# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_Dy
_database_code_depnum_ccdc_archive 'CCDC 1055503'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H113 Dy N24 O52'
_chemical_formula_weight         1949.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   21.655(5)
_cell_length_b                   12.281(3)
_cell_length_c                   16.381(7)
_cell_angle_alpha                90
_cell_angle_beta                 120.371(6)
_cell_angle_gamma                90
_cell_volume                     3759(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_F_000             2030
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.124
_shelx_estimated_absorpt_T_min   0.798
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.854
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15769
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.441
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             3493
_reflns_number_gt                3331
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.001 -0.033 0.000 1141 442 ' '
2 0.500 0.000 0.500 116 38 ' '
3 0.000 0.500 0.500 116 38 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1705P)²+36.1612P] 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         3493
_refine_ls_number_parameters     246
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0905
_refine_ls_wR_factor_ref         0.2489
_refine_ls_wR_factor_gt          0.2459
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      4.472
_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 0.4183(9) 0.3499(11) 0.4594(15) 0.083(5) Uani 0.5 1 d . . P . .
O2W O 0.3890(10) 0.4286(15) 0.3807(18) 0.109(7) Uani 0.5 1 d . . P . .
O3W O 0.4619(13) 0.3612(16) 0.5574(15) 0.099(6) Uani 0.5 1 d . . P . .
O4W O 0.499(2) 0.4302(14) 0.629(2) 0.177(16) Uani 0.5 1 d . . P . .
Dy1 Dy 0.4952(5) 0.5000 0.5052(7) 0.0303(9) Uani 0.5 2 d S T P . .
C1 C 0.6969(7) 0.1554(10) 0.5251(11) 0.083(4) Uani 1 1 d . . . . .
C2 C 0.7711(7) 0.0000 0.5915(7) 0.069(4) Uani 1 2 d DS TU P . .
C3 C 0.7414(5) 0.0000 0.4890(7) 0.055(3) Uani 1 2 d DS TU P . .
C4 C 0.6548(7) 0.1386(10) 0.3575(9) 0.076(3) Uani 1 1 d . . . . .
H4A H 0.6844 0.1186 0.3301 0.091 Uiso 1 1 calc R U . . .
H4B H 0.6536 0.2183 0.3595 0.091 Uiso 1 1 calc R U . . .
C5 C 0.5228(8) 0.1550(10) 0.2743(10) 0.081(3) Uani 1 1 d . . . . .
C6 C 0.5684(10) 0.0000 0.2424(12) 0.066(4) Uani 1 2 d S T P . .
C7 C 0.4888(11) 0.0000 0.1830(10) 0.070(4) Uani 1 2 d S T P . .
C8 C 0.3934(9) 0.1413(12) 0.1650(11) 0.090(4) Uani 1 1 d . . . . .
H8A H 0.3966 0.2204 0.1739 0.108 Uiso 1 1 calc R U . . .
H8B H 0.3705 0.1274 0.0969 0.108 Uiso 1 1 calc R U . . .
C9 C 0.3287(7) 0.1530(10) 0.2504(8) 0.071(3) Uani 1 1 d . . . . .
C10 C 0.3081(9) 0.0000 0.1564(11) 0.069(4) Uani 1 2 d S T P . .
C11 C 0.2566(8) 0.0000 0.1980(11) 0.075(5) Uani 1 2 d DS T P . .
C12 C 0.2398(8) 0.1399(12) 0.3013(10) 0.088(4) Uani 1 1 d . . . . .
H12A H 0.1889 0.1239 0.2593 0.105 Uiso 1 1 calc R U . . .
H12B H 0.2451 0.2193 0.3059 0.105 Uiso 1 1 calc R U . . .
C13 C 0.7989(6) 0.0000 0.4602(7) 0.048 Uani 1 2 d DS TU P . .
H13A H 0.7759 0.0000 0.3918 0.071 Uiso 1 2 calc R U P . .
H13B H 0.8285 0.0645 0.4854 0.071 Uiso 0.5 1 calc R U P . .
H13C H 0.8285 -0.0645 0.4854 0.071 Uiso 0.5 1 calc R U P . .
C14 C 0.4590(13) 0.0000 0.0754(13) 0.110(8) Uani 1 2 d S T P . .
H14A H 0.4749 0.0651 0.0579 0.165 Uiso 0.5 1 calc R U P . .
H14B H 0.4763 -0.0638 0.0582 0.165 Uiso 0.5 1 calc R U P . .
H14C H 0.4071 -0.0013 0.0425 0.165 Uiso 1 2 calc R U P . .
C15 C 0.2771(16) 0.0000 0.0609(16) 0.148(13) Uani 1 2 d S T P . .
H15A H 0.2505 0.0671 0.0356 0.223 Uiso 0.5 1 calc R U P . .
H15B H 0.3138 -0.0057 0.0437 0.223 Uiso 0.5 1 calc R U P . .
H15C H 0.2447 -0.0615 0.0349 0.223 Uiso 0.5 1 calc R U P . .
N1 N 0.7389(5) 0.0979(9) 0.6071(8) 0.075(3) Uani 1 1 d . . . . .
N2 N 0.6881(6) 0.0999(8) 0.4498(8) 0.073(2) Uani 1 1 d . . . . .
N3 N 0.5831(6) 0.1001(8) 0.2953(8) 0.078(3) Uani 1 1 d . . . . .
N4 N 0.4651(6) 0.0979(8) 0.2101(7) 0.075(3) Uani 1 1 d . . . . .
N5 N 0.3486(5) 0.0996(8) 0.1972(8) 0.074(2) Uani 1 1 d . . . . .
N6 N 0.2787(6) 0.0983(8) 0.2585(7) 0.075(3) Uani 1 1 d . . . . .
O1 O 0.6709(7) 0.2472(6) 0.5170(9) 0.105(3) Uani 1 1 d . . . . .
O2 O 0.5200(8) 0.2450(8) 0.3031(11) 0.126(4) Uani 1 1 d . . . . .
O3 O 0.3526(6) 0.2426(7) 0.2900(7) 0.093(3) Uani 1 1 d . . . . .
O4 O 0.8457(8) 0.0000 0.631(2) 0.225(15) Uani 1 2 d DS T P . .
H4 H 0.8579 -0.0550 0.6131 0.337 Uiso 0.5 1 calc R U P . .
O5 O 0.6047(12) 0.0000 0.1911(15) 0.148(8) Uani 1 2 d S T P . .
H5 H 0.5960 -0.0576 0.1606 0.222 Uiso 0.5 1 calc R U P . .
O6 O 0.1821(8) 0.0000 0.1314(19) 0.218(15) Uani 1 2 d DS T P . .
H6 H 0.1595 0.0000 0.1600 0.327 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
O1W O3W 1.40(3) . ?
O1W O2W 1.47(3) . ?
O1W Dy1 2.339(13) . ?
O1W Dy1 2.478(13) 5_666 ?
O2W O2W 1.75(4) 6_565 ?
O2W Dy1 2.34(2) . ?
O2W Dy1 2.41(2) 5_666 ?
O3W O4W 1.33(3) . ?
O3W Dy1 2.186(16) . ?
O3W Dy1 2.403(16) 5_666 ?
O4W O4W 1.71(3) 6_565 ?
O4W Dy1 2.16(2) . ?
O4W Dy1 2.41(2) 5_666 ?
Dy1 Dy1 0.326(10) 5_666 ?
Dy1 O4W 2.16(2) 6_565 ?
Dy1 O3W 2.187(16) 6_565 ?
Dy1 O2W 2.34(2) 6_565 ?
Dy1 O1W 2.339(13) 6_565 ?
Dy1 O2W 2.41(2) 5_666 ?
Dy1 O2W 2.41(2) 2_656 ?
Dy1 O3W 2.403(16) 2_656 ?
C1 O1 1.238(16) . ?
C1 N2 1.336(17) . ?
C1 N1 1.377(19) . ?
C2 C3 1.462(9) . ?
C2 N1 1.476(12) 6 ?
C2 N1 1.476(12) . ?
C2 O4 1.404(10) . ?
C3 C13 1.539(2) . ?
C3 N2 1.581(12) . ?
C3 N2 1.581(12) 6 ?
C4 N2 1.389(17) . ?
C4 N3 1.441(16) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.215(16) . ?
C5 N4 1.353(17) . ?
C5 N3 1.351(18) . ?
C6 O5 1.41(2) . ?
C6 N3 1.443(12) 6 ?
C6 N3 1.443(13) . ?
C6 C7 1.49(3) . ?
C7 N4 1.462(14) 6 ?
C7 N4 1.462(14) . ?
C7 C14 1.54(2) . ?
C8 N5 1.414(16) . ?
C8 N4 1.441(19) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.249(15) . ?
C9 N5 1.325(16) . ?
C9 N6 1.338(17) . ?
C10 C15 1.35(3) . ?
C10 N5 1.456(13) 6 ?
C10 N5 1.456(13) . ?
C10 C11 1.57(3) . ?
C11 N6 1.480(13) 6 ?
C11 N6 1.480(13) . ?
C11 O6 1.419(10) . ?
C12 N6 1.434(18) . ?
C12 N1 1.425(18) 2_656 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 C12 1.425(18) 2_656 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

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
O3W O1W O2W 132.9(15) . . ?
O3W O1W Dy1 66.1(8) . . ?
O2W O1W Dy1 71.7(10) . . ?
O3W O1W Dy1 70.4(8) . 5_666 ?
O2W O1W Dy1 69.9(10) . 5_666 ?
Dy1 O1W Dy1 7.0(2) . 5_666 ?
O1W O2W O2W 131.0(11) . 6_565 ?
O1W O2W Dy1 71.6(10) . . ?
O2W O2W Dy1 68.0(4) 6_565 . ?
O1W O2W Dy1 75.0(10) . 5_666 ?
O2W O2W Dy1 68.7(4) 6_565 5_666 ?
Dy1 O2W Dy1 7.7(3) . 5_666 ?
O4W O3W O1W 146(2) . . ?
O4W O3W Dy1 70.9(11) . . ?
O1W O3W Dy1 78.1(10) . . ?
O4W O3W Dy1 74.2(10) . 5_666 ?
O1W O3W Dy1 76.3(9) . 5_666 ?
Dy1 O3W Dy1 6.1(2) . 5_666 ?
O3W O4W O4W 129.4(16) . 6_565 ?
O3W O4W Dy1 73.4(13) . . ?
O4W O4W Dy1 66.6(5) 6_565 . ?
O3W O4W Dy1 73.6(12) . 5_666 ?
O4W O4W Dy1 69.2(4) 6_565 5_666 ?
Dy1 O4W Dy1 5.1(4) . 5_666 ?
Dy1 Dy1 O4W 139(3) 5_666 . ?
Dy1 Dy1 O4W 139(3) 5_666 6_565 ?
O4W Dy1 O4W 46.8(9) . 6_565 ?
Dy1 Dy1 O3W 128.5(7) 5_666 . ?
O4W Dy1 O3W 35.8(9) . . ?
O4W Dy1 O3W 78.9(8) 6_565 . ?
Dy1 Dy1 O3W 128.5(7) 5_666 6_565 ?
O4W Dy1 O3W 78.9(8) . 6_565 ?
O4W Dy1 O3W 35.8(9) 6_565 6_565 ?
O3W Dy1 O3W 102.4(11) . 6_565 ?
Dy1 Dy1 O2W 99(3) 5_666 . ?
O4W Dy1 O2W 103.0(12) . . ?
O4W Dy1 O2W 121.5(13) 6_565 . ?
O3W Dy1 O2W 71.1(9) . . ?
O3W Dy1 O2W 105.0(9) 6_565 . ?
Dy1 Dy1 O2W 99(3) 5_666 6_565 ?
O4W Dy1 O2W 121.5(13) . 6_565 ?
O4W Dy1 O2W 103.0(12) 6_565 6_565 ?
O3W Dy1 O2W 105.0(9) . 6_565 ?
O3W Dy1 O2W 71.1(9) 6_565 6_565 ?
O2W Dy1 O2W 44.0(9) . 6_565 ?
Dy1 Dy1 O1W 112(2) 5_666 6_565 ?
O4W Dy1 O1W 107.4(9) . 6_565 ?
O4W Dy1 O1W 70.8(10) 6_565 6_565 ?
O3W Dy1 O1W 114.7(8) . 6_565 ?
O3W Dy1 O1W 35.8(7) 6_565 6_565 ?
O2W Dy1 O1W 77.8(7) . 6_565 ?
O2W Dy1 O1W 36.7(7) 6_565 6_565 ?
Dy1 Dy1 O1W 112(2) 5_666 . ?
O4W Dy1 O1W 70.8(10) . . ?
O4W Dy1 O1W 107.4(9) 6_565 . ?
O3W Dy1 O1W 35.8(7) . . ?
O3W Dy1 O1W 114.7(8) 6_565 . ?
O2W Dy1 O1W 36.7(7) . . ?
O2W Dy1 O1W 77.8(7) 6_565 . ?
O1W Dy1 O1W 104.0(9) 6_565 . ?
Dy1 Dy1 O2W 74(3) 5_666 5_666 ?
O4W Dy1 O2W 83.3(12) . 5_666 ?
O4W Dy1 O2W 66.1(12) 6_565 5_666 ?
O3W Dy1 O2W 113.5(9) . 5_666 ?
O3W Dy1 O2W 80.3(9) 6_565 5_666 ?
O2W Dy1 O2W 172.3(3) . 5_666 ?
O2W Dy1 O2W 135.9(8) 6_565 5_666 ?
O1W Dy1 O2W 104.7(6) 6_565 5_666 ?
O1W Dy1 O2W 145.9(7) . 5_666 ?
Dy1 Dy1 O2W 74(3) 5_666 2_656 ?
O4W Dy1 O2W 66.1(12) . 2_656 ?
O4W Dy1 O2W 83.3(12) 6_565 2_656 ?
O3W Dy1 O2W 80.3(9) . 2_656 ?
O3W Dy1 O2W 113.5(9) 6_565 2_656 ?
O2W Dy1 O2W 135.9(8) . 2_656 ?
O2W Dy1 O2W 172.3(3) 6_565 2_656 ?
O1W Dy1 O2W 145.9(7) 6_565 2_656 ?
O1W Dy1 O2W 104.7(6) . 2_656 ?
O2W Dy1 O2W 42.7(8) 5_666 2_656 ?
Dy1 Dy1 O3W 45.4(6) 5_666 2_656 ?
O4W Dy1 O3W 106.0(8) . 2_656 ?
O4W Dy1 O3W 147.1(10) 6_565 2_656 ?
O3W Dy1 O3W 83.6(10) . 2_656 ?
O3W Dy1 O3W 173.9(2) 6_565 2_656 ?
O2W Dy1 O3W 77.5(8) . 2_656 ?
O2W Dy1 O3W 108.4(9) 6_565 2_656 ?
O1W Dy1 O3W 142.0(8) 6_565 2_656 ?
O1W Dy1 O3W 70.7(7) . 2_656 ?
O2W Dy1 O3W 96.6(8) 5_666 2_656 ?
O2W Dy1 O3W 66.3(8) 2_656 2_656 ?
O1 C1 N2 121.5(15) . . ?
O1 C1 N1 127.8(14) . . ?
N2 C1 N1 110.7(12) . . ?
C3 C2 N1 103.1(7) . 6 ?
C3 C2 N1 103.1(7) . . ?
N1 C2 N1 109.0(10) 6 . ?
C3 C2 O4 105.4(14) . . ?
N1 C2 O4 117.0(8) 6 . ?
N1 C2 O4 117.0(8) . . ?
C2 C3 C13 113.4(6) . . ?
C2 C3 N2 105.9(6) . . ?
C13 C3 N2 114.4(6) . . ?
C2 C3 N2 105.9(6) . 6 ?
C13 C3 N2 114.4(6) . 6 ?
N2 C3 N2 101.8(9) . 6 ?
N2 C4 N3 116.0(10) . . ?
N2 C4 H4A 108.3 . . ?
N3 C4 H4A 108.3 . . ?
N2 C4 H4B 108.3 . . ?
N3 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
O2 C5 N4 124.4(15) . . ?
O2 C5 N3 125.9(15) . . ?
N4 C5 N3 109.5(11) . . ?
O5 C6 N3 109.7(9) . 6 ?
O5 C6 N3 109.7(9) . . ?
N3 C6 N3 116.8(13) 6 . ?
O5 C6 C7 114.8(15) . . ?
N3 C6 C7 102.9(9) 6 . ?
N3 C6 C7 102.9(9) . . ?
N4 C7 N4 110.7(13) 6 . ?
N4 C7 C6 105.6(10) 6 . ?
N4 C7 C6 105.6(10) . . ?
N4 C7 C14 109.9(10) 6 . ?
N4 C7 C14 109.9(10) . . ?
C6 C7 C14 115.0(15) . . ?
N5 C8 N4 116.0(12) . . ?
N5 C8 H8A 108.3 . . ?
N4 C8 H8A 108.3 . . ?
N5 C8 H8B 108.3 . . ?
N4 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
O3 C9 N5 126.2(13) . . ?
O3 C9 N6 122.3(12) . . ?
N5 C9 N6 111.4(11) . . ?
C15 C10 N5 111.3(10) . 6 ?
C15 C10 N5 111.3(10) . . ?
N5 C10 N5 114.4(14) 6 . ?
C15 C10 C11 116.9(18) . . ?
N5 C10 C11 101.2(9) 6 . ?
N5 C10 C11 101.2(9) . . ?
N6 C11 N6 109.3(12) 6 . ?
N6 C11 O6 111.8(11) 6 . ?
N6 C11 O6 111.8(11) . . ?
N6 C11 C10 103.3(9) 6 . ?
N6 C11 C10 103.3(9) . . ?
O6 C11 C10 116.6(19) . . ?
N6 C12 N1 115.3(11) . 2_656 ?
N6 C12 H12A 108.4 . . ?
N1 C12 H12A 108.4 2_656 . ?
N6 C12 H12B 108.4 . . ?
N1 C12 H12B 108.4 2_656 . ?
H12A C12 H12B 107.5 . . ?
C3 C13 H13A 109.5 . . ?
C3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C12 123.0(11) . 2_656 ?
C1 N1 C2 112.7(10) . . ?
C12 N1 C2 123.2(11) 2_656 . ?
C1 N2 C4 125.7(11) . . ?
C1 N2 C3 106.7(11) . . ?
C4 N2 C3 125.3(9) . . ?
C5 N3 C4 125.1(10) . . ?
C5 N3 C6 112.4(12) . . ?
C4 N3 C6 122.4(11) . . ?
C5 N4 C8 122.6(11) . . ?
C5 N4 C7 109.5(12) . . ?
C8 N4 C7 126.9(13) . . ?
C9 N5 C8 125.4(11) . . ?
C9 N5 C10 113.4(12) . . ?
C8 N5 C10 120.0(12) . . ?
C9 N6 C12 125.1(11) . . ?
C9 N6 C11 110.3(12) . . ?
C12 N6 C11 123.2(12) . . ?
C2 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C11 O6 H6 109.5 . . ?

_refine_diff_density_max         4.413
_refine_diff_density_min         -5.456
_refine_diff_density_rms         0.195

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Er
_database_code_depnum_ccdc_archive 'CCDC 1055504'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H111 Er N24 O51'
_chemical_formula_weight         1935.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.6886(18)
_cell_length_b                   12.2264(10)
_cell_length_c                   16.420(2)
_cell_angle_alpha                90
_cell_angle_beta                 119.896(2)
_cell_angle_gamma                90
_cell_volume                     3774.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             2014
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    1.239
_shelx_estimated_absorpt_T_min   0.723
_shelx_estimated_absorpt_T_max   0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_T_max  0.771
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15808
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.430
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             3550
_reflns_number_gt                3283
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.471 -0.033 0.000 1124 438 ' '
2 1.000 0.000 0.500 116 32 ' '
3 0.500 0.500 0.500 116 32 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1035P)²+15.3689P] 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         3550
_refine_ls_number_parameters     224
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0689
_refine_ls_wR_factor_ref         0.1848
_refine_ls_wR_factor_gt          0.1809
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.015
_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 -0.0784(3) -0.3490(5) 0.4639(6) 0.088(2) Uani 0.5 1 d . . P . .
O2W O -0.0126(5) -0.4297(6) 0.3619(5) 0.139(3) Uani 0.5 1 d . . P . .
O3W O 0.0339(4) -0.6444(6) 0.4406(5) 0.128(2) Uani 0.5 1 d . . P . .
O4W O -0.1079(5) -0.4301(6) 0.3989(13) 0.236(9) Uani 0.5 1 d . . P . .
Er1 Er 0.0000 -0.5000 0.5000 0.04187(8) Uani 1 4 d S T P . .
C1 C 0.0222(2) -0.1565(4) 0.2748(3) 0.0703(13) Uani 1 1 d . . . . .
C2 C -0.0166(3) 0.0000 0.1784(3) 0.0648(16) Uani 1 2 d DS T P . .
C3 C 0.0669(3) 0.0000 0.2422(4) 0.0639(15) Uani 1 2 d S T P . .
C4 C 0.1524(2) -0.1412(4) 0.3544(3) 0.0742(13) Uani 1 1 d . . . . .
H4A H 0.1497 -0.2210 0.3571 0.089 Uiso 1 1 calc R U . . .
H4B H 0.1814 -0.1239 0.3256 0.089 Uiso 1 1 calc R U . . .
C5 C 0.1966(2) -0.1566(4) 0.5251(3) 0.070 Uani 1 1 d . . . . .
C6 C 0.23620(6) 0.0000 0.48511(10) 0.052 Uani 1 2 d DS T P . .
C7 C 0.2677(2) 0.0000 0.5878(5) 0.072 Uani 1 2 d DS T P . .
C8 C 0.2585(2) -0.1424(4) 0.6956(3) 0.076 Uani 1 1 d . . . . .
H8A H 0.2514 -0.2218 0.6902 0.092 Uiso 1 1 calc R U . . .
H8B H 0.3095 -0.1291 0.7367 0.092 Uiso 1 1 calc R U . . .
C9 C 0.1704(2) -0.1554(3) 0.7451(3) 0.0621(13) Uani 1 1 d . . . . .
C10 C 0.2435(3) 0.0000 0.7984(4) 0.066(2) Uani 1 2 d DS T P . .
C11 C 0.1935(3) 0.0000 0.8399(4) 0.0631(19) Uani 1 2 d S T P . .
C12 C 0.1056(3) -0.1445(4) 0.8338(3) 0.0789(15) Uani 1 1 d . . . . .
H12A H 0.1020 -0.2237 0.8236 0.095 Uiso 1 1 calc R U . . .
H12B H 0.1282 -0.1317 0.9016 0.095 Uiso 1 1 calc R U . . .
C13 C 0.0995(4) 0.0000 0.1846(6) 0.106(3) Uani 1 2 d S T P . .
H13A H 0.0884 -0.0679 0.1495 0.159 Uiso 0.5 1 calc R U P . .
H13B H 0.0815 0.0611 0.1413 0.159 Uiso 0.5 1 calc R U P . .
H13C H 0.1507 0.0068 0.2242 0.159 Uiso 0.5 1 calc R U P . .
C14 C 0.28309(6) 0.0000 0.44663(10) 0.052 Uani 1 2 d DS TU P . .
H14A H 0.2552 0.0000 0.3786 0.077 Uiso 0.5 1 calc R U P . .
H14B H 0.3129 0.0648 0.4677 0.077 Uiso 0.5 1 calc R U P . .
H14C H 0.3129 -0.0648 0.4677 0.077 Uiso 0.5 1 calc R U P . .
C15 C 0.2279(7) 0.0000 0.9388(7) 0.155(6) Uani 1 2 d S T P . .
H15A H 0.2552 0.0668 0.9628 0.232 Uiso 0.5 1 calc R U P . .
H15B H 0.1926 -0.0042 0.9586 0.232 Uiso 0.5 1 calc R U P . .
H15C H 0.2594 -0.0626 0.9631 0.232 Uiso 0.5 1 calc R U P . .
N1 N -0.03545(18) -0.0991(3) 0.2109(2) 0.0672(10) Uani 1 1 d . . . . .
N2 N 0.08200(17) -0.0991(3) 0.2954(2) 0.0632(10) Uani 1 1 d . . . . .
N3 N 0.18709(17) -0.0993(3) 0.4479(2) 0.0667(10) Uani 1 1 d . . . . .
N4 N 0.23814(18) -0.0997(3) 0.6052(2) 0.0688(11) Uani 1 1 d . . . . .
N5 N 0.22173(18) -0.0991(3) 0.7397(2) 0.0643(11) Uani 1 1 d . . . . .
N6 N 0.15136(19) -0.0993(3) 0.8001(3) 0.0661(11) Uani 1 1 d . . . . .
O1 O 0.0204(2) -0.2455(3) 0.3057(3) 0.1172(15) Uani 1 1 d . . . . .
O2 O 0.1715(2) -0.2489(3) 0.5179(3) 0.0952(12) Uani 1 1 d . . . . .
O3 O 0.14699(19) -0.2441(3) 0.7085(2) 0.0860(12) Uani 1 1 d . . . . .
O4 O -0.0416(5) 0.0000 0.0794(3) 0.186(5) Uani 1 2 d DS T P . .
H4 H -0.0292 -0.0575 0.0648 0.278 Uiso 0.5 1 calc R U P . .
O5 O 0.3440(3) 0.0000 0.6344(7) 0.215(6) Uani 1 2 d DS T P . .
H5 H 0.3577 0.0527 0.6157 0.323 Uiso 0.5 1 calc R U P . .
O6 O 0.3167(3) 0.0000 0.8709(7) 0.200(6) Uani 1 2 d DS T P . .
H6 H 0.3424 -0.0034 0.8468 0.300 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
O1W O4W 1.361(14) . ?
O1W O3W 1.374(10) 5_546 ?
O1W Er1 2.376(6) . ?
O2W O3W 1.486(10) 6_545 ?
O2W O2W 1.719(15) 6_545 ?
O2W Er1 2.310(8) . ?
O3W O1W 1.374(10) 5_546 ?
O3W O2W 1.486(10) 6_545 ?
O3W Er1 2.307(8) . ?
O4W O4W 1.708(15) 6_545 ?
O4W Er1 2.256(8) . ?
Er1 O4W 2.256(8) 6_545 ?
Er1 O4W 2.256(8) 2_556 ?
Er1 O4W 2.256(8) 5_546 ?
Er1 O3W 2.307(8) 5_546 ?
Er1 O3W 2.307(8) 6_545 ?
Er1 O3W 2.307(8) 2_556 ?
Er1 O2W 2.310(8) 6_545 ?
Er1 O2W 2.310(8) 2_556 ?
Er1 O2W 2.310(8) 5_546 ?
C1 O1 1.210(6) . ?
C1 N1 1.360(5) . ?
C1 N2 1.360(6) . ?
C2 N1 1.461(5) 6 ?
C2 N1 1.461(5) . ?
C2 O4 1.434(6) . ?
C2 C3 1.577(8) . ?
C3 C13 1.435(12) . ?
C3 N2 1.433(4) 6 ?
C3 N2 1.433(4) . ?
C4 N3 1.426(6) . ?
C4 N2 1.435(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.233(6) . ?
C5 N4 1.357(5) . ?
C5 N3 1.372(6) . ?
C6 C7 1.471(7) . ?
C6 C14 1.4402(17) . ?
C6 N3 1.527(4) . ?
C6 N3 1.527(4) 6 ?
C7 N4 1.470(5) 6 ?
C7 N4 1.471(5) . ?
C7 O5 1.436(6) . ?
C8 N5 1.419(7) . ?
C8 N4 1.421(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.222(5) . ?
C9 N5 1.349(6) . ?
C9 N6 1.351(7) . ?
C10 N5 1.472(5) . ?
C10 N5 1.472(5) 6 ?
C10 C11 1.541(11) . ?
C10 O6 1.434(6) . ?
C11 C15 1.410(11) . ?
C11 N6 1.463(5) . ?
C11 N6 1.463(5) 6 ?
C12 N1 1.432(6) 2_556 ?
C12 N6 1.464(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 C12 1.431(6) 2_556 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4W O1W O3W 129.8(8) . 5_546 ?
O4W O1W Er1 68.1(4) . . ?
O3W O1W Er1 70.2(4) 5_546 . ?
O3W O2W O2W 127.6(4) 6_545 6_545 ?
O3W O2W Er1 71.1(4) 6_545 . ?
O2W O2W Er1 68.15(19) 6_545 . ?
O1W O3W O2W 144.5(7) 5_546 6_545 ?
O1W O3W Er1 75.7(4) 5_546 . ?
O2W O3W Er1 71.3(4) 6_545 . ?
O1W O4W O4W 136.8(6) . 6_545 ?
O1W O4W Er1 77.8(5) . . ?
O4W O4W Er1 67.7(2) 6_545 . ?
O4W Er1 O4W 180.0(4) 6_545 2_556 ?
O4W Er1 O4W 135.5(4) 6_545 5_546 ?
O4W Er1 O4W 44.5(4) 2_556 5_546 ?
O4W Er1 O4W 44.5(4) 6_545 . ?
O4W Er1 O4W 135.5(4) 2_556 . ?
O4W Er1 O4W 180.0 5_546 . ?
O4W Er1 O3W 80.3(4) 6_545 . ?
O4W Er1 O3W 99.7(4) 2_556 . ?
O4W Er1 O3W 65.8(5) 5_546 . ?
O4W Er1 O3W 114.2(5) . . ?
O4W Er1 O3W 99.7(4) 6_545 5_546 ?
O4W Er1 O3W 80.3(4) 2_556 5_546 ?
O4W Er1 O3W 114.2(5) 5_546 5_546 ?
O4W Er1 O3W 65.8(5) . 5_546 ?
O3W Er1 O3W 180.0 . 5_546 ?
O4W Er1 O3W 114.2(5) 6_545 6_545 ?
O4W Er1 O3W 65.8(5) 2_556 6_545 ?
O4W Er1 O3W 99.7(4) 5_546 6_545 ?
O4W Er1 O3W 80.3(4) . 6_545 ?
O3W Er1 O3W 99.8(4) . 6_545 ?
O3W Er1 O3W 80.2(4) 5_546 6_545 ?
O4W Er1 O3W 65.8(5) 6_545 2_556 ?
O4W Er1 O3W 114.2(5) 2_556 2_556 ?
O4W Er1 O3W 80.3(4) 5_546 2_556 ?
O4W Er1 O3W 99.7(4) . 2_556 ?
O3W Er1 O3W 80.2(4) . 2_556 ?
O3W Er1 O3W 99.8(4) 5_546 2_556 ?
O3W Er1 O3W 180.0(4) 6_545 2_556 ?
O4W Er1 O2W 64.2(6) 6_545 6_545 ?
O4W Er1 O2W 115.8(6) 2_556 6_545 ?
O4W Er1 O2W 98.8(5) 5_546 6_545 ?
O4W Er1 O2W 81.2(5) . 6_545 ?
O3W Er1 O2W 37.5(3) . 6_545 ?
O3W Er1 O2W 142.5(3) 5_546 6_545 ?
O3W Er1 O2W 77.1(3) 6_545 6_545 ?
O3W Er1 O2W 102.9(3) 2_556 6_545 ?
O4W Er1 O2W 115.8(6) 6_545 2_556 ?
O4W Er1 O2W 64.2(6) 2_556 2_556 ?
O4W Er1 O2W 81.2(5) 5_546 2_556 ?
O4W Er1 O2W 98.8(5) . 2_556 ?
O3W Er1 O2W 142.5(3) . 2_556 ?
O3W Er1 O2W 37.5(3) 5_546 2_556 ?
O3W Er1 O2W 102.9(3) 6_545 2_556 ?
O3W Er1 O2W 77.1(3) 2_556 2_556 ?
O2W Er1 O2W 180.0(5) 6_545 2_556 ?
O4W Er1 O2W 98.8(5) 6_545 5_546 ?
O4W Er1 O2W 81.2(5) 2_556 5_546 ?
O4W Er1 O2W 64.2(6) 5_546 5_546 ?
O4W Er1 O2W 115.8(6) . 5_546 ?
O3W Er1 O2W 102.9(3) . 5_546 ?
O3W Er1 O2W 77.1(3) 5_546 5_546 ?
O3W Er1 O2W 142.5(3) 6_545 5_546 ?
O3W Er1 O2W 37.5(3) 2_556 5_546 ?
O2W Er1 O2W 136.3(4) 6_545 5_546 ?
O2W Er1 O2W 43.7(4) 2_556 5_546 ?
O4W Er1 O2W 81.2(5) 6_545 . ?
O4W Er1 O2W 98.8(5) 2_556 . ?
O4W Er1 O2W 115.8(6) 5_546 . ?
O4W Er1 O2W 64.2(6) . . ?
O3W Er1 O2W 77.1(3) . . ?
O3W Er1 O2W 102.9(3) 5_546 . ?
O3W Er1 O2W 37.5(3) 6_545 . ?
O3W Er1 O2W 142.5(3) 2_556 . ?
O2W Er1 O2W 43.7(4) 6_545 . ?
O2W Er1 O2W 136.3(4) 2_556 . ?
O2W Er1 O2W 180.0 5_546 . ?
O1 C1 N1 125.3(4) . . ?
O1 C1 N2 125.9(4) . . ?
N1 C1 N2 108.8(4) . . ?
N1 C2 N1 112.0(5) 6 . ?
N1 C2 O4 113.4(3) 6 . ?
N1 C2 O4 113.4(3) . . ?
N1 C2 C3 101.2(3) 6 . ?
N1 C2 C3 101.2(3) . . ?
O4 C2 C3 114.4(6) . . ?
C13 C3 N2 111.3(3) . 6 ?
C13 C3 N2 111.3(3) . . ?
N2 C3 N2 115.5(5) 6 . ?
C13 C3 C2 110.1(5) . . ?
N2 C3 C2 104.0(3) 6 . ?
N2 C3 C2 104.0(3) . . ?
N3 C4 N2 114.3(4) . . ?
N3 C4 H4A 108.7 . . ?
N2 C4 H4A 108.7 . . ?
N3 C4 H4B 108.7 . . ?
N2 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
O2 C5 N4 127.5(5) . . ?
O2 C5 N3 121.5(4) . . ?
N4 C5 N3 110.9(4) . . ?
C7 C6 C14 118.5(2) . . ?
C7 C6 N3 107.0(2) . . ?
C14 C6 N3 109.16(17) . . ?
C7 C6 N3 107.0(2) . 6 ?
C14 C6 N3 109.16(17) . 6 ?
N3 C6 N3 105.3(3) . 6 ?
C6 C7 N4 102.9(3) . 6 ?
C6 C7 N4 102.9(3) . . ?
N4 C7 N4 112.1(5) 6 . ?
C6 C7 O5 111.4(7) . . ?
N4 C7 O5 113.3(3) 6 . ?
N4 C7 O5 113.3(3) . . ?
N5 C8 N4 115.8(4) . . ?
N5 C8 H8A 108.3 . . ?
N4 C8 H8A 108.3 . . ?
N5 C8 H8B 108.3 . . ?
N4 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
O3 C9 N5 125.0(5) . . ?
O3 C9 N6 126.1(5) . . ?
N5 C9 N6 108.8(4) . . ?
N5 C10 N5 110.8(5) . 6 ?
N5 C10 C11 102.9(3) . . ?
N5 C10 C11 102.9(3) 6 . ?
N5 C10 O6 113.9(4) . . ?
N5 C10 O6 113.9(4) 6 . ?
C11 C10 O6 111.4(7) . . ?
C15 C11 N6 111.6(5) . . ?
C15 C11 N6 111.6(5) . 6 ?
N6 C11 N6 112.1(5) . 6 ?
C15 C11 C10 115.1(8) . . ?
N6 C11 C10 102.9(4) . . ?
N6 C11 C10 102.9(4) 6 . ?
N1 C12 N6 114.1(4) 2_556 . ?
N1 C12 H12A 108.7 2_556 . ?
N6 C12 H12A 108.7 . . ?
N1 C12 H12B 108.7 2_556 . ?
N6 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C3 C13 H13A 109.5 . . ?
C3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C14 H14A 109.5 . . ?
C6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C12 122.0(4) . 2_556 ?
C1 N1 C2 113.1(4) . . ?
C12 N1 C2 123.6(4) 2_556 . ?
C1 N2 C4 123.0(4) . . ?
C1 N2 C3 112.6(3) . . ?
C4 N2 C3 123.9(4) . . ?
C5 N3 C4 124.6(4) . . ?
C5 N3 C6 106.4(3) . . ?
C4 N3 C6 127.2(4) . . ?
C5 N4 C8 122.3(4) . . ?
C5 N4 C7 112.3(4) . . ?
C8 N4 C7 124.6(4) . . ?
C9 N5 C8 122.4(4) . . ?
C9 N5 C10 112.5(5) . . ?
C8 N5 C10 124.3(4) . . ?
C9 N6 C12 123.4(4) . . ?
C9 N6 C11 112.9(5) . . ?
C12 N6 C11 122.3(5) . . ?
C2 O4 H4 109.5 . . ?
C7 O5 H5 109.5 . . ?
C10 O6 H6 109.5 . . ?

_refine_diff_density_max         1.933
_refine_diff_density_min         -4.532
_refine_diff_density_rms         0.146

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Ho
_database_code_depnum_ccdc_archive 'CCDC 1055506'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H111 Ho N24 O51'
_chemical_formula_weight         1933.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.792(3)
_cell_length_b                   12.2562(15)
_cell_length_c                   16.386(2)
_cell_angle_alpha                90
_cell_angle_beta                 120.021(4)
_cell_angle_gamma                90
_cell_volume                     3789.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_F_000             2012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.171
_shelx_estimated_absorpt_T_min   0.713
_shelx_estimated_absorpt_T_max   0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.773
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12977
_diffrn_reflns_av_unetI/netI     0.1012
_diffrn_reflns_av_R_equivalents  0.0926
_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       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.435
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             3533
_reflns_number_gt                2655
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 114 33 ' '
2 0.291 -0.020 0.500 1135 439 ' '
3 0.000 0.500 0.000 114 33 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0701P)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         3533
_refine_ls_number_parameters     248
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1346
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.017
_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 0.5784(5) -0.3500(7) 0.0373(8) 0.071(3) Uani 0.5 1 d . . P . .
O2W O 0.5142(7) -0.4290(8) 0.1414(8) 0.094(3) Uani 0.5 1 d . . P . .
O3W O 0.6098(5) -0.4283(9) 0.1100(11) 0.143(6) Uani 0.5 1 d . . P . .
O4W O 0.4678(8) -0.6471(9) 0.0610(11) 0.119(5) Uani 0.5 1 d . . P . .
Ho1 Ho 0.5000 -0.5000 0.0000 0.0422(2) Uani 1 4 d S T P . .
C1 C 0.6977(4) -0.1564(5) 0.0271(6) 0.0606(18) Uani 1 1 d . . . . .
C2 C 0.7323(4) 0.0000 -0.0175(7) 0.055(2) Uani 1 2 d S T P . .
C3 C 0.7666(4) 0.0000 0.0911(7) 0.056(2) Uani 1 2 d DS T P . .
C4 C 0.7566(4) -0.1443(6) 0.1978(5) 0.070(2) Uani 1 1 d . . . . .
H4A H 0.8076 -0.1336 0.2400 0.084 Uiso 1 1 calc R U . . .
H4B H 0.7478 -0.2231 0.1905 0.084 Uiso 1 1 calc R U . . .
C5 C 0.6673(3) -0.1540(5) 0.2463(5) 0.0540(16) Uani 1 1 d . . . . .
C6 C 0.7409(4) 0.0000 0.3004(6) 0.059(2) Uani 1 2 d DS T P . .
C7 C 0.6883(5) 0.0000 0.3403(6) 0.058(2) Uani 1 2 d S T P . .
C8 C 0.6019(4) -0.1454(6) 0.3327(6) 0.074(2) Uani 1 1 d . . . . .
H8A H 0.6238 -0.1347 0.4009 0.089 Uiso 1 1 calc R U . . .
H8B H 0.5980 -0.2241 0.3207 0.089 Uiso 1 1 calc R U . . .
C9 C 0.4731(4) -0.1548(5) 0.2227(5) 0.0639(18) Uani 1 1 d . . . . .
C10 C 0.5126(5) 0.0000 0.3187(6) 0.054(2) Uani 1 2 d S T P . .
C11 C 0.4300(5) 0.0000 0.2570(7) 0.057(2) Uani 1 2 d S T P . .
C12 C 0.3443(3) -0.1403(5) 0.1429(5) 0.0595(18) Uani 1 1 d . . . . .
H12A H 0.3151 -0.1232 0.1712 0.071 Uiso 1 1 calc R U . . .
H12B H 0.3471 -0.2199 0.1404 0.071 Uiso 1 1 calc R U . . .
C13 C 0.7855(7) 0.0000 -0.0434(10) 0.111(4) Uani 1 2 d S T P . .
H13A H 0.8125 -0.0672 -0.0223 0.167 Uiso 0.5 1 calc R U P . .
H13B H 0.7635 0.0055 -0.1114 0.167 Uiso 0.5 1 calc R U P . .
H13C H 0.8170 0.0617 -0.0142 0.167 Uiso 0.5 1 calc R U P . .
C14 C 0.7180(5) 0.0000 0.4364(6) 0.083(3) Uani 1 2 d S T P . .
H14A H 0.7452 -0.0664 0.4621 0.124 Uiso 0.5 1 calc R U P . .
H14B H 0.7491 0.0626 0.4627 0.124 Uiso 0.5 1 calc R U P . .
H14C H 0.6809 0.0038 0.4525 0.124 Uiso 0.5 1 calc R U P . .
C15 C 0.5383(6) 0.0000 0.4214(7) 0.100(4) Uani 1 2 d S T P . .
H15A H 0.5245 0.0676 0.4386 0.149 Uiso 0.5 1 calc R U P . .
H15B H 0.5177 -0.0612 0.4368 0.149 Uiso 0.5 1 calc R U P . .
H15C H 0.5895 -0.0064 0.4560 0.149 Uiso 0.5 1 calc R U P . .
N1 N 0.6910(3) -0.0991(4) -0.0479(4) 0.0570(14) Uani 1 1 d . . . . .
N2 N 0.7374(3) -0.0988(4) 0.1069(4) 0.0597(14) Uani 1 1 d . . . . .
N3 N 0.7194(3) -0.0986(4) 0.2420(4) 0.0576(14) Uani 1 1 d . . . . .
N4 N 0.6477(2) -0.0990(4) 0.3015(4) 0.0559(14) Uani 1 1 d . . . . .
N5 N 0.5311(3) -0.0987(4) 0.2869(4) 0.0579(14) Uani 1 1 d . . . . .
N6 N 0.4137(3) -0.0992(4) 0.2028(4) 0.0542(13) Uani 1 1 d . . . . .
O1 O 0.6735(3) -0.2491(4) 0.0223(4) 0.0874(16) Uani 1 1 d . . . . .
O2 O 0.6436(3) -0.2423(4) 0.2085(4) 0.0821(15) Uani 1 1 d . . . . .
O3 O 0.4741(3) -0.2443(4) 0.1916(5) 0.115(2) Uani 1 1 d . . . . .
O4 O 0.8440(5) 0.0000 0.1389(9) 0.205(6) Uani 1 2 d DS T P . .
H4 H 0.8580 0.0585 0.1283 0.308 Uiso 0.5 1 calc R U P . .
O5 O 0.8153(4) 0.0000 0.3753(8) 0.182(5) Uani 1 2 d DS T P . .
H5 H 0.8411 -0.0049 0.3517 0.273 Uiso 0.5 1 calc R U P . .
O6 O 0.3950(5) 0.0000 0.3102(7) 0.117(3) Uani 1 2 d S T P . .
H6 H 0.3515 0.0000 0.2739 0.176 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
O1W O4W 1.409(16) 5_645 ?
O1W O3W 1.411(16) . ?
O1W Ho1 2.372(8) . ?
O2W O4W 1.516(17) 6_545 ?
O2W O2W 1.74(2) 6_545 ?
O2W Ho1 2.346(10) . ?
O3W O3W 1.76(2) 6_545 ?
O3W Ho1 2.331(10) . ?
O4W O1W 1.409(16) 5_645 ?
O4W O2W 1.516(17) 6_545 ?
O4W Ho1 2.333(10) . ?
Ho1 O3W 2.331(10) 5_645 ?
Ho1 O3W 2.331(10) 6_545 ?
Ho1 O3W 2.331(10) 2_655 ?
Ho1 O4W 2.333(10) 6_545 ?
Ho1 O4W 2.333(10) 2_655 ?
Ho1 O4W 2.333(10) 5_645 ?
Ho1 O2W 2.346(10) 5_645 ?
Ho1 O2W 2.346(10) 6_545 ?
Ho1 O2W 2.346(10) 2_655 ?
C1 O1 1.238(8) . ?
C1 N2 1.351(9) . ?
C1 N1 1.359(8) . ?
C2 C13 1.420(13) . ?
C2 N1 1.444(7) 6 ?
C2 N1 1.444(7) . ?
C2 C3 1.548(13) . ?
C3 N2 1.449(7) . ?
C3 N2 1.449(7) 6 ?
C3 O4 1.463(8) . ?
C4 N2 1.442(8) . ?
C4 N3 1.444(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.224(7) . ?
C5 N3 1.354(8) . ?
C5 N4 1.358(8) . ?
C6 N3 1.465(7) 6 ?
C6 N3 1.465(7) . ?
C6 O5 1.464(8) . ?
C6 C7 1.580(13) . ?
C7 C14 1.371(12) . ?
C7 N4 1.448(7) 6 ?
C7 N4 1.448(7) . ?
C8 N4 1.445(8) . ?
C8 N5 1.453(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.214(8) . ?
C9 N6 1.352(8) . ?
C9 N5 1.359(8) . ?
C10 N5 1.452(7) . ?
C10 N5 1.452(7) 6 ?
C10 C15 1.484(13) . ?
C10 C11 1.562(12) . ?
C11 O6 1.416(11) . ?
C11 N6 1.442(7) . ?
C11 N6 1.442(7) 6 ?
C12 N6 1.420(7) . ?
C12 N1 1.440(8) 2_655 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 C12 1.440(8) 2_655 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4W O1W O3W 135.7(10) 5_645 . ?
O4W O1W Ho1 71.1(5) 5_645 . ?
O3W O1W Ho1 70.9(5) . . ?
O4W O2W O2W 128.0(6) 6_545 6_545 ?
O4W O2W Ho1 70.6(6) 6_545 . ?
O2W O2W Ho1 68.2(3) 6_545 . ?
O1W O3W O3W 132.8(6) . 6_545 ?
O1W O3W Ho1 74.1(6) . . ?
O3W O3W Ho1 67.8(3) 6_545 . ?
O1W O4W O2W 142.5(10) 5_645 6_545 ?
O1W O4W Ho1 74.1(6) 5_645 . ?
O2W O4W Ho1 71.6(5) 6_545 . ?
O3W Ho1 O3W 180.0 . 5_645 ?
O3W Ho1 O3W 44.3(5) . 6_545 ?
O3W Ho1 O3W 135.7(5) 5_645 6_545 ?
O3W Ho1 O3W 135.7(5) . 2_655 ?
O3W Ho1 O3W 44.3(5) 5_645 2_655 ?
O3W Ho1 O3W 180.0(5) 6_545 2_655 ?
O3W Ho1 O4W 77.9(5) . 6_545 ?
O3W Ho1 O4W 102.1(5) 5_645 6_545 ?
O3W Ho1 O4W 111.9(5) 6_545 6_545 ?
O3W Ho1 O4W 68.1(5) 2_655 6_545 ?
O3W Ho1 O4W 102.1(5) . 2_655 ?
O3W Ho1 O4W 77.9(5) 5_645 2_655 ?
O3W Ho1 O4W 68.1(5) 6_545 2_655 ?
O3W Ho1 O4W 111.9(5) 2_655 2_655 ?
O4W Ho1 O4W 180.0(6) 6_545 2_655 ?
O3W Ho1 O4W 68.1(5) . 5_645 ?
O3W Ho1 O4W 111.9(5) 5_645 5_645 ?
O3W Ho1 O4W 102.1(5) 6_545 5_645 ?
O3W Ho1 O4W 77.9(5) 2_655 5_645 ?
O4W Ho1 O4W 78.8(7) 6_545 5_645 ?
O4W Ho1 O4W 101.2(7) 2_655 5_645 ?
O3W Ho1 O4W 111.9(5) . . ?
O3W Ho1 O4W 68.1(5) 5_645 . ?
O3W Ho1 O4W 77.9(5) 6_545 . ?
O3W Ho1 O4W 102.1(5) 2_655 . ?
O4W Ho1 O4W 101.2(7) 6_545 . ?
O4W Ho1 O4W 78.8(7) 2_655 . ?
O4W Ho1 O4W 180.0 5_645 . ?
O3W Ho1 O2W 61.2(5) . . ?
O3W Ho1 O2W 118.8(5) 5_645 . ?
O3W Ho1 O2W 78.4(5) 6_545 . ?
O3W Ho1 O2W 101.6(5) 2_655 . ?
O4W Ho1 O2W 37.8(4) 6_545 . ?
O4W Ho1 O2W 142.2(4) 2_655 . ?
O4W Ho1 O2W 102.5(5) 5_645 . ?
O4W Ho1 O2W 77.5(5) . . ?
O3W Ho1 O2W 118.8(5) . 5_645 ?
O3W Ho1 O2W 61.2(5) 5_645 5_645 ?
O3W Ho1 O2W 101.6(5) 6_545 5_645 ?
O3W Ho1 O2W 78.4(5) 2_655 5_645 ?
O4W Ho1 O2W 142.2(4) 6_545 5_645 ?
O4W Ho1 O2W 37.8(4) 2_655 5_645 ?
O4W Ho1 O2W 77.5(5) 5_645 5_645 ?
O4W Ho1 O2W 102.5(5) . 5_645 ?
O2W Ho1 O2W 180.0 . 5_645 ?
O3W Ho1 O2W 78.4(5) . 6_545 ?
O3W Ho1 O2W 101.6(5) 5_645 6_545 ?
O3W Ho1 O2W 61.2(5) 6_545 6_545 ?
O3W Ho1 O2W 118.8(5) 2_655 6_545 ?
O4W Ho1 O2W 77.5(5) 6_545 6_545 ?
O4W Ho1 O2W 102.5(5) 2_655 6_545 ?
O4W Ho1 O2W 142.2(4) 5_645 6_545 ?
O4W Ho1 O2W 37.8(4) . 6_545 ?
O2W Ho1 O2W 43.5(5) . 6_545 ?
O2W Ho1 O2W 136.5(5) 5_645 6_545 ?
O3W Ho1 O2W 101.6(5) . 2_655 ?
O3W Ho1 O2W 78.4(5) 5_645 2_655 ?
O3W Ho1 O2W 118.8(5) 6_545 2_655 ?
O3W Ho1 O2W 61.2(5) 2_655 2_655 ?
O4W Ho1 O2W 102.5(4) 6_545 2_655 ?
O4W Ho1 O2W 77.5(5) 2_655 2_655 ?
O4W Ho1 O2W 37.8(4) 5_645 2_655 ?
O4W Ho1 O2W 142.2(4) . 2_655 ?
O2W Ho1 O2W 136.5(5) . 2_655 ?
O2W Ho1 O2W 43.5(5) 5_645 2_655 ?
O2W Ho1 O2W 180.0(7) 6_545 2_655 ?
O1 C1 N2 126.0(7) . . ?
O1 C1 N1 124.5(7) . . ?
N2 C1 N1 109.4(6) . . ?
C13 C2 N1 111.0(5) . 6 ?
C13 C2 N1 111.0(5) . . ?
N1 C2 N1 114.5(7) 6 . ?
C13 C2 C3 110.4(9) . . ?
N1 C2 C3 104.8(5) 6 . ?
N1 C2 C3 104.8(5) . . ?
N2 C3 N2 113.3(7) . 6 ?
N2 C3 C2 101.7(5) . . ?
N2 C3 C2 101.7(5) 6 . ?
N2 C3 O4 113.3(5) . . ?
N2 C3 O4 113.3(5) 6 . ?
C2 C3 O4 112.3(8) . . ?
N2 C4 N3 115.1(5) . . ?
N2 C4 H4A 108.5 . . ?
N3 C4 H4A 108.5 . . ?
N2 C4 H4B 108.5 . . ?
N3 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N3 124.7(7) . . ?
O2 C5 N4 125.6(6) . . ?
N3 C5 N4 109.7(5) . . ?
N3 C6 N3 111.2(7) 6 . ?
N3 C6 O5 114.0(5) 6 . ?
N3 C6 O5 114.0(5) . . ?
N3 C6 C7 102.0(5) 6 . ?
N3 C6 C7 102.0(5) . . ?
O5 C6 C7 112.4(9) . . ?
C14 C7 N4 109.8(5) . 6 ?
C14 C7 N4 109.8(5) . . ?
N4 C7 N4 113.9(7) 6 . ?
C14 C7 C6 116.9(8) . . ?
N4 C7 C6 103.3(5) 6 . ?
N4 C7 C6 103.3(5) . . ?
N4 C8 N5 113.9(5) . . ?
N4 C8 H8A 108.8 . . ?
N5 C8 H8A 108.8 . . ?
N4 C8 H8B 108.8 . . ?
N5 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O3 C9 N6 124.7(7) . . ?
O3 C9 N5 125.3(7) . . ?
N6 C9 N5 109.8(6) . . ?
N5 C10 N5 112.8(7) . 6 ?
N5 C10 C15 113.1(5) . . ?
N5 C10 C15 113.1(5) 6 . ?
N5 C10 C11 101.8(5) . . ?
N5 C10 C11 101.8(5) 6 . ?
C15 C10 C11 113.1(8) . . ?
O6 C11 N6 109.7(5) . . ?
O6 C11 N6 109.7(5) . 6 ?
N6 C11 N6 114.9(8) . 6 ?
O6 C11 C10 113.7(8) . . ?
N6 C11 C10 104.4(5) . . ?
N6 C11 C10 104.4(5) 6 . ?
N6 C12 N1 115.5(5) . 2_655 ?
N6 C12 H12A 108.4 . . ?
N1 C12 H12A 108.4 2_655 . ?
N6 C12 H12B 108.4 . . ?
N1 C12 H12B 108.4 2_655 . ?
H12A C12 H12B 107.5 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C12 123.7(5) . 2_655 ?
C1 N1 C2 110.9(6) . . ?
C12 N1 C2 124.9(6) 2_655 . ?
C1 N2 C3 113.0(6) . . ?
C1 N2 C4 120.7(6) . . ?
C3 N2 C4 125.5(6) . . ?
C5 N3 C4 121.9(6) . . ?
C5 N3 C6 112.5(6) . . ?
C4 N3 C6 124.8(6) . . ?
C5 N4 C8 122.9(5) . . ?
C5 N4 C7 112.4(6) . . ?
C8 N4 C7 123.6(6) . . ?
C9 N5 C10 112.5(6) . . ?
C9 N5 C8 122.4(5) . . ?
C10 N5 C8 123.8(6) . . ?
C9 N6 C12 123.2(5) . . ?
C9 N6 C11 111.4(6) . . ?
C12 N6 C11 125.0(6) . . ?
C3 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C11 O6 H6 109.5 . . ?

_refine_diff_density_max         0.833
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.097

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Lu
_database_code_depnum_ccdc_archive 'CCDC 1055507'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H107 Lu N24 O49'
_chemical_formula_weight         1907.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.7182(17)
_cell_length_b                   12.1691(9)
_cell_length_c                   16.4253(12)
_cell_angle_alpha                90
_cell_angle_beta                 120.018(2)
_cell_angle_gamma                90
_cell_volume                     3758.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    1.437
_shelx_estimated_absorpt_T_min   0.656
_shelx_estimated_absorpt_T_max   0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_T_max  0.708
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15851
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.432
_diffrn_reflns_theta_max         25.193
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3541
_reflns_number_gt                3402
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 115 26 ' '
2 0.281 -0.027 0.500 1089 412 ' '
3 0.000 0.500 0.000 115 26 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1041P)²+3.1022P] 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         3541
_refine_ls_number_parameters     234
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1399
_refine_ls_wR_factor_gt          0.1364
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.012
_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 0.5755(5) 0.6495(7) 1.0324(9) 0.078(3) Uani 0.5 1 d . . P . .
O2W O 0.5164(7) 0.5704(7) 1.1395(7) 0.088(3) Uani 0.5 1 d . . P . .
O3W O 0.4741(11) 0.3552(8) 1.0659(11) 0.136(7) Uani 0.5 1 d . . P . .
O4W O 0.6093(6) 0.5668(8) 1.0901(19) 0.235(14) Uani 0.5 1 d . . P . .
Lu1 Lu 0.5000 0.5000 1.0000 0.03741(18) Uani 1 4 d S T P . .
C1 C 0.3031(3) 0.8419(5) 0.9748(5) 0.0576(14) Uani 1 1 d . . . . .
C2 C 0.2698(4) 1.0000 1.0205(6) 0.052 Uani 1 2 d S T P . .
C3 C 0.2318(4) 1.0000 0.9108(6) 0.054 Uani 1 2 d DS T P . .
C4 C 0.2413(4) 0.8558(5) 0.8032(5) 0.063 Uani 1 1 d . . . . .
H4A H 0.2484 0.7761 0.8089 0.076 Uiso 1 1 calc R U . . .
H4B H 0.1904 0.8692 0.7614 0.076 Uiso 1 1 calc R U . . .
C5 C 0.3304(3) 0.8440(4) 0.7546(4) 0.0500(12) Uani 1 1 d . . . . .
C6 C 0.2566(3) 1.0000 0.7007(5) 0.0484(17) Uani 1 2 d DS T P . .
C7 C 0.3088(4) 1.0000 0.6611(5) 0.0495(17) Uani 1 2 d S T P . .
C8 C 0.3957(3) 0.8542(5) 0.6670(5) 0.0659(17) Uani 1 1 d . . . . .
H8A H 0.3994 0.7748 0.6783 0.079 Uiso 1 1 calc R U . . .
H8B H 0.3734 0.8657 0.5990 0.079 Uiso 1 1 calc R U . . .
C9 C 0.5239(3) 0.8435(5) 0.7760(5) 0.0612(15) Uani 1 1 d . . . . .
C10 C 0.4850(4) 1.0000 0.6813(5) 0.0481(17) Uani 1 2 d S T P . .
C11 C 0.5681(4) 1.0000 0.7427(6) 0.0489(17) Uani 1 2 d S T P . .
C12 C 0.6536(3) 0.8579(5) 0.8564(4) 0.0554(14) Uani 1 1 d . . . . .
H12A H 0.6826 0.8749 0.8277 0.066 Uiso 1 1 calc R U . . .
H12B H 0.6507 0.7778 0.8592 0.066 Uiso 1 1 calc R U . . .
C13 C 0.210(2) 1.0000 1.050(2) 0.31(2) Uani 1 2 d S T P . .
H13A H 0.1835 1.0679 1.0291 0.462 Uiso 0.5 1 calc R U P . .
H13B H 0.1786 0.9382 1.0203 0.462 Uiso 0.5 1 calc R U P . .
H13C H 0.2326 0.9939 1.1175 0.462 Uiso 0.5 1 calc R U P . .
C14 C 0.2763(10) 1.0000 0.5655(10) 0.143(7) Uani 1 2 d S T P . .
H14A H 0.2490 0.9329 0.5411 0.215 Uiso 0.5 1 calc R U P . .
H14B H 0.2447 1.0629 0.5408 0.215 Uiso 0.5 1 calc R U P . .
H14C H 0.3119 1.0042 0.5465 0.215 Uiso 0.5 1 calc R U P . .
C15 C 0.4600(7) 1.0000 0.5779(7) 0.090(3) Uani 1 2 d S T P . .
H15A H 0.4739 1.0683 0.5612 0.135 Uiso 0.5 1 calc R U P . .
H15B H 0.4814 0.9387 0.5633 0.135 Uiso 0.5 1 calc R U P . .
H15C H 0.4087 0.9930 0.5426 0.135 Uiso 0.5 1 calc R U P . .
N1 N 0.3114(3) 0.9005(3) 1.0495(3) 0.0510(11) Uani 1 1 d . . . . .
N2 N 0.2615(3) 0.8998(4) 0.8945(3) 0.0538(11) Uani 1 1 d . . . . .
N3 N 0.2792(2) 0.8999(4) 0.7596(3) 0.0516(11) Uani 1 1 d . . . . .
N4 N 0.3500(2) 0.9004(4) 0.6992(4) 0.0526(11) Uani 1 1 d . . . . .
N5 N 0.4661(3) 0.9002(4) 0.7118(4) 0.0553(11) Uani 1 1 d . . . . .
N6 N 0.5835(2) 0.9002(4) 0.7973(3) 0.0518(11) Uani 1 1 d . . . . .
O1 O 0.3261(3) 0.7492(3) 0.9776(4) 0.0817(14) Uani 1 1 d . . . . .
O2 O 0.3539(3) 0.7556(4) 0.7906(4) 0.0741(12) Uani 1 1 d . . . . .
O3 O 0.5227(3) 0.7536(4) 0.8073(6) 0.108(2) Uani 1 1 d . . . . .
O4 O 0.1537(4) 1.0000 0.8617(9) 0.152(5) Uani 1 2 d DS T P . .
H4 H 0.1397 1.0527 0.8802 0.228 Uiso 0.5 1 calc R U P . .
O5 O 0.1828(5) 1.0000 0.6241(9) 0.162(5) Uani 0.5 1 d DS T P . .
H5 H 0.1558 1.0047 0.6461 0.243 Uiso 1 2 calc R U P . .
O6 O 0.6015(7) 1.0000 0.6857(10) 0.151(5) Uani 1 2 d S T P . .
H6 H 0.5919 0.9419 0.6553 0.227 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
O1W O4W 1.324(17) . ?
O1W O3W 1.425(19) 5_667 ?
O1W Lu1 2.325(8) . ?
O2W O3W 1.419(18) 6_565 ?
O2W O2W 1.714(18) 6_565 ?
O2W Lu1 2.301(9) . ?
O3W O1W 1.425(19) 5_667 ?
O3W O2W 1.419(18) 6_565 ?
O3W Lu1 2.281(9) . ?
O4W O4W 1.63(2) 6_565 ?
O4W Lu1 2.230(11) . ?
Lu1 O4W 2.229(11) 5_667 ?
Lu1 O4W 2.229(11) 6_565 ?
Lu1 O4W 2.229(11) 2_657 ?
Lu1 O3W 2.281(9) 6_565 ?
Lu1 O3W 2.281(9) 2_657 ?
Lu1 O3W 2.281(9) 5_667 ?
Lu1 O2W 2.301(10) 5_667 ?
Lu1 O2W 2.301(10) 2_657 ?
Lu1 O2W 2.301(10) 6_565 ?
C1 O1 1.225(7) . ?
C1 N1 1.352(8) . ?
C1 N2 1.363(8) . ?
C2 N1 1.442(6) . ?
C2 N1 1.442(6) 6_575 ?
C2 C3 1.561(13) . ?
C2 C13 1.59(3) . ?
C3 N2 1.465(6) 6_575 ?
C3 N2 1.465(6) . ?
C3 O4 1.470(8) . ?
C4 N3 1.438(7) . ?
C4 N2 1.439(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.211(7) . ?
C5 N3 1.340(7) . ?
C5 N4 1.366(7) . ?
C6 N3 1.479(6) 6_575 ?
C6 N3 1.479(6) . ?
C6 O5 1.461(8) . ?
C6 C7 1.565(11) . ?
C7 C14 1.362(17) . ?
C7 N4 1.449(6) 6_575 ?
C7 N4 1.449(6) . ?
C8 N5 1.438(8) . ?
C8 N4 1.451(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.215(8) . ?
C9 N5 1.355(8) . ?
C9 N6 1.349(8) . ?
C10 N5 1.449(6) . ?
C10 N5 1.449(6) 6_575 ?
C10 C15 1.502(13) . ?
C10 C11 1.566(12) . ?
C11 N6 1.445(6) . ?
C11 N6 1.445(6) 6_575 ?
C11 O6 1.444(13) . ?
C12 N6 1.430(7) . ?
C12 N1 1.435(8) 2_657 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 C12 1.435(8) 2_657 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4W O1W O3W 127.9(13) . 5_667 ?
O4W O1W Lu1 69.2(6) . . ?
O3W O1W Lu1 70.3(5) 5_667 . ?
O3W O2W O2W 129.6(8) 6_565 6_565 ?
O3W O2W Lu1 71.2(6) 6_565 . ?
O2W O2W Lu1 68.1(2) 6_565 . ?
O1W O3W O2W 142.3(10) 5_667 6_565 ?
O1W O3W Lu1 73.7(5) 5_667 . ?
O2W O3W Lu1 72.7(6) 6_565 . ?
O1W O4W O4W 139.4(9) . 6_565 ?
O1W O4W Lu1 77.1(7) . . ?
O4W O4W Lu1 68.6(3) 6_565 . ?
O4W Lu1 O4W 137.2(5) 5_667 6_565 ?
O4W Lu1 O4W 42.8(5) 5_667 2_657 ?
O4W Lu1 O4W 180.0 6_565 2_657 ?
O4W Lu1 O4W 180.0(5) 5_667 . ?
O4W Lu1 O4W 42.8(5) 6_565 . ?
O4W Lu1 O4W 137.2(5) 2_657 . ?
O4W Lu1 O3W 99.4(8) 5_667 6_565 ?
O4W Lu1 O3W 113.6(8) 6_565 6_565 ?
O4W Lu1 O3W 66.4(8) 2_657 6_565 ?
O4W Lu1 O3W 80.6(8) . 6_565 ?
O4W Lu1 O3W 80.6(8) 5_667 2_657 ?
O4W Lu1 O3W 66.4(8) 6_565 2_657 ?
O4W Lu1 O3W 113.6(8) 2_657 2_657 ?
O4W Lu1 O3W 99.4(8) . 2_657 ?
O3W Lu1 O3W 180.0 6_565 2_657 ?
O4W Lu1 O3W 113.6(8) 5_667 5_667 ?
O4W Lu1 O3W 99.4(8) 6_565 5_667 ?
O4W Lu1 O3W 80.6(8) 2_657 5_667 ?
O4W Lu1 O3W 66.4(8) . 5_667 ?
O3W Lu1 O3W 78.8(6) 6_565 5_667 ?
O3W Lu1 O3W 101.2(6) 2_657 5_667 ?
O4W Lu1 O3W 66.4(8) 5_667 . ?
O4W Lu1 O3W 80.6(8) 6_565 . ?
O4W Lu1 O3W 99.4(8) 2_657 . ?
O4W Lu1 O3W 113.6(8) . . ?
O3W Lu1 O3W 101.2(6) 6_565 . ?
O3W Lu1 O3W 78.8(6) 2_657 . ?
O3W Lu1 O3W 180.0 5_667 . ?
O4W Lu1 O2W 67.7(9) 5_667 5_667 ?
O4W Lu1 O2W 96.2(8) 6_565 5_667 ?
O4W Lu1 O2W 83.8(8) 2_657 5_667 ?
O4W Lu1 O2W 112.3(9) . 5_667 ?
O3W Lu1 O2W 143.9(5) 6_565 5_667 ?
O3W Lu1 O2W 36.1(5) 2_657 5_667 ?
O3W Lu1 O2W 76.5(4) 5_667 5_667 ?
O3W Lu1 O2W 103.5(4) . 5_667 ?
O4W Lu1 O2W 83.8(8) 5_667 2_657 ?
O4W Lu1 O2W 112.3(9) 6_565 2_657 ?
O4W Lu1 O2W 67.7(9) 2_657 2_657 ?
O4W Lu1 O2W 96.2(8) . 2_657 ?
O3W Lu1 O2W 103.5(4) 6_565 2_657 ?
O3W Lu1 O2W 76.5(4) 2_657 2_657 ?
O3W Lu1 O2W 36.1(5) 5_667 2_657 ?
O3W Lu1 O2W 143.9(5) . 2_657 ?
O2W Lu1 O2W 43.7(5) 5_667 2_657 ?
O4W Lu1 O2W 96.2(8) 5_667 6_565 ?
O4W Lu1 O2W 67.7(9) 6_565 6_565 ?
O4W Lu1 O2W 112.3(9) 2_657 6_565 ?
O4W Lu1 O2W 83.8(8) . 6_565 ?
O3W Lu1 O2W 76.5(4) 6_565 6_565 ?
O3W Lu1 O2W 103.5(4) 2_657 6_565 ?
O3W Lu1 O2W 143.9(5) 5_667 6_565 ?
O3W Lu1 O2W 36.1(5) . 6_565 ?
O2W Lu1 O2W 136.3(5) 5_667 6_565 ?
O2W Lu1 O2W 180.0 2_657 6_565 ?
O4W Lu1 O2W 112.3(9) 5_667 . ?
O4W Lu1 O2W 83.8(8) 6_565 . ?
O4W Lu1 O2W 96.2(8) 2_657 . ?
O4W Lu1 O2W 67.7(9) . . ?
O3W Lu1 O2W 36.1(5) 6_565 . ?
O3W Lu1 O2W 143.9(5) 2_657 . ?
O3W Lu1 O2W 103.5(4) 5_667 . ?
O3W Lu1 O2W 76.5(4) . . ?
O2W Lu1 O2W 180.0(7) 5_667 . ?
O2W Lu1 O2W 136.3(5) 2_657 . ?
O2W Lu1 O2W 43.7(5) 6_565 . ?
O1 C1 N1 125.8(6) . . ?
O1 C1 N2 124.9(6) . . ?
N1 C1 N2 109.2(5) . . ?
N1 C2 N1 114.2(6) . 6_575 ?
N1 C2 C3 105.3(4) . . ?
N1 C2 C3 105.3(4) 6_575 . ?
N1 C2 C13 111.7(7) . . ?
N1 C2 C13 111.7(7) 6_575 . ?
C3 C2 C13 108.0(15) . . ?
N2 C3 N2 112.7(6) 6_575 . ?
N2 C3 C2 100.6(4) 6_575 . ?
N2 C3 C2 100.6(4) . . ?
N2 C3 O4 113.1(5) 6_575 . ?
N2 C3 O4 113.1(5) . . ?
C2 C3 O4 115.6(8) . . ?
N3 C4 N2 115.4(5) . . ?
N3 C4 H4A 108.4 . . ?
N2 C4 H4A 108.4 . . ?
N3 C4 H4B 108.4 . . ?
N2 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N3 125.5(6) . . ?
O2 C5 N4 125.2(6) . . ?
N3 C5 N4 109.2(5) . . ?
N3 C6 N3 111.0(6) 6_575 . ?
N3 C6 O5 115.2(4) 6_575 . ?
N3 C6 O5 115.2(4) . . ?
N3 C6 C7 101.4(4) 6_575 . ?
N3 C6 C7 101.4(4) . . ?
O5 C6 C7 110.7(8) . . ?
C14 C7 N4 110.5(6) . 6_575 ?
C14 C7 N4 110.5(6) . . ?
N4 C7 N4 113.6(6) 6_575 . ?
C14 C7 C6 114.4(10) . . ?
N4 C7 C6 103.9(4) 6_575 . ?
N4 C7 C6 103.9(4) . . ?
N5 C8 N4 114.2(5) . . ?
N5 C8 H8A 108.7 . . ?
N4 C8 H8A 108.7 . . ?
N5 C8 H8B 108.7 . . ?
N4 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O3 C9 N5 125.4(6) . . ?
O3 C9 N6 124.9(6) . . ?
N5 C9 N6 109.6(5) . . ?
N5 C10 N5 114.0(6) . 6_575 ?
N5 C10 C15 112.7(5) . . ?
N5 C10 C15 112.7(5) 6_575 . ?
N5 C10 C11 102.2(4) . . ?
N5 C10 C11 102.2(4) 6_575 . ?
C15 C10 C11 112.1(7) . . ?
N6 C11 N6 114.3(7) . 6_575 ?
N6 C11 O6 111.5(4) . . ?
N6 C11 O6 111.5(4) 6_575 . ?
N6 C11 C10 103.6(4) . . ?
N6 C11 C10 103.6(4) 6_575 . ?
O6 C11 C10 111.9(8) . . ?
N6 C12 N1 114.3(4) . 2_657 ?
N6 C12 H12A 108.7 . . ?
N1 C12 H12A 108.7 2_657 . ?
N6 C12 H12B 108.7 . . ?
N1 C12 H12B 108.7 2_657 . ?
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 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C12 123.1(5) . 2_657 ?
C1 N1 C2 111.4(6) . . ?
C12 N1 C2 124.5(5) 2_657 . ?
C1 N2 C4 121.6(5) . . ?
C1 N2 C3 113.1(5) . . ?
C4 N2 C3 124.6(6) . . ?
C5 N3 C4 122.7(5) . . ?
C5 N3 C6 113.2(5) . . ?
C4 N3 C6 123.1(5) . . ?
C5 N4 C8 123.1(5) . . ?
C5 N4 C7 112.2(5) . . ?
C8 N4 C7 123.6(6) . . ?
C9 N5 C8 122.3(5) . . ?
C9 N5 C10 112.6(5) . . ?
C8 N5 C10 124.2(6) . . ?
C9 N6 C12 123.3(5) . . ?
C9 N6 C11 112.0(5) . . ?
C12 N6 C11 124.1(5) . . ?
C3 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C11 O6 H6 109.5 . . ?

_refine_diff_density_max         1.263
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.117

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Tb
_database_code_depnum_ccdc_archive 'CCDC 1055508'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H115 N24 O53 Tb'
_chemical_formula_weight         1963.49

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

_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                   21.629(2)
_cell_length_b                   12.2839(12)
_cell_length_c                   16.3898(17)
_cell_angle_alpha                90
_cell_angle_beta                 119.976(3)
_cell_angle_gamma                90
_cell_volume                     3772.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_F_000             2048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.068
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_T_max  0.843
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16198
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.434
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             3533
_reflns_number_gt                3224
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.465 -0.022 0.000 1179 468 ' '
2 1.000 0.000 0.500 117 36 ' '
3 0.500 0.500 0.500 117 36 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1351P)²+39.7782P] 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         3533
_refine_ls_number_parameters     240
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0848
_refine_ls_wR_factor_ref         0.2366
_refine_ls_wR_factor_gt          0.2266
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001

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 -0.0810(7) 0.6520(11) 0.4628(13) 0.075(4) Uani 0.5 1 d . . P . .
O2W O -0.0175(14) 0.5705(13) 0.3556(12) 0.121(9) Uani 0.5 1 d . . P . .
O3W O -0.1085(9) 0.5695(11) 0.3865(17) 0.146(11) Uani 0.5 1 d . . P . .
O4W O 0.0371(11) 0.3571(14) 0.4412(14) 0.093(5) Uani 0.5 1 d . . P . .
Tb1 Tb 0.0000 0.5000 0.5000 0.0414(3) Uani 1 4 d S T P . .
C1 C 0.1971(6) 0.1555(7) 0.5229(9) 0.069(3) Uani 1 1 d . . . . .
C2 C 0.2664(6) 0.0000 0.5868(8) 0.0431(17) Uani 1 2 d S T P . .
C3 C 0.2439(6) 0.0000 0.4908(8) 0.0431(17) Uani 1 2 d DS T P . .
C4 C 0.1531(5) 0.1401(7) 0.3550(7) 0.059(2) Uani 1 1 d . . . . .
H4A H 0.1821 0.1219 0.3262 0.071 Uiso 1 1 calc R U . . .
H4B H 0.1509 0.2196 0.3575 0.071 Uiso 1 1 calc R U . . .
C5 C 0.0206(7) 0.1543(7) 0.2716(8) 0.070(3) Uani 1 1 d . . . . .
C6 C 0.0676(8) 0.0000 0.2409(9) 0.055(3) Uani 1 2 d DS T P . .
C7 C -0.0149(9) 0.0000 0.1809(9) 0.058(3) Uani 1 2 d S T P . .
C8 C -0.1063(5) 0.1430(8) 0.1666(8) 0.069(3) Uani 1 1 d . . . . .
H8A H -0.1287 0.1312 0.0985 0.082 Uiso 1 1 calc R U . . .
H8B H -0.1024 0.2218 0.1774 0.082 Uiso 1 1 calc R U . . .
C9 C -0.1718(5) 0.1548(7) 0.2540(7) 0.060(2) Uani 1 1 d . . . . .
C10 C -0.1933(7) 0.0000 0.1597(9) 0.055(3) Uani 1 2 d S T P . .
C11 C -0.2433(5) 0.0000 0.2001(8) 0.052(3) Uani 1 2 d DS T P . .
C12 C 0.2602(6) 0.1420(8) 0.6972(8) 0.074(3) Uani 1 1 d . . . . .
H12A H 0.3113 0.1280 0.7385 0.088 Uiso 1 1 calc R U . . .
H12B H 0.2534 0.2211 0.6921 0.088 Uiso 1 1 calc R U . . .
C13 C 0.3480(9) 0.0000 0.6357(14) 0.109(8) Uani 1 2 d S T P . .
H13A H 0.3678 0.0000 0.7034 0.163 Uiso 1 2 calc R U P . .
H13B H 0.3639 -0.0645 0.6173 0.163 Uiso 0.5 1 calc R U P . .
H13C H 0.3639 0.0645 0.6173 0.163 Uiso 0.5 1 calc R U P . .
C14 C -0.0411(13) 0.0000 0.0759(12) 0.109(7) Uani 1 2 d S T P . .
H14A H -0.0256 0.0663 0.0592 0.164 Uiso 0.5 1 calc R U P . .
H14B H -0.0216 -0.0625 0.0603 0.164 Uiso 0.5 1 calc R U P . .
H14C H -0.0928 -0.0037 0.0412 0.164 Uiso 0.5 1 calc R U P . .
C15 C -0.2239(15) 0.0000 0.0619(15) 0.146(11) Uani 1 2 d S T P . .
H15A H -0.2510 0.0665 0.0364 0.220 Uiso 0.5 1 calc R U P . .
H15B H -0.1866 -0.0043 0.0456 0.220 Uiso 0.5 1 calc R U P . .
H15C H -0.2555 -0.0622 0.0357 0.220 Uiso 0.5 1 calc R U P . .
N1 N 0.2387(4) 0.0985(6) 0.6040(6) 0.060(2) Uani 1 1 d . . . . .
N2 N 0.1869(4) 0.0991(6) 0.4473(6) 0.062(2) Uani 1 1 d . . . . .
N3 N 0.0823(4) 0.0990(6) 0.2962(6) 0.0566(18) Uani 1 1 d . . . . .
N4 N -0.0368(5) 0.0987(6) 0.2102(6) 0.0595(19) Uani 1 1 d . . . . .
N5 N -0.1528(4) 0.0993(6) 0.1981(6) 0.0585(19) Uani 1 1 d . . . . .
N6 N -0.2225(4) 0.0982(6) 0.2599(5) 0.0556(18) Uani 1 1 d . . . . .
O1 O 0.1715(6) 0.2486(5) 0.5166(7) 0.096(3) Uani 1 1 d . . . . .
O2 O 0.0193(6) 0.2454(6) 0.3043(9) 0.117(4) Uani 1 1 d . . . . .
O3 O -0.1478(5) 0.2423(6) 0.2903(6) 0.081(2) Uani 1 1 d . . . . .
O4 O 0.2799(12) 0.0000 0.4363(16) 0.172 Uani 1 2 d DS TU P . .
H4 H 0.3057 -0.0548 0.4497 0.258 Uiso 0.5 1 calc R U P . .
O5 O 0.0962(13) 0.0000 0.1792(17) 0.179(10) Uani 1 2 d DS T P . .
H5 H 0.0858 -0.0581 0.1494 0.268 Uiso 0.5 1 calc R U P . .
O6 O -0.3195(5) 0.0000 0.1338(13) 0.157(8) Uani 1 2 d DS T P . .
H6 H -0.3264 0.0000 0.0793 0.235 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
O1W O4W 1.38(2) 5_566 ?
O1W O3W 1.48(3) . ?
O1W Tb1 2.420(12) . ?
O2W O4W 1.58(3) 6_565 ?
O2W O2W 1.73(3) 6_565 ?
O2W Tb1 2.366(14) . ?
O3W O3W 1.71(3) 6_565 ?
O3W Tb1 2.310(14) . ?
O4W O1W 1.38(2) 5_566 ?
O4W O2W 1.58(3) 6_565 ?
O4W Tb1 2.330(15) . ?
Tb1 O3W 2.310(14) 6_565 ?
Tb1 O3W 2.310(14) 2_556 ?
Tb1 O3W 2.310(14) 5_566 ?
Tb1 O4W 2.330(15) 5_566 ?
Tb1 O4W 2.330(15) 6_565 ?
Tb1 O4W 2.330(15) 2_556 ?
Tb1 O2W 2.366(14) 6_565 ?
Tb1 O2W 2.366(14) 2_556 ?
Tb1 O2W 2.366(14) 5_566 ?
C1 O1 1.253(13) . ?
C1 N2 1.338(13) . ?
C1 N1 1.368(14) . ?
C2 C3 1.396(16) . ?
C2 N1 1.439(9) . ?
C2 N1 1.439(9) 6 ?
C2 C13 1.53(2) . ?
C3 O4 1.449(2) . ?
C3 N2 1.622(11) 6 ?
C3 N2 1.622(11) . ?
C4 N2 1.405(13) . ?
C4 N3 1.433(12) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.247(12) . ?
C5 N4 1.332(14) . ?
C5 N3 1.366(14) . ?
C6 N3 1.453(10) . ?
C6 N3 1.453(10) 6 ?
C6 O5 1.425(9) . ?
C6 C7 1.55(2) . ?
C7 N4 1.467(10) 6 ?
C7 N4 1.467(10) . ?
C7 C14 1.52(2) . ?
C8 N4 1.412(13) . ?
C8 N5 1.443(12) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.213(12) . ?
C9 N6 1.342(13) . ?
C9 N5 1.360(13) . ?
C10 C15 1.40(2) . ?
C10 N5 1.450(10) 6 ?
C10 N5 1.450(10) . ?
C10 C11 1.526(19) . ?
C11 N6 1.475(10) . ?
C11 N6 1.475(10) 6 ?
C11 O6 1.451(2) . ?
C12 N6 1.422(13) 2_556 ?
C12 N1 1.458(14) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N6 C12 1.422(13) 2_556 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4W O1W O3W 131.7(14) 5_566 . ?
O4W O1W Tb1 69.6(8) 5_566 . ?
O3W O1W Tb1 67.7(7) . . ?
O4W O2W O2W 124.2(10) 6_565 6_565 ?
O4W O2W Tb1 69.1(8) 6_565 . ?
O2W O2W Tb1 68.5(4) 6_565 . ?
O1W O3W O3W 133.0(10) . 6_565 ?
O1W O3W Tb1 75.8(8) . . ?
O3W O3W Tb1 68.3(4) 6_565 . ?
O1W O4W O2W 147.4(14) 5_566 6_565 ?
O1W O4W Tb1 76.8(9) 5_566 . ?
O2W O4W Tb1 71.6(8) 6_565 . ?
O3W Tb1 O3W 180.0 6_565 2_556 ?
O3W Tb1 O3W 136.6(7) 6_565 5_566 ?
O3W Tb1 O3W 43.4(7) 2_556 5_566 ?
O3W Tb1 O3W 43.4(7) 6_565 . ?
O3W Tb1 O3W 136.6(7) 2_556 . ?
O3W Tb1 O3W 180.0 5_566 . ?
O3W Tb1 O4W 79.0(8) 6_565 . ?
O3W Tb1 O4W 101.0(8) 2_556 . ?
O3W Tb1 O4W 68.5(8) 5_566 . ?
O3W Tb1 O4W 111.5(8) . . ?
O3W Tb1 O4W 101.0(8) 6_565 5_566 ?
O3W Tb1 O4W 79.0(8) 2_556 5_566 ?
O3W Tb1 O4W 111.5(8) 5_566 5_566 ?
O3W Tb1 O4W 68.5(8) . 5_566 ?
O4W Tb1 O4W 180.0(9) . 5_566 ?
O3W Tb1 O4W 111.5(8) 6_565 6_565 ?
O3W Tb1 O4W 68.5(8) 2_556 6_565 ?
O3W Tb1 O4W 101.0(8) 5_566 6_565 ?
O3W Tb1 O4W 79.0(8) . 6_565 ?
O4W Tb1 O4W 97.8(10) . 6_565 ?
O4W Tb1 O4W 82.2(10) 5_566 6_565 ?
O3W Tb1 O4W 68.5(8) 6_565 2_556 ?
O3W Tb1 O4W 111.5(8) 2_556 2_556 ?
O3W Tb1 O4W 79.0(8) 5_566 2_556 ?
O3W Tb1 O4W 101.0(8) . 2_556 ?
O4W Tb1 O4W 82.2(10) . 2_556 ?
O4W Tb1 O4W 97.8(10) 5_566 2_556 ?
O4W Tb1 O4W 180.0(6) 6_565 2_556 ?
O3W Tb1 O2W 57.9(10) 6_565 6_565 ?
O3W Tb1 O2W 122.1(10) 2_556 6_565 ?
O3W Tb1 O2W 105.1(8) 5_566 6_565 ?
O3W Tb1 O2W 74.9(8) . 6_565 ?
O4W Tb1 O2W 39.3(7) . 6_565 ?
O4W Tb1 O2W 140.7(7) 5_566 6_565 ?
O4W Tb1 O2W 77.2(7) 6_565 6_565 ?
O4W Tb1 O2W 102.8(7) 2_556 6_565 ?
O3W Tb1 O2W 122.1(10) 6_565 2_556 ?
O3W Tb1 O2W 57.9(10) 2_556 2_556 ?
O3W Tb1 O2W 74.9(8) 5_566 2_556 ?
O3W Tb1 O2W 105.1(8) . 2_556 ?
O4W Tb1 O2W 140.7(7) . 2_556 ?
O4W Tb1 O2W 39.3(7) 5_566 2_556 ?
O4W Tb1 O2W 102.8(7) 6_565 2_556 ?
O4W Tb1 O2W 77.2(7) 2_556 2_556 ?
O2W Tb1 O2W 180.0 6_565 2_556 ?
O3W Tb1 O2W 105.1(8) 6_565 5_566 ?
O3W Tb1 O2W 74.9(8) 2_556 5_566 ?
O3W Tb1 O2W 57.9(10) 5_566 5_566 ?
O3W Tb1 O2W 122.1(10) . 5_566 ?
O4W Tb1 O2W 102.8(7) . 5_566 ?
O4W Tb1 O2W 77.2(7) 5_566 5_566 ?
O4W Tb1 O2W 140.7(7) 6_565 5_566 ?
O4W Tb1 O2W 39.3(7) 2_556 5_566 ?
O2W Tb1 O2W 137.1(7) 6_565 5_566 ?
O2W Tb1 O2W 42.9(7) 2_556 5_566 ?
O3W Tb1 O2W 74.9(8) 6_565 . ?
O3W Tb1 O2W 105.1(8) 2_556 . ?
O3W Tb1 O2W 122.1(10) 5_566 . ?
O3W Tb1 O2W 57.9(10) . . ?
O4W Tb1 O2W 77.2(7) . . ?
O4W Tb1 O2W 102.8(7) 5_566 . ?
O4W Tb1 O2W 39.3(7) 6_565 . ?
O4W Tb1 O2W 140.7(7) 2_556 . ?
O2W Tb1 O2W 42.9(7) 6_565 . ?
O2W Tb1 O2W 137.1(7) 2_556 . ?
O2W Tb1 O2W 180.0 5_566 . ?
O1 C1 N2 122.3(12) . . ?
O1 C1 N1 126.6(11) . . ?
N2 C1 N1 111.1(8) . . ?
C3 C2 N1 106.0(7) . . ?
C3 C2 N1 106.0(7) . 6 ?
N1 C2 N1 114.5(9) . 6 ?
C3 C2 C13 104.6(11) . . ?
N1 C2 C13 112.4(7) . . ?
N1 C2 C13 112.4(7) 6 . ?
C2 C3 O4 134.6(14) . . ?
C2 C3 N2 104.8(6) . 6 ?
O4 C3 N2 104.7(8) . 6 ?
C2 C3 N2 104.8(6) . . ?
O4 C3 N2 104.7(8) . . ?
N2 C3 N2 97.3(8) 6 . ?
N2 C4 N3 113.9(7) . . ?
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 124.8(11) . . ?
O2 C5 N3 123.2(11) . . ?
N4 C5 N3 111.9(8) . . ?
N3 C6 N3 113.6(10) . 6 ?
N3 C6 O5 113.9(8) . . ?
N3 C6 O5 113.9(8) 6 . ?
N3 C6 C7 102.7(7) . . ?
N3 C6 C7 102.7(7) 6 . ?
O5 C6 C7 108.6(14) . . ?
N4 C7 N4 111.4(10) 6 . ?
N4 C7 C14 111.8(8) 6 . ?
N4 C7 C14 111.8(8) . . ?
N4 C7 C6 104.5(8) 6 . ?
N4 C7 C6 104.5(8) . . ?
C14 C7 C6 112.3(13) . . ?
N4 C8 N5 115.5(8) . . ?
N4 C8 H8A 108.4 . . ?
N5 C8 H8A 108.4 . . ?
N4 C8 H8B 108.4 . . ?
N5 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
O3 C9 N6 126.1(10) . . ?
O3 C9 N5 125.1(10) . . ?
N6 C9 N5 108.8(8) . . ?
C15 C10 N5 109.7(9) . 6 ?
C15 C10 N5 109.7(9) . . ?
N5 C10 N5 114.6(10) 6 . ?
C15 C10 C11 117.8(16) . . ?
N5 C10 C11 102.5(7) 6 . ?
N5 C10 C11 102.5(7) . . ?
N6 C11 N6 109.7(9) . 6 ?
N6 C11 C10 103.9(6) . . ?
N6 C11 C10 103.9(6) 6 . ?
N6 C11 O6 110.7(7) . . ?
N6 C11 O6 110.7(7) 6 . ?
C10 C11 O6 117.4(13) . . ?
N6 C12 N1 114.7(8) 2_556 . ?
N6 C12 H12A 108.6 2_556 . ?
N1 C12 H12A 108.6 . . ?
N6 C12 H12B 108.6 2_556 . ?
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 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C2 112.1(9) . . ?
C1 N1 C12 122.8(8) . . ?
C2 N1 C12 124.6(9) . . ?
C1 N2 C4 124.6(8) . . ?
C1 N2 C3 104.1(8) . . ?
C4 N2 C3 128.0(8) . . ?
C5 N3 C4 125.5(8) . . ?
C5 N3 C6 110.8(9) . . ?
C4 N3 C6 122.8(8) . . ?
C5 N4 C8 122.7(8) . . ?
C5 N4 C7 109.8(9) . . ?
C8 N4 C7 126.1(10) . . ?
C9 N5 C8 123.7(8) . . ?
C9 N5 C10 113.1(9) . . ?
C8 N5 C10 122.3(9) . . ?
C9 N6 C12 122.1(8) . 2_556 ?
C9 N6 C11 111.4(9) . . ?
C12 N6 C11 125.3(9) 2_556 . ?
C3 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C11 O6 H6 109.5 . . ?

_refine_diff_density_max         2.795
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.169

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Tm
_database_code_depnum_ccdc_archive 'CCDC 1055509'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H118 N24 O53 Tm'
_chemical_formula_weight         1976.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.734(2)
_cell_length_b                   12.2110(12)
_cell_length_c                   16.448(3)
_cell_angle_alpha                90
_cell_angle_beta                 119.884(3)
_cell_angle_gamma                90
_cell_volume                     3784.8(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_F_000             2062
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.303
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.781
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15915
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_av_R_equivalents  0.0618
_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       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.428
_diffrn_reflns_theta_max         25.197
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             3530
_reflns_number_gt                3287
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 116 38 ' '
2 0.284 -0.022 0.500 1155 467 ' '
3 0.000 0.500 0.000 116 38 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1602P)²+25.6105P] 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         3530
_refine_ls_number_parameters     229
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0935
_refine_ls_wR_factor_ref         0.2556
_refine_ls_wR_factor_gt          0.2492
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_restrained_S_all      5.356
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001

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 0.5789(4) 0.6508(7) 1.0392(8) 0.083(3) Uani 0.5 1 d . . P . .
O2W O 0.4647(6) 0.3556(10) 1.0561(8) 0.137(3) Uani 0.5 1 d . . P . .
O3W O 0.5120(9) 0.5667(9) 1.1359(7) 0.190(6) Uani 0.5 1 d . . P . .
O4W O 0.6080(7) 0.5696(9) 1.0986(18) 0.233(14) Uani 0.5 1 d . . P . .
Tm1 Tm 0.5000 0.5000 1.0000 0.04053(11) Uani 1 4 d S T P . .
C1 C 0.6716(4) 0.1550(5) 1.2452(5) 0.070(2) Uani 1 1 d . . . . .
C2 C 0.6945(5) 0.0000 1.3397(6) 0.070(3) Uani 1 2 d S T P . .
C3 C 0.7417(3) 0.0000 1.2972(7) 0.075(4) Uani 1 2 d DS T P . .
C4 C 0.7592(4) 0.1425(6) 1.1957(5) 0.081(2) Uani 1 1 d . . . . .
H4A H 0.8098 0.1275 1.2366 0.097 Uiso 1 1 calc R U . . .
H4B H 0.7531 0.2222 1.1911 0.097 Uiso 1 1 calc R U . . .
C5 C 0.6960(3) 0.1565(6) 1.0237(5) 0.081 Uani 1 1 d . . . . .
C6 C 0.76988(15) 0.0000 1.09501(7) 0.082(3) Uani 1 2 d DS TU P . .
C7 C 0.74217(6) 0.0000 0.99008(7) 0.090 Uani 1 2 d DS TU P . .
C8 C 0.6524(3) 0.1402(6) 0.8547(5) 0.0805(18) Uani 1 1 d . . . . .
H8A H 0.6813 0.1226 0.8261 0.097 Uiso 1 1 calc R U . . .
H8B H 0.6502 0.2202 0.8577 0.097 Uiso 1 1 calc R U . . .
C9 C 0.5218(4) 0.1570(5) 0.7738(5) 0.077(2) Uani 1 1 d . . . . .
C10 C 0.5678(4) 0.0000 0.7422(6) 0.069(2) Uani 1 2 d S T P . .
C11 C 0.4826(5) 0.0000 0.6782(3) 0.075(3) Uani 1 2 d DS T P . .
C12 C 0.3947(4) 0.1444(6) 0.6664(5) 0.090 Uani 1 1 d . . . . .
H12A H 0.3725 0.1309 0.5988 0.108 Uiso 1 1 calc R U . . .
H12B H 0.3983 0.2239 0.6758 0.108 Uiso 1 1 calc R U . . .
C13 C 0.7246(10) 0.0000 1.4373(10) 0.152(9) Uani 1 2 d S T P . .
H13A H 0.7528 0.0657 1.4630 0.228 Uiso 0.5 1 calc R U P . .
H13B H 0.6872 -0.0017 1.4532 0.228 Uiso 1 2 calc R U P . .
H13C H 0.7546 -0.0640 1.4633 0.228 Uiso 0.5 1 calc R U P . .
C14 C 0.79907(6) 0.0000 0.96571(9) 0.090 Uani 1 2 d DS TU P . .
H14A H 0.8368 0.0489 1.0076 0.135 Uiso 0.5 1 calc R U P . .
H14B H 0.7800 0.0247 0.9015 0.135 Uiso 0.5 1 calc R U P . .
H14C H 0.8178 -0.0736 0.9720 0.135 Uiso 0.5 1 calc R U P . .
C15 C 0.6009(7) 0.0000 0.6856(9) 0.109(5) Uani 1 2 d S T P . .
H15A H 0.5904 -0.0682 0.6510 0.163 Uiso 0.5 1 calc R U P . .
H15B H 0.5829 0.0608 0.6419 0.163 Uiso 0.5 1 calc R U P . .
H15C H 0.6519 0.0074 0.7255 0.163 Uiso 0.5 1 calc R U P . .
N1 N 0.6513(3) 0.1007(5) 1.3007(4) 0.0775(19) Uani 1 1 d . . . . .
N2 N 0.7211(3) 0.0988(4) 1.2390(4) 0.0714(18) Uani 1 1 d . . . . .
N3 N 0.7379(3) 0.0999(5) 1.1035(4) 0.0779(17) Uani 1 1 d . . . . .
N4 N 0.6866(3) 0.0986(5) 0.9469(4) 0.0738(15) Uani 1 1 d . . . . .
N5 N 0.5819(3) 0.0996(4) 0.7950(4) 0.0759(16) Uani 1 1 d . . . . .
N6 N 0.4647(3) 0.0994(5) 0.7115(4) 0.0735(16) Uani 1 1 d . . . . .
O1 O 0.6479(3) 0.2443(4) 1.2080(4) 0.0904(19) Uani 1 1 d . . . . .
O2 O 0.6696(3) 0.2497(4) 1.0152(4) 0.0990(18) Uani 1 1 d . . . . .
O3 O 0.5184(4) 0.2466(4) 0.8032(5) 0.120(2) Uani 1 1 d . . . . .
O4 O 0.8155(3) 0.0000 1.3648(10) 0.210(9) Uani 1 2 d DS T P . .
H4 H 0.8390 -0.0006 1.3375 0.315 Uiso 1 2 calc R U P . .
O5 O 0.8467(6) 0.0000 1.1381(10) 0.228(10) Uani 1 2 d S T P . .
H5 H 0.8597 -0.0568 1.1232 0.342 Uiso 0.5 1 calc R U P . .
O6 O 0.4579(8) 0.0000 0.5800(4) 0.193(8) Uani 1 2 d DS T P . .
H6 H 0.4139 0.0000 0.5506 0.290 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
O1W O4W 1.31(2) . ?
O1W O2W 1.372(15) 5_667 ?
O1W Tm1 2.376(9) . ?
O2W O1W 1.372(15) 5_667 ?
O2W O3W 1.528(15) 6_565 ?
O2W Tm1 2.292(12) . ?
O3W O2W 1.528(15) 6_565 ?
O3W O3W 1.63(2) 6_565 ?
O3W Tm1 2.269(12) . ?
O4W O4W 1.70(2) 6_565 ?
O4W Tm1 2.250(12) . ?
Tm1 O4W 2.251(12) 5_667 ?
Tm1 O4W 2.251(12) 6_565 ?
Tm1 O4W 2.251(12) 2_657 ?
Tm1 O3W 2.269(12) 5_667 ?
Tm1 O3W 2.269(12) 6_565 ?
Tm1 O3W 2.269(12) 2_657 ?
Tm1 O2W 2.292(13) 5_667 ?
Tm1 O2W 2.292(13) 2_657 ?
Tm1 O2W 2.292(13) 6_565 ?
C1 O1 1.231(8) . ?
C1 N2 1.323(10) . ?
C1 N1 1.367(11) . ?
C2 C13 1.399(18) . ?
C2 N1 1.485(8) 6 ?
C2 N1 1.485(8) . ?
C2 C3 1.503(17) . ?
C3 N2 1.466(8) 6 ?
C3 N2 1.466(8) . ?
C3 O4 1.425(7) . ?
C4 N2 1.435(11) . ?
C4 N3 1.444(10) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.250(9) . ?
C5 N3 1.355(9) . ?
C5 N4 1.371(10) . ?
C6 N3 1.445(6) 6 ?
C6 N3 1.445(6) . ?
C6 O5 1.452(13) . ?
C6 C7 1.5185(13) . ?
C7 C14 1.4779(15) . ?
C7 N4 1.600(5) . ?
C7 N4 1.600(5) 6 ?
C8 N4 1.410(9) . ?
C8 N5 1.435(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.213(9) . ?
C9 N6 1.348(8) . ?
C9 N5 1.365(10) . ?
C10 C15 1.433(19) . ?
C10 N5 1.436(7) . ?
C10 N5 1.436(7) 6 ?
C10 C11 1.610(13) . ?
C11 N6 1.462(8) . ?
C11 N6 1.462(8) 6 ?
C11 O6 1.425(7) . ?
C12 N6 1.430(10) . ?
C12 N1 1.454(12) 2_657 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 C12 1.454(12) 2_657 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4W O1W O2W 127.5(12) . 5_667 ?
O4W O1W Tm1 68.3(6) . . ?
O2W O1W Tm1 69.6(6) 5_667 . ?
O1W O2W O3W 143.5(11) 5_667 6_565 ?
O1W O2W Tm1 76.3(7) 5_667 . ?
O3W O2W Tm1 69.6(7) 6_565 . ?
O2W O3W O3W 128.4(6) 6_565 6_565 ?
O2W O3W Tm1 71.3(6) 6_565 . ?
O3W O3W Tm1 68.9(3) 6_565 . ?
O1W O4W O4W 139.1(9) . 6_565 ?
O1W O4W Tm1 78.9(7) . . ?
O4W O4W Tm1 67.8(3) 6_565 . ?
O4W Tm1 O4W 180.0 . 5_667 ?
O4W Tm1 O4W 44.4(6) . 6_565 ?
O4W Tm1 O4W 135.6(6) 5_667 6_565 ?
O4W Tm1 O4W 135.6(6) . 2_657 ?
O4W Tm1 O4W 44.4(6) 5_667 2_657 ?
O4W Tm1 O4W 180.0 6_565 2_657 ?
O4W Tm1 O3W 114.4(9) . 5_667 ?
O4W Tm1 O3W 65.6(9) 5_667 5_667 ?
O4W Tm1 O3W 98.1(8) 6_565 5_667 ?
O4W Tm1 O3W 81.9(8) 2_657 5_667 ?
O4W Tm1 O3W 81.9(8) . 6_565 ?
O4W Tm1 O3W 98.1(8) 5_667 6_565 ?
O4W Tm1 O3W 65.6(9) 6_565 6_565 ?
O4W Tm1 O3W 114.4(9) 2_657 6_565 ?
O3W Tm1 O3W 137.9(6) 5_667 6_565 ?
O4W Tm1 O3W 98.1(8) . 2_657 ?
O4W Tm1 O3W 81.9(8) 5_667 2_657 ?
O4W Tm1 O3W 114.4(9) 6_565 2_657 ?
O4W Tm1 O3W 65.6(9) 2_657 2_657 ?
O3W Tm1 O3W 42.1(5) 5_667 2_657 ?
O3W Tm1 O3W 180.0 6_565 2_657 ?
O4W Tm1 O3W 65.6(9) . . ?
O4W Tm1 O3W 114.4(9) 5_667 . ?
O4W Tm1 O3W 81.9(8) 6_565 . ?
O4W Tm1 O3W 98.1(8) 2_657 . ?
O3W Tm1 O3W 180.0 5_667 . ?
O3W Tm1 O3W 42.1(5) 6_565 . ?
O3W Tm1 O3W 137.9(6) 2_657 . ?
O4W Tm1 O2W 64.0(7) . 5_667 ?
O4W Tm1 O2W 116.0(7) 5_667 5_667 ?
O4W Tm1 O2W 98.2(6) 6_565 5_667 ?
O4W Tm1 O2W 81.8(6) 2_657 5_667 ?
O3W Tm1 O2W 77.1(5) 5_667 5_667 ?
O3W Tm1 O2W 140.9(4) 6_565 5_667 ?
O3W Tm1 O2W 39.1(4) 2_657 5_667 ?
O3W Tm1 O2W 102.9(5) . 5_667 ?
O4W Tm1 O2W 98.2(6) . 2_657 ?
O4W Tm1 O2W 81.8(6) 5_667 2_657 ?
O4W Tm1 O2W 64.0(7) 6_565 2_657 ?
O4W Tm1 O2W 116.0(7) 2_657 2_657 ?
O3W Tm1 O2W 39.1(4) 5_667 2_657 ?
O3W Tm1 O2W 102.9(5) 6_565 2_657 ?
O3W Tm1 O2W 77.1(4) 2_657 2_657 ?
O3W Tm1 O2W 140.9(4) . 2_657 ?
O2W Tm1 O2W 100.6(7) 5_667 2_657 ?
O4W Tm1 O2W 81.8(6) . 6_565 ?
O4W Tm1 O2W 98.2(6) 5_667 6_565 ?
O4W Tm1 O2W 116.0(7) 6_565 6_565 ?
O4W Tm1 O2W 64.0(7) 2_657 6_565 ?
O3W Tm1 O2W 140.9(4) 5_667 6_565 ?
O3W Tm1 O2W 77.1(4) 6_565 6_565 ?
O3W Tm1 O2W 102.9(5) 2_657 6_565 ?
O3W Tm1 O2W 39.1(4) . 6_565 ?
O2W Tm1 O2W 79.4(7) 5_667 6_565 ?
O2W Tm1 O2W 180.0 2_657 6_565 ?
O4W Tm1 O2W 116.0(7) . . ?
O4W Tm1 O2W 64.0(7) 5_667 . ?
O4W Tm1 O2W 81.8(6) 6_565 . ?
O4W Tm1 O2W 98.2(6) 2_657 . ?
O3W Tm1 O2W 102.9(5) 5_667 . ?
O3W Tm1 O2W 39.1(4) 6_565 . ?
O3W Tm1 O2W 140.9(4) 2_657 . ?
O3W Tm1 O2W 77.1(5) . . ?
O2W Tm1 O2W 180.0 5_667 . ?
O2W Tm1 O2W 79.4(7) 2_657 . ?
O2W Tm1 O2W 100.6(7) 6_565 . ?
O1 C1 N2 125.2(8) . . ?
O1 C1 N1 124.5(8) . . ?
N2 C1 N1 110.3(6) . . ?
C13 C2 N1 109.2(8) . 6 ?
C13 C2 N1 109.2(7) . . ?
N1 C2 N1 111.9(7) 6 . ?
C13 C2 C3 119.7(12) . . ?
N1 C2 C3 103.3(6) 6 . ?
N1 C2 C3 103.3(6) . . ?
N2 C3 N2 110.9(8) 6 . ?
N2 C3 C2 104.3(5) 6 . ?
N2 C3 C2 104.3(5) . . ?
N2 C3 O4 111.6(5) 6 . ?
N2 C3 O4 111.6(6) . . ?
C2 C3 O4 113.7(11) . . ?
N2 C4 N3 115.1(6) . . ?
N2 C4 H4A 108.5 . . ?
N3 C4 H4A 108.5 . . ?
N2 C4 H4B 108.5 . . ?
N3 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N3 128.5(7) . . ?
O2 C5 N4 121.1(7) . . ?
N3 C5 N4 110.4(6) . . ?
N3 C6 N3 115.1(5) 6 . ?
N3 C6 O5 116.4(3) 6 . ?
N3 C6 O5 116.4(3) . . ?
N3 C6 C7 99.9(3) 6 . ?
N3 C6 C7 99.9(3) . . ?
O5 C6 C7 105.2(7) . . ?
C14 C7 C6 113.38(14) . . ?
C14 C7 N4 115.4(2) . . ?
C6 C7 N4 106.8(2) . . ?
C14 C7 N4 115.4(2) . 6 ?
C6 C7 N4 106.8(2) . 6 ?
N4 C7 N4 97.7(4) . 6 ?
N4 C8 N5 115.0(6) . . ?
N4 C8 H8A 108.5 . . ?
N5 C8 H8A 108.5 . . ?
N4 C8 H8B 108.5 . . ?
N5 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
O3 C9 N6 123.9(7) . . ?
O3 C9 N5 127.0(7) . . ?
N6 C9 N5 109.1(6) . . ?
C15 C10 N5 111.6(5) . . ?
C15 C10 N5 111.6(5) . 6 ?
N5 C10 N5 115.8(8) . 6 ?
C15 C10 C11 111.1(7) . . ?
N5 C10 C11 103.0(5) . . ?
N5 C10 C11 103.0(5) 6 . ?
N6 C11 N6 112.2(8) . 6 ?
N6 C11 O6 113.9(4) . . ?
N6 C11 O6 113.9(4) 6 . ?
N6 C11 C10 100.9(4) . . ?
N6 C11 C10 100.9(4) 6 . ?
O6 C11 C10 113.7(10) . . ?
N6 C12 N1 114.6(6) . 2_657 ?
N6 C12 H12A 108.6 . . ?
N1 C12 H12A 108.6 2_657 . ?
N6 C12 H12B 108.6 . . ?
N1 C12 H12B 108.6 2_657 . ?
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 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C12 125.5(6) . 2_657 ?
C1 N1 C2 110.2(8) . . ?
C12 N1 C2 123.1(8) 2_657 . ?
C1 N2 C4 122.5(6) . . ?
C1 N2 C3 111.8(7) . . ?
C4 N2 C3 124.5(7) . . ?
C5 N3 C6 117.4(6) . . ?
C5 N3 C4 122.8(6) . . ?
C6 N3 C4 119.2(5) . . ?
C5 N4 C8 124.2(6) . . ?
C5 N4 C7 104.2(4) . . ?
C8 N4 C7 128.7(5) . . ?
C9 N5 C8 123.8(6) . . ?
C9 N5 C10 113.1(6) . . ?
C8 N5 C10 122.6(6) . . ?
C9 N6 C12 122.2(6) . . ?
C9 N6 C11 113.7(6) . . ?
C12 N6 C11 122.5(6) . . ?
C3 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C11 O6 H6 109.5 . . ?

_refine_diff_density_max         8.459
_refine_diff_density_min         -3.105
_refine_diff_density_rms         0.228

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Yb
_database_code_depnum_ccdc_archive 'CCDC 1055510'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H111 N24 O51 Yb'
_chemical_formula_weight         1941.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.7930(13)
_cell_length_b                   12.1907(7)
_cell_length_c                   16.4222(9)
_cell_angle_alpha                90
_cell_angle_beta                 120.043(2)
_cell_angle_gamma                90
_cell_volume                     3776.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_F_000             2018
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    1.365
_shelx_estimated_absorpt_T_min   0.661
_shelx_estimated_absorpt_T_max   0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.701
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16766
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_av_R_equivalents  0.0611
_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       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.432
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3842
_reflns_number_gt                3523
_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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 116 29 ' '
2 0.784 -0.024 0.500 1118 438 ' '
3 0.500 0.500 0.000 116 29 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0825P)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         3842
_refine_ls_number_parameters     244
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.109
_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
O1W O 0.5775(4) 0.8518(6) 1.0379(8) 0.079(3) Uani 0.5 1 d . . P . .
O2W O 0.5145(9) 0.9297(7) 1.1385(8) 0.131(5) Uani 0.5 1 d . . P . .
O3W O 0.4679(8) 1.1453(8) 1.0599(10) 0.118(4) Uani 0.5 1 d . . P . .
O4W O 0.6068(6) 0.9315(8) 1.1064(13) 0.192(9) Uani 0.5 1 d . . P . .
Yb1 Yb 0.5000 1.0000 1.0000 0.04034(17) Uani 1 4 d S T P . .
C1 C -0.1697(3) 0.8450(4) 0.7545(4) 0.0582(13) Uani 1 1 d . . . . .
C2 C -0.2410(4) 1.0000 0.7030(5) 0.061(2) Uani 1 2 d S T P . .
C3 C -0.1927(4) 1.0000 0.6600(5) 0.0587(19) Uani 1 2 d S T P . .
C4 C -0.1049(3) 0.8554(5) 0.6663(5) 0.0734(17) Uani 1 1 d . . . . .
H4A H -0.1018 0.7758 0.6760 0.088 Uiso 1 1 calc R U . . .
H4B H -0.1270 0.8687 0.5986 0.088 Uiso 1 1 calc R U . . .
C5 C 0.0229(3) 0.8441(4) 0.7748(4) 0.0654(15) Uani 1 1 d . . . . .
C6 C -0.0161(5) 1.0000 0.6784(5) 0.0600(19) Uani 1 2 d DS T P . .
C7 C 0.0681(5) 1.0000 0.7422(6) 0.0609(19) Uani 1 2 d S T P . .
C8 C 0.1529(3) 0.8582(5) 0.8551(4) 0.0653(15) Uani 1 1 d . . . . .
H8A H 0.1815 0.8759 0.8260 0.078 Uiso 1 1 calc R U . . .
H8B H 0.1503 0.7781 0.8576 0.078 Uiso 1 1 calc R U . . .
C9 C 0.1968(3) 0.8430(5) 1.0254(5) 0.0638(14) Uani 1 1 d . . . . .
C10 C 0.2322(4) 1.0000 0.9817(6) 0.0534(18) Uani 1 2 d S T P . .
C11 C 0.2663(4) 1.0000 1.0877(6) 0.063(2) Uani 1 2 d DS T P . .
C12 C 0.2573(3) 0.8564(5) 1.1967(5) 0.0715(16) Uani 1 1 d . . . . .
H12A H 0.2492 0.7770 1.1906 0.086 Uiso 1 1 calc R U . . .
H12B H 0.3082 0.8684 1.2384 0.086 Uiso 1 1 calc R U . . .
C13 C -0.3178(5) 1.0000 0.6269(9) 0.116(4) Uani 1 2 d S T P . .
H13A H -0.3285 0.9323 0.5912 0.174 Uiso 0.5 1 calc R U P . .
H13B H -0.3475 1.0058 0.6551 0.174 Uiso 0.5 1 calc R U P . .
H13C H -0.3268 1.0619 0.5852 0.174 Uiso 0.5 1 calc R U P . .
C14 C 0.1023(6) 1.0000 0.6875(8) 0.087(3) Uani 1 2 d S T P . .
H14A H 0.0914 1.0677 0.6518 0.130 Uiso 0.5 1 calc R U P . .
H14B H 0.1532 0.9942 0.7289 0.130 Uiso 0.5 1 calc R U P . .
H14C H 0.0856 0.9381 0.6446 0.130 Uiso 0.5 1 calc R U P . .
C15 C 0.2842(8) 1.0000 0.9553(11) 0.132 Uani 1 2 d S T P . .
H15A H 0.3120 0.9332 0.9774 0.198 Uiso 0.5 1 calc R U P . .
H15B H 0.2617 1.0039 0.8873 0.198 Uiso 0.5 1 calc R U P . .
H15C H 0.3151 1.0629 0.9830 0.198 Uiso 0.5 1 calc R U P . .
N1 N -0.2206(2) 0.9014(4) 0.7597(3) 0.0592(11) Uani 1 1 d . . . . .
N2 N -0.1504(2) 0.8999(4) 0.6985(3) 0.0621(11) Uani 1 1 d . . . . .
N3 N -0.0345(3) 0.8996(4) 0.7117(3) 0.0623(12) Uani 1 1 d . . . . .
N4 N 0.0830(3) 0.9001(4) 0.7967(3) 0.0604(11) Uani 1 1 d . . . . .
N5 N 0.1884(2) 0.9005(4) 0.9502(4) 0.0611(11) Uani 1 1 d . . . . .
N6 N 0.2376(3) 0.9002(4) 1.1053(4) 0.0664(12) Uani 1 1 d . . . . .
O1 O -0.1459(3) 0.7555(3) 0.7903(3) 0.0832(13) Uani 1 1 d . . . . .
O2 O 0.0215(3) 0.7548(4) 0.8065(5) 0.113(2) Uani 1 1 d . . . . .
O3 O 0.1723(3) 0.7502(3) 1.0201(4) 0.0886(14) Uani 1 1 d . . . . .
O4 O -0.2238(9) 1.0000 0.5609(8) 0.232(8) Uani 1 2 d S T P . .
H4 H -0.1921 1.0014 0.5469 0.349 Uiso 1 2 calc R U P . .
O5 O -0.0415(8) 1.0000 0.5766(5) 0.186(5) Uani 1 2 d DS T P . .
H5 H -0.0855 0.9961 0.5469 0.278 Uiso 0.5 1 calc R U P . .
O6 O 0.3436(5) 1.0000 1.1360(8) 0.210(7) Uani 1 2 d DS T P . .
H6 H 0.3571 0.9591 1.1078 0.315 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
O1W O4W 1.378(17) . ?
O1W O3W 1.403(16) 5_677 ?
O1W Yb1 2.335(7) . ?
O2W O3W 1.490(18) 6_575 ?
O2W O2W 1.713(18) 6_575 ?
O2W Yb1 2.299(9) . ?
O3W O1W 1.403(16) 5_677 ?
O3W O2W 1.490(17) 6_575 ?
O3W Yb1 2.298(9) . ?
O4W O4W 1.669(19) 6_575 ?
O4W Yb1 2.257(10) . ?
Yb1 O4W 2.257(10) 6_575 ?
Yb1 O4W 2.257(10) 2_657 ?
Yb1 O4W 2.257(10) 5_677 ?
Yb1 O3W 2.298(9) 5_677 ?
Yb1 O3W 2.298(9) 6_575 ?
Yb1 O3W 2.298(9) 2_657 ?
Yb1 O2W 2.299(9) 6_575 ?
Yb1 O2W 2.299(9) 2_657 ?
Yb1 O2W 2.299(9) 5_677 ?
C1 O1 1.224(7) . ?
C1 N1 1.345(7) . ?
C1 N2 1.363(7) . ?
C2 N1 1.447(6) 6_575 ?
C2 N1 1.447(6) . ?
C2 C13 1.505(12) . ?
C2 C3 1.533(12) . ?
C3 O4 1.415(13) . ?
C3 N2 1.469(6) 6_575 ?
C3 N2 1.469(6) . ?
C4 N3 1.433(8) . ?
C4 N2 1.441(7) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 O2 1.213(7) . ?
C5 N3 1.341(8) . ?
C5 N4 1.357(7) . ?
C6 N3 1.476(6) 6_575 ?
C6 N3 1.476(6) . ?
C6 O5 1.474(8) . ?
C6 C7 1.593(12) . ?
C7 C14 1.426(11) . ?
C7 N4 1.449(6) . ?
C7 N4 1.449(6) 6_575 ?
C8 N4 1.426(7) . ?
C8 N5 1.447(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C9 O3 1.235(7) . ?
C9 N6 1.352(8) . ?
C9 N5 1.351(8) . ?
C10 C15 1.402(15) . ?
C10 N5 1.468(6) 6_575 ?
C10 N5 1.468(6) . ?
C10 C11 1.513(12) . ?
C11 N6 1.461(6) 6_575 ?
C11 N6 1.461(6) . ?
C11 O6 1.460(8) . ?
C12 N1 1.423(7) 2_557 ?
C12 N6 1.440(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 C12 1.423(7) 2_557 ?
O4 H4 0.8300 . ?
O5 H5 0.8300 . ?
O6 H6 0.8300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4W O1W O3W 133.6(9) . 5_677 ?
O4W O1W Yb1 69.5(5) . . ?
O3W O1W Yb1 70.9(5) 5_677 . ?
O3W O2W O2W 127.9(7) 6_575 6_575 ?
O3W O2W Yb1 71.1(5) 6_575 . ?
O2W O2W Yb1 68.1(2) 6_575 . ?
O1W O3W O2W 142.3(9) 5_677 6_575 ?
O1W O3W Yb1 73.8(5) 5_677 . ?
O2W O3W Yb1 71.1(5) 6_575 . ?
O1W O4W O4W 134.9(7) . 6_575 ?
O1W O4W Yb1 75.7(6) . . ?
O4W O4W Yb1 68.3(2) 6_575 . ?
O4W Yb1 O4W 43.4(5) . 6_575 ?
O4W Yb1 O4W 136.6(5) . 2_657 ?
O4W Yb1 O4W 180.0 6_575 2_657 ?
O4W Yb1 O4W 180.0 . 5_677 ?
O4W Yb1 O4W 136.6(5) 6_575 5_677 ?
O4W Yb1 O4W 43.4(5) 2_657 5_677 ?
O4W Yb1 O3W 111.7(6) . . ?
O4W Yb1 O3W 78.5(6) 6_575 . ?
O4W Yb1 O3W 101.5(6) 2_657 . ?
O4W Yb1 O3W 68.2(6) 5_677 . ?
O4W Yb1 O3W 68.3(6) . 5_677 ?
O4W Yb1 O3W 101.5(6) 6_575 5_677 ?
O4W Yb1 O3W 78.5(6) 2_657 5_677 ?
O4W Yb1 O3W 111.8(6) 5_677 5_677 ?
O3W Yb1 O3W 180.0 . 5_677 ?
O4W Yb1 O3W 78.5(6) . 6_575 ?
O4W Yb1 O3W 111.8(6) 6_575 6_575 ?
O4W Yb1 O3W 68.2(6) 2_657 6_575 ?
O4W Yb1 O3W 101.5(6) 5_677 6_575 ?
O3W Yb1 O3W 100.8(6) . 6_575 ?
O3W Yb1 O3W 79.2(6) 5_677 6_575 ?
O4W Yb1 O3W 101.5(6) . 2_657 ?
O4W Yb1 O3W 68.2(6) 6_575 2_657 ?
O4W Yb1 O3W 111.8(6) 2_657 2_657 ?
O4W Yb1 O3W 78.5(6) 5_677 2_657 ?
O3W Yb1 O3W 79.2(6) . 2_657 ?
O3W Yb1 O3W 100.8(6) 5_677 2_657 ?
O3W Yb1 O3W 180.0(3) 6_575 2_657 ?
O4W Yb1 O2W 78.1(6) . 6_575 ?
O4W Yb1 O2W 61.2(7) 6_575 6_575 ?
O4W Yb1 O2W 118.8(7) 2_657 6_575 ?
O4W Yb1 O2W 101.9(6) 5_677 6_575 ?
O3W Yb1 O2W 37.8(4) . 6_575 ?
O3W Yb1 O2W 142.2(4) 5_677 6_575 ?
O3W Yb1 O2W 77.5(4) 6_575 6_575 ?
O3W Yb1 O2W 102.5(4) 2_657 6_575 ?
O4W Yb1 O2W 101.9(6) . 2_657 ?
O4W Yb1 O2W 118.8(7) 6_575 2_657 ?
O4W Yb1 O2W 61.2(7) 2_657 2_657 ?
O4W Yb1 O2W 78.1(6) 5_677 2_657 ?
O3W Yb1 O2W 142.2(4) . 2_657 ?
O3W Yb1 O2W 37.8(4) 5_677 2_657 ?
O3W Yb1 O2W 102.5(4) 6_575 2_657 ?
O3W Yb1 O2W 77.5(4) 2_657 2_657 ?
O2W Yb1 O2W 180.0 6_575 2_657 ?
O4W Yb1 O2W 118.8(7) . 5_677 ?
O4W Yb1 O2W 101.9(6) 6_575 5_677 ?
O4W Yb1 O2W 78.1(6) 2_657 5_677 ?
O4W Yb1 O2W 61.2(7) 5_677 5_677 ?
O3W Yb1 O2W 102.5(4) . 5_677 ?
O3W Yb1 O2W 77.5(4) 5_677 5_677 ?
O3W Yb1 O2W 142.2(5) 6_575 5_677 ?
O3W Yb1 O2W 37.8(4) 2_657 5_677 ?
O2W Yb1 O2W 136.3(4) 6_575 5_677 ?
O2W Yb1 O2W 43.7(4) 2_657 5_677 ?
O4W Yb1 O2W 61.2(7) . . ?
O4W Yb1 O2W 78.1(6) 6_575 . ?
O4W Yb1 O2W 101.9(6) 2_657 . ?
O4W Yb1 O2W 118.8(7) 5_677 . ?
O3W Yb1 O2W 77.5(4) . . ?
O3W Yb1 O2W 102.5(4) 5_677 . ?
O3W Yb1 O2W 37.8(4) 6_575 . ?
O3W Yb1 O2W 142.2(5) 2_657 . ?
O2W Yb1 O2W 43.7(4) 6_575 . ?
O2W Yb1 O2W 136.3(4) 2_657 . ?
O2W Yb1 O2W 180.0 5_677 . ?
O1 C1 N1 126.2(6) . . ?
O1 C1 N2 124.2(6) . . ?
N1 C1 N2 109.6(5) . . ?
N1 C2 N1 112.3(6) 6_575 . ?
N1 C2 C13 113.0(4) 6_575 . ?
N1 C2 C13 113.0(4) . . ?
N1 C2 C3 103.6(4) 6_575 . ?
N1 C2 C3 103.6(4) . . ?
C13 C2 C3 110.6(8) . . ?
O4 C3 N2 109.3(6) . 6_575 ?
O4 C3 N2 109.3(6) . . ?
N2 C3 N2 112.4(6) 6_575 . ?
O4 C3 C2 119.0(10) . . ?
N2 C3 C2 103.3(4) 6_575 . ?
N2 C3 C2 103.3(4) . . ?
N3 C4 N2 114.9(5) . . ?
N3 C4 H4A 108.5 . . ?
N2 C4 H4A 108.5 . . ?
N3 C4 H4B 108.5 . . ?
N2 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 N3 124.8(6) . . ?
O2 C5 N4 124.4(6) . . ?
N3 C5 N4 110.8(5) . . ?
N3 C6 N3 112.0(6) 6_575 . ?
N3 C6 O5 113.8(5) 6_575 . ?
N3 C6 O5 113.8(5) . . ?
N3 C6 C7 101.1(4) 6_575 . ?
N3 C6 C7 101.1(4) . . ?
O5 C6 C7 113.6(8) . . ?
C14 C7 N4 111.3(4) . . ?
C14 C7 N4 111.3(4) . 6_575 ?
N4 C7 N4 114.4(6) . 6_575 ?
C14 C7 C6 112.3(7) . . ?
N4 C7 C6 103.6(4) . . ?
N4 C7 C6 103.6(4) 6_575 . ?
N4 C8 N5 114.3(4) . . ?
N4 C8 H8A 108.7 . . ?
N5 C8 H8A 108.7 . . ?
N4 C8 H8B 108.7 . . ?
N5 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O3 C9 N6 126.2(6) . . ?
O3 C9 N5 123.7(6) . . ?
N6 C9 N5 110.0(5) . . ?
C15 C10 N5 112.0(5) . 6_575 ?
C15 C10 N5 112.0(5) . . ?
N5 C10 N5 111.4(6) 6_575 . ?
C15 C10 C11 110.4(9) . . ?
N5 C10 C11 105.3(4) 6_575 . ?
N5 C10 C11 105.3(4) . . ?
N6 C11 N6 112.8(6) 6_575 . ?
N6 C11 C10 102.4(4) 6_575 . ?
N6 C11 C10 102.4(4) . . ?
N6 C11 O6 112.6(5) 6_575 . ?
N6 C11 O6 112.6(5) . . ?
C10 C11 O6 113.2(8) . . ?
N1 C12 N6 115.6(5) 2_557 . ?
N1 C12 H12A 108.4 2_557 . ?
N6 C12 H12A 108.4 . . ?
N1 C12 H12B 108.4 2_557 . ?
N6 C12 H12B 108.4 . . ?
H12A C12 H12B 107.4 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C1 N1 C12 121.6(5) . 2_557 ?
C1 N1 C2 112.5(5) . . ?
C12 N1 C2 125.1(6) 2_557 . ?
C1 N2 C4 124.3(5) . . ?
C1 N2 C3 111.0(5) . . ?
C4 N2 C3 123.6(5) . . ?
C5 N3 C4 123.6(5) . . ?
C5 N3 C6 112.6(5) . . ?
C4 N3 C6 122.5(6) . . ?
C5 N4 C8 124.2(5) . . ?
C5 N4 C7 111.7(5) . . ?
C8 N4 C7 123.4(5) . . ?
C9 N5 C8 123.9(5) . . ?
C9 N5 C10 109.8(5) . . ?
C8 N5 C10 125.2(5) . . ?
C9 N6 C12 121.9(5) . . ?
C9 N6 C11 112.1(6) . . ?
C12 N6 C11 125.5(6) . . ?
C3 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C11 O6 H6 109.5 . . ?

_refine_diff_density_max         0.856
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.098

_shelxl_version_number           2014/6

