000 0.500 0.000 117 37 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1550305'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O14, Eu H16 O8, Cl3, 18(H2 O)'
_chemical_formula_sum            'C44 H104 Cl3 Eu N24 O40'
_chemical_formula_weight         1867.82

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'
Eu Eu -0.1578 3.6682 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.377(11)
_cell_length_b                   12.519(6)
_cell_length_c                   14.991(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.190(10)
_cell_angle_gamma                90.00
_cell_volume                     3990(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1940
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7421
_exptl_absorpt_correction_T_max  0.7897
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10460
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4095
_reflns_number_gt                3578
_reflns_threshold_expression     >2sigma(I)



_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.
;

_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)+(0.0950P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4095
_refine_ls_number_parameters     267
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1484
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.5234(8) 0.9610(7) 0.2047(10) 0.349(8) Uani 0.50 1 d P . .
Cl2 Cl 0.3528(9) 1.0361(9) 0.2043(11) 0.213(8) Uani 0.25 1 d P . .
O1W O 0.5272(4) 0.9329(5) 0.3678(5) 0.0506(17) Uani 0.50 1 d P . .
O2W O 0.4280(3) 1.1471(5) 0.4455(5) 0.0483(18) Uani 0.50 1 d P . .
O3W O 0.4190(3) 1.0685(5) 0.3662(5) 0.0526(18) Uani 0.50 1 d P . .
O4W O 0.5516(3) 0.8509(5) 0.4500(6) 0.0526(19) Uani 0.50 1 d P . .
Eu1 Eu 0.5000 1.0000 0.5000 0.03021(18) Uani 1 4 d S . .
C1 C 0.6880(2) 0.6541(3) 0.5125(5) 0.0511(14) Uani 1 1 d . . .
C2 C 0.7485(3) 0.5000 0.5683(8) 0.069(3) Uani 1 2 d S . .
C3 C 0.7267(3) 0.5000 0.4576(7) 0.056(2) Uani 1 2 d S . .
C4 C 0.6626(3) 0.6402(4) 0.3429(5) 0.0699(19) Uani 1 1 d . . .
H4A H 0.6915 0.6262 0.3077 0.084 Uiso 1 1 calc R . .
H4B H 0.6591 0.7171 0.3475 0.084 Uiso 1 1 calc R . .
C5 C 0.5454(3) 0.6535(4) 0.2693(5) 0.0610(15) Uani 1 1 d . . .
C6 C 0.5909(5) 0.5000 0.2320(7) 0.065(3) Uani 1 2 d S . .
C7 C 0.5202(5) 0.5000 0.1803(6) 0.058(2) Uani 1 2 d S . .
C8 C 0.4370(3) 0.6434(4) 0.1672(4) 0.0673(17) Uani 1 1 d . . .
H8A H 0.4262 0.6343 0.0998 0.081 Uiso 1 1 calc R . .
H8B H 0.4393 0.7195 0.1801 0.081 Uiso 1 1 calc R . .
C9 C 0.3620(3) 0.6507(4) 0.2565(4) 0.0526(14) Uani 1 1 d . . .
C10 C 0.3502(5) 0.5000 0.1607(6) 0.065(3) Uani 1 2 d S . .
C11 C 0.2981(4) 0.5000 0.2069(6) 0.059(2) Uani 1 2 d S . .
C12 C 0.2706(3) 0.6411(4) 0.3152(5) 0.0679(18) Uani 1 1 d . . .
H12A H 0.2772 0.7177 0.3206 0.081 Uiso 1 1 calc R . .
H12B H 0.2271 0.6292 0.2781 0.081 Uiso 1 1 calc R . .
C13 C 0.8213(3) 0.5000 0.6212(10) 0.103(4) Uani 1 2 d S . .
H13A H 0.8399 0.4369 0.6047 0.155 Uiso 0.50 1 calc PR . .
H13B H 0.8284 0.5010 0.6877 0.155 Uiso 1 2 calc SR . .
H13C H 0.8400 0.5621 0.6034 0.155 Uiso 0.50 1 calc PR . .
C14 C 0.7810(4) 0.5000 0.4171(9) 0.088(4) Uani 1 2 d S . .
H14A H 0.8040 0.5657 0.4331 0.132 Uiso 0.50 1 calc PR . .
H14B H 0.7649 0.4933 0.3500 0.132 Uiso 0.50 1 calc PR . .
H14C H 0.8084 0.4410 0.4425 0.132 Uiso 0.50 1 calc PR . .
C15 C 0.3318(7) 0.5000 0.0505(7) 0.116(5) Uani 1 2 d S . .
H15A H 0.3086 0.4362 0.0261 0.173 Uiso 0.50 1 calc PR . .
H15B H 0.3692 0.5025 0.0322 0.173 Uiso 1 2 calc SR . .
H15C H 0.3062 0.5613 0.0258 0.173 Uiso 0.50 1 calc PR . .
C16 C 0.2315(5) 0.5000 0.1377(9) 0.121(5) Uani 1 2 d S . .
H16A H 0.2251 0.4365 0.0999 0.181 Uiso 0.50 1 calc PR . .
H16B H 0.2258 0.5617 0.0979 0.181 Uiso 0.50 1 calc PR . .
H16C H 0.2016 0.5017 0.1718 0.181 Uiso 1 2 calc SR . .
N1 N 0.71971(18) 0.5981(3) 0.5926(4) 0.0554(12) Uani 1 1 d . . .
N2 N 0.6891(2) 0.5983(3) 0.4351(4) 0.0564(13) Uani 1 1 d . . .
N3 N 0.6007(2) 0.5978(3) 0.2896(4) 0.0606(13) Uani 1 1 d . . .
N4 N 0.4974(2) 0.5975(3) 0.2106(3) 0.0591(12) Uani 1 1 d . . .
N5 N 0.3870(2) 0.5973(3) 0.1985(3) 0.0565(12) Uani 1 1 d . . .
N6 N 0.3111(2) 0.5963(3) 0.2650(4) 0.0578(13) Uani 1 1 d . . .
O1 O 0.66495(17) 0.7439(2) 0.5125(3) 0.0613(11) Uani 1 1 d . . .
O2 O 0.5419(3) 0.7451(3) 0.3010(4) 0.0919(16) Uani 1 1 d . . .
O3 O 0.3815(2) 0.7373(3) 0.2929(4) 0.0811(14) Uani 1 1 d . . .
O4 O 0.5083(5) 0.5000 0.0818(8) 0.084(4) Uani 0.609(15) 2 d SPU . 1
O5 O 0.6287(8) 0.5000 0.1725(11) 0.072(5) Uani 0.391(15) 2 d SPU . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Cl1 0.976(17) 6_575 ?
Cl2 Cl2 0.90(2) 6_575 ?
O1W O4W 1.565(10) . ?
O1W O1W 1.681(12) 6_575 ?
O1W Eu1 2.399(7) . ?
O2W O4W 1.489(11) 5_676 ?
O2W O3W 1.508(10) . ?
O2W Eu1 2.415(6) . ?
O3W O3W 1.715(12) 6_575 ?
O3W Eu1 2.403(7) . ?
O4W O2W 1.489(11) 5_676 ?
O4W Eu1 2.433(6) . ?
Eu1 O1W 2.399(7) 5_676 ?
Eu1 O1W 2.399(7) 2_656 ?
Eu1 O1W 2.399(7) 6_575 ?
Eu1 O3W 2.403(7) 2_656 ?
Eu1 O3W 2.403(7) 5_676 ?
Eu1 O3W 2.403(7) 6_575 ?
Eu1 O2W 2.415(6) 2_656 ?
Eu1 O2W 2.415(6) 6_575 ?
Eu1 O2W 2.415(6) 5_676 ?
C1 O1 1.236(5) . ?
C1 N2 1.361(8) . ?
C1 N1 1.381(7) . ?
C2 N1 1.485(6) 6_565 ?
C2 N1 1.485(6) . ?
C2 C13 1.573(10) . ?
C2 C3 1.578(14) . ?
C3 N2 1.470(5) 6_565 ?
C3 N2 1.470(5) . ?
C3 C14 1.518(10) . ?
C4 N2 1.423(9) . ?
C4 N3 1.467(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.253(6) . ?
C5 N4 1.353(8) . ?
C5 N3 1.368(8) . ?
C6 O5 1.409(18) . ?
C6 N3 1.474(7) . ?
C6 N3 1.474(7) 6_565 ?
C6 C7 1.529(13) . ?
C7 O4 1.416(13) . ?
C7 N4 1.450(6) 6_565 ?
C7 N4 1.450(6) . ?
C8 N4 1.424(8) . ?
C8 N5 1.460(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O3 1.231(6) . ?
C9 N5 1.350(7) . ?
C9 N6 1.365(7) . ?
C10 N5 1.481(6) . ?
C10 N5 1.481(6) 6_565 ?
C10 C11 1.530(14) . ?
C10 C15 1.574(13) . ?
C11 N6 1.463(6) . ?
C11 N6 1.463(6) 6_565 ?
C11 C16 1.527(12) . ?
C12 N1 1.434(8) 2_656 ?
C12 N6 1.461(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N1 C12 1.434(8) 2_656 ?

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
O4W O1W O1W 131.0(4) . 6_575 ?
O4W O1W Eu1 72.3(4) . . ?
O1W O1W Eu1 69.50(15) 6_575 . ?
O4W O2W O3W 139.7(6) 5_676 . ?
O4W O2W Eu1 72.8(3) 5_676 . ?
O3W O2W Eu1 71.3(3) . . ?
O2W O3W O3W 130.8(4) . 6_575 ?
O2W O3W Eu1 72.2(4) . . ?
O3W O3W Eu1 69.10(14) 6_575 . ?
O2W O4W O1W 137.2(6) 5_676 . ?
O2W O4W Eu1 71.5(4) 5_676 . ?
O1W O4W Eu1 70.0(3) . . ?
O1W Eu1 O1W 41.0(3) 5_676 2_656 ?
O1W Eu1 O1W 180.00(16) 5_676 . ?
O1W Eu1 O1W 139.0(3) 2_656 . ?
O1W Eu1 O1W 139.0(3) 5_676 6_575 ?
O1W Eu1 O1W 180.000(1) 2_656 6_575 ?
O1W Eu1 O1W 41.0(3) . 6_575 ?
O1W Eu1 O3W 60.3(3) 5_676 2_656 ?
O1W Eu1 O3W 75.8(3) 2_656 2_656 ?
O1W Eu1 O3W 119.7(3) . 2_656 ?
O1W Eu1 O3W 104.2(3) 6_575 2_656 ?
O1W Eu1 O3W 75.8(3) 5_676 5_676 ?
O1W Eu1 O3W 60.3(3) 2_656 5_676 ?
O1W Eu1 O3W 104.2(3) . 5_676 ?
O1W Eu1 O3W 119.7(3) 6_575 5_676 ?
O3W Eu1 O3W 41.8(3) 2_656 5_676 ?
O1W Eu1 O3W 119.7(3) 5_676 6_575 ?
O1W Eu1 O3W 104.2(3) 2_656 6_575 ?
O1W Eu1 O3W 60.3(3) . 6_575 ?
O1W Eu1 O3W 75.8(3) 6_575 6_575 ?
O3W Eu1 O3W 180.000(1) 2_656 6_575 ?
O3W Eu1 O3W 138.2(3) 5_676 6_575 ?
O1W Eu1 O3W 104.2(3) 5_676 . ?
O1W Eu1 O3W 119.7(3) 2_656 . ?
O1W Eu1 O3W 75.8(3) . . ?
O1W Eu1 O3W 60.3(3) 6_575 . ?
O3W Eu1 O3W 138.2(3) 2_656 . ?
O3W Eu1 O3W 180.000(1) 5_676 . ?
O3W Eu1 O3W 41.8(3) 6_575 . ?
O1W Eu1 O2W 76.6(2) 5_676 2_656 ?
O1W Eu1 O2W 107.6(2) 2_656 2_656 ?
O1W Eu1 O2W 103.4(2) . 2_656 ?
O1W Eu1 O2W 72.4(2) 6_575 2_656 ?
O3W Eu1 O2W 36.5(2) 2_656 2_656 ?
O3W Eu1 O2W 74.9(2) 5_676 2_656 ?
O3W Eu1 O2W 143.5(2) 6_575 2_656 ?
O3W Eu1 O2W 105.1(2) . 2_656 ?
O1W Eu1 O2W 103.4(2) 5_676 6_575 ?
O1W Eu1 O2W 72.4(2) 2_656 6_575 ?
O1W Eu1 O2W 76.6(2) . 6_575 ?
O1W Eu1 O2W 107.6(2) 6_575 6_575 ?
O3W Eu1 O2W 143.5(2) 2_656 6_575 ?
O3W Eu1 O2W 105.1(2) 5_676 6_575 ?
O3W Eu1 O2W 36.5(2) 6_575 6_575 ?
O3W Eu1 O2W 74.9(2) . 6_575 ?
O2W Eu1 O2W 180.000(1) 2_656 6_575 ?
O1W Eu1 O2W 107.6(2) 5_676 5_676 ?
O1W Eu1 O2W 76.6(2) 2_656 5_676 ?
O1W Eu1 O2W 72.4(2) . 5_676 ?
O1W Eu1 O2W 103.4(2) 6_575 5_676 ?
O3W Eu1 O2W 74.9(2) 2_656 5_676 ?
O3W Eu1 O2W 36.5(2) 5_676 5_676 ?
O3W Eu1 O2W 105.1(2) 6_575 5_676 ?
O3W Eu1 O2W 143.5(2) . 5_676 ?
O2W Eu1 O2W 99.4(3) 2_656 5_676 ?
O2W Eu1 O2W 80.6(3) 6_575 5_676 ?
O1W Eu1 O2W 72.4(2) 5_676 . ?
O1W Eu1 O2W 103.4(2) 2_656 . ?
O1W Eu1 O2W 107.6(2) . . ?
O1W Eu1 O2W 76.6(2) 6_575 . ?
O3W Eu1 O2W 105.1(2) 2_656 . ?
O3W Eu1 O2W 143.5(2) 5_676 . ?
O3W Eu1 O2W 74.9(2) 6_575 . ?
O3W Eu1 O2W 36.5(2) . . ?
O2W Eu1 O2W 80.6(3) 2_656 . ?
O2W Eu1 O2W 99.4(3) 6_575 . ?
O2W Eu1 O2W 180.000(1) 5_676 . ?
O1 C1 N2 125.9(6) . . ?
O1 C1 N1 124.2(6) . . ?
N2 C1 N1 109.9(4) . . ?
N1 C2 N1 111.6(6) 6_565 . ?
N1 C2 C13 109.7(5) 6_565 . ?
N1 C2 C13 109.7(5) . . ?
N1 C2 C3 104.1(5) 6_565 . ?
N1 C2 C3 104.1(5) . . ?
C13 C2 C3 117.5(8) . . ?
N2 C3 N2 113.7(6) 6_565 . ?
N2 C3 C14 112.4(5) 6_565 . ?
N2 C3 C14 112.4(5) . . ?
N2 C3 C2 102.0(5) 6_565 . ?
N2 C3 C2 102.0(5) . . ?
C14 C3 C2 113.4(8) . . ?
N2 C4 N3 115.6(4) . . ?
N2 C4 H4A 108.4 . . ?
N3 C4 H4A 108.4 . . ?
N2 C4 H4B 108.4 . . ?
N3 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
O2 C5 N4 126.1(6) . . ?
O2 C5 N3 122.8(6) . . ?
N4 C5 N3 111.1(5) . . ?
O5 C6 N3 111.2(5) . . ?
O5 C6 N3 111.2(5) . 6_565 ?
N3 C6 N3 112.2(7) . 6_565 ?
O5 C6 C7 114.2(10) . . ?
N3 C6 C7 103.8(5) . . ?
N3 C6 C7 103.8(5) 6_565 . ?
O4 C7 N4 110.9(5) . 6_565 ?
O4 C7 N4 110.9(5) . . ?
N4 C7 N4 114.7(7) 6_565 . ?
O4 C7 C6 110.9(8) . . ?
N4 C7 C6 104.5(5) 6_565 . ?
N4 C7 C6 104.5(5) . . ?
N4 C8 N5 114.0(4) . . ?
N4 C8 H8A 108.8 . . ?
N5 C8 H8A 108.8 . . ?
N4 C8 H8B 108.8 . . ?
N5 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O3 C9 N5 124.1(6) . . ?
O3 C9 N6 126.1(6) . . ?
N5 C9 N6 109.8(4) . . ?
N5 C10 N5 110.8(6) . 6_565 ?
N5 C10 C11 103.8(5) . . ?
N5 C10 C11 103.8(5) 6_565 . ?
N5 C10 C15 109.5(6) . . ?
N5 C10 C15 109.5(6) 6_565 . ?
C11 C10 C15 119.2(9) . . ?
N6 C11 N6 111.1(7) . 6_565 ?
N6 C11 C16 112.0(5) . . ?
N6 C11 C16 112.0(5) 6_565 . ?
N6 C11 C10 103.3(5) . . ?
N6 C11 C10 103.3(5) 6_565 . ?
C16 C11 C10 114.4(9) . . ?
N1 C12 N6 114.9(4) 2_656 . ?
N1 C12 H12A 108.6 2_656 . ?
N6 C12 H12A 108.6 . . ?
N1 C12 H12B 108.6 2_656 . ?
N6 C12 H12B 108.6 . . ?
H12A C12 H12B 107.5 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C12 122.0(4) . 2_656 ?
C1 N1 C2 110.6(6) . . ?
C12 N1 C2 126.9(6) 2_656 . ?
C1 N2 C4 121.7(4) . . ?
C1 N2 C3 113.3(6) . . ?
C4 N2 C3 124.5(6) . . ?
C5 N3 C4 124.8(4) . . ?
C5 N3 C6 109.5(6) . . ?
C4 N3 C6 124.2(6) . . ?
C5 N4 C8 122.4(4) . . ?
C5 N4 C7 110.7(6) . . ?
C8 N4 C7 124.9(6) . . ?
C9 N5 C8 121.7(4) . . ?
C9 N5 C10 111.2(6) . . ?
C8 N5 C10 126.3(6) . . ?
C9 N6 C12 121.8(4) . . ?
C9 N6 C11 111.9(6) . . ?
C12 N6 C11 125.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.118

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
####################################################################### 
# 
# 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_complex9
_database_code_depnum_ccdc_archive 'CCDC 1550313'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H86 Cl Lu N26 O37'
_chemical_formula_weight         1781.81

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'
Lu Lu -0.4720 5.8584 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.20(2)
_cell_length_b                   12.287(13)
_cell_length_c                   26.75(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.489(17)
_cell_angle_gamma                90.00
_cell_volume                     6790(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3664
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6350
_exptl_absorpt_correction_T_max  0.7082
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18193
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5777
_reflns_number_gt                4677
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.0855P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5777
_refine_ls_number_parameters     502
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1445
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 1.1266(11) -0.4173(12) 0.9217(6) 0.376(16) Uani 0.50 1 d P . .
N13 N 1.0470(6) 0.3047(9) 1.0592(3) 0.099(3) Uani 1 1 d . . .
O9 O 1.0354(7) 0.3963(8) 1.0834(4) 0.151(5) Uani 1 1 d . . .
O10 O 0.9967(4) 0.2693(8) 1.0241(3) 0.110(3) Uani 1 1 d . . .
O11 O 1.0979(4) 0.2564(9) 1.0712(3) 0.116(3) Uani 1 1 d . . .
O1W O 1.0701(4) -0.5496(7) 0.7842(3) 0.0234(17) Uani 0.50 1 d PU . .
O2W O 1.0804(6) -0.4809(13) 0.8235(6) 0.097(5) Uani 0.50 1 d P . .
O3W O 1.0772(4) -0.3359(7) 0.8265(3) 0.037(2) Uani 0.50 1 d P . .
O4W O 1.0714(6) -0.2697(12) 0.7803(7) 0.095(5) Uani 0.50 1 d P . .
O5W O 0.9480(4) -0.2624(7) 0.7745(3) 0.031(2) Uani 0.50 1 d P . .
O6W O 0.9762(9) -0.3447(14) 0.8222(6) 0.115(6) Uani 0.50 1 d P . .
O7W O 0.9704(4) -0.4694(7) 0.8190(3) 0.0289(19) Uani 0.50 1 d PU . .
O8W O 0.9509(6) -0.5469(12) 0.7762(6) 0.085(4) Uani 0.50 1 d P . .
Lu1 Lu 1.0000 -0.40591(3) 0.7500 0.02290(15) Uani 1 2 d S . .
C1 C 1.1866(3) -0.0642(6) 0.7543(3) 0.0341(16) Uani 1 1 d . . .
C2 C 1.2190(3) 0.0951(5) 0.7224(3) 0.0339(15) Uani 1 1 d . . .
C3 C 1.2506(3) 0.0923(5) 0.7862(3) 0.0360(16) Uani 1 1 d . . .
C4 C 1.1862(3) 0.2486(5) 0.7582(3) 0.0329(15) Uani 1 1 d . . .
C5 C 1.2390(3) -0.0533(6) 0.8520(3) 0.0411(17) Uani 1 1 d . . .
H5A H 1.2854 -0.0433 0.8723 0.049 Uiso 1 1 calc R . .
H5B H 1.2304 -0.1317 0.8487 0.049 Uiso 1 1 calc R . .
C6 C 1.2434(3) 0.2325(6) 0.8548(3) 0.0390(16) Uani 1 1 d . . .
H6A H 1.2385 0.3118 0.8526 0.047 Uiso 1 1 calc R . .
H6B H 1.2894 0.2167 0.8738 0.047 Uiso 1 1 calc R . .
C7 C 1.1519(3) -0.0595(6) 0.8874(3) 0.0393(17) Uani 1 1 d . . .
C8 C 1.2210(3) 0.0894(5) 0.9165(3) 0.0366(16) Uani 1 1 d . . .
C9 C 1.1691(3) 0.0906(5) 0.9439(3) 0.0354(16) Uani 1 1 d . . .
C10 C 1.1575(3) 0.2472(6) 0.8915(3) 0.0366(17) Uani 1 1 d . . .
C11 C 1.0830(3) -0.0525(6) 0.9394(3) 0.0383(16) Uani 1 1 d . . .
H11A H 1.0970 -0.0443 0.9784 0.046 Uiso 1 1 calc R . .
H11B H 1.0800 -0.1306 0.9313 0.046 Uiso 1 1 calc R . .
C12 C 1.0852(3) 0.2371(6) 0.9409(3) 0.0377(16) Uani 1 1 d . . .
H12A H 1.0828 0.3157 0.9342 0.045 Uiso 1 1 calc R . .
H12B H 1.0982 0.2262 0.9797 0.045 Uiso 1 1 calc R . .
C13 C 0.9704(3) -0.0615(6) 0.8792(3) 0.0348(16) Uani 1 1 d . A .
C14 C 0.9981(3) 0.0935(5) 0.9324(2) 0.0318(15) Uani 1 1 d . . .
C15 C 0.9250(3) 0.0957(5) 0.9007(3) 0.0343(15) Uani 1 1 d . A .
C16 C 0.9722(3) 0.2492(5) 0.8791(3) 0.0376(17) Uani 1 1 d . . .
C17 C 1.1460(3) 0.2411(6) 0.6610(3) 0.0374(16) Uani 1 1 d . . .
H17A H 1.1732 0.2346 0.6394 0.045 Uiso 1 1 calc R . .
H17B H 1.1400 0.3188 0.6660 0.045 Uiso 1 1 calc R . .
C18 C 1.1499(3) -0.0498(6) 0.6580(3) 0.0414(17) Uani 1 1 d . . .
H18A H 1.1456 -0.1287 0.6607 0.050 Uiso 1 1 calc R . .
H18B H 1.1766 -0.0366 0.6364 0.050 Uiso 1 1 calc R . .
C19 C 1.2673(4) 0.0994(6) 0.6942(3) 0.050(2) Uani 1 1 d . . .
H19A H 1.2914 0.1671 0.7031 0.075 Uiso 1 1 calc R . .
H19B H 1.2443 0.0954 0.6556 0.075 Uiso 1 1 calc R . .
H19C H 1.2970 0.0385 0.7058 0.075 Uiso 1 1 calc R . .
C20 C 1.3237(3) 0.0893(6) 0.8082(3) 0.0469(19) Uani 1 1 d . . .
H20A H 1.3383 0.0229 0.7966 0.070 Uiso 1 1 calc R . .
H20B H 1.3395 0.0914 0.8471 0.070 Uiso 1 1 calc R . .
H20C H 1.3402 0.1517 0.7950 0.070 Uiso 1 1 calc R . .
C21 C 1.2903(4) 0.0820(7) 0.9545(4) 0.065(3) Uani 1 1 d . . .
H21A H 1.3014 0.1467 0.9768 0.098 Uiso 1 1 calc R . .
H21B H 1.3184 0.0765 0.9341 0.098 Uiso 1 1 calc R . .
H21C H 1.2957 0.0182 0.9771 0.098 Uiso 1 1 calc R . .
C22 C 1.1965(4) 0.0899(7) 1.0060(3) 0.065(3) Uani 1 1 d . . .
H22A H 1.2195 0.0222 1.0188 0.098 Uiso 1 1 calc R . .
H22B H 1.1612 0.0964 1.0190 0.098 Uiso 1 1 calc R . .
H22C H 1.2260 0.1506 1.0191 0.098 Uiso 1 1 calc R . .
N1 N 1.1823(2) -0.0060(5) 0.7108(2) 0.0365(13) Uani 1 1 d . . .
N2 N 1.2233(2) -0.0081(4) 0.7992(2) 0.0365(13) Uani 1 1 d . . .
N3 N 1.1789(2) 0.1924(4) 0.7124(2) 0.0335(13) Uani 1 1 d . . .
N4 N 1.2244(2) 0.1902(4) 0.8014(2) 0.0329(13) Uani 1 1 d . . .
N5 N 1.2027(2) -0.0047(4) 0.8822(2) 0.0371(13) Uani 1 1 d . . .
N6 N 1.1307(2) -0.0058(4) 0.9220(2) 0.0342(13) Uani 1 1 d . . .
N7 N 1.2078(3) 0.1908(4) 0.8866(2) 0.0350(13) Uani 1 1 d . . .
N8 N 1.1343(3) 0.1919(4) 0.9239(2) 0.0353(13) Uani 1 1 d . . .
N9 N 1.0196(2) -0.0045(4) 0.91455(19) 0.0327(12) Uani 1 1 d . A .
N10 N 0.9148(3) -0.0026(4) 0.8700(2) 0.0374(13) Uani 1 1 d . . .
N11 N 1.0215(3) 0.1909(4) 0.9144(2) 0.0342(13) Uani 1 1 d . A .
N12 N 0.9162(3) 0.1930(4) 0.8682(2) 0.0381(14) Uani 1 1 d . . .
O1 O 1.1644(2) -0.1550(4) 0.7547(2) 0.0491(13) Uani 1 1 d . . .
O2 O 1.1298(3) -0.1452(5) 0.8647(2) 0.0629(16) Uani 1 1 d . . .
O3 O 0.9740(2) -0.1499(4) 0.8614(2) 0.0534(14) Uani 1 1 d . . .
O4 O 1.1634(2) 0.3376(4) 0.76014(19) 0.0469(12) Uani 1 1 d . . .
O5 O 1.1396(3) 0.3367(4) 0.8718(2) 0.0539(14) Uani 1 1 d . . .
O6 O 0.9781(3) 0.3377(5) 0.8607(2) 0.0658(17) Uani 1 1 d . A .
O7 O 1.0169(5) 0.0905(7) 0.9873(3) 0.049(3) Uani 0.559(13) 1 d P A 1
O8 O 0.8849(5) 0.0915(8) 0.9283(4) 0.039(3) Uani 0.441(13) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N13 O11 1.210(13) . ?
N13 O10 1.246(11) . ?
N13 O9 1.369(13) . ?
O1W O2W 1.301(17) . ?
O1W O8W 1.509(17) 2_756 ?
O1W Lu1 2.309(7) . ?
O2W O3W 1.785(19) . ?
O2W Lu1 2.308(12) . ?
O3W O4W 1.446(19) . ?
O3W Lu1 2.301(7) . ?
O4W O5W 1.369(18) 2_756 ?
O4W Lu1 2.242(12) . ?
O5W O4W 1.369(18) 2_756 ?
O5W O6W 1.568(19) . ?
O5W Lu1 2.329(8) . ?
O6W O7W 1.538(19) . ?
O6W Lu1 2.307(11) . ?
O7W O8W 1.428(18) . ?
O7W Lu1 2.310(8) . ?
O8W O1W 1.509(17) 2_756 ?
O8W Lu1 2.290(12) . ?
Lu1 O4W 2.242(12) 2_756 ?
Lu1 O8W 2.290(12) 2_756 ?
Lu1 O3W 2.301(7) 2_756 ?
Lu1 O6W 2.307(11) 2_756 ?
Lu1 O2W 2.308(12) 2_756 ?
Lu1 O1W 2.309(7) 2_756 ?
C1 O1 1.220(8) . ?
C1 N1 1.339(9) . ?
C1 N2 1.365(9) . ?
C2 N1 1.456(8) . ?
C2 N3 1.457(8) . ?
C2 C19 1.519(10) . ?
C2 C3 1.590(10) . ?
C3 N4 1.458(8) . ?
C3 N2 1.471(8) . ?
C3 C20 1.509(9) . ?
C4 O4 1.214(8) . ?
C4 N4 1.360(8) . ?
C4 N3 1.364(8) . ?
C5 N2 1.437(9) . ?
C5 N5 1.461(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.430(8) . ?
C6 N7 1.451(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.225(9) . ?
C7 N6 1.354(9) . ?
C7 N5 1.363(9) . ?
C8 N5 1.439(8) . ?
C8 N7 1.450(8) . ?
C8 C21 1.504(10) . ?
C8 C9 1.578(10) . ?
C9 N6 1.451(8) . ?
C9 N8 1.460(8) . ?
C9 C22 1.544(10) . ?
C10 O5 1.221(8) . ?
C10 N8 1.344(9) . ?
C10 N7 1.362(8) . ?
C11 N6 1.423(9) . ?
C11 N9 1.444(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.436(9) . ?
C12 N11 1.446(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.200(8) . ?
C13 N9 1.349(8) . ?
C13 N10 1.374(9) . ?
C14 O7 1.374(11) . ?
C14 N9 1.439(8) . ?
C14 N11 1.455(8) . ?
C14 C15 1.532(10) . ?
C15 O8 1.351(12) . ?
C15 N10 1.430(8) . ?
C15 N12 1.449(8) . ?
C16 O6 1.220(8) . ?
C16 N11 1.357(8) . ?
C16 N12 1.358(9) . ?
C17 N3 1.430(8) . ?
C17 N12 1.440(8) 2_756 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N1 1.434(9) . ?
C18 N10 1.473(8) 2_756 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N10 C18 1.473(8) 2_756 ?
N12 C17 1.440(8) 2_756 ?

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
O11 N13 O10 121.4(12) . . ?
O11 N13 O9 126.7(11) . . ?
O10 N13 O9 111.7(12) . . ?
O2W O1W O8W 138.1(10) . 2_756 ?
O2W O1W Lu1 73.6(6) . . ?
O8W O1W Lu1 70.2(6) 2_756 . ?
O1W O2W O3W 133.3(10) . . ?
O1W O2W Lu1 73.6(6) . . ?
O3W O2W Lu1 67.0(5) . . ?
O4W O3W O2W 121.0(9) . . ?
O4W O3W Lu1 69.2(5) . . ?
O2W O3W Lu1 67.4(4) . . ?
O5W O4W O3W 147.8(11) 2_756 . ?
O5W O4W Lu1 76.1(6) 2_756 . ?
O3W O4W Lu1 73.7(7) . . ?
O4W O5W O6W 134.7(10) 2_756 . ?
O4W O5W Lu1 69.1(6) 2_756 . ?
O6W O5W Lu1 69.5(5) . . ?
O7W O6W O5W 126.7(11) . . ?
O7W O6W Lu1 70.7(5) . . ?
O5W O6W Lu1 71.0(5) . . ?
O8W O7W O6W 134.6(9) . . ?
O8W O7W Lu1 71.1(6) . . ?
O6W O7W Lu1 70.4(5) . . ?
O7W O8W O1W 139.2(10) . 2_756 ?
O7W O8W Lu1 72.7(6) . . ?
O1W O8W Lu1 71.5(5) 2_756 . ?
O4W Lu1 O4W 83.4(8) . 2_756 ?
O4W Lu1 O8W 143.8(6) . . ?
O4W Lu1 O8W 108.8(5) 2_756 . ?
O4W Lu1 O8W 108.8(5) . 2_756 ?
O4W Lu1 O8W 143.8(6) 2_756 2_756 ?
O8W Lu1 O8W 81.7(7) . 2_756 ?
O4W Lu1 O3W 37.1(5) . . ?
O4W Lu1 O3W 103.9(5) 2_756 . ?
O8W Lu1 O3W 107.1(5) . . ?
O8W Lu1 O3W 105.8(4) 2_756 . ?
O4W Lu1 O3W 103.9(5) . 2_756 ?
O4W Lu1 O3W 37.1(5) 2_756 2_756 ?
O8W Lu1 O3W 105.8(4) . 2_756 ?
O8W Lu1 O3W 107.1(5) 2_756 2_756 ?
O3W Lu1 O3W 136.1(4) . 2_756 ?
O4W Lu1 O6W 73.2(7) . 2_756 ?
O4W Lu1 O6W 78.6(6) 2_756 2_756 ?
O8W Lu1 O6W 141.6(7) . 2_756 ?
O8W Lu1 O6W 73.1(6) 2_756 2_756 ?
O3W Lu1 O6W 107.3(5) . 2_756 ?
O3W Lu1 O6W 57.2(5) 2_756 2_756 ?
O4W Lu1 O6W 78.6(6) . . ?
O4W Lu1 O6W 73.2(7) 2_756 . ?
O8W Lu1 O6W 73.1(6) . . ?
O8W Lu1 O6W 141.6(7) 2_756 . ?
O3W Lu1 O6W 57.2(5) . . ?
O3W Lu1 O6W 107.3(5) 2_756 . ?
O6W Lu1 O6W 141.9(9) 2_756 . ?
O4W Lu1 O2W 146.0(7) . 2_756 ?
O4W Lu1 O2W 76.5(6) 2_756 2_756 ?
O8W Lu1 O2W 69.7(6) . 2_756 ?
O8W Lu1 O2W 75.1(5) 2_756 2_756 ?
O3W Lu1 O2W 176.5(5) . 2_756 ?
O3W Lu1 O2W 45.6(5) 2_756 2_756 ?
O6W Lu1 O2W 76.1(7) 2_756 2_756 ?
O6W Lu1 O2W 120.0(6) . 2_756 ?
O4W Lu1 O2W 76.5(6) . . ?
O4W Lu1 O2W 146.0(7) 2_756 . ?
O8W Lu1 O2W 75.1(5) . . ?
O8W Lu1 O2W 69.7(6) 2_756 . ?
O3W Lu1 O2W 45.6(5) . . ?
O3W Lu1 O2W 176.5(5) 2_756 . ?
O6W Lu1 O2W 120.0(6) 2_756 . ?
O6W Lu1 O2W 76.1(6) . . ?
O2W Lu1 O2W 133.0(8) 2_756 . ?
O4W Lu1 O1W 176.6(4) . 2_756 ?
O4W Lu1 O1W 98.2(5) 2_756 2_756 ?
O8W Lu1 O1W 38.3(4) . 2_756 ?
O8W Lu1 O1W 68.1(4) 2_756 2_756 ?
O3W Lu1 O1W 144.3(3) . 2_756 ?
O3W Lu1 O1W 76.1(3) 2_756 2_756 ?
O6W Lu1 O1W 104.2(5) 2_756 2_756 ?
O6W Lu1 O1W 104.6(5) . 2_756 ?
O2W Lu1 O1W 32.7(4) 2_756 2_756 ?
O2W Lu1 O1W 103.3(5) . 2_756 ?
O4W Lu1 O1W 98.2(5) . . ?
O4W Lu1 O1W 176.6(4) 2_756 . ?
O8W Lu1 O1W 68.1(4) . . ?
O8W Lu1 O1W 38.3(4) 2_756 . ?
O3W Lu1 O1W 76.1(3) . . ?
O3W Lu1 O1W 144.3(3) 2_756 . ?
O6W Lu1 O1W 104.6(5) 2_756 . ?
O6W Lu1 O1W 104.2(5) . . ?
O2W Lu1 O1W 103.3(5) 2_756 . ?
O2W Lu1 O1W 32.7(4) . . ?
O1W Lu1 O1W 80.3(4) 2_756 . ?
O1 C1 N1 126.5(6) . . ?
O1 C1 N2 124.5(6) . . ?
N1 C1 N2 108.9(6) . . ?
N1 C2 N3 113.8(5) . . ?
N1 C2 C19 111.5(6) . . ?
N3 C2 C19 112.1(6) . . ?
N1 C2 C3 101.7(5) . . ?
N3 C2 C3 102.4(5) . . ?
C19 C2 C3 114.8(6) . . ?
N4 C3 N2 112.6(6) . . ?
N4 C3 C20 113.1(6) . . ?
N2 C3 C20 111.4(5) . . ?
N4 C3 C2 102.6(5) . . ?
N2 C3 C2 102.3(5) . . ?
C20 C3 C2 114.1(6) . . ?
O4 C4 N4 125.4(6) . . ?
O4 C4 N3 125.4(6) . . ?
N4 C4 N3 109.2(6) . . ?
N2 C5 N5 113.7(6) . . ?
N2 C5 H5A 108.8 . . ?
N5 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
N5 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N4 C6 N7 115.7(5) . . ?
N4 C6 H6A 108.4 . . ?
N7 C6 H6A 108.4 . . ?
N4 C6 H6B 108.4 . . ?
N7 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
O2 C7 N6 125.5(6) . . ?
O2 C7 N5 124.8(7) . . ?
N6 C7 N5 109.7(6) . . ?
N5 C8 N7 112.8(6) . . ?
N5 C8 C21 111.2(6) . . ?
N7 C8 C21 112.0(6) . . ?
N5 C8 C9 102.7(5) . . ?
N7 C8 C9 102.3(5) . . ?
C21 C8 C9 115.2(6) . . ?
N6 C9 N8 113.2(5) . . ?
N6 C9 C22 111.8(6) . . ?
N8 C9 C22 110.3(6) . . ?
N6 C9 C8 103.0(5) . . ?
N8 C9 C8 102.5(5) . . ?
C22 C9 C8 115.6(6) . . ?
O5 C10 N8 126.3(7) . . ?
O5 C10 N7 124.5(7) . . ?
N8 C10 N7 109.1(6) . . ?
N6 C11 N9 113.7(5) . . ?
N6 C11 H11A 108.8 . . ?
N9 C11 H11A 108.8 . . ?
N6 C11 H11B 108.8 . . ?
N9 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
N8 C12 N11 114.3(5) . . ?
N8 C12 H12A 108.7 . . ?
N11 C12 H12A 108.7 . . ?
N8 C12 H12B 108.7 . . ?
N11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N9 126.3(6) . . ?
O3 C13 N10 126.3(6) . . ?
N9 C13 N10 107.3(6) . . ?
O7 C14 N9 108.9(6) . . ?
O7 C14 N11 111.7(6) . . ?
N9 C14 N11 112.1(5) . . ?
O7 C14 C15 116.0(7) . . ?
N9 C14 C15 104.2(5) . . ?
N11 C14 C15 103.7(5) . . ?
O8 C15 N10 106.5(7) . . ?
O8 C15 N12 112.9(7) . . ?
N10 C15 N12 113.3(6) . . ?
O8 C15 C14 118.2(7) . . ?
N10 C15 C14 102.5(5) . . ?
N12 C15 C14 103.2(5) . . ?
O6 C16 N11 125.0(7) . . ?
O6 C16 N12 126.2(7) . . ?
N11 C16 N12 108.8(6) . . ?
N3 C17 N12 113.6(5) . 2_756 ?
N3 C17 H17A 108.8 . . ?
N12 C17 H17A 108.8 2_756 . ?
N3 C17 H17B 108.8 . . ?
N12 C17 H17B 108.8 2_756 . ?
H17A C17 H17B 107.7 . . ?
N1 C18 N10 113.4(5) . 2_756 ?
N1 C18 H18A 108.9 . . ?
N10 C18 H18A 108.9 2_756 . ?
N1 C18 H18B 108.9 . . ?
N10 C18 H18B 108.9 2_756 . ?
H18A C18 H18B 107.7 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C18 120.4(6) . . ?
C1 N1 C2 114.5(5) . . ?
C18 N1 C2 124.7(6) . . ?
C1 N2 C5 121.4(6) . . ?
C1 N2 C3 112.4(6) . . ?
C5 N2 C3 125.7(6) . . ?
C4 N3 C17 120.2(6) . . ?
C4 N3 C2 112.8(5) . . ?
C17 N3 C2 125.6(6) . . ?
C4 N4 C6 121.3(6) . . ?
C4 N4 C3 112.7(5) . . ?
C6 N4 C3 125.3(5) . . ?
C7 N5 C8 112.5(6) . . ?
C7 N5 C5 119.9(6) . . ?
C8 N5 C5 126.6(6) . . ?
C7 N6 C11 120.9(6) . . ?
C7 N6 C9 112.0(6) . . ?
C11 N6 C9 126.5(6) . . ?
C10 N7 C8 113.1(6) . . ?
C10 N7 C6 121.3(6) . . ?
C8 N7 C6 125.6(6) . . ?
C10 N8 C12 121.5(6) . . ?
C10 N8 C9 113.0(6) . . ?
C12 N8 C9 125.1(6) . . ?
C13 N9 C14 112.5(5) . . ?
C13 N9 C11 120.9(6) . . ?
C14 N9 C11 125.1(5) . . ?
C13 N10 C15 113.5(6) . . ?
C13 N10 C18 121.9(6) . 2_756 ?
C15 N10 C18 123.0(6) . 2_756 ?
C16 N11 C12 121.8(6) . . ?
C16 N11 C14 111.7(5) . . ?
C12 N11 C14 124.4(5) . . ?
C16 N12 C17 121.9(6) . 2_756 ?
C16 N12 C15 112.3(5) . . ?
C17 N12 C15 123.7(6) 2_756 . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.152

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.750 0.250 0.000 148 53 ' '
2 1.000 -0.095 0.250 115 35 ' '
3 0.250 0.250 0.500 148 53 ' '
4 0.750 -0.250 0.500 148 53 ' '
5 1.000 0.095 0.750 115 35 ' '
6 0.250 -0.250 1.000 148 53 ' '
7 0.500 0.405 0.250 115 35 ' '
8 0.500 0.595 0.750 115 35 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1550311'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O14, Tm H16 O8, Cl3, 19(H2 O)'
_chemical_formula_sum            'C44 H106 Cl3 N24 O41 Tm'
_chemical_formula_weight         1902.81

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'
Tm Tm -0.3139 5.2483 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.267(2)
_cell_length_b                   12.3118(11)
_cell_length_c                   14.6937(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.292(3)
_cell_angle_gamma                90.00
_cell_volume                     3824.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1972
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_T_max  0.7077
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8582
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.54
_reflns_number_total             4510
_reflns_number_gt                4199
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.0834P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4510
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.0914(9) 1.0000 0.4398(14) 0.517(13) Uani 1 2 d S . .
Cl2 Cl 0.1524(6) 1.0000 1.2982(7) 0.208(6) Uani 0.50 2 d SP . .
O1W O 0.0276(4) 1.0652(5) 0.8715(6) 0.0522(18) Uani 0.50 1 d P . .
O2W O 0.0494(3) 1.1466(5) 0.9511(5) 0.0452(16) Uani 0.50 1 d P . .
O3W O 0.0691(3) 1.1449(5) 1.0523(5) 0.0436(16) Uani 0.50 1 d P . .
O4W O 0.0784(3) 1.0683(5) 1.1313(6) 0.0540(19) Uani 0.50 1 d P . .
Tm1 Tm 0.0000 1.0000 1.0000 0.02407(14) Uani 1 4 d S . .
C1 C 0.3130(2) 0.8439(3) 0.9930(5) 0.0520(14) Uani 1 1 d . . .
C2 C 0.2744(4) 1.0000 1.0468(7) 0.056(2) Uani 1 2 d S . .
C3 C 0.2519(3) 1.0000 0.9362(8) 0.062(3) Uani 1 2 d S . .
C4 C 0.2704(3) 0.8567(4) 0.8167(5) 0.0667(18) Uani 1 1 d . . .
H4A H 0.2772 0.7780 0.8223 0.080 Uiso 1 1 calc R . .
H4B H 0.2261 0.8689 0.7789 0.080 Uiso 1 1 calc R . .
C5 C 0.3608(3) 0.8471(4) 0.7560(4) 0.0565(14) Uani 1 1 d . . .
C6 C 0.2961(4) 1.0000 0.7063(7) 0.063(2) Uani 1 2 d S . .
C7 C 0.3475(5) 1.0000 0.6576(6) 0.062(2) Uani 1 2 d S . .
C8 C 0.4335(4) 0.8545(5) 0.6634(5) 0.0685(18) Uani 1 1 d . . .
H8A H 0.4358 0.7765 0.6775 0.082 Uiso 1 1 calc R . .
H8B H 0.4214 0.8627 0.5936 0.082 Uiso 1 1 calc R . .
C9 C 0.5437(3) 0.8434(4) 0.7640(5) 0.0605(15) Uani 1 1 d . A .
C10 C 0.5170(5) 1.0000 0.6701(6) 0.058(2) Uani 1 2 d S . .
C11 C 0.5872(5) 1.0000 0.7238(6) 0.063(3) Uani 1 2 d S . .
C12 C 0.3411(3) 0.8577(4) 1.1656(5) 0.0645(17) Uani 1 1 d . . .
H12A H 0.3126 0.8713 1.2034 0.077 Uiso 1 1 calc R . .
H12B H 0.3451 0.7788 1.1608 0.077 Uiso 1 1 calc R . .
C13 C 0.2201(5) 1.0000 1.0900(10) 0.087(4) Uani 1 2 d S . .
H13A H 0.1962 0.9331 1.0730 0.131 Uiso 0.50 1 calc PR . .
H13B H 0.1925 1.0614 1.0652 0.131 Uiso 0.50 1 calc PR . .
H13C H 0.2372 1.0055 1.1592 0.131 Uiso 0.50 1 calc PR . .
C14 C 0.1790(4) 1.0000 0.8853(11) 0.102(4) Uani 1 2 d S . .
H14A H 0.1608 1.0657 0.9020 0.153 Uiso 0.50 1 calc PR . .
H14B H 0.1604 0.9371 0.9058 0.153 Uiso 0.50 1 calc PR . .
H14C H 0.1705 0.9972 0.8164 0.153 Uiso 1 2 calc SR . .
C15 C 0.2300(6) 1.0000 0.6358(10) 0.120(6) Uani 1 2 d S . .
H15A H 0.2231 0.9333 0.5988 0.180 Uiso 0.50 1 calc PR . .
H15B H 0.2251 1.0617 0.5930 0.180 Uiso 0.50 1 calc PR . .
H15C H 0.1995 1.0050 0.6703 0.180 Uiso 0.50 1 calc PR . .
C16 C 0.3268(8) 1.0000 0.5472(7) 0.118(5) Uani 1 2 d S . .
H16A H 0.3023 0.9350 0.5231 0.177 Uiso 0.50 1 calc PR . .
H16B H 0.3639 1.0014 0.5260 0.177 Uiso 1 2 calc SR . .
H16C H 0.3010 1.0636 0.5230 0.177 Uiso 0.50 1 calc PR . .
N1 N 0.3124(2) 0.9002(3) 1.0710(4) 0.0562(12) Uani 1 1 d . . .
N2 N 0.2809(2) 0.9011(3) 0.9121(4) 0.0587(13) Uani 1 1 d . . .
N3 N 0.3099(2) 0.9014(3) 0.7653(4) 0.0597(13) Uani 1 1 d . . .
N4 N 0.3848(3) 0.9014(3) 0.6959(3) 0.0586(12) Uani 1 1 d . . .
N5 N 0.4950(3) 0.9007(3) 0.7052(3) 0.0581(12) Uani 1 1 d . A .
N6 N 0.5980(3) 0.9009(3) 0.7831(4) 0.0614(13) Uani 1 1 d . . .
O1 O 0.33672(18) 0.7539(3) 0.9921(3) 0.0601(11) Uani 1 1 d . . .
O2 O 0.3812(3) 0.7610(3) 0.7950(4) 0.0814(14) Uani 1 1 d . . .
O3 O 0.5391(3) 0.7527(3) 0.7949(4) 0.0933(17) Uani 1 1 d . . .
O4 O 0.5062(8) 1.0000 0.5795(8) 0.097(5) Uani 0.599(16) 2 d SP A 1
O5 O 0.6206(11) 1.0000 0.6589(13) 0.090(8) Uani 0.401(16) 2 d SP . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W O2W 1.500(10) . ?
O1W O1W 1.605(12) 6_575 ?
O1W Tm1 2.305(7) . ?
O2W O3W 1.413(10) . ?
O2W Tm1 2.341(6) . ?
O3W O4W 1.459(10) . ?
O3W Tm1 2.324(6) . ?
O4W O4W 1.681(13) 6_575 ?
O4W Tm1 2.315(6) . ?
Tm1 O1W 2.305(7) 2_557 ?
Tm1 O1W 2.305(7) 6_575 ?
Tm1 O1W 2.305(7) 5_577 ?
Tm1 O4W 2.315(7) 5_577 ?
Tm1 O4W 2.315(7) 2_557 ?
Tm1 O4W 2.315(7) 6_575 ?
Tm1 O3W 2.324(6) 5_577 ?
Tm1 O3W 2.324(6) 2_557 ?
Tm1 O3W 2.324(6) 6_575 ?
C1 O1 1.230(5) . ?
C1 N1 1.343(8) . ?
C1 N2 1.374(8) . ?
C2 N1 1.471(6) 6_575 ?
C2 N1 1.471(6) . ?
C2 C13 1.531(11) . ?
C2 C3 1.543(14) . ?
C3 N2 1.472(6) 6_575 ?
C3 N2 1.472(6) . ?
C3 C14 1.560(11) . ?
C4 N3 1.436(8) . ?
C4 N2 1.453(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.223(6) . ?
C5 N4 1.345(8) . ?
C5 N3 1.359(8) . ?
C6 N3 1.467(6) 6_575 ?
C6 N3 1.467(6) . ?
C6 C15 1.510(12) . ?
C6 C7 1.530(14) . ?
C7 N4 1.479(6) 6_575 ?
C7 N4 1.479(6) . ?
C7 C16 1.541(12) . ?
C8 N5 1.432(8) . ?
C8 N4 1.436(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.221(6) . ?
C9 N6 1.353(8) . ?
C9 N5 1.354(8) . ?
C10 O4 1.276(13) . ?
C10 N5 1.469(6) 6_575 ?
C10 N5 1.469(6) . ?
C10 C11 1.515(14) . ?
C11 O5 1.380(15) . ?
C11 N6 1.475(6) 6_575 ?
C11 N6 1.475(6) . ?
C12 N6 1.431(8) 2_657 ?
C12 N1 1.435(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
N6 C12 1.431(8) 2_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
O2W O1W O1W 131.9(4) . 6_575 ?
O2W O1W Tm1 72.5(4) . . ?
O1W O1W Tm1 69.63(16) 6_575 . ?
O3W O2W O1W 136.7(6) . . ?
O3W O2W Tm1 71.7(4) . . ?
O1W O2W Tm1 69.9(3) . . ?
O2W O3W O4W 140.0(6) . . ?
O2W O3W Tm1 73.0(4) . . ?
O4W O3W Tm1 71.3(3) . . ?
O3W O4W O4W 130.3(4) . 6_575 ?
O3W O4W Tm1 72.0(4) . . ?
O4W O4W Tm1 68.71(17) 6_575 . ?
O1W Tm1 O1W 180.00(18) 2_557 6_575 ?
O1W Tm1 O1W 139.3(3) 2_557 . ?
O1W Tm1 O1W 40.7(3) 6_575 . ?
O1W Tm1 O1W 40.7(3) 2_557 5_577 ?
O1W Tm1 O1W 139.3(3) 6_575 5_577 ?
O1W Tm1 O1W 180.000(2) . 5_577 ?
O1W Tm1 O4W 118.9(3) 2_557 5_577 ?
O1W Tm1 O4W 61.1(3) 6_575 5_577 ?
O1W Tm1 O4W 76.6(3) . 5_577 ?
O1W Tm1 O4W 103.4(3) 5_577 5_577 ?
O1W Tm1 O4W 103.4(3) 2_557 2_557 ?
O1W Tm1 O4W 76.6(3) 6_575 2_557 ?
O1W Tm1 O4W 61.1(3) . 2_557 ?
O1W Tm1 O4W 118.9(3) 5_577 2_557 ?
O4W Tm1 O4W 42.6(3) 5_577 2_557 ?
O1W Tm1 O4W 61.1(3) 2_557 . ?
O1W Tm1 O4W 118.9(3) 6_575 . ?
O1W Tm1 O4W 103.4(3) . . ?
O1W Tm1 O4W 76.6(3) 5_577 . ?
O4W Tm1 O4W 180.000(2) 5_577 . ?
O4W Tm1 O4W 137.4(3) 2_557 . ?
O1W Tm1 O4W 76.6(3) 2_557 6_575 ?
O1W Tm1 O4W 103.4(3) 6_575 6_575 ?
O1W Tm1 O4W 118.9(3) . 6_575 ?
O1W Tm1 O4W 61.1(3) 5_577 6_575 ?
O4W Tm1 O4W 137.4(3) 5_577 6_575 ?
O4W Tm1 O4W 180.000(2) 2_557 6_575 ?
O4W Tm1 O4W 42.6(3) . 6_575 ?
O1W Tm1 O3W 77.3(2) 2_557 . ?
O1W Tm1 O3W 102.7(2) 6_575 . ?
O1W Tm1 O3W 71.6(3) . . ?
O1W Tm1 O3W 108.4(3) 5_577 . ?
O4W Tm1 O3W 143.3(2) 5_577 . ?
O4W Tm1 O3W 104.2(2) 2_557 . ?
O4W Tm1 O3W 36.7(2) . . ?
O4W Tm1 O3W 75.8(2) 6_575 . ?
O1W Tm1 O3W 102.7(2) 2_557 5_577 ?
O1W Tm1 O3W 77.3(2) 6_575 5_577 ?
O1W Tm1 O3W 108.4(3) . 5_577 ?
O1W Tm1 O3W 71.6(3) 5_577 5_577 ?
O4W Tm1 O3W 36.7(2) 5_577 5_577 ?
O4W Tm1 O3W 75.8(2) 2_557 5_577 ?
O4W Tm1 O3W 143.3(2) . 5_577 ?
O4W Tm1 O3W 104.2(2) 6_575 5_577 ?
O3W Tm1 O3W 180.000(1) . 5_577 ?
O1W Tm1 O3W 71.6(3) 2_557 2_557 ?
O1W Tm1 O3W 108.4(3) 6_575 2_557 ?
O1W Tm1 O3W 77.3(2) . 2_557 ?
O1W Tm1 O3W 102.7(2) 5_577 2_557 ?
O4W Tm1 O3W 75.8(2) 5_577 2_557 ?
O4W Tm1 O3W 36.7(2) 2_557 2_557 ?
O4W Tm1 O3W 104.2(2) . 2_557 ?
O4W Tm1 O3W 143.3(2) 6_575 2_557 ?
O3W Tm1 O3W 79.7(3) . 2_557 ?
O3W Tm1 O3W 100.3(3) 5_577 2_557 ?
O1W Tm1 O3W 108.4(3) 2_557 6_575 ?
O1W Tm1 O3W 71.6(3) 6_575 6_575 ?
O1W Tm1 O3W 102.7(2) . 6_575 ?
O1W Tm1 O3W 77.3(2) 5_577 6_575 ?
O4W Tm1 O3W 104.2(2) 5_577 6_575 ?
O4W Tm1 O3W 143.3(2) 2_557 6_575 ?
O4W Tm1 O3W 75.8(2) . 6_575 ?
O4W Tm1 O3W 36.7(2) 6_575 6_575 ?
O3W Tm1 O3W 100.3(3) . 6_575 ?
O3W Tm1 O3W 79.7(3) 5_577 6_575 ?
O3W Tm1 O3W 180.000(2) 2_557 6_575 ?
O1 C1 N1 126.4(6) . . ?
O1 C1 N2 124.2(6) . . ?
N1 C1 N2 109.4(4) . . ?
N1 C2 N1 113.4(6) 6_575 . ?
N1 C2 C13 111.6(5) 6_575 . ?
N1 C2 C13 111.6(5) . . ?
N1 C2 C3 103.1(5) 6_575 . ?
N1 C2 C3 103.1(5) . . ?
C13 C2 C3 113.5(8) . . ?
N2 C3 N2 111.6(6) 6_575 . ?
N2 C3 C2 103.4(5) 6_575 . ?
N2 C3 C2 103.4(5) . . ?
N2 C3 C14 110.6(5) 6_575 . ?
N2 C3 C14 110.6(5) . . ?
C2 C3 C14 116.8(8) . . ?
N3 C4 N2 115.1(4) . . ?
N3 C4 H4A 108.5 . . ?
N2 C4 H4A 108.5 . . ?
N3 C4 H4B 108.5 . . ?
N2 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N4 124.9(6) . . ?
O2 C5 N3 125.4(6) . . ?
N4 C5 N3 109.7(5) . . ?
N3 C6 N3 111.7(7) 6_575 . ?
N3 C6 C15 112.6(5) 6_575 . ?
N3 C6 C15 112.6(5) . . ?
N3 C6 C7 103.1(5) 6_575 . ?
N3 C6 C7 103.1(5) . . ?
C15 C6 C7 112.9(9) . . ?
N4 C7 N4 110.4(6) 6_575 . ?
N4 C7 C6 103.6(5) 6_575 . ?
N4 C7 C6 103.6(5) . . ?
N4 C7 C16 110.3(6) 6_575 . ?
N4 C7 C16 110.3(6) . . ?
C6 C7 C16 118.1(9) . . ?
N5 C8 N4 114.7(5) . . ?
N5 C8 H8A 108.6 . . ?
N4 C8 H8A 108.6 . . ?
N5 C8 H8B 108.6 . . ?
N4 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
O3 C9 N6 125.1(7) . . ?
O3 C9 N5 124.8(7) . . ?
N6 C9 N5 110.1(5) . . ?
O4 C10 N5 113.1(6) . 6_575 ?
O4 C10 N5 113.1(6) . . ?
N5 C10 N5 112.6(7) 6_575 . ?
O4 C10 C11 111.6(10) . . ?
N5 C10 C11 102.7(5) 6_575 . ?
N5 C10 C11 102.7(5) . . ?
O5 C11 N6 112.7(7) . 6_575 ?
O5 C11 N6 112.7(6) . . ?
N6 C11 N6 111.7(7) 6_575 . ?
O5 C11 C10 109.4(12) . . ?
N6 C11 C10 104.9(5) 6_575 . ?
N6 C11 C10 104.9(5) . . ?
N6 C12 N1 115.8(4) 2_657 . ?
N6 C12 H12A 108.3 2_657 . ?
N1 C12 H12A 108.3 . . ?
N6 C12 H12B 108.3 2_657 . ?
N1 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 H15A 109.5 . . ?
C6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C16 H16A 109.5 . . ?
C7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C12 121.2(4) . . ?
C1 N1 C2 112.6(6) . . ?
C12 N1 C2 125.9(6) . . ?
C1 N2 C4 121.6(4) . . ?
C1 N2 C3 111.3(6) . . ?
C4 N2 C3 126.4(6) . . ?
C5 N3 C4 122.1(5) . . ?
C5 N3 C6 112.0(6) . . ?
C4 N3 C6 125.3(6) . . ?
C5 N4 C8 121.1(5) . . ?
C5 N4 C7 111.5(6) . . ?
C8 N4 C7 126.6(6) . . ?
C9 N5 C8 122.2(5) . . ?
C9 N5 C10 111.7(6) . . ?
C8 N5 C10 124.0(6) . . ?
C9 N6 C12 123.5(5) . 2_657 ?
C9 N6 C11 110.0(6) . . ?
C12 N6 C11 124.7(6) 2_657 . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.137

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 118 36 ' '
2 0.934 -0.005 0.500 942 298 ' '
3 0.000 0.500 0.000 118 36 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex6
_database_code_depnum_ccdc_archive 'CCDC 1550310'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C44 H52 N24 O14, Er H16 O8, 2(N O3), Cl, 7(H2 O)'
_chemical_formula_sum            'C44 H82 Cl Er N26 O35'
_chemical_formula_weight         1738.07

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'
Er Er -0.2586 4.9576 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.449(18)
_cell_length_b                   12.430(10)
_cell_length_c                   26.83(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.018(11)
_cell_angle_gamma                90.00
_cell_volume                     6940(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3572
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7104
_exptl_absorpt_correction_T_max  0.7634
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14787
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5942
_reflns_number_gt                5379
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.1234P)²+22.9867P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    costr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5942
_refine_ls_number_parameters     502
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1842
_refine_ls_wR_factor_gt          0.1735
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.127
_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
Cl1 Cl 1.1270(13) -0.4149(13) 0.9212(6) 0.309(15) Uani 0.50 1 d P . .
N13 N 1.0461(6) -0.3082(10) 0.5591(4) 0.098(3) Uani 1 1 d . . .
O9 O 1.0369(9) -0.3959(8) 0.5814(4) 0.158(7) Uani 1 1 d . . .
O10 O 1.0981(4) -0.2563(12) 0.5706(4) 0.131(4) Uani 1 1 d . . .
O11 O 0.9960(4) -0.2673(8) 0.5235(3) 0.112(3) Uani 1 1 d . . .
O1W O 1.0709(4) -0.5497(7) 0.7837(3) 0.0284(18) Uani 0.50 1 d PU . .
O2W O 1.0805(8) -0.4831(14) 0.8238(7) 0.091(4) Uani 0.50 1 d PU . .
O3W O 1.0788(4) -0.3354(8) 0.8270(4) 0.040(2) Uani 0.50 1 d PU . .
O4W O 1.0713(7) -0.2662(12) 0.7787(7) 0.083(5) Uani 0.50 1 d P . .
O5W O 0.9472(4) -0.2639(7) 0.7736(4) 0.033(2) Uani 0.50 1 d P . .
O6W O 0.9778(10) -0.3444(12) 0.8215(6) 0.098(6) Uani 0.50 1 d P . .
O7W O 0.9707(4) -0.4703(7) 0.8192(3) 0.0309(19) Uani 0.50 1 d PU . .
O8W O 0.9472(6) -0.5511(13) 0.7730(6) 0.077(4) Uani 0.50 1 d P . .
Er1 Er 1.0000 -0.40629(3) 0.7500 0.02092(18) Uani 1 2 d S . .
C1 C 0.8134(3) -0.0638(6) 0.7464(3) 0.0400(17) Uani 1 1 d . . .
C2 C 0.7804(3) 0.0939(5) 0.7765(3) 0.0321(16) Uani 1 1 d . . .
C3 C 0.7495(3) 0.0907(5) 0.7134(3) 0.0300(15) Uani 1 1 d . . .
C4 C 0.8132(3) 0.2469(5) 0.7420(3) 0.0323(15) Uani 1 1 d . . .
C5 C 0.7608(3) -0.0522(6) 0.6480(3) 0.0396(16) Uani 1 1 d . . .
H5A H 0.7149 -0.0410 0.6273 0.048 Uiso 1 1 calc R . .
H5B H 0.7685 -0.1299 0.6511 0.048 Uiso 1 1 calc R . .
C6 C 0.7556(3) 0.2314(6) 0.6454(3) 0.0370(15) Uani 1 1 d . . .
H6A H 0.7602 0.3098 0.6477 0.044 Uiso 1 1 calc R . .
H6B H 0.7099 0.2153 0.6262 0.044 Uiso 1 1 calc R . .
C7 C 0.8482(3) -0.0586(6) 0.6126(3) 0.0392(16) Uani 1 1 d . . .
C8 C 0.7789(4) 0.0890(5) 0.5830(3) 0.0390(18) Uani 1 1 d . . .
C9 C 0.8302(4) 0.0902(5) 0.5568(3) 0.0343(16) Uani 1 1 d . . .
C10 C 0.8419(3) 0.2457(6) 0.6077(3) 0.0380(16) Uani 1 1 d . . .
C11 C 0.9162(3) -0.0507(6) 0.5599(3) 0.0397(16) Uani 1 1 d . . .
H11A H 0.9018 -0.0402 0.5210 0.048 Uiso 1 1 calc R . .
H11B H 0.9189 -0.1284 0.5667 0.048 Uiso 1 1 calc R . .
C12 C 0.9148(3) 0.2361(6) 0.5592(3) 0.0362(15) Uani 1 1 d . . .
H12A H 0.9014 0.2246 0.5204 0.043 Uiso 1 1 calc R . .
H12B H 0.9170 0.3139 0.5654 0.043 Uiso 1 1 calc R . .
C13 C 1.0299(3) -0.0621(6) 0.6207(3) 0.0346(15) Uani 1 1 d . A .
C14 C 1.0002(4) 0.0942(5) 0.5667(3) 0.0326(16) Uani 1 1 d . . .
C15 C 1.0738(4) 0.0962(5) 0.5981(3) 0.0345(16) Uani 1 1 d . A .
C16 C 1.0272(4) 0.2468(6) 0.6216(3) 0.0397(16) Uani 1 1 d . . .
C17 C 1.1492(3) -0.0486(6) 0.6581(3) 0.0421(17) Uani 1 1 d . . .
H17A H 1.1451 -0.1267 0.6607 0.050 Uiso 1 1 calc R . .
H17B H 1.1755 -0.0354 0.6367 0.050 Uiso 1 1 calc R . .
C18 C 1.1461(3) 0.2386(6) 0.6610(3) 0.0392(16) Uani 1 1 d . . .
H18A H 1.1725 0.2302 0.6393 0.047 Uiso 1 1 calc R A .
H18B H 1.1412 0.3158 0.6657 0.047 Uiso 1 1 calc R . .
C19 C 0.7323(4) 0.0984(6) 0.8047(4) 0.047(2) Uani 1 1 d . . .
H19A H 0.7087 0.1658 0.7960 0.070 Uiso 1 1 calc R . .
H19B H 0.7552 0.0936 0.8433 0.070 Uiso 1 1 calc R . .
H19C H 0.7024 0.0388 0.7926 0.070 Uiso 1 1 calc R . .
C20 C 0.6763(3) 0.0887(6) 0.6896(4) 0.048(2) Uani 1 1 d . . .
H20A H 0.6598 0.1556 0.6981 0.072 Uiso 1 1 calc R . .
H20B H 0.6609 0.0289 0.7048 0.072 Uiso 1 1 calc R . .
H20C H 0.6614 0.0803 0.6509 0.072 Uiso 1 1 calc R . .
C21 C 0.7094(4) 0.0829(7) 0.5434(4) 0.059(2) Uani 1 1 d . . .
H21A H 0.6991 0.1468 0.5210 0.088 Uiso 1 1 calc R . .
H21B H 0.6810 0.0785 0.5631 0.088 Uiso 1 1 calc R . .
H21C H 0.7037 0.0197 0.5210 0.088 Uiso 1 1 calc R . .
C22 C 0.8061(5) 0.0890(7) 0.4921(4) 0.064(3) Uani 1 1 d . . .
H22A H 0.7814 0.1535 0.4777 0.097 Uiso 1 1 calc R . .
H22B H 0.7795 0.0261 0.4781 0.097 Uiso 1 1 calc R . .
H22C H 0.8431 0.0867 0.4817 0.097 Uiso 1 1 calc R . .
N1 N 0.8182(3) -0.0069(4) 0.7895(2) 0.0343(13) Uani 1 1 d . . .
N2 N 0.7766(3) -0.0076(4) 0.7017(2) 0.0350(13) Uani 1 1 d . . .
N3 N 0.8208(3) 0.1915(4) 0.7876(2) 0.0324(12) Uani 1 1 d . . .
N4 N 0.7750(3) 0.1889(4) 0.6991(2) 0.0339(13) Uani 1 1 d . . .
N5 N 0.7978(3) -0.0048(4) 0.6178(2) 0.0372(13) Uani 1 1 d . . .
N6 N 0.8684(3) -0.0059(5) 0.5781(2) 0.0363(13) Uani 1 1 d . . .
N7 N 0.7916(3) 0.1901(4) 0.6133(2) 0.0357(13) Uani 1 1 d . . .
N8 N 0.8654(3) 0.1910(5) 0.5768(2) 0.0344(13) Uani 1 1 d . . .
N9 N 0.9798(3) -0.0048(4) 0.5852(2) 0.0334(12) Uani 1 1 d . A .
N10 N 1.0854(3) -0.0033(5) 0.6297(3) 0.0378(13) Uani 1 1 d . . .
N11 N 0.9781(3) 0.1915(4) 0.5855(2) 0.0334(12) Uani 1 1 d . A .
N12 N 1.0831(3) 0.1926(4) 0.6318(2) 0.0338(12) Uani 1 1 d . A .
O1 O 0.8352(3) -0.1547(4) 0.7459(3) 0.0525(14) Uani 1 1 d . . .
O2 O 0.8701(3) -0.1440(5) 0.6351(3) 0.0626(17) Uani 1 1 d . . .
O3 O 1.0260(3) -0.1498(4) 0.6383(2) 0.0526(14) Uani 1 1 d . . .
O4 O 0.8354(2) 0.3360(4) 0.7401(2) 0.0425(12) Uani 1 1 d . . .
O5 O 0.8594(3) 0.3351(4) 0.6274(2) 0.0520(14) Uani 1 1 d . . .
O6 O 1.0210(3) 0.3342(5) 0.6407(3) 0.0646(17) Uani 1 1 d . A .
O7 O 0.9799(6) 0.0907(7) 0.5114(4) 0.053(4) Uani 0.573(17) 1 d P A 1
O8 O 1.1163(7) 0.0916(10) 0.5719(6) 0.047(4) Uani 0.427(17) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N13 O10 1.267(15) . ?
N13 O11 1.277(13) . ?
N13 O9 1.297(14) . ?
O1W O2W 1.308(19) . ?
O1W O8W 1.421(18) 2_756 ?
O1W Er1 2.334(8) . ?
O2W Er1 2.327(16) . ?
O3W O4W 1.51(2) . ?
O3W Er1 2.331(9) . ?
O4W O5W 1.307(19) 2_756 ?
O4W Er1 2.294(12) . ?
O5W O4W 1.307(19) 2_756 ?
O5W O6W 1.569(19) . ?
O5W Er1 2.346(8) . ?
O6W O7W 1.572(19) . ?
O6W Er1 2.288(11) . ?
O7W O8W 1.528(19) . ?
O7W Er1 2.331(7) . ?
O8W O1W 1.421(18) 2_756 ?
O8W Er1 2.361(13) . ?
Er1 O6W 2.288(11) 2_756 ?
Er1 O4W 2.294(12) 2_756 ?
Er1 O2W 2.327(16) 2_756 ?
Er1 O7W 2.331(7) 2_756 ?
Er1 O3W 2.331(9) 2_756 ?
Er1 O1W 2.334(8) 2_756 ?
C1 O1 1.233(9) . ?
C1 N1 1.324(10) . ?
C1 N2 1.367(10) . ?
C2 N3 1.476(8) . ?
C2 N1 1.480(8) . ?
C2 C19 1.535(10) . ?
C2 C3 1.570(11) . ?
C3 N2 1.451(8) . ?
C3 N4 1.459(8) . ?
C3 C20 1.526(9) . ?
C4 O4 1.225(8) . ?
C4 N4 1.356(9) . ?
C4 N3 1.357(9) . ?
C5 N2 1.457(10) . ?
C5 N5 1.482(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.440(9) . ?
C6 N7 1.476(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.228(10) . ?
C7 N6 1.344(10) . ?
C7 N5 1.368(9) . ?
C8 N5 1.455(9) . ?
C8 N7 1.466(9) . ?
C8 C21 1.525(10) . ?
C8 C9 1.556(12) . ?
C9 N6 1.457(9) . ?
C9 N8 1.471(8) . ?
C9 C22 1.613(11) . ?
C10 O5 1.230(9) . ?
C10 N8 1.326(10) . ?
C10 N7 1.380(9) . ?
C11 N6 1.444(9) . ?
C11 N9 1.449(9) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.440(9) . ?
C12 N8 1.469(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.204(9) . ?
C13 N9 1.369(9) . ?
C13 N10 1.386(9) . ?
C14 O7 1.379(12) . ?
C14 N9 1.464(8) . ?
C14 N11 1.467(8) . ?
C14 C15 1.548(11) . ?
C15 O8 1.385(15) . ?
C15 N10 1.467(9) . ?
C15 N12 1.467(8) . ?
C16 O6 1.230(9) . ?
C16 N11 1.352(9) . ?
C16 N12 1.358(9) . ?
C17 N1 1.419(9) 2_756 ?
C17 N10 1.459(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N3 1.424(9) 2_756 ?
C18 N12 1.453(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N1 C17 1.419(9) 2_756 ?
N3 C18 1.424(9) 2_756 ?

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
O10 N13 O11 116.9(12) . . ?
O10 N13 O9 127.4(13) . . ?
O11 N13 O9 115.6(15) . . ?
O2W O1W O8W 141.3(12) . 2_756 ?
O2W O1W Er1 73.4(8) . . ?
O8W O1W Er1 73.4(6) 2_756 . ?
O1W O2W Er1 74.0(8) . . ?
O4W O3W Er1 69.6(6) . . ?
O5W O4W O3W 145.3(11) 2_756 . ?
O5W O4W Er1 75.8(7) 2_756 . ?
O3W O4W Er1 72.3(6) . . ?
O4W O5W O6W 136.9(10) 2_756 . ?
O4W O5W Er1 71.5(7) 2_756 . ?
O6W O5W Er1 68.2(6) . . ?
O5W O6W O7W 126.6(11) . . ?
O5W O6W Er1 72.2(5) . . ?
O7W O6W Er1 71.6(5) . . ?
O8W O7W O6W 133.2(9) . . ?
O8W O7W Er1 72.1(5) . . ?
O6W O7W Er1 68.7(4) . . ?
O1W O8W O7W 137.3(11) 2_756 . ?
O1W O8W Er1 71.4(6) 2_756 . ?
O7W O8W Er1 69.9(6) . . ?
O6W Er1 O6W 140.7(8) 2_756 . ?
O6W Er1 O4W 71.5(7) 2_756 . ?
O6W Er1 O4W 78.9(6) . . ?
O6W Er1 O4W 78.9(6) 2_756 2_756 ?
O6W Er1 O4W 71.5(7) . 2_756 ?
O4W Er1 O4W 81.3(8) . 2_756 ?
O6W Er1 O2W 76.6(7) 2_756 2_756 ?
O6W Er1 O2W 120.5(7) . 2_756 ?
O4W Er1 O2W 145.0(7) . 2_756 ?
O4W Er1 O2W 78.7(6) 2_756 2_756 ?
O6W Er1 O2W 120.5(7) 2_756 . ?
O6W Er1 O2W 76.6(7) . . ?
O4W Er1 O2W 78.7(6) . . ?
O4W Er1 O2W 145.0(7) 2_756 . ?
O2W Er1 O2W 131.5(9) 2_756 . ?
O6W Er1 O7W 39.8(5) 2_756 2_756 ?
O6W Er1 O7W 176.4(5) . 2_756 ?
O4W Er1 O7W 99.0(5) . 2_756 ?
O4W Er1 O7W 111.2(5) 2_756 2_756 ?
O2W Er1 O7W 62.8(5) 2_756 2_756 ?
O2W Er1 O7W 100.2(5) . 2_756 ?
O6W Er1 O7W 176.4(5) 2_756 . ?
O6W Er1 O7W 39.8(5) . . ?
O4W Er1 O7W 111.2(5) . . ?
O4W Er1 O7W 99.0(5) 2_756 . ?
O2W Er1 O7W 100.2(5) 2_756 . ?
O2W Er1 O7W 62.8(5) . . ?
O7W Er1 O7W 140.1(4) 2_756 . ?
O6W Er1 O3W 106.5(6) 2_756 . ?
O6W Er1 O3W 57.4(6) . . ?
O4W Er1 O3W 38.1(5) . . ?
O4W Er1 O3W 102.3(5) 2_756 . ?
O2W Er1 O3W 176.8(5) 2_756 . ?
O2W Er1 O3W 46.5(5) . . ?
O7W Er1 O3W 119.2(4) 2_756 . ?
O7W Er1 O3W 76.7(4) . . ?
O6W Er1 O3W 57.4(6) 2_756 2_756 ?
O6W Er1 O3W 106.5(6) . 2_756 ?
O4W Er1 O3W 102.3(5) . 2_756 ?
O4W Er1 O3W 38.1(5) 2_756 2_756 ?
O2W Er1 O3W 46.5(5) 2_756 2_756 ?
O2W Er1 O3W 176.8(5) . 2_756 ?
O7W Er1 O3W 76.7(4) 2_756 2_756 ?
O7W Er1 O3W 119.2(4) . 2_756 ?
O3W Er1 O3W 135.6(5) . 2_756 ?
O6W Er1 O1W 105.2(5) 2_756 2_756 ?
O6W Er1 O1W 104.5(5) . 2_756 ?
O4W Er1 O1W 176.6(4) . 2_756 ?
O4W Er1 O1W 99.2(5) 2_756 2_756 ?
O2W Er1 O1W 32.6(5) 2_756 2_756 ?
O2W Er1 O1W 102.5(5) . 2_756 ?
O7W Er1 O1W 77.6(3) 2_756 2_756 ?
O7W Er1 O1W 72.1(3) . 2_756 ?
O3W Er1 O1W 144.4(3) . 2_756 ?
O3W Er1 O1W 76.4(3) 2_756 2_756 ?
O6W Er1 O1W 104.5(5) 2_756 . ?
O6W Er1 O1W 105.2(5) . . ?
O4W Er1 O1W 99.2(5) . . ?
O4W Er1 O1W 176.6(4) 2_756 . ?
O2W Er1 O1W 102.5(5) 2_756 . ?
O2W Er1 O1W 32.6(5) . . ?
O7W Er1 O1W 72.1(3) 2_756 . ?
O7W Er1 O1W 77.6(3) . . ?
O3W Er1 O1W 76.4(3) . . ?
O3W Er1 O1W 144.4(3) 2_756 . ?
O1W Er1 O1W 80.5(5) 2_756 . ?
O1 C1 N1 126.6(8) . . ?
O1 C1 N2 124.8(8) . . ?
N1 C1 N2 108.5(6) . . ?
N3 C2 N1 113.2(5) . . ?
N3 C2 C19 111.3(6) . . ?
N1 C2 C19 111.2(6) . . ?
N3 C2 C3 103.2(5) . . ?
N1 C2 C3 102.4(5) . . ?
C19 C2 C3 115.1(6) . . ?
N2 C3 N4 114.2(6) . . ?
N2 C3 C20 111.6(6) . . ?
N4 C3 C20 111.8(6) . . ?
N2 C3 C2 101.8(5) . . ?
N4 C3 C2 101.8(5) . . ?
C20 C3 C2 115.0(6) . . ?
O4 C4 N4 125.7(7) . . ?
O4 C4 N3 125.5(7) . . ?
N4 C4 N3 108.8(6) . . ?
N2 C5 N5 114.2(6) . . ?
N2 C5 H5A 108.7 . . ?
N5 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
N5 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N4 C6 N7 115.5(5) . . ?
N4 C6 H6A 108.4 . . ?
N7 C6 H6A 108.4 . . ?
N4 C6 H6B 108.4 . . ?
N7 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
O2 C7 N6 125.7(7) . . ?
O2 C7 N5 124.4(7) . . ?
N6 C7 N5 109.8(6) . . ?
N5 C8 N7 112.4(6) . . ?
N5 C8 C21 112.5(6) . . ?
N7 C8 C21 111.3(6) . . ?
N5 C8 C9 102.2(5) . . ?
N7 C8 C9 102.7(5) . . ?
C21 C8 C9 115.1(7) . . ?
N6 C9 N8 113.5(6) . . ?
N6 C9 C8 104.1(5) . . ?
N8 C9 C8 103.4(5) . . ?
N6 C9 C22 108.9(6) . . ?
N8 C9 C22 108.5(6) . . ?
C8 C9 C22 118.6(7) . . ?
O5 C10 N8 126.4(7) . . ?
O5 C10 N7 123.3(7) . . ?
N8 C10 N7 110.2(6) . . ?
N6 C11 N9 114.5(6) . . ?
N6 C11 H11A 108.6 . . ?
N9 C11 H11A 108.6 . . ?
N6 C11 H11B 108.6 . . ?
N9 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N11 C12 N8 114.8(5) . . ?
N11 C12 H12A 108.6 . . ?
N8 C12 H12A 108.6 . . ?
N11 C12 H12B 108.6 . . ?
N8 C12 H12B 108.6 . . ?
H12A C12 H12B 107.5 . . ?
O3 C13 N9 125.5(7) . . ?
O3 C13 N10 127.0(7) . . ?
N9 C13 N10 107.4(6) . . ?
O7 C14 N9 108.6(6) . . ?
O7 C14 N11 112.2(7) . . ?
N9 C14 N11 112.7(6) . . ?
O7 C14 C15 116.2(8) . . ?
N9 C14 C15 103.6(5) . . ?
N11 C14 C15 103.2(5) . . ?
O8 C15 N10 104.6(8) . . ?
O8 C15 N12 112.4(7) . . ?
N10 C15 N12 112.3(6) . . ?
O8 C15 C14 121.4(9) . . ?
N10 C15 C14 103.0(5) . . ?
N12 C15 C14 103.0(5) . . ?
O6 C16 N11 123.9(7) . . ?
O6 C16 N12 126.5(7) . . ?
N11 C16 N12 109.6(6) . . ?
N1 C17 N10 114.6(6) 2_756 . ?
N1 C17 H17A 108.6 2_756 . ?
N10 C17 H17A 108.6 . . ?
N1 C17 H17B 108.6 2_756 . ?
N10 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
N3 C18 N12 114.2(6) 2_756 . ?
N3 C18 H18A 108.7 2_756 . ?
N12 C18 H18A 108.7 . . ?
N3 C18 H18B 108.7 2_756 . ?
N12 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C17 120.8(6) . 2_756 ?
C1 N1 C2 113.3(6) . . ?
C17 N1 C2 125.5(6) 2_756 . ?
C1 N2 C3 113.8(6) . . ?
C1 N2 C5 121.2(6) . . ?
C3 N2 C5 124.6(6) . . ?
C4 N3 C18 120.5(6) . 2_756 ?
C4 N3 C2 112.0(6) . . ?
C18 N3 C2 126.3(6) 2_756 . ?
C4 N4 C6 120.9(6) . . ?
C4 N4 C3 113.9(6) . . ?
C6 N4 C3 124.7(6) . . ?
C7 N5 C8 112.2(6) . . ?
C7 N5 C5 121.2(6) . . ?
C8 N5 C5 125.6(6) . . ?
C7 N6 C11 121.9(6) . . ?
C7 N6 C9 111.5(6) . . ?
C11 N6 C9 126.0(6) . . ?
C10 N7 C8 111.5(6) . . ?
C10 N7 C6 122.6(6) . . ?
C8 N7 C6 125.9(6) . . ?
C10 N8 C12 122.0(6) . . ?
C10 N8 C9 112.3(6) . . ?
C12 N8 C9 125.1(6) . . ?
C13 N9 C11 122.0(6) . . ?
C13 N9 C14 113.1(6) . . ?
C11 N9 C14 123.4(6) . . ?
C13 N10 C17 122.0(6) . . ?
C13 N10 C15 112.9(6) . . ?
C17 N10 C15 123.7(6) . . ?
C16 N11 C12 123.1(6) . . ?
C16 N11 C14 112.1(6) . . ?
C12 N11 C14 123.2(6) . . ?
C16 N12 C18 123.5(6) . . ?
C16 N12 C15 112.0(6) . . ?
C18 N12 C15 122.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.227

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.250 0.000 157 47 ' '
2 0.750 0.250 0.000 157 47 ' '
3 1.000 -0.094 0.250 117 19 ' '
4 0.250 0.250 0.500 157 47 ' '
5 0.750 -0.250 0.500 157 47 ' '
6 1.000 0.094 0.750 117 19 ' '
7 0.500 0.406 0.250 117 19 ' '
8 0.500 0.594 0.750 117 19 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex8
_database_code_depnum_ccdc_archive 'CCDC 1550312'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N24 O14, Yb H16 O8, Cl3, 19(H2 O)'
_chemical_formula_sum            'C44 H106 Cl3 N24 O41 Yb'
_chemical_formula_weight         1906.92

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'
Yb Yb -0.3850 5.5486 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.245(3)
_cell_length_b                   12.3258(13)
_cell_length_c                   14.7424(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.334(4)
_cell_angle_gamma                90.00
_cell_volume                     3837.0(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1974
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6812
_exptl_absorpt_correction_T_max  0.7339
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7983
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         27.53
_reflns_number_total             4564
_reflns_number_gt                3664
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.0778P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4564
_refine_ls_number_parameters     261
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1330
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.9043(9) 1.0000 1.0678(13) 0.482(10) Uani 1 2 d SU . .
Cl2 Cl 0.6496(7) 0.5000 0.7972(9) 0.212(6) Uani 0.50 2 d SP . .
O1W O 0.5278(4) 0.5668(5) 0.3728(6) 0.051(2) Uani 0.50 1 d P . .
O2W O 0.5702(3) 0.6435(6) 0.5541(8) 0.054(2) Uani 0.50 1 d P . .
O3W O 0.5788(4) 0.5702(6) 0.6324(7) 0.058(2) Uani 0.50 1 d P . .
O4W O 0.5501(4) 0.6452(6) 0.4502(7) 0.051(2) Uani 0.50 1 d P . .
Yb1 Yb 0.5000 0.5000 0.5000 0.02665(17) Uani 1 4 d S . .
C1 C 0.6870(3) 0.8443(4) 0.5094(6) 0.0533(18) Uani 1 1 d . . .
C2 C 0.7256(4) 1.0000 0.4541(10) 0.063(3) Uani 1 2 d S . .
C3 C 0.7482(4) 1.0000 0.5629(10) 0.068(3) Uani 1 2 d S . .
C4 C 0.7291(3) 0.8576(5) 0.6821(6) 0.073(2) Uani 1 1 d . . .
H4A H 0.7222 0.7799 0.6771 0.087 Uiso 1 1 calc R . .
H4B H 0.7732 0.8693 0.7189 0.087 Uiso 1 1 calc R . .
C5 C 0.6406(3) 0.8477(5) 0.7445(5) 0.0588(18) Uani 1 1 d . . .
C6 C 0.7050(4) 1.0000 0.7906(8) 0.064(3) Uani 1 2 d S . .
C7 C 0.6536(5) 1.0000 0.8413(7) 0.062(3) Uani 1 2 d S . .
C8 C 0.5660(4) 0.8544(5) 0.8360(6) 0.070(2) Uani 1 1 d . . .
H8A H 0.5635 0.7771 0.8228 0.084 Uiso 1 1 calc R . .
H8B H 0.5777 0.8636 0.9047 0.084 Uiso 1 1 calc R . .
C9 C 0.4567(4) 0.8446(4) 0.7351(6) 0.0610(19) Uani 1 1 d . A .
C10 C 0.4841(4) 1.0000 0.8282(7) 0.058(3) Uani 1 2 d SD . .
C11 C 0.4122(4) 1.0000 0.7733(7) 0.065(3) Uani 1 2 d SD . .
C12 C 0.6599(3) 0.8583(5) 0.3360(6) 0.069(2) Uani 1 1 d . . .
H12A H 0.6566 0.7802 0.3402 0.083 Uiso 1 1 calc R . .
H12B H 0.6883 0.8732 0.2992 0.083 Uiso 1 1 calc R . .
C13 C 0.7791(5) 1.0000 0.4087(10) 0.086(4) Uani 1 2 d S . .
H13A H 0.8033 1.0657 0.4256 0.129 Uiso 0.50 1 calc PR . .
H13B H 0.7612 0.9955 0.3405 0.129 Uiso 0.50 1 calc PR . .
H13C H 0.8063 0.9388 0.4318 0.129 Uiso 0.50 1 calc PR . .
C14 C 0.8209(5) 1.0000 0.6102(13) 0.115(6) Uani 1 2 d S . .
H14A H 0.8383 1.0658 0.5940 0.172 Uiso 0.50 1 calc PR . .
H14B H 0.8389 0.9389 0.5875 0.172 Uiso 0.50 1 calc PR . .
H14C H 0.8308 0.9953 0.6783 0.172 Uiso 0.50 1 calc PR . .
C15 C 0.7694(6) 1.0000 0.8610(12) 0.131(7) Uani 1 2 d S . .
H15A H 0.7756 1.0653 0.8983 0.197 Uiso 0.50 1 calc PR . .
H15B H 0.8003 0.9964 0.8279 0.197 Uiso 1 2 calc SR . .
H15C H 0.7742 0.9383 0.9023 0.197 Uiso 0.50 1 calc PR . .
C16 C 0.6753(9) 1.0000 0.9530(9) 0.138(7) Uani 1 2 d S . .
H16A H 0.6995 1.0644 0.9765 0.208 Uiso 0.50 1 calc PR . .
H16B H 0.7011 0.9373 0.9765 0.208 Uiso 0.50 1 calc PR . .
H16C H 0.6389 0.9983 0.9744 0.208 Uiso 1 2 calc SR . .
N1 N 0.6880(2) 0.9003(4) 0.4305(5) 0.0612(17) Uani 1 1 d . . .
N2 N 0.7189(2) 0.9001(4) 0.5875(5) 0.0629(18) Uani 1 1 d . . .
N3 N 0.6907(3) 0.9021(4) 0.7346(5) 0.0615(16) Uani 1 1 d . . .
N4 N 0.6155(3) 0.9006(4) 0.8030(4) 0.0602(15) Uani 1 1 d . . .
N5 N 0.5050(3) 0.9011(4) 0.7931(4) 0.0575(15) Uani 1 1 d . A .
N6 N 0.4021(3) 0.9009(4) 0.7160(5) 0.0637(17) Uani 1 1 d . . .
O1 O 0.6636(2) 0.7545(3) 0.5089(4) 0.0632(14) Uani 1 1 d . . .
O2 O 0.6197(3) 0.7597(3) 0.7060(4) 0.0805(16) Uani 1 1 d . . .
O3 O 0.4608(3) 0.7529(4) 0.7043(5) 0.0882(18) Uani 1 1 d . . .
O4 O 0.4961(8) 1.0000 0.9213(10) 0.094(6) Uani 0.607(16) 2 d SP A 1
O5 O 0.3781(10) 1.0000 0.8394(14) 0.077(8) Uani 0.393(16) 2 d SP . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W O4W 1.458(12) . ?
O1W O1W 1.647(13) 6_565 ?
O1W Yb1 2.304(7) . ?
O2W O3W 1.430(12) . ?
O2W O4W 1.455(13) . ?
O2W Yb1 2.329(7) . ?
O3W O3W 1.731(14) 6_565 ?
O3W Yb1 2.340(8) . ?
O4W Yb1 2.345(7) . ?
Yb1 O1W 2.304(7) 6_565 ?
Yb1 O1W 2.304(7) 2_656 ?
Yb1 O1W 2.304(7) 5_666 ?
Yb1 O2W 2.329(7) 5_666 ?
Yb1 O2W 2.329(7) 6_565 ?
Yb1 O2W 2.329(7) 2_656 ?
Yb1 O3W 2.340(8) 5_666 ?
Yb1 O3W 2.340(8) 6_565 ?
Yb1 O3W 2.340(8) 2_656 ?
C1 O1 1.222(6) . ?
C1 N2 1.336(9) . ?
C1 N1 1.358(9) . ?
C2 N1 1.466(7) . ?
C2 N1 1.466(7) 6_575 ?
C2 C3 1.523(16) . ?
C2 C13 1.538(12) . ?
C3 N2 1.491(7) . ?
C3 N2 1.491(7) 6_575 ?
C3 C14 1.546(13) . ?
C4 N3 1.431(9) . ?
C4 N2 1.439(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O2 1.244(7) . ?
C5 N4 1.335(9) . ?
C5 N3 1.347(9) . ?
C6 N3 1.440(8) . ?
C6 N3 1.440(8) 6_575 ?
C6 C15 1.482(14) . ?
C6 C7 1.551(16) . ?
C7 N4 1.496(8) . ?
C7 N4 1.496(8) 6_575 ?
C7 C16 1.563(16) . ?
C8 N5 1.427(9) . ?
C8 N4 1.451(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O3 1.231(7) . ?
C9 N5 1.338(9) . ?
C9 N6 1.351(9) . ?
C10 O4 1.314(14) . ?
C10 N5 1.456(7) 6_575 ?
C10 N5 1.456(7) . ?
C10 C11 1.550(2) . ?
C11 O5 1.410(16) . ?
C11 N6 1.461(7) . ?
C11 N6 1.461(7) 6_575 ?
C12 N1 1.432(9) . ?
C12 N6 1.450(9) 2_656 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N6 C12 1.450(9) 2_656 ?

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
O4W O1W O1W 131.5(5) . 6_565 ?
O4W O1W Yb1 73.3(4) . . ?
O1W O1W Yb1 69.06(17) 6_565 . ?
O3W O2W O4W 141.0(7) . . ?
O3W O2W Yb1 72.6(4) . . ?
O4W O2W Yb1 72.5(4) . . ?
O2W O3W O3W 129.2(5) . 6_565 ?
O2W O3W Yb1 71.7(5) . . ?
O3W O3W Yb1 68.30(19) 6_565 . ?
O2W O4W O1W 137.0(7) . . ?
O2W O4W Yb1 71.2(4) . . ?
O1W O4W Yb1 70.2(4) . . ?
O1W Yb1 O1W 41.9(3) 6_565 . ?
O1W Yb1 O1W 180.0(2) 6_565 2_656 ?
O1W Yb1 O1W 138.1(3) . 2_656 ?
O1W Yb1 O1W 138.1(3) 6_565 5_666 ?
O1W Yb1 O1W 180.000(2) . 5_666 ?
O1W Yb1 O1W 41.9(3) 2_656 5_666 ?
O1W Yb1 O2W 103.1(3) 6_565 . ?
O1W Yb1 O2W 71.6(3) . . ?
O1W Yb1 O2W 76.9(3) 2_656 . ?
O1W Yb1 O2W 108.4(3) 5_666 . ?
O1W Yb1 O2W 76.9(3) 6_565 5_666 ?
O1W Yb1 O2W 108.4(3) . 5_666 ?
O1W Yb1 O2W 103.1(3) 2_656 5_666 ?
O1W Yb1 O2W 71.6(3) 5_666 5_666 ?
O2W Yb1 O2W 180.000(1) . 5_666 ?
O1W Yb1 O2W 71.6(3) 6_565 6_565 ?
O1W Yb1 O2W 103.1(3) . 6_565 ?
O1W Yb1 O2W 108.4(3) 2_656 6_565 ?
O1W Yb1 O2W 76.9(3) 5_666 6_565 ?
O2W Yb1 O2W 98.9(4) . 6_565 ?
O2W Yb1 O2W 81.1(4) 5_666 6_565 ?
O1W Yb1 O2W 108.4(3) 6_565 2_656 ?
O1W Yb1 O2W 76.9(3) . 2_656 ?
O1W Yb1 O2W 71.6(3) 2_656 2_656 ?
O1W Yb1 O2W 103.1(3) 5_666 2_656 ?
O2W Yb1 O2W 81.1(4) . 2_656 ?
O2W Yb1 O2W 98.9(4) 5_666 2_656 ?
O2W Yb1 O2W 180.000(1) 6_565 2_656 ?
O1W Yb1 O3W 119.2(3) 6_565 . ?
O1W Yb1 O3W 102.9(3) . . ?
O1W Yb1 O3W 60.8(3) 2_656 . ?
O1W Yb1 O3W 77.1(3) 5_666 . ?
O2W Yb1 O3W 35.7(3) . . ?
O2W Yb1 O3W 144.3(3) 5_666 . ?
O2W Yb1 O3W 75.5(3) 6_565 . ?
O2W Yb1 O3W 104.5(3) 2_656 . ?
O1W Yb1 O3W 60.8(3) 6_565 5_666 ?
O1W Yb1 O3W 77.1(3) . 5_666 ?
O1W Yb1 O3W 119.2(3) 2_656 5_666 ?
O1W Yb1 O3W 102.9(3) 5_666 5_666 ?
O2W Yb1 O3W 144.3(3) . 5_666 ?
O2W Yb1 O3W 35.7(3) 5_666 5_666 ?
O2W Yb1 O3W 104.5(3) 6_565 5_666 ?
O2W Yb1 O3W 75.5(3) 2_656 5_666 ?
O3W Yb1 O3W 180.000(1) . 5_666 ?
O1W Yb1 O3W 102.9(3) 6_565 6_565 ?
O1W Yb1 O3W 119.2(3) . 6_565 ?
O1W Yb1 O3W 77.1(3) 2_656 6_565 ?
O1W Yb1 O3W 60.8(3) 5_666 6_565 ?
O2W Yb1 O3W 75.5(3) . 6_565 ?
O2W Yb1 O3W 104.5(3) 5_666 6_565 ?
O2W Yb1 O3W 35.7(3) 6_565 6_565 ?
O2W Yb1 O3W 144.3(3) 2_656 6_565 ?
O3W Yb1 O3W 43.4(4) . 6_565 ?
O3W Yb1 O3W 136.6(4) 5_666 6_565 ?
O1W Yb1 O3W 77.1(3) 6_565 2_656 ?
O1W Yb1 O3W 60.8(3) . 2_656 ?
O1W Yb1 O3W 102.9(3) 2_656 2_656 ?
O1W Yb1 O3W 119.2(3) 5_666 2_656 ?
O2W Yb1 O3W 104.5(3) . 2_656 ?
O2W Yb1 O3W 75.5(3) 5_666 2_656 ?
O2W Yb1 O3W 144.3(3) 6_565 2_656 ?
O2W Yb1 O3W 35.7(3) 2_656 2_656 ?
O3W Yb1 O3W 136.6(4) . 2_656 ?
O3W Yb1 O3W 43.4(4) 5_666 2_656 ?
O3W Yb1 O3W 180.000(1) 6_565 2_656 ?
O1 C1 N2 125.5(7) . . ?
O1 C1 N1 125.2(7) . . ?
N2 C1 N1 109.2(5) . . ?
N1 C2 N1 114.0(7) . 6_575 ?
N1 C2 C3 103.0(6) . . ?
N1 C2 C3 103.0(6) 6_575 . ?
N1 C2 C13 111.0(6) . . ?
N1 C2 C13 111.0(6) 6_575 . ?
C3 C2 C13 114.4(9) . . ?
N2 C3 N2 111.4(7) . 6_575 ?
N2 C3 C2 103.3(6) . . ?
N2 C3 C2 103.3(6) 6_575 . ?
N2 C3 C14 111.5(6) . . ?
N2 C3 C14 111.5(6) 6_575 . ?
C2 C3 C14 115.3(10) . . ?
N3 C4 N2 116.5(5) . . ?
N3 C4 H4A 108.2 . . ?
N2 C4 H4A 108.2 . . ?
N3 C4 H4B 108.2 . . ?
N2 C4 H4B 108.2 . . ?
H4A C4 H4B 107.3 . . ?
O2 C5 N4 123.2(7) . . ?
O2 C5 N3 125.9(7) . . ?
N4 C5 N3 110.8(6) . . ?
N3 C6 N3 113.8(9) . 6_575 ?
N3 C6 C15 113.1(6) . . ?
N3 C6 C15 113.1(6) 6_575 . ?
N3 C6 C7 102.3(6) . . ?
N3 C6 C7 102.3(5) 6_575 . ?
C15 C6 C7 111.1(11) . . ?
N4 C7 N4 110.0(8) . 6_575 ?
N4 C7 C6 103.5(6) . . ?
N4 C7 C6 103.5(6) 6_575 . ?
N4 C7 C16 110.4(7) . . ?
N4 C7 C16 110.4(7) 6_575 . ?
C6 C7 C16 118.4(11) . . ?
N5 C8 N4 114.2(5) . . ?
N5 C8 H8A 108.7 . . ?
N4 C8 H8A 108.7 . . ?
N5 C8 H8B 108.7 . . ?
N4 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O3 C9 N5 125.2(7) . . ?
O3 C9 N6 124.1(8) . . ?
N5 C9 N6 110.7(5) . . ?
O4 C10 N5 112.8(6) . 6_575 ?
O4 C10 N5 112.8(6) . . ?
N5 C10 N5 113.8(7) 6_575 . ?
O4 C10 C11 112.5(10) . . ?
N5 C10 C11 101.9(5) 6_575 . ?
N5 C10 C11 101.9(5) . . ?
O5 C11 N6 112.4(6) . . ?
O5 C11 N6 112.4(6) . 6_575 ?
N6 C11 N6 113.4(8) . 6_575 ?
O5 C11 C10 109.3(12) . . ?
N6 C11 C10 104.3(5) . . ?
N6 C11 C10 104.3(5) 6_575 . ?
N1 C12 N6 115.8(5) . 2_656 ?
N1 C12 H12A 108.3 . . ?
N6 C12 H12A 108.3 2_656 . ?
N1 C12 H12B 108.3 . . ?
N6 C12 H12B 108.3 2_656 . ?
H12A C12 H12B 107.4 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 H15A 109.5 . . ?
C6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C16 H16A 109.5 . . ?
C7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C12 122.0(5) . . ?
C1 N1 C2 112.6(7) . . ?
C12 N1 C2 125.1(7) . . ?
C1 N2 C4 121.8(5) . . ?
C1 N2 C3 111.7(7) . . ?
C4 N2 C3 126.0(7) . . ?
C5 N3 C4 121.6(5) . . ?
C5 N3 C6 113.3(7) . . ?
C4 N3 C6 124.7(6) . . ?
C5 N4 C8 122.6(5) . . ?
C5 N4 C7 110.0(7) . . ?
C8 N4 C7 126.5(7) . . ?
C9 N5 C8 122.2(5) . . ?
C9 N5 C10 112.5(6) . . ?
C8 N5 C10 123.1(7) . . ?
C9 N6 C12 124.6(5) . 2_656 ?
C9 N6 C11 110.2(6) . . ?
C12 N6 C11 123.8(6) 2_656 . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.543
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.146

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.051 -0.005 0.000 842 319 ' '
2 0.500 0.000 0.500 119 30 ' '
3 0.000 0.500 0.500 119 30 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_complex2
_database_code_depnum_ccdc_archive 'CCDC 1550306'
_audit_update_record             
;
2017-05-16 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C44 H52 N24 O14, Gd H16 O8, 2(N O3), Cl, 8(H2 O)'
_chemical_formula_sum            'C44 H84 Cl Gd N26 O36'
_chemical_formula_weight         1746.07

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'
Gd Gd -0.1653 3.9035 '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           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.316(5)
_cell_length_b                   12.427(3)
_cell_length_c                   26.976(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.573(5)
_cell_angle_gamma                90.00
_cell_volume                     6908(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3596
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7839
_exptl_absorpt_correction_T_max  0.8334
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      223(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  'Bruker Smart Apex2 CCD Detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10314
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5781
_reflns_number_gt                4781
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.
;

_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)+(0.0777P)²+249.5343P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5781
_refine_ls_number_parameters     502
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0983
_refine_ls_wR_factor_ref         0.2541
_refine_ls_wR_factor_gt          0.2462
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      3.729
_refine_ls_shift/su_max          0.000
_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
Cl1 Cl 0.653(7) 1.591(11) 0.415(3) 0.40(10) Uani 0.50 1 d P . .
N13 N 0.546(2) 0.699(5) 0.0536(19) 0.12(2) Uani 1 1 d D . .
O9 O 0.4946(18) 0.743(4) 0.0226(18) 0.102(15) Uani 1 1 d D . .
O10 O 0.597(2) 0.758(5) 0.0696(19) 0.13(2) Uani 1 1 d D . .
O11 O 0.541(4) 0.610(5) 0.073(3) 0.38(11) Uani 1 1 d D . .
O1W O 0.548(2) 1.444(4) 0.221(2) 0.031(11) Uani 0.50 1 d P . .
O2W O 0.590(3) 1.518(4) 0.325(2) 0.040(13) Uani 0.50 1 d P . .
O3W O 0.551(2) 1.738(4) 0.224(2) 0.039(12) Uani 0.50 1 d P . .
O4W O 0.508(4) 1.657(4) 0.170(2) 0.06(2) Uani 0.50 1 d P . .
O5W O 0.572(2) 1.740(4) 0.275(2) 0.036(12) Uani 0.50 1 d P . .
O6W O 0.572(2) 1.445(4) 0.282(2) 0.044(14) Uani 0.50 1 d P . .
O7W O 0.526(3) 1.526(4) 0.178(2) 0.043(14) Uani 0.50 1 d P . .
O8W O 0.584(3) 1.662(4) 0.327(3) 0.057(19) Uani 0.50 1 d P . .
Gd1 Gd 0.5000 1.59025(19) 0.2500 0.0282(9) Uani 1 2 d S . .
C1 C 0.3100(16) 0.935(3) 0.2418(14) 0.026(7) Uani 1 1 d U . .
C2 C 0.2780(16) 1.092(3) 0.2735(15) 0.031(8) Uani 1 1 d . . .
C3 C 0.2469(15) 1.090(3) 0.2108(15) 0.030(8) Uani 1 1 d . . .
C4 C 0.3112(16) 1.245(3) 0.2401(16) 0.033(9) Uani 1 1 d . . .
C5 C 0.2562(18) 0.947(3) 0.1443(17) 0.038(9) Uani 1 1 d . . .
H5A H 0.2100 0.9595 0.1234 0.046 Uiso 1 1 calc R . .
H5B H 0.2631 0.8689 0.1472 0.046 Uiso 1 1 calc R . .
C6 C 0.2549(18) 1.230(3) 0.1422(16) 0.037(9) Uani 1 1 d . . .
H6A H 0.2087 1.2154 0.1221 0.045 Uiso 1 1 calc R . .
H6B H 0.2604 1.3085 0.1446 0.045 Uiso 1 1 calc R . .
C7 C 0.3446(17) 0.938(3) 0.1110(16) 0.034(8) Uani 1 1 d . . .
C8 C 0.2769(16) 1.087(3) 0.0813(15) 0.033(8) Uani 1 1 d . . .
C9 C 0.3290(18) 1.088(3) 0.0543(14) 0.035(8) Uani 1 1 d . . .
C10 C 0.3424(18) 1.243(3) 0.1075(15) 0.033(8) Uani 1 1 d . . .
C11 C 0.4158(18) 0.943(3) 0.0608(17) 0.037(9) Uani 1 1 d . . .
H11A H 0.4188 0.8662 0.0689 0.044 Uiso 1 1 calc R . .
H11B H 0.4015 0.9515 0.0218 0.044 Uiso 1 1 calc R . .
C12 C 0.4141(19) 1.231(3) 0.0584(16) 0.040(9) Uani 1 1 d . . .
H12A H 0.4008 1.2191 0.0198 0.048 Uiso 1 1 calc R . .
H12B H 0.4163 1.3089 0.0644 0.048 Uiso 1 1 calc R . .
C13 C 0.5297(19) 0.935(2) 0.1213(17) 0.034(9) Uani 1 1 d . A .
C14 C 0.5004(19) 1.089(3) 0.0683(14) 0.032(8) Uani 1 1 d . . .
C15 C 0.5746(18) 1.091(3) 0.1005(15) 0.034(8) Uani 1 1 d . A .
C16 C 0.529(2) 1.245(3) 0.1207(16) 0.043(10) Uani 1 1 d . . .
C17 C 0.6513(18) 0.949(3) 0.1612(17) 0.040(9) Uani 1 1 d . . .
H17A H 0.6478 0.8707 0.1639 0.048 Uiso 1 1 calc R . .
H17B H 0.6778 0.9626 0.1401 0.048 Uiso 1 1 calc R . .
C18 C 0.6485(19) 1.236(3) 0.1617(17) 0.042(9) Uani 1 1 d . . .
H18A H 0.6755 1.2272 0.1407 0.050 Uiso 1 1 calc R A .
H18B H 0.6432 1.3136 0.1658 0.050 Uiso 1 1 calc R . .
C19 C 0.2306(19) 1.093(3) 0.3033(19) 0.045(10) Uani 1 1 d . . .
H19A H 0.2043 1.0285 0.2947 0.068 Uiso 1 1 calc R . .
H19B H 0.2026 1.1558 0.2921 0.068 Uiso 1 1 calc R . .
H19C H 0.2553 1.0965 0.3418 0.068 Uiso 1 1 calc R . .
C20 C 0.1720(17) 1.090(4) 0.1862(19) 0.048(11) Uani 1 1 d . . .
H20A H 0.1559 1.1564 0.1954 0.072 Uiso 1 1 calc R . .
H20B H 0.1560 1.0293 0.2002 0.072 Uiso 1 1 calc R . .
H20C H 0.1569 1.0840 0.1474 0.072 Uiso 1 1 calc R . .
C21 C 0.206(2) 1.085(5) 0.040(2) 0.073(15) Uani 1 1 d . . .
H21A H 0.1970 1.1499 0.0186 0.109 Uiso 1 1 calc R . .
H21B H 0.1767 1.0803 0.0589 0.109 Uiso 1 1 calc R . .
H21C H 0.1997 1.0226 0.0168 0.109 Uiso 1 1 calc R . .
C22 C 0.302(3) 1.086(4) -0.0071(19) 0.068(14) Uani 1 1 d . . .
H22A H 0.2776 1.1511 -0.0209 0.102 Uiso 1 1 calc R . .
H22B H 0.2738 1.0239 -0.0201 0.102 Uiso 1 1 calc R . .
H22C H 0.3376 1.0810 -0.0192 0.102 Uiso 1 1 calc R . .
N1 N 0.3154(14) 0.991(2) 0.2863(14) 0.037(8) Uani 1 1 d . . .
N2 N 0.2724(13) 0.990(2) 0.1977(14) 0.034(7) Uani 1 1 d . . .
N3 N 0.3190(14) 1.189(2) 0.2862(13) 0.030(7) Uani 1 1 d . . .
N4 N 0.2733(14) 1.187(2) 0.1963(13) 0.030(7) Uani 1 1 d . . .
N5 N 0.2937(14) 0.992(2) 0.1149(14) 0.036(7) Uani 1 1 d . . .
N6 N 0.3672(15) 0.991(2) 0.0780(13) 0.035(7) Uani 1 1 d . . .
N7 N 0.2912(15) 1.187(2) 0.1123(13) 0.034(7) Uani 1 1 d . . .
N8 N 0.3643(16) 1.188(2) 0.0747(13) 0.036(7) Uani 1 1 d . . .
N9 N 0.4796(15) 0.992(2) 0.0866(12) 0.032(7) Uani 1 1 d . A .
N10 N 0.5865(16) 0.992(2) 0.1319(15) 0.040(8) Uani 1 1 d . . .
N11 N 0.4776(16) 1.187(2) 0.0851(13) 0.036(7) Uani 1 1 d . A .
N12 N 0.5843(16) 1.188(2) 0.1320(14) 0.036(7) Uani 1 1 d . A .
O1 O 0.3318(13) 0.8423(18) 0.2426(13) 0.044(7) Uani 1 1 d . . .
O2 O 0.3674(16) 0.852(2) 0.1338(14) 0.056(9) Uani 1 1 d . . .
O3 O 0.5271(16) 0.847(2) 0.1411(15) 0.061(9) Uani 1 1 d . . .
O4 O 0.3339(13) 1.334(2) 0.2391(11) 0.039(6) Uani 1 1 d . . .
O5 O 0.3606(16) 1.331(2) 0.1274(13) 0.049(8) Uani 1 1 d . . .
O6 O 0.5224(16) 1.333(3) 0.1363(16) 0.072(11) Uani 1 1 d . A .
O7 O 0.483(3) 1.084(5) 0.0139(19) 0.052(18) Uani 0.55(7) 1 d P A 1
O8 O 0.615(3) 1.086(5) 0.071(2) 0.04(2) Uani 0.45(7) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N13 O9 1.250(7) . ?
N13 O11 1.250(7) . ?
N13 O10 1.291(7) . ?
O1W O7W 1.47(7) . ?
O1W O6W 1.54(8) . ?
O1W Gd1 2.40(4) . ?
O2W O6W 1.39(7) . ?
O2W O8W 1.81(7) . ?
O2W Gd1 2.41(6) . ?
O3W O5W 1.27(7) . ?
O3W O4W 1.73(8) . ?
O3W Gd1 2.39(5) . ?
O4W O7W 1.67(7) . ?
O4W Gd1 2.39(5) . ?
O5W O8W 1.64(8) . ?
O5W Gd1 2.38(4) . ?
O6W Gd1 2.36(5) . ?
O7W Gd1 2.38(4) . ?
O8W Gd1 2.38(6) . ?
Gd1 O6W 2.36(5) 2_655 ?
Gd1 O7W 2.38(4) 2_655 ?
Gd1 O5W 2.38(4) 2_655 ?
Gd1 O8W 2.38(6) 2_655 ?
Gd1 O4W 2.39(5) 2_655 ?
Gd1 O3W 2.39(5) 2_655 ?
C1 O1 1.24(4) . ?
C1 N2 1.35(5) . ?
C1 N1 1.35(5) . ?
C2 N1 1.47(4) . ?
C2 N3 1.48(4) . ?
C2 C19 1.56(4) . ?
C2 C3 1.56(5) . ?
C3 N4 1.46(4) . ?
C3 N2 1.46(4) . ?
C3 C20 1.54(4) . ?
C4 O4 1.22(4) . ?
C4 N4 1.36(5) . ?
C4 N3 1.38(5) . ?
C5 N2 1.45(5) . ?
C5 N5 1.47(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.45(4) . ?
C6 N4 1.45(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.25(5) . ?
C7 N6 1.35(5) . ?
C7 N5 1.36(5) . ?
C8 N5 1.44(5) . ?
C8 N7 1.47(5) . ?
C8 C21 1.55(6) . ?
C8 C9 1.59(5) . ?
C9 N8 1.46(5) . ?
C9 N6 1.46(5) . ?
C9 C22 1.53(6) . ?
C10 O5 1.22(4) . ?
C10 N8 1.35(5) . ?
C10 N7 1.38(5) . ?
C11 N9 1.45(5) . ?
C11 N6 1.46(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.43(5) . ?
C12 N8 1.45(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.23(4) . ?
C13 N9 1.35(5) . ?
C13 N10 1.38(5) . ?
C14 O7 1.37(6) . ?
C14 N9 1.45(4) . ?
C14 N11 1.47(4) . ?
C14 C15 1.55(5) . ?
C15 O8 1.41(6) . ?
C15 N12 1.45(5) . ?
C15 N10 1.46(5) . ?
C16 O6 1.20(5) . ?
C16 N12 1.36(5) . ?
C16 N11 1.37(5) . ?
C17 N1 1.42(5) 2_655 ?
C17 N10 1.46(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N3 1.44(5) 2_655 ?
C18 N12 1.47(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
N1 C17 1.42(5) 2_655 ?
N3 C18 1.44(5) 2_655 ?

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
O9 N13 O11 118(5) . . ?
O9 N13 O10 116(5) . . ?
O11 N13 O10 124.7(15) . . ?
O7W O1W O6W 136(4) . . ?
O7W O1W Gd1 71(2) . . ?
O6W O1W Gd1 70(3) . . ?
O6W O2W O8W 133(5) . . ?
O6W O2W Gd1 71(3) . . ?
O8W O2W Gd1 67(2) . . ?
O5W O3W O4W 142(5) . . ?
O5W O3W Gd1 74(3) . . ?
O4W O3W Gd1 69(2) . . ?
O7W O4W O3W 115(5) . . ?
O7W O4W Gd1 69(2) . . ?
O3W O4W Gd1 69(2) . . ?
O3W O5W O8W 142(5) . . ?
O3W O5W Gd1 75(3) . . ?
O8W O5W Gd1 70(2) . . ?
O2W O6W O1W 140(5) . . ?
O2W O6W Gd1 75(3) . . ?
O1W O6W Gd1 72(3) . . ?
O1W O7W O4W 140(4) . . ?
O1W O7W Gd1 73(2) . . ?
O4W O7W Gd1 70(2) . . ?
O5W O8W O2W 122(5) . . ?
O5W O8W Gd1 70(3) . . ?
O2W O8W Gd1 69(3) . . ?
O6W Gd1 O6W 80(3) 2_655 . ?
O6W Gd1 O7W 78(2) 2_655 . ?
O6W Gd1 O7W 72(2) . . ?
O6W Gd1 O7W 72(2) 2_655 2_655 ?
O6W Gd1 O7W 78(2) . 2_655 ?
O7W Gd1 O7W 141(2) . 2_655 ?
O6W Gd1 O5W 175(2) 2_655 . ?
O6W Gd1 O5W 101.5(18) . . ?
O7W Gd1 O5W 98.2(19) . . ?
O7W Gd1 O5W 112.5(19) 2_655 . ?
O6W Gd1 O5W 101.5(18) 2_655 2_655 ?
O6W Gd1 O5W 175(2) . 2_655 ?
O7W Gd1 O5W 112.5(19) . 2_655 ?
O7W Gd1 O5W 98.2(19) 2_655 2_655 ?
O5W Gd1 O5W 78(2) . 2_655 ?
O6W Gd1 O8W 144(2) 2_655 . ?
O6W Gd1 O8W 77(2) . . ?
O7W Gd1 O8W 119(2) . . ?
O7W Gd1 O8W 77(2) 2_655 . ?
O5W Gd1 O8W 40.3(19) . . ?
O5W Gd1 O8W 100.1(19) 2_655 . ?
O6W Gd1 O8W 77(2) 2_655 2_655 ?
O6W Gd1 O8W 144(2) . 2_655 ?
O7W Gd1 O8W 77(2) . 2_655 ?
O7W Gd1 O8W 119(2) 2_655 2_655 ?
O5W Gd1 O8W 100.1(19) . 2_655 ?
O5W Gd1 O8W 40.3(19) 2_655 2_655 ?
O8W Gd1 O8W 136(3) . 2_655 ?
O6W Gd1 O4W 109(2) 2_655 2_655 ?
O6W Gd1 O4W 102(2) . 2_655 ?
O7W Gd1 O4W 171(2) . 2_655 ?
O7W Gd1 O4W 41.2(17) 2_655 2_655 ?
O5W Gd1 O4W 75(2) . 2_655 ?
O5W Gd1 O4W 73(2) 2_655 2_655 ?
O8W Gd1 O4W 52(3) . 2_655 ?
O8W Gd1 O4W 111(2) 2_655 2_655 ?
O6W Gd1 O4W 102(2) 2_655 . ?
O6W Gd1 O4W 109(2) . . ?
O7W Gd1 O4W 41.2(17) . . ?
O7W Gd1 O4W 171(2) 2_655 . ?
O5W Gd1 O4W 73(2) . . ?
O5W Gd1 O4W 75(2) 2_655 . ?
O8W Gd1 O4W 111(2) . . ?
O8W Gd1 O4W 52(3) 2_655 . ?
O4W Gd1 O4W 139(2) 2_655 . ?
O6W Gd1 O3W 144(2) 2_655 . ?
O6W Gd1 O3W 111.3(18) . . ?
O7W Gd1 O3W 74.2(18) . . ?
O7W Gd1 O3W 142.1(19) 2_655 . ?
O5W Gd1 O3W 30.9(18) . . ?
O5W Gd1 O3W 70.3(17) 2_655 . ?
O8W Gd1 O3W 71(2) . . ?
O8W Gd1 O3W 76(2) 2_655 . ?
O4W Gd1 O3W 101.8(19) 2_655 . ?
O4W Gd1 O3W 42(2) . . ?
O6W Gd1 O3W 111.3(18) 2_655 2_655 ?
O6W Gd1 O3W 144(2) . 2_655 ?
O7W Gd1 O3W 142.1(19) . 2_655 ?
O7W Gd1 O3W 74.2(18) 2_655 2_655 ?
O5W Gd1 O3W 70.3(16) . 2_655 ?
O5W Gd1 O3W 30.9(18) 2_655 2_655 ?
O8W Gd1 O3W 76(2) . 2_655 ?
O8W Gd1 O3W 71(2) 2_655 2_655 ?
O4W Gd1 O3W 42(2) 2_655 2_655 ?
O4W Gd1 O3W 101.8(19) . 2_655 ?
O3W Gd1 O3W 80(2) . 2_655 ?
O1 C1 N2 126(3) . . ?
O1 C1 N1 124(3) . . ?
N2 C1 N1 109(3) . . ?
N1 C2 N3 114(3) . . ?
N1 C2 C19 109(3) . . ?
N3 C2 C19 111(3) . . ?
N1 C2 C3 103(3) . . ?
N3 C2 C3 104(3) . . ?
C19 C2 C3 117(3) . . ?
N4 C3 N2 114(2) . . ?
N4 C3 C20 112(3) . . ?
N2 C3 C20 111(3) . . ?
N4 C3 C2 103(3) . . ?
N2 C3 C2 103(3) . . ?
C20 C3 C2 115(3) . . ?
O4 C4 N4 125(4) . . ?
O4 C4 N3 124(4) . . ?
N4 C4 N3 110(3) . . ?
N2 C5 N5 115(3) . . ?
N2 C5 H5A 108.6 . . ?
N5 C5 H5A 108.6 . . ?
N2 C5 H5B 108.6 . . ?
N5 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N7 C6 N4 115(3) . . ?
N7 C6 H6A 108.5 . . ?
N4 C6 H6A 108.5 . . ?
N7 C6 H6B 108.5 . . ?
N4 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
O2 C7 N6 124(3) . . ?
O2 C7 N5 126(3) . . ?
N6 C7 N5 110(3) . . ?
N5 C8 N7 113(3) . . ?
N5 C8 C21 113(4) . . ?
N7 C8 C21 111(3) . . ?
N5 C8 C9 103(3) . . ?
N7 C8 C9 103(3) . . ?
C21 C8 C9 113(3) . . ?
N8 C9 N6 113(3) . . ?
N8 C9 C22 111(3) . . ?
N6 C9 C22 112(3) . . ?
N8 C9 C8 102(3) . . ?
N6 C9 C8 102(3) . . ?
C22 C9 C8 116(3) . . ?
O5 C10 N8 127(3) . . ?
O5 C10 N7 124(3) . . ?
N8 C10 N7 109(3) . . ?
N9 C11 N6 113(3) . . ?
N9 C11 H11A 109.0 . . ?
N6 C11 H11A 109.0 . . ?
N9 C11 H11B 109.0 . . ?
N6 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N11 C12 N8 116(3) . . ?
N11 C12 H12A 108.3 . . ?
N8 C12 H12A 108.3 . . ?
N11 C12 H12B 108.3 . . ?
N8 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
O3 C13 N9 127(4) . . ?
O3 C13 N10 124(4) . . ?
N9 C13 N10 109(3) . . ?
O7 C14 N9 110(4) . . ?
O7 C14 N11 112(4) . . ?
N9 C14 N11 113(2) . . ?
O7 C14 C15 114(3) . . ?
N9 C14 C15 104(3) . . ?
N11 C14 C15 104(3) . . ?
O8 C15 N12 112(4) . . ?
O8 C15 N10 106(4) . . ?
N12 C15 N10 114(3) . . ?
O8 C15 C14 118(4) . . ?
N12 C15 C14 103(3) . . ?
N10 C15 C14 103(3) . . ?
O6 C16 N12 128(4) . . ?
O6 C16 N11 123(4) . . ?
N12 C16 N11 109(3) . . ?
N1 C17 N10 116(3) 2_655 . ?
N1 C17 H17A 108.3 2_655 . ?
N10 C17 H17A 108.3 . . ?
N1 C17 H17B 108.3 2_655 . ?
N10 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
N3 C18 N12 113(3) 2_655 . ?
N3 C18 H18A 109.0 2_655 . ?
N12 C18 H18A 109.0 . . ?
N3 C18 H18B 109.0 2_655 . ?
N12 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C2 C19 H19A 109.5 . . ?
C2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C3 C20 H20A 109.5 . . ?
C3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C22 H22A 109.5 . . ?
C9 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C9 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C17 122(3) . 2_655 ?
C1 N1 C2 112(3) . . ?
C17 N1 C2 125(3) 2_655 . ?
C1 N2 C5 121(3) . . ?
C1 N2 C3 113(3) . . ?
C5 N2 C3 126(3) . . ?
C4 N3 C18 121(3) . 2_655 ?
C4 N3 C2 111(3) . . ?
C18 N3 C2 127(3) 2_655 . ?
C4 N4 C6 121(3) . . ?
C4 N4 C3 112(3) . . ?
C6 N4 C3 126(3) . . ?
C7 N5 C8 112(3) . . ?
C7 N5 C5 121(3) . . ?
C8 N5 C5 126(3) . . ?
C7 N6 C11 121(3) . . ?
C7 N6 C9 113(3) . . ?
C11 N6 C9 125(3) . . ?
C10 N7 C6 122(3) . . ?
C10 N7 C8 112(3) . . ?
C6 N7 C8 126(3) . . ?
C10 N8 C12 122(3) . . ?
C10 N8 C9 114(3) . . ?
C12 N8 C9 125(3) . . ?
C13 N9 C14 112(3) . . ?
C13 N9 C11 121(3) . . ?
C14 N9 C11 124(3) . . ?
C13 N10 C15 111(3) . . ?
C13 N10 C17 124(3) . . ?
C15 N10 C17 123(3) . . ?
C16 N11 C12 123(3) . . ?
C16 N11 C14 111(3) . . ?
C12 N11 C14 124(3) . . ?
C16 N12 C15 113(3) . . ?
C16 N12 C18 122(3) . . ?
C15 N12 C18 124(3) . . ?

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         2.069
_refine_diff_density_min         -3.464
_refine_diff_density_rms         0.184

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.750 0.250 0.000 148 42 ' '
2 0.500 0.092 0.250 117 34 ' '
3 0.250 0.250 0.500 148 42 ' '
4 0.750 -0.250 0.500 148 42 ' '
5 0.500 -0.092 0.750 117 34 ' '
6 0.250 -0.250 1.000 148 42 ' '
7 1.000 0.408 0.750 117 34 ' '
8 1.000 0.592 0.250 117 34 ' '
_platon_squeeze_details          
;
;
