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

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

data_1p
_database_code_depnum_ccdc_archive 'CCDC 1038157'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

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 -0.344 1.329 0.156 2155 885 ' '
2 0.000 0.500 0.500 120 46 ' '
3 0.143 0.064 0.528 26 11 ' '
4 0.357 0.564 0.972 26 11 ' '
5 0.500 0.000 0.000 113 45 ' '
6 0.643 0.436 0.028 26 11 ' '
7 0.857 0.936 0.472 26 11 ' '



_platon_squeeze_details          ?

_vrf_PLAT306_1p                  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O5w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_1p                  
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C120 H126 La2 N72 O44, 4(N O3), 38(O)
;
_chemical_formula_sum            'C120 H126 La2 N76 O94'
_chemical_formula_weight         4414.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.400(2)
_cell_length_b                   17.150(3)
_cell_length_c                   35.343(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.279(2)
_cell_angle_gamma                90
_cell_volume                     9319(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5974
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      20.30

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             4488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.575
_shelx_estimated_absorpt_T_min   0.889
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63492
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.154
_diffrn_reflns_theta_max         26.272
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             17309
_reflns_number_gt                10333
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1693P)²+34.1375P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17309
_refine_ls_number_parameters     1185
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0911
_refine_ls_wR_factor_ref         0.2966
_refine_ls_wR_factor_gt          0.2470
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O5W O 0.7771(8) 0.6666(8) 1.0330(4) 0.128(4) Uiso 1 1 d . . . . .
O21 O 0.6750(7) 0.7040(6) 1.1601(3) 0.092(3) Uiso 1 1 d . . . . .
O20 O 0.5994(10) 0.7635(9) 1.2026(4) 0.140(5) Uiso 1 1 d . . . . .
O22 O 0.6837(9) 0.6655(8) 1.2184(4) 0.138(5) Uiso 1 1 d . . . . .
N40 N 0.6520(10) 0.7122(9) 1.1897(5) 0.111(4) Uiso 1 1 d . . . . .
O23 O 0.9833(10) 0.8652(9) 1.0316(4) 0.150(5) Uiso 1 1 d . . . . .
N41 N 1.0295(11) 0.8113(9) 1.0165(5) 0.117(5) Uiso 1 1 d . . . . .
O24 O 1.0392(10) 0.7996(9) 0.9814(4) 0.146(5) Uiso 1 1 d . . . . .
O6W O 0.2954(7) 0.9197(6) 0.6511(3) 0.097(3) Uiso 1 1 d . . . . .
O25 O 1.0863(9) 0.7878(8) 1.0434(4) 0.133(4) Uiso 1 1 d . . . . .
O7W O 0.7543(7) 0.9938(7) 0.7503(3) 0.101(3) Uiso 1 1 d . . . . .
O10W O 1.0171(8) 0.5381(7) 0.7050(4) 0.124(4) Uiso 1 1 d . . . . .
O9W O 0.1268(8) 0.6521(8) 0.7736(4) 0.127(4) Uiso 1 1 d . . . . .
O8W O 0.9848(10) 0.7967(9) 1.1045(4) 0.155(5) Uiso 1 1 d . . . . .
O11W O 1.1141(9) 0.3320(9) 0.9028(4) 0.143(5) Uiso 1 1 d . . . . .
O14W O 0.3892(10) 0.5622(9) 0.6314(4) 0.154(5) Uiso 1 1 d . . . . .
O13W O 0.1673(11) 0.4907(10) 0.7775(5) 0.173(6) Uiso 1 1 d . . . . .
O12W O 0.3618(11) 0.7585(10) 0.9724(4) 0.163(5) Uiso 1 1 d . . . . .
O15W O 0.8134(9) 0.3103(9) 1.0158(4) 0.145(5) Uiso 1 1 d . . . . .
O16W O 0.8730(11) 1.1845(10) 1.0860(5) 0.169(6) Uiso 1 1 d . . . . .
O17W O 0.6973(11) 0.5412(10) 0.8252(5) 0.180(6) Uiso 1 1 d . . . . .
O18W O 1.2679(13) 0.5498(12) 0.8887(5) 0.202(7) Uiso 1 1 d . . . . .
O19W O 0.2258(13) 0.7113(11) 0.8791(6) 0.206(8) Uiso 1 1 d . . . . .
O21W O 0.6800(12) 1.0706(11) 1.2053(5) 0.189(7) Uiso 1 1 d . . . . .
O20W O 0.5443(15) 0.6096(14) 1.0134(7) 0.243(9) Uiso 1 1 d . . . . .
O22W O 0.9391(19) 1.0911(17) 1.1457(8) 0.304(13) Uiso 1 1 d . . . . .
O23W O 0.8325(18) 1.1854(16) 1.1962(8) 0.284(12) Uiso 1 1 d . . . . .
C1 C 0.4405(5) 0.7520(5) 0.7812(2) 0.0323(19) Uani 1 1 d . . . . .
C2 C 0.5383(6) 0.8422(5) 0.7506(2) 0.034(2) Uani 1 1 d . . . . .
H2A H 0.5299 0.8691 0.7265 0.041 Uiso 1 1 calc R U . . .
H2B H 0.5206 0.8773 0.7702 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6731(5) 0.8263(5) 0.7918(2) 0.0277(18) Uani 1 1 d . . . . .
C4 C 0.8254(6) 0.8384(5) 0.8166(2) 0.036(2) Uani 1 1 d . . . . .
H4A H 0.8638 0.8756 0.8054 0.043 Uiso 1 1 calc R U . . .
H4B H 0.7974 0.8646 0.8370 0.043 Uiso 1 1 calc R U . . .
C5 C 0.8782(6) 0.7566(5) 0.8696(2) 0.0323(19) Uani 1 1 d . . . . .
C6 C 0.9718(6) 0.6779(5) 0.9150(2) 0.037(2) Uani 1 1 d . . . . .
H6A H 1.0348 0.6779 0.9179 0.045 Uiso 1 1 calc R U . . .
H6B H 0.9506 0.7149 0.9330 0.045 Uiso 1 1 calc R U . . .
C7 C 0.8742(6) 0.5941(5) 0.9469(2) 0.033(2) Uani 1 1 d . . . . .
C8 C 0.7860(6) 0.4897(5) 0.9712(2) 0.037(2) Uani 1 1 d . . . . .
H8A H 0.7679 0.5293 0.9888 0.044 Uiso 1 1 calc R U . . .
H8B H 0.8007 0.4433 0.9859 0.044 Uiso 1 1 calc R U . . .
C9 C 0.6457(6) 0.5216(5) 0.9373(2) 0.034(2) Uani 1 1 d . . . . .
C10 C 0.4955(6) 0.5167(5) 0.9101(2) 0.034(2) Uani 1 1 d . . . . .
H10A H 0.4551 0.4816 0.9215 0.041 Uiso 1 1 calc R U . . .
H10B H 0.4936 0.5662 0.9233 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4399(5) 0.5988(4) 0.8569(2) 0.0285(18) Uani 1 1 d . . . . .
C12 C 0.3475(5) 0.6519(5) 0.8037(2) 0.035(2) Uani 1 1 d . . . . .
H12A H 0.2936 0.6302 0.7928 0.041 Uiso 1 1 calc R U . . .
H12B H 0.3326 0.6911 0.8221 0.041 Uiso 1 1 calc R U . . .
C13 C 0.4601(6) 0.7235(5) 0.7174(2) 0.036(2) Uani 1 1 d . . . . .
C14 C 0.4152(7) 0.7715(6) 0.6862(3) 0.047(2) Uani 1 1 d . . . . .
H14A H 0.4542 0.8109 0.6781 0.071 Uiso 1 1 calc R U . . .
H14B H 0.3645 0.7958 0.6955 0.071 Uiso 1 1 calc R U . . .
H14C H 0.3982 0.7382 0.6652 0.071 Uiso 1 1 calc R U . . .
C15 C 0.6857(5) 0.8098(5) 0.7274(2) 0.0304(19) Uani 1 1 d . . . . .
H15 H 0.6806 0.8498 0.7076 0.036 Uiso 1 1 calc R U . . .
C16 C 0.7786(5) 0.8080(5) 0.7477(2) 0.0279(18) Uani 1 1 d . . . . .
H16 H 0.8150 0.8513 0.7398 0.033 Uiso 1 1 calc R U . . .
C17 C 0.9494(6) 0.7399(5) 0.8127(2) 0.0334(19) Uani 1 1 d . . . . .
H17 H 0.9901 0.7795 0.8044 0.040 Uiso 1 1 calc R U . . .
C18 C 0.9906(6) 0.6865(5) 0.8441(2) 0.0311(19) Uani 1 1 d . . . . .
H18 H 1.0532 0.6960 0.8480 0.037 Uiso 1 1 calc R U . . .
C19 C 0.9825(6) 0.5294(5) 0.9158(2) 0.0323(19) Uani 1 1 d . . . . .
C20 C 1.0785(6) 0.5304(7) 0.9300(3) 0.049(3) Uani 1 1 d . . . . .
H20A H 1.1105 0.5641 0.9142 0.074 Uiso 1 1 calc R U . . .
H20B H 1.1017 0.4785 0.9291 0.074 Uiso 1 1 calc R U . . .
H20C H 1.0832 0.5492 0.9557 0.074 Uiso 1 1 calc R U . . .
C21 C 0.9244(6) 0.4674(5) 0.9360(2) 0.034(2) Uani 1 1 d . . . . .
C22 C 0.9706(7) 0.4123(6) 0.9647(3) 0.048(2) Uani 1 1 d . . . . .
H22A H 1.0031 0.4422 0.9835 0.071 Uiso 1 1 calc R U . . .
H22B H 1.0094 0.3789 0.9518 0.071 Uiso 1 1 calc R U . . .
H22C H 0.9282 0.3811 0.9766 0.071 Uiso 1 1 calc R U . . .
C23 C 0.6918(5) 0.3928(5) 0.9330(2) 0.0300(18) Uani 1 1 d . . . . .
H23 H 0.6931 0.3568 0.9546 0.036 Uiso 1 1 calc R U . . .
C24 C 0.5978(6) 0.4010(5) 0.9140(2) 0.0298(18) Uani 1 1 d . . . . .
H24 H 0.5550 0.3720 0.9279 0.036 Uiso 1 1 calc R U . . .
C25 C 0.4324(5) 0.4649(5) 0.8466(2) 0.0286(18) Uani 1 1 d . . . . .
H25 H 0.3888 0.4343 0.8593 0.034 Uiso 1 1 calc R U . . .
C26 C 0.3916(6) 0.5088(5) 0.8118(2) 0.0318(19) Uani 1 1 d . . . . .
H26 H 0.3314 0.4924 0.8058 0.038 Uiso 1 1 calc R U . . .
C27 C 0.4009(6) 0.6593(5) 0.7357(2) 0.034(2) Uani 1 1 d . . . . .
C28 C 0.3129(6) 0.6457(6) 0.7158(3) 0.049(2) Uani 1 1 d . . . . .
H28A H 0.2805 0.6093 0.7301 0.073 Uiso 1 1 calc R U . . .
H28B H 0.3204 0.6249 0.6910 0.073 Uiso 1 1 calc R U . . .
H28C H 0.2818 0.6942 0.7136 0.073 Uiso 1 1 calc R U . . .
C29 C 0.5297(6) 0.6021(5) 0.7158(2) 0.034(2) Uani 1 1 d . . . . .
C30 C 0.6062(6) 0.7102(5) 0.6861(2) 0.036(2) Uani 1 1 d . . . . .
H30A H 0.6262 0.6717 0.6684 0.044 Uiso 1 1 calc R U . . .
H30B H 0.5871 0.7557 0.6716 0.044 Uiso 1 1 calc R U . . .
C31 C 0.7555(6) 0.6932(5) 0.7140(2) 0.032(2) Uani 1 1 d . . . . .
C32 C 0.9029(6) 0.7116(5) 0.7444(2) 0.0333(19) Uani 1 1 d . . . . .
H32A H 0.9164 0.6700 0.7271 0.040 Uiso 1 1 calc R U . . .
H32B H 0.9396 0.7558 0.7391 0.040 Uiso 1 1 calc R U . . .
C33 C 0.9392(5) 0.6105(5) 0.7924(2) 0.0307(19) Uani 1 1 d . . . . .
C34 C 1.0162(6) 0.5397(5) 0.8454(2) 0.036(2) Uani 1 1 d . . . . .
H34A H 1.0203 0.5011 0.8255 0.043 Uiso 1 1 calc R U . . .
H34B H 1.0749 0.5538 0.8541 0.043 Uiso 1 1 calc R U . . .
C35 C 0.9195(6) 0.4419(5) 0.8701(2) 0.034(2) Uani 1 1 d . . . . .
C36 C 0.8343(6) 0.3519(5) 0.9063(2) 0.037(2) Uani 1 1 d . . . . .
H36A H 0.8502 0.3159 0.8866 0.044 Uiso 1 1 calc R U . . .
H36B H 0.8491 0.3275 0.9305 0.044 Uiso 1 1 calc R U . . .
C37 C 0.6909(6) 0.3465(5) 0.8704(2) 0.0308(19) Uani 1 1 d . . . . .
C38 C 0.5354(6) 0.3497(5) 0.8506(2) 0.034(2) Uani 1 1 d . . . . .
H38A H 0.4912 0.3239 0.8645 0.041 Uiso 1 1 calc R U . . .
H38B H 0.5553 0.3129 0.8321 0.041 Uiso 1 1 calc R U . . .
C39 C 0.5035(6) 0.4278(5) 0.7930(2) 0.0326(19) Uani 1 1 d . . . . .
C40 C 0.4291(6) 0.5100(5) 0.7434(2) 0.038(2) Uani 1 1 d . . . . .
H40A H 0.3670 0.5059 0.7373 0.045 Uiso 1 1 calc R U . . .
H40B H 0.4580 0.4737 0.7272 0.045 Uiso 1 1 calc R U . . .
C41 C 0.7058(5) 0.9124(5) 0.9182(2) 0.0263(17) Uani 1 1 d . . . . .
C42 C 0.7688(6) 0.8448(5) 0.9738(2) 0.035(2) Uani 1 1 d . . . . .
H42A H 0.7407 0.8007 0.9610 0.043 Uiso 1 1 calc R U . . .
H42B H 0.8300 0.8324 0.9779 0.043 Uiso 1 1 calc R U . . .
C43 C 0.6643(6) 0.8109(5) 1.0206(2) 0.039(2) Uani 1 1 d . . . . .
C44 C 0.5966(6) 0.7759(5) 1.0798(3) 0.041(2) Uani 1 1 d . . . . .
H44A H 0.6289 0.7563 1.1022 0.049 Uiso 1 1 calc R U . . .
H44B H 0.5778 0.7313 1.0646 0.049 Uiso 1 1 calc R U . . .
C45 C 0.4392(7) 0.8022(5) 1.0760(3) 0.042(2) Uani 1 1 d . . . . .
C46 C 0.2887(7) 0.8375(5) 1.0896(3) 0.058(3) Uani 1 1 d . . . . .
H46A H 0.2615 0.8332 1.1136 0.069 Uiso 1 1 calc R U . . .
H46B H 0.2738 0.7910 1.0750 0.069 Uiso 1 1 calc R U . . .
C47 C 0.9141(6) 0.9491(7) 0.9475(3) 0.049(3) Uani 1 1 d . . . . .
H47A H 0.9295 0.9186 0.9696 0.074 Uiso 1 1 calc R U . . .
H47B H 0.9529 0.9928 0.9464 0.074 Uiso 1 1 calc R U . . .
H47C H 0.9187 0.9175 0.9253 0.074 Uiso 1 1 calc R U . . .
C48 C 0.8218(6) 0.9781(5) 0.9493(2) 0.035(2) Uani 1 1 d . . . . .
C49 C 0.7770(6) 0.8935(5) 1.0425(2) 0.038(2) Uani 1 1 d . . . . .
H49 H 0.8363 0.8734 1.0468 0.046 Uiso 1 1 calc R U . . .
C50 C 0.7197(6) 0.8721(5) 1.0757(2) 0.038(2) Uani 1 1 d . . . . .
H50 H 0.7533 0.8453 1.0962 0.045 Uiso 1 1 calc R U . . .
C51 C 0.5196(6) 0.8661(5) 1.1249(2) 0.035(2) Uani 1 1 d . . . . .
H51 H 0.5459 0.8398 1.1473 0.042 Uiso 1 1 calc R U . . .
C52 C 0.4218(6) 0.8806(5) 1.1286(3) 0.040(2) Uani 1 1 d . . . . .
H52 H 0.4025 0.8607 1.1527 0.048 Uiso 1 1 calc R U . . .
C53 C 0.2140(6) 0.9730(5) 1.0860(2) 0.038(2) Uani 1 1 d D . . . .
C54 C 0.1458(6) 0.9519(7) 1.1160(3) 0.059(3) Uani 1 1 d D . . . .
C55 C 0.7654(6) 1.0974(6) 0.9693(3) 0.047(2) Uani 1 1 d . . . . .
C56 C 0.8362(6) 1.0211(6) 1.0201(3) 0.044(2) Uani 1 1 d . . . . .
H56A H 0.8919 0.9946 1.0218 0.053 Uiso 1 1 calc R U . . .
H56B H 0.8443 1.0718 1.0320 0.053 Uiso 1 1 calc R U . . .
C57 C 0.7269(6) 1.0068(6) 1.0682(3) 0.042(2) Uani 1 1 d . . . . .
C58 C 0.6467(6) 0.9607(6) 1.1228(2) 0.042(2) Uani 1 1 d . . . . .
H58A H 0.6747 0.9282 1.1423 0.051 Uiso 1 1 calc R U . . .
H58B H 0.6548 1.0146 1.1304 0.051 Uiso 1 1 calc R U . . .
C59 C 0.4935(6) 1.0005(5) 1.1245(2) 0.0321(19) Uani 1 1 d . . . . .
C60 C 0.3365(6) 1.0051(5) 1.1366(2) 0.034(2) Uani 1 1 d . . . . .
H60A H 0.3048 0.9724 1.1535 0.041 Uiso 1 1 calc R U . . .
H60B H 0.3531 1.0523 1.1503 0.041 Uiso 1 1 calc R U . . .
N1 N 0.4826(5) 0.7738(4) 0.74998(18) 0.0329(16) Uani 1 1 d . . . . .
N2 N 0.6300(4) 0.8247(4) 0.75728(18) 0.0302(15) Uani 1 1 d . . . . .
N3 N 0.7590(5) 0.8138(4) 0.78796(18) 0.0302(16) Uani 1 1 d . . . . .
N4 N 0.8763(5) 0.7742(4) 0.83214(19) 0.0340(16) Uani 1 1 d . . . . .
N5 N 0.9463(5) 0.7047(4) 0.87714(19) 0.0355(17) Uani 1 1 d . . . . .
N6 N 0.9410(5) 0.6017(4) 0.92421(19) 0.0348(17) Uani 1 1 d . . . . .
N7 N 0.8623(5) 0.5165(4) 0.95441(18) 0.0331(16) Uani 1 1 d . . . . .
N8 N 0.7127(5) 0.4716(4) 0.94497(18) 0.0334(17) Uani 1 1 d . . . . .
N9 N 0.5827(5) 0.4847(4) 0.91530(18) 0.0309(16) Uani 1 1 d . . . . .
N10 N 0.4678(5) 0.5284(4) 0.87088(19) 0.0320(16) Uani 1 1 d . . . . .
N11 N 0.3966(5) 0.5902(4) 0.8234(2) 0.0344(17) Uani 1 1 d . . . . .
N12 N 0.3920(5) 0.6892(4) 0.77429(19) 0.0335(16) Uani 1 1 d . . . . .
N13 N 0.5327(5) 0.6783(4) 0.70520(19) 0.0380(18) Uani 1 1 d . . . . .
N14 N 0.6770(5) 0.7317(4) 0.71186(18) 0.0320(16) Uani 1 1 d . . . . .
N15 N 0.8123(5) 0.7340(4) 0.73731(18) 0.0309(16) Uani 1 1 d . . . . .
N16 N 0.9229(4) 0.6859(4) 0.78276(17) 0.0295(15) Uani 1 1 d . . . . .
N17 N 0.9731(5) 0.6084(4) 0.82936(19) 0.0355(17) Uani 1 1 d . . . . .
N18 N 0.9737(5) 0.5055(4) 0.87597(17) 0.0312(16) Uani 1 1 d . . . . .
N19 N 0.8854(5) 0.4223(4) 0.90340(18) 0.0322(16) Uani 1 1 d . . . . .
N20 N 0.7426(5) 0.3637(4) 0.90283(18) 0.0325(16) Uani 1 1 d . . . . .
N21 N 0.6075(5) 0.3689(4) 0.87669(19) 0.0332(16) Uani 1 1 d . . . . .
N22 N 0.4961(5) 0.4157(4) 0.83063(18) 0.0315(16) Uani 1 1 d . . . . .
N23 N 0.4469(5) 0.4879(4) 0.78236(19) 0.0352(17) Uani 1 1 d . . . . .
N24 N 0.4578(5) 0.5900(4) 0.73502(18) 0.0329(16) Uani 1 1 d . . . . .
N25 N 0.7598(4) 0.9128(4) 0.94928(18) 0.0291(15) Uani 1 1 d . . . . .
N26 N 0.7315(5) 0.8557(4) 1.0101(2) 0.0382(18) Uani 1 1 d . . . . .
N27 N 0.6539(5) 0.8227(4) 1.0584(2) 0.0415(18) Uani 1 1 d . . . . .
N28 N 0.5204(5) 0.8168(4) 1.0915(2) 0.0388(18) Uani 1 1 d . . . . .
N29 N 0.3806(5) 0.8396(4) 1.0968(2) 0.0419(19) Uani 1 1 d . . . . .
N30 N 0.2524(6) 0.9049(4) 1.0693(2) 0.048(2) Uani 1 1 d . . . . .
N31 N 0.8097(5) 1.0324(4) 0.9804(2) 0.0426(19) Uani 1 1 d . . . . .
N32 N 0.7759(5) 0.9771(5) 1.0411(2) 0.0418(19) Uani 1 1 d . . . . .
N33 N 0.6900(5) 0.9483(4) 1.08754(19) 0.0392(18) Uani 1 1 d . . . . .
N34 N 0.5552(5) 0.9437(4) 1.12048(19) 0.0348(17) Uani 1 1 d . . . . .
N35 N 0.4154(5) 0.9640(4) 1.1267(2) 0.0374(18) Uani 1 1 d . . . . .
N36 N 0.2794(5) 1.0258(4) 1.10445(19) 0.0316(16) Uani 1 1 d . . . . .
O1 O 0.4455(4) 0.7900(3) 0.81162(16) 0.0362(14) Uani 1 1 d . . . . .
O2 O 0.6390(4) 0.8376(3) 0.82255(15) 0.0350(14) Uani 1 1 d . . . . .
O1W O 0.5905(5) 0.6739(4) 0.8204(2) 0.0546(18) Uani 1 1 d . . . . .
O3 O 0.8291(4) 0.7824(4) 0.89264(17) 0.0420(15) Uani 1 1 d . . . . .
O2W O 0.6661(4) 0.7031(3) 0.89525(19) 0.0464(16) Uani 1 1 d . . . . .
O4 O 0.8315(4) 0.6477(4) 0.95912(17) 0.0428(15) Uani 1 1 d . . . . .
O3W O 0.5135(5) 0.7668(5) 0.93899(18) 0.063(2) Uani 1 1 d . . . . .
O5 O 0.6423(4) 0.5906(3) 0.94760(17) 0.0434(16) Uani 1 1 d . . . . .
O4W O 0.3739(4) 0.8097(4) 0.88514(18) 0.0456(16) Uani 1 1 d . . . . .
O6 O 0.4532(4) 0.6603(3) 0.87423(16) 0.0361(14) Uani 1 1 d . . . . .
O7 O 0.5839(4) 0.5533(4) 0.70883(17) 0.0443(16) Uani 1 1 d . . . . .
O8 O 0.7717(4) 0.6317(4) 0.69731(17) 0.0408(15) Uani 1 1 d . . . . .
O9 O 0.9262(4) 0.5535(3) 0.77186(16) 0.0399(15) Uani 1 1 d . . . . .
O10 O 0.9072(4) 0.4080(4) 0.84006(15) 0.0424(16) Uani 1 1 d . . . . .
O11 O 0.7151(4) 0.3136(4) 0.84265(16) 0.0422(15) Uani 1 1 d . . . . .
O12 O 0.5498(4) 0.3926(3) 0.77188(16) 0.0402(15) Uani 1 1 d . . . . .
O13 O 0.4926(4) 0.9299(3) 0.87296(16) 0.0362(14) Uani 1 1 d . . . . .
O14 O 0.6488(4) 0.8620(3) 0.91061(15) 0.0355(14) Uani 1 1 d . . . . .
O15 O 0.6192(5) 0.7672(4) 1.00022(18) 0.0495(17) Uani 1 1 d . . . . .
O16 O 0.4215(5) 0.7599(4) 1.04822(19) 0.0521(18) Uani 1 1 d . . . . .
O17 O 0.7458(5) 1.1517(4) 0.9898(2) 0.071(2) Uani 1 1 d . . . . .
O18 O 0.7190(5) 1.0772(4) 1.0753(2) 0.062(2) Uani 1 1 d . . . . .
La1 La 0.53685(3) 0.78651(3) 0.87140(2) 0.03026(18) 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
O21 N40 1.133(16) . ?
O20 N40 1.295(18) . ?
O22 N40 1.360(17) . ?
O23 N41 1.300(19) . ?
N41 O24 1.272(18) . ?
N41 O25 1.318(18) . ?
C1 O1 1.257(10) . ?
C1 N12 1.325(11) . ?
C1 N1 1.363(11) . ?
C2 N2 1.450(11) . ?
C2 N1 1.452(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O2 1.249(9) . ?
C3 N3 1.354(11) . ?
C3 N2 1.355(10) . ?
C4 N4 1.443(11) . ?
C4 N3 1.460(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O3 1.226(10) . ?
C5 N4 1.356(10) . ?
C5 N5 1.389(11) . ?
C6 N6 1.434(11) . ?
C6 N5 1.447(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O4 1.224(10) . ?
C7 N6 1.346(11) . ?
C7 N7 1.371(11) . ?
C8 N7 1.424(11) . ?
C8 N8 1.454(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O5 1.240(10) . ?
C9 N8 1.356(11) . ?
C9 N9 1.365(11) . ?
C10 N10 1.442(10) . ?
C10 N9 1.452(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O6 1.231(9) . ?
C11 N11 1.332(10) . ?
C11 N10 1.365(10) . ?
C12 N12 1.428(10) . ?
C12 N11 1.456(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N13 1.446(11) . ?
C13 N1 1.465(10) . ?
C13 C14 1.511(12) . ?
C13 C27 1.590(13) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N2 1.423(10) . ?
C15 N14 1.450(10) . ?
C15 C16 1.564(11) . ?
C15 H15 0.9800 . ?
C16 N15 1.429(10) . ?
C16 N3 1.473(9) . ?
C16 H16 0.9800 . ?
C17 N16 1.449(10) . ?
C17 N4 1.473(11) . ?
C17 C18 1.546(12) . ?
C17 H17 0.9800 . ?
C18 N5 1.419(11) . ?
C18 N17 1.458(11) . ?
C18 H18 0.9800 . ?
C19 N6 1.435(11) . ?
C19 N18 1.464(10) . ?
C19 C20 1.534(12) . ?
C19 C21 1.586(12) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N7 1.456(11) . ?
C21 N19 1.485(10) . ?
C21 C22 1.531(12) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 N8 1.447(10) . ?
C23 N20 1.448(10) . ?
C23 C24 1.566(12) . ?
C23 H23 0.9800 . ?
C24 N21 1.446(10) . ?
C24 N9 1.455(10) . ?
C24 H24 0.9800 . ?
C25 N22 1.434(10) . ?
C25 N10 1.473(10) . ?
C25 C26 1.545(11) . ?
C25 H25 0.9800 . ?
C26 N23 1.427(11) . ?
C26 N11 1.457(11) . ?
C26 H26 0.9800 . ?
C27 N12 1.470(10) . ?
C27 N24 1.479(11) . ?
C27 C28 1.509(12) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 O7 1.217(10) . ?
C29 N24 1.348(11) . ?
C29 N13 1.361(11) . ?
C30 N14 1.429(11) . ?
C30 N13 1.458(11) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 O8 1.241(10) . ?
C31 N15 1.359(11) . ?
C31 N14 1.376(11) . ?
C32 N16 1.443(10) . ?
C32 N15 1.454(11) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 O9 1.227(10) . ?
C33 N16 1.358(11) . ?
C33 N17 1.379(10) . ?
C34 N18 1.422(11) . ?
C34 N17 1.450(11) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 O10 1.217(10) . ?
C35 N19 1.359(11) . ?
C35 N18 1.382(11) . ?
C36 N20 1.425(11) . ?
C36 N19 1.448(11) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 O11 1.208(10) . ?
C37 N21 1.372(11) . ?
C37 N20 1.389(10) . ?
C38 N21 1.439(10) . ?
C38 N22 1.448(10) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 O12 1.221(10) . ?
C39 N22 1.358(10) . ?
C39 N23 1.387(11) . ?
C40 N23 1.440(10) . ?
C40 N24 1.477(11) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 O14 1.251(10) . ?
C41 N25 1.341(10) . ?
C41 N36 1.354(10) 3_677 ?
C42 N26 1.449(11) . ?
C42 N25 1.454(10) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 O15 1.228(11) . ?
C43 N26 1.357(12) . ?
C43 N27 1.368(11) . ?
C44 N27 1.440(12) . ?
C44 N28 1.447(12) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 O16 1.238(11) . ?
C45 N29 1.357(12) . ?
C45 N28 1.360(12) . ?
C46 N29 1.425(13) . ?
C46 N30 1.455(12) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.511(13) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 N31 1.463(11) . ?
C48 N25 1.472(11) . ?
C48 C53 1.575(12) 3_677 ?
C49 N32 1.434(12) . ?
C49 N26 1.461(11) . ?
C49 C50 1.552(13) . ?
C49 H49 0.9800 . ?
C50 N27 1.431(12) . ?
C50 N33 1.454(11) . ?
C50 H50 0.9800 . ?
C51 N28 1.451(11) . ?
C51 N34 1.452(11) . ?
C51 C52 1.539(13) . ?
C51 H51 0.9800 . ?
C52 N35 1.434(11) . ?
C52 N29 1.443(12) . ?
C52 H52 0.9800 . ?
C53 N30 1.450(11) . ?
C53 N36 1.479(11) . ?
C53 C48 1.575(12) 3_677 ?
C53 C54 1.577(8) . ?
C55 O17 1.226(12) . ?
C55 N31 1.353(12) . ?
C55 N30 1.377(13) 3_677 ?
C56 N32 1.435(12) . ?
C56 N31 1.451(12) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 O18 1.239(11) . ?
C57 N32 1.352(12) . ?
C57 N33 1.358(12) . ?
C58 N34 1.435(12) . ?
C58 N33 1.461(11) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 O13 1.216(10) 3_677 ?
C59 N35 1.362(12) . ?
C59 N34 1.374(11) . ?
C60 N36 1.440(10) . ?
C60 N35 1.464(11) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
N30 C55 1.377(13) 3_677 ?
N36 C41 1.354(10) 3_677 ?
O1 La1 2.472(6) . ?
O2 La1 2.557(6) . ?
O1W La1 2.799(7) . ?
O2W La1 2.556(6) . ?
O3W La1 2.459(6) . ?
O4W La1 2.614(6) . ?
O6 La1 2.523(6) . ?
O13 C59 1.216(10) 3_677 ?
O13 La1 2.553(6) . ?
O14 La1 2.509(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O21 N40 O20 130.0(17) . . ?
O21 N40 O22 119.9(16) . . ?
O20 N40 O22 110.1(15) . . ?
O24 N41 O23 127.5(17) . . ?
O24 N41 O25 123.0(17) . . ?
O23 N41 O25 106.1(16) . . ?
O1 C1 N12 125.8(8) . . ?
O1 C1 N1 122.8(8) . . ?
N12 C1 N1 111.4(7) . . ?
N2 C2 N1 113.8(7) . . ?
N2 C2 H2A 108.8 . . ?
N1 C2 H2A 108.8 . . ?
N2 C2 H2B 108.8 . . ?
N1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
O2 C3 N3 124.9(7) . . ?
O2 C3 N2 125.4(8) . . ?
N3 C3 N2 109.7(7) . . ?
N4 C4 N3 112.8(7) . . ?
N4 C4 H4A 109.0 . . ?
N3 C4 H4A 109.0 . . ?
N4 C4 H4B 109.0 . . ?
N3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
O3 C5 N4 126.1(8) . . ?
O3 C5 N5 126.3(8) . . ?
N4 C5 N5 107.6(7) . . ?
N6 C6 N5 115.1(7) . . ?
N6 C6 H6A 108.5 . . ?
N5 C6 H6A 108.5 . . ?
N6 C6 H6B 108.5 . . ?
N5 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
O4 C7 N6 125.6(8) . . ?
O4 C7 N7 125.5(8) . . ?
N6 C7 N7 108.9(7) . . ?
N7 C8 N8 115.6(7) . . ?
N7 C8 H8A 108.4 . . ?
N8 C8 H8A 108.4 . . ?
N7 C8 H8B 108.4 . . ?
N8 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
O5 C9 N8 126.1(8) . . ?
O5 C9 N9 124.7(8) . . ?
N8 C9 N9 109.2(7) . . ?
N10 C10 N9 113.3(7) . . ?
N10 C10 H10A 108.9 . . ?
N9 C10 H10A 108.9 . . ?
N10 C10 H10B 108.9 . . ?
N9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
O6 C11 N11 126.7(8) . . ?
O6 C11 N10 122.5(7) . . ?
N11 C11 N10 110.7(7) . . ?
N12 C12 N11 114.6(7) . . ?
N12 C12 H12A 108.6 . . ?
N11 C12 H12A 108.6 . . ?
N12 C12 H12B 108.6 . . ?
N11 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N13 C13 N1 113.4(7) . . ?
N13 C13 C14 113.8(7) . . ?
N1 C13 C14 109.3(7) . . ?
N13 C13 C27 102.8(7) . . ?
N1 C13 C27 101.7(6) . . ?
C14 C13 C27 115.1(7) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 N14 113.6(7) . . ?
N2 C15 C16 103.6(6) . . ?
N14 C15 C16 102.6(7) . . ?
N2 C15 H15 112.1 . . ?
N14 C15 H15 112.1 . . ?
C16 C15 H15 112.1 . . ?
N15 C16 N3 114.0(6) . . ?
N15 C16 C15 103.5(6) . . ?
N3 C16 C15 102.2(6) . . ?
N15 C16 H16 112.1 . . ?
N3 C16 H16 112.1 . . ?
C15 C16 H16 112.1 . . ?
N16 C17 N4 113.8(7) . . ?
N16 C17 C18 103.5(6) . . ?
N4 C17 C18 101.2(6) . . ?
N16 C17 H17 112.5 . . ?
N4 C17 H17 112.5 . . ?
C18 C17 H17 112.5 . . ?
N5 C18 N17 114.2(7) . . ?
N5 C18 C17 105.3(7) . . ?
N17 C18 C17 103.2(6) . . ?
N5 C18 H18 111.3 . . ?
N17 C18 H18 111.3 . . ?
C17 C18 H18 111.3 . . ?
N6 C19 N18 115.1(7) . . ?
N6 C19 C20 110.8(7) . . ?
N18 C19 C20 110.7(7) . . ?
N6 C19 C21 102.5(7) . . ?
N18 C19 C21 102.8(6) . . ?
C20 C19 C21 114.7(7) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N7 C21 N19 113.7(7) . . ?
N7 C21 C22 110.7(7) . . ?
N19 C21 C22 110.1(7) . . ?
N7 C21 C19 102.4(7) . . ?
N19 C21 C19 102.4(6) . . ?
C22 C21 C19 117.3(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N8 C23 N20 114.7(7) . . ?
N8 C23 C24 103.1(6) . . ?
N20 C23 C24 103.9(6) . . ?
N8 C23 H23 111.5 . . ?
N20 C23 H23 111.5 . . ?
C24 C23 H23 111.5 . . ?
N21 C24 N9 115.4(7) . . ?
N21 C24 C23 102.5(6) . . ?
N9 C24 C23 102.8(6) . . ?
N21 C24 H24 111.8 . . ?
N9 C24 H24 111.8 . . ?
C23 C24 H24 111.8 . . ?
N22 C25 N10 115.2(7) . . ?
N22 C25 C26 103.3(6) . . ?
N10 C25 C26 102.9(6) . . ?
N22 C25 H25 111.6 . . ?
N10 C25 H25 111.6 . . ?
C26 C25 H25 111.6 . . ?
N23 C26 N11 115.1(7) . . ?
N23 C26 C25 103.0(7) . . ?
N11 C26 C25 103.3(6) . . ?
N23 C26 H26 111.6 . . ?
N11 C26 H26 111.6 . . ?
C25 C26 H26 111.6 . . ?
N12 C27 N24 112.6(6) . . ?
N12 C27 C28 111.0(7) . . ?
N24 C27 C28 112.6(8) . . ?
N12 C27 C13 102.8(7) . . ?
N24 C27 C13 101.3(7) . . ?
C28 C27 C13 115.9(7) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O7 C29 N24 126.1(8) . . ?
O7 C29 N13 124.7(8) . . ?
N24 C29 N13 109.2(8) . . ?
N14 C30 N13 112.7(7) . . ?
N14 C30 H30A 109.1 . . ?
N13 C30 H30A 109.1 . . ?
N14 C30 H30B 109.1 . . ?
N13 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
O8 C31 N15 125.9(8) . . ?
O8 C31 N14 125.5(8) . . ?
N15 C31 N14 108.7(7) . . ?
N16 C32 N15 113.1(7) . . ?
N16 C32 H32A 109.0 . . ?
N15 C32 H32A 109.0 . . ?
N16 C32 H32B 109.0 . . ?
N15 C32 H32B 109.0 . . ?
H32A C32 H32B 107.8 . . ?
O9 C33 N16 126.0(7) . . ?
O9 C33 N17 125.4(8) . . ?
N16 C33 N17 108.5(7) . . ?
N18 C34 N17 114.3(7) . . ?
N18 C34 H34A 108.7 . . ?
N17 C34 H34A 108.7 . . ?
N18 C34 H34B 108.7 . . ?
N17 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
O10 C35 N19 126.0(8) . . ?
O10 C35 N18 124.9(8) . . ?
N19 C35 N18 109.1(7) . . ?
N20 C36 N19 114.6(7) . . ?
N20 C36 H36A 108.6 . . ?
N19 C36 H36A 108.6 . . ?
N20 C36 H36B 108.6 . . ?
N19 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
O11 C37 N21 126.7(8) . . ?
O11 C37 N20 125.5(8) . . ?
N21 C37 N20 107.7(7) . . ?
N21 C38 N22 114.8(7) . . ?
N21 C38 H38A 108.6 . . ?
N22 C38 H38A 108.6 . . ?
N21 C38 H38B 108.6 . . ?
N22 C38 H38B 108.6 . . ?
H38A C38 H38B 107.5 . . ?
O12 C39 N22 127.4(8) . . ?
O12 C39 N23 125.7(8) . . ?
N22 C39 N23 107.0(7) . . ?
N23 C40 N24 113.2(7) . . ?
N23 C40 H40A 108.9 . . ?
N24 C40 H40A 108.9 . . ?
N23 C40 H40B 108.9 . . ?
N24 C40 H40B 108.9 . . ?
H40A C40 H40B 107.8 . . ?
O14 C41 N25 125.0(7) . . ?
O14 C41 N36 123.7(7) . 3_677 ?
N25 C41 N36 111.3(7) . 3_677 ?
N26 C42 N25 113.3(7) . . ?
N26 C42 H42A 108.9 . . ?
N25 C42 H42A 108.9 . . ?
N26 C42 H42B 108.9 . . ?
N25 C42 H42B 108.9 . . ?
H42A C42 H42B 107.7 . . ?
O15 C43 N26 126.8(8) . . ?
O15 C43 N27 124.7(9) . . ?
N26 C43 N27 108.5(8) . . ?
N27 C44 N28 114.4(7) . . ?
N27 C44 H44A 108.7 . . ?
N28 C44 H44A 108.7 . . ?
N27 C44 H44B 108.7 . . ?
N28 C44 H44B 108.7 . . ?
H44A C44 H44B 107.6 . . ?
O16 C45 N29 125.7(10) . . ?
O16 C45 N28 125.7(9) . . ?
N29 C45 N28 108.6(8) . . ?
N29 C46 N30 114.7(8) . . ?
N29 C46 H46A 108.6 . . ?
N30 C46 H46A 108.6 . . ?
N29 C46 H46B 108.6 . . ?
N30 C46 H46B 108.6 . . ?
H46A C46 H46B 107.6 . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N31 C48 N25 112.0(7) . . ?
N31 C48 C47 113.7(8) . . ?
N25 C48 C47 111.2(7) . . ?
N31 C48 C53 101.7(7) . 3_677 ?
N25 C48 C53 102.0(6) . 3_677 ?
C47 C48 C53 115.5(7) . 3_677 ?
N32 C49 N26 114.3(7) . . ?
N32 C49 C50 104.9(7) . . ?
N26 C49 C50 102.7(7) . . ?
N32 C49 H49 111.5 . . ?
N26 C49 H49 111.5 . . ?
C50 C49 H49 111.5 . . ?
N27 C50 N33 115.3(7) . . ?
N27 C50 C49 103.6(7) . . ?
N33 C50 C49 101.9(7) . . ?
N27 C50 H50 111.7 . . ?
N33 C50 H50 111.7 . . ?
C49 C50 H50 111.7 . . ?
N28 C51 N34 115.2(7) . . ?
N28 C51 C52 102.6(7) . . ?
N34 C51 C52 103.8(7) . . ?
N28 C51 H51 111.5 . . ?
N34 C51 H51 111.5 . . ?
C52 C51 H51 111.5 . . ?
N35 C52 N29 115.0(7) . . ?
N35 C52 C51 102.9(7) . . ?
N29 C52 C51 104.0(7) . . ?
N35 C52 H52 111.4 . . ?
N29 C52 H52 111.4 . . ?
C51 C52 H52 111.4 . . ?
N30 C53 N36 112.9(7) . . ?
N30 C53 C48 103.8(7) . 3_677 ?
N36 C53 C48 102.8(6) . 3_677 ?
N30 C53 C54 113.2(8) . . ?
N36 C53 C54 107.8(7) . . ?
C48 C53 C54 116.0(7) 3_677 . ?
O17 C55 N31 126.2(10) . . ?
O17 C55 N30 124.4(10) . 3_677 ?
N31 C55 N30 109.4(8) . 3_677 ?
N32 C56 N31 114.5(7) . . ?
N32 C56 H56A 108.6 . . ?
N31 C56 H56A 108.6 . . ?
N32 C56 H56B 108.6 . . ?
N31 C56 H56B 108.6 . . ?
H56A C56 H56B 107.6 . . ?
O18 C57 N32 125.1(9) . . ?
O18 C57 N33 124.7(9) . . ?
N32 C57 N33 110.2(8) . . ?
N34 C58 N33 114.7(7) . . ?
N34 C58 H58A 108.6 . . ?
N33 C58 H58A 108.6 . . ?
N34 C58 H58B 108.6 . . ?
N33 C58 H58B 108.6 . . ?
H58A C58 H58B 107.6 . . ?
O13 C59 N35 126.9(8) 3_677 . ?
O13 C59 N34 125.6(8) 3_677 . ?
N35 C59 N34 107.4(8) . . ?
N36 C60 N35 114.0(7) . . ?
N36 C60 H60A 108.7 . . ?
N35 C60 H60A 108.7 . . ?
N36 C60 H60B 108.7 . . ?
N35 C60 H60B 108.7 . . ?
H60A C60 H60B 107.6 . . ?
C1 N1 C2 121.2(7) . . ?
C1 N1 C13 111.8(7) . . ?
C2 N1 C13 126.9(7) . . ?
C3 N2 C15 112.8(7) . . ?
C3 N2 C2 124.4(7) . . ?
C15 N2 C2 122.6(6) . . ?
C3 N3 C4 122.3(7) . . ?
C3 N3 C16 111.2(6) . . ?
C4 N3 C16 121.0(7) . . ?
C5 N4 C4 121.4(7) . . ?
C5 N4 C17 113.1(7) . . ?
C4 N4 C17 122.7(7) . . ?
C5 N5 C18 112.1(7) . . ?
C5 N5 C6 122.9(7) . . ?
C18 N5 C6 124.9(7) . . ?
C7 N6 C6 119.9(7) . . ?
C7 N6 C19 113.9(7) . . ?
C6 N6 C19 125.7(7) . . ?
C7 N7 C8 121.1(7) . . ?
C7 N7 C21 112.1(7) . . ?
C8 N7 C21 125.4(7) . . ?
C9 N8 C23 112.2(7) . . ?
C9 N8 C8 123.1(7) . . ?
C23 N8 C8 122.5(7) . . ?
C9 N9 C10 121.3(7) . . ?
C9 N9 C24 111.4(7) . . ?
C10 N9 C24 121.2(7) . . ?
C11 N10 C10 122.8(7) . . ?
C11 N10 C25 110.2(6) . . ?
C10 N10 C25 122.5(7) . . ?
C11 N11 C12 124.3(7) . . ?
C11 N11 C26 111.9(7) . . ?
C12 N11 C26 123.0(7) . . ?
C1 N12 C12 121.3(7) . . ?
C1 N12 C27 111.8(7) . . ?
C12 N12 C27 126.3(7) . . ?
C29 N13 C13 113.2(8) . . ?
C29 N13 C30 121.8(8) . . ?
C13 N13 C30 124.9(7) . . ?
C31 N14 C30 123.2(7) . . ?
C31 N14 C15 111.1(7) . . ?
C30 N14 C15 122.0(7) . . ?
C31 N15 C16 112.5(7) . . ?
C31 N15 C32 123.1(7) . . ?
C16 N15 C32 123.3(7) . . ?
C33 N16 C32 123.6(7) . . ?
C33 N16 C17 112.6(6) . . ?
C32 N16 C17 121.9(7) . . ?
C33 N17 C34 122.0(7) . . ?
C33 N17 C18 111.5(7) . . ?
C34 N17 C18 122.4(7) . . ?
C35 N18 C34 120.8(7) . . ?
C35 N18 C19 112.7(7) . . ?
C34 N18 C19 126.5(7) . . ?
C35 N19 C36 120.4(7) . . ?
C35 N19 C21 112.5(7) . . ?
C36 N19 C21 125.3(7) . . ?
C37 N20 C36 123.9(7) . . ?
C37 N20 C23 111.9(7) . . ?
C36 N20 C23 124.1(7) . . ?
C37 N21 C38 121.8(7) . . ?
C37 N21 C24 113.7(7) . . ?
C38 N21 C24 123.7(7) . . ?
C39 N22 C25 113.1(7) . . ?
C39 N22 C38 122.8(7) . . ?
C25 N22 C38 123.0(7) . . ?
C39 N23 C26 112.4(7) . . ?
C39 N23 C40 122.5(7) . . ?
C26 N23 C40 122.8(7) . . ?
C29 N24 C40 120.6(7) . . ?
C29 N24 C27 112.9(7) . . ?
C40 N24 C27 124.0(7) . . ?
C41 N25 C42 121.1(7) . . ?
C41 N25 C48 112.1(6) . . ?
C42 N25 C48 124.8(7) . . ?
C43 N26 C42 121.1(7) . . ?
C43 N26 C49 112.0(7) . . ?
C42 N26 C49 123.8(7) . . ?
C43 N27 C50 112.7(8) . . ?
C43 N27 C44 122.7(8) . . ?
C50 N27 C44 123.0(7) . . ?
C45 N28 C44 122.5(8) . . ?
C45 N28 C51 112.6(8) . . ?
C44 N28 C51 124.1(8) . . ?
C45 N29 C46 125.1(9) . . ?
C45 N29 C52 112.1(8) . . ?
C46 N29 C52 122.8(8) . . ?
C55 N30 C53 111.4(8) 3_677 . ?
C55 N30 C46 121.0(8) 3_677 . ?
C53 N30 C46 126.4(8) . . ?
C55 N31 C56 120.0(8) . . ?
C55 N31 C48 113.0(8) . . ?
C56 N31 C48 127.0(8) . . ?
C57 N32 C49 111.0(8) . . ?
C57 N32 C56 124.8(8) . . ?
C49 N32 C56 122.5(7) . . ?
C57 N33 C50 111.8(7) . . ?
C57 N33 C58 123.2(8) . . ?
C50 N33 C58 122.8(7) . . ?
C59 N34 C58 122.2(8) . . ?
C59 N34 C51 111.7(7) . . ?
C58 N34 C51 123.7(7) . . ?
C59 N35 C52 113.7(8) . . ?
C59 N35 C60 122.7(7) . . ?
C52 N35 C60 121.7(8) . . ?
C41 N36 C60 122.9(7) 3_677 . ?
C41 N36 C53 110.6(7) 3_677 . ?
C60 N36 C53 124.6(7) . . ?
C1 O1 La1 136.3(5) . . ?
C3 O2 La1 147.1(5) . . ?
C11 O6 La1 141.7(5) . . ?
C59 O13 La1 154.3(6) 3_677 . ?
C41 O14 La1 157.9(5) . . ?
O3W La1 O1 136.6(2) . . ?
O3W La1 O14 70.6(2) . . ?
O1 La1 O14 143.06(19) . . ?
O3W La1 O6 75.0(2) . . ?
O1 La1 O6 77.73(19) . . ?
O14 La1 O6 139.20(18) . . ?
O3W La1 O13 93.3(2) . . ?
O1 La1 O13 81.67(18) . . ?
O14 La1 O13 70.55(19) . . ?
O6 La1 O13 133.41(19) . . ?
O3W La1 O2W 75.9(3) . . ?
O1 La1 O2W 133.7(2) . . ?
O14 La1 O2W 66.99(19) . . ?
O6 La1 O2W 84.09(19) . . ?
O13 La1 O2W 137.4(2) . . ?
O3W La1 O2 146.4(2) . . ?
O1 La1 O2 75.92(19) . . ?
O14 La1 O2 76.48(18) . . ?
O6 La1 O2 131.01(18) . . ?
O13 La1 O2 81.95(19) . . ?
O2W La1 O2 85.2(2) . . ?
O3W La1 O4W 69.2(2) . . ?
O1 La1 O4W 69.5(2) . . ?
O14 La1 O4W 117.10(19) . . ?
O6 La1 O4W 68.0(2) . . ?
O13 La1 O4W 65.7(2) . . ?
O2W La1 O4W 139.7(2) . . ?
O2 La1 O4W 135.1(2) . . ?
O3W La1 O1W 126.6(3) . . ?
O1 La1 O1W 68.9(2) . . ?
O14 La1 O1W 119.5(2) . . ?
O6 La1 O1W 66.7(2) . . ?
O13 La1 O1W 140.12(19) . . ?
O2W La1 O1W 64.7(2) . . ?
O2 La1 O1W 65.51(19) . . ?
O4W La1 O1W 123.1(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C15 C16 N15 124.9(7) . . . . ?
N14 C15 C16 N15 6.4(8) . . . . ?
N2 C15 C16 N3 6.2(8) . . . . ?
N14 C15 C16 N3 -112.2(6) . . . . ?
N16 C17 C18 N5 -126.0(7) . . . . ?
N4 C17 C18 N5 -7.9(8) . . . . ?
N16 C17 C18 N17 -6.0(8) . . . . ?
N4 C17 C18 N17 112.1(7) . . . . ?
N6 C19 C21 N7 -3.2(7) . . . . ?
N18 C19 C21 N7 -122.9(7) . . . . ?
C20 C19 C21 N7 116.9(8) . . . . ?
N6 C19 C21 N19 114.7(7) . . . . ?
N18 C19 C21 N19 -4.9(8) . . . . ?
C20 C19 C21 N19 -125.1(8) . . . . ?
N6 C19 C21 C22 -124.6(8) . . . . ?
N18 C19 C21 C22 115.7(8) . . . . ?
C20 C19 C21 C22 -4.5(11) . . . . ?
N8 C23 C24 N21 124.7(6) . . . . ?
N20 C23 C24 N21 4.8(8) . . . . ?
N8 C23 C24 N9 4.6(8) . . . . ?
N20 C23 C24 N9 -115.3(7) . . . . ?
N22 C25 C26 N23 -8.9(8) . . . . ?
N10 C25 C26 N23 111.2(7) . . . . ?
N22 C25 C26 N11 -129.0(7) . . . . ?
N10 C25 C26 N11 -8.9(8) . . . . ?
N13 C13 C27 N12 123.8(6) . . . . ?
N1 C13 C27 N12 6.2(8) . . . . ?
C14 C13 C27 N12 -111.9(8) . . . . ?
N13 C13 C27 N24 7.3(7) . . . . ?
N1 C13 C27 N24 -110.3(7) . . . . ?
C14 C13 C27 N24 131.6(7) . . . . ?
N13 C13 C27 C28 -114.9(8) . . . . ?
N1 C13 C27 C28 127.5(8) . . . . ?
C14 C13 C27 C28 9.4(11) . . . . ?
N32 C49 C50 N27 122.8(7) . . . . ?
N26 C49 C50 N27 3.0(9) . . . . ?
N32 C49 C50 N33 2.7(9) . . . . ?
N26 C49 C50 N33 -117.1(7) . . . . ?
N28 C51 C52 N35 -121.5(7) . . . . ?
N34 C51 C52 N35 -1.2(8) . . . . ?
N28 C51 C52 N29 -1.3(8) . . . . ?
N34 C51 C52 N29 119.1(7) . . . . ?
O1 C1 N1 C2 1.7(12) . . . . ?
N12 C1 N1 C2 178.7(7) . . . . ?
O1 C1 N1 C13 -175.0(7) . . . . ?
N12 C1 N1 C13 1.9(10) . . . . ?
N2 C2 N1 C1 97.7(9) . . . . ?
N2 C2 N1 C13 -86.0(10) . . . . ?
N13 C13 N1 C1 -114.9(8) . . . . ?
C14 C13 N1 C1 117.0(8) . . . . ?
C27 C13 N1 C1 -5.2(8) . . . . ?
N13 C13 N1 C2 68.6(10) . . . . ?
C14 C13 N1 C2 -59.5(11) . . . . ?
C27 C13 N1 C2 178.3(7) . . . . ?
O2 C3 N2 C15 -179.4(8) . . . . ?
N3 C3 N2 C15 0.7(9) . . . . ?
O2 C3 N2 C2 5.2(13) . . . . ?
N3 C3 N2 C2 -174.8(7) . . . . ?
N14 C15 N2 C3 106.0(8) . . . . ?
C16 C15 N2 C3 -4.5(9) . . . . ?
N14 C15 N2 C2 -78.4(9) . . . . ?
C16 C15 N2 C2 171.0(7) . . . . ?
N1 C2 N2 C3 -94.5(9) . . . . ?
N1 C2 N2 C15 90.5(9) . . . . ?
O2 C3 N3 C4 -22.0(12) . . . . ?
N2 C3 N3 C4 158.0(7) . . . . ?
O2 C3 N3 C16 -176.0(7) . . . . ?
N2 C3 N3 C16 3.9(9) . . . . ?
N4 C4 N3 C3 119.9(8) . . . . ?
N4 C4 N3 C16 -88.5(9) . . . . ?
N15 C16 N3 C3 -117.3(8) . . . . ?
C15 C16 N3 C3 -6.3(8) . . . . ?
N15 C16 N3 C4 88.2(9) . . . . ?
C15 C16 N3 C4 -160.8(7) . . . . ?
O3 C5 N4 C4 12.5(13) . . . . ?
N5 C5 N4 C4 -167.0(7) . . . . ?
O3 C5 N4 C17 174.1(8) . . . . ?
N5 C5 N4 C17 -5.3(9) . . . . ?
N3 C4 N4 C5 -119.4(8) . . . . ?
N3 C4 N4 C17 80.8(10) . . . . ?
N16 C17 N4 C5 118.6(8) . . . . ?
C18 C17 N4 C5 8.3(9) . . . . ?
N16 C17 N4 C4 -80.0(10) . . . . ?
C18 C17 N4 C4 169.7(7) . . . . ?
O3 C5 N5 C18 -180.0(8) . . . . ?
N4 C5 N5 C18 -0.5(9) . . . . ?
O3 C5 N5 C6 -4.3(13) . . . . ?
N4 C5 N5 C6 175.1(7) . . . . ?
N17 C18 N5 C5 -106.8(8) . . . . ?
C17 C18 N5 C5 5.6(9) . . . . ?
N17 C18 N5 C6 77.6(10) . . . . ?
C17 C18 N5 C6 -169.9(7) . . . . ?
N6 C6 N5 C5 100.7(10) . . . . ?
N6 C6 N5 C18 -84.2(10) . . . . ?
O4 C7 N6 C6 5.1(13) . . . . ?
N7 C7 N6 C6 -174.3(7) . . . . ?
O4 C7 N6 C19 176.8(8) . . . . ?
N7 C7 N6 C19 -2.6(9) . . . . ?
N5 C6 N6 C7 -104.3(9) . . . . ?
N5 C6 N6 C19 85.0(10) . . . . ?
N18 C19 N6 C7 114.4(8) . . . . ?
C20 C19 N6 C7 -119.2(8) . . . . ?
C21 C19 N6 C7 3.7(8) . . . . ?
N18 C19 N6 C6 -74.4(10) . . . . ?
C20 C19 N6 C6 52.0(10) . . . . ?
C21 C19 N6 C6 174.8(7) . . . . ?
O4 C7 N7 C8 13.4(12) . . . . ?
N6 C7 N7 C8 -167.2(7) . . . . ?
O4 C7 N7 C21 -179.3(8) . . . . ?
N6 C7 N7 C21 0.1(9) . . . . ?
N8 C8 N7 C7 87.6(9) . . . . ?
N8 C8 N7 C21 -77.9(10) . . . . ?
N19 C21 N7 C7 -107.6(8) . . . . ?
C22 C21 N7 C7 127.9(8) . . . . ?
C19 C21 N7 C7 2.1(8) . . . . ?
N19 C21 N7 C8 59.0(10) . . . . ?
C22 C21 N7 C8 -65.5(10) . . . . ?
C19 C21 N7 C8 168.7(7) . . . . ?
O5 C9 N8 C23 172.7(8) . . . . ?
N9 C9 N8 C23 -9.1(9) . . . . ?
O5 C9 N8 C8 9.0(13) . . . . ?
N9 C9 N8 C8 -172.9(7) . . . . ?
N20 C23 N8 C9 114.6(8) . . . . ?
C24 C23 N8 C9 2.4(8) . . . . ?
N20 C23 N8 C8 -81.5(9) . . . . ?
C24 C23 N8 C8 166.3(7) . . . . ?
N7 C8 N8 C9 -98.6(10) . . . . ?
N7 C8 N8 C23 99.3(9) . . . . ?
O5 C9 N9 C10 -16.6(12) . . . . ?
N8 C9 N9 C10 165.2(7) . . . . ?
O5 C9 N9 C24 -169.3(8) . . . . ?
N8 C9 N9 C24 12.5(9) . . . . ?
N10 C10 N9 C9 124.1(8) . . . . ?
N10 C10 N9 C24 -85.8(9) . . . . ?
N21 C24 N9 C9 -121.0(8) . . . . ?
C23 C24 N9 C9 -10.4(8) . . . . ?
N21 C24 N9 C10 86.2(9) . . . . ?
C23 C24 N9 C10 -163.1(6) . . . . ?
O6 C11 N10 C10 15.6(13) . . . . ?
N11 C11 N10 C10 -163.0(8) . . . . ?
O6 C11 N10 C25 172.2(8) . . . . ?
N11 C11 N10 C25 -6.4(9) . . . . ?
N9 C10 N10 C11 -124.3(8) . . . . ?
N9 C10 N10 C25 81.9(10) . . . . ?
N22 C25 N10 C11 121.1(7) . . . . ?
C26 C25 N10 C11 9.5(8) . . . . ?
N22 C25 N10 C10 -82.2(9) . . . . ?
C26 C25 N10 C10 166.2(7) . . . . ?
O6 C11 N11 C12 -8.1(14) . . . . ?
N10 C11 N11 C12 170.4(7) . . . . ?
O6 C11 N11 C26 -178.5(8) . . . . ?
N10 C11 N11 C26 0.0(10) . . . . ?
N12 C12 N11 C11 99.5(10) . . . . ?
N12 C12 N11 C26 -91.1(10) . . . . ?
N23 C26 N11 C11 -105.6(8) . . . . ?
C25 C26 N11 C11 5.9(9) . . . . ?
N23 C26 N11 C12 83.8(10) . . . . ?
C25 C26 N11 C12 -164.7(7) . . . . ?
O1 C1 N12 C12 -8.4(13) . . . . ?
N1 C1 N12 C12 174.8(7) . . . . ?
O1 C1 N12 C27 179.6(8) . . . . ?
N1 C1 N12 C27 2.7(10) . . . . ?
N11 C12 N12 C1 -91.1(10) . . . . ?
N11 C12 N12 C27 79.8(10) . . . . ?
N24 C27 N12 C1 102.5(8) . . . . ?
C28 C27 N12 C1 -130.3(8) . . . . ?
C13 C27 N12 C1 -5.7(9) . . . . ?
N24 C27 N12 C12 -69.1(10) . . . . ?
C28 C27 N12 C12 58.2(11) . . . . ?
C13 C27 N12 C12 -177.3(7) . . . . ?
O7 C29 N13 C13 -179.7(8) . . . . ?
N24 C29 N13 C13 0.3(10) . . . . ?
O7 C29 N13 C30 -4.1(13) . . . . ?
N24 C29 N13 C30 175.9(7) . . . . ?
N1 C13 N13 C29 103.9(8) . . . . ?
C14 C13 N13 C29 -130.3(8) . . . . ?
C27 C13 N13 C29 -5.1(9) . . . . ?
N1 C13 N13 C30 -71.5(10) . . . . ?
C14 C13 N13 C30 54.3(11) . . . . ?
C27 C13 N13 C30 179.5(7) . . . . ?
N14 C30 N13 C29 -83.1(10) . . . . ?
N14 C30 N13 C13 92.0(9) . . . . ?
O8 C31 N14 C30 -7.9(13) . . . . ?
N15 C31 N14 C30 171.8(7) . . . . ?
O8 C31 N14 C15 -166.6(8) . . . . ?
N15 C31 N14 C15 13.1(9) . . . . ?
N13 C30 N14 C31 111.8(9) . . . . ?
N13 C30 N14 C15 -91.8(9) . . . . ?
N2 C15 N14 C31 -123.0(7) . . . . ?
C16 C15 N14 C31 -11.9(8) . . . . ?
N2 C15 N14 C30 77.9(9) . . . . ?
C16 C15 N14 C30 -170.9(7) . . . . ?
O8 C31 N15 C16 171.2(8) . . . . ?
N14 C31 N15 C16 -8.4(9) . . . . ?
O8 C31 N15 C32 2.9(13) . . . . ?
N14 C31 N15 C32 -176.8(7) . . . . ?
N3 C16 N15 C31 111.0(8) . . . . ?
C15 C16 N15 C31 0.9(8) . . . . ?
N3 C16 N15 C32 -80.7(9) . . . . ?
C15 C16 N15 C32 169.1(7) . . . . ?
N16 C32 N15 C31 -112.4(8) . . . . ?
N16 C32 N15 C16 80.6(9) . . . . ?
O9 C33 N16 C32 -12.3(13) . . . . ?
N17 C33 N16 C32 167.7(7) . . . . ?
O9 C33 N16 C17 -177.1(8) . . . . ?
N17 C33 N16 C17 2.9(9) . . . . ?
N15 C32 N16 C33 108.2(9) . . . . ?
N15 C32 N16 C17 -88.3(9) . . . . ?
N4 C17 N16 C33 -106.7(8) . . . . ?
C18 C17 N16 C33 2.2(9) . . . . ?
N4 C17 N16 C32 88.1(9) . . . . ?
C18 C17 N16 C32 -162.9(7) . . . . ?
O9 C33 N17 C34 14.8(13) . . . . ?
N16 C33 N17 C34 -165.2(7) . . . . ?
O9 C33 N17 C18 172.7(8) . . . . ?
N16 C33 N17 C18 -7.2(9) . . . . ?
N18 C34 N17 C33 -116.7(8) . . . . ?
N18 C34 N17 C18 87.7(10) . . . . ?
N5 C18 N17 C33 121.9(8) . . . . ?
C17 C18 N17 C33 8.2(9) . . . . ?
N5 C18 N17 C34 -80.2(10) . . . . ?
C17 C18 N17 C34 166.1(7) . . . . ?
O10 C35 N18 C34 4.1(13) . . . . ?
N19 C35 N18 C34 -178.1(7) . . . . ?
O10 C35 N18 C19 -174.3(8) . . . . ?
N19 C35 N18 C19 3.5(10) . . . . ?
N17 C34 N18 C35 98.3(9) . . . . ?
N17 C34 N18 C19 -83.6(10) . . . . ?
N6 C19 N18 C35 -109.3(8) . . . . ?
C20 C19 N18 C35 124.1(8) . . . . ?
C21 C19 N18 C35 1.2(9) . . . . ?
N6 C19 N18 C34 72.4(11) . . . . ?
C20 C19 N18 C34 -54.2(11) . . . . ?
C21 C19 N18 C34 -177.1(7) . . . . ?
O10 C35 N19 C36 5.1(13) . . . . ?
N18 C35 N19 C36 -172.7(7) . . . . ?
O10 C35 N19 C21 170.6(8) . . . . ?
N18 C35 N19 C21 -7.2(10) . . . . ?
N20 C36 N19 C35 -98.2(9) . . . . ?
N20 C36 N19 C21 98.3(9) . . . . ?
N7 C21 N19 C35 117.2(8) . . . . ?
C22 C21 N19 C35 -118.0(8) . . . . ?
C19 C21 N19 C35 7.6(9) . . . . ?
N7 C21 N19 C36 -78.1(10) . . . . ?
C22 C21 N19 C36 46.7(11) . . . . ?
C19 C21 N19 C36 172.2(7) . . . . ?
O11 C37 N20 C36 6.9(13) . . . . ?
N21 C37 N20 C36 -177.0(7) . . . . ?
O11 C37 N20 C23 -171.5(8) . . . . ?
N21 C37 N20 C23 4.6(9) . . . . ?
N19 C36 N20 C37 103.4(9) . . . . ?
N19 C36 N20 C23 -78.4(10) . . . . ?
N8 C23 N20 C37 -117.6(8) . . . . ?
C24 C23 N20 C37 -5.9(9) . . . . ?
N8 C23 N20 C36 64.0(10) . . . . ?
C24 C23 N20 C36 175.8(7) . . . . ?
O11 C37 N21 C38 4.5(13) . . . . ?
N20 C37 N21 C38 -171.5(7) . . . . ?
O11 C37 N21 C24 174.9(8) . . . . ?
N20 C37 N21 C24 -1.1(9) . . . . ?
N22 C38 N21 C37 -111.9(9) . . . . ?
N22 C38 N21 C24 78.7(10) . . . . ?
N9 C24 N21 C37 108.5(8) . . . . ?
C23 C24 N21 C37 -2.4(9) . . . . ?
N9 C24 N21 C38 -81.3(10) . . . . ?
C23 C24 N21 C38 167.8(7) . . . . ?
O12 C39 N22 C25 -177.1(8) . . . . ?
N23 C39 N22 C25 2.2(9) . . . . ?
O12 C39 N22 C38 -8.9(13) . . . . ?
N23 C39 N22 C38 170.4(7) . . . . ?
N10 C25 N22 C39 -107.0(8) . . . . ?
C26 C25 N22 C39 4.4(9) . . . . ?
N10 C25 N22 C38 84.9(9) . . . . ?
C26 C25 N22 C38 -163.7(7) . . . . ?
N21 C38 N22 C39 110.0(9) . . . . ?
N21 C38 N22 C25 -83.0(10) . . . . ?
O12 C39 N23 C26 170.5(8) . . . . ?
N22 C39 N23 C26 -8.8(9) . . . . ?
O12 C39 N23 C40 7.3(13) . . . . ?
N22 C39 N23 C40 -171.9(8) . . . . ?
N11 C26 N23 C39 122.7(8) . . . . ?
C25 C26 N23 C39 11.1(9) . . . . ?
N11 C26 N23 C40 -74.2(10) . . . . ?
C25 C26 N23 C40 174.2(7) . . . . ?
N24 C40 N23 C39 -116.2(9) . . . . ?
N24 C40 N23 C26 82.4(10) . . . . ?
O7 C29 N24 C40 -12.0(13) . . . . ?
N13 C29 N24 C40 168.0(7) . . . . ?
O7 C29 N24 C27 -174.8(8) . . . . ?
N13 C29 N24 C27 5.3(9) . . . . ?
N23 C40 N24 C29 105.0(9) . . . . ?
N23 C40 N24 C27 -94.2(9) . . . . ?
N12 C27 N24 C29 -117.0(8) . . . . ?
C28 C27 N24 C29 116.5(8) . . . . ?
C13 C27 N24 C29 -7.9(8) . . . . ?
N12 C27 N24 C40 80.9(9) . . . . ?
C28 C27 N24 C40 -45.5(10) . . . . ?
C13 C27 N24 C40 -169.9(7) . . . . ?
O14 C41 N25 C42 12.9(12) . . . . ?
N36 C41 N25 C42 -167.2(7) 3_677 . . . ?
O14 C41 N25 C48 177.8(8) . . . . ?
N36 C41 N25 C48 -2.3(9) 3_677 . . . ?
N26 C42 N25 C41 -109.7(8) . . . . ?
N26 C42 N25 C48 87.4(10) . . . . ?
N31 C48 N25 C41 116.3(8) . . . . ?
C47 C48 N25 C41 -115.3(8) . . . . ?
C53 C48 N25 C41 8.3(9) 3_677 . . . ?
N31 C48 N25 C42 -79.5(10) . . . . ?
C47 C48 N25 C42 48.9(10) . . . . ?
C53 C48 N25 C42 172.5(7) 3_677 . . . ?
O15 C43 N26 C42 -12.4(14) . . . . ?
N27 C43 N26 C42 168.1(8) . . . . ?
O15 C43 N26 C49 -173.4(9) . . . . ?
N27 C43 N26 C49 7.1(10) . . . . ?
N25 C42 N26 C43 117.7(9) . . . . ?
N25 C42 N26 C49 -83.7(10) . . . . ?
N32 C49 N26 C43 -119.3(8) . . . . ?
C50 C49 N26 C43 -6.2(10) . . . . ?
N32 C49 N26 C42 80.4(10) . . . . ?
C50 C49 N26 C42 -166.6(7) . . . . ?
O15 C43 N27 C50 175.6(9) . . . . ?
N26 C43 N27 C50 -4.9(10) . . . . ?
O15 C43 N27 C44 9.6(14) . . . . ?
N26 C43 N27 C44 -170.9(8) . . . . ?
N33 C50 N27 C43 111.4(9) . . . . ?
C49 C50 N27 C43 0.9(10) . . . . ?
N33 C50 N27 C44 -82.7(10) . . . . ?
C49 C50 N27 C44 166.8(8) . . . . ?
N28 C44 N27 C43 -110.7(10) . . . . ?
N28 C44 N27 C50 84.8(11) . . . . ?
O16 C45 N28 C44 -7.9(13) . . . . ?
N29 C45 N28 C44 170.1(7) . . . . ?
O16 C45 N28 C51 -177.6(8) . . . . ?
N29 C45 N28 C51 0.4(10) . . . . ?
N27 C44 N28 C45 108.7(10) . . . . ?
N27 C44 N28 C51 -82.8(10) . . . . ?
N34 C51 N28 C45 -111.5(9) . . . . ?
C52 C51 N28 C45 0.6(9) . . . . ?
N34 C51 N28 C44 78.9(10) . . . . ?
C52 C51 N28 C44 -169.0(7) . . . . ?
O16 C45 N29 C46 -1.3(14) . . . . ?
N28 C45 N29 C46 -179.3(8) . . . . ?
O16 C45 N29 C52 176.7(8) . . . . ?
N28 C45 N29 C52 -1.3(10) . . . . ?
N30 C46 N29 C45 -99.0(11) . . . . ?
N30 C46 N29 C52 83.2(12) . . . . ?
N35 C52 N29 C45 113.3(9) . . . . ?
C51 C52 N29 C45 1.6(9) . . . . ?
N35 C52 N29 C46 -68.6(11) . . . . ?
C51 C52 N29 C46 179.6(8) . . . . ?
N36 C53 N30 C55 -118.3(8) . . . 3_677 ?
C48 C53 N30 C55 -7.6(10) 3_677 . . 3_677 ?
C54 C53 N30 C55 118.9(9) . . . 3_677 ?
N36 C53 N30 C46 74.8(11) . . . . ?
C48 C53 N30 C46 -174.5(9) 3_677 . . . ?
C54 C53 N30 C46 -48.0(13) . . . . ?
N29 C46 N30 C55 97.7(11) . . . 3_677 ?
N29 C46 N30 C53 -96.6(12) . . . . ?
O17 C55 N31 C56 2.1(15) . . . . ?
N30 C55 N31 C56 -180.0(8) 3_677 . . . ?
O17 C55 N31 C48 179.3(10) . . . . ?
N30 C55 N31 C48 -2.7(11) 3_677 . . . ?
N32 C56 N31 C55 93.3(10) . . . . ?
N32 C56 N31 C48 -83.6(12) . . . . ?
N25 C48 N31 C55 -101.1(9) . . . . ?
C47 C48 N31 C55 131.8(9) . . . . ?
C53 C48 N31 C55 7.1(10) 3_677 . . . ?
N25 C48 N31 C56 75.9(11) . . . . ?
C47 C48 N31 C56 -51.1(12) . . . . ?
C53 C48 N31 C56 -175.9(8) 3_677 . . . ?
O18 C57 N32 C49 174.9(9) . . . . ?
N33 C57 N32 C49 -3.0(11) . . . . ?
O18 C57 N32 C56 9.8(16) . . . . ?
N33 C57 N32 C56 -168.1(8) . . . . ?
N26 C49 N32 C57 111.7(9) . . . . ?
C50 C49 N32 C57 0.0(10) . . . . ?
N26 C49 N32 C56 -82.8(10) . . . . ?
C50 C49 N32 C56 165.5(8) . . . . ?
N31 C56 N32 C57 -110.4(10) . . . . ?
N31 C56 N32 C49 86.1(11) . . . . ?
O18 C57 N33 C50 -172.9(9) . . . . ?
N32 C57 N33 C50 5.0(10) . . . . ?
O18 C57 N33 C58 -9.5(15) . . . . ?
N32 C57 N33 C58 168.5(8) . . . . ?
N27 C50 N33 C57 -116.2(9) . . . . ?
C49 C50 N33 C57 -4.7(9) . . . . ?
N27 C50 N33 C58 80.3(10) . . . . ?
C49 C50 N33 C58 -168.2(8) . . . . ?
N34 C58 N33 C57 115.8(10) . . . . ?
N34 C58 N33 C50 -82.5(11) . . . . ?
O13 C59 N34 C58 6.8(12) 3_677 . . . ?
N35 C59 N34 C58 -170.9(7) . . . . ?
O13 C59 N34 C51 170.1(8) 3_677 . . . ?
N35 C59 N34 C51 -7.6(9) . . . . ?
N33 C58 N34 C59 -114.7(9) . . . . ?
N33 C58 N34 C51 84.0(10) . . . . ?
N28 C51 N34 C59 116.8(8) . . . . ?
C52 C51 N34 C59 5.4(9) . . . . ?
N28 C51 N34 C58 -80.2(10) . . . . ?
C52 C51 N34 C58 168.4(7) . . . . ?
O13 C59 N35 C52 -170.8(8) 3_677 . . . ?
N34 C59 N35 C52 6.8(9) . . . . ?
O13 C59 N35 C60 -6.7(13) 3_677 . . . ?
N34 C59 N35 C60 171.0(7) . . . . ?
N29 C52 N35 C59 -115.8(9) . . . . ?
C51 C52 N35 C59 -3.4(9) . . . . ?
N29 C52 N35 C60 79.9(10) . . . . ?
C51 C52 N35 C60 -167.7(7) . . . . ?
N36 C60 N35 C59 99.2(9) . . . . ?
N36 C60 N35 C52 -97.9(9) . . . . ?
N35 C60 N36 C41 -78.4(10) . . . 3_677 ?
N35 C60 N36 C53 84.1(9) . . . . ?
N30 C53 N36 C41 101.1(8) . . . 3_677 ?
C48 C53 N36 C41 -10.1(8) 3_677 . . 3_677 ?
C54 C53 N36 C41 -133.1(8) . . . 3_677 ?
N30 C53 N36 C60 -63.2(10) . . . . ?
C48 C53 N36 C60 -174.4(7) 3_677 . . . ?
C54 C53 N36 C60 62.6(10) . . . . ?
N12 C1 O1 La1 90.3(10) . . . . ?
N1 C1 O1 La1 -93.2(10) . . . . ?
N3 C3 O2 La1 -113.1(10) . . . . ?
N2 C3 O2 La1 66.9(13) . . . . ?
N11 C11 O6 La1 -69.1(13) . . . . ?
N10 C11 O6 La1 112.5(9) . . . . ?
N25 C41 O14 La1 -165.8(10) . . . . ?
N36 C41 O14 La1 14(2) 3_677 . . . ?

_refine_diff_density_max         1.884
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.164



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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1038158'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
	2(C40 H44 La N25 O20), 4(N O3), 13(O)
;

_chemical_formula_sum            'C40 H44 La N27 O32.50'
_chemical_formula_weight         1561.93

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.3756(18)
_cell_length_b                   32.470(5)
_cell_length_c                   15.176(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.089(5)
_cell_angle_gamma                90
_cell_volume                     6094.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5471
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      21.35

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_F_000             3160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.819
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58226
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.254
_diffrn_reflns_theta_max         27.710
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             13070
_reflns_number_gt                8139
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²+4.0505P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13070
_refine_ls_number_parameters     905
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1575
_refine_ls_wR_factor_gt          0.1325
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9607(4) 0.22703(13) 0.5782(3) 0.0339(11) Uani 1 1 d . . . . .
C2 C 0.9813(4) 0.26863(14) 0.7125(3) 0.0375(11) Uani 1 1 d . . . . .
H2A H 1.0555 0.2591 0.7110 0.045 Uiso 1 1 calc R U . . .
H2B H 0.9831 0.2984 0.7180 0.045 Uiso 1 1 calc R U . . .
C3 C 0.9808(4) 0.22131(14) 0.8385(3) 0.0359(11) Uani 1 1 d . . . . .
C4 C 0.9656(4) 0.18922(15) 0.9840(3) 0.0421(12) Uani 1 1 d . . . . .
H4A H 1.0413 0.1830 0.9761 0.050 Uiso 1 1 calc R U . . .
H4B H 0.9602 0.2028 1.0407 0.050 Uiso 1 1 calc R U . . .
C5 C 0.9502(4) 0.11427(15) 0.9630(3) 0.0380(11) Uani 1 1 d . . . . .
C6 C 0.9068(4) 0.04108(14) 0.9855(3) 0.0391(12) Uani 1 1 d . . . . .
H6A H 0.8968 0.0298 1.0439 0.047 Uiso 1 1 calc R U . . .
H6B H 0.9829 0.0385 0.9731 0.047 Uiso 1 1 calc R U . . .
C7 C 0.8882(4) 0.00522(14) 0.8444(3) 0.0384(12) Uani 1 1 d . . . . .
C8 C 0.8475(4) -0.03944(14) 0.7168(3) 0.0369(11) Uani 1 1 d . . . . .
H8A H 0.9255 -0.0421 0.7151 0.044 Uiso 1 1 calc R U . . .
H8B H 0.8168 -0.0669 0.7132 0.044 Uiso 1 1 calc R U . . .
C9 C 0.8744(4) 0.00955(14) 0.5956(3) 0.0342(11) Uani 1 1 d . . . . .
C10 C 0.8684(4) 0.04776(14) 0.4558(3) 0.0370(11) Uani 1 1 d . . . . .
H10A H 0.9462 0.0455 0.4646 0.044 Uiso 1 1 calc R U . . .
H10B H 0.8489 0.0351 0.3995 0.044 Uiso 1 1 calc R U . . .
C11 C 0.9107(4) 0.12179(14) 0.4693(3) 0.0325(11) Uani 1 1 d . . . . .
C12 C 0.9255(4) 0.19592(13) 0.4335(3) 0.0337(11) Uani 1 1 d . . . . .
H12A H 1.0023 0.1898 0.4367 0.040 Uiso 1 1 calc R U . . .
H12B H 0.9088 0.2080 0.3762 0.040 Uiso 1 1 calc R U . . .
C13 C 0.8322(4) 0.27956(14) 0.5886(3) 0.0353(11) Uani 1 1 d . . . . .
C14 C 0.8550(5) 0.32510(15) 0.5810(4) 0.0488(13) Uani 1 1 d . . . . .
H14A H 0.9213 0.3291 0.5511 0.073 Uiso 1 1 calc R U . . .
H14B H 0.7968 0.3382 0.5481 0.073 Uiso 1 1 calc R U . . .
H14C H 0.8616 0.3370 0.6388 0.073 Uiso 1 1 calc R U . . .
C15 C 0.8470(4) 0.27165(14) 0.8355(3) 0.0350(11) Uani 1 1 d . . . . .
H15 H 0.8635 0.3007 0.8468 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8421(4) 0.24685(14) 0.9223(3) 0.0353(11) Uani 1 1 d . . . . .
H16 H 0.8531 0.2646 0.9742 0.042 Uiso 1 1 calc R U . . .
C17 C 0.8073(4) 0.14687(13) 1.0319(3) 0.0335(11) Uani 1 1 d . . . . .
H17 H 0.8147 0.1578 1.0920 0.040 Uiso 1 1 calc R U . . .
C18 C 0.7870(4) 0.09998(14) 1.0319(3) 0.0358(11) Uani 1 1 d . . . . .
H18 H 0.7848 0.0890 1.0920 0.043 Uiso 1 1 calc R U . . .
C19 C 0.7394(4) -0.00237(14) 0.9349(3) 0.0372(11) Uani 1 1 d . . . . .
C20 C 0.7384(5) -0.02595(18) 1.0213(4) 0.0576(15) Uani 1 1 d . . . . .
H20A H 0.6685 -0.0381 1.0280 0.086 Uiso 1 1 calc R U . . .
H20B H 0.7923 -0.0472 1.0211 0.086 Uiso 1 1 calc R U . . .
H20C H 0.7539 -0.0074 1.0694 0.086 Uiso 1 1 calc R U . . .
C21 C 0.7225(4) -0.02937(14) 0.8482(3) 0.0361(11) Uani 1 1 d . . . . .
C22 C 0.7086(5) -0.07558(15) 0.8628(4) 0.0551(15) Uani 1 1 d . . . . .
H22A H 0.7734 -0.0866 0.8904 0.083 Uiso 1 1 calc R U . . .
H22B H 0.6488 -0.0802 0.9001 0.083 Uiso 1 1 calc R U . . .
H22C H 0.6950 -0.0890 0.8071 0.083 Uiso 1 1 calc R U . . .
C23 C 0.7047(4) -0.02096(13) 0.5983(3) 0.0353(11) Uani 1 1 d . . . . .
H23 H 0.6913 -0.0497 0.5814 0.042 Uiso 1 1 calc R U . . .
C24 C 0.7092(4) 0.00727(14) 0.5158(3) 0.0348(11) Uani 1 1 d . . . . .
H24 H 0.6999 -0.0085 0.4610 0.042 Uiso 1 1 calc R U . . .
C25 C 0.7413(4) 0.10504(14) 0.4067(3) 0.0337(11) Uani 1 1 d . . . . .
H25 H 0.7306 0.0920 0.3488 0.040 Uiso 1 1 calc R U . . .
C26 C 0.7601(4) 0.15178(14) 0.3988(3) 0.0345(11) Uani 1 1 d . . . . .
H26 H 0.7586 0.1608 0.3372 0.041 Uiso 1 1 calc R U . . .
C27 C 0.8137(4) 0.25582(13) 0.4976(3) 0.0334(11) Uani 1 1 d . . . . .
C28 C 0.8187(4) 0.28205(16) 0.4154(3) 0.0473(13) Uani 1 1 d . . . . .
H28A H 0.8898 0.2935 0.4116 0.071 Uiso 1 1 calc R U . . .
H28B H 0.8027 0.2653 0.3644 0.071 Uiso 1 1 calc R U . . .
H28C H 0.7667 0.3039 0.4181 0.071 Uiso 1 1 calc R U . . .
C29 C 0.6626(4) 0.24748(14) 0.5858(3) 0.0366(11) Uani 1 1 d . . . . .
C30 C 0.7022(4) 0.28974(15) 0.7181(3) 0.0399(12) Uani 1 1 d . . . . .
H30A H 0.7308 0.3175 0.7221 0.048 Uiso 1 1 calc R U . . .
H30B H 0.6240 0.2916 0.7189 0.048 Uiso 1 1 calc R U . . .
C31 C 0.6742(4) 0.24400(14) 0.8458(3) 0.0383(12) Uani 1 1 d . . . . .
C32 C 0.6844(4) 0.20611(15) 0.9857(3) 0.0406(12) Uani 1 1 d . . . . .
H32A H 0.7066 0.2178 1.0423 0.049 Uiso 1 1 calc R U . . .
H32B H 0.6065 0.2088 0.9792 0.049 Uiso 1 1 calc R U . . .
C33 C 0.6379(4) 0.13291(15) 0.9662(3) 0.0378(12) Uani 1 1 d . . . . .
C34 C 0.6215(4) 0.05797(15) 0.9915(3) 0.0439(13) Uani 1 1 d . . . . .
H34A H 0.5454 0.0647 0.9838 0.053 Uiso 1 1 calc R U . . .
H34B H 0.6328 0.0465 1.0501 0.053 Uiso 1 1 calc R U . . .
C35 C 0.5843(4) 0.01986(14) 0.8540(3) 0.0400(12) Uani 1 1 d . . . . .
C36 C 0.5738(4) -0.02443(15) 0.7232(3) 0.0389(12) Uani 1 1 d . . . . .
H36A H 0.5829 -0.0539 0.7169 0.047 Uiso 1 1 calc R U . . .
H36B H 0.4969 -0.0189 0.7253 0.047 Uiso 1 1 calc R U . . .
C37 C 0.5655(4) 0.02733(15) 0.6020(3) 0.0398(12) Uani 1 1 d . . . . .
C38 C 0.5825(4) 0.06447(15) 0.4616(4) 0.0437(12) Uani 1 1 d . . . . .
H38A H 0.5082 0.0716 0.4731 0.052 Uiso 1 1 calc R U . . .
H38B H 0.5830 0.0513 0.4043 0.052 Uiso 1 1 calc R U . . .
C39 C 0.6010(4) 0.13992(15) 0.4748(3) 0.0395(11) Uani 1 1 d . . . . .
C40 C 0.6473(4) 0.21277(14) 0.4433(3) 0.0394(12) Uani 1 1 d . . . . .
H40A H 0.5706 0.2164 0.4521 0.047 Uiso 1 1 calc R U . . .
H40B H 0.6622 0.2230 0.3850 0.047 Uiso 1 1 calc R U . . .
N1 N 0.9257(3) 0.25793(11) 0.6292(3) 0.0357(9) Uani 1 1 d . . . . .
N2 N 0.9326(3) 0.25160(12) 0.7893(2) 0.0352(9) Uani 1 1 d . . . . .
N3 N 0.9286(3) 0.21740(12) 0.9150(3) 0.0364(9) Uani 1 1 d . . . . .
N4 N 0.9058(3) 0.15133(12) 0.9855(3) 0.0403(10) Uani 1 1 d . . . . .
N5 N 0.8783(3) 0.08428(11) 0.9860(3) 0.0360(9) Uani 1 1 d . . . . .
N6 N 0.8440(3) 0.01676(11) 0.9214(3) 0.0358(9) Uani 1 1 d . . . . .
N7 N 0.8203(3) -0.02107(12) 0.8007(3) 0.0367(9) Uani 1 1 d . . . . .
N8 N 0.8095(3) -0.01617(12) 0.6412(3) 0.0372(9) Uani 1 1 d . . . . .
N9 N 0.8170(3) 0.02521(11) 0.5250(3) 0.0359(9) Uani 1 1 d . . . . .
N10 N 0.8396(3) 0.09075(11) 0.4521(2) 0.0327(9) Uani 1 1 d . . . . .
N11 N 0.8652(3) 0.15786(11) 0.4415(3) 0.0336(9) Uani 1 1 d . . . . .
N12 N 0.9017(3) 0.22564(11) 0.5015(2) 0.0326(9) Uani 1 1 d . . . . .
N13 N 0.7327(3) 0.27161(12) 0.6335(2) 0.0375(9) Uani 1 1 d . . . . .
N14 N 0.7409(3) 0.26656(12) 0.7947(3) 0.0391(10) Uani 1 1 d . . . . .
N15 N 0.7334(3) 0.22979(12) 0.9167(3) 0.0392(10) Uani 1 1 d . . . . .
N16 N 0.7119(3) 0.16310(12) 0.9855(3) 0.0371(9) Uani 1 1 d . . . . .
N17 N 0.6845(3) 0.09547(12) 0.9849(3) 0.0374(9) Uani 1 1 d . . . . .
N18 N 0.6489(3) 0.02684(12) 0.9265(3) 0.0403(10) Uani 1 1 d . . . . .
N19 N 0.6258(3) -0.01149(12) 0.8063(3) 0.0384(10) Uani 1 1 d . . . . .
N20 N 0.6155(3) -0.00425(12) 0.6463(3) 0.0381(10) Uani 1 1 d . . . . .
N21 N 0.6207(3) 0.03553(12) 0.5272(3) 0.0395(10) Uani 1 1 d . . . . .
N22 N 0.6455(3) 0.10203(12) 0.4586(3) 0.0385(10) Uani 1 1 d . . . . .
N23 N 0.6717(3) 0.16938(12) 0.4466(3) 0.0384(10) Uani 1 1 d . . . . .
N24 N 0.7073(3) 0.23720(11) 0.5080(3) 0.0351(9) Uani 1 1 d . . . . .
N25 N 0.9637(5) 0.13489(18) 0.2169(4) 0.0633(14) Uani 1 1 d . . . . .
N26 N 0.5842(4) 0.12088(15) 0.2121(3) 0.0483(11) Uani 1 1 d . . . . .
N27 N 1.2340(4) 0.13684(13) 0.4290(3) 0.0468(11) Uani 1 1 d . . . . .
O1 O 1.0394(3) 0.20423(10) 0.5974(2) 0.0433(8) Uani 1 1 d . . . . .
O2 O 1.0611(3) 0.20178(10) 0.8178(2) 0.0491(9) Uani 1 1 d . . . . .
O1W O 0.9755(4) 0.12137(17) 0.6993(3) 0.0860(15) Uani 1 1 d . . . . .
O3 O 1.0373(3) 0.10909(11) 0.9305(3) 0.0551(10) Uani 1 1 d . . . . .
O2W O 1.2658(3) 0.20181(12) 0.6577(3) 0.0731(13) Uani 1 1 d . . . . .
O4 O 0.9781(3) 0.01595(11) 0.8209(2) 0.0534(10) Uani 1 1 d . . . . .
O3W O 1.3454(3) 0.11794(12) 0.6416(3) 0.0615(11) Uani 1 1 d . . . . .
O5 O 0.9698(3) 0.01668(10) 0.6145(2) 0.0453(9) Uani 1 1 d . . . . .
O4W O 1.1489(3) 0.06271(11) 0.6297(3) 0.0553(10) Uani 1 1 d . . . . .
O6 O 1.0019(3) 0.11783(10) 0.5032(2) 0.0437(8) Uani 1 1 d . . . . .
O5W O 1.1854(4) 0.12964(15) 0.7808(3) 0.0744(13) Uani 1 1 d . . . . .
O7 O 0.5714(3) 0.23764(11) 0.6069(2) 0.0464(9) Uani 1 1 d . . . . .
O8 O 0.5777(3) 0.23795(11) 0.8316(2) 0.0478(9) Uani 1 1 d . . . . .
O9 O 0.5465(3) 0.13915(11) 0.9365(3) 0.0566(10) Uani 1 1 d . . . . .
O10 O 0.4988(3) 0.03776(12) 0.8356(3) 0.0592(10) Uani 1 1 d . . . . .
O11 O 0.4832(3) 0.04493(11) 0.6236(3) 0.0542(10) Uani 1 1 d . . . . .
O12 O 0.5147(3) 0.14639(11) 0.5087(3) 0.0557(10) Uani 1 1 d . . . . .
O13 O 1.0295(5) 0.1174(2) 0.1735(4) 0.120(2) Uani 1 1 d . . . . .
O14 O 0.9550(4) 0.17345(15) 0.2155(3) 0.0789(14) Uani 1 1 d . . . . .
O15 O 0.8976(6) 0.11405(17) 0.2549(4) 0.126(3) Uani 1 1 d . . . . .
O16 O 0.6272(4) 0.14781(13) 0.1673(3) 0.0822(15) Uani 1 1 d . . . . .
O17 O 0.5291(5) 0.13082(15) 0.2735(3) 0.0883(16) Uani 1 1 d . . . . .
O18 O 0.5995(5) 0.08455(15) 0.1959(4) 0.1039(19) Uani 1 1 d . . . . .
O19 O 1.2277(3) 0.10567(11) 0.4778(2) 0.0561(10) Uani 1 1 d . . . . .
O20 O 1.2075(3) 0.17079(10) 0.4628(2) 0.0527(10) Uani 1 1 d . . . . .
O21 O 1.2633(4) 0.13390(12) 0.3535(3) 0.0786(15) Uani 1 1 d . . . . .
La1 La 1.14736(2) 0.13949(2) 0.61647(2) 0.03663(11) Uani 1 1 d . . . . .
O6W O 0.7553(4) 0.21519(12) 0.2158(3) 0.0663(12) Uani 1 1 d . . . . .
O7W O 0.4748(4) 0.18436(16) 0.7159(3) 0.0877(15) Uani 1 1 d . . . . .
O8W O 0.8487(3) 0.03409(13) 1.2132(3) 0.0652(11) Uani 1 1 d . . . . .
O9W O 0.7026(4) -0.01572(17) 0.2829(4) 0.0954(17) Uani 1 1 d . . . . .
O10W O 1.3707(4) 0.10571(16) 0.8534(5) 0.124(2) Uani 1 1 d . . . . .
O11W O 0.6181(7) 0.1134(3) 0.7309(6) 0.181(3) Uani 1 1 d . . . . .
O12W O 0.7878(17) 0.1593(7) 0.6961(14) 0.213(8) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.249(6) . ?
C1 N1 1.349(6) . ?
C1 N12 1.352(6) . ?
C2 N2 1.443(6) . ?
C2 N1 1.459(6) . ?
C3 O2 1.229(5) . ?
C3 N3 1.355(6) . ?
C3 N2 1.359(6) . ?
C4 N4 1.437(6) . ?
C4 N3 1.453(6) . ?
C5 O3 1.214(6) . ?
C5 N4 1.371(6) . ?
C5 N5 1.373(6) . ?
C6 N5 1.447(6) . ?
C6 N6 1.456(6) . ?
C7 O4 1.231(6) . ?
C7 N7 1.355(6) . ?
C7 N6 1.361(6) . ?
C8 N8 1.438(6) . ?
C8 N7 1.456(6) . ?
C9 O5 1.227(6) . ?
C9 N9 1.362(6) . ?
C9 N8 1.364(6) . ?
C10 N10 1.442(6) . ?
C10 N9 1.446(6) . ?
C11 O6 1.231(6) . ?
C11 N10 1.357(6) . ?
C11 N11 1.360(6) . ?
C12 N12 1.450(5) . ?
C12 N11 1.452(6) . ?
C13 N13 1.452(6) . ?
C13 N1 1.469(6) . ?
C13 C14 1.511(7) . ?
C13 C27 1.592(6) . ?
C15 N14 1.440(6) . ?
C15 N2 1.447(6) . ?
C15 C16 1.547(6) . ?
C16 N3 1.442(6) . ?
C16 N15 1.455(6) . ?
C17 N4 1.438(6) . ?
C17 N16 1.451(6) . ?
C17 C18 1.543(6) . ?
C18 N17 1.440(6) . ?
C18 N5 1.441(6) . ?
C19 N6 1.457(6) . ?
C19 N18 1.469(6) . ?
C19 C20 1.518(7) . ?
C19 C21 1.589(7) . ?
C21 N19 1.455(6) . ?
C21 N7 1.456(6) . ?
C21 C22 1.527(6) . ?
C23 N8 1.439(6) . ?
C23 N20 1.450(6) . ?
C23 C24 1.553(7) . ?
C24 N21 1.444(6) . ?
C24 N9 1.458(6) . ?
C25 N22 1.450(6) . ?
C25 N10 1.451(6) . ?
C25 C26 1.541(6) . ?
C26 N11 1.445(6) . ?
C26 N23 1.451(6) . ?
C27 N24 1.463(6) . ?
C27 N12 1.465(6) . ?
C27 C28 1.514(6) . ?
C29 O7 1.227(6) . ?
C29 N13 1.357(6) . ?
C29 N24 1.364(6) . ?
C30 N14 1.452(6) . ?
C30 N13 1.474(6) . ?
C31 O8 1.222(6) . ?
C31 N15 1.360(6) . ?
C31 N14 1.366(6) . ?
C32 N16 1.437(6) . ?
C32 N15 1.449(6) . ?
C33 O9 1.219(6) . ?
C33 N16 1.366(6) . ?
C33 N17 1.371(6) . ?
C34 N17 1.451(6) . ?
C34 N18 1.461(6) . ?
C35 O10 1.230(6) . ?
C35 N18 1.356(6) . ?
C35 N19 1.360(6) . ?
C36 N20 1.450(6) . ?
C36 N19 1.458(6) . ?
C37 O11 1.223(6) . ?
C37 N20 1.363(6) . ?
C37 N21 1.372(6) . ?
C38 N21 1.436(6) . ?
C38 N22 1.449(6) . ?
C39 O12 1.220(6) . ?
C39 N22 1.374(6) . ?
C39 N23 1.375(6) . ?
C40 N23 1.441(6) . ?
C40 N24 1.446(6) . ?
N25 O13 1.209(7) . ?
N25 O15 1.222(7) . ?
N25 O14 1.257(6) . ?
N26 O17 1.217(6) . ?
N26 O18 1.222(6) . ?
N26 O16 1.240(6) . ?
N27 O21 1.217(6) . ?
N27 O19 1.259(5) . ?
N27 O20 1.264(5) . ?
O1 La1 2.502(3) . ?
O1W La1 2.578(4) . ?
O2W La1 2.563(4) . ?
O3W La1 2.564(4) . ?
O4W La1 2.501(4) . ?
O6 La1 2.542(3) . ?
O5W La1 2.541(4) . ?
O19 La1 2.603(3) . ?
O20 La1 2.675(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 124.8(4) . . ?
O1 C1 N12 124.9(4) . . ?
N1 C1 N12 110.2(4) . . ?
N2 C2 N1 114.3(4) . . ?
O2 C3 N3 125.8(5) . . ?
O2 C3 N2 125.2(5) . . ?
N3 C3 N2 109.0(4) . . ?
N4 C4 N3 113.7(4) . . ?
O3 C5 N4 126.3(4) . . ?
O3 C5 N5 126.8(4) . . ?
N4 C5 N5 106.9(4) . . ?
N5 C6 N6 113.8(4) . . ?
O4 C7 N7 126.0(4) . . ?
O4 C7 N6 124.5(5) . . ?
N7 C7 N6 109.4(4) . . ?
N8 C8 N7 113.7(4) . . ?
O5 C9 N9 125.7(4) . . ?
O5 C9 N8 125.1(5) . . ?
N9 C9 N8 109.2(4) . . ?
N10 C10 N9 113.8(4) . . ?
O6 C11 N10 125.6(4) . . ?
O6 C11 N11 125.6(4) . . ?
N10 C11 N11 108.8(4) . . ?
N12 C12 N11 112.9(4) . . ?
N13 C13 N1 112.8(4) . . ?
N13 C13 C14 112.0(4) . . ?
N1 C13 C14 110.7(4) . . ?
N13 C13 C27 102.9(4) . . ?
N1 C13 C27 102.6(3) . . ?
C14 C13 C27 115.4(4) . . ?
N14 C15 N2 114.3(4) . . ?
N14 C15 C16 104.1(4) . . ?
N2 C15 C16 103.3(4) . . ?
N3 C16 N15 115.5(4) . . ?
N3 C16 C15 103.1(4) . . ?
N15 C16 C15 102.3(4) . . ?
N4 C17 N16 114.5(4) . . ?
N4 C17 C18 103.9(4) . . ?
N16 C17 C18 103.3(4) . . ?
N17 C18 N5 114.6(4) . . ?
N17 C18 C17 103.9(4) . . ?
N5 C18 C17 102.7(4) . . ?
N6 C19 N18 113.0(4) . . ?
N6 C19 C20 111.8(4) . . ?
N18 C19 C20 111.8(4) . . ?
N6 C19 C21 102.1(3) . . ?
N18 C19 C21 102.0(4) . . ?
C20 C19 C21 115.6(4) . . ?
N19 C21 N7 113.3(4) . . ?
N19 C21 C22 111.1(4) . . ?
N7 C21 C22 110.7(4) . . ?
N19 C21 C19 102.8(4) . . ?
N7 C21 C19 102.8(4) . . ?
C22 C21 C19 115.7(4) . . ?
N8 C23 N20 115.0(4) . . ?
N8 C23 C24 104.1(4) . . ?
N20 C23 C24 103.5(4) . . ?
N21 C24 N9 115.5(4) . . ?
N21 C24 C23 103.2(4) . . ?
N9 C24 C23 102.6(4) . . ?
N22 C25 N10 114.1(4) . . ?
N22 C25 C26 103.7(4) . . ?
N10 C25 C26 103.1(4) . . ?
N11 C26 N23 113.9(4) . . ?
N11 C26 C25 103.6(4) . . ?
N23 C26 C25 103.3(4) . . ?
N24 C27 N12 113.0(4) . . ?
N24 C27 C28 112.6(4) . . ?
N12 C27 C28 110.9(4) . . ?
N24 C27 C13 102.0(3) . . ?
N12 C27 C13 101.9(4) . . ?
C28 C27 C13 115.7(4) . . ?
O7 C29 N13 126.0(5) . . ?
O7 C29 N24 124.6(5) . . ?
N13 C29 N24 109.4(4) . . ?
N14 C30 N13 113.8(4) . . ?
O8 C31 N15 125.4(5) . . ?
O8 C31 N14 126.3(5) . . ?
N15 C31 N14 108.2(4) . . ?
N16 C32 N15 114.2(4) . . ?
O9 C33 N16 124.5(5) . . ?
O9 C33 N17 127.0(5) . . ?
N16 C33 N17 108.5(4) . . ?
N17 C34 N18 113.3(4) . . ?
O10 C35 N18 125.6(5) . . ?
O10 C35 N19 124.9(5) . . ?
N18 C35 N19 109.4(4) . . ?
N20 C36 N19 114.1(4) . . ?
O11 C37 N20 126.0(5) . . ?
O11 C37 N21 125.2(5) . . ?
N20 C37 N21 108.8(4) . . ?
N21 C38 N22 114.1(4) . . ?
O12 C39 N22 126.3(5) . . ?
O12 C39 N23 126.0(5) . . ?
N22 C39 N23 107.7(4) . . ?
N23 C40 N24 114.3(4) . . ?
C1 N1 C2 121.5(4) . . ?
C1 N1 C13 112.3(4) . . ?
C2 N1 C13 126.1(4) . . ?
C3 N2 C2 122.2(4) . . ?
C3 N2 C15 112.0(4) . . ?
C2 N2 C15 123.7(4) . . ?
C3 N3 C16 112.5(4) . . ?
C3 N3 C4 122.0(4) . . ?
C16 N3 C4 125.2(4) . . ?
C5 N4 C4 122.5(4) . . ?
C5 N4 C17 112.8(4) . . ?
C4 N4 C17 122.7(4) . . ?
C5 N5 C18 113.5(4) . . ?
C5 N5 C6 121.7(4) . . ?
C18 N5 C6 122.8(4) . . ?
C7 N6 C6 120.1(4) . . ?
C7 N6 C19 113.0(4) . . ?
C6 N6 C19 126.4(4) . . ?
C7 N7 C21 112.7(4) . . ?
C7 N7 C8 121.8(4) . . ?
C21 N7 C8 125.4(4) . . ?
C9 N8 C8 123.0(4) . . ?
C9 N8 C23 111.9(4) . . ?
C8 N8 C23 124.6(4) . . ?
C9 N9 C10 122.0(4) . . ?
C9 N9 C24 112.0(4) . . ?
C10 N9 C24 124.0(4) . . ?
C11 N10 C10 123.6(4) . . ?
C11 N10 C25 112.3(4) . . ?
C10 N10 C25 122.0(4) . . ?
C11 N11 C26 112.2(4) . . ?
C11 N11 C12 123.4(4) . . ?
C26 N11 C12 122.5(4) . . ?
C1 N12 C12 121.1(4) . . ?
C1 N12 C27 112.9(4) . . ?
C12 N12 C27 125.9(4) . . ?
C29 N13 C13 112.9(4) . . ?
C29 N13 C30 121.1(4) . . ?
C13 N13 C30 125.8(4) . . ?
C31 N14 C15 112.1(4) . . ?
C31 N14 C30 123.0(4) . . ?
C15 N14 C30 123.7(4) . . ?
C31 N15 C32 121.6(4) . . ?
C31 N15 C16 112.8(4) . . ?
C32 N15 C16 124.8(4) . . ?
C33 N16 C32 122.7(4) . . ?
C33 N16 C17 111.8(4) . . ?
C32 N16 C17 122.7(4) . . ?
C33 N17 C18 111.7(4) . . ?
C33 N17 C34 122.3(4) . . ?
C18 N17 C34 121.2(4) . . ?
C35 N18 C34 121.2(4) . . ?
C35 N18 C19 112.8(4) . . ?
C34 N18 C19 125.7(4) . . ?
C35 N19 C21 112.8(4) . . ?
C35 N19 C36 120.8(4) . . ?
C21 N19 C36 126.4(4) . . ?
C37 N20 C23 112.0(4) . . ?
C37 N20 C36 124.6(4) . . ?
C23 N20 C36 122.4(4) . . ?
C37 N21 C38 122.6(4) . . ?
C37 N21 C24 112.2(4) . . ?
C38 N21 C24 124.4(4) . . ?
C39 N22 C38 121.9(4) . . ?
C39 N22 C25 112.2(4) . . ?
C38 N22 C25 121.7(4) . . ?
C39 N23 C40 123.8(4) . . ?
C39 N23 C26 112.4(4) . . ?
C40 N23 C26 121.9(4) . . ?
C29 N24 C40 120.5(4) . . ?
C29 N24 C27 112.8(4) . . ?
C40 N24 C27 126.6(4) . . ?
O13 N25 O15 118.2(7) . . ?
O13 N25 O14 121.3(6) . . ?
O15 N25 O14 120.1(6) . . ?
O17 N26 O18 120.4(5) . . ?
O17 N26 O16 119.8(5) . . ?
O18 N26 O16 119.8(5) . . ?
O21 N27 O19 121.2(4) . . ?
O21 N27 O20 122.7(4) . . ?
O19 N27 O20 116.1(4) . . ?
C1 O1 La1 159.0(3) . . ?
C11 O6 La1 150.5(3) . . ?
N27 O19 La1 99.8(3) . . ?
N27 O20 La1 96.2(3) . . ?
O4W La1 O1 148.12(12) . . ?
O4W La1 O5W 78.18(14) . . ?
O1 La1 O5W 107.37(12) . . ?
O4W La1 O6 77.38(12) . . ?
O1 La1 O6 78.00(11) . . ?
O5W La1 O6 136.89(14) . . ?
O4W La1 O2W 139.90(13) . . ?
O1 La1 O2W 70.32(13) . . ?
O5W La1 O2W 77.05(16) . . ?
O6 La1 O2W 140.18(13) . . ?
O4W La1 O3W 73.25(12) . . ?
O1 La1 O3W 138.60(12) . . ?
O5W La1 O3W 71.19(14) . . ?
O6 La1 O3W 132.41(12) . . ?
O2W La1 O3W 69.15(13) . . ?
O4W La1 O1W 74.76(15) . . ?
O1 La1 O1W 78.55(15) . . ?
O5W La1 O1W 67.63(15) . . ?
O6 La1 O1W 71.95(13) . . ?
O2W La1 O1W 122.40(16) . . ?
O3W La1 O1W 131.79(15) . . ?
O4W La1 O19 69.05(12) . . ?
O1 La1 O19 118.63(11) . . ?
O5W La1 O19 132.65(13) . . ?
O6 La1 O19 67.59(12) . . ?
O2W La1 O19 107.37(14) . . ?
O3W La1 O19 67.28(13) . . ?
O1W La1 O19 130.12(15) . . ?
O4W La1 O20 116.57(12) . . ?
O1 La1 O20 75.17(11) . . ?
O5W La1 O20 148.90(14) . . ?
O6 La1 O20 74.21(11) . . ?
O2W La1 O20 74.83(14) . . ?
O3W La1 O20 86.50(13) . . ?
O1W La1 O20 140.59(14) . . ?
O19 La1 O20 47.83(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N14 C15 C16 N3 122.1(4) . . . . ?
N2 C15 C16 N3 2.4(5) . . . . ?
N14 C15 C16 N15 1.9(4) . . . . ?
N2 C15 C16 N15 -117.8(4) . . . . ?
N4 C17 C18 N17 -119.1(4) . . . . ?
N16 C17 C18 N17 0.8(4) . . . . ?
N4 C17 C18 N5 0.6(5) . . . . ?
N16 C17 C18 N5 120.5(4) . . . . ?
N6 C19 C21 N19 -117.7(4) . . . . ?
N18 C19 C21 N19 -0.7(4) . . . . ?
C20 C19 C21 N19 120.8(4) . . . . ?
N6 C19 C21 N7 0.2(4) . . . . ?
N18 C19 C21 N7 117.2(4) . . . . ?
C20 C19 C21 N7 -121.4(4) . . . . ?
N6 C19 C21 C22 121.0(5) . . . . ?
N18 C19 C21 C22 -122.0(5) . . . . ?
C20 C19 C21 C22 -0.6(6) . . . . ?
N8 C23 C24 N21 -121.7(4) . . . . ?
N20 C23 C24 N21 -1.2(4) . . . . ?
N8 C23 C24 N9 -1.3(4) . . . . ?
N20 C23 C24 N9 119.2(4) . . . . ?
N22 C25 C26 N11 118.5(4) . . . . ?
N10 C25 C26 N11 -0.7(4) . . . . ?
N22 C25 C26 N23 -0.6(5) . . . . ?
N10 C25 C26 N23 -119.8(4) . . . . ?
N13 C13 C27 N24 -1.8(4) . . . . ?
N1 C13 C27 N24 115.4(4) . . . . ?
C14 C13 C27 N24 -124.1(4) . . . . ?
N13 C13 C27 N12 -118.7(4) . . . . ?
N1 C13 C27 N12 -1.5(4) . . . . ?
C14 C13 C27 N12 119.0(4) . . . . ?
N13 C13 C27 C28 120.8(4) . . . . ?
N1 C13 C27 C28 -121.9(4) . . . . ?
C14 C13 C27 C28 -1.4(6) . . . . ?
O1 C1 N1 C2 2.4(7) . . . . ?
N12 C1 N1 C2 -174.5(4) . . . . ?
O1 C1 N1 C13 179.4(4) . . . . ?
N12 C1 N1 C13 2.4(5) . . . . ?
N2 C2 N1 C1 -98.6(5) . . . . ?
N2 C2 N1 C13 84.9(5) . . . . ?
N13 C13 N1 C1 109.6(4) . . . . ?
C14 C13 N1 C1 -124.1(4) . . . . ?
C27 C13 N1 C1 -0.4(5) . . . . ?
N13 C13 N1 C2 -73.7(6) . . . . ?
C14 C13 N1 C2 52.7(6) . . . . ?
C27 C13 N1 C2 176.3(4) . . . . ?
O2 C3 N2 C2 -9.9(7) . . . . ?
N3 C3 N2 C2 167.7(4) . . . . ?
O2 C3 N2 C15 -173.9(5) . . . . ?
N3 C3 N2 C15 3.7(5) . . . . ?
N1 C2 N2 C3 110.3(5) . . . . ?
N1 C2 N2 C15 -87.6(5) . . . . ?
N14 C15 N2 C3 -116.3(4) . . . . ?
C16 C15 N2 C3 -3.8(5) . . . . ?
N14 C15 N2 C2 80.0(5) . . . . ?
C16 C15 N2 C2 -167.5(4) . . . . ?
O2 C3 N3 C16 175.6(5) . . . . ?
N2 C3 N3 C16 -2.0(5) . . . . ?
O2 C3 N3 C4 1.6(7) . . . . ?
N2 C3 N3 C4 -176.0(4) . . . . ?
N15 C16 N3 C3 110.3(5) . . . . ?
C15 C16 N3 C3 -0.4(5) . . . . ?
N15 C16 N3 C4 -75.9(6) . . . . ?
C15 C16 N3 C4 173.4(4) . . . . ?
N4 C4 N3 C3 -100.6(5) . . . . ?
N4 C4 N3 C16 86.2(6) . . . . ?
O3 C5 N4 C4 -9.0(8) . . . . ?
N5 C5 N4 C4 169.9(4) . . . . ?
O3 C5 N4 C17 -173.3(5) . . . . ?
N5 C5 N4 C17 5.6(6) . . . . ?
N3 C4 N4 C5 111.0(5) . . . . ?
N3 C4 N4 C17 -86.2(6) . . . . ?
N16 C17 N4 C5 -115.7(5) . . . . ?
C18 C17 N4 C5 -3.8(5) . . . . ?
N16 C17 N4 C4 80.0(6) . . . . ?
C18 C17 N4 C4 -168.1(4) . . . . ?
O3 C5 N5 C18 173.7(5) . . . . ?
N4 C5 N5 C18 -5.1(6) . . . . ?
O3 C5 N5 C6 9.5(8) . . . . ?
N4 C5 N5 C6 -169.3(4) . . . . ?
N17 C18 N5 C5 114.7(5) . . . . ?
C17 C18 N5 C5 2.7(5) . . . . ?
N17 C18 N5 C6 -81.3(5) . . . . ?
C17 C18 N5 C6 166.7(4) . . . . ?
N6 C6 N5 C5 -115.7(5) . . . . ?
N6 C6 N5 C18 81.6(6) . . . . ?
O4 C7 N6 C6 -4.6(7) . . . . ?
N7 C7 N6 C6 172.6(4) . . . . ?
O4 C7 N6 C19 -176.5(5) . . . . ?
N7 C7 N6 C19 0.7(6) . . . . ?
N5 C6 N6 C7 102.7(5) . . . . ?
N5 C6 N6 C19 -86.5(6) . . . . ?
N18 C19 N6 C7 -109.2(5) . . . . ?
C20 C19 N6 C7 123.6(5) . . . . ?
C21 C19 N6 C7 -0.5(5) . . . . ?
N18 C19 N6 C6 79.4(6) . . . . ?
C20 C19 N6 C6 -47.7(6) . . . . ?
C21 C19 N6 C6 -171.9(4) . . . . ?
O4 C7 N7 C21 176.7(5) . . . . ?
N6 C7 N7 C21 -0.5(6) . . . . ?
O4 C7 N7 C8 -1.2(8) . . . . ?
N6 C7 N7 C8 -178.4(4) . . . . ?
N19 C21 N7 C7 110.4(5) . . . . ?
C22 C21 N7 C7 -124.0(5) . . . . ?
C19 C21 N7 C7 0.2(5) . . . . ?
N19 C21 N7 C8 -71.8(5) . . . . ?
C22 C21 N7 C8 53.8(6) . . . . ?
C19 C21 N7 C8 178.0(4) . . . . ?
N8 C8 N7 C7 -92.0(5) . . . . ?
N8 C8 N7 C21 90.4(5) . . . . ?
O5 C9 N8 C8 -2.2(7) . . . . ?
N9 C9 N8 C8 176.5(4) . . . . ?
O5 C9 N8 C23 -174.8(4) . . . . ?
N9 C9 N8 C23 3.9(5) . . . . ?
N7 C8 N8 C9 100.0(5) . . . . ?
N7 C8 N8 C23 -88.4(5) . . . . ?
N20 C23 N8 C9 -113.9(4) . . . . ?
C24 C23 N8 C9 -1.4(5) . . . . ?
N20 C23 N8 C8 73.6(5) . . . . ?
C24 C23 N8 C8 -173.9(4) . . . . ?
O5 C9 N9 C10 9.5(7) . . . . ?
N8 C9 N9 C10 -169.1(4) . . . . ?
O5 C9 N9 C24 173.8(4) . . . . ?
N8 C9 N9 C24 -4.9(5) . . . . ?
N10 C10 N9 C9 -112.7(5) . . . . ?
N10 C10 N9 C24 84.9(5) . . . . ?
N21 C24 N9 C9 115.3(4) . . . . ?
C23 C24 N9 C9 3.8(5) . . . . ?
N21 C24 N9 C10 -80.8(5) . . . . ?
C23 C24 N9 C10 167.7(4) . . . . ?
O6 C11 N10 C10 -12.2(7) . . . . ?
N11 C11 N10 C10 166.7(4) . . . . ?
O6 C11 N10 C25 -176.3(4) . . . . ?
N11 C11 N10 C25 2.6(5) . . . . ?
N9 C10 N10 C11 114.2(5) . . . . ?
N9 C10 N10 C25 -83.2(5) . . . . ?
N22 C25 N10 C11 -112.8(4) . . . . ?
C26 C25 N10 C11 -1.1(5) . . . . ?
N22 C25 N10 C10 82.8(5) . . . . ?
C26 C25 N10 C10 -165.5(4) . . . . ?
O6 C11 N11 C26 175.8(4) . . . . ?
N10 C11 N11 C26 -3.1(5) . . . . ?
O6 C11 N11 C12 11.5(7) . . . . ?
N10 C11 N11 C12 -167.4(4) . . . . ?
N23 C26 N11 C11 113.8(4) . . . . ?
C25 C26 N11 C11 2.3(5) . . . . ?
N23 C26 N11 C12 -81.7(5) . . . . ?
C25 C26 N11 C12 166.8(4) . . . . ?
N12 C12 N11 C11 -107.4(5) . . . . ?
N12 C12 N11 C26 89.8(5) . . . . ?
O1 C1 N12 C12 1.0(7) . . . . ?
N1 C1 N12 C12 177.9(4) . . . . ?
O1 C1 N12 C27 179.5(4) . . . . ?
N1 C1 N12 C27 -3.5(5) . . . . ?
N11 C12 N12 C1 91.4(5) . . . . ?
N11 C12 N12 C27 -87.0(5) . . . . ?
N24 C27 N12 C1 -105.7(4) . . . . ?
C28 C27 N12 C1 126.8(4) . . . . ?
C13 C27 N12 C1 3.0(5) . . . . ?
N24 C27 N12 C12 72.8(5) . . . . ?
C28 C27 N12 C12 -54.8(6) . . . . ?
C13 C27 N12 C12 -178.5(4) . . . . ?
O7 C29 N13 C13 -176.8(4) . . . . ?
N24 C29 N13 C13 0.4(5) . . . . ?
O7 C29 N13 C30 -1.5(7) . . . . ?
N24 C29 N13 C30 175.6(4) . . . . ?
N1 C13 N13 C29 -108.8(4) . . . . ?
C14 C13 N13 C29 125.5(5) . . . . ?
C27 C13 N13 C29 1.0(5) . . . . ?
N1 C13 N13 C30 76.2(5) . . . . ?
C14 C13 N13 C30 -49.5(6) . . . . ?
C27 C13 N13 C30 -174.0(4) . . . . ?
N14 C30 N13 C29 97.7(5) . . . . ?
N14 C30 N13 C13 -87.7(6) . . . . ?
O8 C31 N14 C15 173.1(5) . . . . ?
N15 C31 N14 C15 -6.0(5) . . . . ?
O8 C31 N14 C30 5.3(7) . . . . ?
N15 C31 N14 C30 -173.7(4) . . . . ?
N2 C15 N14 C31 114.3(4) . . . . ?
C16 C15 N14 C31 2.3(5) . . . . ?
N2 C15 N14 C30 -78.1(5) . . . . ?
C16 C15 N14 C30 170.0(4) . . . . ?
N13 C30 N14 C31 -108.2(5) . . . . ?
N13 C30 N14 C15 85.5(5) . . . . ?
O8 C31 N15 C32 -1.7(7) . . . . ?
N14 C31 N15 C32 177.4(4) . . . . ?
O8 C31 N15 C16 -171.6(5) . . . . ?
N14 C31 N15 C16 7.4(5) . . . . ?
N16 C32 N15 C31 107.6(5) . . . . ?
N16 C32 N15 C16 -83.7(6) . . . . ?
N3 C16 N15 C31 -116.9(4) . . . . ?
C15 C16 N15 C31 -5.7(5) . . . . ?
N3 C16 N15 C32 73.5(6) . . . . ?
C15 C16 N15 C32 -175.3(4) . . . . ?
O9 C33 N16 C32 10.0(7) . . . . ?
N17 C33 N16 C32 -170.7(4) . . . . ?
O9 C33 N16 C17 171.5(5) . . . . ?
N17 C33 N16 C17 -9.3(5) . . . . ?
N15 C32 N16 C33 -113.0(5) . . . . ?
N15 C32 N16 C17 87.6(5) . . . . ?
N4 C17 N16 C33 117.3(4) . . . . ?
C18 C17 N16 C33 5.1(5) . . . . ?
N4 C17 N16 C32 -81.2(5) . . . . ?
C18 C17 N16 C32 166.5(4) . . . . ?
O9 C33 N17 C18 -170.9(5) . . . . ?
N16 C33 N17 C18 9.8(5) . . . . ?
O9 C33 N17 C34 -15.4(8) . . . . ?
N16 C33 N17 C34 165.4(4) . . . . ?
N5 C18 N17 C33 -117.6(4) . . . . ?
C17 C18 N17 C33 -6.4(5) . . . . ?
N5 C18 N17 C34 86.5(5) . . . . ?
C17 C18 N17 C34 -162.2(4) . . . . ?
N18 C34 N17 C33 118.4(5) . . . . ?
N18 C34 N17 C18 -88.3(5) . . . . ?
O10 C35 N18 C34 -0.5(8) . . . . ?
N19 C35 N18 C34 -177.7(4) . . . . ?
O10 C35 N18 C19 173.9(5) . . . . ?
N19 C35 N18 C19 -3.3(5) . . . . ?
N17 C34 N18 C35 -103.5(5) . . . . ?
N17 C34 N18 C19 82.9(6) . . . . ?
N6 C19 N18 C35 111.2(4) . . . . ?
C20 C19 N18 C35 -121.7(5) . . . . ?
C21 C19 N18 C35 2.4(5) . . . . ?
N6 C19 N18 C34 -74.7(6) . . . . ?
C20 C19 N18 C34 52.5(6) . . . . ?
C21 C19 N18 C34 176.6(4) . . . . ?
O10 C35 N19 C21 -174.5(5) . . . . ?
N18 C35 N19 C21 2.8(5) . . . . ?
O10 C35 N19 C36 4.9(7) . . . . ?
N18 C35 N19 C36 -177.9(4) . . . . ?
N7 C21 N19 C35 -111.4(4) . . . . ?
C22 C21 N19 C35 123.2(4) . . . . ?
C19 C21 N19 C35 -1.2(5) . . . . ?
N7 C21 N19 C36 69.3(6) . . . . ?
C22 C21 N19 C36 -56.1(6) . . . . ?
C19 C21 N19 C36 179.6(4) . . . . ?
N20 C36 N19 C35 92.4(5) . . . . ?
N20 C36 N19 C21 -88.3(5) . . . . ?
O11 C37 N20 C23 174.0(5) . . . . ?
N21 C37 N20 C23 -4.2(5) . . . . ?
O11 C37 N20 C36 5.3(8) . . . . ?
N21 C37 N20 C36 -172.9(4) . . . . ?
N8 C23 N20 C37 116.1(4) . . . . ?
C24 C23 N20 C37 3.3(5) . . . . ?
N8 C23 N20 C36 -74.8(5) . . . . ?
C24 C23 N20 C36 172.4(4) . . . . ?
N19 C36 N20 C37 -102.0(5) . . . . ?
N19 C36 N20 C23 90.4(5) . . . . ?
O11 C37 N21 C38 -4.5(8) . . . . ?
N20 C37 N21 C38 173.7(4) . . . . ?
O11 C37 N21 C24 -174.9(5) . . . . ?
N20 C37 N21 C24 3.3(5) . . . . ?
N22 C38 N21 C37 109.3(5) . . . . ?
N22 C38 N21 C24 -81.5(6) . . . . ?
N9 C24 N21 C37 -112.4(5) . . . . ?
C23 C24 N21 C37 -1.2(5) . . . . ?
N9 C24 N21 C38 77.5(6) . . . . ?
C23 C24 N21 C38 -171.4(4) . . . . ?
O12 C39 N22 C38 14.8(8) . . . . ?
N23 C39 N22 C38 -165.8(4) . . . . ?
O12 C39 N22 C25 172.0(5) . . . . ?
N23 C39 N22 C25 -8.5(6) . . . . ?
N21 C38 N22 C39 -118.6(5) . . . . ?
N21 C38 N22 C25 86.4(6) . . . . ?
N10 C25 N22 C39 116.9(4) . . . . ?
C26 C25 N22 C39 5.5(5) . . . . ?
N10 C25 N22 C38 -85.9(5) . . . . ?
C26 C25 N22 C38 162.8(4) . . . . ?
O12 C39 N23 C40 -8.0(8) . . . . ?
N22 C39 N23 C40 172.6(4) . . . . ?
O12 C39 N23 C26 -172.4(5) . . . . ?
N22 C39 N23 C26 8.1(6) . . . . ?
N24 C40 N23 C39 110.0(5) . . . . ?
N24 C40 N23 C26 -87.0(5) . . . . ?
N11 C26 N23 C39 -116.2(4) . . . . ?
C25 C26 N23 C39 -4.6(5) . . . . ?
N11 C26 N23 C40 79.0(5) . . . . ?
C25 C26 N23 C40 -169.3(4) . . . . ?
O7 C29 N24 C40 -0.5(7) . . . . ?
N13 C29 N24 C40 -177.7(4) . . . . ?
O7 C29 N24 C27 175.4(4) . . . . ?
N13 C29 N24 C27 -1.8(5) . . . . ?
N23 C40 N24 C29 -96.7(5) . . . . ?
N23 C40 N24 C27 88.0(5) . . . . ?
N12 C27 N24 C29 110.8(4) . . . . ?
C28 C27 N24 C29 -122.5(4) . . . . ?
C13 C27 N24 C29 2.2(5) . . . . ?
N12 C27 N24 C40 -73.5(5) . . . . ?
C28 C27 N24 C40 53.1(6) . . . . ?
C13 C27 N24 C40 177.9(4) . . . . ?
N1 C1 O1 La1 134.7(7) . . . . ?
N12 C1 O1 La1 -48.8(11) . . . . ?
N10 C11 O6 La1 -131.9(5) . . . . ?
N11 C11 O6 La1 49.4(9) . . . . ?
O21 N27 O19 La1 -175.9(5) . . . . ?
O20 N27 O19 La1 3.5(5) . . . . ?
O21 N27 O20 La1 176.0(5) . . . . ?
O19 N27 O20 La1 -3.4(5) . . . . ?

_refine_diff_density_max         1.272
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.103

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

data_10pp
_database_code_depnum_ccdc_archive 'CCDC 1038159'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT430_10pp                
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule. Hydrogen atoms were not identified in 
Fourier difference maps so were not added to model so as not to introduce
unecessary bias. 
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 Dy N24 O20'
_chemical_formula_weight         1449.84

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   22.4385(18)
_cell_length_b                   12.4556(10)
_cell_length_c                   14.7421(13)
_cell_angle_alpha                90
_cell_angle_beta                 114.782(2)
_cell_angle_gamma                90
_cell_volume                     3740.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9511
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      27.72

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_F_000             1458
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.178
_shelx_estimated_absorpt_T_min   0.757
_shelx_estimated_absorpt_T_max   0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10135
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.521
_diffrn_reflns_theta_max         25.246
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             3528
_reflns_number_gt                3472
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0772P)²+8.1114P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3528
_refine_ls_number_parameters     244
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
1 0.390 -0.070 0.500 932.0 283.5
2 0.500 0.278 0.000 120.3 10.9
3 0.000 0.778 0.000 120.3 10.9
_platon_squeeze_details          
; 
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 1.0000 1.0000 0.5000 0.02888(15) Uani 1 4 d S T P . .
N1 N 0.77500(16) 0.4020(3) 0.4180(2) 0.0345(7) Uani 1 1 d . . . . .
N2 N 0.81975(16) 0.4019(3) 0.5837(2) 0.0341(7) Uani 1 1 d . . . . .
N3 N 0.92277(16) 0.4026(3) 0.7335(3) 0.0353(7) Uani 1 1 d . . . . .
N4 N 1.03085(16) 0.4024(3) 0.8089(3) 0.0350(7) Uani 1 1 d . . . . .
N5 N 1.13879(16) 0.4026(3) 0.8094(3) 0.0352(7) Uani 1 1 d . . . . .
N6 N 1.20422(17) 0.4022(3) 0.7312(3) 0.0361(7) Uani 1 1 d . . . . .
O1 O 0.83798(15) 0.2568(2) 0.5014(2) 0.0442(7) Uani 1 1 d . . . . .
O2 O 0.97839(16) 0.2545(3) 0.7166(3) 0.0570(9) Uani 1 1 d . . . . .
O3 O 1.13794(19) 0.2565(3) 0.7132(3) 0.0590(9) Uani 1 1 d . . . . .
O4 O 0.9101(3) 0.9318(5) 0.3601(5) 0.0597(19) Uani 0.5 1 d . . P . .
O5 O 0.9248(3) 0.8560(5) 0.4517(5) 0.0519(16) Uani 0.5 1 d . . P . .
O6 O 0.9524(3) 0.8558(5) 0.5512(5) 0.0551(17) Uani 0.5 1 d . . P . .
O7 O 0.9887(4) 0.9316(5) 0.6413(5) 0.062(2) Uani 0.5 1 d . . P . .
C1 C 0.81423(18) 0.3459(3) 0.5014(3) 0.0337(8) Uani 1 1 d . . . . .
C2 C 0.7809(3) 0.5000 0.5603(4) 0.0301(11) Uani 1 2 d S T P . .
C3 C 0.7489(3) 0.5000 0.4412(4) 0.0299(11) Uani 1 2 d S T P . .
C4 C 0.85686(19) 0.3592(3) 0.6834(3) 0.0356(8) Uani 1 1 d . . . . .
H4A H 0.8331 0.3741 0.7238 0.043 Uiso 1 1 calc R U . . .
H4B H 0.8598 0.2818 0.6790 0.043 Uiso 1 1 calc R U . . .
C5 C 0.9775(2) 0.3444(3) 0.7490(3) 0.0361(8) Uani 1 1 d . . . . .
C6 C 1.0129(3) 0.5000 0.8448(4) 0.0298(11) Uani 1 2 d S T P . .
H6 H 1.0287 0.5000 0.9176 0.036 Uiso 1 2 calc R U P . .
C7 C 0.9373(3) 0.5000 0.7917(4) 0.0300(11) Uani 1 2 d S T P . .
H7 H 0.9174 0.5000 0.8395 0.036 Uiso 1 2 calc R U P . .
C8 C 1.09633(19) 0.3582(3) 0.8521(3) 0.0371(9) Uani 1 1 d . . . . .
H8A H 1.0936 0.2810 0.8423 0.045 Uiso 1 1 calc R U . . .
H8B H 1.1158 0.3717 0.9235 0.045 Uiso 1 1 calc R U . . .
C9 C 1.1577(2) 0.3458(3) 0.7469(3) 0.0366(9) Uani 1 1 d . . . . .
C10 C 1.2222(3) 0.5000 0.7900(4) 0.0319(11) Uani 1 2 d S T P . .
H10 H 1.2686 0.5000 0.8371 0.038 Uiso 1 2 calc R U P . .
C11 C 1.1767(3) 0.5000 0.8447(4) 0.0312(11) Uani 1 2 d S T P . .
H11 H 1.2016 0.5000 0.9175 0.037 Uiso 1 2 calc R U P . .
C12 C 0.7580(2) 0.3586(3) 0.3191(3) 0.0374(9) Uani 1 1 d . . . . .
H12A H 0.7642 0.2814 0.3244 0.045 Uiso 1 1 calc R U . . .
H12B H 0.7119 0.3723 0.2783 0.045 Uiso 1 1 calc R U . . .
C13 C 0.7326(3) 0.5000 0.6080(5) 0.0440(14) Uani 1 2 d S T P . .
H13A H 0.7558 0.5124 0.6785 0.066 Uiso 0.5 1 calc R U P . .
H13B H 0.7107 0.4318 0.5969 0.066 Uiso 0.5 1 calc R U P . .
H13C H 0.7007 0.5558 0.5788 0.066 Uiso 0.5 1 calc R U P . .
C14 C 0.6739(3) 0.5000 0.3913(5) 0.0449(14) Uani 1 2 d S T P . .
H14A H 0.6590 0.5094 0.3206 0.067 Uiso 0.5 1 calc R U P . .
H14B H 0.6577 0.5577 0.4178 0.067 Uiso 0.5 1 calc R U P . .
H14C H 0.6579 0.4329 0.4042 0.067 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.8137(2) 0.5254(15) 0.8929(2) 0.123(6) Uani 0.45 1 d . U P . .
Cl2 Cl 0.9831(8) 0.7017(6) 0.9825(13) 0.117(5) Uani 0.3 1 d . U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O4 2.357(6) . ?
Dy1 O4 2.357(6) 5_776 ?
Dy1 O4 2.357(6) 6_575 ?
Dy1 O4 2.357(6) 2_756 ?
Dy1 O5 2.358(6) 5_776 ?
Dy1 O5 2.358(6) 6_575 ?
Dy1 O5 2.358(6) 2_756 ?
Dy1 O5 2.358(6) . ?
Dy1 O7 2.360(6) 6_575 ?
Dy1 O7 2.360(6) 2_756 ?
Dy1 O7 2.360(6) 5_776 ?
Dy1 O7 2.360(6) . ?
N1 C1 1.366(5) . ?
N1 C12 1.449(5) . ?
N1 C3 1.455(4) . ?
N2 C1 1.360(5) . ?
N2 C4 1.453(5) . ?
N2 C2 1.456(4) . ?
N3 C5 1.361(5) . ?
N3 C7 1.442(4) . ?
N3 C4 1.452(5) . ?
N4 C5 1.359(5) . ?
N4 C8 1.444(5) . ?
N4 C6 1.448(4) . ?
N5 C9 1.363(5) . ?
N5 C11 1.447(4) . ?
N5 C8 1.453(5) . ?
N6 C9 1.356(5) . ?
N6 C12 1.445(5) 2_756 ?
N6 C10 1.451(4) . ?
O1 C1 1.231(5) . ?
O2 C5 1.221(5) . ?
O3 C9 1.223(5) . ?
O4 O5 1.565(10) . ?
O4 O4 1.700(13) 6_575 ?
O5 O6 1.331(10) . ?
O6 O7 1.553(10) . ?
O7 O7 1.705(13) 6_575 ?
C2 N2 1.457(4) 6_565 ?
C2 C13 1.520(8) . ?
C2 C3 1.594(7) . ?
C3 N1 1.455(4) 6_565 ?
C3 C14 1.528(7) . ?
C6 N4 1.448(4) 6_565 ?
C6 C7 1.542(7) . ?
C7 N3 1.442(4) 6_565 ?
C10 N6 1.451(4) 6_565 ?
C10 C11 1.544(8) . ?
C11 N5 1.447(4) 6_565 ?
C12 N6 1.445(5) 2_756 ?
Cl1 Cl1 0.63(4) 6_565 ?
Cl2 Cl2 0.72(3) 2_757 ?

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
O4 Dy1 O4 180.0 . 5_776 ?
O4 Dy1 O4 42.3(3) . 6_575 ?
O4 Dy1 O4 137.7(3) 5_776 6_575 ?
O4 Dy1 O4 137.7(3) . 2_756 ?
O4 Dy1 O4 42.3(3) 5_776 2_756 ?
O4 Dy1 O4 180.0 6_575 2_756 ?
O4 Dy1 O5 141.2(2) . 5_776 ?
O4 Dy1 O5 38.8(2) 5_776 5_776 ?
O4 Dy1 O5 103.4(2) 6_575 5_776 ?
O4 Dy1 O5 76.6(2) 2_756 5_776 ?
O4 Dy1 O5 76.6(2) . 6_575 ?
O4 Dy1 O5 103.4(2) 5_776 6_575 ?
O4 Dy1 O5 38.8(2) 6_575 6_575 ?
O4 Dy1 O5 141.2(2) 2_756 6_575 ?
O5 Dy1 O5 81.0(4) 5_776 6_575 ?
O4 Dy1 O5 103.4(2) . 2_756 ?
O4 Dy1 O5 76.6(2) 5_776 2_756 ?
O4 Dy1 O5 141.2(2) 6_575 2_756 ?
O4 Dy1 O5 38.8(2) 2_756 2_756 ?
O5 Dy1 O5 99.0(4) 5_776 2_756 ?
O5 Dy1 O5 180.0 6_575 2_756 ?
O4 Dy1 O5 38.8(2) . . ?
O4 Dy1 O5 141.2(2) 5_776 . ?
O4 Dy1 O5 76.6(2) 6_575 . ?
O4 Dy1 O5 103.4(2) 2_756 . ?
O5 Dy1 O5 180.0(3) 5_776 . ?
O5 Dy1 O5 99.0(4) 6_575 . ?
O5 Dy1 O5 81.0(4) 2_756 . ?
O4 Dy1 O7 122.2(3) . 6_575 ?
O4 Dy1 O7 57.8(3) 5_776 6_575 ?
O4 Dy1 O7 105.8(3) 6_575 6_575 ?
O4 Dy1 O7 74.2(3) 2_756 6_575 ?
O5 Dy1 O7 77.7(3) 5_776 6_575 ?
O5 Dy1 O7 70.4(3) 6_575 6_575 ?
O5 Dy1 O7 109.6(3) 2_756 6_575 ?
O5 Dy1 O7 102.3(3) . 6_575 ?
O4 Dy1 O7 57.8(3) . 2_756 ?
O4 Dy1 O7 122.2(3) 5_776 2_756 ?
O4 Dy1 O7 74.2(3) 6_575 2_756 ?
O4 Dy1 O7 105.8(3) 2_756 2_756 ?
O5 Dy1 O7 102.3(3) 5_776 2_756 ?
O5 Dy1 O7 109.6(3) 6_575 2_756 ?
O5 Dy1 O7 70.4(3) 2_756 2_756 ?
O5 Dy1 O7 77.7(3) . 2_756 ?
O7 Dy1 O7 180.0 6_575 2_756 ?
O4 Dy1 O7 74.2(3) . 5_776 ?
O4 Dy1 O7 105.8(3) 5_776 5_776 ?
O4 Dy1 O7 57.8(3) 6_575 5_776 ?
O4 Dy1 O7 122.2(3) 2_756 5_776 ?
O5 Dy1 O7 70.4(3) 5_776 5_776 ?
O5 Dy1 O7 77.7(3) 6_575 5_776 ?
O5 Dy1 O7 102.3(3) 2_756 5_776 ?
O5 Dy1 O7 109.7(3) . 5_776 ?
O7 Dy1 O7 137.7(3) 6_575 5_776 ?
O7 Dy1 O7 42.3(3) 2_756 5_776 ?
O4 Dy1 O7 105.8(3) . . ?
O4 Dy1 O7 74.2(3) 5_776 . ?
O4 Dy1 O7 122.2(3) 6_575 . ?
O4 Dy1 O7 57.8(3) 2_756 . ?
O5 Dy1 O7 109.6(3) 5_776 . ?
O5 Dy1 O7 102.3(3) 6_575 . ?
O5 Dy1 O7 77.7(3) 2_756 . ?
O5 Dy1 O7 70.3(3) . . ?
O7 Dy1 O7 42.3(3) 6_575 . ?
O7 Dy1 O7 137.7(3) 2_756 . ?
O7 Dy1 O7 180.0 5_776 . ?
C1 N1 C12 120.9(3) . . ?
C1 N1 C3 112.9(3) . . ?
C12 N1 C3 126.0(4) . . ?
C1 N2 C4 121.0(3) . . ?
C1 N2 C2 113.4(3) . . ?
C4 N2 C2 125.4(4) . . ?
C5 N3 C7 112.7(3) . . ?
C5 N3 C4 122.8(3) . . ?
C7 N3 C4 122.9(4) . . ?
C5 N4 C8 122.7(3) . . ?
C5 N4 C6 112.3(3) . . ?
C8 N4 C6 123.2(4) . . ?
C9 N5 C11 112.0(4) . . ?
C9 N5 C8 122.8(3) . . ?
C11 N5 C8 123.8(4) . . ?
C9 N6 C12 123.5(3) . 2_756 ?
C9 N6 C10 111.9(4) . . ?
C12 N6 C10 123.1(4) 2_756 . ?
O5 O4 O4 127.1(3) . 6_575 ?
O5 O4 Dy1 70.7(3) . . ?
O4 O4 Dy1 68.86(16) 6_575 . ?
O6 O5 O4 141.6(6) . . ?
O6 O5 Dy1 74.1(4) . . ?
O4 O5 Dy1 70.6(3) . . ?
O5 O6 O7 140.9(6) . . ?
O5 O6 Dy1 73.2(4) . . ?
O7 O6 Dy1 70.5(3) . . ?
O6 O7 O7 127.4(4) . 6_575 ?
O6 O7 Dy1 71.1(3) . . ?
O7 O7 Dy1 68.83(16) 6_575 . ?
O1 C1 N2 125.8(4) . . ?
O1 C1 N1 125.3(4) . . ?
N2 C1 N1 108.9(3) . . ?
N2 C2 N2 114.1(4) . 6_565 ?
N2 C2 C13 111.2(3) . . ?
N2 C2 C13 111.2(3) 6_565 . ?
N2 C2 C3 102.1(3) . . ?
N2 C2 C3 102.1(3) 6_565 . ?
C13 C2 C3 115.5(4) . . ?
N1 C3 N1 114.0(4) 6_565 . ?
N1 C3 C14 111.0(3) 6_565 . ?
N1 C3 C14 111.0(3) . . ?
N1 C3 C2 102.6(3) 6_565 . ?
N1 C3 C2 102.6(3) . . ?
C14 C3 C2 115.3(5) . . ?
N3 C4 N2 114.1(3) . . ?
O2 C5 N4 126.0(4) . . ?
O2 C5 N3 125.7(4) . . ?
N4 C5 N3 108.2(3) . . ?
N4 C6 N4 114.1(4) 6_565 . ?
N4 C6 C7 103.3(3) 6_565 . ?
N4 C6 C7 103.3(3) . . ?
N3 C7 N3 114.6(4) 6_565 . ?
N3 C7 C6 103.2(3) 6_565 . ?
N3 C7 C6 103.2(3) . . ?
N4 C8 N5 113.3(3) . . ?
O3 C9 N6 125.2(4) . . ?
O3 C9 N5 125.7(4) . . ?
N6 C9 N5 109.1(3) . . ?
N6 C10 N6 114.1(4) 6_565 . ?
N6 C10 C11 103.5(3) 6_565 . ?
N6 C10 C11 103.5(3) . . ?
N5 C11 N5 113.9(4) . 6_565 ?
N5 C11 C10 103.3(3) . . ?
N5 C11 C10 103.3(3) 6_565 . ?
N6 C12 N1 114.4(3) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 O4 O5 O6 -18.1(13) 6_575 . . . ?
Dy1 O4 O5 O6 23.9(10) . . . . ?
O4 O4 O5 Dy1 -41.9(3) 6_575 . . . ?
O4 O5 O6 O7 -0.7(18) . . . . ?
Dy1 O5 O6 O7 22.7(10) . . . . ?
O4 O5 O6 Dy1 -23.4(10) . . . . ?
O5 O6 O7 O7 19.1(13) . . . 6_575 ?
Dy1 O6 O7 O7 42.1(3) . . . 6_575 ?
O5 O6 O7 Dy1 -23.0(10) . . . . ?
C4 N2 C1 O1 0.9(6) . . . . ?
C2 N2 C1 O1 -174.0(4) . . . . ?
C4 N2 C1 N1 177.7(3) . . . . ?
C2 N2 C1 N1 2.8(5) . . . . ?
C12 N1 C1 O1 -0.3(6) . . . . ?
C3 N1 C1 O1 174.1(4) . . . . ?
C12 N1 C1 N2 -177.1(3) . . . . ?
C3 N1 C1 N2 -2.7(5) . . . . ?
C1 N2 C2 N2 -111.1(4) . . . 6_565 ?
C4 N2 C2 N2 74.2(6) . . . 6_565 ?
C1 N2 C2 C13 122.1(4) . . . . ?
C4 N2 C2 C13 -52.6(5) . . . . ?
C1 N2 C2 C3 -1.7(4) . . . . ?
C4 N2 C2 C3 -176.4(3) . . . . ?
C1 N1 C3 N1 111.7(4) . . . 6_565 ?
C12 N1 C3 N1 -74.2(6) . . . 6_565 ?
C1 N1 C3 C14 -122.2(4) . . . . ?
C12 N1 C3 C14 51.9(5) . . . . ?
C1 N1 C3 C2 1.5(4) . . . . ?
C12 N1 C3 C2 175.6(4) . . . . ?
N2 C2 C3 N1 -118.4(3) . . . 6_565 ?
N2 C2 C3 N1 -0.1(4) 6_565 . . 6_565 ?
C13 C2 C3 N1 120.7(3) . . . 6_565 ?
N2 C2 C3 N1 0.1(4) . . . . ?
N2 C2 C3 N1 118.4(3) 6_565 . . . ?
C13 C2 C3 N1 -120.7(3) . . . . ?
N2 C2 C3 C14 120.9(3) . . . . ?
N2 C2 C3 C14 -120.9(3) 6_565 . . . ?
C13 C2 C3 C14 0.000(1) . . . . ?
C5 N3 C4 N2 -108.0(4) . . . . ?
C7 N3 C4 N2 87.2(5) . . . . ?
C1 N2 C4 N3 99.4(4) . . . . ?
C2 N2 C4 N3 -86.3(5) . . . . ?
C8 N4 C5 O2 -7.6(7) . . . . ?
C6 N4 C5 O2 -172.4(4) . . . . ?
C8 N4 C5 N3 170.6(4) . . . . ?
C6 N4 C5 N3 5.8(5) . . . . ?
C7 N3 C5 O2 172.6(4) . . . . ?
C4 N3 C5 O2 6.4(7) . . . . ?
C7 N3 C5 N4 -5.7(5) . . . . ?
C4 N3 C5 N4 -171.9(3) . . . . ?
C5 N4 C6 N4 -115.0(4) . . . 6_565 ?
C8 N4 C6 N4 80.2(5) . . . 6_565 ?
C5 N4 C6 C7 -3.6(5) . . . . ?
C8 N4 C6 C7 -168.4(4) . . . . ?
C5 N3 C7 N3 114.7(4) . . . 6_565 ?
C4 N3 C7 N3 -79.2(6) . . . 6_565 ?
C5 N3 C7 C6 3.3(5) . . . . ?
C4 N3 C7 C6 169.4(4) . . . . ?
N4 C6 C7 N3 -0.2(4) 6_565 . . 6_565 ?
N4 C6 C7 N3 -119.4(3) . . . 6_565 ?
N4 C6 C7 N3 119.4(3) 6_565 . . . ?
N4 C6 C7 N3 0.2(4) . . . . ?
C5 N4 C8 N5 110.1(4) . . . . ?
C6 N4 C8 N5 -86.7(5) . . . . ?
C9 N5 C8 N4 -107.7(4) . . . . ?
C11 N5 C8 N4 86.6(5) . . . . ?
C12 N6 C9 O3 -7.2(7) 2_756 . . . ?
C10 N6 C9 O3 -173.6(4) . . . . ?
C12 N6 C9 N5 170.4(3) 2_756 . . . ?
C10 N6 C9 N5 3.9(5) . . . . ?
C11 N5 C9 O3 173.4(4) . . . . ?
C8 N5 C9 O3 6.2(7) . . . . ?
C11 N5 C9 N6 -4.1(5) . . . . ?
C8 N5 C9 N6 -171.3(3) . . . . ?
C9 N6 C10 N6 -113.9(4) . . . 6_565 ?
C12 N6 C10 N6 79.6(5) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.2(4) . . . . ?
C12 N6 C10 C11 -168.7(4) 2_756 . . . ?
C9 N5 C11 N5 113.8(4) . . . 6_565 ?
C8 N5 C11 N5 -79.1(5) . . . 6_565 ?
C9 N5 C11 C10 2.5(4) . . . . ?
C8 N5 C11 C10 169.6(3) . . . . ?
N6 C10 C11 N5 119.1(3) 6_565 . . . ?
N6 C10 C11 N5 -0.2(4) . . . . ?
N6 C10 C11 N5 0.2(4) 6_565 . . 6_565 ?
N6 C10 C11 N5 -119.1(3) . . . 6_565 ?
C1 N1 C12 N6 -100.8(4) . . . 2_756 ?
C3 N1 C12 N6 85.6(5) . . . 2_756 ?

_refine_diff_density_max         1.030
_refine_diff_density_min         -3.408
_refine_diff_density_rms         0.116

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

data_11pp
_database_code_depnum_ccdc_archive 'CCDC 1038160'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT075_11pp                
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_11pp                
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;
_vrf_PLAT306_11pp                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_11pp                
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

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 -0.021 0.000 897 300 ' '
_platon_squeeze_details          
;
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 Ho N24 O22'
_chemical_formula_weight         1484.27

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.434(5)
_cell_length_b                   12.421(3)
_cell_length_c                   14.859(3)
_cell_angle_alpha                90
_cell_angle_beta                 115.105(7)
_cell_angle_gamma                90
_cell_volume                     3749.4(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9939
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      27.53

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_F_000             1492
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.238
_shelx_estimated_absorpt_T_min   0.731
_shelx_estimated_absorpt_T_max   0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10122
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.513
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3537
_reflns_number_gt                3515
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0988P)²+6.2300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3537
_refine_ls_number_parameters     246
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1310
_refine_ls_wR_factor_gt          0.1306
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.137
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.9397(5) 0.5000 0.4992(9) 0.135(4) Uani 1 2 d S T P . .
Cl2 Cl 1.0000 0.3037(6) 1.0000 0.173(5) Uani 0.5 2 d S TU P . .
Ho1 Ho 1.0000 1.0000 0.5000 0.02742(16) Uani 1 4 d S T P . .
N1 N 0.77487(17) 0.4020(3) 0.4168(2) 0.0334(7) Uani 1 1 d . . . . .
N2 N 0.82082(16) 0.4015(3) 0.5817(2) 0.0334(7) Uani 1 1 d . . . . .
N3 N 0.92335(16) 0.4028(3) 0.7307(3) 0.0351(7) Uani 1 1 d . . . . .
N4 N 1.03192(16) 0.4022(3) 0.8075(3) 0.0340(7) Uani 1 1 d . . . . .
N5 N 1.13974(17) 0.4019(3) 0.8082(3) 0.0348(7) Uani 1 1 d . . . . .
N6 N 1.20514(17) 0.4023(3) 0.7311(3) 0.0351(7) Uani 1 1 d . . . . .
O1 O 0.83734(16) 0.2569(2) 0.4994(2) 0.0450(7) Uani 1 1 d . . . . .
O2 O 0.97982(18) 0.2549(3) 0.7144(3) 0.0593(10) Uani 1 1 d . . . . .
O3 O 1.1387(2) 0.2561(3) 0.7135(3) 0.0589(9) Uani 1 1 d . . . . .
O4 O 0.9091(3) 0.9307(5) 0.3647(6) 0.0573(18) Uani 0.5 1 d . . P A 1
O6 O 0.9537(4) 0.8562(6) 0.5517(5) 0.0520(16) Uani 0.5 1 d . . P B 1
O5 O 0.9246(3) 0.8572(6) 0.4509(5) 0.0525(16) Uani 0.5 1 d . . P A 2
O7 O 0.9899(4) 0.9331(5) 0.6403(5) 0.0572(19) Uani 0.5 1 d . . P A 2
C1 C 0.81414(18) 0.3453(3) 0.4995(3) 0.0322(8) Uani 1 1 d . . . . .
C2 C 0.7813(3) 0.5000 0.5578(4) 0.0283(10) Uani 1 2 d S T P . .
C3 C 0.7485(3) 0.5000 0.4401(4) 0.0292(11) Uani 1 2 d S T P . .
C4 C 0.8576(2) 0.3588(3) 0.6803(3) 0.0358(8) Uani 1 1 d . . . . .
H4A H 0.8608 0.2813 0.6757 0.043 Uiso 1 1 calc R U . . .
H4B H 0.8336 0.3734 0.7200 0.043 Uiso 1 1 calc R U . . .
C5 C 0.9785(2) 0.3451(3) 0.7468(3) 0.0364(8) Uani 1 1 d . . . . .
C6 C 1.0137(3) 0.5000 0.8426(4) 0.0294(11) Uani 1 2 d S T P . .
H6 H 1.0292 0.5000 0.9150 0.035 Uiso 1 2 calc R U P . .
C7 C 0.9379(3) 0.5000 0.7884(4) 0.0305(11) Uani 1 2 d S T P . .
H7 H 0.9177 0.5000 0.8353 0.037 Uiso 1 2 calc R U P . .
C8 C 1.09770(19) 0.3583(3) 0.8506(3) 0.0357(8) Uani 1 1 d . . . . .
H8A H 1.0951 0.2809 0.8416 0.043 Uiso 1 1 calc R U . . .
H8B H 1.1175 0.3726 0.9214 0.043 Uiso 1 1 calc R U . . .
C9 C 1.1588(2) 0.3455(3) 0.7473(3) 0.0360(8) Uani 1 1 d . . . . .
C10 C 1.2230(3) 0.5000 0.7897(4) 0.0313(11) Uani 1 2 d S T P . .
H10 H 1.2696 0.5000 0.8368 0.038 Uiso 1 2 calc R U P . .
C11 C 1.1779(3) 0.5000 0.8432(4) 0.0302(11) Uani 1 2 d S T P . .
H11 H 1.2030 0.5000 0.9156 0.036 Uiso 1 2 calc R U P . .
C12 C 0.7572(2) 0.3584(3) 0.3186(3) 0.0366(9) Uani 1 1 d . . . . .
H12A H 0.7633 0.2810 0.3239 0.044 Uiso 1 1 calc R U . . .
H12B H 0.7109 0.3722 0.2782 0.044 Uiso 1 1 calc R U . . .
C13 C 0.7330(3) 0.5000 0.6059(5) 0.0438(14) Uani 1 2 d S T P . .
H13A H 0.6998 0.4464 0.5746 0.066 Uiso 0.5 1 calc R U P . .
H13B H 0.7127 0.5695 0.5977 0.066 Uiso 0.5 1 calc R U P . .
H13C H 0.7563 0.4841 0.6754 0.066 Uiso 0.5 1 calc R U P . .
C14 C 0.6737(3) 0.5000 0.3920(5) 0.0446(14) Uani 1 2 d S T P . .
H14A H 0.6579 0.5507 0.4256 0.067 Uiso 0.5 1 calc R U P . .
H14B H 0.6579 0.4293 0.3967 0.067 Uiso 0.5 1 calc R U P . .
H14C H 0.6580 0.5199 0.3233 0.067 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.8173(2) 0.530(2) 0.8916(3) 0.192(10) Uani 0.5 1 d . U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O4 2.337(7) . ?
Ho1 O4 2.337(7) 5_776 ?
Ho1 O4 2.337(7) 6_575 ?
Ho1 O4 2.337(7) 2_756 ?
Ho1 O7 2.343(6) . ?
Ho1 O7 2.343(6) 6_575 ?
Ho1 O7 2.343(6) 2_756 ?
Ho1 O7 2.343(6) 5_776 ?
Ho1 O5 2.344(6) . ?
Ho1 O5 2.344(6) 5_776 ?
Ho1 O5 2.344(6) 6_575 ?
Ho1 O5 2.344(6) 2_756 ?
N1 C1 1.366(5) . ?
N1 C12 1.445(5) . ?
N1 C3 1.458(4) . ?
N2 C1 1.359(5) . ?
N2 C4 1.443(5) . ?
N2 C2 1.463(4) . ?
N3 C5 1.360(5) . ?
N3 C7 1.436(4) . ?
N3 C4 1.447(5) . ?
N4 C5 1.355(5) . ?
N4 C8 1.443(5) . ?
N4 C6 1.448(4) . ?
N5 C9 1.348(5) . ?
N5 C8 1.443(5) . ?
N5 C11 1.453(4) . ?
N6 C9 1.359(5) . ?
N6 C12 1.445(5) 2_756 ?
N6 C10 1.447(4) . ?
O1 C1 1.216(5) . ?
O2 C5 1.224(5) . ?
O3 C9 1.223(5) . ?
O4 O4 1.722(13) 6_575 ?
O7 O7 1.662(12) 6_575 ?
C2 N2 1.463(4) 6_565 ?
C2 C13 1.529(8) . ?
C2 C3 1.584(7) . ?
C3 N1 1.458(4) 6_565 ?
C3 C14 1.519(8) . ?
C6 N4 1.448(4) 6_565 ?
C6 C7 1.543(7) . ?
C7 N3 1.436(4) 6_565 ?
C10 N6 1.447(4) 6_565 ?
C10 C11 1.531(8) . ?
C11 N5 1.453(4) 6_565 ?
C12 N6 1.445(5) 2_756 ?
Cl1 Cl1 0.75(5) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ho1 O4 180.0 . 5_776 ?
O4 Ho1 O4 43.2(3) . 6_575 ?
O4 Ho1 O4 136.8(3) 5_776 6_575 ?
O4 Ho1 O4 136.8(3) . 2_756 ?
O4 Ho1 O4 43.2(3) 5_776 2_756 ?
O4 Ho1 O4 180.0 6_575 2_756 ?
O7 Ho1 O7 41.5(3) . 6_575 ?
O7 Ho1 O7 138.5(3) . 2_756 ?
O7 Ho1 O7 180.0 6_575 2_756 ?
O7 Ho1 O7 180.0 . 5_776 ?
O7 Ho1 O7 138.5(3) 6_575 5_776 ?
O7 Ho1 O7 41.5(3) 2_756 5_776 ?
O7 Ho1 O5 71.3(3) . . ?
O7 Ho1 O5 102.5(3) 6_575 . ?
O7 Ho1 O5 77.5(3) 2_756 . ?
O7 Ho1 O5 108.7(3) 5_776 . ?
O7 Ho1 O5 108.7(3) . 5_776 ?
O7 Ho1 O5 77.5(3) 6_575 5_776 ?
O7 Ho1 O5 102.5(3) 2_756 5_776 ?
O7 Ho1 O5 71.3(3) 5_776 5_776 ?
O5 Ho1 O5 180.0 . 5_776 ?
O7 Ho1 O5 102.5(3) . 6_575 ?
O7 Ho1 O5 71.3(3) 6_575 6_575 ?
O7 Ho1 O5 108.7(3) 2_756 6_575 ?
O7 Ho1 O5 77.5(3) 5_776 6_575 ?
O5 Ho1 O5 98.4(4) . 6_575 ?
O5 Ho1 O5 81.6(4) 5_776 6_575 ?
O7 Ho1 O5 77.5(3) . 2_756 ?
O7 Ho1 O5 108.7(3) 6_575 2_756 ?
O7 Ho1 O5 71.3(3) 2_756 2_756 ?
O7 Ho1 O5 102.5(3) 5_776 2_756 ?
O5 Ho1 O5 81.6(4) . 2_756 ?
O5 Ho1 O5 98.4(4) 5_776 2_756 ?
O5 Ho1 O5 180.0 6_575 2_756 ?
C1 N1 C12 120.7(3) . . ?
C1 N1 C3 112.9(3) . . ?
C12 N1 C3 126.0(4) . . ?
C1 N2 C4 121.3(3) . . ?
C1 N2 C2 112.8(3) . . ?
C4 N2 C2 125.5(4) . . ?
C5 N3 C7 112.3(4) . . ?
C5 N3 C4 122.9(3) . . ?
C7 N3 C4 123.3(4) . . ?
C5 N4 C8 123.1(3) . . ?
C5 N4 C6 112.0(4) . . ?
C8 N4 C6 123.2(4) . . ?
C9 N5 C8 123.4(3) . . ?
C9 N5 C11 111.7(4) . . ?
C8 N5 C11 123.5(4) . . ?
C9 N6 C12 123.5(3) . 2_756 ?
C9 N6 C10 111.5(4) . . ?
C12 N6 C10 123.4(4) 2_756 . ?
O4 O4 Ho1 68.39(16) 6_575 . ?
O7 O7 Ho1 69.23(15) 6_575 . ?
O1 C1 N2 125.6(4) . . ?
O1 C1 N1 125.3(4) . . ?
N2 C1 N1 109.1(3) . . ?
N2 C2 N2 113.4(4) . 6_565 ?
N2 C2 C13 111.3(3) . . ?
N2 C2 C13 111.3(3) 6_565 . ?
N2 C2 C3 102.6(3) . . ?
N2 C2 C3 102.6(3) 6_565 . ?
C13 C2 C3 115.3(5) . . ?
N1 C3 N1 113.2(4) 6_565 . ?
N1 C3 C14 111.5(3) 6_565 . ?
N1 C3 C14 111.5(3) . . ?
N1 C3 C2 102.5(3) 6_565 . ?
N1 C3 C2 102.5(3) . . ?
C14 C3 C2 114.9(5) . . ?
N2 C4 N3 113.9(3) . . ?
O2 C5 N4 125.4(4) . . ?
O2 C5 N3 125.8(4) . . ?
N4 C5 N3 108.8(3) . . ?
N4 C6 N4 114.1(4) . 6_565 ?
N4 C6 C7 103.2(3) . . ?
N4 C6 C7 103.2(3) 6_565 . ?
N3 C7 N3 114.5(4) . 6_565 ?
N3 C7 C6 103.5(3) . . ?
N3 C7 C6 103.5(3) 6_565 . ?
N4 C8 N5 113.5(3) . . ?
O3 C9 N5 125.5(4) . . ?
O3 C9 N6 125.0(4) . . ?
N5 C9 N6 109.5(3) . . ?
N6 C10 N6 114.0(4) 6_565 . ?
N6 C10 C11 103.7(3) 6_565 . ?
N6 C10 C11 103.7(3) . . ?
N5 C11 N5 114.1(4) . 6_565 ?
N5 C11 C10 103.5(3) . . ?
N5 C11 C10 103.5(3) 6_565 . ?
N6 C12 N1 114.0(3) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N2 C1 O1 -0.2(6) . . . . ?
C2 N2 C1 O1 -173.6(4) . . . . ?
C4 N2 C1 N1 177.4(3) . . . . ?
C2 N2 C1 N1 3.9(5) . . . . ?
C12 N1 C1 O1 0.2(6) . . . . ?
C3 N1 C1 O1 173.5(4) . . . . ?
C12 N1 C1 N2 -177.3(3) . . . . ?
C3 N1 C1 N2 -4.0(5) . . . . ?
C1 N2 C2 N2 -112.1(4) . . . 6_565 ?
C4 N2 C2 N2 74.7(6) . . . 6_565 ?
C1 N2 C2 C13 121.5(4) . . . . ?
C4 N2 C2 C13 -51.6(5) . . . . ?
C1 N2 C2 C3 -2.3(4) . . . . ?
C4 N2 C2 C3 -175.4(4) . . . . ?
C1 N1 C3 N1 112.1(4) . . . 6_565 ?
C12 N1 C3 N1 -74.9(6) . . . 6_565 ?
C1 N1 C3 C14 -121.1(4) . . . . ?
C12 N1 C3 C14 51.9(5) . . . . ?
C1 N1 C3 C2 2.4(4) . . . . ?
C12 N1 C3 C2 175.4(4) . . . . ?
N2 C2 C3 N1 -117.7(3) . . . 6_565 ?
N2 C2 C3 N1 0.1(4) 6_565 . . 6_565 ?
C13 C2 C3 N1 121.2(3) . . . 6_565 ?
N2 C2 C3 N1 -0.1(4) . . . . ?
N2 C2 C3 N1 117.7(3) 6_565 . . . ?
C13 C2 C3 N1 -121.2(3) . . . . ?
N2 C2 C3 C14 121.1(3) . . . . ?
N2 C2 C3 C14 -121.1(3) 6_565 . . . ?
C13 C2 C3 C14 0.000(1) . . . . ?
C1 N2 C4 N3 100.9(4) . . . . ?
C2 N2 C4 N3 -86.5(5) . . . . ?
C5 N3 C4 N2 -108.1(4) . . . . ?
C7 N3 C4 N2 87.1(5) . . . . ?
C8 N4 C5 O2 -6.9(7) . . . . ?
C6 N4 C5 O2 -172.8(4) . . . . ?
C8 N4 C5 N3 171.1(3) . . . . ?
C6 N4 C5 N3 5.2(5) . . . . ?
C7 N3 C5 O2 173.0(4) . . . . ?
C4 N3 C5 O2 6.7(7) . . . . ?
C7 N3 C5 N4 -5.0(5) . . . . ?
C4 N3 C5 N4 -171.3(4) . . . . ?
C5 N4 C6 N4 -114.6(4) . . . 6_565 ?
C8 N4 C6 N4 79.6(5) . . . 6_565 ?
C5 N4 C6 C7 -3.3(4) . . . . ?
C8 N4 C6 C7 -169.2(4) . . . . ?
C5 N3 C7 N3 114.6(4) . . . 6_565 ?
C4 N3 C7 N3 -79.2(6) . . . 6_565 ?
C5 N3 C7 C6 2.7(5) . . . . ?
C4 N3 C7 C6 169.0(4) . . . . ?
N4 C6 C7 N3 0.3(4) . . . . ?
N4 C6 C7 N3 119.4(3) 6_565 . . . ?
N4 C6 C7 N3 -119.4(3) . . . 6_565 ?
N4 C6 C7 N3 -0.3(4) 6_565 . . 6_565 ?
C5 N4 C8 N5 108.6(4) . . . . ?
C6 N4 C8 N5 -87.1(5) . . . . ?
C9 N5 C8 N4 -107.8(4) . . . . ?
C11 N5 C8 N4 86.8(5) . . . . ?
C8 N5 C9 O3 7.0(7) . . . . ?
C11 N5 C9 O3 174.0(4) . . . . ?
C8 N5 C9 N6 -171.5(3) . . . . ?
C11 N5 C9 N6 -4.5(5) . . . . ?
C12 N6 C9 O3 -7.9(7) 2_756 . . . ?
C10 N6 C9 O3 -174.0(4) . . . . ?
C12 N6 C9 N5 170.6(4) 2_756 . . . ?
C10 N6 C9 N5 4.5(5) . . . . ?
C9 N6 C10 N6 -114.6(4) . . . 6_565 ?
C12 N6 C10 N6 79.3(6) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.6(5) . . . . ?
C12 N6 C10 C11 -168.7(4) 2_756 . . . ?
C9 N5 C11 N5 114.4(4) . . . 6_565 ?
C8 N5 C11 N5 -78.7(5) . . . 6_565 ?
C9 N5 C11 C10 2.7(5) . . . . ?
C8 N5 C11 C10 169.6(4) . . . . ?
N6 C10 C11 N5 119.3(3) 6_565 . . . ?
N6 C10 C11 N5 0.0(4) . . . . ?
N6 C10 C11 N5 0.0(4) 6_565 . . 6_565 ?
N6 C10 C11 N5 -119.3(3) . . . 6_565 ?
C1 N1 C12 N6 -101.3(4) . . . 2_756 ?
C3 N1 C12 N6 86.3(5) . . . 2_756 ?

_refine_diff_density_max         2.323
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.132

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

data_12pp
_database_code_depnum_ccdc_archive 'CCDC 1038161'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

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
1 -0.004 -0.153 0.000 1118.7 401.4
2 1.000 0.063 0.500 26.4 8.6
3 0.500 0.563 0.500 26.4 8.6
_platon_squeeze_details          
; 
;




_vrf_CHEMW01_12pp                
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

_vrf_PLAT075_12pp                
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_PLAT306_12pp                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_12pp                
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
	C40 H44 N24 O12, Er O8, 3(Cl), 6(O)
;
_chemical_formula_sum            'C40 H44 Cl3 Er N24 O26'
_chemical_formula_weight         1544.55

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.429(3)
_cell_length_b                   12.4151(15)
_cell_length_c                   14.8727(18)
_cell_angle_alpha                90
_cell_angle_beta                 115.035(4)
_cell_angle_gamma                90
_cell_volume                     3752.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9403
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      26.18

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_F_000             1546
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.308
_shelx_estimated_absorpt_T_min   0.719
_shelx_estimated_absorpt_T_max   0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10090
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.511
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3559
_reflns_number_gt                3520
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1575P)²+15.5937P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3559
_refine_ls_number_parameters     249
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.2199
_refine_ls_wR_factor_gt          0.2190
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_restrained_S_all      1.228
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 1.0000 0.3042(14) 0.0000 0.107(4) Uiso 1 2 d S . P . .
O2WB O 0.8297(9) 0.9549(15) 0.2012(14) 0.090(5) Uiso 0.5 1 d . . P A 2
O2WA O 1.0042(9) 0.9561(15) 0.8066(13) 0.090(5) Uiso 0.5 1 d . . P B 1
Er1 Er 1.0000 0.0000 0.5000 0.0270(3) Uani 1 4 d S T P . .
N1 N 0.7753(3) 0.4012(5) 0.4174(4) 0.0333(12) Uani 1 1 d . . . . .
N2 N 0.8210(3) 0.4017(4) 0.5819(4) 0.0320(12) Uani 1 1 d . . . . .
N3 N 0.9233(3) 0.4026(5) 0.7306(4) 0.0345(12) Uani 1 1 d . . . . .
N4 N 1.0319(3) 0.4023(5) 0.8070(4) 0.0339(12) Uani 1 1 d . . . . .
N5 N 0.8603(3) 0.4020(5) 0.1915(4) 0.0340(12) Uani 1 1 d . . . . .
N6 N 0.7946(3) 0.4022(5) 0.2684(4) 0.0339(12) Uani 1 1 d . . . . .
O1 O 0.8374(3) 0.2563(4) 0.4991(4) 0.0447(12) Uani 1 1 d . . . . .
O2 O 0.9798(3) 0.2542(5) 0.7141(5) 0.0590(16) Uani 1 1 d . . . . .
O3 O 0.8616(4) 0.2552(5) 0.2863(5) 0.0578(16) Uani 1 1 d . . . . .
O4 O 0.9101(6) -0.0691(9) 0.3642(9) 0.055(3) Uani 0.5 1 d . . P C 1
O6 O 0.9550(6) -0.1440(10) 0.5535(9) 0.051(3) Uani 0.5 1 d . . P D 1
O5 O 0.9254(6) -0.1433(9) 0.4500(9) 0.050(3) Uani 0.5 1 d . . P C 2
O7 O 0.9909(8) -0.0672(9) 0.6403(9) 0.059(3) Uani 0.5 1 d . . P C 2
C1 C 0.8144(3) 0.3453(5) 0.4987(5) 0.0317(13) Uani 1 1 d . . . . .
C2 C 0.7813(4) 0.5000 0.5582(7) 0.0284(18) Uani 1 2 d S T P . .
C3 C 0.7485(4) 0.5000 0.4404(7) 0.0291(18) Uani 1 2 d S T P . .
C4 C 0.8577(3) 0.3585(6) 0.6797(5) 0.0357(14) Uani 1 1 d . . . . .
H4A H 0.8610 0.2810 0.6746 0.043 Uiso 1 1 calc R U . . .
H4B H 0.8335 0.3723 0.7193 0.043 Uiso 1 1 calc R U . . .
C5 C 0.9789(4) 0.3448(6) 0.7475(5) 0.0356(14) Uani 1 1 d . . . . .
C6 C 1.0134(5) 0.5000 0.8424(6) 0.0298(18) Uani 1 2 d S T P . .
H6 H 1.0290 0.5000 0.9147 0.036 Uiso 1 2 calc R U P . .
C7 C 0.9380(5) 0.5000 0.7890(7) 0.0316(19) Uani 1 2 d S T P . .
H7 H 0.9178 0.5000 0.8359 0.038 Uiso 1 2 calc R U P . .
C8 C 0.9022(3) 0.3583(6) 0.1490(5) 0.0352(14) Uani 1 1 d . . . . .
H8A H 0.8827 0.3730 0.0783 0.042 Uiso 1 1 calc R U . . .
H8B H 0.9046 0.2808 0.1577 0.042 Uiso 1 1 calc R U . . .
C9 C 0.8412(4) 0.3450(6) 0.2524(5) 0.0353(15) Uani 1 1 d . . . . .
C10 C 0.7769(4) 0.5000 0.2104(7) 0.0303(19) Uani 1 2 d S T P . .
H10 H 0.7304 0.5000 0.1634 0.036 Uiso 1 2 calc R U P . .
C11 C 0.8221(4) 0.5000 0.1569(6) 0.0298(19) Uani 1 2 d S T P . .
H11 H 0.7969 0.5000 0.0847 0.036 Uiso 1 2 calc R U P . .
C12 C 0.7578(4) 0.3581(6) 0.3193(5) 0.0354(15) Uani 1 1 d . . . . .
H12A H 0.7642 0.2807 0.3245 0.042 Uiso 1 1 calc R U . . .
H12B H 0.7114 0.3714 0.2793 0.042 Uiso 1 1 calc R U . . .
C13 C 0.7337(5) 0.5000 0.6061(8) 0.041(2) Uani 1 2 d S T P . .
H13A H 0.7084 0.5653 0.5892 0.061 Uiso 0.25 1 calc R U P . .
H13B H 0.7046 0.4393 0.5825 0.061 Uiso 0.25 1 calc R U P . .
H13C H 0.7578 0.4954 0.6768 0.061 Uiso 0.5 2 calc R U P . .
C14 C 0.6731(5) 0.5000 0.3912(8) 0.043(2) Uani 1 2 d S T P . .
H14A H 0.6571 0.5655 0.4076 0.064 Uiso 0.25 1 calc R U P . .
H14B H 0.6578 0.4950 0.3206 0.064 Uiso 0.5 2 calc R U P . .
H14C H 0.6571 0.4395 0.4148 0.064 Uiso 0.25 1 calc R U P . .
Cl1 Cl 0.8181(4) 0.5338(18) 0.8933(5) 0.144(9) Uani 0.5 1 d . U P . .
Cl2 Cl 0.9411(14) 0.5000 0.496(2) 0.207(10) Uani 0.5 2 d S TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2WB O2WB 1.12(4) 6_575 ?
O2WA O2WA 1.09(4) 6_575 ?
Er1 O4 2.332(11) . ?
Er1 O4 2.332(11) 5_756 ?
Er1 O4 2.332(11) 6 ?
Er1 O4 2.332(11) 2_756 ?
Er1 O7 2.335(11) 6 ?
Er1 O7 2.335(11) 2_756 ?
Er1 O7 2.335(11) 5_756 ?
Er1 O7 2.335(11) . ?
Er1 O5 2.337(10) 5_756 ?
Er1 O5 2.337(10) 6 ?
Er1 O5 2.337(10) 2_756 ?
Er1 O5 2.337(10) . ?
N1 C1 1.347(9) . ?
N1 C12 1.444(9) . ?
N1 C3 1.469(7) . ?
N2 C1 1.373(9) . ?
N2 C4 1.438(9) . ?
N2 C2 1.463(7) . ?
N3 C5 1.366(9) . ?
N3 C7 1.443(8) . ?
N3 C4 1.448(9) . ?
N4 C5 1.348(9) . ?
N4 C8 1.448(8) 2_756 ?
N4 C6 1.450(8) . ?
N5 C9 1.354(9) . ?
N5 C8 1.443(9) . ?
N5 C11 1.450(7) . ?
N6 C9 1.364(9) . ?
N6 C12 1.444(9) . ?
N6 C10 1.444(7) . ?
O1 C1 1.219(9) . ?
O2 C5 1.232(9) . ?
O3 C9 1.230(9) . ?
O4 O4 1.72(2) 6 ?
O7 O7 1.67(2) 6 ?
C2 N2 1.463(7) 6_565 ?
C2 C13 1.514(13) . ?
C2 C3 1.587(13) . ?
C3 N1 1.469(7) 6_565 ?
C3 C14 1.532(13) . ?
C6 N4 1.450(8) 6_565 ?
C6 C7 1.533(13) . ?
C7 N3 1.443(8) 6_565 ?
C8 N4 1.447(8) 2_756 ?
C10 N6 1.444(7) 6_565 ?
C10 C11 1.531(13) . ?
C11 N5 1.450(7) 6_565 ?
Cl1 Cl1 0.84(4) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Er1 O4 180.0 . 5_756 ?
O4 Er1 O4 43.2(6) . 6 ?
O4 Er1 O4 136.8(6) 5_756 6 ?
O4 Er1 O4 136.8(6) . 2_756 ?
O4 Er1 O4 43.2(6) 5_756 2_756 ?
O4 Er1 O4 180.0(6) 6 2_756 ?
O7 Er1 O7 180.0 6 2_756 ?
O7 Er1 O7 138.1(6) 6 5_756 ?
O7 Er1 O7 41.9(6) 2_756 5_756 ?
O7 Er1 O7 41.9(6) 6 . ?
O7 Er1 O7 138.1(6) 2_756 . ?
O7 Er1 O7 180.0 5_756 . ?
O7 Er1 O5 76.4(4) 6 5_756 ?
O7 Er1 O5 103.6(4) 2_756 5_756 ?
O7 Er1 O5 72.0(5) 5_756 5_756 ?
O7 Er1 O5 108.0(5) . 5_756 ?
O7 Er1 O5 72.0(5) 6 6 ?
O7 Er1 O5 108.0(5) 2_756 6 ?
O7 Er1 O5 76.4(4) 5_756 6 ?
O7 Er1 O5 103.6(4) . 6 ?
O5 Er1 O5 80.9(6) 5_756 6 ?
O7 Er1 O5 108.0(5) 6 2_756 ?
O7 Er1 O5 72.0(5) 2_756 2_756 ?
O7 Er1 O5 103.6(4) 5_756 2_756 ?
O7 Er1 O5 76.4(4) . 2_756 ?
O5 Er1 O5 99.1(6) 5_756 2_756 ?
O5 Er1 O5 180.0 6 2_756 ?
O7 Er1 O5 103.6(4) 6 . ?
O7 Er1 O5 76.4(4) 2_756 . ?
O7 Er1 O5 108.0(5) 5_756 . ?
O7 Er1 O5 72.0(5) . . ?
O5 Er1 O5 180.0 5_756 . ?
O5 Er1 O5 99.1(6) 6 . ?
O5 Er1 O5 80.9(6) 2_756 . ?
C1 N1 C12 120.8(6) . . ?
C1 N1 C3 113.4(6) . . ?
C12 N1 C3 125.5(6) . . ?
C1 N2 C4 121.2(6) . . ?
C1 N2 C2 112.7(6) . . ?
C4 N2 C2 125.7(6) . . ?
C5 N3 C7 111.8(6) . . ?
C5 N3 C4 123.0(6) . . ?
C7 N3 C4 123.7(6) . . ?
C5 N4 C8 123.0(6) . 2_756 ?
C5 N4 C6 112.0(6) . . ?
C8 N4 C6 123.1(6) 2_756 . ?
C9 N5 C8 123.1(6) . . ?
C9 N5 C11 111.7(6) . . ?
C8 N5 C11 123.8(6) . . ?
C9 N6 C12 122.9(6) . . ?
C9 N6 C10 111.8(6) . . ?
C12 N6 C10 123.9(6) . . ?
O4 O4 Er1 68.4(3) 6 . ?
O7 O7 Er1 69.1(3) 6 . ?
O1 C1 N1 125.8(7) . . ?
O1 C1 N2 125.0(7) . . ?
N1 C1 N2 109.1(6) . . ?
N2 C2 N2 113.1(7) . 6_565 ?
N2 C2 C13 111.4(5) . . ?
N2 C2 C13 111.4(5) 6_565 . ?
N2 C2 C3 102.5(5) . . ?
N2 C2 C3 102.5(5) 6_565 . ?
C13 C2 C3 115.4(8) . . ?
N1 C3 N1 113.3(7) . 6_565 ?
N1 C3 C14 111.5(5) . . ?
N1 C3 C14 111.5(5) 6_565 . ?
N1 C3 C2 102.3(5) . . ?
N1 C3 C2 102.3(5) 6_565 . ?
C14 C3 C2 115.4(8) . . ?
N2 C4 N3 114.1(6) . . ?
O2 C5 N4 126.0(7) . . ?
O2 C5 N3 125.0(7) . . ?
N4 C5 N3 108.9(6) . . ?
N4 C6 N4 113.4(8) . 6_565 ?
N4 C6 C7 103.5(5) . . ?
N4 C6 C7 103.5(5) 6_565 . ?
N3 C7 N3 113.9(8) . 6_565 ?
N3 C7 C6 103.5(5) . . ?
N3 C7 C6 103.5(5) 6_565 . ?
N5 C8 N4 113.0(5) . 2_756 ?
O3 C9 N5 125.4(7) . . ?
O3 C9 N6 125.5(7) . . ?
N5 C9 N6 109.0(6) . . ?
N6 C10 N6 114.4(8) . 6_565 ?
N6 C10 C11 103.6(5) . . ?
N6 C10 C11 103.6(5) 6_565 . ?
N5 C11 N5 114.0(7) . 6_565 ?
N5 C11 C10 103.7(5) . . ?
N5 C11 C10 103.7(5) 6_565 . ?
N6 C12 N1 114.8(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 O1 -1.2(11) . . . . ?
C3 N1 C1 O1 172.8(7) . . . . ?
C12 N1 C1 N2 -177.5(6) . . . . ?
C3 N1 C1 N2 -3.5(8) . . . . ?
C4 N2 C1 O1 0.7(10) . . . . ?
C2 N2 C1 O1 -172.8(7) . . . . ?
C4 N2 C1 N1 177.0(6) . . . . ?
C2 N2 C1 N1 3.5(8) . . . . ?
C1 N2 C2 N2 -111.7(7) . . . 6_565 ?
C4 N2 C2 N2 75.2(10) . . . 6_565 ?
C1 N2 C2 C13 121.9(7) . . . . ?
C4 N2 C2 C13 -51.2(9) . . . . ?
C1 N2 C2 C3 -2.1(7) . . . . ?
C4 N2 C2 C3 -175.2(6) . . . . ?
C1 N1 C3 N1 111.3(7) . . . 6_565 ?
C12 N1 C3 N1 -75.0(10) . . . 6_565 ?
C1 N1 C3 C14 -121.8(8) . . . . ?
C12 N1 C3 C14 51.8(9) . . . . ?
C1 N1 C3 C2 2.1(8) . . . . ?
C12 N1 C3 C2 175.7(6) . . . . ?
N2 C2 C3 N1 0.1(7) . . . . ?
N2 C2 C3 N1 117.4(6) 6_565 . . . ?
C13 C2 C3 N1 -121.3(4) . . . . ?
N2 C2 C3 N1 -117.4(6) . . . 6_565 ?
N2 C2 C3 N1 -0.1(7) 6_565 . . 6_565 ?
C13 C2 C3 N1 121.2(4) . . . 6_565 ?
N2 C2 C3 C14 121.3(4) . . . . ?
N2 C2 C3 C14 -121.3(4) 6_565 . . . ?
C13 C2 C3 C14 0.000(2) . . . . ?
C1 N2 C4 N3 101.1(8) . . . . ?
C2 N2 C4 N3 -86.4(8) . . . . ?
C5 N3 C4 N2 -108.8(8) . . . . ?
C7 N3 C4 N2 86.8(8) . . . . ?
C8 N4 C5 O2 -8.5(12) 2_756 . . . ?
C6 N4 C5 O2 -173.1(8) . . . . ?
C8 N4 C5 N3 170.7(6) 2_756 . . . ?
C6 N4 C5 N3 6.2(8) . . . . ?
C7 N3 C5 O2 173.2(8) . . . . ?
C4 N3 C5 O2 7.2(12) . . . . ?
C7 N3 C5 N4 -6.1(8) . . . . ?
C4 N3 C5 N4 -172.1(6) . . . . ?
C5 N4 C6 N4 -115.3(7) . . . 6_565 ?
C8 N4 C6 N4 80.1(9) 2_756 . . 6_565 ?
C5 N4 C6 C7 -3.9(8) . . . . ?
C8 N4 C6 C7 -168.4(6) 2_756 . . . ?
C5 N3 C7 N3 115.1(7) . . . 6_565 ?
C4 N3 C7 N3 -79.0(10) . . . 6_565 ?
C5 N3 C7 C6 3.4(8) . . . . ?
C4 N3 C7 C6 169.4(6) . . . . ?
N4 C6 C7 N3 0.2(7) . . . . ?
N4 C6 C7 N3 118.8(6) 6_565 . . . ?
N4 C6 C7 N3 -118.8(6) . . . 6_565 ?
N4 C6 C7 N3 -0.2(7) 6_565 . . 6_565 ?
C9 N5 C8 N4 -107.6(8) . . . 2_756 ?
C11 N5 C8 N4 87.2(8) . . . 2_756 ?
C8 N5 C9 O3 7.5(11) . . . . ?
C11 N5 C9 O3 174.2(7) . . . . ?
C8 N5 C9 N6 -171.3(6) . . . . ?
C11 N5 C9 N6 -4.5(8) . . . . ?
C12 N6 C9 O3 -7.2(11) . . . . ?
C10 N6 C9 O3 -174.4(7) . . . . ?
C12 N6 C9 N5 171.5(6) . . . . ?
C10 N6 C9 N5 4.4(8) . . . . ?
C9 N6 C10 N6 -114.6(7) . . . 6_565 ?
C12 N6 C10 N6 78.5(10) . . . 6_565 ?
C9 N6 C10 C11 -2.5(8) . . . . ?
C12 N6 C10 C11 -169.5(6) . . . . ?
C9 N5 C11 N5 114.9(7) . . . 6_565 ?
C8 N5 C11 N5 -78.5(9) . . . 6_565 ?
C9 N5 C11 C10 2.8(8) . . . . ?
C8 N5 C11 C10 169.5(6) . . . . ?
N6 C10 C11 N5 -0.2(7) . . . . ?
N6 C10 C11 N5 119.6(6) 6_565 . . . ?
N6 C10 C11 N5 -119.6(6) . . . 6_565 ?
N6 C10 C11 N5 0.2(7) 6_565 . . 6_565 ?
C9 N6 C12 N1 108.4(8) . . . . ?
C10 N6 C12 N1 -86.0(8) . . . . ?
C1 N1 C12 N6 -101.2(8) . . . . ?
C3 N1 C12 N6 85.6(8) . . . . ?

_refine_diff_density_max         2.561
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.256

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

data_13pp
_database_code_depnum_ccdc_archive 'CCDC 1038162'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;



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
1 -0.004 -0.172 0.000 1100.6 394.6
2 0.000 0.182 0.500 120.3 17.1
3 0.500 0.682 0.500 120.3 17.1
_platon_squeeze_details          
;
;



_vrf_PLAT075_13pp                
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_13pp                
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

_vrf_PLAT430_13pp                
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
	C40 H44 N24 O12, O8 Tm, 3(Cl)

;
_chemical_formula_sum            'C40 H44 Cl3 N24 O20 Tm'
_chemical_formula_weight         1450.22

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.438(3)
_cell_length_b                   12.3991(18)
_cell_length_c                   14.869(2)
_cell_angle_alpha                90
_cell_angle_beta                 115.027(2)
_cell_angle_gamma                90
_cell_volume                     3748.4(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8161
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.02

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             1452
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.363
_shelx_estimated_absorpt_T_min   0.710
_shelx_estimated_absorpt_T_max   0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10004
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.511
_diffrn_reflns_theta_max         25.242
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             3511
_reflns_number_gt                3483
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc

_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1756P)²+8.4590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3511
_refine_ls_number_parameters     238
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.2275
_refine_ls_wR_factor_gt          0.2265
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_restrained_S_all      1.232
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 1.0000 1.0000 0.5000 0.0264(3) Uani 1 4 d S T P . .
N1 N 0.7757(3) 0.4016(5) 0.4174(4) 0.0328(12) Uani 1 1 d . . . . .
N2 N 0.8213(3) 0.4020(5) 0.5814(4) 0.0325(12) Uani 1 1 d . . . . .
N3 N 0.9235(3) 0.4026(5) 0.7304(5) 0.0342(13) Uani 1 1 d . . . . .
N4 N 1.0314(3) 0.4021(5) 0.8075(4) 0.0331(12) Uani 1 1 d . . . . .
N5 N 1.1398(3) 0.4017(5) 0.8090(4) 0.0337(12) Uani 1 1 d . . . . .
N6 N 1.2053(3) 0.4019(5) 0.7317(5) 0.0345(13) Uani 1 1 d . . . . .
O1 O 0.8377(3) 0.2558(4) 0.4990(4) 0.0441(13) Uani 1 1 d . . . . .
O2 O 0.9797(3) 0.2537(5) 0.7152(5) 0.0576(17) Uani 1 1 d . . . . .
O3 O 1.1378(4) 0.2555(5) 0.7134(5) 0.0558(16) Uani 1 1 d . . . . .
O4 O 0.9098(6) 0.9307(9) 0.3649(9) 0.054(3) Uani 0.5 1 d . . P A 1
O6 O 0.9554(6) 0.8561(10) 0.5531(9) 0.048(3) Uani 0.5 1 d . . P B 1
O5 O 0.9257(6) 0.8573(10) 0.4511(9) 0.050(3) Uani 0.5 1 d . . P A 2
O7 O 0.9894(8) 0.9325(9) 0.6380(10) 0.057(3) Uani 0.5 1 d . . P A 2
C1 C 0.8142(3) 0.3456(6) 0.4985(5) 0.0306(14) Uani 1 1 d . . . . .
C2 C 0.7808(5) 0.5000 0.5576(7) 0.0285(19) Uani 1 2 d S T P . .
C3 C 0.7492(5) 0.5000 0.4410(7) 0.0286(19) Uani 1 2 d S T P . .
C4 C 0.8576(4) 0.3587(6) 0.6793(5) 0.0352(15) Uani 1 1 d . . . . .
H4A H 0.8607 0.2811 0.6744 0.042 Uiso 1 1 calc R U . . .
H4B H 0.8333 0.3730 0.7188 0.042 Uiso 1 1 calc R U . . .
C5 C 0.9789(4) 0.3443(6) 0.7475(5) 0.0350(15) Uani 1 1 d . . . . .
C6 C 1.0131(5) 0.5000 0.8421(6) 0.0284(19) Uani 1 2 d S T P . .
H6 H 1.0283 0.5000 0.9144 0.034 Uiso 1 2 calc R U P . .
C7 C 0.9382(5) 0.5000 0.7883(7) 0.031(2) Uani 1 2 d S T P . .
H7 H 0.9179 0.5000 0.8351 0.037 Uiso 1 2 calc R U P . .
C8 C 1.0981(3) 0.3585(6) 0.8514(5) 0.0344(15) Uani 1 1 d . . . . .
H8A H 1.1177 0.3735 0.9220 0.041 Uiso 1 1 calc R U . . .
H8B H 1.0959 0.2808 0.8431 0.041 Uiso 1 1 calc R U . . .
C9 C 1.1585(4) 0.3446(6) 0.7475(5) 0.0344(15) Uani 1 1 d . . . . .
C10 C 1.2230(5) 0.5000 0.7901(7) 0.0301(19) Uani 1 2 d S T P . .
H10 H 1.2695 0.5000 0.8372 0.036 Uiso 1 2 calc R U P . .
C11 C 1.1778(5) 0.5000 0.8437(6) 0.0288(19) Uani 1 2 d S T P . .
H11 H 1.2029 0.5000 0.9160 0.035 Uiso 1 2 calc R U P . .
C12 C 0.7581(4) 0.3584(6) 0.3190(5) 0.0357(15) Uani 1 1 d . . . . .
H12A H 0.7644 0.2808 0.3241 0.043 Uiso 1 1 calc R U . . .
H12B H 0.7117 0.3718 0.2790 0.043 Uiso 1 1 calc R U . . .
C13 C 0.7333(6) 0.5000 0.6052(9) 0.042(2) Uani 1 2 d S T P . .
H13A H 0.7078 0.5652 0.5879 0.063 Uiso 0.5 1 calc R U P . .
H13B H 0.7044 0.4390 0.5819 0.063 Uiso 0.5 1 calc R U P . .
H13C H 0.7573 0.4958 0.6760 0.063 Uiso 1 2 calc R U P . .
C14 C 0.6734(5) 0.5000 0.3906(8) 0.042(2) Uani 1 2 d S T P . .
H14A H 0.6573 0.5652 0.4072 0.063 Uiso 0.5 1 calc R U P . .
H14B H 0.6585 0.4958 0.3199 0.063 Uiso 1 2 calc R U P . .
H14C H 0.6572 0.4390 0.4133 0.063 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.8179(4) 0.5329(18) 0.8930(5) 0.140(9) Uani 0.5 1 d . U P . .
Cl2 Cl 1.0000 0.3024(11) 1.0000 0.191(11) Uani 0.5 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O7 2.320(11) 6_575 ?
Tm1 O7 2.320(11) 2_756 ?
Tm1 O7 2.320(11) 5_776 ?
Tm1 O7 2.320(11) . ?
Tm1 O5 2.326(11) 5_776 ?
Tm1 O5 2.326(11) 6_575 ?
Tm1 O5 2.326(11) 2_756 ?
Tm1 O5 2.326(11) . ?
Tm1 O4 2.331(11) . ?
Tm1 O4 2.331(11) 5_776 ?
Tm1 O4 2.331(11) 2_756 ?
Tm1 O4 2.331(11) 6_575 ?
N1 C1 1.342(10) . ?
N1 C12 1.447(9) . ?
N1 C3 1.464(8) . ?
N2 C1 1.367(9) . ?
N2 C4 1.438(9) . ?
N2 C2 1.468(8) . ?
N3 C5 1.366(10) . ?
N3 C7 1.437(8) . ?
N3 C4 1.453(9) . ?
N4 C5 1.345(10) . ?
N4 C6 1.445(7) . ?
N4 C8 1.460(9) . ?
N5 C9 1.356(10) . ?
N5 C8 1.434(9) . ?
N5 C11 1.452(8) . ?
N6 C9 1.368(10) . ?
N6 C12 1.434(9) 2_756 ?
N6 C10 1.449(8) . ?
O1 C1 1.231(9) . ?
O2 C5 1.225(9) . ?
O3 C9 1.222(9) . ?
O4 O4 1.72(2) 6_575 ?
O7 O7 1.67(2) 6_575 ?
C2 N2 1.468(8) 6_565 ?
C2 C13 1.508(14) . ?
C2 C3 1.572(13) . ?
C3 N1 1.464(8) 6_565 ?
C3 C14 1.541(13) . ?
C6 N4 1.445(7) 6_565 ?
C6 C7 1.526(13) . ?
C7 N3 1.437(8) 6_565 ?
C10 N6 1.449(8) 6_565 ?
C10 C11 1.533(13) . ?
C11 N5 1.451(8) 6_565 ?
C12 N6 1.434(9) 2_756 ?
Cl1 Cl1 0.81(5) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Tm1 O7 180.0 6_575 2_756 ?
O7 Tm1 O7 137.7(6) 6_575 5_776 ?
O7 Tm1 O7 42.3(6) 2_756 5_776 ?
O7 Tm1 O7 42.3(6) 6_575 . ?
O7 Tm1 O7 137.7(6) 2_756 . ?
O7 Tm1 O7 180.0 5_776 . ?
O7 Tm1 O5 77.1(5) 6_575 5_776 ?
O7 Tm1 O5 102.9(5) 2_756 5_776 ?
O7 Tm1 O5 71.0(5) 5_776 5_776 ?
O7 Tm1 O5 109.0(5) . 5_776 ?
O7 Tm1 O5 71.0(5) 6_575 6_575 ?
O7 Tm1 O5 109.0(5) 2_756 6_575 ?
O7 Tm1 O5 77.1(5) 5_776 6_575 ?
O7 Tm1 O5 102.9(5) . 6_575 ?
O5 Tm1 O5 81.0(7) 5_776 6_575 ?
O7 Tm1 O5 109.0(5) 6_575 2_756 ?
O7 Tm1 O5 71.0(5) 2_756 2_756 ?
O7 Tm1 O5 102.9(5) 5_776 2_756 ?
O7 Tm1 O5 77.1(5) . 2_756 ?
O5 Tm1 O5 99.0(7) 5_776 2_756 ?
O5 Tm1 O5 180.0 6_575 2_756 ?
O7 Tm1 O5 102.9(5) 6_575 . ?
O7 Tm1 O5 77.1(5) 2_756 . ?
O7 Tm1 O5 109.0(5) 5_776 . ?
O7 Tm1 O5 71.0(5) . . ?
O5 Tm1 O5 180.0(5) 5_776 . ?
O5 Tm1 O5 99.0(7) 6_575 . ?
O5 Tm1 O5 81.0(7) 2_756 . ?
O4 Tm1 O4 180.0 . 5_776 ?
O4 Tm1 O4 136.7(6) . 2_756 ?
O4 Tm1 O4 43.3(6) 5_776 2_756 ?
O4 Tm1 O4 43.3(6) . 6_575 ?
O4 Tm1 O4 136.7(6) 5_776 6_575 ?
O4 Tm1 O4 180.0 2_756 6_575 ?
C1 N1 C12 120.9(6) . . ?
C1 N1 C3 112.8(6) . . ?
C12 N1 C3 125.9(6) . . ?
C1 N2 C4 121.5(6) . . ?
C1 N2 C2 112.5(6) . . ?
C4 N2 C2 125.4(6) . . ?
C5 N3 C7 111.9(7) . . ?
C5 N3 C4 122.9(6) . . ?
C7 N3 C4 123.6(7) . . ?
C5 N4 C6 112.5(6) . . ?
C5 N4 C8 123.0(6) . . ?
C6 N4 C8 122.9(6) . . ?
C9 N5 C8 123.2(6) . . ?
C9 N5 C11 112.0(6) . . ?
C8 N5 C11 123.5(6) . . ?
C9 N6 C12 123.1(6) . 2_756 ?
C9 N6 C10 111.6(6) . . ?
C12 N6 C10 123.9(7) 2_756 . ?
O4 O4 Tm1 68.4(3) 6_575 . ?
O7 O7 Tm1 68.8(3) 6_575 . ?
O1 C1 N1 125.8(7) . . ?
O1 C1 N2 124.9(7) . . ?
N1 C1 N2 109.3(6) . . ?
N2 C2 N2 111.7(8) . 6_565 ?
N2 C2 C13 112.1(5) . . ?
N2 C2 C13 112.1(5) 6_565 . ?
N2 C2 C3 102.1(5) . . ?
N2 C2 C3 102.1(5) 6_565 . ?
C13 C2 C3 116.1(8) . . ?
N1 C3 N1 112.9(8) . 6_565 ?
N1 C3 C14 111.1(5) . . ?
N1 C3 C14 111.1(5) 6_565 . ?
N1 C3 C2 103.0(5) . . ?
N1 C3 C2 103.1(5) 6_565 . ?
C14 C3 C2 115.2(8) . . ?
N2 C4 N3 113.9(6) . . ?
O2 C5 N4 126.5(7) . . ?
O2 C5 N3 125.2(7) . . ?
N4 C5 N3 108.3(6) . . ?
N4 C6 N4 114.4(7) 6_565 . ?
N4 C6 C7 103.2(5) 6_565 . ?
N4 C6 C7 103.2(5) . . ?
N3 C7 N3 114.3(8) 6_565 . ?
N3 C7 C6 103.7(5) 6_565 . ?
N3 C7 C6 103.7(5) . . ?
N5 C8 N4 113.7(6) . . ?
O3 C9 N5 125.4(7) . . ?
O3 C9 N6 125.6(7) . . ?
N5 C9 N6 109.0(6) . . ?
N6 C10 N6 114.2(8) . 6_565 ?
N6 C10 C11 103.7(5) . . ?
N6 C10 C11 103.7(5) 6_565 . ?
N5 C11 N5 114.2(8) 6_565 . ?
N5 C11 C10 103.5(5) 6_565 . ?
N5 C11 C10 103.5(5) . . ?
N6 C12 N1 114.8(6) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 O1 -0.2(11) . . . . ?
C3 N1 C1 O1 173.2(7) . . . . ?
C12 N1 C1 N2 -177.7(6) . . . . ?
C3 N1 C1 N2 -4.3(8) . . . . ?
C4 N2 C1 O1 -0.6(11) . . . . ?
C2 N2 C1 O1 -172.4(7) . . . . ?
C4 N2 C1 N1 176.9(6) . . . . ?
C2 N2 C1 N1 5.1(8) . . . . ?
C1 N2 C2 N2 -112.1(7) . . . 6_565 ?
C4 N2 C2 N2 76.5(10) . . . 6_565 ?
C1 N2 C2 C13 121.2(8) . . . . ?
C4 N2 C2 C13 -50.2(10) . . . . ?
C1 N2 C2 C3 -3.6(8) . . . . ?
C4 N2 C2 C3 -175.1(6) . . . . ?
C1 N1 C3 N1 112.4(7) . . . 6_565 ?
C12 N1 C3 N1 -74.6(10) . . . 6_565 ?
C1 N1 C3 C14 -122.0(8) . . . . ?
C12 N1 C3 C14 51.0(10) . . . . ?
C1 N1 C3 C2 1.9(8) . . . . ?
C12 N1 C3 C2 174.9(6) . . . . ?
N2 C2 C3 N1 1.0(7) . . . . ?
N2 C2 C3 N1 116.6(6) 6_565 . . . ?
C13 C2 C3 N1 -121.2(5) . . . . ?
N2 C2 C3 N1 -116.6(6) . . . 6_565 ?
N2 C2 C3 N1 -1.0(7) 6_565 . . 6_565 ?
C13 C2 C3 N1 121.2(5) . . . 6_565 ?
N2 C2 C3 C14 122.2(5) . . . . ?
N2 C2 C3 C14 -122.2(5) 6_565 . . . ?
C13 C2 C3 C14 0.000(2) . . . . ?
C1 N2 C4 N3 101.5(8) . . . . ?
C2 N2 C4 N3 -87.7(8) . . . . ?
C5 N3 C4 N2 -108.7(8) . . . . ?
C7 N3 C4 N2 86.8(8) . . . . ?
C6 N4 C5 O2 -172.5(8) . . . . ?
C8 N4 C5 O2 -6.4(12) . . . . ?
C6 N4 C5 N3 5.6(8) . . . . ?
C8 N4 C5 N3 171.8(6) . . . . ?
C7 N3 C5 O2 172.7(8) . . . . ?
C4 N3 C5 O2 6.5(12) . . . . ?
C7 N3 C5 N4 -5.5(8) . . . . ?
C4 N3 C5 N4 -171.7(6) . . . . ?
C5 N4 C6 N4 -114.9(7) . . . 6_565 ?
C8 N4 C6 N4 79.0(9) . . . 6_565 ?
C5 N4 C6 C7 -3.5(8) . . . . ?
C8 N4 C6 C7 -169.6(6) . . . . ?
C5 N3 C7 N3 115.4(8) . . . 6_565 ?
C4 N3 C7 N3 -78.5(10) . . . 6_565 ?
C5 N3 C7 C6 3.2(8) . . . . ?
C4 N3 C7 C6 169.3(6) . . . . ?
N4 C6 C7 N3 -0.1(7) 6_565 . . 6_565 ?
N4 C6 C7 N3 -119.5(6) . . . 6_565 ?
N4 C6 C7 N3 119.5(6) 6_565 . . . ?
N4 C6 C7 N3 0.1(7) . . . . ?
C9 N5 C8 N4 -107.0(8) . . . . ?
C11 N5 C8 N4 87.3(8) . . . . ?
C5 N4 C8 N5 108.2(8) . . . . ?
C6 N4 C8 N5 -87.1(8) . . . . ?
C8 N5 C9 O3 7.5(12) . . . . ?
C11 N5 C9 O3 174.6(8) . . . . ?
C8 N5 C9 N6 -171.2(6) . . . . ?
C11 N5 C9 N6 -4.1(8) . . . . ?
C12 N6 C9 O3 -7.3(12) 2_756 . . . ?
C10 N6 C9 O3 -174.7(8) . . . . ?
C12 N6 C9 N5 171.4(6) 2_756 . . . ?
C10 N6 C9 N5 4.0(8) . . . . ?
C9 N6 C10 N6 -114.5(7) . . . 6_565 ?
C12 N6 C10 N6 78.2(10) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.3(8) . . . . ?
C12 N6 C10 C11 -169.6(6) 2_756 . . . ?
C9 N5 C11 N5 114.3(7) . . . 6_565 ?
C8 N5 C11 N5 -78.6(9) . . . 6_565 ?
C9 N5 C11 C10 2.5(8) . . . . ?
C8 N5 C11 C10 169.6(6) . . . . ?
N6 C10 C11 N5 -119.5(6) . . . 6_565 ?
N6 C10 C11 N5 0.1(7) 6_565 . . 6_565 ?
N6 C10 C11 N5 -0.1(7) . . . . ?
N6 C10 C11 N5 119.5(6) 6_565 . . . ?
C1 N1 C12 N6 -101.7(8) . . . 2_756 ?
C3 N1 C12 N6 85.9(9) . . . 2_756 ?

_refine_diff_density_max         3.683
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.294

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

data_14pp
_database_code_depnum_ccdc_archive 'CCDC 1038163'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
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
1 0.500 0.056 0.000 117.2 15.4
2 1.021 0.007 0.500 1112.9 392.9
3 0.000 0.556 0.000 117.2 15.4
_platon_squeeze_details          
;
;


_vrf_PLAT075_14pp                
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_14pp                
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

_vrf_PLAT430_14pp                
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 N24 O20 Yb'
_chemical_formula_weight         1464.41

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.429(10)
_cell_length_b                   12.394(6)
_cell_length_c                   14.895(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.018(4)
_cell_angle_gamma                90
_cell_volume                     3752(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8487
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      26.03

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             1466
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.425
_shelx_estimated_absorpt_T_min   0.700
_shelx_estimated_absorpt_T_max   0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9992
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.933
_diffrn_reflns_theta_max         25.245
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3528
_reflns_number_gt                3501
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1698P)²+9.9148P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3528
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0725
_refine_ls_wR_factor_ref         0.2262
_refine_ls_wR_factor_gt          0.2252
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_restrained_S_all      1.248
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 1.0000 1.0000 0.5000 0.0266(3) Uani 1 4 d S T P . .
N1 N 0.7755(3) 0.4013(5) 0.4168(5) 0.0331(13) Uani 1 1 d . . . . .
N2 N 0.8213(3) 0.4014(5) 0.5808(5) 0.0333(13) Uani 1 1 d . . . . .
N3 N 0.9234(3) 0.4024(5) 0.7298(5) 0.0337(13) Uani 1 1 d . . . . .
N4 N 1.0314(3) 0.4021(5) 0.8072(5) 0.0336(13) Uani 1 1 d . . . . .
N5 N 1.1402(3) 0.4015(5) 0.8091(5) 0.0338(13) Uani 1 1 d . . . . .
N6 N 1.2054(3) 0.4017(5) 0.7320(5) 0.0345(13) Uani 1 1 d . . . . .
O1 O 0.8377(3) 0.2558(4) 0.4988(4) 0.0436(13) Uani 1 1 d . . . . .
O2 O 0.9798(3) 0.2536(5) 0.7148(5) 0.0569(17) Uani 1 1 d . . . . .
O3 O 1.1381(4) 0.2553(5) 0.7139(5) 0.0566(16) Uani 1 1 d . . . . .
O4 O 0.9098(6) 0.9310(9) 0.3653(9) 0.053(3) Uani 0.5 1 d . . P A 1
O6 O 0.9553(6) 0.8563(10) 0.5530(9) 0.049(3) Uani 0.5 1 d . . P B 1
O5 O 0.9258(6) 0.8580(10) 0.4505(9) 0.048(3) Uani 0.5 1 d . . P A 2
O7 O 0.9902(8) 0.9336(9) 0.6379(10) 0.058(4) Uani 0.5 1 d . . P A 2
C1 C 0.8144(3) 0.3449(6) 0.4986(5) 0.0312(14) Uani 1 1 d . . . . .
C2 C 0.7810(5) 0.5000 0.5569(7) 0.0281(19) Uani 1 2 d S T P . .
C3 C 0.7489(5) 0.5000 0.4401(7) 0.0289(19) Uani 1 2 d S T P . .
C4 C 0.8575(4) 0.3584(6) 0.6789(5) 0.0350(15) Uani 1 1 d . . . . .
H4A H 0.8606 0.2807 0.6743 0.042 Uiso 1 1 calc R U . . .
H4B H 0.8332 0.3731 0.7181 0.042 Uiso 1 1 calc R U . . .
C5 C 0.9790(4) 0.3442(6) 0.7476(5) 0.0353(15) Uani 1 1 d . . . . .
C6 C 1.0131(5) 0.5000 0.8419(7) 0.030(2) Uani 1 2 d S T P . .
H6 H 1.0283 0.5000 0.9140 0.036 Uiso 1 2 calc R U P . .
C7 C 0.9386(5) 0.5000 0.7882(7) 0.031(2) Uani 1 2 d S T P . .
H7 H 0.9182 0.5000 0.8349 0.037 Uiso 1 2 calc R U P . .
C8 C 1.0980(3) 0.3583(6) 0.8514(5) 0.0341(15) Uani 1 1 d . . . . .
H8A H 1.1175 0.3733 0.9219 0.041 Uiso 1 1 calc R U . . .
H8B H 1.0957 0.2805 0.8432 0.041 Uiso 1 1 calc R U . . .
C9 C 1.1586(4) 0.3439(6) 0.7477(5) 0.0353(15) Uani 1 1 d . . . . .
C10 C 1.2228(5) 0.5000 0.7901(7) 0.030(2) Uani 1 2 d S T P . .
H10 H 1.2693 0.5000 0.8371 0.036 Uiso 1 2 calc R U P . .
C11 C 1.1780(5) 0.5000 0.8437(7) 0.0289(19) Uani 1 2 d S T P . .
H11 H 1.2033 0.5000 0.9159 0.035 Uiso 1 2 calc R U P . .
C12 C 0.7577(4) 0.3582(6) 0.3185(5) 0.0357(15) Uani 1 1 d . . . . .
H12A H 0.7637 0.2806 0.3235 0.043 Uiso 1 1 calc R U . . .
H12B H 0.7113 0.3721 0.2788 0.043 Uiso 1 1 calc R U . . .
C13 C 0.7334(6) 0.5000 0.6051(9) 0.041(2) Uani 1 2 d S T P . .
H13A H 0.7080 0.4347 0.5880 0.062 Uiso 0.5 1 calc R U P . .
H13B H 0.7576 0.5043 0.6757 0.062 Uiso 1 2 calc R U P . .
H13C H 0.7045 0.5610 0.5819 0.062 Uiso 0.5 1 calc R U P . .
C14 C 0.6732(5) 0.5000 0.3901(9) 0.042(3) Uani 1 2 d S T P . .
H14A H 0.6572 0.5654 0.4066 0.064 Uiso 0.5 1 calc R U P . .
H14B H 0.6583 0.4955 0.3196 0.064 Uiso 1 2 calc R U P . .
H14C H 0.6571 0.4391 0.4130 0.064 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.8183(4) 0.527(5) 0.8926(5) 0.184(19) Uani 0.5 1 d . . P . .
Cl2 Cl 1.0000 0.3033(15) 1.0000 0.132(5) Uiso 0.5 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O7 2.308(11) . ?
Yb1 O7 2.308(11) 6_575 ?
Yb1 O7 2.308(11) 2_756 ?
Yb1 O7 2.308(11) 5_776 ?
Yb1 O5 2.318(11) 5_776 ?
Yb1 O5 2.318(11) 6_575 ?
Yb1 O5 2.318(11) 2_756 ?
Yb1 O5 2.318(11) . ?
Yb1 O4 2.328(11) . ?
Yb1 O4 2.328(11) 5_776 ?
Yb1 O4 2.328(11) 2_756 ?
Yb1 O4 2.328(11) 6_575 ?
N1 C1 1.355(10) . ?
N1 C12 1.446(9) . ?
N1 C3 1.466(8) . ?
N2 C1 1.361(10) . ?
N2 C4 1.440(9) . ?
N2 C2 1.472(8) . ?
N3 C5 1.364(10) . ?
N3 C7 1.444(8) . ?
N3 C4 1.452(9) . ?
N4 C5 1.343(10) . ?
N4 C6 1.445(8) . ?
N4 C8 1.458(9) . ?
N5 C9 1.355(10) . ?
N5 C8 1.444(9) . ?
N5 C11 1.452(8) . ?
N6 C9 1.369(10) . ?
N6 C12 1.439(9) 2_756 ?
N6 C10 1.450(8) . ?
O1 C1 1.221(9) . ?
O2 C5 1.228(10) . ?
O3 C9 1.214(10) . ?
O4 O4 1.71(2) 6_575 ?
O7 O7 1.65(2) 6_575 ?
C2 N2 1.472(8) 6_565 ?
C2 C13 1.517(14) . ?
C2 C3 1.577(14) . ?
C3 N1 1.467(8) 6_565 ?
C3 C14 1.538(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 N4 1.445(8) 6_565 ?
C6 C7 1.517(14) . ?
C6 H6 0.9800 . ?
C7 N3 1.444(8) 6_565 ?
C7 H7 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 N6 1.450(8) 6_565 ?
C10 C11 1.525(14) . ?
C10 H10 0.9800 . ?
C11 N5 1.452(8) 6_565 ?
C11 H11 0.9800 . ?
C12 N6 1.439(9) 2_756 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
Cl1 Cl1 0.67(11) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Yb1 O7 41.8(6) . 6_575 ?
O7 Yb1 O7 138.2(6) . 2_756 ?
O7 Yb1 O7 180.0 6_575 2_756 ?
O7 Yb1 O7 180.0 . 5_776 ?
O7 Yb1 O7 138.2(6) 6_575 5_776 ?
O7 Yb1 O7 41.8(6) 2_756 5_776 ?
O7 Yb1 O5 108.3(5) . 5_776 ?
O7 Yb1 O5 76.8(5) 6_575 5_776 ?
O7 Yb1 O5 103.2(5) 2_756 5_776 ?
O7 Yb1 O5 71.7(5) 5_776 5_776 ?
O7 Yb1 O5 103.2(5) . 6_575 ?
O7 Yb1 O5 71.7(5) 6_575 6_575 ?
O7 Yb1 O5 108.3(5) 2_756 6_575 ?
O7 Yb1 O5 76.8(5) 5_776 6_575 ?
O5 Yb1 O5 81.2(7) 5_776 6_575 ?
O7 Yb1 O5 76.8(5) . 2_756 ?
O7 Yb1 O5 108.3(5) 6_575 2_756 ?
O7 Yb1 O5 71.7(5) 2_756 2_756 ?
O7 Yb1 O5 103.2(5) 5_776 2_756 ?
O5 Yb1 O5 98.8(7) 5_776 2_756 ?
O5 Yb1 O5 180.0 6_575 2_756 ?
O7 Yb1 O5 71.7(5) . . ?
O7 Yb1 O5 103.2(5) 6_575 . ?
O7 Yb1 O5 76.8(5) 2_756 . ?
O7 Yb1 O5 108.3(5) 5_776 . ?
O5 Yb1 O5 180.0 5_776 . ?
O5 Yb1 O5 98.8(7) 6_575 . ?
O5 Yb1 O5 81.2(7) 2_756 . ?
O4 Yb1 O4 180.0 . 5_776 ?
O4 Yb1 O4 136.9(6) . 2_756 ?
O4 Yb1 O4 43.1(6) 5_776 2_756 ?
O4 Yb1 O4 43.1(6) . 6_575 ?
O4 Yb1 O4 136.9(6) 5_776 6_575 ?
O4 Yb1 O4 180.0 2_756 6_575 ?
C1 N1 C12 121.1(6) . . ?
C1 N1 C3 112.9(6) . . ?
C12 N1 C3 125.6(7) . . ?
C1 N2 C4 121.5(6) . . ?
C1 N2 C2 112.7(6) . . ?
C4 N2 C2 125.2(7) . . ?
C5 N3 C7 111.3(7) . . ?
C5 N3 C4 123.2(6) . . ?
C7 N3 C4 123.9(7) . . ?
C5 N4 C6 112.5(6) . . ?
C5 N4 C8 122.9(6) . . ?
C6 N4 C8 122.9(7) . . ?
C9 N5 C8 122.9(6) . . ?
C9 N5 C11 112.5(6) . . ?
C8 N5 C11 123.4(6) . . ?
C9 N6 C12 123.1(6) . 2_756 ?
C9 N6 C10 111.7(6) . . ?
C12 N6 C10 123.9(7) 2_756 . ?
O4 O4 Yb1 68.4(3) 6_575 . ?
O7 O7 Yb1 69.1(3) 6_575 . ?
O1 C1 N1 125.5(7) . . ?
O1 C1 N2 125.3(7) . . ?
N1 C1 N2 109.2(6) . . ?
N2 C2 N2 112.3(8) 6_565 . ?
N2 C2 C13 111.7(5) 6_565 . ?
N2 C2 C13 111.7(5) . . ?
N2 C2 C3 102.3(5) 6_565 . ?
N2 C2 C3 102.3(5) . . ?
C13 C2 C3 115.9(8) . . ?
N1 C3 N1 113.1(8) . 6_565 ?
N1 C3 C14 111.2(5) . . ?
N1 C3 C14 111.2(5) 6_565 . ?
N1 C3 C2 102.7(5) . . ?
N1 C3 C2 102.7(5) 6_565 . ?
C14 C3 C2 115.4(8) . . ?
N2 C4 N3 113.8(6) . . ?
N2 C4 H4A 108.8 . . ?
N3 C4 H4A 108.8 . . ?
N2 C4 H4B 108.8 . . ?
N3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
O2 C5 N4 126.5(7) . . ?
O2 C5 N3 124.9(7) . . ?
N4 C5 N3 108.6(6) . . ?
N4 C6 N4 114.3(8) 6_565 . ?
N4 C6 C7 103.2(5) 6_565 . ?
N4 C6 C7 103.2(5) . . ?
N4 C6 H6 111.8 6_565 . ?
N4 C6 H6 111.8 . . ?
C7 C6 H6 111.8 . . ?
N3 C7 N3 113.8(8) . 6_565 ?
N3 C7 C6 104.1(5) . . ?
N3 C7 C6 104.1(5) 6_565 . ?
N3 C7 H7 111.5 . . ?
N3 C7 H7 111.5 6_565 . ?
C6 C7 H7 111.5 . . ?
N5 C8 N4 113.6(6) . . ?
N5 C8 H8A 108.8 . . ?
N4 C8 H8A 108.8 . . ?
N5 C8 H8B 108.8 . . ?
N4 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O3 C9 N5 125.8(7) . . ?
O3 C9 N6 125.9(7) . . ?
N5 C9 N6 108.4(6) . . ?
N6 C10 N6 114.5(8) 6_565 . ?
N6 C10 C11 104.0(5) 6_565 . ?
N6 C10 C11 104.0(5) . . ?
N6 C10 H10 111.3 6_565 . ?
N6 C10 H10 111.3 . . ?
C11 C10 H10 111.3 . . ?
N5 C11 N5 114.6(8) 6_565 . ?
N5 C11 C10 103.3(5) 6_565 . ?
N5 C11 C10 103.3(5) . . ?
N5 C11 H11 111.7 6_565 . ?
N5 C11 H11 111.7 . . ?
C10 C11 H11 111.7 . . ?
N6 C12 N1 114.6(6) 2_756 . ?
N6 C12 H12A 108.6 2_756 . ?
N1 C12 H12A 108.6 . . ?
N6 C12 H12B 108.6 2_756 . ?
N1 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 O1 0.1(11) . . . . ?
C3 N1 C1 O1 173.4(7) . . . . ?
C12 N1 C1 N2 -177.6(6) . . . . ?
C3 N1 C1 N2 -4.3(8) . . . . ?
C4 N2 C1 O1 -0.8(11) . . . . ?
C2 N2 C1 O1 -172.9(7) . . . . ?
C4 N2 C1 N1 176.9(6) . . . . ?
C2 N2 C1 N1 4.7(8) . . . . ?
C1 N2 C2 N2 -112.2(7) . . . 6_565 ?
C4 N2 C2 N2 76.1(10) . . . 6_565 ?
C1 N2 C2 C13 121.5(8) . . . . ?
C4 N2 C2 C13 -50.3(10) . . . . ?
C1 N2 C2 C3 -3.2(8) . . . . ?
C4 N2 C2 C3 -175.0(6) . . . . ?
C1 N1 C3 N1 112.1(7) . . . 6_565 ?
C12 N1 C3 N1 -75.0(10) . . . 6_565 ?
C1 N1 C3 C14 -121.9(8) . . . . ?
C12 N1 C3 C14 51.0(10) . . . . ?
C1 N1 C3 C2 2.2(8) . . . . ?
C12 N1 C3 C2 175.1(6) . . . . ?
N2 C2 C3 N1 117.0(6) 6_565 . . . ?
N2 C2 C3 N1 0.6(7) . . . . ?
C13 C2 C3 N1 -121.2(5) . . . . ?
N2 C2 C3 N1 -0.6(7) 6_565 . . 6_565 ?
N2 C2 C3 N1 -117.0(6) . . . 6_565 ?
C13 C2 C3 N1 121.2(5) . . . 6_565 ?
N2 C2 C3 C14 -121.8(5) 6_565 . . . ?
N2 C2 C3 C14 121.8(5) . . . . ?
C13 C2 C3 C14 0.000(3) . . . . ?
C1 N2 C4 N3 101.5(8) . . . . ?
C2 N2 C4 N3 -87.5(9) . . . . ?
C5 N3 C4 N2 -108.9(8) . . . . ?
C7 N3 C4 N2 87.3(9) . . . . ?
C6 N4 C5 O2 -173.0(8) . . . . ?
C8 N4 C5 O2 -7.5(12) . . . . ?
C6 N4 C5 N3 6.2(9) . . . . ?
C8 N4 C5 N3 171.7(6) . . . . ?
C7 N3 C5 O2 173.2(8) . . . . ?
C4 N3 C5 O2 7.6(12) . . . . ?
C7 N3 C5 N4 -6.0(9) . . . . ?
C4 N3 C5 N4 -171.6(6) . . . . ?
C5 N4 C6 N4 -115.1(8) . . . 6_565 ?
C8 N4 C6 N4 79.4(10) . . . 6_565 ?
C5 N4 C6 C7 -3.8(8) . . . . ?
C8 N4 C6 C7 -169.3(6) . . . . ?
C5 N3 C7 N3 116.2(8) . . . 6_565 ?
C4 N3 C7 N3 -78.4(10) . . . 6_565 ?
C5 N3 C7 C6 3.5(8) . . . . ?
C4 N3 C7 C6 169.0(7) . . . . ?
N4 C6 C7 N3 119.4(6) 6_565 . . . ?
N4 C6 C7 N3 0.1(8) . . . . ?
N4 C6 C7 N3 -0.1(8) 6_565 . . 6_565 ?
N4 C6 C7 N3 -119.4(6) . . . 6_565 ?
C9 N5 C8 N4 -106.6(8) . . . . ?
C11 N5 C8 N4 87.0(8) . . . . ?
C5 N4 C8 N5 108.6(8) . . . . ?
C6 N4 C8 N5 -87.4(8) . . . . ?
C8 N5 C9 O3 7.0(12) . . . . ?
C11 N5 C9 O3 174.7(8) . . . . ?
C8 N5 C9 N6 -171.6(6) . . . . ?
C11 N5 C9 N6 -3.9(9) . . . . ?
C12 N6 C9 O3 -7.4(12) 2_756 . . . ?
C10 N6 C9 O3 -174.9(8) . . . . ?
C12 N6 C9 N5 171.2(6) 2_756 . . . ?
C10 N6 C9 N5 3.7(9) . . . . ?
C9 N6 C10 N6 -114.8(8) . . . 6_565 ?
C12 N6 C10 N6 77.8(10) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.1(8) . . . . ?
C12 N6 C10 C11 -169.4(7) 2_756 . . . ?
C9 N5 C11 N5 114.1(8) . . . 6_565 ?
C8 N5 C11 N5 -78.3(10) . . . 6_565 ?
C9 N5 C11 C10 2.5(8) . . . . ?
C8 N5 C11 C10 170.2(6) . . . . ?
N6 C10 C11 N5 0.2(7) 6_565 . . 6_565 ?
N6 C10 C11 N5 -119.9(6) . . . 6_565 ?
N6 C10 C11 N5 119.9(6) 6_565 . . . ?
N6 C10 C11 N5 -0.2(7) . . . . ?
C1 N1 C12 N6 -101.4(8) . . . 2_756 ?
C3 N1 C12 N6 86.2(9) . . . 2_756 ?

_refine_diff_density_max         3.537
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.278

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

data_15pp
_database_code_depnum_ccdc_archive 'CCDC 1038164'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_15pp                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_15pp                
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
In the case of O1w, this distance is between two half occupied atoms so 
does not represent a hydrogen bond. 
;

_vrf_PLAT075_15pp                
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_15pp                
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;




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
1 -0.001 -0.003 0.000 1090.8 452.4
2 0.500 0.048 0.500 121.8 37.9
3 1.000 0.548 0.500 121.7 37.9
_platon_squeeze_details          
;
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 Lu N24 O22'
_chemical_formula_weight         1494.31

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.372(5)
_cell_length_b                   12.330(3)
_cell_length_c                   14.778(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.881(7)
_cell_angle_gamma                90
_cell_volume                     3698.2(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7912
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      25.66

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             1500
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.520
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11014
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.942
_diffrn_reflns_theta_max         27.629
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4085
_reflns_number_gt                3926
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1690P)²+6.0134P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4085
_refine_ls_number_parameters     241
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0742
_refine_ls_wR_factor_ref         0.2261
_refine_ls_wR_factor_gt          0.2233
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.196
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.9454(11) 0.5000 0.4967(16) 0.142(7) Uiso 1 2 d S . P . .
Lu1 Lu 1.0000 1.0000 0.5000 0.0280(2) Uani 1 4 d S T P . .
N1 N 0.7759(3) 0.4010(5) 0.4183(4) 0.0342(12) Uani 1 1 d . . . . .
N2 N 0.8212(3) 0.4018(5) 0.5823(4) 0.0328(11) Uani 1 1 d . . . . .
N3 N 0.9231(3) 0.4025(5) 0.7320(4) 0.0352(12) Uani 1 1 d . . . . .
N4 N 1.0312(3) 0.4021(5) 0.8083(4) 0.0338(11) Uani 1 1 d . . . . .
N5 N 1.1396(3) 0.4016(5) 0.8093(4) 0.0349(12) Uani 1 1 d . . . . .
N6 N 1.2047(3) 0.4015(5) 0.7313(4) 0.0350(12) Uani 1 1 d . . . . .
O1 O 0.8384(3) 0.2552(4) 0.5007(4) 0.0443(12) Uani 1 1 d . . . . .
O2 O 0.9795(3) 0.2539(5) 0.7149(5) 0.0571(16) Uani 1 1 d . . . . .
O3 O 1.1378(3) 0.2544(5) 0.7141(5) 0.0571(15) Uani 1 1 d . . . . .
O4 O 0.9104(6) 0.9310(9) 0.3663(9) 0.055(3) Uani 0.5 1 d . . P A 1
O6 O 0.9553(6) 0.8567(9) 0.5534(8) 0.048(3) Uani 0.5 1 d . . P B 1
O5 O 0.9255(6) 0.8584(10) 0.4513(9) 0.052(3) Uani 0.5 1 d . . P A 2
O7 O 0.9895(7) 0.9331(9) 0.6373(9) 0.055(3) Uani 0.5 1 d . . P A 2
C1 C 0.8145(3) 0.3446(5) 0.5001(5) 0.0317(13) Uani 1 1 d . . . . .
C2 C 0.7814(4) 0.5000 0.5589(7) 0.0278(17) Uani 1 2 d S T P . .
C3 C 0.7498(4) 0.5000 0.4418(7) 0.0291(17) Uani 1 2 d S T P . .
C4 C 0.8577(3) 0.3581(6) 0.6799(5) 0.0358(14) Uani 1 1 d . . . . .
H4A H 0.8612 0.2802 0.6744 0.043 Uiso 1 1 calc R U . . .
H4B H 0.8332 0.3712 0.7196 0.043 Uiso 1 1 calc R U . . .
C5 C 0.9785(3) 0.3444(6) 0.7481(5) 0.0350(14) Uani 1 1 d . . . . .
C6 C 1.0131(4) 0.5000 0.8436(6) 0.0290(17) Uani 1 2 d S T P . .
H6 H 1.0285 0.5000 0.9163 0.035 Uiso 1 2 calc R U P . .
C7 C 0.9377(4) 0.5000 0.7898(7) 0.0310(18) Uani 1 2 d S T P . .
H7 H 0.9174 0.5000 0.8371 0.037 Uiso 1 2 calc R U P . .
C8 C 1.0974(3) 0.3580(6) 0.8522(5) 0.0354(14) Uani 1 1 d . . . . .
H8A H 1.1170 0.3730 0.9232 0.043 Uiso 1 1 calc R U . . .
H8B H 1.0950 0.2799 0.8437 0.043 Uiso 1 1 calc R U . . .
C9 C 1.1580(3) 0.3443(6) 0.7477(5) 0.0360(14) Uani 1 1 d . . . . .
C10 C 1.2222(4) 0.5000 0.7898(6) 0.0307(18) Uani 1 2 d S T P . .
H10 H 1.2688 0.5000 0.8371 0.037 Uiso 1 2 calc R U P . .
C11 C 1.1770(4) 0.5000 0.8437(6) 0.0297(18) Uani 1 2 d S T P . .
H11 H 1.2022 0.5000 0.9163 0.036 Uiso 1 2 calc R U P . .
C12 C 0.7585(3) 0.3577(6) 0.3192(5) 0.0364(14) Uani 1 1 d . . . . .
H12A H 0.7648 0.2797 0.3242 0.044 Uiso 1 1 calc R U . . .
H12B H 0.7121 0.3712 0.2789 0.044 Uiso 1 1 calc R U . . .
C13 C 0.7328(5) 0.5000 0.6054(8) 0.042(2) Uani 1 2 d S T P . .
H13A H 0.7076 0.4341 0.5881 0.063 Uiso 0.5 1 calc R U P . .
H13B H 0.7561 0.5050 0.6766 0.063 Uiso 1 2 calc R U P . .
H13C H 0.7036 0.5609 0.5809 0.063 Uiso 0.5 1 calc R U P . .
C14 C 0.6735(5) 0.5000 0.3921(8) 0.044(2) Uani 1 2 d S T P . .
H14A H 0.6576 0.5659 0.4087 0.066 Uiso 0.5 1 calc R U P . .
H14B H 0.6582 0.4951 0.3211 0.066 Uiso 1 2 calc R U P . .
H14C H 0.6575 0.4390 0.4158 0.066 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.8169(4) 0.529(3) 0.8922(4) 0.154(11) Uani 0.5 1 d . U P . .
Cl2 Cl 1.0000 0.6987(11) 1.0000 0.193(11) Uani 0.5 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O7 2.292(10) 6_575 ?
Lu1 O7 2.292(10) 2_756 ?
Lu1 O7 2.292(10) 5_776 ?
Lu1 O7 2.292(10) . ?
Lu1 O4 2.305(10) . ?
Lu1 O4 2.305(10) 5_776 ?
Lu1 O4 2.305(10) 2_756 ?
Lu1 O4 2.305(10) 6_575 ?
Lu1 O5 2.310(11) 5_776 ?
Lu1 O5 2.310(11) 6_575 ?
Lu1 O5 2.310(11) 2_756 ?
Lu1 O5 2.310(11) . ?
N1 C1 1.346(9) . ?
N1 C12 1.450(8) . ?
N1 C3 1.458(7) . ?
N2 C1 1.357(9) . ?
N2 C4 1.431(8) . ?
N2 C2 1.455(7) . ?
N3 C5 1.362(9) . ?
N3 C7 1.431(7) . ?
N3 C4 1.444(9) . ?
N4 C5 1.344(9) . ?
N4 C6 1.439(7) . ?
N4 C8 1.449(8) . ?
N5 C9 1.348(9) . ?
N5 C11 1.440(7) . ?
N5 C8 1.443(8) . ?
N6 C9 1.364(9) . ?
N6 C12 1.428(9) 2_756 ?
N6 C10 1.447(7) . ?
O1 C1 1.225(9) . ?
O2 C5 1.224(9) . ?
O3 C9 1.221(9) . ?
O4 O4 1.70(2) 6_575 ?
O7 O7 1.65(2) 6_575 ?
C2 N2 1.455(7) 6_565 ?
C2 C13 1.513(12) . ?
C2 C3 1.570(12) . ?
C3 N1 1.458(7) 6_565 ?
C3 C14 1.547(12) . ?
C6 N4 1.439(7) 6_565 ?
C6 C7 1.532(12) . ?
C7 N3 1.431(7) 6_565 ?
C10 N6 1.447(7) 6_565 ?
C10 C11 1.529(12) . ?
C11 N5 1.440(7) 6_565 ?
C12 N6 1.428(9) 2_756 ?
Cl1 Cl1 0.71(6) 6_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Lu1 O7 180.0 6_575 2_756 ?
O7 Lu1 O7 137.8(6) 6_575 5_776 ?
O7 Lu1 O7 42.2(6) 2_756 5_776 ?
O7 Lu1 O7 42.2(6) 6_575 . ?
O7 Lu1 O7 137.8(6) 2_756 . ?
O7 Lu1 O7 180.0 5_776 . ?
O4 Lu1 O4 180.0 . 5_776 ?
O4 Lu1 O4 136.7(6) . 2_756 ?
O4 Lu1 O4 43.3(6) 5_776 2_756 ?
O4 Lu1 O4 43.3(6) . 6_575 ?
O4 Lu1 O4 136.7(6) 5_776 6_575 ?
O4 Lu1 O4 180.0 2_756 6_575 ?
O7 Lu1 O5 77.4(5) 6_575 5_776 ?
O7 Lu1 O5 102.6(5) 2_756 5_776 ?
O7 Lu1 O5 71.0(5) 5_776 5_776 ?
O7 Lu1 O5 109.0(5) . 5_776 ?
O7 Lu1 O5 71.0(4) 6_575 6_575 ?
O7 Lu1 O5 109.0(4) 2_756 6_575 ?
O7 Lu1 O5 77.4(5) 5_776 6_575 ?
O7 Lu1 O5 102.6(5) . 6_575 ?
O5 Lu1 O5 81.8(7) 5_776 6_575 ?
O7 Lu1 O5 109.0(4) 6_575 2_756 ?
O7 Lu1 O5 71.0(4) 2_756 2_756 ?
O7 Lu1 O5 102.6(5) 5_776 2_756 ?
O7 Lu1 O5 77.4(5) . 2_756 ?
O5 Lu1 O5 98.2(7) 5_776 2_756 ?
O5 Lu1 O5 180.0 6_575 2_756 ?
O7 Lu1 O5 102.6(5) 6_575 . ?
O7 Lu1 O5 77.4(5) 2_756 . ?
O7 Lu1 O5 109.0(5) 5_776 . ?
O7 Lu1 O5 71.0(5) . . ?
O5 Lu1 O5 180.0 5_776 . ?
O5 Lu1 O5 98.2(7) 6_575 . ?
O5 Lu1 O5 81.8(7) 2_756 . ?
C1 N1 C12 121.0(6) . . ?
C1 N1 C3 112.8(6) . . ?
C12 N1 C3 125.8(6) . . ?
C1 N2 C4 120.6(6) . . ?
C1 N2 C2 113.1(6) . . ?
C4 N2 C2 125.8(6) . . ?
C5 N3 C7 112.0(6) . . ?
C5 N3 C4 122.5(6) . . ?
C7 N3 C4 124.1(6) . . ?
C5 N4 C6 112.4(6) . . ?
C5 N4 C8 123.0(6) . . ?
C6 N4 C8 122.9(6) . . ?
C9 N5 C11 112.5(6) . . ?
C9 N5 C8 123.0(6) . . ?
C11 N5 C8 123.3(6) . . ?
C9 N6 C12 123.3(6) . 2_756 ?
C9 N6 C10 111.3(6) . . ?
C12 N6 C10 123.9(6) 2_756 . ?
O4 O4 Lu1 68.3(3) 6_575 . ?
O7 O7 Lu1 68.9(3) 6_575 . ?
O1 C1 N1 125.8(6) . . ?
O1 C1 N2 125.3(6) . . ?
N1 C1 N2 108.9(6) . . ?
N2 C2 N2 112.5(7) 6_565 . ?
N2 C2 C13 112.2(5) 6_565 . ?
N2 C2 C13 112.2(5) . . ?
N2 C2 C3 102.1(5) 6_565 . ?
N2 C2 C3 102.1(5) . . ?
C13 C2 C3 115.0(8) . . ?
N1 C3 N1 113.8(7) . 6_565 ?
N1 C3 C14 111.1(5) . . ?
N1 C3 C14 111.1(5) 6_565 . ?
N1 C3 C2 102.9(5) . . ?
N1 C3 C2 102.8(5) 6_565 . ?
C14 C3 C2 114.8(8) . . ?
N2 C4 N3 114.5(6) . . ?
O2 C5 N4 126.1(6) . . ?
O2 C5 N3 125.3(7) . . ?
N4 C5 N3 108.5(6) . . ?
N4 C6 N4 114.0(7) . 6_565 ?
N4 C6 C7 103.2(5) . . ?
N4 C6 C7 103.2(5) 6_565 . ?
N3 C7 N3 114.3(8) . 6_565 ?
N3 C7 C6 103.5(5) . . ?
N3 C7 C6 103.5(5) 6_565 . ?
N5 C8 N4 113.4(5) . . ?
O3 C9 N5 125.7(7) . . ?
O3 C9 N6 125.3(7) . . ?
N5 C9 N6 108.9(6) . . ?
N6 C10 N6 114.3(7) . 6_565 ?
N6 C10 C11 103.8(5) . . ?
N6 C10 C11 103.8(5) 6_565 . ?
N5 C11 N5 114.9(7) . 6_565 ?
N5 C11 C10 103.3(5) . . ?
N5 C11 C10 103.3(5) 6_565 . ?
N6 C12 N1 114.8(6) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 O1 0.3(10) . . . . ?
C3 N1 C1 O1 174.3(6) . . . . ?
C12 N1 C1 N2 -178.1(6) . . . . ?
C3 N1 C1 N2 -4.1(8) . . . . ?
C4 N2 C1 O1 -1.2(10) . . . . ?
C2 N2 C1 O1 -173.6(6) . . . . ?
C4 N2 C1 N1 177.3(6) . . . . ?
C2 N2 C1 N1 4.9(8) . . . . ?
C1 N2 C2 N2 -112.2(7) . . . 6_565 ?
C4 N2 C2 N2 75.9(9) . . . 6_565 ?
C1 N2 C2 C13 120.2(7) . . . . ?
C4 N2 C2 C13 -51.8(9) . . . . ?
C1 N2 C2 C3 -3.5(7) . . . . ?
C4 N2 C2 C3 -175.4(6) . . . . ?
C1 N1 C3 N1 112.3(7) . . . 6_565 ?
C12 N1 C3 N1 -74.0(10) . . . 6_565 ?
C1 N1 C3 C14 -121.4(7) . . . . ?
C12 N1 C3 C14 52.2(9) . . . . ?
C1 N1 C3 C2 1.8(7) . . . . ?
C12 N1 C3 C2 175.5(6) . . . . ?
N2 C2 C3 N1 117.5(5) 6_565 . . . ?
N2 C2 C3 N1 0.9(7) . . . . ?
C13 C2 C3 N1 -120.8(4) . . . . ?
N2 C2 C3 N1 -0.9(7) 6_565 . . 6_565 ?
N2 C2 C3 N1 -117.5(5) . . . 6_565 ?
C13 C2 C3 N1 120.8(4) . . . 6_565 ?
N2 C2 C3 C14 -121.7(4) 6_565 . . . ?
N2 C2 C3 C14 121.7(4) . . . . ?
C13 C2 C3 C14 0.000(2) . . . . ?
C1 N2 C4 N3 102.4(7) . . . . ?
C2 N2 C4 N3 -86.2(8) . . . . ?
C5 N3 C4 N2 -108.4(8) . . . . ?
C7 N3 C4 N2 85.7(8) . . . . ?
C6 N4 C5 O2 -173.2(7) . . . . ?
C8 N4 C5 O2 -7.7(11) . . . . ?
C6 N4 C5 N3 5.3(8) . . . . ?
C8 N4 C5 N3 170.8(6) . . . . ?
C7 N3 C5 O2 173.4(7) . . . . ?
C4 N3 C5 O2 5.9(11) . . . . ?
C7 N3 C5 N4 -5.1(8) . . . . ?
C4 N3 C5 N4 -172.5(6) . . . . ?
C5 N4 C6 N4 -114.6(7) . . . 6_565 ?
C8 N4 C6 N4 79.9(9) . . . 6_565 ?
C5 N4 C6 C7 -3.4(7) . . . . ?
C8 N4 C6 C7 -168.9(6) . . . . ?
C5 N3 C7 N3 114.7(7) . . . 6_565 ?
C4 N3 C7 N3 -78.0(10) . . . 6_565 ?
C5 N3 C7 C6 2.8(8) . . . . ?
C4 N3 C7 C6 170.0(6) . . . . ?
N4 C6 C7 N3 0.3(7) . . . . ?
N4 C6 C7 N3 119.3(5) 6_565 . . . ?
N4 C6 C7 N3 -119.3(5) . . . 6_565 ?
N4 C6 C7 N3 -0.3(7) 6_565 . . 6_565 ?
C9 N5 C8 N4 -106.9(8) . . . . ?
C11 N5 C8 N4 86.7(8) . . . . ?
C5 N4 C8 N5 108.4(7) . . . . ?
C6 N4 C8 N5 -87.6(8) . . . . ?
C11 N5 C9 O3 174.2(7) . . . . ?
C8 N5 C9 O3 6.5(11) . . . . ?
C11 N5 C9 N6 -3.8(8) . . . . ?
C8 N5 C9 N6 -171.5(6) . . . . ?
C12 N6 C9 O3 -7.2(11) 2_756 . . . ?
C10 N6 C9 O3 -174.2(7) . . . . ?
C12 N6 C9 N5 170.9(6) 2_756 . . . ?
C10 N6 C9 N5 3.9(8) . . . . ?
C9 N6 C10 N6 -114.7(7) . . . 6_565 ?
C12 N6 C10 N6 78.4(9) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.4(8) . . . . ?
C12 N6 C10 C11 -169.3(6) 2_756 . . . ?
C9 N5 C11 N5 114.0(7) . . . 6_565 ?
C8 N5 C11 N5 -78.4(9) . . . 6_565 ?
C9 N5 C11 C10 2.2(7) . . . . ?
C8 N5 C11 C10 169.9(6) . . . . ?
N6 C10 C11 N5 0.2(7) . . . . ?
N6 C10 C11 N5 119.9(5) 6_565 . . . ?
N6 C10 C11 N5 -119.9(5) . . . 6_565 ?
N6 C10 C11 N5 -0.2(7) 6_565 . . 6_565 ?
C1 N1 C12 N6 -101.5(8) . . . 2_756 ?
C3 N1 C12 N6 85.3(8) . . . 2_756 ?

_refine_diff_density_max         3.521
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.274

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

data_2p
_database_code_depnum_ccdc_archive 'CCDC 1038165'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_2p                  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_2p                  
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            2'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H132 Ce2 N76 O64'
_chemical_formula_weight         3943.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   15.375(4)
_cell_length_b                   17.143(4)
_cell_length_c                   35.259(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.376(3)
_cell_angle_gamma                90
_cell_volume                     9277(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    5294
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      19.46

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_F_000             4024
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.587
_shelx_estimated_absorpt_T_min   0.858
_shelx_estimated_absorpt_T_max   0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48454
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.157
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             16483
_reflns_number_gt                9955
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0736P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16483
_refine_ls_number_parameters     1180
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1473
_refine_ls_wR_factor_gt          0.1329
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_restrained_S_all      0.933
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

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
1 -0.002 0.021 -0.002 1728.1 626.4
2 0.000 0.500 0.000 114.3 9.1
3 0.235 0.939 0.838 51.3 9.4
4 0.265 0.439 0.662 51.3 9.1
5 0.500 0.000 0.500 114.3 8.9
6 0.735 0.561 0.338 51.3 9.4
7 0.765 0.061 0.162 51.3 9.2
_platon_squeeze_details          
; 
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5592(3) 0.2456(3) 0.71913(15) 0.0336(12) Uani 1 1 d . . . . .
C2 C 0.4623(3) 0.1565(3) 0.74987(14) 0.0323(12) Uani 1 1 d . . . . .
H2A H 0.4803 0.1208 0.7305 0.039 Uiso 1 1 calc R U . . .
H2B H 0.4700 0.1303 0.7742 0.039 Uiso 1 1 calc R U . . .
C3 C 0.3276(3) 0.1745(3) 0.70785(14) 0.0288(11) Uani 1 1 d . . . . .
C4 C 0.1755(3) 0.1629(3) 0.68323(14) 0.0355(12) Uani 1 1 d . . . . .
H4A H 0.2033 0.1367 0.6628 0.043 Uiso 1 1 calc R U . . .
H4B H 0.1371 0.1257 0.6945 0.043 Uiso 1 1 calc R U . . .
C5 C 0.1212(3) 0.2439(3) 0.62997(14) 0.0334(12) Uani 1 1 d . . . . .
C6 C 0.0273(3) 0.3213(3) 0.58476(14) 0.0366(12) Uani 1 1 d . . . . .
H6A H -0.0359 0.3211 0.5819 0.044 Uiso 1 1 calc R U . . .
H6B H 0.0484 0.2844 0.5666 0.044 Uiso 1 1 calc R U . . .
C7 C 0.1256(3) 0.4054(3) 0.55251(14) 0.0332(12) Uani 1 1 d . . . . .
C8 C 0.2144(3) 0.5109(3) 0.52771(13) 0.0358(12) Uani 1 1 d . . . . .
H8A H 0.2330 0.4715 0.5101 0.043 Uiso 1 1 calc R U . . .
H8B H 0.1999 0.5576 0.5131 0.043 Uiso 1 1 calc R U . . .
C9 C 0.3528(3) 0.4770(3) 0.56313(13) 0.0328(12) Uani 1 1 d . . . . .
C10 C 0.5042(3) 0.4822(3) 0.59016(13) 0.0350(12) Uani 1 1 d . . . . .
H10A H 0.5062 0.4326 0.5769 0.042 Uiso 1 1 calc R U . . .
H10B H 0.5448 0.5173 0.5789 0.042 Uiso 1 1 calc R U . . .
C11 C 0.5591(3) 0.4008(3) 0.64299(14) 0.0297(11) Uani 1 1 d . . . . .
C12 C 0.6539(3) 0.3484(3) 0.69638(14) 0.0315(12) Uani 1 1 d . . . . .
H12A H 0.7077 0.3706 0.7073 0.038 Uiso 1 1 calc R U . . .
H12B H 0.6692 0.3094 0.6780 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5412(3) 0.2763(3) 0.78299(13) 0.0333(12) Uani 1 1 d . . . . .
C14 C 0.5860(4) 0.2283(3) 0.81453(15) 0.0475(15) Uani 1 1 d . . . . .
H14A H 0.6335 0.1999 0.8047 0.071 Uiso 1 1 calc R U . . .
H14B H 0.6077 0.2623 0.8345 0.071 Uiso 1 1 calc R U . . .
H14C H 0.5450 0.1923 0.8243 0.071 Uiso 1 1 calc R U . . .
C15 C 0.3129(3) 0.1902(3) 0.77256(13) 0.0287(11) Uani 1 1 d . . . . .
H15 H 0.3173 0.1501 0.7924 0.034 Uiso 1 1 calc R U . . .
C16 C 0.2223(3) 0.1914(3) 0.75199(13) 0.0286(11) Uani 1 1 d . . . . .
H16 H 0.1859 0.1479 0.7597 0.034 Uiso 1 1 calc R U . . .
C17 C 0.0515(3) 0.2602(3) 0.68667(13) 0.0316(12) Uani 1 1 d . . . . .
H17 H 0.0110 0.2204 0.6949 0.038 Uiso 1 1 calc R U . . .
C18 C 0.0092(3) 0.3134(3) 0.65595(13) 0.0314(12) Uani 1 1 d . . . . .
H18 H -0.0535 0.3035 0.6523 0.038 Uiso 1 1 calc R U . . .
C19 C 0.0158(3) 0.4724(3) 0.58389(13) 0.0307(11) Uani 1 1 d . . . . .
C20 C -0.0800(3) 0.4719(3) 0.56949(16) 0.0504(15) Uani 1 1 d . . . . .
H20A H -0.0844 0.4571 0.5432 0.076 Uiso 1 1 calc R U . . .
H20B H -0.1116 0.4353 0.5840 0.076 Uiso 1 1 calc R U . . .
H20C H -0.1042 0.5231 0.5722 0.076 Uiso 1 1 calc R U . . .
C21 C 0.0750(3) 0.5332(3) 0.56372(13) 0.0342(12) Uani 1 1 d . . . . .
C22 C 0.0277(4) 0.5890(3) 0.53504(15) 0.0466(14) Uani 1 1 d . . . . .
H22A H -0.0123 0.6210 0.5480 0.070 Uiso 1 1 calc R U . . .
H22B H 0.0696 0.6216 0.5236 0.070 Uiso 1 1 calc R U . . .
H22C H -0.0037 0.5592 0.5157 0.070 Uiso 1 1 calc R U . . .
C23 C 0.3083(3) 0.6068(3) 0.56661(14) 0.0319(12) Uani 1 1 d . . . . .
H23 H 0.3073 0.6431 0.5451 0.038 Uiso 1 1 calc R U . . .
C24 C 0.4010(3) 0.5982(3) 0.58579(13) 0.0317(12) Uani 1 1 d . . . . .
H24 H 0.4441 0.6267 0.5718 0.038 Uiso 1 1 calc R U . . .
C25 C 0.5674(3) 0.5340(3) 0.65339(13) 0.0308(11) Uani 1 1 d . . . . .
H25 H 0.6110 0.5638 0.6403 0.037 Uiso 1 1 calc R U . . .
C26 C 0.6087(3) 0.4902(3) 0.68819(14) 0.0314(12) Uani 1 1 d . . . . .
H26 H 0.6690 0.5068 0.6941 0.038 Uiso 1 1 calc R U . . .
C27 C 0.5993(3) 0.3404(3) 0.76485(14) 0.0321(12) Uani 1 1 d . . . . .
C28 C 0.6879(3) 0.3541(3) 0.78482(16) 0.0498(15) Uani 1 1 d . . . . .
H28A H 0.7220 0.3073 0.7839 0.075 Uiso 1 1 calc R U . . .
H28B H 0.7170 0.3956 0.7724 0.075 Uiso 1 1 calc R U . . .
H28C H 0.6808 0.3680 0.8108 0.075 Uiso 1 1 calc R U . . .
C29 C 0.4700(3) 0.3974(3) 0.78452(13) 0.0341(12) Uani 1 1 d . . . . .
C30 C 0.3944(3) 0.2896(3) 0.81448(13) 0.0358(12) Uani 1 1 d . . . . .
H30A H 0.4133 0.2442 0.8292 0.043 Uiso 1 1 calc R U . . .
H30B H 0.3743 0.3283 0.8320 0.043 Uiso 1 1 calc R U . . .
C31 C 0.2448(3) 0.3072(3) 0.78627(13) 0.0307(12) Uani 1 1 d . . . . .
C32 C 0.0973(3) 0.2883(3) 0.75582(13) 0.0347(12) Uani 1 1 d . . . . .
H32A H 0.0840 0.3301 0.7731 0.042 Uiso 1 1 calc R U . . .
H32B H 0.0606 0.2441 0.7612 0.042 Uiso 1 1 calc R U . . .
C33 C 0.0600(3) 0.3900(3) 0.70771(14) 0.0314(12) Uani 1 1 d . . . . .
C34 C -0.0169(3) 0.4604(3) 0.65473(13) 0.0337(12) Uani 1 1 d . . . . .
H34A H -0.0759 0.4463 0.6461 0.040 Uiso 1 1 calc R U . . .
H34B H -0.0206 0.4992 0.6746 0.040 Uiso 1 1 calc R U . . .
C35 C 0.0811(3) 0.5583(3) 0.62972(15) 0.0346(12) Uani 1 1 d . . . . .
C36 C 0.1656(3) 0.6485(3) 0.59321(14) 0.0351(12) Uani 1 1 d . . . . .
H36A H 0.1512 0.6727 0.5688 0.042 Uiso 1 1 calc R U . . .
H36B H 0.1494 0.6845 0.6128 0.042 Uiso 1 1 calc R U . . .
C37 C 0.3087(3) 0.6537(3) 0.62944(15) 0.0322(12) Uani 1 1 d . . . . .
C38 C 0.4644(3) 0.6499(3) 0.64958(14) 0.0343(12) Uani 1 1 d . . . . .
H38A H 0.5087 0.6764 0.6359 0.041 Uiso 1 1 calc R U . . .
H38B H 0.4440 0.6861 0.6682 0.041 Uiso 1 1 calc R U . . .
C39 C 0.4982(3) 0.5711(3) 0.70716(14) 0.0306(11) Uani 1 1 d . . . . .
C40 C 0.5700(3) 0.4891(3) 0.75665(14) 0.0354(12) Uani 1 1 d . . . . .
H40A H 0.5401 0.5250 0.7727 0.042 Uiso 1 1 calc R U . . .
H40B H 0.6320 0.4942 0.7630 0.042 Uiso 1 1 calc R U . . .
C41 C 0.4929(3) 0.0005(3) 0.62557(13) 0.0332(12) Uani 1 1 d . . . . .
C42 C 0.3372(3) 0.0063(3) 0.63675(13) 0.0339(12) Uani 1 1 d . . . . .
H42A H 0.3054 -0.0251 0.6542 0.041 Uiso 1 1 calc R U . . .
H42B H 0.3551 0.0539 0.6499 0.041 Uiso 1 1 calc R U . . .
C43 C 0.2954(3) 0.0887(3) 0.58268(13) 0.0300(11) Uani 1 1 d . . . . .
C44 C 0.2307(3) 0.1553(3) 0.52666(14) 0.0388(13) Uani 1 1 d . . . . .
H44A H 0.2576 0.1999 0.5396 0.047 Uiso 1 1 calc R U . . .
H44B H 0.1692 0.1667 0.5221 0.047 Uiso 1 1 calc R U . . .
C45 C 0.3382(3) 0.1893(3) 0.47983(15) 0.0361(13) Uani 1 1 d . . . . .
C46 C 0.4043(3) 0.2245(3) 0.42041(16) 0.0441(14) Uani 1 1 d . . . . .
H46A H 0.4240 0.2683 0.4361 0.053 Uiso 1 1 calc R U . . .
H46B H 0.3715 0.2454 0.3984 0.053 Uiso 1 1 calc R U . . .
C47 C 0.5617(4) 0.1982(3) 0.42350(16) 0.0420(14) Uani 1 1 d . . . . .
C48 C 0.4217(3) -0.1191(3) 0.62945(15) 0.0382(13) Uani 1 1 d . . . . .
H48 H 0.4029 -0.1390 0.6537 0.046 Uiso 1 1 calc R U . . .
C49 C 0.2135(3) -0.0251(3) 0.58723(15) 0.0370(13) Uani 1 1 d . . . . .
C50 C 0.1457(4) -0.0466(4) 0.61552(17) 0.0593(17) Uani 1 1 d . . . . .
H50A H 0.1027 -0.0804 0.6034 0.089 Uiso 1 1 calc R U . . .
H50B H 0.1738 -0.0728 0.6369 0.089 Uiso 1 1 calc R U . . .
H50C H 0.1180 0.0000 0.6240 0.089 Uiso 1 1 calc R U . . .
C51 C 0.1788(3) 0.0227(3) 0.55125(14) 0.0354(12) Uani 1 1 d . . . . .
C52 C 0.0854(3) 0.0511(3) 0.55248(16) 0.0514(16) Uani 1 1 d . . . . .
H52A H 0.0811 0.0867 0.5733 0.077 Uiso 1 1 calc R U . . .
H52B H 0.0685 0.0772 0.5291 0.077 Uiso 1 1 calc R U . . .
H52C H 0.0476 0.0074 0.5558 0.077 Uiso 1 1 calc R U . . .
C53 C 0.2241(3) 0.1074(3) 0.45783(14) 0.0363(12) Uani 1 1 d . . . . .
H53 H 0.1648 0.1279 0.4535 0.044 Uiso 1 1 calc R U . . .
C54 C 0.2807(3) 0.1275(3) 0.42443(14) 0.0336(12) Uani 1 1 d . . . . .
H54 H 0.2469 0.1541 0.4038 0.040 Uiso 1 1 calc R U . . .
C55 C 0.4793(3) 0.1343(3) 0.37476(14) 0.0348(12) Uani 1 1 d . . . . .
H55 H 0.4523 0.1601 0.3523 0.042 Uiso 1 1 calc R U . . .
C56 C 0.2876(4) -0.1625(3) 0.58986(18) 0.0527(16) Uani 1 1 d . . . . .
H56A H 0.2595 -0.1674 0.6137 0.063 Uiso 1 1 calc R U . . .
H56B H 0.2729 -0.2084 0.5747 0.063 Uiso 1 1 calc R U . . .
C57 C 0.2322(4) -0.0967(3) 0.53143(18) 0.0450(14) Uani 1 1 d . . . . .
C58 C 0.1630(3) -0.0198(3) 0.48074(15) 0.0448(14) Uani 1 1 d . . . . .
H58A H 0.1075 0.0073 0.4793 0.054 Uiso 1 1 calc R U . . .
H58B H 0.1537 -0.0705 0.4689 0.054 Uiso 1 1 calc R U . . .
C59 C 0.2740(3) -0.0074(3) 0.43142(16) 0.0447(14) Uani 1 1 d . . . . .
C60 C 0.3530(3) 0.0406(3) 0.37732(14) 0.0395(13) Uani 1 1 d . . . . .
H60A H 0.3442 -0.0132 0.3694 0.047 Uiso 1 1 calc R U . . .
H60B H 0.3249 0.0736 0.3579 0.047 Uiso 1 1 calc R U . . .
N1 N 0.5183(3) 0.2254(2) 0.75027(11) 0.0325(10) Uani 1 1 d . . . . .
N2 N 0.3709(2) 0.1744(2) 0.74255(10) 0.0302(9) Uani 1 1 d . . . . .
N3 N 0.2420(2) 0.1866(2) 0.71181(11) 0.0307(9) Uani 1 1 d . . . . .
N4 N 0.1242(2) 0.2261(2) 0.66755(11) 0.0318(10) Uani 1 1 d . . . . .
N5 N 0.0533(3) 0.2946(2) 0.62260(11) 0.0330(10) Uani 1 1 d . . . . .
N6 N 0.0580(3) 0.3987(2) 0.57517(11) 0.0349(10) Uani 1 1 d . . . . .
N7 N 0.1367(3) 0.4834(2) 0.54479(11) 0.0366(10) Uani 1 1 d . . . . .
N8 N 0.2865(3) 0.5284(2) 0.55463(11) 0.0327(10) Uani 1 1 d . . . . .
N9 N 0.4166(2) 0.5143(2) 0.58484(11) 0.0315(10) Uani 1 1 d . . . . .
N10 N 0.5313(2) 0.4704(2) 0.62970(11) 0.0295(9) Uani 1 1 d . . . . .
N11 N 0.6041(2) 0.4094(2) 0.67679(12) 0.0337(10) Uani 1 1 d . . . . .
N12 N 0.6088(3) 0.3103(2) 0.72625(11) 0.0333(10) Uani 1 1 d . . . . .
N13 N 0.4683(3) 0.3211(2) 0.79551(11) 0.0336(10) Uani 1 1 d . . . . .
N14 N 0.3226(3) 0.2677(2) 0.78827(11) 0.0318(10) Uani 1 1 d . . . . .
N15 N 0.1876(3) 0.2661(2) 0.76263(11) 0.0321(10) Uani 1 1 d . . . . .
N16 N 0.0771(2) 0.3139(2) 0.71697(11) 0.0321(10) Uani 1 1 d . . . . .
N17 N 0.0266(3) 0.3919(2) 0.67061(11) 0.0330(10) Uani 1 1 d . . . . .
N18 N 0.0262(3) 0.4944(2) 0.62342(11) 0.0316(10) Uani 1 1 d . . . . .
N19 N 0.1147(2) 0.5777(2) 0.59600(11) 0.0332(10) Uani 1 1 d . . . . .
N20 N 0.2581(3) 0.6358(2) 0.59709(11) 0.0337(10) Uani 1 1 d . . . . .
N21 N 0.3926(2) 0.6313(2) 0.62311(11) 0.0325(10) Uani 1 1 d . . . . .
N22 N 0.5038(2) 0.5846(2) 0.66922(11) 0.0323(10) Uani 1 1 d . . . . .
N23 N 0.5529(3) 0.5115(2) 0.71783(11) 0.0322(10) Uani 1 1 d . . . . .
N24 N 0.5432(2) 0.4098(2) 0.76517(11) 0.0307(9) Uani 1 1 d . . . . .
N25 N 0.4142(3) -0.0360(2) 0.62729(11) 0.0343(10) Uani 1 1 d . . . . .
N26 N 0.2796(2) 0.0264(2) 0.60493(11) 0.0311(10) Uani 1 1 d . . . . .
N27 N 0.2401(2) 0.0882(2) 0.55093(11) 0.0298(9) Uani 1 1 d . . . . .
N28 N 0.2697(3) 0.1450(2) 0.49025(11) 0.0359(10) Uani 1 1 d . . . . .
N29 N 0.3468(3) 0.1772(2) 0.44172(12) 0.0378(10) Uani 1 1 d . . . . .
N30 N 0.4799(3) 0.1839(2) 0.40772(12) 0.0364(10) Uani 1 1 d . . . . .
N31 N 0.3798(3) -0.1603(2) 0.59763(13) 0.0414(11) Uani 1 1 d . . . . .
N32 N 0.2529(3) -0.0931(2) 0.56964(14) 0.0451(12) Uani 1 1 d . . . . .
N33 N 0.1901(3) -0.0315(2) 0.52033(12) 0.0384(10) Uani 1 1 d . . . . .
N34 N 0.2245(3) 0.0243(2) 0.45872(12) 0.0414(11) Uani 1 1 d . . . . .
N35 N 0.3107(3) 0.0526(2) 0.41290(12) 0.0380(10) Uani 1 1 d . . . . .
N36 N 0.4450(3) 0.0569(2) 0.37942(11) 0.0365(10) Uani 1 1 d . . . . .
N38 N 0.6475(6) 0.7179(6) 0.6930(3) 0.144(4) Uani 1 1 d D U . . .
O1 O 0.5550(2) 0.21019(19) 0.68816(9) 0.0341(8) Uani 1 1 d . . . . .
O2 O 0.3619(2) 0.16352(18) 0.67711(9) 0.0341(8) Uani 1 1 d . . . . .
O1W O 0.3360(2) 0.2971(2) 0.60639(11) 0.0489(10) Uani 1 1 d . . . . .
O3 O 0.1707(2) 0.2187(2) 0.60690(10) 0.0419(9) Uani 1 1 d . . . . .
O2W O 0.4093(2) 0.3276(2) 0.68101(11) 0.0574(11) Uani 1 1 d . . . . .
O4 O 0.1669(2) 0.3526(2) 0.53954(10) 0.0449(9) Uani 1 1 d . . . . .
O3W O 0.6271(2) 0.1894(2) 0.61553(10) 0.0453(9) Uani 1 1 d . . . . .
O5 O 0.3559(2) 0.40830(19) 0.55303(10) 0.0445(9) Uani 1 1 d . . . . .
O4W O 0.4880(2) 0.2321(3) 0.56161(10) 0.0595(12) Uani 1 1 d . . . . .
O6 O 0.5464(2) 0.33738(18) 0.62631(9) 0.0344(8) Uani 1 1 d . . . . .
O7 O 0.4161(2) 0.4468(2) 0.79132(10) 0.0444(9) Uani 1 1 d . . . . .
O8 O 0.2285(2) 0.36806(19) 0.80269(9) 0.0383(9) Uani 1 1 d . . . . .
O9 O 0.0731(2) 0.44665(19) 0.72804(9) 0.0391(9) Uani 1 1 d . . . . .
O10 O 0.0936(2) 0.5917(2) 0.65981(9) 0.0444(9) Uani 1 1 d . . . . .
O11 O 0.2846(2) 0.6865(2) 0.65733(10) 0.0423(9) Uani 1 1 d . . . . .
O12 O 0.4511(2) 0.6074(2) 0.72834(9) 0.0392(9) Uani 1 1 d . . . . .
O13 O 0.5078(2) 0.07051(19) 0.62772(9) 0.0361(8) Uani 1 1 d . . . . .
O14 O 0.3523(2) 0.13790(18) 0.59006(9) 0.0339(8) Uani 1 1 d . . . . .
O15 O 0.3823(2) 0.2327(2) 0.50028(10) 0.0474(10) Uani 1 1 d . . . . .
O16 O 0.5802(2) 0.2404(2) 0.45114(11) 0.0481(10) Uani 1 1 d . . . . .
O17 O 0.2518(3) -0.1513(2) 0.51105(13) 0.0674(12) Uani 1 1 d . . . . .
O18 O 0.2816(2) -0.0775(2) 0.42491(11) 0.0549(11) Uani 1 1 d . . . . .
O22 O 0.6732(4) 0.7037(3) 0.66089(17) 0.0936(17) Uani 1 1 d D U . . .
O23 O 0.6008(5) 0.7678(6) 0.7103(4) 0.260(7) Uani 1 1 d D U . . .
O24 O 0.6819(5) 0.6651(5) 0.7188(2) 0.161(3) Uani 1 1 d D U . . .
Ce1 Ce 0.46447(2) 0.21279(2) 0.62902(2) 0.03111(10) Uani 1 1 d . . . . .
O5W O 0.7048(3) 0.0785(3) 0.84968(15) 0.0976(17) Uani 1 1 d . . . . .
O6W O 0.2470(3) 0.0051(3) 0.75017(17) 0.1024(18) Uani 1 1 d . . . . .
O8W O 0.2240(4) 0.3331(4) 0.46682(16) 0.140(3) Uani 1 1 d . . . . .
O9W O 0.3630(4) 0.7576(5) 0.47287(17) 0.147(3) Uani 1 1 d . . . . .
O19 O 0.4170(5) 0.2886(4) 0.9546(3) 0.170(3) Uani 1 1 d . . . . .
N37 N 0.4688(7) 0.3178(7) 0.9828(3) 0.140(3) Uani 1 1 d . . . . .
O20 O 0.4560(7) 0.2981(6) 1.0177(2) 0.202(4) Uani 1 1 d . . . . .
O21 O 0.5153(5) 0.3631(7) 0.9665(3) 0.217(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.248(6) . ?
C1 N1 1.343(6) . ?
C1 N12 1.360(6) . ?
C2 N2 1.446(6) . ?
C2 N1 1.460(6) . ?
C3 O2 1.247(5) . ?
C3 N3 1.348(6) . ?
C3 N2 1.358(6) . ?
C4 N4 1.431(6) . ?
C4 N3 1.450(6) . ?
C5 O3 1.225(6) . ?
C5 N4 1.358(6) . ?
C5 N5 1.371(6) . ?
C6 N5 1.445(6) . ?
C6 N6 1.455(6) . ?
C7 O4 1.211(6) . ?
C7 N6 1.353(6) . ?
C7 N7 1.376(6) . ?
C8 N8 1.448(6) . ?
C8 N7 1.448(6) . ?
C9 O5 1.233(5) . ?
C9 N9 1.367(6) . ?
C9 N8 1.367(6) . ?
C10 N10 1.446(6) . ?
C10 N9 1.457(6) . ?
C11 O6 1.246(5) . ?
C11 N10 1.342(6) . ?
C11 N11 1.350(6) . ?
C12 N11 1.447(6) . ?
C12 N12 1.450(6) . ?
C13 N13 1.449(6) . ?
C13 N1 1.473(6) . ?
C13 C14 1.516(6) . ?
C13 C27 1.576(7) . ?
C15 N14 1.444(6) . ?
C15 N2 1.449(6) . ?
C15 C16 1.532(6) . ?
C16 N15 1.446(6) . ?
C16 N3 1.468(6) . ?
C17 N16 1.447(6) . ?
C17 N4 1.462(6) . ?
C17 C18 1.530(6) . ?
C18 N5 1.428(6) . ?
C18 N17 1.461(6) . ?
C19 N18 1.444(6) . ?
C19 N6 1.461(6) . ?
C19 C20 1.529(7) . ?
C19 C21 1.580(7) . ?
C21 N7 1.466(6) . ?
C21 N19 1.473(6) . ?
C21 C22 1.544(7) . ?
C23 N8 1.443(6) . ?
C23 N20 1.447(6) . ?
C23 C24 1.549(7) . ?
C24 N21 1.446(6) . ?
C24 N9 1.457(6) . ?
C25 N22 1.444(6) . ?
C25 N10 1.462(6) . ?
C25 C26 1.543(6) . ?
C26 N23 1.438(6) . ?
C26 N11 1.444(6) . ?
C27 N24 1.469(6) . ?
C27 N12 1.471(6) . ?
C27 C28 1.514(7) . ?
C29 O7 1.218(6) . ?
C29 N13 1.364(6) . ?
C29 N24 1.367(6) . ?
C30 N14 1.448(6) . ?
C30 N13 1.456(6) . ?
C31 O8 1.226(5) . ?
C31 N15 1.370(6) . ?
C31 N14 1.373(6) . ?
C32 N15 1.446(6) . ?
C32 N16 1.454(6) . ?
C33 O9 1.216(5) . ?
C33 N16 1.368(6) . ?
C33 N17 1.377(6) . ?
C34 N18 1.444(6) . ?
C34 N17 1.447(6) . ?
C35 O10 1.211(6) . ?
C35 N19 1.365(6) . ?
C35 N18 1.391(6) . ?
C36 N20 1.438(6) . ?
C36 N19 1.450(6) . ?
C37 O11 1.210(6) . ?
C37 N21 1.376(6) . ?
C37 N20 1.376(6) . ?
C38 N22 1.432(6) . ?
C38 N21 1.439(6) . ?
C39 O12 1.239(5) . ?
C39 N23 1.361(6) . ?
C39 N22 1.365(6) . ?
C40 N23 1.431(6) . ?
C40 N24 1.458(6) . ?
C41 O13 1.223(6) . ?
C41 N25 1.366(6) . ?
C41 N36 1.389(6) 3_656 ?
C42 N26 1.429(6) . ?
C42 N25 1.444(6) . ?
C43 O14 1.233(5) . ?
C43 N26 1.355(6) . ?
C43 N27 1.365(6) . ?
C44 N27 1.436(6) . ?
C44 N28 1.459(6) . ?
C45 O15 1.215(6) . ?
C45 N28 1.367(6) . ?
C45 N29 1.374(6) . ?
C46 N29 1.443(6) . ?
C46 N30 1.449(6) . ?
C47 O16 1.234(6) . ?
C47 N31 1.366(7) 3_656 ?
C47 N30 1.367(7) . ?
C48 N25 1.431(6) . ?
C48 N31 1.445(6) . ?
C48 C55 1.559(7) 3_656 ?
C49 N26 1.458(6) . ?
C49 N32 1.469(6) . ?
C49 C50 1.530(7) . ?
C49 C51 1.576(7) . ?
C51 N33 1.450(6) . ?
C51 N27 1.466(6) . ?
C51 C52 1.520(7) . ?
C53 N34 1.426(6) . ?
C53 N28 1.455(6) . ?
C53 C54 1.544(7) . ?
C54 N35 1.431(6) . ?
C54 N29 1.434(6) . ?
C55 N30 1.440(6) . ?
C55 N36 1.440(6) . ?
C55 C48 1.559(7) 3_656 ?
C56 N31 1.428(6) . ?
C56 N32 1.470(7) . ?
C57 O17 1.228(6) . ?
C57 N33 1.339(7) . ?
C57 N32 1.367(7) . ?
C58 N33 1.447(6) . ?
C58 N34 1.468(6) . ?
C59 O18 1.230(6) . ?
C59 N35 1.360(7) . ?
C59 N34 1.375(6) . ?
C60 N36 1.439(6) . ?
C60 N35 1.462(6) . ?
N31 C47 1.366(7) 3_656 ?
N36 C41 1.389(6) 3_656 ?
N38 O22 1.244(9) . ?
N38 O23 1.294(11) . ?
N38 O24 1.367(9) . ?
O1 Ce1 2.439(3) . ?
O2 Ce1 2.528(3) . ?
O1W Ce1 2.538(3) . ?
O2W Ce1 2.853(4) . ?
O3W Ce1 2.603(3) . ?
O4W Ce1 2.448(4) . ?
O6 Ce1 2.484(3) . ?
O13 Ce1 2.530(3) . ?
O14 Ce1 2.496(3) . ?
O19 N37 1.332(10) . ?
N37 O21 1.221(12) . ?
N37 O20 1.305(11) . ?

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 C1 N1 125.9(5) . . ?
O1 C1 N12 123.9(5) . . ?
N1 C1 N12 110.2(4) . . ?
N2 C2 N1 113.4(4) . . ?
O2 C3 N3 125.3(4) . . ?
O2 C3 N2 125.0(4) . . ?
N3 C3 N2 109.7(4) . . ?
N4 C4 N3 114.0(4) . . ?
O3 C5 N4 125.6(5) . . ?
O3 C5 N5 126.4(5) . . ?
N4 C5 N5 108.0(4) . . ?
N5 C6 N6 115.3(4) . . ?
O4 C7 N6 126.7(5) . . ?
O4 C7 N7 125.3(5) . . ?
N6 C7 N7 107.9(4) . . ?
N8 C8 N7 114.4(4) . . ?
O5 C9 N9 124.8(5) . . ?
O5 C9 N8 126.4(5) . . ?
N9 C9 N8 108.8(4) . . ?
N10 C10 N9 112.9(4) . . ?
O6 C11 N10 125.0(4) . . ?
O6 C11 N11 124.7(5) . . ?
N10 C11 N11 110.3(4) . . ?
N11 C12 N12 114.2(4) . . ?
N13 C13 N1 113.6(4) . . ?
N13 C13 C14 113.0(4) . . ?
N1 C13 C14 109.3(4) . . ?
N13 C13 C27 102.7(4) . . ?
N1 C13 C27 102.2(4) . . ?
C14 C13 C27 115.6(4) . . ?
N14 C15 N2 113.5(4) . . ?
N14 C15 C16 103.8(4) . . ?
N2 C15 C16 103.8(4) . . ?
N15 C16 N3 113.6(4) . . ?
N15 C16 C15 103.2(4) . . ?
N3 C16 C15 102.9(4) . . ?
N16 C17 N4 114.3(4) . . ?
N16 C17 C18 103.3(4) . . ?
N4 C17 C18 102.5(4) . . ?
N5 C18 N17 114.4(4) . . ?
N5 C18 C17 104.2(4) . . ?
N17 C18 C17 103.7(4) . . ?
N18 C19 N6 113.8(4) . . ?
N18 C19 C20 111.9(4) . . ?
N6 C19 C20 110.9(4) . . ?
N18 C19 C21 103.2(4) . . ?
N6 C19 C21 101.5(4) . . ?
C20 C19 C21 115.1(4) . . ?
N7 C21 N19 113.8(4) . . ?
N7 C21 C22 110.8(4) . . ?
N19 C21 C22 110.0(4) . . ?
N7 C21 C19 103.1(4) . . ?
N19 C21 C19 102.6(4) . . ?
C22 C21 C19 116.2(4) . . ?
N8 C23 N20 114.4(4) . . ?
N8 C23 C24 103.3(4) . . ?
N20 C23 C24 103.0(4) . . ?
N21 C24 N9 115.6(4) . . ?
N21 C24 C23 103.3(4) . . ?
N9 C24 C23 103.5(4) . . ?
N22 C25 N10 115.2(4) . . ?
N22 C25 C26 104.0(4) . . ?
N10 C25 C26 102.5(4) . . ?
N23 C26 N11 115.1(4) . . ?
N23 C26 C25 102.6(4) . . ?
N11 C26 C25 103.5(4) . . ?
N24 C27 N12 112.4(4) . . ?
N24 C27 C28 112.6(4) . . ?
N12 C27 C28 110.4(4) . . ?
N24 C27 C13 102.4(4) . . ?
N12 C27 C13 102.7(4) . . ?
C28 C27 C13 115.8(4) . . ?
O7 C29 N13 125.9(5) . . ?
O7 C29 N24 125.4(5) . . ?
N13 C29 N24 108.7(4) . . ?
N14 C30 N13 113.0(4) . . ?
O8 C31 N15 125.7(5) . . ?
O8 C31 N14 126.7(5) . . ?
N15 C31 N14 107.6(4) . . ?
N15 C32 N16 112.7(4) . . ?
O9 C33 N16 126.7(5) . . ?
O9 C33 N17 125.5(5) . . ?
N16 C33 N17 107.7(4) . . ?
N18 C34 N17 113.6(4) . . ?
O10 C35 N19 126.8(5) . . ?
O10 C35 N18 125.1(5) . . ?
N19 C35 N18 108.1(4) . . ?
N20 C36 N19 113.7(4) . . ?
O11 C37 N21 126.6(5) . . ?
O11 C37 N20 126.2(5) . . ?
N21 C37 N20 107.0(4) . . ?
N22 C38 N21 115.3(4) . . ?
O12 C39 N23 125.7(5) . . ?
O12 C39 N22 125.3(4) . . ?
N23 C39 N22 109.0(4) . . ?
N23 C40 N24 114.1(4) . . ?
O13 C41 N25 127.6(5) . . ?
O13 C41 N36 125.1(5) . 3_656 ?
N25 C41 N36 107.4(4) . 3_656 ?
N26 C42 N25 114.7(4) . . ?
O14 C43 N26 124.5(4) . . ?
O14 C43 N27 125.2(4) . . ?
N26 C43 N27 110.3(4) . . ?
N27 C44 N28 113.2(4) . . ?
O15 C45 N28 126.4(5) . . ?
O15 C45 N29 126.2(5) . . ?
N28 C45 N29 107.4(5) . . ?
N29 C46 N30 114.7(4) . . ?
O16 C47 N31 125.5(6) . 3_656 ?
O16 C47 N30 126.3(5) . . ?
N31 C47 N30 108.2(5) 3_656 . ?
N25 C48 N31 114.5(4) . . ?
N25 C48 C55 103.7(4) . 3_656 ?
N31 C48 C55 103.8(4) . 3_656 ?
N26 C49 N32 111.5(4) . . ?
N26 C49 C50 110.6(4) . . ?
N32 C49 C50 113.4(4) . . ?
N26 C49 C51 103.0(4) . . ?
N32 C49 C51 101.6(4) . . ?
C50 C49 C51 116.0(4) . . ?
N33 C51 N27 112.3(4) . . ?
N33 C51 C52 112.4(4) . . ?
N27 C51 C52 111.3(4) . . ?
N33 C51 C49 102.8(4) . . ?
N27 C51 C49 102.5(4) . . ?
C52 C51 C49 114.8(4) . . ?
N34 C53 N28 115.1(4) . . ?
N34 C53 C54 103.8(4) . . ?
N28 C53 C54 103.5(4) . . ?
N35 C54 N29 114.9(4) . . ?
N35 C54 C53 102.8(4) . . ?
N29 C54 C53 103.0(4) . . ?
N30 C55 N36 115.9(4) . . ?
N30 C55 C48 102.4(4) . 3_656 ?
N36 C55 C48 102.9(4) . 3_656 ?
N31 C56 N32 113.6(4) . . ?
O17 C57 N33 126.6(6) . . ?
O17 C57 N32 124.0(6) . . ?
N33 C57 N32 109.3(5) . . ?
N33 C58 N34 115.1(4) . . ?
O18 C59 N35 127.2(5) . . ?
O18 C59 N34 125.4(5) . . ?
N35 C59 N34 107.4(5) . . ?
N36 C60 N35 114.5(4) . . ?
C1 N1 C2 120.4(4) . . ?
C1 N1 C13 112.6(4) . . ?
C2 N1 C13 126.9(4) . . ?
C3 N2 C2 125.5(4) . . ?
C3 N2 C15 111.6(4) . . ?
C2 N2 C15 122.8(4) . . ?
C3 N3 C4 122.5(4) . . ?
C3 N3 C16 111.5(4) . . ?
C4 N3 C16 120.6(4) . . ?
C5 N4 C4 122.2(4) . . ?
C5 N4 C17 112.2(4) . . ?
C4 N4 C17 122.9(4) . . ?
C5 N5 C18 112.3(4) . . ?
C5 N5 C6 122.9(4) . . ?
C18 N5 C6 124.7(4) . . ?
C7 N6 C6 119.1(4) . . ?
C7 N6 C19 114.7(4) . . ?
C6 N6 C19 125.8(4) . . ?
C7 N7 C8 120.9(4) . . ?
C7 N7 C21 112.6(4) . . ?
C8 N7 C21 124.8(4) . . ?
C9 N8 C23 112.3(4) . . ?
C9 N8 C8 122.8(4) . . ?
C23 N8 C8 122.8(4) . . ?
C9 N9 C10 121.5(4) . . ?
C9 N9 C24 111.1(4) . . ?
C10 N9 C24 121.5(4) . . ?
C11 N10 C10 121.9(4) . . ?
C11 N10 C25 111.2(4) . . ?
C10 N10 C25 121.7(4) . . ?
C11 N11 C26 111.4(4) . . ?
C11 N11 C12 124.9(4) . . ?
C26 N11 C12 123.0(4) . . ?
C1 N12 C12 121.3(4) . . ?
C1 N12 C27 111.8(4) . . ?
C12 N12 C27 126.3(4) . . ?
C29 N13 C13 113.3(4) . . ?
C29 N13 C30 120.9(4) . . ?
C13 N13 C30 125.6(4) . . ?
C31 N14 C15 111.4(4) . . ?
C31 N14 C30 122.3(4) . . ?
C15 N14 C30 122.8(4) . . ?
C31 N15 C16 112.3(4) . . ?
C31 N15 C32 122.8(4) . . ?
C16 N15 C32 123.7(4) . . ?
C33 N16 C17 113.0(4) . . ?
C33 N16 C32 122.7(4) . . ?
C17 N16 C32 122.5(4) . . ?
C33 N17 C34 121.6(4) . . ?
C33 N17 C18 111.4(4) . . ?
C34 N17 C18 122.6(4) . . ?
C35 N18 C19 113.1(4) . . ?
C35 N18 C34 119.8(4) . . ?
C19 N18 C34 127.0(4) . . ?
C35 N19 C36 119.8(4) . . ?
C35 N19 C21 112.7(4) . . ?
C36 N19 C21 125.6(4) . . ?
C37 N20 C36 123.6(4) . . ?
C37 N20 C23 113.1(4) . . ?
C36 N20 C23 123.3(4) . . ?
C37 N21 C38 121.6(4) . . ?
C37 N21 C24 113.1(4) . . ?
C38 N21 C24 124.8(4) . . ?
C39 N22 C38 123.9(4) . . ?
C39 N22 C25 111.1(4) . . ?
C38 N22 C25 124.0(4) . . ?
C39 N23 C40 122.8(4) . . ?
C39 N23 C26 112.0(4) . . ?
C40 N23 C26 122.9(4) . . ?
C29 N24 C40 119.9(4) . . ?
C29 N24 C27 112.3(4) . . ?
C40 N24 C27 125.5(4) . . ?
C41 N25 C48 112.9(4) . . ?
C41 N25 C42 121.4(4) . . ?
C48 N25 C42 123.5(4) . . ?
C43 N26 C42 121.4(4) . . ?
C43 N26 C49 111.9(4) . . ?
C42 N26 C49 125.1(4) . . ?
C43 N27 C44 121.4(4) . . ?
C43 N27 C51 111.5(4) . . ?
C44 N27 C51 125.1(4) . . ?
C45 N28 C53 112.2(4) . . ?
C45 N28 C44 122.2(4) . . ?
C53 N28 C44 122.8(4) . . ?
C45 N29 C54 113.5(4) . . ?
C45 N29 C46 121.5(4) . . ?
C54 N29 C46 123.6(4) . . ?
C47 N30 C55 113.4(4) . . ?
C47 N30 C46 121.5(4) . . ?
C55 N30 C46 124.5(4) . . ?
C47 N31 C56 124.1(5) 3_656 . ?
C47 N31 C48 112.2(4) 3_656 . ?
C56 N31 C48 123.7(4) . . ?
C57 N32 C49 112.0(4) . . ?
C57 N32 C56 119.9(5) . . ?
C49 N32 C56 125.8(5) . . ?
C57 N33 C58 120.2(5) . . ?
C57 N33 C51 113.1(5) . . ?
C58 N33 C51 126.6(4) . . ?
C59 N34 C53 112.4(4) . . ?
C59 N34 C58 124.6(4) . . ?
C53 N34 C58 121.7(4) . . ?
C59 N35 C54 113.2(4) . . ?
C59 N35 C60 121.5(4) . . ?
C54 N35 C60 122.6(4) . . ?
C41 N36 C60 122.4(4) 3_656 . ?
C41 N36 C55 112.3(4) 3_656 . ?
C60 N36 C55 122.6(4) . . ?
O22 N38 O23 140.7(12) . . ?
O22 N38 O24 110.2(11) . . ?
O23 N38 O24 109.0(10) . . ?
C1 O1 Ce1 137.4(3) . . ?
C3 O2 Ce1 147.7(3) . . ?
C11 O6 Ce1 142.9(3) . . ?
C41 O13 Ce1 153.9(3) . . ?
C43 O14 Ce1 158.0(3) . . ?
O1 Ce1 O4W 136.34(12) . . ?
O1 Ce1 O6 77.49(11) . . ?
O4W Ce1 O6 75.06(12) . . ?
O1 Ce1 O14 143.36(10) . . ?
O4W Ce1 O14 70.84(11) . . ?
O6 Ce1 O14 139.15(10) . . ?
O1 Ce1 O2 76.56(11) . . ?
O4W Ce1 O2 146.12(11) . . ?
O6 Ce1 O2 130.60(10) . . ?
O14 Ce1 O2 76.08(10) . . ?
O1 Ce1 O13 81.95(10) . . ?
O4W Ce1 O13 93.37(13) . . ?
O6 Ce1 O13 133.91(11) . . ?
O14 Ce1 O13 70.63(10) . . ?
O2 Ce1 O13 82.27(10) . . ?
O1 Ce1 O1W 132.35(11) . . ?
O4W Ce1 O1W 76.96(13) . . ?
O6 Ce1 O1W 83.39(11) . . ?
O14 Ce1 O1W 67.70(11) . . ?
O2 Ce1 O1W 84.07(11) . . ?
O13 Ce1 O1W 138.13(11) . . ?
O1 Ce1 O3W 69.34(11) . . ?
O4W Ce1 O3W 69.22(12) . . ?
O6 Ce1 O3W 68.33(11) . . ?
O14 Ce1 O3W 117.40(10) . . ?
O2 Ce1 O3W 135.63(11) . . ?
O13 Ce1 O3W 65.88(11) . . ?
O1W Ce1 O3W 140.19(12) . . ?
O1 Ce1 O2W 68.86(11) . . ?
O4W Ce1 O2W 126.67(13) . . ?
O6 Ce1 O2W 66.55(11) . . ?
O14 Ce1 O2W 119.13(11) . . ?
O2 Ce1 O2W 65.08(10) . . ?
O13 Ce1 O2W 139.95(11) . . ?
O1W Ce1 O2W 63.49(12) . . ?
O3W Ce1 O2W 123.26(11) . . ?
O21 N37 O20 137.1(13) . . ?
O21 N37 O19 103.3(10) . . ?
O20 N37 O19 119.3(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N14 C15 C16 N15 -7.0(4) . . . . ?
N2 C15 C16 N15 -125.8(4) . . . . ?
N14 C15 C16 N3 111.4(4) . . . . ?
N2 C15 C16 N3 -7.4(4) . . . . ?
N16 C17 C18 N5 127.4(4) . . . . ?
N4 C17 C18 N5 8.3(5) . . . . ?
N16 C17 C18 N17 7.3(5) . . . . ?
N4 C17 C18 N17 -111.8(4) . . . . ?
N18 C19 C21 N7 121.9(4) . . . . ?
N6 C19 C21 N7 3.9(4) . . . . ?
C20 C19 C21 N7 -116.0(4) . . . . ?
N18 C19 C21 N19 3.5(5) . . . . ?
N6 C19 C21 N19 -114.6(4) . . . . ?
C20 C19 C21 N19 125.6(4) . . . . ?
N18 C19 C21 C22 -116.6(4) . . . . ?
N6 C19 C21 C22 125.3(4) . . . . ?
C20 C19 C21 C22 5.5(6) . . . . ?
N8 C23 C24 N21 -125.3(4) . . . . ?
N20 C23 C24 N21 -6.0(5) . . . . ?
N8 C23 C24 N9 -4.5(5) . . . . ?
N20 C23 C24 N9 114.9(4) . . . . ?
N22 C25 C26 N23 9.8(4) . . . . ?
N10 C25 C26 N23 -110.6(4) . . . . ?
N22 C25 C26 N11 129.9(4) . . . . ?
N10 C25 C26 N11 9.5(5) . . . . ?
N13 C13 C27 N24 -7.9(4) . . . . ?
N1 C13 C27 N24 110.0(4) . . . . ?
C14 C13 C27 N24 -131.4(4) . . . . ?
N13 C13 C27 N12 -124.6(4) . . . . ?
N1 C13 C27 N12 -6.7(4) . . . . ?
C14 C13 C27 N12 111.9(4) . . . . ?
N13 C13 C27 C28 115.0(4) . . . . ?
N1 C13 C27 C28 -127.1(4) . . . . ?
C14 C13 C27 C28 -8.5(6) . . . . ?
N26 C49 C51 N33 125.2(4) . . . . ?
N32 C49 C51 N33 9.6(4) . . . . ?
C50 C49 C51 N33 -113.9(5) . . . . ?
N26 C49 C51 N27 8.5(4) . . . . ?
N32 C49 C51 N27 -107.0(4) . . . . ?
C50 C49 C51 N27 129.4(4) . . . . ?
N26 C49 C51 C52 -112.4(4) . . . . ?
N32 C49 C51 C52 132.1(4) . . . . ?
C50 C49 C51 C52 8.6(6) . . . . ?
N34 C53 C54 N35 -4.2(5) . . . . ?
N28 C53 C54 N35 116.3(4) . . . . ?
N34 C53 C54 N29 -124.0(4) . . . . ?
N28 C53 C54 N29 -3.5(5) . . . . ?
O1 C1 N1 C2 -0.4(7) . . . . ?
N12 C1 N1 C2 -178.8(4) . . . . ?
O1 C1 N1 C13 176.2(4) . . . . ?
N12 C1 N1 C13 -2.2(5) . . . . ?
N2 C2 N1 C1 -96.9(5) . . . . ?
N2 C2 N1 C13 87.0(5) . . . . ?
N13 C13 N1 C1 115.6(4) . . . . ?
C14 C13 N1 C1 -117.2(5) . . . . ?
C27 C13 N1 C1 5.7(5) . . . . ?
N13 C13 N1 C2 -68.0(6) . . . . ?
C14 C13 N1 C2 59.1(6) . . . . ?
C27 C13 N1 C2 -177.9(4) . . . . ?
O2 C3 N2 C2 -4.4(7) . . . . ?
N3 C3 N2 C2 174.4(4) . . . . ?
O2 C3 N2 C15 179.0(4) . . . . ?
N3 C3 N2 C15 -2.2(5) . . . . ?
N1 C2 N2 C3 92.7(5) . . . . ?
N1 C2 N2 C15 -91.1(5) . . . . ?
N14 C15 N2 C3 -105.8(4) . . . . ?
C16 C15 N2 C3 6.2(5) . . . . ?
N14 C15 N2 C2 77.5(5) . . . . ?
C16 C15 N2 C2 -170.5(4) . . . . ?
O2 C3 N3 C4 21.4(7) . . . . ?
N2 C3 N3 C4 -157.4(4) . . . . ?
O2 C3 N3 C16 175.6(4) . . . . ?
N2 C3 N3 C16 -3.1(5) . . . . ?
N4 C4 N3 C3 -119.3(5) . . . . ?
N4 C4 N3 C16 88.8(5) . . . . ?
N15 C16 N3 C3 117.5(4) . . . . ?
C15 C16 N3 C3 6.7(5) . . . . ?
N15 C16 N3 C4 -87.7(5) . . . . ?
C15 C16 N3 C4 161.5(4) . . . . ?
O3 C5 N4 C4 -12.9(7) . . . . ?
N5 C5 N4 C4 166.9(4) . . . . ?
O3 C5 N4 C17 -174.9(5) . . . . ?
N5 C5 N4 C17 4.9(5) . . . . ?
N3 C4 N4 C5 119.5(5) . . . . ?
N3 C4 N4 C17 -80.5(6) . . . . ?
N16 C17 N4 C5 -119.4(4) . . . . ?
C18 C17 N4 C5 -8.3(5) . . . . ?
N16 C17 N4 C4 78.8(6) . . . . ?
C18 C17 N4 C4 -170.1(4) . . . . ?
O3 C5 N5 C18 -179.1(5) . . . . ?
N4 C5 N5 C18 1.1(5) . . . . ?
O3 C5 N5 C6 4.4(8) . . . . ?
N4 C5 N5 C6 -175.4(4) . . . . ?
N17 C18 N5 C5 106.4(5) . . . . ?
C17 C18 N5 C5 -6.1(5) . . . . ?
N17 C18 N5 C6 -77.2(5) . . . . ?
C17 C18 N5 C6 170.3(4) . . . . ?
N6 C6 N5 C5 -100.2(5) . . . . ?
N6 C6 N5 C18 83.7(6) . . . . ?
O4 C7 N6 C6 -2.3(7) . . . . ?
N7 C7 N6 C6 174.4(4) . . . . ?
O4 C7 N6 C19 -175.0(5) . . . . ?
N7 C7 N6 C19 1.6(5) . . . . ?
N5 C6 N6 C7 103.4(5) . . . . ?
N5 C6 N6 C19 -84.7(6) . . . . ?
N18 C19 N6 C7 -113.7(5) . . . . ?
C20 C19 N6 C7 119.2(5) . . . . ?
C21 C19 N6 C7 -3.6(5) . . . . ?
N18 C19 N6 C6 74.2(6) . . . . ?
C20 C19 N6 C6 -53.0(6) . . . . ?
C21 C19 N6 C6 -175.7(4) . . . . ?
O4 C7 N7 C8 -15.9(7) . . . . ?
N6 C7 N7 C8 167.4(4) . . . . ?
O4 C7 N7 C21 178.1(5) . . . . ?
N6 C7 N7 C21 1.3(5) . . . . ?
N8 C8 N7 C7 -87.0(5) . . . . ?
N8 C8 N7 C21 77.3(6) . . . . ?
N19 C21 N7 C7 106.9(5) . . . . ?
C22 C21 N7 C7 -128.4(4) . . . . ?
C19 C21 N7 C7 -3.4(5) . . . . ?
N19 C21 N7 C8 -58.4(6) . . . . ?
C22 C21 N7 C8 66.2(6) . . . . ?
C19 C21 N7 C8 -168.8(4) . . . . ?
O5 C9 N8 C23 -172.4(5) . . . . ?
N9 C9 N8 C23 7.4(5) . . . . ?
O5 C9 N8 C8 -8.6(8) . . . . ?
N9 C9 N8 C8 171.1(4) . . . . ?
N20 C23 N8 C9 -112.7(4) . . . . ?
C24 C23 N8 C9 -1.5(5) . . . . ?
N20 C23 N8 C8 83.6(5) . . . . ?
C24 C23 N8 C8 -165.2(4) . . . . ?
N7 C8 N8 C9 97.3(5) . . . . ?
N7 C8 N8 C23 -100.6(5) . . . . ?
O5 C9 N9 C10 15.9(7) . . . . ?
N8 C9 N9 C10 -163.8(4) . . . . ?
O5 C9 N9 C24 169.2(5) . . . . ?
N8 C9 N9 C24 -10.5(5) . . . . ?
N10 C10 N9 C9 -123.1(5) . . . . ?
N10 C10 N9 C24 86.4(5) . . . . ?
N21 C24 N9 C9 121.3(4) . . . . ?
C23 C24 N9 C9 9.2(5) . . . . ?
N21 C24 N9 C10 -85.4(5) . . . . ?
C23 C24 N9 C10 162.5(4) . . . . ?
O6 C11 N10 C10 -17.2(7) . . . . ?
N11 C11 N10 C10 161.8(4) . . . . ?
O6 C11 N10 C25 -171.9(4) . . . . ?
N11 C11 N10 C25 7.0(5) . . . . ?
N9 C10 N10 C11 125.0(5) . . . . ?
N9 C10 N10 C25 -82.9(5) . . . . ?
N22 C25 N10 C11 -122.5(4) . . . . ?
C26 C25 N10 C11 -10.3(5) . . . . ?
N22 C25 N10 C10 82.6(5) . . . . ?
C26 C25 N10 C10 -165.2(4) . . . . ?
O6 C11 N11 C26 178.9(4) . . . . ?
N10 C11 N11 C26 -0.1(5) . . . . ?
O6 C11 N11 C12 8.5(7) . . . . ?
N10 C11 N11 C12 -170.4(4) . . . . ?
N23 C26 N11 C11 104.9(5) . . . . ?
C25 C26 N11 C11 -6.2(5) . . . . ?
N23 C26 N11 C12 -84.5(5) . . . . ?
C25 C26 N11 C12 164.3(4) . . . . ?
N12 C12 N11 C11 -98.9(5) . . . . ?
N12 C12 N11 C26 91.9(5) . . . . ?
O1 C1 N12 C12 7.0(7) . . . . ?
N1 C1 N12 C12 -174.6(4) . . . . ?
O1 C1 N12 C27 178.7(4) . . . . ?
N1 C1 N12 C27 -2.8(5) . . . . ?
N11 C12 N12 C1 90.9(5) . . . . ?
N11 C12 N12 C27 -79.6(6) . . . . ?
N24 C27 N12 C1 -103.2(4) . . . . ?
C28 C27 N12 C1 130.2(4) . . . . ?
C13 C27 N12 C1 6.1(5) . . . . ?
N24 C27 N12 C12 68.1(5) . . . . ?
C28 C27 N12 C12 -58.6(6) . . . . ?
C13 C27 N12 C12 177.4(4) . . . . ?
O7 C29 N13 C13 179.7(5) . . . . ?
N24 C29 N13 C13 -1.5(5) . . . . ?
O7 C29 N13 C30 5.5(7) . . . . ?
N24 C29 N13 C30 -175.7(4) . . . . ?
N1 C13 N13 C29 -103.4(5) . . . . ?
C14 C13 N13 C29 131.4(4) . . . . ?
C27 C13 N13 C29 6.1(5) . . . . ?
N1 C13 N13 C30 70.4(6) . . . . ?
C14 C13 N13 C30 -54.7(6) . . . . ?
C27 C13 N13 C30 180.0(4) . . . . ?
N14 C30 N13 C29 82.2(5) . . . . ?
N14 C30 N13 C13 -91.2(5) . . . . ?
O8 C31 N14 C15 166.7(4) . . . . ?
N15 C31 N14 C15 -12.8(5) . . . . ?
O8 C31 N14 C30 7.4(7) . . . . ?
N15 C31 N14 C30 -172.2(4) . . . . ?
N2 C15 N14 C31 124.3(4) . . . . ?
C16 C15 N14 C31 12.3(5) . . . . ?
N2 C15 N14 C30 -76.5(5) . . . . ?
C16 C15 N14 C30 171.5(4) . . . . ?
N13 C30 N14 C31 -111.5(5) . . . . ?
N13 C30 N14 C15 91.4(5) . . . . ?
O8 C31 N15 C16 -171.7(4) . . . . ?
N14 C31 N15 C16 7.9(5) . . . . ?
O8 C31 N15 C32 -3.6(7) . . . . ?
N14 C31 N15 C32 176.0(4) . . . . ?
N3 C16 N15 C31 -110.9(4) . . . . ?
C15 C16 N15 C31 -0.3(5) . . . . ?
N3 C16 N15 C32 81.1(5) . . . . ?
C15 C16 N15 C32 -168.2(4) . . . . ?
N16 C32 N15 C31 113.0(5) . . . . ?
N16 C32 N15 C16 -80.3(6) . . . . ?
O9 C33 N16 C17 178.3(5) . . . . ?
N17 C33 N16 C17 -3.0(5) . . . . ?
O9 C33 N16 C32 13.3(7) . . . . ?
N17 C33 N16 C32 -168.0(4) . . . . ?
N4 C17 N16 C33 107.5(4) . . . . ?
C18 C17 N16 C33 -3.0(5) . . . . ?
N4 C17 N16 C32 -87.4(5) . . . . ?
C18 C17 N16 C32 162.0(4) . . . . ?
N15 C32 N16 C33 -108.9(5) . . . . ?
N15 C32 N16 C17 87.5(5) . . . . ?
O9 C33 N17 C34 -15.8(7) . . . . ?
N16 C33 N17 C34 165.4(4) . . . . ?
O9 C33 N17 C18 -173.0(4) . . . . ?
N16 C33 N17 C18 8.2(5) . . . . ?
N18 C34 N17 C33 117.7(5) . . . . ?
N18 C34 N17 C18 -87.7(5) . . . . ?
N5 C18 N17 C33 -122.6(4) . . . . ?
C17 C18 N17 C33 -9.8(5) . . . . ?
N5 C18 N17 C34 80.5(5) . . . . ?
C17 C18 N17 C34 -166.7(4) . . . . ?
O10 C35 N18 C19 172.9(5) . . . . ?
N19 C35 N18 C19 -4.7(5) . . . . ?
O10 C35 N18 C34 -3.8(7) . . . . ?
N19 C35 N18 C34 178.6(4) . . . . ?
N6 C19 N18 C35 109.6(4) . . . . ?
C20 C19 N18 C35 -123.7(5) . . . . ?
C21 C19 N18 C35 0.5(5) . . . . ?
N6 C19 N18 C34 -74.0(6) . . . . ?
C20 C19 N18 C34 52.7(6) . . . . ?
C21 C19 N18 C34 176.9(4) . . . . ?
N17 C34 N18 C35 -98.3(5) . . . . ?
N17 C34 N18 C19 85.5(6) . . . . ?
O10 C35 N19 C36 -5.3(7) . . . . ?
N18 C35 N19 C36 172.2(4) . . . . ?
O10 C35 N19 C21 -170.3(5) . . . . ?
N18 C35 N19 C21 7.2(5) . . . . ?
N20 C36 N19 C35 97.5(5) . . . . ?
N20 C36 N19 C21 -99.6(5) . . . . ?
N7 C21 N19 C35 -117.3(4) . . . . ?
C22 C21 N19 C35 117.6(5) . . . . ?
C19 C21 N19 C35 -6.6(5) . . . . ?
N7 C21 N19 C36 78.7(6) . . . . ?
C22 C21 N19 C36 -46.4(6) . . . . ?
C19 C21 N19 C36 -170.6(4) . . . . ?
O11 C37 N20 C36 -5.5(8) . . . . ?
N21 C37 N20 C36 178.0(4) . . . . ?
O11 C37 N20 C23 171.5(5) . . . . ?
N21 C37 N20 C23 -5.0(5) . . . . ?
N19 C36 N20 C37 -104.3(5) . . . . ?
N19 C36 N20 C23 79.1(6) . . . . ?
N8 C23 N20 C37 118.3(4) . . . . ?
C24 C23 N20 C37 7.0(5) . . . . ?
N8 C23 N20 C36 -64.7(6) . . . . ?
C24 C23 N20 C36 -176.1(4) . . . . ?
O11 C37 N21 C38 -3.9(7) . . . . ?
N20 C37 N21 C38 172.6(4) . . . . ?
O11 C37 N21 C24 -175.9(5) . . . . ?
N20 C37 N21 C24 0.6(5) . . . . ?
N22 C38 N21 C37 112.1(5) . . . . ?
N22 C38 N21 C24 -76.9(6) . . . . ?
N9 C24 N21 C37 -108.7(5) . . . . ?
C23 C24 N21 C37 3.6(5) . . . . ?
N9 C24 N21 C38 79.6(6) . . . . ?
C23 C24 N21 C38 -168.2(4) . . . . ?
O12 C39 N22 C38 8.8(7) . . . . ?
N23 C39 N22 C38 -171.1(4) . . . . ?
O12 C39 N22 C25 177.7(4) . . . . ?
N23 C39 N22 C25 -2.1(5) . . . . ?
N21 C38 N22 C39 -111.1(5) . . . . ?
N21 C38 N22 C25 81.4(6) . . . . ?
N10 C25 N22 C39 106.3(4) . . . . ?
C26 C25 N22 C39 -5.1(5) . . . . ?
N10 C25 N22 C38 -84.8(5) . . . . ?
C26 C25 N22 C38 163.8(4) . . . . ?
O12 C39 N23 C40 -7.4(7) . . . . ?
N22 C39 N23 C40 172.4(4) . . . . ?
O12 C39 N23 C26 -170.5(4) . . . . ?
N22 C39 N23 C26 9.3(5) . . . . ?
N24 C40 N23 C39 117.8(5) . . . . ?
N24 C40 N23 C26 -80.9(5) . . . . ?
N11 C26 N23 C39 -123.6(4) . . . . ?
C25 C26 N23 C39 -11.9(5) . . . . ?
N11 C26 N23 C40 73.3(6) . . . . ?
C25 C26 N23 C40 -175.0(4) . . . . ?
O7 C29 N24 C40 10.8(7) . . . . ?
N13 C29 N24 C40 -168.0(4) . . . . ?
O7 C29 N24 C27 174.4(5) . . . . ?
N13 C29 N24 C27 -4.4(5) . . . . ?
N23 C40 N24 C29 -105.0(5) . . . . ?
N23 C40 N24 C27 93.7(5) . . . . ?
N12 C27 N24 C29 117.3(4) . . . . ?
C28 C27 N24 C29 -117.2(5) . . . . ?
C13 C27 N24 C29 7.8(5) . . . . ?
N12 C27 N24 C40 -80.2(5) . . . . ?
C28 C27 N24 C40 45.3(6) . . . . ?
C13 C27 N24 C40 170.3(4) . . . . ?
O13 C41 N25 C48 -171.3(5) . . . . ?
N36 C41 N25 C48 9.1(5) 3_656 . . . ?
O13 C41 N25 C42 -7.7(8) . . . . ?
N36 C41 N25 C42 172.7(4) 3_656 . . . ?
N31 C48 N25 C41 -117.3(5) . . . . ?
C55 C48 N25 C41 -4.9(5) 3_656 . . . ?
N31 C48 N25 C42 79.5(6) . . . . ?
C55 C48 N25 C42 -168.2(4) 3_656 . . . ?
N26 C42 N25 C41 100.9(5) . . . . ?
N26 C42 N25 C48 -97.2(5) . . . . ?
O14 C43 N26 C42 -9.2(7) . . . . ?
N27 C43 N26 C42 170.0(4) . . . . ?
O14 C43 N26 C49 -175.0(4) . . . . ?
N27 C43 N26 C49 4.1(5) . . . . ?
N25 C42 N26 C43 -80.2(6) . . . . ?
N25 C42 N26 C49 83.7(5) . . . . ?
N32 C49 N26 C43 100.2(5) . . . . ?
C50 C49 N26 C43 -132.6(4) . . . . ?
C51 C49 N26 C43 -8.0(5) . . . . ?
N32 C49 N26 C42 -65.0(6) . . . . ?
C50 C49 N26 C42 62.2(6) . . . . ?
C51 C49 N26 C42 -173.2(4) . . . . ?
O14 C43 N27 C44 -13.8(7) . . . . ?
N26 C43 N27 C44 167.0(4) . . . . ?
O14 C43 N27 C51 -178.7(4) . . . . ?
N26 C43 N27 C51 2.2(5) . . . . ?
N28 C44 N27 C43 108.5(5) . . . . ?
N28 C44 N27 C51 -88.8(5) . . . . ?
N33 C51 N27 C43 -116.5(5) . . . . ?
C52 C51 N27 C43 116.4(5) . . . . ?
C49 C51 N27 C43 -6.8(5) . . . . ?
N33 C51 N27 C44 79.3(6) . . . . ?
C52 C51 N27 C44 -47.8(6) . . . . ?
C49 C51 N27 C44 -171.0(4) . . . . ?
O15 C45 N28 C53 172.5(5) . . . . ?
N29 C45 N28 C53 -5.9(5) . . . . ?
O15 C45 N28 C44 11.3(8) . . . . ?
N29 C45 N28 C44 -167.2(4) . . . . ?
N34 C53 N28 C45 118.4(5) . . . . ?
C54 C53 N28 C45 5.9(5) . . . . ?
N34 C53 N28 C44 -80.4(5) . . . . ?
C54 C53 N28 C44 167.0(4) . . . . ?
N27 C44 N28 C45 -116.1(5) . . . . ?
N27 C44 N28 C53 84.6(5) . . . . ?
O15 C45 N29 C54 -175.0(5) . . . . ?
N28 C45 N29 C54 3.4(6) . . . . ?
O15 C45 N29 C46 -8.4(8) . . . . ?
N28 C45 N29 C46 170.1(4) . . . . ?
N35 C54 N29 C45 -110.8(5) . . . . ?
C53 C54 N29 C45 0.2(5) . . . . ?
N35 C54 N29 C46 82.9(6) . . . . ?
C53 C54 N29 C46 -166.1(4) . . . . ?
N30 C46 N29 C45 111.3(5) . . . . ?
N30 C46 N29 C54 -83.4(6) . . . . ?
O16 C47 N30 C55 177.9(5) . . . . ?
N31 C47 N30 C55 0.4(6) 3_656 . . . ?
O16 C47 N30 C46 6.1(8) . . . . ?
N31 C47 N30 C46 -171.3(4) 3_656 . . . ?
N36 C55 N30 C47 109.8(5) . . . . ?
C48 C55 N30 C47 -1.3(5) 3_656 . . . ?
N36 C55 N30 C46 -78.7(6) . . . . ?
C48 C55 N30 C46 170.1(4) 3_656 . . . ?
N29 C46 N30 C47 -108.7(5) . . . . ?
N29 C46 N30 C55 80.5(6) . . . . ?
N32 C56 N31 C47 -99.7(6) . . . 3_656 ?
N32 C56 N31 C48 81.9(6) . . . . ?
N25 C48 N31 C47 114.0(5) . . . 3_656 ?
C55 C48 N31 C47 1.6(5) 3_656 . . 3_656 ?
N25 C48 N31 C56 -67.5(6) . . . . ?
C55 C48 N31 C56 -179.8(4) 3_656 . . . ?
O17 C57 N32 C49 -174.2(5) . . . . ?
N33 C57 N32 C49 7.3(6) . . . . ?
O17 C57 N32 C56 -10.7(8) . . . . ?
N33 C57 N32 C56 170.8(4) . . . . ?
N26 C49 N32 C57 -119.7(5) . . . . ?
C50 C49 N32 C57 114.7(5) . . . . ?
C51 C49 N32 C57 -10.6(5) . . . . ?
N26 C49 N32 C56 78.0(6) . . . . ?
C50 C49 N32 C56 -47.6(7) . . . . ?
C51 C49 N32 C56 -172.9(4) . . . . ?
N31 C56 N32 C57 101.7(6) . . . . ?
N31 C56 N32 C49 -97.2(6) . . . . ?
O17 C57 N33 C58 -0.1(8) . . . . ?
N32 C57 N33 C58 178.4(4) . . . . ?
O17 C57 N33 C51 -178.5(5) . . . . ?
N32 C57 N33 C51 0.0(6) . . . . ?
N34 C58 N33 C57 -94.1(6) . . . . ?
N34 C58 N33 C51 84.0(6) . . . . ?
N27 C51 N33 C57 103.1(5) . . . . ?
C52 C51 N33 C57 -130.4(5) . . . . ?
C49 C51 N33 C57 -6.4(5) . . . . ?
N27 C51 N33 C58 -75.2(6) . . . . ?
C52 C51 N33 C58 51.3(6) . . . . ?
C49 C51 N33 C58 175.3(4) . . . . ?
O18 C59 N34 C53 -176.2(5) . . . . ?
N35 C59 N34 C53 2.6(6) . . . . ?
O18 C59 N34 C58 -9.2(9) . . . . ?
N35 C59 N34 C58 169.6(5) . . . . ?
N28 C53 N34 C59 -111.2(5) . . . . ?
C54 C53 N34 C59 1.2(6) . . . . ?
N28 C53 N34 C58 81.4(6) . . . . ?
C54 C53 N34 C58 -166.2(4) . . . . ?
N33 C58 N34 C59 108.8(6) . . . . ?
N33 C58 N34 C53 -85.3(6) . . . . ?
O18 C59 N35 C54 173.0(5) . . . . ?
N34 C59 N35 C54 -5.7(6) . . . . ?
O18 C59 N35 C60 11.2(9) . . . . ?
N34 C59 N35 C60 -167.5(4) . . . . ?
N29 C54 N35 C59 117.4(5) . . . . ?
C53 C54 N35 C59 6.2(5) . . . . ?
N29 C54 N35 C60 -81.1(6) . . . . ?
C53 C54 N35 C60 167.7(4) . . . . ?
N36 C60 N35 C59 -116.0(5) . . . . ?
N36 C60 N35 C54 84.0(6) . . . . ?
N35 C60 N36 C41 115.5(5) . . . 3_656 ?
N35 C60 N36 C55 -84.7(6) . . . . ?
N30 C55 N36 C41 -117.4(5) . . . 3_656 ?
C48 C55 N36 C41 -6.5(5) 3_656 . . 3_656 ?
N30 C55 N36 C60 81.0(6) . . . . ?
C48 C55 N36 C60 -168.1(4) 3_656 . . . ?
N1 C1 O1 Ce1 90.0(6) . . . . ?
N12 C1 O1 Ce1 -91.8(6) . . . . ?
N3 C3 O2 Ce1 114.5(6) . . . . ?
N2 C3 O2 Ce1 -67.0(8) . . . . ?
N10 C11 O6 Ce1 -110.0(5) . . . . ?
N11 C11 O6 Ce1 71.2(7) . . . . ?
N25 C41 O13 Ce1 -10.8(11) . . . . ?
N36 C41 O13 Ce1 168.7(4) 3_656 . . . ?
N26 C43 O14 Ce1 -15.6(11) . . . . ?
N27 C43 O14 Ce1 165.4(5) . . . . ?

_refine_diff_density_max         0.898
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.092

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1038166'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_2                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_2                   
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Ce N27 O33'
_chemical_formula_weight         1571.14

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.322(2)
_cell_length_b                   32.346(6)
_cell_length_c                   15.145(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.505(2)
_cell_angle_gamma                90
_cell_volume                     6030.7(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6980
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      21.54

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_F_000             3180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.875
_shelx_estimated_absorpt_T_min   0.838
_shelx_estimated_absorpt_T_max   0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41193
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.770
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             10852
_reflns_number_gt                7795
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0705P)²+7.4580P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10852
_refine_ls_number_parameters     913
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1398
_refine_ls_wR_factor_gt          0.1241
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.029
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O8W O 0.7028(3) 1.01530(16) 0.2867(3) 0.0789(15) Uani 1 1 d . . . . .
C1 C 0.9628(4) 0.77325(14) 0.5791(3) 0.0282(11) Uani 1 1 d . . . . .
C2 C 0.9256(4) 0.80399(14) 0.4339(3) 0.0279(10) Uani 1 1 d . . . . .
H2A H 0.9078 0.7917 0.3767 0.033 Uiso 1 1 calc R U . . .
H2B H 1.0027 0.8102 0.4365 0.033 Uiso 1 1 calc R U . . .
C3 C 0.9121(4) 0.87815(15) 0.4689(3) 0.0281(11) Uani 1 1 d . . . . .
C4 C 0.8691(4) 0.95247(14) 0.4576(3) 0.0307(11) Uani 1 1 d . . . . .
H4A H 0.8501 0.9653 0.4010 0.037 Uiso 1 1 calc R U . . .
H4B H 0.9472 0.9547 0.4675 0.037 Uiso 1 1 calc R U . . .
C5 C 0.8748(4) 0.99082(15) 0.5975(3) 0.0310(11) Uani 1 1 d . . . . .
C6 C 0.8479(4) 1.03978(15) 0.7182(3) 0.0309(11) Uani 1 1 d . . . . .
H6A H 0.8173 1.0674 0.7145 0.037 Uiso 1 1 calc R U . . .
H6B H 0.9262 1.0424 0.7171 0.037 Uiso 1 1 calc R U . . .
C7 C 0.8891(4) 0.99524(15) 0.8464(3) 0.0320(11) Uani 1 1 d . . . . .
C8 C 0.9064(4) 0.95931(14) 0.9877(3) 0.0312(11) Uani 1 1 d . . . . .
H8A H 0.8953 0.9705 1.0460 0.037 Uiso 1 1 calc R U . . .
H8B H 0.9830 0.9620 0.9764 0.037 Uiso 1 1 calc R U . . .
C9 C 0.9508(4) 0.88571(15) 0.9667(3) 0.0338(12) Uani 1 1 d . . . . .
C10 C 0.9658(4) 0.81055(15) 0.9881(3) 0.0323(11) Uani 1 1 d . . . . .
H10A H 0.9586 0.7969 1.0445 0.039 Uiso 1 1 calc R U . . .
H10B H 1.0422 0.8165 0.9817 0.039 Uiso 1 1 calc R U . . .
C11 C 0.9812(4) 0.77937(15) 0.8414(3) 0.0306(11) Uani 1 1 d . . . . .
C12 C 0.9828(4) 0.73218(15) 0.7146(3) 0.0294(11) Uani 1 1 d . . . . .
H12A H 0.9861 0.7023 0.7201 0.035 Uiso 1 1 calc R U . . .
H12B H 1.0568 0.7423 0.7136 0.035 Uiso 1 1 calc R U . . .
C13 C 0.8151(4) 0.74411(14) 0.4987(3) 0.0268(10) Uani 1 1 d . . . . .
C14 C 0.8186(4) 0.71794(16) 0.4161(3) 0.0396(13) Uani 1 1 d . . . . .
H14A H 0.7619 0.6976 0.4164 0.059 Uiso 1 1 calc R U . . .
H14B H 0.8877 0.7044 0.4146 0.059 Uiso 1 1 calc R U . . .
H14C H 0.8083 0.7353 0.3650 0.059 Uiso 1 1 calc R U . . .
C15 C 0.7602(4) 0.84825(14) 0.3990(3) 0.0291(11) Uani 1 1 d . . . . .
H15 H 0.7580 0.8393 0.3372 0.035 Uiso 1 1 calc R U . . .
C16 C 0.7407(4) 0.89524(14) 0.4072(3) 0.0269(10) Uani 1 1 d . . . . .
H16 H 0.7294 0.9085 0.3493 0.032 Uiso 1 1 calc R U . . .
C17 C 0.7097(4) 0.99321(14) 0.5164(3) 0.0291(11) Uani 1 1 d . . . . .
H17 H 0.7006 1.0090 0.4614 0.035 Uiso 1 1 calc R U . . .
C18 C 0.7046(4) 1.02153(14) 0.5988(3) 0.0281(11) Uani 1 1 d . . . . .
H18 H 0.6909 1.0504 0.5820 0.034 Uiso 1 1 calc R U . . .
C19 C 0.7225(4) 1.02977(14) 0.8495(3) 0.0289(11) Uani 1 1 d . . . . .
C20 C 0.7097(5) 1.07604(16) 0.8645(4) 0.0450(14) Uani 1 1 d . . . . .
H20A H 0.7730 1.0865 0.8963 0.067 Uiso 1 1 calc R U . . .
H20B H 0.6468 1.0809 0.8982 0.067 Uiso 1 1 calc R U . . .
H20C H 0.7013 1.0899 0.8086 0.067 Uiso 1 1 calc R U . . .
C21 C 0.7390(4) 1.00250(15) 0.9358(3) 0.0306(11) Uani 1 1 d . . . . .
C22 C 0.7385(5) 1.02594(18) 1.0222(4) 0.0477(14) Uani 1 1 d . . . . .
H22A H 0.7491 1.0070 1.0705 0.072 Uiso 1 1 calc R U . . .
H22B H 0.6700 1.0398 1.0268 0.072 Uiso 1 1 calc R U . . .
H22C H 0.7960 1.0460 1.0241 0.072 Uiso 1 1 calc R U . . .
C23 C 0.7865(4) 0.90003(14) 1.0329(3) 0.0281(11) Uani 1 1 d . . . . .
H23 H 0.7843 0.9111 1.0930 0.034 Uiso 1 1 calc R U . . .
C24 C 0.8068(4) 0.85291(14) 1.0332(3) 0.0279(11) Uani 1 1 d . . . . .
H24 H 0.8135 0.8419 1.0935 0.033 Uiso 1 1 calc R U . . .
C25 C 0.8424(4) 0.75298(15) 0.9242(3) 0.0283(10) Uani 1 1 d . . . . .
H25 H 0.8534 0.7351 0.9761 0.034 Uiso 1 1 calc R U . . .
C26 C 0.8481(4) 0.72804(14) 0.8364(3) 0.0278(11) Uani 1 1 d . . . . .
H26 H 0.8654 0.6989 0.8474 0.033 Uiso 1 1 calc R U . . .
C27 C 0.8342(4) 0.72045(14) 0.5901(3) 0.0278(10) Uani 1 1 d . . . . .
C28 C 0.8573(4) 0.67468(15) 0.5823(4) 0.0409(13) Uani 1 1 d . . . . .
H28A H 0.8701 0.6631 0.6403 0.061 Uiso 1 1 calc R U . . .
H28B H 0.9204 0.6707 0.5483 0.061 Uiso 1 1 calc R U . . .
H28C H 0.7960 0.6612 0.5535 0.061 Uiso 1 1 calc R U . . .
C29 C 0.6635(4) 0.75228(14) 0.5858(3) 0.0290(11) Uani 1 1 d . . . . .
C30 C 0.6478(4) 0.78713(14) 0.4430(3) 0.0313(11) Uani 1 1 d . . . . .
H30A H 0.6631 0.7769 0.3846 0.038 Uiso 1 1 calc R U . . .
H30B H 0.5708 0.7833 0.4512 0.038 Uiso 1 1 calc R U . . .
C31 C 0.6008(4) 0.86008(15) 0.4751(3) 0.0321(11) Uani 1 1 d . . . . .
C32 C 0.5828(4) 0.93569(15) 0.4614(3) 0.0341(12) Uani 1 1 d . . . . .
H32A H 0.5080 0.9286 0.4721 0.041 Uiso 1 1 calc R U . . .
H32B H 0.5838 0.9488 0.4038 0.041 Uiso 1 1 calc R U . . .
C33 C 0.5658(4) 0.97281(15) 0.6023(3) 0.0330(12) Uani 1 1 d . . . . .
C34 C 0.5742(4) 1.02495(15) 0.7231(3) 0.0329(11) Uani 1 1 d . . . . .
H34A H 0.4968 1.0196 0.7246 0.040 Uiso 1 1 calc R U . . .
H34B H 0.5839 1.0546 0.7168 0.040 Uiso 1 1 calc R U . . .
C35 C 0.5832(4) 0.98062(15) 0.8540(3) 0.0339(12) Uani 1 1 d . . . . .
C36 C 0.6211(4) 0.94223(15) 0.9916(3) 0.0343(12) Uani 1 1 d . . . . .
H36A H 0.6329 0.9537 1.0505 0.041 Uiso 1 1 calc R U . . .
H36B H 0.5446 0.9356 0.9837 0.041 Uiso 1 1 calc R U . . .
C37 C 0.6372(4) 0.86709(15) 0.9663(3) 0.0311(11) Uani 1 1 d . . . . .
C38 C 0.6838(4) 0.79365(15) 0.9863(3) 0.0322(11) Uani 1 1 d . . . . .
H38A H 0.6055 0.7910 0.9791 0.039 Uiso 1 1 calc R U . . .
H38B H 0.7059 0.7821 1.0434 0.039 Uiso 1 1 calc R U . . .
C39 C 0.6738(4) 0.75554(14) 0.8463(3) 0.0296(11) Uani 1 1 d . . . . .
C40 C 0.7032(4) 0.71013(15) 0.7177(3) 0.0329(11) Uani 1 1 d . . . . .
H40A H 0.6246 0.7083 0.7178 0.039 Uiso 1 1 calc R U . . .
H40B H 0.7317 0.6822 0.7219 0.039 Uiso 1 1 calc R U . . .
N1 N 0.9036(3) 0.77439(11) 0.5020(2) 0.0264(9) Uani 1 1 d . . . . .
N2 N 0.8658(3) 0.84211(12) 0.4413(3) 0.0285(9) Uani 1 1 d . . . . .
N3 N 0.8402(3) 0.90941(11) 0.4531(3) 0.0278(9) Uani 1 1 d . . . . .
N4 N 0.8167(3) 0.97498(12) 0.5262(3) 0.0297(9) Uani 1 1 d . . . . .
N5 N 0.8100(3) 1.01667(12) 0.6423(3) 0.0295(9) Uani 1 1 d . . . . .
N6 N 0.8201(3) 1.02142(12) 0.8022(3) 0.0305(9) Uani 1 1 d . . . . .
N7 N 0.8445(3) 0.98350(12) 0.9233(3) 0.0303(9) Uani 1 1 d . . . . .
N8 N 0.8782(3) 0.91587(12) 0.9872(3) 0.0324(9) Uani 1 1 d . . . . .
N9 N 0.9066(3) 0.84871(12) 0.9883(3) 0.0297(9) Uani 1 1 d . . . . .
N10 N 0.9290(3) 0.78269(12) 0.9178(3) 0.0295(9) Uani 1 1 d . . . . .
N11 N 0.9333(3) 0.74872(12) 0.7911(2) 0.0287(9) Uani 1 1 d . . . . .
N12 N 0.9271(3) 0.74237(11) 0.6306(2) 0.0273(9) Uani 1 1 d . . . . .
N13 N 0.7086(3) 0.76284(12) 0.5082(3) 0.0289(9) Uani 1 1 d . . . . .
N14 N 0.6720(3) 0.83055(12) 0.4468(3) 0.0308(9) Uani 1 1 d . . . . .
N15 N 0.6458(3) 0.89822(12) 0.4595(3) 0.0306(9) Uani 1 1 d . . . . .
N16 N 0.6205(3) 0.96504(12) 0.5275(3) 0.0322(9) Uani 1 1 d . . . . .
N17 N 0.6158(3) 1.00462(12) 0.6464(3) 0.0317(9) Uani 1 1 d . . . . .
N18 N 0.6257(3) 1.01193(12) 0.8066(3) 0.0311(9) Uani 1 1 d . . . . .
N19 N 0.6485(3) 0.97352(12) 0.9270(3) 0.0339(10) Uani 1 1 d . . . . .
N20 N 0.6836(3) 0.90449(12) 0.9854(3) 0.0308(9) Uani 1 1 d . . . . .
N21 N 0.7119(3) 0.83691(12) 0.9854(3) 0.0284(9) Uani 1 1 d . . . . .
N22 N 0.7335(3) 0.77000(12) 0.9180(3) 0.0310(9) Uani 1 1 d . . . . .
N23 N 0.7413(3) 0.73305(12) 0.7952(2) 0.0290(9) Uani 1 1 d . . . . .
N24 N 0.7338(3) 0.72810(12) 0.6337(3) 0.0297(9) Uani 1 1 d . . . . .
N25 N 0.9622(4) 0.86474(17) 0.2177(3) 0.0478(12) Uani 1 1 d . . . . .
N26 N 0.5843(4) 0.87870(15) 0.2115(3) 0.0396(11) Uani 1 1 d . . . . .
N27 N 1.2336(4) 0.86318(13) 0.4291(3) 0.0402(11) Uani 1 1 d . . . . .
O1 O 1.0408(3) 0.79597(10) 0.5978(2) 0.0366(8) Uani 1 1 d . . . . .
O2 O 1.0040(3) 0.88234(10) 0.5026(2) 0.0351(8) Uani 1 1 d . . . . .
O1W O 0.9785(4) 0.87740(18) 0.6959(3) 0.0775(14) Uani 1 1 d . . . . .
O3 O 0.9701(3) 0.98369(11) 0.6167(2) 0.0377(8) Uani 1 1 d . . . . .
O2W O 1.1481(3) 0.93642(11) 0.6301(3) 0.0466(10) Uani 1 1 d . . . . .
O4 O 0.9785(3) 0.98430(11) 0.8236(2) 0.0435(9) Uani 1 1 d . . . . .
O3W O 1.3440(3) 0.88275(12) 0.6427(3) 0.0511(10) Uani 1 1 d . . . . .
O5 O 1.0388(3) 0.89104(11) 0.9347(3) 0.0483(10) Uani 1 1 d . . . . .
O4W O 1.2664(3) 0.79863(12) 0.6551(3) 0.0577(11) Uani 1 1 d . . . . .
O6 O 1.0611(3) 0.79902(11) 0.8216(2) 0.0407(9) Uani 1 1 d . . . . .
O5W O 1.1849(3) 0.86889(15) 0.7784(3) 0.0655(13) Uani 1 1 d . . . . .
O7 O 0.5724(3) 0.76211(11) 0.6067(2) 0.0375(8) Uani 1 1 d . . . . .
O6W O 0.8480(3) 0.96589(13) 0.2135(3) 0.0533(10) Uani 1 1 d . . . . .
O8 O 0.5149(3) 0.85362(11) 0.5090(3) 0.0464(10) Uani 1 1 d . . . . .
O7W O 0.7539(3) 0.78417(12) 0.2166(2) 0.0493(10) Uani 1 1 d . . . . .
O9 O 0.4841(3) 0.95515(11) 0.6239(3) 0.0473(10) Uani 1 1 d . . . . .
O10 O 0.4979(3) 0.96279(12) 0.8343(3) 0.0497(10) Uani 1 1 d . . . . .
O9W O 0.4755(3) 0.81549(13) 0.7154(3) 0.0602(11) Uani 1 1 d . . . . .
O11 O 0.5449(3) 0.86074(11) 0.9362(3) 0.0467(10) Uani 1 1 d . . . . .
O10W O 0.6181(5) 0.8870(2) 0.7298(5) 0.117(2) Uani 1 1 d . . . . .
O12 O 0.5775(3) 0.76140(11) 0.8312(2) 0.0385(9) Uani 1 1 d . . . . .
O11W O 0.3702(4) 0.89423(15) 0.8504(5) 0.105(2) Uani 1 1 d . U . . .
O13 O 0.6265(4) 0.85147(13) 0.1657(3) 0.0652(13) Uani 1 1 d . . . . .
O14 O 0.5981(5) 0.91547(14) 0.1949(3) 0.0874(17) Uani 1 1 d . . . . .
O15 O 0.5314(4) 0.86849(14) 0.2748(3) 0.0691(13) Uani 1 1 d . . . . .
O16 O 1.0308(5) 0.88213(18) 0.1764(4) 0.0952(18) Uani 1 1 d . . . . .
O17 O 0.9547(3) 0.82595(14) 0.2165(3) 0.0597(11) Uani 1 1 d . . . . .
O18 O 0.8950(5) 0.88523(16) 0.2555(4) 0.098(2) Uani 1 1 d . . . . .
O19 O 1.2296(3) 0.89423(11) 0.4786(3) 0.0487(10) Uani 1 1 d . . . . .
O20 O 1.2065(3) 0.82911(11) 0.4624(2) 0.0443(9) Uani 1 1 d . . . . .
O21 O 1.2638(4) 0.86633(12) 0.3536(3) 0.0643(13) Uani 1 1 d . . . . .
Ce01 Ce 1.14852(2) 0.86043(2) 0.61515(2) 0.03109(11) Uani 1 1 d . . . . .
O12A O 0.7867(14) 0.8401(6) 0.6746(13) 0.206(6) Uiso 0.631(13) 1 d . U P A 1
O12B O 0.809(3) 0.8499(9) 0.770(2) 0.206(6) Uiso 0.369(13) 1 d . U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.233(5) . ?
C1 N1 1.350(6) . ?
C1 N12 1.353(6) . ?
C2 N1 1.442(6) . ?
C2 N2 1.444(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O2 1.229(5) . ?
C3 N2 1.356(6) . ?
C3 N3 1.359(6) . ?
C4 N3 1.438(6) . ?
C4 N4 1.444(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O3 1.220(5) . ?
C5 N5 1.358(6) . ?
C5 N4 1.369(6) . ?
C6 N5 1.432(6) . ?
C6 N6 1.457(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O4 1.221(6) . ?
C7 N6 1.356(6) . ?
C7 N7 1.363(6) . ?
C8 N7 1.442(6) . ?
C8 N8 1.447(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O5 1.220(6) . ?
C9 N9 1.360(6) . ?
C9 N8 1.368(6) . ?
C10 N9 1.434(6) . ?
C10 N10 1.453(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O6 1.220(6) . ?
C11 N10 1.352(6) . ?
C11 N11 1.368(6) . ?
C12 N11 1.436(6) . ?
C12 N12 1.456(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N13 1.458(6) . ?
C13 N1 1.465(6) . ?
C13 C14 1.512(6) . ?
C13 C27 1.590(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N2 1.439(6) . ?
C15 N14 1.450(6) . ?
C15 C16 1.545(7) . ?
C15 H15 0.9800 . ?
C16 N15 1.444(6) . ?
C16 N3 1.457(6) . ?
C16 H16 0.9800 . ?
C17 N16 1.443(6) . ?
C17 N4 1.446(6) . ?
C17 C18 1.551(7) . ?
C17 H17 0.9800 . ?
C18 N5 1.439(6) . ?
C18 N17 1.444(6) . ?
C18 H18 0.9800 . ?
C19 N6 1.452(6) . ?
C19 N18 1.453(6) . ?
C19 C20 1.523(7) . ?
C19 C21 1.583(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 N19 1.458(6) . ?
C21 N7 1.459(6) . ?
C21 C22 1.512(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 N20 1.437(6) . ?
C23 N8 1.444(6) . ?
C23 C24 1.544(6) . ?
C23 H23 0.9800 . ?
C24 N9 1.438(6) . ?
C24 N21 1.445(6) . ?
C24 H24 0.9800 . ?
C25 N10 1.442(6) . ?
C25 N22 1.450(6) . ?
C25 C26 1.560(7) . ?
C25 H25 0.9800 . ?
C26 N23 1.441(6) . ?
C26 N11 1.443(6) . ?
C26 H26 0.9800 . ?
C27 N24 1.449(6) . ?
C27 N12 1.459(6) . ?
C27 C28 1.513(7) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 O7 1.222(6) . ?
C29 N24 1.354(6) . ?
C29 N13 1.365(6) . ?
C30 N14 1.436(6) . ?
C30 N13 1.446(6) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 O8 1.214(6) . ?
C31 N14 1.378(6) . ?
C31 N15 1.378(6) . ?
C32 N15 1.441(6) . ?
C32 N16 1.442(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 O9 1.214(6) . ?
C33 N17 1.360(6) . ?
C33 N16 1.366(7) . ?
C34 N17 1.448(6) . ?
C34 N18 1.452(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 O10 1.225(6) . ?
C35 N19 1.358(6) . ?
C35 N18 1.359(6) . ?
C36 N20 1.449(6) . ?
C36 N19 1.458(6) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 O11 1.225(6) . ?
C37 N21 1.364(6) . ?
C37 N20 1.364(6) . ?
C38 N21 1.441(6) . ?
C38 N22 1.443(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 O12 1.213(5) . ?
C39 N22 1.368(6) . ?
C39 N23 1.369(6) . ?
C40 N23 1.449(6) . ?
C40 N24 1.463(6) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
N25 O16 1.212(6) . ?
N25 O18 1.223(6) . ?
N25 O17 1.258(6) . ?
N26 O15 1.227(6) . ?
N26 O14 1.229(6) . ?
N26 O13 1.249(6) . ?
N27 O21 1.221(6) . ?
N27 O19 1.255(5) . ?
N27 O20 1.263(5) . ?
O1 Ce01 2.480(3) . ?
O2 Ce01 2.513(3) . ?
O1W Ce01 2.532(4) . ?
O2W Ce01 2.468(4) . ?
O3W Ce01 2.532(3) . ?
O4W Ce01 2.529(4) . ?
O5W Ce01 2.508(4) . ?
O19 Ce01 2.579(4) . ?
O20 Ce01 2.652(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 124.7(4) . . ?
O1 C1 N12 125.3(4) . . ?
N1 C1 N12 110.0(4) . . ?
N1 C2 N2 113.5(4) . . ?
N1 C2 H2A 108.9 . . ?
N2 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
N2 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
O2 C3 N2 126.2(4) . . ?
O2 C3 N3 124.9(4) . . ?
N2 C3 N3 108.9(4) . . ?
N3 C4 N4 113.9(4) . . ?
N3 C4 H4A 108.8 . . ?
N4 C4 H4A 108.8 . . ?
N3 C4 H4B 108.8 . . ?
N4 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
O3 C5 N5 125.3(5) . . ?
O3 C5 N4 125.6(5) . . ?
N5 C5 N4 109.0(4) . . ?
N5 C6 N6 114.0(4) . . ?
N5 C6 H6A 108.7 . . ?
N6 C6 H6A 108.7 . . ?
N5 C6 H6B 108.7 . . ?
N6 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O4 C7 N6 126.5(5) . . ?
O4 C7 N7 124.3(5) . . ?
N6 C7 N7 109.2(4) . . ?
N7 C8 N8 113.8(4) . . ?
N7 C8 H8A 108.8 . . ?
N8 C8 H8A 108.8 . . ?
N7 C8 H8B 108.8 . . ?
N8 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O5 C9 N9 126.3(5) . . ?
O5 C9 N8 126.2(5) . . ?
N9 C9 N8 107.5(4) . . ?
N9 C10 N10 113.1(4) . . ?
N9 C10 H10A 109.0 . . ?
N10 C10 H10A 109.0 . . ?
N9 C10 H10B 109.0 . . ?
N10 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O6 C11 N10 126.1(5) . . ?
O6 C11 N11 124.9(5) . . ?
N10 C11 N11 108.9(4) . . ?
N11 C12 N12 114.9(4) . . ?
N11 C12 H12A 108.5 . . ?
N12 C12 H12A 108.5 . . ?
N11 C12 H12B 108.5 . . ?
N12 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
N13 C13 N1 113.0(4) . . ?
N13 C13 C14 111.9(4) . . ?
N1 C13 C14 110.8(4) . . ?
N13 C13 C27 102.3(4) . . ?
N1 C13 C27 102.1(3) . . ?
C14 C13 C27 116.2(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 N14 114.0(4) . . ?
N2 C15 C16 103.9(4) . . ?
N14 C15 C16 103.1(4) . . ?
N2 C15 H15 111.8 . . ?
N14 C15 H15 111.8 . . ?
C16 C15 H15 111.8 . . ?
N15 C16 N3 113.7(4) . . ?
N15 C16 C15 104.0(4) . . ?
N3 C16 C15 102.6(3) . . ?
N15 C16 H16 112.0 . . ?
N3 C16 H16 112.0 . . ?
C15 C16 H16 112.0 . . ?
N16 C17 N4 115.2(4) . . ?
N16 C17 C18 102.8(4) . . ?
N4 C17 C18 103.1(4) . . ?
N16 C17 H17 111.7 . . ?
N4 C17 H17 111.7 . . ?
C18 C17 H17 111.7 . . ?
N5 C18 N17 114.7(4) . . ?
N5 C18 C17 103.7(4) . . ?
N17 C18 C17 103.7(4) . . ?
N5 C18 H18 111.4 . . ?
N17 C18 H18 111.4 . . ?
C17 C18 H18 111.4 . . ?
N6 C19 N18 112.8(4) . . ?
N6 C19 C20 110.5(4) . . ?
N18 C19 C20 111.6(4) . . ?
N6 C19 C21 103.0(3) . . ?
N18 C19 C21 102.8(4) . . ?
C20 C19 C21 115.7(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N19 C21 N7 113.6(4) . . ?
N19 C21 C22 111.7(4) . . ?
N7 C21 C22 111.2(4) . . ?
N19 C21 C19 102.3(4) . . ?
N7 C21 C19 102.1(4) . . ?
C22 C21 C19 115.5(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N20 C23 N8 114.6(4) . . ?
N20 C23 C24 103.9(4) . . ?
N8 C23 C24 102.8(4) . . ?
N20 C23 H23 111.7 . . ?
N8 C23 H23 111.7 . . ?
C24 C23 H23 111.7 . . ?
N9 C24 N21 114.8(4) . . ?
N9 C24 C23 103.5(4) . . ?
N21 C24 C23 102.9(3) . . ?
N9 C24 H24 111.6 . . ?
N21 C24 H24 111.6 . . ?
C23 C24 H24 111.6 . . ?
N10 C25 N22 115.3(4) . . ?
N10 C25 C26 103.0(4) . . ?
N22 C25 C26 102.6(4) . . ?
N10 C25 H25 111.7 . . ?
N22 C25 H25 111.7 . . ?
C26 C25 H25 111.7 . . ?
N23 C26 N11 114.4(4) . . ?
N23 C26 C25 103.7(4) . . ?
N11 C26 C25 103.1(4) . . ?
N23 C26 H26 111.7 . . ?
N11 C26 H26 111.7 . . ?
C25 C26 H26 111.7 . . ?
N24 C27 N12 113.3(4) . . ?
N24 C27 C28 111.7(4) . . ?
N12 C27 C28 111.2(4) . . ?
N24 C27 C13 102.6(4) . . ?
N12 C27 C13 102.5(3) . . ?
C28 C27 C13 115.1(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O7 C29 N24 125.8(5) . . ?
O7 C29 N13 124.8(4) . . ?
N24 C29 N13 109.3(4) . . ?
N14 C30 N13 113.7(4) . . ?
N14 C30 H30A 108.8 . . ?
N13 C30 H30A 108.8 . . ?
N14 C30 H30B 108.8 . . ?
N13 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
O8 C31 N14 126.2(5) . . ?
O8 C31 N15 126.3(5) . . ?
N14 C31 N15 107.5(4) . . ?
N15 C32 N16 114.2(4) . . ?
N15 C32 H32A 108.7 . . ?
N16 C32 H32A 108.7 . . ?
N15 C32 H32B 108.7 . . ?
N16 C32 H32B 108.7 . . ?
H32A C32 H32B 107.6 . . ?
O9 C33 N17 125.9(5) . . ?
O9 C33 N16 125.6(5) . . ?
N17 C33 N16 108.5(4) . . ?
N17 C34 N18 114.2(4) . . ?
N17 C34 H34A 108.7 . . ?
N18 C34 H34A 108.7 . . ?
N17 C34 H34B 108.7 . . ?
N18 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
O10 C35 N19 126.2(5) . . ?
O10 C35 N18 124.7(5) . . ?
N19 C35 N18 109.1(4) . . ?
N20 C36 N19 113.7(4) . . ?
N20 C36 H36A 108.8 . . ?
N19 C36 H36A 108.8 . . ?
N20 C36 H36B 108.8 . . ?
N19 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
O11 C37 N21 124.5(5) . . ?
O11 C37 N20 127.0(5) . . ?
N21 C37 N20 108.5(4) . . ?
N21 C38 N22 113.5(4) . . ?
N21 C38 H38A 108.9 . . ?
N22 C38 H38A 108.9 . . ?
N21 C38 H38B 108.9 . . ?
N22 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
O12 C39 N22 125.7(5) . . ?
O12 C39 N23 126.1(5) . . ?
N22 C39 N23 108.2(4) . . ?
N23 C40 N24 114.5(4) . . ?
N23 C40 H40A 108.6 . . ?
N24 C40 H40A 108.6 . . ?
N23 C40 H40B 108.6 . . ?
N24 C40 H40B 108.6 . . ?
H40A C40 H40B 107.6 . . ?
C1 N1 C2 121.6(4) . . ?
C1 N1 C13 112.7(4) . . ?
C2 N1 C13 125.7(4) . . ?
C3 N2 C15 112.3(4) . . ?
C3 N2 C2 123.3(4) . . ?
C15 N2 C2 122.6(4) . . ?
C3 N3 C4 123.7(4) . . ?
C3 N3 C16 112.2(4) . . ?
C4 N3 C16 121.9(4) . . ?
C5 N4 C4 121.4(4) . . ?
C5 N4 C17 111.8(4) . . ?
C4 N4 C17 124.5(4) . . ?
C5 N5 C6 123.0(4) . . ?
C5 N5 C18 112.1(4) . . ?
C6 N5 C18 124.5(4) . . ?
C7 N6 C19 112.8(4) . . ?
C7 N6 C6 121.3(4) . . ?
C19 N6 C6 125.9(4) . . ?
C7 N7 C8 120.5(4) . . ?
C7 N7 C21 112.9(4) . . ?
C8 N7 C21 126.1(4) . . ?
C9 N8 C23 112.8(4) . . ?
C9 N8 C8 122.3(4) . . ?
C23 N8 C8 122.3(4) . . ?
C9 N9 C10 123.2(4) . . ?
C9 N9 C24 112.9(4) . . ?
C10 N9 C24 121.9(4) . . ?
C11 N10 C25 112.7(4) . . ?
C11 N10 C10 122.1(4) . . ?
C25 N10 C10 124.9(4) . . ?
C11 N11 C12 122.1(4) . . ?
C11 N11 C26 112.1(4) . . ?
C12 N11 C26 123.6(4) . . ?
C1 N12 C12 121.2(4) . . ?
C1 N12 C27 112.6(4) . . ?
C12 N12 C27 126.1(4) . . ?
C29 N13 C30 120.4(4) . . ?
C29 N13 C13 112.6(4) . . ?
C30 N13 C13 126.8(4) . . ?
C31 N14 C30 123.8(4) . . ?
C31 N14 C15 112.5(4) . . ?
C30 N14 C15 121.6(4) . . ?
C31 N15 C32 121.9(4) . . ?
C31 N15 C16 112.1(4) . . ?
C32 N15 C16 121.2(4) . . ?
C33 N16 C32 122.7(4) . . ?
C33 N16 C17 112.7(4) . . ?
C32 N16 C17 124.0(4) . . ?
C33 N17 C18 112.2(4) . . ?
C33 N17 C34 124.7(4) . . ?
C18 N17 C34 122.1(4) . . ?
C35 N18 C34 120.8(4) . . ?
C35 N18 C19 112.8(4) . . ?
C34 N18 C19 126.4(4) . . ?
C35 N19 C21 112.9(4) . . ?
C35 N19 C36 121.2(4) . . ?
C21 N19 C36 125.6(4) . . ?
C37 N20 C23 111.7(4) . . ?
C37 N20 C36 122.8(4) . . ?
C23 N20 C36 120.8(4) . . ?
C37 N21 C38 122.5(4) . . ?
C37 N21 C24 112.0(4) . . ?
C38 N21 C24 122.2(4) . . ?
C39 N22 C38 121.4(4) . . ?
C39 N22 C25 112.6(4) . . ?
C38 N22 C25 125.1(4) . . ?
C39 N23 C26 112.4(4) . . ?
C39 N23 C40 123.1(4) . . ?
C26 N23 C40 123.4(4) . . ?
C29 N24 C27 113.1(4) . . ?
C29 N24 C40 120.8(4) . . ?
C27 N24 C40 125.9(4) . . ?
O16 N25 O18 119.5(6) . . ?
O16 N25 O17 120.5(6) . . ?
O18 N25 O17 119.7(5) . . ?
O15 N26 O14 120.2(5) . . ?
O15 N26 O13 119.5(5) . . ?
O14 N26 O13 120.3(5) . . ?
O21 N27 O19 120.9(4) . . ?
O21 N27 O20 122.9(5) . . ?
O19 N27 O20 116.2(4) . . ?
C1 O1 Ce01 159.0(3) . . ?
C3 O2 Ce01 149.7(3) . . ?
N27 O19 Ce01 99.6(3) . . ?
N27 O20 Ce01 95.8(3) . . ?
O2W Ce01 O1 147.54(12) . . ?
O2W Ce01 O5W 78.58(14) . . ?
O1 Ce01 O5W 105.54(12) . . ?
O2W Ce01 O2 77.11(11) . . ?
O1 Ce01 O2 78.77(11) . . ?
O5W Ce01 O2 136.77(14) . . ?
O2W Ce01 O4W 140.25(12) . . ?
O1 Ce01 O4W 70.11(12) . . ?
O5W Ce01 O4W 76.96(15) . . ?
O2 Ce01 O4W 140.17(12) . . ?
O2W Ce01 O3W 72.95(12) . . ?
O1 Ce01 O3W 139.32(12) . . ?
O5W Ce01 O3W 71.25(13) . . ?
O2 Ce01 O3W 132.25(12) . . ?
O4W Ce01 O3W 69.74(12) . . ?
O2W Ce01 O1W 74.61(15) . . ?
O1 Ce01 O1W 77.46(15) . . ?
O5W Ce01 O1W 67.43(15) . . ?
O2 Ce01 O1W 71.91(13) . . ?
O4W Ce01 O1W 122.31(16) . . ?
O3W Ce01 O1W 131.30(15) . . ?
O2W Ce01 O19 69.75(13) . . ?
O1 Ce01 O19 119.74(12) . . ?
O5W Ce01 O19 133.26(13) . . ?
O2 Ce01 O19 67.95(12) . . ?
O4W Ce01 O19 106.75(14) . . ?
O3W Ce01 O19 67.17(13) . . ?
O1W Ce01 O19 130.79(15) . . ?
O2W Ce01 O20 117.53(12) . . ?
O1 Ce01 O20 75.51(11) . . ?
O5W Ce01 O20 149.10(14) . . ?
O2 Ce01 O20 74.11(11) . . ?
O4W Ce01 O20 74.50(13) . . ?
O3W Ce01 O20 87.82(13) . . ?
O1W Ce01 O20 139.85(14) . . ?
O19 Ce01 O20 48.23(11) . . ?

_refine_diff_density_max         1.069
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.099

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

data_3pp
_database_code_depnum_ccdc_archive 'CCDC 1038167'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT075_3pp                 
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_3pp                 
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

_vrf_PLAT306_3pp                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_3pp                 
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

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
1 0.250 -0.004 -0.009 721.7 217.6
2 0.750 -0.006 -0.008 721.7 217.6
_platon_squeeze_details          
; 
;




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 N25 O21 Pr2'
_chemical_formula_weight         1599.17

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'
Pr Pr -0.2180 2.8214 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           53
_space_group_name_H-M_alt        'P m n a'
_space_group_name_Hall           '-P 2ac 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.508(17)
_cell_length_b                   10.756(7)
_cell_length_c                   14.224(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3902(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2786
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      23.36

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_F_000             1592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.409
_shelx_estimated_absorpt_T_min   0.756
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17863
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.597
_diffrn_reflns_theta_max         29.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.745
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.745
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.745
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             4055
_reflns_number_gt                2206
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1274P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4055
_refine_ls_number_parameters     226
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.2063
_refine_ls_wR_factor_gt          0.1643
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.951
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6237(3) 0.2520(5) -0.0927(5) 0.0426(15) Uani 1 1 d . . . . .
C2 C 0.6678(3) 0.3433(6) 0.0474(5) 0.0488(16) Uani 1 1 d . . . . .
H2A H 0.6594 0.2622 0.0731 0.059 Uiso 1 1 calc R U . . .
H2B H 0.7057 0.3521 0.0482 0.059 Uiso 1 1 calc R U . . .
C3 C 0.6156(3) 0.4121(6) 0.1826(5) 0.0493(17) Uani 1 1 d . . . . .
C4 C 0.5956(3) 0.5019(7) 0.3379(5) 0.0564(18) Uani 1 1 d . . . . .
H4A H 0.6196 0.5460 0.3791 0.068 Uiso 1 1 calc R U . . .
H4B H 0.5953 0.4155 0.3574 0.068 Uiso 1 1 calc R U . . .
C5 C 0.5000 0.4788(10) 0.3398(6) 0.056(3) Uani 1 2 d S T P . .
C6 C 0.6693(3) 0.5612(6) 0.1153(5) 0.0458(16) Uani 1 1 d . . . . .
H6 H 0.7077 0.5561 0.1136 0.055 Uiso 1 1 calc R U . . .
C7 C 0.6493(3) 0.6088(6) 0.2112(5) 0.0508(17) Uani 1 1 d . . . . .
H7 H 0.6781 0.6256 0.2550 0.061 Uiso 1 1 calc R U . . .
C8 C 0.5304(3) 0.6861(6) 0.3641(5) 0.0462(16) Uani 1 1 d . . . . .
C9 C 0.5568(3) 0.7346(6) 0.4511(5) 0.061(2) Uani 1 1 d . . . . .
H9A H 0.5469 0.6845 0.5041 0.092 Uiso 1 1 calc R U . . .
H9B H 0.5941 0.7311 0.4430 0.092 Uiso 1 1 calc R U . . .
H9C H 0.5463 0.8191 0.4617 0.092 Uiso 1 1 calc R U . . .
C10 C 0.5955(3) 0.7993(6) 0.2541(5) 0.0463(16) Uani 1 1 d . . . . .
H10A H 0.5930 0.8829 0.2290 0.056 Uiso 1 1 calc R U . . .
H10B H 0.6174 0.8028 0.3098 0.056 Uiso 1 1 calc R U . . .
C11 C 0.5000 0.7998(9) 0.2333(7) 0.050(2) Uani 1 2 d S T P . .
N1 N 0.6498(2) 0.3486(5) -0.0497(4) 0.0505(14) Uani 1 1 d . . . . .
N2 N 0.6451(2) 0.4384(4) 0.1074(4) 0.0452(13) Uani 1 1 d . . . . .
N3 N 0.6154(2) 0.5086(5) 0.2441(4) 0.0482(13) Uani 1 1 d . . . . .
N4 N 0.5433(2) 0.5528(5) 0.3510(4) 0.0482(14) Uani 1 1 d . . . . .
N5 N 0.6204(3) 0.7224(6) 0.1863(4) 0.0531(16) Uani 1 1 d . . . . .
N6 N 0.5441(2) 0.7590(4) 0.2811(4) 0.0442(13) Uani 1 1 d . . . . .
O1 O 0.6075(2) 0.1578(4) -0.0542(3) 0.0551(12) Uani 1 1 d . . . . .
O2 O 0.59209(19) 0.3112(4) 0.1958(3) 0.0523(12) Uani 1 1 d . . . . .
O1W O 0.5000 0.2774(6) 0.0082(5) 0.060(2) Uani 1 2 d S T P . .
O3 O 0.5000 0.3687(6) 0.3282(4) 0.0518(18) Uani 1 2 d S T P . .
O2W O 0.4416(2) 0.0842(4) 0.1086(4) 0.0721(15) Uani 1 1 d . . . . .
O4 O 0.5000 0.8633(6) 0.1632(4) 0.0501(17) Uani 1 2 d S T P . .
Pr1 Pr 0.5000 0.24886(4) 0.17883(4) 0.0457(2) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.5037(2) 0.13019(16) 0.0517(6) Uani 1 2 d S T P . .
Cl2 Cl 0.5000 0.0786(5) 0.3334(4) 0.104(2) Uani 0.5 2 d S T P . .
N7 N 0.5000 0.0786(5) 0.3334(4) 0.104(2) Uani 0.5 2 d S TU P . .
O5 O 0.5442(4) 0.1121(9) 0.3046(7) 0.060(3) Uani 0.5 1 d . . P . .
O6 O 0.5000 0.0143(13) 0.4122(9) 0.079(5) Uani 0.5 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.224(7) . ?
C1 N5 1.362(9) 4_565 ?
C1 N1 1.376(8) . ?
C2 N2 1.453(8) . ?
C2 N1 1.457(8) . ?
C3 O2 1.255(8) . ?
C3 N2 1.337(8) . ?
C3 N3 1.358(8) . ?
C4 N3 1.428(8) . ?
C4 N4 1.453(10) . ?
C5 O3 1.195(13) . ?
C5 N4 1.371(8) 8_655 ?
C5 N4 1.371(8) . ?
C6 N1 1.435(8) 4_565 ?
C6 N2 1.463(8) . ?
C6 C7 1.543(9) . ?
C7 N3 1.460(8) . ?
C7 N5 1.471(9) . ?
C8 N6 1.461(9) . ?
C8 N4 1.483(8) . ?
C8 C9 1.502(10) . ?
C8 C8 1.550(14) 8_655 ?
C10 N5 1.421(9) . ?
C10 N6 1.431(9) . ?
C11 O4 1.209(11) . ?
C11 N6 1.386(8) . ?
C11 N6 1.386(8) 8_655 ?
N1 C6 1.435(8) 4_565 ?
N5 C1 1.362(9) 4_565 ?
O2 Pr1 2.455(5) . ?
O1W Pr1 2.446(7) . ?
O3 Pr1 2.486(6) . ?
O2W Pr1 2.521(5) . ?
Pr1 O2 2.455(5) 8_655 ?
Pr1 O2W 2.521(5) 8_655 ?
Pr1 O5 2.576(10) . ?
Pr1 O5 2.576(10) 8_655 ?
Pr1 Cl1 2.827(3) . ?
Pr1 Cl2 2.862(6) . ?
Cl2 O5 1.252(10) . ?
Cl2 O5 1.252(10) 8_655 ?
Cl2 O6 1.316(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N5 125.7(6) . 4_565 ?
O1 C1 N1 126.1(6) . . ?
N5 C1 N1 108.2(6) 4_565 . ?
N2 C2 N1 113.8(5) . . ?
O2 C3 N2 124.9(6) . . ?
O2 C3 N3 124.2(6) . . ?
N2 C3 N3 110.9(6) . . ?
N3 C4 N4 115.1(6) . . ?
O3 C5 N4 126.2(5) . 8_655 ?
O3 C5 N4 126.2(5) . . ?
N4 C5 N4 107.4(9) 8_655 . ?
N1 C6 N2 114.4(5) 4_565 . ?
N1 C6 C7 103.6(5) 4_565 . ?
N2 C6 C7 103.1(5) . . ?
N3 C7 N5 113.1(6) . . ?
N3 C7 C6 103.6(5) . . ?
N5 C7 C6 103.2(5) . . ?
N6 C8 N4 111.4(5) . . ?
N6 C8 C9 111.8(5) . . ?
N4 C8 C9 109.9(6) . . ?
N6 C8 C8 103.9(3) . 8_655 ?
N4 C8 C8 102.9(4) . 8_655 ?
C9 C8 C8 116.6(4) . 8_655 ?
N5 C10 N6 114.6(5) . . ?
O4 C11 N6 125.7(4) . . ?
O4 C11 N6 125.7(4) . 8_655 ?
N6 C11 N6 108.6(9) . 8_655 ?
C1 N1 C6 112.9(5) . 4_565 ?
C1 N1 C2 123.0(5) . . ?
C6 N1 C2 122.1(5) 4_565 . ?
C3 N2 C2 123.0(5) . . ?
C3 N2 C6 111.6(5) . . ?
C2 N2 C6 120.7(6) . . ?
C3 N3 C4 124.4(6) . . ?
C3 N3 C7 110.7(5) . . ?
C4 N3 C7 123.1(6) . . ?
C5 N4 C4 120.4(6) . . ?
C5 N4 C8 113.3(6) . . ?
C4 N4 C8 125.7(6) . . ?
C1 N5 C10 125.0(6) 4_565 . ?
C1 N5 C7 111.8(6) 4_565 . ?
C10 N5 C7 123.0(6) . . ?
C11 N6 C10 121.0(6) . . ?
C11 N6 C8 111.8(6) . . ?
C10 N6 C8 126.8(6) . . ?
C3 O2 Pr1 132.8(4) . . ?
C5 O3 Pr1 129.2(6) . . ?
O1W Pr1 O2 93.64(12) . . ?
O1W Pr1 O2 93.64(12) . 8_655 ?
O2 Pr1 O2 146.2(2) . 8_655 ?
O1W Pr1 O3 141.5(2) . . ?
O2 Pr1 O3 76.94(11) . . ?
O2 Pr1 O3 76.94(11) 8_655 . ?
O1W Pr1 O2W 72.25(17) . . ?
O2 Pr1 O2W 142.79(17) . . ?
O2 Pr1 O2W 70.46(17) 8_655 . ?
O3 Pr1 O2W 134.70(15) . . ?
O1W Pr1 O2W 72.25(17) . 8_655 ?
O2 Pr1 O2W 70.47(17) . 8_655 ?
O2 Pr1 O2W 142.79(17) 8_655 8_655 ?
O3 Pr1 O2W 134.70(15) . 8_655 ?
O2W Pr1 O2W 72.4(3) . 8_655 ?
O1W Pr1 O5 139.5(2) . . ?
O2 Pr1 O5 70.7(3) . . ?
O2 Pr1 O5 120.4(2) 8_655 . ?
O3 Pr1 O5 72.7(3) . . ?
O2W Pr1 O5 97.6(3) . . ?
O2W Pr1 O5 67.4(3) 8_655 . ?
O1W Pr1 O5 139.5(2) . 8_655 ?
O2 Pr1 O5 120.4(2) . 8_655 ?
O2 Pr1 O5 70.7(3) 8_655 8_655 ?
O3 Pr1 O5 72.7(3) . 8_655 ?
O2W Pr1 O5 67.4(3) . 8_655 ?
O2W Pr1 O5 97.6(3) 8_655 8_655 ?
O5 Pr1 O5 51.9(5) . 8_655 ?
O1W Pr1 Cl1 68.61(15) . . ?
O2 Pr1 Cl1 76.07(10) . . ?
O2 Pr1 Cl1 76.07(10) 8_655 . ?
O3 Pr1 Cl1 72.92(16) . . ?
O2W Pr1 Cl1 125.76(13) . . ?
O2W Pr1 Cl1 125.76(13) 8_655 . ?
O5 Pr1 Cl1 136.4(2) . . ?
O5 Pr1 Cl1 136.4(2) 8_655 . ?
O1W Pr1 Cl2 147.43(18) . . ?
O2 Pr1 Cl2 95.68(11) . . ?
O2 Pr1 Cl2 95.68(11) 8_655 . ?
O3 Pr1 Cl2 71.04(19) . . ?
O2W Pr1 Cl2 81.65(15) . . ?
O2W Pr1 Cl2 81.65(15) 8_655 . ?
O5 Pr1 Cl2 25.9(2) . . ?
O5 Pr1 Cl2 25.9(2) 8_655 . ?
Cl1 Pr1 Cl2 143.96(12) . . ?
O5 Cl2 O5 128.4(11) . 8_655 ?
O5 Cl2 O6 115.4(5) . . ?
O5 Cl2 O6 115.4(5) 8_655 . ?
O5 Cl2 Pr1 64.2(5) . . ?
O5 Cl2 Pr1 64.2(5) 8_655 . ?
O6 Cl2 Pr1 171.9(7) . . ?
Cl2 O5 Pr1 89.9(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C6 C7 N3 118.1(5) 4_565 . . . ?
N2 C6 C7 N3 -1.4(6) . . . . ?
N1 C6 C7 N5 0.0(7) 4_565 . . . ?
N2 C6 C7 N5 -119.5(6) . . . . ?
O1 C1 N1 C6 172.9(6) . . . 4_565 ?
N5 C1 N1 C6 -5.4(8) 4_565 . . 4_565 ?
O1 C1 N1 C2 8.5(10) . . . . ?
N5 C1 N1 C2 -169.7(6) 4_565 . . . ?
N2 C2 N1 C1 -119.7(7) . . . . ?
N2 C2 N1 C6 77.4(8) . . . 4_565 ?
O2 C3 N2 C2 -21.2(10) . . . . ?
N3 C3 N2 C2 157.7(6) . . . . ?
O2 C3 N2 C6 -177.1(6) . . . . ?
N3 C3 N2 C6 1.8(7) . . . . ?
N1 C2 N2 C3 118.8(7) . . . . ?
N1 C2 N2 C6 -87.5(7) . . . . ?
N1 C6 N2 C3 -111.9(7) 4_565 . . . ?
C7 C6 N2 C3 -0.1(7) . . . . ?
N1 C6 N2 C2 91.6(7) 4_565 . . . ?
C7 C6 N2 C2 -156.6(5) . . . . ?
O2 C3 N3 C4 10.6(10) . . . . ?
N2 C3 N3 C4 -168.3(6) . . . . ?
O2 C3 N3 C7 176.1(6) . . . . ?
N2 C3 N3 C7 -2.8(8) . . . . ?
N4 C4 N3 C3 -100.4(7) . . . . ?
N4 C4 N3 C7 95.8(8) . . . . ?
N5 C7 N3 C3 113.6(6) . . . . ?
C6 C7 N3 C3 2.6(7) . . . . ?
N5 C7 N3 C4 -80.7(8) . . . . ?
C6 C7 N3 C4 168.3(6) . . . . ?
O3 C5 N4 C4 7.6(12) . . . . ?
N4 C5 N4 C4 -176.6(4) 8_655 . . . ?
O3 C5 N4 C8 -179.9(8) . . . . ?
N4 C5 N4 C8 -4.1(10) 8_655 . . . ?
N3 C4 N4 C5 89.3(8) . . . . ?
N3 C4 N4 C8 -82.2(8) . . . . ?
N6 C8 N4 C5 -108.2(7) . . . . ?
C9 C8 N4 C5 127.4(7) . . . . ?
C8 C8 N4 C5 2.5(6) 8_655 . . . ?
N6 C8 N4 C4 63.8(8) . . . . ?
C9 C8 N4 C4 -60.6(8) . . . . ?
C8 C8 N4 C4 174.5(5) 8_655 . . . ?
N6 C10 N5 C1 101.0(8) . . . 4_565 ?
N6 C10 N5 C7 -83.7(8) . . . . ?
N3 C7 N5 C1 -114.5(7) . . . 4_565 ?
C6 C7 N5 C1 -3.2(8) . . . 4_565 ?
N3 C7 N5 C10 69.7(8) . . . . ?
C6 C7 N5 C10 -179.1(6) . . . . ?
O4 C11 N6 C10 5.4(12) . . . . ?
N6 C11 N6 C10 -172.7(4) 8_655 . . . ?
O4 C11 N6 C8 178.9(8) . . . . ?
N6 C11 N6 C8 0.8(9) 8_655 . . . ?
N5 C10 N6 C11 -90.0(7) . . . . ?
N5 C10 N6 C8 97.5(7) . . . . ?
N4 C8 N6 C11 109.6(7) . . . . ?
C9 C8 N6 C11 -127.1(7) . . . . ?
C8 C8 N6 C11 -0.5(5) 8_655 . . . ?
N4 C8 N6 C10 -77.4(8) . . . . ?
C9 C8 N6 C10 46.0(8) . . . . ?
C8 C8 N6 C10 172.6(5) 8_655 . . . ?
N2 C3 O2 Pr1 -102.2(8) . . . . ?
N3 C3 O2 Pr1 79.1(8) . . . . ?
N4 C5 O3 Pr1 92.5(8) 8_655 . . . ?
N4 C5 O3 Pr1 -92.5(8) . . . . ?
O5 Cl2 O5 Pr1 -1.7(13) 8_655 . . . ?
O6 Cl2 O5 Pr1 -171.0(8) . . . . ?

_refine_diff_density_max         0.912
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.154

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

data_3p
_database_code_depnum_ccdc_archive 'CCDC 1038168'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_3p                  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_3p                  
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;


_vrf_PLAT244_3p                  
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of 
RESPONSE: This is the central nitrogen atom of nitrate. It is to be
expected chemically that the oxygen atoms have larger displacement
parameters than 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H132 N76 O56 Pr2'
_chemical_formula_weight         3816.83

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.507(8)
_cell_length_b                   17.145(9)
_cell_length_c                   35.161(19)
_cell_angle_alpha                90
_cell_angle_beta                 93.370(8)
_cell_angle_gamma                90
_cell_volume                     9332(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5941
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      19.98

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_F_000             3900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.612
_shelx_estimated_absorpt_T_min   0.852
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48978
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.322
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             16726
_reflns_number_gt                9843
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0664P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16726
_refine_ls_number_parameters     1151
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1202
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0528(3) 0.7537(3) 0.71782(14) 0.0386(11) Uani 1 1 d . . . . .
C2 C 0.9573(3) 0.8426(3) 0.74813(14) 0.0461(13) Uani 1 1 d . . . . .
H2A H 0.9647 0.8693 0.7724 0.055 Uiso 1 1 calc R U . . .
H2B H 0.9747 0.8783 0.7286 0.055 Uiso 1 1 calc R U . . .
C3 C 0.8258(3) 0.8236(2) 0.70640(13) 0.0380(11) Uani 1 1 d . . . . .
C4 C 0.6757(3) 0.8351(3) 0.68128(14) 0.0479(13) Uani 1 1 d . . . . .
H4A H 0.6380 0.8734 0.6920 0.057 Uiso 1 1 calc R U . . .
H4B H 0.7038 0.8599 0.6605 0.057 Uiso 1 1 calc R U . . .
C5 C 0.6217(3) 0.7517(3) 0.62841(15) 0.0460(13) Uani 1 1 d . . . . .
C6 C 0.5284(3) 0.6755(3) 0.58377(13) 0.0483(13) Uani 1 1 d . . . . .
H6A H 0.5484 0.7127 0.5654 0.058 Uiso 1 1 calc R U . . .
H6B H 0.4657 0.6756 0.5815 0.058 Uiso 1 1 calc R U . . .
C7 C 0.6265(3) 0.5907(3) 0.55150(14) 0.0435(12) Uani 1 1 d . . . . .
C8 C 0.7151(3) 0.4869(3) 0.52761(12) 0.0429(12) Uani 1 1 d . . . . .
H8A H 0.7329 0.5266 0.5101 0.051 Uiso 1 1 calc R U . . .
H8B H 0.7009 0.4403 0.5129 0.051 Uiso 1 1 calc R U . . .
C9 C 0.8512(3) 0.5206(3) 0.56297(13) 0.0433(12) Uani 1 1 d . . . . .
C10 C 1.0007(3) 0.5164(3) 0.58945(13) 0.0422(12) Uani 1 1 d . . . . .
H10A H 1.0022 0.5656 0.5759 0.051 Uiso 1 1 calc R U . . .
H10B H 1.0410 0.4812 0.5782 0.051 Uiso 1 1 calc R U . . .
C11 C 1.0533(3) 0.5999(3) 0.64189(13) 0.0390(11) Uani 1 1 d . . . . .
C12 C 1.1474(3) 0.6535(3) 0.69506(13) 0.0432(12) Uani 1 1 d . . . . .
H12A H 1.1617 0.6925 0.6765 0.052 Uiso 1 1 calc R U . . .
H12B H 1.2012 0.6322 0.7061 0.052 Uiso 1 1 calc R U . . .
C13 C 1.0363(3) 0.7250(3) 0.78159(13) 0.0443(12) Uani 1 1 d . . . . .
C14 C 1.0790(4) 0.7730(3) 0.81386(15) 0.0658(16) Uani 1 1 d . . . . .
H14A H 1.0377 0.8088 0.8233 0.099 Uiso 1 1 calc R U . . .
H14B H 1.1267 0.8016 0.8046 0.099 Uiso 1 1 calc R U . . .
H14C H 1.0995 0.7389 0.8341 0.099 Uiso 1 1 calc R U . . .
C15 C 0.8101(3) 0.8102(3) 0.77142(13) 0.0402(12) Uani 1 1 d . . . . .
H15 H 0.8144 0.8506 0.7912 0.048 Uiso 1 1 calc R U . . .
C16 C 0.7203(3) 0.8082(3) 0.75053(12) 0.0393(12) Uani 1 1 d . . . . .
H16 H 0.6841 0.8519 0.7578 0.047 Uiso 1 1 calc R U . . .
C17 C 0.5528(3) 0.7384(3) 0.68540(13) 0.0406(12) Uani 1 1 d . . . . .
H17 H 0.5123 0.7786 0.6929 0.049 Uiso 1 1 calc R U . . .
C18 C 0.5116(3) 0.6836(3) 0.65491(13) 0.0413(12) Uani 1 1 d . . . . .
H18 H 0.4495 0.6934 0.6509 0.050 Uiso 1 1 calc R U . . .
C19 C 0.5184(3) 0.5247(3) 0.58353(13) 0.0419(12) Uani 1 1 d . . . . .
C20 C 0.4236(3) 0.5227(4) 0.57038(15) 0.0653(16) Uani 1 1 d . . . . .
H20A H 0.4005 0.4719 0.5751 0.098 Uiso 1 1 calc R U . . .
H20B H 0.4175 0.5339 0.5436 0.098 Uiso 1 1 calc R U . . .
H20C H 0.3928 0.5610 0.5841 0.098 Uiso 1 1 calc R U . . .
C21 C 0.5776(3) 0.4628(3) 0.56356(13) 0.0430(12) Uani 1 1 d . . . . .
C22 C 0.5301(4) 0.4080(3) 0.53559(15) 0.0612(15) Uani 1 1 d . . . . .
H22A H 0.5712 0.3788 0.5220 0.092 Uiso 1 1 calc R U . . .
H22B H 0.4941 0.4379 0.5178 0.092 Uiso 1 1 calc R U . . .
H22C H 0.4949 0.3729 0.5492 0.092 Uiso 1 1 calc R U . . .
C23 C 0.8089(3) 0.3918(3) 0.56718(13) 0.0386(11) Uani 1 1 d . . . . .
H23 H 0.8077 0.3549 0.5459 0.046 Uiso 1 1 calc R U . . .
C24 C 0.8999(3) 0.4005(2) 0.58555(13) 0.0391(11) Uani 1 1 d . . . . .
H24 H 0.9424 0.3716 0.5716 0.047 Uiso 1 1 calc R U . . .
C25 C 1.0639(3) 0.4671(3) 0.65298(13) 0.0397(12) Uani 1 1 d . . . . .
H25 H 1.1071 0.4368 0.6401 0.048 Uiso 1 1 calc R U . . .
C26 C 1.1045(3) 0.5113(3) 0.68759(13) 0.0387(11) Uani 1 1 d . . . . .
H26 H 1.1644 0.4953 0.6936 0.046 Uiso 1 1 calc R U . . .
C27 C 1.0944(3) 0.6616(3) 0.76375(14) 0.0442(12) Uani 1 1 d . . . . .
C28 C 1.1825(3) 0.6497(3) 0.78367(16) 0.0658(16) Uani 1 1 d . . . . .
H28A H 1.2150 0.6973 0.7829 0.099 Uiso 1 1 calc R U . . .
H28B H 1.2125 0.6091 0.7711 0.099 Uiso 1 1 calc R U . . .
H28C H 1.1760 0.6352 0.8097 0.099 Uiso 1 1 calc R U . . .
C29 C 0.9674(3) 0.6039(3) 0.78341(13) 0.0422(12) Uani 1 1 d . . . . .
C30 C 0.8893(3) 0.7103(3) 0.81305(13) 0.0466(12) Uani 1 1 d . . . . .
H30A H 0.8693 0.6708 0.8302 0.056 Uiso 1 1 calc R U . . .
H30B H 0.9075 0.7552 0.8282 0.056 Uiso 1 1 calc R U . . .
C31 C 0.7421(3) 0.6940(3) 0.78530(13) 0.0422(12) Uani 1 1 d . . . . .
C32 C 0.5967(3) 0.7124(3) 0.75478(13) 0.0450(12) Uani 1 1 d . . . . .
H32A H 0.5604 0.7569 0.7600 0.054 Uiso 1 1 calc R U . . .
H32B H 0.5832 0.6711 0.7723 0.054 Uiso 1 1 calc R U . . .
C33 C 0.5613(3) 0.6098(3) 0.70716(13) 0.0391(11) Uani 1 1 d . . . . .
C34 C 0.4870(3) 0.5378(3) 0.65468(14) 0.0464(13) Uani 1 1 d . . . . .
H34A H 0.4284 0.5507 0.6456 0.056 Uiso 1 1 calc R U . . .
H34B H 0.4834 0.4993 0.6747 0.056 Uiso 1 1 calc R U . . .
C35 C 0.5837(3) 0.4408(3) 0.62960(14) 0.0429(12) Uani 1 1 d . . . . .
C36 C 0.6679(3) 0.3491(3) 0.59381(14) 0.0491(13) Uani 1 1 d . . . . .
H36A H 0.6527 0.3136 0.6138 0.059 Uiso 1 1 calc R U . . .
H36B H 0.6542 0.3236 0.5696 0.059 Uiso 1 1 calc R U . . .
C37 C 0.8091(3) 0.3468(3) 0.62956(14) 0.0415(12) Uani 1 1 d . . . . .
C38 C 0.9635(3) 0.3509(3) 0.64961(13) 0.0429(12) Uani 1 1 d . . . . .
H38A H 0.9443 0.3146 0.6685 0.052 Uiso 1 1 calc R U . . .
H38B H 1.0078 0.3250 0.6359 0.052 Uiso 1 1 calc R U . . .
C39 C 0.9944(3) 0.4306(3) 0.70680(14) 0.0409(12) Uani 1 1 d . . . . .
C40 C 1.0673(3) 0.5130(3) 0.75620(14) 0.0505(13) Uani 1 1 d . . . . .
H40A H 1.1290 0.5087 0.7622 0.061 Uiso 1 1 calc R U . . .
H40B H 1.0387 0.4769 0.7725 0.061 Uiso 1 1 calc R U . . .
C41 C 1.2672(3) 1.1530(3) 0.47422(13) 0.0469(13) Uani 1 1 d . . . . .
H41A H 1.2409 1.1979 0.4614 0.056 Uiso 1 1 calc R U . . .
H41B H 1.3283 1.1640 0.4790 0.056 Uiso 1 1 calc R U . . .
C42 C 1.1609(3) 1.1864(3) 0.52138(15) 0.0454(13) Uani 1 1 d . . . . .
C43 C 1.0966(3) 1.2216(3) 0.58075(15) 0.0556(14) Uani 1 1 d . . . . .
H43A H 1.0781 1.2665 0.5655 0.067 Uiso 1 1 calc R U . . .
H43B H 1.1293 1.2408 0.6032 0.067 Uiso 1 1 calc R U . . .
C44 C 0.9399(4) 1.1957(3) 0.57718(16) 0.0502(14) Uani 1 1 d . . . . .
C45 C 0.7902(4) 1.1626(3) 0.59081(16) 0.0608(15) Uani 1 1 d . . . . .
H45A H 0.7765 1.2092 0.5760 0.073 Uiso 1 1 calc R U . . .
H45B H 0.7628 1.1673 0.6148 0.073 Uiso 1 1 calc R U . . .
C46 C 1.4102(3) 1.0472(3) 0.44897(16) 0.0643(16) Uani 1 1 d . . . . .
H46A H 1.4268 1.0708 0.4731 0.096 Uiso 1 1 calc R U . . .
H46B H 1.4158 1.0846 0.4290 0.096 Uiso 1 1 calc R U . . .
H46C H 1.4470 1.0033 0.4448 0.096 Uiso 1 1 calc R U . . .
C47 C 1.3170(3) 1.0199(3) 0.44902(14) 0.0448(12) Uani 1 1 d . . . . .
C48 C 1.2743(3) 1.1039(3) 0.54286(13) 0.0466(13) Uani 1 1 d . . . . .
H48 H 1.3335 1.1234 0.5472 0.056 Uiso 1 1 calc R U . . .
C49 C 1.2173(3) 1.1236(3) 0.57609(13) 0.0459(13) Uani 1 1 d . . . . .
H49 H 1.2507 1.1493 0.5970 0.055 Uiso 1 1 calc R U . . .
C50 C 1.0206(3) 1.1314(3) 0.62602(13) 0.0451(13) Uani 1 1 d . . . . .
H50 H 1.0479 1.1567 0.6486 0.054 Uiso 1 1 calc R U . . .
C51 C 0.9233(3) 1.1173(3) 0.63021(14) 0.0474(13) Uani 1 1 d . . . . .
H51 H 0.9049 1.1377 0.6545 0.057 Uiso 1 1 calc R U . . .
C52 C 0.7167(3) 1.0269(3) 0.58719(13) 0.0430(12) Uani 1 1 d . . . . .
C53 C 0.6491(3) 1.0467(3) 0.61536(16) 0.0659(16) Uani 1 1 d . . . . .
H53A H 0.6768 1.0702 0.6377 0.099 Uiso 1 1 calc R U . . .
H53B H 0.6200 0.9999 0.6224 0.099 Uiso 1 1 calc R U . . .
H53C H 0.6080 1.0826 0.6038 0.099 Uiso 1 1 calc R U . . .
C54 C 1.2626(4) 0.9008(3) 0.46812(17) 0.0560(14) Uani 1 1 d . . . . .
C55 C 1.3308(3) 0.9748(3) 0.51948(15) 0.0578(15) Uani 1 1 d . . . . .
H55A H 1.3868 1.0002 0.5215 0.069 Uiso 1 1 calc R U . . .
H55B H 1.3376 0.9233 0.5308 0.069 Uiso 1 1 calc R U . . .
C56 C 1.2222(3) 0.9884(3) 0.56856(15) 0.0506(13) Uani 1 1 d . . . . .
C57 C 1.1456(3) 1.0364(3) 0.62283(14) 0.0521(14) Uani 1 1 d . . . . .
H57A H 1.1741 1.0692 0.6422 0.062 Uiso 1 1 calc R U . . .
H57B H 1.1541 0.9826 0.6307 0.062 Uiso 1 1 calc R U . . .
C58 C 0.9926(3) 0.9983(3) 0.62584(12) 0.0421(12) Uani 1 1 d . . . . .
C59 C 0.8380(3) 0.9936(3) 0.63707(13) 0.0421(12) Uani 1 1 d . . . . .
H59A H 0.8063 1.0254 0.6543 0.050 Uiso 1 1 calc R U . . .
H59B H 0.8540 0.9456 0.6503 0.050 Uiso 1 1 calc R U . . .
C60 C 0.7967(3) 0.9135(3) 0.58183(13) 0.0361(11) Uani 1 1 d . . . . .
N1 N 1.0139(2) 0.7758(2) 0.74882(10) 0.0407(10) Uani 1 1 d . . . . .
N2 N 0.8676(2) 0.8250(2) 0.74101(10) 0.0392(9) Uani 1 1 d . . . . .
N3 N 0.7405(3) 0.8118(2) 0.71011(10) 0.0399(9) Uani 1 1 d . . . . .
N4 N 0.6244(3) 0.7712(2) 0.66644(11) 0.0438(10) Uani 1 1 d . . . . .
N5 N 0.5560(3) 0.7012(2) 0.62120(11) 0.0449(10) Uani 1 1 d . . . . .
N6 N 0.5589(3) 0.5987(2) 0.57417(11) 0.0447(10) Uani 1 1 d . . . . .
N7 N 0.6385(3) 0.5134(2) 0.54474(11) 0.0446(10) Uani 1 1 d . . . . .
N8 N 0.7875(3) 0.4695(2) 0.55431(10) 0.0419(10) Uani 1 1 d . . . . .
N9 N 0.9150(3) 0.4841(2) 0.58441(10) 0.0393(9) Uani 1 1 d . . . . .
N10 N 1.0284(2) 0.5293(2) 0.62885(10) 0.0379(9) Uani 1 1 d . . . . .
N11 N 1.0989(2) 0.5917(2) 0.67583(11) 0.0396(9) Uani 1 1 d . . . . .
N12 N 1.1015(3) 0.6906(2) 0.72479(11) 0.0428(10) Uani 1 1 d . . . . .
N13 N 0.9635(3) 0.6799(2) 0.79392(11) 0.0441(10) Uani 1 1 d . . . . .
N14 N 0.8194(3) 0.7325(2) 0.78712(11) 0.0411(10) Uani 1 1 d . . . . .
N15 N 0.6858(3) 0.7344(2) 0.76166(10) 0.0402(10) Uani 1 1 d . . . . .
N16 N 0.5760(2) 0.6861(2) 0.71620(10) 0.0422(10) Uani 1 1 d . . . . .
N17 N 0.5279(2) 0.6069(2) 0.67049(10) 0.0407(10) Uani 1 1 d . . . . .
N18 N 0.5313(3) 0.5036(2) 0.62371(10) 0.0426(10) Uani 1 1 d . . . . .
N19 N 0.6156(2) 0.4193(2) 0.59585(10) 0.0412(10) Uani 1 1 d . . . . .
N20 N 0.7591(2) 0.3634(2) 0.59754(10) 0.0375(9) Uani 1 1 d . . . . .
N21 N 0.8914(2) 0.3689(2) 0.62317(10) 0.0402(9) Uani 1 1 d . . . . .
N22 N 1.0014(2) 0.4178(2) 0.66897(10) 0.0397(10) Uani 1 1 d . . . . .
N23 N 1.0491(3) 0.4903(2) 0.71713(10) 0.0418(10) Uani 1 1 d . . . . .
N24 N 1.0402(2) 0.5917(2) 0.76489(10) 0.0406(10) Uani 1 1 d . . . . .
N25 N 1.2575(2) 1.0858(2) 0.44938(10) 0.0390(9) Uani 1 1 d . . . . .
N26 N 1.2283(3) 1.1418(2) 0.51056(10) 0.0442(10) Uani 1 1 d . . . . .
N27 N 1.1523(3) 1.1746(2) 0.55907(11) 0.0462(10) Uani 1 1 d . . . . .
N28 N 1.0206(3) 1.1814(2) 0.59277(12) 0.0479(11) Uani 1 1 d . . . . .
N29 N 0.8823(3) 1.1586(2) 0.59846(12) 0.0491(11) Uani 1 1 d . . . . .
N30 N 0.7546(3) 1.0957(2) 0.57041(13) 0.0526(11) Uani 1 1 d . . . . .
N31 N 1.3044(3) 0.9661(2) 0.47989(12) 0.0499(11) Uani 1 1 d . . . . .
N32 N 1.2707(3) 1.0196(2) 0.54130(11) 0.0492(11) Uani 1 1 d . . . . .
N33 N 1.1860(3) 1.0483(2) 0.58745(11) 0.0463(10) Uani 1 1 d . . . . .
N34 N 1.0537(3) 1.0536(2) 0.62090(11) 0.0443(10) Uani 1 1 d . . . . .
N35 N 0.9150(3) 1.0340(2) 0.62843(11) 0.0418(10) Uani 1 1 d . . . . .
N36 N 0.7819(2) 0.9749(2) 0.60440(10) 0.0380(9) Uani 1 1 d . . . . .
O1 O 1.0473(2) 0.78916(18) 0.68662(9) 0.0435(8) Uani 1 1 d . . . . .
O2 O 0.8597(2) 0.83357(18) 0.67564(8) 0.0431(8) Uani 1 1 d . . . . .
O1W O 0.9033(3) 0.6692(3) 0.68041(13) 0.0903(14) Uani 1 1 d . . . . .
O3 O 0.6706(2) 0.7774(2) 0.60538(9) 0.0559(9) Uani 1 1 d . . . . .
O2W O 1.1216(2) 0.80746(19) 0.61399(10) 0.0596(10) Uani 1 1 d . . . . .
O4 O 0.6672(2) 0.6439(2) 0.53877(10) 0.0592(10) Uani 1 1 d . . . . .
O3W O 0.9845(2) 0.7687(3) 0.56107(10) 0.0768(12) Uani 1 1 d . . . . .
O5 O 0.8540(2) 0.58880(18) 0.55266(10) 0.0553(9) Uani 1 1 d . . . . .
O4W O 0.8366(2) 0.70436(19) 0.60503(11) 0.0654(10) Uani 1 1 d . . . . .
O6 O 1.0389(2) 0.66197(17) 0.62531(9) 0.0468(8) Uani 1 1 d . . . . .
O7 O 0.9141(2) 0.5547(2) 0.79077(10) 0.0592(10) Uani 1 1 d . . . . .
O8 O 0.7260(2) 0.63341(19) 0.80210(9) 0.0517(9) Uani 1 1 d . . . . .
O9 O 0.5728(2) 0.55461(19) 0.72861(9) 0.0501(9) Uani 1 1 d . . . . .
O10 O 0.5985(2) 0.4087(2) 0.66003(9) 0.0569(9) Uani 1 1 d . . . . .
O11 O 0.7857(2) 0.3139(2) 0.65773(9) 0.0539(9) Uani 1 1 d . . . . .
O12 O 0.9494(2) 0.39501(19) 0.72784(9) 0.0517(9) Uani 1 1 d . . . . .
O13 O 1.0061(2) 0.92767(18) 0.62767(9) 0.0458(8) Uani 1 1 d . . . . .
O14 O 0.8521(2) 0.86237(17) 0.58945(8) 0.0425(8) Uani 1 1 d . . . . .
O15 O 1.1184(2) 1.2308(2) 0.50108(10) 0.0600(10) Uani 1 1 d . . . . .
O16 O 0.9227(2) 1.23858(19) 0.55003(11) 0.0613(10) Uani 1 1 d . . . . .
O17 O 1.2440(3) 0.8453(2) 0.48803(12) 0.0781(12) Uani 1 1 d . . . . .
O18 O 1.2121(2) 0.9196(2) 0.57473(11) 0.0690(11) Uani 1 1 d . . . . .
Pr1 Pr 0.96174(2) 0.78753(2) 0.62760(2) 0.04144(10) Uani 1 1 d . . . . .
O21 O 0.1761(5) 0.2923(5) 0.6600(2) 0.183(4) Uani 1 1 d D U . . .
O23 O 0.0999(6) 0.2300(6) 0.7068(3) 0.257(6) Uani 1 1 d D U . . .
N37 N 0.1502(6) 0.2850(6) 0.6931(3) 0.170(5) Uani 1 1 d D U . . .
O22 O 0.1817(6) 0.3366(5) 0.7192(3) 0.239(5) Uani 1 1 d D U . . .
O24 O 0.5789(7) 0.2080(5) 0.5487(3) 0.312(8) Uani 1 1 d D U . . .
O25 O 0.4770(6) 0.1411(8) 0.5359(4) 0.301(7) Uani 1 1 d D U . . .
N38 N 0.5290(8) 0.1822(7) 0.5202(3) 0.198(4) Uani 1 1 d D U . . .
O26 O 0.5436(7) 0.2012(6) 0.4843(3) 0.259(5) Uani 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.252(5) . ?
C1 N1 1.332(6) . ?
C1 N12 1.335(6) . ?
C2 N2 1.431(6) . ?
C2 N1 1.443(6) . ?
C3 O2 1.242(5) . ?
C3 N2 1.345(6) . ?
C3 N3 1.352(6) . ?
C4 N4 1.433(6) . ?
C4 N3 1.441(6) . ?
C5 O3 1.224(5) . ?
C5 N5 1.349(6) . ?
C5 N4 1.377(6) . ?
C6 N5 1.429(6) . ?
C6 N6 1.447(6) . ?
C7 O4 1.210(5) . ?
C7 N6 1.360(6) . ?
C7 N7 1.361(6) . ?
C8 N7 1.437(6) . ?
C8 N8 1.452(6) . ?
C9 O5 1.226(5) . ?
C9 N8 1.343(6) . ?
C9 N9 1.360(6) . ?
C10 N9 1.440(6) . ?
C10 N10 1.443(6) . ?
C11 O6 1.228(5) . ?
C11 N10 1.343(6) . ?
C11 N11 1.358(6) . ?
C12 N11 1.443(5) . ?
C12 N12 1.447(6) . ?
C13 N13 1.456(6) . ?
C13 N1 1.469(6) . ?
C13 C14 1.521(6) . ?
C13 C27 1.567(7) . ?
C15 N14 1.446(5) . ?
C15 N2 1.454(5) . ?
C15 C16 1.535(6) . ?
C16 N15 1.436(5) . ?
C16 N3 1.475(5) . ?
C17 N16 1.436(6) . ?
C17 N4 1.443(6) . ?
C17 C18 1.536(6) . ?
C18 N5 1.437(6) . ?
C18 N17 1.441(6) . ?
C19 N18 1.461(5) . ?
C19 N6 1.462(6) . ?
C19 C20 1.515(6) . ?
C19 C21 1.593(7) . ?
C21 N19 1.454(6) . ?
C21 N7 1.469(6) . ?
C21 C22 1.518(7) . ?
C23 N20 1.439(5) . ?
C23 N8 1.439(5) . ?
C23 C24 1.524(6) . ?
C24 N21 1.443(5) . ?
C24 N9 1.453(5) . ?
C25 N22 1.427(5) . ?
C25 N10 1.450(5) . ?
C25 C26 1.537(6) . ?
C26 N23 1.433(5) . ?
C26 N11 1.440(5) . ?
C27 N24 1.467(6) . ?
C27 N12 1.467(6) . ?
C27 C28 1.512(7) . ?
C29 O7 1.220(5) . ?
C29 N24 1.352(6) . ?
C29 N13 1.355(6) . ?
C30 N14 1.427(6) . ?
C30 N13 1.462(6) . ?
C31 O8 1.228(5) . ?
C31 N15 1.359(6) . ?
C31 N14 1.366(6) . ?
C32 N15 1.440(6) . ?
C32 N16 1.448(6) . ?
C33 O9 1.217(5) . ?
C33 N16 1.361(6) . ?
C33 N17 1.362(6) . ?
C34 N17 1.441(6) . ?
C34 N18 1.445(6) . ?
C35 O10 1.214(5) . ?
C35 N18 1.357(6) . ?
C35 N19 1.363(6) . ?
C36 N20 1.433(6) . ?
C36 N19 1.455(6) . ?
C37 O11 1.214(5) . ?
C37 N20 1.359(6) . ?
C37 N21 1.364(6) . ?
C38 N22 1.441(6) . ?
C38 N21 1.445(6) . ?
C39 O12 1.211(5) . ?
C39 N22 1.359(6) . ?
C39 N23 1.365(6) . ?
C40 N23 1.440(6) . ?
C40 N24 1.450(6) . ?
C41 N25 1.448(5) . ?
C41 N26 1.458(6) . ?
C42 O15 1.212(6) . ?
C42 N27 1.355(6) . ?
C42 N26 1.366(6) . ?
C43 N27 1.434(6) . ?
C43 N28 1.450(6) . ?
C44 O16 1.221(6) . ?
C44 N29 1.357(6) . ?
C44 N28 1.359(7) . ?
C45 N29 1.439(6) . ?
C45 N30 1.445(6) . ?
C46 C47 1.519(7) . ?
C47 N31 1.446(6) . ?
C47 N25 1.459(6) . ?
C47 C52 1.568(7) 3_776 ?
C48 N32 1.447(6) . ?
C48 N26 1.458(6) . ?
C48 C49 1.544(6) . ?
C49 N27 1.438(6) . ?
C49 N33 1.442(6) . ?
C50 N34 1.445(6) . ?
C50 N28 1.450(6) . ?
C50 C51 1.543(7) . ?
C51 N35 1.434(6) . ?
C51 N29 1.438(6) . ?
C52 N36 1.452(6) . ?
C52 N30 1.458(6) . ?
C52 C53 1.523(6) . ?
C52 C47 1.569(7) 3_776 ?
C54 O17 1.225(6) . ?
C54 N31 1.347(7) . ?
C54 N30 1.367(7) 3_776 ?
C55 N31 1.435(6) . ?
C55 N32 1.461(6) . ?
C56 O18 1.211(6) . ?
C56 N33 1.362(6) . ?
C56 N32 1.362(6) . ?
C57 N33 1.440(6) . ?
C57 N34 1.453(6) . ?
C58 O13 1.230(5) . ?
C58 N35 1.358(6) . ?
C58 N34 1.358(6) . ?
C59 N35 1.429(6) . ?
C59 N36 1.436(6) . ?
C60 O14 1.246(5) . ?
C60 N25 1.342(6) 3_776 ?
C60 N36 1.346(5) . ?
N25 C60 1.342(6) 3_776 ?
N30 C54 1.367(7) 3_776 ?
O1 Pr1 2.397(3) . ?
O2 Pr1 2.509(3) . ?
O1W Pr1 2.930(5) . ?
O2W Pr1 2.574(3) . ?
O3W Pr1 2.408(4) . ?
O4W Pr1 2.499(4) . ?
O6 Pr1 2.466(3) . ?
O13 Pr1 2.499(3) . ?
O14 Pr1 2.463(3) . ?
O21 N37 1.261(10) . ?
O23 N37 1.332(12) . ?
N37 O22 1.344(10) . ?
O24 N38 1.309(11) . ?
O25 N38 1.226(11) . ?
N38 O26 1.335(10) . ?

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 C1 N1 124.7(5) . . ?
O1 C1 N12 124.2(4) . . ?
N1 C1 N12 111.0(4) . . ?
N2 C2 N1 114.7(4) . . ?
O2 C3 N2 125.4(4) . . ?
O2 C3 N3 124.8(4) . . ?
N2 C3 N3 109.7(4) . . ?
N4 C4 N3 113.2(4) . . ?
O3 C5 N5 126.7(5) . . ?
O3 C5 N4 124.7(5) . . ?
N5 C5 N4 108.6(4) . . ?
N5 C6 N6 114.2(4) . . ?
O4 C7 N6 125.3(5) . . ?
O4 C7 N7 126.2(5) . . ?
N6 C7 N7 108.5(4) . . ?
N7 C8 N8 114.9(4) . . ?
O5 C9 N8 126.4(5) . . ?
O5 C9 N9 124.5(5) . . ?
N8 C9 N9 109.1(4) . . ?
N9 C10 N10 113.4(4) . . ?
O6 C11 N10 125.4(4) . . ?
O6 C11 N11 125.2(4) . . ?
N10 C11 N11 109.4(4) . . ?
N11 C12 N12 113.3(4) . . ?
N13 C13 N1 113.4(4) . . ?
N13 C13 C14 112.1(4) . . ?
N1 C13 C14 109.7(4) . . ?
N13 C13 C27 103.0(4) . . ?
N1 C13 C27 102.2(4) . . ?
C14 C13 C27 116.0(4) . . ?
N14 C15 N2 112.9(4) . . ?
N14 C15 C16 103.2(4) . . ?
N2 C15 C16 103.3(4) . . ?
N15 C16 N3 113.8(4) . . ?
N15 C16 C15 103.4(4) . . ?
N3 C16 C15 102.8(4) . . ?
N16 C17 N4 115.2(4) . . ?
N16 C17 C18 102.7(4) . . ?
N4 C17 C18 102.5(4) . . ?
N5 C18 N17 115.0(4) . . ?
N5 C18 C17 104.3(4) . . ?
N17 C18 C17 103.6(4) . . ?
N18 C19 N6 113.3(4) . . ?
N18 C19 C20 111.4(4) . . ?
N6 C19 C20 111.9(4) . . ?
N18 C19 C21 102.2(3) . . ?
N6 C19 C21 102.3(4) . . ?
C20 C19 C21 115.1(4) . . ?
N19 C21 N7 114.4(4) . . ?
N19 C21 C22 110.3(4) . . ?
N7 C21 C22 111.9(4) . . ?
N19 C21 C19 102.4(3) . . ?
N7 C21 C19 102.0(4) . . ?
C22 C21 C19 115.3(4) . . ?
N20 C23 N8 114.9(4) . . ?
N20 C23 C24 104.1(4) . . ?
N8 C23 C24 103.5(4) . . ?
N21 C24 N9 114.8(4) . . ?
N21 C24 C23 102.7(4) . . ?
N9 C24 C23 103.4(4) . . ?
N22 C25 N10 115.0(4) . . ?
N22 C25 C26 103.7(4) . . ?
N10 C25 C26 103.0(4) . . ?
N23 C26 N11 114.9(4) . . ?
N23 C26 C25 102.3(4) . . ?
N11 C26 C25 103.3(4) . . ?
N24 C27 N12 112.2(4) . . ?
N24 C27 C28 112.4(4) . . ?
N12 C27 C28 111.3(4) . . ?
N24 C27 C13 102.3(4) . . ?
N12 C27 C13 102.4(4) . . ?
C28 C27 C13 115.7(4) . . ?
O7 C29 N24 126.1(5) . . ?
O7 C29 N13 124.4(5) . . ?
N24 C29 N13 109.5(4) . . ?
N14 C30 N13 112.9(4) . . ?
O8 C31 N15 125.7(5) . . ?
O8 C31 N14 126.1(5) . . ?
N15 C31 N14 108.2(4) . . ?
N15 C32 N16 113.3(4) . . ?
O9 C33 N16 125.9(4) . . ?
O9 C33 N17 126.3(4) . . ?
N16 C33 N17 107.7(4) . . ?
N17 C34 N18 114.0(4) . . ?
O10 C35 N18 125.1(5) . . ?
O10 C35 N19 125.8(5) . . ?
N18 C35 N19 109.1(4) . . ?
N20 C36 N19 113.8(4) . . ?
O11 C37 N20 126.2(5) . . ?
O11 C37 N21 126.3(5) . . ?
N20 C37 N21 107.4(4) . . ?
N22 C38 N21 114.3(4) . . ?
O12 C39 N22 126.8(5) . . ?
O12 C39 N23 125.9(5) . . ?
N22 C39 N23 107.3(4) . . ?
N23 C40 N24 114.2(4) . . ?
N25 C41 N26 113.0(4) . . ?
O15 C42 N27 126.1(5) . . ?
O15 C42 N26 125.8(5) . . ?
N27 C42 N26 108.0(5) . . ?
N27 C43 N28 114.4(4) . . ?
O16 C44 N29 126.3(6) . . ?
O16 C44 N28 125.3(5) . . ?
N29 C44 N28 108.2(5) . . ?
N29 C45 N30 113.7(4) . . ?
N31 C47 N25 111.9(4) . . ?
N31 C47 C46 111.6(4) . . ?
N25 C47 C46 111.4(4) . . ?
N31 C47 C52 103.3(4) . 3_776 ?
N25 C47 C52 102.8(4) . 3_776 ?
C46 C47 C52 115.4(4) . 3_776 ?
N32 C48 N26 113.5(4) . . ?
N32 C48 C49 102.9(4) . . ?
N26 C48 C49 102.5(4) . . ?
N27 C49 N33 114.9(4) . . ?
N27 C49 C48 103.7(4) . . ?
N33 C49 C48 103.4(4) . . ?
N34 C50 N28 115.4(4) . . ?
N34 C50 C51 102.9(4) . . ?
N28 C50 C51 102.5(4) . . ?
N35 C51 N29 114.9(4) . . ?
N35 C51 C50 103.7(4) . . ?
N29 C51 C50 103.8(4) . . ?
N36 C52 N30 112.3(4) . . ?
N36 C52 C53 110.8(4) . . ?
N30 C52 C53 113.0(4) . . ?
N36 C52 C47 102.4(4) . 3_776 ?
N30 C52 C47 102.0(4) . 3_776 ?
C53 C52 C47 115.6(4) . 3_776 ?
O17 C54 N31 126.5(6) . . ?
O17 C54 N30 124.2(6) . 3_776 ?
N31 C54 N30 109.3(5) . 3_776 ?
N31 C55 N32 114.2(4) . . ?
O18 C56 N33 125.9(5) . . ?
O18 C56 N32 126.2(5) . . ?
N33 C56 N32 107.9(5) . . ?
N33 C57 N34 114.0(4) . . ?
O13 C58 N35 126.2(4) . . ?
O13 C58 N34 125.1(5) . . ?
N35 C58 N34 108.7(4) . . ?
N35 C59 N36 114.4(4) . . ?
O14 C60 N25 124.9(4) . 3_776 ?
O14 C60 N36 124.3(4) . . ?
N25 C60 N36 110.8(4) 3_776 . ?
C1 N1 C2 121.1(4) . . ?
C1 N1 C13 112.1(4) . . ?
C2 N1 C13 126.8(4) . . ?
C3 N2 C2 125.0(4) . . ?
C3 N2 C15 112.2(4) . . ?
C2 N2 C15 122.7(4) . . ?
C3 N3 C4 122.5(4) . . ?
C3 N3 C16 111.3(4) . . ?
C4 N3 C16 120.7(4) . . ?
C5 N4 C4 121.6(4) . . ?
C5 N4 C17 111.9(4) . . ?
C4 N4 C17 123.8(4) . . ?
C5 N5 C6 123.5(4) . . ?
C5 N5 C18 111.9(4) . . ?
C6 N5 C18 124.2(4) . . ?
C7 N6 C6 120.1(4) . . ?
C7 N6 C19 113.6(4) . . ?
C6 N6 C19 126.0(4) . . ?
C7 N7 C8 120.4(4) . . ?
C7 N7 C21 113.5(4) . . ?
C8 N7 C21 124.8(4) . . ?
C9 N8 C23 112.3(4) . . ?
C9 N8 C8 122.9(4) . . ?
C23 N8 C8 123.3(4) . . ?
C9 N9 C10 121.8(4) . . ?
C9 N9 C24 110.8(4) . . ?
C10 N9 C24 121.7(4) . . ?
C11 N10 C10 121.9(4) . . ?
C11 N10 C25 111.8(4) . . ?
C10 N10 C25 122.0(4) . . ?
C11 N11 C26 111.7(4) . . ?
C11 N11 C12 124.5(4) . . ?
C26 N11 C12 123.1(4) . . ?
C1 N12 C12 121.4(4) . . ?
C1 N12 C27 111.9(4) . . ?
C12 N12 C27 126.3(4) . . ?
C29 N13 C13 112.4(4) . . ?
C29 N13 C30 121.2(4) . . ?
C13 N13 C30 126.3(4) . . ?
C31 N14 C30 122.1(4) . . ?
C31 N14 C15 111.1(4) . . ?
C30 N14 C15 123.1(4) . . ?
C31 N15 C16 112.3(4) . . ?
C31 N15 C32 123.0(4) . . ?
C16 N15 C32 123.6(4) . . ?
C33 N16 C17 113.1(4) . . ?
C33 N16 C32 122.9(4) . . ?
C17 N16 C32 122.9(4) . . ?
C33 N17 C18 112.1(4) . . ?
C33 N17 C34 122.0(4) . . ?
C18 N17 C34 122.7(4) . . ?
C35 N18 C34 120.9(4) . . ?
C35 N18 C19 113.0(4) . . ?
C34 N18 C19 125.8(4) . . ?
C35 N19 C21 112.9(4) . . ?
C35 N19 C36 120.0(4) . . ?
C21 N19 C36 126.0(4) . . ?
C37 N20 C36 123.5(4) . . ?
C37 N20 C23 112.3(4) . . ?
C36 N20 C23 124.0(4) . . ?
C37 N21 C24 113.1(4) . . ?
C37 N21 C38 122.1(4) . . ?
C24 N21 C38 124.2(4) . . ?
C39 N22 C25 112.7(4) . . ?
C39 N22 C38 122.5(4) . . ?
C25 N22 C38 123.5(4) . . ?
C39 N23 C26 112.7(4) . . ?
C39 N23 C40 122.7(4) . . ?
C26 N23 C40 122.1(4) . . ?
C29 N24 C40 120.4(4) . . ?
C29 N24 C27 112.4(4) . . ?
C40 N24 C27 125.5(4) . . ?
C60 N25 C41 121.6(4) 3_776 . ?
C60 N25 C47 111.4(4) 3_776 . ?
C41 N25 C47 125.2(4) . . ?
C42 N26 C41 122.3(4) . . ?
C42 N26 C48 112.3(4) . . ?
C41 N26 C48 122.1(4) . . ?
C42 N27 C43 122.2(4) . . ?
C42 N27 C49 113.0(4) . . ?
C43 N27 C49 123.4(4) . . ?
C44 N28 C50 112.9(4) . . ?
C44 N28 C43 122.7(4) . . ?
C50 N28 C43 123.7(5) . . ?
C44 N29 C51 112.6(5) . . ?
C44 N29 C45 123.5(5) . . ?
C51 N29 C45 123.9(4) . . ?
C54 N30 C45 120.2(5) 3_776 . ?
C54 N30 C52 112.2(4) 3_776 . ?
C45 N30 C52 126.4(4) . . ?
C54 N31 C55 119.2(5) . . ?
C54 N31 C47 112.6(4) . . ?
C55 N31 C47 128.2(4) . . ?
C56 N32 C48 112.8(4) . . ?
C56 N32 C55 123.9(4) . . ?
C48 N32 C55 121.4(4) . . ?
C56 N33 C57 121.8(4) . . ?
C56 N33 C49 112.6(4) . . ?
C57 N33 C49 122.4(4) . . ?
C58 N34 C50 111.9(4) . . ?
C58 N34 C57 122.9(4) . . ?
C50 N34 C57 122.4(4) . . ?
C58 N35 C59 123.4(4) . . ?
C58 N35 C51 112.0(4) . . ?
C59 N35 C51 123.2(4) . . ?
C60 N36 C59 122.0(4) . . ?
C60 N36 C52 111.9(4) . . ?
C59 N36 C52 124.8(4) . . ?
C1 O1 Pr1 139.3(3) . . ?
C3 O2 Pr1 149.2(3) . . ?
C11 O6 Pr1 144.7(3) . . ?
C58 O13 Pr1 154.2(3) . . ?
C60 O14 Pr1 158.3(3) . . ?
O1 Pr1 O3W 137.52(12) . . ?
O1 Pr1 O14 142.63(10) . . ?
O3W Pr1 O14 71.12(11) . . ?
O1 Pr1 O6 78.08(11) . . ?
O3W Pr1 O6 75.66(12) . . ?
O14 Pr1 O6 139.24(10) . . ?
O1 Pr1 O13 81.34(10) . . ?
O3W Pr1 O13 94.23(13) . . ?
O14 Pr1 O13 71.40(10) . . ?
O6 Pr1 O13 134.83(11) . . ?
O1 Pr1 O4W 131.42(11) . . ?
O3W Pr1 O4W 76.73(14) . . ?
O14 Pr1 O4W 68.05(11) . . ?
O6 Pr1 O4W 81.99(11) . . ?
O13 Pr1 O4W 139.24(11) . . ?
O1 Pr1 O2 75.67(11) . . ?
O3W Pr1 O2 146.14(11) . . ?
O14 Pr1 O2 76.13(10) . . ?
O6 Pr1 O2 128.53(10) . . ?
O13 Pr1 O2 83.19(10) . . ?
O4W Pr1 O2 83.37(12) . . ?
O1 Pr1 O2W 70.69(11) . . ?
O3W Pr1 O2W 68.88(13) . . ?
O14 Pr1 O2W 118.08(11) . . ?
O6 Pr1 O2W 68.64(11) . . ?
O13 Pr1 O2W 66.70(10) . . ?
O4W Pr1 O2W 138.99(12) . . ?
O2 Pr1 O2W 137.35(11) . . ?
O1 Pr1 O1W 68.63(12) . . ?
O3W Pr1 O1W 126.26(14) . . ?
O14 Pr1 O1W 118.45(12) . . ?
O6 Pr1 O1W 65.49(11) . . ?
O13 Pr1 O1W 139.50(11) . . ?
O4W Pr1 O1W 62.79(12) . . ?
O2 Pr1 O1W 63.91(11) . . ?
O2W Pr1 O1W 123.16(11) . . ?
O21 N37 O23 129.0(12) . . ?
O21 N37 O22 116.2(12) . . ?
O23 N37 O22 114.6(11) . . ?
O25 N38 O24 102.9(11) . . ?
O25 N38 O26 135.9(14) . . ?
O24 N38 O26 121.1(13) . . ?

_refine_diff_density_max         0.638
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.073



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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1038169'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_3                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 

This distances substantially below 2.65 Angstroms correspond to atoms that 
are half occupied due to disorder. These are not meaningful contacts. 
;




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
1 0.500 -0.113 0.000 122.5 11.2
2 0.310 -0.055 0.500 1028.3 460.5
3 0.000 0.387 0.000 122.4 11.2
_platon_squeeze_details          
;
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 N24 O34 Pr'
_chemical_formula_weight         1545.90

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.63(2)
_cell_length_b                   12.723(14)
_cell_length_c                   14.913(16)
_cell_angle_alpha                90
_cell_angle_beta                 116.085(10)
_cell_angle_gamma                90
_cell_volume                     3856(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6134
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      25.67

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_F_000             1566
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.724
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10024
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.520
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             3593
_reflns_number_gt                3435
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1524P)²+13.4130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3593
_refine_ls_number_parameters     249
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0707
_refine_ls_wR_factor_ref         0.2239
_refine_ls_wR_factor_gt          0.2198
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.153
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.5940(9) 0.5000 0.1231(14) 0.161(6) Uiso 1 2 d S . P . .
O2W O 1.0029(7) 0.9535(11) 0.8094(10) 0.086(4) Uiso 0.5 1 d . . P . .
O3W O 1.0000 0.679(2) 1.0000 0.233(10) Uiso 1 2 d S . P . .
O4W O 0.8185(11) 0.5000 0.8917(16) 0.182(7) Uiso 1 2 d S . P . .
O5W O 1.1381(18) 1.0000 0.940(3) 0.300(15) Uiso 1 2 d S . P . .
O6W O 0.8199(9) 0.9541(14) 0.1939(14) 0.123(6) Uiso 0.5 1 d . . P . .
O7W O 1.2844(11) 0.3126(19) 0.9739(17) 0.146(7) Uiso 0.5 1 d . . P . .
Pr1 Pr 1.0000 1.0000 0.5000 0.0331(3) Uani 1 4 d S T P . .
N1 N 0.7725(3) 0.4030(4) 0.4143(4) 0.0426(11) Uani 1 1 d . . . . .
N2 N 0.8200(2) 0.4030(4) 0.5795(4) 0.0405(11) Uani 1 1 d . . . . .
N3 N 0.9251(3) 0.4038(4) 0.7317(4) 0.0431(12) Uani 1 1 d . . . . .
N4 N 1.0348(2) 0.4036(4) 0.8099(4) 0.0417(11) Uani 1 1 d . . . . .
N5 N 1.1430(3) 0.4038(4) 0.8109(4) 0.0423(11) Uani 1 1 d . . . . .
N6 N 1.2084(3) 0.4041(4) 0.7347(4) 0.0432(11) Uani 1 1 d . . . . .
O1 O 0.8348(2) 0.2592(3) 0.4973(4) 0.0535(11) Uani 1 1 d . . . . .
O2 O 0.9812(3) 0.2578(4) 0.7161(5) 0.0711(16) Uani 1 1 d . . . . .
O3 O 1.1421(3) 0.2597(4) 0.7162(5) 0.0689(15) Uani 1 1 d . . . . .
O4 O 0.9034(5) 0.9318(7) 0.3538(8) 0.067(3) Uani 0.5 1 d . . P A 1
O6 O 0.9513(5) 0.8505(8) 0.5513(8) 0.061(3) Uani 0.5 1 d . . P A 1
O5 O 0.9213(5) 0.8506(8) 0.4475(7) 0.056(2) Uani 0.5 1 d . . P B 2
O7 O 0.9903(6) 0.9308(7) 0.6484(8) 0.063(3) Uani 0.5 1 d . . P A 2
C1 C 0.8120(3) 0.3471(4) 0.4971(5) 0.0393(12) Uani 1 1 d . . . . .
C2 C 0.7803(4) 0.5000 0.5552(7) 0.0378(17) Uani 1 2 d S T P . .
C3 C 0.7464(4) 0.5000 0.4379(7) 0.0371(17) Uani 1 2 d S T P . .
C4 C 0.8588(3) 0.3606(5) 0.6805(5) 0.0442(14) Uani 1 1 d . . . . .
H4A H 0.8355 0.3748 0.7205 0.053 Uiso 1 1 calc R U . . .
H4B H 0.8619 0.2850 0.6760 0.053 Uiso 1 1 calc R U . . .
C5 C 0.9809(3) 0.3474(5) 0.7492(5) 0.0432(13) Uani 1 1 d . . . . .
C6 C 1.0165(4) 0.5000 0.8449(6) 0.0372(17) Uani 1 2 d S T P . .
H6 H 1.0326 0.5000 0.9176 0.045 Uiso 1 2 calc R U P . .
C7 C 0.9405(4) 0.5000 0.7903(6) 0.0386(18) Uani 1 2 d S T P . .
H7 H 0.9212 0.5000 0.8376 0.046 Uiso 1 2 calc R U P . .
C8 C 1.1009(3) 0.3602(5) 0.8534(5) 0.0425(13) Uani 1 1 d . . . . .
H8A H 1.0980 0.2846 0.8437 0.051 Uiso 1 1 calc R U . . .
H8B H 1.1212 0.3734 0.9247 0.051 Uiso 1 1 calc R U . . .
C9 C 1.1620(3) 0.3472(5) 0.7496(5) 0.0439(14) Uani 1 1 d . . . . .
C10 C 1.2263(4) 0.5000 0.7942(6) 0.0404(18) Uani 1 2 d S T P . .
H10 H 1.2728 0.5000 0.8426 0.048 Uiso 1 2 calc R U P . .
C11 C 1.1809(4) 0.5000 0.8462(6) 0.0370(17) Uani 1 2 d S T P . .
H11 H 1.2062 0.5000 0.9190 0.044 Uiso 1 2 calc R U P . .
C12 C 0.7538(3) 0.3609(5) 0.3146(5) 0.0452(14) Uani 1 1 d . . . . .
H12A H 0.7075 0.3752 0.2737 0.054 Uiso 1 1 calc R U . . .
H12B H 0.7595 0.2852 0.3193 0.054 Uiso 1 1 calc R U . . .
C13 C 0.7326(5) 0.5000 0.6037(8) 0.056(2) Uani 1 2 d S T P . .
H13A H 0.7144 0.4309 0.5991 0.083 Uiso 0.5 1 calc R U P . .
H13B H 0.6977 0.5492 0.5695 0.083 Uiso 0.5 1 calc R U P . .
H13C H 0.7559 0.5199 0.6726 0.083 Uiso 0.5 1 calc R U P . .
C14 C 0.6708(5) 0.5000 0.3893(8) 0.057(2) Uani 1 2 d S T P . .
H14A H 0.6553 0.4306 0.3928 0.086 Uiso 0.5 1 calc R U P . .
H14B H 0.6543 0.5210 0.3207 0.086 Uiso 0.5 1 calc R U P . .
H14C H 0.6557 0.5484 0.4240 0.086 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2W O2W 1.18(3) 6_575 ?
O6W O6W 1.17(4) 6_575 ?
Pr1 O4 2.468(9) . ?
Pr1 O4 2.468(9) 5_776 ?
Pr1 O4 2.468(9) 6_575 ?
Pr1 O4 2.468(9) 2_756 ?
Pr1 O7 2.479(9) 6_575 ?
Pr1 O7 2.479(9) 2_756 ?
Pr1 O7 2.479(9) 5_776 ?
Pr1 O7 2.479(9) . ?
Pr1 O6 2.483(9) 5_776 ?
Pr1 O6 2.483(9) 2_756 ?
Pr1 O6 2.483(9) 6_575 ?
Pr1 O6 2.483(9) . ?
N1 C1 1.364(8) . ?
N1 C12 1.457(8) . ?
N1 C3 1.476(7) . ?
N2 C1 1.361(8) . ?
N2 C4 1.473(8) . ?
N2 C2 1.475(6) . ?
N3 C5 1.375(8) . ?
N3 C7 1.455(7) . ?
N3 C4 1.458(8) . ?
N4 C5 1.359(8) . ?
N4 C8 1.452(8) . ?
N4 C6 1.462(7) . ?
N5 C9 1.372(8) . ?
N5 C11 1.454(7) . ?
N5 C8 1.467(8) . ?
N6 C9 1.372(8) . ?
N6 C12 1.458(8) 2_756 ?
N6 C10 1.458(7) . ?
O1 C1 1.230(7) . ?
O2 C5 1.244(8) . ?
O3 C9 1.222(8) . ?
O4 O4 1.736(18) 6_575 ?
O7 O7 1.760(18) 6_575 ?
C2 N2 1.475(6) 6_565 ?
C2 C13 1.541(12) . ?
C2 C3 1.571(13) . ?
C3 N1 1.476(7) 6_565 ?
C3 C14 1.536(12) . ?
C6 N4 1.462(7) 6_565 ?
C6 C7 1.545(12) . ?
C7 N3 1.455(7) 6_565 ?
C10 N6 1.458(7) 6_565 ?
C10 C11 1.535(12) . ?
C11 N5 1.454(7) 6_565 ?
C12 N6 1.458(8) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Pr1 O4 180.0 . 5_776 ?
O4 Pr1 O4 41.2(4) . 6_575 ?
O4 Pr1 O4 138.8(4) 5_776 6_575 ?
O4 Pr1 O4 138.8(4) . 2_756 ?
O4 Pr1 O4 41.2(4) 5_776 2_756 ?
O4 Pr1 O4 180.0 6_575 2_756 ?
O7 Pr1 O7 180.0 6_575 2_756 ?
O7 Pr1 O7 138.4(4) 6_575 5_776 ?
O7 Pr1 O7 41.6(4) 2_756 5_776 ?
O7 Pr1 O7 41.6(4) 6_575 . ?
O7 Pr1 O7 138.4(4) 2_756 . ?
O7 Pr1 O7 180.0 5_776 . ?
O4 Pr1 O6 109.8(4) . 5_776 ?
O4 Pr1 O6 70.2(4) 5_776 5_776 ?
O4 Pr1 O6 78.4(4) 6_575 5_776 ?
O4 Pr1 O6 101.6(4) 2_756 5_776 ?
O4 Pr1 O6 78.4(4) . 2_756 ?
O4 Pr1 O6 101.6(4) 5_776 2_756 ?
O4 Pr1 O6 109.8(4) 6_575 2_756 ?
O4 Pr1 O6 70.2(4) 2_756 2_756 ?
O6 Pr1 O6 100.0(5) 5_776 2_756 ?
O4 Pr1 O6 101.6(4) . 6_575 ?
O4 Pr1 O6 78.4(4) 5_776 6_575 ?
O4 Pr1 O6 70.2(4) 6_575 6_575 ?
O4 Pr1 O6 109.8(4) 2_756 6_575 ?
O6 Pr1 O6 80.0(5) 5_776 6_575 ?
O6 Pr1 O6 180.0 2_756 6_575 ?
O4 Pr1 O6 70.2(4) . . ?
O4 Pr1 O6 109.8(4) 5_776 . ?
O4 Pr1 O6 101.6(4) 6_575 . ?
O4 Pr1 O6 78.4(4) 2_756 . ?
O6 Pr1 O6 180.0 5_776 . ?
O6 Pr1 O6 80.0(5) 2_756 . ?
O6 Pr1 O6 100.0(5) 6_575 . ?
C1 N1 C12 120.8(5) . . ?
C1 N1 C3 113.1(5) . . ?
C12 N1 C3 125.7(6) . . ?
C1 N2 C4 121.0(5) . . ?
C1 N2 C2 113.0(5) . . ?
C4 N2 C2 125.6(6) . . ?
C5 N3 C7 111.5(6) . . ?
C5 N3 C4 123.4(5) . . ?
C7 N3 C4 123.5(6) . . ?
C5 N4 C8 122.9(5) . . ?
C5 N4 C6 111.5(5) . . ?
C8 N4 C6 123.9(5) . . ?
C9 N5 C11 112.0(6) . . ?
C9 N5 C8 122.9(5) . . ?
C11 N5 C8 123.7(6) . . ?
C9 N6 C12 123.0(5) . 2_756 ?
C9 N6 C10 111.7(6) . . ?
C12 N6 C10 123.7(6) 2_756 . ?
O4 O4 Pr1 69.4(2) 6_575 . ?
O7 O7 Pr1 69.2(2) 6_575 . ?
O1 C1 N2 125.8(6) . . ?
O1 C1 N1 125.6(6) . . ?
N2 C1 N1 108.6(5) . . ?
N2 C2 N2 113.5(7) 6_565 . ?
N2 C2 C13 111.2(5) 6_565 . ?
N2 C2 C13 111.2(5) . . ?
N2 C2 C3 102.7(5) 6_565 . ?
N2 C2 C3 102.7(5) . . ?
C13 C2 C3 115.0(7) . . ?
N1 C3 N1 113.4(7) 6_565 . ?
N1 C3 C14 111.5(5) 6_565 . ?
N1 C3 C14 111.5(5) . . ?
N1 C3 C2 102.4(5) 6_565 . ?
N1 C3 C2 102.4(5) . . ?
C14 C3 C2 115.0(7) . . ?
N3 C4 N2 114.2(5) . . ?
O2 C5 N4 125.9(6) . . ?
O2 C5 N3 124.6(6) . . ?
N4 C5 N3 109.4(5) . . ?
N4 C6 N4 114.0(7) 6_565 . ?
N4 C6 C7 103.7(4) 6_565 . ?
N4 C6 C7 103.7(4) . . ?
N3 C7 N3 114.6(7) 6_565 . ?
N3 C7 C6 103.6(5) 6_565 . ?
N3 C7 C6 103.6(5) . . ?
N4 C8 N5 113.6(5) . . ?
O3 C9 N6 125.8(6) . . ?
O3 C9 N5 125.6(6) . . ?
N6 C9 N5 108.6(5) . . ?
N6 C10 N6 113.7(7) 6_565 . ?
N6 C10 C11 103.8(5) 6_565 . ?
N6 C10 C11 103.8(5) . . ?
N5 C11 N5 114.7(7) . 6_565 ?
N5 C11 C10 103.7(5) . . ?
N5 C11 C10 103.7(5) 6_565 . ?
N1 C12 N6 113.9(5) . 2_756 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N2 C1 O1 0.2(9) . . . . ?
C2 N2 C1 O1 -173.1(6) . . . . ?
C4 N2 C1 N1 178.0(5) . . . . ?
C2 N2 C1 N1 4.8(7) . . . . ?
C12 N1 C1 O1 -0.5(9) . . . . ?
C3 N1 C1 O1 172.9(6) . . . . ?
C12 N1 C1 N2 -178.3(5) . . . . ?
C3 N1 C1 N2 -4.9(7) . . . . ?
C1 N2 C2 N2 -112.8(6) . . . 6_565 ?
C4 N2 C2 N2 74.3(9) . . . 6_565 ?
C1 N2 C2 C13 120.8(7) . . . . ?
C4 N2 C2 C13 -52.1(8) . . . . ?
C1 N2 C2 C3 -2.8(7) . . . . ?
C4 N2 C2 C3 -175.6(5) . . . . ?
C1 N1 C3 N1 112.6(6) . . . 6_565 ?
C12 N1 C3 N1 -74.3(9) . . . 6_565 ?
C1 N1 C3 C14 -120.5(7) . . . . ?
C12 N1 C3 C14 52.6(9) . . . . ?
C1 N1 C3 C2 3.0(7) . . . . ?
C12 N1 C3 C2 176.0(5) . . . . ?
N2 C2 C3 N1 0.1(6) 6_565 . . 6_565 ?
N2 C2 C3 N1 -117.9(5) . . . 6_565 ?
C13 C2 C3 N1 121.1(4) . . . 6_565 ?
N2 C2 C3 N1 117.9(5) 6_565 . . . ?
N2 C2 C3 N1 -0.1(6) . . . . ?
C13 C2 C3 N1 -121.1(4) . . . . ?
N2 C2 C3 C14 -121.0(4) 6_565 . . . ?
N2 C2 C3 C14 121.0(4) . . . . ?
C13 C2 C3 C14 0.000(2) . . . . ?
C5 N3 C4 N2 -108.7(7) . . . . ?
C7 N3 C4 N2 86.9(7) . . . . ?
C1 N2 C4 N3 101.5(6) . . . . ?
C2 N2 C4 N3 -86.2(7) . . . . ?
C8 N4 C5 O2 -7.1(10) . . . . ?
C6 N4 C5 O2 -172.8(7) . . . . ?
C8 N4 C5 N3 171.4(5) . . . . ?
C6 N4 C5 N3 5.7(7) . . . . ?
C7 N3 C5 O2 173.0(7) . . . . ?
C4 N3 C5 O2 6.9(10) . . . . ?
C7 N3 C5 N4 -5.5(7) . . . . ?
C4 N3 C5 N4 -171.6(5) . . . . ?
C5 N4 C6 N4 -115.6(6) . . . 6_565 ?
C8 N4 C6 N4 78.9(8) . . . 6_565 ?
C5 N4 C6 C7 -3.5(7) . . . . ?
C8 N4 C6 C7 -169.1(5) . . . . ?
C5 N3 C7 N3 115.1(7) . . . 6_565 ?
C4 N3 C7 N3 -78.8(9) . . . 6_565 ?
C5 N3 C7 C6 3.1(7) . . . . ?
C4 N3 C7 C6 169.1(6) . . . . ?
N4 C6 C7 N3 -0.2(6) 6_565 . . 6_565 ?
N4 C6 C7 N3 -119.6(5) . . . 6_565 ?
N4 C6 C7 N3 119.6(5) 6_565 . . . ?
N4 C6 C7 N3 0.2(6) . . . . ?
C5 N4 C8 N5 109.6(6) . . . . ?
C6 N4 C8 N5 -86.5(7) . . . . ?
C9 N5 C8 N4 -108.8(6) . . . . ?
C11 N5 C8 N4 86.0(7) . . . . ?
C12 N6 C9 O3 -7.5(10) 2_756 . . . ?
C10 N6 C9 O3 -173.4(7) . . . . ?
C12 N6 C9 N5 170.7(5) 2_756 . . . ?
C10 N6 C9 N5 4.8(7) . . . . ?
C11 N5 C9 O3 173.8(7) . . . . ?
C8 N5 C9 O3 7.0(10) . . . . ?
C11 N5 C9 N6 -4.5(7) . . . . ?
C8 N5 C9 N6 -171.2(5) . . . . ?
C9 N6 C10 N6 -115.4(7) . . . 6_565 ?
C12 N6 C10 N6 78.9(9) 2_756 . . 6_565 ?
C9 N6 C10 C11 -3.2(7) . . . . ?
C12 N6 C10 C11 -169.0(5) 2_756 . . . ?
C9 N5 C11 N5 114.7(7) . . . 6_565 ?
C8 N5 C11 N5 -78.7(8) . . . 6_565 ?
C9 N5 C11 C10 2.4(7) . . . . ?
C8 N5 C11 C10 169.0(5) . . . . ?
N6 C10 C11 N5 119.6(5) 6_565 . . . ?
N6 C10 C11 N5 0.5(6) . . . . ?
N6 C10 C11 N5 -0.5(6) 6_565 . . 6_565 ?
N6 C10 C11 N5 -119.6(5) . . . 6_565 ?
C1 N1 C12 N6 -101.0(7) . . . 2_756 ?
C3 N1 C12 N6 86.5(7) . . . 2_756 ?

_refine_diff_density_max         1.474
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.200

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

data_4pp
_database_code_depnum_ccdc_archive 'CCDC 1038170'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_4pp                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) 
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_4pp                 
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. O1wa and O1wb are half occupied
so the short contact between them is meaningless. 
;

_vrf_PLAT241_4pp                 
;
PROBLEM:  'MainMol' Ueq as Compared to Neighbors of         O5 Check 
RESPONSE: This is the oxygen atom of a bound bidentate nitrogen atom. 
This would be expected to have a smaller adp than the nitrogen on chemical
grounds. 
;



_vrf_PLAT242_4pp                 
;
PROBLEM:  'MainMol' Ueq as Compared to Neighbors of          Check N7
RESPONSE: This is the central nitrogen of a nitrate group. The surrounding
atoms almost always have larger adps than this atom. 
;


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
1 0.250 -0.053 -0.007 713.7 236.6
2 0.750 -0.057 -0.014 713.7 236.5
_platon_squeeze_details          
;
;


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H46 Cl2 N26 Nd2 O30'
_chemical_formula_weight         1730.41

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           53
_space_group_name_H-M_alt        'P m n a'
_space_group_name_Hall           '-P 2ac 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.819(15)
_cell_length_b                   10.779(6)
_cell_length_c                   14.304(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3981(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1311
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      21.44

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_F_000             1724
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.443
_shelx_estimated_absorpt_T_min   0.697
_shelx_estimated_absorpt_T_max   0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14037
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.628
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             3634
_reflns_number_gt                2304
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1918P)²+21.0285P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3634
_refine_ls_number_parameters     241
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.3194
_refine_ls_wR_factor_gt          0.2810
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.075
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1WA O 0.2300(11) 1.272(2) 0.123(2) 0.107(8) Uiso 0.5 1 d . . P . .
O1WB O 0.1958(11) 1.134(3) 0.026(2) 0.133(10) Uiso 0.5 1 d . . P . .
O4WA O 0.2500 0.879(3) 0.2500 0.047(5) Uiso 0.40(3) 2 d S U P A 1
O4WB O 0.2281(10) 0.879(2) 0.2126(19) 0.047(5) Uiso 0.302(13) 1 d . U P A 2
C1 C 0.0000 0.9807(18) 0.1611(11) 0.057(5) Uani 1 2 d S T P . .
H1 H 0.0000 0.9971 0.2285 0.069 Uiso 1 2 calc R U P . .
C2 C 0.0943(5) 0.9962(13) 0.1640(8) 0.055(3) Uani 1 1 d . . . . .
H2A H 0.0929 0.9094 0.1463 0.066 Uiso 1 1 calc R U . . .
H2B H 0.1185 1.0371 0.1223 0.066 Uiso 1 1 calc R U . . .
C3 C 0.1137(4) 0.9106(11) 0.3182(7) 0.044(3) Uani 1 1 d . . . . .
C4 C 0.1658(5) 0.8417(11) 0.4541(8) 0.052(3) Uani 1 1 d . . . . .
H4A H 0.1572 0.7608 0.4288 0.062 Uiso 1 1 calc R U . . .
H4B H 0.2032 0.8499 0.4535 0.062 Uiso 1 1 calc R U . . .
C5 C 0.1214(5) 0.7543(10) 0.5923(9) 0.050(3) Uani 1 1 d . . . . .
C6 C 0.0562(6) 1.2291(11) 0.0508(9) 0.057(3) Uani 1 1 d . . . . .
H6A H 0.0930 1.2183 0.0560 0.086 Uiso 1 1 calc R U . . .
H6B H 0.0484 1.3156 0.0434 0.086 Uiso 1 1 calc R U . . .
H6C H 0.0437 1.1840 -0.0025 0.086 Uiso 1 1 calc R U . . .
C7 C 0.0304(5) 1.1811(10) 0.1376(8) 0.048(3) Uani 1 1 d . . . . .
C8 C 0.1474(5) 1.1063(10) 0.2890(8) 0.052(3) Uani 1 1 d . . . . .
H8 H 0.1754 1.1223 0.2445 0.063 Uiso 1 1 calc R U . . .
C9 C 0.1677(5) 1.0614(10) 0.3841(8) 0.052(3) Uani 1 1 d . . . . .
H9 H 0.2056 1.0561 0.3852 0.063 Uiso 1 1 calc R U . . .
C10 C 0.0000 1.2944(16) 0.2663(11) 0.048(4) Uani 1 2 d S T P . .
C11 C 0.0947(5) 1.2963(11) 0.2456(8) 0.047(3) Uani 1 1 d . . . . .
H11A H 0.1165 1.2984 0.1904 0.056 Uiso 1 1 calc R U . . .
H11B H 0.0925 1.3802 0.2697 0.056 Uiso 1 1 calc R U . . .
N1 N 0.0430(4) 1.0507(9) 0.1504(6) 0.048(2) Uani 1 1 d . . . . .
N2 N 0.1139(4) 1.0050(8) 0.2589(6) 0.047(2) Uani 1 1 d . . . . .
N3 N 0.1432(3) 0.9383(8) 0.3934(6) 0.045(2) Uani 1 1 d . . . . .
N4 N 0.1480(4) 0.8483(8) 0.5484(7) 0.047(2) Uani 1 1 d . . . . .
N5 N 0.0436(4) 1.2568(8) 0.2183(8) 0.048(2) Uani 1 1 d . . . . .
N6 N 0.1191(4) 1.2202(9) 0.3142(7) 0.050(2) Uani 1 1 d . . . . .
O1 O 0.0000 0.8640(9) 0.1762(7) 0.052(3) Uani 1 2 d S T P . .
O2 O 0.0912(3) 0.8110(7) 0.3070(5) 0.051(2) Uani 1 1 d . . . . .
N7 N 0.0000 0.5774(11) 0.1676(9) 0.047(3) Uani 1 2 d S TU P . .
O3 O 0.1058(3) 0.6602(7) 0.5564(5) 0.053(2) Uani 1 1 d . . . . .
O4 O 0.0000 1.3649(11) 0.3345(8) 0.055(3) Uani 1 2 d S T P . .
O3W O 0.0000 0.7773(11) 0.4926(9) 0.060(3) Uani 1 2 d S T P . .
Nd1 Nd 0.0000 0.74814(7) 0.32339(6) 0.0482(4) Uani 1 2 d S T P . .
O2W O -0.0575(4) 0.5848(7) 0.3925(7) 0.068(2) Uani 1 1 d . . . . .
Cl1 Cl 0.0000 1.0025(4) 0.3706(3) 0.0523(10) Uani 1 2 d S T P . .
O6 O 0.0000 0.5122(17) 0.0921(12) 0.125(6) Uani 1 2 d S TU P . .
O5 O 0.0412(5) 0.6083(12) 0.1975(9) 0.103(4) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4WB O4WB 1.56(6) 3 ?
C1 O1 1.28(2) . ?
C1 N1 1.351(14) 8 ?
C1 N1 1.351(14) . ?
C2 N2 1.453(14) . ?
C2 N1 1.462(16) . ?
C3 O2 1.230(13) . ?
C3 N2 1.325(14) . ?
C3 N3 1.351(14) . ?
C4 N4 1.427(15) . ?
C4 N3 1.476(14) . ?
C5 O3 1.206(13) . ?
C5 N6 1.367(16) 4_576 ?
C5 N4 1.375(14) . ?
C6 C7 1.500(17) . ?
C7 N1 1.454(14) . ?
C7 N5 1.455(15) . ?
C7 C7 1.57(2) 8 ?
C8 N2 1.457(15) . ?
C8 N6 1.473(14) . ?
C8 C9 1.535(17) . ?
C9 N4 1.462(15) 4_576 ?
C9 N3 1.476(14) . ?
C10 O4 1.237(19) . ?
C10 N5 1.380(14) 8 ?
C10 N5 1.380(14) . ?
C11 N6 1.425(15) . ?
C11 N5 1.439(15) . ?
N4 C9 1.462(15) 4_576 ?
N6 C5 1.367(16) 4_576 ?
O1 Nd1 2.448(11) . ?
O2 Nd1 2.461(8) . ?
N7 O5 1.195(14) . ?
N7 O5 1.195(14) 8 ?
N7 O6 1.288(19) . ?
N7 Nd1 2.890(13) . ?
O3W Nd1 2.440(13) . ?
Nd1 O2 2.461(8) 8 ?
Nd1 O2W 2.507(9) 8 ?
Nd1 O2W 2.507(9) . ?
Nd1 O5 2.579(12) . ?
Nd1 O5 2.579(12) 8 ?
Nd1 Cl1 2.824(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 124.7(8) . 8 ?
O1 C1 N1 124.7(8) . . ?
N1 C1 N1 110.5(16) 8 . ?
N2 C2 N1 114.4(9) . . ?
O2 C3 N2 126.1(10) . . ?
O2 C3 N3 124.2(10) . . ?
N2 C3 N3 109.7(10) . . ?
N4 C4 N3 113.2(9) . . ?
O3 C5 N6 124.8(11) . 4_576 ?
O3 C5 N4 126.3(12) . . ?
N6 C5 N4 108.7(10) 4_576 . ?
N1 C7 N5 112.9(9) . . ?
N1 C7 C6 109.8(9) . . ?
N5 C7 C6 111.0(10) . . ?
N1 C7 C7 102.9(6) . 8 ?
N5 C7 C7 103.6(6) . 8 ?
C6 C7 C7 116.4(7) . 8 ?
N2 C8 N6 113.8(10) . . ?
N2 C8 C9 103.2(9) . . ?
N6 C8 C9 102.5(9) . . ?
N4 C9 N3 112.9(9) 4_576 . ?
N4 C9 C8 104.8(9) 4_576 . ?
N3 C9 C8 102.5(9) . . ?
O4 C10 N5 124.9(7) . 8 ?
O4 C10 N5 124.9(7) . . ?
N5 C10 N5 109.5(14) 8 . ?
N6 C11 N5 114.9(10) . . ?
C1 N1 C7 111.7(11) . . ?
C1 N1 C2 120.3(11) . . ?
C7 N1 C2 127.5(10) . . ?
C3 N2 C2 123.1(10) . . ?
C3 N2 C8 112.9(9) . . ?
C2 N2 C8 122.1(10) . . ?
C3 N3 C4 122.4(9) . . ?
C3 N3 C9 111.6(9) . . ?
C4 N3 C9 121.2(9) . . ?
C5 N4 C4 123.7(10) . . ?
C5 N4 C9 111.2(10) . 4_576 ?
C4 N4 C9 123.0(10) . 4_576 ?
C10 N5 C11 121.8(10) . . ?
C10 N5 C7 111.6(10) . . ?
C11 N5 C7 126.6(10) . . ?
C5 N6 C11 125.3(10) 4_576 . ?
C5 N6 C8 112.6(9) 4_576 . ?
C11 N6 C8 122.0(10) . . ?
C1 O1 Nd1 130.4(9) . . ?
C3 O2 Nd1 132.7(7) . . ?
O5 N7 O5 126.1(17) . 8 ?
O5 N7 O6 116.9(8) . . ?
O5 N7 O6 116.9(8) 8 . ?
O5 N7 Nd1 63.0(8) . . ?
O5 N7 Nd1 63.0(8) 8 . ?
O6 N7 Nd1 173.5(11) . . ?
O3W Nd1 O1 141.9(3) . . ?
O3W Nd1 O2 93.4(2) . . ?
O1 Nd1 O2 77.16(19) . . ?
O3W Nd1 O2 93.4(2) . 8 ?
O1 Nd1 O2 77.16(19) . 8 ?
O2 Nd1 O2 146.1(4) . 8 ?
O3W Nd1 O2W 72.5(3) . 8 ?
O1 Nd1 O2W 134.2(3) . 8 ?
O2 Nd1 O2W 70.4(3) . 8 ?
O2 Nd1 O2W 142.9(3) 8 8 ?
O3W Nd1 O2W 72.5(3) . . ?
O1 Nd1 O2W 134.2(3) . . ?
O2 Nd1 O2W 142.9(3) . . ?
O2 Nd1 O2W 70.4(3) 8 . ?
O2W Nd1 O2W 72.7(4) 8 . ?
O3W Nd1 O5 140.2(4) . . ?
O1 Nd1 O5 72.4(4) . . ?
O2 Nd1 O5 72.5(4) . . ?
O2 Nd1 O5 119.3(4) 8 . ?
O2W Nd1 O5 67.7(4) 8 . ?
O2W Nd1 O5 96.3(4) . . ?
O3W Nd1 O5 140.2(4) . 8 ?
O1 Nd1 O5 72.4(4) . 8 ?
O2 Nd1 O5 119.3(4) . 8 ?
O2 Nd1 O5 72.5(4) 8 8 ?
O2W Nd1 O5 96.3(4) 8 8 ?
O2W Nd1 O5 67.7(4) . 8 ?
O5 Nd1 O5 48.8(6) . 8 ?
O3W Nd1 Cl1 68.8(3) . . ?
O1 Nd1 Cl1 73.2(2) . . ?
O2 Nd1 Cl1 75.84(18) . . ?
O2 Nd1 Cl1 75.84(18) 8 . ?
O2W Nd1 Cl1 126.0(2) 8 . ?
O2W Nd1 Cl1 126.0(2) . . ?
O5 Nd1 Cl1 137.3(3) . . ?
O5 Nd1 Cl1 137.3(3) 8 . ?
O3W Nd1 N7 147.8(3) . . ?
O1 Nd1 N7 70.2(3) . . ?
O2 Nd1 N7 95.85(19) . . ?
O2 Nd1 N7 95.85(19) 8 . ?
O2W Nd1 N7 81.8(3) 8 . ?
O2W Nd1 N7 81.8(3) . . ?
O5 Nd1 N7 24.4(3) . . ?
O5 Nd1 N7 24.4(3) 8 . ?
Cl1 Nd1 N7 143.4(2) . . ?
N7 O5 Nd1 92.6(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C8 C9 N4 -117.2(9) . . . 4_576 ?
N6 C8 C9 N4 1.3(12) . . . 4_576 ?
N2 C8 C9 N3 1.0(11) . . . . ?
N6 C8 C9 N3 119.4(10) . . . . ?
O1 C1 N1 C7 -177.9(13) . . . . ?
N1 C1 N1 C7 4.2(17) 8 . . . ?
O1 C1 N1 C2 -5(2) . . . . ?
N1 C1 N1 C2 176.7(8) 8 . . . ?
N5 C7 N1 C1 108.5(12) . . . . ?
C6 C7 N1 C1 -127.0(12) . . . . ?
C7 C7 N1 C1 -2.5(10) 8 . . . ?
N5 C7 N1 C2 -63.3(15) . . . . ?
C6 C7 N1 C2 61.2(14) . . . . ?
C7 C7 N1 C2 -174.3(9) 8 . . . ?
N2 C2 N1 C1 -90.6(14) . . . . ?
N2 C2 N1 C7 80.6(14) . . . . ?
O2 C3 N2 C2 -10.6(18) . . . . ?
N3 C3 N2 C2 167.9(10) . . . . ?
O2 C3 N2 C8 -175.6(11) . . . . ?
N3 C3 N2 C8 2.9(13) . . . . ?
N1 C2 N2 C3 102.3(13) . . . . ?
N1 C2 N2 C8 -94.0(13) . . . . ?
N6 C8 N2 C3 -112.6(11) . . . . ?
C9 C8 N2 C3 -2.4(12) . . . . ?
N6 C8 N2 C2 82.2(13) . . . . ?
C9 C8 N2 C2 -167.6(10) . . . . ?
O2 C3 N3 C4 20.8(17) . . . . ?
N2 C3 N3 C4 -157.8(10) . . . . ?
O2 C3 N3 C9 176.3(10) . . . . ?
N2 C3 N3 C9 -2.2(13) . . . . ?
N4 C4 N3 C3 -118.5(11) . . . . ?
N4 C4 N3 C9 88.2(13) . . . . ?
N4 C9 N3 C3 112.9(11) 4_576 . . . ?
C8 C9 N3 C3 0.6(12) . . . . ?
N4 C9 N3 C4 -91.2(12) 4_576 . . . ?
C8 C9 N3 C4 156.5(10) . . . . ?
O3 C5 N4 C4 -6.7(19) . . . . ?
N6 C5 N4 C4 168.3(10) 4_576 . . . ?
O3 C5 N4 C9 -171.2(12) . . . 4_576 ?
N6 C5 N4 C9 3.9(14) 4_576 . . 4_576 ?
N3 C4 N4 C5 119.1(12) . . . . ?
N3 C4 N4 C9 -78.2(13) . . . 4_576 ?
O4 C10 N5 C11 1(2) . . . . ?
N5 C10 N5 C11 172.1(8) 8 . . . ?
O4 C10 N5 C7 -175.9(14) . . . . ?
N5 C10 N5 C7 -5.0(17) 8 . . . ?
N6 C11 N5 C10 87.4(14) . . . . ?
N6 C11 N5 C7 -96.0(13) . . . . ?
N1 C7 N5 C10 -107.7(12) . . . . ?
C6 C7 N5 C10 128.6(12) . . . . ?
C7 C7 N5 C10 2.9(10) 8 . . . ?
N1 C7 N5 C11 75.5(14) . . . . ?
C6 C7 N5 C11 -48.3(15) . . . . ?
C7 C7 N5 C11 -173.9(9) 8 . . . ?
N5 C11 N6 C5 -99.5(15) . . . 4_576 ?
N5 C11 N6 C8 83.9(14) . . . . ?
N2 C8 N6 C5 111.6(12) . . . 4_576 ?
C9 C8 N6 C5 1.0(13) . . . 4_576 ?
N2 C8 N6 C11 -71.4(14) . . . . ?
C9 C8 N6 C11 177.9(10) . . . . ?
N1 C1 O1 Nd1 -91.2(14) 8 . . . ?
N1 C1 O1 Nd1 91.2(14) . . . . ?
N2 C3 O2 Nd1 -78.1(14) . . . . ?
N3 C3 O2 Nd1 103.6(12) . . . . ?
O5 N7 O5 Nd1 -2(2) 8 . . . ?
O6 N7 O5 Nd1 172.7(13) . . . . ?

_refine_diff_density_max         1.992
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.209

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

data_4p
_database_code_depnum_ccdc_archive 'CCDC 1038171'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

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
1 -0.002 -0.015 -0.002 1635.1 598.2
2 0.000 0.500 0.000 115.1 13.3
3 0.121 0.741 0.472 6.4 0.0
4 0.236 0.062 0.837 51.9 8.9
5 0.264 0.562 0.663 51.9 8.9
6 0.379 0.241 0.028 6.8 0.7
7 0.500 1.000 0.500 115.1 13.3
8 0.621 0.759 0.972 6.1 0.0
9 0.736 0.438 0.337 51.9 9.6
10 0.764 0.938 0.163 51.9 9.5
11 0.879 0.259 0.528 6.6 0.6
_platon_squeeze_details          
;
;


_vrf_PLAT306_4p                  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_4p                  
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H126 N78 Nd2 O94'
_chemical_formula_weight         4453.46

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   15.4080(17)
_cell_length_b                   17.0805(19)
_cell_length_c                   35.289(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.8520(10)
_cell_angle_gamma                90
_cell_volume                     9275.6(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9998
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      25.06

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_F_000             4528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.678
_shelx_estimated_absorpt_T_min   0.838
_shelx_estimated_absorpt_T_max   0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48495
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.155
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             16526
_reflns_number_gt                12506
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1635P)²+27.8386P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16526
_refine_ls_number_parameters     1270
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.2487
_refine_ls_wR_factor_gt          0.2276
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.048
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7W O 0.7228(6) 0.8278(6) 0.9657(2) 0.109(3) Uani 1 1 d . . . . .
O8W O 0.5125(9) 0.7034(8) 0.8938(3) 0.160(5) Uani 1 1 d . . . . .
O10W O -0.3744(6) 0.1578(9) 0.7739(3) 0.143(5) Uani 1 1 d . . . . .
O9W O -0.3311(9) -0.0035(8) 0.7791(4) 0.161(5) Uiso 1 1 d . . . . .
O16W O -0.1370(9) 0.2593(9) 0.9722(4) 0.165(5) Uiso 1 1 d . . . . .
O11W O -0.3702(9) 0.3171(8) 0.9133(4) 0.159(5) Uiso 1 1 d . . . . .
O12W O 0.7775(10) 0.0464(9) 0.8922(4) 0.180(5) Uiso 1 1 d . . . . .
O13W O -0.1783(10) 0.4356(10) 0.7941(5) 0.190(6) Uiso 1 1 d . . . . .
O14W O -0.2722(11) 0.2060(9) 0.8832(5) 0.187(6) Uiso 1 1 d . . . . .
O42 O 0.2004(10) 0.0356(10) 0.8231(5) 0.189(6) Uiso 1 1 d . . . . .
O43 O -0.0402(15) -0.1080(14) 0.9870(7) 0.266(9) Uiso 1 1 d . . . . .
N39 N -0.1142(10) 0.0363(11) 0.6324(5) 0.175(7) Uiso 1 1 d D . . . .
O45 O -0.0795(16) 0.0002(13) 0.6040(6) 0.314(12) Uiso 1 1 d D . . . .
O46 O -0.145(2) -0.0108(15) 0.6558(7) 0.406(19) Uiso 1 1 d D . . . .
O44 O -0.1206(12) 0.1033(10) 0.6318(5) 0.230(8) Uiso 1 1 d D . . . .
O26 O 0.2534(5) 0.4969(4) 0.7516(3) 0.118(3) Uani 1 1 d . . . . .
C1 C -0.0568(4) 0.2577(4) 0.78261(18) 0.0297(14) Uani 1 1 d . . . . .
C2 C -0.1520(4) 0.1554(4) 0.80549(19) 0.0305(14) Uani 1 1 d . . . . .
H2A H -0.1679 0.1944 0.8239 0.037 Uiso 1 1 calc R U . . .
H2B H -0.2053 0.1327 0.7946 0.037 Uiso 1 1 calc R U . . .
C3 C -0.0559(4) 0.1045(3) 0.85772(17) 0.0254(13) Uani 1 1 d . . . . .
C4 C -0.0002(4) 0.0221(4) 0.91075(17) 0.0294(13) Uani 1 1 d . . . . .
H4A H -0.0009 0.0722 0.9237 0.035 Uiso 1 1 calc R U . . .
H4B H -0.0409 -0.0122 0.9227 0.035 Uiso 1 1 calc R U . . .
C5 C 0.1500(4) 0.0261(4) 0.93698(17) 0.0277(13) Uani 1 1 d . . . . .
C6 C 0.2859(4) -0.0081(4) 0.97234(17) 0.0315(14) Uani 1 1 d . . . . .
H6A H 0.2993 -0.0547 0.9872 0.038 Uiso 1 1 calc R U . . .
H6B H 0.2674 0.0321 0.9896 0.038 Uiso 1 1 calc R U . . .
C7 C 0.3760(4) 0.0962(4) 0.94790(17) 0.0320(14) Uani 1 1 d . . . . .
C8 C 0.4744(4) 0.1809(4) 0.91482(18) 0.0319(14) Uani 1 1 d . . . . .
H8A H 0.5374 0.1806 0.9169 0.038 Uiso 1 1 calc R U . . .
H8B H 0.4544 0.2182 0.9332 0.038 Uiso 1 1 calc R U . . .
C9 C 0.3775(4) 0.2562(4) 0.86995(18) 0.0301(14) Uani 1 1 d . . . . .
C10 C 0.3231(4) 0.3387(4) 0.81756(18) 0.0320(14) Uani 1 1 d . . . . .
H10A H 0.3609 0.3772 0.8067 0.038 Uiso 1 1 calc R U . . .
H10B H 0.2946 0.3636 0.8383 0.038 Uiso 1 1 calc R U . . .
C11 C 0.1721(4) 0.3283(3) 0.79283(16) 0.0250(13) Uani 1 1 d . . . . .
C12 C 0.0390(4) 0.3470(4) 0.75125(17) 0.0278(13) Uani 1 1 d . . . . .
H12A H 0.0208 0.3828 0.7707 0.033 Uiso 1 1 calc R U . . .
H12B H 0.0311 0.3733 0.7270 0.033 Uiso 1 1 calc R U . . .
C13 C -0.0974(4) 0.1643(4) 0.73668(18) 0.0314(14) Uani 1 1 d . . . . .
C14 C -0.1869(4) 0.1506(5) 0.7173(2) 0.0435(17) Uani 1 1 d . . . . .
H14A H -0.1805 0.1350 0.6915 0.065 Uiso 1 1 calc R U . . .
H14B H -0.2202 0.1981 0.7179 0.065 Uiso 1 1 calc R U . . .
H14C H -0.2164 0.1101 0.7305 0.065 Uiso 1 1 calc R U . . .
C15 C -0.1077(4) 0.0128(4) 0.81331(17) 0.0280(13) Uani 1 1 d . . . . .
H15 H -0.1678 -0.0039 0.8077 0.034 Uiso 1 1 calc R U . . .
C16 C -0.0651(4) -0.0306(3) 0.84778(17) 0.0273(13) Uani 1 1 d . . . . .
H16 H -0.1080 -0.0607 0.8613 0.033 Uiso 1 1 calc R U . . .
C17 C 0.1003(4) -0.0951(4) 0.91450(18) 0.0285(13) Uani 1 1 d . . . . .
H17 H 0.0568 -0.1233 0.9286 0.034 Uiso 1 1 calc R U . . .
C18 C 0.1921(4) -0.1038(3) 0.93347(16) 0.0259(13) Uani 1 1 d . . . . .
H18 H 0.1924 -0.1399 0.9550 0.031 Uiso 1 1 calc R U . . .
C19 C 0.4255(4) -0.0318(4) 0.93616(16) 0.0270(13) Uani 1 1 d . . . . .
C20 C 0.4727(5) -0.0872(4) 0.9638(2) 0.0411(16) Uani 1 1 d . . . . .
H20A H 0.5065 -0.0575 0.9823 0.062 Uiso 1 1 calc R U . . .
H20B H 0.5104 -0.1207 0.9502 0.062 Uiso 1 1 calc R U . . .
H20C H 0.4311 -0.1185 0.9764 0.062 Uiso 1 1 calc R U . . .
C21 C 0.4844(4) 0.0292(4) 0.91558(17) 0.0292(13) Uani 1 1 d . . . . .
C22 C 0.5795(4) 0.0296(5) 0.9297(2) 0.0424(17) Uani 1 1 d . . . . .
H22A H 0.6036 -0.0218 0.9270 0.064 Uiso 1 1 calc R U . . .
H22B H 0.5837 0.0447 0.9559 0.064 Uiso 1 1 calc R U . . .
H22C H 0.6112 0.0662 0.9150 0.064 Uiso 1 1 calc R U . . .
C23 C 0.4910(4) 0.1882(4) 0.84399(18) 0.0299(14) Uani 1 1 d . . . . .
H23 H 0.5535 0.1984 0.8474 0.036 Uiso 1 1 calc R U . . .
C24 C 0.4473(4) 0.2423(4) 0.81299(18) 0.0299(14) Uani 1 1 d . . . . .
H24 H 0.4870 0.2829 0.8046 0.036 Uiso 1 1 calc R U . . .
C25 C 0.2790(4) 0.3112(4) 0.74871(16) 0.0273(13) Uani 1 1 d . . . . .
H25 H 0.3157 0.3549 0.7413 0.033 Uiso 1 1 calc R U . . .
C26 C 0.1879(4) 0.3133(4) 0.72828(18) 0.0293(13) Uani 1 1 d . . . . .
H26 H 0.1839 0.3534 0.7084 0.035 Uiso 1 1 calc R U . . .
C27 C -0.0397(4) 0.2280(4) 0.71837(17) 0.0291(13) Uani 1 1 d . . . . .
C28 C -0.0833(5) 0.2761(4) 0.6866(2) 0.0432(17) Uani 1 1 d . . . . .
H28A H -0.0444 0.3164 0.6790 0.065 Uiso 1 1 calc R U . . .
H28B H -0.1353 0.2995 0.6953 0.065 Uiso 1 1 calc R U . . .
H28C H -0.0979 0.2427 0.6653 0.065 Uiso 1 1 calc R U . . .
C29 C 0.0307(4) 0.1062(4) 0.71627(17) 0.0317(14) Uani 1 1 d . . . . .
C30 C -0.0699(4) 0.0148(4) 0.74440(18) 0.0322(14) Uani 1 1 d . . . . .
H30A H -0.1320 0.0105 0.7388 0.039 Uiso 1 1 calc R U . . .
H30B H -0.0411 -0.0214 0.7280 0.039 Uiso 1 1 calc R U . . .
C31 C 0.0039(4) -0.0673(4) 0.79352(18) 0.0289(13) Uani 1 1 d . . . . .
C32 C 0.0368(4) -0.1473(4) 0.85099(18) 0.0294(14) Uani 1 1 d . . . . .
H32 H 0.0176 -0.1984 0.8470 0.035 Uiso 1 1 calc R U . . .
C33 C 0.1922(4) -0.1510(3) 0.87105(17) 0.0274(13) Uani 1 1 d . . . . .
C34 C 0.3351(4) -0.1470(4) 0.90664(18) 0.0292(13) Uani 1 1 d . . . . .
H34A H 0.3497 -0.1716 0.9309 0.035 Uiso 1 1 calc R U . . .
H34B H 0.3513 -0.1829 0.8869 0.035 Uiso 1 1 calc R U . . .
C35 C 0.4201(4) -0.0555(4) 0.87017(17) 0.0291(13) Uani 1 1 d . . . . .
C36 C 0.5165(4) 0.0424(4) 0.84494(18) 0.0309(14) Uani 1 1 d . . . . .
H36A H 0.5751 0.0569 0.8536 0.037 Uiso 1 1 calc R U . . .
H36B H 0.5212 0.0037 0.8250 0.037 Uiso 1 1 calc R U . . .
C37 C 0.4402(4) 0.1123(4) 0.79222(17) 0.0276(13) Uani 1 1 d . . . . .
C38 C 0.4023(4) 0.2142(4) 0.74436(18) 0.0315(14) Uani 1 1 d . . . . .
H38A H 0.4392 0.2584 0.7389 0.038 Uiso 1 1 calc R U . . .
H38B H 0.4157 0.1723 0.7270 0.038 Uiso 1 1 calc R U . . .
C39 C 0.2560(4) 0.1962(4) 0.71427(17) 0.0301(14) Uani 1 1 d . . . . .
C40 C 0.1064(4) 0.2133(4) 0.68659(18) 0.0318(14) Uani 1 1 d . . . . .
H40A H 0.0882 0.2589 0.6718 0.038 Uiso 1 1 calc R U . . .
H40B H 0.1261 0.1740 0.6691 0.038 Uiso 1 1 calc R U . . .
C41 C 0.2673(5) 0.3443(4) 0.97224(18) 0.0336(14) Uani 1 1 d . . . . .
H41A H 0.2395 0.3002 0.9593 0.040 Uiso 1 1 calc R U . . .
H41B H 0.3285 0.3318 0.9765 0.040 Uiso 1 1 calc R U . . .
C42 C 0.2045(4) 0.4133(3) 0.91717(16) 0.0255(13) Uani 1 1 d . . . . .
C43 C 0.1637(4) 0.4977(4) 0.86323(17) 0.0313(14) Uani 1 1 d . . . . .
H43 H 0.1758 0.4863 0.8383 0.038 Uiso 1 1 calc R U . . .
C44 C 0.0081(4) 0.5028(4) 0.87550(17) 0.0295(14) Uani 1 1 d . . . . .
C45 C -0.1460(4) 0.5434(4) 0.87809(18) 0.0355(15) Uani 1 1 d . . . . .
H45A H -0.1734 0.5773 0.8590 0.043 Uiso 1 1 calc R U . . .
H45B H -0.1550 0.4897 0.8699 0.043 Uiso 1 1 calc R U . . .
C46 C -0.2268(5) 0.4945(4) 0.9317(2) 0.0396(16) Uani 1 1 d . . . . .
C47 C -0.3370(5) 0.4808(5) 0.9809(2) 0.0427(17) Uani 1 1 d . . . . .
H47A H -0.3921 0.5082 0.9799 0.051 Uiso 1 1 calc R U . . .
H47B H -0.3463 0.4303 0.9688 0.051 Uiso 1 1 calc R U . . .
C48 C 0.3208(4) 0.4780(4) 0.94834(18) 0.0312(14) Uani 1 1 d . . . . .
C49 C 0.4141(4) 0.4477(5) 0.9466(2) 0.0437(17) Uani 1 1 d . . . . .
H49A H 0.4307 0.4214 0.9699 0.066 Uiso 1 1 calc R U . . .
H49B H 0.4527 0.4910 0.9430 0.066 Uiso 1 1 calc R U . . .
H49C H 0.4175 0.4119 0.9258 0.066 Uiso 1 1 calc R U . . .
C50 C 0.2863(4) 0.5277(4) 0.91322(19) 0.0339(15) Uani 1 1 d . . . . .
C51 C 0.3552(5) 0.5510(5) 0.8852(2) 0.052(2) Uani 1 1 d . . . . .
H51A H 0.3828 0.5048 0.8761 0.078 Uiso 1 1 calc R U . . .
H51B H 0.3981 0.5840 0.8979 0.078 Uiso 1 1 calc R U . . .
H51C H 0.3279 0.5789 0.8642 0.078 Uiso 1 1 calc R U . . .
C52 C 0.0795(4) 0.6233(4) 0.87146(19) 0.0330(15) Uani 1 1 d . . . . .
H52 H 0.0986 0.6440 0.8474 0.040 Uiso 1 1 calc R U . . .
C53 C -0.0188(4) 0.6376(4) 0.87594(18) 0.0325(14) Uani 1 1 d . . . . .
H53 H -0.0458 0.6640 0.8537 0.039 Uiso 1 1 calc R U . . .
C54 C -0.2179(4) 0.6301(4) 0.92534(18) 0.0335(15) Uani 1 1 d . . . . .
H54 H -0.2510 0.6574 0.9049 0.040 Uiso 1 1 calc R U . . .
C55 C -0.2754(4) 0.6094(4) 0.95883(18) 0.0335(15) Uani 1 1 d . . . . .
H55 H -0.3343 0.6305 0.9549 0.040 Uiso 1 1 calc R U . . .
C56 C 0.2645(5) 0.5973(4) 0.9690(2) 0.0399(17) Uani 1 1 d . . . . .
C57 C 0.2132(5) 0.6650(4) 0.9114(3) 0.0463(19) Uani 1 1 d . . . . .
H57A H 0.2274 0.7108 0.9267 0.056 Uiso 1 1 calc R U . . .
H57B H 0.2417 0.6706 0.8876 0.056 Uiso 1 1 calc R U . . .
C58 C 0.0631(5) 0.7008(4) 0.9248(2) 0.0347(15) Uani 1 1 d . . . . .
C59 C -0.0950(5) 0.7277(4) 0.9213(2) 0.0398(17) Uani 1 1 d . . . . .
H59 H -0.1070 0.7799 0.9155 0.048 Uiso 1 1 calc R U . . .
C60 C -0.1610(4) 0.6900(4) 0.98076(19) 0.0328(15) Uani 1 1 d . . . . .
N1 N -0.1060(3) 0.1940(3) 0.77547(16) 0.0304(12) Uani 1 1 d . . . . .
N2 N -0.1018(3) 0.0950(3) 0.82475(15) 0.0293(11) Uani 1 1 d . . . . .
N3 N -0.0286(3) 0.0332(3) 0.87119(14) 0.0264(11) Uani 1 1 d . . . . .
N4 N 0.0859(3) -0.0110(3) 0.91532(14) 0.0285(11) Uani 1 1 d . . . . .
N5 N 0.2143(3) -0.0256(3) 0.94542(15) 0.0292(11) Uani 1 1 d . . . . .
N6 N 0.3644(3) 0.0182(3) 0.95515(15) 0.0308(12) Uani 1 1 d . . . . .
N7 N 0.4430(3) 0.1040(3) 0.92432(15) 0.0312(12) Uani 1 1 d . . . . .
N8 N 0.4467(4) 0.2072(3) 0.87716(15) 0.0328(12) Uani 1 1 d . . . . .
N9 N 0.3755(4) 0.2747(3) 0.83253(15) 0.0320(12) Uani 1 1 d . . . . .
N10 N 0.2578(3) 0.3152(3) 0.78899(14) 0.0272(11) Uani 1 1 d . . . . .
N11 N 0.1301(3) 0.3295(3) 0.75817(14) 0.0272(11) Uani 1 1 d . . . . .
N12 N -0.0160(4) 0.2787(3) 0.75109(15) 0.0297(12) Uani 1 1 d . . . . .
N13 N -0.0423(3) 0.0940(3) 0.73591(15) 0.0296(11) Uani 1 1 d . . . . .
N14 N -0.0510(3) -0.0075(3) 0.78340(15) 0.0311(12) Uani 1 1 d . . . . .
N15 N -0.0023(3) -0.0807(3) 0.83141(15) 0.0297(11) Uani 1 1 d . . . . .
N16 N 0.1087(3) -0.1275(3) 0.87739(14) 0.0287(11) Uani 1 1 d . . . . .
N17 N 0.2424(3) -0.1341(3) 0.90321(14) 0.0282(11) Uani 1 1 d . . . . .
N18 N 0.3853(3) -0.0760(3) 0.90381(14) 0.0295(11) Uani 1 1 d . . . . .
N19 N 0.4744(3) 0.0066(3) 0.87604(14) 0.0290(11) Uani 1 1 d . . . . .
N20 N 0.4740(3) 0.1103(3) 0.82904(14) 0.0291(11) Uani 1 1 d . . . . .
N21 N 0.4222(3) 0.1882(3) 0.78283(15) 0.0300(12) Uani 1 1 d . . . . .
N22 N 0.3128(3) 0.2368(3) 0.73768(14) 0.0288(11) Uani 1 1 d . . . . .
N23 N 0.1785(3) 0.2350(3) 0.71273(15) 0.0299(11) Uani 1 1 d . . . . .
N24 N 0.0327(4) 0.1829(3) 0.70593(15) 0.0323(12) Uani 1 1 d . . . . .
N25 N 0.2590(3) 0.4125(3) 0.94816(14) 0.0278(11) Uani 1 1 d . . . . .
N26 N 0.2211(3) 0.4762(3) 0.89490(14) 0.0291(11) Uani 1 1 d . . . . .
N27 N 0.0867(4) 0.5378(3) 0.87312(15) 0.0316(12) Uani 1 1 d . . . . .
N28 N -0.0540(4) 0.5594(3) 0.88062(15) 0.0329(12) Uani 1 1 d . . . . .
N29 N -0.1876(4) 0.5548(3) 0.91332(15) 0.0337(12) Uani 1 1 d . . . . .
N30 N -0.2756(4) 0.5252(3) 0.95931(16) 0.0362(13) Uani 1 1 d . . . . .
N31 N 0.3094(4) 0.5318(3) 0.97985(17) 0.0389(13) Uani 1 1 d . . . . .
N32 N 0.2478(4) 0.5952(3) 0.93117(19) 0.0418(14) Uani 1 1 d . . . . .
N33 N 0.1210(4) 0.6632(3) 0.90349(18) 0.0401(14) Uani 1 1 d . . . . .
N34 N -0.0181(4) 0.6871(3) 0.90938(16) 0.0351(13) Uani 1 1 d . . . . .
N35 N -0.1508(4) 0.6797(3) 0.94299(16) 0.0359(13) Uani 1 1 d . . . . .
N36 N -0.2294(4) 0.6453(3) 0.99155(14) 0.0316(12) Uani 1 1 d . . . . .
N37 N 0.8469(6) 0.7943(6) 0.8088(4) 0.083(3) Uani 1 1 d . . . . .
O1 O -0.0519(3) 0.2941(2) 0.81294(13) 0.0314(10) Uani 1 1 d . . . . .
O2 O -0.0422(3) 0.1672(2) 0.87431(13) 0.0327(10) Uani 1 1 d . . . . .
O1W O 0.1599(3) 0.2066(3) 0.89203(16) 0.0461(13) Uani 1 1 d . . . . .
O3 O 0.1478(3) 0.0949(3) 0.94648(14) 0.0409(11) Uani 1 1 d . . . . .
O2W O 0.0127(4) 0.2727(4) 0.93732(14) 0.0562(15) Uani 1 1 d . . . . .
O4 O 0.3351(3) 0.1497(3) 0.96146(14) 0.0407(11) Uani 1 1 d . . . . .
O3W O -0.1237(3) 0.3135(3) 0.88477(15) 0.0425(12) Uani 1 1 d . . . . .
O5 O 0.3285(3) 0.2812(3) 0.89337(13) 0.0398(11) Uani 1 1 d . . . . .
O4W O 0.0914(4) 0.1761(4) 0.81818(19) 0.0679(17) Uani 1 1 d . . . . .
O6 O 0.1373(3) 0.3379(2) 0.82366(12) 0.0312(10) Uani 1 1 d . . . . .
O7 O 0.0842(3) 0.0566(3) 0.70935(14) 0.0403(11) Uani 1 1 d . . . . .
O8 O 0.0499(3) -0.1039(3) 0.77228(13) 0.0370(11) Uani 1 1 d . . . . .
O9 O 0.2164(3) -0.1849(3) 0.84291(13) 0.0375(11) Uani 1 1 d . . . . .
O10 O 0.4057(3) -0.0889(3) 0.83984(12) 0.0390(11) Uani 1 1 d . . . . .
O11 O 0.4288(3) 0.0555(3) 0.77145(12) 0.0369(11) Uani 1 1 d . . . . .
O12 O 0.2724(3) 0.1348(3) 0.69771(13) 0.0366(11) Uani 1 1 d . . . . .
O13 O 0.1478(3) 0.3636(2) 0.90926(12) 0.0301(10) Uani 1 1 d . . . . .
O14 O -0.0060(3) 0.4324(2) 0.87292(13) 0.0327(10) Uani 1 1 d . . . . .
O15 O -0.2187(4) 0.4248(3) 0.92491(16) 0.0537(15) Uani 1 1 d . . . . .
O16 O 0.2458(4) 0.6497(3) 0.99070(19) 0.0633(17) Uani 1 1 d . . . . .
O17 O 0.0806(4) 0.7426(3) 0.95218(15) 0.0464(12) Uani 1 1 d . . . . .
O18 O -0.1168(3) 0.7328(3) 1.00131(14) 0.0438(12) Uani 1 1 d . . . . .
O19 O 0.8991(6) 0.7392(6) 0.7998(3) 0.115(3) Uani 1 1 d . . . . .
O20 O 0.8182(7) 0.8404(5) 0.7835(3) 0.110(3) Uani 1 1 d . . . . .
O21 O 0.8257(5) 0.8001(5) 0.8418(2) 0.086(2) Uani 1 1 d . . . . .
Nd1 Nd 0.03552(2) 0.29194(2) 0.87126(2) 0.02803(15) Uani 1 1 d . . . . .
O17W O 0.7962(5) 0.4224(5) 0.6495(2) 0.081(2) Uani 1 1 d . . . . .
O5W O 0.5168(7) 0.0414(6) 0.7041(2) 0.124(4) Uani 1 1 d . . . . .
O22 O 0.4146(6) 0.7131(5) 0.9573(4) 0.123(4) Uani 1 1 d . . . . .
N38 N 0.4655(6) 0.6844(6) 0.9826(3) 0.080(2) Uani 1 1 d . . . . .
O23 O 0.4569(9) 0.6994(7) 1.0175(3) 0.139(4) Uani 1 1 d . . . . .
O24 O 0.5147(6) 0.6339(7) 0.9702(3) 0.131(4) Uani 1 1 d . . . . .
O6W O 0.6100(7) 0.8362(7) 0.9021(2) 0.125(4) Uani 1 1 d . . . . .
O15W O 0.3106(7) 0.8110(6) 1.0143(3) 0.127(4) 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
N39 O44 1.148(14) . ?
N39 O46 1.265(16) . ?
N39 O45 1.313(15) . ?
C1 O1 1.237(8) . ?
C1 N1 1.343(8) . ?
C1 N12 1.352(8) . ?
C2 N2 1.441(8) . ?
C2 N1 1.461(8) . ?
C3 O2 1.234(7) . ?
C3 N2 1.341(8) . ?
C3 N3 1.366(8) . ?
C4 N4 1.443(8) . ?
C4 N3 1.455(8) . ?
C5 O3 1.224(8) . ?
C5 N5 1.350(8) . ?
C5 N4 1.374(8) . ?
C6 N5 1.450(8) . ?
C6 N6 1.451(8) . ?
C7 O4 1.222(8) . ?
C7 N7 1.364(8) . ?
C7 N6 1.370(9) . ?
C8 N7 1.445(8) . ?
C8 N8 1.446(8) . ?
C9 O5 1.224(8) . ?
C9 N9 1.357(8) . ?
C9 N8 1.370(8) . ?
C10 N9 1.443(8) . ?
C10 N10 1.445(8) . ?
C11 O6 1.247(7) . ?
C11 N10 1.352(8) . ?
C11 N11 1.355(8) . ?
C12 N12 1.442(8) . ?
C12 N11 1.444(8) . ?
C13 N13 1.471(8) . ?
C13 N1 1.472(8) . ?
C13 C14 1.526(9) . ?
C13 C27 1.565(9) . ?
C15 N14 1.445(8) . ?
C15 N2 1.461(8) . ?
C15 C16 1.543(9) . ?
C16 N15 1.435(8) . ?
C16 N3 1.462(8) . ?
C17 N16 1.434(8) . ?
C17 N4 1.453(8) . ?
C17 C18 1.543(9) . ?
C18 N5 1.436(8) . ?
C18 N17 1.446(7) . ?
C19 N6 1.459(8) . ?
C19 N18 1.478(8) . ?
C19 C20 1.518(9) . ?
C19 C21 1.582(9) . ?
C21 N19 1.449(8) . ?
C21 N7 1.468(8) . ?
C21 C22 1.523(9) . ?
C23 N8 1.422(8) . ?
C23 N20 1.450(8) . ?
C23 C24 1.559(9) . ?
C24 N9 1.443(8) . ?
C24 N21 1.447(8) . ?
C25 N22 1.435(8) . ?
C25 N10 1.476(7) . ?
C25 C26 1.546(9) . ?
C26 N11 1.440(8) . ?
C26 N23 1.451(8) . ?
C27 N24 1.443(8) . ?
C27 N12 1.474(8) . ?
C27 C28 1.520(9) . ?
C29 O7 1.215(8) . ?
C29 N24 1.361(9) . ?
C29 N13 1.367(8) . ?
C30 N14 1.444(8) . ?
C30 N13 1.453(8) . ?
C31 O8 1.228(7) . ?
C31 N14 1.362(8) . ?
C31 N15 1.365(8) . ?
C32 N15 1.446(8) . ?
C32 N16 1.452(8) . ?
C33 O9 1.224(7) . ?
C33 N17 1.371(8) . ?
C33 N16 1.377(8) . ?
C34 N18 1.444(8) . ?
C34 N17 1.445(8) . ?
C35 O10 1.224(8) . ?
C35 N19 1.359(8) . ?
C35 N18 1.373(8) . ?
C36 N20 1.433(8) . ?
C36 N19 1.439(8) . ?
C37 O11 1.224(8) . ?
C37 N21 1.364(8) . ?
C37 N20 1.376(8) . ?
C38 N22 1.441(8) . ?
C38 N21 1.446(8) . ?
C39 O12 1.233(8) . ?
C39 N22 1.362(9) . ?
C39 N23 1.365(8) . ?
C40 N24 1.450(8) . ?
C40 N23 1.455(8) . ?
C41 N36 1.443(8) 3_567 ?
C41 N25 1.444(8) . ?
C42 O13 1.240(7) . ?
C42 N25 1.345(8) . ?
C42 N26 1.363(8) . ?
C43 N27 1.429(8) . ?
C43 N26 1.438(8) . ?
C44 O14 1.224(8) . ?
C44 N27 1.357(9) . ?
C44 N28 1.379(8) . ?
C45 N29 1.440(8) . ?
C45 N28 1.441(9) . ?
C46 O15 1.222(9) . ?
C46 N30 1.366(8) . ?
C46 N29 1.373(9) . ?
C47 N31 1.446(9) 3_567 ?
C47 N30 1.456(9) . ?
C48 N31 1.460(8) . ?
C48 N25 1.468(8) . ?
C48 C49 1.531(9) . ?
C48 C50 1.574(10) . ?
C50 N32 1.456(9) . ?
C50 N26 1.462(8) . ?
C50 C51 1.539(9) . ?
C52 N33 1.442(9) . ?
C52 N27 1.464(8) . ?
C52 C53 1.551(10) . ?
C53 N34 1.451(8) . ?
C53 N28 1.455(9) . ?
C54 N29 1.440(8) . ?
C54 N35 1.453(9) . ?
C54 C55 1.553(9) . ?
C55 N30 1.437(9) . ?
C55 N36 1.460(8) . ?
C56 O16 1.221(9) . ?
C56 N32 1.349(10) . ?
C56 N31 1.360(10) . ?
C57 N33 1.434(10) . ?
C57 N32 1.469(9) . ?
C58 O17 1.220(9) . ?
C58 N33 1.357(9) . ?
C58 N34 1.360(10) . ?
C59 N35 1.436(9) . ?
C59 N34 1.454(9) . ?
C60 O18 1.215(8) . ?
C60 N35 1.361(9) . ?
C60 N36 1.370(9) . ?
N31 C47 1.446(9) 3_567 ?
N36 C41 1.443(8) 3_567 ?
N37 O21 1.229(13) . ?
N37 O20 1.255(12) . ?
N37 O19 1.287(13) . ?
O1 Nd1 2.403(5) . ?
O2 Nd1 2.449(4) . ?
O1W Nd1 2.488(5) . ?
O2W Nd1 2.397(5) . ?
O3W Nd1 2.549(5) . ?
O4W Nd1 2.886(7) . ?
O6 Nd1 2.483(4) . ?
O13 Nd1 2.461(4) . ?
O14 Nd1 2.485(4) . ?
O22 N38 1.256(12) . ?
N38 O24 1.244(13) . ?
N38 O23 1.271(13) . ?

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
O44 N39 O46 127.7(18) . . ?
O44 N39 O45 119.4(17) . . ?
O46 N39 O45 112.5(16) . . ?
O1 C1 N1 125.4(6) . . ?
O1 C1 N12 124.6(6) . . ?
N1 C1 N12 110.0(6) . . ?
N2 C2 N1 113.3(5) . . ?
O2 C3 N2 126.0(6) . . ?
O2 C3 N3 124.5(6) . . ?
N2 C3 N3 109.5(5) . . ?
N4 C4 N3 112.9(5) . . ?
O3 C5 N5 126.8(6) . . ?
O3 C5 N4 124.5(6) . . ?
N5 C5 N4 108.7(5) . . ?
N5 C6 N6 114.4(5) . . ?
O4 C7 N7 125.9(6) . . ?
O4 C7 N6 125.5(6) . . ?
N7 C7 N6 108.6(5) . . ?
N7 C8 N8 114.1(5) . . ?
O5 C9 N9 126.2(6) . . ?
O5 C9 N8 126.1(6) . . ?
N9 C9 N8 107.7(5) . . ?
N9 C10 N10 113.8(5) . . ?
O6 C11 N10 124.9(6) . . ?
O6 C11 N11 125.4(6) . . ?
N10 C11 N11 109.7(5) . . ?
N12 C12 N11 113.5(5) . . ?
N13 C13 N1 112.1(5) . . ?
N13 C13 C14 112.1(6) . . ?
N1 C13 C14 110.4(5) . . ?
N13 C13 C27 102.7(5) . . ?
N1 C13 C27 102.9(5) . . ?
C14 C13 C27 116.2(6) . . ?
N14 C15 N2 113.6(5) . . ?
N14 C15 C16 102.2(5) . . ?
N2 C15 C16 103.0(5) . . ?
N15 C16 N3 115.1(5) . . ?
N15 C16 C15 103.8(5) . . ?
N3 C16 C15 102.9(5) . . ?
N16 C17 N4 114.9(5) . . ?
N16 C17 C18 103.6(5) . . ?
N4 C17 C18 103.0(5) . . ?
N5 C18 N17 115.0(5) . . ?
N5 C18 C17 103.7(5) . . ?
N17 C18 C17 103.1(5) . . ?
N6 C19 N18 113.5(5) . . ?
N6 C19 C20 111.7(5) . . ?
N18 C19 C20 110.3(5) . . ?
N6 C19 C21 102.9(5) . . ?
N18 C19 C21 102.1(5) . . ?
C20 C19 C21 116.0(5) . . ?
N19 C21 N7 114.0(5) . . ?
N19 C21 C22 111.8(5) . . ?
N7 C21 C22 110.4(5) . . ?
N19 C21 C19 103.3(5) . . ?
N7 C21 C19 102.2(5) . . ?
C22 C21 C19 114.7(5) . . ?
N8 C23 N20 115.0(5) . . ?
N8 C23 C24 103.5(5) . . ?
N20 C23 C24 103.0(5) . . ?
N9 C24 N21 114.4(5) . . ?
N9 C24 C23 102.0(5) . . ?
N21 C24 C23 103.2(5) . . ?
N22 C25 N10 113.8(5) . . ?
N22 C25 C26 103.1(5) . . ?
N10 C25 C26 102.0(5) . . ?
N11 C26 N23 113.5(5) . . ?
N11 C26 C25 104.0(5) . . ?
N23 C26 C25 103.1(5) . . ?
N24 C27 N12 112.7(5) . . ?
N24 C27 C28 112.6(5) . . ?
N12 C27 C28 110.2(5) . . ?
N24 C27 C13 102.6(5) . . ?
N12 C27 C13 102.0(5) . . ?
C28 C27 C13 116.2(6) . . ?
O7 C29 N24 126.4(6) . . ?
O7 C29 N13 125.4(6) . . ?
N24 C29 N13 108.2(5) . . ?
N14 C30 N13 113.3(5) . . ?
O8 C31 N14 126.3(6) . . ?
O8 C31 N15 125.7(6) . . ?
N14 C31 N15 108.0(5) . . ?
N15 C32 N16 114.2(5) . . ?
O9 C33 N17 126.2(6) . . ?
O9 C33 N16 126.4(6) . . ?
N17 C33 N16 107.3(5) . . ?
N18 C34 N17 113.4(5) . . ?
O10 C35 N19 125.5(6) . . ?
O10 C35 N18 125.1(6) . . ?
N19 C35 N18 109.4(5) . . ?
N20 C36 N19 115.3(5) . . ?
O11 C37 N21 125.9(6) . . ?
O11 C37 N20 125.6(6) . . ?
N21 C37 N20 108.4(5) . . ?
N22 C38 N21 113.1(5) . . ?
O12 C39 N22 125.4(6) . . ?
O12 C39 N23 126.4(6) . . ?
N22 C39 N23 108.1(5) . . ?
N24 C40 N23 112.5(5) . . ?
N36 C41 N25 113.2(5) 3_567 . ?
O13 C42 N25 125.5(6) . . ?
O13 C42 N26 124.0(6) . . ?
N25 C42 N26 110.4(5) . . ?
N27 C43 N26 114.8(5) . . ?
O14 C44 N27 125.7(6) . . ?
O14 C44 N28 125.2(6) . . ?
N27 C44 N28 109.1(6) . . ?
N29 C45 N28 113.6(5) . . ?
O15 C46 N30 125.4(7) . . ?
O15 C46 N29 126.0(6) . . ?
N30 C46 N29 108.6(6) . . ?
N31 C47 N30 114.3(6) 3_567 . ?
N31 C48 N25 112.3(5) . . ?
N31 C48 C49 113.1(6) . . ?
N25 C48 C49 110.7(6) . . ?
N31 C48 C50 102.2(5) . . ?
N25 C48 C50 102.3(5) . . ?
C49 C48 C50 115.6(5) . . ?
N32 C50 N26 112.6(5) . . ?
N32 C50 C51 112.5(6) . . ?
N26 C50 C51 110.7(6) . . ?
N32 C50 C48 102.4(5) . . ?
N26 C50 C48 102.8(5) . . ?
C51 C50 C48 115.3(6) . . ?
N33 C52 N27 114.2(6) . . ?
N33 C52 C53 104.0(5) . . ?
N27 C52 C53 103.0(5) . . ?
N34 C53 N28 115.5(5) . . ?
N34 C53 C52 102.0(6) . . ?
N28 C53 C52 103.8(5) . . ?
N29 C54 N35 114.4(5) . . ?
N29 C54 C55 103.1(5) . . ?
N35 C54 C55 103.2(5) . . ?
N30 C55 N36 114.3(6) . . ?
N30 C55 C54 103.8(5) . . ?
N36 C55 C54 103.5(5) . . ?
O16 C56 N32 126.9(7) . . ?
O16 C56 N31 124.1(7) . . ?
N32 C56 N31 109.0(6) . . ?
N33 C57 N32 114.0(6) . . ?
O17 C58 N33 126.2(7) . . ?
O17 C58 N34 125.4(7) . . ?
N33 C58 N34 108.3(6) . . ?
N35 C59 N34 113.5(5) . . ?
O18 C60 N35 125.0(6) . . ?
O18 C60 N36 125.8(6) . . ?
N35 C60 N36 109.2(6) . . ?
C1 N1 C2 121.3(5) . . ?
C1 N1 C13 112.2(5) . . ?
C2 N1 C13 126.1(5) . . ?
C3 N2 C2 124.7(5) . . ?
C3 N2 C15 112.3(5) . . ?
C2 N2 C15 122.2(5) . . ?
C3 N3 C4 121.5(5) . . ?
C3 N3 C16 111.4(5) . . ?
C4 N3 C16 122.3(5) . . ?
C5 N4 C4 120.9(5) . . ?
C5 N4 C17 111.1(5) . . ?
C4 N4 C17 121.7(5) . . ?
C5 N5 C18 112.5(5) . . ?
C5 N5 C6 122.3(5) . . ?
C18 N5 C6 123.1(5) . . ?
C7 N6 C6 119.8(5) . . ?
C7 N6 C19 113.0(5) . . ?
C6 N6 C19 125.6(5) . . ?
C7 N7 C8 120.1(5) . . ?
C7 N7 C21 113.2(5) . . ?
C8 N7 C21 126.1(5) . . ?
C9 N8 C23 112.8(5) . . ?
C9 N8 C8 123.5(5) . . ?
C23 N8 C8 123.6(5) . . ?
C9 N9 C10 121.2(5) . . ?
C9 N9 C24 113.2(5) . . ?
C10 N9 C24 123.0(5) . . ?
C11 N10 C10 122.3(5) . . ?
C11 N10 C25 111.6(5) . . ?
C10 N10 C25 120.3(5) . . ?
C11 N11 C26 111.9(5) . . ?
C11 N11 C12 124.9(5) . . ?
C26 N11 C12 123.1(5) . . ?
C1 N12 C12 120.5(5) . . ?
C1 N12 C27 112.4(5) . . ?
C12 N12 C27 126.9(5) . . ?
C29 N13 C30 120.1(5) . . ?
C29 N13 C13 112.1(5) . . ?
C30 N13 C13 125.5(5) . . ?
C31 N14 C30 122.7(5) . . ?
C31 N14 C15 112.2(5) . . ?
C30 N14 C15 122.2(5) . . ?
C31 N15 C16 112.1(5) . . ?
C31 N15 C32 123.5(5) . . ?
C16 N15 C32 123.4(5) . . ?
C33 N16 C17 112.9(5) . . ?
C33 N16 C32 121.2(5) . . ?
C17 N16 C32 125.1(5) . . ?
C33 N17 C34 123.5(5) . . ?
C33 N17 C18 112.7(5) . . ?
C34 N17 C18 123.8(5) . . ?
C35 N18 C34 120.6(5) . . ?
C35 N18 C19 111.7(5) . . ?
C34 N18 C19 125.5(5) . . ?
C35 N19 C36 120.8(5) . . ?
C35 N19 C21 112.9(5) . . ?
C36 N19 C21 126.2(5) . . ?
C37 N20 C36 122.3(5) . . ?
C37 N20 C23 111.9(5) . . ?
C36 N20 C23 121.9(5) . . ?
C37 N21 C38 123.4(5) . . ?
C37 N21 C24 112.6(5) . . ?
C38 N21 C24 122.1(5) . . ?
C39 N22 C25 112.6(5) . . ?
C39 N22 C38 122.9(5) . . ?
C25 N22 C38 123.4(5) . . ?
C39 N23 C26 111.2(5) . . ?
C39 N23 C40 122.7(5) . . ?
C26 N23 C40 122.2(5) . . ?
C29 N24 C27 113.9(5) . . ?
C29 N24 C40 120.0(5) . . ?
C27 N24 C40 126.0(5) . . ?
C42 N25 C41 121.3(5) . . ?
C42 N25 C48 112.0(5) . . ?
C41 N25 C48 125.0(5) . . ?
C42 N26 C43 121.6(5) . . ?
C42 N26 C50 111.4(5) . . ?
C43 N26 C50 124.9(5) . . ?
C44 N27 C43 123.9(5) . . ?
C44 N27 C52 112.1(5) . . ?
C43 N27 C52 122.0(5) . . ?
C44 N28 C45 123.1(6) . . ?
C44 N28 C53 111.3(5) . . ?
C45 N28 C53 122.5(6) . . ?
C46 N29 C54 112.0(5) . . ?
C46 N29 C45 122.1(6) . . ?
C54 N29 C45 122.7(6) . . ?
C46 N30 C55 112.0(6) . . ?
C46 N30 C47 124.5(6) . . ?
C55 N30 C47 121.9(5) . . ?
C56 N31 C47 120.8(6) . 3_567 ?
C56 N31 C48 112.5(6) . . ?
C47 N31 C48 126.6(6) 3_567 . ?
C56 N32 C50 113.0(6) . . ?
C56 N32 C57 119.8(6) . . ?
C50 N32 C57 125.6(6) . . ?
C58 N33 C57 123.7(6) . . ?
C58 N33 C52 112.4(6) . . ?
C57 N33 C52 123.9(6) . . ?
C58 N34 C53 113.3(5) . . ?
C58 N34 C59 123.3(6) . . ?
C53 N34 C59 122.7(6) . . ?
C60 N35 C59 123.3(6) . . ?
C60 N35 C54 112.4(5) . . ?
C59 N35 C54 122.5(6) . . ?
C60 N36 C41 121.9(6) . 3_567 ?
C60 N36 C55 111.4(5) . . ?
C41 N36 C55 123.3(5) 3_567 . ?
O21 N37 O20 121.6(11) . . ?
O21 N37 O19 119.4(10) . . ?
O20 N37 O19 119.0(13) . . ?
C1 O1 Nd1 137.8(4) . . ?
C3 O2 Nd1 143.8(4) . . ?
C11 O6 Nd1 149.5(4) . . ?
C42 O13 Nd1 158.7(4) . . ?
C44 O14 Nd1 154.9(4) . . ?
O2W Nd1 O1 137.03(18) . . ?
O2W Nd1 O2 75.06(18) . . ?
O1 Nd1 O2 78.24(15) . . ?
O2W Nd1 O13 70.82(17) . . ?
O1 Nd1 O13 143.87(14) . . ?
O2 Nd1 O13 137.81(15) . . ?
O2W Nd1 O6 146.05(17) . . ?
O1 Nd1 O6 76.23(15) . . ?
O2 Nd1 O6 129.20(14) . . ?
O13 Nd1 O6 76.15(14) . . ?
O2W Nd1 O14 93.40(19) . . ?
O1 Nd1 O14 82.62(14) . . ?
O2 Nd1 O14 135.40(15) . . ?
O13 Nd1 O14 71.42(15) . . ?
O6 Nd1 O14 83.24(14) . . ?
O2W Nd1 O1W 77.4(2) . . ?
O1 Nd1 O1W 130.66(16) . . ?
O2 Nd1 O1W 81.31(15) . . ?
O13 Nd1 O1W 67.73(16) . . ?
O6 Nd1 O1W 83.19(16) . . ?
O14 Nd1 O1W 138.93(16) . . ?
O2W Nd1 O3W 69.45(19) . . ?
O1 Nd1 O3W 69.77(16) . . ?
O2 Nd1 O3W 68.88(15) . . ?
O13 Nd1 O3W 118.89(15) . . ?
O6 Nd1 O3W 136.67(16) . . ?
O14 Nd1 O3W 66.75(15) . . ?
O1W Nd1 O3W 139.77(17) . . ?
O2W Nd1 O4W 126.9(2) . . ?
O1 Nd1 O4W 68.10(16) . . ?
O2 Nd1 O4W 66.06(16) . . ?
O13 Nd1 O4W 118.09(16) . . ?
O6 Nd1 O4W 63.83(16) . . ?
O14 Nd1 O4W 139.73(16) . . ?
O1W Nd1 O4W 62.57(18) . . ?
O3W Nd1 O4W 122.76(17) . . ?
O24 N38 O22 113.0(12) . . ?
O24 N38 O23 125.2(12) . . ?
O22 N38 O23 121.2(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N14 C15 C16 N15 -11.0(6) . . . . ?
N2 C15 C16 N15 -129.1(5) . . . . ?
N14 C15 C16 N3 109.3(5) . . . . ?
N2 C15 C16 N3 -8.8(6) . . . . ?
N16 C17 C18 N5 124.9(5) . . . . ?
N4 C17 C18 N5 4.9(6) . . . . ?
N16 C17 C18 N17 4.7(6) . . . . ?
N4 C17 C18 N17 -115.3(5) . . . . ?
N6 C19 C21 N19 -122.3(5) . . . . ?
N18 C19 C21 N19 -4.4(6) . . . . ?
C20 C19 C21 N19 115.5(6) . . . . ?
N6 C19 C21 N7 -3.6(6) . . . . ?
N18 C19 C21 N7 114.2(5) . . . . ?
C20 C19 C21 N7 -125.8(6) . . . . ?
N6 C19 C21 C22 115.8(6) . . . . ?
N18 C19 C21 C22 -126.3(6) . . . . ?
C20 C19 C21 C22 -6.4(8) . . . . ?
N8 C23 C24 N9 -8.6(6) . . . . ?
N20 C23 C24 N9 111.5(5) . . . . ?
N8 C23 C24 N21 -127.5(5) . . . . ?
N20 C23 C24 N21 -7.4(6) . . . . ?
N22 C25 C26 N11 126.2(5) . . . . ?
N10 C25 C26 N11 8.0(6) . . . . ?
N22 C25 C26 N23 7.5(6) . . . . ?
N10 C25 C26 N23 -110.7(5) . . . . ?
N13 C13 C27 N24 6.9(6) . . . . ?
N1 C13 C27 N24 123.4(5) . . . . ?
C14 C13 C27 N24 -115.8(6) . . . . ?
N13 C13 C27 N12 -110.0(5) . . . . ?
N1 C13 C27 N12 6.6(6) . . . . ?
C14 C13 C27 N12 127.3(6) . . . . ?
N13 C13 C27 C28 130.1(6) . . . . ?
N1 C13 C27 C28 -113.3(6) . . . . ?
C14 C13 C27 C28 7.4(8) . . . . ?
N31 C48 C50 N32 -9.3(6) . . . . ?
N25 C48 C50 N32 107.1(5) . . . . ?
C49 C48 C50 N32 -132.5(6) . . . . ?
N31 C48 C50 N26 -126.2(5) . . . . ?
N25 C48 C50 N26 -9.8(6) . . . . ?
C49 C48 C50 N26 110.5(6) . . . . ?
N31 C48 C50 C51 113.3(6) . . . . ?
N25 C48 C50 C51 -130.3(6) . . . . ?
C49 C48 C50 C51 -10.0(9) . . . . ?
N33 C52 C53 N34 2.4(6) . . . . ?
N27 C52 C53 N34 121.9(5) . . . . ?
N33 C52 C53 N28 -117.9(5) . . . . ?
N27 C52 C53 N28 1.6(6) . . . . ?
N29 C54 C55 N30 -4.4(7) . . . . ?
N35 C54 C55 N30 -123.7(5) . . . . ?
N29 C54 C55 N36 115.2(5) . . . . ?
N35 C54 C55 N36 -4.1(6) . . . . ?
O1 C1 N1 C2 -7.5(9) . . . . ?
N12 C1 N1 C2 175.4(5) . . . . ?
O1 C1 N1 C13 180.0(6) . . . . ?
N12 C1 N1 C13 2.8(7) . . . . ?
N2 C2 N1 C1 -90.1(7) . . . . ?
N2 C2 N1 C13 81.3(8) . . . . ?
N13 C13 N1 C1 103.6(6) . . . . ?
C14 C13 N1 C1 -130.7(6) . . . . ?
C27 C13 N1 C1 -6.1(7) . . . . ?
N13 C13 N1 C2 -68.5(8) . . . . ?
C14 C13 N1 C2 57.2(8) . . . . ?
C27 C13 N1 C2 -178.2(5) . . . . ?
O2 C3 N2 C2 -8.2(9) . . . . ?
N3 C3 N2 C2 169.7(5) . . . . ?
O2 C3 N2 C15 -178.4(5) . . . . ?
N3 C3 N2 C15 -0.6(7) . . . . ?
N1 C2 N2 C3 97.2(7) . . . . ?
N1 C2 N2 C15 -93.5(7) . . . . ?
N14 C15 N2 C3 -103.6(6) . . . . ?
C16 C15 N2 C3 6.2(6) . . . . ?
N14 C15 N2 C2 85.9(7) . . . . ?
C16 C15 N2 C2 -164.3(5) . . . . ?
O2 C3 N3 C4 16.2(9) . . . . ?
N2 C3 N3 C4 -161.7(5) . . . . ?
O2 C3 N3 C16 172.0(5) . . . . ?
N2 C3 N3 C16 -5.9(7) . . . . ?
N4 C4 N3 C3 -125.0(6) . . . . ?
N4 C4 N3 C16 81.8(7) . . . . ?
N15 C16 N3 C3 121.4(5) . . . . ?
C15 C16 N3 C3 9.3(6) . . . . ?
N15 C16 N3 C4 -82.9(7) . . . . ?
C15 C16 N3 C4 164.9(5) . . . . ?
O3 C5 N4 C4 -17.5(9) . . . . ?
N5 C5 N4 C4 162.9(5) . . . . ?
O3 C5 N4 C17 -170.0(6) . . . . ?
N5 C5 N4 C17 10.4(7) . . . . ?
N3 C4 N4 C5 124.5(6) . . . . ?
N3 C4 N4 C17 -85.9(7) . . . . ?
N16 C17 N4 C5 -121.3(6) . . . . ?
C18 C17 N4 C5 -9.3(6) . . . . ?
N16 C17 N4 C4 86.5(7) . . . . ?
C18 C17 N4 C4 -161.5(5) . . . . ?
O3 C5 N5 C18 173.5(6) . . . . ?
N4 C5 N5 C18 -6.9(7) . . . . ?
O3 C5 N5 C6 9.3(10) . . . . ?
N4 C5 N5 C6 -171.1(5) . . . . ?
N17 C18 N5 C5 112.8(6) . . . . ?
C17 C18 N5 C5 1.0(6) . . . . ?
N17 C18 N5 C6 -83.2(7) . . . . ?
C17 C18 N5 C6 165.0(5) . . . . ?
N6 C6 N5 C5 -97.7(7) . . . . ?
N6 C6 N5 C18 99.9(7) . . . . ?
O4 C7 N6 C6 16.2(10) . . . . ?
N7 C7 N6 C6 -166.2(5) . . . . ?
O4 C7 N6 C19 -177.4(6) . . . . ?
N7 C7 N6 C19 0.1(7) . . . . ?
N5 C6 N6 C7 88.2(7) . . . . ?
N5 C6 N6 C19 -76.3(8) . . . . ?
N18 C19 N6 C7 -107.2(6) . . . . ?
C20 C19 N6 C7 127.4(6) . . . . ?
C21 C19 N6 C7 2.3(6) . . . . ?
N18 C19 N6 C6 58.2(8) . . . . ?
C20 C19 N6 C6 -67.2(8) . . . . ?
C21 C19 N6 C6 167.7(5) . . . . ?
O4 C7 N7 C8 3.2(10) . . . . ?
N6 C7 N7 C8 -174.3(5) . . . . ?
O4 C7 N7 C21 174.7(6) . . . . ?
N6 C7 N7 C21 -2.9(7) . . . . ?
N8 C8 N7 C7 -103.8(7) . . . . ?
N8 C8 N7 C21 85.9(8) . . . . ?
N19 C21 N7 C7 114.9(6) . . . . ?
C22 C21 N7 C7 -118.3(6) . . . . ?
C19 C21 N7 C7 4.1(6) . . . . ?
N19 C21 N7 C8 -74.3(7) . . . . ?
C22 C21 N7 C8 52.5(8) . . . . ?
C19 C21 N7 C8 175.0(5) . . . . ?
O5 C9 N8 C23 179.7(6) . . . . ?
N9 C9 N8 C23 -3.0(7) . . . . ?
O5 C9 N8 C8 -3.2(10) . . . . ?
N9 C9 N8 C8 174.0(6) . . . . ?
N20 C23 N8 C9 -104.1(6) . . . . ?
C24 C23 N8 C9 7.5(7) . . . . ?
N20 C23 N8 C8 78.9(8) . . . . ?
C24 C23 N8 C8 -169.6(5) . . . . ?
N7 C8 N8 C9 98.0(7) . . . . ?
N7 C8 N8 C23 -85.2(7) . . . . ?
O5 C9 N9 C10 11.5(10) . . . . ?
N8 C9 N9 C10 -165.7(6) . . . . ?
O5 C9 N9 C24 173.8(6) . . . . ?
N8 C9 N9 C24 -3.5(7) . . . . ?
N10 C10 N9 C9 -119.6(6) . . . . ?
N10 C10 N9 C24 79.9(7) . . . . ?
N21 C24 N9 C9 118.3(6) . . . . ?
C23 C24 N9 C9 7.7(7) . . . . ?
N21 C24 N9 C10 -79.8(7) . . . . ?
C23 C24 N9 C10 169.6(6) . . . . ?
O6 C11 N10 C10 -23.2(9) . . . . ?
N11 C11 N10 C10 156.5(5) . . . . ?
O6 C11 N10 C25 -176.4(6) . . . . ?
N11 C11 N10 C25 3.4(7) . . . . ?
N9 C10 N10 C11 121.5(6) . . . . ?
N9 C10 N10 C25 -87.6(7) . . . . ?
N22 C25 N10 C11 -117.5(6) . . . . ?
C26 C25 N10 C11 -7.2(6) . . . . ?
N22 C25 N10 C10 88.7(7) . . . . ?
C26 C25 N10 C10 -160.9(5) . . . . ?
O6 C11 N11 C26 -177.7(6) . . . . ?
N10 C11 N11 C26 2.5(7) . . . . ?
O6 C11 N11 C12 4.0(10) . . . . ?
N10 C11 N11 C12 -175.7(5) . . . . ?
N23 C26 N11 C11 104.5(6) . . . . ?
C25 C26 N11 C11 -6.8(7) . . . . ?
N23 C26 N11 C12 -77.3(7) . . . . ?
C25 C26 N11 C12 171.4(5) . . . . ?
N12 C12 N11 C11 -91.3(7) . . . . ?
N12 C12 N11 C26 90.7(7) . . . . ?
O1 C1 N12 C12 1.1(9) . . . . ?
N1 C1 N12 C12 178.2(5) . . . . ?
O1 C1 N12 C27 -175.1(6) . . . . ?
N1 C1 N12 C27 2.1(7) . . . . ?
N11 C12 N12 C1 96.6(6) . . . . ?
N11 C12 N12 C27 -87.8(7) . . . . ?
N24 C27 N12 C1 -114.9(6) . . . . ?
C28 C27 N12 C1 118.4(6) . . . . ?
C13 C27 N12 C1 -5.6(6) . . . . ?
N24 C27 N12 C12 69.2(8) . . . . ?
C28 C27 N12 C12 -57.5(8) . . . . ?
C13 C27 N12 C12 178.5(5) . . . . ?
O7 C29 N13 C30 -11.3(10) . . . . ?
N24 C29 N13 C30 168.6(5) . . . . ?
O7 C29 N13 C13 -175.2(6) . . . . ?
N24 C29 N13 C13 4.8(7) . . . . ?
N14 C30 N13 C29 104.1(7) . . . . ?
N14 C30 N13 C13 -94.4(7) . . . . ?
N1 C13 N13 C29 -117.2(6) . . . . ?
C14 C13 N13 C29 118.1(6) . . . . ?
C27 C13 N13 C29 -7.4(7) . . . . ?
N1 C13 N13 C30 80.0(7) . . . . ?
C14 C13 N13 C30 -44.7(8) . . . . ?
C27 C13 N13 C30 -170.2(5) . . . . ?
O8 C31 N14 C30 7.7(10) . . . . ?
N15 C31 N14 C30 -171.2(6) . . . . ?
O8 C31 N14 C15 168.9(6) . . . . ?
N15 C31 N14 C15 -10.0(7) . . . . ?
N13 C30 N14 C31 -117.3(6) . . . . ?
N13 C30 N14 C15 83.3(7) . . . . ?
N2 C15 N14 C31 123.4(6) . . . . ?
C16 C15 N14 C31 13.1(6) . . . . ?
N2 C15 N14 C30 -75.3(7) . . . . ?
C16 C15 N14 C30 174.4(5) . . . . ?
O8 C31 N15 C16 -177.0(6) . . . . ?
N14 C31 N15 C16 1.9(7) . . . . ?
O8 C31 N15 C32 -8.3(10) . . . . ?
N14 C31 N15 C32 170.6(5) . . . . ?
N3 C16 N15 C31 -105.6(6) . . . . ?
C15 C16 N15 C31 6.1(7) . . . . ?
N3 C16 N15 C32 85.7(7) . . . . ?
C15 C16 N15 C32 -162.7(5) . . . . ?
N16 C32 N15 C31 111.2(7) . . . . ?
N16 C32 N15 C16 -81.3(7) . . . . ?
O9 C33 N16 C17 175.0(6) . . . . ?
N17 C33 N16 C17 -0.9(7) . . . . ?
O9 C33 N16 C32 4.9(10) . . . . ?
N17 C33 N16 C32 -171.0(5) . . . . ?
N4 C17 N16 C33 109.0(6) . . . . ?
C18 C17 N16 C33 -2.5(7) . . . . ?
N4 C17 N16 C32 -81.4(7) . . . . ?
C18 C17 N16 C32 167.1(5) . . . . ?
N15 C32 N16 C33 -113.4(6) . . . . ?
N15 C32 N16 C17 77.8(7) . . . . ?
O9 C33 N17 C34 7.2(10) . . . . ?
N16 C33 N17 C34 -176.9(5) . . . . ?
O9 C33 N17 C18 -171.6(6) . . . . ?
N16 C33 N17 C18 4.3(7) . . . . ?
N18 C34 N17 C33 103.7(6) . . . . ?
N18 C34 N17 C18 -77.7(7) . . . . ?
N5 C18 N17 C33 -117.9(6) . . . . ?
C17 C18 N17 C33 -5.7(6) . . . . ?
N5 C18 N17 C34 63.3(8) . . . . ?
C17 C18 N17 C34 175.5(5) . . . . ?
O10 C35 N18 C34 7.5(10) . . . . ?
N19 C35 N18 C34 -171.2(5) . . . . ?
O10 C35 N18 C19 171.4(6) . . . . ?
N19 C35 N18 C19 -7.3(7) . . . . ?
N17 C34 N18 C35 -98.3(7) . . . . ?
N17 C34 N18 C19 100.1(7) . . . . ?
N6 C19 N18 C35 117.2(6) . . . . ?
C20 C19 N18 C35 -116.7(6) . . . . ?
C21 C19 N18 C35 7.2(6) . . . . ?
N6 C19 N18 C34 -79.9(7) . . . . ?
C20 C19 N18 C34 46.3(8) . . . . ?
C21 C19 N18 C34 170.1(5) . . . . ?
O10 C35 N19 C36 4.2(10) . . . . ?
N18 C35 N19 C36 -177.1(5) . . . . ?
O10 C35 N19 C21 -174.7(6) . . . . ?
N18 C35 N19 C21 4.1(7) . . . . ?
N20 C36 N19 C35 96.4(7) . . . . ?
N20 C36 N19 C21 -84.8(8) . . . . ?
N7 C21 N19 C35 -109.6(6) . . . . ?
C22 C21 N19 C35 124.4(6) . . . . ?
C19 C21 N19 C35 0.5(7) . . . . ?
N7 C21 N19 C36 71.6(8) . . . . ?
C22 C21 N19 C36 -54.4(8) . . . . ?
C19 C21 N19 C36 -178.3(5) . . . . ?
O11 C37 N20 C36 13.3(9) . . . . ?
N21 C37 N20 C36 -166.4(5) . . . . ?
O11 C37 N20 C23 171.6(6) . . . . ?
N21 C37 N20 C23 -8.2(7) . . . . ?
N19 C36 N20 C37 -116.3(6) . . . . ?
N19 C36 N20 C23 87.5(7) . . . . ?
N8 C23 N20 C37 121.5(6) . . . . ?
C24 C23 N20 C37 9.7(6) . . . . ?
N8 C23 N20 C36 -80.1(7) . . . . ?
C24 C23 N20 C36 168.0(5) . . . . ?
O11 C37 N21 C38 -12.4(10) . . . . ?
N20 C37 N21 C38 167.3(5) . . . . ?
O11 C37 N21 C24 -177.0(6) . . . . ?
N20 C37 N21 C24 2.8(7) . . . . ?
N22 C38 N21 C37 109.8(7) . . . . ?
N22 C38 N21 C24 -87.1(7) . . . . ?
N9 C24 N21 C37 -106.7(6) . . . . ?
C23 C24 N21 C37 3.1(7) . . . . ?
N9 C24 N21 C38 88.5(7) . . . . ?
C23 C24 N21 C38 -161.6(5) . . . . ?
O12 C39 N22 C25 172.1(6) . . . . ?
N23 C39 N22 C25 -8.4(7) . . . . ?
O12 C39 N22 C38 3.5(9) . . . . ?
N23 C39 N22 C38 -177.0(5) . . . . ?
N10 C25 N22 C39 109.8(6) . . . . ?
C26 C25 N22 C39 0.1(6) . . . . ?
N10 C25 N22 C38 -81.7(7) . . . . ?
C26 C25 N22 C38 168.6(5) . . . . ?
N21 C38 N22 C39 -112.8(6) . . . . ?
N21 C38 N22 C25 79.8(7) . . . . ?
O12 C39 N23 C26 -166.7(6) . . . . ?
N22 C39 N23 C26 13.7(7) . . . . ?
O12 C39 N23 C40 -8.4(10) . . . . ?
N22 C39 N23 C40 172.0(5) . . . . ?
N11 C26 N23 C39 -125.0(6) . . . . ?
C25 C26 N23 C39 -13.1(6) . . . . ?
N11 C26 N23 C40 76.6(7) . . . . ?
C25 C26 N23 C40 -171.5(5) . . . . ?
N24 C40 N23 C39 113.1(6) . . . . ?
N24 C40 N23 C26 -91.0(7) . . . . ?
O7 C29 N24 C27 -179.7(6) . . . . ?
N13 C29 N24 C27 0.4(7) . . . . ?
O7 C29 N24 C40 -3.8(10) . . . . ?
N13 C29 N24 C40 176.2(5) . . . . ?
N12 C27 N24 C29 104.2(6) . . . . ?
C28 C27 N24 C29 -130.4(6) . . . . ?
C13 C27 N24 C29 -4.8(7) . . . . ?
N12 C27 N24 C40 -71.4(8) . . . . ?
C28 C27 N24 C40 54.0(8) . . . . ?
C13 C27 N24 C40 179.6(6) . . . . ?
N23 C40 N24 C29 -83.6(7) . . . . ?
N23 C40 N24 C27 91.8(7) . . . . ?
O13 C42 N25 C41 11.9(9) . . . . ?
N26 C42 N25 C41 -167.1(5) . . . . ?
O13 C42 N25 C48 177.7(5) . . . . ?
N26 C42 N25 C48 -1.3(7) . . . . ?
N36 C41 N25 C42 -108.5(7) 3_567 . . . ?
N36 C41 N25 C48 87.6(7) 3_567 . . . ?
N31 C48 N25 C42 116.0(6) . . . . ?
C49 C48 N25 C42 -116.5(6) . . . . ?
C50 C48 N25 C42 7.2(6) . . . . ?
N31 C48 N25 C41 -78.8(7) . . . . ?
C49 C48 N25 C41 48.6(8) . . . . ?
C50 C48 N25 C41 172.4(5) . . . . ?
O13 C42 N26 C43 10.9(9) . . . . ?
N25 C42 N26 C43 -170.1(5) . . . . ?
O13 C42 N26 C50 175.0(5) . . . . ?
N25 C42 N26 C50 -6.0(7) . . . . ?
N27 C43 N26 C42 77.8(7) . . . . ?
N27 C43 N26 C50 -84.1(7) . . . . ?
N32 C50 N26 C42 -99.5(6) . . . . ?
C51 C50 N26 C42 133.6(6) . . . . ?
C48 C50 N26 C42 9.9(6) . . . . ?
N32 C50 N26 C43 64.0(8) . . . . ?
C51 C50 N26 C43 -62.9(8) . . . . ?
C48 C50 N26 C43 173.4(5) . . . . ?
O14 C44 N27 C43 6.8(10) . . . . ?
N28 C44 N27 C43 -172.1(5) . . . . ?
O14 C44 N27 C52 171.1(6) . . . . ?
N28 C44 N27 C52 -7.8(7) . . . . ?
N26 C43 N27 C44 -99.3(7) . . . . ?
N26 C43 N27 C52 97.9(7) . . . . ?
N33 C52 N27 C44 115.8(6) . . . . ?
C53 C52 N27 C44 3.6(7) . . . . ?
N33 C52 N27 C43 -79.5(7) . . . . ?
C53 C52 N27 C43 168.3(5) . . . . ?
O14 C44 N28 C45 -9.3(10) . . . . ?
N27 C44 N28 C45 169.6(5) . . . . ?
O14 C44 N28 C53 -170.1(6) . . . . ?
N27 C44 N28 C53 8.9(7) . . . . ?
N29 C45 N28 C44 115.6(7) . . . . ?
N29 C45 N28 C53 -85.8(7) . . . . ?
N34 C53 N28 C44 -117.0(6) . . . . ?
C52 C53 N28 C44 -6.3(7) . . . . ?
N34 C53 N28 C45 82.2(8) . . . . ?
C52 C53 N28 C45 -167.1(5) . . . . ?
O15 C46 N29 C54 173.8(7) . . . . ?
N30 C46 N29 C54 -7.2(8) . . . . ?
O15 C46 N29 C45 13.6(12) . . . . ?
N30 C46 N29 C45 -167.4(6) . . . . ?
N35 C54 N29 C46 118.4(6) . . . . ?
C55 C54 N29 C46 7.2(7) . . . . ?
N35 C54 N29 C45 -81.6(7) . . . . ?
C55 C54 N29 C45 167.2(6) . . . . ?
N28 C45 N29 C46 -117.2(7) . . . . ?
N28 C45 N29 C54 84.7(8) . . . . ?
O15 C46 N30 C55 -177.1(7) . . . . ?
N29 C46 N30 C55 4.0(8) . . . . ?
O15 C46 N30 C47 -10.8(12) . . . . ?
N29 C46 N30 C47 170.2(6) . . . . ?
N36 C55 N30 C46 -111.5(6) . . . . ?
C54 C55 N30 C46 0.5(7) . . . . ?
N36 C55 N30 C47 81.9(8) . . . . ?
C54 C55 N30 C47 -166.2(6) . . . . ?
N31 C47 N30 C46 109.4(8) 3_567 . . . ?
N31 C47 N30 C55 -85.7(8) 3_567 . . . ?
O16 C56 N31 C47 1.4(10) . . . 3_567 ?
N32 C56 N31 C47 179.2(6) . . . 3_567 ?
O16 C56 N31 C48 178.6(7) . . . . ?
N32 C56 N31 C48 -3.6(8) . . . . ?
N25 C48 N31 C56 -100.7(6) . . . . ?
C49 C48 N31 C56 133.2(6) . . . . ?
C50 C48 N31 C56 8.3(7) . . . . ?
N25 C48 N31 C47 76.3(8) . . . 3_567 ?
C49 C48 N31 C47 -49.9(8) . . . 3_567 ?
C50 C48 N31 C47 -174.8(6) . . . 3_567 ?
O16 C56 N32 C50 174.3(7) . . . . ?
N31 C56 N32 C50 -3.4(8) . . . . ?
O16 C56 N32 C57 8.1(11) . . . . ?
N31 C56 N32 C57 -169.6(6) . . . . ?
N26 C50 N32 C56 117.9(6) . . . . ?
C51 C50 N32 C56 -116.2(7) . . . . ?
C48 C50 N32 C56 8.2(7) . . . . ?
N26 C50 N32 C57 -76.9(8) . . . . ?
C51 C50 N32 C57 49.0(9) . . . . ?
C48 C50 N32 C57 173.4(6) . . . . ?
N33 C57 N32 C56 -99.4(8) . . . . ?
N33 C57 N32 C50 96.3(8) . . . . ?
O17 C58 N33 C57 2.7(11) . . . . ?
N34 C58 N33 C57 179.7(6) . . . . ?
O17 C58 N33 C52 -175.6(6) . . . . ?
N34 C58 N33 C52 1.4(7) . . . . ?
N32 C57 N33 C58 99.7(8) . . . . ?
N32 C57 N33 C52 -82.2(9) . . . . ?
N27 C52 N33 C58 -114.0(6) . . . . ?
C53 C52 N33 C58 -2.5(7) . . . . ?
N27 C52 N33 C57 67.7(8) . . . . ?
C53 C52 N33 C57 179.2(6) . . . . ?
O17 C58 N34 C53 177.4(6) . . . . ?
N33 C58 N34 C53 0.4(7) . . . . ?
O17 C58 N34 C59 6.8(10) . . . . ?
N33 C58 N34 C59 -170.3(6) . . . . ?
N28 C53 N34 C58 110.0(6) . . . . ?
C52 C53 N34 C58 -1.8(7) . . . . ?
N28 C53 N34 C59 -79.3(8) . . . . ?
C52 C53 N34 C59 168.9(6) . . . . ?
N35 C59 N34 C58 -107.4(7) . . . . ?
N35 C59 N34 C53 82.9(8) . . . . ?
O18 C60 N35 C59 -10.2(11) . . . . ?
N36 C60 N35 C59 169.0(6) . . . . ?
O18 C60 N35 C54 -175.0(6) . . . . ?
N36 C60 N35 C54 4.2(8) . . . . ?
N34 C59 N35 C60 109.9(7) . . . . ?
N34 C59 N35 C54 -86.7(8) . . . . ?
N29 C54 N35 C60 -111.0(6) . . . . ?
C55 C54 N35 C60 0.2(7) . . . . ?
N29 C54 N35 C59 84.0(7) . . . . ?
C55 C54 N35 C59 -164.8(6) . . . . ?
O18 C60 N36 C41 12.1(10) . . . 3_567 ?
N35 C60 N36 C41 -167.0(6) . . . 3_567 ?
O18 C60 N36 C55 172.0(7) . . . . ?
N35 C60 N36 C55 -7.1(7) . . . . ?
N30 C55 N36 C60 119.1(6) . . . . ?
C54 C55 N36 C60 6.9(7) . . . . ?
N30 C55 N36 C41 -81.4(7) . . . 3_567 ?
C54 C55 N36 C41 166.5(5) . . . 3_567 ?
N1 C1 O1 Nd1 90.7(8) . . . . ?
N12 C1 O1 Nd1 -92.5(8) . . . . ?
N2 C3 O2 Nd1 -69.4(9) . . . . ?
N3 C3 O2 Nd1 113.1(7) . . . . ?
N10 C11 O6 Nd1 -114.9(8) . . . . ?
N11 C11 O6 Nd1 65.4(11) . . . . ?
N25 C42 O13 Nd1 -168.4(7) . . . . ?
N26 C42 O13 Nd1 10.5(15) . . . . ?
N27 C44 O14 Nd1 13.4(14) . . . . ?
N28 C44 O14 Nd1 -167.9(6) . . . . ?

_refine_diff_density_max         2.204
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.164

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1038172'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_4                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_4                   
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

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 0.868 -0.014 0.000 1113 440 ' '
2 0.500 0.000 0.500 117 15 ' '
3 1.000 0.500 0.500 117 15 ' '
_platon_squeeze_details          ?


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl0 N24 Nd O22'
_chemical_formula_weight         1357.23

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.295(13)
_cell_length_b                   12.542(7)
_cell_length_c                   14.812(8)
_cell_angle_alpha                90
_cell_angle_beta                 116.125(6)
_cell_angle_gamma                90
_cell_volume                     3719(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6258
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      25.75

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_F_000             1376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.773
_shelx_estimated_absorpt_T_min   0.818
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9931
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.531
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3489
_reflns_number_gt                3394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+4.7454P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3489
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.5920(4) 0.5000 0.1244(6) 0.185(4) Uani 1 2 d S T P . .
Nd1 Nd 1.0000 1.0000 0.5000 0.03280(13) Uani 1 4 d S T P . .
N1 N 0.77215(12) 0.40291(19) 0.41404(19) 0.0394(6) Uani 1 1 d . . . . .
N2 N 0.82034(12) 0.40335(19) 0.57991(19) 0.0391(6) Uani 1 1 d . . . . .
N3 N 0.92497(12) 0.40366(19) 0.7304(2) 0.0411(6) Uani 1 1 d . . . . .
N4 N 1.03476(12) 0.40332(19) 0.80903(19) 0.0397(6) Uani 1 1 d . . . . .
N5 N 1.14317(12) 0.4032(2) 0.8107(2) 0.0412(6) Uani 1 1 d . . . . .
N6 N 1.20886(12) 0.40352(19) 0.7344(2) 0.0410(6) Uani 1 1 d . . . . .
O1 O 0.83523(12) 0.25862(17) 0.49712(19) 0.0520(6) Uani 1 1 d . . . . .
O2 O 0.98181(13) 0.2582(2) 0.7154(2) 0.0701(8) Uani 1 1 d . . . . .
O3 O 1.14214(15) 0.2591(2) 0.7163(2) 0.0681(7) Uani 1 1 d . . . . .
O4 O 0.9037(3) 0.9308(4) 0.3554(4) 0.0653(14) Uani 0.5 1 d . . P A 1
O6 O 0.9515(3) 0.8515(4) 0.5525(4) 0.0602(13) Uani 0.5 1 d . . P B 1
O5 O 0.9210(3) 0.8518(4) 0.4477(4) 0.0603(13) Uani 0.5 1 d . . P A 2
O7 O 0.9897(3) 0.9311(4) 0.6464(4) 0.0615(14) Uani 0.5 1 d . . P A 2
C1 C 0.81254(14) 0.3473(2) 0.4969(2) 0.0397(7) Uani 1 1 d . . . . .
C2 C 0.78077(19) 0.5000 0.5558(3) 0.0376(9) Uani 1 2 d S T P . .
C3 C 0.74673(19) 0.5000 0.4381(3) 0.0366(9) Uani 1 2 d S T P . .
C4 C 0.85843(15) 0.3606(2) 0.6792(2) 0.0441(7) Uani 1 1 d . . . . .
H4A H 0.8615 0.2838 0.6742 0.053 Uiso 1 1 calc R U . . .
H4B H 0.8347 0.3748 0.7193 0.053 Uiso 1 1 calc R U . . .
C5 C 0.98063(16) 0.3468(2) 0.7478(2) 0.0444(7) Uani 1 1 d . . . . .
C6 C 1.0170(2) 0.5000 0.8438(3) 0.0374(9) Uani 1 2 d S T P . .
H6 H 1.0333 0.5000 0.9170 0.045 Uiso 1 2 calc R U P . .
C7 C 0.9400(2) 0.5000 0.7887(3) 0.0383(9) Uani 1 2 d S T P . .
H7 H 0.9201 0.5000 0.8360 0.046 Uiso 1 2 calc R U P . .
C8 C 1.10113(14) 0.3596(2) 0.8521(2) 0.0425(7) Uani 1 1 d . . . . .
H8A H 1.1218 0.3724 0.9240 0.051 Uiso 1 1 calc R U . . .
H8B H 1.0982 0.2830 0.8418 0.051 Uiso 1 1 calc R U . . .
C9 C 1.16243(16) 0.3469(2) 0.7500(2) 0.0435(7) Uani 1 1 d . . . . .
C10 C 1.2271(2) 0.5000 0.7926(3) 0.0386(9) Uani 1 2 d S T P . .
H10 H 1.2745 0.5000 0.8408 0.046 Uiso 1 2 calc R U P . .
C11 C 1.1816(2) 0.5000 0.8464(3) 0.0380(9) Uani 1 2 d S T P . .
H11 H 1.2076 0.5000 0.9197 0.046 Uiso 1 2 calc R U P . .
C12 C 0.75384(16) 0.3607(2) 0.3152(3) 0.0455(7) Uani 1 1 d . . . . .
H12A H 0.7598 0.2840 0.3202 0.055 Uiso 1 1 calc R U . . .
H12B H 0.7068 0.3747 0.2739 0.055 Uiso 1 1 calc R U . . .
C13 C 0.7335(2) 0.5000 0.6050(4) 0.0532(12) Uani 1 2 d S T P . .
H13A H 0.7122 0.4317 0.5955 0.080 Uiso 0.5 1 calc R U P . .
H13B H 0.7003 0.5543 0.5749 0.080 Uiso 0.5 1 calc R U P . .
H13C H 0.7583 0.5140 0.6756 0.080 Uiso 0.5 1 calc R U P . .
C14 C 0.6710(2) 0.5000 0.3891(4) 0.0551(12) Uani 1 2 d S T P . .
H14A H 0.6545 0.4793 0.3199 0.083 Uiso 0.5 1 calc R U P . .
H14B H 0.6551 0.5702 0.3929 0.083 Uiso 0.5 1 calc R U P . .
H14C H 0.6554 0.4505 0.4234 0.083 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O4 2.429(5) . ?
Nd1 O4 2.429(5) 5_776 ?
Nd1 O4 2.429(5) 6_575 ?
Nd1 O4 2.429(5) 2_756 ?
Nd1 O7 2.437(5) 6_575 ?
Nd1 O7 2.437(5) 2_756 ?
Nd1 O7 2.437(5) 5_776 ?
Nd1 O7 2.437(5) . ?
Nd1 O5 2.440(5) . ?
Nd1 O5 2.440(5) 5_776 ?
Nd1 O5 2.440(5) 6_575 ?
Nd1 O5 2.440(5) 2_756 ?
N1 C1 1.353(4) . ?
N1 C12 1.437(4) . ?
N1 C3 1.452(3) . ?
N2 C1 1.360(4) . ?
N2 C4 1.439(4) . ?
N2 C2 1.448(3) . ?
N3 C5 1.354(4) . ?
N3 C7 1.436(3) . ?
N3 C4 1.441(4) . ?
N4 C5 1.348(4) . ?
N4 C8 1.437(4) . ?
N4 C6 1.439(3) . ?
N5 C9 1.353(4) . ?
N5 C8 1.435(4) . ?
N5 C11 1.446(3) . ?
N6 C9 1.356(4) . ?
N6 C12 1.434(4) 2_756 ?
N6 C10 1.437(3) . ?
O1 C1 1.221(4) . ?
O2 C5 1.215(4) . ?
O3 C9 1.211(4) . ?
O4 O4 1.735(9) 6_575 ?
O7 O7 1.728(9) 6_575 ?
C2 N2 1.448(3) 6_565 ?
C2 C13 1.522(6) . ?
C2 C3 1.565(6) . ?
C3 N1 1.452(3) 6_565 ?
C3 C14 1.517(6) . ?
C6 N4 1.439(3) 6_565 ?
C6 C7 1.544(6) . ?
C7 N3 1.436(3) 6_565 ?
C10 N6 1.437(3) 6_565 ?
C10 C11 1.540(6) . ?
C11 N5 1.446(3) 6_565 ?
C12 N6 1.434(4) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Nd1 O4 180.0 . 5_776 ?
O4 Nd1 O4 41.8(2) . 6_575 ?
O4 Nd1 O4 138.2(2) 5_776 6_575 ?
O4 Nd1 O4 138.2(2) . 2_756 ?
O4 Nd1 O4 41.8(2) 5_776 2_756 ?
O4 Nd1 O4 180.0 6_575 2_756 ?
O7 Nd1 O7 180.0 6_575 2_756 ?
O7 Nd1 O7 138.5(2) 6_575 5_776 ?
O7 Nd1 O7 41.5(2) 2_756 5_776 ?
O7 Nd1 O7 41.5(2) 6_575 . ?
O7 Nd1 O7 138.5(2) 2_756 . ?
O7 Nd1 O7 180.0 5_776 . ?
O7 Nd1 O5 102.39(18) 6_575 . ?
O7 Nd1 O5 77.61(17) 2_756 . ?
O7 Nd1 O5 108.99(18) 5_776 . ?
O7 Nd1 O5 71.01(18) . . ?
O7 Nd1 O5 77.61(18) 6_575 5_776 ?
O7 Nd1 O5 102.39(18) 2_756 5_776 ?
O7 Nd1 O5 71.01(18) 5_776 5_776 ?
O7 Nd1 O5 108.99(18) . 5_776 ?
O5 Nd1 O5 180.0 . 5_776 ?
O7 Nd1 O5 71.01(18) 6_575 6_575 ?
O7 Nd1 O5 108.99(18) 2_756 6_575 ?
O7 Nd1 O5 77.61(17) 5_776 6_575 ?
O7 Nd1 O5 102.39(18) . 6_575 ?
O5 Nd1 O5 99.2(3) . 6_575 ?
O5 Nd1 O5 80.8(3) 5_776 6_575 ?
O7 Nd1 O5 108.99(18) 6_575 2_756 ?
O7 Nd1 O5 71.01(18) 2_756 2_756 ?
O7 Nd1 O5 102.39(17) 5_776 2_756 ?
O7 Nd1 O5 77.61(17) . 2_756 ?
O5 Nd1 O5 80.8(3) . 2_756 ?
O5 Nd1 O5 99.2(3) 5_776 2_756 ?
O5 Nd1 O5 180.0 6_575 2_756 ?
C1 N1 C12 120.7(3) . . ?
C1 N1 C3 112.7(3) . . ?
C12 N1 C3 126.3(3) . . ?
C1 N2 C4 121.0(3) . . ?
C1 N2 C2 112.9(3) . . ?
C4 N2 C2 125.8(3) . . ?
C5 N3 C7 112.2(3) . . ?
C5 N3 C4 123.2(3) . . ?
C7 N3 C4 123.0(3) . . ?
C5 N4 C8 122.6(3) . . ?
C5 N4 C6 112.2(3) . . ?
C8 N4 C6 123.7(3) . . ?
C9 N5 C8 122.9(3) . . ?
C9 N5 C11 111.7(3) . . ?
C8 N5 C11 123.9(3) . . ?
C9 N6 C12 123.3(3) . 2_756 ?
C9 N6 C10 111.9(3) . . ?
C12 N6 C10 123.2(3) 2_756 . ?
O4 O4 Nd1 69.08(11) 6_575 . ?
O7 O7 Nd1 69.24(11) 6_575 . ?
O1 C1 N1 125.6(3) . . ?
O1 C1 N2 125.5(3) . . ?
N1 C1 N2 108.8(2) . . ?
N2 C2 N2 113.6(3) 6_565 . ?
N2 C2 C13 110.9(2) 6_565 . ?
N2 C2 C13 110.9(2) . . ?
N2 C2 C3 102.6(2) 6_565 . ?
N2 C2 C3 102.6(2) . . ?
C13 C2 C3 115.8(4) . . ?
N1 C3 N1 114.0(3) 6_565 . ?
N1 C3 C14 110.8(2) 6_565 . ?
N1 C3 C14 110.8(2) . . ?
N1 C3 C2 102.9(2) 6_565 . ?
N1 C3 C2 102.9(2) . . ?
C14 C3 C2 115.1(4) . . ?
N2 C4 N3 113.9(2) . . ?
O2 C5 N4 125.3(3) . . ?
O2 C5 N3 125.7(3) . . ?
N4 C5 N3 108.9(3) . . ?
N4 C6 N4 114.8(3) . 6_565 ?
N4 C6 C7 103.2(2) . . ?
N4 C6 C7 103.2(2) 6_565 . ?
N3 C7 N3 114.5(4) . 6_565 ?
N3 C7 C6 103.2(2) . . ?
N3 C7 C6 103.2(2) 6_565 . ?
N5 C8 N4 113.8(2) . . ?
O3 C9 N5 125.2(3) . . ?
O3 C9 N6 125.5(3) . . ?
N5 C9 N6 109.3(3) . . ?
N6 C10 N6 114.7(4) 6_565 . ?
N6 C10 C11 103.5(2) 6_565 . ?
N6 C10 C11 103.5(2) . . ?
N5 C11 N5 114.2(3) 6_565 . ?
N5 C11 C10 103.3(2) 6_565 . ?
N5 C11 C10 103.3(2) . . ?
N6 C12 N1 114.5(2) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 O1 -2.1(4) . . . . ?
C3 N1 C1 O1 172.8(3) . . . . ?
C12 N1 C1 N2 -178.3(2) . . . . ?
C3 N1 C1 N2 -3.4(3) . . . . ?
C4 N2 C1 O1 0.7(4) . . . . ?
C2 N2 C1 O1 -172.6(3) . . . . ?
C4 N2 C1 N1 176.9(2) . . . . ?
C2 N2 C1 N1 3.6(3) . . . . ?
C1 N2 C2 N2 -112.4(3) . . . 6_565 ?
C4 N2 C2 N2 74.7(4) . . . 6_565 ?
C1 N2 C2 C13 121.9(3) . . . . ?
C4 N2 C2 C13 -51.0(4) . . . . ?
C1 N2 C2 C3 -2.4(3) . . . . ?
C4 N2 C2 C3 -175.3(3) . . . . ?
C1 N1 C3 N1 112.5(3) . . . 6_565 ?
C12 N1 C3 N1 -73.0(4) . . . 6_565 ?
C1 N1 C3 C14 -121.7(3) . . . . ?
C12 N1 C3 C14 52.8(4) . . . . ?
C1 N1 C3 C2 1.8(3) . . . . ?
C12 N1 C3 C2 176.4(3) . . . . ?
N2 C2 C3 N1 -0.3(3) 6_565 . . 6_565 ?
N2 C2 C3 N1 -118.4(2) . . . 6_565 ?
C13 C2 C3 N1 120.65(19) . . . 6_565 ?
N2 C2 C3 N1 118.4(2) 6_565 . . . ?
N2 C2 C3 N1 0.3(3) . . . . ?
C13 C2 C3 N1 -120.66(19) . . . . ?
N2 C2 C3 C14 -120.95(19) 6_565 . . . ?
N2 C2 C3 C14 120.95(19) . . . . ?
C13 C2 C3 C14 0.000(1) . . . . ?
C1 N2 C4 N3 101.3(3) . . . . ?
C2 N2 C4 N3 -86.4(4) . . . . ?
C5 N3 C4 N2 -108.9(3) . . . . ?
C7 N3 C4 N2 86.7(4) . . . . ?
C8 N4 C5 O2 -6.7(5) . . . . ?
C6 N4 C5 O2 -173.3(4) . . . . ?
C8 N4 C5 N3 171.9(3) . . . . ?
C6 N4 C5 N3 5.3(4) . . . . ?
C7 N3 C5 O2 173.2(4) . . . . ?
C4 N3 C5 O2 7.2(5) . . . . ?
C7 N3 C5 N4 -5.4(4) . . . . ?
C4 N3 C5 N4 -171.3(3) . . . . ?
C5 N4 C6 N4 -114.6(3) . . . 6_565 ?
C8 N4 C6 N4 79.0(4) . . . 6_565 ?
C5 N4 C6 C7 -3.0(4) . . . . ?
C8 N4 C6 C7 -169.5(3) . . . . ?
C5 N3 C7 N3 114.7(3) . . . 6_565 ?
C4 N3 C7 N3 -79.4(4) . . . 6_565 ?
C5 N3 C7 C6 3.3(4) . . . . ?
C4 N3 C7 C6 169.3(3) . . . . ?
N4 C6 C7 N3 -0.2(3) . . . . ?
N4 C6 C7 N3 119.7(3) 6_565 . . . ?
N4 C6 C7 N3 -119.7(3) . . . 6_565 ?
N4 C6 C7 N3 0.2(3) 6_565 . . 6_565 ?
C9 N5 C8 N4 -109.1(3) . . . . ?
C11 N5 C8 N4 85.9(4) . . . . ?
C5 N4 C8 N5 109.3(3) . . . . ?
C6 N4 C8 N5 -85.6(4) . . . . ?
C8 N5 C9 O3 7.2(5) . . . . ?
C11 N5 C9 O3 173.9(3) . . . . ?
C8 N5 C9 N6 -171.6(3) . . . . ?
C11 N5 C9 N6 -5.0(4) . . . . ?
C12 N6 C9 O3 -7.7(5) 2_756 . . . ?
C10 N6 C9 O3 -174.1(3) . . . . ?
C12 N6 C9 N5 171.2(3) 2_756 . . . ?
C10 N6 C9 N5 4.8(4) . . . . ?
C9 N6 C10 N6 -114.6(3) . . . 6_565 ?
C12 N6 C10 N6 78.9(4) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.6(3) . . . . ?
C12 N6 C10 C11 -169.1(3) 2_756 . . . ?
C9 N5 C11 N5 114.7(3) . . . 6_565 ?
C8 N5 C11 N5 -78.8(4) . . . 6_565 ?
C9 N5 C11 C10 3.2(3) . . . . ?
C8 N5 C11 C10 169.7(3) . . . . ?
N6 C10 C11 N5 0.3(3) 6_565 . . 6_565 ?
N6 C10 C11 N5 -119.7(3) . . . 6_565 ?
N6 C10 C11 N5 119.7(3) 6_565 . . . ?
N6 C10 C11 N5 -0.3(3) . . . . ?
C1 N1 C12 N6 -100.4(3) . . . 2_756 ?
C3 N1 C12 N6 85.5(4) . . . 2_756 ?

_refine_diff_density_max         0.539
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.067



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

data_6pp
_database_code_depnum_ccdc_archive 'CCDC 1038173'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT430_6pp                 
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This is the moderately close approach of two 
bound nitrates. It is not evidence of a significant
interaction. 
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.019 0.009 562 146 ' '
2 0.750 -0.022 0.012 562 146 ' '
_platon_squeeze_details          ?


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl2 N26 O29 Sm2'
_chemical_formula_weight         1724.61

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           53
_space_group_name_H-M_alt        'P m n a'
_space_group_name_Hall           '-P 2ac 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   25.712(9)
_cell_length_b                   10.726(4)
_cell_length_c                   14.392(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3969(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4684
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      23.43

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.617
_shelx_estimated_absorpt_T_min   0.669
_shelx_estimated_absorpt_T_max   0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19851
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.584
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3681
_reflns_number_gt                2766
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1131P)²+28.6903P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3681
_refine_ls_number_parameters     237
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.2159
_refine_ls_wR_factor_gt          0.2009
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.055
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4W O 0.2209(7) 1.2543(14) 0.1058(13) 0.082(5) Uiso 0.5 1 d . . P . .
O3WA O 0.2500 0.877(3) 0.2500 0.081(4) Uiso 0.5 2 d S U P A 1
O3WB O 0.2310(6) 0.8663(19) 0.2205(11) 0.081(4) Uiso 0.5 1 d . U P B 2
C1 C 0.0000 0.9719(11) 0.1641(7) 0.043(3) Uani 1 2 d S T P . .
C2 C 0.0944(4) 0.9901(8) 0.1657(5) 0.045(2) Uani 1 1 d . . . . .
H2A H 0.0930 0.9023 0.1496 0.054 Uiso 1 1 calc R U . . .
H2B H 0.1186 1.0301 0.1234 0.054 Uiso 1 1 calc R U . . .
C3 C 0.1140(3) 0.9065(8) 0.3218(6) 0.0408(19) Uani 1 1 d . . . . .
C4 C 0.1666(4) 0.8401(8) 0.4565(6) 0.047(2) Uani 1 1 d . . . . .
H4A H 0.1580 0.7584 0.4320 0.057 Uiso 1 1 calc R U . . .
H4B H 0.2042 0.8480 0.4559 0.057 Uiso 1 1 calc R U . . .
C5 C 0.1225(3) 1.2460(7) 0.4059(6) 0.0385(19) Uani 1 1 d . . . . .
C6 C 0.0576(4) 1.2215(8) 0.0507(6) 0.049(2) Uani 1 1 d . . . . .
H6A H 0.0946 1.2155 0.0587 0.074 Uiso 1 1 calc R U . . .
H6B H 0.0481 1.3068 0.0399 0.074 Uiso 1 1 calc R U . . .
H6C H 0.0472 1.1717 -0.0016 0.074 Uiso 1 1 calc R U . . .
C7 C 0.0306(3) 1.1748(7) 0.1372(6) 0.0421(19) Uani 1 1 d . . . . .
C8 C 0.1479(3) 1.1045(8) 0.2891(6) 0.0421(19) Uani 1 1 d . . . . .
H8 H 0.1762 1.1205 0.2450 0.051 Uiso 1 1 calc R U . . .
C9 C 0.1682(3) 1.0593(8) 0.3844(6) 0.0439(19) Uani 1 1 d . . . . .
H9 H 0.2063 1.0546 0.3855 0.053 Uiso 1 1 calc R U . . .
C10 C 0.0000 1.2922(11) 0.2650(9) 0.042(3) Uani 1 2 d S T P . .
C11 C 0.0949(3) 1.2941(8) 0.2433(6) 0.0409(18) Uani 1 1 d . . . . .
H11A H 0.0924 1.3786 0.2669 0.049 Uiso 1 1 calc R U . . .
H11B H 0.1166 1.2960 0.1883 0.049 Uiso 1 1 calc R U . . .
N1 N 0.0427(3) 1.0444(6) 0.1519(5) 0.0430(16) Uani 1 1 d . . . . .
N2 N 0.1142(3) 1.0019(6) 0.2593(4) 0.0414(16) Uani 1 1 d . . . . .
N3 N 0.1443(3) 0.9357(6) 0.3954(5) 0.0393(15) Uani 1 1 d . . . . .
N4 N 0.1488(3) 1.1521(6) 0.4492(5) 0.0405(15) Uani 1 1 d . . . . .
N5 N 0.0436(3) 1.2520(6) 0.2174(5) 0.0395(16) Uani 1 1 d . . . . .
N6 N 0.1199(3) 1.2166(7) 0.3132(5) 0.0432(17) Uani 1 1 d . . . . .
O1 O 0.0000 0.8599(8) 0.1799(5) 0.047(2) Uani 1 2 d S T P . .
O2 O 0.0905(2) 0.8073(5) 0.3110(4) 0.0448(14) Uani 1 1 d . . . . .
N7 N 0.0000 0.5754(9) 0.1672(6) 0.044(3) Uani 1 2 d S T P . .
O3 O 0.1061(2) 1.3407(5) 0.4418(4) 0.0476(14) Uani 1 1 d . . . . .
O4 O 0.0000 1.3611(7) 0.3330(5) 0.045(2) Uani 1 2 d S T P . .
O1W O 0.0000 0.7770(7) 0.4931(6) 0.051(2) Uani 1 2 d S T P . .
Sm1 Sm 0.0000 0.74660(5) 0.32701(4) 0.0389(3) Uani 1 2 d S T P . .
O2W O -0.0570(3) 0.5841(5) 0.3954(5) 0.0611(18) Uani 1 1 d . . . . .
Cl1 Cl 0.0000 1.0011(3) 0.3711(2) 0.0441(7) Uani 1 2 d S T P . .
O6 O 0.0000 0.5107(11) 0.0962(8) 0.092(4) Uani 1 2 d S TU P . .
O5 O 0.0406(3) 0.6087(7) 0.2026(5) 0.074(2) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3WB O3WB 1.30(3) 3 ?
C1 O1 1.223(15) . ?
C1 N1 1.357(10) . ?
C1 N1 1.357(10) 8 ?
C2 N2 1.446(10) . ?
C2 N1 1.464(11) . ?
C3 O2 1.233(10) . ?
C3 N3 1.352(10) . ?
C3 N2 1.362(10) . ?
C4 N4 1.436(11) 4_576 ?
C4 N3 1.469(11) . ?
C5 O3 1.216(9) . ?
C5 N4 1.363(10) . ?
C5 N6 1.373(10) . ?
C6 C7 1.510(12) . ?
C7 N1 1.449(10) . ?
C7 N5 1.459(10) . ?
C7 C7 1.574(18) 8 ?
C8 N6 1.443(11) . ?
C8 N2 1.465(10) . ?
C8 C9 1.545(12) . ?
C9 N4 1.452(10) . ?
C9 N3 1.470(10) . ?
C10 O4 1.226(14) . ?
C10 N5 1.382(10) . ?
C10 N5 1.382(10) 8 ?
C11 N5 1.444(11) . ?
C11 N6 1.454(11) . ?
N4 C4 1.436(11) 4_576 ?
O1 Sm1 2.441(8) . ?
O2 Sm1 2.428(6) . ?
N7 O5 1.215(9) . ?
N7 O5 1.215(9) 8 ?
N7 O6 1.236(13) . ?
N7 Sm1 2.943(9) . ?
O1W Sm1 2.412(9) . ?
Sm1 O2 2.428(6) 8 ?
Sm1 O2W 2.481(6) . ?
Sm1 O2W 2.481(6) 8 ?
Sm1 O5 2.545(7) . ?
Sm1 O5 2.545(7) 8 ?
Sm1 Cl1 2.803(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 125.9(5) . . ?
O1 C1 N1 125.9(5) . 8 ?
N1 C1 N1 108.1(10) . 8 ?
N2 C2 N1 114.3(7) . . ?
O2 C3 N3 125.5(8) . . ?
O2 C3 N2 124.5(8) . . ?
N3 C3 N2 109.9(7) . . ?
N4 C4 N3 113.6(7) 4_576 . ?
O3 C5 N4 126.5(8) . . ?
O3 C5 N6 126.0(8) . . ?
N4 C5 N6 107.4(7) . . ?
N1 C7 N5 112.5(7) . . ?
N1 C7 C6 110.0(7) . . ?
N5 C7 C6 111.1(7) . . ?
N1 C7 C7 102.4(5) . 8 ?
N5 C7 C7 103.2(4) . 8 ?
C6 C7 C7 117.3(5) . 8 ?
N6 C8 N2 113.7(7) . . ?
N6 C8 C9 102.5(7) . . ?
N2 C8 C9 102.9(6) . . ?
N4 C9 N3 113.9(7) . . ?
N4 C9 C8 103.8(6) . . ?
N3 C9 C8 103.7(7) . . ?
O4 C10 N5 125.7(5) . . ?
O4 C10 N5 125.7(5) . 8 ?
N5 C10 N5 108.3(10) . 8 ?
N5 C11 N6 113.8(7) . . ?
C1 N1 C7 113.5(7) . . ?
C1 N1 C2 119.3(7) . . ?
C7 N1 C2 126.8(7) . . ?
C3 N2 C2 123.3(7) . . ?
C3 N2 C8 111.9(7) . . ?
C2 N2 C8 123.2(7) . . ?
C3 N3 C4 122.2(7) . . ?
C3 N3 C9 111.4(7) . . ?
C4 N3 C9 122.1(7) . . ?
C5 N4 C4 123.2(7) . 4_576 ?
C5 N4 C9 112.5(7) . . ?
C4 N4 C9 122.4(7) 4_576 . ?
C10 N5 C11 121.0(7) . . ?
C10 N5 C7 112.6(7) . . ?
C11 N5 C7 126.2(7) . . ?
C5 N6 C8 113.6(7) . . ?
C5 N6 C11 124.2(7) . . ?
C8 N6 C11 122.1(7) . . ?
C1 O1 Sm1 130.6(7) . . ?
C3 O2 Sm1 133.5(5) . . ?
O5 N7 O5 118.3(10) . 8 ?
O5 N7 O6 120.8(5) . . ?
O5 N7 O6 120.8(5) 8 . ?
O5 N7 Sm1 59.2(5) . . ?
O5 N7 Sm1 59.2(5) 8 . ?
O6 N7 Sm1 175.6(9) . . ?
O1W Sm1 O2 93.31(15) . 8 ?
O1W Sm1 O2 93.31(15) . . ?
O2 Sm1 O2 146.9(3) 8 . ?
O1W Sm1 O1 142.4(3) . . ?
O2 Sm1 O1 77.53(14) 8 . ?
O2 Sm1 O1 77.53(14) . . ?
O1W Sm1 O2W 72.7(2) . . ?
O2 Sm1 O2W 70.1(2) 8 . ?
O2 Sm1 O2W 142.4(2) . . ?
O1 Sm1 O2W 133.9(2) . . ?
O1W Sm1 O2W 72.7(2) . 8 ?
O2 Sm1 O2W 142.4(2) 8 8 ?
O2 Sm1 O2W 70.1(2) . 8 ?
O1 Sm1 O2W 133.9(2) . 8 ?
O2W Sm1 O2W 72.4(3) . 8 ?
O1W Sm1 O5 140.8(2) . . ?
O2 Sm1 O5 118.8(2) 8 . ?
O2 Sm1 O5 72.3(2) . . ?
O1 Sm1 O5 71.3(2) . . ?
O2W Sm1 O5 96.5(2) . . ?
O2W Sm1 O5 68.2(2) 8 . ?
O1W Sm1 O5 140.8(2) . 8 ?
O2 Sm1 O5 72.3(2) 8 8 ?
O2 Sm1 O5 118.8(2) . 8 ?
O1 Sm1 O5 71.3(2) . 8 ?
O2W Sm1 O5 68.2(2) . 8 ?
O2W Sm1 O5 96.5(2) 8 8 ?
O5 Sm1 O5 48.4(4) . 8 ?
O1W Sm1 Cl1 69.1(2) . . ?
O2 Sm1 Cl1 76.12(14) 8 . ?
O2 Sm1 Cl1 76.12(14) . . ?
O1 Sm1 Cl1 73.2(2) . . ?
O2W Sm1 Cl1 126.49(15) . . ?
O2W Sm1 Cl1 126.49(15) 8 . ?
O5 Sm1 Cl1 136.48(19) . . ?
O5 Sm1 Cl1 136.48(19) 8 . ?
O1W Sm1 N7 149.2(3) . . ?
O2 Sm1 N7 95.35(14) 8 . ?
O2 Sm1 N7 95.35(14) . . ?
O1 Sm1 N7 68.5(3) . . ?
O2W Sm1 N7 82.6(2) . . ?
O2W Sm1 N7 82.6(2) 8 . ?
O5 Sm1 N7 24.22(19) . . ?
O5 Sm1 N7 24.22(19) 8 . ?
Cl1 Sm1 N7 141.7(2) . . ?
N7 O5 Sm1 96.5(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 C8 C9 N4 0.1(8) . . . . ?
N2 C8 C9 N4 -118.1(7) . . . . ?
N6 C8 C9 N3 119.4(7) . . . . ?
N2 C8 C9 N3 1.1(8) . . . . ?
O1 C1 N1 C7 -178.1(10) . . . . ?
N1 C1 N1 C7 4.4(12) 8 . . . ?
O1 C1 N1 C2 -5.5(15) . . . . ?
N1 C1 N1 C2 177.1(5) 8 . . . ?
N5 C7 N1 C1 107.5(9) . . . . ?
C6 C7 N1 C1 -128.1(8) . . . . ?
C7 C7 N1 C1 -2.7(7) 8 . . . ?
N5 C7 N1 C2 -64.5(10) . . . . ?
C6 C7 N1 C2 59.9(10) . . . . ?
C7 C7 N1 C2 -174.6(6) 8 . . . ?
N2 C2 N1 C1 -90.9(10) . . . . ?
N2 C2 N1 C7 80.6(10) . . . . ?
O2 C3 N2 C2 -11.0(13) . . . . ?
N3 C3 N2 C2 167.2(7) . . . . ?
O2 C3 N2 C8 -176.7(8) . . . . ?
N3 C3 N2 C8 1.4(9) . . . . ?
N1 C2 N2 C3 102.0(9) . . . . ?
N1 C2 N2 C8 -93.9(9) . . . . ?
N6 C8 N2 C3 -111.7(8) . . . . ?
C9 C8 N2 C3 -1.6(9) . . . . ?
N6 C8 N2 C2 82.6(9) . . . . ?
C9 C8 N2 C2 -167.3(7) . . . . ?
O2 C3 N3 C4 20.3(13) . . . . ?
N2 C3 N3 C4 -157.8(7) . . . . ?
O2 C3 N3 C9 177.5(8) . . . . ?
N2 C3 N3 C9 -0.6(9) . . . . ?
N4 C4 N3 C3 -117.3(8) 4_576 . . . ?
N4 C4 N3 C9 87.9(9) 4_576 . . . ?
N4 C9 N3 C3 111.7(8) . . . . ?
C8 C9 N3 C3 -0.4(9) . . . . ?
N4 C9 N3 C4 -91.0(9) . . . . ?
C8 C9 N3 C4 156.8(7) . . . . ?
O3 C5 N4 C4 -8.3(13) . . . 4_576 ?
N6 C5 N4 C4 169.3(7) . . . 4_576 ?
O3 C5 N4 C9 -173.3(8) . . . . ?
N6 C5 N4 C9 4.3(9) . . . . ?
N3 C9 N4 C5 -114.7(7) . . . . ?
C8 C9 N4 C5 -2.7(9) . . . . ?
N3 C9 N4 C4 80.1(9) . . . 4_576 ?
C8 C9 N4 C4 -167.8(7) . . . 4_576 ?
O4 C10 N5 C11 -2.6(16) . . . . ?
N5 C10 N5 C11 171.5(6) 8 . . . ?
O4 C10 N5 C7 -177.6(10) . . . . ?
N5 C10 N5 C7 -3.6(12) 8 . . . ?
N6 C11 N5 C10 89.0(10) . . . . ?
N6 C11 N5 C7 -96.7(9) . . . . ?
N1 C7 N5 C10 -107.5(9) . . . . ?
C6 C7 N5 C10 128.7(9) . . . . ?
C7 C7 N5 C10 2.1(7) 8 . . . ?
N1 C7 N5 C11 77.8(10) . . . . ?
C6 C7 N5 C11 -46.0(10) . . . . ?
C7 C7 N5 C11 -172.6(6) 8 . . . ?
O3 C5 N6 C8 173.3(8) . . . . ?
N4 C5 N6 C8 -4.3(10) . . . . ?
O3 C5 N6 C11 -2.3(14) . . . . ?
N4 C5 N6 C11 -179.8(7) . . . . ?
N2 C8 N6 C5 112.9(8) . . . . ?
C9 C8 N6 C5 2.5(9) . . . . ?
N2 C8 N6 C11 -71.5(10) . . . . ?
C9 C8 N6 C11 178.2(7) . . . . ?
N5 C11 N6 C5 -100.8(9) . . . . ?
N5 C11 N6 C8 84.0(10) . . . . ?
N1 C1 O1 Sm1 91.5(10) . . . . ?
N1 C1 O1 Sm1 -91.5(10) 8 . . . ?
N3 C3 O2 Sm1 103.8(9) . . . . ?
N2 C3 O2 Sm1 -78.3(10) . . . . ?
O5 N7 O5 Sm1 -4.1(12) 8 . . . ?
O6 N7 O5 Sm1 174.8(10) . . . . ?

_refine_diff_density_max         2.561
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.155



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

data_6
_database_code_depnum_ccdc_archive 'CCDC 1038174'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_6                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) 
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_6                   
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;


_vrf_PLAT075_6                   
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_6                   
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

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 -0.001 -0.020 0.000 1231 447 ' '
2 0.500 0.000 0.500 120 12 ' '
3 1.000 0.500 0.500 120 12 ' '
_platon_squeeze_details          ?

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 N24 O20 Sm'
_chemical_formula_weight         1331.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.308(10)
_cell_length_b                   12.540(6)
_cell_length_c                   14.747(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.685(4)
_cell_angle_gamma                90
_cell_volume                     3718(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5407
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      24.13

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             1348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.861
_shelx_estimated_absorpt_T_min   0.801
_shelx_estimated_absorpt_T_max   0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9884
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.532
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             3482
_reflns_number_gt                3323
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0518P)²+3.2968P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3482
_refine_ls_number_parameters     225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.1017
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.121
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 1.0000 1.0000 0.5000 0.03602(14) Uani 1 4 d S T P . .
N1 N 0.77308(14) 0.4025(2) 0.4147(2) 0.0430(6) Uani 1 1 d . . . . .
N2 N 0.82035(13) 0.40229(19) 0.5807(2) 0.0424(6) Uani 1 1 d . . . . .
N3 N 0.92412(14) 0.40308(19) 0.7316(2) 0.0437(7) Uani 1 1 d . . . . .
N4 N 1.03399(13) 0.4028(2) 0.8111(2) 0.0425(6) Uani 1 1 d . . . . .
N5 N 1.14270(14) 0.4031(2) 0.8118(2) 0.0448(7) Uani 1 1 d . . . . .
N6 N 1.20783(14) 0.4032(2) 0.7346(2) 0.0442(7) Uani 1 1 d . . . . .
O1 O 0.83586(13) 0.25832(18) 0.4980(2) 0.0546(6) Uani 1 1 d . . . . .
O2 O 0.98116(14) 0.2571(2) 0.7164(2) 0.0707(8) Uani 1 1 d . . . . .
O3 O 1.14136(16) 0.2580(2) 0.7169(2) 0.0705(8) Uani 1 1 d . . . . .
O4 O 0.9053(3) 0.9308(4) 0.3574(4) 0.0709(17) Uani 0.5 1 d . . P A 1
O6 O 0.9521(3) 0.8528(4) 0.5530(4) 0.0610(14) Uani 0.5 1 d . . P A 1
O5 O 0.9218(3) 0.8524(4) 0.4472(4) 0.0608(14) Uani 0.5 1 d . . P B 2
O7 O 0.9890(3) 0.9312(4) 0.6442(4) 0.0643(15) Uani 0.5 1 d . . P A 2
C1 C 0.81281(15) 0.3468(2) 0.4980(3) 0.0418(8) Uani 1 1 d . . . . .
C2 C 0.7802(2) 0.5000 0.5563(4) 0.0399(10) Uani 1 2 d S T P . .
C3 C 0.7468(2) 0.5000 0.4386(4) 0.0402(10) Uani 1 2 d S T P . .
C4 C 0.85782(17) 0.3600(3) 0.6800(3) 0.0472(8) Uani 1 1 d . . . . .
H4A H 0.8609 0.2833 0.6753 0.057 Uiso 1 1 calc R U . . .
H4B H 0.8338 0.3744 0.7200 0.057 Uiso 1 1 calc R U . . .
C5 C 0.97977(18) 0.3462(2) 0.7491(3) 0.0453(8) Uani 1 1 d . . . . .
C6 C 1.0155(2) 0.5000 0.8452(3) 0.0413(10) Uani 1 2 d S T P . .
H6 H 1.0311 0.5000 0.9184 0.050 Uiso 1 2 calc R U P . .
C7 C 0.9389(2) 0.5000 0.7902(4) 0.0418(10) Uani 1 2 d S T P . .
H7 H 0.9188 0.5000 0.8376 0.050 Uiso 1 2 calc R U P . .
C8 C 1.10047(17) 0.3593(3) 0.8534(3) 0.0473(8) Uani 1 1 d . . . . .
H8A H 1.1210 0.3718 0.9254 0.057 Uiso 1 1 calc R U . . .
H8B H 1.0976 0.2827 0.8429 0.057 Uiso 1 1 calc R U . . .
C9 C 1.16158(18) 0.3463(3) 0.7504(3) 0.0473(8) Uani 1 1 d . . . . .
C10 C 1.2259(2) 0.5000 0.7933(3) 0.0409(11) Uani 1 2 d S T P . .
H10 H 1.2731 0.5000 0.8412 0.049 Uiso 1 2 calc R U P . .
C11 C 1.1810(2) 0.5000 0.8471(3) 0.0395(10) Uani 1 2 d S T P . .
H11 H 1.2068 0.5000 0.9204 0.047 Uiso 1 2 calc R U P . .
C12 C 0.75465(18) 0.3605(3) 0.3151(3) 0.0486(9) Uani 1 1 d . . . . .
H12A H 0.7603 0.2836 0.3198 0.058 Uiso 1 1 calc R U . . .
H12B H 0.7079 0.3750 0.2742 0.058 Uiso 1 1 calc R U . . .
C13 C 0.7331(3) 0.5000 0.6061(5) 0.0622(15) Uani 1 2 d S T P . .
H13A H 0.7123 0.4314 0.5976 0.093 Uiso 0.5 1 calc R U P . .
H13B H 0.6996 0.5537 0.5756 0.093 Uiso 0.5 1 calc R U P . .
H13C H 0.7577 0.5150 0.6766 0.093 Uiso 0.5 1 calc R U P . .
C14 C 0.6712(2) 0.5000 0.3897(4) 0.0604(14) Uani 1 2 d S T P . .
H14A H 0.6554 0.4353 0.4066 0.091 Uiso 0.5 1 calc R U P . .
H14B H 0.6555 0.5600 0.4135 0.091 Uiso 0.5 1 calc R U P . .
H14C H 0.6551 0.5047 0.3179 0.091 Uiso 1 2 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O7 2.404(5) . ?
Sm1 O7 2.404(5) 6_575 ?
Sm1 O7 2.404(5) 2_756 ?
Sm1 O7 2.404(5) 5_776 ?
Sm1 O4 2.405(5) . ?
Sm1 O4 2.405(5) 5_776 ?
Sm1 O4 2.405(5) 2_756 ?
Sm1 O4 2.405(5) 6_575 ?
Sm1 O6 2.425(5) . ?
Sm1 O6 2.425(5) 5_776 ?
Sm1 O6 2.425(5) 2_756 ?
Sm1 O6 2.425(5) 6_575 ?
N1 C1 1.356(4) . ?
N1 C12 1.443(4) . ?
N1 C3 1.463(4) . ?
N2 C1 1.350(4) . ?
N2 C4 1.436(4) . ?
N2 C2 1.467(3) . ?
N3 C5 1.356(4) . ?
N3 C4 1.443(4) . ?
N3 C7 1.444(4) . ?
N4 C5 1.358(4) . ?
N4 C8 1.444(4) . ?
N4 C6 1.445(4) . ?
N5 C9 1.355(5) . ?
N5 C8 1.438(4) . ?
N5 C11 1.447(4) . ?
N6 C9 1.355(5) . ?
N6 C12 1.434(4) 2_756 ?
N6 C10 1.444(4) . ?
O1 C1 1.223(4) . ?
O2 C5 1.222(4) . ?
O3 C9 1.217(4) . ?
O4 O4 1.736(10) 6_575 ?
O7 O7 1.724(10) 6_575 ?
C2 N2 1.467(3) 6_565 ?
C2 C13 1.521(7) . ?
C2 C3 1.564(7) . ?
C3 N1 1.463(4) 6_565 ?
C3 C14 1.518(7) . ?
C6 N4 1.445(4) 6_565 ?
C6 C7 1.541(7) . ?
C7 N3 1.444(4) 6_565 ?
C10 N6 1.444(4) 6_565 ?
C10 C11 1.524(7) . ?
C11 N5 1.447(4) 6_565 ?
C12 N6 1.434(4) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Sm1 O7 42.0(2) . 6_575 ?
O7 Sm1 O7 138.0(2) . 2_756 ?
O7 Sm1 O7 180.0 6_575 2_756 ?
O7 Sm1 O7 180.0 . 5_776 ?
O7 Sm1 O7 138.0(2) 6_575 5_776 ?
O7 Sm1 O7 42.0(2) 2_756 5_776 ?
O4 Sm1 O4 180.0 . 5_776 ?
O4 Sm1 O4 137.7(2) . 2_756 ?
O4 Sm1 O4 42.3(2) 5_776 2_756 ?
O4 Sm1 O4 42.3(2) . 6_575 ?
O4 Sm1 O4 137.7(2) 5_776 6_575 ?
O4 Sm1 O4 180.0 2_756 6_575 ?
O4 Sm1 O6 70.4(2) . . ?
O4 Sm1 O6 109.6(2) 5_776 . ?
O4 Sm1 O6 77.7(2) 2_756 . ?
O4 Sm1 O6 102.3(2) 6_575 . ?
O4 Sm1 O6 109.6(2) . 5_776 ?
O4 Sm1 O6 70.4(2) 5_776 5_776 ?
O4 Sm1 O6 102.3(2) 2_756 5_776 ?
O4 Sm1 O6 77.7(2) 6_575 5_776 ?
O6 Sm1 O6 180.0 . 5_776 ?
O4 Sm1 O6 77.7(2) . 2_756 ?
O4 Sm1 O6 102.3(2) 5_776 2_756 ?
O4 Sm1 O6 70.4(2) 2_756 2_756 ?
O4 Sm1 O6 109.6(2) 6_575 2_756 ?
O6 Sm1 O6 80.9(3) . 2_756 ?
O6 Sm1 O6 99.1(3) 5_776 2_756 ?
O4 Sm1 O6 102.3(2) . 6_575 ?
O4 Sm1 O6 77.7(2) 5_776 6_575 ?
O4 Sm1 O6 109.6(2) 2_756 6_575 ?
O4 Sm1 O6 70.4(2) 6_575 6_575 ?
O6 Sm1 O6 99.1(3) . 6_575 ?
O6 Sm1 O6 80.9(3) 5_776 6_575 ?
O6 Sm1 O6 180.0(3) 2_756 6_575 ?
C1 N1 C12 121.3(3) . . ?
C1 N1 C3 112.7(3) . . ?
C12 N1 C3 125.7(3) . . ?
C1 N2 C4 121.4(3) . . ?
C1 N2 C2 112.6(3) . . ?
C4 N2 C2 125.6(3) . . ?
C5 N3 C4 123.3(3) . . ?
C5 N3 C7 112.1(3) . . ?
C4 N3 C7 123.1(3) . . ?
C5 N4 C8 122.8(3) . . ?
C5 N4 C6 111.7(3) . . ?
C8 N4 C6 124.3(3) . . ?
C9 N5 C8 122.4(3) . . ?
C9 N5 C11 112.1(3) . . ?
C8 N5 C11 124.1(3) . . ?
C9 N6 C12 123.2(3) . 2_756 ?
C9 N6 C10 112.0(3) . . ?
C12 N6 C10 123.2(3) 2_756 . ?
O4 O4 Sm1 68.85(12) 6_575 . ?
O7 O7 Sm1 68.98(12) 6_575 . ?
O1 C1 N2 125.4(3) . . ?
O1 C1 N1 125.3(3) . . ?
N2 C1 N1 109.2(3) . . ?
N2 C2 N2 113.2(4) 6_565 . ?
N2 C2 C13 110.9(3) 6_565 . ?
N2 C2 C13 110.9(3) . . ?
N2 C2 C3 102.7(3) 6_565 . ?
N2 C2 C3 102.7(3) . . ?
C13 C2 C3 116.0(4) . . ?
N1 C3 N1 113.3(4) 6_565 . ?
N1 C3 C14 111.3(2) 6_565 . ?
N1 C3 C14 111.3(2) . . ?
N1 C3 C2 102.6(2) 6_565 . ?
N1 C3 C2 102.6(2) . . ?
C14 C3 C2 115.2(4) . . ?
N2 C4 N3 114.2(3) . . ?
O2 C5 N3 125.7(3) . . ?
O2 C5 N4 125.2(3) . . ?
N3 C5 N4 109.2(3) . . ?
N4 C6 N4 115.0(4) . 6_565 ?
N4 C6 C7 103.6(3) . . ?
N4 C6 C7 103.6(3) 6_565 . ?
N3 C7 N3 114.6(4) . 6_565 ?
N3 C7 C6 103.2(3) . . ?
N3 C7 C6 103.2(3) 6_565 . ?
N5 C8 N4 114.3(3) . . ?
O3 C9 N5 125.6(4) . . ?
O3 C9 N6 125.8(4) . . ?
N5 C9 N6 108.6(3) . . ?
N6 C10 N6 114.5(4) 6_565 . ?
N6 C10 C11 103.7(3) 6_565 . ?
N6 C10 C11 103.7(3) . . ?
N5 C11 N5 114.3(4) 6_565 . ?
N5 C11 C10 103.4(3) 6_565 . ?
N5 C11 C10 103.4(3) . . ?
N6 C12 N1 114.3(3) 2_756 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N2 C1 O1 0.1(5) . . . . ?
C2 N2 C1 O1 -173.0(3) . . . . ?
C4 N2 C1 N1 177.3(3) . . . . ?
C2 N2 C1 N1 4.2(4) . . . . ?
C12 N1 C1 O1 -0.7(5) . . . . ?
C3 N1 C1 O1 173.0(3) . . . . ?
C12 N1 C1 N2 -177.9(3) . . . . ?
C3 N1 C1 N2 -4.2(4) . . . . ?
C1 N2 C2 N2 -112.5(4) . . . 6_565 ?
C4 N2 C2 N2 74.8(5) . . . 6_565 ?
C1 N2 C2 C13 122.1(4) . . . . ?
C4 N2 C2 C13 -50.6(5) . . . . ?
C1 N2 C2 C3 -2.5(4) . . . . ?
C4 N2 C2 C3 -175.2(3) . . . . ?
C1 N1 C3 N1 112.4(4) . . . 6_565 ?
C12 N1 C3 N1 -74.2(5) . . . 6_565 ?
C1 N1 C3 C14 -121.2(4) . . . . ?
C12 N1 C3 C14 52.1(5) . . . . ?
C1 N1 C3 C2 2.5(4) . . . . ?
C12 N1 C3 C2 175.9(3) . . . . ?
N2 C2 C3 N1 0.0(3) 6_565 . . 6_565 ?
N2 C2 C3 N1 -117.7(3) . . . 6_565 ?
C13 C2 C3 N1 121.1(2) . . . 6_565 ?
N2 C2 C3 N1 117.7(3) 6_565 . . . ?
N2 C2 C3 N1 0.0(3) . . . . ?
C13 C2 C3 N1 -121.1(2) . . . . ?
N2 C2 C3 C14 -121.1(2) 6_565 . . . ?
N2 C2 C3 C14 121.1(2) . . . . ?
C13 C2 C3 C14 0.000(1) . . . . ?
C1 N2 C4 N3 101.3(4) . . . . ?
C2 N2 C4 N3 -86.6(4) . . . . ?
C5 N3 C4 N2 -108.6(4) . . . . ?
C7 N3 C4 N2 86.7(4) . . . . ?
C4 N3 C5 O2 7.1(6) . . . . ?
C7 N3 C5 O2 173.3(4) . . . . ?
C4 N3 C5 N4 -171.3(3) . . . . ?
C7 N3 C5 N4 -5.1(4) . . . . ?
C8 N4 C5 O2 -5.7(6) . . . . ?
C6 N4 C5 O2 -173.6(4) . . . . ?
C8 N4 C5 N3 172.7(3) . . . . ?
C6 N4 C5 N3 4.8(4) . . . . ?
C5 N4 C6 N4 -115.0(4) . . . 6_565 ?
C8 N4 C6 N4 77.4(5) . . . 6_565 ?
C5 N4 C6 C7 -2.6(4) . . . . ?
C8 N4 C6 C7 -170.3(3) . . . . ?
C5 N3 C7 N3 114.8(4) . . . 6_565 ?
C4 N3 C7 N3 -79.0(5) . . . 6_565 ?
C5 N3 C7 C6 3.3(4) . . . . ?
C4 N3 C7 C6 169.5(3) . . . . ?
N4 C6 C7 N3 -0.4(4) . . . . ?
N4 C6 C7 N3 120.1(3) 6_565 . . . ?
N4 C6 C7 N3 -120.1(3) . . . 6_565 ?
N4 C6 C7 N3 0.4(4) 6_565 . . 6_565 ?
C9 N5 C8 N4 -108.8(4) . . . . ?
C11 N5 C8 N4 85.6(4) . . . . ?
C5 N4 C8 N5 108.7(4) . . . . ?
C6 N4 C8 N5 -84.9(4) . . . . ?
C8 N5 C9 O3 6.6(5) . . . . ?
C11 N5 C9 O3 173.8(4) . . . . ?
C8 N5 C9 N6 -171.9(3) . . . . ?
C11 N5 C9 N6 -4.8(4) . . . . ?
C12 N6 C9 O3 -7.7(6) 2_756 . . . ?
C10 N6 C9 O3 -173.9(4) . . . . ?
C12 N6 C9 N5 170.8(3) 2_756 . . . ?
C10 N6 C9 N5 4.6(4) . . . . ?
C9 N6 C10 N6 -114.8(4) . . . 6_565 ?
C12 N6 C10 N6 79.0(5) 2_756 . . 6_565 ?
C9 N6 C10 C11 -2.7(4) . . . . ?
C12 N6 C10 C11 -168.9(3) 2_756 . . . ?
C9 N5 C11 N5 114.7(4) . . . 6_565 ?
C8 N5 C11 N5 -78.5(5) . . . 6_565 ?
C9 N5 C11 C10 3.0(4) . . . . ?
C8 N5 C11 C10 169.9(3) . . . . ?
N6 C10 C11 N5 0.2(3) 6_565 . . 6_565 ?
N6 C10 C11 N5 -119.7(3) . . . 6_565 ?
N6 C10 C11 N5 119.7(3) 6_565 . . . ?
N6 C10 C11 N5 -0.2(3) . . . . ?
C1 N1 C12 N6 -100.7(4) . . . 2_756 ?
C3 N1 C12 N6 86.5(4) . . . 2_756 ?

_refine_diff_density_max         0.911
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.070



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

data_7p
_database_code_depnum_ccdc_archive 'CCDC 1038175'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_7p                  
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_7p                  
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

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 -0.001 -0.021 0.000 1244 498 ' '
2 0.500 0.142 0.500 23 3 ' '
3 1.000 0.358 0.500 23 3 ' '
4 1.000 0.642 0.500 23 3 ' '
5 0.500 0.858 0.500 23 3 ' '
_platon_squeeze_details          ?

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Eu N24 O22'
_chemical_formula_weight         1364.95

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.329(10)
_cell_length_b                   12.544(6)
_cell_length_c                   14.897(7)
_cell_angle_alpha                90
_cell_angle_beta                 116.150(5)
_cell_angle_gamma                90
_cell_volume                     3746(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3836
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      24.08

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             1382
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.912
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9690
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.523
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             3475
_reflns_number_gt                3202
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1012P)²+18.4386P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3475
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1666
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 1.0000 1.0000 0.5000 0.0246(2) Uani 1 4 d S T P . .
N1 N 0.7721(2) 0.4025(3) 0.4137(3) 0.0280(10) Uani 1 1 d . . . . .
N2 N 0.8208(2) 0.4023(3) 0.5807(4) 0.0298(10) Uani 1 1 d . . . . .
N3 N 0.9256(2) 0.4029(4) 0.7329(4) 0.0329(11) Uani 1 1 d . . . . .
N4 N 1.0360(2) 0.4025(4) 0.8131(4) 0.0323(11) Uani 1 1 d . . . . .
N5 N 1.1444(2) 0.4029(4) 0.8132(4) 0.0324(11) Uani 1 1 d . . . . .
N6 N 1.2091(3) 0.4035(4) 0.7347(4) 0.0351(11) Uani 1 1 d . . . . .
O1 O 0.8360(2) 0.2580(3) 0.4972(3) 0.0423(11) Uani 1 1 d . . . . .
O2 O 0.9830(2) 0.2567(4) 0.7184(4) 0.0609(15) Uani 1 1 d . . . . .
O3 O 1.1424(3) 0.2578(4) 0.7181(4) 0.0603(14) Uani 1 1 d . . . . .
O4 O 0.9039(4) 0.9311(7) 0.3598(7) 0.051(3) Uani 0.5 1 d . . P A 1
O6 O 0.9542(5) 0.8530(7) 0.5540(8) 0.050(2) Uani 0.5 1 d . . P A 1
O5 O 0.9222(5) 0.8522(7) 0.4478(7) 0.046(2) Uani 0.5 1 d . . P B 2
O7 O 0.9895(5) 0.9313(6) 0.6433(7) 0.049(2) Uani 0.5 1 d . . P A 2
C1 C 0.8128(3) 0.3468(4) 0.4972(5) 0.0319(13) Uani 1 1 d . . . . .
C2 C 0.7806(4) 0.5000 0.5565(7) 0.0312(18) Uani 1 2 d S T P . .
C3 C 0.7463(4) 0.5000 0.4381(6) 0.0276(16) Uani 1 2 d S T P . .
C4 C 0.8584(3) 0.3603(4) 0.6805(5) 0.0334(13) Uani 1 1 d . . . . .
H4A H 0.8611 0.2835 0.6763 0.040 Uiso 1 1 calc R U . . .
H4B H 0.8342 0.3756 0.7195 0.040 Uiso 1 1 calc R U . . .
C5 C 0.9817(3) 0.3461(4) 0.7512(5) 0.0357(13) Uani 1 1 d . . . . .
C6 C 1.0175(4) 0.5000 0.8471(6) 0.0270(16) Uani 1 2 d S T P . .
H6 H 1.0332 0.5000 0.9198 0.032 Uiso 1 2 calc R U P . .
C7 C 0.9404(4) 0.5000 0.7912(6) 0.0297(17) Uani 1 2 d S T P . .
H7 H 0.9202 0.5000 0.8377 0.036 Uiso 1 2 calc R U P . .
C8 C 1.1022(3) 0.3595(4) 0.8559(5) 0.0346(13) Uani 1 1 d . . . . .
H8A H 1.0994 0.2828 0.8467 0.042 Uiso 1 1 calc R U . . .
H8B H 1.1230 0.3735 0.9273 0.042 Uiso 1 1 calc R U . . .
C9 C 1.1630(3) 0.3462(4) 0.7521(4) 0.0343(13) Uani 1 1 d . . . . .
C10 C 1.2281(4) 0.5000 0.7939(6) 0.0279(16) Uani 1 2 d S T P . .
H10 H 1.2756 0.5000 0.8410 0.034 Uiso 1 2 calc R U P . .
C11 C 1.1834(4) 0.5000 0.8487(6) 0.0311(17) Uani 1 2 d S T P . .
H11 H 1.2097 0.5000 0.9215 0.037 Uiso 1 2 calc R U P . .
C12 C 0.7528(3) 0.3600(5) 0.3149(5) 0.0361(14) Uani 1 1 d . . . . .
H12A H 0.7058 0.3748 0.2741 0.043 Uiso 1 1 calc R U . . .
H12B H 0.7584 0.2832 0.3195 0.043 Uiso 1 1 calc R U . . .
C13 C 0.7333(4) 0.5000 0.6039(7) 0.038(2) Uani 1 2 d S T P . .
H13A H 0.7209 0.4280 0.6098 0.057 Uiso 0.5 1 calc R U P . .
H13B H 0.6941 0.5402 0.5630 0.057 Uiso 0.5 1 calc R U P . .
H13C H 0.7548 0.5318 0.6691 0.057 Uiso 0.5 1 calc R U P . .
C14 C 0.6711(4) 0.5000 0.3894(8) 0.045(2) Uani 1 2 d S T P . .
H14A H 0.6555 0.5383 0.4308 0.067 Uiso 0.5 1 calc R U P . .
H14B H 0.6552 0.4279 0.3812 0.067 Uiso 0.5 1 calc R U P . .
H14C H 0.6548 0.5338 0.3251 0.067 Uiso 0.5 1 calc R U P . .
O1W O 0.9140(4) 0.5000 0.5010(7) 0.074(2) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4 2.400(8) . ?
Eu1 O4 2.400(8) 5_776 ?
Eu1 O4 2.400(8) 6_575 ?
Eu1 O4 2.400(8) 2_756 ?
Eu1 O7 2.408(9) 6_575 ?
Eu1 O7 2.408(9) 2_756 ?
Eu1 O7 2.408(9) 5_776 ?
Eu1 O7 2.408(9) . ?
Eu1 O6 2.412(8) . ?
Eu1 O6 2.412(8) 5_776 ?
Eu1 O6 2.412(8) 2_756 ?
Eu1 O6 2.412(8) 6_575 ?
N1 C1 1.366(8) . ?
N1 C12 1.442(8) . ?
N1 C3 1.464(6) . ?
N2 C1 1.366(8) . ?
N2 C4 1.446(8) . ?
N2 C2 1.467(6) . ?
N3 C5 1.361(8) . ?
N3 C7 1.447(6) . ?
N3 C4 1.454(7) . ?
N4 C5 1.354(8) . ?
N4 C8 1.432(7) . ?
N4 C6 1.452(6) . ?
N5 C9 1.355(7) . ?
N5 C11 1.454(7) . ?
N5 C8 1.456(7) . ?
N6 C9 1.372(8) . ?
N6 C10 1.447(6) . ?
N6 C12 1.456(7) 2_756 ?
O1 C1 1.230(7) . ?
O2 C5 1.228(7) . ?
O3 C9 1.222(7) . ?
O4 O4 1.729(17) 6_575 ?
O7 O7 1.723(16) 6_575 ?
C2 N2 1.467(6) 6_565 ?
C2 C13 1.508(11) . ?
C2 C3 1.584(12) . ?
C3 N1 1.464(6) 6_565 ?
C3 C14 1.507(12) . ?
C6 N4 1.452(6) 6_565 ?
C6 C7 1.546(11) . ?
C7 N3 1.447(6) 6_565 ?
C10 N6 1.447(6) 6_565 ?
C10 C11 1.544(11) . ?
C11 N5 1.454(6) 6_565 ?
C12 N6 1.456(7) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Eu1 O4 180.0 . 5_776 ?
O4 Eu1 O4 42.2(4) . 6_575 ?
O4 Eu1 O4 137.8(4) 5_776 6_575 ?
O4 Eu1 O4 137.8(4) . 2_756 ?
O4 Eu1 O4 42.2(4) 5_776 2_756 ?
O4 Eu1 O4 180.0 6_575 2_756 ?
O7 Eu1 O7 180.0 6_575 2_756 ?
O7 Eu1 O7 138.1(4) 6_575 5_776 ?
O7 Eu1 O7 41.9(4) 2_756 5_776 ?
O7 Eu1 O7 41.9(4) 6_575 . ?
O7 Eu1 O7 138.1(4) 2_756 . ?
O7 Eu1 O7 180.0 5_776 . ?
O4 Eu1 O6 70.5(4) . . ?
O4 Eu1 O6 109.5(4) 5_776 . ?
O4 Eu1 O6 102.6(3) 6_575 . ?
O4 Eu1 O6 77.4(3) 2_756 . ?
O4 Eu1 O6 109.5(4) . 5_776 ?
O4 Eu1 O6 70.5(4) 5_776 5_776 ?
O4 Eu1 O6 77.4(3) 6_575 5_776 ?
O4 Eu1 O6 102.6(3) 2_756 5_776 ?
O6 Eu1 O6 180.0 . 5_776 ?
O4 Eu1 O6 77.4(3) . 2_756 ?
O4 Eu1 O6 102.6(3) 5_776 2_756 ?
O4 Eu1 O6 109.5(4) 6_575 2_756 ?
O4 Eu1 O6 70.5(4) 2_756 2_756 ?
O6 Eu1 O6 80.3(5) . 2_756 ?
O6 Eu1 O6 99.7(5) 5_776 2_756 ?
O4 Eu1 O6 102.6(3) . 6_575 ?
O4 Eu1 O6 77.4(3) 5_776 6_575 ?
O4 Eu1 O6 70.5(4) 6_575 6_575 ?
O4 Eu1 O6 109.5(4) 2_756 6_575 ?
O6 Eu1 O6 99.7(5) . 6_575 ?
O6 Eu1 O6 80.3(5) 5_776 6_575 ?
O6 Eu1 O6 180.0 2_756 6_575 ?
C1 N1 C12 121.4(5) . . ?
C1 N1 C3 112.2(5) . . ?
C12 N1 C3 126.1(5) . . ?
C1 N2 C4 122.3(5) . . ?
C1 N2 C2 112.4(5) . . ?
C4 N2 C2 124.8(5) . . ?
C5 N3 C7 112.0(5) . . ?
C5 N3 C4 123.9(5) . . ?
C7 N3 C4 122.7(5) . . ?
C5 N4 C8 123.0(5) . . ?
C5 N4 C6 111.8(5) . . ?
C8 N4 C6 123.9(5) . . ?
C9 N5 C11 111.9(5) . . ?
C9 N5 C8 123.1(5) . . ?
C11 N5 C8 123.6(5) . . ?
C9 N6 C10 111.4(5) . . ?
C9 N6 C12 123.7(5) . 2_756 ?
C10 N6 C12 122.9(5) . 2_756 ?
O4 O4 Eu1 68.9(2) 6_575 . ?
O7 O7 Eu1 69.0(2) 6_575 . ?
O1 C1 N1 125.1(6) . . ?
O1 C1 N2 125.2(6) . . ?
N1 C1 N2 109.7(5) . . ?
N2 C2 N2 113.3(6) . 6_565 ?
N2 C2 C13 111.4(4) . . ?
N2 C2 C13 111.3(4) 6_565 . ?
N2 C2 C3 102.5(4) . . ?
N2 C2 C3 102.5(4) 6_565 . ?
C13 C2 C3 115.3(7) . . ?
N1 C3 N1 113.3(6) . 6_565 ?
N1 C3 C14 110.9(4) . . ?
N1 C3 C14 110.9(4) 6_565 . ?
N1 C3 C2 103.1(4) . . ?
N1 C3 C2 103.1(4) 6_565 . ?
C14 C3 C2 115.2(7) . . ?
N2 C4 N3 114.4(5) . . ?
O2 C5 N4 125.3(6) . . ?
O2 C5 N3 125.3(6) . . ?
N4 C5 N3 109.4(5) . . ?
N4 C6 N4 114.8(6) 6_565 . ?
N4 C6 C7 103.4(4) 6_565 . ?
N4 C6 C7 103.4(4) . . ?
N3 C7 N3 114.7(7) 6_565 . ?
N3 C7 C6 103.2(4) 6_565 . ?
N3 C7 C6 103.2(4) . . ?
N4 C8 N5 113.9(5) . . ?
O3 C9 N5 125.8(6) . . ?
O3 C9 N6 125.0(6) . . ?
N5 C9 N6 109.2(5) . . ?
N6 C10 N6 113.5(6) . 6_565 ?
N6 C10 C11 103.8(4) . . ?
N6 C10 C11 103.8(4) 6_565 . ?
N5 C11 N5 113.8(7) . 6_565 ?
N5 C11 C10 103.3(4) . . ?
N5 C11 C10 103.3(4) 6_565 . ?
N1 C12 N6 113.6(5) . 2_756 ?

_refine_diff_density_max         2.809
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.137



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

data_8pp
_database_code_depnum_ccdc_archive 'CCDC 1038176'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;


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 0.002 -0.021 0.000 840 316 ' '
_platon_squeeze_details          ?


_vrf_PLAT075_8pp                 
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_8pp                 
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

_vrf_PLAT306_8pp                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_8pp                 
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 Gd N24 O21'
_chemical_formula_weight         1460.59

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.397(3)
_cell_length_b                   12.4587(16)
_cell_length_c                   14.729(2)
_cell_angle_alpha                90
_cell_angle_beta                 115.102(4)
_cell_angle_gamma                90
_cell_volume                     3721.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9163
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_F_000             1470
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.073
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10621
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.527
_diffrn_reflns_theta_max         27.666
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             4079
_reflns_number_gt                3866
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1546P)²+27.5617P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4079
_refine_ls_number_parameters     254
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0736
_refine_ls_wR_factor_ref         0.2280
_refine_ls_wR_factor_gt          0.2240
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O8 O 1.1099(12) 1.0000 0.4939(17) 0.075(6) Uani 0.5 2 d S T P . .
Gd1 Gd 1.0000 1.0000 0.5000 0.0224(2) Uani 1 4 d S T P . .
N1 N 0.2742(2) 0.9019(4) 0.4164(4) 0.0223(10) Uani 1 1 d . . . . .
N2 N 0.3200(2) 0.9018(3) 0.5824(4) 0.0208(9) Uani 1 1 d . . . . .
N3 N 0.4230(2) 0.9027(4) 0.7326(4) 0.0228(10) Uani 1 1 d . . . . .
N4 N 0.5316(2) 0.9025(3) 0.8093(4) 0.0209(9) Uani 1 1 d . . . . .
N5 N 0.6395(2) 0.9029(4) 0.8101(4) 0.0229(10) Uani 1 1 d . . . . .
N6 N 0.7055(3) 0.9028(4) 0.7334(4) 0.0249(10) Uani 1 1 d . . . . .
O1 O 0.3366(2) 0.7567(3) 0.4998(4) 0.0318(10) Uani 1 1 d . . . . .
O2 O 0.4787(2) 0.7544(4) 0.7167(5) 0.0464(14) Uani 1 1 d . . . . .
O3 O 0.6386(3) 0.7566(4) 0.7149(4) 0.0459(13) Uani 1 1 d . . . . .
O4 O 0.9089(4) 0.9321(6) 0.3595(7) 0.037(2) Uani 0.5 1 d . . P A 1
O6 O 0.9525(5) 0.8557(7) 0.5505(7) 0.035(2) Uani 0.5 1 d . . P A 1
O5 O 0.9248(4) 0.8552(7) 0.4515(8) 0.036(2) Uani 0.5 1 d . . P A 2
O7 O 0.9899(6) 0.9327(7) 0.6442(7) 0.041(2) Uani 0.5 1 d . . P B 2
C1 C 0.3132(3) 0.8457(4) 0.4998(4) 0.0207(11) Uani 1 1 d . . . . .
C2 C 0.2802(4) 1.0000 0.5582(6) 0.0196(15) Uani 1 2 d S T P . .
C3 C 0.2482(4) 1.0000 0.4396(6) 0.0188(14) Uani 1 2 d S T P . .
C4 C 0.3568(3) 0.8591(4) 0.6821(4) 0.0236(12) Uani 1 1 d . . . . .
H4A H 0.3597 0.7818 0.6778 0.028 Uiso 1 1 calc R U . . .
H4B H 0.3329 0.8744 0.7222 0.028 Uiso 1 1 calc R U . . .
C5 C 0.4778(3) 0.8455(4) 0.7492(4) 0.0226(11) Uani 1 1 d . . . . .
C6 C 0.5138(4) 1.0000 0.8463(5) 0.0181(14) Uani 1 2 d S T P . .
H6 H 0.5299 1.0000 0.9194 0.022 Uiso 1 2 calc R U P . .
C7 C 0.4380(4) 1.0000 0.7921(5) 0.0179(14) Uani 1 2 d S T P . .
H7 H 0.4178 1.0000 0.8395 0.021 Uiso 1 2 calc R U P . .
C8 C 0.5974(3) 0.8585(4) 0.8531(4) 0.0229(11) Uani 1 1 d . . . . .
H8A H 0.5948 0.7813 0.8436 0.027 Uiso 1 1 calc R U . . .
H8B H 0.6171 0.8724 0.9246 0.027 Uiso 1 1 calc R U . . .
C9 C 0.6587(3) 0.8458(4) 0.7483(4) 0.0243(12) Uani 1 1 d . . . . .
C10 C 0.7234(4) 1.0000 0.7919(5) 0.0183(14) Uani 1 2 d S T P . .
H10 H 0.7700 1.0000 0.8397 0.022 Uiso 1 2 calc R U P . .
C11 C 0.6773(4) 1.0000 0.8456(5) 0.0179(14) Uani 1 2 d S T P . .
H11 H 0.7022 1.0000 0.9187 0.021 Uiso 1 2 calc R U P . .
C12 C 0.2568(3) 0.8592(4) 0.3173(4) 0.0256(12) Uani 1 1 d . . . . .
H12A H 0.2104 0.8732 0.2766 0.031 Uiso 1 1 calc R U . . .
H12B H 0.2627 0.7820 0.3224 0.031 Uiso 1 1 calc R U . . .
C13 C 0.2326(5) 1.0000 0.6058(7) 0.0305(18) Uani 1 2 d S T P . .
H13A H 0.2073 1.0651 0.5886 0.046 Uiso 0.5 1 calc R U P . .
H13B H 0.2035 0.9395 0.5818 0.046 Uiso 0.5 1 calc R U P . .
H13C H 0.2566 0.9953 0.6773 0.046 Uiso 1 2 calc R U P . .
C14 C 0.1733(4) 1.0000 0.3911(7) 0.0297(18) Uani 1 2 d S T P . .
H14A H 0.1574 1.0654 0.4076 0.045 Uiso 0.5 1 calc R U P . .
H14B H 0.1576 0.9947 0.3196 0.045 Uiso 1 2 calc R U P . .
H14C H 0.1574 0.9399 0.4154 0.045 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.9454(3) 0.5000 0.5039(5) 0.0564(14) Uani 0.5 2 d S T P . .
Cl2 Cl 0.8141(3) 0.5288(8) 0.8921(4) 0.051(4) Uani 0.25 1 d . U P . .
Cl3 Cl 0.9841(7) 0.7025(8) 0.9839(14) 0.069(4) Uani 0.25 1 d . U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O8 Gd1 2.50(2) . ?
Gd1 O4 2.361(8) . ?
Gd1 O4 2.361(8) 5_776 ?
Gd1 O4 2.361(8) 6_575 ?
Gd1 O4 2.361(8) 2_756 ?
Gd1 O5 2.363(8) 5_776 ?
Gd1 O5 2.363(8) 6_575 ?
Gd1 O5 2.363(8) 2_756 ?
Gd1 O5 2.363(8) . ?
Gd1 O6 2.364(9) . ?
Gd1 O6 2.364(9) 5_776 ?
Gd1 O6 2.364(8) 6_575 ?
Gd1 O6 2.364(8) 2_756 ?
N1 C1 1.361(7) . ?
N1 C12 1.442(7) . ?
N1 C3 1.456(6) . ?
N2 C1 1.353(8) . ?
N2 C4 1.447(7) . ?
N2 C2 1.467(6) . ?
N3 C5 1.349(7) . ?
N3 C7 1.449(6) . ?
N3 C4 1.453(7) . ?
N4 C5 1.355(7) . ?
N4 C8 1.443(7) . ?
N4 C6 1.454(6) . ?
N5 C9 1.361(8) . ?
N5 C11 1.442(6) . ?
N5 C8 1.449(7) . ?
N6 C9 1.357(8) . ?
N6 C10 1.442(6) . ?
N6 C12 1.450(8) 2_656 ?
O1 C1 1.228(7) . ?
O2 C5 1.235(7) . ?
O3 C9 1.222(7) . ?
O4 O4 1.691(16) 6_575 ?
O7 O7 1.676(17) 6_575 ?
C2 N2 1.467(6) 6_575 ?
C2 C13 1.504(12) . ?
C2 C3 1.581(11) . ?
C3 N1 1.456(6) 6_575 ?
C3 C14 1.521(11) . ?
C6 N4 1.454(6) 6_575 ?
C6 C7 1.538(10) . ?
C7 N3 1.449(6) 6_575 ?
C10 N6 1.442(6) 6_575 ?
C10 C11 1.543(11) . ?
C11 N5 1.442(6) 6_575 ?
C12 N6 1.451(8) 2_656 ?
Cl2 Cl2 0.72(2) 6_565 ?
Cl3 Cl3 0.67(3) 2_757 ?

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
O4 Gd1 O4 180.0 . 5_776 ?
O4 Gd1 O4 42.0(4) . 6_575 ?
O4 Gd1 O4 138.0(4) 5_776 6_575 ?
O4 Gd1 O4 138.0(4) . 2_756 ?
O4 Gd1 O4 42.0(4) 5_776 2_756 ?
O4 Gd1 O4 180.0 6_575 2_756 ?
O5 Gd1 O5 80.5(5) 5_776 6_575 ?
O5 Gd1 O5 99.5(5) 5_776 2_756 ?
O5 Gd1 O5 180.0 6_575 2_756 ?
O5 Gd1 O5 180.0 5_776 . ?
O5 Gd1 O5 99.5(5) 6_575 . ?
O5 Gd1 O5 80.5(5) 2_756 . ?
O4 Gd1 O6 70.5(3) . . ?
O4 Gd1 O6 109.5(3) 5_776 . ?
O4 Gd1 O6 102.2(3) 6_575 . ?
O4 Gd1 O6 77.8(3) 2_756 . ?
O4 Gd1 O6 109.5(3) . 5_776 ?
O4 Gd1 O6 70.5(3) 5_776 5_776 ?
O4 Gd1 O6 77.8(3) 6_575 5_776 ?
O4 Gd1 O6 102.2(3) 2_756 5_776 ?
O6 Gd1 O6 180.0 . 5_776 ?
O4 Gd1 O6 102.2(3) . 6_575 ?
O4 Gd1 O6 77.8(3) 5_776 6_575 ?
O4 Gd1 O6 70.5(3) 6_575 6_575 ?
O4 Gd1 O6 109.5(3) 2_756 6_575 ?
O6 Gd1 O6 99.0(5) . 6_575 ?
O6 Gd1 O6 81.0(5) 5_776 6_575 ?
O4 Gd1 O6 77.8(3) . 2_756 ?
O4 Gd1 O6 102.2(3) 5_776 2_756 ?
O4 Gd1 O6 109.5(3) 6_575 2_756 ?
O4 Gd1 O6 70.5(3) 2_756 2_756 ?
O6 Gd1 O6 81.0(5) . 2_756 ?
O6 Gd1 O6 99.0(5) 5_776 2_756 ?
O6 Gd1 O6 180.0 6_575 2_756 ?
C1 N1 C12 121.2(5) . . ?
C1 N1 C3 112.7(5) . . ?
C12 N1 C3 125.7(5) . . ?
C1 N2 C4 121.4(4) . . ?
C1 N2 C2 112.8(5) . . ?
C4 N2 C2 125.3(5) . . ?
C5 N3 C7 111.9(5) . . ?
C5 N3 C4 123.2(5) . . ?
C7 N3 C4 123.2(5) . . ?
C5 N4 C8 123.3(5) . . ?
C5 N4 C6 111.9(5) . . ?
C8 N4 C6 122.8(5) . . ?
C9 N5 C11 112.1(5) . . ?
C9 N5 C8 122.8(5) . . ?
C11 N5 C8 123.6(5) . . ?
C9 N6 C10 112.4(5) . . ?
C9 N6 C12 123.1(5) . 2_656 ?
C10 N6 C12 123.2(5) . 2_656 ?
O4 O4 Gd1 69.0(2) 6_575 . ?
O7 O7 Gd1 69.4(2) 6_575 . ?
O1 C1 N2 125.6(5) . . ?
O1 C1 N1 125.1(5) . . ?
N2 C1 N1 109.3(4) . . ?
N2 C2 N2 113.1(6) . 6_575 ?
N2 C2 C13 111.5(4) . . ?
N2 C2 C13 111.5(4) 6_575 . ?
N2 C2 C3 102.2(4) . . ?
N2 C2 C3 102.2(4) 6_575 . ?
C13 C2 C3 115.9(6) . . ?
N1 C3 N1 114.1(6) . 6_575 ?
N1 C3 C14 111.2(4) . . ?
N1 C3 C14 111.2(4) 6_575 . ?
N1 C3 C2 102.8(4) . . ?
N1 C3 C2 102.8(4) 6_575 . ?
C14 C3 C2 114.3(7) . . ?
N2 C4 N3 113.6(5) . . ?
O2 C5 N3 125.3(5) . . ?
O2 C5 N4 125.4(5) . . ?
N3 C5 N4 109.2(5) . . ?
N4 C6 N4 113.2(6) 6_575 . ?
N4 C6 C7 102.9(4) 6_575 . ?
N4 C6 C7 102.9(4) . . ?
N3 C7 N3 113.5(6) . 6_575 ?
N3 C7 C6 103.6(4) . . ?
N3 C7 C6 103.6(4) 6_575 . ?
N4 C8 N5 112.9(4) . . ?
O3 C9 N6 126.1(6) . . ?
O3 C9 N5 125.2(6) . . ?
N6 C9 N5 108.7(5) . . ?
N6 C10 N6 114.4(6) 6_575 . ?
N6 C10 C11 103.2(4) 6_575 . ?
N6 C10 C11 103.2(4) . . ?
N5 C11 N5 114.1(6) . 6_575 ?
N5 C11 C10 103.4(4) . . ?
N5 C11 C10 103.4(4) 6_575 . ?
N1 C12 N6 114.6(5) . 2_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N2 C1 O1 -0.4(9) . . . . ?
C2 N2 C1 O1 -173.3(5) . . . . ?
C4 N2 C1 N1 177.4(5) . . . . ?
C2 N2 C1 N1 4.5(7) . . . . ?
C12 N1 C1 O1 0.0(9) . . . . ?
C3 N1 C1 O1 174.0(5) . . . . ?
C12 N1 C1 N2 -177.8(5) . . . . ?
C3 N1 C1 N2 -3.9(7) . . . . ?
C1 N2 C2 N2 -112.3(6) . . . 6_575 ?
C4 N2 C2 N2 75.2(9) . . . 6_575 ?
C1 N2 C2 C13 121.2(6) . . . . ?
C4 N2 C2 C13 -51.3(8) . . . . ?
C1 N2 C2 C3 -3.2(6) . . . . ?
C4 N2 C2 C3 -175.7(5) . . . . ?
C1 N1 C3 N1 112.3(6) . . . 6_575 ?
C12 N1 C3 N1 -74.1(8) . . . 6_575 ?
C1 N1 C3 C14 -121.0(6) . . . . ?
C12 N1 C3 C14 52.7(8) . . . . ?
C1 N1 C3 C2 1.7(6) . . . . ?
C12 N1 C3 C2 175.4(5) . . . . ?
N2 C2 C3 N1 0.8(6) . . . . ?
N2 C2 C3 N1 118.0(5) 6_575 . . . ?
C13 C2 C3 N1 -120.6(4) . . . . ?
N2 C2 C3 N1 -118.0(5) . . . 6_575 ?
N2 C2 C3 N1 -0.8(6) 6_575 . . 6_575 ?
C13 C2 C3 N1 120.6(4) . . . 6_575 ?
N2 C2 C3 C14 121.4(4) . . . . ?
N2 C2 C3 C14 -121.4(4) 6_575 . . . ?
C13 C2 C3 C14 0.000(2) . . . . ?
C1 N2 C4 N3 100.7(6) . . . . ?
C2 N2 C4 N3 -87.3(7) . . . . ?
C5 N3 C4 N2 -108.3(6) . . . . ?
C7 N3 C4 N2 88.1(7) . . . . ?
C7 N3 C5 O2 171.9(6) . . . . ?
C4 N3 C5 O2 6.6(10) . . . . ?
C7 N3 C5 N4 -6.3(7) . . . . ?
C4 N3 C5 N4 -171.6(5) . . . . ?
C8 N4 C5 O2 -7.4(10) . . . . ?
C6 N4 C5 O2 -171.6(6) . . . . ?
C8 N4 C5 N3 170.9(5) . . . . ?
C6 N4 C5 N3 6.7(7) . . . . ?
C5 N4 C6 N4 -114.6(6) . . . 6_575 ?
C8 N4 C6 N4 81.1(7) . . . 6_575 ?
C5 N4 C6 C7 -4.2(6) . . . . ?
C8 N4 C6 C7 -168.5(5) . . . . ?
C5 N3 C7 N3 115.2(6) . . . 6_575 ?
C4 N3 C7 N3 -79.5(8) . . . 6_575 ?
C5 N3 C7 C6 3.5(7) . . . . ?
C4 N3 C7 C6 168.8(5) . . . . ?
N4 C6 C7 N3 118.3(5) 6_575 . . . ?
N4 C6 C7 N3 0.4(6) . . . . ?
N4 C6 C7 N3 -0.4(6) 6_575 . . 6_575 ?
N4 C6 C7 N3 -118.3(5) . . . 6_575 ?
C5 N4 C8 N5 110.0(6) . . . . ?
C6 N4 C8 N5 -87.5(6) . . . . ?
C9 N5 C8 N4 -108.3(6) . . . . ?
C11 N5 C8 N4 87.0(6) . . . . ?
C10 N6 C9 O3 -173.6(6) . . . . ?
C12 N6 C9 O3 -6.6(10) 2_656 . . . ?
C10 N6 C9 N5 4.2(7) . . . . ?
C12 N6 C9 N5 171.3(5) 2_656 . . . ?
C11 N5 C9 O3 173.6(6) . . . . ?
C8 N5 C9 O3 7.3(9) . . . . ?
C11 N5 C9 N6 -4.3(7) . . . . ?
C8 N5 C9 N6 -170.6(5) . . . . ?
C9 N6 C10 N6 -113.9(6) . . . 6_575 ?
C12 N6 C10 N6 79.1(8) 2_656 . . 6_575 ?
C9 N6 C10 C11 -2.5(6) . . . . ?
C12 N6 C10 C11 -169.5(5) 2_656 . . . ?
C9 N5 C11 N5 114.2(6) . . . 6_575 ?
C8 N5 C11 N5 -79.6(8) . . . 6_575 ?
C9 N5 C11 C10 2.6(6) . . . . ?
C8 N5 C11 C10 168.8(5) . . . . ?
N6 C10 C11 N5 119.3(5) 6_575 . . . ?
N6 C10 C11 N5 -0.1(6) . . . . ?
N6 C10 C11 N5 0.1(6) 6_575 . . 6_575 ?
N6 C10 C11 N5 -119.3(5) . . . 6_575 ?
C1 N1 C12 N6 -101.2(6) . . . 2_656 ?
C3 N1 C12 N6 85.6(7) . . . 2_656 ?

_refine_diff_density_max         1.654
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.225



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

data_9pp
_database_code_depnum_ccdc_archive 'CCDC 1038177'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_vrf_PLAT306_9pp                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) O1w etc
RESPONSE: The majority of hydrogen atoms were not located in this study.
The addition of hydrogens to water molecules in structures such as this is 
a difficult problem. The model employed does not have hydrogen atoms on
the water molecules. To add them at arbitrary positions would be an 
extremely dubious procedure. 
;

_vrf_PLAT430_9pp                 
;
PROBLEM: Short Inter D...A Contact 
RESPONSE: This contact is suggestive of a hydrogen bond between water and
another molecule (often water). Hydrogen atoms were not identified in 
Fourier difference maps so were not added. 
;

_vrf_PLAT075_9pp                 
;
PROBLEM: Occupancy      2.000 greater than 1.0 for ......  
RESPONSE: This is a false alert. The atom involved is sited close to a
mirror plane but does not reside on it. The mirror plane generates
two orientations that are close together but independent. The
CIF checker generates a false alert because these atoms are close
together but not the same atom. 
;

_vrf_CHEMW01_9pp                 
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.
RESPONSE: This is a false alert. The hydrogen atom involved is sited 
close to a mirror plane but does not reside on it. The mirror plane
generates two orientations that are close together but independent. 
The CIF checker generates a false alert because these atoms are close
together but not the same atom. (It double counts the atoms needlessly)
;

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 -0.021 0.000 869 162 ' '
_platon_squeeze_details          ?


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H44 Cl3 N24 O20 Tb'
_chemical_formula_weight         1446.26

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.443(5)
_cell_length_b                   12.472(2)
_cell_length_c                   14.880(3)
_cell_angle_alpha                90
_cell_angle_beta                 115.094(7)
_cell_angle_gamma                90
_cell_volume                     3772.1(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9112
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_F_000             1456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.116
_shelx_estimated_absorpt_T_min   0.753
_shelx_estimated_absorpt_T_max   0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10163
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.932
_diffrn_reflns_theta_max         25.242
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3547
_reflns_number_gt                3498
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1059P)²+17.8902P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3547
_refine_ls_number_parameters     236
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1671
_refine_ls_wR_factor_gt          0.1665
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.4389(8) 1.0000 0.4999(11) 0.0795(12) Uiso 0.2157(16) 2 d S U P . .
Cl2 Cl 0.8178(3) 0.5316(4) 0.8942(4) 0.0795(12) Uiso 0.3839(8) 1 d . U P . .
Cl3 Cl 0.9812(4) 0.6956(7) 0.9819(6) 0.0795(12) Uiso 0.2583(8) 1 d . U P . .
Tb1 Tb 1.0000 1.0000 0.5000 0.0283(2) Uani 1 4 d S T P . .
N1 N 0.2748(2) 0.9018(3) 0.4169(3) 0.0340(9) Uani 1 1 d . . . . .
N2 N 0.3207(2) 0.9021(3) 0.5814(3) 0.0341(9) Uani 1 1 d . . . . .
N3 N 0.4235(2) 0.9028(3) 0.7305(3) 0.0352(9) Uani 1 1 d . . . . .
N4 N 0.5321(2) 0.9023(3) 0.8070(3) 0.0347(9) Uani 1 1 d . . . . .
N5 N 0.6398(2) 0.9025(3) 0.8081(3) 0.0357(9) Uani 1 1 d . . . . .
N6 N 0.7054(2) 0.9025(3) 0.7315(3) 0.0356(10) Uani 1 1 d . . . . .
O1 O 0.3370(2) 0.7574(3) 0.4995(3) 0.0458(10) Uani 1 1 d . . . . .
O2 O 0.4795(2) 0.7558(4) 0.7140(4) 0.0614(13) Uani 1 1 d . . . . .
O3 O 0.6387(3) 0.7570(4) 0.7130(4) 0.0599(12) Uani 1 1 d . . . . .
O4 O 0.9084(4) 0.9308(7) 0.3629(7) 0.059(2) Uani 0.5 1 d . . P A 1
O6 O 0.9534(4) 0.8539(7) 0.5510(7) 0.052(2) Uani 0.5 1 d . . P B 1
O5 O 0.9244(4) 0.8551(7) 0.4515(7) 0.054(2) Uani 0.5 1 d . . P A 2
O7 O 0.9901(5) 0.9324(6) 0.6424(7) 0.057(2) Uani 0.5 1 d . . P A 2
C1 C 0.3139(2) 0.8459(4) 0.4990(4) 0.0332(11) Uani 1 1 d . . . . .
C2 C 0.2813(3) 1.0000 0.5582(5) 0.0291(14) Uani 1 2 d S T P . .
C3 C 0.2485(3) 1.0000 0.4401(5) 0.0304(14) Uani 1 2 d S T P . .
C4 C 0.3577(3) 0.8594(4) 0.6802(4) 0.0381(12) Uani 1 1 d . . . . .
H4A H 0.3338 0.8740 0.7199 0.046 Uiso 1 1 calc R U . . .
H4B H 0.3608 0.7822 0.6756 0.046 Uiso 1 1 calc R U . . .
C5 C 0.4786(3) 0.8453(4) 0.7472(4) 0.0376(11) Uani 1 1 d . . . . .
C6 C 0.5138(4) 1.0000 0.8428(5) 0.0311(14) Uani 1 2 d S T P . .
H6 H 0.5293 1.0000 0.9151 0.037 Uiso 1 2 calc R U P . .
C7 C 0.4384(4) 1.0000 0.7885(5) 0.0322(15) Uani 1 2 d S T P . .
H7 H 0.4182 1.0000 0.8354 0.039 Uiso 1 2 calc R U P . .
C8 C 0.5977(3) 0.8590(4) 0.8505(4) 0.0362(11) Uani 1 1 d . . . . .
H8A H 0.5953 0.7818 0.8417 0.043 Uiso 1 1 calc R U . . .
H8B H 0.6173 0.8735 0.9212 0.043 Uiso 1 1 calc R U . . .
C9 C 0.6589(3) 0.8460(4) 0.7467(4) 0.0370(11) Uani 1 1 d . . . . .
C10 C 0.7233(3) 1.0000 0.7899(5) 0.0312(14) Uani 1 2 d S T P . .
H10 H 0.7698 1.0000 0.8369 0.037 Uiso 1 2 calc R U P . .
C11 C 0.6779(3) 1.0000 0.8433(5) 0.0307(14) Uani 1 2 d S T P . .
H11 H 0.7029 1.0000 0.9156 0.037 Uiso 1 2 calc R U P . .
C12 C 0.2572(3) 0.8591(4) 0.3189(4) 0.0375(11) Uani 1 1 d . . . . .
H12A H 0.2109 0.8730 0.2787 0.045 Uiso 1 1 calc R U . . .
H12B H 0.2632 0.7820 0.3239 0.045 Uiso 1 1 calc R U . . .
C13 C 0.2336(4) 1.0000 0.6064(6) 0.0436(18) Uani 1 2 d S T P . .
H13A H 0.2085 1.0652 0.5898 0.065 Uiso 0.5 1 calc R U P . .
H13B H 0.2044 0.9398 0.5826 0.065 Uiso 0.5 1 calc R U P . .
H13C H 0.2578 0.9950 0.6771 0.065 Uiso 1 2 calc R U P . .
C14 C 0.1734(4) 1.0000 0.3916(7) 0.0449(19) Uani 1 2 d S T P . .
H14A H 0.1576 1.0652 0.4081 0.067 Uiso 0.5 1 calc R U P . .
H14B H 0.1579 0.9950 0.3209 0.067 Uiso 1 2 calc R U P . .
H14C H 0.1576 0.9398 0.4153 0.067 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl2 Cl2 0.789(11) 6_565 ?
Cl3 Cl3 0.785(15) 2_757 ?
Tb1 O4 2.362(8) . ?
Tb1 O4 2.362(8) 5_776 ?
Tb1 O4 2.362(8) 6_575 ?
Tb1 O4 2.362(8) 2_756 ?
Tb1 O5 2.373(8) . ?
Tb1 O5 2.373(8) 5_776 ?
Tb1 O5 2.373(8) 6_575 ?
Tb1 O5 2.373(8) 2_756 ?
Tb1 O7 2.376(8) . ?
Tb1 O7 2.376(8) 6_575 ?
Tb1 O7 2.376(8) 2_756 ?
Tb1 O7 2.376(8) 5_776 ?
N1 C1 1.356(7) . ?
N1 C12 1.441(7) . ?
N1 C3 1.463(5) . ?
N2 C1 1.364(7) . ?
N2 C4 1.448(7) . ?
N2 C2 1.461(5) . ?
N3 C5 1.358(7) . ?
N3 C7 1.443(6) . ?
N3 C4 1.448(7) . ?
N4 C5 1.353(7) . ?
N4 C8 1.439(6) . ?
N4 C6 1.456(6) . ?
N5 C9 1.360(7) . ?
N5 C8 1.445(7) . ?
N5 C11 1.451(6) . ?
N6 C9 1.355(7) . ?
N6 C12 1.446(7) 2_656 ?
N6 C10 1.449(6) . ?
O1 C1 1.218(6) . ?
O2 C5 1.224(7) . ?
O3 C9 1.224(7) . ?
O4 O4 1.727(16) 6_575 ?
O7 O7 1.686(16) 6_575 ?
C2 N2 1.461(5) 6_575 ?
C2 C13 1.520(10) . ?
C2 C3 1.592(10) . ?
C3 N1 1.463(6) 6_575 ?
C3 C14 1.527(10) . ?
C6 N4 1.456(6) 6_575 ?
C6 C7 1.534(10) . ?
C7 N3 1.443(6) 6_575 ?
C10 N6 1.449(6) 6_575 ?
C10 C11 1.535(10) . ?
C11 N5 1.451(6) 6_575 ?
C12 N6 1.446(7) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O4 180.0 . 5_776 ?
O4 Tb1 O4 42.9(4) . 6_575 ?
O4 Tb1 O4 137.1(4) 5_776 6_575 ?
O4 Tb1 O4 137.1(4) . 2_756 ?
O4 Tb1 O4 42.9(4) 5_776 2_756 ?
O4 Tb1 O4 180.0 6_575 2_756 ?
O5 Tb1 O5 180.0 . 5_776 ?
O5 Tb1 O5 99.2(5) . 6_575 ?
O5 Tb1 O5 80.8(5) 5_776 6_575 ?
O5 Tb1 O5 80.8(5) . 2_756 ?
O5 Tb1 O5 99.2(5) 5_776 2_756 ?
O5 Tb1 O5 180.0 6_575 2_756 ?
O5 Tb1 O7 71.1(3) . . ?
O5 Tb1 O7 108.9(3) 5_776 . ?
O5 Tb1 O7 102.5(3) 6_575 . ?
O5 Tb1 O7 77.5(3) 2_756 . ?
O5 Tb1 O7 102.5(3) . 6_575 ?
O5 Tb1 O7 77.5(3) 5_776 6_575 ?
O5 Tb1 O7 71.1(3) 6_575 6_575 ?
O5 Tb1 O7 108.9(3) 2_756 6_575 ?
O7 Tb1 O7 41.5(4) . 6_575 ?
O5 Tb1 O7 77.5(3) . 2_756 ?
O5 Tb1 O7 102.5(3) 5_776 2_756 ?
O5 Tb1 O7 108.9(3) 6_575 2_756 ?
O5 Tb1 O7 71.1(3) 2_756 2_756 ?
O7 Tb1 O7 138.5(4) . 2_756 ?
O7 Tb1 O7 180.0 6_575 2_756 ?
O5 Tb1 O7 108.9(3) . 5_776 ?
O5 Tb1 O7 71.1(3) 5_776 5_776 ?
O5 Tb1 O7 77.5(3) 6_575 5_776 ?
O5 Tb1 O7 102.5(3) 2_756 5_776 ?
O7 Tb1 O7 180.0 . 5_776 ?
O7 Tb1 O7 138.5(4) 6_575 5_776 ?
O7 Tb1 O7 41.5(4) 2_756 5_776 ?
C1 N1 C12 121.1(4) . . ?
C1 N1 C3 112.9(5) . . ?
C12 N1 C3 125.7(5) . . ?
C1 N2 C4 121.4(4) . . ?
C1 N2 C2 113.0(5) . . ?
C4 N2 C2 125.2(5) . . ?
C5 N3 C7 111.8(5) . . ?
C5 N3 C4 123.1(4) . . ?
C7 N3 C4 123.4(5) . . ?
C5 N4 C8 123.4(4) . . ?
C5 N4 C6 111.8(5) . . ?
C8 N4 C6 122.9(5) . . ?
C9 N5 C8 123.3(4) . . ?
C9 N5 C11 111.8(5) . . ?
C8 N5 C11 123.5(5) . . ?
C9 N6 C12 123.3(4) . 2_656 ?
C9 N6 C10 111.9(5) . . ?
C12 N6 C10 123.4(5) 2_656 . ?
O4 O4 Tb1 68.6(2) 6_575 . ?
O7 O7 Tb1 69.2(2) 6_575 . ?
O1 C1 N1 125.6(5) . . ?
O1 C1 N2 125.1(5) . . ?
N1 C1 N2 109.2(4) . . ?
N2 C2 N2 113.5(6) . 6_575 ?
N2 C2 C13 111.4(4) . . ?
N2 C2 C13 111.4(4) 6_575 . ?
N2 C2 C3 102.2(4) . . ?
N2 C2 C3 102.2(4) 6_575 . ?
C13 C2 C3 115.6(6) . . ?
N1 C3 N1 113.7(6) . 6_575 ?
N1 C3 C14 111.3(4) . . ?
N1 C3 C14 111.3(4) 6_575 . ?
N1 C3 C2 102.6(4) . . ?
N1 C3 C2 102.6(4) 6_575 . ?
C14 C3 C2 115.0(6) . . ?
N3 C4 N2 114.1(4) . . ?
O2 C5 N4 125.7(5) . . ?
O2 C5 N3 125.2(5) . . ?
N4 C5 N3 109.1(5) . . ?
N4 C6 N4 113.6(6) . 6_575 ?
N4 C6 C7 103.1(4) . . ?
N4 C6 C7 103.1(4) 6_575 . ?
N3 C7 N3 114.3(6) 6_575 . ?
N3 C7 C6 103.8(4) 6_575 . ?
N3 C7 C6 103.8(4) . . ?
N4 C8 N5 113.4(4) . . ?
O3 C9 N6 125.6(5) . . ?
O3 C9 N5 125.3(5) . . ?
N6 C9 N5 109.1(5) . . ?
N6 C10 N6 114.1(6) . 6_575 ?
N6 C10 C11 103.6(4) . . ?
N6 C10 C11 103.6(4) 6_575 . ?
N5 C11 N5 113.8(6) 6_575 . ?
N5 C11 C10 103.4(4) 6_575 . ?
N5 C11 C10 103.4(4) . . ?
N1 C12 N6 114.6(4) . 2_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 O1 -0.7(8) . . . . ?
C3 N1 C1 O1 173.3(5) . . . . ?
C12 N1 C1 N2 -177.7(4) . . . . ?
C3 N1 C1 N2 -3.7(6) . . . . ?
C4 N2 C1 O1 0.3(8) . . . . ?
C2 N2 C1 O1 -173.1(5) . . . . ?
C4 N2 C1 N1 177.3(4) . . . . ?
C2 N2 C1 N1 4.0(6) . . . . ?
C1 N2 C2 N2 -111.7(5) . . . 6_575 ?
C4 N2 C2 N2 75.2(7) . . . 6_575 ?
C1 N2 C2 C13 121.5(6) . . . . ?
C4 N2 C2 C13 -51.6(7) . . . . ?
C1 N2 C2 C3 -2.5(6) . . . . ?
C4 N2 C2 C3 -175.6(5) . . . . ?
C1 N1 C3 N1 112.0(5) . . . 6_575 ?
C12 N1 C3 N1 -74.4(7) . . . 6_575 ?
C1 N1 C3 C14 -121.4(6) . . . . ?
C12 N1 C3 C14 52.2(7) . . . . ?
C1 N1 C3 C2 2.1(6) . . . . ?
C12 N1 C3 C2 175.7(5) . . . . ?
N2 C2 C3 N1 0.3(5) . . . . ?
N2 C2 C3 N1 117.9(4) 6_575 . . . ?
C13 C2 C3 N1 -120.9(3) . . . . ?
N2 C2 C3 N1 -117.9(4) . . . 6_575 ?
N2 C2 C3 N1 -0.3(5) 6_575 . . 6_575 ?
C13 C2 C3 N1 120.9(3) . . . 6_575 ?
N2 C2 C3 C14 121.2(3) . . . . ?
N2 C2 C3 C14 -121.2(3) 6_575 . . . ?
C13 C2 C3 C14 0.000(2) . . . . ?
C5 N3 C4 N2 -108.5(6) . . . . ?
C7 N3 C4 N2 87.1(6) . . . . ?
C1 N2 C4 N3 100.8(6) . . . . ?
C2 N2 C4 N3 -86.6(6) . . . . ?
C8 N4 C5 O2 -8.2(9) . . . . ?
C6 N4 C5 O2 -173.1(6) . . . . ?
C8 N4 C5 N3 171.0(5) . . . . ?
C6 N4 C5 N3 6.2(6) . . . . ?
C7 N3 C5 O2 173.6(6) . . . . ?
C4 N3 C5 O2 7.6(9) . . . . ?
C7 N3 C5 N4 -5.7(6) . . . . ?
C4 N3 C5 N4 -171.7(5) . . . . ?
C5 N4 C6 N4 -114.9(6) . . . 6_575 ?
C8 N4 C6 N4 80.1(7) . . . 6_575 ?
C5 N4 C6 C7 -4.2(6) . . . . ?
C8 N4 C6 C7 -169.1(5) . . . . ?
C5 N3 C7 N3 115.3(6) . . . 6_575 ?
C4 N3 C7 N3 -78.7(7) . . . 6_575 ?
C5 N3 C7 C6 2.9(6) . . . . ?
C4 N3 C7 C6 168.9(5) . . . . ?
N4 C6 C7 N3 -119.1(4) . . . 6_575 ?
N4 C6 C7 N3 -0.7(6) 6_575 . . 6_575 ?
N4 C6 C7 N3 0.7(6) . . . . ?
N4 C6 C7 N3 119.1(4) 6_575 . . . ?
C5 N4 C8 N5 109.2(6) . . . . ?
C6 N4 C8 N5 -87.6(6) . . . . ?
C9 N5 C8 N4 -107.4(6) . . . . ?
C11 N5 C8 N4 87.3(6) . . . . ?
C12 N6 C9 O3 -7.0(9) 2_656 . . . ?
C10 N6 C9 O3 -174.0(6) . . . . ?
C12 N6 C9 N5 171.1(5) 2_656 . . . ?
C10 N6 C9 N5 4.1(6) . . . . ?
C8 N5 C9 O3 7.0(9) . . . . ?
C11 N5 C9 O3 173.8(6) . . . . ?
C8 N5 C9 N6 -171.1(5) . . . . ?
C11 N5 C9 N6 -4.3(6) . . . . ?
C9 N6 C10 N6 -114.2(6) . . . 6_575 ?
C12 N6 C10 N6 78.8(7) 2_656 . . 6_575 ?
C9 N6 C10 C11 -2.3(6) . . . . ?
C12 N6 C10 C11 -169.3(5) 2_656 . . . ?
C9 N5 C11 N5 114.2(5) . . . 6_575 ?
C8 N5 C11 N5 -79.0(7) . . . 6_575 ?
C9 N5 C11 C10 2.7(6) . . . . ?
C8 N5 C11 C10 169.5(5) . . . . ?
N6 C10 C11 N5 -119.2(4) . . . 6_575 ?
N6 C10 C11 N5 0.2(5) 6_575 . . 6_575 ?
N6 C10 C11 N5 -0.2(5) . . . . ?
N6 C10 C11 N5 119.2(4) 6_575 . . . ?
C1 N1 C12 N6 -101.0(6) . . . 2_656 ?
C3 N1 C12 N6 85.8(6) . . . 2_656 ?

_refine_diff_density_max         2.000
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.152



