# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_mo_d8v4660_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc2747g3
_database_code_depnum_ccdc_archive 'CCDC 2059654'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.13667729.v1 2021
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-01-29 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_mo_d8v4660_0m_a     
;
PROBLEM: D-H Without Acceptor       O13      --H13B     .     Please Check
RESPONSE: Disordered water, discussed in _refine_special_details.
;
# Added during the CSD deposition process: Friday 29 January 2021 01:11 PM
# end Validation Reply Form

_audit_creation_date             2021-01-28
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H45 Gd2 N10 O9, N O3, 2.5(H2 O)'
_chemical_formula_sum            'C39 H50 Gd2 N11 O14.50'
_chemical_formula_weight         1219.40
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-x, -y, z+1/2'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   17.6388(4)
_cell_length_b                   17.6388(4)
_cell_length_c                   29.2421(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9098.0(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.267
_cell_measurement_theta_min      2.388
_shelx_estimated_absorpt_T_max   0.842
_shelx_estimated_absorpt_T_min   0.510
_exptl_absorpt_coefficient_mu    2.969
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1066 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.8245.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4840
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.1310
0.00 0.00 1.00 0.1260
-1.00 -1.00 0.00 0.0210
1.00 1.00 0.00 0.0300
1.00 -1.00 0.00 0.0500
-1.00 1.00 0.00 0.0070

_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            153158
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.873
_diffrn_reflns_theta_min         1.809
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10100
_reflns_number_total             10847
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 
;
 Flack x determined using 4263 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.554
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+9.8797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0680
_refine_special_details          
;
The nitrate counterion and one water of crystallization were modelled as disordered over two sites with geometric and displacement ellipsoid restraints used.  In all cases water H atoms were identified from difference peaks which corresponded with likely hydrogen bonding interactions.  Water H atoms were refined using a riding model with geometric restraints.  One of the water molecules lies on a special position, hence a fractional value in the chemical formula.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

420_ALERT_2_B D-H Without Acceptor       O13      --H13B     .     Please Check

Disordered water, discussed above

#===============================================================================
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .        O13 Check
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .       O13A Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .        O13 Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .       O13A Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .        O13 Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .       O13A Check

AFIX 1 used to control H atoms on this disordered water.

213_ALERT_2_C Atom C13             has ADP max/min Ratio .....        3.6 prolat
213_ALERT_2_C Atom C31             has ADP max/min Ratio .....        3.5 prolat
218_ALERT_3_C Constrained U(ij) Components(s) for O13        .          6 Check
218_ALERT_3_C Constrained U(ij) Components(s) for O13A       .          6 Check

See above

220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.5 Ratio
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O4 Check
260_ALERT_2_C Large Average Ueq of Residue Including       O10      0.110 Check
342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00918 Ang.
601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         81 Ang**3
911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         10 Report
976_ALERT_2_C Check Calcd Resid. Dens.  0.62A   From O5             -0.46 eA-3
976_ALERT_2_C Check Calcd Resid. Dens.  0.57A   From O15            -0.43 eA-3
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-Gd1 = O2-Gd2 = O2-C10
 0.84 with sigma of 0.02
 O14-H14A = O16-H16E = O16-H16D = O15-H15
 0.84 with sigma of 0.02
 O13A-H13D = O13A-H13C
 0.84 with sigma of 0.02
 O13-H13A
 0.84 with sigma of 0.02
 H13B-O13
 0.84 with sigma of 0.02
 H16E-H16D_$2
 1.35 with sigma of 0.04
 H15_$1-H15 = H14A-H14A_$2 = H16E-H16D
 1.35 with sigma of 0.04
 H13D-H13C
 1.35 with sigma of 0.04
 H13A-H13B
 1.35 with sigma of 0.04
 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim
O12-N11
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O10, O11, O12, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10A, O11A, O12A, N11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, O6, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, O11, O12, N11}
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, O11A, O12A, N11A}
5. Others
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5)
 N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5)
6.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O15, H15, O16, H16D, H16E
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C21(H21), C23(H23), C26(H26), C27(H27)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.85672(2) 0.39536(2) 0.60332(2) 0.01821(6) Uani 1 1 d D . . . .
Gd2 Gd 0.95042(2) 0.31748(2) 0.50870(2) 0.01999(7) Uani 1 1 d D . . . .
O1 O 0.8235(2) 0.3517(2) 0.53089(12) 0.0207(7) Uani 1 1 d . . . . .
O2 O 0.9152(2) 0.2791(2) 0.58075(12) 0.0243(8) Uani 1 1 d D . . . .
O3 O 0.9626(2) 0.4303(2) 0.55465(14) 0.0264(9) Uani 1 1 d . . . . .
O4 O 0.8246(3) 0.5130(4) 0.5497(2) 0.0559(15) Uani 1 1 d . . . . .
O5 O 0.7383(3) 0.4659(3) 0.59065(16) 0.0421(11) Uani 1 1 d . . . . .
O6 O 0.7070(3) 0.5526(3) 0.5399(2) 0.0577(16) Uani 1 1 d . . . A 1
O7 O 1.0750(3) 0.3128(3) 0.56544(15) 0.0342(10) Uani 1 1 d D . . . .
O8 O 1.0457(3) 0.2163(2) 0.52363(13) 0.0276(8) Uani 1 1 d D . . . .
O9 O 1.1342(4) 0.2059(4) 0.57554(19) 0.0587(17) Uani 1 1 d D . . . .
N10 N 1.0868(3) 0.2455(3) 0.55559(17) 0.0350(13) Uani 1 1 d D . . . .
N1 N 0.7446(3) 0.3160(3) 0.61604(14) 0.0211(9) Uani 1 1 d . . . . .
N2 N 0.8780(3) 0.3730(3) 0.44313(15) 0.0242(10) Uani 1 1 d . . . . .
N3 N 0.9265(3) 0.3386(4) 0.66855(16) 0.0315(13) Uani 1 1 d . . . . .
N4 N 0.8947(3) 0.1921(3) 0.49714(16) 0.0257(10) Uani 1 1 d . . . . .
N5 N 0.8960(3) 0.5188(3) 0.63627(18) 0.0343(13) Uani 1 1 d . . . . .
N6 N 1.0614(3) 0.3797(3) 0.47322(16) 0.0268(11) Uani 1 1 d . . . . .
N7 N 0.7951(3) 0.4224(3) 0.68447(16) 0.0283(11) Uani 1 1 d . . . . .
N8 N 0.9874(3) 0.2614(3) 0.42684(15) 0.0276(11) Uani 1 1 d . . . . .
N9 N 0.7548(3) 0.5122(5) 0.5618(2) 0.0473(15) Uani 1 1 d . . . . .
C1 C 0.7558(3) 0.3470(3) 0.51291(18) 0.0207(11) Uani 1 1 d . . . . .
C2 C 0.6915(3) 0.3251(3) 0.53877(18) 0.0242(11) Uani 1 1 d . . . . .
C3 C 0.6200(3) 0.3251(4) 0.5181(2) 0.0275(13) Uani 1 1 d . . . . .
H3 H 0.577230 0.310571 0.535810 0.033 Uiso 1 1 calc R U . . .
C4 C 0.6088(4) 0.3455(4) 0.4725(2) 0.0316(13) Uani 1 1 d . . . . .
C5 C 0.6717(4) 0.3631(3) 0.4472(2) 0.0281(13) Uani 1 1 d . . . . .
H5 H 0.665476 0.376019 0.415857 0.034 Uiso 1 1 calc R U . . .
C6 C 0.7445(3) 0.3626(3) 0.46569(18) 0.0223(11) Uani 1 1 d . . . . .
C7 C 0.5294(4) 0.3464(5) 0.4526(2) 0.0430(18) Uani 1 1 d . . . . .
H7A H 0.514667 0.294760 0.443985 0.064 Uiso 1 1 calc R U . . .
H7B H 0.528263 0.379100 0.425555 0.064 Uiso 1 1 calc R U . . .
H7C H 0.493803 0.365879 0.475550 0.064 Uiso 1 1 calc R U . . .
C8 C 0.6912(3) 0.3056(3) 0.5873(2) 0.0238(11) Uani 1 1 d . . . . .
H8 H 0.646227 0.282756 0.598780 0.029 Uiso 1 1 calc R U . . .
C9 C 0.8067(4) 0.3788(3) 0.43458(18) 0.0264(13) Uani 1 1 d . . . . .
H9 H 0.793311 0.395402 0.404755 0.032 Uiso 1 1 calc R U . . .
C10 C 0.9213(3) 0.2114(3) 0.6000(2) 0.0254(12) Uani 1 1 d D . . . .
C11 C 0.9384(3) 0.2044(4) 0.6477(2) 0.0336(15) Uani 1 1 d . . . . .
C12 C 0.9498(4) 0.1333(5) 0.6679(2) 0.0414(18) Uani 1 1 d . . . . .
H12 H 0.963989 0.130905 0.699173 0.050 Uiso 1 1 calc R U . . .
C13 C 0.9412(4) 0.0673(5) 0.6439(3) 0.049(2) Uani 1 1 d . . . . .
C14 C 0.9215(4) 0.0727(4) 0.5974(3) 0.0372(17) Uani 1 1 d . . . . .
H14 H 0.914974 0.027387 0.580324 0.045 Uiso 1 1 calc R U . . .
C15 C 0.9112(3) 0.1430(4) 0.5752(2) 0.0280(13) Uani 1 1 d . . . . .
C16 C 0.9527(5) -0.0107(6) 0.6644(4) 0.073(3) Uani 1 1 d . . . . .
H16A H 0.992183 -0.037620 0.647314 0.110 Uiso 1 1 calc R U . . .
H16B H 0.905158 -0.039319 0.662756 0.110 Uiso 1 1 calc R U . . .
H16C H 0.968226 -0.005642 0.696448 0.110 Uiso 1 1 calc R U . . .
C17 C 0.9440(3) 0.2699(5) 0.67756(19) 0.0370(17) Uani 1 1 d . . . . .
H17 H 0.962924 0.260528 0.707443 0.044 Uiso 1 1 calc R U . . .
C18 C 0.8918(4) 0.1386(3) 0.5266(2) 0.0302(13) Uani 1 1 d . . . . .
H18 H 0.875273 0.090667 0.515706 0.036 Uiso 1 1 calc R U . . .
C19 C 1.0089(3) 0.4893(3) 0.5534(2) 0.0224(11) Uani 1 1 d . . . . .
C20 C 0.9972(3) 0.5551(3) 0.5817(2) 0.0268(12) Uani 1 1 d . . . . .
C21 C 1.0458(3) 0.6173(3) 0.5784(2) 0.0274(12) Uani 1 1 d . . . . .
H21 H 1.035238 0.660635 0.596560 0.033 Uiso 1 1 calc R U . . .
C22 C 1.1087(3) 0.6192(4) 0.5500(2) 0.0291(13) Uani 1 1 d . . . . .
C23 C 1.1216(3) 0.5558(4) 0.5245(2) 0.0259(12) Uani 1 1 d . . . . .
H23 H 1.165562 0.554736 0.505747 0.031 Uiso 1 1 calc R U . . .
C24 C 1.0740(3) 0.4918(3) 0.52407(19) 0.0223(11) Uani 1 1 d . . . . .
C25 C 1.1563(4) 0.6907(5) 0.5471(3) 0.0443(18) Uani 1 1 d . . . . .
H25A H 1.125517 0.732081 0.534660 0.067 Uiso 1 1 calc R U . . .
H25B H 1.199868 0.681657 0.527008 0.067 Uiso 1 1 calc R U . . .
H25C H 1.174258 0.704379 0.577689 0.067 Uiso 1 1 calc R U . . .
C26 C 0.9419(4) 0.5649(4) 0.6181(2) 0.0346(15) Uani 1 1 d . . . . .
H26 H 0.939913 0.614756 0.630312 0.042 Uiso 1 1 calc R U . . .
C27 C 1.0969(3) 0.4376(3) 0.48928(19) 0.0254(11) Uani 1 1 d . . . . .
H27 H 1.145639 0.446201 0.476437 0.030 Uiso 1 1 calc R U . . .
C28 C 0.7281(3) 0.3031(4) 0.66485(18) 0.0250(12) Uani 1 1 d . . . . .
H28A H 0.769172 0.273091 0.679136 0.030 Uiso 1 1 calc R U . . .
H28B H 0.679874 0.274892 0.668300 0.030 Uiso 1 1 calc R U . . .
C29 C 0.7221(3) 0.3801(4) 0.68754(19) 0.0263(13) Uani 1 1 d . . . . .
H29A H 0.681507 0.409888 0.672525 0.032 Uiso 1 1 calc R U . . .
H29B H 0.708083 0.373472 0.720081 0.032 Uiso 1 1 calc R U . . .
C30 C 0.9284(4) 0.3913(6) 0.7073(2) 0.0449(19) Uani 1 1 d . . . . .
H30A H 0.949061 0.441046 0.697712 0.054 Uiso 1 1 calc R U . . .
H30B H 0.960190 0.370938 0.732295 0.054 Uiso 1 1 calc R U . . .
C31 C 0.8451(3) 0.3995(5) 0.72302(18) 0.0367(16) Uani 1 1 d . . . . .
H31A H 0.827298 0.350551 0.735661 0.044 Uiso 1 1 calc R U . . .
H31B H 0.842051 0.437943 0.747608 0.044 Uiso 1 1 calc R U . . .
C32 C 0.8538(4) 0.5491(5) 0.6765(3) 0.048(2) Uani 1 1 d . . . . .
H32A H 0.840865 0.602894 0.670940 0.058 Uiso 1 1 calc R U . . .
H32B H 0.886780 0.546742 0.703850 0.058 Uiso 1 1 calc R U . . .
C33 C 0.7810(4) 0.5044(4) 0.6857(2) 0.0348(16) Uani 1 1 d . . . . .
H33A H 0.760687 0.518567 0.716132 0.042 Uiso 1 1 calc R U . . .
H33B H 0.742468 0.517725 0.662461 0.042 Uiso 1 1 calc R U . . .
C34 C 0.9277(4) 0.3842(4) 0.40317(19) 0.0326(14) Uani 1 1 d . . . . .
H34A H 0.971772 0.416153 0.411448 0.039 Uiso 1 1 calc R U . . .
H34B H 0.899631 0.409230 0.378063 0.039 Uiso 1 1 calc R U . . .
C35 C 0.9539(4) 0.3057(4) 0.38855(19) 0.0357(15) Uani 1 1 d . . . . .
H35A H 0.910082 0.277450 0.375946 0.043 Uiso 1 1 calc R U . . .
H35B H 0.992006 0.310879 0.363914 0.043 Uiso 1 1 calc R U . . .
C36 C 0.8857(4) 0.1714(4) 0.4488(2) 0.0351(15) Uani 1 1 d . . . . .
H36A H 0.847028 0.204202 0.434313 0.042 Uiso 1 1 calc R U . . .
H36B H 0.868741 0.118053 0.446289 0.042 Uiso 1 1 calc R U . . .
C37 C 0.9614(4) 0.1814(4) 0.4251(2) 0.0358(15) Uani 1 1 d . . . . .
H37A H 0.999674 0.148635 0.440076 0.043 Uiso 1 1 calc R U . . .
H37B H 0.956859 0.165293 0.392840 0.043 Uiso 1 1 calc R U . . .
C38 C 1.0999(4) 0.3445(4) 0.4336(2) 0.0349(15) Uani 1 1 d . . . . .
H38A H 1.155162 0.342547 0.439437 0.042 Uiso 1 1 calc R U . . .
H38B H 1.091420 0.376113 0.406082 0.042 Uiso 1 1 calc R U . . .
C39 C 1.0704(4) 0.2644(4) 0.4248(2) 0.0331(15) Uani 1 1 d . . . . .
H39A H 1.087527 0.247234 0.394292 0.040 Uiso 1 1 calc R U . . .
H39B H 1.091791 0.229484 0.447939 0.040 Uiso 1 1 calc R U . . .
O10 O 0.5386(11) 0.2962(11) 0.7091(5) 0.107(6) Uani 0.5 1 d D . P B 1
O11 O 0.5257(13) 0.2658(11) 0.6380(7) 0.166(12) Uani 0.5 1 d D . P B 1
O12 O 0.5102(13) 0.3784(9) 0.6611(6) 0.123(8) Uani 0.5 1 d D . P B 1
N11 N 0.5231(6) 0.3117(7) 0.6703(4) 0.047(3) Uani 0.5 1 d D . P B 1
O10A O 0.4287(11) 0.2905(8) 0.5491(4) 0.091(6) Uani 0.5 1 d D . P C 2
O11A O 0.5100(7) 0.2446(10) 0.5938(7) 0.114(7) Uani 0.5 1 d D . P C 2
O12A O 0.4237(14) 0.3174(10) 0.6196(6) 0.150(10) Uani 0.5 1 d D . P C 2
N11A N 0.4532(6) 0.2841(6) 0.5878(3) 0.035(2) Uani 0.5 1 d D . P C 2
O13 O 0.437800 0.264370 0.561150 0.092 Uani 0.5 1 d D . P D 1
H13A H 0.435470 0.294050 0.589850 0.110 Uiso 0.5 1 d D U P E 1
H13B H 0.402240 0.305990 0.546630 0.110 Uiso 0.5 1 d D U P F 1
O13A O 0.532020 0.302410 0.706160 0.043 Uani 0.5 1 d D . P G 2
H13C H 0.535730 0.347780 0.715580 0.051 Uiso 0.5 1 d D U P H 2
H13D H 0.521250 0.308890 0.677430 0.051 Uiso 0.5 1 d D U P I 2
O14 O 1.060260 0.060260 0.500000 0.045 Uani 1 2 d DS T P . .
H14A H 1.061250 0.100540 0.515750 0.054 Uiso 1 1 d D U . . .
O15 O 0.798350 0.201650 0.750000 0.062 Uani 1 2 d DS T P . .
H15 H 0.796640 0.154710 0.739500 0.074 Uiso 1 1 d D U . . .
O16 O 0.949400 -0.050600 0.500000 0.053 Uani 1 2 d DS T P . .
H16D H 0.919680 -0.043180 0.478650 0.064 Uiso 0.5 1 d D U P . .
H16E H 0.982770 -0.017230 0.500000 0.064 Uiso 1 2 d DS 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
Gd1 Gd2 3.5035(4) . ?
Gd1 O1 2.329(3) . ?
Gd1 O2 2.388(4) . ?
Gd1 O3 2.428(4) . ?
Gd1 O4 2.663(6) . ?
Gd1 O5 2.460(5) . ?
Gd1 N1 2.452(5) . ?
Gd1 N3 2.482(5) . ?
Gd1 N5 2.479(5) . ?
Gd1 N7 2.653(5) . ?
Gd2 O1 2.408(4) . ?
Gd2 O2 2.298(4) . ?
Gd2 O3 2.411(4) . ?
Gd2 O7 2.754(5) . ?
Gd2 O8 2.490(4) . ?
Gd2 N2 2.503(5) . ?
Gd2 N4 2.443(5) . ?
Gd2 N6 2.472(5) . ?
Gd2 N8 2.671(4) . ?
O1 C1 1.307(7) . ?
O2 C10 1.326(7) . ?
O3 C19 1.324(7) . ?
O4 N9 1.282(8) . ?
O5 N9 1.209(9) . ?
O6 N9 1.276(9) . ?
O7 N10 1.240(7) . ?
O8 N10 1.290(7) . ?
O9 N10 1.235(7) . ?
N1 C8 1.275(7) . ?
N1 C28 1.475(7) . ?
N2 C9 1.286(8) . ?
N2 C34 1.475(7) . ?
N3 C17 1.277(10) . ?
N3 C30 1.466(9) . ?
N4 C18 1.279(8) . ?
N4 C36 1.467(8) . ?
N5 C26 1.266(8) . ?
N5 C32 1.491(8) . ?
N6 C27 1.287(8) . ?
N6 C38 1.479(7) . ?
N7 C29 1.492(7) . ?
N7 C31 1.488(8) . ?
N7 C33 1.468(9) . ?
N8 C35 1.488(7) . ?
N8 C37 1.483(9) . ?
N8 C39 1.466(9) . ?
C1 C2 1.417(8) . ?
C1 C6 1.422(7) . ?
C2 C3 1.400(8) . ?
C2 C8 1.461(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.395(8) . ?
C4 C5 1.369(9) . ?
C4 C7 1.517(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(9) . ?
C6 C9 1.454(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.430(8) . ?
C10 C15 1.420(9) . ?
C11 C12 1.400(10) . ?
C11 C17 1.452(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.368(13) . ?
C13 C14 1.406(12) . ?
C13 C16 1.516(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.411(8) . ?
C15 C18 1.464(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.440(8) . ?
C19 C24 1.433(8) . ?
C20 C21 1.397(8) . ?
C20 C26 1.452(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(9) . ?
C22 C23 1.364(9) . ?
C22 C25 1.516(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.406(8) . ?
C24 C27 1.454(8) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.516(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.546(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.530(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.521(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.516(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.528(10) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
O10 N11 1.199(14) . ?
O11 N11 1.245(14) . ?
O12 N11 1.229(14) . ?
O10A N11A 1.217(12) . ?
O11A N11A 1.235(13) . ?
O12A N11A 1.215(13) . ?
O13 H13A 0.9900 . ?
O13 H13A 0.9900 . ?
O13 H13B 1.0548 . ?
O13A H13C 0.8489 . ?
O13A H13D 0.8689 . ?
O14 H14A 0.8469 7_646 ?
O14 H14A 0.8469 . ?
O15 H15 0.8836 8_666 ?
O15 H15 0.8836 . ?
O16 H16D 0.8257 . ?
O16 H16D 0.8257 7_646 ?
O16 H16E 0.8324 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 Gd2 43.18(10) . . ?
O1 Gd1 O2 64.75(13) . . ?
O1 Gd1 O3 75.20(14) . . ?
O1 Gd1 O4 70.64(17) . . ?
O1 Gd1 O5 79.44(14) . . ?
O1 Gd1 N1 75.28(14) . . ?
O1 Gd1 N3 133.66(17) . . ?
O1 Gd1 N5 135.59(17) . . ?
O1 Gd1 N7 140.33(14) . . ?
O2 Gd1 Gd2 40.65(9) . . ?
O2 Gd1 O3 73.94(13) . . ?
O2 Gd1 O4 126.74(16) . . ?
O2 Gd1 O5 139.45(15) . . ?
O2 Gd1 N1 84.27(15) . . ?
O2 Gd1 N3 69.60(16) . . ?
O2 Gd1 N5 137.76(17) . . ?
O2 Gd1 N7 125.35(15) . . ?
O3 Gd1 Gd2 43.41(9) . . ?
O3 Gd1 O4 67.68(16) . . ?
O3 Gd1 O5 115.89(16) . . ?
O3 Gd1 N1 148.71(14) . . ?
O3 Gd1 N3 99.86(15) . . ?
O3 Gd1 N5 77.88(15) . . ?
O3 Gd1 N7 142.54(15) . . ?
O4 Gd1 Gd2 86.59(13) . . ?
O5 Gd1 Gd2 118.69(11) . . ?
O5 Gd1 O4 48.42(18) . . ?
O5 Gd1 N3 137.85(16) . . ?
O5 Gd1 N5 81.46(18) . . ?
O5 Gd1 N7 72.29(16) . . ?
N1 Gd1 Gd2 106.05(11) . . ?
N1 Gd1 O4 111.30(17) . . ?
N1 Gd1 O5 68.09(17) . . ?
N1 Gd1 N3 93.04(17) . . ?
N1 Gd1 N5 131.91(16) . . ?
N1 Gd1 N7 68.69(15) . . ?
N3 Gd1 Gd2 102.40(12) . . ?
N3 Gd1 O4 150.8(2) . . ?
N3 Gd1 N7 65.70(16) . . ?
N5 Gd1 Gd2 121.29(12) . . ?
N5 Gd1 O4 66.7(2) . . ?
N5 Gd1 N3 85.2(2) . . ?
N5 Gd1 N7 66.98(17) . . ?
N7 Gd1 Gd2 165.95(13) . . ?
N7 Gd1 O4 107.44(18) . . ?
O1 Gd2 Gd1 41.44(8) . . ?
O1 Gd2 O3 74.11(13) . . ?
O1 Gd2 O7 125.94(12) . . ?
O1 Gd2 O8 139.46(14) . . ?
O1 Gd2 N2 68.52(14) . . ?
O1 Gd2 N4 83.68(15) . . ?
O1 Gd2 N6 137.60(14) . . ?
O1 Gd2 N8 124.14(15) . . ?
O2 Gd2 Gd1 42.60(10) . . ?
O2 Gd2 O1 64.88(13) . . ?
O2 Gd2 O3 75.88(14) . . ?
O2 Gd2 O7 69.78(14) . . ?
O2 Gd2 O8 79.09(14) . . ?
O2 Gd2 N2 132.79(15) . . ?
O2 Gd2 N4 75.64(16) . . ?
O2 Gd2 N6 136.81(16) . . ?
O2 Gd2 N8 141.12(15) . . ?
O3 Gd2 Gd1 43.80(9) . . ?
O3 Gd2 O7 67.53(14) . . ?
O3 Gd2 O8 115.69(14) . . ?
O3 Gd2 N2 98.61(15) . . ?
O3 Gd2 N4 149.33(14) . . ?
O3 Gd2 N6 78.29(15) . . ?
O3 Gd2 N8 141.59(15) . . ?
O7 Gd2 Gd1 84.97(9) . . ?
O8 Gd2 Gd1 117.45(9) . . ?
O8 Gd2 O7 48.27(13) . . ?
O8 Gd2 N2 139.38(14) . . ?
O8 Gd2 N8 74.14(14) . . ?
N2 Gd2 Gd1 102.17(10) . . ?
N2 Gd2 O7 151.68(16) . . ?
N2 Gd2 N8 65.36(15) . . ?
N4 Gd2 Gd1 105.93(11) . . ?
N4 Gd2 O7 112.14(15) . . ?
N4 Gd2 O8 69.34(16) . . ?
N4 Gd2 N2 92.44(16) . . ?
N4 Gd2 N6 131.44(16) . . ?
N4 Gd2 N8 68.82(16) . . ?
N6 Gd2 Gd1 122.08(12) . . ?
N6 Gd2 O7 68.56(15) . . ?
N6 Gd2 O8 81.76(15) . . ?
N6 Gd2 N2 84.81(17) . . ?
N6 Gd2 N8 66.11(17) . . ?
N8 Gd2 Gd1 165.51(12) . . ?
N8 Gd2 O7 109.51(15) . . ?
Gd1 O1 Gd2 95.38(14) . . ?
C1 O1 Gd1 128.1(3) . . ?
C1 O1 Gd2 136.5(3) . . ?
Gd2 O2 Gd1 96.74(15) . . ?
C10 O2 Gd1 133.7(3) . . ?
C10 O2 Gd2 129.3(4) . . ?
Gd2 O3 Gd1 92.78(13) . . ?
C19 O3 Gd1 133.7(3) . . ?
C19 O3 Gd2 133.6(3) . . ?
N9 O4 Gd1 91.8(5) . . ?
N9 O5 Gd1 104.0(5) . . ?
N10 O7 Gd2 91.3(3) . . ?
N10 O8 Gd2 102.8(3) . . ?
O7 N10 O8 117.1(5) . . ?
O9 N10 O7 123.1(6) . . ?
O9 N10 O8 119.8(6) . . ?
C8 N1 Gd1 125.3(4) . . ?
C8 N1 C28 117.9(5) . . ?
C28 N1 Gd1 113.2(3) . . ?
C9 N2 Gd2 132.8(4) . . ?
C9 N2 C34 114.6(5) . . ?
C34 N2 Gd2 110.8(4) . . ?
C17 N3 Gd1 131.4(4) . . ?
C17 N3 C30 116.0(6) . . ?
C30 N3 Gd1 110.4(5) . . ?
C18 N4 Gd2 126.2(4) . . ?
C18 N4 C36 117.4(5) . . ?
C36 N4 Gd2 113.7(4) . . ?
C26 N5 Gd1 125.4(4) . . ?
C26 N5 C32 114.9(5) . . ?
C32 N5 Gd1 118.8(4) . . ?
C27 N6 Gd2 125.8(4) . . ?
C27 N6 C38 113.3(5) . . ?
C38 N6 Gd2 120.4(4) . . ?
C29 N7 Gd1 108.5(3) . . ?
C31 N7 Gd1 112.7(3) . . ?
C31 N7 C29 109.3(5) . . ?
C33 N7 Gd1 105.6(4) . . ?
C33 N7 C29 110.2(5) . . ?
C33 N7 C31 110.4(5) . . ?
C35 N8 Gd2 112.5(3) . . ?
C37 N8 Gd2 107.9(3) . . ?
C37 N8 C35 110.6(5) . . ?
C39 N8 Gd2 105.5(4) . . ?
C39 N8 C35 110.3(5) . . ?
C39 N8 C37 110.0(5) . . ?
O5 N9 O4 115.7(7) . . ?
O5 N9 O6 124.6(6) . . ?
O6 N9 O4 119.3(7) . . ?
O1 C1 C2 122.2(5) . . ?
O1 C1 C6 120.5(5) . . ?
C2 C1 C6 117.3(5) . . ?
C1 C2 C8 125.9(5) . . ?
C3 C2 C1 119.4(5) . . ?
C3 C2 C8 114.6(5) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.7(6) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C7 119.9(6) . . ?
C5 C4 C3 117.4(6) . . ?
C5 C4 C7 122.7(6) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.4(5) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C9 122.6(5) . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 C9 116.8(5) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 127.0(5) . . ?
N1 C8 H8 116.5 . . ?
C2 C8 H8 116.5 . . ?
N2 C9 C6 126.9(5) . . ?
N2 C9 H9 116.5 . . ?
C6 C9 H9 116.5 . . ?
O2 C10 C11 120.6(6) . . ?
O2 C10 C15 122.6(5) . . ?
C15 C10 C11 116.8(5) . . ?
C10 C11 C17 122.1(6) . . ?
C12 C11 C10 121.2(7) . . ?
C12 C11 C17 116.7(6) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.0(7) . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C14 117.8(6) . . ?
C12 C13 C16 123.7(8) . . ?
C14 C13 C16 118.5(9) . . ?
C13 C14 H14 118.8 . . ?
C13 C14 C15 122.4(7) . . ?
C15 C14 H14 118.8 . . ?
C10 C15 C18 124.8(5) . . ?
C14 C15 C10 119.6(6) . . ?
C14 C15 C18 115.6(6) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C11 127.9(5) . . ?
N3 C17 H17 116.1 . . ?
C11 C17 H17 116.1 . . ?
N4 C18 C15 127.3(6) . . ?
N4 C18 H18 116.3 . . ?
C15 C18 H18 116.3 . . ?
O3 C19 C20 121.9(5) . . ?
O3 C19 C24 122.3(5) . . ?
C24 C19 C20 115.8(5) . . ?
C19 C20 C26 127.9(5) . . ?
C21 C20 C19 120.3(5) . . ?
C21 C20 C26 111.7(5) . . ?
C20 C21 H21 118.2 . . ?
C22 C21 C20 123.6(6) . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C25 119.8(6) . . ?
C23 C22 C21 116.1(5) . . ?
C23 C22 C25 124.0(6) . . ?
C22 C23 H23 117.9 . . ?
C22 C23 C24 124.3(5) . . ?
C24 C23 H23 117.9 . . ?
C19 C24 C27 128.4(5) . . ?
C23 C24 C19 119.8(5) . . ?
C23 C24 C27 111.6(5) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C20 131.3(6) . . ?
N5 C26 H26 114.3 . . ?
C20 C26 H26 114.3 . . ?
N6 C27 C24 129.9(5) . . ?
N6 C27 H27 115.0 . . ?
C24 C27 H27 115.0 . . ?
N1 C28 H28A 110.2 . . ?
N1 C28 H28B 110.2 . . ?
N1 C28 C29 107.4(5) . . ?
H28A C28 H28B 108.5 . . ?
C29 C28 H28A 110.2 . . ?
C29 C28 H28B 110.2 . . ?
N7 C29 C28 111.2(5) . . ?
N7 C29 H29A 109.4 . . ?
N7 C29 H29B 109.4 . . ?
C28 C29 H29A 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
N3 C30 H30A 110.6 . . ?
N3 C30 H30B 110.6 . . ?
N3 C30 C31 105.6(5) . . ?
H30A C30 H30B 108.8 . . ?
C31 C30 H30A 110.6 . . ?
C31 C30 H30B 110.6 . . ?
N7 C31 C30 111.3(5) . . ?
N7 C31 H31A 109.4 . . ?
N7 C31 H31B 109.4 . . ?
C30 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
N5 C32 H32A 109.2 . . ?
N5 C32 H32B 109.2 . . ?
N5 C32 C33 112.0(5) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
N7 C33 C32 111.1(6) . . ?
N7 C33 H33A 109.4 . . ?
N7 C33 H33B 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
N2 C34 H34A 110.5 . . ?
N2 C34 H34B 110.5 . . ?
N2 C34 C35 106.3(5) . . ?
H34A C34 H34B 108.7 . . ?
C35 C34 H34A 110.5 . . ?
C35 C34 H34B 110.5 . . ?
N8 C35 C34 112.8(5) . . ?
N8 C35 H35A 109.0 . . ?
N8 C35 H35B 109.0 . . ?
C34 C35 H35A 109.0 . . ?
C34 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
N4 C36 H36A 110.0 . . ?
N4 C36 H36B 110.0 . . ?
N4 C36 C37 108.3(6) . . ?
H36A C36 H36B 108.4 . . ?
C37 C36 H36A 110.0 . . ?
C37 C36 H36B 110.0 . . ?
N8 C37 C36 111.6(5) . . ?
N8 C37 H37A 109.3 . . ?
N8 C37 H37B 109.3 . . ?
C36 C37 H37A 109.3 . . ?
C36 C37 H37B 109.3 . . ?
H37A C37 H37B 108.0 . . ?
N6 C38 H38A 109.4 . . ?
N6 C38 H38B 109.4 . . ?
N6 C38 C39 111.3(5) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
N8 C39 C38 111.6(5) . . ?
N8 C39 H39A 109.3 . . ?
N8 C39 H39B 109.3 . . ?
C38 C39 H39A 109.3 . . ?
C38 C39 H39B 109.3 . . ?
H39A C39 H39B 108.0 . . ?
O10 N11 O11 124.2(19) . . ?
O10 N11 O12 117.9(16) . . ?
O12 N11 O11 117.5(19) . . ?
O10A N11A O11A 118.2(15) . . ?
O12A N11A O10A 121.0(18) . . ?
O12A N11A O11A 120.7(18) . . ?
H13A O13 H13A 0.0 . . ?
H13A O13 H13B 87.0 . . ?
H13A O13 H13B 87.0 . . ?
H13C O13A H13D 101.9 . . ?
H14A O14 H14A 105.1 . 7_646 ?
H15 O15 H15 100.6 . 8_666 ?
H16D O16 H16D 140.6 . 7_646 ?
H16D O16 H16E 109.7 . . ?
H16E O16 H16D 109.7 . 7_646 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O14 H14A O8 0.85 2.07 2.850(4) 152.1 . yes
O15 H15 O6 0.88 2.00 2.878(6) 174.8 5_646 yes
O16 H16E O14 0.83 1.93 2.765 180.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O1 C1 C2 -38.2(7) . . . . ?
Gd1 O1 C1 C6 142.9(4) . . . . ?
Gd1 O2 C10 C11 -42.8(8) . . . . ?
Gd1 O2 C10 C15 136.9(5) . . . . ?
Gd1 O3 C19 C20 -7.7(9) . . . . ?
Gd1 O3 C19 C24 172.1(4) . . . . ?
Gd1 O4 N9 O5 3.4(6) . . . . ?
Gd1 O4 N9 O6 -169.1(6) . . . . ?
Gd1 O5 N9 O4 -3.7(7) . . . . ?
Gd1 O5 N9 O6 168.2(6) . . . . ?
Gd1 N1 C8 C2 13.2(9) . . . . ?
Gd1 N1 C28 C29 54.6(5) . . . . ?
Gd1 N3 C17 C11 11.2(9) . . . . ?
Gd1 N3 C30 C31 65.6(7) . . . . ?
Gd1 N5 C26 C20 -17.1(11) . . . . ?
Gd1 N5 C32 C33 -11.1(9) . . . . ?
Gd1 N7 C29 C28 38.0(5) . . . . ?
Gd1 N7 C31 C30 19.1(8) . . . . ?
Gd1 N7 C33 C32 -55.7(6) . . . . ?
Gd2 O1 C1 C2 138.1(5) . . . . ?
Gd2 O1 C1 C6 -40.8(8) . . . . ?
Gd2 O2 C10 C11 144.0(4) . . . . ?
Gd2 O2 C10 C15 -36.3(8) . . . . ?
Gd2 O3 C19 C20 171.3(4) . . . . ?
Gd2 O3 C19 C24 -8.9(9) . . . . ?
Gd2 O7 N10 O8 6.9(5) . . . . ?
Gd2 O7 N10 O9 -171.4(6) . . . . ?
Gd2 O8 N10 O7 -7.9(6) . . . . ?
Gd2 O8 N10 O9 170.5(6) . . . . ?
Gd2 N2 C9 C6 9.6(9) . . . . ?
Gd2 N2 C34 C35 63.9(6) . . . . ?
Gd2 N4 C18 C15 9.1(9) . . . . ?
Gd2 N4 C36 C37 52.9(6) . . . . ?
Gd2 N6 C27 C24 -16.2(9) . . . . ?
Gd2 N6 C38 C39 -9.1(7) . . . . ?
Gd2 N8 C35 C34 17.7(7) . . . . ?
Gd2 N8 C37 C36 38.3(6) . . . . ?
Gd2 N8 C39 C38 -55.5(5) . . . . ?
O1 C1 C2 C3 176.6(5) . . . . ?
O1 C1 C2 C8 0.2(9) . . . . ?
O1 C1 C6 C5 -175.3(5) . . . . ?
O1 C1 C6 C9 4.7(8) . . . . ?
O2 C10 C11 C12 -175.8(5) . . . . ?
O2 C10 C11 C17 4.8(8) . . . . ?
O2 C10 C15 C14 177.4(5) . . . . ?
O2 C10 C15 C18 -1.1(9) . . . . ?
O3 C19 C20 C21 -177.9(6) . . . . ?
O3 C19 C20 C26 7.4(10) . . . . ?
O3 C19 C24 C23 -179.5(5) . . . . ?
O3 C19 C24 C27 5.8(9) . . . . ?
N1 C28 C29 N7 -62.2(6) . . . . ?
N2 C34 C35 N8 -52.5(7) . . . . ?
N3 C30 C31 N7 -54.4(9) . . . . ?
N4 C36 C37 N8 -61.7(7) . . . . ?
N5 C32 C33 N7 46.8(9) . . . . ?
N6 C38 C39 N8 45.4(7) . . . . ?
C1 C2 C3 C4 0.3(9) . . . . ?
C1 C2 C8 N1 11.7(10) . . . . ?
C1 C6 C9 N2 8.5(9) . . . . ?
C2 C1 C6 C5 5.8(8) . . . . ?
C2 C1 C6 C9 -174.2(5) . . . . ?
C2 C3 C4 C5 2.7(9) . . . . ?
C2 C3 C4 C7 -178.2(6) . . . . ?
C3 C2 C8 N1 -164.8(6) . . . . ?
C3 C4 C5 C6 -1.4(9) . . . . ?
C4 C5 C6 C1 -2.9(9) . . . . ?
C4 C5 C6 C9 177.1(6) . . . . ?
C5 C6 C9 N2 -171.6(6) . . . . ?
C6 C1 C2 C3 -4.5(8) . . . . ?
C6 C1 C2 C8 179.1(5) . . . . ?
C7 C4 C5 C6 179.6(6) . . . . ?
C8 N1 C28 C29 -105.4(6) . . . . ?
C8 C2 C3 C4 177.1(6) . . . . ?
C9 N2 C34 C35 -103.1(6) . . . . ?
C10 C11 C12 C13 -3.7(9) . . . . ?
C10 C11 C17 N3 9.2(9) . . . . ?
C10 C15 C18 N4 14.0(10) . . . . ?
C11 C10 C15 C14 -2.9(8) . . . . ?
C11 C10 C15 C18 178.6(5) . . . . ?
C11 C12 C13 C14 1.2(10) . . . . ?
C11 C12 C13 C16 -179.8(6) . . . . ?
C12 C11 C17 N3 -170.3(6) . . . . ?
C12 C13 C14 C15 0.4(9) . . . . ?
C13 C14 C15 C10 0.5(9) . . . . ?
C13 C14 C15 C18 179.2(6) . . . . ?
C14 C15 C18 N4 -164.6(6) . . . . ?
C15 C10 C11 C12 4.5(8) . . . . ?
C15 C10 C11 C17 -174.9(5) . . . . ?
C16 C13 C14 C15 -178.7(6) . . . . ?
C17 N3 C30 C31 -99.2(7) . . . . ?
C17 C11 C12 C13 175.7(6) . . . . ?
C18 N4 C36 C37 -109.7(6) . . . . ?
C19 C20 C21 C22 -2.7(10) . . . . ?
C19 C20 C26 N5 6.5(12) . . . . ?
C19 C24 C27 N6 8.2(10) . . . . ?
C20 C19 C24 C23 0.3(8) . . . . ?
C20 C19 C24 C27 -174.4(6) . . . . ?
C20 C21 C22 C23 0.1(9) . . . . ?
C20 C21 C22 C25 177.3(6) . . . . ?
C21 C20 C26 N5 -168.6(8) . . . . ?
C21 C22 C23 C24 2.8(9) . . . . ?
C22 C23 C24 C19 -3.0(9) . . . . ?
C22 C23 C24 C27 172.5(5) . . . . ?
C23 C24 C27 N6 -166.9(6) . . . . ?
C24 C19 C20 C21 2.3(9) . . . . ?
C24 C19 C20 C26 -172.3(6) . . . . ?
C25 C22 C23 C24 -174.3(6) . . . . ?
C26 N5 C32 C33 158.9(7) . . . . ?
C26 C20 C21 C22 172.8(6) . . . . ?
C27 N6 C38 C39 162.9(5) . . . . ?
C28 N1 C8 C2 170.6(6) . . . . ?
C29 N7 C31 C30 139.9(6) . . . . ?
C29 N7 C33 C32 -172.7(5) . . . . ?
C30 N3 C17 C11 172.0(6) . . . . ?
C31 N7 C29 C28 -85.2(6) . . . . ?
C31 N7 C33 C32 66.4(7) . . . . ?
C32 N5 C26 C20 173.8(7) . . . . ?
C33 N7 C29 C28 153.2(5) . . . . ?
C33 N7 C31 C30 -98.8(7) . . . . ?
C34 N2 C9 C6 172.8(5) . . . . ?
C35 N8 C37 C36 -85.1(6) . . . . ?
C35 N8 C39 C38 66.3(6) . . . . ?
C36 N4 C18 C15 169.4(6) . . . . ?
C37 N8 C35 C34 138.4(6) . . . . ?
C37 N8 C39 C38 -171.5(5) . . . . ?
C38 N6 C27 C24 172.3(6) . . . . ?
C39 N8 C35 C34 -99.7(6) . . . . ?
C39 N8 C37 C36 152.8(5) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_original_sample_id D8V4660
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4644_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc2747rd
_database_code_depnum_ccdc_archive 'CCDC 2059663'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.13667729.v1 2021
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-01-29 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_mo_d8v4644_0m_a     
;
PROBLEM: D-H Without Acceptor       O13      --H13B     .     Please Check
RESPONSE: Disordered water, discussed in _refine_special_details.
;
# Added during the CSD deposition process: Friday 29 January 2021 01:12 PM
# end Validation Reply Form

_audit_creation_date             2021-01-29
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H45 N10 O9 Y2, N O3, 2.5(H2 O), 1.5[H2O]'
_chemical_formula_sum            'C39 H53 N11 O16 Y2'
_chemical_formula_weight         1109.74
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+3/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+1/4'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   17.6029(6)
_cell_length_b                   17.6029(6)
_cell_length_c                   29.0488(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9001.1(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.550
_cell_measurement_theta_min      2.401
_shelx_estimated_absorpt_T_max   0.752
_shelx_estimated_absorpt_T_min   0.449
_exptl_absorpt_coefficient_mu    2.650
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1086 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.6882.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4560
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 1.00 0.00 0.0420
-1.00 -1.00 0.00 0.0620
1.00 -1.00 0.00 0.0350
-1.00 1.00 0.00 0.0570
0.00 0.00 -1.00 0.1800
0.00 0.00 1.00 0.1760

_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.114
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            126935
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.818
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6911
_reflns_number_total             7955
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Flack x determined using 2703 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         7955
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+10.1103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0835
_refine_special_details          
;
One of the nitrate ligands was modelled as disordered, consistent with peaks in a difference map.  The nitrate counterion and one water of crystallization were modelled as disordered over two sites with geometric and displacement ellipsoid restraints used.  In all cases water H atoms were identified from difference peaks which corresponded with likely hydrogen bonding interactions.  Water H atoms were refined using a riding model with geometric restraints.  One of the water molecules lies on a special position, hence a fractional value in the chemical formula.  The solvent masking routine of Olex2 was used to account for peaks which appear to correspond with 1.5 disordered water molecules.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

420_ALERT_2_B D-H Without Acceptor       O13      --H13B     .     Please Check

Disordered water, discussed above

#===============================================================================
090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       7.15 Note

Non-centrysymmetric diffraction pattern and relatively weak data

161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .        O13 Check
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .       O13A Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .        O13 Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .       O13A Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .        O13 Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .       O13A Check

Disordered water, discussed above

213_ALERT_2_C Atom C13             has ADP max/min Ratio .....        3.2 prolat
213_ALERT_2_C Atom C16             has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C17             has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C30             has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C32             has ADP max/min Ratio .....        3.1 prolat

Noted but no action taken

218_ALERT_3_C Constrained U(ij) Components(s) for O13        .          6 Check
218_ALERT_3_C Constrained U(ij) Components(s) for O13A       .          6 Check

Disordered water, discussed above

220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.8 Ratio
220_ALERT_2_C NonSolvent   Resd 1  N   Ueq(max)/Ueq(min) Range        3.1 Ratio
220_ALERT_2_C NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        4.2 Ratio
234_ALERT_4_C Large Hirshfeld Difference Y1       --O4       .       0.18 Ang.
234_ALERT_4_C Large Hirshfeld Difference O4A      --N9       .       0.20 Ang.
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00885 Ang.
911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.595          3 Report
976_ALERT_2_C Check Calcd Resid. Dens.  0.41A   From O16            -0.45 eA-3

Noted but no action taken

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13-H13B = O13-H13A = O13A-H13C = O13A-H13D = O16-H16D = O16-H16E = O14-H14A
 0.84 with sigma of 0.02
 O15-H15
 0.84 with sigma of 0.02
 H16E-H16D_$1 = H14A_$1-H14A
 1.35 with sigma of 0.04
 H13B-H13A = H13C-H13D = H16D-H16E
 1.35 with sigma of 0.04
 H15_$2-H15
 1.35 with sigma of 0.04
 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim
O12-N11
 with sigma of 0.02
 N9-O4A \\sim N9-O4 \\sim N9-O5 \\sim N9-O6
 with sigma of 0.02
3. Restrained planarity
 O4A, O5, O6, N9
 with sigma of 0.1
 O4, O5, O6, N9
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 O10, O11, O12, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10A, O11A, O12A, N11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, O6, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, O5, O6, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, O11, O12, N11}
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, O11A, O12A, N11A}
6. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5)
 N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5)
7.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O16, H16D, H16E
7.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C21(H21), C23(H23), C26(H26), C27(H27)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Y1 Y 0.14204(3) 0.60961(3) 0.39656(2) 0.01994(13) Uani 1 1 d . . . . .
Y2 Y 0.05192(3) 0.68493(3) 0.49237(2) 0.02088(13) Uani 1 1 d . . . . .
O1 O 0.1752(2) 0.6487(2) 0.46944(11) 0.0212(8) Uani 1 1 d . . . . .
O2 O 0.0849(2) 0.7236(2) 0.41987(12) 0.0237(9) Uani 1 1 d . . . . .
O3 O 0.0408(2) 0.5733(2) 0.44658(12) 0.0242(9) Uani 1 1 d . . . . .
O4 O 0.1761(6) 0.4857(7) 0.4519(3) 0.048(3) Uani 0.467(12) 1 d D . P A 1
O4A O 0.2248(8) 0.4041(6) 0.4202(5) 0.090(5) Uani 0.533(12) 1 d D . P A 2
O5 O 0.2469(3) 0.5323(3) 0.41341(18) 0.0549(14) Uani 1 1 d D . . . .
O6 O 0.2976(3) 0.4560(3) 0.46359(18) 0.0553(14) Uani 1 1 d D . . B 1
O7 O -0.0749(3) 0.6888(2) 0.43434(14) 0.0370(11) Uani 1 1 d D . . . .
O8 O -0.0418(2) 0.7832(2) 0.47744(12) 0.0276(9) Uani 1 1 d D . . . .
O9 O -0.1325(3) 0.7972(3) 0.42688(17) 0.0588(16) Uani 1 1 d D . . . .
N10 N -0.0847(3) 0.7567(3) 0.44558(16) 0.0339(13) Uani 1 1 d D . . . .
N1 N 0.2529(3) 0.6869(3) 0.38445(14) 0.0222(10) Uani 1 1 d . . . . .
N2 N 0.1209(3) 0.6271(3) 0.55748(14) 0.0252(11) Uani 1 1 d . . . . .
N3 N 0.0718(3) 0.6653(4) 0.33229(16) 0.0362(14) Uani 1 1 d . . . . .
N4 N 0.1092(3) 0.8077(3) 0.50427(16) 0.0278(11) Uani 1 1 d . . . . .
N5 N 0.1041(3) 0.4869(3) 0.36426(17) 0.0341(13) Uani 1 1 d . . . . .
N6 N -0.0594(3) 0.6268(3) 0.52727(14) 0.0242(11) Uani 1 1 d . . . . .
N7 N 0.2037(3) 0.5834(3) 0.31530(15) 0.0277(12) Uani 1 1 d . . . . .
N8 N 0.0161(3) 0.7421(3) 0.57466(15) 0.0293(12) Uani 1 1 d . . . . .
N9 N 0.2485(4) 0.4756(5) 0.4377(2) 0.068(2) Uani 1 1 d D . . . .
C1 C 0.2438(3) 0.6527(3) 0.48767(18) 0.0205(12) Uani 1 1 d . . . . .
C2 C 0.3085(3) 0.6738(3) 0.46173(17) 0.0240(12) Uani 1 1 d . . . . .
C3 C 0.3795(3) 0.6734(3) 0.48214(19) 0.0282(14) Uani 1 1 d . . . . .
H3 H 0.421907 0.688934 0.464284 0.034 Uiso 1 1 calc R U . . .
C4 C 0.3919(4) 0.6511(4) 0.52787(19) 0.0317(14) Uani 1 1 d . . . . .
C5 C 0.3276(4) 0.6339(3) 0.55360(19) 0.0292(14) Uani 1 1 d . . . . .
H5 H 0.333547 0.619763 0.584944 0.035 Uiso 1 1 calc R U . . .
C6 C 0.2549(3) 0.6368(3) 0.53510(18) 0.0242(13) Uani 1 1 d . . . . .
C7 C 0.4703(4) 0.6479(5) 0.5477(2) 0.0465(19) Uani 1 1 d . . . . .
H7A H 0.490475 0.699546 0.550667 0.070 Uiso 1 1 calc R U . . .
H7B H 0.503198 0.618186 0.527324 0.070 Uiso 1 1 calc R U . . .
H7C H 0.468426 0.623861 0.578110 0.070 Uiso 1 1 calc R U . . .
C8 C 0.3075(3) 0.6957(3) 0.41311(19) 0.0259(13) Uani 1 1 d . . . . .
H8 H 0.352240 0.719032 0.401549 0.031 Uiso 1 1 calc R U . . .
C9 C 0.1920(4) 0.6211(3) 0.56615(17) 0.0260(14) Uani 1 1 d . . . . .
H9 H 0.205143 0.604525 0.596239 0.031 Uiso 1 1 calc R U . . .
C10 C 0.0796(3) 0.7919(3) 0.40088(19) 0.0264(13) Uani 1 1 d . . . . .
C11 C 0.0611(3) 0.7995(4) 0.3538(2) 0.0353(15) Uani 1 1 d . . . . .
C12 C 0.0521(4) 0.8714(5) 0.3340(3) 0.048(2) Uani 1 1 d . . . . .
H12 H 0.038633 0.874874 0.302440 0.057 Uiso 1 1 calc R U . . .
C13 C 0.0621(4) 0.9376(5) 0.3588(3) 0.051(2) Uani 1 1 d . . . . .
C14 C 0.0821(4) 0.9304(4) 0.4048(3) 0.0419(18) Uani 1 1 d . . . . .
H14 H 0.089557 0.975178 0.422492 0.050 Uiso 1 1 calc R U . . .
C15 C 0.0917(3) 0.8590(4) 0.4264(2) 0.0319(15) Uani 1 1 d . . . . .
C16 C 0.0510(5) 1.0151(5) 0.3376(4) 0.078(3) Uani 1 1 d . . . . .
H16A H 0.010411 1.042018 0.353958 0.117 Uiso 1 1 calc R U . . .
H16B H 0.037073 1.009411 0.305135 0.117 Uiso 1 1 calc R U . . .
H16C H 0.098320 1.044176 0.339974 0.117 Uiso 1 1 calc R U . . .
C17 C 0.0544(3) 0.7350(5) 0.3235(2) 0.0395(18) Uani 1 1 d . . . . .
H17 H 0.034996 0.744885 0.293598 0.047 Uiso 1 1 calc R U . . .
C18 C 0.1123(4) 0.8621(3) 0.4749(2) 0.0310(13) Uani 1 1 d . . . . .
H18 H 0.129882 0.909676 0.486054 0.037 Uiso 1 1 calc R U . . .
C19 C -0.0072(3) 0.5153(3) 0.44780(18) 0.0213(12) Uani 1 1 d . . . . .
C20 C 0.0041(3) 0.4497(3) 0.41957(19) 0.0239(12) Uani 1 1 d . . . . .
C21 C -0.0447(3) 0.3872(3) 0.42299(19) 0.0253(12) Uani 1 1 d . . . . .
H21 H -0.033865 0.343673 0.404800 0.030 Uiso 1 1 calc R U . . .
C22 C -0.1079(3) 0.3851(4) 0.45139(19) 0.0287(13) Uani 1 1 d . . . . .
C23 C -0.1200(3) 0.4496(4) 0.47709(18) 0.0265(13) Uani 1 1 d . . . . .
H23 H -0.163927 0.451299 0.496098 0.032 Uiso 1 1 calc R U . . .
C24 C -0.0719(3) 0.5128(3) 0.47698(17) 0.0206(12) Uani 1 1 d . . . . .
C25 C -0.1565(4) 0.3158(4) 0.4535(2) 0.0448(18) Uani 1 1 d . . . . .
H25A H -0.126275 0.272761 0.464560 0.067 Uiso 1 1 calc R U . . .
H25B H -0.176175 0.304344 0.422674 0.067 Uiso 1 1 calc R U . . .
H25C H -0.199083 0.324649 0.474549 0.067 Uiso 1 1 calc R U . . .
C26 C 0.0607(3) 0.4393(4) 0.3833(2) 0.0314(14) Uani 1 1 d . . . . .
H26 H 0.065501 0.388717 0.372382 0.038 Uiso 1 1 calc R U . . .
C27 C -0.0954(3) 0.5683(3) 0.51187(18) 0.0248(13) Uani 1 1 d . . . . .
H27 H -0.144173 0.559953 0.524963 0.030 Uiso 1 1 calc R U . . .
C28 C 0.2700(3) 0.7028(3) 0.33575(18) 0.0247(13) Uani 1 1 d . . . . .
H28A H 0.318418 0.731073 0.333021 0.030 Uiso 1 1 calc R U . . .
H28B H 0.229004 0.733695 0.321823 0.030 Uiso 1 1 calc R U . . .
C29 C 0.2760(3) 0.6258(3) 0.31146(18) 0.0256(13) Uani 1 1 d . . . . .
H29A H 0.288436 0.633792 0.278570 0.031 Uiso 1 1 calc R U . . .
H29B H 0.317546 0.595757 0.325492 0.031 Uiso 1 1 calc R U . . .
C30 C 0.0695(4) 0.6136(5) 0.2920(2) 0.051(2) Uani 1 1 d . . . . .
H30A H 0.037663 0.635182 0.267188 0.061 Uiso 1 1 calc R U . . .
H30B H 0.048821 0.563338 0.300832 0.061 Uiso 1 1 calc R U . . .
C31 C 0.1528(3) 0.6065(4) 0.27632(18) 0.0375(16) Uani 1 1 d . . . . .
H31A H 0.156245 0.568245 0.251398 0.045 Uiso 1 1 calc R U . . .
H31B H 0.170096 0.655809 0.263791 0.045 Uiso 1 1 calc R U . . .
C32 C 0.1472(4) 0.4554(4) 0.3240(2) 0.050(2) Uani 1 1 d . . . . .
H32A H 0.114180 0.456097 0.296405 0.060 Uiso 1 1 calc R U . . .
H32B H 0.161159 0.401983 0.330351 0.060 Uiso 1 1 calc R U . . .
C33 C 0.2190(4) 0.5009(4) 0.3142(2) 0.0362(16) Uani 1 1 d . . . . .
H33A H 0.258130 0.488310 0.337380 0.043 Uiso 1 1 calc R U . . .
H33B H 0.238977 0.486811 0.283478 0.043 Uiso 1 1 calc R U . . .
C34 C 0.0710(4) 0.6167(4) 0.59799(19) 0.0327(15) Uani 1 1 d . . . . .
H34A H 0.098520 0.589997 0.622936 0.039 Uiso 1 1 calc R U . . .
H34B H 0.025597 0.586500 0.589625 0.039 Uiso 1 1 calc R U . . .
C35 C 0.0482(4) 0.6956(4) 0.61332(17) 0.0342(15) Uani 1 1 d . . . . .
H35A H 0.009744 0.691493 0.638085 0.041 Uiso 1 1 calc R U . . .
H35B H 0.093125 0.721927 0.626161 0.041 Uiso 1 1 calc R U . . .
C36 C 0.1204(4) 0.8274(4) 0.5527(2) 0.0349(15) Uani 1 1 d . . . . .
H36A H 0.139827 0.880033 0.555317 0.042 Uiso 1 1 calc R U . . .
H36B H 0.157971 0.792697 0.566869 0.042 Uiso 1 1 calc R U . . .
C37 C 0.0455(4) 0.8206(4) 0.5770(2) 0.0364(15) Uani 1 1 d . . . . .
H37A H 0.051733 0.835595 0.609663 0.044 Uiso 1 1 calc R U . . .
H37B H 0.008405 0.855671 0.562715 0.044 Uiso 1 1 calc R U . . .
C38 C -0.0985(4) 0.6628(3) 0.56717(19) 0.0340(15) Uani 1 1 d . . . . .
H38A H -0.091355 0.630839 0.594880 0.041 Uiso 1 1 calc R U . . .
H38B H -0.153627 0.666107 0.560808 0.041 Uiso 1 1 calc R U . . .
C39 C -0.0673(4) 0.7422(4) 0.5764(2) 0.0341(16) Uani 1 1 d . . . . .
H39A H -0.087329 0.777923 0.553061 0.041 Uiso 1 1 calc R U . . .
H39B H -0.084300 0.759662 0.607077 0.041 Uiso 1 1 calc R U . . .
O10 O 0.4566(9) 0.7070(9) 0.2926(5) 0.099(5) Uani 0.5 1 d D . P C 1
O11 O 0.4758(8) 0.7369(8) 0.3650(6) 0.115(7) Uani 0.5 1 d D . P C 1
O12 O 0.4936(11) 0.6269(8) 0.3413(5) 0.116(6) Uani 0.5 1 d D . P C 1
N11 N 0.4762(6) 0.6919(6) 0.3317(4) 0.049(3) Uani 0.5 1 d D . P C 1
O10A O 0.5734(10) 0.7149(8) 0.4513(4) 0.100(5) Uani 0.5 1 d D . P D 2
O11A O 0.4888(7) 0.7641(8) 0.4083(5) 0.097(5) Uani 0.5 1 d D . P D 2
O12A O 0.5688(12) 0.6876(8) 0.3799(5) 0.142(8) Uani 0.5 1 d D . P D 2
N11A N 0.5450(6) 0.7211(6) 0.4123(3) 0.033(2) Uani 0.5 1 d D . P D 2
O13 O 0.562200 0.735630 0.438850 0.092 Uani 0.5 1 d D . P E 1
H13A H 0.564530 0.705950 0.410150 0.110 Uiso 0.5 1 d D U P F 1
H13B H 0.597760 0.694010 0.453370 0.110 Uiso 0.5 1 d D U P G 1
O13A O 0.467980 0.697590 0.293840 0.043 Uani 0.5 1 d D . P H 2
H13C H 0.464270 0.652220 0.284420 0.051 Uiso 0.5 1 d D U P I 2
H13D H 0.478750 0.691110 0.322570 0.051 Uiso 0.5 1 d D U P J 2
O14 O -0.060260 0.939740 0.500000 0.045 Uani 1 2 d DS T P . .
H14A H -0.061250 0.899460 0.484250 0.054 Uiso 1 1 d D U . . .
O15 O 0.1976(3) 0.8024(3) 0.250000 0.0463(18) Uani 1 2 d DS T P . .
H15 H 0.194(3) 0.846(3) 0.264(2) 0.056 Uiso 1 1 d D U . . .
O16 O 0.050600 1.050600 0.500000 0.053 Uani 1 2 d DS T P . .
H16D H 0.080320 1.043180 0.521350 0.064 Uiso 0.5 1 d D U P . .
H16E H 0.017230 1.017230 0.500000 0.064 Uiso 1 2 d DS 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
Y1 Y2 3.4669(7) . ?
Y1 O1 2.301(3) . ?
Y1 O2 2.344(4) . ?
Y1 O3 2.387(4) . ?
Y1 O4 2.776(11) . ?
Y1 O5 2.344(5) . ?
Y1 N1 2.405(5) . ?
Y1 N3 2.444(5) . ?
Y1 N5 2.448(5) . ?
Y1 N7 2.639(4) . ?
Y2 O1 2.357(4) . ?
Y2 O2 2.288(3) . ?
Y2 O3 2.380(4) . ?
Y2 O7 2.798(5) . ?
Y2 O8 2.430(4) . ?
Y2 N2 2.468(5) . ?
Y2 N4 2.410(5) . ?
Y2 N6 2.433(5) . ?
Y2 N8 2.669(4) . ?
O1 C1 1.322(7) . ?
O2 C10 1.327(7) . ?
O3 C19 1.326(7) . ?
O4 N9 1.351(11) . ?
O4A N9 1.419(12) . ?
O5 N9 1.223(8) . ?
O6 N9 1.197(8) . ?
O7 N10 1.252(6) . ?
O8 N10 1.282(6) . ?
O9 N10 1.229(6) . ?
N1 C8 1.280(7) . ?
N1 C28 1.473(7) . ?
N2 C9 1.281(8) . ?
N2 C34 1.480(7) . ?
N3 C17 1.290(9) . ?
N3 C30 1.482(8) . ?
N4 C18 1.284(7) . ?
N4 C36 1.463(7) . ?
N5 C26 1.262(8) . ?
N5 C32 1.500(7) . ?
N6 C27 1.289(7) . ?
N6 C38 1.489(7) . ?
N7 C29 1.480(7) . ?
N7 C31 1.501(7) . ?
N7 C33 1.476(8) . ?
N8 C35 1.500(7) . ?
N8 C37 1.477(8) . ?
N8 C39 1.469(8) . ?
C1 C2 1.414(8) . ?
C1 C6 1.419(7) . ?
C2 C3 1.383(8) . ?
C2 C8 1.464(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(8) . ?
C4 C5 1.390(9) . ?
C4 C7 1.496(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(9) . ?
C6 C9 1.454(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.414(8) . ?
C10 C15 1.411(9) . ?
C11 C12 1.398(10) . ?
C11 C17 1.442(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.381(12) . ?
C13 C14 1.386(11) . ?
C13 C16 1.510(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.415(9) . ?
C15 C18 1.454(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.430(8) . ?
C19 C24 1.420(8) . ?
C20 C21 1.400(8) . ?
C20 C26 1.460(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.385(8) . ?
C22 C23 1.375(9) . ?
C22 C25 1.493(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.399(8) . ?
C24 C27 1.468(8) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.532(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.540(9) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.522(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.514(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.500(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.525(9) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
O10 N11 1.218(13) . ?
O11 N11 1.249(13) . ?
O12 N11 1.216(13) . ?
O10A N11A 1.243(12) . ?
O11A N11A 1.251(13) . ?
O12A N11A 1.188(12) . ?
O13 H13A 0.9847 . ?
O13 H13A 0.9847 . ?
O13 H13B 1.0519 . ?
O13A H13C 0.8467 . ?
O13A H13D 0.8634 . ?
O14 H14A 0.8440 . ?
O14 H14A 0.8440 7_466 ?
O15 H15 0.87(3) . ?
O15 H15 0.87(3) 8_665 ?
O16 H16D 0.8218 . ?
O16 H16D 0.8218 7_466 ?
O16 H16E 0.8307 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 Y2 42.53(10) . . ?
O1 Y1 O2 65.60(13) . . ?
O1 Y1 O3 73.11(13) . . ?
O1 Y1 O4 69.3(2) . . ?
O1 Y1 O5 77.42(15) . . ?
O1 Y1 N1 76.09(13) . . ?
O1 Y1 N3 135.30(17) . . ?
O1 Y1 N5 133.30(16) . . ?
O1 Y1 N7 140.44(14) . . ?
O2 Y1 Y2 40.93(8) . . ?
O2 Y1 O3 74.49(13) . . ?
O2 Y1 O4 126.7(2) . . ?
O2 Y1 O5 140.73(15) . . ?
O2 Y1 N1 84.63(15) . . ?
O2 Y1 N3 70.15(16) . . ?
O2 Y1 N5 138.51(16) . . ?
O2 Y1 N7 125.78(15) . . ?
O3 Y1 Y2 43.27(9) . . ?
O3 Y1 O4 66.3(2) . . ?
O3 Y1 N1 147.83(13) . . ?
O3 Y1 N3 101.21(15) . . ?
O3 Y1 N5 78.10(14) . . ?
O3 Y1 N7 143.61(14) . . ?
O4 Y1 Y2 86.2(2) . . ?
O5 Y1 Y2 114.49(13) . . ?
O5 Y1 O3 107.80(18) . . ?
O5 Y1 O4 41.7(3) . . ?
O5 Y1 N1 73.73(19) . . ?
O5 Y1 N3 142.21(17) . . ?
O5 Y1 N5 77.44(19) . . ?
O5 Y1 N7 76.19(17) . . ?
N1 Y1 Y2 105.81(11) . . ?
N1 Y1 O4 110.7(2) . . ?
N1 Y1 N3 94.13(17) . . ?
N1 Y1 N5 131.63(16) . . ?
N1 Y1 N7 68.55(15) . . ?
N3 Y1 Y2 103.20(12) . . ?
N3 Y1 O4 150.1(3) . . ?
N3 Y1 N5 85.6(2) . . ?
N3 Y1 N7 66.11(16) . . ?
N5 Y1 Y2 121.37(11) . . ?
N5 Y1 O4 65.6(3) . . ?
N5 Y1 N7 67.34(16) . . ?
N7 Y1 Y2 166.71(12) . . ?
N7 Y1 O4 107.0(2) . . ?
O1 Y2 Y1 41.29(8) . . ?
O1 Y2 O3 72.24(13) . . ?
O1 Y2 O7 124.79(12) . . ?
O1 Y2 O8 140.07(13) . . ?
O1 Y2 N2 69.65(13) . . ?
O1 Y2 N4 84.11(15) . . ?
O1 Y2 N6 138.22(15) . . ?
O1 Y2 N8 124.90(14) . . ?
O2 Y2 Y1 42.16(10) . . ?
O2 Y2 O1 65.59(13) . . ?
O2 Y2 O3 75.64(13) . . ?
O2 Y2 O7 68.94(13) . . ?
O2 Y2 O8 78.24(13) . . ?
O2 Y2 N2 134.71(15) . . ?
O2 Y2 N4 76.07(15) . . ?
O2 Y2 N6 135.49(15) . . ?
O2 Y2 N8 140.54(15) . . ?
O3 Y2 Y1 43.41(9) . . ?
O3 Y2 O7 67.52(13) . . ?
O3 Y2 O8 115.60(14) . . ?
O3 Y2 N2 97.37(14) . . ?
O3 Y2 N4 148.72(14) . . ?
O3 Y2 N6 79.59(14) . . ?
O3 Y2 N8 142.39(14) . . ?
O7 Y2 Y1 83.73(8) . . ?
O8 Y2 Y1 116.09(9) . . ?
O8 Y2 O7 48.21(13) . . ?
O8 Y2 N2 139.89(13) . . ?
O8 Y2 N6 80.04(15) . . ?
O8 Y2 N8 74.39(13) . . ?
N2 Y2 Y1 103.43(10) . . ?
N2 Y2 O7 149.80(15) . . ?
N2 Y2 N8 65.50(15) . . ?
N4 Y2 Y1 105.46(11) . . ?
N4 Y2 O7 113.51(15) . . ?
N4 Y2 O8 70.81(16) . . ?
N4 Y2 N2 93.09(16) . . ?
N4 Y2 N6 130.91(16) . . ?
N4 Y2 N8 68.41(16) . . ?
N6 Y2 Y1 122.85(11) . . ?
N6 Y2 O7 67.57(14) . . ?
N6 Y2 N2 84.45(16) . . ?
N6 Y2 N8 66.12(16) . . ?
N8 Y2 Y1 166.20(12) . . ?
N8 Y2 O7 110.00(14) . . ?
Y1 O1 Y2 96.18(14) . . ?
C1 O1 Y1 128.0(3) . . ?
C1 O1 Y2 135.6(3) . . ?
Y2 O2 Y1 96.91(14) . . ?
C10 O2 Y1 133.3(3) . . ?
C10 O2 Y2 129.4(3) . . ?
Y2 O3 Y1 93.32(13) . . ?
C19 O3 Y1 134.3(3) . . ?
C19 O3 Y2 132.3(3) . . ?
N9 O4 Y1 97.5(6) . . ?
N9 O5 Y1 127.8(5) . . ?
N10 O7 Y2 88.6(3) . . ?
N10 O8 Y2 105.6(3) . . ?
O7 N10 O8 117.1(5) . . ?
O9 N10 O7 122.2(5) . . ?
O9 N10 O8 120.8(5) . . ?
C8 N1 Y1 125.6(4) . . ?
C8 N1 C28 116.6(5) . . ?
C28 N1 Y1 114.4(3) . . ?
C9 N2 Y2 131.7(4) . . ?
C9 N2 C34 114.4(5) . . ?
C34 N2 Y2 111.6(4) . . ?
C17 N3 Y1 130.7(4) . . ?
C17 N3 C30 114.9(6) . . ?
C30 N3 Y1 111.7(5) . . ?
C18 N4 Y2 126.2(4) . . ?
C18 N4 C36 117.1(5) . . ?
C36 N4 Y2 114.1(4) . . ?
C26 N5 Y1 125.6(4) . . ?
C26 N5 C32 113.9(5) . . ?
C32 N5 Y1 119.1(4) . . ?
C27 N6 Y2 126.0(3) . . ?
C27 N6 C38 112.5(5) . . ?
C38 N6 Y2 121.1(4) . . ?
C29 N7 Y1 109.5(3) . . ?
C29 N7 C31 108.7(5) . . ?
C31 N7 Y1 112.5(3) . . ?
C33 N7 Y1 105.5(3) . . ?
C33 N7 C29 109.8(5) . . ?
C33 N7 C31 111.0(5) . . ?
C35 N8 Y2 112.1(3) . . ?
C37 N8 Y2 108.2(3) . . ?
C37 N8 C35 110.1(5) . . ?
C39 N8 Y2 105.5(3) . . ?
C39 N8 C35 110.5(5) . . ?
C39 N8 C37 110.4(5) . . ?
O5 N9 O4 92.7(8) . . ?
O5 N9 O4A 120.8(7) . . ?
O6 N9 O4 121.7(7) . . ?
O6 N9 O5 127.9(7) . . ?
O1 C1 C2 122.4(5) . . ?
O1 C1 C6 120.2(5) . . ?
C2 C1 C6 117.3(5) . . ?
C1 C2 C8 125.0(5) . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 C8 115.2(5) . . ?
C2 C3 H3 118.4 . . ?
C2 C3 C4 123.3(5) . . ?
C4 C3 H3 118.4 . . ?
C3 C4 C7 121.3(6) . . ?
C5 C4 C3 116.3(6) . . ?
C5 C4 C7 122.4(5) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 C4 122.3(5) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C9 122.4(5) . . ?
C5 C6 C1 120.6(5) . . ?
C5 C6 C9 117.0(5) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 127.2(5) . . ?
N1 C8 H8 116.4 . . ?
C2 C8 H8 116.4 . . ?
N2 C9 C6 127.3(5) . . ?
N2 C9 H9 116.3 . . ?
C6 C9 H9 116.3 . . ?
O2 C10 C11 120.3(6) . . ?
O2 C10 C15 122.0(5) . . ?
C15 C10 C11 117.7(6) . . ?
C10 C11 C17 122.3(6) . . ?
C12 C11 C10 120.6(7) . . ?
C12 C11 C17 117.1(6) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 C11 122.4(7) . . ?
C13 C12 H12 118.8 . . ?
C12 C13 C14 117.2(6) . . ?
C12 C13 C16 122.2(8) . . ?
C14 C13 C16 120.6(9) . . ?
C13 C14 H14 118.7 . . ?
C13 C14 C15 122.6(7) . . ?
C15 C14 H14 118.7 . . ?
C10 C15 C14 119.5(6) . . ?
C10 C15 C18 125.3(5) . . ?
C14 C15 C18 115.2(6) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C11 127.6(5) . . ?
N3 C17 H17 116.2 . . ?
C11 C17 H17 116.2 . . ?
N4 C18 C15 127.2(6) . . ?
N4 C18 H18 116.4 . . ?
C15 C18 H18 116.4 . . ?
O3 C19 C20 121.2(5) . . ?
O3 C19 C24 123.4(5) . . ?
C24 C19 C20 115.4(5) . . ?
C19 C20 C26 127.5(5) . . ?
C21 C20 C19 120.6(5) . . ?
C21 C20 C26 111.8(5) . . ?
C20 C21 H21 118.1 . . ?
C22 C21 C20 123.7(6) . . ?
C22 C21 H21 118.1 . . ?
C21 C22 C25 120.4(6) . . ?
C23 C22 C21 115.3(5) . . ?
C23 C22 C25 124.3(6) . . ?
C22 C23 H23 118.0 . . ?
C22 C23 C24 124.1(5) . . ?
C24 C23 H23 118.0 . . ?
C19 C24 C27 128.2(5) . . ?
C23 C24 C19 120.8(5) . . ?
C23 C24 C27 110.9(5) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C20 130.3(6) . . ?
N5 C26 H26 114.8 . . ?
C20 C26 H26 114.8 . . ?
N6 C27 C24 129.2(5) . . ?
N6 C27 H27 115.4 . . ?
C24 C27 H27 115.4 . . ?
N1 C28 H28A 110.4 . . ?
N1 C28 H28B 110.4 . . ?
N1 C28 C29 106.8(5) . . ?
H28A C28 H28B 108.6 . . ?
C29 C28 H28A 110.4 . . ?
C29 C28 H28B 110.4 . . ?
N7 C29 C28 110.6(5) . . ?
N7 C29 H29A 109.5 . . ?
N7 C29 H29B 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
N3 C30 H30A 110.8 . . ?
N3 C30 H30B 110.8 . . ?
N3 C30 C31 105.0(5) . . ?
H30A C30 H30B 108.8 . . ?
C31 C30 H30A 110.8 . . ?
C31 C30 H30B 110.8 . . ?
N7 C31 C30 111.5(5) . . ?
N7 C31 H31A 109.3 . . ?
N7 C31 H31B 109.3 . . ?
C30 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
N5 C32 H32A 109.3 . . ?
N5 C32 H32B 109.3 . . ?
N5 C32 C33 111.8(5) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
N7 C33 C32 111.2(5) . . ?
N7 C33 H33A 109.4 . . ?
N7 C33 H33B 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
N2 C34 H34A 110.5 . . ?
N2 C34 H34B 110.5 . . ?
N2 C34 C35 106.1(5) . . ?
H34A C34 H34B 108.7 . . ?
C35 C34 H34A 110.5 . . ?
C35 C34 H34B 110.5 . . ?
N8 C35 C34 112.4(4) . . ?
N8 C35 H35A 109.1 . . ?
N8 C35 H35B 109.1 . . ?
C34 C35 H35A 109.1 . . ?
C34 C35 H35B 109.1 . . ?
H35A C35 H35B 107.9 . . ?
N4 C36 H36A 110.0 . . ?
N4 C36 H36B 110.0 . . ?
N4 C36 C37 108.4(5) . . ?
H36A C36 H36B 108.4 . . ?
C37 C36 H36A 110.0 . . ?
C37 C36 H36B 110.0 . . ?
N8 C37 C36 111.1(5) . . ?
N8 C37 H37A 109.4 . . ?
N8 C37 H37B 109.4 . . ?
C36 C37 H37A 109.4 . . ?
C36 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
N6 C38 H38A 109.4 . . ?
N6 C38 H38B 109.4 . . ?
N6 C38 C39 111.1(5) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
N8 C39 C38 110.7(5) . . ?
N8 C39 H39A 109.5 . . ?
N8 C39 H39B 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 108.1 . . ?
O10 N11 O11 125.6(15) . . ?
O12 N11 O10 119.4(15) . . ?
O12 N11 O11 114.9(16) . . ?
O10A N11A O11A 117.2(13) . . ?
O12A N11A O10A 122.5(16) . . ?
O12A N11A O11A 120.3(15) . . ?
H13A O13 H13A 0.0 . . ?
H13A O13 H13B 86.9 . . ?
H13A O13 H13B 86.9 . . ?
H13C O13A H13D 101.8 . . ?
H14A O14 H14A 105.0 . 7_466 ?
H15 O15 H15 96(6) . 8_665 ?
H16D O16 H16D 140.5 . 7_466 ?
H16D O16 H16E 109.7 . . ?
H16E O16 H16D 109.7 . 7_466 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O14 H14A O8 0.84 2.08 2.850(4) 150.8 . yes
O16 H16E O14 0.83 1.93 2.760 180.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C1 C2 35.9(7) . . . . ?
Y1 O1 C1 C6 -145.1(4) . . . . ?
Y1 O2 C10 C11 44.8(8) . . . . ?
Y1 O2 C10 C15 -135.5(5) . . . . ?
Y1 O3 C19 C20 12.1(8) . . . . ?
Y1 O3 C19 C24 -168.7(4) . . . . ?
Y1 O4 N9 O5 4.8(5) . . . . ?
Y1 O4 N9 O6 143.6(8) . . . . ?
Y1 O5 N9 O4 -7.1(8) . . . . ?
Y1 O5 N9 O4A 81.1(10) . . . . ?
Y1 O5 N9 O6 -141.9(6) . . . . ?
Y1 N1 C8 C2 -12.7(9) . . . . ?
Y1 N1 C28 C29 -55.3(5) . . . . ?
Y1 N3 C17 C11 -11.4(10) . . . . ?
Y1 N3 C30 C31 -64.7(7) . . . . ?
Y1 N5 C26 C20 21.4(10) . . . . ?
Y1 N5 C32 C33 9.8(9) . . . . ?
Y1 N7 C29 C28 -36.1(5) . . . . ?
Y1 N7 C31 C30 -19.4(7) . . . . ?
Y1 N7 C33 C32 55.1(6) . . . . ?
Y2 O1 C1 C2 -137.8(4) . . . . ?
Y2 O1 C1 C6 41.3(8) . . . . ?
Y2 O2 C10 C11 -144.1(4) . . . . ?
Y2 O2 C10 C15 35.5(7) . . . . ?
Y2 O3 C19 C20 -172.1(4) . . . . ?
Y2 O3 C19 C24 7.1(8) . . . . ?
Y2 O7 N10 O8 -6.4(5) . . . . ?
Y2 O7 N10 O9 172.8(6) . . . . ?
Y2 O8 N10 O7 7.7(6) . . . . ?
Y2 O8 N10 O9 -171.6(5) . . . . ?
Y2 N2 C9 C6 -11.2(9) . . . . ?
Y2 N2 C34 C35 -64.3(5) . . . . ?
Y2 N4 C18 C15 -9.2(9) . . . . ?
Y2 N4 C36 C37 -54.7(6) . . . . ?
Y2 N6 C27 C24 14.5(8) . . . . ?
Y2 N6 C38 C39 8.8(7) . . . . ?
Y2 N8 C35 C34 -17.9(7) . . . . ?
Y2 N8 C37 C36 -36.6(6) . . . . ?
Y2 N8 C39 C38 55.4(5) . . . . ?
O1 C1 C2 C3 -176.9(5) . . . . ?
O1 C1 C2 C8 2.1(9) . . . . ?
O1 C1 C6 C5 174.0(5) . . . . ?
O1 C1 C6 C9 -4.6(8) . . . . ?
O2 C10 C11 C12 177.1(5) . . . . ?
O2 C10 C11 C17 -6.1(9) . . . . ?
O2 C10 C15 C14 -177.2(5) . . . . ?
O2 C10 C15 C18 1.3(9) . . . . ?
O3 C19 C20 C21 176.6(5) . . . . ?
O3 C19 C20 C26 -7.3(9) . . . . ?
O3 C19 C24 C23 -179.4(5) . . . . ?
O3 C19 C24 C27 -3.9(9) . . . . ?
N1 C28 C29 N7 60.2(6) . . . . ?
N2 C34 C35 N8 52.1(7) . . . . ?
N3 C30 C31 N7 53.1(8) . . . . ?
N4 C36 C37 N8 61.1(7) . . . . ?
N5 C32 C33 N7 -45.5(9) . . . . ?
N6 C38 C39 N8 -45.1(7) . . . . ?
C1 C2 C3 C4 1.5(9) . . . . ?
C1 C2 C8 N1 -13.3(10) . . . . ?
C1 C6 C9 N2 -8.0(9) . . . . ?
C2 C1 C6 C5 -6.9(8) . . . . ?
C2 C1 C6 C9 174.5(5) . . . . ?
C2 C3 C4 C5 -4.3(9) . . . . ?
C2 C3 C4 C7 176.9(6) . . . . ?
C3 C2 C8 N1 165.7(6) . . . . ?
C3 C4 C5 C6 1.4(9) . . . . ?
C4 C5 C6 C1 4.2(9) . . . . ?
C4 C5 C6 C9 -177.1(5) . . . . ?
C5 C6 C9 N2 173.4(6) . . . . ?
C6 C1 C2 C3 4.1(8) . . . . ?
C6 C1 C2 C8 -176.9(5) . . . . ?
C7 C4 C5 C6 -179.8(6) . . . . ?
C8 N1 C28 C29 105.3(6) . . . . ?
C8 C2 C3 C4 -177.5(6) . . . . ?
C9 N2 C34 C35 100.7(6) . . . . ?
C10 C11 C12 C13 1.3(9) . . . . ?
C10 C11 C17 N3 -8.4(10) . . . . ?
C10 C15 C18 N4 -13.9(10) . . . . ?
C11 C10 C15 C14 2.5(8) . . . . ?
C11 C10 C15 C18 -179.0(6) . . . . ?
C11 C12 C13 C14 0.3(10) . . . . ?
C11 C12 C13 C16 -178.9(6) . . . . ?
C12 C11 C17 N3 168.5(6) . . . . ?
C12 C13 C14 C15 -0.4(10) . . . . ?
C13 C14 C15 C10 -1.0(9) . . . . ?
C13 C14 C15 C18 -179.6(6) . . . . ?
C14 C15 C18 N4 164.7(6) . . . . ?
C15 C10 C11 C12 -2.6(8) . . . . ?
C15 C10 C11 C17 174.2(5) . . . . ?
C16 C13 C14 C15 178.8(6) . . . . ?
C17 N3 C30 C31 98.9(7) . . . . ?
C17 C11 C12 C13 -175.7(6) . . . . ?
C18 N4 C36 C37 108.3(6) . . . . ?
C19 C20 C21 C22 3.1(9) . . . . ?
C19 C20 C26 N5 -11.2(11) . . . . ?
C19 C24 C27 N6 -8.2(10) . . . . ?
C20 C19 C24 C23 -0.1(8) . . . . ?
C20 C19 C24 C27 175.4(5) . . . . ?
C20 C21 C22 C23 -0.5(9) . . . . ?
C20 C21 C22 C25 -179.2(6) . . . . ?
C21 C20 C26 N5 165.2(6) . . . . ?
C21 C22 C23 C24 -2.5(8) . . . . ?
C22 C23 C24 C19 2.8(9) . . . . ?
C22 C23 C24 C27 -173.4(5) . . . . ?
C23 C24 C27 N6 167.6(6) . . . . ?
C24 C19 C20 C21 -2.7(8) . . . . ?
C24 C19 C20 C26 173.5(6) . . . . ?
C25 C22 C23 C24 176.2(6) . . . . ?
C26 N5 C32 C33 -157.4(7) . . . . ?
C26 C20 C21 C22 -173.5(6) . . . . ?
C27 N6 C38 C39 -164.8(5) . . . . ?
C28 N1 C8 C2 -170.8(6) . . . . ?
C29 N7 C31 C30 -140.7(6) . . . . ?
C29 N7 C33 C32 172.9(5) . . . . ?
C30 N3 C17 C11 -171.2(6) . . . . ?
C31 N7 C29 C28 87.0(5) . . . . ?
C31 N7 C33 C32 -66.9(6) . . . . ?
C32 N5 C26 C20 -172.4(7) . . . . ?
C33 N7 C29 C28 -151.5(5) . . . . ?
C33 N7 C31 C30 98.5(6) . . . . ?
C34 N2 C9 C6 -172.4(5) . . . . ?
C35 N8 C37 C36 86.2(6) . . . . ?
C35 N8 C39 C38 -65.9(6) . . . . ?
C36 N4 C18 C15 -169.8(6) . . . . ?
C37 N8 C35 C34 -138.3(6) . . . . ?
C37 N8 C39 C38 172.0(5) . . . . ?
C38 N6 C27 C24 -172.3(5) . . . . ?
C39 N8 C35 C34 99.5(6) . . . . ?
C39 N8 C37 C36 -151.5(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.219 0.781 0.750 91.9 27.9 '3 H2O'
2 0.281 0.281 0.000 91.9 27.1 '3 H2O'
3 0.719 0.719 0.500 91.9 26.8 '3 H2O'
4 0.781 0.219 0.250 91.9 28.4 '3 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_original_sample_id D8V4644
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4671_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc2747j5
_database_code_depnum_ccdc_archive 'CCDC 2059656'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.13667729.v1 2021
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-02-03 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_audit_creation_date             2021-02-03
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H45 Lu2 N10 O9, N O3, 2.5(H2 O)'
_chemical_formula_sum            'C39 H50 Lu2 N11 O14.50'
_chemical_formula_weight         1254.84
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Lu Lu -0.4720 5.8584 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+3/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+1/4'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   17.5856(5)
_cell_length_b                   17.5856(5)
_cell_length_c                   28.9382(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8949.2(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.697
_cell_measurement_theta_min      2.672
_shelx_estimated_absorpt_T_max   0.760
_shelx_estimated_absorpt_T_min   0.359
_exptl_absorpt_coefficient_mu    4.467
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.7640.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 1.00 0.00 0.0280
-1.00 -1.00 0.00 0.0370
0.00 0.00 -1.00 0.1430
0.00 0.00 1.00 0.1440
-1.00 1.00 0.00 0.0200
1.00 -1.00 0.00 0.0320

_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.065
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            117907
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.823
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10520
_reflns_number_total             11099
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.967
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 
;
 Flack x determined using 4500 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11099
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.544
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0266P)²+14.4997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0572
_refine_special_details          
;
One of the nitrate ligands was modelled as disordered, consistent with peaks in a difference map.  The nitrate counterion and one water of crystallization were modelled as disordered over two sites with geometric and displacement ellipsoid restraints used.  In all cases water H atoms were identified from difference peaks which corresponded with likely hydrogen bonding interactions.  Water H atoms were refined using a riding model with geometric restraints.  One of the water molecules lies on a special position, hence a fractional value in the chemical formula.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

420_ALERT_2_B D-H Without Acceptor       O13      --H13B     .     Please Check

See above

#===============================================================================
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.69 Report

This rogue peak does not correspond to anything chemically sensible. It refines to 1/3 of an oxygen site.

161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .        O13 Check
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .       O13A Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .        O13 Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .       O13A Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .        O13 Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .       O13A Check
213_ALERT_2_C Atom O4A             has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom O4              has ADP max/min Ratio .....        3.8 prolat
213_ALERT_2_C Atom C16             has ADP max/min Ratio .....        3.1 prolat
218_ALERT_3_C Constrained U(ij) Components(s) for O13        .          6 Check
218_ALERT_3_C Constrained U(ij) Components(s) for O13A       .          6 Check
220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        4.4 Ratio
220_ALERT_2_C NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        4.8 Ratio
222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.2 Ratio
234_ALERT_4_C Large Hirshfeld Difference O4A      --N9       .       0.19 Ang.

All pertain to disorder, discussed above.

342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00873 Ang.
601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         77 Ang**3
911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         12 Report
971_ALERT_2_C Check Calcd Resid. Dens.  2.94A   From O9              2.08 eA-3
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-Lu1 = O2-Lu2 = O2-C10
 0.84 with sigma of 0.02
 O16-H16D = O16-H16E = O14-H14A = O13A-H13C = O13A-H13D = O13-H13A = O13-H13B
 0.84 with sigma of 0.02
 O15-H15_$2
 0.84 with sigma of 0.02
 H16D_$3-H16E
 1.35 with sigma of 0.04
 H13B-H13A = H13D-H13C = H16E_$1-H16D_$4
 1.35 with sigma of 0.04
 H15_$2-H15
 1.35 with sigma of 0.04
 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim
O12-N11
 with sigma of 0.02
 O4A-N9 \\sim O4-N9
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O10, O11, O12, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10A, O11A, O12A, N11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, O11, O12, N11}
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, O11A, O12A, N11A}
5. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5)
 N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5)
6.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O16, H16D, H16E
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C21(H21), C23(H23), C26(H26), C27(H27)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Lu1 Lu 0.14166(2) 0.61176(2) 0.39634(2) 0.01650(5) Uani 1 1 d D . . . .
Lu2 Lu 0.05391(2) 0.68437(2) 0.49297(2) 0.01699(5) Uani 1 1 d D . . . .
O1 O 0.1738(2) 0.6470(2) 0.46949(12) 0.0182(7) Uani 1 1 d . . . . .
O2 O 0.0841(2) 0.7209(2) 0.42092(12) 0.0204(8) Uani 1 1 d D . . . .
O3 O 0.0428(2) 0.5760(2) 0.44662(13) 0.0211(8) Uani 1 1 d . . . . .
O5 O 0.2428(3) 0.5338(3) 0.41490(16) 0.0345(10) Uani 1 1 d . . . . .
O6 O 0.3018(3) 0.4632(3) 0.4646(2) 0.0516(14) Uani 1 1 d . . . A 1
O7 O -0.0807(3) 0.6893(3) 0.43220(15) 0.0372(11) Uani 1 1 d D . . . .
O8 O -0.0390(2) 0.7785(2) 0.47703(13) 0.0258(8) Uani 1 1 d D . . . .
O9 O -0.1318(4) 0.8013(3) 0.4300(2) 0.0595(17) Uani 1 1 d D . . . .
N10 N -0.0856(3) 0.7563(3) 0.44604(18) 0.0315(12) Uani 1 1 d D . . . .
N1 N 0.2503(3) 0.6893(3) 0.38504(15) 0.0194(9) Uani 1 1 d . . . . .
N2 N 0.1189(3) 0.6251(3) 0.55702(15) 0.0231(10) Uani 1 1 d . . . . .
N3 N 0.0712(3) 0.6651(4) 0.33262(16) 0.0311(12) Uani 1 1 d . . . . .
N4 N 0.1119(3) 0.8041(3) 0.50493(16) 0.0240(10) Uani 1 1 d . . . . .
N5 N 0.1068(3) 0.4899(3) 0.36505(18) 0.0309(12) Uani 1 1 d . . . . .
N6 N -0.0584(3) 0.6298(3) 0.52597(16) 0.0218(9) Uani 1 1 d . . . . .
N7 N 0.2046(3) 0.5863(3) 0.31577(16) 0.0246(10) Uani 1 1 d . . . . .
N8 N 0.0179(3) 0.7418(3) 0.57467(16) 0.0264(10) Uani 1 1 d . . . . .
N9 N 0.2501(4) 0.4746(5) 0.4391(2) 0.0520(18) Uani 1 1 d D . . . .
C1 C 0.2420(3) 0.6518(3) 0.48785(18) 0.0187(10) Uani 1 1 d . . . . .
C2 C 0.3069(3) 0.6743(3) 0.46198(17) 0.0205(10) Uani 1 1 d . . . . .
C3 C 0.3784(3) 0.6732(3) 0.48265(19) 0.0248(12) Uani 1 1 d . . . . .
H3 H 0.421311 0.687867 0.464792 0.030 Uiso 1 1 calc R U . . .
C4 C 0.3897(4) 0.6514(4) 0.52837(19) 0.0283(12) Uani 1 1 d . . . . .
C5 C 0.3259(4) 0.6345(3) 0.55438(19) 0.0249(12) Uani 1 1 d . . . . .
H5 H 0.331912 0.621650 0.586056 0.030 Uiso 1 1 calc R U . . .
C6 C 0.2530(3) 0.6358(3) 0.53539(18) 0.0219(11) Uani 1 1 d . . . . .
C7 C 0.4691(4) 0.6489(5) 0.5483(2) 0.0428(18) Uani 1 1 d . . . . .
H7A H 0.486811 0.700815 0.554193 0.064 Uiso 1 1 calc R U . . .
H7B H 0.503377 0.624064 0.526236 0.064 Uiso 1 1 calc R U . . .
H7C H 0.468604 0.620156 0.577286 0.064 Uiso 1 1 calc R U . . .
C8 C 0.3049(3) 0.6969(3) 0.41355(19) 0.0215(11) Uani 1 1 d . . . . .
H8 H 0.349659 0.720222 0.401854 0.026 Uiso 1 1 calc R U . . .
C9 C 0.1902(4) 0.6194(3) 0.56623(18) 0.0241(12) Uani 1 1 d . . . . .
H9 H 0.203018 0.602750 0.596456 0.029 Uiso 1 1 calc R U . . .
C10 C 0.0790(3) 0.7894(3) 0.40216(19) 0.0218(11) Uani 1 1 d D . . . .
C11 C 0.0610(3) 0.7982(4) 0.3543(2) 0.0314(14) Uani 1 1 d . . . . .
C12 C 0.0516(4) 0.8712(5) 0.3348(3) 0.044(2) Uani 1 1 d . . . . .
H12 H 0.037976 0.875012 0.303152 0.053 Uiso 1 1 calc R U . . .
C13 C 0.0612(4) 0.9369(5) 0.3598(3) 0.048(2) Uani 1 1 d . . . . .
C14 C 0.0820(4) 0.9288(4) 0.4060(3) 0.0392(17) Uani 1 1 d . . . . .
H14 H 0.089762 0.973410 0.423921 0.047 Uiso 1 1 calc R U . . .
C15 C 0.0920(3) 0.8573(3) 0.4274(2) 0.0275(12) Uani 1 1 d . . . . .
C16 C 0.0512(5) 1.0153(5) 0.3393(4) 0.071(3) Uani 1 1 d . . . . .
H16A H 0.012058 1.042935 0.356612 0.106 Uiso 1 1 calc R U . . .
H16B H 0.035691 1.010778 0.306911 0.106 Uiso 1 1 calc R U . . .
H16C H 0.099430 1.043100 0.341148 0.106 Uiso 1 1 calc R U . . .
C17 C 0.0539(4) 0.7340(5) 0.3241(2) 0.0342(15) Uani 1 1 d . . . . .
H17 H 0.034107 0.744045 0.294133 0.041 Uiso 1 1 calc R U . . .
C18 C 0.1136(3) 0.8593(3) 0.4760(2) 0.0279(12) Uani 1 1 d . . . . .
H18 H 0.130945 0.906818 0.487510 0.033 Uiso 1 1 calc R U . . .
C19 C -0.0054(3) 0.5170(3) 0.44762(17) 0.0161(9) Uani 1 1 d . . . . .
C20 C 0.0063(3) 0.4514(3) 0.41955(19) 0.0203(10) Uani 1 1 d . . . . .
C21 C -0.0424(3) 0.3886(3) 0.4232(2) 0.0236(11) Uani 1 1 d . . . . .
H21 H -0.031264 0.344601 0.405403 0.028 Uiso 1 1 calc R U . . .
C22 C -0.1058(3) 0.3874(3) 0.4514(2) 0.0259(12) Uani 1 1 d . . . . .
C23 C -0.1184(3) 0.4516(3) 0.47727(19) 0.0227(11) Uani 1 1 d . . . . .
H23 H -0.162193 0.452890 0.496500 0.027 Uiso 1 1 calc R U . . .
C24 C -0.0701(3) 0.5158(3) 0.47697(18) 0.0186(10) Uani 1 1 d . . . . .
C25 C -0.1544(4) 0.3178(4) 0.4543(3) 0.0450(18) Uani 1 1 d . . . . .
H25A H -0.127832 0.278504 0.472097 0.067 Uiso 1 1 calc R U . . .
H25B H -0.164764 0.298775 0.423078 0.067 Uiso 1 1 calc R U . . .
H25C H -0.202508 0.330350 0.469597 0.067 Uiso 1 1 calc R U . . .
C26 C 0.0632(3) 0.4411(3) 0.3836(2) 0.0259(12) Uani 1 1 d . . . . .
H26 H 0.068563 0.390570 0.372405 0.031 Uiso 1 1 calc R U . . .
C27 C -0.0937(3) 0.5711(3) 0.51080(18) 0.0207(10) Uani 1 1 d . . . . .
H27 H -0.142655 0.562932 0.523747 0.025 Uiso 1 1 calc R U . . .
C28 C 0.2672(3) 0.7075(3) 0.33637(18) 0.0219(11) Uani 1 1 d . . . . .
H28A H 0.314621 0.737497 0.334008 0.026 Uiso 1 1 calc R U . . .
H28B H 0.225108 0.737109 0.322476 0.026 Uiso 1 1 calc R U . . .
C29 C 0.2760(3) 0.6310(4) 0.31186(19) 0.0237(12) Uani 1 1 d . . . . .
H29A H 0.288213 0.639477 0.278865 0.028 Uiso 1 1 calc R U . . .
H29B H 0.318489 0.602156 0.325954 0.028 Uiso 1 1 calc R U . . .
C30 C 0.0693(4) 0.6135(6) 0.2925(2) 0.0439(19) Uani 1 1 d . . . . .
H30A H 0.037005 0.634613 0.267583 0.053 Uiso 1 1 calc R U . . .
H30B H 0.049319 0.562922 0.301398 0.053 Uiso 1 1 calc R U . . .
C31 C 0.1526(3) 0.6075(5) 0.27663(19) 0.0347(15) Uani 1 1 d . . . . .
H31A H 0.156560 0.568748 0.251946 0.042 Uiso 1 1 calc R U . . .
H31B H 0.168833 0.656922 0.263551 0.042 Uiso 1 1 calc R U . . .
C32 C 0.1507(4) 0.4582(5) 0.3252(3) 0.047(2) Uani 1 1 d . . . . .
H32A H 0.117732 0.457358 0.297447 0.056 Uiso 1 1 calc R U . . .
H32B H 0.165627 0.405214 0.332219 0.056 Uiso 1 1 calc R U . . .
C33 C 0.2217(4) 0.5047(4) 0.3148(2) 0.0337(15) Uani 1 1 d . . . . .
H33A H 0.261373 0.493082 0.338008 0.040 Uiso 1 1 calc R U . . .
H33B H 0.241582 0.490662 0.283969 0.040 Uiso 1 1 calc R U . . .
C34 C 0.0686(4) 0.6146(4) 0.59743(19) 0.0289(13) Uani 1 1 d . . . . .
H34A H 0.095536 0.586731 0.622277 0.035 Uiso 1 1 calc R U . . .
H34B H 0.022655 0.585458 0.588666 0.035 Uiso 1 1 calc R U . . .
C35 C 0.0474(4) 0.6935(4) 0.61333(18) 0.0313(13) Uani 1 1 d . . . . .
H35A H 0.008056 0.689755 0.637695 0.038 Uiso 1 1 calc R U . . .
H35B H 0.092657 0.718334 0.627010 0.038 Uiso 1 1 calc R U . . .
C36 C 0.1257(4) 0.8238(4) 0.5533(2) 0.0319(14) Uani 1 1 d . . . . .
H36A H 0.147353 0.875642 0.555604 0.038 Uiso 1 1 calc R U . . .
H36B H 0.161831 0.787485 0.567401 0.038 Uiso 1 1 calc R U . . .
C37 C 0.0488(4) 0.8201(4) 0.5779(2) 0.0323(14) Uani 1 1 d . . . . .
H37A H 0.055139 0.834476 0.610782 0.039 Uiso 1 1 calc R U . . .
H37B H 0.012990 0.856456 0.563468 0.039 Uiso 1 1 calc R U . . .
C38 C -0.0993(4) 0.6666(4) 0.5652(2) 0.0296(13) Uani 1 1 d . . . . .
H38A H -0.095692 0.633830 0.592984 0.036 Uiso 1 1 calc R U . . .
H38B H -0.153759 0.672355 0.557295 0.036 Uiso 1 1 calc R U . . .
C39 C -0.0651(4) 0.7449(4) 0.5759(2) 0.0299(13) Uani 1 1 d . . . . .
H39A H -0.083455 0.782398 0.552952 0.036 Uiso 1 1 calc R U . . .
H39B H -0.082010 0.761850 0.606903 0.036 Uiso 1 1 calc R U . . .
O10 O 0.4503(7) 0.7052(8) 0.2938(5) 0.073(4) Uani 0.5 1 d D . P B 1
O11 O 0.4729(9) 0.7352(8) 0.3680(6) 0.094(5) Uani 0.5 1 d D . P B 1
O12 O 0.5032(12) 0.6275(9) 0.3414(6) 0.108(7) Uani 0.5 1 d D . P B 1
N11 N 0.4762(7) 0.6913(6) 0.3326(5) 0.049(3) Uani 0.5 1 d D . P B 1
O10A O -0.2804(8) 0.5777(9) 0.5506(4) 0.080(5) Uani 0.5 1 d D . P C 2
O11A O -0.2276(7) 0.4884(7) 0.5869(4) 0.061(3) Uani 0.5 1 d D . P C 2
O12A O -0.3086(8) 0.5585(10) 0.6232(4) 0.080(4) Uani 0.5 1 d D . P C 2
N11A N -0.2740(6) 0.5434(6) 0.5880(3) 0.031(2) Uani 0.5 1 d D . P C 2
O13 O -0.264370 0.562200 0.561150 0.092 Uani 0.5 1 d D . P D 1
H13A H -0.294050 0.564530 0.589850 0.110 Uiso 0.5 1 d D U P E 1
H13B H -0.305990 0.597760 0.546630 0.110 Uiso 0.5 1 d D U P F 1
O13A O 0.197590 1.032020 0.543840 0.043 Uani 0.5 1 d D . P G 2
H13C H 0.152220 1.035730 0.534420 0.051 Uiso 0.5 1 d D U P H 2
H13D H 0.191110 1.021250 0.572570 0.051 Uiso 0.5 1 d D U P I 2
O14 O -0.060260 0.939740 0.500000 0.045 Uani 1 2 d DS T P . .
H14A H -0.061250 0.899460 0.484250 0.054 Uiso 1 1 d D U . . .
O15 O 0.3059(2) 0.3059(2) 0.500000 0.0371(15) Uani 1 2 d DS T P . .
H15 H 0.305(3) 0.351(2) 0.488(2) 0.044 Uiso 1 1 d D U . . .
O16 O 0.050600 1.050600 0.500000 0.053 Uani 1 2 d DS T P . .
H16D H 0.080320 1.043180 0.521350 0.064 Uiso 0.5 1 d D U P . .
H16E H 0.017230 1.017230 0.500000 0.064 Uiso 1 2 d DS U P . .
O4 O 0.1810(7) 0.4648(13) 0.4539(5) 0.072(8) Uani 0.407(18) 1 d D . P A 1
O4A O 0.2230(8) 0.4062(6) 0.4231(6) 0.088(6) Uani 0.593(18) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 Lu2 3.4395(3) . ?
Lu1 O1 2.277(3) . ?
Lu1 O2 2.283(4) . ?
Lu1 O3 2.352(4) . ?
Lu1 O5 2.309(4) . ?
Lu1 N1 2.369(5) . ?
Lu1 N3 2.411(5) . ?
Lu1 N5 2.405(5) . ?
Lu1 N7 2.619(5) . ?
Lu1 O4 3.152(18) . ?
Lu2 O1 2.311(4) . ?
Lu2 O2 2.245(4) . ?
Lu2 O3 2.339(4) . ?
Lu2 O7 2.950(5) . ?
Lu2 O8 2.372(4) . ?
Lu2 N2 2.414(5) . ?
Lu2 N4 2.365(5) . ?
Lu2 N6 2.394(5) . ?
Lu2 N8 2.648(5) . ?
O1 C1 1.313(7) . ?
O2 C10 1.325(6) . ?
O3 C19 1.340(6) . ?
O5 N9 1.263(8) . ?
O6 N9 1.187(8) . ?
O7 N10 1.246(7) . ?
O8 N10 1.276(7) . ?
O9 N10 1.227(7) . ?
N1 C8 1.273(7) . ?
N1 C28 1.475(7) . ?
N2 C9 1.285(8) . ?
N2 C34 1.478(7) . ?
N3 C17 1.274(9) . ?
N3 C30 1.475(8) . ?
N4 C18 1.283(8) . ?
N4 C36 1.462(8) . ?
N5 C26 1.271(8) . ?
N5 C32 1.496(8) . ?
N6 C27 1.281(7) . ?
N6 C38 1.493(7) . ?
N7 C29 1.486(7) . ?
N7 C31 1.503(8) . ?
N7 C33 1.467(9) . ?
N8 C35 1.497(8) . ?
N8 C37 1.485(8) . ?
N8 C39 1.461(8) . ?
N9 O4 1.299(12) . ?
N9 O4A 1.374(12) . ?
C1 C2 1.421(7) . ?
C1 C6 1.417(7) . ?
C2 C3 1.393(8) . ?
C2 C8 1.458(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(8) . ?
C4 C5 1.383(9) . ?
C4 C7 1.511(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.395(8) . ?
C6 C9 1.449(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.429(8) . ?
C10 C15 1.419(9) . ?
C11 C12 1.412(10) . ?
C11 C17 1.434(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(13) . ?
C13 C14 1.393(12) . ?
C13 C16 1.512(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.414(8) . ?
C15 C18 1.456(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.426(7) . ?
C19 C24 1.420(7) . ?
C20 C21 1.402(7) . ?
C20 C26 1.455(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.381(8) . ?
C22 C23 1.372(9) . ?
C22 C25 1.496(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.413(8) . ?
C24 C27 1.442(8) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.529(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.537(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.522(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.510(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.529(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.535(9) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
O10 N11 1.235(14) . ?
O11 N11 1.284(14) . ?
O12 N11 1.245(14) . ?
O10A N11A 1.243(12) . ?
O11A N11A 1.266(12) . ?
O12A N11A 1.216(12) . ?
O13 H13A 0.9818 . ?
O13 H13A 0.9818 . ?
O13 H13B 1.0504 . ?
O13A H13C 0.8457 . ?
O13A H13D 0.8603 . ?
O14 H14A 0.8424 7_466 ?
O14 H14A 0.8425 . ?
O15 H15 0.86(3) 7_556 ?
O15 H15 0.86(3) . ?
O16 H16D 0.8197 . ?
O16 H16D 0.8197 7_466 ?
O16 H16E 0.8299 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Lu1 Lu2 41.81(9) . . ?
O1 Lu1 O2 65.90(14) . . ?
O1 Lu1 O3 71.43(13) . . ?
O1 Lu1 O5 75.76(15) . . ?
O1 Lu1 N1 76.78(14) . . ?
O1 Lu1 N3 137.11(17) . . ?
O1 Lu1 N5 130.99(17) . . ?
O1 Lu1 N7 140.27(14) . . ?
O1 Lu1 O4 71.2(4) . . ?
O2 Lu1 Lu2 40.16(9) . . ?
O2 Lu1 O3 72.82(13) . . ?
O2 Lu1 O5 140.18(15) . . ?
O2 Lu1 N1 85.23(15) . . ?
O2 Lu1 N3 71.56(16) . . ?
O2 Lu1 N5 138.83(17) . . ?
O2 Lu1 N7 127.45(15) . . ?
O2 Lu1 O4 128.4(3) . . ?
O3 Lu1 Lu2 42.70(9) . . ?
O3 Lu1 N1 146.61(14) . . ?
O3 Lu1 N3 101.39(15) . . ?
O3 Lu1 N5 78.82(15) . . ?
O3 Lu1 N7 144.77(14) . . ?
O3 Lu1 O4 67.4(3) . . ?
O5 Lu1 Lu2 112.14(12) . . ?
O5 Lu1 O3 105.45(16) . . ?
O5 Lu1 N1 75.67(17) . . ?
O5 Lu1 N3 143.56(17) . . ?
O5 Lu1 N5 75.84(18) . . ?
O5 Lu1 N7 77.31(16) . . ?
O5 Lu1 O4 38.9(2) . . ?
N1 Lu1 Lu2 105.09(11) . . ?
N1 Lu1 N3 94.87(18) . . ?
N1 Lu1 N5 131.76(16) . . ?
N1 Lu1 N7 68.59(15) . . ?
N1 Lu1 O4 111.6(2) . . ?
N3 Lu1 Lu2 104.29(12) . . ?
N3 Lu1 N7 66.58(16) . . ?
N3 Lu1 O4 146.7(3) . . ?
N5 Lu1 Lu2 121.49(12) . . ?
N5 Lu1 N3 85.8(2) . . ?
N5 Lu1 N7 67.69(16) . . ?
N5 Lu1 O4 61.6(4) . . ?
N7 Lu1 Lu2 167.58(12) . . ?
N7 Lu1 O4 103.8(3) . . ?
O4 Lu1 Lu2 88.5(3) . . ?
O1 Lu2 Lu1 41.07(9) . . ?
O1 Lu2 O3 71.09(13) . . ?
O1 Lu2 O7 124.44(12) . . ?
O1 Lu2 O8 140.36(13) . . ?
O1 Lu2 N2 70.79(14) . . ?
O1 Lu2 N4 84.38(15) . . ?
O1 Lu2 N6 139.11(14) . . ?
O1 Lu2 N8 126.10(14) . . ?
O2 Lu2 Lu1 40.99(10) . . ?
O2 Lu2 O1 65.95(13) . . ?
O2 Lu2 O3 73.75(13) . . ?
O2 Lu2 O7 68.14(14) . . ?
O2 Lu2 O8 77.45(14) . . ?
O2 Lu2 N2 136.43(15) . . ?
O2 Lu2 N4 77.26(15) . . ?
O2 Lu2 N6 132.84(16) . . ?
O2 Lu2 N8 140.96(15) . . ?
O3 Lu2 Lu1 43.00(9) . . ?
O3 Lu2 O7 67.39(13) . . ?
O3 Lu2 O8 113.58(14) . . ?
O3 Lu2 N2 97.36(15) . . ?
O3 Lu2 N4 147.71(14) . . ?
O3 Lu2 N6 80.40(14) . . ?
O3 Lu2 N8 143.41(14) . . ?
O7 Lu2 Lu1 83.48(9) . . ?
O8 Lu2 Lu1 114.22(9) . . ?
O8 Lu2 O7 46.41(13) . . ?
O8 Lu2 N2 140.97(14) . . ?
O8 Lu2 N6 77.83(15) . . ?
O8 Lu2 N8 75.08(14) . . ?
N2 Lu2 Lu1 104.57(10) . . ?
N2 Lu2 O7 148.26(15) . . ?
N2 Lu2 N8 65.94(15) . . ?
N4 Lu2 Lu1 104.83(11) . . ?
N4 Lu2 O7 114.03(15) . . ?
N4 Lu2 O8 72.81(16) . . ?
N4 Lu2 N2 93.86(17) . . ?
N4 Lu2 N6 130.87(16) . . ?
N4 Lu2 N8 68.47(16) . . ?
N6 Lu2 Lu1 123.06(11) . . ?
N6 Lu2 O7 65.66(15) . . ?
N6 Lu2 N2 84.91(16) . . ?
N6 Lu2 N8 66.38(16) . . ?
N8 Lu2 Lu1 167.12(11) . . ?
N8 Lu2 O7 109.20(14) . . ?
Lu1 O1 Lu2 97.12(14) . . ?
C1 O1 Lu1 128.3(3) . . ?
C1 O1 Lu2 134.1(3) . . ?
Lu2 O2 Lu1 98.85(14) . . ?
C10 O2 Lu1 131.8(3) . . ?
C10 O2 Lu2 128.7(3) . . ?
Lu2 O3 Lu1 94.30(13) . . ?
C19 O3 Lu1 133.5(3) . . ?
C19 O3 Lu2 132.1(3) . . ?
N9 O5 Lu1 134.2(4) . . ?
N10 O7 Lu2 83.8(3) . . ?
N10 O8 Lu2 111.4(3) . . ?
O7 N10 O8 118.1(5) . . ?
O9 N10 O7 122.2(6) . . ?
O9 N10 O8 119.6(5) . . ?
C8 N1 Lu1 125.4(4) . . ?
C8 N1 C28 116.4(5) . . ?
C28 N1 Lu1 114.8(3) . . ?
C9 N2 Lu2 130.9(4) . . ?
C9 N2 C34 114.2(5) . . ?
C34 N2 Lu2 112.2(4) . . ?
C17 N3 Lu1 129.9(4) . . ?
C17 N3 C30 115.3(6) . . ?
C30 N3 Lu1 112.0(5) . . ?
C18 N4 Lu2 126.0(4) . . ?
C18 N4 C36 116.2(5) . . ?
C36 N4 Lu2 115.0(4) . . ?
C26 N5 Lu1 126.7(4) . . ?
C26 N5 C32 112.7(5) . . ?
C32 N5 Lu1 119.4(4) . . ?
C27 N6 Lu2 125.9(4) . . ?
C27 N6 C38 112.1(5) . . ?
C38 N6 Lu2 121.8(4) . . ?
C29 N7 Lu1 109.6(3) . . ?
C29 N7 C31 109.1(5) . . ?
C31 N7 Lu1 111.8(3) . . ?
C33 N7 Lu1 105.7(4) . . ?
C33 N7 C29 110.0(5) . . ?
C33 N7 C31 110.7(5) . . ?
C35 N8 Lu2 111.6(3) . . ?
C37 N8 Lu2 108.8(3) . . ?
C37 N8 C35 110.6(5) . . ?
C39 N8 Lu2 106.0(3) . . ?
C39 N8 C35 110.4(5) . . ?
C39 N8 C37 109.2(5) . . ?
O5 N9 O4 101.4(10) . . ?
O5 N9 O4A 120.0(8) . . ?
O6 N9 O5 124.1(7) . . ?
O6 N9 O4 119.2(8) . . ?
O1 C1 C2 122.5(5) . . ?
O1 C1 C6 120.3(5) . . ?
C6 C1 C2 117.2(5) . . ?
C1 C2 C8 124.3(5) . . ?
C3 C2 C1 119.7(5) . . ?
C3 C2 C8 116.0(5) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.7(5) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C7 120.1(6) . . ?
C5 C4 C3 117.4(6) . . ?
C5 C4 C7 122.4(6) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(5) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C9 122.2(5) . . ?
C5 C6 C1 120.7(5) . . ?
C5 C6 C9 117.1(5) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 127.8(5) . . ?
N1 C8 H8 116.1 . . ?
C2 C8 H8 116.1 . . ?
N2 C9 C6 126.9(5) . . ?
N2 C9 H9 116.6 . . ?
C6 C9 H9 116.6 . . ?
O2 C10 C11 120.7(6) . . ?
O2 C10 C15 122.9(5) . . ?
C15 C10 C11 116.4(5) . . ?
C10 C11 C17 121.7(6) . . ?
C12 C11 C10 120.8(7) . . ?
C12 C11 C17 117.5(6) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 C11 122.7(7) . . ?
C13 C12 H12 118.7 . . ?
C12 C13 C14 116.9(6) . . ?
C12 C13 C16 123.2(8) . . ?
C14 C13 C16 120.0(9) . . ?
C13 C14 H14 118.5 . . ?
C13 C14 C15 123.0(7) . . ?
C15 C14 H14 118.5 . . ?
C10 C15 C18 124.1(5) . . ?
C14 C15 C10 120.2(6) . . ?
C14 C15 C18 115.7(6) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C11 127.5(5) . . ?
N3 C17 H17 116.2 . . ?
C11 C17 H17 116.2 . . ?
N4 C18 C15 127.3(5) . . ?
N4 C18 H18 116.4 . . ?
C15 C18 H18 116.4 . . ?
O3 C19 C20 121.5(5) . . ?
O3 C19 C24 122.2(5) . . ?
C24 C19 C20 116.4(5) . . ?
C19 C20 C26 127.4(5) . . ?
C21 C20 C19 120.4(5) . . ?
C21 C20 C26 112.1(5) . . ?
C20 C21 H21 118.3 . . ?
C22 C21 C20 123.3(5) . . ?
C22 C21 H21 118.3 . . ?
C21 C22 C25 120.4(6) . . ?
C23 C22 C21 116.1(5) . . ?
C23 C22 C25 123.4(6) . . ?
C22 C23 H23 118.1 . . ?
C22 C23 C24 123.8(5) . . ?
C24 C23 H23 118.1 . . ?
C19 C24 C27 128.8(5) . . ?
C23 C24 C19 119.9(5) . . ?
C23 C24 C27 111.3(5) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C20 129.2(5) . . ?
N5 C26 H26 115.4 . . ?
C20 C26 H26 115.4 . . ?
N6 C27 C24 129.6(5) . . ?
N6 C27 H27 115.2 . . ?
C24 C27 H27 115.2 . . ?
N1 C28 H28A 110.6 . . ?
N1 C28 H28B 110.6 . . ?
N1 C28 C29 105.8(5) . . ?
H28A C28 H28B 108.7 . . ?
C29 C28 H28A 110.6 . . ?
C29 C28 H28B 110.6 . . ?
N7 C29 C28 110.1(4) . . ?
N7 C29 H29A 109.6 . . ?
N7 C29 H29B 109.6 . . ?
C28 C29 H29A 109.6 . . ?
C28 C29 H29B 109.6 . . ?
H29A C29 H29B 108.2 . . ?
N3 C30 H30A 110.8 . . ?
N3 C30 H30B 110.8 . . ?
N3 C30 C31 104.8(5) . . ?
H30A C30 H30B 108.9 . . ?
C31 C30 H30A 110.8 . . ?
C31 C30 H30B 110.8 . . ?
N7 C31 C30 111.8(5) . . ?
N7 C31 H31A 109.3 . . ?
N7 C31 H31B 109.3 . . ?
C30 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
N5 C32 H32A 109.2 . . ?
N5 C32 H32B 109.2 . . ?
N5 C32 C33 112.0(5) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
N7 C33 C32 110.7(5) . . ?
N7 C33 H33A 109.5 . . ?
N7 C33 H33B 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
N2 C34 H34A 110.6 . . ?
N2 C34 H34B 110.6 . . ?
N2 C34 C35 105.9(5) . . ?
H34A C34 H34B 108.7 . . ?
C35 C34 H34A 110.6 . . ?
C35 C34 H34B 110.6 . . ?
N8 C35 C34 112.3(4) . . ?
N8 C35 H35A 109.1 . . ?
N8 C35 H35B 109.1 . . ?
C34 C35 H35A 109.1 . . ?
C34 C35 H35B 109.1 . . ?
H35A C35 H35B 107.9 . . ?
N4 C36 H36A 110.3 . . ?
N4 C36 H36B 110.3 . . ?
N4 C36 C37 106.9(5) . . ?
H36A C36 H36B 108.6 . . ?
C37 C36 H36A 110.3 . . ?
C37 C36 H36B 110.3 . . ?
N8 C37 C36 109.5(5) . . ?
N8 C37 H37A 109.8 . . ?
N8 C37 H37B 109.8 . . ?
C36 C37 H37A 109.8 . . ?
C36 C37 H37B 109.8 . . ?
H37A C37 H37B 108.2 . . ?
N6 C38 H38A 109.5 . . ?
N6 C38 H38B 109.5 . . ?
N6 C38 C39 110.7(5) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
N8 C39 C38 110.6(5) . . ?
N8 C39 H39A 109.5 . . ?
N8 C39 H39B 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 108.1 . . ?
O10 N11 O11 126.1(15) . . ?
O10 N11 O12 120.3(15) . . ?
O12 N11 O11 113.3(16) . . ?
O10A N11A O11A 114.2(12) . . ?
O12A N11A O10A 125.3(14) . . ?
O12A N11A O11A 120.6(13) . . ?
H13A O13 H13A 0.0 . . ?
H13A O13 H13B 86.7 . . ?
H13A O13 H13B 86.7 . . ?
H13C O13A H13D 101.7 . . ?
H14A O14 H14A 104.9 . 7_466 ?
H15 O15 H15 101(6) . 7_556 ?
H16D O16 H16D 140.5 . 7_466 ?
H16D O16 H16E 109.8 . . ?
H16E O16 H16D 109.8 . 7_466 ?
N9 O4 Lu1 85.6(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O14 H14A O8 0.84 2.17 2.936(4) 150.6 . yes
O16 H16E O14 0.83 1.93 2.757 180.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Lu1 O1 C1 C2 34.1(7) . . . . ?
Lu1 O1 C1 C6 -147.2(4) . . . . ?
Lu1 O2 C10 C11 45.1(7) . . . . ?
Lu1 O2 C10 C15 -134.0(5) . . . . ?
Lu1 O3 C19 C20 13.4(7) . . . . ?
Lu1 O3 C19 C24 -167.5(4) . . . . ?
Lu1 O5 N9 O6 -138.2(6) . . . . ?
Lu1 O5 N9 O4 -0.6(12) . . . . ?
Lu1 O5 N9 O4A 73.6(11) . . . . ?
Lu1 N1 C8 C2 -13.9(8) . . . . ?
Lu1 N1 C28 C29 -57.1(5) . . . . ?
Lu1 N3 C17 C11 -11.5(10) . . . . ?
Lu1 N3 C30 C31 -64.7(7) . . . . ?
Lu1 N5 C26 C20 20.2(10) . . . . ?
Lu1 N5 C32 C33 9.2(9) . . . . ?
Lu1 N7 C29 C28 -35.4(5) . . . . ?
Lu1 N7 C31 C30 -18.5(7) . . . . ?
Lu1 N7 C33 C32 54.3(6) . . . . ?
Lu2 O1 C1 C2 -135.9(4) . . . . ?
Lu2 O1 C1 C6 42.8(7) . . . . ?
Lu2 O2 C10 C11 -146.4(4) . . . . ?
Lu2 O2 C10 C15 34.5(7) . . . . ?
Lu2 O3 C19 C20 -170.5(4) . . . . ?
Lu2 O3 C19 C24 8.6(7) . . . . ?
Lu2 O7 N10 O8 -4.7(5) . . . . ?
Lu2 O7 N10 O9 173.2(7) . . . . ?
Lu2 O8 N10 O7 6.3(6) . . . . ?
Lu2 O8 N10 O9 -171.7(5) . . . . ?
Lu2 N2 C9 C6 -12.4(9) . . . . ?
Lu2 N2 C34 C35 -64.5(5) . . . . ?
Lu2 N4 C18 C15 -10.9(9) . . . . ?
Lu2 N4 C36 C37 -56.9(6) . . . . ?
Lu2 N6 C27 C24 12.5(8) . . . . ?
Lu2 N6 C38 C39 6.7(7) . . . . ?
Lu2 N8 C35 C34 -17.2(6) . . . . ?
Lu2 N8 C37 C36 -36.2(6) . . . . ?
Lu2 N8 C39 C38 54.2(5) . . . . ?
O1 C1 C2 C3 -175.6(5) . . . . ?
O1 C1 C2 C8 2.4(9) . . . . ?
O1 C1 C6 C5 174.6(5) . . . . ?
O1 C1 C6 C9 -4.8(8) . . . . ?
O2 C10 C11 C12 176.6(5) . . . . ?
O2 C10 C11 C17 -5.3(8) . . . . ?
O2 C10 C15 C14 -176.8(5) . . . . ?
O2 C10 C15 C18 1.4(9) . . . . ?
O3 C19 C20 C21 176.2(5) . . . . ?
O3 C19 C20 C26 -7.3(9) . . . . ?
O3 C19 C24 C23 -178.9(5) . . . . ?
O3 C19 C24 C27 -3.2(8) . . . . ?
O5 N9 O4 Lu1 0.3(6) . . . . ?
O6 N9 O4 Lu1 140.6(8) . . . . ?
N1 C28 C29 N7 60.0(6) . . . . ?
N2 C34 C35 N8 51.1(7) . . . . ?
N3 C30 C31 N7 52.2(8) . . . . ?
N4 C36 C37 N8 60.9(7) . . . . ?
N5 C32 C33 N7 -44.6(9) . . . . ?
N6 C38 C39 N8 -42.8(7) . . . . ?
C1 C2 C3 C4 -0.6(9) . . . . ?
C1 C2 C8 N1 -12.1(9) . . . . ?
C1 C6 C9 N2 -8.1(9) . . . . ?
C2 C1 C6 C5 -6.6(8) . . . . ?
C2 C1 C6 C9 174.0(5) . . . . ?
C2 C3 C4 C5 -3.7(9) . . . . ?
C2 C3 C4 C7 178.0(6) . . . . ?
C3 C2 C8 N1 166.0(6) . . . . ?
C3 C4 C5 C6 2.7(9) . . . . ?
C4 C5 C6 C1 2.4(9) . . . . ?
C4 C5 C6 C9 -178.1(6) . . . . ?
C5 C6 C9 N2 172.5(6) . . . . ?
C6 C1 C2 C3 5.7(8) . . . . ?
C6 C1 C2 C8 -176.3(5) . . . . ?
C7 C4 C5 C6 -178.9(6) . . . . ?
C8 N1 C28 C29 103.1(5) . . . . ?
C8 C2 C3 C4 -178.8(6) . . . . ?
C9 N2 C34 C35 99.0(6) . . . . ?
C10 C11 C12 C13 2.0(10) . . . . ?
C10 C11 C17 N3 -9.6(10) . . . . ?
C10 C15 C18 N4 -12.7(10) . . . . ?
C11 C10 C15 C14 4.1(8) . . . . ?
C11 C10 C15 C18 -177.7(5) . . . . ?
C11 C12 C13 C14 0.8(10) . . . . ?
C11 C12 C13 C16 -180.0(6) . . . . ?
C12 C11 C17 N3 168.6(6) . . . . ?
C12 C13 C14 C15 -1.0(10) . . . . ?
C13 C14 C15 C10 -1.6(9) . . . . ?
C13 C14 C15 C18 -179.9(6) . . . . ?
C14 C15 C18 N4 165.6(6) . . . . ?
C15 C10 C11 C12 -4.3(8) . . . . ?
C15 C10 C11 C17 173.8(5) . . . . ?
C16 C13 C14 C15 179.8(6) . . . . ?
C17 N3 C30 C31 98.2(7) . . . . ?
C17 C11 C12 C13 -176.3(6) . . . . ?
C18 N4 C36 C37 105.5(6) . . . . ?
C19 C20 C21 C22 3.8(9) . . . . ?
C19 C20 C26 N5 -10.9(10) . . . . ?
C19 C24 C27 N6 -8.5(9) . . . . ?
C20 C19 C24 C23 0.3(7) . . . . ?
C20 C19 C24 C27 175.9(5) . . . . ?
C20 C21 C22 C23 -1.5(9) . . . . ?
C20 C21 C22 C25 -178.8(6) . . . . ?
C21 C20 C26 N5 165.8(6) . . . . ?
C21 C22 C23 C24 -1.3(9) . . . . ?
C22 C23 C24 C19 2.0(8) . . . . ?
C22 C23 C24 C27 -174.4(5) . . . . ?
C23 C24 C27 N6 167.5(6) . . . . ?
C24 C19 C20 C21 -2.9(8) . . . . ?
C24 C19 C20 C26 173.5(5) . . . . ?
C25 C22 C23 C24 175.8(6) . . . . ?
C26 N5 C32 C33 -158.7(7) . . . . ?
C26 C20 C21 C22 -173.2(6) . . . . ?
C27 N6 C38 C39 -168.2(5) . . . . ?
C28 N1 C8 C2 -171.7(5) . . . . ?
C29 N7 C31 C30 -139.9(6) . . . . ?
C29 N7 C33 C32 172.5(5) . . . . ?
C30 N3 C17 C11 -170.6(6) . . . . ?
C31 N7 C29 C28 87.2(5) . . . . ?
C31 N7 C33 C32 -67.0(7) . . . . ?
C32 N5 C26 C20 -172.9(7) . . . . ?
C33 N7 C29 C28 -151.2(5) . . . . ?
C33 N7 C31 C30 99.0(7) . . . . ?
C34 N2 C9 C6 -172.1(6) . . . . ?
C35 N8 C37 C36 86.7(6) . . . . ?
C35 N8 C39 C38 -66.8(6) . . . . ?
C36 N4 C18 C15 -171.0(6) . . . . ?
C37 N8 C35 C34 -138.5(5) . . . . ?
C37 N8 C39 C38 171.4(5) . . . . ?
C38 N6 C27 C24 -172.9(5) . . . . ?
C39 N8 C35 C34 100.4(6) . . . . ?
C39 N8 C37 C36 -151.6(5) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_original_sample_id D8V4671
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4658_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc2747k6
_database_code_depnum_ccdc_archive 'CCDC 2059657'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.13667729.v1 2021
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-02-03 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_audit_creation_date             2021-02-03
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H45 Lu N10 O9 Yb, N O3, 2.5(H2 O)'
_chemical_formula_sum            'C39 H50 Lu N11 O14.50 Yb'
_chemical_formula_weight         1252.91
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Lu Lu -0.4720 5.8584 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+3/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+1/4'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   17.5896(7)
_cell_length_b                   17.5896(7)
_cell_length_c                   28.9543(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8958.3(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9161
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.270
_cell_measurement_theta_min      2.683
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.346
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1398 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.6572.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4944
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.2090
0.00 0.00 -1.00 0.2390
1.00 1.00 0.00 0.0120
-1.00 -1.00 0.00 0.0400
-1.00 1.00 0.00 0.0200
1.00 -1.00 0.00 0.0340

_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.068
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            115628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.822
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9589
_reflns_number_total             10256
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.028
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 
;
 Flack x determined using 4066 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10256
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.217
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0248P)²+25.7606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0669
_refine_special_details          
;
Both metal centres were modelled as substitionally disordered.  One of the nitrate ligands was modelled as disordered, consistent with peaks in a difference map.  The nitrate counterion and one water of crystallization were modelled as disordered over two sites with geometric and displacement ellipsoid restraints used.  In all cases water H atoms were identified from difference peaks which corresponded with likely hydrogen bonding interactions.  Water H atoms were refined using a riding model with geometric restraints.  One of the water molecules lies on a special position, hence a fractional value in the chemical formula.  
There is an additional peak corresponding with approximately 1/3 of an oxygen atom. It does not make chemical sense to model this peak.
#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

420_ALERT_2_B D-H Without Acceptor       O13      --H13B     .     Please Check

Disordered water, discussed above.

#===============================================================================
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.10 Report
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .        O13 Check
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .       O13A Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .        O13 Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .       O13A Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .        O13 Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .       O13A Check
213_ALERT_2_C Atom O4              has ADP max/min Ratio .....        3.3 prolat
213_ALERT_2_C Atom C13             has ADP max/min Ratio .....        3.4 prolat
213_ALERT_2_C Atom C16             has ADP max/min Ratio .....        3.5 prolat
213_ALERT_2_C Atom C30             has ADP max/min Ratio .....        3.2 prolat
218_ALERT_3_C Constrained U(ij) Components(s) for O13        .          6 Check
218_ALERT_3_C Constrained U(ij) Components(s) for O13A       .          6 Check

All of these pertain to the discussion above

220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        4.5 Ratio
220_ALERT_2_C NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        4.7 Ratio
222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.5 Ratio
342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01118 Ang.
601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         77 Ang**3

See above - no chemical justification for modelling 1/3 water.

911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         11 Report
971_ALERT_2_C Check Calcd Resid. Dens.  3.02A   From O9              1.98 eA-3
975_ALERT_2_C Check Calcd Resid. Dens.  1.08A   From O7              0.52 eA-3

All noted.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Yb1, Lu1A}
{Lu2, Yb2A}
3. Restrained distances
 O13A-H13C = O13A-H13D = O13-H13A = O13-H13B = O16-H16D = C4-C3 = O16-H16E =
 O14-H14A
 0.84 with sigma of 0.02
 O15-H15
 0.84 with sigma of 0.02
 H14A-H14A_$5
 1.35 with sigma of 0.04
 H16D-H16E = H13D-H13C = H13A-H13B
 1.35 with sigma of 0.04
 H15-H15_$1
 1.35 with sigma of 0.04
 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim
O12-N11
 with sigma of 0.02
 N9-O4 \\sim N9-O4A \\sim N9-O5 \\sim N9-O6
 with sigma of 0.02
4. Restrained planarity
 O4, N9, O5, O6
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(Yb1) = Uanis(Lu1A)
Uanis(Lu2) = Uanis(Yb2A)
6. Rigid body (RIGU) restrains
 O10, O11, O12, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10A, O11A, O12A, N11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N9, O6, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, N9, O6, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, O11, O12, N11}
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, O11A, O12A, N11A}
8. Others
 Sof(O4A)=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Sof(Lu1A)=Sof(Yb2A)=1-FVAR(2)
 Sof(Yb1)=Sof(Lu2)=FVAR(2)
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5)
 N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5)
9.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O16, H16D, H16E
9.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
9.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C21(H21), C23(H23), C26(H26), C27(H27)
9.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.14161(2) 0.61214(2) 0.39634(2) 0.01641(10) Uani 0.73(7) 1 d . . P A 1
Lu2 Lu 0.05412(2) 0.68485(2) 0.49308(2) 0.01753(10) Uani 0.73(7) 1 d . . P A 1
Lu1A Lu 0.14161(2) 0.61214(2) 0.39634(2) 0.01641(10) Uani 0.27(7) 1 d . . P A 2
Yb2A Yb 0.05412(2) 0.68485(2) 0.49308(2) 0.01753(10) Uani 0.27(7) 1 d . . P A 2
O1 O 0.1745(3) 0.6471(3) 0.46960(15) 0.0176(9) Uani 1 1 d . . . . .
O2 O 0.0840(3) 0.7229(3) 0.42056(16) 0.0209(10) Uani 1 1 d . . . . .
O3 O 0.0430(3) 0.5760(3) 0.44708(16) 0.0209(10) Uani 1 1 d . . . . .
O4 O 0.1818(9) 0.4614(17) 0.4529(6) 0.080(10) Uani 0.41(2) 1 d D . P B 1
O5 O 0.2425(3) 0.5338(3) 0.4148(2) 0.0347(13) Uani 1 1 d D . . . .
O6 O 0.3016(4) 0.4629(4) 0.4649(2) 0.0495(17) Uani 1 1 d D . . C 1
O7 O -0.0807(4) 0.6897(3) 0.43215(19) 0.0364(14) Uani 1 1 d D . . . .
O8 O -0.0391(3) 0.7792(3) 0.47725(17) 0.0262(11) Uani 1 1 d D . . . .
O9 O -0.1317(5) 0.8016(4) 0.4300(3) 0.060(2) Uani 1 1 d D . . . .
N10 N -0.0852(4) 0.7566(4) 0.4460(2) 0.0315(15) Uani 1 1 d D . . . .
N1 N 0.2508(3) 0.6895(3) 0.38490(19) 0.0189(12) Uani 1 1 d . . . . .
N2 N 0.1195(4) 0.6256(3) 0.55714(18) 0.0212(12) Uani 1 1 d . . . . .
N3 N 0.0713(3) 0.6659(5) 0.3326(2) 0.0302(16) Uani 1 1 d . . . . .
N4 N 0.1126(4) 0.8050(3) 0.5052(2) 0.0249(13) Uani 1 1 d . . . . .
N5 N 0.1067(4) 0.4898(4) 0.3648(2) 0.0320(16) Uani 1 1 d . . . . .
N6 N -0.0581(4) 0.6302(3) 0.5263(2) 0.0215(12) Uani 1 1 d . . . . .
N7 N 0.2046(3) 0.5865(4) 0.3157(2) 0.0246(13) Uani 1 1 d . . . . .
N8 N 0.0182(4) 0.7422(4) 0.5748(2) 0.0271(14) Uani 1 1 d . . . . .
N9 N 0.2494(4) 0.4746(5) 0.4390(3) 0.049(2) Uani 1 1 d D . . . .
C1 C 0.2430(4) 0.6520(4) 0.4877(2) 0.0200(14) Uani 1 1 d . . . . .
C2 C 0.3071(4) 0.6742(4) 0.4620(2) 0.0206(14) Uani 1 1 d . . . . .
C3 C 0.3793(4) 0.6723(4) 0.4838(2) 0.0251(16) Uani 1 1 d D . . . .
H3 H 0.422460 0.686783 0.466147 0.030 Uiso 1 1 calc R U . . .
C4 C 0.3899(5) 0.6516(5) 0.5269(3) 0.0309(17) Uani 1 1 d D . . . .
C5 C 0.3265(5) 0.6344(4) 0.5541(2) 0.0247(15) Uani 1 1 d . . . . .
H5 H 0.333270 0.621528 0.585731 0.030 Uiso 1 1 calc R U . . .
C6 C 0.2535(4) 0.6359(4) 0.5353(2) 0.0213(14) Uani 1 1 d . . . . .
C7 C 0.4695(5) 0.6485(6) 0.5478(3) 0.042(2) Uani 1 1 d . . . . .
H7A H 0.489931 0.700193 0.550363 0.063 Uiso 1 1 calc R U . . .
H7B H 0.502702 0.617970 0.528010 0.063 Uiso 1 1 calc R U . . .
H7C H 0.466868 0.625467 0.578609 0.063 Uiso 1 1 calc R U . . .
C8 C 0.3054(4) 0.6971(4) 0.4136(2) 0.0204(14) Uani 1 1 d . . . . .
H8 H 0.350252 0.720524 0.401997 0.025 Uiso 1 1 calc R U . . .
C9 C 0.1909(5) 0.6195(4) 0.5661(2) 0.0244(15) Uani 1 1 d . . . . .
H9 H 0.203934 0.602470 0.596251 0.029 Uiso 1 1 calc R U . . .
C10 C 0.0789(4) 0.7910(4) 0.4019(3) 0.0225(15) Uani 1 1 d . . . . .
C11 C 0.0612(4) 0.7994(5) 0.3545(3) 0.0317(18) Uani 1 1 d . . . . .
C12 C 0.0514(5) 0.8716(6) 0.3348(3) 0.044(3) Uani 1 1 d . . . . .
H12 H 0.037048 0.875255 0.303277 0.052 Uiso 1 1 calc R U . . .
C13 C 0.0621(5) 0.9380(6) 0.3601(4) 0.052(3) Uani 1 1 d . . . . .
C14 C 0.0824(5) 0.9295(5) 0.4060(4) 0.039(2) Uani 1 1 d . . . . .
H14 H 0.089902 0.974014 0.423993 0.047 Uiso 1 1 calc R U . . .
C15 C 0.0925(4) 0.8578(4) 0.4275(3) 0.0276(16) Uani 1 1 d . . . . .
C16 C 0.0517(6) 1.0159(6) 0.3392(5) 0.075(5) Uani 1 1 d . . . . .
H16A H 0.010074 1.042241 0.355010 0.113 Uiso 1 1 calc R U . . .
H16B H 0.039560 1.010861 0.306321 0.113 Uiso 1 1 calc R U . . .
H16C H 0.098743 1.045178 0.342757 0.113 Uiso 1 1 calc R U . . .
C17 C 0.0538(4) 0.7351(6) 0.3242(3) 0.036(2) Uani 1 1 d . . . . .
H17 H 0.033555 0.745144 0.294410 0.043 Uiso 1 1 calc R U . . .
C18 C 0.1141(4) 0.8601(4) 0.4760(3) 0.0282(16) Uani 1 1 d . . . . .
H18 H 0.131224 0.907781 0.487367 0.034 Uiso 1 1 calc R U . . .
C19 C -0.0054(4) 0.5171(4) 0.4477(2) 0.0164(13) Uani 1 1 d . . . . .
C20 C 0.0060(4) 0.4515(4) 0.4200(2) 0.0192(13) Uani 1 1 d . . . . .
C21 C -0.0430(4) 0.3889(4) 0.4233(3) 0.0241(15) Uani 1 1 d . . . . .
H21 H -0.032342 0.345249 0.405088 0.029 Uiso 1 1 calc R U . . .
C22 C -0.1062(4) 0.3877(4) 0.4516(3) 0.0269(16) Uani 1 1 d . . . . .
C23 C -0.1189(4) 0.4517(4) 0.4774(2) 0.0237(15) Uani 1 1 d . . . . .
H23 H -0.162694 0.452938 0.496591 0.028 Uiso 1 1 calc R U . . .
C24 C -0.0704(4) 0.5162(4) 0.4772(2) 0.0168(13) Uani 1 1 d . . . . .
C25 C -0.1549(5) 0.3181(6) 0.4542(3) 0.043(2) Uani 1 1 d . . . . .
H25A H -0.127788 0.278160 0.471077 0.064 Uiso 1 1 calc R U . . .
H25B H -0.166411 0.300394 0.422890 0.064 Uiso 1 1 calc R U . . .
H25C H -0.202347 0.330286 0.470309 0.064 Uiso 1 1 calc R U . . .
C26 C 0.0628(4) 0.4417(4) 0.3835(3) 0.0266(16) Uani 1 1 d . . . . .
H26 H 0.067456 0.391326 0.372064 0.032 Uiso 1 1 calc R U . . .
C27 C -0.0938(4) 0.5717(4) 0.5113(2) 0.0213(14) Uani 1 1 d . . . . .
H27 H -0.142595 0.563559 0.524381 0.026 Uiso 1 1 calc R U . . .
C28 C 0.2674(4) 0.7073(4) 0.3364(2) 0.0234(15) Uani 1 1 d . . . . .
H28A H 0.314987 0.737107 0.333976 0.028 Uiso 1 1 calc R U . . .
H28B H 0.225456 0.737153 0.322636 0.028 Uiso 1 1 calc R U . . .
C29 C 0.2759(4) 0.6308(4) 0.3117(2) 0.0228(15) Uani 1 1 d . . . . .
H29A H 0.287837 0.639449 0.278713 0.027 Uiso 1 1 calc R U . . .
H29B H 0.318316 0.601762 0.325612 0.027 Uiso 1 1 calc R U . . .
C30 C 0.0687(5) 0.6141(7) 0.2923(3) 0.045(3) Uani 1 1 d . . . . .
H30A H 0.036476 0.635509 0.267454 0.054 Uiso 1 1 calc R U . . .
H30B H 0.048547 0.563658 0.301189 0.054 Uiso 1 1 calc R U . . .
C31 C 0.1523(4) 0.6082(6) 0.2766(2) 0.034(2) Uani 1 1 d . . . . .
H31A H 0.156298 0.569626 0.251760 0.041 Uiso 1 1 calc R U . . .
H31B H 0.168643 0.657639 0.263641 0.041 Uiso 1 1 calc R U . . .
C32 C 0.1498(5) 0.4591(6) 0.3249(3) 0.046(3) Uani 1 1 d . . . . .
H32A H 0.116639 0.459092 0.297319 0.055 Uiso 1 1 calc R U . . .
H32B H 0.164303 0.405799 0.331498 0.055 Uiso 1 1 calc R U . . .
C33 C 0.2213(4) 0.5051(5) 0.3146(3) 0.0332(19) Uani 1 1 d . . . . .
H33A H 0.260926 0.493135 0.337779 0.040 Uiso 1 1 calc R U . . .
H33B H 0.241124 0.490996 0.283758 0.040 Uiso 1 1 calc R U . . .
C34 C 0.0696(5) 0.6148(5) 0.5978(2) 0.0307(17) Uani 1 1 d . . . . .
H34A H 0.096907 0.587228 0.622569 0.037 Uiso 1 1 calc R U . . .
H34B H 0.023716 0.585348 0.589241 0.037 Uiso 1 1 calc R U . . .
C35 C 0.0480(5) 0.6939(5) 0.6136(2) 0.0302(17) Uani 1 1 d . . . . .
H35A H 0.008703 0.690081 0.637995 0.036 Uiso 1 1 calc R U . . .
H35B H 0.093173 0.718927 0.627274 0.036 Uiso 1 1 calc R U . . .
C36 C 0.1257(5) 0.8247(5) 0.5535(3) 0.0338(19) Uani 1 1 d . . . . .
H36A H 0.147173 0.876558 0.555941 0.041 Uiso 1 1 calc R U . . .
H36B H 0.161970 0.788495 0.567674 0.041 Uiso 1 1 calc R U . . .
C37 C 0.0493(5) 0.8207(5) 0.5782(3) 0.0340(19) Uani 1 1 d . . . . .
H37A H 0.055695 0.834855 0.611040 0.041 Uiso 1 1 calc R U . . .
H37B H 0.013350 0.857135 0.563879 0.041 Uiso 1 1 calc R U . . .
C38 C -0.0988(5) 0.6668(4) 0.5658(3) 0.0303(18) Uani 1 1 d . . . . .
H38A H -0.094552 0.633986 0.593478 0.036 Uiso 1 1 calc R U . . .
H38B H -0.153363 0.672157 0.558137 0.036 Uiso 1 1 calc R U . . .
C39 C -0.0650(5) 0.7454(5) 0.5764(3) 0.0302(18) Uani 1 1 d . . . . .
H39A H -0.083659 0.782731 0.553460 0.036 Uiso 1 1 calc R U . . .
H39B H -0.081648 0.762201 0.607392 0.036 Uiso 1 1 calc R U . . .
O10 O 0.4520(9) 0.7062(10) 0.2940(6) 0.072(4) Uani 0.5 1 d D . P D 1
O11 O 0.4745(11) 0.7358(10) 0.3678(7) 0.096(7) Uani 0.5 1 d D . P D 1
O12 O 0.5019(14) 0.6274(11) 0.3416(7) 0.106(8) Uani 0.5 1 d D . P D 1
N11 N 0.4762(8) 0.6918(8) 0.3330(6) 0.051(4) Uani 0.5 1 d D . P D 1
O10A O 0.5779(12) 0.7193(10) 0.4497(5) 0.082(6) Uani 0.5 1 d D . P E 2
O11A O 0.4881(8) 0.7714(9) 0.4128(5) 0.062(4) Uani 0.5 1 d D . P E 2
O12A O 0.5592(12) 0.6920(10) 0.3767(5) 0.080(5) Uani 0.5 1 d D . P E 2
N11A N 0.5432(7) 0.7254(7) 0.4123(4) 0.028(3) Uani 0.5 1 d D . P E 2
O13 O 0.562200 0.735630 0.438850 0.092 Uani 0.5 1 d D . P F 1
H13A H 0.564530 0.705950 0.410150 0.110 Uiso 0.5 1 d D U P G 1
H13B H 0.597760 0.694010 0.453370 0.110 Uiso 0.5 1 d D U P H 1
O13A O 0.467980 0.697590 0.293840 0.043 Uani 0.5 1 d D . P I 2
H13C H 0.464270 0.652220 0.284420 0.051 Uiso 0.5 1 d D U P J 2
H13D H 0.478750 0.691110 0.322570 0.051 Uiso 0.5 1 d D U P K 2
O14 O -0.060260 0.939740 0.500000 0.045 Uani 1 2 d DS T P . .
H14A H -0.061250 0.899460 0.484250 0.054 Uiso 1 1 d D U . . .
O16 O 0.050600 1.050600 0.500000 0.053 Uani 1 2 d DS T P . .
H16D H 0.080320 1.043180 0.521350 0.064 Uiso 0.5 1 d D U P . .
H16E H 0.017230 1.017230 0.500000 0.064 Uiso 1 2 d DS U P . .
O15 O 0.1935(3) 0.8065(3) 0.250000 0.0362(19) Uani 1 2 d DS T P . .
O4A O 0.2240(10) 0.4075(7) 0.4226(7) 0.084(7) Uani 0.59(2) 1 d D . P B 2
H15 H 0.200(3) 0.854(2) 0.252(15) 0.32(17) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 Lu2 3.4424(4) . ?
Yb1 O1 2.283(4) . ?
Yb1 O2 2.305(5) . ?
Yb1 O3 2.360(5) . ?
Yb1 O5 2.309(6) . ?
Yb1 N1 2.376(6) . ?
Yb1 N3 2.414(6) . ?
Yb1 N5 2.417(6) . ?
Yb1 N7 2.625(6) . ?
Lu2 O1 2.321(5) . ?
Lu2 O2 2.266(5) . ?
Lu2 O3 2.341(5) . ?
Lu2 O8 2.378(5) . ?
Lu2 N2 2.418(6) . ?
Lu2 N4 2.377(6) . ?
Lu2 N6 2.397(6) . ?
Lu2 N8 2.649(6) . ?
Lu1A Yb2A 3.4424(4) . ?
Lu1A O1 2.283(4) . ?
Lu1A O2 2.305(5) . ?
Lu1A O3 2.360(5) . ?
Lu1A O5 2.309(6) . ?
Lu1A N1 2.376(6) . ?
Lu1A N3 2.414(6) . ?
Lu1A N5 2.417(6) . ?
Lu1A N7 2.625(6) . ?
Yb2A O1 2.321(5) . ?
Yb2A O2 2.266(5) . ?
Yb2A O3 2.341(5) . ?
Yb2A O7 2.956(7) . ?
Yb2A O8 2.378(5) . ?
Yb2A N10 3.075(7) . ?
Yb2A N2 2.418(6) . ?
Yb2A N4 2.377(6) . ?
Yb2A N6 2.397(6) . ?
Yb2A N8 2.649(6) . ?
O1 C1 1.316(9) . ?
O2 C10 1.318(9) . ?
O3 C19 1.341(8) . ?
O4 N9 1.276(14) . ?
O5 N9 1.261(9) . ?
O6 N9 1.203(9) . ?
O7 N10 1.247(8) . ?
O8 N10 1.278(8) . ?
O9 N10 1.229(8) . ?
N1 C8 1.277(9) . ?
N1 C28 1.468(9) . ?
N2 C9 1.288(10) . ?
N2 C34 1.480(8) . ?
N3 C17 1.279(12) . ?
N3 C30 1.482(10) . ?
N4 C18 1.287(10) . ?
N4 C36 1.459(10) . ?
N5 C26 1.267(10) . ?
N5 C32 1.483(10) . ?
N6 C27 1.281(9) . ?
N6 C38 1.495(9) . ?
N7 C29 1.479(9) . ?
N7 C31 1.508(10) . ?
N7 C33 1.463(11) . ?
N8 C35 1.504(10) . ?
N8 C37 1.488(10) . ?
N8 C39 1.464(10) . ?
N9 O4A 1.349(13) . ?
C1 C2 1.407(10) . ?
C1 C6 1.420(9) . ?
C2 C3 1.417(10) . ?
C2 C8 1.458(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.314(10) . ?
C4 C5 1.399(11) . ?
C4 C7 1.527(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(11) . ?
C6 C9 1.446(10) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.417(11) . ?
C10 C15 1.410(11) . ?
C11 C12 1.401(12) . ?
C11 C17 1.436(13) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(17) . ?
C13 C14 1.384(15) . ?
C13 C16 1.509(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.417(10) . ?
C15 C18 1.454(11) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.420(10) . ?
C19 C24 1.426(9) . ?
C20 C21 1.402(10) . ?
C20 C26 1.463(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.382(10) . ?
C22 C23 1.368(11) . ?
C22 C25 1.496(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.420(10) . ?
C24 C27 1.448(10) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.532(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.543(11) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.525(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.515(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.523(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.536(12) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
O10 N11 1.233(15) . ?
O11 N11 1.271(16) . ?
O12 N11 1.244(16) . ?
O10A N11A 1.247(13) . ?
O11A N11A 1.264(14) . ?
O12A N11A 1.219(13) . ?
O13 H13A 0.9822 . ?
O13 H13A 0.9822 . ?
O13 H13B 1.0507 . ?
O13A H13C 0.8459 . ?
O13A H13D 0.8607 . ?
O14 H14A 0.8428 . ?
O14 H14A 0.8428 7_466 ?
O16 H16D 0.8200 . ?
O16 H16D 0.8200 7_466 ?
O16 H16E 0.8301 . ?
O15 H15 0.85(3) 8_665 ?
O15 H15 0.85(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Yb1 Lu2 42.02(12) . . ?
O1 Yb1 O2 66.48(17) . . ?
O1 Yb1 O3 71.36(16) . . ?
O1 Yb1 O5 75.62(19) . . ?
O1 Yb1 N1 76.74(17) . . ?
O1 Yb1 N3 137.2(2) . . ?
O1 Yb1 N5 130.9(2) . . ?
O1 Yb1 N7 140.01(17) . . ?
O2 Yb1 Lu2 40.70(12) . . ?
O2 Yb1 O3 73.46(17) . . ?
O2 Yb1 O5 140.53(19) . . ?
O2 Yb1 N1 85.07(19) . . ?
O2 Yb1 N3 71.1(2) . . ?
O2 Yb1 N5 139.1(2) . . ?
O2 Yb1 N7 126.99(19) . . ?
O3 Yb1 Lu2 42.70(11) . . ?
O3 Yb1 N1 146.59(17) . . ?
O3 Yb1 N3 101.81(19) . . ?
O3 Yb1 N5 78.96(19) . . ?
O3 Yb1 N7 144.90(18) . . ?
O5 Yb1 Lu2 112.17(15) . . ?
O5 Yb1 O3 105.1(2) . . ?
O5 Yb1 N1 75.7(2) . . ?
O5 Yb1 N3 143.5(2) . . ?
O5 Yb1 N5 75.6(2) . . ?
O5 Yb1 N7 77.2(2) . . ?
N1 Yb1 Lu2 105.19(14) . . ?
N1 Yb1 N3 94.8(2) . . ?
N1 Yb1 N5 131.5(2) . . ?
N1 Yb1 N7 68.46(19) . . ?
N3 Yb1 Lu2 104.30(15) . . ?
N3 Yb1 N5 86.0(3) . . ?
N3 Yb1 N7 66.7(2) . . ?
N5 Yb1 Lu2 121.64(15) . . ?
N5 Yb1 N7 67.6(2) . . ?
N7 Yb1 Lu2 167.64(15) . . ?
O1 Lu2 Yb1 41.19(11) . . ?
O1 Lu2 O3 71.05(16) . . ?
O1 Lu2 O8 140.58(17) . . ?
O1 Lu2 N2 70.59(18) . . ?
O1 Lu2 N4 84.43(19) . . ?
O1 Lu2 N6 138.95(18) . . ?
O1 Lu2 N8 126.06(18) . . ?
O2 Lu2 Yb1 41.56(13) . . ?
O2 Lu2 O1 66.49(17) . . ?
O2 Lu2 O3 74.53(17) . . ?
O2 Lu2 O8 77.02(17) . . ?
O2 Lu2 N2 136.70(19) . . ?
O2 Lu2 N4 76.9(2) . . ?
O2 Lu2 N6 132.9(2) . . ?
O2 Lu2 N8 140.42(19) . . ?
O3 Lu2 Yb1 43.13(11) . . ?
O3 Lu2 O8 113.82(18) . . ?
O3 Lu2 N2 97.08(18) . . ?
O3 Lu2 N4 147.96(18) . . ?
O3 Lu2 N6 80.29(18) . . ?
O3 Lu2 N8 143.15(18) . . ?
O8 Lu2 Yb1 114.25(12) . . ?
O8 Lu2 N2 140.95(17) . . ?
O8 Lu2 N6 77.82(19) . . ?
O8 Lu2 N8 75.02(18) . . ?
N2 Lu2 Yb1 104.56(13) . . ?
N2 Lu2 N8 65.98(19) . . ?
N4 Lu2 Yb1 104.90(14) . . ?
N4 Lu2 O8 72.9(2) . . ?
N4 Lu2 N2 93.7(2) . . ?
N4 Lu2 N6 130.8(2) . . ?
N4 Lu2 N8 68.4(2) . . ?
N6 Lu2 Yb1 123.04(14) . . ?
N6 Lu2 N2 84.9(2) . . ?
N6 Lu2 N8 66.3(2) . . ?
N8 Lu2 Yb1 167.19(15) . . ?
O1 Lu1A Yb2A 42.02(12) . . ?
O1 Lu1A O2 66.48(17) . . ?
O1 Lu1A O3 71.36(16) . . ?
O1 Lu1A O5 75.62(19) . . ?
O1 Lu1A N1 76.74(17) . . ?
O1 Lu1A N3 137.2(2) . . ?
O1 Lu1A N5 130.9(2) . . ?
O1 Lu1A N7 140.01(17) . . ?
O2 Lu1A Yb2A 40.70(12) . . ?
O2 Lu1A O3 73.46(17) . . ?
O2 Lu1A O5 140.53(19) . . ?
O2 Lu1A N1 85.07(19) . . ?
O2 Lu1A N3 71.1(2) . . ?
O2 Lu1A N5 139.1(2) . . ?
O2 Lu1A N7 126.99(19) . . ?
O3 Lu1A Yb2A 42.70(11) . . ?
O3 Lu1A N1 146.59(17) . . ?
O3 Lu1A N3 101.81(19) . . ?
O3 Lu1A N5 78.96(19) . . ?
O3 Lu1A N7 144.90(18) . . ?
O5 Lu1A Yb2A 112.17(15) . . ?
O5 Lu1A O3 105.1(2) . . ?
O5 Lu1A N1 75.7(2) . . ?
O5 Lu1A N3 143.5(2) . . ?
O5 Lu1A N5 75.6(2) . . ?
O5 Lu1A N7 77.2(2) . . ?
N1 Lu1A Yb2A 105.19(14) . . ?
N1 Lu1A N3 94.8(2) . . ?
N1 Lu1A N5 131.5(2) . . ?
N1 Lu1A N7 68.46(19) . . ?
N3 Lu1A Yb2A 104.30(15) . . ?
N3 Lu1A N5 86.0(3) . . ?
N3 Lu1A N7 66.7(2) . . ?
N5 Lu1A Yb2A 121.64(15) . . ?
N5 Lu1A N7 67.6(2) . . ?
N7 Lu1A Yb2A 167.64(15) . . ?
O1 Yb2A Lu1A 41.19(11) . . ?
O1 Yb2A O3 71.05(16) . . ?
O1 Yb2A O7 124.40(15) . . ?
O1 Yb2A O8 140.58(17) . . ?
O1 Yb2A N10 135.62(17) . . ?
O1 Yb2A N2 70.59(18) . . ?
O1 Yb2A N4 84.43(19) . . ?
O1 Yb2A N6 138.95(18) . . ?
O1 Yb2A N8 126.06(18) . . ?
O2 Yb2A Lu1A 41.56(13) . . ?
O2 Yb2A O1 66.49(17) . . ?
O2 Yb2A O3 74.53(17) . . ?
O2 Yb2A O7 67.95(17) . . ?
O2 Yb2A O8 77.02(17) . . ?
O2 Yb2A N10 69.70(18) . . ?
O2 Yb2A N2 136.70(19) . . ?
O2 Yb2A N4 76.9(2) . . ?
O2 Yb2A N6 132.9(2) . . ?
O2 Yb2A N8 140.42(19) . . ?
O3 Yb2A Lu1A 43.13(11) . . ?
O3 Yb2A O7 67.48(16) . . ?
O3 Yb2A O8 113.82(18) . . ?
O3 Yb2A N10 90.99(18) . . ?
O3 Yb2A N2 97.08(18) . . ?
O3 Yb2A N4 147.96(18) . . ?
O3 Yb2A N6 80.29(18) . . ?
O3 Yb2A N8 143.15(18) . . ?
O7 Yb2A Lu1A 83.31(11) . . ?
O7 Yb2A N10 23.75(15) . . ?
O8 Yb2A Lu1A 114.25(12) . . ?
O8 Yb2A O7 46.52(16) . . ?
O8 Yb2A N10 22.84(17) . . ?
O8 Yb2A N2 140.95(17) . . ?
O8 Yb2A N6 77.82(19) . . ?
O8 Yb2A N8 75.02(18) . . ?
N10 Yb2A Lu1A 98.52(12) . . ?
N2 Yb2A Lu1A 104.56(13) . . ?
N2 Yb2A O7 148.34(19) . . ?
N2 Yb2A N10 153.59(19) . . ?
N2 Yb2A N8 65.98(19) . . ?
N4 Yb2A Lu1A 104.90(14) . . ?
N4 Yb2A O7 114.19(19) . . ?
N4 Yb2A O8 72.9(2) . . ?
N4 Yb2A N10 92.6(2) . . ?
N4 Yb2A N2 93.7(2) . . ?
N4 Yb2A N6 130.8(2) . . ?
N4 Yb2A N8 68.4(2) . . ?
N6 Yb2A Lu1A 123.04(14) . . ?
N6 Yb2A O7 65.80(18) . . ?
N6 Yb2A N10 71.7(2) . . ?
N6 Yb2A N2 84.9(2) . . ?
N6 Yb2A N8 66.3(2) . . ?
N8 Yb2A Lu1A 167.19(15) . . ?
N8 Yb2A O7 109.31(18) . . ?
N8 Yb2A N10 92.81(19) . . ?
Yb1 O1 Lu2 96.79(18) . . ?
Lu1A O1 Yb2A 96.79(18) . . ?
C1 O1 Yb1 128.2(4) . . ?
C1 O1 Lu2 134.4(4) . . ?
C1 O1 Lu1A 128.2(4) . . ?
C1 O1 Yb2A 134.4(4) . . ?
Lu2 O2 Yb1 97.74(18) . . ?
Yb2A O2 Lu1A 97.74(18) . . ?
C10 O2 Yb1 132.4(4) . . ?
C10 O2 Lu2 129.2(4) . . ?
C10 O2 Lu1A 132.4(4) . . ?
C10 O2 Yb2A 129.2(4) . . ?
Lu2 O3 Yb1 94.16(16) . . ?
Yb2A O3 Lu1A 94.16(16) . . ?
C19 O3 Yb1 133.1(4) . . ?
C19 O3 Lu2 132.6(4) . . ?
C19 O3 Lu1A 133.1(4) . . ?
C19 O3 Yb2A 132.6(4) . . ?
N9 O5 Yb1 134.1(5) . . ?
N9 O5 Lu1A 134.1(5) . . ?
N10 O7 Yb2A 83.5(4) . . ?
N10 O8 Lu2 110.9(4) . . ?
N10 O8 Yb2A 110.9(4) . . ?
O7 N10 Yb2A 72.8(4) . . ?
O7 N10 O8 118.8(6) . . ?
O8 N10 Yb2A 46.2(3) . . ?
O9 N10 Yb2A 164.1(6) . . ?
O9 N10 O7 122.0(7) . . ?
O9 N10 O8 119.2(7) . . ?
C8 N1 Yb1 125.3(5) . . ?
C8 N1 Lu1A 125.3(5) . . ?
C8 N1 C28 116.6(6) . . ?
C28 N1 Yb1 114.6(4) . . ?
C28 N1 Lu1A 114.6(4) . . ?
C9 N2 Lu2 130.9(5) . . ?
C9 N2 Yb2A 130.9(5) . . ?
C9 N2 C34 114.0(6) . . ?
C34 N2 Lu2 112.5(4) . . ?
C34 N2 Yb2A 112.5(4) . . ?
C17 N3 Yb1 130.0(6) . . ?
C17 N3 Lu1A 130.0(6) . . ?
C17 N3 C30 115.3(7) . . ?
C30 N3 Yb1 112.2(6) . . ?
C30 N3 Lu1A 112.2(6) . . ?
C18 N4 Lu2 125.5(5) . . ?
C18 N4 Yb2A 125.5(5) . . ?
C18 N4 C36 116.7(6) . . ?
C36 N4 Lu2 114.9(5) . . ?
C36 N4 Yb2A 114.9(5) . . ?
C26 N5 Yb1 126.0(5) . . ?
C26 N5 Lu1A 126.0(5) . . ?
C26 N5 C32 113.7(7) . . ?
C32 N5 Yb1 119.2(5) . . ?
C32 N5 Lu1A 119.2(5) . . ?
C27 N6 Lu2 126.1(5) . . ?
C27 N6 Yb2A 126.1(5) . . ?
C27 N6 C38 111.8(6) . . ?
C38 N6 Lu2 121.9(5) . . ?
C38 N6 Yb2A 121.9(5) . . ?
C29 N7 Yb1 109.7(4) . . ?
C29 N7 Lu1A 109.7(4) . . ?
C29 N7 C31 109.0(6) . . ?
C31 N7 Yb1 111.5(4) . . ?
C31 N7 Lu1A 111.5(4) . . ?
C33 N7 Yb1 105.8(4) . . ?
C33 N7 Lu1A 105.8(4) . . ?
C33 N7 C29 110.1(6) . . ?
C33 N7 C31 110.7(6) . . ?
C35 N8 Lu2 111.7(4) . . ?
C35 N8 Yb2A 111.7(4) . . ?
C37 N8 Lu2 108.9(4) . . ?
C37 N8 Yb2A 108.9(4) . . ?
C37 N8 C35 110.3(6) . . ?
C39 N8 Lu2 106.3(4) . . ?
C39 N8 Yb2A 106.3(4) . . ?
C39 N8 C35 110.3(6) . . ?
C39 N8 C37 109.3(6) . . ?
O5 N9 O4 103.6(13) . . ?
O5 N9 O4A 119.6(9) . . ?
O6 N9 O4 118.9(11) . . ?
O6 N9 O5 124.1(8) . . ?
O1 C1 C2 122.9(6) . . ?
O1 C1 C6 119.5(6) . . ?
C2 C1 C6 117.7(7) . . ?
C1 C2 C3 118.4(6) . . ?
C1 C2 C8 124.6(6) . . ?
C3 C2 C8 116.9(6) . . ?
C2 C3 H3 118.1 . . ?
C4 C3 C2 123.9(7) . . ?
C4 C3 H3 118.1 . . ?
C3 C4 C5 118.9(8) . . ?
C3 C4 C7 121.2(8) . . ?
C5 C4 C7 119.9(7) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(7) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C9 122.7(7) . . ?
C5 C6 C1 120.2(7) . . ?
C5 C6 C9 117.1(6) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 127.6(6) . . ?
N1 C8 H8 116.2 . . ?
C2 C8 H8 116.2 . . ?
N2 C9 C6 126.9(7) . . ?
N2 C9 H9 116.5 . . ?
C6 C9 H9 116.5 . . ?
O2 C10 C11 120.5(7) . . ?
O2 C10 C15 122.1(7) . . ?
C15 C10 C11 117.4(7) . . ?
C10 C11 C17 121.9(7) . . ?
C12 C11 C10 121.0(9) . . ?
C12 C11 C17 117.1(8) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.1(9) . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C16 122.4(11) . . ?
C14 C13 C12 116.7(8) . . ?
C14 C13 C16 120.9(12) . . ?
C13 C14 H14 118.3 . . ?
C13 C14 C15 123.4(10) . . ?
C15 C14 H14 118.3 . . ?
C10 C15 C14 119.3(8) . . ?
C10 C15 C18 125.0(7) . . ?
C14 C15 C18 115.6(8) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C11 127.7(7) . . ?
N3 C17 H17 116.2 . . ?
C11 C17 H17 116.2 . . ?
N4 C18 C15 127.5(7) . . ?
N4 C18 H18 116.3 . . ?
C15 C18 H18 116.3 . . ?
O3 C19 C20 122.0(6) . . ?
O3 C19 C24 121.8(6) . . ?
C20 C19 C24 116.3(6) . . ?
C19 C20 C26 126.9(6) . . ?
C21 C20 C19 120.8(6) . . ?
C21 C20 C26 112.1(6) . . ?
C20 C21 H21 118.4 . . ?
C22 C21 C20 123.2(7) . . ?
C22 C21 H21 118.4 . . ?
C21 C22 C25 120.2(7) . . ?
C23 C22 C21 116.3(7) . . ?
C23 C22 C25 123.5(7) . . ?
C22 C23 H23 118.1 . . ?
C22 C23 C24 123.8(7) . . ?
C24 C23 H23 118.1 . . ?
C19 C24 C27 128.9(6) . . ?
C23 C24 C19 119.6(6) . . ?
C23 C24 C27 111.4(6) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C20 130.2(7) . . ?
N5 C26 H26 114.9 . . ?
C20 C26 H26 114.9 . . ?
N6 C27 C24 129.3(6) . . ?
N6 C27 H27 115.3 . . ?
C24 C27 H27 115.3 . . ?
N1 C28 H28A 110.5 . . ?
N1 C28 H28B 110.5 . . ?
N1 C28 C29 106.2(6) . . ?
H28A C28 H28B 108.7 . . ?
C29 C28 H28A 110.5 . . ?
C29 C28 H28B 110.5 . . ?
N7 C29 C28 110.1(6) . . ?
N7 C29 H29A 109.6 . . ?
N7 C29 H29B 109.6 . . ?
C28 C29 H29A 109.6 . . ?
C28 C29 H29B 109.6 . . ?
H29A C29 H29B 108.2 . . ?
N3 C30 H30A 110.9 . . ?
N3 C30 H30B 110.9 . . ?
N3 C30 C31 104.2(6) . . ?
H30A C30 H30B 108.9 . . ?
C31 C30 H30A 110.9 . . ?
C31 C30 H30B 110.9 . . ?
N7 C31 C30 112.2(6) . . ?
N7 C31 H31A 109.2 . . ?
N7 C31 H31B 109.2 . . ?
C30 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
N5 C32 H32A 109.1 . . ?
N5 C32 H32B 109.1 . . ?
N5 C32 C33 112.4(6) . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 H32A 109.1 . . ?
C33 C32 H32B 109.1 . . ?
N7 C33 C32 110.5(7) . . ?
N7 C33 H33A 109.6 . . ?
N7 C33 H33B 109.6 . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
N2 C34 H34A 110.6 . . ?
N2 C34 H34B 110.6 . . ?
N2 C34 C35 105.7(6) . . ?
H34A C34 H34B 108.7 . . ?
C35 C34 H34A 110.6 . . ?
C35 C34 H34B 110.6 . . ?
N8 C35 C34 112.4(6) . . ?
N8 C35 H35A 109.1 . . ?
N8 C35 H35B 109.1 . . ?
C34 C35 H35A 109.1 . . ?
C34 C35 H35B 109.1 . . ?
H35A C35 H35B 107.9 . . ?
N4 C36 H36A 110.2 . . ?
N4 C36 H36B 110.2 . . ?
N4 C36 C37 107.4(7) . . ?
H36A C36 H36B 108.5 . . ?
C37 C36 H36A 110.2 . . ?
C37 C36 H36B 110.2 . . ?
N8 C37 C36 109.6(6) . . ?
N8 C37 H37A 109.7 . . ?
N8 C37 H37B 109.7 . . ?
C36 C37 H37A 109.7 . . ?
C36 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
N6 C38 H38A 109.5 . . ?
N6 C38 H38B 109.5 . . ?
N6 C38 C39 110.8(6) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
N8 C39 C38 110.3(6) . . ?
N8 C39 H39A 109.6 . . ?
N8 C39 H39B 109.6 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
O10 N11 O11 126.3(18) . . ?
O10 N11 O12 119.8(18) . . ?
O12 N11 O11 113.8(19) . . ?
O10A N11A O11A 114.8(15) . . ?
O12A N11A O10A 125.5(17) . . ?
O12A N11A O11A 119.7(15) . . ?
H13A O13 H13A 0.0 . . ?
H13A O13 H13B 86.8 . . ?
H13A O13 H13B 86.8 . . ?
H13C O13A H13D 101.8 . . ?
H14A O14 H14A 105.0 . 7_466 ?
H16D O16 H16D 140.5 . 7_466 ?
H16D O16 H16E 109.8 . . ?
H16E O16 H16D 109.8 . 7_466 ?
H15 O15 H15 105(8) . 8_665 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C30 H30A O4 0.99 2.04 2.898(18) 143.8 2_554 yes
O13A H13C O16 0.85 2.06 2.899 169.4 2_654 yes
O13A H13D O12A 0.86 2.11 2.888(19) 149.7 . yes
O14 H14A O8 0.84 2.16 2.924(5) 150.5 . yes
O16 H16D O13A 0.82 2.17 2.899 147.8 4_465 yes
O16 H16E O14 0.83 1.93 2.758 180.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Yb1 O1 C1 C2 33.7(9) . . . . ?
Yb1 O1 C1 C6 -147.5(5) . . . . ?
Yb1 O2 C10 C11 44.7(9) . . . . ?
Yb1 O2 C10 C15 -133.6(6) . . . . ?
Yb1 O3 C19 C20 14.5(10) . . . . ?
Yb1 O3 C19 C24 -166.8(4) . . . . ?
Yb1 O5 N9 O4 1.9(15) . . . . ?
Yb1 O5 N9 O6 -138.0(7) . . . . ?
Yb1 N1 C8 C2 -13.4(10) . . . . ?
Yb1 N1 C28 C29 -57.0(6) . . . . ?
Yb1 N3 C17 C11 -10.8(12) . . . . ?
Yb1 N3 C30 C31 -64.8(9) . . . . ?
Yb1 N5 C26 C20 19.2(13) . . . . ?
Yb1 N5 C32 C33 10.2(12) . . . . ?
Yb1 N7 C29 C28 -35.1(7) . . . . ?
Yb1 N7 C31 C30 -18.8(9) . . . . ?
Yb1 N7 C33 C32 54.2(7) . . . . ?
Lu2 O1 C1 C2 -135.5(6) . . . . ?
Lu2 O1 C1 C6 43.3(9) . . . . ?
Lu2 O2 C10 C11 -146.7(5) . . . . ?
Lu2 O2 C10 C15 35.0(9) . . . . ?
Lu2 O3 C19 C20 -170.8(5) . . . . ?
Lu2 O3 C19 C24 7.9(9) . . . . ?
Lu2 O8 N10 O7 6.9(8) . . . . ?
Lu2 O8 N10 O9 -171.9(7) . . . . ?
Lu2 N2 C9 C6 -11.8(11) . . . . ?
Lu2 N2 C34 C35 -64.2(7) . . . . ?
Lu2 N4 C18 C15 -11.0(12) . . . . ?
Lu2 N4 C36 C37 -56.4(8) . . . . ?
Lu2 N6 C27 C24 12.3(11) . . . . ?
Lu2 N6 C38 C39 7.3(9) . . . . ?
Lu2 N8 C35 C34 -17.2(8) . . . . ?
Lu2 N8 C37 C36 -36.0(8) . . . . ?
Lu2 N8 C39 C38 54.2(7) . . . . ?
Lu1A O1 C1 C2 33.7(9) . . . . ?
Lu1A O1 C1 C6 -147.5(5) . . . . ?
Lu1A O2 C10 C11 44.7(9) . . . . ?
Lu1A O2 C10 C15 -133.6(6) . . . . ?
Lu1A O3 C19 C20 14.5(10) . . . . ?
Lu1A O3 C19 C24 -166.8(4) . . . . ?
Lu1A O5 N9 O4A 75.4(14) . . . . ?
Lu1A N1 C8 C2 -13.4(10) . . . . ?
Lu1A N1 C28 C29 -57.0(6) . . . . ?
Lu1A N3 C17 C11 -10.8(12) . . . . ?
Lu1A N3 C30 C31 -64.8(9) . . . . ?
Lu1A N5 C26 C20 19.2(13) . . . . ?
Lu1A N5 C32 C33 10.2(12) . . . . ?
Lu1A N7 C29 C28 -35.1(7) . . . . ?
Lu1A N7 C31 C30 -18.8(9) . . . . ?
Lu1A N7 C33 C32 54.2(7) . . . . ?
Yb2A O1 C1 C2 -135.5(6) . . . . ?
Yb2A O1 C1 C6 43.3(9) . . . . ?
Yb2A O2 C10 C11 -146.7(5) . . . . ?
Yb2A O2 C10 C15 35.0(9) . . . . ?
Yb2A O3 C19 C20 -170.8(5) . . . . ?
Yb2A O3 C19 C24 7.9(9) . . . . ?
Yb2A O7 N10 O8 -5.2(6) . . . . ?
Yb2A O7 N10 O9 173.5(8) . . . . ?
Yb2A O8 N10 O7 6.9(8) . . . . ?
Yb2A O8 N10 O9 -171.9(7) . . . . ?
Yb2A N2 C9 C6 -11.8(11) . . . . ?
Yb2A N2 C34 C35 -64.2(7) . . . . ?
Yb2A N4 C18 C15 -11.0(12) . . . . ?
Yb2A N4 C36 C37 -56.4(8) . . . . ?
Yb2A N6 C27 C24 12.3(11) . . . . ?
Yb2A N6 C38 C39 7.3(9) . . . . ?
Yb2A N8 C35 C34 -17.2(8) . . . . ?
Yb2A N8 C37 C36 -36.0(8) . . . . ?
Yb2A N8 C39 C38 54.2(7) . . . . ?
O1 C1 C2 C3 -175.4(7) . . . . ?
O1 C1 C2 C8 2.6(11) . . . . ?
O1 C1 C6 C5 174.4(7) . . . . ?
O1 C1 C6 C9 -4.7(11) . . . . ?
O2 C10 C11 C12 176.4(7) . . . . ?
O2 C10 C11 C17 -4.7(11) . . . . ?
O2 C10 C15 C14 -176.9(7) . . . . ?
O2 C10 C15 C18 0.8(11) . . . . ?
O3 C19 C20 C21 176.3(6) . . . . ?
O3 C19 C20 C26 -8.7(11) . . . . ?
O3 C19 C24 C23 -178.5(6) . . . . ?
O3 C19 C24 C27 -3.4(11) . . . . ?
N1 C28 C29 N7 60.0(7) . . . . ?
N2 C34 C35 N8 50.7(9) . . . . ?
N3 C30 C31 N7 52.4(11) . . . . ?
N4 C36 C37 N8 60.6(9) . . . . ?
N5 C32 C33 N7 -45.3(11) . . . . ?
N6 C38 C39 N8 -43.1(9) . . . . ?
C1 C2 C3 C4 -0.7(12) . . . . ?
C1 C2 C8 N1 -12.4(12) . . . . ?
C1 C6 C9 N2 -8.6(12) . . . . ?
C2 C1 C6 C5 -6.8(10) . . . . ?
C2 C1 C6 C9 174.1(7) . . . . ?
C2 C3 C4 C5 -3.7(12) . . . . ?
C2 C3 C4 C7 178.1(8) . . . . ?
C3 C2 C8 N1 165.7(7) . . . . ?
C3 C4 C5 C6 2.7(12) . . . . ?
C4 C5 C6 C1 2.5(11) . . . . ?
C4 C5 C6 C9 -178.3(7) . . . . ?
C5 C6 C9 N2 172.3(7) . . . . ?
C6 C1 C2 C3 5.8(10) . . . . ?
C6 C1 C2 C8 -176.1(7) . . . . ?
C7 C4 C5 C6 -179.1(8) . . . . ?
C8 N1 C28 C29 103.4(7) . . . . ?
C8 C2 C3 C4 -178.9(7) . . . . ?
C9 N2 C34 C35 99.7(7) . . . . ?
C10 C11 C12 C13 3.1(12) . . . . ?
C10 C11 C17 N3 -10.3(12) . . . . ?
C10 C15 C18 N4 -12.1(13) . . . . ?
C11 C10 C15 C14 4.7(10) . . . . ?
C11 C10 C15 C18 -177.6(7) . . . . ?
C11 C12 C13 C14 -0.5(12) . . . . ?
C11 C12 C13 C16 -180.0(8) . . . . ?
C12 C11 C17 N3 168.6(8) . . . . ?
C12 C13 C14 C15 0.1(12) . . . . ?
C13 C14 C15 C10 -2.3(12) . . . . ?
C13 C14 C15 C18 179.8(7) . . . . ?
C14 C15 C18 N4 165.7(8) . . . . ?
C15 C10 C11 C12 -5.1(10) . . . . ?
C15 C10 C11 C17 173.7(7) . . . . ?
C16 C13 C14 C15 179.6(8) . . . . ?
C17 N3 C30 C31 98.7(9) . . . . ?
C17 C11 C12 C13 -175.7(8) . . . . ?
C18 N4 C36 C37 105.3(8) . . . . ?
C19 C20 C21 C22 2.6(11) . . . . ?
C19 C20 C26 N5 -9.7(13) . . . . ?
C19 C24 C27 N6 -7.9(12) . . . . ?
C20 C19 C24 C23 0.3(9) . . . . ?
C20 C19 C24 C27 175.4(6) . . . . ?
C20 C21 C22 C23 -0.5(11) . . . . ?
C20 C21 C22 C25 -178.5(8) . . . . ?
C21 C20 C26 N5 165.6(8) . . . . ?
C21 C22 C23 C24 -1.7(11) . . . . ?
C22 C23 C24 C19 1.9(11) . . . . ?
C22 C23 C24 C27 -174.1(7) . . . . ?
C23 C24 C27 N6 167.6(7) . . . . ?
C24 C19 C20 C21 -2.4(10) . . . . ?
C24 C19 C20 C26 172.6(7) . . . . ?
C25 C22 C23 C24 176.2(8) . . . . ?
C26 N5 C32 C33 -158.5(8) . . . . ?
C26 C20 C21 C22 -173.0(7) . . . . ?
C27 N6 C38 C39 -167.8(7) . . . . ?
C28 N1 C8 C2 -171.4(7) . . . . ?
C29 N7 C31 C30 -140.0(8) . . . . ?
C29 N7 C33 C32 172.6(7) . . . . ?
C30 N3 C17 C11 -170.8(7) . . . . ?
C31 N7 C29 C28 87.3(7) . . . . ?
C31 N7 C33 C32 -66.7(8) . . . . ?
C32 N5 C26 C20 -173.1(8) . . . . ?
C33 N7 C29 C28 -151.1(6) . . . . ?
C33 N7 C31 C30 98.7(8) . . . . ?
C34 N2 C9 C6 -172.0(7) . . . . ?
C35 N8 C37 C36 86.9(8) . . . . ?
C35 N8 C39 C38 -67.0(8) . . . . ?
C36 N4 C18 C15 -170.6(8) . . . . ?
C37 N8 C35 C34 -138.4(7) . . . . ?
C37 N8 C39 C38 171.7(6) . . . . ?
C38 N6 C27 C24 -172.8(7) . . . . ?
C39 N8 C35 C34 100.8(7) . . . . ?
C39 N8 C37 C36 -151.8(7) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_submission_original_sample_id D8V4658
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_d8v4640_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc2747m8
_database_code_depnum_ccdc_archive 'CCDC 2059659'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv.13667729.v1 2021
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-02-03 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_audit_creation_date             2021-02-03
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H45 Gd N10 O9 Yb, N O3, 2.5(H2 O)'
_chemical_formula_sum            'C39 H50 Gd N11 O14.50 Yb'
_chemical_formula_weight         1235.19
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-x, -y, z+1/2'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   17.6212(3)
_cell_length_b                   17.6212(3)
_cell_length_c                   29.1165(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9040.9(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.730
_cell_measurement_theta_min      2.396
_shelx_estimated_absorpt_T_max   0.808
_shelx_estimated_absorpt_T_min   0.318
_exptl_absorpt_coefficient_mu    3.590
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1494 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.6621.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             4888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.0310
0.00 -1.00 0.00 0.0290
-1.00 0.00 0.00 0.0330
1.00 0.00 0.00 0.0220
0.00 0.00 -1.00 0.1610
0.00 0.00 1.00 0.2070

_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.062
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            70720
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.814
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7863
_reflns_number_total             8257
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Flack x determined using 3329 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8257
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+18.7897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0618
_refine_special_details          
;
Both metal centres were modelled as substitionally disordered.  One of the nitrate ligands was modelled as disordered, consistent with peaks in a difference map.  The nitrate counterion and one water of crystallization were modelled as disordered over two sites with geometric and displacement ellipsoid restraints used.  In all cases water H atoms were identified from difference peaks which corresponded with likely hydrogen bonding interactions.  Water H atoms were refined using a riding model with geometric restraints.  One of the water molecules lies on a special position, hence a fractional value in the chemical formula.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

420_ALERT_2_B D-H Without Acceptor       O13      --H13B     .     Please Check

Disordered water, as discussed above.

#===============================================================================
090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       7.40 Note

Weak non-centrosymmetric data set cut at 0.83 A resolution

161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .        O13 Check
161_ALERT_4_C Missing or Zero s.u. (esd) on x-coordinate for .       O13A Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .        O13 Check
162_ALERT_4_C Missing or Zero s.u. (esd) on y-coordinate for .       O13A Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .        O13 Check
163_ALERT_4_C Missing or Zero s.u. (esd) on z-coordinate for .       O13A Check

Disordered water, discussed above

213_ALERT_2_C Atom C13             has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C16             has ADP max/min Ratio .....        3.4 prolat
218_ALERT_3_C Constrained U(ij) Components(s) for O13        .          6 Check
218_ALERT_3_C Constrained U(ij) Components(s) for O13A       .          6 Check
220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.8 Ratio
220_ALERT_2_C NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        4.8 Ratio
222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.1 Ratio

Disordered water, discussed above

241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O5 Check
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         O7 Check

Disordered nitrate

342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............      0.011 Ang.
601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .         81 Ang**3
911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          6 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          4 Note
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Yb1, Gd1A}
{Gd2, Yb2A}
3. Restrained distances
 O13A-H13C = O13A-H13D = O13-H13A = O13-H13B = O16-H16D = O16-H16E = O14-H14A
 0.84 with sigma of 0.02
 O15-H15
 0.84 with sigma of 0.02
 H16E-H16D_$1
 1.35 with sigma of 0.04
 H16E-H16D = H13B-H13A = H13D-H13C
 1.35 with sigma of 0.04
 H14A-H14A_$1
 1.35 with sigma of 0.04
 H15-H15_$2
 1.35 with sigma of 0.04
 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim
O12-N11
 with sigma of 0.02
 N9-O4 \\sim N9-O4A \\sim N9-O5 \\sim N9-O6
 with sigma of 0.02
4. Restrained planarity
 O4, O4A, O5, N9
 with sigma of 0.1
 O4, O5, O6, N9
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(Yb1) = Uanis(Gd1A)
Uanis(Gd2) = Uanis(Yb2A)
6. Rigid body (RIGU) restrains
 O10, O11, O12, N11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10A, O11A, O12A, N11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O5, O6, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, O4A, O5, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, O11, O12, N11}
{O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, O11A, O12A, N11A}
8. Others
 Sof(Yb2A)=Sof(Gd1A)=1-FVAR(1)
 Sof(Yb1)=Sof(Gd2)=FVAR(1)
 Sof(O4A)=1-FVAR(2)
 Sof(O4)=FVAR(2)
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5)
 N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5)
9.a Everything fixed:
 O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O16, H16D, H16E
9.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30B,H30A), C31(H31A,H31B), C32(H32B,
 H32A), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
9.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C21(H21), C23(H23), C26(H26), C27(H27)
9.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.85718(2) 0.39136(2) 0.60345(2) 0.01597(10) Uani 0.511(9) 1 d . . P A 1
Yb2A Yb 0.94782(2) 0.31576(2) 0.50770(2) 0.01712(11) Uani 0.489(9) 1 d . . P A
2
Gd1A Gd 0.85718(2) 0.39136(2) 0.60345(2) 0.01597(10) Uani 0.489(9) 1 d . . P A
2
Gd2 Gd 0.94782(2) 0.31576(2) 0.50770(2) 0.01712(11) Uani 0.511(9) 1 d . . P A 1
O1 O 0.8246(3) 0.3523(3) 0.53074(15) 0.0208(10) Uani 1 1 d . . . . .
O2 O 0.9151(3) 0.2771(3) 0.58038(16) 0.0226(11) Uani 1 1 d . . . . .
O3 O 0.9598(3) 0.4267(3) 0.55372(16) 0.0225(11) Uani 1 1 d . . . . .
O4 O 0.8224(6) 0.5138(9) 0.5482(4) 0.058(4) Uani 0.576(17) 1 d D . P A 1
O4A O 0.7761(14) 0.5905(10) 0.5729(9) 0.099(10) Uani 0.424(17) 1 d D . P A 2
O5 O 0.7478(4) 0.4666(4) 0.5878(2) 0.0487(16) Uani 1 1 d D . . . .
O6 O 0.7014(4) 0.5435(4) 0.5371(2) 0.0569(19) Uani 1 1 d D . . B 1
O7 O 1.0767(4) 0.3108(3) 0.5664(2) 0.0430(16) Uani 1 1 d D . . . .
O8 O 1.0426(3) 0.2182(3) 0.52316(16) 0.0266(11) Uani 1 1 d D . . . .
O9 O 1.1314(4) 0.2014(4) 0.5735(3) 0.063(2) Uani 1 1 d D . . . .
N10 N 1.0851(4) 0.2426(4) 0.5549(2) 0.0344(16) Uani 1 1 d D . . . .
N1 N 0.7468(3) 0.3130(3) 0.61587(19) 0.0199(12) Uani 1 1 d . . . . .
N2 N 0.8787(4) 0.3734(3) 0.44301(19) 0.0234(13) Uani 1 1 d . . . . .
N3 N 0.9277(3) 0.3369(4) 0.6678(2) 0.0279(15) Uani 1 1 d . . . . .
N4 N 0.8913(4) 0.1928(3) 0.4961(2) 0.0254(13) Uani 1 1 d . . . . .
N5 N 0.8939(4) 0.5143(4) 0.6355(2) 0.0306(15) Uani 1 1 d . . . . .
N6 N 1.0595(3) 0.3745(3) 0.4732(2) 0.0235(13) Uani 1 1 d . . . . .
N7 N 0.7949(3) 0.4177(4) 0.6848(2) 0.0252(14) Uani 1 1 d . . . . .
N8 N 0.9841(4) 0.2590(4) 0.4257(2) 0.0267(14) Uani 1 1 d . . . . .
N9 N 0.7524(4) 0.5196(6) 0.5612(3) 0.058(2) Uani 1 1 d D . . . .
C1 C 0.7559(4) 0.3471(4) 0.5124(2) 0.0196(14) Uani 1 1 d . . . . .
C2 C 0.6919(4) 0.3254(4) 0.5386(2) 0.0219(15) Uani 1 1 d . . . . .
C3 C 0.6197(4) 0.3258(4) 0.5178(2) 0.0242(16) Uani 1 1 d . . . . .
H3 H 0.576887 0.311030 0.535535 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6091(5) 0.3470(5) 0.4725(3) 0.0299(17) Uani 1 1 d . . . . .
C5 C 0.6722(5) 0.3642(4) 0.4466(3) 0.0263(17) Uani 1 1 d . . . . .
H5 H 0.665912 0.377249 0.415150 0.032 Uiso 1 1 calc R U . . .
C6 C 0.7445(4) 0.3632(4) 0.4652(2) 0.0203(14) Uani 1 1 d . . . . .
C7 C 0.5292(5) 0.3486(6) 0.4526(3) 0.041(2) Uani 1 1 d . . . . .
H7A H 0.512754 0.296627 0.445810 0.062 Uiso 1 1 calc R U . . .
H7B H 0.528909 0.378647 0.424329 0.062 Uiso 1 1 calc R U . . .
H7C H 0.494436 0.371380 0.474988 0.062 Uiso 1 1 calc R U . . .
C8 C 0.6931(4) 0.3039(4) 0.5870(2) 0.0207(15) Uani 1 1 d . . . . .
H8 H 0.648401 0.280324 0.598450 0.025 Uiso 1 1 calc R U . . .
C9 C 0.8066(5) 0.3793(4) 0.4342(2) 0.0244(16) Uani 1 1 d . . . . .
H9 H 0.793281 0.395991 0.404220 0.029 Uiso 1 1 calc R U . . .
C10 C 0.9210(4) 0.2092(4) 0.5993(3) 0.0231(15) Uani 1 1 d . . . . .
C11 C 0.9389(4) 0.2024(5) 0.6466(3) 0.0325(19) Uani 1 1 d . . . . .
C12 C 0.9489(5) 0.1307(6) 0.6665(3) 0.041(2) Uani 1 1 d . . . . .
H12 H 0.962408 0.127533 0.698030 0.049 Uiso 1 1 calc R U . . .
C13 C 0.9398(5) 0.0644(5) 0.6416(4) 0.044(3) Uani 1 1 d . . . . .
C14 C 0.9199(4) 0.0710(5) 0.5956(3) 0.036(2) Uani 1 1 d . . . . .
H14 H 0.913190 0.026127 0.578011 0.043 Uiso 1 1 calc R U . . .
C15 C 0.9093(4) 0.1418(4) 0.5741(3) 0.0274(17) Uani 1 1 d . . . . .
C16 C 0.9512(6) -0.0131(6) 0.6631(5) 0.069(4) Uani 1 1 d . . . . .
H16A H 0.987535 -0.042267 0.644743 0.103 Uiso 1 1 calc R U . . .
H16B H 0.902563 -0.040113 0.664101 0.103 Uiso 1 1 calc R U . . .
H16C H 0.970783 -0.007147 0.694406 0.103 Uiso 1 1 calc R U . . .
C17 C 0.9447(4) 0.2673(6) 0.6764(3) 0.037(2) Uani 1 1 d . . . . .
H17 H 0.963617 0.257464 0.706404 0.044 Uiso 1 1 calc R U . . .
C18 C 0.8893(4) 0.1384(4) 0.5253(3) 0.0268(16) Uani 1 1 d . . . . .
H18 H 0.872995 0.090486 0.514098 0.032 Uiso 1 1 calc R U . . .
C19 C 1.0075(4) 0.4855(4) 0.5527(2) 0.0184(14) Uani 1 1 d . . . . .
C20 C 0.9956(4) 0.5512(4) 0.5812(2) 0.0211(14) Uani 1 1 d . . . . .
C21 C 1.0443(4) 0.6137(4) 0.5776(3) 0.0238(15) Uani 1 1 d . . . . .
H21 H 1.033434 0.657538 0.595380 0.029 Uiso 1 1 calc R U . . .
C22 C 1.1074(4) 0.6147(4) 0.5493(3) 0.0263(16) Uani 1 1 d . . . . .
C23 C 1.1202(4) 0.5518(4) 0.5234(2) 0.0229(15) Uani 1 1 d . . . . .
H23 H 1.163911 0.550841 0.504261 0.027 Uiso 1 1 calc R U . . .
C24 C 1.0717(4) 0.4877(4) 0.5233(2) 0.0198(15) Uani 1 1 d . . . . .
C25 C 1.1555(5) 0.6854(5) 0.5466(3) 0.044(2) Uani 1 1 d . . . . .
H25A H 1.123456 0.728786 0.538384 0.066 Uiso 1 1 calc R U . . .
H25B H 1.194891 0.678604 0.523232 0.066 Uiso 1 1 calc R U . . .
H25C H 1.179338 0.694734 0.576496 0.066 Uiso 1 1 calc R U . . .
C26 C 0.9392(4) 0.5612(4) 0.6175(3) 0.0295(17) Uani 1 1 d . . . . .
H26 H 0.936162 0.611200 0.629588 0.035 Uiso 1 1 calc R U . . .
C27 C 1.0950(4) 0.4329(4) 0.4886(2) 0.0212(14) Uani 1 1 d . . . . .
H27 H 1.143624 0.441606 0.475520 0.025 Uiso 1 1 calc R U . . .
C28 C 0.7298(4) 0.2978(4) 0.6643(2) 0.0228(16) Uani 1 1 d . . . . .
H28A H 0.771139 0.267681 0.678367 0.027 Uiso 1 1 calc R U . . .
H28B H 0.681897 0.268800 0.667003 0.027 Uiso 1 1 calc R U . . .
C29 C 0.7224(4) 0.3747(4) 0.6885(2) 0.0252(17) Uani 1 1 d . . . . .
H29A H 0.680790 0.404246 0.674243 0.030 Uiso 1 1 calc R U . . .
H29B H 0.709685 0.366645 0.721244 0.030 Uiso 1 1 calc R U . . .
C30 C 0.9296(5) 0.3884(7) 0.7074(3) 0.044(2) Uani 1 1 d . . . . .
H30B H 0.950558 0.438377 0.698390 0.053 Uiso 1 1 calc R U . . .
H30A H 0.961300 0.367016 0.732267 0.053 Uiso 1 1 calc R U . . .
C31 C 0.8467(4) 0.3964(6) 0.7232(2) 0.035(2) Uani 1 1 d . . . . .
H31A H 0.829649 0.347714 0.736593 0.042 Uiso 1 1 calc R U . . .
H31B H 0.843790 0.435618 0.747449 0.042 Uiso 1 1 calc R U . . .
C32 C 0.8512(5) 0.5448(6) 0.6754(3) 0.046(3) Uani 1 1 d . . . . .
H32B H 0.836585 0.597981 0.668920 0.055 Uiso 1 1 calc R U . . .
H32A H 0.884547 0.544801 0.702705 0.055 Uiso 1 1 calc R U . . .
C33 C 0.7798(4) 0.4989(5) 0.6860(3) 0.0325(19) Uani 1 1 d . . . . .
H33A H 0.760639 0.512933 0.716831 0.039 Uiso 1 1 calc R U . . .
H33B H 0.739868 0.511320 0.663284 0.039 Uiso 1 1 calc R U . . .
C34 C 0.9280(5) 0.3836(5) 0.4026(3) 0.0334(18) Uani 1 1 d . . . . .
H34A H 0.972916 0.414485 0.410678 0.040 Uiso 1 1 calc R U . . .
H34B H 0.899964 0.409582 0.377655 0.040 Uiso 1 1 calc R U . . .
C35 C 0.9520(5) 0.3057(5) 0.3874(2) 0.0309(17) Uani 1 1 d . . . . .
H35A H 0.907633 0.279034 0.374175 0.037 Uiso 1 1 calc R U . . .
H35B H 0.990631 0.310709 0.362851 0.037 Uiso 1 1 calc R U . . .
C36 C 0.8793(5) 0.1723(5) 0.4480(3) 0.0313(18) Uani 1 1 d . . . . .
H36A H 0.841369 0.206546 0.433880 0.038 Uiso 1 1 calc R U . . .
H36B H 0.860387 0.119547 0.445739 0.038 Uiso 1 1 calc R U . . .
C37 C 0.9558(5) 0.1798(5) 0.4232(3) 0.0324(18) Uani 1 1 d . . . . .
H37A H 0.993239 0.145261 0.437593 0.039 Uiso 1 1 calc R U . . .
H37B H 0.949862 0.164802 0.390684 0.039 Uiso 1 1 calc R U . . .
C38 C 1.0982(5) 0.3393(4) 0.4331(3) 0.0321(19) Uani 1 1 d . . . . .
H38A H 1.153399 0.336571 0.439152 0.038 Uiso 1 1 calc R U . . .
H38B H 1.090263 0.371346 0.405606 0.038 Uiso 1 1 calc R U . . .
C39 C 1.0673(5) 0.2592(5) 0.4240(3) 0.0313(19) Uani 1 1 d . . . . .
H39A H 1.084425 0.241728 0.393351 0.038 Uiso 1 1 calc R U . . .
H39B H 1.087597 0.223657 0.447271 0.038 Uiso 1 1 calc R U . . .
O10 O 0.5441(12) 0.2938(11) 0.7082(6) 0.094(6) Uani 0.5 1 d D . P C 1
O11 O 0.5280(12) 0.2631(11) 0.6371(8) 0.131(10) Uani 0.5 1 d D . P C 1
O12 O 0.5037(15) 0.3732(11) 0.6592(8) 0.124(9) Uani 0.5 1 d D . P C 1
N11 N 0.5246(8) 0.3086(8) 0.6695(6) 0.047(4) Uani 0.5 1 d D . P C 1
O10A O 0.4267(13) 0.2860(11) 0.5486(5) 0.102(7) Uani 0.5 1 d D . P D 2
O11A O 0.5097(9) 0.2374(12) 0.5917(8) 0.110(8) Uani 0.5 1 d D . P D 2
O12A O 0.4285(16) 0.3137(12) 0.6191(7) 0.150(11) Uani 0.5 1 d D . P D 2
N11A N 0.4537(7) 0.2787(8) 0.5874(4) 0.034(3) Uani 0.5 1 d D . P D 2
O13 O 0.437800 0.264370 0.561150 0.092 Uani 0.5 1 d D . P E 1
H13A H 0.435470 0.294050 0.589850 0.110 Uiso 0.5 1 d D U P F 1
H13B H 0.402240 0.305990 0.546630 0.110 Uiso 0.5 1 d D U P G 1
O13A O 0.532020 0.302410 0.706160 0.043 Uani 0.5 1 d D . P H 2
H13C H 0.535730 0.347780 0.715580 0.051 Uiso 0.5 1 d D U P I 2
H13D H 0.521250 0.308890 0.677430 0.051 Uiso 0.5 1 d D U P J 2
O14 O 1.060260 0.060260 0.500000 0.045 Uani 1 2 d DS T P . .
H14A H 1.061250 0.100540 0.515750 0.054 Uiso 1 1 d D U . . .
O15 O 0.8031(3) 0.1969(3) 0.750000 0.044(2) Uani 1 2 d DS T P . .
H15 H 0.846(3) 0.196(4) 0.764(3) 0.052 Uiso 1 1 d D U . . .
O16 O 0.949400 -0.050600 0.500000 0.053 Uani 1 2 d DS T P . .
H16D H 0.919680 -0.043180 0.478650 0.064 Uiso 0.5 1 d D U P . .
H16E H 0.982770 -0.017230 0.500000 0.064 Uiso 1 2 d DS 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
Yb1 Gd2 3.4782(4) . ?
Yb1 O1 2.299(4) . ?
Yb1 O2 2.355(5) . ?
Yb1 O3 2.399(5) . ?
Yb1 O4 2.760(15) . ?
Yb1 O5 2.383(6) . ?
Yb1 N1 2.412(6) . ?
Yb1 N3 2.445(6) . ?
Yb1 N5 2.446(6) . ?
Yb1 N7 2.651(6) . ?
Yb2A Gd1A 3.4782(4) . ?
Yb2A O1 2.363(5) . ?
Yb2A O2 2.297(5) . ?
Yb2A O3 2.380(5) . ?
Yb2A O7 2.844(7) . ?
Yb2A O8 2.439(5) . ?
Yb2A N10 3.066(7) . ?
Yb2A N2 2.463(6) . ?
Yb2A N4 2.409(6) . ?
Yb2A N6 2.440(6) . ?
Yb2A N8 2.666(6) . ?
Gd1A O1 2.299(4) . ?
Gd1A O2 2.355(5) . ?
Gd1A O3 2.399(5) . ?
Gd1A O5 2.383(6) . ?
Gd1A N1 2.412(6) . ?
Gd1A N3 2.445(6) . ?
Gd1A N5 2.446(6) . ?
Gd1A N7 2.651(6) . ?
Gd2 O1 2.363(5) . ?
Gd2 O2 2.297(5) . ?
Gd2 O3 2.380(5) . ?
Gd2 O7 2.844(7) . ?
Gd2 O8 2.439(5) . ?
Gd2 N2 2.463(6) . ?
Gd2 N4 2.409(6) . ?
Gd2 N6 2.440(6) . ?
Gd2 N8 2.666(6) . ?
O1 C1 1.325(8) . ?
O2 C10 1.321(9) . ?
O3 C19 1.334(8) . ?
O4 N9 1.294(12) . ?
O4A N9 1.360(16) . ?
O5 N9 1.217(9) . ?
O6 N9 1.215(9) . ?
O7 N10 1.256(8) . ?
O8 N10 1.265(8) . ?
O9 N10 1.219(8) . ?
N1 C8 1.276(9) . ?
N1 C28 1.466(9) . ?
N2 C9 1.300(10) . ?
N2 C34 1.474(9) . ?
N3 C17 1.287(12) . ?
N3 C30 1.466(10) . ?
N4 C18 1.284(9) . ?
N4 C36 1.460(10) . ?
N5 C26 1.263(10) . ?
N5 C32 1.484(10) . ?
N6 C27 1.286(9) . ?
N6 C38 1.486(9) . ?
N7 C29 1.490(9) . ?
N7 C31 1.492(10) . ?
N7 C33 1.455(11) . ?
N8 C35 1.500(9) . ?
N8 C37 1.483(10) . ?
N8 C39 1.467(10) . ?
C1 C2 1.415(10) . ?
C1 C6 1.419(9) . ?
C2 C3 1.408(10) . ?
C2 C8 1.461(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(10) . ?
C4 C5 1.377(11) . ?
C4 C7 1.522(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(11) . ?
C6 C9 1.446(10) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.416(11) . ?
C10 C15 1.413(11) . ?
C11 C12 1.402(12) . ?
C11 C17 1.440(13) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(15) . ?
C13 C14 1.390(14) . ?
C13 C16 1.515(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.407(10) . ?
C15 C18 1.464(11) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.441(10) . ?
C19 C24 1.418(10) . ?
C20 C21 1.399(10) . ?
C20 C26 1.462(10) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(10) . ?
C22 C23 1.360(11) . ?
C22 C25 1.509(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.416(10) . ?
C24 C27 1.456(10) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.533(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 C31 1.537(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 C33 1.528(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.502(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.535(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.537(11) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
O10 N11 1.205(15) . ?
O11 N11 1.241(15) . ?
O12 N11 1.234(16) . ?
O10A N11A 1.233(14) . ?
O11A N11A 1.232(15) . ?
O12A N11A 1.196(14) . ?
O13 H13A 0.9867 . ?
O13 H13A 0.9867 . ?
O13 H13B 1.0532 . ?
O13A H13C 0.8477 . ?
O13A H13D 0.8653 . ?
O14 H14A 0.8452 . ?
O14 H14A 0.8452 7_646 ?
O15 H15 0.86(3) . ?
O15 H15 0.86(3) 8_666 ?
O16 H16D 0.8233 7_646 ?
O16 H16D 0.8233 . ?
O16 H16E 0.8316 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Yb1 Gd2 42.45(12) . . ?
O1 Yb1 O2 65.77(17) . . ?
O1 Yb1 O3 73.16(16) . . ?
O1 Yb1 O4 69.0(3) . . ?
O1 Yb1 O5 77.78(19) . . ?
O1 Yb1 N1 76.41(18) . . ?
O1 Yb1 N3 135.7(2) . . ?
O1 Yb1 N5 133.1(2) . . ?
O1 Yb1 N7 140.48(17) . . ?
O2 Yb1 Gd2 40.98(11) . . ?
O2 Yb1 O3 73.94(17) . . ?
O2 Yb1 O4 126.7(3) . . ?
O2 Yb1 O5 140.47(19) . . ?
O2 Yb1 N1 84.40(19) . . ?
O2 Yb1 N3 70.31(19) . . ?
O2 Yb1 N5 138.7(2) . . ?
O2 Yb1 N7 125.72(19) . . ?
O3 Yb1 Gd2 43.07(11) . . ?
O3 Yb1 O4 67.2(2) . . ?
O3 Yb1 N1 147.86(17) . . ?
O3 Yb1 N3 100.47(19) . . ?
O3 Yb1 N5 78.52(18) . . ?
O3 Yb1 N7 143.69(17) . . ?
O4 Yb1 Gd2 86.2(2) . . ?
O5 Yb1 Gd2 115.55(15) . . ?
O5 Yb1 O3 110.5(2) . . ?
O5 Yb1 O4 43.5(3) . . ?
O5 Yb1 N1 72.2(2) . . ?
O5 Yb1 N3 140.9(2) . . ?
O5 Yb1 N5 78.2(2) . . ?
O5 Yb1 N7 74.8(2) . . ?
N1 Yb1 Gd2 105.73(14) . . ?
N1 Yb1 O4 110.9(3) . . ?
N1 Yb1 N3 94.0(2) . . ?
N1 Yb1 N5 131.5(2) . . ?
N1 Yb1 N7 68.44(19) . . ?
N3 Yb1 Gd2 103.35(14) . . ?
N3 Yb1 O4 150.1(3) . . ?
N3 Yb1 N5 85.4(2) . . ?
N3 Yb1 N7 66.1(2) . . ?
N5 Yb1 Gd2 121.57(15) . . ?
N5 Yb1 O4 65.8(3) . . ?
N5 Yb1 N7 67.3(2) . . ?
N7 Yb1 Gd2 166.70(15) . . ?
N7 Yb1 O4 107.0(3) . . ?
O1 Yb2A Gd1A 41.05(11) . . ?
O1 Yb2A O3 72.40(17) . . ?
O1 Yb2A O7 124.86(16) . . ?
O1 Yb2A O8 140.28(17) . . ?
O1 Yb2A N10 135.44(17) . . ?
O1 Yb2A N2 69.50(18) . . ?
O1 Yb2A N4 84.53(19) . . ?
O1 Yb2A N6 137.94(19) . . ?
O1 Yb2A N8 125.25(18) . . ?
O2 Yb2A Gd1A 42.25(12) . . ?
O2 Yb2A O1 65.68(17) . . ?
O2 Yb2A O3 75.36(17) . . ?
O2 Yb2A O7 68.75(18) . . ?
O2 Yb2A O8 78.05(17) . . ?
O2 Yb2A N10 70.16(18) . . ?
O2 Yb2A N2 134.64(19) . . ?
O2 Yb2A N4 76.05(19) . . ?
O2 Yb2A N6 135.1(2) . . ?
O2 Yb2A N8 140.70(18) . . ?
O3 Yb2A Gd1A 43.51(11) . . ?
O3 Yb2A O7 67.41(17) . . ?
O3 Yb2A O8 114.50(18) . . ?
O3 Yb2A N10 91.32(18) . . ?
O3 Yb2A N2 97.78(18) . . ?
O3 Yb2A N4 148.75(18) . . ?
O3 Yb2A N6 79.15(18) . . ?
O3 Yb2A N8 142.30(18) . . ?
O7 Yb2A Gd1A 84.06(11) . . ?
O7 Yb2A N10 24.17(16) . . ?
O8 Yb2A Gd1A 115.88(11) . . ?
O8 Yb2A O7 47.21(16) . . ?
O8 Yb2A N10 23.18(17) . . ?
O8 Yb2A N2 140.43(17) . . ?
O8 Yb2A N6 79.82(19) . . ?
O8 Yb2A N8 74.71(17) . . ?
N10 Yb2A Gd1A 99.44(12) . . ?
N2 Yb2A Gd1A 103.16(13) . . ?
N2 Yb2A O7 150.19(19) . . ?
N2 Yb2A N10 155.05(19) . . ?
N2 Yb2A N8 65.73(19) . . ?
N4 Yb2A Gd1A 105.50(14) . . ?
N4 Yb2A O7 112.79(19) . . ?
N4 Yb2A O8 71.0(2) . . ?
N4 Yb2A N10 90.7(2) . . ?
N4 Yb2A N2 93.4(2) . . ?
N4 Yb2A N6 131.1(2) . . ?
N4 Yb2A N8 68.6(2) . . ?
N6 Yb2A Gd1A 122.54(14) . . ?
N6 Yb2A O7 67.48(19) . . ?
N6 Yb2A N10 74.2(2) . . ?
N6 Yb2A N2 84.8(2) . . ?
N6 Yb2A N8 66.2(2) . . ?
N8 Yb2A Gd1A 166.30(14) . . ?
N8 Yb2A O7 109.58(18) . . ?
N8 Yb2A N10 93.10(18) . . ?
O1 Gd1A Yb2A 42.45(12) . . ?
O1 Gd1A O2 65.77(17) . . ?
O1 Gd1A O3 73.16(16) . . ?
O1 Gd1A O5 77.78(19) . . ?
O1 Gd1A N1 76.41(18) . . ?
O1 Gd1A N3 135.7(2) . . ?
O1 Gd1A N5 133.1(2) . . ?
O1 Gd1A N7 140.48(17) . . ?
O2 Gd1A Yb2A 40.98(11) . . ?
O2 Gd1A O3 73.94(17) . . ?
O2 Gd1A O5 140.47(19) . . ?
O2 Gd1A N1 84.40(19) . . ?
O2 Gd1A N3 70.31(19) . . ?
O2 Gd1A N5 138.7(2) . . ?
O2 Gd1A N7 125.72(19) . . ?
O3 Gd1A Yb2A 43.07(11) . . ?
O3 Gd1A N1 147.86(17) . . ?
O3 Gd1A N3 100.47(19) . . ?
O3 Gd1A N5 78.52(18) . . ?
O3 Gd1A N7 143.69(17) . . ?
O5 Gd1A Yb2A 115.55(15) . . ?
O5 Gd1A O3 110.5(2) . . ?
O5 Gd1A N1 72.2(2) . . ?
O5 Gd1A N3 140.9(2) . . ?
O5 Gd1A N5 78.2(2) . . ?
O5 Gd1A N7 74.8(2) . . ?
N1 Gd1A Yb2A 105.73(14) . . ?
N1 Gd1A N3 94.0(2) . . ?
N1 Gd1A N5 131.5(2) . . ?
N1 Gd1A N7 68.44(19) . . ?
N3 Gd1A Yb2A 103.35(14) . . ?
N3 Gd1A N5 85.4(2) . . ?
N3 Gd1A N7 66.1(2) . . ?
N5 Gd1A Yb2A 121.57(15) . . ?
N5 Gd1A N7 67.3(2) . . ?
N7 Gd1A Yb2A 166.70(15) . . ?
O1 Gd2 Yb1 41.05(11) . . ?
O1 Gd2 O3 72.40(17) . . ?
O1 Gd2 O7 124.86(16) . . ?
O1 Gd2 O8 140.28(17) . . ?
O1 Gd2 N2 69.50(18) . . ?
O1 Gd2 N4 84.53(19) . . ?
O1 Gd2 N6 137.94(19) . . ?
O1 Gd2 N8 125.25(18) . . ?
O2 Gd2 Yb1 42.25(12) . . ?
O2 Gd2 O1 65.68(17) . . ?
O2 Gd2 O3 75.36(17) . . ?
O2 Gd2 O7 68.75(18) . . ?
O2 Gd2 O8 78.05(17) . . ?
O2 Gd2 N2 134.64(19) . . ?
O2 Gd2 N4 76.05(19) . . ?
O2 Gd2 N6 135.1(2) . . ?
O2 Gd2 N8 140.70(18) . . ?
O3 Gd2 Yb1 43.51(11) . . ?
O3 Gd2 O7 67.41(17) . . ?
O3 Gd2 O8 114.50(18) . . ?
O3 Gd2 N2 97.78(18) . . ?
O3 Gd2 N4 148.75(18) . . ?
O3 Gd2 N6 79.15(18) . . ?
O3 Gd2 N8 142.30(18) . . ?
O7 Gd2 Yb1 84.06(11) . . ?
O8 Gd2 Yb1 115.88(11) . . ?
O8 Gd2 O7 47.21(16) . . ?
O8 Gd2 N2 140.43(17) . . ?
O8 Gd2 N6 79.82(19) . . ?
O8 Gd2 N8 74.71(17) . . ?
N2 Gd2 Yb1 103.16(13) . . ?
N2 Gd2 O7 150.19(19) . . ?
N2 Gd2 N8 65.73(19) . . ?
N4 Gd2 Yb1 105.50(14) . . ?
N4 Gd2 O7 112.79(19) . . ?
N4 Gd2 O8 71.0(2) . . ?
N4 Gd2 N2 93.4(2) . . ?
N4 Gd2 N6 131.1(2) . . ?
N4 Gd2 N8 68.6(2) . . ?
N6 Gd2 Yb1 122.54(14) . . ?
N6 Gd2 O7 67.48(19) . . ?
N6 Gd2 N2 84.8(2) . . ?
N6 Gd2 N8 66.2(2) . . ?
N8 Gd2 Yb1 166.30(14) . . ?
N8 Gd2 O7 109.58(18) . . ?
Yb1 O1 Gd2 96.50(17) . . ?
Gd1A O1 Yb2A 96.50(17) . . ?
C1 O1 Yb1 128.3(4) . . ?
C1 O1 Yb2A 134.9(4) . . ?
C1 O1 Gd1A 128.3(4) . . ?
C1 O1 Gd2 134.9(4) . . ?
Yb2A O2 Gd1A 96.78(18) . . ?
Gd2 O2 Yb1 96.78(18) . . ?
C10 O2 Yb1 133.6(4) . . ?
C10 O2 Yb2A 129.3(5) . . ?
C10 O2 Gd1A 133.6(4) . . ?
C10 O2 Gd2 129.3(5) . . ?
Yb2A O3 Gd1A 93.42(16) . . ?
Gd2 O3 Yb1 93.42(16) . . ?
C19 O3 Yb1 133.7(4) . . ?
C19 O3 Yb2A 132.9(4) . . ?
C19 O3 Gd1A 133.7(4) . . ?
C19 O3 Gd2 132.9(4) . . ?
N9 O4 Yb1 95.9(8) . . ?
N9 O5 Yb1 119.6(6) . . ?
N9 O5 Gd1A 119.6(6) . . ?
N10 O7 Yb2A 87.9(4) . . ?
N10 O7 Gd2 87.9(4) . . ?
N10 O8 Yb2A 107.5(4) . . ?
N10 O8 Gd2 107.5(4) . . ?
O7 N10 Yb2A 68.0(4) . . ?
O7 N10 O8 116.8(6) . . ?
O8 N10 Yb2A 49.3(3) . . ?
O9 N10 Yb2A 167.8(6) . . ?
O9 N10 O7 122.0(7) . . ?
O9 N10 O8 121.2(7) . . ?
C8 N1 Yb1 124.9(5) . . ?
C8 N1 Gd1A 124.9(5) . . ?
C8 N1 C28 117.2(6) . . ?
C28 N1 Yb1 114.4(4) . . ?
C28 N1 Gd1A 114.4(4) . . ?
C9 N2 Yb2A 131.9(5) . . ?
C9 N2 Gd2 131.9(5) . . ?
C9 N2 C34 114.1(6) . . ?
C34 N2 Yb2A 111.7(5) . . ?
C34 N2 Gd2 111.7(5) . . ?
C17 N3 Yb1 129.9(5) . . ?
C17 N3 Gd1A 129.9(5) . . ?
C17 N3 C30 115.6(7) . . ?
C30 N3 Yb1 111.7(6) . . ?
C30 N3 Gd1A 111.7(6) . . ?
C18 N4 Yb2A 126.1(5) . . ?
C18 N4 Gd2 126.1(5) . . ?
C18 N4 C36 116.6(6) . . ?
C36 N4 Yb2A 114.7(5) . . ?
C36 N4 Gd2 114.7(5) . . ?
C26 N5 Yb1 126.1(5) . . ?
C26 N5 Gd1A 126.1(5) . . ?
C26 N5 C32 114.1(6) . . ?
C32 N5 Yb1 119.0(5) . . ?
C32 N5 Gd1A 119.0(5) . . ?
C27 N6 Yb2A 126.0(5) . . ?
C27 N6 Gd2 126.0(5) . . ?
C27 N6 C38 112.7(6) . . ?
C38 N6 Yb2A 121.1(5) . . ?
C38 N6 Gd2 121.1(5) . . ?
C29 N7 Yb1 109.3(4) . . ?
C29 N7 Gd1A 109.3(4) . . ?
C29 N7 C31 110.1(6) . . ?
C31 N7 Yb1 111.8(4) . . ?
C31 N7 Gd1A 111.8(4) . . ?
C33 N7 Yb1 105.7(4) . . ?
C33 N7 Gd1A 105.7(4) . . ?
C33 N7 C29 109.9(6) . . ?
C33 N7 C31 109.9(6) . . ?
C35 N8 Yb2A 111.7(4) . . ?
C35 N8 Gd2 111.7(4) . . ?
C37 N8 Yb2A 108.4(4) . . ?
C37 N8 Gd2 108.4(4) . . ?
C37 N8 C35 110.7(6) . . ?
C39 N8 Yb2A 105.7(4) . . ?
C39 N8 Gd2 105.7(4) . . ?
C39 N8 C35 110.5(6) . . ?
C39 N8 C37 109.7(6) . . ?
O5 N9 O4 100.9(10) . . ?
O5 N9 O4A 124.4(12) . . ?
O6 N9 O4 124.4(9) . . ?
O6 N9 O5 125.7(8) . . ?
O1 C1 C2 122.1(6) . . ?
O1 C1 C6 120.4(6) . . ?
C2 C1 C6 117.5(6) . . ?
C1 C2 C8 125.3(6) . . ?
C3 C2 C1 119.3(6) . . ?
C3 C2 C8 115.4(6) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.2(7) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C7 119.4(7) . . ?
C5 C4 C3 118.2(7) . . ?
C5 C4 C7 122.4(7) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.7(7) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C9 122.4(7) . . ?
C5 C6 C1 120.8(7) . . ?
C5 C6 C9 116.7(6) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C2 127.8(7) . . ?
N1 C8 H8 116.1 . . ?
C2 C8 H8 116.1 . . ?
N2 C9 C6 126.9(7) . . ?
N2 C9 H9 116.6 . . ?
C6 C9 H9 116.6 . . ?
O2 C10 C11 120.0(7) . . ?
O2 C10 C15 122.2(7) . . ?
C15 C10 C11 117.8(7) . . ?
C10 C11 C17 122.4(7) . . ?
C12 C11 C10 120.4(8) . . ?
C12 C11 C17 117.2(8) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.0(8) . . ?
C13 C12 H12 119.0 . . ?
C12 C13 C14 117.5(7) . . ?
C12 C13 C16 122.0(10) . . ?
C14 C13 C16 120.5(11) . . ?
C13 C14 H14 118.8 . . ?
C13 C14 C15 122.5(9) . . ?
C15 C14 H14 118.8 . . ?
C10 C15 C18 125.0(7) . . ?
C14 C15 C10 119.6(7) . . ?
C14 C15 C18 115.3(8) . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C11 128.5(7) . . ?
N3 C17 H17 115.8 . . ?
C11 C17 H17 115.8 . . ?
N4 C18 C15 127.4(7) . . ?
N4 C18 H18 116.3 . . ?
C15 C18 H18 116.3 . . ?
O3 C19 C20 121.3(6) . . ?
O3 C19 C24 122.6(6) . . ?
C24 C19 C20 116.2(6) . . ?
C19 C20 C26 127.8(6) . . ?
C21 C20 C19 120.0(6) . . ?
C21 C20 C26 112.1(6) . . ?
C20 C21 H21 118.4 . . ?
C22 C21 C20 123.2(7) . . ?
C22 C21 H21 118.4 . . ?
C21 C22 C25 119.6(7) . . ?
C23 C22 C21 117.0(7) . . ?
C23 C22 C25 123.4(7) . . ?
C22 C23 H23 118.3 . . ?
C22 C23 C24 123.4(7) . . ?
C24 C23 H23 118.3 . . ?
C19 C24 C27 128.6(7) . . ?
C23 C24 C19 120.2(7) . . ?
C23 C24 C27 111.0(6) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 C20 130.6(7) . . ?
N5 C26 H26 114.7 . . ?
C20 C26 H26 114.7 . . ?
N6 C27 C24 129.5(6) . . ?
N6 C27 H27 115.3 . . ?
C24 C27 H27 115.3 . . ?
N1 C28 H28A 110.2 . . ?
N1 C28 H28B 110.2 . . ?
N1 C28 C29 107.3(6) . . ?
H28A C28 H28B 108.5 . . ?
C29 C28 H28A 110.2 . . ?
C29 C28 H28B 110.2 . . ?
N7 C29 C28 110.1(6) . . ?
N7 C29 H29A 109.6 . . ?
N7 C29 H29B 109.6 . . ?
C28 C29 H29A 109.6 . . ?
C28 C29 H29B 109.6 . . ?
H29A C29 H29B 108.2 . . ?
N3 C30 H30B 110.6 . . ?
N3 C30 H30A 110.6 . . ?
N3 C30 C31 105.7(6) . . ?
H30B C30 H30A 108.7 . . ?
C31 C30 H30B 110.6 . . ?
C31 C30 H30A 110.6 . . ?
N7 C31 C30 112.4(6) . . ?
N7 C31 H31A 109.1 . . ?
N7 C31 H31B 109.1 . . ?
C30 C31 H31A 109.1 . . ?
C30 C31 H31B 109.1 . . ?
H31A C31 H31B 107.9 . . ?
N5 C32 H32B 109.1 . . ?
N5 C32 H32A 109.1 . . ?
N5 C32 C33 112.7(6) . . ?
H32B C32 H32A 107.8 . . ?
C33 C32 H32B 109.1 . . ?
C33 C32 H32A 109.1 . . ?
N7 C33 C32 111.4(7) . . ?
N7 C33 H33A 109.4 . . ?
N7 C33 H33B 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
N2 C34 H34A 110.3 . . ?
N2 C34 H34B 110.3 . . ?
N2 C34 C35 106.9(6) . . ?
H34A C34 H34B 108.6 . . ?
C35 C34 H34A 110.3 . . ?
C35 C34 H34B 110.3 . . ?
N8 C35 C34 112.9(6) . . ?
N8 C35 H35A 109.0 . . ?
N8 C35 H35B 109.0 . . ?
C34 C35 H35A 109.0 . . ?
C34 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
N4 C36 H36A 110.2 . . ?
N4 C36 H36B 110.2 . . ?
N4 C36 C37 107.6(6) . . ?
H36A C36 H36B 108.5 . . ?
C37 C36 H36A 110.2 . . ?
C37 C36 H36B 110.2 . . ?
N8 C37 C36 110.7(6) . . ?
N8 C37 H37A 109.5 . . ?
N8 C37 H37B 109.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
N6 C38 H38A 109.4 . . ?
N6 C38 H38B 109.4 . . ?
N6 C38 C39 111.0(6) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
N8 C39 C38 110.5(6) . . ?
N8 C39 H39A 109.6 . . ?
N8 C39 H39B 109.6 . . ?
C38 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
O10 N11 O11 124(2) . . ?
O10 N11 O12 120.8(19) . . ?
O12 N11 O11 115(2) . . ?
O11A N11A O10A 117.7(18) . . ?
O12A N11A O10A 121(2) . . ?
O12A N11A O11A 121(2) . . ?
H13A O13 H13A 0.0 . . ?
H13A O13 H13B 86.9 . . ?
H13A O13 H13B 86.9 . . ?
H13C O13A H13D 101.8 . . ?
H14A O14 H14A 105.1 . 7_646 ?
H15 O15 H15 102(7) . 8_666 ?
H16D O16 H16D 140.6 . 7_646 ?
H16D O16 H16E 109.7 . . ?
H16E O16 H16D 109.7 . 7_646 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O14 H14A O8 0.85 2.11 2.880(5) 151.3 . yes
O16 H16E O14 0.83 1.93 2.763 180.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Yb1 O1 C1 C2 -35.3(9) . . . . ?
Yb1 O1 C1 C6 145.1(5) . . . . ?
Yb1 O2 C10 C11 -43.8(9) . . . . ?
Yb1 O2 C10 C15 135.5(6) . . . . ?
Yb1 O3 C19 C20 -10.8(10) . . . . ?
Yb1 O3 C19 C24 170.0(5) . . . . ?
Yb1 O4 N9 O5 -1.8(7) . . . . ?
Yb1 O4 N9 O6 -150.3(10) . . . . ?
Yb1 O5 N9 O4 2.4(10) . . . . ?
Yb1 O5 N9 O6 150.3(8) . . . . ?
Yb1 N1 C8 C2 12.6(10) . . . . ?
Yb1 N1 C28 C29 55.6(6) . . . . ?
Yb1 N3 C17 C11 12.2(12) . . . . ?
Yb1 N3 C30 C31 64.2(8) . . . . ?
Yb1 N5 C26 C20 -17.3(13) . . . . ?
Yb1 N5 C32 C33 -9.5(11) . . . . ?
Yb1 N7 C29 C28 36.3(7) . . . . ?
Yb1 N7 C31 C30 17.6(9) . . . . ?
Yb1 N7 C33 C32 -53.9(7) . . . . ?
Yb2A O1 C1 C2 136.8(6) . . . . ?
Yb2A O1 C1 C6 -42.8(10) . . . . ?
Yb2A O2 C10 C11 144.8(5) . . . . ?
Yb2A O2 C10 C15 -36.0(9) . . . . ?
Yb2A O3 C19 C20 171.3(5) . . . . ?
Yb2A O3 C19 C24 -7.8(10) . . . . ?
Yb2A O7 N10 O8 7.3(6) . . . . ?
Yb2A O7 N10 O9 -172.1(8) . . . . ?
Yb2A O8 N10 O7 -8.9(8) . . . . ?
Yb2A O8 N10 O9 170.5(7) . . . . ?
Yb2A N2 C9 C6 11.1(11) . . . . ?
Yb2A N2 C34 C35 63.4(7) . . . . ?
Yb2A N4 C18 C15 10.6(11) . . . . ?
Yb2A N4 C36 C37 54.7(7) . . . . ?
Yb2A N6 C27 C24 -14.0(11) . . . . ?
Yb2A N6 C38 C39 -9.8(9) . . . . ?
Yb2A N8 C35 C34 17.1(8) . . . . ?
Yb2A N8 C37 C36 36.8(7) . . . . ?
Yb2A N8 C39 C38 -55.5(7) . . . . ?
Gd1A O1 C1 C2 -35.3(9) . . . . ?
Gd1A O1 C1 C6 145.1(5) . . . . ?
Gd1A O2 C10 C11 -43.8(9) . . . . ?
Gd1A O2 C10 C15 135.5(6) . . . . ?
Gd1A O3 C19 C20 -10.8(10) . . . . ?
Gd1A O3 C19 C24 170.0(5) . . . . ?
Gd1A O5 N9 O4A -84.8(16) . . . . ?
Gd1A N1 C8 C2 12.6(10) . . . . ?
Gd1A N1 C28 C29 55.6(6) . . . . ?
Gd1A N3 C17 C11 12.2(12) . . . . ?
Gd1A N3 C30 C31 64.2(8) . . . . ?
Gd1A N5 C26 C20 -17.3(13) . . . . ?
Gd1A N5 C32 C33 -9.5(11) . . . . ?
Gd1A N7 C29 C28 36.3(7) . . . . ?
Gd1A N7 C31 C30 17.6(9) . . . . ?
Gd1A N7 C33 C32 -53.9(7) . . . . ?
Gd2 O1 C1 C2 136.8(6) . . . . ?
Gd2 O1 C1 C6 -42.8(10) . . . . ?
Gd2 O2 C10 C11 144.8(5) . . . . ?
Gd2 O2 C10 C15 -36.0(9) . . . . ?
Gd2 O3 C19 C20 171.3(5) . . . . ?
Gd2 O3 C19 C24 -7.8(10) . . . . ?
Gd2 O7 N10 O8 7.3(6) . . . . ?
Gd2 O7 N10 O9 -172.1(8) . . . . ?
Gd2 O8 N10 O7 -8.9(8) . . . . ?
Gd2 O8 N10 O9 170.5(7) . . . . ?
Gd2 N2 C9 C6 11.1(11) . . . . ?
Gd2 N2 C34 C35 63.4(7) . . . . ?
Gd2 N4 C18 C15 10.6(11) . . . . ?
Gd2 N4 C36 C37 54.7(7) . . . . ?
Gd2 N6 C27 C24 -14.0(11) . . . . ?
Gd2 N6 C38 C39 -9.8(9) . . . . ?
Gd2 N8 C35 C34 17.1(8) . . . . ?
Gd2 N8 C37 C36 36.8(7) . . . . ?
Gd2 N8 C39 C38 -55.5(7) . . . . ?
O1 C1 C2 C3 175.9(7) . . . . ?
O1 C1 C2 C8 -2.1(11) . . . . ?
O1 C1 C6 C5 -174.5(7) . . . . ?
O1 C1 C6 C9 5.3(11) . . . . ?
O2 C10 C11 C12 -177.0(7) . . . . ?
O2 C10 C11 C17 5.5(11) . . . . ?
O2 C10 C15 C14 177.1(7) . . . . ?
O2 C10 C15 C18 -0.3(11) . . . . ?
O3 C19 C20 C21 -176.6(6) . . . . ?
O3 C19 C20 C26 7.6(11) . . . . ?
O3 C19 C24 C23 179.5(6) . . . . ?
O3 C19 C24 C27 4.1(11) . . . . ?
N1 C28 C29 N7 -60.6(8) . . . . ?
N2 C34 C35 N8 -51.2(9) . . . . ?
N3 C30 C31 N7 -51.9(11) . . . . ?
N4 C36 C37 N8 -60.8(8) . . . . ?
N5 C32 C33 N7 44.9(11) . . . . ?
N6 C38 C39 N8 45.8(9) . . . . ?
C1 C2 C3 C4 -0.1(11) . . . . ?
C1 C2 C8 N1 13.0(12) . . . . ?
C1 C6 C9 N2 8.2(11) . . . . ?
C2 C1 C6 C5 5.9(10) . . . . ?
C2 C1 C6 C9 -174.3(7) . . . . ?
C2 C3 C4 C5 3.5(11) . . . . ?
C2 C3 C4 C7 -178.1(8) . . . . ?
C3 C2 C8 N1 -165.1(7) . . . . ?
C3 C4 C5 C6 -2.1(11) . . . . ?
C4 C5 C6 C1 -2.7(11) . . . . ?
C4 C5 C6 C9 177.6(7) . . . . ?
C5 C6 C9 N2 -172.1(7) . . . . ?
C6 C1 C2 C3 -4.5(10) . . . . ?
C6 C1 C2 C8 177.5(7) . . . . ?
C7 C4 C5 C6 179.5(8) . . . . ?
C8 N1 C28 C29 -104.6(7) . . . . ?
C8 C2 C3 C4 178.1(7) . . . . ?
C9 N2 C34 C35 -101.3(7) . . . . ?
C10 C11 C12 C13 -1.9(12) . . . . ?
C10 C11 C17 N3 8.2(12) . . . . ?
C10 C15 C18 N4 12.4(13) . . . . ?
C11 C10 C15 C14 -3.7(10) . . . . ?
C11 C10 C15 C18 179.0(7) . . . . ?
C11 C12 C13 C14 -0.1(12) . . . . ?
C11 C12 C13 C16 179.5(8) . . . . ?
C12 C11 C17 N3 -169.4(8) . . . . ?
C12 C13 C14 C15 0.2(12) . . . . ?
C13 C14 C15 C10 1.8(11) . . . . ?
C13 C14 C15 C18 179.4(7) . . . . ?
C14 C15 C18 N4 -165.1(8) . . . . ?
C15 C10 C11 C12 3.7(10) . . . . ?
C15 C10 C11 C17 -173.8(7) . . . . ?
C16 C13 C14 C15 -179.5(8) . . . . ?
C17 N3 C30 C31 -98.9(9) . . . . ?
C17 C11 C12 C13 175.8(7) . . . . ?
C18 N4 C36 C37 -108.1(8) . . . . ?
C19 C20 C21 C22 -3.7(11) . . . . ?
C19 C20 C26 N5 7.9(14) . . . . ?
C19 C24 C27 N6 8.1(12) . . . . ?
C20 C19 C24 C23 0.4(10) . . . . ?
C20 C19 C24 C27 -175.1(7) . . . . ?
C20 C21 C22 C23 1.7(11) . . . . ?
C20 C21 C22 C25 178.3(8) . . . . ?
C21 C20 C26 N5 -168.2(9) . . . . ?
C21 C22 C23 C24 1.5(11) . . . . ?
C22 C23 C24 C19 -2.5(11) . . . . ?
C22 C23 C24 C27 173.7(7) . . . . ?
C23 C24 C27 N6 -167.7(7) . . . . ?
C24 C19 C20 C21 2.6(10) . . . . ?
C24 C19 C20 C26 -173.3(7) . . . . ?
C25 C22 C23 C24 -175.0(8) . . . . ?
C26 N5 C32 C33 160.5(8) . . . . ?
C26 C20 C21 C22 172.7(7) . . . . ?
C27 N6 C38 C39 164.6(7) . . . . ?
C28 N1 C8 C2 170.4(7) . . . . ?
C29 N7 C31 C30 139.4(8) . . . . ?
C29 N7 C33 C32 -171.8(7) . . . . ?
C30 N3 C17 C11 171.6(7) . . . . ?
C31 N7 C29 C28 -86.9(7) . . . . ?
C31 N7 C33 C32 66.9(8) . . . . ?
C32 N5 C26 C20 173.6(9) . . . . ?
C33 N7 C29 C28 151.9(6) . . . . ?
C33 N7 C31 C30 -99.4(8) . . . . ?
C34 N2 C9 C6 171.8(7) . . . . ?
C35 N8 C37 C36 -86.1(8) . . . . ?
C35 N8 C39 C38 65.5(8) . . . . ?
C36 N4 C18 C15 171.2(7) . . . . ?
C37 N8 C35 C34 138.0(7) . . . . ?
C37 N8 C39 C38 -172.2(6) . . . . ?
C38 N6 C27 C24 171.9(7) . . . . ?
C39 N8 C35 C34 -100.3(8) . . . . ?
C39 N8 C37 C36 151.7(7) . . . . ?

