# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_04Nd
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H54 N25 Nd O20, N O3, Cl, 6(H2 O)'
_chemical_formula_sum            'C40 H66 Cl N26 Nd O29'
_chemical_formula_weight         1554.88

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'
Nd Nd -0.1943 3.0179 '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           orthorhombic
_symmetry_space_group_name_H-M   'P c 21 n'
_symmetry_space_group_name_Hall  'P -2n -2ac'

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

_cell_length_a                   14.639(6)
_cell_length_b                   17.452(7)
_cell_length_c                   23.468(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5996(4)
_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          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3188
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7769
_exptl_absorpt_correction_T_max  0.8373
_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            39504
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.10
_reflns_number_total             10238
_reflns_number_gt                7320
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0844P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.320(16)
_refine_ls_number_reflns         10238
_refine_ls_number_parameters     831
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1414
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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 -0.2770(5) 0.7953(11) 0.2393(6) 0.313(9) Uani 0.821(12) 1 d P A 1
Cl1' Cl -0.2707(10) 0.7461(11) 0.2897(6) 0.069(7) Uani 0.179(12) 1 d P A 2
N26 N -0.2749(6) 0.8066(6) 0.4950(4) 0.086(4) Uani 1 1 d D . .
O16 O -0.2009(6) 0.8256(6) 0.5174(4) 0.098(3) Uani 1 1 d D . .
O17 O -0.2976(8) 0.8511(10) 0.4559(5) 0.240(11) Uani 1 1 d D . .
O18 O -0.3238(12) 0.7540(9) 0.5144(7) 0.231(9) Uani 1 1 d D . .
N25 N 0.2749(5) 0.5510(5) 0.6352(3) 0.0456(19) Uani 1 1 d . . .
O1W O 0.2335(4) 0.7085(6) 0.6865(2) 0.0528(15) Uani 1 1 d . . .
O2W O 0.1915(7) 0.8370(4) 0.6147(3) 0.069(2) Uani 1 1 d . . .
O3W O 0.0670(4) 0.7075(6) 0.6243(2) 0.0560(16) Uani 1 1 d . . .
O4W O 0.2063(5) 0.7868(4) 0.4983(3) 0.0557(17) Uani 1 1 d . . .
O5W O 0.3713(5) 0.7657(4) 0.5863(2) 0.0537(17) Uani 1 1 d . . .
O13 O 0.1953(4) 0.5689(5) 0.6197(3) 0.0481(18) Uani 1 1 d . . .
O14 O 0.3371(4) 0.5972(4) 0.6215(3) 0.0527(17) Uani 1 1 d . . .
O15 O 0.2890(4) 0.4908(4) 0.6608(3) 0.0615(19) Uani 1 1 d . . .
Nd1 Nd 0.22129(3) 0.70311(9) 0.582448(14) 0.03484(13) Uani 1 1 d . . .
C1 C 0.0887(6) 0.6075(4) 0.4709(3) 0.0351(19) Uani 1 1 d . . .
C2 C -0.0016(6) 0.5732(5) 0.3922(3) 0.043(2) Uani 1 1 d . . .
C3 C 0.0869(6) 0.5230(5) 0.3930(3) 0.040(2) Uani 1 1 d . . .
C4 C 0.0814(6) 0.5975(6) 0.3069(4) 0.048(2) Uani 1 1 d . . .
C5 C 0.2163(6) 0.5146(5) 0.4682(3) 0.039(2) Uani 1 1 d . . .
H5A H 0.2177 0.5237 0.5094 0.046 Uiso 1 1 calc R . .
H5B H 0.2139 0.4591 0.4623 0.046 Uiso 1 1 calc R . .
C6 C 0.2145(6) 0.5134(6) 0.3170(4) 0.051(2) Uani 1 1 d . . .
H6A H 0.2146 0.5218 0.2757 0.061 Uiso 1 1 calc R . .
H6B H 0.2105 0.4580 0.3234 0.061 Uiso 1 1 calc R . .
C7 C 0.3403(5) 0.6065(5) 0.4649(3) 0.0340(19) Uani 1 1 d . . .
C8 C 0.3437(6) 0.5141(5) 0.3924(3) 0.041(2) Uani 1 1 d . . .
C9 C 0.4366(6) 0.5616(5) 0.3919(3) 0.040(2) Uani 1 1 d . . .
C10 C 0.3592(6) 0.5815(5) 0.3055(3) 0.037(2) Uani 1 1 d . . .
C11 C 0.4867(6) 0.6755(5) 0.4574(3) 0.042(2) Uani 1 1 d . . .
H11A H 0.4691 0.6908 0.4961 0.050 Uiso 1 1 calc R . .
H11B H 0.5461 0.6498 0.4598 0.050 Uiso 1 1 calc R . .
C12 C 0.5147(6) 0.6311(6) 0.3091(4) 0.044(2) Uani 1 1 d . . .
H12A H 0.5720 0.6085 0.3227 0.053 Uiso 1 1 calc R . .
H12B H 0.5127 0.6248 0.2676 0.053 Uiso 1 1 calc R . .
C13 C 0.4786(6) 0.8184(5) 0.4440(3) 0.038(2) Uani 1 1 d . . .
C14 C 0.5554(6) 0.7451(5) 0.3736(3) 0.038(2) Uani 1 1 d . . .
H14 H 0.6155 0.7218 0.3820 0.045 Uiso 1 1 calc R . .
C15 C 0.5647(5) 0.8318(5) 0.3601(3) 0.0349(19) Uani 1 1 d . . .
H15 H 0.6290 0.8491 0.3599 0.042 Uiso 1 1 calc R . .
C16 C 0.5015(7) 0.7677(5) 0.2805(3) 0.040(2) Uani 1 1 d . . .
C17 C 0.5211(6) 0.9492(6) 0.4176(4) 0.044(2) Uani 1 1 d . . .
H17A H 0.5816 0.9669 0.4054 0.053 Uiso 1 1 calc R . .
H17B H 0.5160 0.9572 0.4588 0.053 Uiso 1 1 calc R . .
C18 C 0.5202(6) 0.9087(5) 0.2710(3) 0.042(2) Uani 1 1 d . . .
H18A H 0.5786 0.9352 0.2760 0.050 Uiso 1 1 calc R . .
H18B H 0.5142 0.8957 0.2305 0.050 Uiso 1 1 calc R . .
C19 C 0.3778(6) 1.0268(5) 0.4180(4) 0.039(2) Uani 1 1 d . . .
C20 C 0.4549(6) 1.0192(5) 0.3284(3) 0.038(2) Uani 1 1 d . . .
H20 H 0.5089 1.0521 0.3217 0.046 Uiso 1 1 calc R . .
C21 C 0.3631(6) 1.0656(5) 0.3227(3) 0.040(2) Uani 1 1 d . . .
H21 H 0.3745 1.1185 0.3093 0.048 Uiso 1 1 calc R . .
C22 C 0.3637(6) 0.9623(6) 0.2592(3) 0.048(2) Uani 1 1 d . . .
C23 C 0.2450(6) 1.1071(6) 0.3938(4) 0.048(2) Uani 1 1 d . . .
H23A H 0.2447 1.1557 0.3730 0.058 Uiso 1 1 calc R . .
H23B H 0.2477 1.1192 0.4346 0.058 Uiso 1 1 calc R . .
C24 C 0.2331(6) 1.0464(5) 0.2521(4) 0.034(2) Uani 1 1 d . . .
H24A H 0.2304 1.0224 0.2144 0.041 Uiso 1 1 calc R . .
H24B H 0.2361 1.1020 0.2465 0.041 Uiso 1 1 calc R . .
C25 C 0.1185(6) 1.0225(6) 0.4203(4) 0.043(2) Uani 1 1 d . . .
C26 C 0.1117(6) 1.0715(5) 0.3291(3) 0.043(2) Uani 1 1 d . . .
H26 H 0.1025 1.1255 0.3177 0.052 Uiso 1 1 calc R . .
C27 C 0.0192(6) 1.0322(5) 0.3411(3) 0.043(2) Uani 1 1 d . . .
H27 H -0.0320 1.0692 0.3429 0.052 Uiso 1 1 calc R . .
C28 C 0.0845(7) 0.9751(6) 0.2610(4) 0.049(2) Uani 1 1 d . . .
C29 C -0.0328(7) 0.9582(6) 0.4308(4) 0.049(2) Uani 1 1 d . . .
H29A H -0.0163 0.9621 0.4712 0.059 Uiso 1 1 calc R . .
H29B H -0.0908 0.9852 0.4254 0.059 Uiso 1 1 calc R . .
C30 C -0.0694(7) 0.9354(6) 0.2840(4) 0.049(2) Uani 1 1 d . . .
H30A H -0.0726 0.9251 0.2430 0.058 Uiso 1 1 calc R . .
H30B H -0.1235 0.9653 0.2944 0.058 Uiso 1 1 calc R . .
C31 C -0.0200(6) 0.8200(6) 0.4509(4) 0.041(2) Uani 1 1 d . . .
C32 C -0.1076(6) 0.8529(6) 0.3717(4) 0.044(2) Uani 1 1 d . . .
H32 H -0.1690 0.8760 0.3758 0.053 Uiso 1 1 calc R . .
C33 C -0.1097(6) 0.7644(6) 0.3798(3) 0.046(2) Uani 1 1 d . . .
H33 H -0.1725 0.7444 0.3844 0.055 Uiso 1 1 calc R . .
C34 C -0.0547(7) 0.7954(7) 0.2884(4) 0.055(3) Uani 1 1 d . . .
C35 C -0.0527(6) 0.6833(5) 0.4632(3) 0.049(3) Uani 1 1 d . . .
H35A H -0.1140 0.6608 0.4627 0.059 Uiso 1 1 calc R . .
H35B H -0.0374 0.6951 0.5029 0.059 Uiso 1 1 calc R . .
C36 C -0.0716(8) 0.6567(7) 0.3127(4) 0.060(3) Uani 1 1 d . . .
H36A H -0.1303 0.6356 0.3252 0.072 Uiso 1 1 calc R . .
H36B H -0.0688 0.6521 0.2711 0.072 Uiso 1 1 calc R . .
C37 C -0.0912(8) 0.5307(7) 0.3986(5) 0.063(3) Uani 1 1 d . . .
H37A H -0.0930 0.5058 0.4355 0.095 Uiso 1 1 calc R . .
H37B H -0.0964 0.4925 0.3688 0.095 Uiso 1 1 calc R . .
H37C H -0.1414 0.5667 0.3957 0.095 Uiso 1 1 calc R . .
C38 C 0.0736(8) 0.4375(6) 0.3922(4) 0.061(3) Uani 1 1 d . . .
H38A H 0.0433 0.4215 0.4270 0.091 Uiso 1 1 calc R . .
H38B H 0.1325 0.4124 0.3894 0.091 Uiso 1 1 calc R . .
H38C H 0.0363 0.4234 0.3597 0.091 Uiso 1 1 calc R . .
C39 C 0.3548(8) 0.4277(6) 0.3923(4) 0.058(3) Uani 1 1 d . . .
H39A H 0.3854 0.4119 0.3575 0.087 Uiso 1 1 calc R . .
H39B H 0.2951 0.4036 0.3942 0.087 Uiso 1 1 calc R . .
H39C H 0.3909 0.4122 0.4249 0.087 Uiso 1 1 calc R . .
C40 C 0.5225(8) 0.5150(8) 0.4078(4) 0.058(4) Uani 1 1 d . . .
H40A H 0.5175 0.4975 0.4469 0.087 Uiso 1 1 calc R . .
H40B H 0.5762 0.5471 0.4038 0.087 Uiso 1 1 calc R . .
H40C H 0.5277 0.4711 0.3827 0.087 Uiso 1 1 calc R . .
N1 N 0.0139(5) 0.6258(4) 0.4410(3) 0.0377(17) Uani 1 1 d . . .
N2 N 0.1340(5) 0.5478(4) 0.4456(3) 0.0383(17) Uani 1 1 d . . .
N3 N 0.0027(5) 0.6108(4) 0.3378(3) 0.0455(19) Uani 1 1 d . . .
N4 N 0.1336(5) 0.5495(4) 0.3409(3) 0.0404(17) Uani 1 1 d . . .
N5 N 0.2993(5) 0.5428(4) 0.4442(3) 0.0350(16) Uani 1 1 d . . .
N6 N 0.4197(5) 0.6220(4) 0.4356(3) 0.0392(17) Uani 1 1 d . . .
N7 N 0.3008(5) 0.5409(4) 0.3402(3) 0.0411(18) Uani 1 1 d . . .
N8 N 0.4379(5) 0.5896(4) 0.3344(3) 0.0409(18) Uani 1 1 d . . .
N9 N 0.4959(5) 0.7427(4) 0.4230(3) 0.0394(17) Uani 1 1 d . . .
N10 N 0.5113(6) 0.8681(5) 0.4047(3) 0.041(2) Uani 1 1 d . . .
N11 N 0.5141(4) 0.7112(6) 0.3224(3) 0.0463(19) Uani 1 1 d . . .
N12 N 0.5216(5) 0.8381(4) 0.3041(3) 0.0387(17) Uani 1 1 d . . .
N13 N 0.4495(5) 0.9938(5) 0.3878(3) 0.048(2) Uani 1 1 d . . .
N14 N 0.3265(5) 1.0651(5) 0.3786(3) 0.0445(18) Uani 1 1 d . . .
N15 N 0.4477(5) 0.9598(4) 0.2864(3) 0.0429(18) Uani 1 1 d . . .
N16 N 0.3146(5) 1.0215(5) 0.2806(3) 0.0436(18) Uani 1 1 d . . .
N17 N 0.1603(5) 1.0673(4) 0.3824(3) 0.0434(18) Uani 1 1 d . . .
N18 N 0.0381(6) 0.9961(5) 0.3965(3) 0.047(2) Uani 1 1 d . . .
N19 N 0.1499(5) 1.0280(5) 0.2830(3) 0.0470(19) Uani 1 1 d . . .
N20 N 0.0098(5) 0.9796(4) 0.2953(3) 0.0428(18) Uani 1 1 d . . .
N21 N -0.0451(6) 0.8786(5) 0.4164(3) 0.042(2) Uani 1 1 d . . .
N22 N -0.0540(5) 0.7536(5) 0.4310(3) 0.0468(19) Uani 1 1 d . . .
N23 N -0.0714(5) 0.8623(4) 0.3148(3) 0.0451(19) Uani 1 1 d . . .
N24 N -0.0677(6) 0.7392(6) 0.3283(4) 0.051(2) Uani 1 1 d . . .
O1 O 0.1137(4) 0.6390(3) 0.5163(2) 0.0403(14) Uani 1 1 d . . .
O2 O 0.3114(4) 0.6453(4) 0.5055(2) 0.0458(15) Uani 1 1 d . . .
O3 O 0.4411(4) 0.8332(4) 0.4875(2) 0.0505(16) Uani 1 1 d . . .
O4 O 0.3675(4) 1.0233(4) 0.4679(2) 0.0498(16) Uani 1 1 d . . .
O5 O 0.1424(5) 1.0081(4) 0.4697(3) 0.0622(19) Uani 1 1 d . . .
O6 O 0.0260(4) 0.8292(4) 0.4942(2) 0.0499(16) Uani 1 1 d . . .
O7 O 0.1011(5) 0.6188(4) 0.2622(2) 0.0581(18) Uani 1 1 d . . .
O8 O 0.3448(4) 0.6025(4) 0.2578(2) 0.0498(16) Uani 1 1 d . . .
O9 O 0.4744(5) 0.7561(4) 0.2334(2) 0.0603(19) Uani 1 1 d . . .
O10 O 0.3439(4) 0.9190(4) 0.2189(2) 0.0511(16) Uani 1 1 d . . .
O11 O 0.0947(5) 0.9365(4) 0.2193(2) 0.061(2) Uani 1 1 d . . .
O12 O -0.0297(6) 0.7857(5) 0.2401(3) 0.076(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N26 O17 1.248(2) . ?
N26 O16 1.249(2) . ?
N26 O18 1.249(2) . ?
N25 O15 1.229(10) . ?
N25 O14 1.258(9) . ?
N25 O13 1.259(10) . ?
O1W Nd1 2.450(5) . ?
O2W Nd1 2.494(7) . ?
O3W Nd1 2.464(5) . ?
O4W Nd1 2.466(6) . ?
O5W Nd1 2.455(6) . ?
O13 Nd1 2.529(8) . ?
O14 Nd1 2.670(6) . ?
Nd1 O2 2.454(5) . ?
Nd1 O1 2.479(5) . ?
C1 O1 1.253(9) . ?
C1 N1 1.340(11) . ?
C1 N2 1.370(10) . ?
C2 N3 1.437(11) . ?
C2 N1 1.485(11) . ?
C2 C37 1.513(13) . ?
C2 C3 1.564(13) . ?
C3 N4 1.475(10) . ?
C3 N2 1.478(10) . ?
C3 C38 1.506(14) . ?
C4 O7 1.151(10) . ?
C4 N3 1.380(12) . ?
C4 N4 1.386(12) . ?
C5 N5 1.425(10) . ?
C5 N2 1.439(11) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.455(10) . ?
C6 N7 1.458(11) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.243(9) . ?
C7 N5 1.354(10) . ?
C7 N6 1.378(10) . ?
C8 N7 1.454(10) . ?
C8 N5 1.467(10) . ?
C8 C39 1.517(13) . ?
C8 C9 1.593(13) . ?
C9 N8 1.434(10) . ?
C9 N6 1.492(10) . ?
C9 C40 1.543(13) . ?
C10 O8 1.198(9) . ?
C10 N8 1.344(11) . ?
C10 N7 1.378(11) . ?
C11 N9 1.430(10) . ?
C11 N6 1.448(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.434(14) . ?
C12 N8 1.464(11) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.187(9) . ?
C13 N10 1.354(11) . ?
C13 N9 1.433(11) . ?
C14 N9 1.451(10) . ?
C14 N11 1.468(10) . ?
C14 C15 1.551(12) . ?
C14 H14 0.9900 . ?
C15 N10 1.451(10) . ?
C15 N12 1.462(10) . ?
C15 H15 0.9900 . ?
C16 O9 1.192(9) . ?
C16 N12 1.380(11) . ?
C16 N11 1.403(12) . ?
C17 N10 1.454(12) . ?
C17 N13 1.482(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N15 1.432(11) . ?
C18 N12 1.457(11) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 O4 1.182(9) . ?
C19 N14 1.367(11) . ?
C19 N13 1.391(12) . ?
C20 N15 1.435(10) . ?
C20 N13 1.465(10) . ?
C20 C21 1.574(12) . ?
C20 H20 0.9900 . ?
C21 N14 1.416(10) . ?
C21 N16 1.440(11) . ?
C21 H21 0.9900 . ?
C22 O10 1.245(11) . ?
C22 N16 1.354(12) . ?
C22 N15 1.386(11) . ?
C23 N14 1.445(12) . ?
C23 N17 1.447(12) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 N16 1.435(11) . ?
C24 N19 1.454(11) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 O5 1.236(10) . ?
C25 N17 1.335(12) . ?
C25 N18 1.381(12) . ?
C26 N19 1.436(11) . ?
C26 N17 1.439(10) . ?
C26 C27 1.544(12) . ?
C26 H26 0.9900 . ?
C27 N20 1.419(11) . ?
C27 N18 1.472(11) . ?
C27 H27 0.9900 . ?
C28 O11 1.198(11) . ?
C28 N20 1.359(12) . ?
C28 N19 1.426(12) . ?
C29 N21 1.441(13) . ?
C29 N18 1.471(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 N20 1.419(11) . ?
C30 N23 1.467(11) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 O6 1.230(10) . ?
C31 N22 1.345(12) . ?
C31 N21 1.355(12) . ?
C32 N23 1.447(10) . ?
C32 N21 1.461(11) . ?
C32 C33 1.556(14) . ?
C32 H32 0.9900 . ?
C33 N24 1.427(12) . ?
C33 N22 1.463(10) . ?
C33 H33 0.9900 . ?
C34 O12 1.204(11) . ?
C34 N23 1.344(12) . ?
C34 N24 1.369(13) . ?
C35 N22 1.441(11) . ?
C35 N1 1.494(11) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C36 N3 1.474(13) . ?
C36 N24 1.486(12) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?

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
O17 N26 O16 112.0(9) . . ?
O17 N26 O18 124.9(13) . . ?
O16 N26 O18 122.6(12) . . ?
O15 N25 O14 123.4(8) . . ?
O15 N25 O13 120.6(8) . . ?
O14 N25 O13 116.0(8) . . ?
N25 O13 Nd1 100.9(5) . . ?
N25 O14 Nd1 94.1(5) . . ?
O1W Nd1 O2 135.3(2) . . ?
O1W Nd1 O5W 83.2(2) . . ?
O2 Nd1 O5W 74.3(2) . . ?
O1W Nd1 O3W 70.63(18) . . ?
O2 Nd1 O3W 143.1(2) . . ?
O5W Nd1 O3W 142.3(3) . . ?
O1W Nd1 O4W 141.4(3) . . ?
O2 Nd1 O4W 72.7(2) . . ?
O5W Nd1 O4W 81.1(2) . . ?
O3W Nd1 O4W 102.6(2) . . ?
O1W Nd1 O1 133.5(2) . . ?
O2 Nd1 O1 72.2(2) . . ?
O5W Nd1 O1 142.41(18) . . ?
O3W Nd1 O1 71.4(2) . . ?
O4W Nd1 O1 73.1(2) . . ?
O1W Nd1 O2W 71.0(3) . . ?
O2 Nd1 O2W 134.6(2) . . ?
O5W Nd1 O2W 74.2(3) . . ?
O3W Nd1 O2W 71.9(3) . . ?
O4W Nd1 O2W 70.9(2) . . ?
O1 Nd1 O2W 120.1(3) . . ?
O1W Nd1 O13 72.7(3) . . ?
O2 Nd1 O13 87.4(2) . . ?
O5W Nd1 O13 122.3(2) . . ?
O3W Nd1 O13 75.7(3) . . ?
O4W Nd1 O13 144.3(2) . . ?
O1 Nd1 O13 72.7(2) . . ?
O2W Nd1 O13 137.44(17) . . ?
O1W Nd1 O14 68.8(3) . . ?
O2 Nd1 O14 68.07(19) . . ?
O5W Nd1 O14 74.2(2) . . ?
O3W Nd1 O14 117.8(2) . . ?
O4W Nd1 O14 137.9(2) . . ?
O1 Nd1 O14 107.80(19) . . ?
O2W Nd1 O14 130.9(3) . . ?
O13 Nd1 O14 48.4(2) . . ?
O1 C1 N1 125.5(8) . . ?
O1 C1 N2 124.2(8) . . ?
N1 C1 N2 110.4(7) . . ?
N3 C2 N1 113.3(7) . . ?
N3 C2 C37 110.5(8) . . ?
N1 C2 C37 111.0(8) . . ?
N3 C2 C3 103.3(7) . . ?
N1 C2 C3 102.1(6) . . ?
C37 C2 C3 116.3(8) . . ?
N4 C3 N2 112.5(7) . . ?
N4 C3 C38 111.1(8) . . ?
N2 C3 C38 111.2(7) . . ?
N4 C3 C2 101.4(7) . . ?
N2 C3 C2 103.5(6) . . ?
C38 C3 C2 116.6(8) . . ?
O7 C4 N3 129.3(10) . . ?
O7 C4 N4 125.6(9) . . ?
N3 C4 N4 105.0(7) . . ?
N5 C5 N2 115.5(7) . . ?
N5 C5 H5A 108.4 . . ?
N2 C5 H5A 108.4 . . ?
N5 C5 H5B 108.4 . . ?
N2 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
N4 C6 N7 114.7(7) . . ?
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 N5 124.9(8) . . ?
O2 C7 N6 124.2(8) . . ?
N5 C7 N6 110.9(7) . . ?
N7 C8 N5 113.4(7) . . ?
N7 C8 C39 111.4(7) . . ?
N5 C8 C39 112.9(7) . . ?
N7 C8 C9 101.2(6) . . ?
N5 C8 C9 102.0(6) . . ?
C39 C8 C9 115.2(8) . . ?
N8 C9 N6 114.1(7) . . ?
N8 C9 C40 113.3(7) . . ?
N6 C9 C40 110.0(8) . . ?
N8 C9 C8 101.3(7) . . ?
N6 C9 C8 102.8(6) . . ?
C40 C9 C8 114.8(8) . . ?
O8 C10 N8 126.3(9) . . ?
O8 C10 N7 126.9(8) . . ?
N8 C10 N7 106.7(7) . . ?
N9 C11 N6 113.1(6) . . ?
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 112.9(7) . . ?
N11 C12 H12A 109.0 . . ?
N8 C12 H12A 109.0 . . ?
N11 C12 H12B 109.0 . . ?
N8 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N10 127.6(9) . . ?
O3 C13 N9 125.3(8) . . ?
N10 C13 N9 107.1(7) . . ?
N9 C14 N11 113.3(7) . . ?
N9 C14 C15 104.1(6) . . ?
N11 C14 C15 105.2(7) . . ?
N9 C14 H14 111.3 . . ?
N11 C14 H14 111.3 . . ?
C15 C14 H14 111.3 . . ?
N10 C15 N12 112.5(7) . . ?
N10 C15 C14 103.4(7) . . ?
N12 C15 C14 102.6(6) . . ?
N10 C15 H15 112.5 . . ?
N12 C15 H15 112.5 . . ?
C14 C15 H15 112.5 . . ?
O9 C16 N12 126.4(8) . . ?
O9 C16 N11 125.1(9) . . ?
N12 C16 N11 108.5(7) . . ?
N10 C17 N13 110.1(7) . . ?
N10 C17 H17A 109.6 . . ?
N13 C17 H17A 109.6 . . ?
N10 C17 H17B 109.6 . . ?
N13 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
N15 C18 N12 113.7(7) . . ?
N15 C18 H18A 108.8 . . ?
N12 C18 H18A 108.8 . . ?
N15 C18 H18B 108.8 . . ?
N12 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
O4 C19 N14 128.8(8) . . ?
O4 C19 N13 125.4(9) . . ?
N14 C19 N13 105.8(7) . . ?
N15 C20 N13 115.6(7) . . ?
N15 C20 C21 104.5(6) . . ?
N13 C20 C21 101.0(6) . . ?
N15 C20 H20 111.7 . . ?
N13 C20 H20 111.7 . . ?
C21 C20 H20 111.7 . . ?
N14 C21 N16 116.5(7) . . ?
N14 C21 C20 103.9(6) . . ?
N16 C21 C20 101.8(7) . . ?
N14 C21 H21 111.3 . . ?
N16 C21 H21 111.3 . . ?
C20 C21 H21 111.3 . . ?
O10 C22 N16 128.3(8) . . ?
O10 C22 N15 122.4(9) . . ?
N16 C22 N15 109.0(8) . . ?
N14 C23 N17 114.7(8) . . ?
N14 C23 H23A 108.6 . . ?
N17 C23 H23A 108.6 . . ?
N14 C23 H23B 108.6 . . ?
N17 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
N16 C24 N19 113.4(7) . . ?
N16 C24 H24A 108.9 . . ?
N19 C24 H24A 108.9 . . ?
N16 C24 H24B 108.9 . . ?
N19 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
O5 C25 N17 127.9(8) . . ?
O5 C25 N18 123.6(9) . . ?
N17 C25 N18 108.4(7) . . ?
N19 C26 N17 115.8(7) . . ?
N19 C26 C27 104.0(7) . . ?
N17 C26 C27 104.7(7) . . ?
N19 C26 H26 110.6 . . ?
N17 C26 H26 110.6 . . ?
C27 C26 H26 110.6 . . ?
N20 C27 N18 114.2(7) . . ?
N20 C27 C26 103.6(7) . . ?
N18 C27 C26 100.7(7) . . ?
N20 C27 H27 112.5 . . ?
N18 C27 H27 112.5 . . ?
C26 C27 H27 112.5 . . ?
O11 C28 N20 128.1(10) . . ?
O11 C28 N19 125.1(9) . . ?
N20 C28 N19 106.7(8) . . ?
N21 C29 N18 113.1(7) . . ?
N21 C29 H29A 109.0 . . ?
N18 C29 H29A 109.0 . . ?
N21 C29 H29B 109.0 . . ?
N18 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
N20 C30 N23 113.4(7) . . ?
N20 C30 H30A 108.9 . . ?
N23 C30 H30A 108.9 . . ?
N20 C30 H30B 108.9 . . ?
N23 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
O6 C31 N22 127.0(9) . . ?
O6 C31 N21 123.0(9) . . ?
N22 C31 N21 110.0(8) . . ?
N23 C32 N21 113.5(7) . . ?
N23 C32 C33 103.4(7) . . ?
N21 C32 C33 103.3(7) . . ?
N23 C32 H32 112.0 . . ?
N21 C32 H32 112.0 . . ?
C33 C32 H32 112.0 . . ?
N24 C33 N22 114.6(8) . . ?
N24 C33 C32 101.2(7) . . ?
N22 C33 C32 102.5(7) . . ?
N24 C33 H33 112.5 . . ?
N22 C33 H33 112.5 . . ?
C32 C33 H33 112.5 . . ?
O12 C34 N23 127.7(10) . . ?
O12 C34 N24 125.8(11) . . ?
N23 C34 N24 106.4(8) . . ?
N22 C35 N1 113.5(7) . . ?
N22 C35 H35A 108.9 . . ?
N1 C35 H35A 108.9 . . ?
N22 C35 H35B 108.9 . . ?
N1 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
N3 C36 N24 113.6(8) . . ?
N3 C36 H36A 108.8 . . ?
N24 C36 H36A 108.8 . . ?
N3 C36 H36B 108.8 . . ?
N24 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
C2 C37 H37A 109.5 . . ?
C2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C38 H38A 109.5 . . ?
C3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C8 C39 H39A 109.5 . . ?
C8 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C8 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C9 C40 H40A 109.5 . . ?
C9 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C9 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C1 N1 C2 112.5(7) . . ?
C1 N1 C35 120.7(7) . . ?
C2 N1 C35 125.8(7) . . ?
C1 N2 C5 123.4(7) . . ?
C1 N2 C3 111.1(7) . . ?
C5 N2 C3 125.5(7) . . ?
C4 N3 C2 115.2(8) . . ?
C4 N3 C36 119.8(8) . . ?
C2 N3 C36 124.8(8) . . ?
C4 N4 C6 119.2(7) . . ?
C4 N4 C3 114.3(7) . . ?
C6 N4 C3 124.2(8) . . ?
C7 N5 C5 121.3(7) . . ?
C7 N5 C8 112.4(7) . . ?
C5 N5 C8 125.9(7) . . ?
C7 N6 C11 121.4(7) . . ?
C7 N6 C9 110.1(7) . . ?
C11 N6 C9 125.9(7) . . ?
C10 N7 C8 113.3(7) . . ?
C10 N7 C6 119.1(7) . . ?
C8 N7 C6 125.7(8) . . ?
C10 N8 C9 115.3(7) . . ?
C10 N8 C12 120.3(7) . . ?
C9 N8 C12 124.1(7) . . ?
C11 N9 C13 123.0(6) . . ?
C11 N9 C14 122.1(7) . . ?
C13 N9 C14 110.7(7) . . ?
C13 N10 C15 113.7(8) . . ?
C13 N10 C17 121.1(8) . . ?
C15 N10 C17 121.4(8) . . ?
C16 N11 C12 122.2(7) . . ?
C16 N11 C14 110.1(8) . . ?
C12 N11 C14 124.7(8) . . ?
C16 N12 C18 122.4(6) . . ?
C16 N12 C15 112.7(7) . . ?
C18 N12 C15 123.4(7) . . ?
C19 N13 C20 113.6(7) . . ?
C19 N13 C17 120.7(7) . . ?
C20 N13 C17 124.7(7) . . ?
C19 N14 C21 115.0(7) . . ?
C19 N14 C23 122.2(7) . . ?
C21 N14 C23 122.6(7) . . ?
C22 N15 C18 124.1(8) . . ?
C22 N15 C20 110.9(7) . . ?
C18 N15 C20 124.7(7) . . ?
C22 N16 C24 120.0(7) . . ?
C22 N16 C21 113.5(7) . . ?
C24 N16 C21 124.6(7) . . ?
C25 N17 C26 112.5(7) . . ?
C25 N17 C23 123.4(7) . . ?
C26 N17 C23 124.1(7) . . ?
C25 N18 C29 122.0(8) . . ?
C25 N18 C27 112.0(8) . . ?
C29 N18 C27 122.9(7) . . ?
C28 N19 C26 110.7(7) . . ?
C28 N19 C24 121.6(7) . . ?
C26 N19 C24 125.9(8) . . ?
C28 N20 C30 121.0(8) . . ?
C28 N20 C27 114.1(8) . . ?
C30 N20 C27 125.0(7) . . ?
C31 N21 C29 123.5(8) . . ?
C31 N21 C32 111.5(8) . . ?
C29 N21 C32 122.9(8) . . ?
C31 N22 C35 123.1(7) . . ?
C31 N22 C33 112.3(8) . . ?
C35 N22 C33 123.2(8) . . ?
C34 N23 C32 113.2(8) . . ?
C34 N23 C30 121.7(7) . . ?
C32 N23 C30 124.2(8) . . ?
C34 N24 C33 114.7(9) . . ?
C34 N24 C36 122.0(9) . . ?
C33 N24 C36 119.5(9) . . ?
C1 O1 Nd1 156.3(6) . . ?
C7 O2 Nd1 166.2(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.102

# 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 0.071 0.227 0.881 31 7 ' '
2 0.119 0.257 0.381 14 8 ' '
3 0.227 0.799 0.348 104 26 ' '
4 0.273 0.799 0.848 104 26 ' '
5 0.221 0.963 0.074 19 10 ' '
6 0.225 0.123 0.059 14 8 ' '
7 0.275 0.120 0.560 15 8 ' '
8 0.278 0.961 0.575 18 10 ' '
9 0.429 0.226 0.381 31 7 ' '
10 0.380 0.257 0.881 14 8 ' '
11 0.571 0.727 0.619 31 7 ' '
12 0.727 0.299 0.152 104 26 ' '
13 0.619 0.757 0.119 14 8 ' '
14 0.773 0.299 0.652 104 26 ' '
15 0.721 0.463 0.425 19 10 ' '
16 0.725 0.623 0.441 14 8 ' '
17 0.778 0.463 0.925 19 10 ' '
18 0.775 0.623 0.941 14 8 ' '
19 0.929 0.726 0.119 31 7 ' '
20 0.880 0.757 0.619 14 8 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997810'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_06Sm
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H54 N25 Sm O20, N O3, Cl, 6(H2 O)'
_chemical_formula_sum            'C40 H66 Cl N26 O29 Sm'
_chemical_formula_weight         1560.99

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'
Sm Sm -0.1638 3.4418 '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           orthorhombic
_symmetry_space_group_name_H-M   'P c 21 n'
_symmetry_space_group_name_Hall  'P -2n -2ac'

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

_cell_length_a                   14.6418(17)
_cell_length_b                   17.407(2)
_cell_length_c                   23.369(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5956.0(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3196
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7327
_exptl_absorpt_correction_T_max  0.7709
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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            36773
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.10
_reflns_number_total             10279
_reflns_number_gt                8731
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0830P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.104(12)
_refine_ls_number_reflns         10279
_refine_ls_number_parameters     831
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1305
_refine_ls_wR_factor_gt          0.1248
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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 0.2782(3) 0.5547(10) 0.2571(5) 0.293(8) Uani 0.797(12) 1 d P A 1
Cl1' Cl 0.2732(7) 0.5088(9) 0.2093(5) 0.068(6) Uani 0.203(12) 1 d P A 2
N26 N 0.2261(5) 0.5698(5) 0.5038(4) 0.062(2) Uani 1 1 d . . .
O16 O 0.2989(4) 0.5856(4) 0.4823(3) 0.0763(19) Uani 1 1 d . . .
O17 O 0.1973(6) 0.6068(9) 0.5402(5) 0.175(6) Uani 1 1 d . . .
O18 O 0.1759(9) 0.5178(8) 0.4820(5) 0.164(5) Uani 1 1 d . . .
O1W O 0.2683(3) -0.0293(4) 0.68561(18) 0.0419(11) Uani 1 1 d . . .
O2W O 0.3102(5) 0.0969(3) 0.6123(2) 0.0486(15) Uani 1 1 d . . .
O3W O 0.1312(3) 0.0266(3) 0.58540(18) 0.0404(12) Uani 1 1 d . . .
O4W O 0.4314(3) -0.0317(4) 0.62372(17) 0.0416(10) Uani 1 1 d . . .
O5W O 0.2942(3) 0.0464(3) 0.4991(2) 0.0437(12) Uani 1 1 d . . .
N25 N 0.2227(3) -0.1874(3) 0.6345(2) 0.0344(14) Uani 1 1 d . . .
O13 O 0.3039(3) -0.1690(3) 0.6192(2) 0.0383(13) Uani 1 1 d . . .
O14 O 0.1612(3) -0.1395(3) 0.6215(2) 0.0428(12) Uani 1 1 d . . .
O15 O 0.2086(3) -0.2470(3) 0.6612(3) 0.0507(14) Uani 1 1 d . . .
Sm1 Sm 0.279370(16) -0.03626(3) 0.582280(11) 0.02623(10) Uani 1 1 d . . .
C1 C 0.4120(4) -0.1318(3) 0.4718(2) 0.0275(13) Uani 1 1 d . . .
C2 C 0.5032(4) -0.1664(4) 0.3933(3) 0.0330(15) Uani 1 1 d . . .
C3 C 0.4143(5) -0.2170(4) 0.3935(3) 0.0369(16) Uani 1 1 d . . .
C4 C 0.4209(5) -0.1418(4) 0.3085(3) 0.0364(16) Uani 1 1 d . . .
C5 C 0.2852(4) -0.2239(4) 0.4692(3) 0.0305(15) Uani 1 1 d . . .
H5A H 0.2879 -0.2791 0.4642 0.037 Uiso 1 1 calc R . .
H5B H 0.2840 -0.2136 0.5100 0.037 Uiso 1 1 calc R . .
C6 C 0.2878(4) -0.2252(4) 0.3170(3) 0.0382(17) Uani 1 1 d . . .
H6A H 0.2915 -0.2802 0.3232 0.046 Uiso 1 1 calc R . .
H6B H 0.2882 -0.2165 0.2760 0.046 Uiso 1 1 calc R . .
C7 C 0.1614(4) -0.1325(4) 0.4653(2) 0.0283(14) Uani 1 1 d . . .
C8 C 0.1581(4) -0.2260(4) 0.3927(3) 0.0320(14) Uani 1 1 d . . .
C9 C 0.0643(4) -0.1771(4) 0.3922(3) 0.0319(14) Uani 1 1 d . . .
C10 C 0.1402(4) -0.1569(4) 0.3063(3) 0.0291(14) Uani 1 1 d . . .
C11 C 0.0146(4) -0.0630(4) 0.4581(2) 0.0330(16) Uani 1 1 d . . .
H11A H -0.0439 -0.0889 0.4604 0.040 Uiso 1 1 calc R . .
H11B H 0.0319 -0.0478 0.4965 0.040 Uiso 1 1 calc R . .
C12 C -0.0143(5) -0.1064(5) 0.3095(3) 0.0390(18) Uani 1 1 d . . .
H12A H -0.0118 -0.1123 0.2682 0.047 Uiso 1 1 calc R . .
H12B H -0.0715 -0.1284 0.3225 0.047 Uiso 1 1 calc R . .
C13 C 0.0221(4) 0.0789(4) 0.4440(3) 0.0287(14) Uani 1 1 d . . .
C14 C -0.0547(4) 0.0063(4) 0.3737(2) 0.0297(14) Uani 1 1 d . . .
H14 H -0.1142 -0.0169 0.3820 0.036 Uiso 1 1 calc R . .
C15 C -0.0634(4) 0.0929(4) 0.3602(2) 0.0253(13) Uani 1 1 d . . .
H15 H -0.1271 0.1102 0.3599 0.030 Uiso 1 1 calc R . .
C16 C -0.0005(5) 0.0284(4) 0.2812(3) 0.0337(16) Uani 1 1 d . . .
C17 C -0.0199(5) 0.2111(5) 0.4164(3) 0.0344(16) Uani 1 1 d . . .
H17A H -0.0797 0.2284 0.4042 0.041 Uiso 1 1 calc R . .
H17B H -0.0151 0.2197 0.4574 0.041 Uiso 1 1 calc R . .
C18 C -0.0205(4) 0.1705(4) 0.2705(3) 0.0341(15) Uani 1 1 d . . .
H18A H -0.0156 0.1578 0.2302 0.041 Uiso 1 1 calc R . .
H18B H -0.0781 0.1970 0.2762 0.041 Uiso 1 1 calc R . .
C19 C 0.1207(5) 0.2899(4) 0.4172(3) 0.0310(15) Uani 1 1 d . . .
C20 C 0.0440(4) 0.2820(4) 0.3281(3) 0.0349(15) Uani 1 1 d . . .
H20 H -0.0093 0.3148 0.3213 0.042 Uiso 1 1 calc R . .
C21 C 0.1373(4) 0.3270(4) 0.3215(3) 0.0328(15) Uani 1 1 d . . .
H21 H 0.1271 0.3793 0.3076 0.039 Uiso 1 1 calc R . .
C22 C 0.1350(5) 0.2229(4) 0.2587(3) 0.0363(16) Uani 1 1 d . . .
C23 C 0.2547(5) 0.3694(4) 0.3938(3) 0.0372(16) Uani 1 1 d . . .
H23A H 0.2550 0.4181 0.3736 0.045 Uiso 1 1 calc R . .
H23B H 0.2519 0.3805 0.4344 0.045 Uiso 1 1 calc R . .
C24 C 0.2693(4) 0.3074(4) 0.2518(3) 0.0278(14) Uani 1 1 d . . .
H24A H 0.2724 0.2855 0.2137 0.033 Uiso 1 1 calc R . .
H24B H 0.2666 0.3628 0.2478 0.033 Uiso 1 1 calc R . .
C25 C 0.3829(5) 0.2841(4) 0.4202(3) 0.0343(16) Uani 1 1 d . . .
C26 C 0.3881(4) 0.3328(4) 0.3284(3) 0.0363(15) Uani 1 1 d . . .
H26 H 0.3971 0.3862 0.3163 0.044 Uiso 1 1 calc R . .
C27 C 0.4809(4) 0.2945(4) 0.3422(3) 0.0355(15) Uani 1 1 d . . .
H27 H 0.5310 0.3317 0.3445 0.043 Uiso 1 1 calc R . .
C28 C 0.4165(5) 0.2365(5) 0.2607(3) 0.0426(18) Uani 1 1 d . . .
C29 C 0.5330(5) 0.2202(4) 0.4311(3) 0.0343(15) Uani 1 1 d . . .
H29A H 0.5903 0.2472 0.4255 0.041 Uiso 1 1 calc R . .
H29B H 0.5172 0.2241 0.4713 0.041 Uiso 1 1 calc R . .
C30 C 0.5722(5) 0.1977(4) 0.2846(3) 0.0406(17) Uani 1 1 d . . .
H30A H 0.6246 0.2280 0.2963 0.049 Uiso 1 1 calc R . .
H30B H 0.5778 0.1881 0.2439 0.049 Uiso 1 1 calc R . .
C31 C 0.5206(4) 0.0831(4) 0.4520(3) 0.0298(14) Uani 1 1 d . . .
C32 C 0.6086(4) 0.1150(4) 0.3725(3) 0.0363(17) Uani 1 1 d . . .
H32 H 0.6693 0.1380 0.3771 0.044 Uiso 1 1 calc R . .
C33 C 0.6111(5) 0.0270(4) 0.3803(3) 0.0381(16) Uani 1 1 d . . .
H33 H 0.6735 0.0078 0.3853 0.046 Uiso 1 1 calc R . .
C34 C 0.5584(5) 0.0556(5) 0.2885(3) 0.0442(19) Uani 1 1 d . . .
C35 C 0.5535(4) -0.0559(4) 0.4636(3) 0.0328(16) Uani 1 1 d . . .
H35A H 0.5384 -0.0442 0.5031 0.039 Uiso 1 1 calc R . .
H35B H 0.6141 -0.0784 0.4632 0.039 Uiso 1 1 calc R . .
C36 C 0.5730(6) -0.0822(5) 0.3131(3) 0.047(2) Uani 1 1 d . . .
H36A H 0.6311 -0.1034 0.3253 0.056 Uiso 1 1 calc R . .
H36B H 0.5701 -0.0865 0.2718 0.056 Uiso 1 1 calc R . .
C37 C 0.5925(5) -0.2088(5) 0.4003(4) 0.048(2) Uani 1 1 d . . .
H37A H 0.5939 -0.2334 0.4371 0.072 Uiso 1 1 calc R . .
H37B H 0.6423 -0.1731 0.3975 0.072 Uiso 1 1 calc R . .
H37C H 0.5981 -0.2469 0.3708 0.072 Uiso 1 1 calc R . .
C38 C 0.4289(6) -0.3020(5) 0.3924(3) 0.0459(19) Uani 1 1 d . . .
H38A H 0.4566 -0.3180 0.4277 0.069 Uiso 1 1 calc R . .
H38B H 0.4681 -0.3151 0.3610 0.069 Uiso 1 1 calc R . .
H38C H 0.3712 -0.3274 0.3879 0.069 Uiso 1 1 calc R . .
C39 C 0.1457(6) -0.3116(4) 0.3920(3) 0.049(2) Uani 1 1 d . . .
H39A H 0.1165 -0.3267 0.3570 0.074 Uiso 1 1 calc R . .
H39B H 0.1084 -0.3267 0.4239 0.074 Uiso 1 1 calc R . .
H39C H 0.2042 -0.3362 0.3948 0.074 Uiso 1 1 calc R . .
C40 C -0.0219(6) -0.2232(6) 0.4085(3) 0.042(2) Uani 1 1 d . . .
H40A H -0.0169 -0.2404 0.4474 0.063 Uiso 1 1 calc R . .
H40B H -0.0276 -0.2669 0.3836 0.063 Uiso 1 1 calc R . .
H40C H -0.0749 -0.1911 0.4046 0.063 Uiso 1 1 calc R . .
N1 N 0.4877(4) -0.1128(3) 0.4417(2) 0.0303(12) Uani 1 1 d . . .
N2 N 0.3674(3) -0.1910(3) 0.4457(2) 0.0288(12) Uani 1 1 d . . .
N3 N 0.4989(4) -0.1284(3) 0.3381(2) 0.0357(13) Uani 1 1 d . . .
N4 N 0.3679(3) -0.1898(3) 0.3414(2) 0.0314(12) Uani 1 1 d . . .
N5 N 0.2021(3) -0.1967(3) 0.4448(2) 0.0281(12) Uani 1 1 d . . .
N6 N 0.0832(4) -0.1169(3) 0.4356(2) 0.0315(12) Uani 1 1 d . . .
N7 N 0.2008(3) -0.1975(3) 0.3402(2) 0.0332(13) Uani 1 1 d . . .
N8 N 0.0616(3) -0.1500(3) 0.3351(2) 0.0327(13) Uani 1 1 d . . .
N9 N 0.0050(4) 0.0047(4) 0.4233(2) 0.0348(13) Uani 1 1 d . . .
N10 N -0.0109(4) 0.1292(4) 0.4047(3) 0.0345(15) Uani 1 1 d . . .
N11 N -0.0138(3) -0.0266(4) 0.3228(2) 0.0355(14) Uani 1 1 d . . .
N12 N -0.0206(3) 0.0990(3) 0.3043(2) 0.0318(12) Uani 1 1 d . . .
N13 N 0.0500(4) 0.2560(3) 0.3872(2) 0.0376(14) Uani 1 1 d . . .
N14 N 0.1730(3) 0.3274(3) 0.3778(2) 0.0343(13) Uani 1 1 d . . .
N15 N 0.0527(4) 0.2206(3) 0.2859(2) 0.0364(13) Uani 1 1 d . . .
N16 N 0.1856(4) 0.2811(4) 0.2794(2) 0.0369(13) Uani 1 1 d . . .
N17 N 0.3394(4) 0.3296(3) 0.3818(2) 0.0340(12) Uani 1 1 d . . .
N18 N 0.4611(4) 0.2587(4) 0.3968(3) 0.0399(15) Uani 1 1 d . . .
N19 N 0.3509(4) 0.2876(3) 0.2822(2) 0.0382(13) Uani 1 1 d . . .
N20 N 0.4912(4) 0.2411(3) 0.2947(2) 0.0354(13) Uani 1 1 d . . .
N21 N 0.5461(4) 0.1403(4) 0.4169(2) 0.0339(14) Uani 1 1 d . . .
N22 N 0.5552(4) 0.0145(4) 0.4315(2) 0.0372(14) Uani 1 1 d . . .
N23 N 0.5742(4) 0.1245(3) 0.3149(2) 0.0364(13) Uani 1 1 d . . .
N24 N 0.5704(4) -0.0004(4) 0.3286(3) 0.0387(15) Uani 1 1 d . . .
O1 O 0.3873(3) -0.1006(3) 0.51725(17) 0.0321(10) Uani 1 1 d . . .
O2 O 0.1894(3) -0.0946(3) 0.50617(18) 0.0370(11) Uani 1 1 d . . .
O3 O 0.0611(3) 0.0951(3) 0.48741(18) 0.0407(11) Uani 1 1 d . . .
O4 O 0.1317(3) 0.2864(3) 0.46787(18) 0.0396(11) Uani 1 1 d . . .
O5 O 0.3576(3) 0.2709(3) 0.4694(2) 0.0509(13) Uani 1 1 d . . .
O6 O 0.4743(3) 0.0893(3) 0.49483(18) 0.0383(11) Uani 1 1 d . . .
O7 O 0.4020(4) -0.1182(3) 0.26237(19) 0.0480(13) Uani 1 1 d . . .
O8 O 0.1564(3) -0.1365(3) 0.25774(17) 0.0362(11) Uani 1 1 d . . .
O9 O 0.0249(4) 0.0162(3) 0.2326(2) 0.0519(14) Uani 1 1 d . . .
O10 O 0.1566(3) 0.1789(3) 0.21908(19) 0.0421(12) Uani 1 1 d . . .
O11 O 0.4056(3) 0.1973(3) 0.21889(19) 0.0478(13) Uani 1 1 d . . .
O12 O 0.5350(4) 0.0463(4) 0.2388(2) 0.0619(16) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N26 O17 1.148(12) . ?
N26 O16 1.210(9) . ?
N26 O18 1.272(13) . ?
O1W Sm1 2.423(4) . ?
O2W Sm1 2.463(6) . ?
O3W Sm1 2.431(5) . ?
O4W Sm1 2.429(4) . ?
O5W Sm1 2.428(5) . ?
N25 O15 1.227(8) . ?
N25 O14 1.265(7) . ?
N25 O13 1.283(7) . ?
O13 Sm1 2.492(6) . ?
O14 Sm1 2.658(5) . ?
Sm1 O2 2.436(4) . ?
Sm1 O1 2.463(4) . ?
C1 O1 1.246(7) . ?
C1 N1 1.354(8) . ?
C1 N2 1.363(8) . ?
C2 N3 1.450(8) . ?
C2 N1 1.484(8) . ?
C2 C37 1.510(10) . ?
C2 C3 1.572(10) . ?
C3 N4 1.472(8) . ?
C3 N2 1.473(8) . ?
C3 C38 1.494(11) . ?
C4 O7 1.186(8) . ?
C4 N3 1.356(9) . ?
C4 N4 1.374(9) . ?
C5 N5 1.424(7) . ?
C5 N2 1.441(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N4 1.443(8) . ?
C6 N7 1.467(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O2 1.230(7) . ?
C7 N5 1.355(8) . ?
C7 N6 1.365(8) . ?
C8 N7 1.462(8) . ?
C8 N5 1.470(8) . ?
C8 C39 1.502(10) . ?
C8 C9 1.616(9) . ?
C9 N8 1.415(8) . ?
C9 N6 1.484(8) . ?
C9 C40 1.544(10) . ?
C10 O8 1.212(7) . ?
C10 N8 1.339(8) . ?
C10 N7 1.384(8) . ?
C11 N9 1.438(8) . ?
C11 N6 1.472(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N11 1.423(11) . ?
C12 N8 1.473(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 O3 1.198(7) . ?
C13 N10 1.358(9) . ?
C13 N9 1.402(9) . ?
C14 N11 1.449(8) . ?
C14 N9 1.452(8) . ?
C14 C15 1.546(9) . ?
C14 H14 0.9800 . ?
C15 N10 1.438(8) . ?
C15 N12 1.454(7) . ?
C15 H15 0.9800 . ?
C16 O9 1.215(8) . ?
C16 N12 1.373(9) . ?
C16 N11 1.378(10) . ?
C17 N13 1.457(9) . ?
C17 N10 1.458(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N15 1.428(9) . ?
C18 N12 1.474(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 O4 1.196(7) . ?
C19 N14 1.364(9) . ?
C19 N13 1.382(9) . ?
C20 N13 1.456(8) . ?
C20 N15 1.460(9) . ?
C20 C21 1.582(9) . ?
C20 H20 0.9800 . ?
C21 N14 1.415(8) . ?
C21 N16 1.451(9) . ?
C21 H21 0.9800 . ?
C22 O10 1.242(8) . ?
C22 N16 1.346(9) . ?
C22 N15 1.364(9) . ?
C23 N17 1.448(9) . ?
C23 N14 1.451(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 N19 1.431(8) . ?
C24 N16 1.459(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 O5 1.229(8) . ?
C25 N18 1.344(9) . ?
C25 N17 1.356(9) . ?
C26 N17 1.440(8) . ?
C26 N19 1.442(9) . ?
C26 C27 1.546(10) . ?
C26 H26 0.9800 . ?
C27 N18 1.449(9) . ?
C27 N20 1.457(9) . ?
C27 H27 0.9800 . ?
C28 O11 1.203(9) . ?
C28 N20 1.354(9) . ?
C28 N19 1.401(10) . ?
C29 N21 1.443(9) . ?
C29 N18 1.483(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N20 1.426(9) . ?
C30 N23 1.457(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 O6 1.214(7) . ?
C31 N21 1.343(9) . ?
C31 N22 1.382(9) . ?
C32 N23 1.447(8) . ?
C32 N21 1.452(8) . ?
C32 C33 1.544(11) . ?
C32 H32 0.9800 . ?
C33 N24 1.429(9) . ?
C33 N22 1.464(8) . ?
C33 H33 0.9800 . ?
C34 O12 1.222(9) . ?
C34 N24 1.364(10) . ?
C34 N23 1.368(9) . ?
C35 N22 1.438(9) . ?
C35 N1 1.474(8) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N24 1.468(9) . ?
C36 N3 1.472(9) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?

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
O17 N26 O16 120.3(10) . . ?
O17 N26 O18 118.9(10) . . ?
O16 N26 O18 120.3(10) . . ?
O15 N25 O14 124.0(5) . . ?
O15 N25 O13 120.6(5) . . ?
O14 N25 O13 115.3(6) . . ?
N25 O13 Sm1 101.3(4) . . ?
N25 O14 Sm1 93.8(3) . . ?
O1W Sm1 O5W 140.7(2) . . ?
O1W Sm1 O4W 70.28(14) . . ?
O5W Sm1 O4W 102.57(17) . . ?
O1W Sm1 O3W 83.56(14) . . ?
O5W Sm1 O3W 80.64(16) . . ?
O4W Sm1 O3W 142.31(19) . . ?
O1W Sm1 O2 135.41(18) . . ?
O5W Sm1 O2 73.20(17) . . ?
O4W Sm1 O2 143.20(17) . . ?
O3W Sm1 O2 74.14(16) . . ?
O1W Sm1 O1 132.89(15) . . ?
O5W Sm1 O1 73.63(15) . . ?
O4W Sm1 O1 70.89(15) . . ?
O3W Sm1 O1 142.77(14) . . ?
O2 Sm1 O1 72.95(15) . . ?
O1W Sm1 O2W 71.4(2) . . ?
O5W Sm1 O2W 69.78(18) . . ?
O4W Sm1 O2W 71.8(2) . . ?
O3W Sm1 O2W 74.4(2) . . ?
O2 Sm1 O2W 134.40(18) . . ?
O1 Sm1 O2W 119.11(19) . . ?
O1W Sm1 O13 73.2(2) . . ?
O5W Sm1 O13 144.42(17) . . ?
O4W Sm1 O13 76.1(2) . . ?
O3W Sm1 O13 122.38(17) . . ?
O2 Sm1 O13 86.78(17) . . ?
O1 Sm1 O13 72.48(15) . . ?
O2W Sm1 O13 138.36(14) . . ?
O1W Sm1 O14 69.28(19) . . ?
O5W Sm1 O14 137.31(16) . . ?
O4W Sm1 O14 118.78(17) . . ?
O3W Sm1 O14 73.31(16) . . ?
O2 Sm1 O14 67.52(15) . . ?
O1 Sm1 O14 108.85(15) . . ?
O2W Sm1 O14 131.08(19) . . ?
O13 Sm1 O14 49.29(15) . . ?
O1 C1 N1 125.0(6) . . ?
O1 C1 N2 124.8(6) . . ?
N1 C1 N2 110.1(5) . . ?
N3 C2 N1 112.6(6) . . ?
N3 C2 C37 110.9(6) . . ?
N1 C2 C37 110.9(6) . . ?
N3 C2 C3 102.8(5) . . ?
N1 C2 C3 102.9(5) . . ?
C37 C2 C3 116.3(6) . . ?
N4 C3 N2 111.8(5) . . ?
N4 C3 C38 111.8(6) . . ?
N2 C3 C38 112.6(6) . . ?
N4 C3 C2 101.5(5) . . ?
N2 C3 C2 102.5(5) . . ?
C38 C3 C2 115.9(6) . . ?
O7 C4 N3 126.9(7) . . ?
O7 C4 N4 126.0(7) . . ?
N3 C4 N4 107.1(6) . . ?
N5 C5 N2 115.5(5) . . ?
N5 C5 H5A 108.4 . . ?
N2 C5 H5A 108.4 . . ?
N5 C5 H5B 108.4 . . ?
N2 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
N4 C6 N7 114.8(6) . . ?
N4 C6 H6A 108.6 . . ?
N7 C6 H6A 108.6 . . ?
N4 C6 H6B 108.6 . . ?
N7 C6 H6B 108.6 . . ?
H6A C6 H6B 107.5 . . ?
O2 C7 N5 124.7(6) . . ?
O2 C7 N6 124.6(6) . . ?
N5 C7 N6 110.7(5) . . ?
N7 C8 N5 113.0(5) . . ?
N7 C8 C39 112.3(6) . . ?
N5 C8 C39 113.9(6) . . ?
N7 C8 C9 100.3(5) . . ?
N5 C8 C9 101.3(5) . . ?
C39 C8 C9 114.8(6) . . ?
N8 C9 N6 114.5(6) . . ?
N8 C9 C40 112.5(5) . . ?
N6 C9 C40 110.6(6) . . ?
N8 C9 C8 101.9(5) . . ?
N6 C9 C8 102.0(5) . . ?
C40 C9 C8 114.8(6) . . ?
O8 C10 N8 127.8(6) . . ?
O8 C10 N7 124.1(6) . . ?
N8 C10 N7 108.0(5) . . ?
N9 C11 N6 112.8(5) . . ?
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 114.2(5) . . ?
N11 C12 H12A 108.7 . . ?
N8 C12 H12A 108.7 . . ?
N11 C12 H12B 108.7 . . ?
N8 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N10 126.2(7) . . ?
O3 C13 N9 126.4(6) . . ?
N10 C13 N9 107.3(6) . . ?
N11 C14 N9 113.5(5) . . ?
N11 C14 C15 104.6(5) . . ?
N9 C14 C15 103.3(5) . . ?
N11 C14 H14 111.6 . . ?
N9 C14 H14 111.6 . . ?
C15 C14 H14 111.6 . . ?
N10 C15 N12 112.8(5) . . ?
N10 C15 C14 103.8(5) . . ?
N12 C15 C14 102.6(5) . . ?
N10 C15 H15 112.3 . . ?
N12 C15 H15 112.3 . . ?
C14 C15 H15 112.3 . . ?
O9 C16 N12 126.1(7) . . ?
O9 C16 N11 125.5(7) . . ?
N12 C16 N11 108.4(5) . . ?
N13 C17 N10 111.9(6) . . ?
N13 C17 H17A 109.2 . . ?
N10 C17 H17A 109.2 . . ?
N13 C17 H17B 109.2 . . ?
N10 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
N15 C18 N12 112.4(5) . . ?
N15 C18 H18A 109.1 . . ?
N12 C18 H18A 109.1 . . ?
N15 C18 H18B 109.1 . . ?
N12 C18 H18B 109.1 . . ?
H18A C18 H18B 107.9 . . ?
O4 C19 N14 128.1(6) . . ?
O4 C19 N13 125.5(6) . . ?
N14 C19 N13 106.4(5) . . ?
N13 C20 N15 114.0(6) . . ?
N13 C20 C21 101.2(5) . . ?
N15 C20 C21 102.8(5) . . ?
N13 C20 H20 112.6 . . ?
N15 C20 H20 112.6 . . ?
C21 C20 H20 112.6 . . ?
N14 C21 N16 116.9(5) . . ?
N14 C21 C20 103.3(5) . . ?
N16 C21 C20 102.4(5) . . ?
N14 C21 H21 111.1 . . ?
N16 C21 H21 111.1 . . ?
C20 C21 H21 111.1 . . ?
O10 C22 N16 126.4(6) . . ?
O10 C22 N15 123.7(7) . . ?
N16 C22 N15 109.9(6) . . ?
N17 C23 N14 114.5(6) . . ?
N17 C23 H23A 108.6 . . ?
N14 C23 H23A 108.6 . . ?
N17 C23 H23B 108.6 . . ?
N14 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
N19 C24 N16 114.0(6) . . ?
N19 C24 H24A 108.8 . . ?
N16 C24 H24A 108.8 . . ?
N19 C24 H24B 108.8 . . ?
N16 C24 H24B 108.8 . . ?
H24A C24 H24B 107.6 . . ?
O5 C25 N18 125.2(7) . . ?
O5 C25 N17 125.9(6) . . ?
N18 C25 N17 108.9(5) . . ?
N17 C26 N19 116.2(5) . . ?
N17 C26 C27 103.7(5) . . ?
N19 C26 C27 104.7(6) . . ?
N17 C26 H26 110.6 . . ?
N19 C26 H26 110.6 . . ?
C27 C26 H26 110.6 . . ?
N18 C27 N20 114.7(6) . . ?
N18 C27 C26 101.2(5) . . ?
N20 C27 C26 101.9(5) . . ?
N18 C27 H27 112.7 . . ?
N20 C27 H27 112.7 . . ?
C26 C27 H27 112.7 . . ?
O11 C28 N20 128.1(7) . . ?
O11 C28 N19 124.1(7) . . ?
N20 C28 N19 107.9(6) . . ?
N21 C29 N18 113.9(6) . . ?
N21 C29 H29A 108.8 . . ?
N18 C29 H29A 108.8 . . ?
N21 C29 H29B 108.8 . . ?
N18 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
N20 C30 N23 113.5(5) . . ?
N20 C30 H30A 108.9 . . ?
N23 C30 H30A 108.9 . . ?
N20 C30 H30B 108.9 . . ?
N23 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
O6 C31 N21 126.3(6) . . ?
O6 C31 N22 124.6(6) . . ?
N21 C31 N22 109.1(5) . . ?
N23 C32 N21 114.3(5) . . ?
N23 C32 C33 103.4(6) . . ?
N21 C32 C33 103.4(5) . . ?
N23 C32 H32 111.7 . . ?
N21 C32 H32 111.7 . . ?
C33 C32 H32 111.7 . . ?
N24 C33 N22 114.0(6) . . ?
N24 C33 C32 102.8(6) . . ?
N22 C33 C32 103.3(5) . . ?
N24 C33 H33 112.0 . . ?
N22 C33 H33 112.0 . . ?
C32 C33 H33 112.0 . . ?
O12 C34 N24 126.5(8) . . ?
O12 C34 N23 126.3(7) . . ?
N24 C34 N23 107.2(6) . . ?
N22 C35 N1 113.7(5) . . ?
N22 C35 H35A 108.8 . . ?
N1 C35 H35A 108.8 . . ?
N22 C35 H35B 108.8 . . ?
N1 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
N24 C36 N3 114.3(6) . . ?
N24 C36 H36A 108.7 . . ?
N3 C36 H36A 108.7 . . ?
N24 C36 H36B 108.7 . . ?
N3 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C2 C37 H37A 109.5 . . ?
C2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C38 H38A 109.5 . . ?
C3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C8 C39 H39A 109.5 . . ?
C8 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C8 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C9 C40 H40A 109.5 . . ?
C9 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C9 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C1 N1 C35 121.2(5) . . ?
C1 N1 C2 111.6(5) . . ?
C35 N1 C2 126.0(5) . . ?
C1 N2 C5 122.0(5) . . ?
C1 N2 C3 112.3(5) . . ?
C5 N2 C3 125.6(5) . . ?
C4 N3 C2 114.3(5) . . ?
C4 N3 C36 120.8(6) . . ?
C2 N3 C36 124.8(6) . . ?
C4 N4 C6 119.8(6) . . ?
C4 N4 C3 113.4(5) . . ?
C6 N4 C3 124.3(6) . . ?
C7 N5 C5 120.6(5) . . ?
C7 N5 C8 112.7(5) . . ?
C5 N5 C8 126.2(5) . . ?
C7 N6 C11 121.1(5) . . ?
C7 N6 C9 111.4(5) . . ?
C11 N6 C9 124.5(5) . . ?
C10 N7 C8 112.3(5) . . ?
C10 N7 C6 120.9(6) . . ?
C8 N7 C6 124.7(6) . . ?
C10 N8 C9 114.9(5) . . ?
C10 N8 C12 119.3(5) . . ?
C9 N8 C12 125.1(5) . . ?
C13 N9 C11 122.9(5) . . ?
C13 N9 C14 111.5(5) . . ?
C11 N9 C14 121.7(6) . . ?
C13 N10 C15 113.3(6) . . ?
C13 N10 C17 122.3(6) . . ?
C15 N10 C17 121.2(6) . . ?
C16 N11 C12 121.7(6) . . ?
C16 N11 C14 111.2(6) . . ?
C12 N11 C14 124.3(6) . . ?
C16 N12 C15 112.3(5) . . ?
C16 N12 C18 123.1(5) . . ?
C15 N12 C18 122.9(5) . . ?
C19 N13 C20 113.1(5) . . ?
C19 N13 C17 121.1(5) . . ?
C20 N13 C17 124.7(5) . . ?
C19 N14 C21 114.7(5) . . ?
C19 N14 C23 122.0(5) . . ?
C21 N14 C23 123.2(5) . . ?
C22 N15 C18 124.3(6) . . ?
C22 N15 C20 111.8(5) . . ?
C18 N15 C20 123.5(5) . . ?
C22 N16 C21 113.0(5) . . ?
C22 N16 C24 122.7(6) . . ?
C21 N16 C24 122.4(5) . . ?
C25 N17 C26 111.3(5) . . ?
C25 N17 C23 123.7(5) . . ?
C26 N17 C23 125.0(6) . . ?
C25 N18 C27 112.8(6) . . ?
C25 N18 C29 122.3(6) . . ?
C27 N18 C29 121.9(5) . . ?
C28 N19 C24 123.2(6) . . ?
C28 N19 C26 110.8(5) . . ?
C24 N19 C26 123.7(6) . . ?
C28 N20 C30 123.0(6) . . ?
C28 N20 C27 113.6(6) . . ?
C30 N20 C27 123.4(5) . . ?
C31 N21 C29 122.6(5) . . ?
C31 N21 C32 112.7(6) . . ?
C29 N21 C32 122.7(6) . . ?
C31 N22 C35 123.2(5) . . ?
C31 N22 C33 111.1(6) . . ?
C35 N22 C33 124.2(6) . . ?
C34 N23 C32 112.2(6) . . ?
C34 N23 C30 123.0(6) . . ?
C32 N23 C30 123.9(6) . . ?
C34 N24 C33 113.3(6) . . ?
C34 N24 C36 121.8(7) . . ?
C33 N24 C36 121.4(7) . . ?
C1 O1 Sm1 155.5(4) . . ?
C7 O2 Sm1 166.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.102

# 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 0.067 0.484 0.377 28 7 ' '
2 0.118 0.521 0.876 16 8 ' '
3 0.225 0.061 0.848 104 27 ' '
4 0.275 0.061 0.348 104 27 ' '
5 0.215 0.219 0.572 20 10 ' '
6 0.218 0.389 0.557 14 9 ' '
7 0.284 0.219 0.072 20 10 ' '
8 0.282 0.389 0.057 14 9 ' '
9 0.433 0.484 0.877 28 7 ' '
10 0.381 0.521 0.376 16 8 ' '
11 0.567 0.984 0.123 28 7 ' '
12 0.619 0.021 0.624 16 8 ' '
13 0.725 0.561 0.652 104 27 ' '
14 0.775 0.561 0.152 104 27 ' '
15 0.715 0.719 0.928 20 10 ' '
16 0.718 0.889 0.943 14 9 ' '
17 0.785 0.719 0.428 20 10 ' '
18 0.782 0.889 0.443 14 9 ' '
19 0.933 -0.016 0.623 28 7 ' '
20 0.881 0.021 0.124 16 8 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997811'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_07Eu
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H54 N25 Eu O20, N O3, Cl, 6(H2 O)'
_chemical_formula_sum            'C40 H66 Cl Eu N26 O29'
_chemical_formula_weight         1562.60

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           orthorhombic
_symmetry_space_group_name_H-M   'P c 21 n'
_symmetry_space_group_name_Hall  'P -2n -2ac'

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

_cell_length_a                   14.641(3)
_cell_length_b                   17.416(4)
_cell_length_c                   23.351(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5954(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          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3200
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_T_max  0.7516
_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            39356
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.10
_reflns_number_total             10497
_reflns_number_gt                8393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0943P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.551(13)
_refine_ls_number_reflns         10497
_refine_ls_number_parameters     831
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1515
_refine_ls_wR_factor_gt          0.1421
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.003
_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 0.7218(4) 0.8890(11) -0.2579(6) 0.301(10) Uani 0.809(13) 1 d P A 1
Cl1' Cl 0.7269(9) 0.8414(11) -0.2083(6) 0.068(7) Uani 0.191(13) 1 d P A 2
N26 N -0.2774(5) 0.9023(4) -0.0019(3) 0.068(3) Uani 1 1 d D . .
O16 O -0.3245(9) 0.8485(7) 0.0176(5) 0.174(6) Uani 1 1 d D . .
O17 O -0.2007(5) 0.9190(5) 0.0179(4) 0.086(3) Uani 1 1 d D . .
O18 O -0.3020(7) 0.9442(8) -0.0425(5) 0.178(7) Uani 1 1 d D . .
O1W O 0.2325(3) 0.8034(5) 0.1848(2) 0.0435(13) Uani 1 1 d . . .
O2W O 0.0687(3) 0.8007(5) 0.12406(19) 0.0438(12) Uani 1 1 d . . .
O3W O 0.1891(6) 0.9293(4) 0.1119(3) 0.0505(18) Uani 1 1 d . . .
O4W O 0.3678(4) 0.8597(4) 0.0857(2) 0.0411(14) Uani 1 1 d . . .
O5W O 0.2049(4) 0.8796(4) -0.0005(3) 0.0463(15) Uani 1 1 d . . .
N25 N 0.2762(4) 0.6466(4) 0.1343(3) 0.0401(18) Uani 1 1 d . . .
O13 O 0.1968(4) 0.6654(4) 0.1193(3) 0.0433(17) Uani 1 1 d . . .
O14 O 0.3389(4) 0.6937(4) 0.1215(3) 0.0453(14) Uani 1 1 d . . .
O15 O 0.2915(4) 0.5869(4) 0.1606(3) 0.0524(17) Uani 1 1 d . . .
Eu1 Eu 0.220354(19) 0.79717(7) 0.082254(12) 0.02884(12) Uani 1 1 d . . .
C1 C 0.0871(5) 0.7021(4) -0.0277(3) 0.0261(16) Uani 1 1 d . . .
C2 C -0.0038(5) 0.6682(5) -0.1065(3) 0.0347(18) Uani 1 1 d . . .
C3 C 0.0848(6) 0.6180(5) -0.1065(3) 0.040(2) Uani 1 1 d . . .
C4 C 0.0780(6) 0.6931(5) -0.1922(4) 0.040(2) Uani 1 1 d . . .
C5 C 0.2146(4) 0.6090(5) -0.0307(3) 0.0304(17) Uani 1 1 d . . .
H5A H 0.2161 0.6184 0.0107 0.036 Uiso 1 1 calc R . .
H5B H 0.2121 0.5534 -0.0365 0.036 Uiso 1 1 calc R . .
C6 C 0.2130(5) 0.6091(5) -0.1824(4) 0.039(2) Uani 1 1 d . . .
H6A H 0.2094 0.5537 -0.1755 0.047 Uiso 1 1 calc R . .
H6B H 0.2128 0.6169 -0.2239 0.047 Uiso 1 1 calc R . .
C7 C 0.3391(5) 0.7023(5) -0.0346(3) 0.0310(17) Uani 1 1 d . . .
C8 C 0.3421(5) 0.6086(5) -0.1075(3) 0.0357(18) Uani 1 1 d . . .
C9 C 0.4345(5) 0.6569(5) -0.1080(3) 0.0372(19) Uani 1 1 d . . .
C10 C 0.3591(5) 0.6767(5) -0.1939(3) 0.0330(18) Uani 1 1 d . . .
C11 C 0.4843(5) 0.7713(5) -0.0422(3) 0.036(2) Uani 1 1 d . . .
H11A H 0.4669 0.7864 -0.0033 0.043 Uiso 1 1 calc R . .
H11B H 0.5435 0.7453 -0.0399 0.043 Uiso 1 1 calc R . .
C12 C 0.5131(6) 0.7284(5) -0.1918(4) 0.037(2) Uani 1 1 d . . .
H12A H 0.5712 0.7059 -0.1794 0.044 Uiso 1 1 calc R . .
H12B H 0.5093 0.7228 -0.2335 0.044 Uiso 1 1 calc R . .
C13 C 0.4780(5) 0.9129(5) -0.0554(3) 0.0311(17) Uani 1 1 d . . .
C14 C 0.5539(5) 0.8405(5) -0.1263(3) 0.0357(19) Uani 1 1 d . . .
H14 H 0.6141 0.8173 -0.1180 0.043 Uiso 1 1 calc R . .
C15 C 0.5623(5) 0.9261(5) -0.1400(3) 0.0304(17) Uani 1 1 d . . .
H15 H 0.6268 0.9431 -0.1406 0.036 Uiso 1 1 calc R . .
C16 C 0.4981(6) 0.8628(6) -0.2198(3) 0.038(2) Uani 1 1 d . . .
C17 C 0.5193(6) 1.0458(6) -0.0820(3) 0.040(2) Uani 1 1 d . . .
H17A H 0.5798 1.0637 -0.0940 0.048 Uiso 1 1 calc R . .
H17B H 0.5136 1.0542 -0.0406 0.048 Uiso 1 1 calc R . .
C18 C 0.5186(5) 1.0042(5) -0.2295(3) 0.0364(19) Uani 1 1 d . . .
H18A H 0.5770 1.0309 -0.2248 0.044 Uiso 1 1 calc R . .
H18B H 0.5121 0.9909 -0.2701 0.044 Uiso 1 1 calc R . .
C19 C 0.3774(6) 1.1225(5) -0.0825(3) 0.0355(19) Uani 1 1 d . . .
C20 C 0.4548(5) 1.1152(5) -0.1720(3) 0.0370(19) Uani 1 1 d . . .
H20 H 0.5085 1.1485 -0.1788 0.044 Uiso 1 1 calc R . .
C21 C 0.3623(5) 1.1598(5) -0.1784(3) 0.0381(19) Uani 1 1 d . . .
H21 H 0.3731 1.2126 -0.1925 0.046 Uiso 1 1 calc R . .
C22 C 0.3647(6) 1.0574(6) -0.2415(3) 0.048(2) Uani 1 1 d . . .
C23 C 0.2444(6) 1.2037(5) -0.1066(4) 0.044(2) Uani 1 1 d . . .
H23A H 0.2469 1.2160 -0.0657 0.053 Uiso 1 1 calc R . .
H23B H 0.2438 1.2522 -0.1279 0.053 Uiso 1 1 calc R . .
C24 C 0.2302(5) 1.1414(4) -0.2482(4) 0.0290(17) Uani 1 1 d . . .
H24A H 0.2330 1.1974 -0.2525 0.035 Uiso 1 1 calc R . .
H24B H 0.2272 1.1191 -0.2867 0.035 Uiso 1 1 calc R . .
C25 C 0.1170(6) 1.1179(5) -0.0796(3) 0.036(2) Uani 1 1 d . . .
C26 C 0.1110(5) 1.1671(5) -0.1715(3) 0.0346(18) Uani 1 1 d . . .
H26 H 0.1020 1.2212 -0.1833 0.042 Uiso 1 1 calc R . .
C27 C 0.0183(5) 1.1275(5) -0.1586(3) 0.0400(19) Uani 1 1 d . . .
H27 H -0.0326 1.1648 -0.1561 0.048 Uiso 1 1 calc R . .
C28 C 0.0840(6) 1.0707(6) -0.2393(3) 0.044(2) Uani 1 1 d . . .
C29 C -0.0340(6) 1.0540(5) -0.0686(3) 0.0382(19) Uani 1 1 d . . .
H29A H -0.0174 1.0572 -0.0280 0.046 Uiso 1 1 calc R . .
H29B H -0.0917 1.0818 -0.0738 0.046 Uiso 1 1 calc R . .
C30 C -0.0715(5) 1.0307(5) -0.2163(3) 0.041(2) Uani 1 1 d . . .
H30A H -0.0750 1.0198 -0.2574 0.049 Uiso 1 1 calc R . .
H30B H -0.1255 1.0610 -0.2060 0.049 Uiso 1 1 calc R . .
C31 C -0.0206(5) 0.9159(5) -0.0483(3) 0.0335(18) Uani 1 1 d . . .
C32 C -0.1096(5) 0.9493(6) -0.1276(3) 0.042(2) Uani 1 1 d . . .
H32 H -0.1709 0.9726 -0.1232 0.051 Uiso 1 1 calc R . .
C33 C -0.1113(6) 0.8605(6) -0.1189(3) 0.046(2) Uani 1 1 d . . .
H33 H -0.1742 0.8410 -0.1136 0.055 Uiso 1 1 calc R . .
C34 C -0.0578(6) 0.8898(6) -0.2120(4) 0.045(2) Uani 1 1 d . . .
C35 C -0.0535(5) 0.7785(4) -0.0359(3) 0.033(2) Uani 1 1 d . . .
H35A H -0.1147 0.7557 -0.0361 0.040 Uiso 1 1 calc R . .
H35B H -0.0381 0.7909 0.0039 0.040 Uiso 1 1 calc R . .
C36 C -0.0730(6) 0.7524(6) -0.1876(4) 0.048(3) Uani 1 1 d . . .
H36A H -0.0691 0.7481 -0.2293 0.058 Uiso 1 1 calc R . .
H36B H -0.1317 0.7304 -0.1757 0.058 Uiso 1 1 calc R . .
C37 C -0.0934(7) 0.6261(7) -0.1003(5) 0.059(3) Uani 1 1 d . . .
H37A H -0.0955 0.6009 -0.0633 0.088 Uiso 1 1 calc R . .
H37B H -0.0987 0.5880 -0.1304 0.088 Uiso 1 1 calc R . .
H37C H -0.1434 0.6624 -0.1032 0.088 Uiso 1 1 calc R . .
C38 C 0.0714(7) 0.5327(6) -0.1081(4) 0.048(2) Uani 1 1 d . . .
H38A H 0.0416 0.5161 -0.0731 0.072 Uiso 1 1 calc R . .
H38B H 0.1303 0.5075 -0.1114 0.072 Uiso 1 1 calc R . .
H38C H 0.0337 0.5192 -0.1407 0.072 Uiso 1 1 calc R . .
C39 C 0.3531(7) 0.5233(5) -0.1080(4) 0.050(2) Uani 1 1 d . . .
H39A H 0.3832 0.5077 -0.1432 0.076 Uiso 1 1 calc R . .
H39B H 0.2935 0.4992 -0.1058 0.076 Uiso 1 1 calc R . .
H39C H 0.3898 0.5076 -0.0755 0.076 Uiso 1 1 calc R . .
C40 C 0.5231(8) 0.6105(8) -0.0915(4) 0.055(3) Uani 1 1 d . . .
H40A H 0.5178 0.5922 -0.0524 0.082 Uiso 1 1 calc R . .
H40B H 0.5761 0.6437 -0.0947 0.082 Uiso 1 1 calc R . .
H40C H 0.5300 0.5671 -0.1171 0.082 Uiso 1 1 calc R . .
N1 N 0.0125(5) 0.7210(4) -0.0576(3) 0.0343(15) Uani 1 1 d . . .
N2 N 0.1327(4) 0.6428(4) -0.0538(2) 0.0333(15) Uani 1 1 d . . .
N3 N 0.0011(4) 0.7066(4) -0.1620(3) 0.0370(16) Uani 1 1 d . . .
N4 N 0.1308(4) 0.6450(4) -0.1586(3) 0.0353(15) Uani 1 1 d . . .
N5 N 0.2977(4) 0.6379(4) -0.0556(3) 0.0321(15) Uani 1 1 d . . .
N6 N 0.4174(4) 0.7172(4) -0.0636(3) 0.0315(14) Uani 1 1 d . . .
N7 N 0.2987(4) 0.6367(4) -0.1600(3) 0.0365(16) Uani 1 1 d . . .
N8 N 0.4373(4) 0.6847(4) -0.1653(3) 0.0361(16) Uani 1 1 d . . .
N9 N 0.4946(5) 0.8390(4) -0.0761(3) 0.0350(16) Uani 1 1 d . . .
N10 N 0.5103(5) 0.9639(5) -0.0945(3) 0.0345(19) Uani 1 1 d . . .
N11 N 0.5133(4) 0.8080(5) -0.1780(2) 0.0402(18) Uani 1 1 d . . .
N12 N 0.5205(4) 0.9325(4) -0.1953(2) 0.0347(15) Uani 1 1 d . . .
N13 N 0.4484(5) 1.0893(4) -0.1122(3) 0.0430(18) Uani 1 1 d . . .
N14 N 0.3262(4) 1.1611(4) -0.1220(3) 0.0364(15) Uani 1 1 d . . .
N15 N 0.4473(4) 1.0544(4) -0.2139(3) 0.0387(16) Uani 1 1 d . . .
N16 N 0.3139(5) 1.1151(4) -0.2202(3) 0.0406(16) Uani 1 1 d . . .
N17 N 0.1597(4) 1.1625(4) -0.1183(3) 0.0384(16) Uani 1 1 d . . .
N18 N 0.0384(5) 1.0920(5) -0.1034(3) 0.0421(18) Uani 1 1 d . . .
N19 N 0.1481(4) 1.1218(4) -0.2178(3) 0.0418(17) Uani 1 1 d . . .
N20 N 0.0077(4) 1.0754(4) -0.2057(3) 0.0389(16) Uani 1 1 d . . .
N21 N -0.0478(5) 0.9737(4) -0.0838(3) 0.0336(16) Uani 1 1 d . . .
N22 N -0.0558(5) 0.8486(4) -0.0685(3) 0.0401(17) Uani 1 1 d . . .
N23 N -0.0748(4) 0.9571(4) -0.1847(3) 0.0392(16) Uani 1 1 d . . .
N24 N -0.0715(6) 0.8336(5) -0.1719(3) 0.0417(19) Uani 1 1 d . . .
O1 O 0.1122(3) 0.7335(3) 0.0172(2) 0.0352(12) Uani 1 1 d . . .
O2 O 0.3101(4) 0.7401(4) 0.0064(2) 0.0415(14) Uani 1 1 d . . .
O3 O 0.4385(4) 0.9284(3) -0.0120(2) 0.0448(14) Uani 1 1 d . . .
O4 O 0.3678(4) 1.1200(4) -0.0322(2) 0.0445(14) Uani 1 1 d . . .
O5 O 0.1416(4) 1.1037(4) -0.0304(2) 0.0549(17) Uani 1 1 d . . .
O6 O 0.0253(4) 0.9235(3) -0.0051(2) 0.0409(13) Uani 1 1 d . . .
O7 O 0.0980(4) 0.7148(4) -0.2381(2) 0.0495(15) Uani 1 1 d . . .
O8 O 0.3433(4) 0.6978(3) -0.2426(2) 0.0417(14) Uani 1 1 d . . .
O9 O 0.4734(4) 0.8511(4) -0.2670(2) 0.0536(17) Uani 1 1 d . . .
O10 O 0.3429(4) 1.0132(4) -0.2811(2) 0.0464(15) Uani 1 1 d . . .
O11 O 0.0930(4) 1.0321(4) -0.2814(2) 0.0517(17) Uani 1 1 d . . .
O12 O -0.0342(5) 0.8805(4) -0.2606(3) 0.065(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N26 O17 1.249(2) . ?
N26 O18 1.249(2) . ?
N26 O16 1.250(2) . ?
O1W Eu1 2.403(5) . ?
O2W Eu1 2.426(4) . ?
O3W Eu1 2.446(7) . ?
O4W Eu1 2.420(6) . ?
O5W Eu1 2.418(6) . ?
N25 O15 1.227(9) . ?
N25 O13 1.258(9) . ?
N25 O14 1.266(9) . ?
N25 Eu1 3.004(7) . ?
O13 Eu1 2.477(7) . ?
O14 Eu1 2.665(6) . ?
Eu1 O2 2.419(5) . ?
Eu1 O1 2.458(5) . ?
C1 O1 1.240(8) . ?
C1 N1 1.336(10) . ?
C1 N2 1.372(10) . ?
C2 N3 1.459(10) . ?
C2 N1 1.486(10) . ?
C2 C37 1.510(12) . ?
C2 C3 1.565(12) . ?
C3 N4 1.469(10) . ?
C3 N2 1.481(9) . ?
C3 C38 1.498(13) . ?
C4 O7 1.172(10) . ?
C4 N3 1.350(11) . ?
C4 N4 1.383(11) . ?
C5 N5 1.440(9) . ?
C5 N2 1.441(9) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.442(10) . ?
C6 N4 1.465(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.238(9) . ?
C7 N6 1.356(9) . ?
C7 N5 1.365(10) . ?
C8 N7 1.463(10) . ?
C8 N5 1.468(10) . ?
C8 C39 1.495(12) . ?
C8 C9 1.593(12) . ?
C9 N8 1.422(10) . ?
C9 N6 1.497(10) . ?
C9 C40 1.577(13) . ?
C10 O8 1.216(9) . ?
C10 N8 1.333(10) . ?
C10 N7 1.377(10) . ?
C11 N9 1.428(10) . ?
C11 N6 1.447(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.423(13) . ?
C12 N8 1.482(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.198(9) . ?
C13 N10 1.358(11) . ?
C13 N9 1.397(11) . ?
C14 N9 1.458(9) . ?
C14 N11 1.461(10) . ?
C14 C15 1.530(11) . ?
C14 H14 0.9900 . ?
C15 N12 1.435(9) . ?
C15 N10 1.465(10) . ?
C15 H15 0.9900 . ?
C16 O9 1.178(9) . ?
C16 N12 1.379(11) . ?
C16 N11 1.383(12) . ?
C17 N10 1.462(12) . ?
C17 N13 1.467(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N15 1.410(10) . ?
C18 N12 1.482(10) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 O4 1.185(9) . ?
C19 N14 1.367(10) . ?
C19 N13 1.376(11) . ?
C20 N15 1.446(10) . ?
C20 N13 1.472(9) . ?
C20 C21 1.567(11) . ?
C20 H20 0.9900 . ?
C21 N14 1.418(10) . ?
C21 N16 1.438(11) . ?
C21 H21 0.9900 . ?
C22 O10 1.244(11) . ?
C22 N16 1.345(12) . ?
C22 N15 1.372(11) . ?
C23 N17 1.458(11) . ?
C23 N14 1.453(11) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C24 N19 1.436(10) . ?
C24 N16 1.463(10) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 O5 1.229(9) . ?
C25 N18 1.356(11) . ?
C25 N17 1.346(11) . ?
C26 N17 1.434(9) . ?
C26 N19 1.445(10) . ?
C26 C27 1.551(11) . ?
C26 H26 0.9900 . ?
C27 N20 1.434(11) . ?
C27 N18 1.460(10) . ?
C27 H27 0.9900 . ?
C28 O11 1.198(10) . ?
C28 N20 1.368(11) . ?
C28 N19 1.388(12) . ?
C29 N21 1.457(11) . ?
C29 N18 1.491(11) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 N20 1.419(10) . ?
C30 N23 1.478(10) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 O6 1.219(9) . ?
C31 N21 1.364(11) . ?
C31 N22 1.365(11) . ?
C32 N21 1.429(10) . ?
C32 N23 1.435(10) . ?
C32 C33 1.560(14) . ?
C32 H32 0.9900 . ?
C33 N22 1.446(10) . ?
C33 N24 1.446(11) . ?
C33 H33 0.9900 . ?
C34 O12 1.197(10) . ?
C34 N23 1.357(11) . ?
C34 N24 1.370(11) . ?
C35 N22 1.438(10) . ?
C35 N1 1.482(9) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C36 N24 1.460(11) . ?
C36 N3 1.473(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?

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
O17 N26 O18 113.8(8) . . ?
O17 N26 O16 122.4(9) . . ?
O18 N26 O16 123.8(10) . . ?
O15 N25 O13 121.9(7) . . ?
O15 N25 O14 122.3(7) . . ?
O13 N25 O14 115.8(7) . . ?
O15 N25 Eu1 172.3(5) . . ?
O13 N25 Eu1 53.7(4) . . ?
O14 N25 Eu1 62.4(4) . . ?
N25 O13 Eu1 102.1(5) . . ?
N25 O14 Eu1 92.7(4) . . ?
O1W Eu1 O5W 140.9(3) . . ?
O1W Eu1 O2 135.0(2) . . ?
O5W Eu1 O2 73.2(2) . . ?
O1W Eu1 O4W 83.17(17) . . ?
O5W Eu1 O4W 80.94(19) . . ?
O2 Eu1 O4W 74.00(19) . . ?
O1W Eu1 O2W 70.46(16) . . ?
O5W Eu1 O2W 102.7(2) . . ?
O2 Eu1 O2W 143.4(2) . . ?
O4W Eu1 O2W 142.3(2) . . ?
O1W Eu1 O3W 71.9(3) . . ?
O5W Eu1 O3W 69.5(2) . . ?
O2 Eu1 O3W 134.1(2) . . ?
O4W Eu1 O3W 74.6(2) . . ?
O2W Eu1 O3W 72.0(3) . . ?
O1W Eu1 O1 133.09(19) . . ?
O5W Eu1 O1 73.37(19) . . ?
O2 Eu1 O1 73.31(18) . . ?
O4W Eu1 O1 142.97(16) . . ?
O2W Eu1 O1 70.75(18) . . ?
O3W Eu1 O1 118.6(2) . . ?
O1W Eu1 O13 72.8(3) . . ?
O5W Eu1 O13 144.7(2) . . ?
O2 Eu1 O13 87.1(2) . . ?
O4W Eu1 O13 122.0(2) . . ?
O2W Eu1 O13 75.9(2) . . ?
O3W Eu1 O13 138.32(17) . . ?
O1 Eu1 O13 73.01(19) . . ?
O1W Eu1 O14 68.9(2) . . ?
O5W Eu1 O14 137.54(19) . . ?
O2 Eu1 O14 67.66(18) . . ?
O4W Eu1 O14 73.28(19) . . ?
O2W Eu1 O14 118.3(2) . . ?
O3W Eu1 O14 131.3(2) . . ?
O1 Eu1 O14 109.10(18) . . ?
O13 Eu1 O14 48.99(19) . . ?
O1W Eu1 N25 67.4(3) . . ?
O5W Eu1 N25 150.1(2) . . ?
O2 Eu1 N25 77.8(2) . . ?
O4W Eu1 N25 97.9(2) . . ?
O2W Eu1 N25 96.2(2) . . ?
O3W Eu1 N25 139.2(2) . . ?
O1 Eu1 N25 91.81(19) . . ?
O13 Eu1 N25 24.17(19) . . ?
O14 Eu1 N25 24.90(16) . . ?
O1 C1 N1 125.1(7) . . ?
O1 C1 N2 124.3(7) . . ?
N1 C1 N2 110.6(6) . . ?
N3 C2 N1 113.0(7) . . ?
N3 C2 C37 110.5(7) . . ?
N1 C2 C37 111.5(7) . . ?
N3 C2 C3 102.5(6) . . ?
N1 C2 C3 102.3(6) . . ?
C37 C2 C3 116.6(8) . . ?
N4 C3 N2 112.2(6) . . ?
N4 C3 C38 111.0(7) . . ?
N2 C3 C38 111.8(7) . . ?
N4 C3 C2 101.5(6) . . ?
N2 C3 C2 103.2(6) . . ?
C38 C3 C2 116.5(7) . . ?
O7 C4 N3 129.0(9) . . ?
O7 C4 N4 125.1(8) . . ?
N3 C4 N4 105.9(7) . . ?
N5 C5 N2 114.1(6) . . ?
N5 C5 H5A 108.7 . . ?
N2 C5 H5A 108.7 . . ?
N5 C5 H5B 108.7 . . ?
N2 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N7 C6 N4 115.8(7) . . ?
N7 C6 H6A 108.3 . . ?
N4 C6 H6A 108.3 . . ?
N7 C6 H6B 108.3 . . ?
N4 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
O2 C7 N6 125.0(7) . . ?
O2 C7 N5 124.2(7) . . ?
N6 C7 N5 110.8(6) . . ?
N7 C8 N5 112.5(6) . . ?
N7 C8 C39 111.8(7) . . ?
N5 C8 C39 113.6(7) . . ?
N7 C8 C9 100.7(6) . . ?
N5 C8 C9 101.5(6) . . ?
C39 C8 C9 115.7(7) . . ?
N8 C9 N6 114.7(7) . . ?
N8 C9 C40 112.4(7) . . ?
N6 C9 C40 109.1(7) . . ?
N8 C9 C8 102.2(6) . . ?
N6 C9 C8 102.9(6) . . ?
C40 C9 C8 115.2(8) . . ?
O8 C10 N8 127.0(8) . . ?
O8 C10 N7 124.6(7) . . ?
N8 C10 N7 108.3(6) . . ?
N9 C11 N6 114.7(6) . . ?
N9 C11 H11A 108.6 . . ?
N6 C11 H11A 108.6 . . ?
N9 C11 H11B 108.6 . . ?
N6 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N11 C12 N8 114.0(6) . . ?
N11 C12 H12A 108.7 . . ?
N8 C12 H12A 108.7 . . ?
N11 C12 H12B 108.7 . . ?
N8 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
O3 C13 N10 126.1(8) . . ?
O3 C13 N9 125.8(7) . . ?
N10 C13 N9 108.0(7) . . ?
N9 C14 N11 114.6(6) . . ?
N9 C14 C15 103.5(6) . . ?
N11 C14 C15 103.7(6) . . ?
N9 C14 H14 111.5 . . ?
N11 C14 H14 111.5 . . ?
C15 C14 H14 111.5 . . ?
N12 C15 N10 113.4(6) . . ?
N12 C15 C14 103.3(6) . . ?
N10 C15 C14 104.1(6) . . ?
N12 C15 H15 111.8 . . ?
N10 C15 H15 111.8 . . ?
C14 C15 H15 111.8 . . ?
O9 C16 N12 127.8(8) . . ?
O9 C16 N11 126.1(9) . . ?
N12 C16 N11 106.1(6) . . ?
N10 C17 N13 110.1(7) . . ?
N10 C17 H17A 109.6 . . ?
N13 C17 H17A 109.6 . . ?
N10 C17 H17B 109.6 . . ?
N13 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
N15 C18 N12 113.4(6) . . ?
N15 C18 H18A 108.9 . . ?
N12 C18 H18A 108.9 . . ?
N15 C18 H18B 108.9 . . ?
N12 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
O4 C19 N14 128.6(8) . . ?
O4 C19 N13 125.0(8) . . ?
N14 C19 N13 106.3(6) . . ?
N15 C20 N13 114.3(7) . . ?
N15 C20 C21 103.6(6) . . ?
N13 C20 C21 100.8(6) . . ?
N15 C20 H20 112.4 . . ?
N13 C20 H20 112.4 . . ?
C21 C20 H20 112.4 . . ?
N14 C21 N16 117.1(7) . . ?
N14 C21 C20 104.1(6) . . ?
N16 C21 C20 102.8(7) . . ?
N14 C21 H21 110.8 . . ?
N16 C21 H21 110.8 . . ?
C20 C21 H21 110.8 . . ?
O10 C22 N16 126.5(8) . . ?
O10 C22 N15 123.5(9) . . ?
N16 C22 N15 109.9(8) . . ?
N17 C23 N14 113.8(7) . . ?
N17 C23 H23A 108.8 . . ?
N14 C23 H23A 108.8 . . ?
N17 C23 H23B 108.8 . . ?
N14 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N19 C24 N16 113.9(7) . . ?
N19 C24 H24A 108.8 . . ?
N16 C24 H24A 108.8 . . ?
N19 C24 H24B 108.8 . . ?
N16 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
O5 C25 N18 124.3(8) . . ?
O5 C25 N17 127.5(8) . . ?
N18 C25 N17 108.1(7) . . ?
N17 C26 N19 115.4(6) . . ?
N17 C26 C27 104.0(6) . . ?
N19 C26 C27 103.4(7) . . ?
N17 C26 H26 111.2 . . ?
N19 C26 H26 111.2 . . ?
C27 C26 H26 111.2 . . ?
N20 C27 N18 115.5(7) . . ?
N20 C27 C26 103.1(6) . . ?
N18 C27 C26 100.6(6) . . ?
N20 C27 H27 112.2 . . ?
N18 C27 H27 112.2 . . ?
C26 C27 H27 112.2 . . ?
O11 C28 N20 126.5(9) . . ?
O11 C28 N19 125.6(8) . . ?
N20 C28 N19 107.8(7) . . ?
N21 C29 N18 113.1(7) . . ?
N21 C29 H29A 109.0 . . ?
N18 C29 H29A 109.0 . . ?
N21 C29 H29B 109.0 . . ?
N18 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
N20 C30 N23 114.6(6) . . ?
N20 C30 H30A 108.6 . . ?
N23 C30 H30A 108.6 . . ?
N20 C30 H30B 108.6 . . ?
N23 C30 H30B 108.6 . . ?
H30A C30 H30B 107.6 . . ?
O6 C31 N21 125.8(8) . . ?
O6 C31 N22 126.0(8) . . ?
N21 C31 N22 108.2(7) . . ?
N21 C32 N23 114.3(7) . . ?
N21 C32 C33 102.3(6) . . ?
N23 C32 C33 102.7(7) . . ?
N21 C32 H32 112.2 . . ?
N23 C32 H32 112.2 . . ?
C33 C32 H32 112.2 . . ?
N22 C33 N24 115.1(7) . . ?
N22 C33 C32 103.8(7) . . ?
N24 C33 C32 101.8(7) . . ?
N22 C33 H33 111.8 . . ?
N24 C33 H33 111.8 . . ?
C32 C33 H33 111.8 . . ?
O12 C34 N23 128.0(9) . . ?
O12 C34 N24 126.3(9) . . ?
N23 C34 N24 105.7(8) . . ?
N22 C35 N1 114.1(6) . . ?
N22 C35 H35A 108.7 . . ?
N1 C35 H35A 108.7 . . ?
N22 C35 H35B 108.7 . . ?
N1 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
N24 C36 N3 114.3(8) . . ?
N24 C36 H36A 108.7 . . ?
N3 C36 H36A 108.7 . . ?
N24 C36 H36B 108.7 . . ?
N3 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
C2 C37 H37A 109.5 . . ?
C2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C38 H38A 109.5 . . ?
C3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C8 C39 H39A 109.5 . . ?
C8 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C8 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C9 C40 H40A 109.5 . . ?
C9 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C9 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C1 N1 C35 121.4(6) . . ?
C1 N1 C2 112.3(6) . . ?
C35 N1 C2 125.2(6) . . ?
C1 N2 C5 123.1(6) . . ?
C1 N2 C3 111.0(6) . . ?
C5 N2 C3 125.9(7) . . ?
C4 N3 C2 115.2(7) . . ?
C4 N3 C36 119.8(7) . . ?
C2 N3 C36 124.9(7) . . ?
C4 N4 C3 114.1(6) . . ?
C4 N4 C6 120.1(7) . . ?
C3 N4 C6 123.6(7) . . ?
C7 N5 C5 121.2(6) . . ?
C7 N5 C8 112.6(6) . . ?
C5 N5 C8 126.0(7) . . ?
C7 N6 C11 121.7(6) . . ?
C7 N6 C9 110.7(6) . . ?
C11 N6 C9 125.6(6) . . ?
C10 N7 C6 121.2(7) . . ?
C10 N7 C8 111.8(6) . . ?
C6 N7 C8 124.8(7) . . ?
C10 N8 C9 114.3(7) . . ?
C10 N8 C12 119.1(7) . . ?
C9 N8 C12 126.1(7) . . ?
C13 N9 C11 123.4(5) . . ?
C13 N9 C14 111.4(6) . . ?
C11 N9 C14 121.5(7) . . ?
C13 N10 C17 122.3(7) . . ?
C13 N10 C15 112.0(8) . . ?
C17 N10 C15 122.5(7) . . ?
C16 N11 C12 120.9(7) . . ?
C16 N11 C14 112.4(8) . . ?
C12 N11 C14 124.4(7) . . ?
C16 N12 C15 113.9(6) . . ?
C16 N12 C18 120.9(6) . . ?
C15 N12 C18 123.9(7) . . ?
C19 N13 C17 120.6(7) . . ?
C19 N13 C20 113.4(7) . . ?
C17 N13 C20 124.8(6) . . ?
C19 N14 C21 114.4(6) . . ?
C19 N14 C23 122.4(7) . . ?
C21 N14 C23 123.0(7) . . ?
C22 N15 C18 123.7(7) . . ?
C22 N15 C20 110.9(7) . . ?
C18 N15 C20 125.0(6) . . ?
C22 N16 C21 112.6(7) . . ?
C22 N16 C24 122.2(7) . . ?
C21 N16 C24 123.1(7) . . ?
C25 N17 C26 112.6(7) . . ?
C25 N17 C23 123.5(7) . . ?
C26 N17 C23 123.9(7) . . ?
C25 N18 C27 113.0(7) . . ?
C25 N18 C29 121.9(7) . . ?
C27 N18 C29 121.8(7) . . ?
C28 N19 C24 122.7(7) . . ?
C28 N19 C26 111.4(6) . . ?
C24 N19 C26 123.7(7) . . ?
C28 N20 C30 122.3(8) . . ?
C28 N20 C27 112.9(7) . . ?
C30 N20 C27 124.7(7) . . ?
C31 N21 C32 113.7(7) . . ?
C31 N21 C29 121.2(7) . . ?
C32 N21 C29 123.2(7) . . ?
C31 N22 C35 122.5(6) . . ?
C31 N22 C33 111.8(7) . . ?
C35 N22 C33 124.4(7) . . ?
C34 N23 C32 114.8(7) . . ?
C34 N23 C30 120.5(7) . . ?
C32 N23 C30 123.9(7) . . ?
C34 N24 C33 114.3(8) . . ?
C34 N24 C36 121.6(8) . . ?
C33 N24 C36 121.4(9) . . ?
C1 O1 Eu1 155.9(5) . . ?
C7 O2 Eu1 166.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.107

# 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 0.064 0.317 0.379 28 7 ' '
2 0.114 0.354 0.878 15 8 ' '
3 0.225 0.895 0.848 104 27 ' '
4 0.275 0.895 0.348 104 27 ' '
5 0.217 0.057 0.572 18 10 ' '
6 0.218 0.222 0.558 13 9 ' '
7 0.282 0.057 0.072 18 10 ' '
8 0.281 0.222 0.058 13 9 ' '
9 0.436 0.317 0.879 28 7 ' '
10 0.386 0.354 0.378 15 8 ' '
11 0.564 0.817 0.121 28 7 ' '
12 0.614 0.854 0.622 15 8 ' '
13 0.725 0.395 0.652 104 27 ' '
14 0.775 0.395 0.152 104 27 ' '
15 0.717 0.557 0.928 18 10 ' '
16 0.718 0.722 0.942 13 9 ' '
17 0.782 0.557 0.428 18 10 ' '
18 0.781 0.722 0.442 13 9 ' '
19 0.936 0.817 0.621 28 7 ' '
20 0.886 0.854 0.122 15 8 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997812'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_08Gd
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Gd N24 O18, 2(N O3), Cl, 16(H2 O)'
_chemical_formula_sum            'C40 H88 Cl Gd N26 O40'
_chemical_formula_weight         1766.06

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.306(5)
_cell_length_b                   14.142(2)
_cell_length_c                   13.4153(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6698.0(16)
_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       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3644
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_T_max  0.8194
_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            41241
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6252
_reflns_number_gt                5129
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0470P)²+42.1714P] 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         6252
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1542
_refine_ls_wR_factor_gt          0.1480
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
O5W O 0.2747(2) 0.2500 0.6164(5) 0.0550(19) Uani 1 2 d S . .
Cl1 Cl 0.2353(2) -0.2500 0.9089(8) 0.219(4) Uani 1 2 d S . .
O1W O 0.34079(13) 0.1226(3) 0.4958(3) 0.0438(11) Uani 1 1 d . . .
O2W O 0.34980(19) 0.2500 0.6534(5) 0.0453(16) Uani 1 2 d S . .
O3W O 0.35536(19) 0.2500 0.3307(5) 0.0447(16) Uani 1 2 d S . .
O4W O 0.42173(16) 0.1430(4) 0.4024(4) 0.0620(15) Uani 1 1 d . . .
Gd1 Gd 0.384101(11) 0.2500 0.49965(3) 0.02897(14) Uani 1 2 d S . .
N13 N 0.3833(3) -0.2500 1.0817(8) 0.050(2) Uani 1 2 d S . .
N14 N 0.3666(3) -0.2500 0.6666(9) 0.069(3) Uani 1 2 d SD . .
O7 O 0.3994(4) -0.2500 1.0027(7) 0.093(3) Uani 1 2 d S . .
O8 O 0.3478(3) -0.2500 1.0890(10) 0.101(4) Uani 1 2 d S . .
O9 O 0.4001(3) -0.2500 1.1617(8) 0.093(3) Uani 1 2 d S . .
O10 O 0.40145(19) -0.2500 0.6866(6) 0.0517(18) Uani 1 2 d SD . .
O11 O 0.3423(2) -0.2500 0.7250(7) 0.077(3) Uani 1 2 d SD . .
O12 O 0.3584(3) -0.2500 0.5788(8) 0.206(11) Uani 1 2 d SD . .
C1 C 0.43933(16) 0.1224(4) 0.6725(4) 0.0260(12) Uani 1 1 d . . .
C2 C 0.49043(16) 0.1142(4) 0.7811(4) 0.0319(13) Uani 1 1 d . . .
C3 C 0.46573(18) 0.0234(4) 0.7921(4) 0.0334(14) Uani 1 1 d . . .
C4 C 0.46720(18) 0.1070(5) 0.9437(4) 0.0386(16) Uani 1 1 d . . .
C5 C 0.40407(17) -0.0228(4) 0.6980(4) 0.0333(13) Uani 1 1 d . . .
H5A H 0.3939 -0.0034 0.6332 0.040 Uiso 1 1 calc R . .
H5B H 0.4159 -0.0850 0.6894 0.040 Uiso 1 1 calc R . .
C6 C 0.43585(19) -0.0473(5) 0.9524(5) 0.0423(16) Uani 1 1 d . . .
H6A H 0.4416 -0.0422 1.0236 0.051 Uiso 1 1 calc R . .
H6B H 0.4446 -0.1094 0.9295 0.051 Uiso 1 1 calc R . .
C7 C 0.33590(17) -0.0132(4) 0.7415(4) 0.0304(13) Uani 1 1 d . . .
C8 C 0.37574(18) -0.0884(4) 0.8577(4) 0.0341(14) Uani 1 1 d . . .
H8 H 0.3867 -0.1516 0.8441 0.041 Uiso 1 1 calc R . .
C9 C 0.33480(18) -0.0952(4) 0.8934(5) 0.0366(14) Uani 1 1 d . . .
H9 H 0.3267 -0.1620 0.9002 0.044 Uiso 1 1 calc R . .
C10 C 0.3714(2) -0.0269(5) 1.0202(4) 0.0397(15) Uani 1 1 d . . .
C11 C 0.27265(18) -0.0415(5) 0.8147(5) 0.0418(16) Uani 1 1 d . . .
H11A H 0.2642 -0.0326 0.7457 0.050 Uiso 1 1 calc R . .
H11B H 0.2622 -0.1015 0.8385 0.050 Uiso 1 1 calc R . .
C12 C 0.3038(2) -0.0539(5) 1.0593(5) 0.0410(16) Uani 1 1 d . . .
H12A H 0.2901 -0.1135 1.0489 0.049 Uiso 1 1 calc R . .
H12B H 0.3141 -0.0545 1.1271 0.049 Uiso 1 1 calc R . .
C13 C 0.24123(17) 0.1107(5) 0.8313(5) 0.0413(16) Uani 1 1 d . . .
C14 C 0.2464(2) 0.0242(5) 0.9787(5) 0.0454(17) Uani 1 1 d . . .
H14 H 0.2293 -0.0307 0.9884 0.055 Uiso 1 1 calc R . .
C15 C 0.22604(18) 0.1191(5) 1.0016(5) 0.0433(15) Uani 1 1 d . . .
H15 H 0.2006 0.1089 1.0305 0.052 Uiso 1 1 calc R . .
C16 C 0.28032(19) 0.1060(5) 1.0996(5) 0.0399(16) Uani 1 1 d . . .
C17 C 0.2032(3) 0.2500 0.8840(8) 0.048(3) Uani 1 2 d S . .
H17A H 0.1955 0.2500 0.8138 0.058 Uiso 1 2 calc SR . .
H17B H 0.1802 0.2500 0.9246 0.058 Uiso 1 2 calc SR . .
C18 C 0.2421(3) 0.2500 1.1262(7) 0.039(2) Uani 1 2 d S . .
H18A H 0.2559 0.2500 1.1895 0.047 Uiso 1 2 calc SR . .
H18B H 0.2150 0.2500 1.1415 0.047 Uiso 1 2 calc SR . .
C19 C 0.5044(3) 0.2500 0.9063(6) 0.039(2) Uani 1 2 d S . .
H19A H 0.5074 0.2500 0.9790 0.046 Uiso 1 2 calc SR . .
H19B H 0.5299 0.2500 0.8769 0.046 Uiso 1 2 calc SR . .
C20 C 0.4853(2) 0.2500 0.6517(6) 0.0330(19) Uani 1 2 d S . .
H20A H 0.5131 0.2500 0.6517 0.040 Uiso 1 2 calc SR . .
H20B H 0.4770 0.2500 0.5820 0.040 Uiso 1 2 calc SR . .
C21 C 0.53233(18) 0.0934(6) 0.7605(6) 0.054(2) Uani 1 1 d . . .
H21A H 0.5431 0.0592 0.8165 0.081 Uiso 1 1 calc R . .
H21B H 0.5459 0.1525 0.7515 0.081 Uiso 1 1 calc R . .
H21C H 0.5345 0.0554 0.7006 0.081 Uiso 1 1 calc R . .
C22 C 0.4840(2) -0.0707(6) 0.7627(6) 0.057(2) Uani 1 1 d . . .
H22A H 0.4900 -0.0698 0.6921 0.085 Uiso 1 1 calc R . .
H22B H 0.4666 -0.1220 0.7764 0.085 Uiso 1 1 calc R . .
H22C H 0.5071 -0.0798 0.8008 0.085 Uiso 1 1 calc R . .
N1 N 0.47240(13) 0.1632(3) 0.6979(3) 0.0273(10) Uani 1 1 d . . .
N2 N 0.43296(13) 0.0444(3) 0.7281(3) 0.0288(11) Uani 1 1 d . . .
N3 N 0.48501(14) 0.1637(4) 0.8767(3) 0.0346(12) Uani 1 1 d . . .
N4 N 0.45652(15) 0.0256(4) 0.8991(4) 0.0346(12) Uani 1 1 d . . .
N5 N 0.37307(14) -0.0317(4) 0.7678(4) 0.0336(12) Uani 1 1 d . . .
N6 N 0.31352(15) -0.0474(3) 0.8160(4) 0.0338(11) Uani 1 1 d . . .
N7 N 0.39503(15) -0.0415(4) 0.9389(4) 0.0359(12) Uani 1 1 d . . .
N8 N 0.33497(16) -0.0480(4) 0.9882(4) 0.0388(13) Uani 1 1 d . . .
N9 N 0.25775(15) 0.0344(4) 0.8751(4) 0.0396(13) Uani 1 1 d . . .
N10 N 0.22401(14) 0.1641(4) 0.9039(4) 0.0395(13) Uani 1 1 d . . .
N11 N 0.27748(16) 0.0238(4) 1.0498(4) 0.0407(13) Uani 1 1 d . . .
N12 N 0.25131(15) 0.1640(4) 1.0718(4) 0.0387(12) Uani 1 1 d . . .
O1 O 0.41797(12) 0.1500(3) 0.6050(3) 0.0335(9) Uani 1 1 d . . .
O2 O 0.32454(12) 0.0201(3) 0.6630(3) 0.0384(10) Uani 1 1 d . . .
O3 O 0.24073(13) 0.1290(4) 0.7425(3) 0.0485(12) Uani 1 1 d . . .
O4 O 0.46149(14) 0.1267(4) 1.0319(3) 0.0481(12) Uani 1 1 d . . .
O5 O 0.38098(15) -0.0021(4) 1.1021(4) 0.0560(14) Uani 1 1 d . . .
O6 O 0.30437(14) 0.1260(3) 1.1623(3) 0.0454(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Gd1 2.364(4) . ?
O2W Gd1 2.392(7) . ?
O3W Gd1 2.484(6) . ?
O4W Gd1 2.399(5) . ?
Gd1 O1 2.330(4) 7_565 ?
Gd1 O1 2.330(4) . ?
Gd1 O1W 2.364(4) 7_565 ?
Gd1 O4W 2.399(5) 7_565 ?
N13 O7 1.202(13) . ?
N13 O9 1.225(12) . ?
N13 O8 1.258(12) . ?
N14 O11 1.163(14) . ?
N14 O12 1.213(14) . ?
N14 O10 1.259(12) . ?
C1 O1 1.242(7) . ?
C1 N1 1.346(7) . ?
C1 N2 1.351(7) . ?
C2 N1 1.459(7) . ?
C2 N3 1.473(7) . ?
C2 C21 1.533(8) . ?
C2 C3 1.560(9) . ?
C3 N2 1.471(7) . ?
C3 N4 1.472(7) . ?
C3 C22 1.530(9) . ?
C4 O4 1.232(7) . ?
C4 N4 1.351(8) . ?
C4 N3 1.359(8) . ?
C5 N5 1.445(8) . ?
C5 N2 1.451(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.451(8) . ?
C6 N7 1.455(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.223(7) . ?
C7 N6 1.363(8) . ?
C7 N5 1.383(8) . ?
C8 N7 1.445(8) . ?
C8 N5 1.453(7) . ?
C8 C9 1.525(9) . ?
C8 H8 0.9900 . ?
C9 N8 1.436(8) . ?
C9 N6 1.449(8) . ?
C9 H9 0.9900 . ?
C10 O5 1.201(8) . ?
C10 N7 1.389(8) . ?
C10 N8 1.389(9) . ?
C11 N9 1.444(8) . ?
C11 N6 1.445(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.444(8) . ?
C12 N8 1.460(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.220(8) . ?
C13 N9 1.360(9) . ?
C13 N10 1.374(9) . ?
C14 N9 1.454(8) . ?
C14 N11 1.455(9) . ?
C14 C15 1.553(10) . ?
C14 H14 0.9900 . ?
C15 N12 1.443(8) . ?
C15 N10 1.459(8) . ?
C15 H15 0.9900 . ?
C16 O6 1.229(8) . ?
C16 N11 1.343(9) . ?
C16 N12 1.364(8) . ?
C17 N10 1.443(7) 7_565 ?
C17 N10 1.443(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.455(7) . ?
C18 N12 1.455(7) 7_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.456(7) 7_565 ?
C19 N3 1.456(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.449(6) 7_565 ?
C20 N1 1.449(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O1 74.8(2) 7_565 . ?
O1 Gd1 O1W 83.25(15) 7_565 7_565 ?
O1 Gd1 O1W 143.92(15) . 7_565 ?
O1 Gd1 O1W 143.92(15) 7_565 . ?
O1 Gd1 O1W 83.25(15) . . ?
O1W Gd1 O1W 99.3(2) 7_565 . ?
O1 Gd1 O2W 74.75(16) 7_565 . ?
O1 Gd1 O2W 74.75(16) . . ?
O1W Gd1 O2W 72.03(15) 7_565 . ?
O1W Gd1 O2W 72.03(15) . . ?
O1 Gd1 O4W 115.37(17) 7_565 . ?
O1 Gd1 O4W 70.28(16) . . ?
O1W Gd1 O4W 145.79(16) 7_565 . ?
O1W Gd1 O4W 82.27(19) . . ?
O2W Gd1 O4W 138.53(14) . . ?
O1 Gd1 O4W 70.28(16) 7_565 7_565 ?
O1 Gd1 O4W 115.37(17) . 7_565 ?
O1W Gd1 O4W 82.27(19) 7_565 7_565 ?
O1W Gd1 O4W 145.79(16) . 7_565 ?
O2W Gd1 O4W 138.53(14) . 7_565 ?
O4W Gd1 O4W 78.2(3) . 7_565 ?
O1 Gd1 O3W 139.76(11) 7_565 . ?
O1 Gd1 O3W 139.76(11) . . ?
O1W Gd1 O3W 73.48(14) 7_565 . ?
O1W Gd1 O3W 73.48(14) . . ?
O2W Gd1 O3W 125.5(2) . . ?
O4W Gd1 O3W 74.33(17) . . ?
O4W Gd1 O3W 74.33(17) 7_565 . ?
O7 N13 O9 123.0(11) . . ?
O7 N13 O8 122.6(11) . . ?
O9 N13 O8 114.3(11) . . ?
O11 N14 O12 118.5(11) . . ?
O11 N14 O10 125.3(12) . . ?
O12 N14 O10 116.2(13) . . ?
O1 C1 N1 125.3(5) . . ?
O1 C1 N2 123.9(5) . . ?
N1 C1 N2 110.8(5) . . ?
N1 C2 N3 112.6(5) . . ?
N1 C2 C21 112.0(5) . . ?
N3 C2 C21 111.9(5) . . ?
N1 C2 C3 102.7(4) . . ?
N3 C2 C3 103.7(5) . . ?
C21 C2 C3 113.5(5) . . ?
N2 C3 N4 113.0(5) . . ?
N2 C3 C22 110.9(5) . . ?
N4 C3 C22 111.3(5) . . ?
N2 C3 C2 102.6(4) . . ?
N4 C3 C2 101.4(5) . . ?
C22 C3 C2 117.1(5) . . ?
O4 C4 N4 124.9(6) . . ?
O4 C4 N3 125.3(7) . . ?
N4 C4 N3 109.8(5) . . ?
N5 C5 N2 114.2(5) . . ?
N5 C5 H5A 108.7 . . ?
N2 C5 H5A 108.7 . . ?
N5 C5 H5B 108.7 . . ?
N2 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N4 C6 N7 113.4(5) . . ?
N4 C6 H6A 108.9 . . ?
N7 C6 H6A 108.9 . . ?
N4 C6 H6B 108.9 . . ?
N7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N6 125.4(6) . . ?
O2 C7 N5 127.1(6) . . ?
N6 C7 N5 107.3(5) . . ?
N7 C8 N5 113.7(5) . . ?
N7 C8 C9 103.9(5) . . ?
N5 C8 C9 103.5(5) . . ?
N7 C8 H8 111.7 . . ?
N5 C8 H8 111.7 . . ?
C9 C8 H8 111.7 . . ?
N8 C9 N6 114.8(5) . . ?
N8 C9 C8 104.1(5) . . ?
N6 C9 C8 103.8(5) . . ?
N8 C9 H9 111.2 . . ?
N6 C9 H9 111.2 . . ?
C8 C9 H9 111.2 . . ?
O5 C10 N7 126.4(7) . . ?
O5 C10 N8 127.3(7) . . ?
N7 C10 N8 106.3(5) . . ?
N9 C11 N6 113.5(5) . . ?
N9 C11 H11A 108.9 . . ?
N6 C11 H11A 108.9 . . ?
N9 C11 H11B 108.9 . . ?
N6 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N11 C12 N8 112.6(5) . . ?
N11 C12 H12A 109.1 . . ?
N8 C12 H12A 109.1 . . ?
N11 C12 H12B 109.1 . . ?
N8 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N9 126.7(7) . . ?
O3 C13 N10 124.6(7) . . ?
N9 C13 N10 108.7(6) . . ?
N9 C14 N11 114.7(6) . . ?
N9 C14 C15 103.3(6) . . ?
N11 C14 C15 102.8(6) . . ?
N9 C14 H14 111.8 . . ?
N11 C14 H14 111.8 . . ?
C15 C14 H14 111.8 . . ?
N12 C15 N10 115.1(5) . . ?
N12 C15 C14 102.9(5) . . ?
N10 C15 C14 102.8(5) . . ?
N12 C15 H15 111.8 . . ?
N10 C15 H15 111.8 . . ?
C14 C15 H15 111.8 . . ?
O6 C16 N11 126.3(7) . . ?
O6 C16 N12 124.6(6) . . ?
N11 C16 N12 109.1(6) . . ?
N10 C17 N10 114.5(8) 7_565 . ?
N10 C17 H17A 108.6 7_565 . ?
N10 C17 H17A 108.6 . . ?
N10 C17 H17B 108.6 7_565 . ?
N10 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
N12 C18 N12 113.5(7) . 7_565 ?
N12 C18 H18A 108.9 . . ?
N12 C18 H18A 108.9 7_565 . ?
N12 C18 H18B 108.9 . . ?
N12 C18 H18B 108.9 7_565 . ?
H18A C18 H18B 107.7 . . ?
N3 C19 N3 114.0(7) 7_565 . ?
N3 C19 H19A 108.8 7_565 . ?
N3 C19 H19A 108.8 . . ?
N3 C19 H19B 108.8 7_565 . ?
N3 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
N1 C20 N1 115.9(7) 7_565 . ?
N1 C20 H20A 108.3 7_565 . ?
N1 C20 H20A 108.3 . . ?
N1 C20 H20B 108.3 7_565 . ?
N1 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C22 H22A 109.5 . . ?
C3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C20 121.8(5) . . ?
C1 N1 C2 111.6(5) . . ?
C20 N1 C2 126.3(5) . . ?
C1 N2 C5 119.9(5) . . ?
C1 N2 C3 110.9(5) . . ?
C5 N2 C3 125.7(5) . . ?
C4 N3 C19 122.1(6) . . ?
C4 N3 C2 110.8(5) . . ?
C19 N3 C2 125.1(6) . . ?
C4 N4 C6 121.8(5) . . ?
C4 N4 C3 112.9(5) . . ?
C6 N4 C3 125.2(5) . . ?
C7 N5 C5 122.5(5) . . ?
C7 N5 C8 112.1(5) . . ?
C5 N5 C8 122.5(5) . . ?
C7 N6 C11 123.3(5) . . ?
C7 N6 C9 112.9(5) . . ?
C11 N6 C9 123.6(5) . . ?
C10 N7 C8 112.2(5) . . ?
C10 N7 C6 120.3(5) . . ?
C8 N7 C6 122.3(5) . . ?
C10 N8 C9 112.2(5) . . ?
C10 N8 C12 120.6(5) . . ?
C9 N8 C12 123.3(5) . . ?
C13 N9 C11 120.2(6) . . ?
C13 N9 C14 111.9(6) . . ?
C11 N9 C14 124.3(6) . . ?
C13 N10 C17 123.8(6) . . ?
C13 N10 C15 112.0(6) . . ?
C17 N10 C15 123.9(6) . . ?
C16 N11 C12 124.5(6) . . ?
C16 N11 C14 112.3(6) . . ?
C12 N11 C14 123.0(6) . . ?
C16 N12 C15 112.2(6) . . ?
C16 N12 C18 122.2(6) . . ?
C15 N12 C18 123.8(6) . . ?
C1 O1 Gd1 160.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.110

# 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 0.000 768 298 ' '
2 0.500 0.150 0.500 769 297 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997813'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_09Tb
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Tb N24 O18, 2(N O3), Cl, 16(H2 O)'
_chemical_formula_sum            'C40 H88 Cl N26 O40 Tb'
_chemical_formula_weight         1767.73

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.381(3)
_cell_length_b                   14.2066(13)
_cell_length_c                   13.4355(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6753.2(11)
_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       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3648
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_T_max  0.7685
_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            44674
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6302
_reflns_number_gt                4787
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0628P)²+26.8047P] 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         6302
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1495
_refine_ls_wR_factor_gt          0.1411
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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 0.2655(2) -0.2500 0.4082(6) 0.209(3) Uani 1 2 d S . .
O5W O 0.2259(2) 0.2500 0.1187(6) 0.077(2) Uani 1 2 d S . .
O1W O 0.15848(12) 0.1229(3) -0.0034(3) 0.0419(10) Uani 1 1 d . . .
O2W O 0.14989(16) 0.2500 0.1540(4) 0.0415(14) Uani 1 2 d S . .
O3W O 0.14501(18) 0.2500 -0.1674(4) 0.0467(15) Uani 1 2 d S . .
O4W O 0.07820(14) 0.1450(3) -0.0962(3) 0.0564(13) Uani 1 1 d . . .
Tb1 Tb 0.115958(10) 0.2500 0.00093(3) 0.02880(14) Uani 1 2 d S . .
N13 N 0.1164(3) -0.2500 0.5828(8) 0.055(2) Uani 1 2 d S . .
N14 N 0.1326(2) -0.2500 0.1661(6) 0.0485(19) Uani 1 2 d SD . .
O7 O 0.1008(4) -0.2500 0.5020(6) 0.094(3) Uani 1 2 d S . .
O8 O 0.0993(2) -0.2500 0.6614(7) 0.090(3) Uani 1 2 d S . .
O9 O 0.1523(3) -0.2500 0.5892(9) 0.109(4) Uani 1 2 d S . .
O10 O 0.09879(18) -0.2500 0.1878(5) 0.0509(16) Uani 1 2 d SD . .
O11 O 0.1583(2) -0.2500 0.2270(6) 0.076(2) Uani 1 2 d SD . .
O12 O 0.1407(3) -0.2500 0.0790(7) 0.209(10) Uani 1 2 d SD . .
C1 C 0.25921(16) 0.1122(5) 0.3332(5) 0.0409(14) Uani 1 1 d . . .
C2 C 0.27378(16) 0.1199(5) 0.5041(4) 0.0414(14) Uani 1 1 d . . .
H2 H 0.2992 0.1103 0.5332 0.050 Uiso 1 1 calc R . .
C3 C 0.25390(17) 0.0242(5) 0.4804(4) 0.0392(15) Uani 1 1 d . . .
H3 H 0.2710 -0.0302 0.4903 0.047 Uiso 1 1 calc R . .
C4 C 0.21963(17) 0.1069(4) 0.6009(4) 0.0399(14) Uani 1 1 d . . .
C5 C 0.22734(17) -0.0415(4) 0.3156(5) 0.0436(15) Uani 1 1 d . . .
H5A H 0.2357 -0.0323 0.2467 0.052 Uiso 1 1 calc R . .
H5B H 0.2378 -0.1015 0.3389 0.052 Uiso 1 1 calc R . .
C6 C 0.19589(17) -0.0531(4) 0.5608(4) 0.0407(14) Uani 1 1 d . . .
H6A H 0.1854 -0.0525 0.6283 0.049 Uiso 1 1 calc R . .
H6B H 0.2093 -0.1128 0.5516 0.049 Uiso 1 1 calc R . .
C7 C 0.16400(16) -0.0129(4) 0.2428(4) 0.0319(12) Uani 1 1 d . . .
C8 C 0.16563(17) -0.0947(4) 0.3946(4) 0.0355(13) Uani 1 1 d . . .
H8 H 0.1739 -0.1609 0.4018 0.043 Uiso 1 1 calc R . .
C9 C 0.12427(16) -0.0887(4) 0.3581(4) 0.0335(13) Uani 1 1 d . . .
H9 H 0.1135 -0.1515 0.3437 0.040 Uiso 1 1 calc R . .
C10 C 0.1286(2) -0.0268(5) 0.5205(4) 0.0425(15) Uani 1 1 d . . .
C11 C 0.09618(16) -0.0223(4) 0.1986(4) 0.0340(13) Uani 1 1 d . . .
H11A H 0.0843 -0.0842 0.1905 0.041 Uiso 1 1 calc R . .
H11B H 0.1063 -0.0033 0.1337 0.041 Uiso 1 1 calc R . .
C12 C 0.06418(19) -0.0486(5) 0.4526(4) 0.0460(16) Uani 1 1 d . . .
H12A H 0.0582 -0.0445 0.5237 0.055 Uiso 1 1 calc R . .
H12B H 0.0556 -0.1102 0.4286 0.055 Uiso 1 1 calc R . .
C13 C 0.06113(15) 0.1221(4) 0.1727(4) 0.0279(11) Uani 1 1 d . . .
C14 C 0.03443(16) 0.0249(4) 0.2937(4) 0.0323(12) Uani 1 1 d . . .
C15 C 0.00986(16) 0.1149(4) 0.2825(4) 0.0336(13) Uani 1 1 d . . .
C16 C 0.03294(16) 0.1077(5) 0.4442(4) 0.0396(14) Uani 1 1 d . . .
C17 C 0.0145(2) 0.2500 0.1513(6) 0.0331(18) Uani 1 2 d S . .
H17A H -0.0132 0.2500 0.1515 0.040 Uiso 1 2 calc SR . .
H17B H 0.0228 0.2500 0.0816 0.040 Uiso 1 2 calc SR . .
C18 C -0.0036(2) 0.2500 0.4080(6) 0.0344(18) Uani 1 2 d S . .
H18A H -0.0057 0.2500 0.4807 0.041 Uiso 1 2 calc SR . .
H18B H -0.0293 0.2500 0.3807 0.041 Uiso 1 2 calc SR . .
C19 C 0.2572(3) 0.2500 0.6279(6) 0.043(2) Uani 1 2 d S . .
H19A H 0.2429 0.2500 0.6903 0.051 Uiso 1 2 calc SR . .
H19B H 0.2842 0.2500 0.6449 0.051 Uiso 1 2 calc SR . .
C20 C 0.2973(2) 0.2500 0.3859(7) 0.051(2) Uani 1 2 d S . .
H20A H 0.3051 0.2500 0.3159 0.061 Uiso 1 2 calc SR . .
H20B H 0.3203 0.2500 0.4268 0.061 Uiso 1 2 calc SR . .
C21 C 0.01569(19) -0.0699(5) 0.2628(5) 0.0541(18) Uani 1 1 d . . .
H21A H -0.0056 -0.0829 0.3063 0.081 Uiso 1 1 calc R . .
H21B H 0.0341 -0.1204 0.2682 0.081 Uiso 1 1 calc R . .
H21C H 0.0069 -0.0656 0.1946 0.081 Uiso 1 1 calc R . .
C22 C -0.03211(16) 0.0946(5) 0.2602(5) 0.0487(17) Uani 1 1 d . . .
H22A H -0.0433 0.0619 0.3163 0.073 Uiso 1 1 calc R . .
H22B H -0.0340 0.0556 0.2012 0.073 Uiso 1 1 calc R . .
H22C H -0.0454 0.1534 0.2492 0.073 Uiso 1 1 calc R . .
N1 N 0.27590(13) 0.1648(4) 0.4062(4) 0.0407(12) Uani 1 1 d . . .
N2 N 0.24245(14) 0.0344(4) 0.3770(4) 0.0397(12) Uani 1 1 d . . .
N3 N 0.24857(13) 0.1639(3) 0.5734(4) 0.0379(11) Uani 1 1 d . . .
N4 N 0.22233(14) 0.0234(4) 0.5507(4) 0.0404(12) Uani 1 1 d . . .
N5 N 0.18671(14) -0.0469(3) 0.3172(3) 0.0361(11) Uani 1 1 d . . .
N6 N 0.12721(13) -0.0305(3) 0.2688(3) 0.0360(11) Uani 1 1 d . . .
N7 N 0.16488(14) -0.0473(4) 0.4889(3) 0.0387(12) Uani 1 1 d . . .
N8 N 0.10464(14) -0.0419(4) 0.4400(3) 0.0372(11) Uani 1 1 d . . .
N9 N 0.06745(13) 0.0454(3) 0.2292(3) 0.0307(10) Uani 1 1 d . . .
N10 N 0.02782(12) 0.1635(3) 0.1987(3) 0.0286(10) Uani 1 1 d . . .
N11 N 0.04359(13) 0.0255(3) 0.3993(3) 0.0355(11) Uani 1 1 d . . .
N12 N 0.01532(13) 0.1632(3) 0.3770(3) 0.0375(11) Uani 1 1 d . . .
O1 O 0.25995(12) 0.1295(3) 0.2442(3) 0.0471(11) Uani 1 1 d . . .
O2 O 0.17526(11) 0.0216(3) 0.1642(3) 0.0379(9) Uani 1 1 d . . .
O3 O 0.08236(11) 0.1498(3) 0.1062(3) 0.0333(9) Uani 1 1 d . . .
O4 O 0.19545(12) 0.1257(3) 0.6647(3) 0.0471(11) Uani 1 1 d . . .
O5 O 0.11885(13) -0.0026(4) 0.6031(3) 0.0555(13) Uani 1 1 d . . .
O6 O 0.03844(13) 0.1259(3) 0.5329(3) 0.0496(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Tb1 2.351(4) . ?
O2W Tb1 2.382(5) . ?
O3W Tb1 2.484(6) . ?
O4W Tb1 2.390(4) . ?
Tb1 O3 2.332(4) 7_565 ?
Tb1 O3 2.332(4) . ?
Tb1 O1W 2.351(4) 7_565 ?
Tb1 O4W 2.390(4) 7_565 ?
N13 O7 1.217(12) . ?
N13 O8 1.219(11) . ?
N13 O9 1.274(12) . ?
N14 O12 1.204(11) . ?
N14 O11 1.224(10) . ?
N14 O10 1.231(9) . ?
C1 O1 1.221(7) . ?
C1 N1 1.368(8) . ?
C1 N2 1.386(8) . ?
C2 N3 1.432(7) . ?
C2 N1 1.463(7) . ?
C2 C3 1.564(9) . ?
C2 H2 0.9900 . ?
C3 N2 1.455(7) . ?
C3 N4 1.462(7) . ?
C3 H3 0.9900 . ?
C4 O4 1.240(7) . ?
C4 N3 1.357(8) . ?
C4 N4 1.368(8) . ?
C5 N5 1.440(7) . ?
C5 N2 1.459(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.440(8) . ?
C6 N7 1.464(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.231(6) . ?
C7 N5 1.370(7) . ?
C7 N6 1.371(7) . ?
C8 N7 1.435(7) . ?
C8 N5 1.448(7) . ?
C8 C9 1.545(8) . ?
C8 H8 0.9900 . ?
C9 N8 1.460(7) . ?
C9 N6 1.460(7) . ?
C9 H9 0.9900 . ?
C10 O5 1.212(7) . ?
C10 N7 1.385(8) . ?
C10 N8 1.390(8) . ?
C11 N6 1.453(7) . ?
C11 N9 1.459(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.445(8) . ?
C12 N11 1.467(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.231(6) . ?
C13 N9 1.347(7) . ?
C13 N10 1.362(7) . ?
C14 N11 1.455(7) . ?
C14 N9 1.483(7) . ?
C14 C15 1.553(8) . ?
C14 C21 1.558(8) . ?
C15 N12 1.456(7) . ?
C15 N10 1.466(6) . ?
C15 C22 1.542(8) . ?
C16 O6 1.234(7) . ?
C16 N12 1.351(7) . ?
C16 N11 1.369(8) . ?
C17 N10 1.462(6) . ?
C17 N10 1.462(6) 7_565 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.464(6) . ?
C18 N12 1.464(6) 7_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.458(7) 7_565 ?
C19 N3 1.458(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.454(7) . ?
C20 N1 1.454(7) 7_565 ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

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
O3 Tb1 O3 75.21(18) 7_565 . ?
O3 Tb1 O1W 144.06(13) 7_565 . ?
O3 Tb1 O1W 82.66(13) . . ?
O3 Tb1 O1W 82.66(13) 7_565 7_565 ?
O3 Tb1 O1W 144.06(13) . 7_565 ?
O1W Tb1 O1W 100.4(2) . 7_565 ?
O3 Tb1 O2W 74.52(14) 7_565 . ?
O3 Tb1 O2W 74.52(14) . . ?
O1W Tb1 O2W 72.46(13) . . ?
O1W Tb1 O2W 72.46(13) 7_565 . ?
O3 Tb1 O4W 115.29(16) 7_565 . ?
O3 Tb1 O4W 70.46(14) . . ?
O1W Tb1 O4W 82.23(16) . . ?
O1W Tb1 O4W 145.45(14) 7_565 . ?
O2W Tb1 O4W 138.87(12) . . ?
O3 Tb1 O4W 70.46(14) 7_565 7_565 ?
O3 Tb1 O4W 115.29(16) . 7_565 ?
O1W Tb1 O4W 145.45(14) . 7_565 ?
O1W Tb1 O4W 82.23(16) 7_565 7_565 ?
O2W Tb1 O4W 138.87(12) . 7_565 ?
O4W Tb1 O4W 77.2(2) . 7_565 ?
O3 Tb1 O3W 139.73(10) 7_565 . ?
O3 Tb1 O3W 139.73(10) . . ?
O1W Tb1 O3W 73.32(13) . . ?
O1W Tb1 O3W 73.32(13) 7_565 . ?
O2W Tb1 O3W 125.3(2) . . ?
O4W Tb1 O3W 74.58(15) . . ?
O4W Tb1 O3W 74.58(15) 7_565 . ?
O7 N13 O8 123.2(11) . . ?
O7 N13 O9 120.9(11) . . ?
O8 N13 O9 115.9(11) . . ?
O12 N14 O11 118.3(9) . . ?
O12 N14 O10 117.4(9) . . ?
O11 N14 O10 124.3(8) . . ?
O1 C1 N1 125.7(6) . . ?
O1 C1 N2 125.9(6) . . ?
N1 C1 N2 108.5(5) . . ?
N3 C2 N1 115.2(5) . . ?
N3 C2 C3 103.4(5) . . ?
N1 C2 C3 102.7(5) . . ?
N3 C2 H2 111.6 . . ?
N1 C2 H2 111.6 . . ?
C3 C2 H2 111.6 . . ?
N2 C3 N4 113.9(5) . . ?
N2 C3 C2 103.5(5) . . ?
N4 C3 C2 102.6(5) . . ?
N2 C3 H3 112.1 . . ?
N4 C3 H3 112.1 . . ?
C2 C3 H3 112.1 . . ?
O4 C4 N3 125.5(6) . . ?
O4 C4 N4 125.1(6) . . ?
N3 C4 N4 109.3(5) . . ?
N5 C5 N2 113.4(5) . . ?
N5 C5 H5A 108.9 . . ?
N2 C5 H5A 108.9 . . ?
N5 C5 H5B 108.9 . . ?
N2 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N4 C6 N7 112.5(5) . . ?
N4 C6 H6A 109.1 . . ?
N7 C6 H6A 109.1 . . ?
N4 C6 H6B 109.1 . . ?
N7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 N5 125.2(5) . . ?
O2 C7 N6 126.8(5) . . ?
N5 C7 N6 107.9(5) . . ?
N7 C8 N5 115.1(5) . . ?
N7 C8 C9 103.7(4) . . ?
N5 C8 C9 103.6(4) . . ?
N7 C8 H8 111.3 . . ?
N5 C8 H8 111.3 . . ?
C9 C8 H8 111.3 . . ?
N8 C9 N6 113.3(5) . . ?
N8 C9 C8 103.7(4) . . ?
N6 C9 C8 102.9(4) . . ?
N8 C9 H9 112.1 . . ?
N6 C9 H9 112.1 . . ?
C8 C9 H9 112.1 . . ?
O5 C10 N7 127.1(6) . . ?
O5 C10 N8 125.7(6) . . ?
N7 C10 N8 107.1(5) . . ?
N6 C11 N9 113.3(4) . . ?
N6 C11 H11A 108.9 . . ?
N9 C11 H11A 108.9 . . ?
N6 C11 H11B 108.9 . . ?
N9 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N8 C12 N11 112.8(5) . . ?
N8 C12 H12A 109.0 . . ?
N11 C12 H12A 109.0 . . ?
N8 C12 H12B 109.0 . . ?
N11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N9 124.5(5) . . ?
O3 C13 N10 125.2(5) . . ?
N9 C13 N10 110.3(5) . . ?
N11 C14 N9 113.1(4) . . ?
N11 C14 C15 102.4(4) . . ?
N9 C14 C15 102.8(4) . . ?
N11 C14 C21 111.1(5) . . ?
N9 C14 C21 110.4(5) . . ?
C15 C14 C21 116.6(5) . . ?
N12 C15 N10 113.1(4) . . ?
N12 C15 C22 112.7(5) . . ?
N10 C15 C22 110.9(5) . . ?
N12 C15 C14 103.2(4) . . ?
N10 C15 C14 102.7(4) . . ?
C22 C15 C14 113.8(5) . . ?
O6 C16 N12 126.6(6) . . ?
O6 C16 N11 124.1(6) . . ?
N12 C16 N11 109.3(5) . . ?
N10 C17 N10 114.5(6) . 7_565 ?
N10 C17 H17A 108.6 . . ?
N10 C17 H17A 108.6 7_565 . ?
N10 C17 H17B 108.6 . . ?
N10 C17 H17B 108.6 7_565 . ?
H17A C17 H17B 107.6 . . ?
N12 C18 N12 114.8(6) . 7_565 ?
N12 C18 H18A 108.6 . . ?
N12 C18 H18A 108.6 7_565 . ?
N12 C18 H18B 108.6 . . ?
N12 C18 H18B 108.6 7_565 . ?
H18A C18 H18B 107.5 . . ?
N3 C19 N3 114.0(7) 7_565 . ?
N3 C19 H19A 108.8 7_565 . ?
N3 C19 H19A 108.8 . . ?
N3 C19 H19B 108.8 7_565 . ?
N3 C19 H19B 108.8 . . ?
H19A C19 H19B 107.6 . . ?
N1 C20 N1 112.7(7) . 7_565 ?
N1 C20 H20A 109.0 . . ?
N1 C20 H20A 109.0 7_565 . ?
N1 C20 H20B 109.0 . . ?
N1 C20 H20B 109.0 7_565 . ?
H20A C20 H20B 107.8 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C20 123.1(6) . . ?
C1 N1 C2 112.6(5) . . ?
C20 N1 C2 123.9(6) . . ?
C1 N2 C3 111.5(5) . . ?
C1 N2 C5 120.4(5) . . ?
C3 N2 C5 124.7(5) . . ?
C4 N3 C2 112.7(5) . . ?
C4 N3 C19 121.5(6) . . ?
C2 N3 C19 124.2(6) . . ?
C4 N4 C6 124.2(5) . . ?
C4 N4 C3 111.4(5) . . ?
C6 N4 C3 124.3(5) . . ?
C7 N5 C5 123.7(5) . . ?
C7 N5 C8 112.7(5) . . ?
C5 N5 C8 123.4(5) . . ?
C7 N6 C11 122.5(5) . . ?
C7 N6 C9 112.3(4) . . ?
C11 N6 C9 121.7(5) . . ?
C10 N7 C8 112.8(5) . . ?
C10 N7 C6 120.3(5) . . ?
C8 N7 C6 122.9(5) . . ?
C10 N8 C12 121.5(5) . . ?
C10 N8 C9 111.5(5) . . ?
C12 N8 C9 122.0(5) . . ?
C13 N9 C11 119.3(4) . . ?
C13 N9 C14 111.0(4) . . ?
C11 N9 C14 125.7(4) . . ?
C13 N10 C17 121.9(5) . . ?
C13 N10 C15 111.7(4) . . ?
C17 N10 C15 126.2(5) . . ?
C16 N11 C14 111.9(5) . . ?
C16 N11 C12 122.2(5) . . ?
C14 N11 C12 125.7(5) . . ?
C16 N12 C15 111.7(5) . . ?
C16 N12 C18 120.8(5) . . ?
C15 N12 C18 125.7(5) . . ?
C13 O3 Tb1 161.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.120

# 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 0.000 794 301 ' '
2 0.500 0.650 0.500 794 301 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997814'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_10Dy
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Dy N24 O18, 2(N O3), Cl, 16(H2 O)'
_chemical_formula_sum            'C40 H88 Cl Dy N26 O40'
_chemical_formula_weight         1771.31

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.375(4)
_cell_length_b                   14.1652(17)
_cell_length_c                   13.4397(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6734.6(14)
_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          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3652
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_T_max  0.7673
_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            44904
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6324
_reflns_number_gt                4504
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0656P)²+18.0916P] 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         6324
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1441
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.051
_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
O5W O 0.2255(2) 0.2500 0.6193(5) 0.074(2) Uani 1 2 d S . .
Cl1 Cl 0.2652(2) -0.2500 0.9083(6) 0.210(3) Uani 1 2 d S . .
O1W O 0.15831(12) 0.1238(3) 0.4964(3) 0.0410(9) Uani 1 1 d . . .
O2W O 0.14965(16) 0.2500 0.6549(4) 0.0419(14) Uani 1 2 d S . .
O3W O 0.14466(17) 0.2500 0.3354(4) 0.0478(15) Uani 1 2 d S . .
O4W O 0.07840(13) 0.1457(3) 0.4052(3) 0.0545(12) Uani 1 1 d . . .
Dy1 Dy 0.115844(10) 0.2500 0.50182(2) 0.02902(14) Uani 1 2 d S . .
N13 N 0.1165(3) -0.2500 1.0830(7) 0.056(2) Uani 1 2 d S . .
N14 N 0.1326(3) -0.2500 0.6658(6) 0.0517(19) Uani 1 2 d SD . .
O7 O 0.1010(4) -0.2500 1.0024(6) 0.097(3) Uani 1 2 d S . .
O8 O 0.0987(2) -0.2500 1.1616(6) 0.088(3) Uani 1 2 d S . .
O9 O 0.1528(3) -0.2500 1.0903(9) 0.116(4) Uani 1 2 d S . .
O10 O 0.09888(19) -0.2500 0.6880(5) 0.0491(15) Uani 1 2 d SD . .
O11 O 0.1581(2) -0.2500 0.7265(6) 0.077(2) Uani 1 2 d SD . .
O12 O 0.1413(3) -0.2500 0.5802(6) 0.220(10) Uani 1 2 d SD . .
C1 C 0.25940(15) 0.1119(4) 0.8336(4) 0.0404(14) Uani 1 1 d . . .
C2 C 0.27395(17) 0.1196(5) 1.0029(4) 0.0415(14) Uani 1 1 d . . .
H2 H 0.2994 0.1096 1.0318 0.050 Uiso 1 1 calc R . .
C3 C 0.25379(18) 0.0240(5) 0.9811(4) 0.0429(15) Uani 1 1 d . . .
H3 H 0.2708 -0.0306 0.9912 0.052 Uiso 1 1 calc R . .
C4 C 0.21955(17) 0.1058(4) 1.1012(4) 0.0392(14) Uani 1 1 d . . .
C5 C 0.22768(17) -0.0412(4) 0.8157(4) 0.0436(15) Uani 1 1 d . . .
H5A H 0.2360 -0.0320 0.7468 0.052 Uiso 1 1 calc R . .
H5B H 0.2383 -0.1012 0.8391 0.052 Uiso 1 1 calc R . .
C6 C 0.19597(18) -0.0519(4) 1.0621(4) 0.0430(15) Uani 1 1 d . . .
H6A H 0.1856 -0.0502 1.1297 0.052 Uiso 1 1 calc R . .
H6B H 0.2092 -0.1122 1.0537 0.052 Uiso 1 1 calc R . .
C7 C 0.16414(17) -0.0123(4) 0.7432(4) 0.0359(13) Uani 1 1 d . . .
C8 C 0.16561(17) -0.0947(4) 0.8941(4) 0.0373(14) Uani 1 1 d . . .
H8 H 0.1738 -0.1612 0.9014 0.045 Uiso 1 1 calc R . .
C9 C 0.12416(16) -0.0886(4) 0.8588(4) 0.0343(13) Uani 1 1 d . . .
H9 H 0.1134 -0.1516 0.8446 0.041 Uiso 1 1 calc R . .
C10 C 0.1292(2) -0.0270(4) 1.0198(4) 0.0435(15) Uani 1 1 d . . .
C11 C 0.09645(16) -0.0223(4) 0.6993(4) 0.0355(13) Uani 1 1 d . . .
H11A H 0.0846 -0.0844 0.6913 0.043 Uiso 1 1 calc R . .
H11B H 0.1066 -0.0035 0.6344 0.043 Uiso 1 1 calc R . .
C12 C 0.06450(19) -0.0487(5) 0.9526(4) 0.0486(16) Uani 1 1 d . . .
H12A H 0.0584 -0.0453 1.0236 0.058 Uiso 1 1 calc R . .
H12B H 0.0560 -0.1102 0.9279 0.058 Uiso 1 1 calc R . .
C13 C 0.06128(15) 0.1221(4) 0.6736(3) 0.0275(12) Uani 1 1 d . . .
C14 C 0.03433(16) 0.0235(4) 0.7946(4) 0.0364(13) Uani 1 1 d . . .
C15 C 0.00992(15) 0.1144(4) 0.7821(4) 0.0331(12) Uani 1 1 d . . .
C16 C 0.03323(16) 0.1071(5) 0.9446(4) 0.0405(14) Uani 1 1 d . . .
C17 C 0.0147(2) 0.2500 0.6516(5) 0.0321(17) Uani 1 2 d S . .
H17A H -0.0130 0.2500 0.6518 0.038 Uiso 1 2 calc SR . .
H17B H 0.0230 0.2500 0.5820 0.038 Uiso 1 2 calc SR . .
C18 C -0.0032(2) 0.2500 0.9085(6) 0.039(2) Uani 1 2 d S . .
H18A H -0.0290 0.2500 0.8825 0.047 Uiso 1 2 calc SR . .
H18B H -0.0048 0.2500 0.9813 0.047 Uiso 1 2 calc SR . .
C19 C 0.2577(3) 0.2500 1.1273(6) 0.045(2) Uani 1 2 d S . .
H19A H 0.2848 0.2500 1.1424 0.054 Uiso 1 2 calc SR . .
H19B H 0.2440 0.2500 1.1906 0.054 Uiso 1 2 calc SR . .
C20 C 0.2981(2) 0.2500 0.8867(7) 0.052(3) Uani 1 2 d S . .
H20A H 0.3208 0.2500 0.9285 0.063 Uiso 1 2 calc SR . .
H20B H 0.3062 0.2500 0.8170 0.063 Uiso 1 2 calc SR . .
C21 C 0.01610(19) -0.0699(5) 0.7629(5) 0.0539(17) Uani 1 1 d . . .
H21A H 0.0103 -0.0677 0.6924 0.081 Uiso 1 1 calc R . .
H21B H -0.0070 -0.0796 0.8004 0.081 Uiso 1 1 calc R . .
H21C H 0.0335 -0.1214 0.7759 0.081 Uiso 1 1 calc R . .
C22 C -0.03185(17) 0.0945(5) 0.7604(5) 0.0501(16) Uani 1 1 d . . .
H22A H -0.0430 0.0613 0.8163 0.075 Uiso 1 1 calc R . .
H22B H -0.0339 0.0559 0.7010 0.075 Uiso 1 1 calc R . .
H22C H -0.0451 0.1537 0.7501 0.075 Uiso 1 1 calc R . .
N1 N 0.27617(14) 0.1648(4) 0.9067(3) 0.0427(12) Uani 1 1 d . . .
N2 N 0.24248(14) 0.0344(4) 0.8762(3) 0.0413(12) Uani 1 1 d . . .
N3 N 0.24859(13) 0.1644(3) 1.0740(3) 0.0386(11) Uani 1 1 d . . .
N4 N 0.22242(14) 0.0235(3) 1.0505(3) 0.0391(11) Uani 1 1 d . . .
N5 N 0.18710(14) -0.0471(3) 0.8178(3) 0.0359(11) Uani 1 1 d . . .
N6 N 0.12732(14) -0.0306(3) 0.7687(3) 0.0375(11) Uani 1 1 d . . .
N7 N 0.16470(14) -0.0468(4) 0.9902(3) 0.0400(12) Uani 1 1 d . . .
N8 N 0.10480(14) -0.0419(3) 0.9406(3) 0.0374(11) Uani 1 1 d . . .
N9 N 0.06760(12) 0.0453(3) 0.7289(3) 0.0294(10) Uani 1 1 d . . .
N10 N 0.02790(12) 0.1631(3) 0.6987(3) 0.0295(10) Uani 1 1 d . . .
N11 N 0.04396(14) 0.0256(3) 0.9002(3) 0.0374(11) Uani 1 1 d . . .
N12 N 0.01568(13) 0.1634(3) 0.8764(3) 0.0357(11) Uani 1 1 d . . .
O1 O 0.25993(12) 0.1293(3) 0.7448(3) 0.0461(10) Uani 1 1 d . . .
O2 O 0.17531(11) 0.0218(3) 0.6648(3) 0.0389(9) Uani 1 1 d . . .
O3 O 0.08230(11) 0.1502(2) 0.6062(3) 0.0339(9) Uani 1 1 d . . .
O4 O 0.19548(12) 0.1261(3) 1.1649(3) 0.0498(11) Uani 1 1 d . . .
O5 O 0.11897(13) -0.0020(4) 1.1030(3) 0.0551(12) Uani 1 1 d . . .
O6 O 0.03867(12) 0.1257(3) 1.0335(3) 0.0491(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Dy1 2.337(4) . ?
O2W Dy1 2.380(5) . ?
O3W Dy1 2.458(6) . ?
O4W Dy1 2.372(4) . ?
Dy1 O3 2.318(3) 7_565 ?
Dy1 O3 2.318(3) . ?
Dy1 O1W 2.337(4) 7_565 ?
Dy1 O4W 2.372(4) 7_565 ?
N13 O7 1.214(11) . ?
N13 O8 1.229(10) . ?
N13 O9 1.286(12) . ?
N14 O12 1.190(11) . ?
N14 O11 1.217(10) . ?
N14 O10 1.230(10) . ?
C1 O1 1.219(7) . ?
C1 N1 1.371(7) . ?
C1 N2 1.374(8) . ?
C2 N1 1.446(7) . ?
C2 N3 1.456(7) . ?
C2 C3 1.558(9) . ?
C2 H2 0.9900 . ?
C3 N4 1.450(7) . ?
C3 N2 1.473(7) . ?
C3 H3 0.9900 . ?
C4 O4 1.241(7) . ?
C4 N4 1.354(7) . ?
C4 N3 1.370(8) . ?
C5 N5 1.438(7) . ?
C5 N2 1.443(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.429(8) . ?
C6 N7 1.471(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.225(6) . ?
C7 N6 1.372(7) . ?
C7 N5 1.381(7) . ?
C8 N5 1.444(7) . ?
C8 N7 1.459(6) . ?
C8 C9 1.544(8) . ?
C8 H8 0.9900 . ?
C9 N8 1.454(7) . ?
C9 N6 1.468(6) . ?
C9 H9 0.9900 . ?
C10 O5 1.227(7) . ?
C10 N7 1.348(8) . ?
C10 N8 1.386(8) . ?
C11 N6 1.440(7) . ?
C11 N9 1.454(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.438(8) . ?
C12 N11 1.460(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.237(6) . ?
C13 N9 1.337(6) . ?
C13 N10 1.359(7) . ?
C14 N11 1.459(7) . ?
C14 N9 1.503(7) . ?
C14 C21 1.532(8) . ?
C14 C15 1.559(8) . ?
C15 N12 1.459(7) . ?
C15 N10 1.463(6) . ?
C15 C22 1.532(8) . ?
C16 O6 1.238(7) . ?
C16 N11 1.354(8) . ?
C16 N12 1.364(7) . ?
C17 N10 1.460(6) . ?
C17 N10 1.460(6) 7_565 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.461(6) 7_565 ?
C18 N12 1.461(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.445(6) . ?
C19 N3 1.445(6) 7_565 ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.459(6) 7_565 ?
C20 N1 1.459(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

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
O3 Dy1 O3 75.12(17) 7_565 . ?
O3 Dy1 O1W 83.19(13) 7_565 7_565 ?
O3 Dy1 O1W 144.52(12) . 7_565 ?
O3 Dy1 O1W 144.52(12) 7_565 . ?
O3 Dy1 O1W 83.19(13) . . ?
O1W Dy1 O1W 99.9(2) 7_565 . ?
O3 Dy1 O4W 115.18(15) 7_565 . ?
O3 Dy1 O4W 70.47(14) . . ?
O1W Dy1 O4W 144.98(13) 7_565 . ?
O1W Dy1 O4W 82.26(15) . . ?
O3 Dy1 O4W 70.47(13) 7_565 7_565 ?
O3 Dy1 O4W 115.18(15) . 7_565 ?
O1W Dy1 O4W 82.26(15) 7_565 7_565 ?
O1W Dy1 O4W 144.98(13) . 7_565 ?
O4W Dy1 O4W 77.1(2) . 7_565 ?
O3 Dy1 O2W 74.57(14) 7_565 . ?
O3 Dy1 O2W 74.57(14) . . ?
O1W Dy1 O2W 72.76(12) 7_565 . ?
O1W Dy1 O2W 72.76(12) . . ?
O4W Dy1 O2W 138.94(11) . . ?
O4W Dy1 O2W 138.94(11) 7_565 . ?
O3 Dy1 O3W 139.74(10) 7_565 . ?
O3 Dy1 O3W 139.74(10) . . ?
O1W Dy1 O3W 72.84(12) 7_565 . ?
O1W Dy1 O3W 72.84(12) . . ?
O4W Dy1 O3W 74.55(15) . . ?
O4W Dy1 O3W 74.55(15) 7_565 . ?
O2W Dy1 O3W 125.3(2) . . ?
O7 N13 O8 122.4(11) . . ?
O7 N13 O9 121.2(10) . . ?
O8 N13 O9 116.4(10) . . ?
O12 N14 O11 117.2(10) . . ?
O12 N14 O10 119.0(10) . . ?
O11 N14 O10 123.8(8) . . ?
O1 C1 N1 125.7(6) . . ?
O1 C1 N2 125.1(6) . . ?
N1 C1 N2 109.1(5) . . ?
N1 C2 N3 115.3(5) . . ?
N1 C2 C3 104.0(4) . . ?
N3 C2 C3 102.7(5) . . ?
N1 C2 H2 111.4 . . ?
N3 C2 H2 111.4 . . ?
C3 C2 H2 111.4 . . ?
N4 C3 N2 114.1(5) . . ?
N4 C3 C2 103.5(5) . . ?
N2 C3 C2 102.6(5) . . ?
N4 C3 H3 112.0 . . ?
N2 C3 H3 112.0 . . ?
C2 C3 H3 112.0 . . ?
O4 C4 N4 126.8(6) . . ?
O4 C4 N3 123.9(6) . . ?
N4 C4 N3 109.3(5) . . ?
N5 C5 N2 113.2(5) . . ?
N5 C5 H5A 108.9 . . ?
N2 C5 H5A 108.9 . . ?
N5 C5 H5B 108.9 . . ?
N2 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N4 C6 N7 112.6(5) . . ?
N4 C6 H6A 109.1 . . ?
N7 C6 H6A 109.1 . . ?
N4 C6 H6B 109.1 . . ?
N7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 N6 126.5(5) . . ?
O2 C7 N5 125.1(5) . . ?
N6 C7 N5 108.1(5) . . ?
N5 C8 N7 115.0(5) . . ?
N5 C8 C9 104.8(4) . . ?
N7 C8 C9 103.0(4) . . ?
N5 C8 H8 111.2 . . ?
N7 C8 H8 111.2 . . ?
C9 C8 H8 111.2 . . ?
N8 C9 N6 113.9(4) . . ?
N8 C9 C8 104.0(4) . . ?
N6 C9 C8 102.3(4) . . ?
N8 C9 H9 112.0 . . ?
N6 C9 H9 112.0 . . ?
C8 C9 H9 112.0 . . ?
O5 C10 N7 127.1(6) . . ?
O5 C10 N8 124.1(6) . . ?
N7 C10 N8 108.7(5) . . ?
N6 C11 N9 114.1(4) . . ?
N6 C11 H11A 108.7 . . ?
N9 C11 H11A 108.7 . . ?
N6 C11 H11B 108.7 . . ?
N9 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N8 C12 N11 113.0(5) . . ?
N8 C12 H12A 109.0 . . ?
N11 C12 H12A 109.0 . . ?
N8 C12 H12B 109.0 . . ?
N11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N9 124.7(5) . . ?
O3 C13 N10 124.5(5) . . ?
N9 C13 N10 110.8(4) . . ?
N11 C14 N9 112.6(4) . . ?
N11 C14 C21 112.7(5) . . ?
N9 C14 C21 110.1(4) . . ?
N11 C14 C15 102.6(4) . . ?
N9 C14 C15 101.6(4) . . ?
C21 C14 C15 116.7(5) . . ?
N12 C15 N10 112.3(4) . . ?
N12 C15 C22 112.8(5) . . ?
N10 C15 C22 111.1(4) . . ?
N12 C15 C14 102.8(4) . . ?
N10 C15 C14 103.4(4) . . ?
C22 C15 C14 113.8(5) . . ?
O6 C16 N11 124.3(6) . . ?
O6 C16 N12 126.4(6) . . ?
N11 C16 N12 109.2(5) . . ?
N10 C17 N10 114.9(6) . 7_565 ?
N10 C17 H17A 108.5 . . ?
N10 C17 H17A 108.5 7_565 . ?
N10 C17 H17B 108.5 . . ?
N10 C17 H17B 108.5 7_565 . ?
H17A C17 H17B 107.5 . . ?
N12 C18 N12 114.2(6) 7_565 . ?
N12 C18 H18A 108.7 7_565 . ?
N12 C18 H18A 108.7 . . ?
N12 C18 H18B 108.7 7_565 . ?
N12 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
N3 C19 N3 114.2(6) . 7_565 ?
N3 C19 H19A 108.7 . . ?
N3 C19 H19A 108.7 7_565 . ?
N3 C19 H19B 108.7 . . ?
N3 C19 H19B 108.7 7_565 . ?
H19A C19 H19B 107.6 . . ?
N1 C20 N1 111.6(7) 7_565 . ?
N1 C20 H20A 109.3 7_565 . ?
N1 C20 H20A 109.3 . . ?
N1 C20 H20B 109.3 7_565 . ?
N1 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C2 112.0(5) . . ?
C1 N1 C20 123.4(6) . . ?
C2 N1 C20 124.0(6) . . ?
C1 N2 C5 121.1(5) . . ?
C1 N2 C3 111.1(5) . . ?
C5 N2 C3 124.3(5) . . ?
C4 N3 C19 122.9(5) . . ?
C4 N3 C2 111.9(5) . . ?
C19 N3 C2 123.6(6) . . ?
C4 N4 C6 122.7(5) . . ?
C4 N4 C3 112.2(5) . . ?
C6 N4 C3 125.1(5) . . ?
C7 N5 C5 123.5(5) . . ?
C7 N5 C8 111.9(5) . . ?
C5 N5 C8 124.5(5) . . ?
C7 N6 C11 122.9(4) . . ?
C7 N6 C9 112.6(4) . . ?
C11 N6 C9 121.5(5) . . ?
C10 N7 C8 112.3(5) . . ?
C10 N7 C6 121.2(5) . . ?
C8 N7 C6 122.8(5) . . ?
C10 N8 C12 122.7(5) . . ?
C10 N8 C9 110.9(5) . . ?
C12 N8 C9 121.4(5) . . ?
C13 N9 C11 120.1(4) . . ?
C13 N9 C14 111.3(4) . . ?
C11 N9 C14 125.1(4) . . ?
C13 N10 C17 122.0(5) . . ?
C13 N10 C15 111.5(4) . . ?
C17 N10 C15 126.3(5) . . ?
C16 N11 C14 112.4(5) . . ?
C16 N11 C12 122.7(5) . . ?
C14 N11 C12 124.8(5) . . ?
C16 N12 C15 111.6(5) . . ?
C16 N12 C18 120.0(5) . . ?
C15 N12 C18 126.3(5) . . ?
C13 O3 Dy1 161.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.769
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.103

# 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 0.149 0.500 796 299 ' '
2 0.500 0.079 0.000 797 299 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997815'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_11Ho
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Ho N24 O18, 2(N O3), Cl, 16(H2 O)'
_chemical_formula_sum            'C40 H88 Cl Ho N26 O40'
_chemical_formula_weight         1773.74

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.361(5)
_cell_length_b                   14.168(2)
_cell_length_c                   13.4332(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6729.9(16)
_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          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3656
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_T_max  0.7484
_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            45795
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         25.99
_reflns_number_total             6754
_reflns_number_gt                4771
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0725P)²+17.4381P] 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         6754
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1540
_refine_ls_wR_factor_gt          0.1438
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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 0.2349(2) -0.2500 0.0914(6) 0.205(3) Uani 1 2 d S . .
O5W O 0.2746(2) 0.2500 0.3795(6) 0.077(2) Uani 1 2 d S . .
O1W O 0.35035(17) 0.2500 0.3452(4) 0.0421(14) Uani 1 2 d S . .
O2W O 0.34192(12) 0.1244(3) 0.5023(3) 0.0417(10) Uani 1 1 d . . .
O3W O 0.35539(17) 0.2500 0.6630(4) 0.0417(14) Uani 1 2 d S . .
O4W O 0.42128(14) 0.1456(3) 0.5933(3) 0.0530(12) Uani 1 1 d . . .
Ho1 Ho 0.384158(10) 0.2500 0.49721(2) 0.02834(14) Uani 1 2 d S . .
N13 N 0.3833(3) -0.2500 -0.0833(7) 0.055(2) Uani 1 2 d S . .
N14 N 0.3668(3) -0.2500 0.3339(6) 0.050(2) Uani 1 2 d SD . .
O7 O 0.3995(4) -0.2500 -0.0028(6) 0.097(3) Uani 1 2 d S . .
O8 O 0.4013(2) -0.2500 -0.1629(6) 0.086(3) Uani 1 2 d S . .
O9 O 0.3471(3) -0.2500 -0.0898(9) 0.114(4) Uani 1 2 d S . .
O10 O 0.4011(2) -0.2500 0.3109(5) 0.0517(16) Uani 1 2 d SD . .
O11 O 0.3419(2) -0.2500 0.2734(6) 0.079(2) Uani 1 2 d SD . .
O12 O 0.3586(3) -0.2500 0.4196(7) 0.216(10) Uani 1 2 d SD . .
C1 C 0.24045(17) 0.1125(5) 0.1660(5) 0.0421(15) Uani 1 1 d . . .
C2 C 0.22603(17) 0.1194(5) -0.0033(4) 0.0422(15) Uani 1 1 d . . .
H2 H 0.2006 0.1095 -0.0323 0.051 Uiso 1 1 calc R . .
C3 C 0.24592(18) 0.0241(5) 0.0185(4) 0.0421(15) Uani 1 1 d . . .
H3 H 0.2287 -0.0303 0.0087 0.050 Uiso 1 1 calc R . .
C4 C 0.28047(18) 0.1063(5) -0.1012(4) 0.0418(15) Uani 1 1 d . . .
C5 C 0.27219(17) -0.0410(4) 0.1840(4) 0.0409(15) Uani 1 1 d . . .
H5A H 0.2615 -0.1011 0.1612 0.049 Uiso 1 1 calc R . .
H5B H 0.2639 -0.0311 0.2528 0.049 Uiso 1 1 calc R . .
C6 C 0.30386(19) -0.0515(4) -0.0620(4) 0.0430(15) Uani 1 1 d . . .
H6A H 0.3143 -0.0502 -0.1295 0.052 Uiso 1 1 calc R . .
H6B H 0.2906 -0.1118 -0.0535 0.052 Uiso 1 1 calc R . .
C7 C 0.33557(17) -0.0120(4) 0.2564(4) 0.0337(13) Uani 1 1 d . . .
C8 C 0.33418(17) -0.0946(4) 0.1054(4) 0.0349(14) Uani 1 1 d . . .
H8 H 0.3261 -0.1611 0.0981 0.042 Uiso 1 1 calc R . .
C9 C 0.37535(18) -0.0877(4) 0.1411(4) 0.0375(14) Uani 1 1 d . . .
H9 H 0.3861 -0.1508 0.1553 0.045 Uiso 1 1 calc R . .
C10 C 0.3710(2) -0.0268(4) -0.0201(4) 0.0417(15) Uani 1 1 d . . .
C11 C 0.40345(17) -0.0220(4) 0.3004(4) 0.0351(13) Uani 1 1 d . . .
H11A H 0.4154 -0.0840 0.3085 0.042 Uiso 1 1 calc R . .
H11B H 0.3933 -0.0032 0.3654 0.042 Uiso 1 1 calc R . .
C12 C 0.4358(2) -0.0489(5) 0.0475(4) 0.0468(16) Uani 1 1 d . . .
H12A H 0.4420 -0.0453 -0.0235 0.056 Uiso 1 1 calc R . .
H12B H 0.4442 -0.1105 0.0722 0.056 Uiso 1 1 calc R . .
C13 C 0.43864(16) 0.1226(4) 0.3263(4) 0.0279(12) Uani 1 1 d . . .
C14 C 0.46517(17) 0.0242(4) 0.2059(4) 0.0348(13) Uani 1 1 d . . .
C15 C 0.48981(16) 0.1139(4) 0.2175(4) 0.0330(13) Uani 1 1 d . . .
C16 C 0.46683(17) 0.1071(5) 0.0547(4) 0.0412(15) Uani 1 1 d . . .
C17 C 0.4854(2) 0.2500 0.3483(5) 0.0325(18) Uani 1 2 d S . .
H17A H 0.4772 0.2500 0.4180 0.039 Uiso 1 2 calc SR . .
H17B H 0.5131 0.2500 0.3478 0.039 Uiso 1 2 calc SR . .
C18 C 0.5034(3) 0.2500 0.0918(6) 0.038(2) Uani 1 2 d S . .
H18A H 0.5290 0.2500 0.1194 0.046 Uiso 1 2 calc SR . .
H18B H 0.5056 0.2500 0.0191 0.046 Uiso 1 2 calc SR . .
C19 C 0.2425(3) 0.2500 -0.1290(6) 0.043(2) Uani 1 2 d S . .
H19A H 0.2568 0.2500 -0.1915 0.052 Uiso 1 2 calc SR . .
H19B H 0.2155 0.2500 -0.1457 0.052 Uiso 1 2 calc SR . .
C20 C 0.2021(3) 0.2500 0.1126(7) 0.052(3) Uani 1 2 d S . .
H20A H 0.1944 0.2500 0.1826 0.063 Uiso 1 2 calc SR . .
H20B H 0.1792 0.2500 0.0717 0.063 Uiso 1 2 calc SR . .
C21 C 0.4838(2) -0.0695(5) 0.2375(5) 0.0559(19) Uani 1 1 d . . .
H21A H 0.4894 -0.0676 0.3082 0.084 Uiso 1 1 calc R . .
H21B H 0.5070 -0.0784 0.2004 0.084 Uiso 1 1 calc R . .
H21C H 0.4666 -0.1213 0.2238 0.084 Uiso 1 1 calc R . .
C22 C 0.53195(18) 0.0951(5) 0.2394(5) 0.0512(17) Uani 1 1 d . . .
H22A H 0.5432 0.0622 0.1834 0.077 Uiso 1 1 calc R . .
H22B H 0.5342 0.0566 0.2988 0.077 Uiso 1 1 calc R . .
H22C H 0.5449 0.1546 0.2497 0.077 Uiso 1 1 calc R . .
N1 N 0.22369(14) 0.1656(4) 0.0920(3) 0.0411(12) Uani 1 1 d . . .
N2 N 0.25746(14) 0.0341(4) 0.1227(3) 0.0402(12) Uani 1 1 d . . .
N3 N 0.25127(14) 0.1644(4) -0.0741(3) 0.0372(11) Uani 1 1 d . . .
N4 N 0.27752(14) 0.0230(4) -0.0516(3) 0.0382(12) Uani 1 1 d . . .
N5 N 0.31297(14) -0.0472(3) 0.1818(3) 0.0356(11) Uani 1 1 d . . .
N6 N 0.37250(14) -0.0307(3) 0.2311(3) 0.0363(11) Uani 1 1 d . . .
N7 N 0.33497(15) -0.0465(4) 0.0097(3) 0.0392(12) Uani 1 1 d . . .
N8 N 0.39507(14) -0.0416(3) 0.0594(3) 0.0371(12) Uani 1 1 d . . .
N9 N 0.43224(13) 0.0457(3) 0.2708(3) 0.0286(10) Uani 1 1 d . . .
N10 N 0.47207(13) 0.1638(3) 0.3011(3) 0.0302(10) Uani 1 1 d . . .
N11 N 0.45613(14) 0.0252(3) 0.1005(3) 0.0357(11) Uani 1 1 d . . .
N12 N 0.48406(13) 0.1631(3) 0.1231(3) 0.0357(11) Uani 1 1 d . . .
O1 O 0.23983(13) 0.1299(3) 0.2547(3) 0.0473(11) Uani 1 1 d . . .
O2 O 0.32442(11) 0.0223(3) 0.3343(3) 0.0391(10) Uani 1 1 d . . .
O3 O 0.41754(11) 0.1507(3) 0.3932(3) 0.0339(9) Uani 1 1 d . . .
O4 O 0.30439(13) 0.1265(3) -0.1652(3) 0.0479(11) Uani 1 1 d . . .
O5 O 0.38100(13) -0.0016(4) -0.1026(3) 0.0574(13) Uani 1 1 d . . .
O6 O 0.46126(13) 0.1259(3) -0.0336(3) 0.0501(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Ho1 2.366(5) . ?
O2W Ho1 2.325(4) . ?
O3W Ho1 2.449(5) . ?
O4W Ho1 2.362(4) . ?
Ho1 O3 2.307(3) . ?
Ho1 O3 2.307(3) 7_565 ?
Ho1 O2W 2.325(4) 7_565 ?
Ho1 O4W 2.362(4) 7_565 ?
N13 O7 1.223(12) . ?
N13 O8 1.243(11) . ?
N13 O9 1.282(12) . ?
N14 O12 1.186(11) . ?
N14 O11 1.197(10) . ?
N14 O10 1.251(10) . ?
C1 O1 1.217(7) . ?
C1 N1 1.380(8) . ?
C1 N2 1.391(8) . ?
C2 N1 1.440(7) . ?
C2 N3 1.452(7) . ?
C2 C3 1.550(10) . ?
C2 H2 0.9900 . ?
C3 N4 1.462(8) . ?
C3 N2 1.465(7) . ?
C3 H3 0.9900 . ?
C4 O4 1.240(7) . ?
C4 N4 1.359(8) . ?
C4 N3 1.370(8) . ?
C5 N2 1.442(7) . ?
C5 N5 1.445(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.415(8) . ?
C6 N7 1.464(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.220(6) . ?
C7 N5 1.375(7) . ?
C7 N6 1.375(7) . ?
C8 N5 1.438(7) . ?
C8 N7 1.454(7) . ?
C8 C9 1.536(8) . ?
C8 H8 0.9900 . ?
C9 N8 1.455(7) . ?
C9 N6 1.458(7) . ?
C9 H9 0.9900 . ?
C10 O5 1.217(7) . ?
C10 N7 1.364(9) . ?
C10 N8 1.382(8) . ?
C11 N6 1.442(7) . ?
C11 N9 1.454(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.452(8) . ?
C12 N11 1.458(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.234(6) . ?
C13 N9 1.339(6) . ?
C13 N10 1.362(7) . ?
C14 N11 1.452(7) . ?
C14 N9 1.486(7) . ?
C14 C21 1.540(8) . ?
C14 C15 1.550(8) . ?
C15 N12 1.462(7) . ?
C15 N10 1.467(6) . ?
C15 C22 1.542(8) . ?
C16 O6 1.232(7) . ?
C16 N12 1.358(7) . ?
C16 N11 1.366(8) . ?
C17 N10 1.454(6) 7_565 ?
C17 N10 1.454(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.469(6) 7_565 ?
C18 N12 1.469(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.453(6) 7_565 ?
C19 N3 1.453(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.445(7) . ?
C20 N1 1.445(7) 7_565 ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

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
O3 Ho1 O3 75.12(18) . 7_565 ?
O3 Ho1 O2W 83.10(14) . . ?
O3 Ho1 O2W 144.42(13) 7_565 . ?
O3 Ho1 O2W 144.42(13) . 7_565 ?
O3 Ho1 O2W 83.10(14) 7_565 7_565 ?
O2W Ho1 O2W 99.9(2) . 7_565 ?
O3 Ho1 O4W 115.36(16) . 7_565 ?
O3 Ho1 O4W 70.42(14) 7_565 7_565 ?
O2W Ho1 O4W 145.14(13) . 7_565 ?
O2W Ho1 O4W 82.04(16) 7_565 7_565 ?
O3 Ho1 O4W 70.42(14) . . ?
O3 Ho1 O4W 115.36(16) 7_565 . ?
O2W Ho1 O4W 82.04(16) . . ?
O2W Ho1 O4W 145.14(13) 7_565 . ?
O4W Ho1 O4W 77.5(2) 7_565 . ?
O3 Ho1 O1W 74.69(14) . . ?
O3 Ho1 O1W 74.69(14) 7_565 . ?
O2W Ho1 O1W 72.59(13) . . ?
O2W Ho1 O1W 72.59(13) 7_565 . ?
O4W Ho1 O1W 138.82(11) 7_565 . ?
O4W Ho1 O1W 138.82(11) . . ?
O3 Ho1 O3W 139.76(10) . . ?
O3 Ho1 O3W 139.76(10) 7_565 . ?
O2W Ho1 O3W 72.92(12) . . ?
O2W Ho1 O3W 72.92(12) 7_565 . ?
O4W Ho1 O3W 74.55(15) 7_565 . ?
O4W Ho1 O3W 74.55(15) . . ?
O1W Ho1 O3W 125.1(2) . . ?
O7 N13 O8 121.4(11) . . ?
O7 N13 O9 121.8(10) . . ?
O8 N13 O9 116.8(10) . . ?
O12 N14 O11 118.7(10) . . ?
O12 N14 O10 118.3(10) . . ?
O11 N14 O10 123.0(9) . . ?
O1 C1 N1 126.0(6) . . ?
O1 C1 N2 125.3(6) . . ?
N1 C1 N2 108.7(5) . . ?
N1 C2 N3 114.7(5) . . ?
N1 C2 C3 104.7(5) . . ?
N3 C2 C3 103.2(5) . . ?
N1 C2 H2 111.3 . . ?
N3 C2 H2 111.3 . . ?
C3 C2 H2 111.3 . . ?
N4 C3 N2 113.8(5) . . ?
N4 C3 C2 103.5(5) . . ?
N2 C3 C2 102.9(5) . . ?
N4 C3 H3 112.0 . . ?
N2 C3 H3 112.0 . . ?
C2 C3 H3 112.0 . . ?
O4 C4 N4 126.4(6) . . ?
O4 C4 N3 124.0(6) . . ?
N4 C4 N3 109.5(5) . . ?
N2 C5 N5 113.2(5) . . ?
N2 C5 H5A 108.9 . . ?
N5 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
N5 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
N4 C6 N7 113.2(5) . . ?
N4 C6 H6A 108.9 . . ?
N7 C6 H6A 108.9 . . ?
N4 C6 H6B 108.9 . . ?
N7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 N5 125.6(5) . . ?
O2 C7 N6 126.5(5) . . ?
N5 C7 N6 107.6(5) . . ?
N5 C8 N7 115.0(5) . . ?
N5 C8 C9 104.0(4) . . ?
N7 C8 C9 103.2(5) . . ?
N5 C8 H8 111.4 . . ?
N7 C8 H8 111.4 . . ?
C9 C8 H8 111.4 . . ?
N8 C9 N6 114.2(5) . . ?
N8 C9 C8 104.3(5) . . ?
N6 C9 C8 103.2(5) . . ?
N8 C9 H9 111.5 . . ?
N6 C9 H9 111.5 . . ?
C8 C9 H9 111.5 . . ?
O5 C10 N7 126.8(6) . . ?
O5 C10 N8 124.7(7) . . ?
N7 C10 N8 108.5(5) . . ?
N6 C11 N9 114.3(4) . . ?
N6 C11 H11A 108.7 . . ?
N9 C11 H11A 108.7 . . ?
N6 C11 H11B 108.7 . . ?
N9 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N8 C12 N11 112.6(5) . . ?
N8 C12 H12A 109.1 . . ?
N11 C12 H12A 109.1 . . ?
N8 C12 H12B 109.1 . . ?
N11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N9 124.5(5) . . ?
O3 C13 N10 124.6(5) . . ?
N9 C13 N10 110.9(5) . . ?
N11 C14 N9 113.4(5) . . ?
N11 C14 C21 111.8(5) . . ?
N9 C14 C21 110.5(5) . . ?
N11 C14 C15 102.3(4) . . ?
N9 C14 C15 102.3(4) . . ?
C21 C14 C15 116.1(5) . . ?
N12 C15 N10 112.0(4) . . ?
N12 C15 C22 112.5(5) . . ?
N10 C15 C22 110.6(4) . . ?
N12 C15 C14 103.0(4) . . ?
N10 C15 C14 103.4(4) . . ?
C22 C15 C14 114.9(5) . . ?
O6 C16 N12 126.6(6) . . ?
O6 C16 N11 124.9(6) . . ?
N12 C16 N11 108.4(5) . . ?
N10 C17 N10 114.2(6) 7_565 . ?
N10 C17 H17A 108.7 7_565 . ?
N10 C17 H17A 108.7 . . ?
N10 C17 H17B 108.7 7_565 . ?
N10 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N12 C18 N12 113.8(6) 7_565 . ?
N12 C18 H18A 108.8 7_565 . ?
N12 C18 H18A 108.8 . . ?
N12 C18 H18B 108.8 7_565 . ?
N12 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
N3 C19 N3 113.2(6) 7_565 . ?
N3 C19 H19A 108.9 7_565 . ?
N3 C19 H19A 108.9 . . ?
N3 C19 H19B 108.9 7_565 . ?
N3 C19 H19B 108.9 . . ?
H19A C19 H19B 107.8 . . ?
N1 C20 N1 111.8(7) . 7_565 ?
N1 C20 H20A 109.3 . . ?
N1 C20 H20A 109.3 7_565 . ?
N1 C20 H20B 109.3 . . ?
N1 C20 H20B 109.3 7_565 . ?
H20A C20 H20B 107.9 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 H22A 109.5 . . ?
C15 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C15 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C2 111.6(5) . . ?
C1 N1 C20 122.7(6) . . ?
C2 N1 C20 125.2(6) . . ?
C1 N2 C5 120.5(5) . . ?
C1 N2 C3 110.8(5) . . ?
C5 N2 C3 125.1(5) . . ?
C4 N3 C2 111.9(5) . . ?
C4 N3 C19 121.9(5) . . ?
C2 N3 C19 124.6(6) . . ?
C4 N4 C6 123.3(5) . . ?
C4 N4 C3 111.4(5) . . ?
C6 N4 C3 125.1(5) . . ?
C7 N5 C8 112.7(5) . . ?
C7 N5 C5 122.9(5) . . ?
C8 N5 C5 124.3(5) . . ?
C7 N6 C11 123.0(4) . . ?
C7 N6 C9 112.1(5) . . ?
C11 N6 C9 122.0(5) . . ?
C10 N7 C8 111.9(5) . . ?
C10 N7 C6 121.2(5) . . ?
C8 N7 C6 123.0(5) . . ?
C10 N8 C12 122.4(5) . . ?
C10 N8 C9 110.8(5) . . ?
C12 N8 C9 121.8(5) . . ?
C13 N9 C11 120.1(4) . . ?
C13 N9 C14 111.2(4) . . ?
C11 N9 C14 125.0(4) . . ?
C13 N10 C17 122.2(5) . . ?
C13 N10 C15 110.8(4) . . ?
C17 N10 C15 126.8(5) . . ?
C16 N11 C14 112.7(5) . . ?
C16 N11 C12 121.9(5) . . ?
C14 N11 C12 125.3(5) . . ?
C16 N12 C15 111.8(5) . . ?
C16 N12 C18 120.3(5) . . ?
C15 N12 C18 125.6(5) . . ?
C13 O3 Ho1 161.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.782
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.109


# 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 -0.002 0.000 804 291 ' '
2 0.500 0.150 -0.500 804 291 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997816'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_12Er
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Er N24 O18, 2(N O3), Cl, 15(H2 O)'
_chemical_formula_sum            'C40 H86 Cl Er N26 O39'
_chemical_formula_weight         1758.06

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.370(4)
_cell_length_b                   14.1610(17)
_cell_length_c                   13.4086(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6716.0(14)
_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          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3620
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7107
_exptl_absorpt_correction_T_max  0.7562
_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            45017
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6300
_reflns_number_gt                4915
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0415P)²+38.0632P] 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         6300
_refine_ls_number_parameters     442
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1396
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_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
O5W O 0.2253(2) 0.2500 0.3791(6) 0.068(2) Uiso 1 2 d S . .
Cl1 Cl 0.2657(3) -0.2500 0.0910(7) 0.211(4) Uani 1 2 d S . .
O1W O 0.15786(13) 0.1252(3) 0.5025(3) 0.0405(10) Uani 1 1 d . . .
O2W O 0.14950(18) 0.2500 0.3452(4) 0.0399(15) Uani 1 2 d S . .
O3W O 0.14428(19) 0.2500 0.6620(4) 0.0421(16) Uani 1 2 d S . .
O4W O 0.07859(15) 0.1465(4) 0.5927(3) 0.0551(14) Uani 1 1 d . . .
Er1 Er 0.115562(11) 0.2500 0.49689(3) 0.02847(13) Uani 1 2 d S . .
N13 N 0.1169(3) -0.2500 -0.0854(7) 0.052(2) Uani 1 2 d S . .
N14 N 0.1328(3) -0.2500 0.3345(7) 0.047(2) Uani 1 2 d SD . .
O7 O 0.1013(4) -0.2500 -0.0035(7) 0.098(3) Uani 1 2 d S . .
O8 O 0.0989(3) -0.2500 -0.1626(7) 0.088(3) Uani 1 2 d S . .
O9 O 0.1520(3) -0.2500 -0.0894(10) 0.114(4) Uani 1 2 d S . .
O10 O 0.0987(2) -0.2500 0.3108(6) 0.0507(18) Uani 1 2 d SD . .
O11 O 0.1412(3) -0.2500 0.4192(8) 0.216(11) Uani 1 2 d SD . .
O12 O 0.1584(2) -0.2500 0.2729(6) 0.074(2) Uani 1 2 d SD . .
C1 C 0.06125(17) 0.1224(4) 0.3268(4) 0.0281(13) Uani 1 1 d . . .
C2 C 0.00993(18) 0.1143(4) 0.2177(4) 0.0331(14) Uani 1 1 d . . .
C3 C 0.03476(18) 0.0239(4) 0.2059(4) 0.0351(14) Uani 1 1 d . . .
C4 C 0.03323(18) 0.1071(5) 0.0553(5) 0.0398(16) Uani 1 1 d . . .
C5 C 0.09642(18) -0.0222(4) 0.3003(4) 0.0358(14) Uani 1 1 d . . .
H5A H 0.1064 -0.0040 0.3657 0.043 Uiso 1 1 calc R . .
H5B H 0.0844 -0.0842 0.3076 0.043 Uiso 1 1 calc R . .
C6 C 0.0647(2) -0.0483(5) 0.0477(5) 0.0443(17) Uani 1 1 d . . .
H6A H 0.0563 -0.1100 0.0724 0.053 Uiso 1 1 calc R . .
H6B H 0.0585 -0.0449 -0.0235 0.053 Uiso 1 1 calc R . .
C7 C 0.16449(19) -0.0122(4) 0.2571(5) 0.0342(14) Uani 1 1 d . . .
C8 C 0.12462(18) -0.0879(4) 0.1415(4) 0.0344(14) Uani 1 1 d . . .
H8 H 0.1138 -0.1509 0.1558 0.041 Uiso 1 1 calc R . .
C9 C 0.16596(19) -0.0950(4) 0.1052(4) 0.0360(15) Uani 1 1 d . . .
H9 H 0.1742 -0.1615 0.0981 0.043 Uiso 1 1 calc R . .
C10 C 0.1292(2) -0.0271(5) -0.0199(4) 0.0404(16) Uani 1 1 d . . .
C11 C 0.22802(18) -0.0409(5) 0.1838(5) 0.0401(16) Uani 1 1 d . . .
H11A H 0.2363 -0.0317 0.2529 0.048 Uiso 1 1 calc R . .
H11B H 0.2385 -0.1011 0.1605 0.048 Uiso 1 1 calc R . .
C12 C 0.1960(2) -0.0519(5) -0.0618(5) 0.0412(16) Uani 1 1 d . . .
H12A H 0.2092 -0.1123 -0.0536 0.049 Uiso 1 1 calc R . .
H12B H 0.1856 -0.0502 -0.1294 0.049 Uiso 1 1 calc R . .
C13 C 0.25959(17) 0.1122(5) 0.1672(5) 0.0389(16) Uani 1 1 d . . .
C14 C 0.2538(2) 0.0235(5) 0.0185(4) 0.0424(16) Uani 1 1 d . . .
H14 H 0.2709 -0.0311 0.0084 0.051 Uiso 1 1 calc R . .
C15 C 0.27395(18) 0.1188(5) -0.0039(5) 0.0420(16) Uani 1 1 d . . .
H15 H 0.2993 0.1085 -0.0330 0.050 Uiso 1 1 calc R . .
C16 C 0.2199(2) 0.1072(5) -0.1012(5) 0.0395(16) Uani 1 1 d . . .
C17 C 0.2979(3) 0.2500 0.1128(7) 0.051(3) Uani 1 2 d S . .
H17A H 0.3207 0.2500 0.0713 0.062 Uiso 1 2 calc SR . .
H17B H 0.3059 0.2500 0.1828 0.062 Uiso 1 2 calc SR . .
C18 C 0.2579(3) 0.2500 -0.1283(7) 0.043(2) Uani 1 2 d S . .
H18A H 0.2439 0.2500 -0.1914 0.052 Uiso 1 2 calc SR . .
H18B H 0.2849 0.2500 -0.1442 0.052 Uiso 1 2 calc SR . .
C19 C -0.0033(3) 0.2500 0.0922(7) 0.039(2) Uani 1 2 d S . .
H19A H -0.0057 0.2500 0.0193 0.047 Uiso 1 2 calc SR . .
H19B H -0.0289 0.2500 0.1201 0.047 Uiso 1 2 calc SR . .
C20 C 0.0147(3) 0.2500 0.3484(6) 0.032(2) Uani 1 2 d S . .
H20A H 0.0231 0.2500 0.4181 0.039 Uiso 1 2 calc SR . .
H20B H -0.0130 0.2500 0.3484 0.039 Uiso 1 2 calc SR . .
C21 C -0.03161(19) 0.0951(6) 0.2391(5) 0.0510(19) Uani 1 1 d . . .
H21A H -0.0428 0.0624 0.1829 0.061 Uiso 1 1 calc R . .
H21B H -0.0447 0.1545 0.2498 0.061 Uiso 1 1 calc R . .
H21C H -0.0338 0.0563 0.2985 0.061 Uiso 1 1 calc R . .
C22 C 0.0165(2) -0.0697(5) 0.2378(6) 0.0522(19) Uani 1 1 d . . .
H22A H 0.0107 -0.0676 0.3085 0.063 Uiso 1 1 calc R . .
H22B H 0.0338 -0.1213 0.2246 0.063 Uiso 1 1 calc R . .
H22C H -0.0067 -0.0793 0.2004 0.063 Uiso 1 1 calc R . .
N1 N 0.02790(14) 0.1639(3) 0.3010(3) 0.0294(11) Uani 1 1 d . . .
N2 N 0.06787(14) 0.0459(3) 0.2705(3) 0.0279(11) Uani 1 1 d . . .
N3 N 0.01575(15) 0.1632(4) 0.1227(4) 0.0359(12) Uani 1 1 d . . .
N4 N 0.04403(15) 0.0255(4) 0.1003(4) 0.0363(12) Uani 1 1 d . . .
N5 N 0.12756(15) -0.0306(4) 0.2314(3) 0.0360(12) Uani 1 1 d . . .
N6 N 0.18724(15) -0.0463(3) 0.1817(4) 0.0338(12) Uani 1 1 d . . .
N7 N 0.10510(15) -0.0416(4) 0.0593(4) 0.0368(13) Uani 1 1 d . . .
N8 N 0.16499(15) -0.0470(4) 0.0101(4) 0.0389(13) Uani 1 1 d . . .
N9 N 0.24299(16) 0.0343(4) 0.1234(4) 0.0396(13) Uani 1 1 d . . .
N10 N 0.27639(15) 0.1648(4) 0.0930(4) 0.0401(13) Uani 1 1 d . . .
N11 N 0.22261(15) 0.0230(4) -0.0512(4) 0.0385(13) Uani 1 1 d . . .
N12 N 0.24890(15) 0.1644(4) -0.0740(4) 0.0373(12) Uani 1 1 d . . .
O1 O 0.08241(12) 0.1509(3) 0.3936(3) 0.0338(10) Uani 1 1 d . . .
O2 O 0.17550(12) 0.0227(3) 0.3350(3) 0.0358(10) Uani 1 1 d . . .
O3 O 0.26024(13) 0.1297(3) 0.2552(3) 0.0443(11) Uani 1 1 d . . .
O4 O 0.03863(14) 0.1258(4) -0.0336(3) 0.0485(12) Uani 1 1 d . . .
O5 O 0.11927(15) -0.0021(4) -0.1031(3) 0.0565(14) Uani 1 1 d . . .
O6 O 0.19573(14) 0.1266(3) -0.1648(3) 0.0476(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Er1 2.317(4) . ?
O2W Er1 2.362(6) . ?
O3W Er1 2.436(6) . ?
O4W Er1 2.347(5) . ?
Er1 O1 2.294(4) . ?
Er1 O1 2.294(4) 7_565 ?
Er1 O1W 2.317(4) 7_565 ?
Er1 O4W 2.347(5) 7_565 ?
N13 O8 1.216(12) . ?
N13 O7 1.228(12) . ?
N13 O9 1.241(13) . ?
N14 O11 1.174(12) . ?
N14 O12 1.226(11) . ?
N14 O10 1.249(11) . ?
C1 O1 1.236(7) . ?
C1 N2 1.340(7) . ?
C1 N1 1.363(8) . ?
C2 N3 1.464(8) . ?
C2 N1 1.465(7) . ?
C2 C21 1.522(9) . ?
C2 C3 1.561(9) . ?
C3 N4 1.454(8) . ?
C3 N2 1.490(7) . ?
C3 C22 1.536(9) . ?
C4 O4 1.236(8) . ?
C4 N3 1.354(8) . ?
C4 N4 1.357(9) . ?
C5 N5 1.443(8) . ?
C5 N2 1.453(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.440(9) . ?
C6 N4 1.458(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.220(7) . ?
C7 N5 1.376(8) . ?
C7 N6 1.380(8) . ?
C8 N7 1.456(8) . ?
C8 N5 1.457(7) . ?
C8 C9 1.544(9) . ?
C8 H8 0.9900 . ?
C9 N6 1.446(8) . ?
C9 N8 1.446(7) . ?
C9 H9 0.9900 . ?
C10 O5 1.222(8) . ?
C10 N8 1.358(9) . ?
C10 N7 1.376(8) . ?
C11 N9 1.440(8) . ?
C11 N6 1.445(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.424(8) . ?
C12 N8 1.463(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.206(8) . ?
C13 N10 1.378(8) . ?
C13 N9 1.380(9) . ?
C14 N11 1.447(8) . ?
C14 N9 1.465(8) . ?
C14 C15 1.554(10) . ?
C14 H14 0.9900 . ?
C15 N12 1.445(8) . ?
C15 N10 1.455(8) . ?
C15 H15 0.9900 . ?
C16 O6 1.238(8) . ?
C16 N12 1.357(9) . ?
C16 N11 1.372(8) . ?
C17 N10 1.451(7) . ?
C17 N10 1.451(7) 7_565 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.449(7) . ?
C18 N12 1.449(7) 7_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.460(7) 7_565 ?
C19 N3 1.460(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.452(6) . ?
C20 N1 1.452(6) 7_565 ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Er1 O1 75.4(2) . 7_565 ?
O1 Er1 O1W 144.71(14) . 7_565 ?
O1 Er1 O1W 83.29(15) 7_565 7_565 ?
O1 Er1 O1W 83.29(15) . . ?
O1 Er1 O1W 144.71(14) 7_565 . ?
O1W Er1 O1W 99.4(2) 7_565 . ?
O1 Er1 O4W 70.37(15) . . ?
O1 Er1 O4W 115.32(17) 7_565 . ?
O1W Er1 O4W 144.90(15) 7_565 . ?
O1W Er1 O4W 82.28(18) . . ?
O1 Er1 O4W 115.32(17) . 7_565 ?
O1 Er1 O4W 70.37(15) 7_565 7_565 ?
O1W Er1 O4W 82.28(18) 7_565 7_565 ?
O1W Er1 O4W 144.90(15) . 7_565 ?
O4W Er1 O4W 77.3(3) . 7_565 ?
O1 Er1 O2W 74.92(16) . . ?
O1 Er1 O2W 74.92(16) 7_565 . ?
O1W Er1 O2W 72.53(14) 7_565 . ?
O1W Er1 O2W 72.53(14) . . ?
O4W Er1 O2W 139.01(13) . . ?
O4W Er1 O2W 139.01(13) 7_565 . ?
O1 Er1 O3W 139.64(11) . . ?
O1 Er1 O3W 139.64(11) 7_565 . ?
O1W Er1 O3W 72.61(14) 7_565 . ?
O1W Er1 O3W 72.61(14) . . ?
O4W Er1 O3W 74.61(17) . . ?
O4W Er1 O3W 74.61(17) 7_565 . ?
O2W Er1 O3W 124.8(2) . . ?
O8 N13 O7 121.8(12) . . ?
O8 N13 O9 119.0(12) . . ?
O7 N13 O9 119.2(12) . . ?
O11 N14 O12 117.8(10) . . ?
O11 N14 O10 119.3(10) . . ?
O12 N14 O10 122.9(9) . . ?
O1 C1 N2 124.5(6) . . ?
O1 C1 N1 124.5(5) . . ?
N2 C1 N1 110.9(5) . . ?
N3 C2 N1 112.1(5) . . ?
N3 C2 C21 112.6(5) . . ?
N1 C2 C21 111.1(5) . . ?
N3 C2 C3 102.8(5) . . ?
N1 C2 C3 103.1(5) . . ?
C21 C2 C3 114.6(5) . . ?
N4 C3 N2 112.7(5) . . ?
N4 C3 C22 112.3(5) . . ?
N2 C3 C22 110.5(5) . . ?
N4 C3 C2 102.3(5) . . ?
N2 C3 C2 102.2(5) . . ?
C22 C3 C2 116.3(5) . . ?
O4 C4 N3 126.0(7) . . ?
O4 C4 N4 124.6(6) . . ?
N3 C4 N4 109.4(5) . . ?
N5 C5 N2 114.1(5) . . ?
N5 C5 H5A 108.7 . . ?
N2 C5 H5A 108.7 . . ?
N5 C5 H5B 108.7 . . ?
N2 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N7 C6 N4 113.5(5) . . ?
N7 C6 H6A 108.9 . . ?
N4 C6 H6A 108.9 . . ?
N7 C6 H6B 108.9 . . ?
N4 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N5 126.5(6) . . ?
O2 C7 N6 125.7(6) . . ?
N5 C7 N6 107.7(5) . . ?
N7 C8 N5 114.1(5) . . ?
N7 C8 C9 103.9(5) . . ?
N5 C8 C9 103.2(5) . . ?
N7 C8 H8 111.7 . . ?
N5 C8 H8 111.7 . . ?
C9 C8 H8 111.7 . . ?
N6 C9 N8 114.5(5) . . ?
N6 C9 C8 103.8(5) . . ?
N8 C9 C8 103.0(5) . . ?
N6 C9 H9 111.7 . . ?
N8 C9 H9 111.7 . . ?
C8 C9 H9 111.7 . . ?
O5 C10 N8 126.7(6) . . ?
O5 C10 N7 124.8(7) . . ?
N8 C10 N7 108.5(5) . . ?
N9 C11 N6 113.3(5) . . ?
N9 C11 H11A 108.9 . . ?
N6 C11 H11A 108.9 . . ?
N9 C11 H11B 108.9 . . ?
N6 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N11 C12 N8 113.2(5) . . ?
N11 C12 H12A 108.9 . . ?
N8 C12 H12A 108.9 . . ?
N11 C12 H12B 108.9 . . ?
N8 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
O3 C13 N10 126.0(7) . . ?
O3 C13 N9 126.1(6) . . ?
N10 C13 N9 107.9(6) . . ?
N11 C14 N9 114.8(5) . . ?
N11 C14 C15 103.2(5) . . ?
N9 C14 C15 102.4(5) . . ?
N11 C14 H14 111.9 . . ?
N9 C14 H14 111.9 . . ?
C15 C14 H14 111.9 . . ?
N12 C15 N10 114.6(5) . . ?
N12 C15 C14 103.5(5) . . ?
N10 C15 C14 104.1(5) . . ?
N12 C15 H15 111.4 . . ?
N10 C15 H15 111.4 . . ?
C14 C15 H15 111.4 . . ?
O6 C16 N12 125.0(6) . . ?
O6 C16 N11 125.3(7) . . ?
N12 C16 N11 109.6(6) . . ?
N10 C17 N10 112.6(8) . 7_565 ?
N10 C17 H17A 109.1 . . ?
N10 C17 H17A 109.1 7_565 . ?
N10 C17 H17B 109.1 . . ?
N10 C17 H17B 109.1 7_565 . ?
H17A C17 H17B 107.8 . . ?
N12 C18 N12 113.5(7) . 7_565 ?
N12 C18 H18A 108.9 . . ?
N12 C18 H18A 108.9 7_565 . ?
N12 C18 H18B 108.9 . . ?
N12 C18 H18B 108.9 7_565 . ?
H18A C18 H18B 107.7 . . ?
N3 C19 N3 114.6(7) 7_565 . ?
N3 C19 H19A 108.6 7_565 . ?
N3 C19 H19A 108.6 . . ?
N3 C19 H19B 108.6 7_565 . ?
N3 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
N1 C20 N1 114.2(7) . 7_565 ?
N1 C20 H20A 108.7 . . ?
N1 C20 H20A 108.7 7_565 . ?
N1 C20 H20B 108.7 . . ?
N1 C20 H20B 108.7 7_565 . ?
H20A C20 H20B 107.6 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C22 H22A 109.5 . . ?
C3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C20 122.0(5) . . ?
C1 N1 C2 111.2(5) . . ?
C20 N1 C2 126.7(6) . . ?
C1 N2 C5 120.2(5) . . ?
C1 N2 C3 111.1(5) . . ?
C5 N2 C3 124.6(5) . . ?
C4 N3 C19 121.2(6) . . ?
C4 N3 C2 111.5(5) . . ?
C19 N3 C2 125.3(6) . . ?
C4 N4 C3 112.5(5) . . ?
C4 N4 C6 122.5(5) . . ?
C3 N4 C6 124.9(5) . . ?
C7 N5 C5 123.3(5) . . ?
C7 N5 C8 112.4(5) . . ?
C5 N5 C8 121.4(5) . . ?
C7 N6 C11 123.3(5) . . ?
C7 N6 C9 112.5(5) . . ?
C11 N6 C9 124.0(5) . . ?
C10 N7 C6 122.7(5) . . ?
C10 N7 C8 110.9(5) . . ?
C6 N7 C8 121.5(5) . . ?
C10 N8 C9 112.4(5) . . ?
C10 N8 C12 121.0(5) . . ?
C9 N8 C12 122.8(5) . . ?
C13 N9 C11 120.5(5) . . ?
C13 N9 C14 112.4(6) . . ?
C11 N9 C14 124.0(6) . . ?
C13 N10 C17 122.9(6) . . ?
C13 N10 C15 112.1(6) . . ?
C17 N10 C15 124.5(6) . . ?
C16 N11 C12 123.5(6) . . ?
C16 N11 C14 111.4(6) . . ?
C12 N11 C14 124.9(6) . . ?
C16 N12 C15 111.8(6) . . ?
C16 N12 C18 122.0(6) . . ?
C15 N12 C18 124.6(6) . . ?
C1 O1 Er1 161.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.106

# 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 0.150 -0.500 783 283 ' '
2 0.500 0.082 0.000 782 283 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997817'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_13Tm
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Tm N24 O18, 2(N O3), Cl, 17(H2 O)'
_chemical_formula_sum            'C40 H90 Cl N26 O41 Tm'
_chemical_formula_weight         1795.76

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.285(5)
_cell_length_b                   14.1423(19)
_cell_length_c                   13.3923(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6682.9(16)
_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          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3704
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6466
_exptl_absorpt_correction_T_max  0.7253
_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            43285
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6715
_reflns_number_gt                4614
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0756P)²+9.3812P] 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         6715
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1542
_refine_ls_wR_factor_gt          0.1440
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
O5W O 0.2251(2) 0.2500 -0.1227(6) 0.082(3) Uani 1 2 d S . .
Cl1 Cl 0.2658(2) -0.2500 -0.4091(5) 0.199(3) Uani 1 2 d S . .
O1W O 0.15758(12) 0.1254(3) 0.0011(2) 0.0384(10) Uani 1 1 d . . .
O2W O 0.14968(16) 0.2500 -0.1542(4) 0.0408(15) Uani 1 2 d S . .
O3W O 0.14410(17) 0.2500 0.1610(4) 0.0423(15) Uani 1 2 d S . .
O4W O 0.07878(13) 0.1469(3) 0.0914(3) 0.0519(12) Uani 1 1 d . . .
Tm1 Tm 0.115686(10) 0.2500 -0.00398(2) 0.02869(14) Uani 1 2 d S . .
N13 N 0.1163(3) -0.2500 -0.5859(7) 0.053(2) Uani 1 2 d S . .
N14 N 0.1329(2) -0.2500 -0.1666(7) 0.052(2) Uani 1 2 d S . .
O7 O 0.1010(4) -0.2500 -0.5027(6) 0.097(3) Uani 1 2 d S . .
O8 O 0.0993(2) -0.2500 -0.6621(6) 0.086(3) Uani 1 2 d S . .
O9 O 0.1524(3) -0.2500 -0.5917(9) 0.113(4) Uani 1 2 d S . .
O10 O 0.09873(19) -0.2500 -0.1898(5) 0.0512(17) Uani 1 2 d S . .
O11 O 0.1585(2) -0.2500 -0.2265(6) 0.083(3) Uani 1 2 d S . .
O12 O 0.1413(3) -0.2118(7) -0.0826(6) 0.063(3) Uani 0.50 1 d P . .
C1 C 0.06151(16) 0.1227(4) -0.1737(4) 0.0283(13) Uani 1 1 d . . .
C2 C 0.01017(15) 0.1137(4) -0.2828(4) 0.0334(14) Uani 1 1 d . . .
C3 C 0.03492(16) 0.0233(4) -0.2941(4) 0.0333(14) Uani 1 1 d . . .
C4 C 0.03349(17) 0.1079(5) -0.4455(4) 0.0414(16) Uani 1 1 d . . .
C5 C 0.09675(16) -0.0214(4) -0.1997(4) 0.0347(14) Uani 1 1 d . . .
H5A H 0.0848 -0.0835 -0.1915 0.042 Uiso 1 1 calc R . .
H5B H 0.1069 -0.0025 -0.1346 0.042 Uiso 1 1 calc R . .
C6 C 0.06439(19) -0.0481(5) -0.4528(4) 0.0495(18) Uani 1 1 d . . .
H6A H 0.0581 -0.0446 -0.5239 0.059 Uiso 1 1 calc R . .
H6B H 0.0559 -0.1098 -0.4281 0.059 Uiso 1 1 calc R . .
C7 C 0.16460(17) -0.0114(4) -0.2439(4) 0.0332(14) Uani 1 1 d . . .
C8 C 0.12476(18) -0.0883(5) -0.3603(4) 0.0405(15) Uani 1 1 d . . .
H8 H 0.1140 -0.1516 -0.3460 0.049 Uiso 1 1 calc R . .
C9 C 0.16656(17) -0.0943(5) -0.3953(4) 0.0382(15) Uani 1 1 d . . .
H9 H 0.1749 -0.1608 -0.4024 0.046 Uiso 1 1 calc R . .
C10 C 0.1290(2) -0.0270(5) -0.5208(4) 0.0416(16) Uani 1 1 d . . .
C11 C 0.22774(17) -0.0411(4) -0.3167(4) 0.0396(15) Uani 1 1 d . . .
H11A H 0.2383 -0.1012 -0.3402 0.048 Uiso 1 1 calc R . .
H11B H 0.2360 -0.0320 -0.2475 0.048 Uiso 1 1 calc R . .
C12 C 0.19626(18) -0.0518(5) -0.5629(4) 0.0438(16) Uani 1 1 d . . .
H12A H 0.2096 -0.1121 -0.5543 0.053 Uiso 1 1 calc R . .
H12B H 0.1859 -0.0505 -0.6307 0.053 Uiso 1 1 calc R . .
C13 C 0.25994(16) 0.1117(5) -0.3338(5) 0.0422(16) Uani 1 1 d . . .
C14 C 0.25387(18) 0.0253(5) -0.4823(4) 0.0426(16) Uani 1 1 d . . .
H14 H 0.2710 -0.0294 -0.4922 0.051 Uiso 1 1 calc R . .
C15 C 0.27419(17) 0.1188(5) -0.5040(4) 0.0441(16) Uani 1 1 d . . .
H15 H 0.2997 0.1082 -0.5329 0.053 Uiso 1 1 calc R . .
C16 C 0.21990(18) 0.1050(5) -0.6021(4) 0.0436(16) Uani 1 1 d . . .
C17 C 0.2979(2) 0.2500 -0.3881(6) 0.047(2) Uani 1 2 d S . .
H17A H 0.3208 0.2500 -0.4295 0.057 Uiso 1 2 calc SR . .
H17B H 0.3059 0.2500 -0.3180 0.057 Uiso 1 2 calc SR . .
C18 C 0.2574(3) 0.2500 -0.6283(6) 0.048(3) Uani 1 2 d S . .
H18A H 0.2429 0.2500 -0.6906 0.057 Uiso 1 2 calc SR . .
H18B H 0.2844 0.2500 -0.6460 0.057 Uiso 1 2 calc SR . .
C19 C -0.0030(2) 0.2500 -0.4079(6) 0.040(2) Uani 1 2 d S . .
H19A H -0.0051 0.2500 -0.4809 0.048 Uiso 1 2 calc SR . .
H19B H -0.0288 0.2500 -0.3808 0.048 Uiso 1 2 calc SR . .
C20 C 0.0150(2) 0.2500 -0.1505(6) 0.0335(19) Uani 1 2 d S . .
H20A H -0.0128 0.2500 -0.1500 0.040 Uiso 1 2 calc SR . .
H20B H 0.0236 0.2500 -0.0809 0.040 Uiso 1 2 calc SR . .
C21 C -0.03137(17) 0.0945(5) -0.2608(5) 0.0481(17) Uani 1 1 d . . .
H21A H -0.0336 0.0623 -0.1971 0.072 Uiso 1 1 calc R . .
H21B H -0.0419 0.0550 -0.3131 0.072 Uiso 1 1 calc R . .
H21C H -0.0451 0.1539 -0.2582 0.072 Uiso 1 1 calc R . .
C22 C 0.0162(2) -0.0686(5) -0.2626(5) 0.0552(19) Uani 1 1 d . . .
H22A H 0.0102 -0.0659 -0.1920 0.083 Uiso 1 1 calc R . .
H22B H 0.0334 -0.1208 -0.2749 0.083 Uiso 1 1 calc R . .
H22C H -0.0069 -0.0778 -0.3006 0.083 Uiso 1 1 calc R . .
N1 N 0.02822(13) 0.1633(3) -0.1987(3) 0.0308(11) Uani 1 1 d . . .
N2 N 0.06803(12) 0.0461(3) -0.2293(3) 0.0280(10) Uani 1 1 d . . .
N3 N 0.01589(13) 0.1626(4) -0.3768(3) 0.0357(12) Uani 1 1 d . . .
N4 N 0.04410(13) 0.0250(4) -0.4004(3) 0.0357(12) Uani 1 1 d . . .
N5 N 0.12799(14) -0.0305(4) -0.2695(3) 0.0378(12) Uani 1 1 d . . .
N6 N 0.18723(14) -0.0469(3) -0.3188(3) 0.0346(12) Uani 1 1 d . . .
N7 N 0.10516(14) -0.0416(4) -0.4415(3) 0.0357(12) Uani 1 1 d . . .
N8 N 0.16496(15) -0.0472(4) -0.4911(3) 0.0402(13) Uani 1 1 d . . .
N9 N 0.24291(14) 0.0350(4) -0.3775(3) 0.0393(13) Uani 1 1 d . . .
N10 N 0.27643(14) 0.1653(4) -0.4081(3) 0.0413(13) Uani 1 1 d . . .
N11 N 0.22253(14) 0.0232(4) -0.5521(3) 0.0389(12) Uani 1 1 d . . .
N12 N 0.24908(13) 0.1643(4) -0.5746(3) 0.0365(12) Uani 1 1 d . . .
O1 O 0.08276(11) 0.1506(3) -0.1072(3) 0.0348(9) Uani 1 1 d . . .
O2 O 0.17598(11) 0.0225(3) -0.1656(3) 0.0372(10) Uani 1 1 d . . .
O3 O 0.26035(12) 0.1301(3) -0.2458(3) 0.0452(11) Uani 1 1 d . . .
O4 O 0.03870(13) 0.1261(4) -0.5341(3) 0.0504(12) Uani 1 1 d . . .
O5 O 0.11916(13) -0.0016(4) -0.6038(3) 0.0563(13) Uani 1 1 d . . .
O6 O 0.19580(13) 0.1274(3) -0.6662(3) 0.0497(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Tm1 2.301(4) . ?
O2W Tm1 2.343(5) . ?
O3W Tm1 2.426(5) . ?
O4W Tm1 2.336(4) . ?
Tm1 O1 2.289(4) . ?
Tm1 O1 2.289(4) 7_565 ?
Tm1 O1W 2.301(4) 7_565 ?
Tm1 O4W 2.336(4) 7_565 ?
N13 O8 1.184(10) . ?
N13 O7 1.238(11) . ?
N13 O9 1.275(11) . ?
N14 O11 1.210(10) . ?
N14 O10 1.243(10) . ?
N14 O12 1.283(10) 7 ?
N14 O12 1.283(10) . ?
O12 O12 1.082(19) 7 ?
C1 O1 1.229(6) . ?
C1 N2 1.334(7) . ?
C1 N1 1.350(7) . ?
C2 N3 1.450(7) . ?
C2 N1 1.471(6) . ?
C2 C21 1.520(8) . ?
C2 C3 1.556(8) . ?
C3 N4 1.460(7) . ?
C3 N2 1.490(7) . ?
C3 C22 1.517(9) . ?
C4 O4 1.227(7) . ?
C4 N3 1.353(8) . ?
C4 N4 1.372(8) . ?
C5 N2 1.448(7) . ?
C5 N5 1.451(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.440(8) . ?
C6 N7 1.449(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.220(6) . ?
C7 N5 1.363(7) . ?
C7 N6 1.377(7) . ?
C8 N7 1.449(7) . ?
C8 N5 1.470(7) . ?
C8 C9 1.550(8) . ?
C8 H8 0.9900 . ?
C9 N6 1.425(7) . ?
C9 N8 1.447(7) . ?
C9 H9 0.9900 . ?
C10 O5 1.219(7) . ?
C10 N8 1.361(9) . ?
C10 N7 1.369(8) . ?
C11 N6 1.432(7) . ?
C11 N9 1.451(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.416(8) . ?
C12 N8 1.465(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.208(7) . ?
C13 N9 1.371(8) . ?
C13 N10 1.379(8) . ?
C14 N11 1.448(7) . ?
C14 N9 1.462(7) . ?
C14 C15 1.533(10) . ?
C14 H14 0.9900 . ?
C15 N10 1.444(7) . ?
C15 N12 1.446(7) . ?
C15 H15 0.9900 . ?
C16 O6 1.249(7) . ?
C16 N11 1.341(8) . ?
C16 N12 1.378(8) . ?
C17 N10 1.444(7) . ?
C17 N10 1.444(7) 7_565 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.440(6) . ?
C18 N12 1.440(6) 7_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.466(6) 7_565 ?
C19 N3 1.466(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.463(6) 7_565 ?
C20 N1 1.463(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tm1 O1 75.80(19) . 7_565 ?
O1 Tm1 O1W 144.53(12) . 7_565 ?
O1 Tm1 O1W 82.73(14) 7_565 7_565 ?
O1 Tm1 O1W 82.73(14) . . ?
O1 Tm1 O1W 144.53(12) 7_565 . ?
O1W Tm1 O1W 100.0(2) 7_565 . ?
O1 Tm1 O4W 70.35(14) . . ?
O1 Tm1 O4W 115.53(16) 7_565 . ?
O1W Tm1 O4W 145.11(13) 7_565 . ?
O1W Tm1 O4W 82.17(16) . . ?
O1 Tm1 O4W 115.53(16) . 7_565 ?
O1 Tm1 O4W 70.35(14) 7_565 7_565 ?
O1W Tm1 O4W 82.17(16) 7_565 7_565 ?
O1W Tm1 O4W 145.11(13) . 7_565 ?
O4W Tm1 O4W 77.3(2) . 7_565 ?
O1 Tm1 O2W 74.99(14) . . ?
O1 Tm1 O2W 74.99(14) 7_565 . ?
O1W Tm1 O2W 72.33(12) 7_565 . ?
O1W Tm1 O2W 72.33(12) . . ?
O4W Tm1 O2W 139.05(12) . . ?
O4W Tm1 O2W 139.05(12) 7_565 . ?
O1 Tm1 O3W 139.45(10) . . ?
O1 Tm1 O3W 139.45(10) 7_565 . ?
O1W Tm1 O3W 73.00(12) 7_565 . ?
O1W Tm1 O3W 73.00(12) . . ?
O4W Tm1 O3W 74.48(15) . . ?
O4W Tm1 O3W 74.48(15) 7_565 . ?
O2W Tm1 O3W 124.8(2) . . ?
O8 N13 O7 123.6(11) . . ?
O8 N13 O9 117.1(10) . . ?
O7 N13 O9 119.3(10) . . ?
O11 N14 O10 124.0(9) . . ?
O11 N14 O12 114.1(8) . 7 ?
O10 N14 O12 116.3(8) . 7 ?
O11 N14 O12 114.1(8) . . ?
O10 N14 O12 116.3(8) . . ?
O12 N14 O12 49.9(9) 7 . ?
O12 O12 N14 65.1(5) 7 . ?
O1 C1 N2 124.0(5) . . ?
O1 C1 N1 125.0(5) . . ?
N2 C1 N1 110.9(5) . . ?
N3 C2 N1 112.2(5) . . ?
N3 C2 C21 112.8(5) . . ?
N1 C2 C21 110.8(5) . . ?
N3 C2 C3 103.2(4) . . ?
N1 C2 C3 102.9(4) . . ?
C21 C2 C3 114.4(5) . . ?
N4 C3 N2 113.0(4) . . ?
N4 C3 C22 112.4(5) . . ?
N2 C3 C22 111.3(5) . . ?
N4 C3 C2 101.9(4) . . ?
N2 C3 C2 101.8(4) . . ?
C22 C3 C2 115.6(5) . . ?
O4 C4 N3 127.3(6) . . ?
O4 C4 N4 124.3(6) . . ?
N3 C4 N4 108.3(5) . . ?
N2 C5 N5 114.5(4) . . ?
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 . . ?
N4 C6 N7 113.4(5) . . ?
N4 C6 H6A 108.9 . . ?
N7 C6 H6A 108.9 . . ?
N4 C6 H6B 108.9 . . ?
N7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N5 127.3(5) . . ?
O2 C7 N6 125.3(5) . . ?
N5 C7 N6 107.1(5) . . ?
N7 C8 N5 113.9(5) . . ?
N7 C8 C9 104.6(5) . . ?
N5 C8 C9 101.9(5) . . ?
N7 C8 H8 111.9 . . ?
N5 C8 H8 111.9 . . ?
C9 C8 H8 111.9 . . ?
N6 C9 N8 116.2(5) . . ?
N6 C9 C8 104.1(5) . . ?
N8 C9 C8 101.9(5) . . ?
N6 C9 H9 111.3 . . ?
N8 C9 H9 111.3 . . ?
C8 C9 H9 111.3 . . ?
O5 C10 N8 126.4(6) . . ?
O5 C10 N7 125.3(6) . . ?
N8 C10 N7 108.4(5) . . ?
N6 C11 N9 113.6(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 . . ?
N11 C12 N8 113.1(5) . . ?
N11 C12 H12A 109.0 . . ?
N8 C12 H12A 109.0 . . ?
N11 C12 H12B 109.0 . . ?
N8 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N9 126.3(6) . . ?
O3 C13 N10 125.5(7) . . ?
N9 C13 N10 108.2(5) . . ?
N11 C14 N9 114.8(5) . . ?
N11 C14 C15 104.6(5) . . ?
N9 C14 C15 103.0(5) . . ?
N11 C14 H14 111.3 . . ?
N9 C14 H14 111.3 . . ?
C15 C14 H14 111.3 . . ?
N10 C15 N12 114.4(5) . . ?
N10 C15 C14 104.5(5) . . ?
N12 C15 C14 102.7(5) . . ?
N10 C15 H15 111.6 . . ?
N12 C15 H15 111.6 . . ?
C14 C15 H15 111.6 . . ?
O6 C16 N11 127.5(6) . . ?
O6 C16 N12 122.6(7) . . ?
N11 C16 N12 109.9(5) . . ?
N10 C17 N10 112.2(7) . 7_565 ?
N10 C17 H17A 109.2 . . ?
N10 C17 H17A 109.2 7_565 . ?
N10 C17 H17B 109.2 . . ?
N10 C17 H17B 109.2 7_565 . ?
H17A C17 H17B 107.9 . . ?
N12 C18 N12 114.7(7) . 7_565 ?
N12 C18 H18A 108.6 . . ?
N12 C18 H18A 108.6 7_565 . ?
N12 C18 H18B 108.6 . . ?
N12 C18 H18B 108.6 7_565 . ?
H18A C18 H18B 107.6 . . ?
N3 C19 N3 115.1(6) 7_565 . ?
N3 C19 H19A 108.5 7_565 . ?
N3 C19 H19A 108.5 . . ?
N3 C19 H19B 108.5 7_565 . ?
N3 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
N1 C20 N1 114.0(6) 7_565 . ?
N1 C20 H20A 108.8 7_565 . ?
N1 C20 H20A 108.8 . . ?
N1 C20 H20B 108.8 7_565 . ?
N1 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C22 H22A 109.5 . . ?
C3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C20 121.7(5) . . ?
C1 N1 C2 111.3(5) . . ?
C20 N1 C2 126.8(5) . . ?
C1 N2 C5 120.2(4) . . ?
C1 N2 C3 111.4(5) . . ?
C5 N2 C3 124.4(5) . . ?
C4 N3 C2 112.5(5) . . ?
C4 N3 C19 119.8(5) . . ?
C2 N3 C19 125.8(5) . . ?
C4 N4 C6 122.4(5) . . ?
C4 N4 C3 112.5(5) . . ?
C6 N4 C3 125.0(5) . . ?
C7 N5 C5 122.7(4) . . ?
C7 N5 C8 113.1(5) . . ?
C5 N5 C8 121.5(5) . . ?
C7 N6 C9 113.5(5) . . ?
C7 N6 C11 123.0(5) . . ?
C9 N6 C11 123.5(5) . . ?
C10 N7 C6 122.6(5) . . ?
C10 N7 C8 111.0(5) . . ?
C6 N7 C8 121.5(5) . . ?
C10 N8 C9 113.1(5) . . ?
C10 N8 C12 121.4(5) . . ?
C9 N8 C12 122.1(5) . . ?
C13 N9 C11 120.6(5) . . ?
C13 N9 C14 111.6(5) . . ?
C11 N9 C14 124.5(5) . . ?
C13 N10 C17 123.0(6) . . ?
C13 N10 C15 111.6(6) . . ?
C17 N10 C15 124.8(6) . . ?
C16 N11 C12 123.4(5) . . ?
C16 N11 C14 110.9(5) . . ?
C12 N11 C14 125.5(5) . . ?
C16 N12 C18 122.1(6) . . ?
C16 N12 C15 111.2(5) . . ?
C18 N12 C15 125.1(6) . . ?
C1 O1 Tm1 160.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.503
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.124


# 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 0.002 0.000 786 327 ' '
2 0.500 0.648 -0.500 786 327 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997818'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_14Yb
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Yb N24 O18, 2(N O3), Cl, 14(H2 O)'
_chemical_formula_sum            'C40 H84 Cl N26 O38 Yb'
_chemical_formula_weight         1745.82

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'
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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.396(4)
_cell_length_b                   14.1853(18)
_cell_length_c                   13.4031(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6729.6(15)
_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          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3588
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6292
_exptl_absorpt_correction_T_max  0.6983
_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            45163
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6317
_reflns_number_gt                4559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0651P)²+13.0544P] 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         6317
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1268
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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 0.2346(2) -0.2500 0.9057(7) 0.249(4) Uani 1 2 d S . .
O5W O 0.2241(2) -0.2500 1.1178(5) 0.079(2) Uani 1 2 d S . .
O1W O 0.34359(12) 0.1269(3) 0.4959(2) 0.0476(10) Uani 1 1 d . . .
O2W O 0.35720(16) 0.2500 0.3379(4) 0.0527(15) Uani 1 2 d S . .
O3W O 0.35211(15) 0.2500 0.6516(3) 0.0451(13) Uani 1 2 d S . .
O4W O 0.42230(13) 0.1483(3) 0.4060(3) 0.0678(13) Uani 1 1 d . . .
Yb1 Yb 0.385583(9) 0.2500 0.50189(2) 0.03381(13) Uani 1 2 d S . .
N13 N 0.3826(3) -0.2500 1.0826(8) 0.071(3) Uani 1 2 d S . .
N14 N 0.3687(3) -0.2500 0.6591(6) 0.064(2) Uani 1 2 d S . .
O7 O 0.3976(4) -0.2500 1.0008(6) 0.120(4) Uani 1 2 d S . .
O8 O 0.4013(3) -0.2500 1.1592(7) 0.118(3) Uani 1 2 d S . .
O9 O 0.3474(3) -0.2500 1.0883(10) 0.136(4) Uani 1 2 d S . .
O10 O 0.3433(2) -0.2500 0.7220(6) 0.095(2) Uani 1 2 d S . .
O11 O 0.3599(3) -0.2500 0.5759(7) 0.241(10) Uani 1 2 d S . .
O12 O 0.4026(2) -0.2500 0.6822(6) 0.0723(19) Uani 1 2 d S . .
C1 C 0.43941(15) 0.1230(4) 0.6714(3) 0.0370(12) Uani 1 1 d . . .
C2 C 0.49066(15) 0.1144(4) 0.7807(4) 0.0428(13) Uani 1 1 d . . .
C3 C 0.46582(16) 0.0243(4) 0.7935(4) 0.0419(13) Uani 1 1 d . . .
C4 C 0.46672(15) 0.1097(4) 0.9441(4) 0.0440(14) Uani 1 1 d . . .
C5 C 0.40458(16) -0.0228(4) 0.6973(4) 0.0399(13) Uani 1 1 d . . .
H5A H 0.4165 -0.0849 0.6913 0.048 Uiso 1 1 calc R . .
H5B H 0.3948 -0.0053 0.6314 0.048 Uiso 1 1 calc R . .
C6 C 0.43528(19) -0.0441(4) 0.9527(4) 0.0538(16) Uani 1 1 d . . .
H6A H 0.4443 -0.1060 0.9308 0.065 Uiso 1 1 calc R . .
H6B H 0.4410 -0.0381 1.0240 0.065 Uiso 1 1 calc R . .
C7 C 0.33608(16) -0.0132(4) 0.7418(4) 0.0403(13) Uani 1 1 d . . .
C8 C 0.37533(16) -0.0870(4) 0.8573(4) 0.0421(13) Uani 1 1 d . . .
H8 H 0.3860 -0.1501 0.8431 0.051 Uiso 1 1 calc R . .
C9 C 0.33444(16) -0.0934(4) 0.8920(4) 0.0423(13) Uani 1 1 d . . .
H9 H 0.3262 -0.1599 0.8982 0.051 Uiso 1 1 calc R . .
C10 C 0.3708(2) -0.0243(4) 1.0184(4) 0.0510(15) Uani 1 1 d . . .
C11 C 0.27230(17) -0.0409(4) 0.8120(4) 0.0493(15) Uani 1 1 d . . .
H11A H 0.2641 -0.0319 0.7428 0.059 Uiso 1 1 calc R . .
H11B H 0.2619 -0.1010 0.8355 0.059 Uiso 1 1 calc R . .
C12 C 0.30385(17) -0.0515(4) 1.0588(4) 0.0491(15) Uani 1 1 d . . .
H12A H 0.3142 -0.0499 1.1266 0.059 Uiso 1 1 calc R . .
H12B H 0.2906 -0.1117 1.0505 0.059 Uiso 1 1 calc R . .
C13 C 0.24071(16) 0.1123(5) 0.8298(4) 0.0488(15) Uani 1 1 d . . .
C14 C 0.24637(18) 0.0251(5) 0.9777(4) 0.0492(15) Uani 1 1 d . . .
H14 H 0.2294 -0.0295 0.9878 0.059 Uiso 1 1 calc R . .
C15 C 0.22606(17) 0.1193(5) 0.9986(4) 0.0483(14) Uani 1 1 d . . .
H15 H 0.2005 0.1087 1.0266 0.058 Uiso 1 1 calc R . .
C16 C 0.27914(17) 0.1056(4) 1.0985(4) 0.0471(14) Uani 1 1 d . . .
C17 C 0.2020(3) 0.2500 0.8818(6) 0.055(2) Uani 1 2 d S . .
H17A H 0.1942 0.2500 0.8117 0.066 Uiso 1 2 calc SR . .
H17B H 0.1792 0.2500 0.9230 0.066 Uiso 1 2 calc SR . .
C18 C 0.2421(3) 0.2500 1.1255(6) 0.051(2) Uani 1 2 d S . .
H18A H 0.2565 0.2500 1.1879 0.061 Uiso 1 2 calc SR . .
H18B H 0.2152 0.2500 1.1429 0.061 Uiso 1 2 calc SR . .
C19 C 0.5043(2) 0.2500 0.9081(6) 0.049(2) Uani 1 2 d S . .
H19A H 0.5299 0.2500 0.8804 0.059 Uiso 1 2 calc SR . .
H19B H 0.5065 0.2500 0.9809 0.059 Uiso 1 2 calc SR . .
C20 C 0.4862(2) 0.2500 0.6504(5) 0.0418(19) Uani 1 2 d S . .
H20A H 0.5139 0.2500 0.6513 0.050 Uiso 1 2 calc SR . .
H20B H 0.4782 0.2500 0.5804 0.050 Uiso 1 2 calc SR . .
C21 C 0.53234(18) 0.0958(6) 0.7596(5) 0.0650(19) Uani 1 1 d . . .
H21A H 0.5436 0.0639 0.8163 0.098 Uiso 1 1 calc R . .
H21B H 0.5452 0.1552 0.7484 0.098 Uiso 1 1 calc R . .
H21C H 0.5347 0.0565 0.7007 0.098 Uiso 1 1 calc R . .
C22 C 0.4840(2) -0.0686(5) 0.7653(5) 0.066(2) Uani 1 1 d . . .
H22A H 0.4903 -0.0681 0.6949 0.100 Uiso 1 1 calc R . .
H22B H 0.4666 -0.1197 0.7789 0.100 Uiso 1 1 calc R . .
H22C H 0.5069 -0.0774 0.8042 0.100 Uiso 1 1 calc R . .
N1 N 0.47278(12) 0.1635(3) 0.6977(3) 0.0370(10) Uani 1 1 d . . .
N2 N 0.43259(12) 0.0447(3) 0.7270(3) 0.0386(10) Uani 1 1 d . . .
N3 N 0.48510(13) 0.1638(3) 0.8769(3) 0.0445(11) Uani 1 1 d . . .
N4 N 0.45581(13) 0.0276(4) 0.8992(3) 0.0441(11) Uani 1 1 d . . .
N5 N 0.37299(14) -0.0295(3) 0.7672(3) 0.0419(11) Uani 1 1 d . . .
N6 N 0.31367(14) -0.0454(3) 0.8151(3) 0.0451(12) Uani 1 1 d . . .
N7 N 0.39522(14) -0.0404(3) 0.9399(3) 0.0464(12) Uani 1 1 d . . .
N8 N 0.33450(14) -0.0466(4) 0.9880(3) 0.0457(12) Uani 1 1 d . . .
N9 N 0.25733(13) 0.0352(4) 0.8731(3) 0.0459(12) Uani 1 1 d . . .
N10 N 0.22411(13) 0.1639(3) 0.9027(3) 0.0469(12) Uani 1 1 d . . .
N11 N 0.27697(14) 0.0248(3) 1.0476(3) 0.0452(11) Uani 1 1 d . . .
N12 N 0.25062(13) 0.1638(3) 1.0706(3) 0.0452(11) Uani 1 1 d . . .
O1 O 0.41834(10) 0.1507(2) 0.6041(2) 0.0387(8) Uani 1 1 d . . .
O2 O 0.32538(11) 0.0227(3) 0.6626(3) 0.0489(10) Uani 1 1 d . . .
O3 O 0.24069(12) 0.1294(3) 0.7405(3) 0.0544(11) Uani 1 1 d . . .
O4 O 0.46187(13) 0.1278(3) 1.0324(3) 0.0611(12) Uani 1 1 d . . .
O5 O 0.37987(14) 0.0012(4) 1.1018(3) 0.0696(14) Uani 1 1 d . . .
O6 O 0.30340(12) 0.1265(3) 1.1636(3) 0.0581(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Yb1 2.295(4) . ?
O2W Yb1 2.416(5) . ?
O3W Yb1 2.330(5) . ?
O4W Yb1 2.328(4) . ?
Yb1 O1 2.281(3) 7_565 ?
Yb1 O1 2.281(3) . ?
Yb1 O1W 2.295(4) 7_565 ?
Yb1 O4W 2.328(4) 7_565 ?
N13 O7 1.218(12) . ?
N13 O8 1.220(11) . ?
N13 O9 1.250(12) . ?
N14 O11 1.158(11) . ?
N14 O10 1.232(10) . ?
N14 O12 1.240(10) . ?
C1 O1 1.235(6) . ?
C1 N2 1.359(6) . ?
C1 N1 1.360(7) . ?
C2 N1 1.457(6) . ?
C2 N3 1.482(6) . ?
C2 C21 1.525(8) . ?
C2 C3 1.561(8) . ?
C3 N4 1.461(6) . ?
C3 N2 1.504(6) . ?
C3 C22 1.514(8) . ?
C4 O4 1.223(7) . ?
C4 N3 1.350(7) . ?
C4 N4 1.367(7) . ?
C5 N2 1.434(7) . ?
C5 N5 1.462(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N7 1.429(8) . ?
C6 N4 1.441(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.237(6) . ?
C7 N6 1.342(7) . ?
C7 N5 1.370(7) . ?
C8 N5 1.460(6) . ?
C8 N7 1.469(7) . ?
C8 C9 1.523(8) . ?
C8 H8 0.9900 . ?
C9 N6 1.437(7) . ?
C9 N8 1.449(6) . ?
C9 H9 0.9900 . ?
C10 O5 1.218(7) . ?
C10 N7 1.381(8) . ?
C10 N8 1.384(9) . ?
C11 N9 1.455(7) . ?
C11 N6 1.467(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N8 1.443(7) . ?
C12 N11 1.449(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.221(7) . ?
C13 N10 1.354(7) . ?
C13 N9 1.371(8) . ?
C14 N11 1.431(7) . ?
C14 N9 1.461(7) . ?
C14 C15 1.543(9) . ?
C14 H14 0.9900 . ?
C15 N10 1.435(7) . ?
C15 N12 1.445(7) . ?
C15 H15 0.9900 . ?
C16 O6 1.260(7) . ?
C16 N11 1.337(7) . ?
C16 N12 1.356(7) . ?
C17 N10 1.477(6) 7_565 ?
C17 N10 1.477(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.459(6) . ?
C18 N12 1.459(6) 7_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.459(6) . ?
C19 N3 1.459(6) 7_565 ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.461(6) 7_565 ?
C20 N1 1.461(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Yb1 O1 76.24(17) 7_565 . ?
O1 Yb1 O1W 145.10(11) 7_565 . ?
O1 Yb1 O1W 83.14(13) . . ?
O1 Yb1 O1W 83.14(13) 7_565 7_565 ?
O1 Yb1 O1W 145.10(11) . 7_565 ?
O1W Yb1 O1W 99.1(2) . 7_565 ?
O1 Yb1 O4W 115.48(16) 7_565 . ?
O1 Yb1 O4W 70.44(14) . . ?
O1W Yb1 O4W 82.57(17) . . ?
O1W Yb1 O4W 144.46(12) 7_565 . ?
O1 Yb1 O4W 70.44(14) 7_565 7_565 ?
O1 Yb1 O4W 115.48(16) . 7_565 ?
O1W Yb1 O4W 144.46(12) . 7_565 ?
O1W Yb1 O4W 82.57(17) 7_565 7_565 ?
O4W Yb1 O4W 76.6(2) . 7_565 ?
O1 Yb1 O3W 75.01(13) 7_565 . ?
O1 Yb1 O3W 75.01(13) . . ?
O1W Yb1 O3W 72.60(12) . . ?
O1W Yb1 O3W 72.60(12) 7_565 . ?
O4W Yb1 O3W 139.37(12) . . ?
O4W Yb1 O3W 139.37(12) 7_565 . ?
O1 Yb1 O2W 139.24(10) 7_565 . ?
O1 Yb1 O2W 139.24(10) . . ?
O1W Yb1 O2W 72.46(12) . . ?
O1W Yb1 O2W 72.46(12) 7_565 . ?
O4W Yb1 O2W 74.35(15) . . ?
O4W Yb1 O2W 74.35(15) 7_565 . ?
O3W Yb1 O2W 124.9(2) . . ?
O7 N13 O8 121.5(12) . . ?
O7 N13 O9 119.3(11) . . ?
O8 N13 O9 119.3(12) . . ?
O11 N14 O10 117.6(10) . . ?
O11 N14 O12 120.1(11) . . ?
O10 N14 O12 122.3(8) . . ?
O1 C1 N2 123.6(5) . . ?
O1 C1 N1 125.4(5) . . ?
N2 C1 N1 111.0(4) . . ?
N1 C2 N3 112.4(4) . . ?
N1 C2 C21 111.2(4) . . ?
N3 C2 C21 111.8(5) . . ?
N1 C2 C3 103.4(4) . . ?
N3 C2 C3 102.5(4) . . ?
C21 C2 C3 115.1(5) . . ?
N4 C3 N2 112.2(4) . . ?
N4 C3 C22 111.9(5) . . ?
N2 C3 C22 110.6(5) . . ?
N4 C3 C2 102.5(4) . . ?
N2 C3 C2 102.6(4) . . ?
C22 C3 C2 116.5(5) . . ?
O4 C4 N3 126.4(6) . . ?
O4 C4 N4 124.4(5) . . ?
N3 C4 N4 109.1(5) . . ?
N2 C5 N5 113.2(4) . . ?
N2 C5 H5A 108.9 . . ?
N5 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
N5 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
N7 C6 N4 114.5(5) . . ?
N7 C6 H6A 108.6 . . ?
N4 C6 H6A 108.6 . . ?
N7 C6 H6B 108.6 . . ?
N4 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
O2 C7 N6 126.0(5) . . ?
O2 C7 N5 125.1(5) . . ?
N6 C7 N5 108.9(5) . . ?
N5 C8 N7 113.5(5) . . ?
N5 C8 C9 103.4(4) . . ?
N7 C8 C9 104.6(4) . . ?
N5 C8 H8 111.6 . . ?
N7 C8 H8 111.6 . . ?
C9 C8 H8 111.6 . . ?
N6 C9 N8 114.9(5) . . ?
N6 C9 C8 103.8(4) . . ?
N8 C9 C8 104.0(4) . . ?
N6 C9 H9 111.2 . . ?
N8 C9 H9 111.2 . . ?
C8 C9 H9 111.2 . . ?
O5 C10 N7 125.7(7) . . ?
O5 C10 N8 125.6(6) . . ?
N7 C10 N8 108.6(5) . . ?
N9 C11 N6 112.3(4) . . ?
N9 C11 H11A 109.1 . . ?
N6 C11 H11A 109.1 . . ?
N9 C11 H11B 109.1 . . ?
N6 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
N8 C12 N11 112.9(4) . . ?
N8 C12 H12A 109.0 . . ?
N11 C12 H12A 109.0 . . ?
N8 C12 H12B 109.0 . . ?
N11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
O3 C13 N10 126.8(6) . . ?
O3 C13 N9 125.0(6) . . ?
N10 C13 N9 108.2(5) . . ?
N11 C14 N9 115.3(5) . . ?
N11 C14 C15 103.7(5) . . ?
N9 C14 C15 102.3(5) . . ?
N11 C14 H14 111.7 . . ?
N9 C14 H14 111.7 . . ?
C15 C14 H14 111.7 . . ?
N10 C15 N12 115.7(5) . . ?
N10 C15 C14 104.0(4) . . ?
N12 C15 C14 102.7(5) . . ?
N10 C15 H15 111.3 . . ?
N12 C15 H15 111.3 . . ?
C14 C15 H15 111.3 . . ?
O6 C16 N11 126.5(6) . . ?
O6 C16 N12 123.7(6) . . ?
N11 C16 N12 109.8(5) . . ?
N10 C17 N10 111.6(7) 7_565 . ?
N10 C17 H17A 109.3 7_565 . ?
N10 C17 H17A 109.3 . . ?
N10 C17 H17B 109.3 7_565 . ?
N10 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
N12 C18 N12 113.8(6) . 7_565 ?
N12 C18 H18A 108.8 . . ?
N12 C18 H18A 108.8 7_565 . ?
N12 C18 H18B 108.8 . . ?
N12 C18 H18B 108.8 7_565 . ?
H18A C18 H18B 107.7 . . ?
N3 C19 N3 113.8(6) . 7_565 ?
N3 C19 H19A 108.8 . . ?
N3 C19 H19A 108.8 7_565 . ?
N3 C19 H19B 108.8 . . ?
N3 C19 H19B 108.8 7_565 . ?
H19A C19 H19B 107.7 . . ?
N1 C20 N1 114.3(6) 7_565 . ?
N1 C20 H20A 108.7 7_565 . ?
N1 C20 H20A 108.7 . . ?
N1 C20 H20B 108.7 7_565 . ?
N1 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C22 H22A 109.5 . . ?
C3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C2 111.9(4) . . ?
C1 N1 C20 121.7(5) . . ?
C2 N1 C20 126.2(5) . . ?
C1 N2 C5 121.0(4) . . ?
C1 N2 C3 110.1(4) . . ?
C5 N2 C3 125.2(4) . . ?
C4 N3 C19 120.6(5) . . ?
C4 N3 C2 112.1(5) . . ?
C19 N3 C2 125.7(5) . . ?
C4 N4 C6 121.6(4) . . ?
C4 N4 C3 112.7(5) . . ?
C6 N4 C3 125.6(5) . . ?
C7 N5 C8 110.7(4) . . ?
C7 N5 C5 124.0(4) . . ?
C8 N5 C5 121.5(5) . . ?
C7 N6 C9 112.6(5) . . ?
C7 N6 C11 123.7(5) . . ?
C9 N6 C11 123.5(5) . . ?
C10 N7 C6 122.4(5) . . ?
C10 N7 C8 110.4(5) . . ?
C6 N7 C8 123.3(5) . . ?
C10 N8 C12 121.0(4) . . ?
C10 N8 C9 111.6(5) . . ?
C12 N8 C9 124.1(5) . . ?
C13 N9 C11 120.7(4) . . ?
C13 N9 C14 111.8(5) . . ?
C11 N9 C14 124.3(5) . . ?
C13 N10 C15 112.8(5) . . ?
C13 N10 C17 122.7(5) . . ?
C15 N10 C17 124.1(5) . . ?
C16 N11 C14 112.0(5) . . ?
C16 N11 C12 123.3(5) . . ?
C14 N11 C12 124.5(5) . . ?
C16 N12 C15 111.4(5) . . ?
C16 N12 C18 121.7(5) . . ?
C15 N12 C18 125.4(6) . . ?
C1 O1 Yb1 160.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.022
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.091

# 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 0.000 792 268 ' '
2 0.500 0.149 0.500 793 268 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997819'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_15Lu
_publ_requested_journal_name     CrystEngComm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H56 Lu N24 O18, 2(N O3), Cl, 15(H2 O)'
_chemical_formula_sum            'C40 H86 Cl Lu N26 O39'
_chemical_formula_weight         1765.77

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           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   35.247(13)
_cell_length_b                   14.129(5)
_cell_length_c                   13.384(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6665(4)
_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          0.25
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3632
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_T_max  0.7038
_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            44595
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.16
_diffrn_reflns_theta_max         25.20
_reflns_number_total             6235
_reflns_number_gt                3983
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0768P)²+3.6066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6235
_refine_ls_number_parameters     445
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1512
_refine_ls_wR_factor_gt          0.1387
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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 0.2664(3) -0.2500 0.9061(8) 0.279(4) Uani 1 2 d S . .
O5W O 0.2762(2) -0.2500 1.1147(6) 0.081(2) Uani 1 2 d S . .
O1W O 0.15576(13) 0.1273(3) 0.4966(3) 0.0482(11) Uani 1 1 d . . .
O2W O 0.14148(18) 0.2500 0.3363(5) 0.0591(18) Uani 1 2 d S . .
O3W O 0.14738(17) 0.2500 0.6509(4) 0.0495(16) Uani 1 2 d S . .
O4W O 0.07681(14) 0.1485(4) 0.4047(3) 0.0701(15) Uani 1 1 d . . .
Lu1 Lu 0.113678(10) 0.2500 0.50039(2) 0.03530(15) Uani 1 2 d S . .
N13 N 0.1183(3) -0.2500 1.0832(11) 0.079(3) Uani 1 2 d S . .
N14 N 0.13126(19) -0.2500 0.6578(5) 0.070(2) Uani 1 2 d SD . .
O7 O 0.1016(4) -0.2500 1.0006(7) 0.117(4) Uani 1 2 d S . .
O8 O 0.0997(3) -0.2500 1.1623(8) 0.123(4) Uani 1 2 d S . .
O9 O 0.1531(3) -0.2500 1.0925(11) 0.144(5) Uani 1 2 d S . .
O10 O 0.09696(19) -0.2500 0.6814(6) 0.074(2) Uani 1 2 d SD . .
O11 O 0.1568(2) -0.2500 0.7226(6) 0.092(3) Uani 1 2 d SD . .
O12 O 0.1397(3) -0.2500 0.5673(6) 0.240(10) Uani 1 2 d SD . .
C1 C 0.05972(17) 0.1224(4) 0.6691(4) 0.0400(15) Uani 1 1 d . . .
C2 C 0.00884(17) 0.1146(5) 0.7795(4) 0.0483(17) Uani 1 1 d . . .
C3 C 0.03376(17) 0.0235(5) 0.7918(4) 0.0485(17) Uani 1 1 d . . .
C4 C 0.03269(17) 0.1090(5) 0.9431(4) 0.0470(17) Uani 1 1 d . . .
C5 C 0.09483(18) -0.0219(4) 0.6957(4) 0.0413(15) Uani 1 1 d . . .
H5A H 0.1049 -0.0031 0.6303 0.050 Uiso 1 1 calc R . .
H5B H 0.0830 -0.0842 0.6880 0.050 Uiso 1 1 calc R . .
C6 C 0.0639(2) -0.0450(5) 0.9519(5) 0.0559(18) Uani 1 1 d . . .
H6A H 0.0550 -0.1071 0.9293 0.067 Uiso 1 1 calc R . .
H6B H 0.0580 -0.0394 1.0232 0.067 Uiso 1 1 calc R . .
C7 C 0.16358(19) -0.0137(4) 0.7395(4) 0.0419(15) Uani 1 1 d . . .
C8 C 0.12386(18) -0.0881(4) 0.8555(4) 0.0420(15) Uani 1 1 d . . .
H8 H 0.1130 -0.1512 0.8413 0.050 Uiso 1 1 calc R . .
C9 C 0.16539(18) -0.0938(4) 0.8902(4) 0.0450(16) Uani 1 1 d . . .
H9 H 0.1737 -0.1604 0.8970 0.054 Uiso 1 1 calc R . .
C10 C 0.1289(2) -0.0254(5) 1.0166(5) 0.0490(17) Uani 1 1 d . . .
C11 C 0.22674(19) -0.0409(5) 0.8095(4) 0.0513(17) Uani 1 1 d . . .
H11A H 0.2348 -0.0305 0.7403 0.062 Uiso 1 1 calc R . .
H11B H 0.2373 -0.1015 0.8315 0.062 Uiso 1 1 calc R . .
C12 C 0.19651(18) -0.0524(5) 1.0585(4) 0.0479(16) Uani 1 1 d . . .
H12A H 0.1864 -0.0516 1.1267 0.057 Uiso 1 1 calc R . .
H12B H 0.2099 -0.1125 1.0488 0.057 Uiso 1 1 calc R . .
C13 C 0.25892(18) 0.1121(5) 0.8267(5) 0.0496(17) Uani 1 1 d . . .
C14 C 0.2537(2) 0.0243(5) 0.9752(5) 0.0514(18) Uani 1 1 d . . .
H14 H 0.2707 -0.0308 0.9848 0.062 Uiso 1 1 calc R . .
C15 C 0.27414(19) 0.1186(5) 0.9987(4) 0.0495(16) Uani 1 1 d . . .
H15 H 0.2998 0.1083 1.0270 0.059 Uiso 1 1 calc R . .
C16 C 0.2206(2) 0.1070(5) 1.0968(5) 0.0504(17) Uani 1 1 d . . .
C17 C 0.2982(3) 0.2500 0.8779(7) 0.060(3) Uani 1 2 d S . .
H17A H 0.3055 0.2500 0.8073 0.071 Uiso 1 2 calc SR . .
H17B H 0.3214 0.2500 0.9183 0.071 Uiso 1 2 calc SR . .
C18 C 0.2575(3) 0.2500 1.1255(7) 0.051(2) Uani 1 2 d S . .
H18A H 0.2843 0.2500 1.1448 0.061 Uiso 1 2 calc SR . .
H18B H 0.2423 0.2500 1.1868 0.061 Uiso 1 2 calc SR . .
C19 C -0.0049(3) 0.2500 0.9075(6) 0.049(2) Uani 1 2 d S . .
H19A H -0.0309 0.2500 0.8812 0.059 Uiso 1 2 calc SR . .
H19B H -0.0066 0.2500 0.9806 0.059 Uiso 1 2 calc SR . .
C20 C 0.0132(2) 0.2500 0.6499(6) 0.044(2) Uani 1 2 d S . .
H20A H 0.0210 0.2500 0.5796 0.053 Uiso 1 2 calc SR . .
H20B H -0.0146 0.2500 0.6514 0.053 Uiso 1 2 calc SR . .
C21 C -0.0335(2) 0.0952(6) 0.7581(5) 0.073(2) Uani 1 1 d . . .
H21A H -0.0448 0.0636 0.8152 0.110 Uiso 1 1 calc R . .
H21B H -0.0357 0.0552 0.6996 0.110 Uiso 1 1 calc R . .
H21C H -0.0465 0.1547 0.7462 0.110 Uiso 1 1 calc R . .
C22 C 0.0163(2) -0.0721(6) 0.7647(5) 0.079(3) Uani 1 1 d . . .
H22A H -0.0051 -0.0848 0.8085 0.118 Uiso 1 1 calc R . .
H22B H 0.0351 -0.1215 0.7724 0.118 Uiso 1 1 calc R . .
H22C H 0.0076 -0.0706 0.6960 0.118 Uiso 1 1 calc R . .
N1 N 0.02662(12) 0.1631(3) 0.6959(3) 0.0352(11) Uani 1 1 d . . .
N2 N 0.06650(14) 0.0444(3) 0.7250(3) 0.0378(12) Uani 1 1 d . . .
N3 N 0.01394(14) 0.1632(4) 0.8756(3) 0.0463(13) Uani 1 1 d . . .
N4 N 0.04375(14) 0.0273(4) 0.8983(3) 0.0440(13) Uani 1 1 d . . .
N5 N 0.12664(15) -0.0299(4) 0.7668(3) 0.0414(12) Uani 1 1 d . . .
N6 N 0.18584(16) -0.0465(4) 0.8123(3) 0.0467(13) Uani 1 1 d . . .
N7 N 0.10435(16) -0.0401(4) 0.9389(4) 0.0499(14) Uani 1 1 d . . .
N8 N 0.16509(17) -0.0460(4) 0.9872(3) 0.0484(14) Uani 1 1 d . . .
N9 N 0.24214(15) 0.0343(4) 0.8718(4) 0.0479(13) Uani 1 1 d . . .
N10 N 0.27556(15) 0.1648(4) 0.9003(4) 0.0508(14) Uani 1 1 d . . .
N11 N 0.22293(15) 0.0248(4) 1.0465(4) 0.0459(13) Uani 1 1 d . . .
N12 N 0.24925(14) 0.1635(4) 1.0682(4) 0.0464(13) Uani 1 1 d . . .
O1 O 0.08108(11) 0.1509(3) 0.6025(3) 0.0394(10) Uani 1 1 d . . .
O2 O 0.17425(12) 0.0215(3) 0.6602(3) 0.0518(12) Uani 1 1 d . . .
O3 O 0.25899(13) 0.1296(3) 0.7382(3) 0.0585(13) Uani 1 1 d . . .
O4 O 0.03773(14) 0.1272(4) 1.0320(3) 0.0623(14) Uani 1 1 d . . .
O5 O 0.11937(14) 0.0012(4) 1.1014(4) 0.0679(15) Uani 1 1 d . . .
O6 O 0.19680(13) 0.1258(3) 1.1614(3) 0.0599(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1W Lu1 2.282(4) . ?
O2W Lu1 2.405(6) . ?
O3W Lu1 2.339(5) . ?
O4W Lu1 2.320(4) . ?
Lu1 O1 2.269(4) . ?
Lu1 O1 2.269(4) 7_565 ?
Lu1 O1W 2.282(4) 7_565 ?
Lu1 O4W 2.320(4) 7_565 ?
N13 O9 1.232(12) . ?
N13 O8 1.244(12) . ?
N13 O7 1.253(14) . ?
N14 O12 1.248(2) . ?
N14 O10 1.249(2) . ?
N14 O11 1.249(2) . ?
C1 O1 1.234(7) . ?
C1 N1 1.349(7) . ?
C1 N2 1.353(7) . ?
C2 N1 1.454(7) . ?
C2 N3 1.468(7) . ?
C2 C21 1.543(9) . ?
C2 C3 1.567(10) . ?
C3 N4 1.470(7) . ?
C3 N2 1.489(7) . ?
C3 C22 1.528(9) . ?
C4 O4 1.230(7) . ?
C4 N3 1.357(7) . ?
C4 N4 1.358(8) . ?
C5 N2 1.424(7) . ?
C5 N5 1.475(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N4 1.436(8) . ?
C6 N7 1.438(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 O2 1.231(7) . ?
C7 N6 1.334(7) . ?
C7 N5 1.371(8) . ?
C8 N5 1.447(7) . ?
C8 N7 1.475(8) . ?
C8 C9 1.538(8) . ?
C8 H8 0.9900 . ?
C9 N6 1.433(7) . ?
C9 N8 1.464(7) . ?
C9 H9 0.9900 . ?
C10 O5 1.241(7) . ?
C10 N8 1.367(9) . ?
C10 N7 1.368(9) . ?
C11 N6 1.444(8) . ?
C11 N9 1.456(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 N11 1.444(8) . ?
C12 N8 1.464(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 O3 1.210(7) . ?
C13 N10 1.367(8) . ?
C13 N9 1.386(8) . ?
C14 N11 1.445(8) . ?
C14 N9 1.449(8) . ?
C14 C15 1.546(10) . ?
C14 H14 0.9900 . ?
C15 N12 1.428(8) . ?
C15 N10 1.470(7) . ?
C15 H15 0.9900 . ?
C16 O6 1.234(7) . ?
C16 N12 1.343(8) . ?
C16 N11 1.345(8) . ?
C17 N10 1.476(7) . ?
C17 N10 1.476(7) 7_565 ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 N12 1.472(7) . ?
C18 N12 1.472(7) 7_565 ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 N3 1.460(6) 7_565 ?
C19 N3 1.460(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 N1 1.454(6) 7_565 ?
C20 N1 1.454(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Lu1 O1 76.20(19) . 7_565 ?
O1 Lu1 O1W 144.23(13) . 7_565 ?
O1 Lu1 O1W 82.75(15) 7_565 7_565 ?
O1 Lu1 O1W 82.75(15) . . ?
O1 Lu1 O1W 144.23(13) 7_565 . ?
O1W Lu1 O1W 98.9(2) 7_565 . ?
O1 Lu1 O4W 70.58(16) . . ?
O1 Lu1 O4W 115.47(18) 7_565 . ?
O1W Lu1 O4W 145.19(14) 7_565 . ?
O1W Lu1 O4W 83.23(18) . . ?
O1 Lu1 O4W 115.47(18) . 7_565 ?
O1 Lu1 O4W 70.58(16) 7_565 7_565 ?
O1W Lu1 O4W 83.23(18) 7_565 7_565 ?
O1W Lu1 O4W 145.19(14) . 7_565 ?
O4W Lu1 O4W 76.3(3) . 7_565 ?
O1 Lu1 O3W 74.83(15) . . ?
O1 Lu1 O3W 74.83(15) 7_565 . ?
O1W Lu1 O3W 71.90(13) 7_565 . ?
O1W Lu1 O3W 71.90(13) . . ?
O4W Lu1 O3W 139.45(13) . . ?
O4W Lu1 O3W 139.45(13) 7_565 . ?
O1 Lu1 O2W 139.15(11) . . ?
O1 Lu1 O2W 139.15(11) 7_565 . ?
O1W Lu1 O2W 73.43(13) 7_565 . ?
O1W Lu1 O2W 73.43(13) . . ?
O4W Lu1 O2W 73.99(16) . . ?
O4W Lu1 O2W 73.99(16) 7_565 . ?
O3W Lu1 O2W 125.4(2) . . ?
O9 N13 O8 116.0(14) . . ?
O9 N13 O7 123.7(13) . . ?
O8 N13 O7 120.3(13) . . ?
O12 N14 O10 118.4(8) . . ?
O12 N14 O11 120.2(8) . . ?
O10 N14 O11 121.4(8) . . ?
O1 C1 N1 125.5(6) . . ?
O1 C1 N2 123.9(6) . . ?
N1 C1 N2 110.6(5) . . ?
N1 C2 N3 113.6(5) . . ?
N1 C2 C21 110.9(5) . . ?
N3 C2 C21 111.3(5) . . ?
N1 C2 C3 103.1(5) . . ?
N3 C2 C3 102.9(5) . . ?
C21 C2 C3 114.5(6) . . ?
N4 C3 N2 112.9(5) . . ?
N4 C3 C22 111.1(5) . . ?
N2 C3 C22 110.3(5) . . ?
N4 C3 C2 101.9(5) . . ?
N2 C3 C2 102.0(5) . . ?
C22 C3 C2 118.3(6) . . ?
O4 C4 N3 126.7(7) . . ?
O4 C4 N4 124.3(6) . . ?
N3 C4 N4 109.0(5) . . ?
N2 C5 N5 113.9(4) . . ?
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 113.3(5) . . ?
N4 C6 H6A 108.9 . . ?
N7 C6 H6A 108.9 . . ?
N4 C6 H6B 108.9 . . ?
N7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N6 126.2(6) . . ?
O2 C7 N5 125.9(6) . . ?
N6 C7 N5 107.8(5) . . ?
N5 C8 N7 113.1(5) . . ?
N5 C8 C9 102.3(5) . . ?
N7 C8 C9 103.9(5) . . ?
N5 C8 H8 112.3 . . ?
N7 C8 H8 112.3 . . ?
C9 C8 H8 112.3 . . ?
N6 C9 N8 115.7(5) . . ?
N6 C9 C8 103.5(5) . . ?
N8 C9 C8 103.7(5) . . ?
N6 C9 H9 111.1 . . ?
N8 C9 H9 111.1 . . ?
C8 C9 H9 111.1 . . ?
O5 C10 N8 125.4(7) . . ?
O5 C10 N7 124.8(7) . . ?
N8 C10 N7 109.8(5) . . ?
N6 C11 N9 113.4(5) . . ?
N6 C11 H11A 108.9 . . ?
N9 C11 H11A 108.9 . . ?
N6 C11 H11B 108.9 . . ?
N9 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N11 C12 N8 111.7(5) . . ?
N11 C12 H12A 109.3 . . ?
N8 C12 H12A 109.3 . . ?
N11 C12 H12B 109.3 . . ?
N8 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
O3 C13 N10 126.4(7) . . ?
O3 C13 N9 126.1(6) . . ?
N10 C13 N9 107.5(5) . . ?
N11 C14 N9 114.7(5) . . ?
N11 C14 C15 102.2(5) . . ?
N9 C14 C15 104.0(5) . . ?
N11 C14 H14 111.8 . . ?
N9 C14 H14 111.8 . . ?
C15 C14 H14 111.8 . . ?
N12 C15 N10 114.0(5) . . ?
N12 C15 C14 103.3(5) . . ?
N10 C15 C14 102.5(5) . . ?
N12 C15 H15 112.1 . . ?
N10 C15 H15 112.1 . . ?
C14 C15 H15 112.1 . . ?
O6 C16 N12 125.7(7) . . ?
O6 C16 N11 125.3(7) . . ?
N12 C16 N11 108.9(6) . . ?
N10 C17 N10 109.4(7) . 7_565 ?
N10 C17 H17A 109.8 . . ?
N10 C17 H17A 109.8 7_565 . ?
N10 C17 H17B 109.8 . . ?
N10 C17 H17B 109.8 7_565 . ?
H17A C17 H17B 108.2 . . ?
N12 C18 N12 112.2(7) . 7_565 ?
N12 C18 H18A 109.2 . . ?
N12 C18 H18A 109.2 7_565 . ?
N12 C18 H18B 109.2 . . ?
N12 C18 H18B 109.2 7_565 . ?
H18A C18 H18B 107.9 . . ?
N3 C19 N3 114.3(7) 7_565 . ?
N3 C19 H19A 108.7 7_565 . ?
N3 C19 H19A 108.7 . . ?
N3 C19 H19B 108.7 7_565 . ?
N3 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
N1 C20 N1 115.4(6) 7_565 . ?
N1 C20 H20A 108.4 7_565 . ?
N1 C20 H20A 108.4 . . ?
N1 C20 H20B 108.4 7_565 . ?
N1 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C3 C22 H22A 109.5 . . ?
C3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 N1 C20 121.8(5) . . ?
C1 N1 C2 112.2(5) . . ?
C20 N1 C2 125.8(5) . . ?
C1 N2 C5 120.4(5) . . ?
C1 N2 C3 110.9(5) . . ?
C5 N2 C3 125.3(5) . . ?
C4 N3 C19 120.1(6) . . ?
C4 N3 C2 112.3(5) . . ?
C19 N3 C2 126.4(6) . . ?
C4 N4 C6 121.8(5) . . ?
C4 N4 C3 113.0(5) . . ?
C6 N4 C3 125.2(6) . . ?
C7 N5 C8 112.2(5) . . ?
C7 N5 C5 122.5(5) . . ?
C8 N5 C5 121.5(5) . . ?
C7 N6 C9 113.4(5) . . ?
C7 N6 C11 123.3(5) . . ?
C9 N6 C11 123.1(5) . . ?
C10 N7 C6 122.8(5) . . ?
C10 N7 C8 110.5(6) . . ?
C6 N7 C8 122.1(5) . . ?
C10 N8 C9 111.1(5) . . ?
C10 N8 C12 122.1(5) . . ?
C9 N8 C12 122.9(5) . . ?
C13 N9 C14 111.9(5) . . ?
C13 N9 C11 119.2(5) . . ?
C14 N9 C11 125.5(5) . . ?
C13 N10 C15 112.9(6) . . ?
C13 N10 C17 122.0(6) . . ?
C15 N10 C17 124.3(6) . . ?
C16 N11 C12 123.9(6) . . ?
C16 N11 C14 112.4(6) . . ?
C12 N11 C14 123.6(5) . . ?
C16 N12 C15 112.5(6) . . ?
C16 N12 C18 119.6(6) . . ?
C15 N12 C18 126.0(6) . . ?
C1 O1 Lu1 160.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.099


# 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 0.150 0.500 776 283 ' '
2 0.500 0.082 0.000 776 283 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 997820'
