# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_gdcf3abs
_database_code_depnum_ccdc_archive 'CCDC 1882453'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H18 F9 Gd O18 S3'
_chemical_formula_weight         766.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

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

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

_cell_length_a                   13.811(3)
_cell_length_b                   13.811(3)
_cell_length_c                   7.338(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1212.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1548
_cell_measurement_theta_min      2.7759
_cell_measurement_theta_max      31.5218

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.100
_exptl_crystal_F_000             746
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    3.133
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            3325
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.7759
_diffrn_reflns_theta_max         31.5218
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.8984
_diffrn_measured_fraction_theta_full 0.9863
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1343
_reflns_number_gt                1255
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0203P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1343
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0469
_refine_ls_wR_factor_gt          0.0447
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.333333 0.666667 0.250000 0.00907(7) Uani 1 6 d S T P . .
OW1 O 0.20962(12) 0.54639(11) 0.48481(18) 0.0145(3) Uani 1 1 d . . . . .
H11 H 0.144(2) 0.505(2) 0.470(4) 0.038(8) Uiso 1 1 d . . . . .
H12 H 0.230(3) 0.518(3) 0.562(4) 0.051(9) Uiso 1 1 d . . . . .
OW2 O 0.14425(17) 0.65281(18) 0.250000 0.0157(4) Uani 1 2 d S T P . .
H21 H 0.108(2) 0.647(2) 0.340(3) 0.038(8) Uiso 1 1 d . . . . .
S S 0.32008(5) 0.37909(5) 0.750000 0.01213(13) Uani 1 2 d S T P . .
O3 O 0.38387(11) 0.39887(12) 0.91681(17) 0.0175(3) Uani 1 1 d . . . . .
O4 O 0.24749(16) 0.42733(16) 0.750000 0.0167(4) Uani 1 2 d S T P . .
C C 0.2227(3) 0.2281(3) 0.750000 0.0216(6) Uiso 1 2 d S . P . .
F1 F 0.15825(12) 0.19888(11) 0.6029(2) 0.0367(3) Uani 1 1 d . . . . .
F2 F 0.27934(16) 0.17385(15) 0.750000 0.0282(4) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd OW1 2.4102(14) 3_565 ?
Gd OW1 2.4102(14) 12_566 ?
Gd OW1 2.4102(14) 10_556 ?
Gd OW1 2.4102(14) 2_665 ?
Gd OW1 2.4102(14) 11_666 ?
Gd OW1 2.4103(14) . ?
Gd OW2 2.521(2) . ?
Gd OW2 2.521(2) 3_565 ?
Gd OW2 2.521(2) 2_665 ?
S O3 1.4521(13) . ?
S O3 1.4521(13) 10_557 ?
S O4 1.4551(19) . ?
S C 1.831(3) . ?
C F1 1.327(2) . ?
C F2 1.327(3) . ?
C F1 1.327(2) 10_557 ?

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
OW1 Gd OW1 91.27(7) 3_565 12_566 ?
OW1 Gd OW1 139.07(3) 3_565 10_556 ?
OW1 Gd OW1 74.54(6) 12_566 10_556 ?
OW1 Gd OW1 74.54(6) 3_565 2_665 ?
OW1 Gd OW1 139.07(3) 12_566 2_665 ?
OW1 Gd OW1 139.07(3) 10_556 2_665 ?
OW1 Gd OW1 139.07(3) 3_565 11_666 ?
OW1 Gd OW1 74.54(6) 12_566 11_666 ?
OW1 Gd OW1 74.54(5) 10_556 11_666 ?
OW1 Gd OW1 91.27(7) 2_665 11_666 ?
OW1 Gd OW1 74.54(6) 3_565 . ?
OW1 Gd OW1 139.07(3) 12_566 . ?
OW1 Gd OW1 91.27(7) 10_556 . ?
OW1 Gd OW1 74.54(5) 2_665 . ?
OW1 Gd OW1 139.07(3) 11_666 . ?
OW1 Gd OW2 72.92(5) 3_565 . ?
OW1 Gd OW2 72.92(5) 12_566 . ?
OW1 Gd OW2 66.25(5) 10_556 . ?
OW1 Gd OW2 134.14(4) 2_665 . ?
OW1 Gd OW2 134.14(4) 11_666 . ?
OW1 Gd OW2 66.25(5) . . ?
OW1 Gd OW2 66.25(5) 3_565 3_565 ?
OW1 Gd OW2 66.25(5) 12_566 3_565 ?
OW1 Gd OW2 134.14(4) 10_556 3_565 ?
OW1 Gd OW2 72.92(5) 2_665 3_565 ?
OW1 Gd OW2 72.92(5) 11_666 3_565 ?
OW1 Gd OW2 134.14(4) . 3_565 ?
OW2 Gd OW2 120.0 . 3_565 ?
OW1 Gd OW2 134.14(4) 3_565 2_665 ?
OW1 Gd OW2 134.14(4) 12_566 2_665 ?
OW1 Gd OW2 72.92(5) 10_556 2_665 ?
OW1 Gd OW2 66.25(5) 2_665 2_665 ?
OW1 Gd OW2 66.25(5) 11_666 2_665 ?
OW1 Gd OW2 72.92(5) . 2_665 ?
OW2 Gd OW2 120.000(1) . 2_665 ?
OW2 Gd OW2 120.0 3_565 2_665 ?
O3 S O3 114.92(12) . 10_557 ?
O3 S O4 113.96(7) . . ?
O3 S O4 113.96(7) 10_557 . ?
O3 S C 104.20(8) . . ?
O3 S C 104.20(8) 10_557 . ?
O4 S C 103.85(13) . . ?
F1 C F2 108.87(17) . . ?
F1 C F1 108.9(2) . 10_557 ?
F2 C F1 108.87(17) . 10_557 ?
F1 C S 110.21(16) . . ?
F2 C S 109.8(2) . . ?
F1 C S 110.21(16) 10_557 . ?

_refine_diff_density_max         0.893
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_15cr5gda
_database_code_depnum_ccdc_archive 'CCDC 1882459'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H36 Cl3 Gd O13'
_chemical_formula_weight         627.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.161(2)
_cell_length_b                   17.174(3)
_cell_length_c                   15.221(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.74(2)
_cell_angle_gamma                90
_cell_volume                     2392.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9380
_cell_measurement_theta_min      2.9057
_cell_measurement_theta_max      28.8528

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_F_000             1260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.118
_exptl_absorpt_coefficient_mu    3.160
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            13705
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.906
_diffrn_reflns_theta_max         28.852
_diffrn_reflns_theta_full        25.493
_diffrn_measured_fraction_theta_max 0.8852
_diffrn_measured_fraction_theta_full 0.9707
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             5582
_reflns_number_gt                4912
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1010P)²+2.3707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5582
_refine_ls_number_parameters     293
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1458
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.64260(2) 0.32025(2) 0.78206(2) 0.01196(12) Uani 1 1 d D . . . .
Cl1 Cl 0.83576(16) 0.33018(8) 0.50821(9) 0.0226(3) Uani 1 1 d . . . . .
Cl2 Cl 0.30553(14) 0.24835(8) 0.56428(8) 0.0226(3) Uani 1 1 d . . . . .
Cl3 Cl 0.14787(15) 0.33835(9) 0.83544(9) 0.0230(3) Uani 1 1 d . . . . .
O1 O 0.6715(5) 0.5381(2) 0.6082(3) 0.0258(9) Uani 1 1 d . . . . .
O2 O 0.4461(4) 0.5528(2) 0.7306(3) 0.0241(8) Uani 1 1 d . . . . .
O3 O 0.6454(4) 0.6139(2) 0.8612(3) 0.0265(9) Uani 1 1 d . . . . .
O4 O 0.9095(5) 0.5392(2) 0.8675(3) 0.0261(9) Uani 1 1 d . . . . .
O5 O 0.9548(4) 0.5615(2) 0.6891(3) 0.0234(8) Uani 1 1 d . . . . .
C1 C 0.7940(7) 0.5629(3) 0.5608(4) 0.0216(11) Uani 1 1 d . . . . .
H1A H 0.800020 0.619311 0.561234 0.026 Uiso 1 1 calc R U . . .
H1B H 0.782852 0.545732 0.500143 0.026 Uiso 1 1 calc R U . . .
C2 C 0.9315(7) 0.5288(3) 0.6035(4) 0.0264(12) Uani 1 1 d . . . . .
H2A H 0.922077 0.472653 0.607734 0.032 Uiso 1 1 calc R U . . .
H2B H 1.014184 0.540271 0.568133 0.032 Uiso 1 1 calc R U . . .
C3 C 1.0572(6) 0.5197(3) 0.7441(4) 0.0239(12) Uani 1 1 d . . . . .
H3A H 1.154731 0.526056 0.723033 0.029 Uiso 1 1 calc R U . . .
H3B H 1.033352 0.464671 0.743116 0.029 Uiso 1 1 calc R U . . .
C4 C 1.0517(7) 0.5509(3) 0.8371(4) 0.0283(13) Uani 1 1 d . . . . .
H4A H 1.122940 0.524031 0.875250 0.034 Uiso 1 1 calc R U . . .
H4B H 1.075076 0.605979 0.837907 0.034 Uiso 1 1 calc R U . . .
C5 C 0.8718(7) 0.5900(4) 0.9361(4) 0.0299(13) Uani 1 1 d . . . . .
H5A H 0.905451 0.642257 0.923845 0.036 Uiso 1 1 calc R U . . .
H5B H 0.918883 0.572959 0.991172 0.036 Uiso 1 1 calc R U . . .
C6 C 0.7110(8) 0.5903(4) 0.9435(4) 0.0308(14) Uani 1 1 d . . . . .
H6A H 0.677294 0.538705 0.958640 0.037 Uiso 1 1 calc R U . . .
H6B H 0.684298 0.626159 0.989367 0.037 Uiso 1 1 calc R U . . .
C7 C 0.4897(7) 0.6226(3) 0.8630(4) 0.0274(12) Uani 1 1 d . . . . .
H7A H 0.465734 0.669851 0.894089 0.033 Uiso 1 1 calc R U . . .
H7B H 0.447688 0.578704 0.892920 0.033 Uiso 1 1 calc R U . . .
C8 C 0.4293(6) 0.6265(3) 0.7687(4) 0.0262(12) Uani 1 1 d . . . . .
H8A H 0.326739 0.640816 0.767133 0.031 Uiso 1 1 calc R U . . .
H8B H 0.481728 0.665355 0.736342 0.031 Uiso 1 1 calc R U . . .
C9 C 0.4195(6) 0.5516(3) 0.6373(4) 0.0258(12) Uani 1 1 d . . . . .
H9A H 0.332543 0.582055 0.622399 0.031 Uiso 1 1 calc R U . . .
H9B H 0.400396 0.498451 0.618633 0.031 Uiso 1 1 calc R U . . .
C10 C 0.5449(6) 0.5834(4) 0.5873(4) 0.0281(13) Uani 1 1 d . . . . .
H10A H 0.521117 0.581172 0.524578 0.034 Uiso 1 1 calc R U . . .
H10B H 0.562756 0.637354 0.603435 0.034 Uiso 1 1 calc R U . . .
OW1 O 0.6957(5) 0.1874(2) 0.7618(3) 0.0196(8) Uani 1 1 d D . . . .
HW11 H 0.744(6) 0.165(3) 0.719(3) 0.029 Uiso 1 1 d D U . . .
HW12 H 0.638(5) 0.149(2) 0.782(3) 0.029 Uiso 1 1 d D U . . .
OW2 O 0.5833(5) 0.3345(2) 0.6297(3) 0.0205(8) Uani 1 1 d D . . . .
HW21 H 0.648(5) 0.335(4) 0.587(3) 0.031 Uiso 1 1 d D U . . .
HW22 H 0.503(3) 0.312(3) 0.605(3) 0.031 Uiso 1 1 d D U . . .
OW3 O 0.7251(4) 0.4501(2) 0.7584(2) 0.0192(8) Uani 1 1 d D . . . .
HW31 H 0.792(5) 0.479(2) 0.790(3) 0.029 Uiso 1 1 d D U . . .
HW32 H 0.703(6) 0.479(2) 0.710(2) 0.029 Uiso 1 1 d D U . . .
OW4 O 0.8732(4) 0.3043(2) 0.7078(2) 0.0153(7) Uani 1 1 d D . . . .
HW41 H 0.964(2) 0.315(3) 0.730(3) 0.023 Uiso 1 1 d D U . . .
HW42 H 0.880(5) 0.305(3) 0.6491(5) 0.023 Uiso 1 1 d D U . . .
OW5 O 0.5632(4) 0.2704(2) 0.9188(2) 0.0190(7) Uani 1 1 d D . . . .
HW51 H 0.481(3) 0.244(3) 0.929(3) 0.028 Uiso 1 1 d D U . . .
HW52 H 0.624(4) 0.259(3) 0.965(2) 0.028 Uiso 1 1 d D U . . .
OW6 O 0.4569(4) 0.4130(2) 0.8167(3) 0.0217(8) Uani 1 1 d D . . . .
HW61 H 0.455(7) 0.458(2) 0.787(4) 0.033 Uiso 1 1 d D U . . .
HW62 H 0.3624(14) 0.3988(12) 0.818(6) 0.17(7) Uiso 1 1 d D . . . .
OW7 O 0.8321(4) 0.3402(2) 0.8919(2) 0.0198(8) Uani 1 1 d D . . . .
HW71 H 0.835(6) 0.320(3) 0.9463(16) 0.030 Uiso 1 1 d D U . . .
HW72 H 0.925(2) 0.337(4) 0.875(3) 0.030 Uiso 1 1 d D U . . .
OW8 O 0.4073(4) 0.2544(2) 0.7586(2) 0.0195(8) Uani 1 1 d D . . . .
HW81 H 0.329(4) 0.273(4) 0.786(3) 0.029 Uiso 1 1 d D U . . .
HW82 H 0.377(5) 0.251(4) 0.7017(10) 0.029 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd OW1 2.356(3) . ?
Gd OW2 2.369(4) . ?
Gd OW7 2.377(4) . ?
Gd OW3 2.387(4) . ?
Gd OW5 2.395(4) . ?
Gd OW6 2.408(4) . ?
Gd OW8 2.445(4) . ?
Gd OW4 2.458(4) . ?
O1 C10 1.419(7) . ?
O1 C1 1.428(7) . ?
O2 C8 1.404(6) . ?
O2 C9 1.430(7) . ?
O3 C6 1.422(7) . ?
O3 C7 1.436(7) . ?
O4 C5 1.416(7) . ?
O4 C4 1.418(8) . ?
O5 C3 1.421(6) . ?
O5 C2 1.426(7) . ?
C1 C2 1.508(8) . ?
C3 C4 1.516(9) . ?
C5 C6 1.483(9) . ?
C7 C8 1.515(9) . ?
C9 C10 1.510(8) . ?

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
OW1 Gd OW2 90.62(15) . . ?
OW1 Gd OW7 94.80(15) . . ?
OW2 Gd OW7 143.07(14) . . ?
OW1 Gd OW3 144.70(15) . . ?
OW2 Gd OW3 79.37(13) . . ?
OW7 Gd OW3 75.25(13) . . ?
OW1 Gd OW5 80.82(14) . . ?
OW2 Gd OW5 145.32(13) . . ?
OW7 Gd OW5 71.48(13) . . ?
OW3 Gd OW5 125.20(13) . . ?
OW1 Gd OW6 145.26(14) . . ?
OW2 Gd OW6 90.86(14) . . ?
OW7 Gd OW6 104.48(14) . . ?
OW3 Gd OW6 69.33(13) . . ?
OW5 Gd OW6 78.41(13) . . ?
OW1 Gd OW8 73.67(14) . . ?
OW2 Gd OW8 75.26(13) . . ?
OW7 Gd OW8 141.12(13) . . ?
OW3 Gd OW8 133.88(13) . . ?
OW5 Gd OW8 70.07(12) . . ?
OW6 Gd OW8 73.20(13) . . ?
OW1 Gd OW4 69.19(14) . . ?
OW2 Gd OW4 73.94(13) . . ?
OW7 Gd OW4 74.03(13) . . ?
OW3 Gd OW4 75.51(13) . . ?
OW5 Gd OW4 131.51(12) . . ?
OW6 Gd OW4 143.74(13) . . ?
OW8 Gd OW4 130.71(12) . . ?
C10 O1 C1 112.2(4) . . ?
C8 O2 C9 113.9(4) . . ?
C6 O3 C7 113.0(5) . . ?
C5 O4 C4 114.5(4) . . ?
C3 O5 C2 113.9(4) . . ?
O1 C1 C2 109.1(4) . . ?
O5 C2 C1 109.0(5) . . ?
O5 C3 C4 108.7(5) . . ?
O4 C4 C3 109.1(5) . . ?
O4 C5 C6 109.7(5) . . ?
O3 C6 C5 108.2(5) . . ?
O3 C7 C8 107.8(5) . . ?
O2 C8 C7 108.0(4) . . ?
O2 C9 C10 113.4(5) . . ?
O1 C10 C9 108.8(5) . . ?

_refine_diff_density_max         3.654
_refine_diff_density_min         -2.257
_refine_diff_density_rms         0.256

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

data_gddotaa
_database_code_depnum_ccdc_archive 'CCDC 1882455'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H34 Gd N4 Na O13'
_chemical_formula_weight         670.71

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.632(2)
_cell_length_b                   9.152(2)
_cell_length_c                   15.614(3)
_cell_angle_alpha                83.01(2)
_cell_angle_beta                 85.17(2)
_cell_angle_gamma                81.32(2)
_cell_volume                     1207.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16390
_cell_measurement_theta_min      3.1490
_cell_measurement_theta_max      36.8960

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_F_000             674
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.098
_exptl_absorpt_coefficient_mu    2.836
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.8b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19544
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.807
_diffrn_reflns_theta_max         36.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10253
_reflns_number_gt                9658
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10253
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1241
_refine_ls_wR_factor_gt          0.1202
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.90763(2) 0.74911(2) 0.69308(2) 0.00822(4) Uani 1 1 d . . . . .
O1 O 0.9918(2) 0.9845(2) 0.69039(13) 0.0126(3) Uani 1 1 d . . . . .
O2 O 1.1142(3) 1.1317(2) 0.75601(14) 0.0171(4) Uani 1 1 d . . . . .
C2 C 1.0296(3) 1.0315(3) 0.75770(17) 0.0117(4) Uani 1 1 d . . . . .
C1 C 0.9758(3) 0.9602(3) 0.84637(17) 0.0134(4) Uani 1 1 d . . . . .
H1A H 1.066159 0.901860 0.872941 0.016 Uiso 1 1 calc R U . . .
H1B H 0.935249 1.038377 0.882456 0.016 Uiso 1 1 calc R U . . .
N1 N 0.8546(3) 0.8639(2) 0.84479(14) 0.0108(3) Uani 1 1 d . . . . .
C9 C 0.6947(3) 0.9523(3) 0.85259(17) 0.0138(4) Uani 1 1 d . . . . .
H9A H 0.692628 1.019809 0.896124 0.017 Uiso 1 1 calc R U . . .
H9B H 0.618659 0.885302 0.871875 0.017 Uiso 1 1 calc R U . . .
C10 C 0.6474(3) 1.0414(3) 0.76784(18) 0.0138(4) Uani 1 1 d . . . . .
H10A H 0.542843 1.095943 0.776403 0.017 Uiso 1 1 calc R U . . .
H10B H 0.719231 1.113160 0.750391 0.017 Uiso 1 1 calc R U . . .
N4 N 0.6487(3) 0.9445(3) 0.69794(14) 0.0109(3) Uani 1 1 d . . . . .
C3 C 0.6454(3) 1.0395(3) 0.61373(16) 0.0118(4) Uani 1 1 d . . . . .
H3A H 0.699091 1.124027 0.617726 0.014 Uiso 1 1 calc R U . . .
H3B H 0.537130 1.077463 0.602390 0.014 Uiso 1 1 calc R U . . .
C4 C 0.7218(3) 0.9584(3) 0.53827(17) 0.0125(4) Uani 1 1 d . . . . .
O3 O 0.6955(2) 1.0174(2) 0.46330(13) 0.0138(3) Uani 1 1 d . . . . .
O4 O 0.8134(2) 0.8379(2) 0.55511(12) 0.0124(3) Uani 1 1 d . . . . .
C11 C 0.5072(3) 0.8659(3) 0.71226(17) 0.0129(4) Uani 1 1 d . . . . .
H11A H 0.414811 0.936471 0.698285 0.015 Uiso 1 1 calc R U . . .
H11B H 0.494616 0.828772 0.772961 0.015 Uiso 1 1 calc R U . . .
C12 C 0.5176(3) 0.7367(3) 0.65820(17) 0.0129(4) Uani 1 1 d . . . . .
H12A H 0.422140 0.691612 0.669169 0.016 Uiso 1 1 calc R U . . .
H12B H 0.526400 0.773768 0.597340 0.016 Uiso 1 1 calc R U . . .
N3 N 0.6544(3) 0.6228(2) 0.67843(14) 0.0109(3) Uani 1 1 d . . . . .
C5 C 0.6958(3) 0.5300(3) 0.60568(17) 0.0131(4) Uani 1 1 d . . . . .
H5A H 0.680736 0.592704 0.551468 0.016 Uiso 1 1 calc R U . . .
H5B H 0.625061 0.456086 0.609906 0.016 Uiso 1 1 calc R U . . .
C6 C 0.8645(3) 0.4513(3) 0.60483(16) 0.0109(4) Uani 1 1 d . . . . .
O5 O 0.9642(2) 0.5170(2) 0.63516(13) 0.0121(3) Uani 1 1 d . . . . .
O6 O 1.1028(3) 0.6684(2) 0.42711(14) 0.0153(4) Uani 1 1 d . . . . .
C13 C 0.6146(3) 0.5251(3) 0.75831(18) 0.0132(4) Uani 1 1 d . . . . .
H13A H 0.551022 0.454016 0.743740 0.016 Uiso 1 1 calc R U . . .
H13B H 0.552152 0.585549 0.799118 0.016 Uiso 1 1 calc R U . . .
C14 C 0.7585(3) 0.4408(3) 0.80150(17) 0.0130(4) Uani 1 1 d . . . . .
H14A H 0.725095 0.381597 0.853679 0.016 Uiso 1 1 calc R U . . .
H14B H 0.816739 0.373668 0.762820 0.016 Uiso 1 1 calc R U . . .
N2 N 0.8627(3) 0.5439(2) 0.82387(14) 0.0104(3) Uani 1 1 d . . . . .
C7 C 1.0201(3) 0.4599(3) 0.84178(18) 0.0137(4) Uani 1 1 d . . . . .
H7A H 1.046721 0.383885 0.802662 0.016 Uiso 1 1 calc R U . . .
H7B H 1.016641 0.410618 0.900403 0.016 Uiso 1 1 calc R U . . .
C8 C 1.1470(3) 0.5615(3) 0.83089(17) 0.0126(4) Uani 1 1 d . . . . .
O7 O 1.1313(2) 0.6715(2) 0.77359(13) 0.0143(3) Uani 1 1 d . . . . .
O8 O 1.2601(3) 0.5288(3) 0.87885(14) 0.0169(4) Uani 1 1 d . . . . .
C15 C 0.8678(3) 0.7439(3) 0.91926(16) 0.0115(4) Uani 1 1 d . . . . .
H15A H 0.817500 0.783539 0.971134 0.014 Uiso 1 1 calc R U . . .
H15B H 0.977831 0.711401 0.928930 0.014 Uiso 1 1 calc R U . . .
C16 C 0.7920(3) 0.6119(3) 0.90264(18) 0.0150(4) Uani 1 1 d . . . . .
H16A H 0.802571 0.537163 0.952301 0.018 Uiso 1 1 calc R U . . .
H16B H 0.680808 0.643714 0.896343 0.018 Uiso 1 1 calc R U . . .
OW1 O 1.1390(2) 0.7449(2) 0.59008(13) 0.0132(3) Uani 1 1 d . . . . .
HW11 H 1.176(6) 0.831(5) 0.583(3) 0.020 Uiso 1 1 d . U . . .
HW12 H 1.125(6) 0.732(5) 0.539(3) 0.020 Uiso 1 1 d . U . . .
OW2 O 0.5251(3) 0.7184(3) 1.07817(18) 0.0231(5) Uani 1 1 d . . . . .
HW21 H 0.603(7) 0.639(7) 1.088(4) 0.035 Uiso 1 1 d . U . . .
HW22 H 0.567(7) 0.780(7) 1.076(4) 0.035 Uiso 1 1 d . U . . .
OW3 O 1.2928(3) 1.0715(3) 0.90154(18) 0.0240(5) Uani 1 1 d . . . . .
HW31 H 1.231(7) 1.111(6) 0.866(4) 0.036 Uiso 1 1 d . U . . .
HW32 H 1.302(7) 0.990(7) 0.912(4) 0.036 Uiso 1 1 d . U . . .
OW4 O 1.2734(3) 0.3738(3) 0.6173(2) 0.0289(6) Uani 1 1 d . . . . .
HW41 H 1.182(8) 0.434(7) 0.624(4) 0.043 Uiso 1 1 d . U . . .
HW42 H 1.313(8) 0.357(7) 0.664(4) 0.043 Uiso 1 1 d . U . . .
OW5 O 1.3691(4) 0.7690(4) 0.9298(2) 0.0343(6) Uani 1 1 d . . . . .
HW51 H 1.287(9) 0.741(8) 0.924(5) 0.051 Uiso 1 1 d . U . . .
HW52 H 1.414(8) 0.762(7) 0.971(5) 0.051 Uiso 1 1 d . U . . .
Na Na 0.87044(15) 0.82438(14) 0.39993(8) 0.0161(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O7 2.364(2) . ?
Gd O1 2.369(2) . ?
Gd O4 2.373(2) . ?
Gd O5 2.376(2) . ?
Gd OW1 2.455(2) . ?
Gd N4 2.645(2) . ?
Gd N2 2.646(2) . ?
Gd N3 2.661(2) . ?
Gd N1 2.684(2) . ?
O1 C2 1.268(3) . ?
O1 Na 2.492(2) 2_776 ?
O2 C2 1.252(3) . ?
O2 Na 2.415(3) 2_776 ?
C2 C1 1.524(4) . ?
C2 Na 2.781(3) 2_776 ?
C1 N1 1.469(4) . ?
N1 C9 1.494(4) . ?
N1 C15 1.498(3) . ?
C9 C10 1.520(4) . ?
C10 N4 1.486(4) . ?
N4 C3 1.485(3) . ?
N4 C11 1.496(4) . ?
C3 C4 1.519(4) . ?
C4 O3 1.252(3) . ?
C4 O4 1.269(3) . ?
C4 Na 2.742(3) . ?
O3 Na 2.398(3) . ?
O4 Na 2.446(2) . ?
C11 C12 1.522(4) . ?
C12 N3 1.480(4) . ?
N3 C5 1.488(4) . ?
N3 C13 1.491(4) . ?
C5 C6 1.524(4) . ?
C6 O6 1.243(3) 2_766 ?
C6 O5 1.273(3) . ?
O6 Na 2.318(3) . ?
C13 C14 1.522(4) . ?
C14 N2 1.487(3) . ?
N2 C7 1.488(3) . ?
N2 C16 1.489(4) . ?
C7 C8 1.527(4) . ?
C8 O8 1.258(3) . ?
C8 O7 1.261(4) . ?
C15 C16 1.516(4) . ?
OW4 Na 2.399(3) 2_766 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Gd O1 82.07(8) . . ?
O7 Gd O4 146.11(7) . . ?
O1 Gd O4 86.17(7) . . ?
O7 Gd O5 86.92(7) . . ?
O1 Gd O5 143.73(7) . . ?
O4 Gd O5 84.02(7) . . ?
O7 Gd OW1 72.77(7) . . ?
O1 Gd OW1 74.51(7) . . ?
O4 Gd OW1 73.48(7) . . ?
O5 Gd OW1 69.22(7) . . ?
O7 Gd N4 138.54(7) . . ?
O1 Gd N4 74.09(7) . . ?
O4 Gd N4 66.01(7) . . ?
O5 Gd N4 131.35(7) . . ?
OW1 Gd N4 129.58(7) . . ?
O7 Gd N2 66.70(7) . . ?
O1 Gd N2 130.52(7) . . ?
O4 Gd N2 139.88(7) . . ?
O5 Gd N2 74.03(7) . . ?
OW1 Gd N2 125.77(7) . . ?
N4 Gd N2 104.62(7) . . ?
O7 Gd N3 132.07(7) . . ?
O1 Gd N3 141.98(7) . . ?
O4 Gd N3 72.50(7) . . ?
O5 Gd N3 66.17(7) . . ?
OW1 Gd N3 125.62(7) . . ?
N4 Gd N3 68.59(7) . . ?
N2 Gd N3 68.01(7) . . ?
O7 Gd N1 71.67(7) . . ?
O1 Gd N1 66.26(7) . . ?
O4 Gd N1 131.05(7) . . ?
O5 Gd N1 141.18(7) . . ?
OW1 Gd N1 129.61(7) . . ?
N4 Gd N1 67.82(7) . . ?
N2 Gd N1 67.88(7) . . ?
N3 Gd N1 104.71(7) . . ?
C2 O1 Gd 122.43(17) . . ?
C2 O1 Na 89.28(16) . 2_776 ?
Gd O1 Na 144.40(9) . 2_776 ?
C2 O2 Na 93.21(17) . 2_776 ?
O2 C2 O1 123.6(2) . . ?
O2 C2 C1 117.1(2) . . ?
O1 C2 C1 119.3(2) . . ?
O2 C2 Na 60.09(15) . 2_776 ?
O1 C2 Na 63.61(14) . 2_776 ?
C1 C2 Na 176.84(18) . 2_776 ?
N1 C1 C2 114.4(2) . . ?
C1 N1 C9 110.3(2) . . ?
C1 N1 C15 110.0(2) . . ?
C9 N1 C15 108.1(2) . . ?
C1 N1 Gd 105.82(15) . . ?
C9 N1 Gd 111.41(15) . . ?
C15 N1 Gd 111.16(15) . . ?
N1 C9 C10 112.6(2) . . ?
N4 C10 C9 111.9(2) . . ?
C3 N4 C10 108.4(2) . . ?
C3 N4 C11 110.3(2) . . ?
C10 N4 C11 109.1(2) . . ?
C3 N4 Gd 107.57(15) . . ?
C10 N4 Gd 111.37(16) . . ?
C11 N4 Gd 110.16(16) . . ?
N4 C3 C4 113.5(2) . . ?
O3 C4 O4 124.0(2) . . ?
O3 C4 C3 118.0(2) . . ?
O4 C4 C3 117.9(2) . . ?
O3 C4 Na 60.91(15) . . ?
O4 C4 Na 63.11(14) . . ?
C3 C4 Na 176.70(19) . . ?
C4 O3 Na 91.94(17) . . ?
C4 O4 Gd 124.80(17) . . ?
C4 O4 Na 89.31(16) . . ?
Gd O4 Na 143.46(9) . . ?
N4 C11 C12 113.0(2) . . ?
N3 C12 C11 111.6(2) . . ?
C12 N3 C5 109.9(2) . . ?
C12 N3 C13 109.5(2) . . ?
C5 N3 C13 108.9(2) . . ?
C12 N3 Gd 110.90(16) . . ?
C5 N3 Gd 105.60(15) . . ?
C13 N3 Gd 111.91(15) . . ?
N3 C5 C6 112.9(2) . . ?
O6 C6 O5 124.4(2) 2_766 . ?
O6 C6 C5 119.0(2) 2_766 . ?
O5 C6 C5 116.5(2) . . ?
C6 O5 Gd 125.39(17) . . ?
C6 O6 Na 120.95(18) 2_766 . ?
N3 C13 C14 113.3(2) . . ?
N2 C14 C13 111.5(2) . . ?
C14 N2 C7 109.6(2) . . ?
C14 N2 C16 108.7(2) . . ?
C7 N2 C16 109.3(2) . . ?
C14 N2 Gd 111.16(15) . . ?
C7 N2 Gd 106.51(15) . . ?
C16 N2 Gd 111.54(16) . . ?
N2 C7 C8 111.8(2) . . ?
O8 C8 O7 124.9(3) . . ?
O8 C8 C7 117.8(3) . . ?
O7 C8 C7 117.3(2) . . ?
C8 O7 Gd 125.28(18) . . ?
N1 C15 C16 111.6(2) . . ?
N2 C16 C15 112.8(2) . . ?
O6 Na O3 139.68(9) . . ?
O6 Na OW4 94.48(10) . 2_766 ?
O3 Na OW4 108.85(10) . 2_766 ?
O6 Na O2 102.49(9) . 2_776 ?
O3 Na O2 111.38(9) . 2_776 ?
OW4 Na O2 85.80(10) 2_766 2_776 ?
O6 Na O4 90.15(8) . . ?
O3 Na O4 54.73(7) . . ?
OW4 Na O4 99.14(10) 2_766 . ?
O2 Na O4 166.08(9) 2_776 . ?
O6 Na O1 92.95(9) . 2_776 ?
O3 Na O1 89.96(8) . 2_776 ?
OW4 Na O1 139.55(11) 2_766 2_776 ?
O2 Na O1 53.79(7) 2_776 2_776 ?
O4 Na O1 120.56(9) . 2_776 ?
O6 Na C4 115.66(9) . . ?
O3 Na C4 27.15(7) . . ?
OW4 Na C4 105.90(10) 2_766 . ?
O2 Na C4 138.52(10) 2_776 . ?
O4 Na C4 27.58(8) . . ?
O1 Na C4 106.39(9) 2_776 . ?
O6 Na C2 97.77(9) . 2_776 ?
O3 Na C2 102.69(9) . 2_776 ?
OW4 Na C2 112.44(11) 2_766 2_776 ?
O2 Na C2 26.70(7) 2_776 2_776 ?
O4 Na C2 146.57(9) . 2_776 ?
O1 Na C2 27.11(7) 2_776 2_776 ?
C4 Na C2 126.16(9) . 2_776 ?

_refine_diff_density_max         1.926
_refine_diff_density_min         -3.321
_refine_diff_density_rms         0.259

####################################################################### 
# 
# 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_ludotafa
_database_code_depnum_ccdc_archive 'CCDC 1882454'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H33.20 Cl K2 Lu N4 O12.85'
_chemical_formula_weight         775.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   37.315(2)
_cell_length_b                   8.885(2)
_cell_length_c                   16.592(2)
_cell_angle_alpha                90
_cell_angle_beta                 111.12(2)
_cell_angle_gamma                90
_cell_volume                     5131.5(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7724
_cell_measurement_theta_min      2.0519
_cell_measurement_theta_max      28.7825

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_F_000             3088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.041
_exptl_absorpt_coefficient_mu    4.346
_shelx_estimated_absorpt_T_min   0.644
_shelx_estimated_absorpt_T_max   0.884
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_detector                 'CCD plate'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            16620
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.340
_diffrn_reflns_theta_max         28.783
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5965
_reflns_number_gt                5014
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0163P)²+37.0695P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5965
_refine_ls_number_parameters     376
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0641
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu Lu 0.14697(2) 0.30677(2) 0.61526(2) 0.00933(5) Uani 1 1 d . . . . .
Cl1 Cl 0.000000 0.49720(18) 0.250000 0.0214(3) Uani 1 2 d S T P . .
O1 O 0.19959(8) 0.1731(3) 0.69641(18) 0.0163(6) Uani 1 1 d . . . . .
O2 O 0.23023(9) 0.0464(4) 0.81836(19) 0.0215(7) Uani 1 1 d . . . . .
O3 O 0.16804(9) 0.4339(3) 0.74077(18) 0.0184(7) Uani 1 1 d . . . . .
O4 O 0.15961(11) 0.6356(4) 0.8134(2) 0.0374(10) Uani 1 1 d . . . . .
O5 O 0.14922(8) 0.5467(3) 0.56977(18) 0.0147(6) Uani 1 1 d . . . . .
O6 O 0.15114(9) 0.6670(3) 0.45267(19) 0.0176(7) Uani 1 1 d . . . . .
O7 O 0.18203(8) 0.2866(3) 0.52951(17) 0.0132(6) Uani 1 1 d . . . . .
O8 O 0.21393(9) 0.1321(4) 0.47367(19) 0.0190(7) Uani 1 1 d . . . . .
C1 C 0.20050(12) 0.1011(5) 0.7637(3) 0.0172(9) Uani 1 1 d . . . . .
C2 C 0.16257(12) 0.0835(5) 0.7775(3) 0.0183(9) Uani 1 1 d . . . . .
H2A H 0.162005 -0.013045 0.804290 0.022 Uiso 1 1 calc R U . . .
H2B H 0.160217 0.161870 0.815964 0.022 Uiso 1 1 calc R U . . .
C3 C 0.09294(12) 0.1200(5) 0.7063(3) 0.0160(9) Uani 1 1 d . . . . .
H3A H 0.091363 0.055803 0.752167 0.019 Uiso 1 1 calc R U . . .
H3B H 0.071822 0.094415 0.653571 0.019 Uiso 1 1 calc R U . . .
C4 C 0.08952(12) 0.2824(5) 0.7288(3) 0.0151(9) Uani 1 1 d . . . . .
H4A H 0.064892 0.297889 0.734902 0.018 Uiso 1 1 calc R U . . .
H4B H 0.109505 0.305367 0.783828 0.018 Uiso 1 1 calc R U . . .
C5 C 0.14740(14) 0.5382(5) 0.7578(3) 0.0218(10) Uani 1 1 d . . . . .
C6 C 0.10495(13) 0.5354(5) 0.7023(3) 0.0184(10) Uani 1 1 d . . . . .
H6A H 0.090018 0.559641 0.737840 0.022 Uiso 1 1 calc R U . . .
H6B H 0.099737 0.611659 0.657684 0.022 Uiso 1 1 calc R U . . .
C7 C 0.05599(12) 0.3969(5) 0.5877(3) 0.0176(9) Uani 1 1 d . . . . .
H7A H 0.038298 0.459721 0.603534 0.021 Uiso 1 1 calc R U . . .
H7B H 0.044774 0.297305 0.574107 0.021 Uiso 1 1 calc R U . . .
C8 C 0.06171(13) 0.4628(5) 0.5085(3) 0.0175(9) Uani 1 1 d . . . . .
H8A H 0.037261 0.464898 0.460668 0.021 Uiso 1 1 calc R U . . .
H8B H 0.070835 0.565592 0.520660 0.021 Uiso 1 1 calc R U . . .
C9 C 0.13764(12) 0.5720(5) 0.4877(3) 0.0134(8) Uani 1 1 d . . . . .
C10 C 0.10547(12) 0.4703(5) 0.4314(3) 0.0138(9) Uani 1 1 d . . . . .
H10A H 0.085000 0.531949 0.392860 0.017 Uiso 1 1 calc R U . . .
H10B H 0.115216 0.407055 0.396274 0.017 Uiso 1 1 calc R U . . .
C11 C 0.07075(12) 0.2388(5) 0.4329(3) 0.0159(9) Uani 1 1 d . . . . .
H11A H 0.054786 0.268970 0.374877 0.019 Uiso 1 1 calc R U . . .
H11B H 0.054347 0.192273 0.459805 0.019 Uiso 1 1 calc R U . . .
C12 C 0.10048(12) 0.1268(5) 0.4288(3) 0.0142(9) Uani 1 1 d . . . . .
H12A H 0.087637 0.037970 0.397662 0.017 Uiso 1 1 calc R U . . .
H12B H 0.115304 0.170702 0.397260 0.017 Uiso 1 1 calc R U . . .
C13 C 0.16316(12) 0.0277(5) 0.5095(3) 0.0166(9) Uani 1 1 d . . . . .
H13A H 0.157218 -0.036377 0.459020 0.020 Uiso 1 1 calc R U . . .
H13B H 0.177178 -0.032055 0.559972 0.020 Uiso 1 1 calc R U . . .
C14 C 0.18811(12) 0.1575(5) 0.5020(3) 0.0149(9) Uani 1 1 d . . . . .
C15 C 0.10840(13) -0.0357(5) 0.5510(3) 0.0188(10) Uani 1 1 d . . . . .
H15A H 0.109223 -0.130725 0.522909 0.023 Uiso 1 1 calc R U . . .
H15B H 0.081649 -0.009576 0.537874 0.023 Uiso 1 1 calc R U . . .
C16 C 0.12810(13) -0.0533(5) 0.6474(3) 0.0169(9) Uani 1 1 d . . . . .
H16A H 0.114244 -0.126643 0.668339 0.020 Uiso 1 1 calc R U . . .
H16B H 0.153936 -0.091093 0.659961 0.020 Uiso 1 1 calc R U . . .
N3 N 0.08972(10) 0.3736(4) 0.4835(2) 0.0122(7) Uani 1 1 d . . . . .
N1 N 0.13003(10) 0.0933(4) 0.6942(2) 0.0126(7) Uani 1 1 d . . . . .
N2 N 0.09293(10) 0.3868(4) 0.6616(2) 0.0122(7) Uani 1 1 d . . . . .
N4 N 0.12697(10) 0.0820(4) 0.5169(2) 0.0128(7) Uani 1 1 d . . . . .
OW1 O 0.03801(12) 0.7913(5) 0.6956(3) 0.0475(11) Uani 1 1 d D . . . .
HW1A H 0.0274(17) 0.710(5) 0.710(3) 0.071 Uiso 1 1 d D U . . .
HW1B H 0.0285(18) 0.792(7) 0.6375(5) 0.071 Uiso 1 1 d D U . . .
OW2 O 0.03549(11) 0.7798(4) 0.3734(3) 0.0353(10) Uani 1 1 d . . . . .
HW2A H 0.0250(19) 0.844(8) 0.337(4) 0.053 Uiso 1 1 d . U . . .
HW2B H 0.0268(19) 0.706(8) 0.346(4) 0.053 Uiso 1 1 d . U . . .
OW3 O 0.24076(11) 0.5771(5) 0.3659(3) 0.0309(10) Uani 0.85 1 d D . P . .
HW3A H 0.2184(8) 0.577(7) 0.321(2) 0.046 Uiso 0.85 1 d D U P . .
HW3B H 0.2570(11) 0.630(6) 0.348(3) 0.046 Uiso 0.85 1 d D U P . .
OW4 O 0.20874(9) 0.7300(4) 0.6745(2) 0.0254(8) Uani 1 1 d D . . . .
HW4A H 0.1871(6) 0.682(4) 0.642(3) 0.038 Uiso 1 1 d D U . . .
HW4B H 0.2275(8) 0.661(4) 0.684(3) 0.038 Uiso 1 1 d D U . . .
OW5 O 0.000000 -0.0057(6) 0.250000 0.0424(14) Uani 1 2 d S T P . .
OW6 O -0.0193(13) 0.171(6) 0.463(2) 0.0621(16) Uani 0.25 1 d D . P . .
HW6A H -0.030(4) 0.21(2) 0.500(7) 0.093 Uiso 0.25 1 d D U P . .
HW6B H -0.001(4) 0.108(16) 0.495(9) 0.093 Uiso 0.25 1 d D U P . .
K1 K 0.23456(3) 0.26019(14) 0.35101(7) 0.0192(2) Uani 0.85 1 d . . P . .
K2 K 0.22504(4) 0.5479(2) 0.50988(10) 0.0493(5) Uani 0.85 1 d . . P . .
K3 K 0.2265(2) 0.3654(10) 0.3598(5) 0.0302(16) Uiso 0.15 1 d . . P . .
K4 K 0.2330(5) 0.652(2) 0.4827(12) 0.105(5) Uiso 0.15 1 d . . P . .
Cl2 Cl -0.0151(2) 0.1415(10) 0.4840(3) 0.0621(16) Uani 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu O3 2.248(3) . ?
Lu O7 2.260(3) . ?
Lu O5 2.273(3) . ?
Lu O1 2.274(3) . ?
Lu N2 2.506(3) . ?
Lu N1 2.512(3) . ?
Lu N3 2.516(3) . ?
Lu N4 2.517(3) . ?
Lu K1 4.2925(12) 7_556 ?
Lu K2 4.4499(19) . ?
O1 C1 1.277(5) . ?
O1 K1 2.898(3) 7_556 ?
O1 K3 3.230(8) 7_556 ?
O2 C1 1.250(5) . ?
O2 K2 2.735(3) 4_546 ?
O2 K1 2.771(3) 6_556 ?
O2 K4 3.224(19) 4_546 ?
O3 C5 1.299(6) . ?
O3 K3 2.956(9) 6_566 ?
O4 C5 1.226(5) . ?
O4 K3 2.334(9) 6_566 ?
O4 K1 2.795(4) 6_566 ?
O5 C9 1.291(5) . ?
O5 K2 3.319(3) . ?
O6 C9 1.231(5) . ?
O6 K2 2.782(3) . ?
O6 K4 2.915(18) . ?
O7 C14 1.285(5) . ?
O7 K2 2.906(3) . ?
O7 K1 3.057(3) 7_556 ?
O8 C14 1.235(5) . ?
O8 K1 2.676(3) . ?
O8 K2 2.714(3) 7_556 ?
O8 K3 2.854(8) 7_556 ?
O8 K3 2.955(9) . ?
O8 K1 3.007(3) 7_556 ?
O8 K4 3.128(18) 7_556 ?
C1 C2 1.521(6) . ?
C2 N1 1.477(5) . ?
C3 N1 1.487(5) . ?
C3 C4 1.507(6) . ?
C4 N2 1.491(5) . ?
C5 C6 1.519(7) . ?
C5 K3 2.953(9) 6_566 ?
C6 N2 1.478(5) . ?
C7 N2 1.481(5) . ?
C7 C8 1.523(6) . ?
C8 N3 1.485(5) . ?
C9 C10 1.524(6) . ?
C9 K2 3.155(4) . ?
C10 N3 1.482(5) . ?
C11 N3 1.487(5) . ?
C11 C12 1.511(6) . ?
C12 N4 1.493(5) . ?
C13 N4 1.480(5) . ?
C13 C14 1.516(6) . ?
C14 K1 3.121(4) 7_556 ?
C14 K3 3.191(9) 7_556 ?
C15 N4 1.476(5) . ?
C15 C16 1.509(6) . ?
C16 N1 1.505(5) . ?
OW3 K3 1.947(10) . ?
OW3 K4 2.165(18) . ?
OW3 K2 2.669(4) . ?
OW3 K1 2.829(5) . ?
OW3 K4 3.359(18) 7_566 ?
OW4 K1 2.735(4) 6_566 ?
OW4 K3 3.023(9) 6_566 ?
OW4 K2 3.412(4) . ?
K1 K3 1.008(8) . ?
K1 K2 3.547(2) 7_556 ?
K1 K2 3.779(2) . ?
K2 K4 1.115(18) . ?
K2 K3 2.989(8) . ?
K2 K4 3.073(19) 7_566 ?
K3 K4 3.217(19) . ?
K4 K4 2.11(4) 7_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Lu O7 122.31(10) . . ?
O3 Lu O5 78.10(10) . . ?
O7 Lu O5 76.48(10) . . ?
O3 Lu O1 76.99(11) . . ?
O7 Lu O1 76.07(10) . . ?
O5 Lu O1 123.98(10) . . ?
O3 Lu N2 67.96(11) . . ?
O7 Lu N2 158.08(11) . . ?
O5 Lu N2 88.03(11) . . ?
O1 Lu N2 125.82(10) . . ?
O3 Lu N1 88.06(11) . . ?
O7 Lu N1 125.44(11) . . ?
O5 Lu N1 158.08(11) . . ?
O1 Lu N1 67.84(10) . . ?
N2 Lu N1 70.91(11) . . ?
O3 Lu N3 126.18(11) . . ?
O7 Lu N3 88.55(10) . . ?
O5 Lu N3 67.13(11) . . ?
O1 Lu N3 156.82(11) . . ?
N2 Lu N3 70.98(11) . . ?
N1 Lu N3 109.69(11) . . ?
O3 Lu N4 157.36(11) . . ?
O7 Lu N4 68.44(10) . . ?
O5 Lu N4 124.52(11) . . ?
O1 Lu N4 87.74(11) . . ?
N2 Lu N4 109.92(11) . . ?
N1 Lu N4 70.57(11) . . ?
N3 Lu N4 70.33(11) . . ?
O3 Lu K1 87.07(8) . 7_556 ?
O7 Lu K1 43.00(7) . 7_556 ?
O5 Lu K1 90.79(8) . 7_556 ?
O1 Lu K1 38.89(7) . 7_556 ?
N2 Lu K1 154.70(8) . 7_556 ?
N1 Lu K1 105.56(8) . 7_556 ?
N3 Lu K1 131.16(8) . 7_556 ?
N4 Lu K1 91.46(8) . 7_556 ?
O3 Lu K2 93.56(8) . . ?
O7 Lu K2 35.07(8) . . ?
O5 Lu K2 46.40(8) . . ?
O1 Lu K2 86.34(7) . . ?
N2 Lu K2 134.18(8) . . ?
N1 Lu K2 153.09(8) . . ?
N3 Lu K2 90.92(8) . . ?
N4 Lu K2 102.14(8) . . ?
K1 Lu K2 47.84(3) 7_556 . ?
C1 O1 Lu 121.6(3) . . ?
C1 O1 K1 125.6(3) . 7_556 ?
Lu O1 K1 111.59(11) . 7_556 ?
C1 O1 K3 116.3(3) . 7_556 ?
Lu O1 K3 121.93(17) . 7_556 ?
K1 O1 K3 17.90(15) 7_556 7_556 ?
C1 O2 K2 143.4(3) . 4_546 ?
C1 O2 K1 119.9(3) . 6_556 ?
K2 O2 K1 80.22(9) 4_546 6_556 ?
C1 O2 K4 124.6(4) . 4_546 ?
K2 O2 K4 19.4(3) 4_546 4_546 ?
K1 O2 K4 96.5(3) 6_556 4_546 ?
C5 O3 Lu 121.5(3) . . ?
C5 O3 K3 77.2(3) . 6_566 ?
Lu O3 K3 148.19(19) . 6_566 ?
C5 O4 K3 108.0(4) . 6_566 ?
C5 O4 K1 118.2(3) . 6_566 ?
K3 O4 K1 20.2(2) 6_566 6_566 ?
C9 O5 Lu 118.4(3) . . ?
C9 O5 K2 71.4(2) . . ?
Lu O5 K2 103.88(11) . . ?
C9 O6 K2 95.8(2) . . ?
C9 O6 K4 118.0(4) . . ?
K2 O6 K4 22.4(4) . . ?
C14 O7 Lu 120.7(3) . . ?
C14 O7 K2 119.9(2) . . ?
Lu O7 K2 118.39(11) . . ?
C14 O7 K1 80.8(2) . 7_556 ?
Lu O7 K1 106.71(10) . 7_556 ?
K2 O7 K1 72.96(7) . 7_556 ?
C14 O8 K1 133.5(3) . . ?
C14 O8 K2 144.1(3) . 7_556 ?
K1 O8 K2 82.31(9) . 7_556 ?
C14 O8 K3 94.1(3) . 7_556 ?
K1 O8 K3 113.35(19) . 7_556 ?
K2 O8 K3 64.86(18) 7_556 7_556 ?
C14 O8 K3 116.1(3) . . ?
K1 O8 K3 19.84(16) . . ?
K2 O8 K3 99.00(18) 7_556 . ?
K3 O8 K3 111.5(2) 7_556 . ?
C14 O8 K1 83.6(2) . 7_556 ?
K1 O8 K1 109.98(11) . 7_556 ?
K2 O8 K1 82.51(9) 7_556 7_556 ?
K3 O8 K1 19.58(17) 7_556 7_556 ?
K3 O8 K1 101.64(18) . 7_556 ?
C14 O8 K4 125.1(4) . 7_556 ?
K1 O8 K4 100.8(3) . 7_556 ?
K2 O8 K4 20.5(3) 7_556 7_556 ?
K3 O8 K4 64.9(4) 7_556 7_556 ?
K3 O8 K4 118.7(4) . 7_556 ?
K1 O8 K4 84.4(3) 7_556 7_556 ?
O2 C1 O1 124.5(4) . . ?
O2 C1 C2 118.8(4) . . ?
O1 C1 C2 116.7(4) . . ?
N1 C2 C1 110.5(3) . . ?
N1 C3 C4 110.6(3) . . ?
N2 C4 C3 111.9(3) . . ?
O4 C5 O3 125.3(5) . . ?
O4 C5 C6 119.4(4) . . ?
O3 C5 C6 115.3(4) . . ?
O4 C5 K3 48.7(3) . 6_566 ?
O3 C5 K3 77.4(3) . 6_566 ?
C6 C5 K3 164.1(4) . 6_566 ?
N2 C6 C5 111.7(4) . . ?
N2 C7 C8 111.0(3) . . ?
N3 C8 C7 111.6(3) . . ?
O6 C9 O5 125.4(4) . . ?
O6 C9 C10 118.9(4) . . ?
O5 C9 C10 115.7(4) . . ?
O6 C9 K2 61.3(2) . . ?
O5 C9 K2 85.8(2) . . ?
C10 C9 K2 125.7(3) . . ?
N3 C10 C9 112.1(3) . . ?
N3 C11 C12 110.4(3) . . ?
N4 C12 C11 111.7(3) . . ?
N4 C13 C14 111.4(3) . . ?
O8 C14 O7 124.1(4) . . ?
O8 C14 C13 118.6(4) . . ?
O7 C14 C13 117.2(4) . . ?
O8 C14 K1 73.2(2) . 7_556 ?
O7 C14 K1 75.2(2) . 7_556 ?
C13 C14 K1 122.4(3) . 7_556 ?
O8 C14 K3 63.2(3) . 7_556 ?
O7 C14 K3 93.4(3) . 7_556 ?
C13 C14 K3 112.1(3) . 7_556 ?
K1 C14 K3 18.34(15) 7_556 7_556 ?
N4 C15 C16 111.3(4) . . ?
N1 C16 C15 111.8(3) . . ?
C10 N3 C8 108.7(3) . . ?
C10 N3 C11 110.2(3) . . ?
C8 N3 C11 110.3(3) . . ?
C10 N3 Lu 104.6(2) . . ?
C8 N3 Lu 110.2(2) . . ?
C11 N3 Lu 112.5(2) . . ?
C2 N1 C3 112.0(3) . . ?
C2 N1 C16 107.6(3) . . ?
C3 N1 C16 109.5(3) . . ?
C2 N1 Lu 104.8(2) . . ?
C3 N1 Lu 111.8(2) . . ?
C16 N1 Lu 111.0(2) . . ?
C6 N2 C7 111.3(3) . . ?
C6 N2 C4 107.9(3) . . ?
C7 N2 C4 110.6(3) . . ?
C6 N2 Lu 104.4(2) . . ?
C7 N2 Lu 112.1(2) . . ?
C4 N2 Lu 110.4(2) . . ?
C15 N4 C13 111.7(3) . . ?
C15 N4 C12 109.1(3) . . ?
C13 N4 C12 107.9(3) . . ?
C15 N4 Lu 112.6(2) . . ?
C13 N4 Lu 104.2(2) . . ?
C12 N4 Lu 111.1(2) . . ?
K3 OW3 K4 102.8(6) . . ?
K3 OW3 K2 79.0(3) . . ?
K4 OW3 K2 23.9(5) . . ?
K3 OW3 K1 11.9(2) . . ?
K4 OW3 K1 110.6(5) . . ?
K2 OW3 K1 86.79(12) . . ?
K3 OW3 K4 137.0(4) . 7_566 ?
K4 OW3 K4 37.6(8) . 7_566 ?
K2 OW3 K4 60.0(3) . 7_566 ?
K1 OW3 K4 140.5(3) . 7_566 ?
K1 OW4 K3 19.34(16) 6_566 6_566 ?
K1 OW4 K2 140.96(13) 6_566 . ?
K3 OW4 K2 130.1(2) 6_566 . ?
K3 K1 O8 95.9(4) . . ?
K3 K1 OW4 96.7(4) . 6_565 ?
O8 K1 OW4 137.84(11) . 6_565 ?
K3 K1 O2 160.2(5) . 6 ?
O8 K1 O2 73.62(10) . 6 ?
OW4 K1 O2 81.30(10) 6_565 6 ?
K3 K1 O4 53.1(5) . 6_565 ?
O8 K1 O4 76.82(10) . 6_565 ?
OW4 K1 O4 79.17(11) 6_565 6_565 ?
O2 K1 O4 107.38(11) 6 6_565 ?
K3 K1 OW3 23.5(4) . . ?
O8 K1 OW3 113.19(11) . . ?
OW4 K1 OW3 92.75(11) 6_565 . ?
O2 K1 OW3 173.17(12) 6 . ?
O4 K1 OW3 74.55(12) 6_565 . ?
K3 K1 O1 100.0(4) . 7_556 ?
O8 K1 O1 142.92(10) . 7_556 ?
OW4 K1 O1 73.07(10) 6_565 7_556 ?
O2 K1 O1 98.24(10) 6 7_556 ?
O4 K1 O1 138.56(10) 6_565 7_556 ?
OW3 K1 O1 76.68(11) . 7_556 ?
K3 K1 O8 71.6(4) . 7_556 ?
O8 K1 O8 70.02(11) . 7_556 ?
OW4 K1 O8 151.82(10) 6_565 7_556 ?
O2 K1 O8 118.30(10) 6 7_556 ?
O4 K1 O8 110.49(11) 6_565 7_556 ?
OW3 K1 O8 66.10(10) . 7_556 ?
O1 K1 O8 83.61(9) 7_556 7_556 ?
K3 K1 O7 108.5(5) . 7_556 ?
O8 K1 O7 87.34(9) . 7_556 ?
OW4 K1 O7 125.61(9) 6_565 7_556 ?
O2 K1 O7 88.12(9) 6 7_556 ?
O4 K1 O7 153.27(10) 6_565 7_556 ?
OW3 K1 O7 92.67(10) . 7_556 ?
O1 K1 O7 55.89(8) 7_556 7_556 ?
O8 K1 O7 43.06(8) 7_556 7_556 ?
K3 K1 C14 84.7(5) . 7_556 ?
O8 K1 C14 86.76(11) . 7_556 ?
OW4 K1 C14 134.37(11) 6_565 7_556 ?
O2 K1 C14 110.83(11) 6 7_556 ?
O4 K1 C14 131.77(12) 6_565 7_556 ?
OW3 K1 C14 71.03(11) . 7_556 ?
O1 K1 C14 61.88(10) 7_556 7_556 ?
O8 K1 C14 23.16(9) 7_556 7_556 ?
O7 K1 C14 23.98(9) 7_556 7_556 ?
K3 K1 K2 134.4(4) . 7_556 ?
O8 K1 K2 49.31(7) . 7_556 ?
OW4 K1 K2 128.65(8) 6_565 7_556 ?
O2 K1 K2 49.45(7) 6 7_556 ?
O4 K1 K2 123.88(8) 6_565 7_556 ?
OW3 K1 K2 135.14(10) . 7_556 ?
O1 K1 K2 97.55(7) 7_556 7_556 ?
O8 K1 K2 69.05(7) 7_556 7_556 ?
O7 K1 K2 51.57(6) 7_556 7_556 ?
C14 K1 K2 67.40(9) 7_556 7_556 ?
K3 K1 K2 33.3(4) . . ?
O8 K1 K2 68.41(8) . . ?
OW4 K1 K2 129.79(8) 6_565 . ?
O2 K1 K2 141.98(8) 6 . ?
O4 K1 K2 66.04(9) 6_565 . ?
OW3 K1 K2 44.85(9) . . ?
O1 K1 K2 110.67(8) 7_556 . ?
O8 K1 K2 45.41(6) 7_556 . ?
O7 K1 K2 88.24(6) 7_556 . ?
C14 K1 K2 65.74(8) 7_556 . ?
K2 K1 K2 101.11(5) 7_556 . ?
K4 K2 OW3 51.8(9) . . ?
K4 K2 O8 101.2(9) . 7_556 ?
OW3 K2 O8 72.57(11) . 7_556 ?
K4 K2 O2 105.9(9) . 4_556 ?
OW3 K2 O2 133.19(12) . 4_556 ?
O8 K2 O2 73.59(10) 7_556 4_556 ?
K4 K2 O6 85.5(9) . . ?
OW3 K2 O6 99.67(12) . . ?
O8 K2 O6 161.97(12) 7_556 . ?
O2 K2 O6 121.00(10) 4_556 . ?
K4 K2 O7 161.1(9) . . ?
OW3 K2 O7 119.10(13) . . ?
O8 K2 O7 89.74(10) 7_556 . ?
O2 K2 O7 91.93(10) 4_556 . ?
O6 K2 O7 79.78(9) . . ?
K4 K2 K3 91.5(9) . . ?
OW3 K2 K3 39.75(18) . . ?
O8 K2 K3 59.83(17) 7_556 . ?
O2 K2 K3 132.69(18) 4_556 . ?
O6 K2 K3 103.65(17) . . ?
O7 K2 K3 80.63(17) . . ?
K4 K2 K4 24.5(12) . 7_566 ?
OW3 K2 K4 71.2(4) . 7_566 ?
O8 K2 K4 96.3(3) 7_556 7_566 ?
O2 K2 K4 81.5(3) 4_556 7_566 ?
O6 K2 K4 96.4(3) . 7_566 ?
O7 K2 K4 169.4(3) . 7_566 ?
K3 K2 K4 110.0(4) . 7_566 ?
K4 K2 C9 108.1(9) . . ?
OW3 K2 C9 116.12(13) . . ?
O8 K2 C9 147.81(13) 7_556 . ?
O2 K2 C9 109.81(11) 4_556 . ?
O6 K2 C9 22.84(9) . . ?
O7 K2 C9 58.53(10) . . ?
K3 K2 C9 105.59(17) . . ?
K4 K2 C9 115.9(3) 7_566 . ?
K4 K2 O5 120.2(9) . . ?
OW3 K2 O5 138.93(11) . . ?
O8 K2 O5 137.96(11) 7_556 . ?
O2 K2 O5 87.37(9) 4_556 . ?
O6 K2 O5 41.95(8) . . ?
O7 K2 O5 53.08(8) . . ?
K3 K2 O5 121.45(17) . . ?
K4 K2 O5 117.9(3) 7_566 . ?
C9 K2 O5 22.82(9) . . ?
K4 K2 OW4 94.6(9) . . ?
OW3 K2 OW4 146.09(14) . . ?
O8 K2 OW4 125.72(10) 7_556 . ?
O2 K2 OW4 52.13(9) 4_556 . ?
O6 K2 OW4 69.64(9) . . ?
O7 K2 OW4 91.39(9) . . ?
K3 K2 OW4 170.51(17) . . ?
K4 K2 OW4 78.0(3) 7_566 . ?
C9 K2 OW4 65.56(10) . . ?
O5 K2 OW4 49.08(8) . . ?
K4 K2 K1 142.3(9) . 7_556 ?
OW3 K2 K1 118.59(11) . 7_556 ?
O8 K2 K1 48.37(7) 7_556 7_556 ?
O2 K2 K1 50.33(8) 4_556 7_556 ?
O6 K2 K1 130.70(9) . 7_556 ?
O7 K2 K1 55.47(7) . 7_556 ?
K3 K2 K1 89.58(16) . 7_556 ?
K4 K2 K1 123.5(3) 7_566 7_556 ?
C9 K2 K1 107.90(10) . 7_556 ?
O5 K2 K1 90.63(7) . 7_556 ?
OW4 K2 K1 90.09(7) . 7_556 ?
K1 K3 OW3 144.5(7) . . ?
K1 K3 O4 106.6(6) . 6_565 ?
OW3 K3 O4 105.1(4) . 6_565 ?
K1 K3 O8 88.8(5) . 7_556 ?
OW3 K3 O8 80.8(3) . 7_556 ?
O4 K3 O8 133.4(3) 6_565 7_556 ?
K1 K3 C5 118.3(6) . 6_565 ?
OW3 K3 C5 87.0(3) . 6_565 ?
O4 K3 C5 23.27(14) 6_565 6_565 ?
O8 K3 C5 145.2(3) 7_556 6_565 ?
K1 K3 O8 64.2(4) . . ?
OW3 K3 O8 138.4(4) . . ?
O4 K3 O8 79.0(2) 6_565 . ?
O8 K3 O8 68.5(2) 7_556 . ?
C5 K3 O8 102.3(3) 6_565 . ?
K1 K3 O3 130.5(6) . 6_565 ?
OW3 K3 O3 64.8(3) . 6_565 ?
O4 K3 O3 48.46(18) 6_565 6_565 ?
O8 K3 O3 140.5(3) 7_556 6_565 ?
C5 K3 O3 25.41(13) 6_565 6_565 ?
O8 K3 O3 126.9(3) . 6_565 ?
K1 K3 K2 136.0(6) . . ?
OW3 K3 K2 61.3(3) . . ?
O4 K3 K2 86.4(3) 6_565 . ?
O8 K3 K2 55.31(16) 7_556 . ?
C5 K3 K2 90.3(2) 6_565 . ?
O8 K3 K2 78.0(2) . . ?
O3 K3 K2 89.9(2) 6_565 . ?
K1 K3 OW4 64.0(4) . 6_565 ?
OW3 K3 OW4 106.3(3) . 6_565 ?
O4 K3 OW4 81.2(2) 6_565 6_565 ?
O8 K3 OW4 142.7(3) 7_556 6_565 ?
C5 K3 OW4 72.0(2) 6_565 6_565 ?
O8 K3 OW4 115.2(3) . 6_565 ?
O3 K3 OW4 69.57(19) 6_565 6_565 ?
K2 K3 OW4 159.4(3) . 6_565 ?
K1 K3 C14 76.9(4) . 7_556 ?
OW3 K3 C14 80.9(3) . 7_556 ?
O4 K3 C14 155.4(3) 6_565 7_556 ?
O8 K3 C14 22.72(11) 7_556 7_556 ?
C5 K3 C14 164.5(3) 6_565 7_556 ?
O8 K3 C14 81.0(2) . 7_556 ?
O3 K3 C14 145.5(3) 6_565 7_556 ?
K2 K3 C14 75.47(19) . 7_556 ?
OW4 K3 C14 120.7(3) 6_565 7_556 ?
K1 K3 K4 150.2(7) . . ?
OW3 K3 K4 41.0(4) . . ?
O4 K3 K4 92.2(4) 6_565 . ?
O8 K3 K4 61.7(4) 7_556 . ?
C5 K3 K4 88.0(4) 6_565 . ?
O8 K3 K4 98.2(4) . . ?
O3 K3 K4 79.3(4) 6_565 . ?
K2 K3 K4 20.3(3) . . ?
OW4 K3 K4 143.7(4) 6_565 . ?
C14 K3 K4 76.6(4) 7_556 . ?
K1 K3 O1 62.1(4) . 7_556 ?
OW3 K3 O1 82.7(3) . 7_556 ?
O4 K3 O1 145.8(3) 6_565 7_556 ?
O8 K3 O1 80.4(2) 7_556 7_556 ?
C5 K3 O1 130.3(3) 6_565 7_556 ?
O8 K3 O1 117.3(3) . 7_556 ?
O3 K3 O1 111.9(2) 6_565 7_556 ?
K2 K3 O1 124.9(3) . 7_556 ?
OW4 K3 O1 64.82(17) 6_565 7_556 ?
C14 K3 O1 57.75(16) 7_556 7_556 ?
K4 K3 O1 113.0(4) . 7_556 ?
K2 K4 K4 142.8(18) . 7_566 ?
K2 K4 OW3 104.3(11) . . ?
K4 K4 OW3 103.6(12) 7_566 . ?
K2 K4 O6 72.1(9) . . ?
K4 K4 O6 120.0(12) 7_566 . ?
OW3 K4 O6 109.3(7) . . ?
K2 K4 K2 155.5(12) . 7_566 ?
K4 K4 K2 12.7(7) 7_566 7_566 ?
OW3 K4 K2 94.1(6) . 7_566 ?
O6 K4 K2 117.1(6) . 7_566 ?
K2 K4 O8 58.3(8) . 7_556 ?
K4 K4 O8 109.5(11) 7_566 7_556 ?
OW3 K4 O8 71.4(5) . 7_556 ?
O6 K4 O8 127.8(6) . 7_556 ?
K2 K4 O8 114.8(5) 7_566 7_556 ?
K2 K4 O2 54.7(8) . 4_556 ?
K4 K4 O2 88.2(10) 7_566 4_556 ?
OW3 K4 O2 133.0(7) . 4_556 ?
O6 K4 O2 102.8(5) . 4_556 ?
K2 K4 O2 100.9(5) 7_566 4_556 ?
O8 K4 O2 61.8(3) 7_556 4_556 ?
K2 K4 K3 68.2(9) . . ?
K4 K4 K3 136.5(12) 7_566 . ?
OW3 K4 K3 36.2(3) . . ?
O6 K4 K3 95.4(5) . . ?
K2 K4 K3 129.3(6) 7_566 . ?
O8 K4 K3 53.4(3) 7_556 . ?
O2 K4 K3 109.0(5) 4_556 . ?
K2 K4 OW3 109.9(11) . 7_566 ?
K4 K4 OW3 38.8(8) 7_566 7_566 ?
OW3 K4 OW3 142.4(8) . 7_566 ?
O6 K4 OW3 95.8(5) . 7_566 ?
K2 K4 OW3 48.8(3) 7_566 7_566 ?
O8 K4 OW3 114.5(5) 7_556 7_566 ?
O2 K4 OW3 62.7(3) 4_556 7_566 ?
K3 K4 OW3 167.4(6) . 7_566 ?
K2 K4 K1 64.5(8) . . ?
K4 K4 K1 136.0(11) 7_566 . ?
OW3 K4 K1 40.0(3) . . ?
O6 K4 K1 99.3(5) . . ?
K2 K4 K1 130.5(5) 7_566 . ?
O8 K4 K1 46.6(2) 7_556 . ?
O2 K4 K1 102.4(5) 4_556 . ?
K3 K4 K1 6.99(16) . . ?
OW3 K4 K1 161.0(6) 7_566 . ?
K2 K4 K1 29.0(7) . 7_556 ?
K4 K4 K1 120.3(11) 7_566 7_556 ?
OW3 K4 K1 101.9(6) . 7_556 ?
O6 K4 K1 100.2(5) . 7_556 ?
K2 K4 K1 131.6(5) 7_566 7_556 ?
O8 K4 K1 35.9(2) 7_556 7_556 ?
O2 K4 K1 37.9(2) 4_556 7_556 ?
K3 K4 K1 71.7(4) . 7_556 ?
OW3 K4 K1 100.6(4) 7_566 7_556 ?
K1 K4 K1 65.4(3) . 7_556 ?
K2 K4 K3 125.4(11) . 7_566 ?
K4 K4 K3 26.5(8) 7_566 7_566 ?
OW3 K4 K3 128.5(7) . 7_566 ?
O6 K4 K3 98.7(4) . 7_566 ?
K2 K4 K3 34.5(2) 7_566 7_566 ?
O8 K4 K3 121.9(5) 7_556 7_566 ?
O2 K4 K3 77.1(3) 4_556 7_566 ?
K3 K4 K3 163.0(5) . 7_566 ?
OW3 K4 K3 15.50(17) 7_566 7_566 ?
K1 K4 K3 161.6(5) . 7_566 ?
K1 K4 K3 114.7(4) 7_556 7_566 ?

_refine_diff_density_max         1.335
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.142

####################################################################### 
# 
# 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_glutbabs
_database_code_depnum_ccdc_archive 'CCDC 1882457'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H40 Cl Lu N8 O20'
_chemical_formula_weight         826.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.064(3)
_cell_length_b                   11.133(3)
_cell_length_c                   13.009(4)
_cell_angle_alpha                90.70(2)
_cell_angle_beta                 91.64(2)
_cell_angle_gamma                110.49(3)
_cell_volume                     1500.0(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11554
_cell_measurement_theta_min      3.1339
_cell_measurement_theta_max      36.8664

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_F_000             832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.216
_exptl_absorpt_coefficient_mu    3.473
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            12699
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.134
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6777
_reflns_number_gt                6293
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6777
_refine_ls_number_parameters     425
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1319
_refine_ls_wR_factor_gt          0.1283
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu Lu 0.61154(2) 0.73712(2) 0.71066(2) 0.01183(10) Uani 1 1 d . . . . .
Cl1 Cl 1.01198(12) 0.66022(12) 0.33259(9) 0.0187(2) Uani 1 1 d . . . . .
O3 O 0.6091(3) 0.9277(3) 0.6532(3) 0.0151(7) Uani 1 1 d . . . . .
O7 O 0.6609(4) 1.0734(4) 0.5304(3) 0.0203(8) Uani 1 1 d . . . . .
O4 O 0.7523(3) 0.8077(3) 0.8421(2) 0.0150(7) Uani 1 1 d . . . . .
O8 O 0.9480(4) 0.9156(4) 0.9095(3) 0.0282(9) Uani 1 1 d . . . . .
O2 O 0.6142(3) 0.6854(3) 0.5449(3) 0.0173(7) Uani 1 1 d . . . . .
O6 O 0.6560(4) 0.5791(4) 0.4149(3) 0.0218(8) Uani 1 1 d . . . . .
O1 O 0.5428(3) 0.5422(3) 0.7840(3) 0.0160(7) Uani 1 1 d . . . . .
O5 O 0.5769(4) 0.3754(4) 0.8567(3) 0.0225(8) Uani 1 1 d . . . . .
O11 O 0.9668(4) 0.5641(4) 0.2503(3) 0.0310(9) Uani 1 1 d . . . . .
O12 O 1.1444(4) 0.7389(4) 0.3163(3) 0.0278(9) Uani 1 1 d . . . . .
O13 O 0.9343(4) 0.7402(4) 0.3336(3) 0.0278(9) Uani 1 1 d . . . . .
O14 O 1.0054(5) 0.5972(5) 0.4291(3) 0.0387(11) Uani 1 1 d . . . . .
OW1 O 1.2035(4) 0.7382(4) 0.5931(3) 0.0212(8) Uani 1 1 d D . . . .
OW2 O 0.7935(4) 1.0072(4) 0.1201(3) 0.0250(8) Uani 1 1 d D . . . .
OW3 O 0.2289(4) 0.7614(4) 0.8160(3) 0.0271(9) Uani 1 1 d D . . . .
OW4 O 1.2717(4) 0.7677(4) 0.1254(3) 0.0235(8) Uani 1 1 d D . . . .
OW5 O 0.6140(4) 0.9985(4) 0.9611(3) 0.0206(8) Uani 1 1 d D . . . .
OW6 O 1.0912(5) 0.6172(6) -0.0241(5) 0.0538(15) Uani 1 1 d D . . . .
OW7 O 0.4970(3) 0.7892(3) 0.8394(3) 0.0177(7) Uani 1 1 d D . . . .
OW8 O 0.3945(3) 0.6535(4) 0.6622(3) 0.0190(7) Uiso 1 1 d D . . . .
N2 N 0.8324(4) 0.8844(4) 0.6475(3) 0.0138(8) Uani 1 1 d . . . . .
N1 N 0.7628(4) 0.6126(4) 0.6818(3) 0.0143(8) Uani 1 1 d . . . . .
N11 N 0.5698(4) 0.9562(5) 0.2674(4) 0.0219(10) Uani 1 1 d . . . . .
H11A H 0.509077 0.983867 0.283165 0.026 Uiso 1 1 calc R U . . .
H11B H 0.620276 0.990869 0.218601 0.026 Uiso 1 1 calc R U . . .
N12 N 0.6806(5) 0.8173(5) 0.2936(4) 0.0213(9) Uani 1 1 d . . . . .
H12A H 0.691563 0.755063 0.326416 0.026 Uiso 1 1 calc R U . . .
H12B H 0.730697 0.852485 0.244730 0.026 Uiso 1 1 calc R U . . .
N13 N 0.5078(4) 0.8058(4) 0.3939(3) 0.0192(9) Uani 1 1 d . . . . .
H13A H 0.447058 0.833511 0.409673 0.023 Uiso 1 1 calc R U . . .
H13B H 0.517961 0.743397 0.426950 0.023 Uiso 1 1 calc R U . . .
N21 N 0.7193(5) 0.5608(5) 0.1503(4) 0.0256(10) Uani 1 1 d . . . . .
H21A H 0.641296 0.528777 0.170260 0.031 Uiso 1 1 calc R U . . .
H21B H 0.778190 0.535631 0.176978 0.031 Uiso 1 1 calc R U . . .
N22 N 0.6589(4) 0.6880(5) 0.0373(3) 0.0217(9) Uani 1 1 d . . . . .
H22A H 0.580693 0.656403 0.056811 0.026 Uiso 1 1 calc R U . . .
H22B H 0.678874 0.745187 -0.009282 0.026 Uiso 1 1 calc R U . . .
N23 N 0.8702(5) 0.6991(5) 0.0479(4) 0.0326(12) Uani 1 1 d . . . . .
H23A H 0.929353 0.674475 0.074638 0.039 Uiso 1 1 calc R U . . .
H23B H 0.889015 0.756245 0.001325 0.039 Uiso 1 1 calc R U . . .
C2 C 0.9101(5) 0.8102(5) 0.6087(4) 0.0163(10) Uani 1 1 d . . . . .
H2A H 0.999839 0.865739 0.607214 0.020 Uiso 1 1 calc R U . . .
H2B H 0.881045 0.780205 0.538873 0.020 Uiso 1 1 calc R U . . .
C1 C 0.8993(5) 0.6963(5) 0.6750(4) 0.0178(10) Uani 1 1 d . . . . .
H1A H 0.948283 0.647983 0.645674 0.021 Uiso 1 1 calc R U . . .
H1B H 0.935288 0.726242 0.743397 0.021 Uiso 1 1 calc R U . . .
C3 C 0.7512(5) 0.5247(5) 0.7679(4) 0.0169(10) Uani 1 1 d . . . . .
H3A H 0.809585 0.569541 0.824200 0.020 Uiso 1 1 calc R U . . .
H3B H 0.775834 0.453238 0.745770 0.020 Uiso 1 1 calc R U . . .
C4 C 0.6121(5) 0.4736(5) 0.8056(4) 0.0150(9) Uani 1 1 d . . . . .
C5 C 0.7161(5) 0.5366(5) 0.5851(4) 0.0176(10) Uani 1 1 d . . . . .
H5A H 0.651107 0.454971 0.600895 0.021 Uiso 1 1 calc R U . . .
H5B H 0.787414 0.519348 0.554511 0.021 Uiso 1 1 calc R U . . .
C6 C 0.6594(5) 0.6041(5) 0.5086(4) 0.0171(10) Uani 1 1 d . . . . .
C7 C 0.8075(5) 0.9655(5) 0.5670(4) 0.0153(9) Uani 1 1 d . . . . .
H7A H 0.800765 0.922909 0.500503 0.018 Uiso 1 1 calc R U . . .
H7B H 0.879577 1.046014 0.566194 0.018 Uiso 1 1 calc R U . . .
C8 C 0.6837(5) 0.9925(5) 0.5846(4) 0.0134(9) Uani 1 1 d . . . . .
C9 C 0.8967(5) 0.9641(5) 0.7384(4) 0.0159(9) Uani 1 1 d . . . . .
H9A H 0.869470 1.037864 0.742957 0.019 Uiso 1 1 calc R U . . .
H9B H 0.989351 0.995398 0.730182 0.019 Uiso 1 1 calc R U . . .
C10 C 0.8655(5) 0.8899(5) 0.8377(4) 0.0181(10) Uani 1 1 d . . . . .
C11 C 0.5856(5) 0.8593(5) 0.3187(4) 0.0173(10) Uani 1 1 d . . . . .
C12 C 0.7488(5) 0.6485(5) 0.0789(4) 0.0207(11) Uani 1 1 d . . . . .
H71 H 0.525(5) 0.855(4) 0.886(4) 0.031 Uiso 1 1 d D U . . .
H72 H 0.4120(14) 0.774(5) 0.830(5) 0.031 Uiso 1 1 d D U . . .
H81 H 0.336(4) 0.682(4) 0.632(4) 0.031 Uiso 1 1 d D U . . .
H82 H 0.361(5) 0.5677(8) 0.654(5) 0.031 Uiso 1 1 d D U . . .
H11 H 1.141(4) 0.685(4) 0.551(3) 0.031 Uiso 1 1 d D U . . .
H12 H 1.238(5) 0.809(3) 0.556(3) 0.031 Uiso 1 1 d D U . . .
H22 H 0.871(3) 1.001(6) 0.109(5) 0.031 Uiso 1 1 d D U . . .
H31 H 0.168(4) 0.782(6) 0.849(3) 0.031 Uiso 1 1 d D U . . .
H32 H 0.200(5) 0.747(6) 0.7502(14) 0.031 Uiso 1 1 d D U . . .
H41 H 1.248(6) 0.775(6) 0.1900(16) 0.031 Uiso 1 1 d D U . . .
H42 H 1.315(5) 0.713(5) 0.129(4) 0.031 Uiso 1 1 d D U . . .
H51 H 0.651(5) 1.075(4) 0.933(6) 0.031 Uiso 0.5 1 d D U P . .
H51A H 0.544(7) 1.004(8) 0.991(8) 0.031 Uiso 0.5 1 d D U P . .
H52 H 0.676(4) 0.989(6) 1.003(4) 0.031 Uiso 1 1 d D U . . .
H61 H 1.137(5) 0.642(6) 0.035(3) 0.031 Uiso 1 1 d D U . . .
H62 H 1.046(7) 0.533(2) -0.017(6) 0.031 Uiso 0.5 1 d D U P . .
H62A H 1.173(3) 0.621(9) -0.033(11) 0.031 Uiso 0.5 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu O4 2.219(3) . ?
Lu O2 2.229(3) . ?
Lu O1 2.266(3) . ?
Lu O3 2.267(3) . ?
Lu OW7 2.316(3) . ?
Lu OW8 2.316(4) . ?
Lu N1 2.551(4) . ?
Lu N2 2.584(4) . ?
Cl1 O14 1.437(4) . ?
Cl1 O13 1.438(4) . ?
Cl1 O12 1.443(4) . ?
Cl1 O11 1.452(4) . ?
O3 C8 1.280(6) . ?
O7 C8 1.239(6) . ?
O4 C10 1.270(6) . ?
O8 C10 1.244(6) . ?
O2 C6 1.269(6) . ?
O6 C6 1.245(6) . ?
O1 C4 1.285(6) . ?
O5 C4 1.235(6) . ?
N2 C7 1.472(6) . ?
N2 C9 1.475(6) . ?
N2 C2 1.479(6) . ?
N1 C3 1.475(6) . ?
N1 C1 1.477(6) . ?
N1 C5 1.482(6) . ?
N11 C11 1.335(7) . ?
N12 C11 1.338(7) . ?
N13 C11 1.326(7) . ?
N21 C12 1.319(7) . ?
N22 C12 1.325(7) . ?
N23 C12 1.337(7) . ?
C2 C1 1.514(7) . ?
C3 C4 1.539(7) . ?
C5 C6 1.503(7) . ?
C7 C8 1.524(6) . ?
C9 C10 1.524(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Lu O2 137.73(13) . . ?
O4 Lu O1 88.15(13) . . ?
O2 Lu O1 102.09(13) . . ?
O4 Lu O3 99.20(13) . . ?
O2 Lu O3 85.32(13) . . ?
O1 Lu O3 159.54(13) . . ?
O4 Lu OW7 74.90(13) . . ?
O2 Lu OW7 146.40(13) . . ?
O1 Lu OW7 83.40(13) . . ?
O3 Lu OW7 80.19(13) . . ?
O4 Lu OW8 145.00(12) . . ?
O2 Lu OW8 76.87(13) . . ?
O1 Lu OW8 76.56(13) . . ?
O3 Lu OW8 86.81(13) . . ?
OW7 Lu OW8 72.23(13) . . ?
O4 Lu N1 78.42(13) . . ?
O2 Lu N1 68.61(13) . . ?
O1 Lu N1 67.29(13) . . ?
O3 Lu N1 132.79(13) . . ?
OW7 Lu N1 140.69(13) . . ?
OW8 Lu N1 121.88(13) . . ?
O4 Lu N2 69.44(13) . . ?
O2 Lu N2 74.23(13) . . ?
O1 Lu N2 133.54(13) . . ?
O3 Lu N2 66.72(13) . . ?
OW7 Lu N2 125.39(13) . . ?
OW8 Lu N2 141.91(13) . . ?
N1 Lu N2 68.57(13) . . ?
O14 Cl1 O13 110.3(3) . . ?
O14 Cl1 O12 108.9(3) . . ?
O13 Cl1 O12 109.1(3) . . ?
O14 Cl1 O11 109.2(3) . . ?
O13 Cl1 O11 110.1(3) . . ?
O12 Cl1 O11 109.3(3) . . ?
C8 O3 Lu 123.9(3) . . ?
C10 O4 Lu 125.9(3) . . ?
C6 O2 Lu 126.1(3) . . ?
C4 O1 Lu 126.2(3) . . ?
C7 N2 C9 110.0(4) . . ?
C7 N2 C2 111.2(4) . . ?
C9 N2 C2 111.0(4) . . ?
C7 N2 Lu 107.6(3) . . ?
C9 N2 Lu 104.8(3) . . ?
C2 N2 Lu 112.0(3) . . ?
C3 N1 C1 109.0(4) . . ?
C3 N1 C5 109.3(4) . . ?
C1 N1 C5 110.7(4) . . ?
C3 N1 Lu 108.5(3) . . ?
C1 N1 Lu 113.1(3) . . ?
C5 N1 Lu 106.2(3) . . ?
N2 C2 C1 111.9(4) . . ?
N1 C1 C2 110.4(4) . . ?
N1 C3 C4 111.0(4) . . ?
O5 C4 O1 125.1(5) . . ?
O5 C4 C3 119.1(4) . . ?
O1 C4 C3 115.7(4) . . ?
N1 C5 C6 112.6(4) . . ?
O6 C6 O2 122.4(5) . . ?
O6 C6 C5 121.0(4) . . ?
O2 C6 C5 116.6(4) . . ?
N2 C7 C8 111.8(4) . . ?
O7 C8 O3 124.6(5) . . ?
O7 C8 C7 118.0(4) . . ?
O3 C8 C7 117.4(4) . . ?
N2 C9 C10 112.1(4) . . ?
O8 C10 O4 124.4(5) . . ?
O8 C10 C9 119.5(5) . . ?
O4 C10 C9 116.1(4) . . ?
N13 C11 N11 120.0(5) . . ?
N13 C11 N12 120.6(5) . . ?
N11 C11 N12 119.4(5) . . ?
N21 C12 N22 120.5(5) . . ?
N21 C12 N23 120.3(5) . . ?
N22 C12 N23 119.2(5) . . ?

_refine_diff_density_max         1.992
_refine_diff_density_min         -3.142
_refine_diff_density_rms         0.239

####################################################################### 
# 
# 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_lugd18ca
_database_code_depnum_ccdc_archive 'CCDC 1882461'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H48 Cl3 Lu O18'
_chemical_formula_weight         761.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.308(4)
_cell_length_b                   18.561(9)
_cell_length_c                   15.946(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.07(4)
_cell_angle_gamma                90
_cell_volume                     2983(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7567
_cell_measurement_theta_min      2.9835
_cell_measurement_theta_max      28.8384

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_F_000             1544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.205
_exptl_absorpt_coefficient_mu    3.645
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            16846
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.9835
_diffrn_reflns_theta_max         28.8384
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.9189
_diffrn_measured_fraction_theta_full 0.9927
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7168
_reflns_number_gt                5078
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0924P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7168
_refine_ls_number_parameters     379
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1765
_refine_ls_wR_factor_gt          0.1512
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Lu Lu 0.67864(2) 0.75161(2) 0.11348(2) 0.01274(12) Uani 1 1 d . . . . .
OW1 O 0.8605(4) 0.7804(2) 0.0615(2) 0.0218(9) Uani 1 1 d D . . . .
HW11 H 0.862(5) 0.778(4) 0.0054(8) 0.033 Uiso 1 1 d D U . . .
HW12 H 0.943(2) 0.794(3) 0.087(3) 0.033 Uiso 1 1 d D U . . .
OW2 O 0.6178(5) 0.74871(18) -0.0356(3) 0.0173(10) Uani 1 1 d D . . . .
HW21 H 0.568(4) 0.7858(11) -0.060(4) 0.026 Uiso 1 1 d D U . . .
HW22 H 0.570(4) 0.7091(10) -0.055(4) 0.026 Uiso 1 1 d D U . . .
OW3 O 0.6072(4) 0.6348(2) 0.0808(3) 0.0172(8) Uani 1 1 d D . . . .
HW31 H 0.5218(15) 0.620(3) 0.069(4) 0.026 Uiso 1 1 d D U . . .
HW32 H 0.654(4) 0.5944(16) 0.098(4) 0.026 Uiso 1 1 d D U . . .
OW4 O 0.8409(4) 0.6727(2) 0.1789(3) 0.0211(9) Uani 1 1 d D . . . .
HW41 H 0.832(5) 0.650(3) 0.227(2) 0.032 Uiso 1 1 d D U . . .
HW42 H 0.920(3) 0.658(3) 0.169(3) 0.032 Uiso 1 1 d D U . . .
OW5 O 0.6344(4) 0.7308(2) 0.2469(3) 0.0210(9) Uani 1 1 d D . . . .
HW51 H 0.553(2) 0.739(3) 0.256(4) 0.032 Uiso 1 1 d D U . . .
HW52 H 0.677(4) 0.707(3) 0.294(2) 0.032 Uiso 1 1 d D U . . .
OW6 O 0.4486(4) 0.75343(19) 0.0991(3) 0.0162(9) Uani 1 1 d D . . . .
HW61 H 0.395(3) 0.7149(12) 0.093(4) 0.024 Uiso 1 1 d D U . . .
HW62 H 0.395(3) 0.7911(12) 0.081(4) 0.024 Uiso 1 1 d D U . . .
OW7 O 0.6061(4) 0.8665(2) 0.0764(3) 0.0214(9) Uani 1 1 d D . . . .
HW71 H 0.656(4) 0.9043(19) 0.098(4) 0.032 Uiso 1 1 d D U . . .
HW72 H 0.526(2) 0.885(3) 0.055(4) 0.032 Uiso 1 1 d D U . . .
OW8 O 0.8096(4) 0.8300(2) 0.2118(3) 0.0223(9) Uani 1 1 d D . . . .
HW81 H 0.809(5) 0.832(3) 0.2680(9) 0.033 Uiso 1 1 d D U . . .
HW82 H 0.870(5) 0.863(2) 0.204(3) 0.033 Uiso 1 1 d D U . . .
OW9 O 0.7387(5) 0.5082(3) 0.1037(3) 0.0269(10) Uani 1 1 d D . . . .
HW91 H 0.729(6) 0.470(2) 0.068(3) 0.040 Uiso 1 1 d D U . . .
HW92 H 0.806(4) 0.496(3) 0.147(2) 0.040 Uiso 1 1 d D U . . .
OW10 O 1.0859(4) 0.8426(3) 0.1419(3) 0.0357(12) Uani 1 1 d D . . . .
H101 H 1.067(7) 0.883(2) 0.168(5) 0.054 Uiso 1 1 d D U . . .
H102 H 1.155(4) 0.855(3) 0.119(4) 0.054 Uiso 1 1 d D U . . .
OW11 O 1.0744(5) 0.6153(3) 0.1612(3) 0.0346(11) Uani 1 1 d D . . . .
H111 H 1.067(6) 0.5685(10) 0.174(4) 0.052 Uiso 1 1 d D U . . .
H112 H 1.146(4) 0.617(3) 0.137(4) 0.052 Uiso 1 1 d D U . . .
OW12 O 0.7542(5) 0.9844(3) 0.1007(3) 0.0384(13) Uani 1 1 d D . . . .
H121 H 0.755(7) 1.021(3) 0.064(3) 0.058 Uiso 1 1 d D U . . .
H122 H 0.825(4) 0.992(4) 0.143(3) 0.058 Uiso 1 1 d D U . . .
O1 O 0.4024(5) 0.74339(19) -0.2001(3) 0.0199(10) Uani 1 1 d . . . . .
O2 O 0.5127(4) 0.8734(2) -0.1329(3) 0.0226(9) Uani 1 1 d . . . . .
O3 O 0.7702(4) 0.8945(2) -0.1804(2) 0.0248(9) Uani 1 1 d . . . . .
O4 O 0.9321(4) 0.7846(3) -0.0940(3) 0.0275(10) Uani 1 1 d . . . . .
O5 O 0.8421(4) 0.6471(2) -0.1174(2) 0.0285(10) Uani 1 1 d . . . . .
O6 O 0.5661(4) 0.6256(2) -0.1394(3) 0.0251(10) Uani 1 1 d . . . . .
Cl1 Cl 0.29852(14) 0.61112(8) 0.04550(9) 0.0204(3) Uani 1 1 d . . . . .
Cl2 Cl 0.30146(14) 0.89404(8) 0.03970(10) 0.0207(3) Uani 1 1 d . . . . .
Cl3 Cl 1.00230(14) 0.96997(9) 0.25186(9) 0.0286(3) Uani 1 1 d . . . . .
C1 C 0.3236(6) 0.8028(4) -0.1853(4) 0.0302(16) Uani 1 1 d . . . . .
H1A H 0.308676 0.800863 -0.127232 0.036 Uiso 1 1 calc R U . . .
H1B H 0.238178 0.801158 -0.224735 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3939(6) 0.8708(4) -0.1980(4) 0.0299(16) Uani 1 1 d . . . . .
H2A H 0.415207 0.871409 -0.254396 0.036 Uiso 1 1 calc R U . . .
H2B H 0.338304 0.912137 -0.193085 0.036 Uiso 1 1 calc R U . . .
C3 C 0.5787(6) 0.9408(3) -0.1278(4) 0.0255(13) Uani 1 1 d . . . . .
H3A H 0.632190 0.946700 -0.070511 0.031 Uiso 1 1 calc R U . . .
H3B H 0.513061 0.978974 -0.137397 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6669(6) 0.9481(3) -0.1922(4) 0.0271(13) Uani 1 1 d . . . . .
H4A H 0.613040 0.943794 -0.249685 0.033 Uiso 1 1 calc R U . . .
H4B H 0.706883 0.995638 -0.186916 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8746(7) 0.9087(4) -0.1081(4) 0.0303(15) Uani 1 1 d . . . . .
H5A H 0.841898 0.904275 -0.055509 0.036 Uiso 1 1 calc R U . . .
H5B H 0.907897 0.957267 -0.111351 0.036 Uiso 1 1 calc R U . . .
C6 C 0.9839(6) 0.8547(4) -0.1086(4) 0.0303(15) Uani 1 1 d . . . . .
H6A H 1.010725 0.855662 -0.163423 0.036 Uiso 1 1 calc R U . . .
H6B H 1.060514 0.865933 -0.063850 0.036 Uiso 1 1 calc R U . . .
C7 C 1.0238(6) 0.7295(4) -0.1028(4) 0.0311(15) Uani 1 1 d . . . . .
H7A H 1.110965 0.740916 -0.068873 0.037 Uiso 1 1 calc R U . . .
H7B H 1.030584 0.724876 -0.162326 0.037 Uiso 1 1 calc R U . . .
C8 C 0.9723(6) 0.6591(4) -0.0712(4) 0.0323(16) Uani 1 1 d . . . . .
H8A H 1.028965 0.619252 -0.079897 0.039 Uiso 1 1 calc R U . . .
H8B H 0.972967 0.662501 -0.010382 0.039 Uiso 1 1 calc R U . . .
C9 C 0.7878(7) 0.5820(4) -0.0919(4) 0.0329(16) Uani 1 1 d . . . . .
H9A H 0.778046 0.585962 -0.032885 0.039 Uiso 1 1 calc R U . . .
H9B H 0.847013 0.542076 -0.095733 0.039 Uiso 1 1 calc R U . . .
C10 C 0.6561(7) 0.5685(4) -0.1489(4) 0.0333(15) Uani 1 1 d . . . . .
H10A H 0.665609 0.565940 -0.208045 0.040 Uiso 1 1 calc R U . . .
H10B H 0.621058 0.522810 -0.134078 0.040 Uiso 1 1 calc R U . . .
C11 C 0.4406(6) 0.6178(4) -0.1955(4) 0.0310(16) Uani 1 1 d . . . . .
H11A H 0.403160 0.571220 -0.186476 0.037 Uiso 1 1 calc R U . . .
H11B H 0.451117 0.620085 -0.254502 0.037 Uiso 1 1 calc R U . . .
C12 C 0.3493(6) 0.6760(4) -0.1797(4) 0.0278(15) Uani 1 1 d . . . . .
H12A H 0.261700 0.668647 -0.215183 0.033 Uiso 1 1 calc R U . . .
H12B H 0.341792 0.675553 -0.120026 0.033 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu OW1 2.266(4) . ?
Lu OW7 2.296(4) . ?
Lu OW5 2.300(4) . ?
Lu OW4 2.302(4) . ?
Lu OW3 2.314(4) . ?
Lu OW2 2.329(5) . ?
Lu OW6 2.334(5) . ?
Lu OW8 2.348(4) . ?
O1 C1 1.419(7) . ?
O1 C12 1.431(7) . ?
O2 C3 1.418(7) . ?
O2 C2 1.431(7) . ?
O3 C5 1.428(7) . ?
O3 C4 1.441(7) . ?
O4 C7 1.419(8) . ?
O4 C6 1.443(8) . ?
O5 C8 1.407(7) . ?
O5 C9 1.426(7) . ?
O6 C11 1.418(7) . ?
O6 C10 1.438(7) . ?
C1 C2 1.490(9) . ?
C3 C4 1.513(8) . ?
C5 C6 1.510(9) . ?
C7 C8 1.536(10) . ?
C9 C10 1.488(9) . ?
C11 C12 1.488(9) . ?

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
OW1 Lu OW7 86.39(16) . . ?
OW1 Lu OW5 135.79(14) . . ?
OW7 Lu OW5 106.07(16) . . ?
OW1 Lu OW4 74.77(15) . . ?
OW7 Lu OW4 150.94(15) . . ?
OW5 Lu OW4 74.93(15) . . ?
OW1 Lu OW3 112.77(15) . . ?
OW7 Lu OW3 137.82(18) . . ?
OW5 Lu OW3 86.35(15) . . ?
OW4 Lu OW3 70.91(15) . . ?
OW1 Lu OW2 72.50(16) . . ?
OW7 Lu OW2 75.82(14) . . ?
OW5 Lu OW2 151.32(16) . . ?
OW4 Lu OW2 117.57(15) . . ?
OW3 Lu OW2 75.12(13) . . ?
OW1 Lu OW6 149.50(15) . . ?
OW7 Lu OW6 72.04(14) . . ?
OW5 Lu OW6 72.53(16) . . ?
OW4 Lu OW6 132.89(14) . . ?
OW3 Lu OW6 73.89(13) . . ?
OW2 Lu OW6 81.29(17) . . ?
OW1 Lu OW8 72.18(15) . . ?
OW7 Lu OW8 72.95(15) . . ?
OW5 Lu OW8 71.55(15) . . ?
OW4 Lu OW8 80.22(17) . . ?
OW3 Lu OW8 147.43(15) . . ?
OW2 Lu OW8 133.66(14) . . ?
OW6 Lu OW8 119.14(15) . . ?
C1 O1 C12 112.5(5) . . ?
C3 O2 C2 113.5(5) . . ?
C5 O3 C4 112.9(5) . . ?
C7 O4 C6 110.9(5) . . ?
C8 O5 C9 111.9(5) . . ?
C11 O6 C10 112.4(5) . . ?
O1 C1 C2 108.9(5) . . ?
O2 C2 C1 107.3(5) . . ?
O2 C3 C4 112.9(5) . . ?
O3 C4 C3 112.4(5) . . ?
O3 C5 C6 108.1(5) . . ?
O4 C6 C5 107.2(5) . . ?
O4 C7 C8 107.3(5) . . ?
O5 C8 C7 108.7(5) . . ?
O5 C9 C10 109.3(5) . . ?
O6 C10 C9 109.8(5) . . ?
O6 C11 C12 110.1(5) . . ?
O1 C12 C11 108.0(5) . . ?

_refine_diff_density_max         3.330
_refine_diff_density_min         -3.158
_refine_diff_density_rms         0.266

####################################################################### 
# 
# 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_ggdabs
_database_code_depnum_ccdc_archive 'CCDC 1882458'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H24 Gd N5 O11'
_chemical_formula_weight         559.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   11.236(2)
_cell_length_b                   8.6040(10)
_cell_length_c                   18.677(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.10(2)
_cell_angle_gamma                90
_cell_volume                     1805.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5681
_cell_measurement_theta_min      2.8337
_cell_measurement_theta_max      31.6257

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_F_000             1108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.206
_exptl_absorpt_coefficient_mu    3.743
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            10400
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.834
_diffrn_reflns_theta_max         31.626
_diffrn_reflns_theta_full        26.315
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5151
_reflns_number_gt                4461
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5151
_refine_ls_number_parameters     277
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.24891(2) 0.81550(2) 0.11799(2) 0.00703(4) Uani 1 1 d . . . . .
O1 O 0.43868(18) 0.7006(2) 0.14735(10) 0.0130(4) Uani 1 1 d . . . . .
O2 O 0.05402(18) 0.7180(2) 0.15486(10) 0.0118(4) Uani 1 1 d . . . . .
O3 O 0.12543(18) 0.8373(2) 0.01569(9) 0.0107(4) Uani 1 1 d . . . . .
O4 O 0.37308(18) 0.8579(2) 0.01708(9) 0.0107(4) Uani 1 1 d . . . . .
O5 O 0.56244(18) 0.5663(3) 0.21649(10) 0.0152(4) Uani 1 1 d . . . . .
O6 O -0.06758(18) 0.6030(3) 0.23201(10) 0.0160(4) Uani 1 1 d . . . . .
O7 O 0.0251(2) 0.7284(2) -0.07431(10) 0.0173(5) Uani 1 1 d . . . . .
O8 O 0.4523(2) 0.7828(3) -0.08712(11) 0.0251(6) Uani 1 1 d . . . . .
C1 C 0.4599(3) 0.6024(3) 0.19579(13) 0.0120(6) Uani 1 1 d . . . . .
C2 C 0.3550(2) 0.5277(3) 0.23413(14) 0.0128(6) Uani 1 1 d . . . . .
H2A H 0.370509 0.417555 0.239995 0.015 Uiso 1 1 calc R U . . .
H2B H 0.347559 0.573109 0.281452 0.015 Uiso 1 1 calc R U . . .
C3 C 0.1402(2) 0.5548(3) 0.24422(14) 0.0129(5) Uani 1 1 d . . . . .
H3A H 0.161523 0.614526 0.286373 0.015 Uiso 1 1 calc R U . . .
H3B H 0.119484 0.450461 0.259479 0.015 Uiso 1 1 calc R U . . .
C4 C 0.0340(3) 0.6294(3) 0.20749(14) 0.0125(6) Uani 1 1 d . . . . .
C5 C 0.3935(3) 0.7592(4) -0.03196(14) 0.0135(6) Uani 1 1 d . . . . .
C6 C 0.3449(3) 0.5960(3) -0.02366(16) 0.0185(6) Uani 1 1 d . . . . .
H6A H 0.307511 0.566137 -0.068430 0.022 Uiso 1 1 calc R U . . .
H6B H 0.411402 0.526110 -0.015784 0.022 Uiso 1 1 calc R U . . .
C7 C 0.1382(3) 0.5635(3) 0.00277(14) 0.0128(5) Uani 1 1 d . . . . .
H7A H 0.083352 0.521044 0.037740 0.015 Uiso 1 1 calc R U . . .
H7B H 0.140266 0.493010 -0.037753 0.015 Uiso 1 1 calc R U . . .
C8 C 0.0925(3) 0.7215(3) -0.02218(14) 0.0106(5) Uani 1 1 d . . . . .
C9 C 0.2197(3) 0.4171(3) 0.14461(14) 0.0137(6) Uani 1 1 d . . . . .
H9A H 0.135200 0.412955 0.134013 0.016 Uiso 1 1 calc R U . . .
H9B H 0.241163 0.320471 0.168036 0.016 Uiso 1 1 calc R U . . .
C10 C 0.2871(3) 0.4290(3) 0.07528(14) 0.0135(6) Uani 1 1 d . . . . .
H10A H 0.371820 0.427335 0.085374 0.016 Uiso 1 1 calc R U . . .
H10B H 0.268752 0.339234 0.045828 0.016 Uiso 1 1 calc R U . . .
N1 N 0.2579(2) 0.5727(3) 0.03479(11) 0.0098(4) Uani 1 1 d . . . . .
N2 N 0.2421(2) 0.5482(3) 0.19514(11) 0.0094(4) Uani 1 1 d . . . . .
OW1 O 0.38076(19) 1.0330(2) 0.14039(10) 0.0153(4) Uani 1 1 d D . . . .
HW1 H 0.428(4) 1.094(5) 0.1141(14) 0.091(19) Uiso 1 1 d D . . . .
HW2 H 0.399(3) 1.055(4) 0.1861(6) 0.035(11) Uiso 1 1 d D . . . .
OW2 O 0.11743(19) 1.0409(2) 0.12863(10) 0.0146(4) Uani 1 1 d D . . . .
HW3 H 0.074(3) 1.101(4) 0.0992(12) 0.037(11) Uiso 1 1 d D . . . .
HW4 H 0.100(4) 1.075(4) 0.1729(7) 0.073(16) Uiso 1 1 d D . . . .
OW3 O 0.2452(2) 0.8771(2) 0.24909(10) 0.0134(4) Uani 1 1 d D . . . .
HW5 H 0.3121(18) 0.914(5) 0.2690(19) 0.055(14) Uiso 1 1 d D . . . .
HW6 H 0.187(2) 0.942(4) 0.263(2) 0.090(19) Uiso 1 1 d D . . . .
C20 C 0.2529(3) 0.3258(3) 0.40517(14) 0.0100(5) Uani 1 1 d . . . . .
N21 N 0.3570(2) 0.3662(3) 0.43256(12) 0.0145(5) Uani 1 1 d . . . . .
H21A H 0.360539 0.435229 0.465819 0.017 Uiso 1 1 calc R U . . .
H21B H 0.421250 0.323536 0.417106 0.017 Uiso 1 1 calc R U . . .
N22 N 0.1518(2) 0.3889(3) 0.42750(12) 0.0146(5) Uani 1 1 d . . . . .
H22A H 0.152826 0.458126 0.460693 0.017 Uiso 1 1 calc R U . . .
H22B H 0.085304 0.360493 0.408779 0.017 Uiso 1 1 calc R U . . .
N23 N 0.2497(2) 0.2165(3) 0.35484(12) 0.0134(5) Uani 1 1 d . . . . .
H23A H 0.314639 0.173497 0.340679 0.016 Uiso 1 1 calc R U . . .
H23B H 0.182764 0.188834 0.336460 0.016 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O3 2.367(2) . ?
Gd O4 2.3750(19) . ?
Gd O1 2.413(2) . ?
Gd OW1 2.423(2) . ?
Gd O2 2.445(2) . ?
Gd OW2 2.446(2) . ?
Gd OW3 2.5056(19) . ?
Gd N1 2.606(2) . ?
Gd N2 2.715(2) . ?
O1 C1 1.260(3) . ?
O2 C4 1.264(3) . ?
O3 C8 1.277(3) . ?
O4 C5 1.270(3) . ?
O5 C1 1.254(3) . ?
O6 C4 1.252(3) . ?
O7 C8 1.234(3) . ?
O8 C5 1.242(3) . ?
C1 C2 1.522(4) . ?
C2 N2 1.472(3) . ?
C3 N2 1.469(3) . ?
C3 C4 1.518(4) . ?
C5 C6 1.514(4) . ?
C6 N1 1.481(3) . ?
C7 N1 1.473(4) . ?
C7 C8 1.526(4) . ?
C9 N2 1.492(3) . ?
C9 C10 1.505(4) . ?
C10 N1 1.486(3) . ?
C20 N21 1.323(4) . ?
C20 N22 1.326(4) . ?
C20 N23 1.330(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
O3 Gd O4 72.03(7) . . ?
O3 Gd O1 137.10(7) . . ?
O4 Gd O1 73.93(7) . . ?
O3 Gd OW1 115.82(7) . . ?
O4 Gd OW1 70.03(7) . . ?
O1 Gd OW1 74.78(7) . . ?
O3 Gd O2 74.37(7) . . ?
O4 Gd O2 143.49(7) . . ?
O1 Gd O2 125.94(7) . . ?
OW1 Gd O2 139.83(7) . . ?
O3 Gd OW2 69.49(6) . . ?
O4 Gd OW2 107.36(7) . . ?
O1 Gd OW2 147.15(7) . . ?
OW1 Gd OW2 75.09(7) . . ?
O2 Gd OW2 73.02(7) . . ?
O3 Gd OW3 139.59(7) . . ?
O4 Gd OW3 138.91(7) . . ?
O1 Gd OW3 83.15(7) . . ?
OW1 Gd OW3 71.27(7) . . ?
O2 Gd OW3 77.36(7) . . ?
OW2 Gd OW3 75.04(7) . . ?
O3 Gd N1 66.75(7) . . ?
O4 Gd N1 68.08(7) . . ?
O1 Gd N1 76.82(7) . . ?
OW1 Gd N1 134.27(7) . . ?
O2 Gd N1 85.88(7) . . ?
OW2 Gd N1 135.07(7) . . ?
OW3 Gd N1 138.86(7) . . ?
O3 Gd N2 118.58(7) . . ?
O4 Gd N2 124.64(7) . . ?
O1 Gd N2 63.77(7) . . ?
OW1 Gd N2 125.49(7) . . ?
O2 Gd N2 62.21(7) . . ?
OW2 Gd N2 127.65(7) . . ?
OW3 Gd N2 70.13(7) . . ?
N1 Gd N2 68.80(7) . . ?
C1 O1 Gd 127.15(18) . . ?
C4 O2 Gd 125.90(19) . . ?
C8 O3 Gd 123.68(18) . . ?
C5 O4 Gd 125.20(18) . . ?
O5 C1 O1 124.1(3) . . ?
O5 C1 C2 117.5(2) . . ?
O1 C1 C2 118.4(3) . . ?
N2 C2 C1 112.6(2) . . ?
N2 C3 C4 110.3(2) . . ?
O6 C4 O2 123.9(3) . . ?
O6 C4 C3 118.3(2) . . ?
O2 C4 C3 117.8(3) . . ?
O8 C5 O4 125.8(3) . . ?
O8 C5 C6 115.4(3) . . ?
O4 C5 C6 118.7(2) . . ?
N1 C6 C5 116.1(2) . . ?
N1 C7 C8 112.5(2) . . ?
O7 C8 O3 125.2(3) . . ?
O7 C8 C7 119.3(3) . . ?
O3 C8 C7 115.4(2) . . ?
N2 C9 C10 114.1(2) . . ?
N1 C10 C9 112.5(2) . . ?
C7 N1 C6 108.2(2) . . ?
C7 N1 C10 111.3(2) . . ?
C6 N1 C10 110.0(2) . . ?
C7 N1 Gd 104.43(16) . . ?
C6 N1 Gd 110.92(17) . . ?
C10 N1 Gd 111.87(15) . . ?
C3 N2 C2 111.6(2) . . ?
C3 N2 C9 107.0(2) . . ?
C2 N2 C9 111.5(2) . . ?
C3 N2 Gd 108.74(16) . . ?
C2 N2 Gd 109.79(16) . . ?
C9 N2 Gd 108.03(15) . . ?
N21 C20 N22 121.9(3) . . ?
N21 C20 N23 118.8(3) . . ?
N22 C20 N23 119.3(3) . . ?

_refine_diff_density_max         0.639
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_gddtpaa
_database_code_depnum_ccdc_archive 'CCDC 1882462'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H32 Gd N7 O13'
_chemical_formula_weight         675.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   15.505(3)
_cell_length_b                   17.707(3)
_cell_length_c                   17.389(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.97(2)
_cell_angle_gamma                90
_cell_volume                     4771.3(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14909
_cell_measurement_theta_min      3.1080
_cell_measurement_theta_max      27.5290

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_F_000             2712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.158
_exptl_absorpt_coefficient_mu    2.859
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.8b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 8.3359
_diffrn_reflns_number            25675
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.870
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             9944
_reflns_number_gt                8419
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0867P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9944
_refine_ls_number_parameters     703
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1284
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.22459(2) 0.23700(2) 0.17997(2) 0.01162(10) Uani 1 1 d . . . . .
Gd2 Gd -0.26879(2) 0.22834(2) 0.00774(2) 0.01175(10) Uani 1 1 d . . . . .
O1 O 0.3464(2) 0.1624(2) 0.14979(19) 0.0164(7) Uani 1 1 d . . . . .
O2 O 0.4098(2) 0.0543(2) 0.1234(2) 0.0238(9) Uani 1 1 d . . . . .
O3 O 0.2523(2) 0.2874(2) 0.05928(19) 0.0170(8) Uani 1 1 d . . . . .
O4 O 0.3190(3) 0.2803(2) -0.0506(2) 0.0239(9) Uani 1 1 d . . . . .
O5 O 0.1599(2) 0.1161(2) 0.22176(19) 0.0153(7) Uani 1 1 d . . . . .
O6 O 0.0430(2) 0.0462(2) 0.2423(2) 0.0187(8) Uani 1 1 d . . . . .
H61 H 0.085(4) 0.005(4) 0.262(3) 0.028 Uiso 1 1 d . U . . .
O7 O 0.1402(2) 0.26775(18) 0.2862(2) 0.0156(8) Uani 1 1 d . . . . .
O8 O 0.0505(2) 0.3386(2) 0.3530(2) 0.0201(8) Uani 1 1 d . . . . .
O9 O 0.3517(3) 0.4554(2) 0.1546(3) 0.0340(10) Uani 1 1 d . . . . .
O10 O 0.3086(2) 0.34743(19) 0.2077(2) 0.0163(8) Uani 1 1 d . . . . .
N1 N 0.2078(3) 0.1364(2) 0.0591(2) 0.0159(9) Uani 1 1 d . . . . .
N2 N 0.0625(3) 0.2188(2) 0.1333(2) 0.0143(9) Uani 1 1 d . . . . .
N3 N 0.1436(2) 0.3680(2) 0.1676(2) 0.0132(9) Uani 1 1 d . . . . .
C1 C 0.1161(3) 0.1184(3) 0.0447(3) 0.0165(10) Uani 1 1 d . . . . .
H1A H 0.098086 0.080686 0.081299 0.020 Uiso 1 1 calc R U . . .
H1B H 0.107689 0.097790 -0.006645 0.020 Uiso 1 1 calc R U . . .
C2 C 0.0620(3) 0.1887(3) 0.0525(3) 0.0156(10) Uani 1 1 d . . . . .
H2A H 0.083452 0.227453 0.018696 0.019 Uiso 1 1 calc R U . . .
H2B H 0.002988 0.177467 0.035992 0.019 Uiso 1 1 calc R U . . .
C3 C 0.0141(3) 0.2912(3) 0.1338(3) 0.0183(11) Uani 1 1 d . . . . .
H3A H -0.007726 0.299513 0.184679 0.022 Uiso 1 1 calc R U . . .
H3B H -0.034905 0.287894 0.097774 0.022 Uiso 1 1 calc R U . . .
C4 C 0.0699(3) 0.3577(3) 0.1122(3) 0.0169(11) Uani 1 1 d . . . . .
H4A H 0.091475 0.349691 0.061137 0.020 Uiso 1 1 calc R U . . .
H4B H 0.035071 0.403249 0.110796 0.020 Uiso 1 1 calc R U . . .
C5 C 0.2606(3) 0.0709(3) 0.0833(3) 0.0172(10) Uani 1 1 d . . . . .
H5A H 0.272538 0.039990 0.038816 0.021 Uiso 1 1 calc R U . . .
H5B H 0.229156 0.040340 0.119165 0.021 Uiso 1 1 calc R U . . .
C6 C 0.3450(3) 0.0977(3) 0.1213(3) 0.0144(10) Uani 1 1 d . . . . .
C7 C 0.2453(3) 0.1720(3) -0.0098(3) 0.0178(11) Uani 1 1 d . . . . .
H7A H 0.202369 0.170432 -0.051666 0.021 Uiso 1 1 calc R U . . .
H7B H 0.294021 0.141770 -0.025006 0.021 Uiso 1 1 calc R U . . .
C8 C 0.2750(3) 0.2523(3) 0.0006(3) 0.0163(11) Uani 1 1 d . . . . .
C9 C 0.0197(3) 0.1634(3) 0.1825(3) 0.0188(11) Uani 1 1 d . . . . .
H9A H -0.025003 0.137592 0.152264 0.023 Uiso 1 1 calc R U . . .
H9B H -0.007731 0.189891 0.223884 0.023 Uiso 1 1 calc R U . . .
C10 C 0.0816(3) 0.1056(3) 0.2165(3) 0.0148(10) Uani 1 1 d . . . . .
C11 C 0.1133(3) 0.3942(3) 0.2429(3) 0.0166(11) Uani 1 1 d . . . . .
H11A H 0.059830 0.422060 0.234903 0.020 Uiso 1 1 calc R U . . .
H11B H 0.155737 0.428300 0.265957 0.020 Uiso 1 1 calc R U . . .
C12 C 0.0982(3) 0.3281(3) 0.2984(3) 0.0145(10) Uani 1 1 d . . . . .
C13 C 0.2050(3) 0.4231(3) 0.1378(3) 0.0161(10) Uani 1 1 d . . . . .
H13A H 0.187355 0.473749 0.151770 0.019 Uiso 1 1 calc R U . . .
H13B H 0.204781 0.420043 0.082130 0.019 Uiso 1 1 calc R U . . .
C14 C 0.2957(3) 0.4079(3) 0.1706(3) 0.0213(12) Uani 1 1 d . . . . .
O11 O -0.2330(2) 0.2879(2) 0.12479(19) 0.0177(8) Uani 1 1 d . . . . .
O12 O -0.1765(2) 0.2922(2) 0.2428(2) 0.0213(8) Uani 1 1 d . . . . .
O13 O -0.1536(2) 0.1501(2) 0.04782(19) 0.0171(8) Uani 1 1 d . . . . .
O14 O -0.1097(2) 0.0313(2) 0.0664(2) 0.0259(9) Uani 1 1 d . . . . .
O15 O -0.3452(2) 0.11259(19) -0.02864(19) 0.0163(7) Uani 1 1 d . . . . .
O16 O -0.4703(2) 0.0565(2) -0.0617(2) 0.0218(8) Uani 1 1 d D . . . .
H161 H -0.429(3) 0.025(3) -0.079(3) 0.033 Uiso 1 1 d D U . . .
O17 O -0.3559(2) 0.2575(2) -0.1021(2) 0.0190(8) Uani 1 1 d . . . . .
O18 O -0.4490(2) 0.3272(2) -0.1724(2) 0.0200(8) Uani 1 1 d . . . . .
O19 O -0.1786(2) 0.3327(2) -0.0270(2) 0.0164(7) Uani 1 1 d . . . . .
O20 O -0.1201(2) 0.4332(2) 0.0312(2) 0.0208(8) Uani 1 1 d . . . . .
OW1 O 0.3099(2) 0.2056(2) 0.2931(2) 0.0191(8) Uani 1 1 d D . . . .
HW11 H 0.305(4) 0.225(2) 0.3406(11) 0.029 Uiso 1 1 d D U . . .
HW12 H 0.335(3) 0.1605(15) 0.300(3) 0.029 Uiso 1 1 d D U . . .
OW2 O -0.1903(2) 0.1873(2) -0.1015(2) 0.0188(8) Uani 1 1 d D . . . .
HW21 H -0.193(4) 0.203(3) -0.1508(10) 0.028 Uiso 1 1 d D U . . .
HW22 H -0.155(3) 0.147(2) -0.101(3) 0.028 Uiso 1 1 d D U . . .
N4 N -0.2879(3) 0.1389(2) 0.1370(2) 0.0160(9) Uani 1 1 d . . . . .
N5 N -0.4297(3) 0.2242(2) 0.0542(2) 0.0132(9) Uani 1 1 d . . . . .
N6 N -0.3402(3) 0.3649(2) 0.0114(2) 0.0138(9) Uani 1 1 d . . . . .
C15 C -0.3800(3) 0.1269(3) 0.1500(3) 0.0178(11) Uani 1 1 d . . . . .
H15A H -0.387088 0.110320 0.202556 0.021 Uiso 1 1 calc R U . . .
H15B H -0.401857 0.087466 0.115916 0.021 Uiso 1 1 calc R U . . .
C16 C -0.4317(3) 0.1984(3) 0.1358(3) 0.0175(11) Uani 1 1 d . . . . .
H16A H -0.491139 0.189420 0.149055 0.021 Uiso 1 1 calc R U . . .
H16B H -0.408900 0.238030 0.169162 0.021 Uiso 1 1 calc R U . . .
C17 C -0.4724(3) 0.3003(3) 0.0487(3) 0.0171(11) Uani 1 1 d . . . . .
H17A H -0.519490 0.302167 0.083886 0.021 Uiso 1 1 calc R U . . .
H17B H -0.496365 0.307369 -0.003076 0.021 Uiso 1 1 calc R U . . .
C18 C -0.4096(3) 0.3636(3) 0.0676(3) 0.0147(10) Uani 1 1 d . . . . .
H18A H -0.439919 0.411539 0.066471 0.018 Uiso 1 1 calc R U . . .
H18B H -0.384689 0.356414 0.119047 0.018 Uiso 1 1 calc R U . . .
C19 C -0.2445(3) 0.1781(3) 0.2040(3) 0.0180(11) Uani 1 1 d . . . . .
H19A H -0.194560 0.148604 0.220613 0.022 Uiso 1 1 calc R U . . .
H19B H -0.283972 0.178779 0.246091 0.022 Uiso 1 1 calc R U . . .
C20 C -0.2153(3) 0.2585(3) 0.1893(3) 0.0146(10) Uani 1 1 d . . . . .
C21 C -0.2424(3) 0.0692(3) 0.1190(3) 0.0191(11) Uani 1 1 d . . . . .
H21A H -0.280507 0.036702 0.088489 0.023 Uiso 1 1 calc R U . . .
H21B H -0.227025 0.042959 0.166469 0.023 Uiso 1 1 calc R U . . .
C22 C -0.1613(3) 0.0846(3) 0.0750(3) 0.0173(11) Uani 1 1 d . . . . .
C23 C -0.4798(3) 0.1706(3) 0.0040(3) 0.0161(10) Uani 1 1 d . . . . .
H23A H -0.508472 0.198801 -0.037353 0.019 Uiso 1 1 calc R U . . .
H23B H -0.524118 0.147077 0.033927 0.019 Uiso 1 1 calc R U . . .
C24 C -0.4252(3) 0.1099(3) -0.0303(3) 0.0162(10) Uani 1 1 d . . . . .
C25 C -0.3744(3) 0.3863(3) -0.0660(3) 0.0165(10) Uani 1 1 d . . . . .
H25A H -0.332137 0.417516 -0.090848 0.020 Uiso 1 1 calc R U . . .
H25B H -0.426199 0.416300 -0.060658 0.020 Uiso 1 1 calc R U . . .
C26 C -0.3957(3) 0.3184(3) -0.1173(3) 0.0153(10) Uani 1 1 d . . . . .
C27 C -0.2723(3) 0.4182(3) 0.0370(3) 0.0166(11) Uani 1 1 d . . . . .
H27A H -0.271563 0.422161 0.092613 0.020 Uiso 1 1 calc R U . . .
H27B H -0.285034 0.467783 0.015769 0.020 Uiso 1 1 calc R U . . .
C28 C -0.1838(3) 0.3928(3) 0.0116(3) 0.0130(10) Uani 1 1 d . . . . .
C29 C 0.0438(3) 0.1380(3) 0.4095(3) 0.0160(10) Uani 1 1 d . . . . .
N7 N -0.0152(3) 0.1918(3) 0.4002(2) 0.0195(9) Uani 1 1 d . . . . .
H7C H -0.067680 0.183423 0.412331 0.023 Uiso 1 1 calc R U . . .
H7D H -0.001024 0.235055 0.382044 0.023 Uiso 1 1 calc R U . . .
N8 N 0.0240(3) 0.0706(2) 0.4374(2) 0.0175(9) Uani 1 1 d . . . . .
H8A H -0.028047 0.061057 0.449861 0.021 Uiso 1 1 calc R U . . .
H8B H 0.063260 0.036551 0.442928 0.021 Uiso 1 1 calc R U . . .
N9 N 0.1252(3) 0.1521(2) 0.3909(2) 0.0178(9) Uani 1 1 d . . . . .
H9 H 0.140329 0.196206 0.375582 0.021 Uiso 1 1 calc R U . . .
N10 N 0.1855(3) 0.0924(3) 0.3974(3) 0.0192(9) Uani 1 1 d D . . . .
HN1 H 0.2344(16) 0.106(3) 0.423(2) 0.029 Uiso 1 1 d D U . . .
HN2 H 0.203(3) 0.080(3) 0.3499(13) 0.029 Uiso 1 1 d D U . . .
C30 C 0.5367(3) 0.1271(3) 0.7649(3) 0.0180(11) Uani 1 1 d . . . . .
N11 N 0.4782(3) 0.1814(3) 0.7756(2) 0.0213(10) Uani 1 1 d . . . . .
H11C H 0.424990 0.173984 0.762141 0.026 Uiso 1 1 calc R U . . .
H11D H 0.493841 0.223780 0.795910 0.026 Uiso 1 1 calc R U . . .
N12 N 0.5145(3) 0.0622(2) 0.7342(2) 0.0201(10) Uani 1 1 d . . . . .
H12A H 0.553136 0.028452 0.726425 0.024 Uiso 1 1 calc R U . . .
H12B H 0.461338 0.053339 0.721691 0.024 Uiso 1 1 calc R U . . .
N13 N 0.6186(3) 0.1427(2) 0.7849(2) 0.0189(9) Uani 1 1 d . . . . .
H13 H 0.634485 0.187173 0.799252 0.023 Uiso 1 1 calc R U . . .
N14 N 0.6782(3) 0.0823(3) 0.7815(3) 0.0246(10) Uani 1 1 d D . . . .
HN3 H 0.691(3) 0.065(3) 0.8292(15) 0.037 Uiso 1 1 d D U . . .
HN4 H 0.7289(16) 0.099(3) 0.764(3) 0.037 Uiso 1 1 d D U . . .
OW3 O 0.9163(2) 0.0652(2) 0.9056(2) 0.0227(8) Uani 1 1 d D . . . .
HW31 H 0.9665(17) 0.081(3) 0.887(2) 0.034 Uiso 1 1 d D U . . .
HW32 H 0.929(3) 0.052(3) 0.9546(12) 0.034 Uiso 1 1 d D U . . .
OW4 O 0.8732(3) 0.0635(2) 0.6963(2) 0.0239(9) Uani 1 1 d D . . . .
HW41 H 0.865(4) 0.1110(11) 0.713(2) 0.036 Uiso 1 1 d D U . . .
HW42 H 0.875(4) 0.067(3) 0.6449(5) 0.036 Uiso 1 1 d D U . . .
OW5 O 0.4100(2) 0.0785(2) 0.3271(2) 0.0280(9) Uani 1 1 d D . . . .
HW51 H 0.451(3) 0.103(3) 0.302(2) 0.042 Uiso 1 1 d D U . . .
HW52 H 0.425(3) 0.083(4) 0.3773(7) 0.042 Uiso 1 1 d D U . . .
OW6 O 0.3856(3) 0.0788(2) 0.4892(2) 0.0316(10) Uani 1 1 d D . . . .
HW61 H 0.360(4) 0.1241(17) 0.483(3) 0.047 Uiso 1 1 d D U . . .
HW62 H 0.378(4) 0.067(3) 0.5388(12) 0.047 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.334(3) . ?
Gd1 O7 2.363(4) . ?
Gd1 O1 2.377(3) . ?
Gd1 O10 2.390(3) . ?
Gd1 OW1 2.398(3) . ?
Gd1 O5 2.483(3) . ?
Gd1 N2 2.634(4) . ?
Gd1 N3 2.643(4) . ?
Gd1 N1 2.760(4) . ?
Gd2 O11 2.342(3) . ?
Gd2 O13 2.347(3) . ?
Gd2 O17 2.358(4) . ?
Gd2 OW2 2.404(3) . ?
Gd2 O19 2.407(3) . ?
Gd2 O15 2.440(3) . ?
Gd2 N5 2.650(4) . ?
Gd2 N6 2.661(4) . ?
Gd2 N4 2.773(4) . ?
O1 C6 1.248(6) . ?
O2 C6 1.263(6) . ?
O3 C8 1.256(6) . ?
O4 C8 1.243(6) . ?
O5 C10 1.228(6) . ?
O6 C10 1.297(6) . ?
O7 C12 1.274(6) . ?
O8 C12 1.236(6) . ?
O9 C14 1.248(6) . ?
O10 C14 1.261(6) . ?
N1 C1 1.471(6) . ?
N1 C5 1.473(6) . ?
N1 C7 1.488(6) . ?
N2 C9 1.475(7) . ?
N2 C3 1.485(7) . ?
N2 C2 1.501(6) . ?
N3 C13 1.469(6) . ?
N3 C11 1.481(6) . ?
N3 C4 1.481(6) . ?
C1 C2 1.509(7) . ?
C3 C4 1.515(7) . ?
C5 C6 1.523(7) . ?
C7 C8 1.503(8) . ?
C9 C10 1.510(7) . ?
C11 C12 1.540(7) . ?
C13 C14 1.524(7) . ?
O11 C20 1.258(6) . ?
O12 C20 1.244(6) . ?
O13 C22 1.260(6) . ?
O14 C22 1.249(6) . ?
O15 C24 1.241(6) . ?
O16 C24 1.287(6) . ?
O17 C26 1.266(6) . ?
O18 C26 1.253(6) . ?
O19 C28 1.263(6) . ?
O20 C28 1.257(6) . ?
N4 C21 1.460(7) . ?
N4 C15 1.469(6) . ?
N4 C19 1.496(6) . ?
N5 C23 1.490(6) . ?
N5 C16 1.492(6) . ?
N5 C17 1.503(6) . ?
N6 C27 1.473(6) . ?
N6 C18 1.479(6) . ?
N6 C25 1.479(6) . ?
C15 C16 1.513(7) . ?
C17 C18 1.514(7) . ?
C19 C20 1.518(7) . ?
C21 C22 1.520(7) . ?
C23 C24 1.505(7) . ?
C25 C26 1.526(7) . ?
C27 C28 1.522(7) . ?
C29 N8 1.327(7) . ?
C29 N7 1.328(7) . ?
C29 N9 1.337(7) . ?
N9 N10 1.415(6) . ?
C30 N12 1.309(6) . ?
C30 N13 1.334(6) . ?
C30 N11 1.339(7) . ?
N13 N14 1.416(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Gd1 O7 137.62(12) . . ?
O3 Gd1 O1 80.90(12) . . ?
O7 Gd1 O1 139.95(12) . . ?
O3 Gd1 O10 75.65(12) . . ?
O7 Gd1 O10 88.09(12) . . ?
O1 Gd1 O10 93.86(12) . . ?
O3 Gd1 OW1 135.43(13) . . ?
O7 Gd1 OW1 73.56(12) . . ?
O1 Gd1 OW1 68.42(12) . . ?
O10 Gd1 OW1 75.07(12) . . ?
O3 Gd1 O5 132.97(12) . . ?
O7 Gd1 O5 74.32(11) . . ?
O1 Gd1 O5 85.29(12) . . ?
O10 Gd1 O5 150.39(11) . . ?
OW1 Gd1 O5 77.15(12) . . ?
O3 Gd1 N2 88.44(13) . . ?
O7 Gd1 N2 73.83(13) . . ?
O1 Gd1 N2 128.35(12) . . ?
O10 Gd1 N2 132.07(12) . . ?
OW1 Gd1 N2 135.93(13) . . ?
O5 Gd1 N2 66.05(12) . . ?
O3 Gd1 N3 72.10(13) . . ?
O7 Gd1 N3 65.64(12) . . ?
O1 Gd1 N3 148.01(12) . . ?
O10 Gd1 N3 63.40(12) . . ?
OW1 Gd1 N3 121.15(12) . . ?
O5 Gd1 N3 125.79(12) . . ?
N2 Gd1 N3 68.70(12) . . ?
O3 Gd1 N1 65.01(13) . . ?
O7 Gd1 N1 134.73(12) . . ?
O1 Gd1 N1 61.85(12) . . ?
O10 Gd1 N1 135.86(12) . . ?
OW1 Gd1 N1 120.67(12) . . ?
O5 Gd1 N1 68.81(12) . . ?
N2 Gd1 N1 67.82(13) . . ?
N3 Gd1 N1 118.18(12) . . ?
O11 Gd2 O13 81.53(12) . . ?
O11 Gd2 O17 135.82(13) . . ?
O13 Gd2 O17 141.12(12) . . ?
O11 Gd2 OW2 135.36(13) . . ?
O13 Gd2 OW2 69.84(12) . . ?
O17 Gd2 OW2 73.61(13) . . ?
O11 Gd2 O19 75.53(12) . . ?
O13 Gd2 O19 94.89(12) . . ?
O17 Gd2 O19 87.15(12) . . ?
OW2 Gd2 O19 73.69(12) . . ?
O11 Gd2 O15 134.60(12) . . ?
O13 Gd2 O15 86.49(12) . . ?
O17 Gd2 O15 73.40(12) . . ?
OW2 Gd2 O15 78.21(12) . . ?
O19 Gd2 O15 149.42(11) . . ?
O11 Gd2 N5 86.83(13) . . ?
O13 Gd2 N5 127.43(12) . . ?
O17 Gd2 N5 74.57(13) . . ?
OW2 Gd2 N5 137.78(13) . . ?
O19 Gd2 N5 131.22(12) . . ?
O15 Gd2 N5 66.56(12) . . ?
O11 Gd2 N6 69.91(12) . . ?
O13 Gd2 N6 147.39(12) . . ?
O17 Gd2 N6 65.99(12) . . ?
OW2 Gd2 N6 121.05(12) . . ?
O19 Gd2 N6 63.52(12) . . ?
O15 Gd2 N6 124.80(12) . . ?
N5 Gd2 N6 67.72(12) . . ?
O11 Gd2 N4 65.26(13) . . ?
O13 Gd2 N4 61.56(12) . . ?
O17 Gd2 N4 134.99(13) . . ?
OW2 Gd2 N4 122.62(13) . . ?
O19 Gd2 N4 136.14(12) . . ?
O15 Gd2 N4 70.50(12) . . ?
N5 Gd2 N4 66.98(12) . . ?
N6 Gd2 N4 116.31(12) . . ?
C6 O1 Gd1 126.5(3) . . ?
C8 O3 Gd1 127.3(3) . . ?
C10 O5 Gd1 121.2(3) . . ?
C12 O7 Gd1 128.6(3) . . ?
C14 O10 Gd1 121.0(3) . . ?
C1 N1 C5 113.7(4) . . ?
C1 N1 C7 110.9(4) . . ?
C5 N1 C7 109.5(4) . . ?
C1 N1 Gd1 109.5(3) . . ?
C5 N1 Gd1 104.7(3) . . ?
C7 N1 Gd1 108.1(3) . . ?
C9 N2 C3 109.5(4) . . ?
C9 N2 C2 108.6(4) . . ?
C3 N2 C2 109.0(4) . . ?
C9 N2 Gd1 110.2(3) . . ?
C3 N2 Gd1 111.7(3) . . ?
C2 N2 Gd1 107.8(3) . . ?
C13 N3 C11 109.4(4) . . ?
C13 N3 C4 110.3(4) . . ?
C11 N3 C4 110.6(4) . . ?
C13 N3 Gd1 107.5(3) . . ?
C11 N3 Gd1 111.5(3) . . ?
C4 N3 Gd1 107.4(3) . . ?
N1 C1 C2 110.1(4) . . ?
N2 C2 C1 113.0(4) . . ?
N2 C3 C4 112.1(4) . . ?
N3 C4 C3 111.7(4) . . ?
N1 C5 C6 109.8(4) . . ?
O1 C6 O2 123.0(5) . . ?
O1 C6 C5 117.4(4) . . ?
O2 C6 C5 119.5(4) . . ?
N1 C7 C8 115.4(4) . . ?
O4 C8 O3 124.0(5) . . ?
O4 C8 C7 117.7(5) . . ?
O3 C8 C7 118.3(5) . . ?
N2 C9 C10 112.7(4) . . ?
O5 C10 O6 124.4(5) . . ?
O5 C10 C9 122.6(5) . . ?
O6 C10 C9 113.0(4) . . ?
N3 C11 C12 112.1(4) . . ?
O8 C12 O7 125.2(5) . . ?
O8 C12 C11 118.4(4) . . ?
O7 C12 C11 116.3(4) . . ?
N3 C13 C14 110.5(4) . . ?
O9 C14 O10 126.0(5) . . ?
O9 C14 C13 115.9(5) . . ?
O10 C14 C13 118.0(5) . . ?
C20 O11 Gd2 128.7(3) . . ?
C22 O13 Gd2 125.1(3) . . ?
C24 O15 Gd2 120.9(3) . . ?
C26 O17 Gd2 128.1(3) . . ?
C28 O19 Gd2 117.8(3) . . ?
C21 N4 C15 113.0(4) . . ?
C21 N4 C19 110.6(4) . . ?
C15 N4 C19 111.1(4) . . ?
C21 N4 Gd2 104.1(3) . . ?
C15 N4 Gd2 109.8(3) . . ?
C19 N4 Gd2 108.0(3) . . ?
C23 N5 C16 109.6(4) . . ?
C23 N5 C17 108.2(4) . . ?
C16 N5 C17 108.2(4) . . ?
C23 N5 Gd2 108.5(3) . . ?
C16 N5 Gd2 110.5(3) . . ?
C17 N5 Gd2 111.9(3) . . ?
C27 N6 C18 109.8(4) . . ?
C27 N6 C25 109.9(4) . . ?
C18 N6 C25 111.1(4) . . ?
C27 N6 Gd2 107.2(3) . . ?
C18 N6 Gd2 108.4(3) . . ?
C25 N6 Gd2 110.4(3) . . ?
N4 C15 C16 111.5(4) . . ?
N5 C16 C15 112.5(4) . . ?
N5 C17 C18 111.8(4) . . ?
N6 C18 C17 110.1(4) . . ?
N4 C19 C20 115.6(4) . . ?
O12 C20 O11 123.6(5) . . ?
O12 C20 C19 117.6(4) . . ?
O11 C20 C19 118.8(4) . . ?
N4 C21 C22 111.8(4) . . ?
O14 C22 O13 125.6(5) . . ?
O14 C22 C21 118.0(5) . . ?
O13 C22 C21 116.4(4) . . ?
N5 C23 C24 113.4(4) . . ?
O15 C24 O16 124.5(5) . . ?
O15 C24 C23 122.7(4) . . ?
O16 C24 C23 112.9(4) . . ?
N6 C25 C26 113.1(4) . . ?
O18 C26 O17 124.7(5) . . ?
O18 C26 C25 118.2(4) . . ?
O17 C26 C25 117.1(4) . . ?
N6 C27 C28 111.5(4) . . ?
O20 C28 O19 124.0(5) . . ?
O20 C28 C27 117.5(4) . . ?
O19 C28 C27 118.5(4) . . ?
N8 C29 N7 121.5(5) . . ?
N8 C29 N9 119.3(5) . . ?
N7 C29 N9 119.2(5) . . ?
C29 N9 N10 117.9(4) . . ?
N12 C30 N13 121.5(5) . . ?
N12 C30 N11 121.2(5) . . ?
N13 C30 N11 117.3(5) . . ?
C30 N13 N14 116.8(4) . . ?

_refine_diff_density_max         3.210
_refine_diff_density_min         -1.988
_refine_diff_density_rms         0.207

####################################################################### 
# 
# 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_ggdegtaa
_database_code_depnum_ccdc_archive 'CCDC 1882460'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H32 Gd N5 O13'
_chemical_formula_weight         647.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.842(2)
_cell_length_b                   9.2670(10)
_cell_length_c                   16.890(2)
_cell_angle_alpha                90
_cell_angle_beta                 119.87(2)
_cell_angle_gamma                90
_cell_volume                     2285.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    26504
_cell_measurement_theta_min      3.2350
_cell_measurement_theta_max      36.8970

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_F_000             1300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.175
_exptl_absorpt_coefficient_mu    2.977
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.8b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35036
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.263
_diffrn_reflns_theta_max         36.865
_diffrn_reflns_theta_full        26.315
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10000
_reflns_number_gt                9384
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0683P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10000
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_restrained_S_all      1.213
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.78605(2) 0.23311(2) 0.55434(2) 0.00680(4) Uani 1 1 d . . . . .
O1 O 0.77506(9) -0.03398(18) 0.53454(10) 0.0120(3) Uani 1 1 d . . . . .
O2 O 0.93504(9) 0.11261(17) 0.59537(10) 0.0106(2) Uani 1 1 d . . . . .
O3 O 0.62821(10) 0.2048(2) 0.45551(10) 0.0126(3) Uani 1 1 d . . . . .
O4 O 0.48318(9) 0.1949(2) 0.42562(10) 0.0151(3) Uani 1 1 d . . . . .
O5 O 0.74547(9) 0.43967(18) 0.45540(10) 0.0129(3) Uani 1 1 d . . . . .
O6 O 0.78184(11) 0.6386(2) 0.40562(11) 0.0180(3) Uani 1 1 d . . . . .
O7 O 0.87695(9) 0.18598(18) 0.71562(9) 0.0116(3) Uani 1 1 d . . . . .
O8 O 0.88972(11) 0.21469(19) 0.85315(11) 0.0136(3) Uani 1 1 d . . . . .
O9 O 0.76589(9) 0.43637(17) 0.62758(10) 0.0125(3) Uani 1 1 d . . . . .
O10 O 0.81852(10) 0.64188(19) 0.70511(10) 0.0140(3) Uani 1 1 d . . . . .
N1 N 0.92032(10) 0.41425(19) 0.60379(11) 0.0086(3) Uani 1 1 d . . . . .
N2 N 0.69846(10) 0.1208(2) 0.63213(10) 0.0098(3) Uani 1 1 d . . . . .
C1 C 0.86083(13) -0.1109(2) 0.57904(14) 0.0137(3) Uani 1 1 d . . . . .
H1A H 0.852361 -0.208182 0.554948 0.016 Uiso 1 1 calc R U . . .
H1B H 0.883106 -0.116956 0.644106 0.016 Uiso 1 1 calc R U . . .
C2 C 0.92908(13) -0.0315(2) 0.56221(13) 0.0123(3) Uani 1 1 d . . . . .
H2A H 0.988405 -0.078378 0.594237 0.015 Uiso 1 1 calc R U . . .
H2B H 0.908965 -0.030347 0.497487 0.015 Uiso 1 1 calc R U . . .
C3 C 1.00143(12) 0.2018(2) 0.58839(14) 0.0113(3) Uani 1 1 d . . . . .
H3A H 0.981015 0.224160 0.524994 0.014 Uiso 1 1 calc R U . . .
H3B H 1.059972 0.152697 0.614288 0.014 Uiso 1 1 calc R U . . .
C4 C 1.00992(11) 0.3381(2) 0.64115(12) 0.0105(3) Uani 1 1 d . . . . .
H4A H 1.032306 0.314028 0.704698 0.013 Uiso 1 1 calc R U . . .
H4B H 1.054151 0.401902 0.638413 0.013 Uiso 1 1 calc R U . . .
C5 C 0.70603(13) -0.0988(2) 0.55071(13) 0.0126(3) Uani 1 1 d . . . . .
H5A H 0.714305 -0.202592 0.556061 0.015 Uiso 1 1 calc R U . . .
H5B H 0.645606 -0.078640 0.499574 0.015 Uiso 1 1 calc R U . . .
C6 C 0.71362(13) -0.0387(2) 0.63729(13) 0.0123(3) Uani 1 1 d . . . . .
H6A H 0.668838 -0.085653 0.648719 0.015 Uiso 1 1 calc R U . . .
H6B H 0.773960 -0.060183 0.688154 0.015 Uiso 1 1 calc R U . . .
C7 C 0.74022(12) 0.1777(2) 0.72592(13) 0.0118(3) Uani 1 1 d . . . . .
H7A H 0.726656 0.113322 0.762906 0.014 Uiso 1 1 calc R U . . .
H7B H 0.713949 0.271321 0.724950 0.014 Uiso 1 1 calc R U . . .
C8 C 0.60005(12) 0.1565(2) 0.57903(13) 0.0122(3) Uani 1 1 d . . . . .
H8A H 0.588248 0.240630 0.605749 0.015 Uiso 1 1 calc R U . . .
H8B H 0.564965 0.076752 0.583164 0.015 Uiso 1 1 calc R U . . .
C9 C 0.56757(12) 0.1867(2) 0.47882(13) 0.0102(3) Uani 1 1 d . . . . .
C10 C 0.90353(12) 0.5007(2) 0.52280(12) 0.0107(3) Uani 1 1 d . . . . .
H10A H 0.928979 0.449794 0.490360 0.013 Uiso 1 1 calc R U . . .
H10B H 0.935631 0.591976 0.543472 0.013 Uiso 1 1 calc R U . . .
C11 C 0.84397(12) 0.1926(2) 0.76857(12) 0.0095(3) Uani 1 1 d . . . . .
C12 C 0.82732(12) 0.5323(2) 0.66722(12) 0.0098(3) Uani 1 1 d . . . . .
C13 C 0.80207(12) 0.5310(2) 0.45653(12) 0.0103(3) Uani 1 1 d . . . . .
C14 C 0.92080(11) 0.5083(2) 0.67496(12) 0.0107(3) Uani 1 1 d . . . . .
H14A H 0.945824 0.601385 0.672590 0.013 Uiso 1 1 calc R U . . .
H14B H 0.961607 0.466270 0.734251 0.013 Uiso 1 1 calc R U . . .
C50 C 0.47575(14) 0.0912(3) 0.20853(15) 0.0172(4) Uani 1 1 d . . . . .
N51 N 0.56631(13) 0.1017(3) 0.26456(14) 0.0232(4) Uani 1 1 d . . . . .
H51A H 0.603383 0.073508 0.246551 0.028 Uiso 1 1 calc R U . . .
H51B H 0.587398 0.136627 0.318534 0.028 Uiso 1 1 calc R U . . .
N52 N 0.44330(14) 0.0374(3) 0.12544(15) 0.0282(5) Uani 1 1 d . . . . .
H52A H 0.385151 0.033000 0.088902 0.034 Uiso 1 1 calc R U . . .
H52B H 0.480366 0.006917 0.108000 0.034 Uiso 1 1 calc R U . . .
N53 N 0.41790(12) 0.1380(3) 0.23480(12) 0.0193(4) Uani 1 1 d . . . . .
H53A H 0.359830 0.133290 0.197918 0.023 Uiso 1 1 calc R U . . .
H53B H 0.438519 0.173086 0.288682 0.023 Uiso 1 1 calc R U . . .
OW1 O 0.78421(10) 0.16725(19) 0.41430(10) 0.0131(3) Uani 1 1 d . . . . .
HW11 H 0.785347 0.073930 0.409523 0.020 Uiso 1 1 d R U . . .
HW12 H 0.831642 0.203162 0.413770 0.020 Uiso 1 1 d R U . . .
OW2 O 0.75028(13) -0.0887(2) 0.32349(12) 0.0203(3) Uani 1 1 d . . . . .
HW21 H 0.761(3) -0.169(5) 0.350(3) 0.030 Uiso 1 1 d . U . . .
HW22 H 0.770(2) -0.108(4) 0.282(2) 0.030 Uiso 1 1 d . U . . .
OW3 O 0.59817(14) 0.5265(3) 0.6028(2) 0.0359(5) Uani 1 1 d . . . . .
HW31 H 0.586(3) 0.591(5) 0.588(3) 0.054 Uiso 1 1 d . U . . .
HW32 H 0.648(3) 0.510(5) 0.605(3) 0.054 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O3 2.3457(16) . ?
Gd O9 2.3689(15) . ?
Gd O5 2.4055(15) . ?
Gd O7 2.4086(15) . ?
Gd OW1 2.4279(14) . ?
Gd O1 2.4921(17) . ?
Gd O2 2.5083(14) . ?
Gd N1 2.5976(17) . ?
Gd N2 2.6300(16) . ?
O1 C1 1.442(2) . ?
O1 C5 1.450(2) . ?
O2 C2 1.433(3) . ?
O2 C3 1.442(2) . ?
O3 C9 1.275(2) . ?
O4 C9 1.249(2) . ?
O5 C13 1.268(2) . ?
O6 C13 1.248(3) . ?
O7 C11 1.268(2) . ?
O8 C11 1.257(2) . ?
O9 C12 1.272(2) . ?
O10 C12 1.248(3) . ?
N1 C14 1.481(2) . ?
N1 C10 1.486(2) . ?
N1 C4 1.492(2) . ?
N2 C7 1.474(3) . ?
N2 C8 1.476(2) . ?
N2 C6 1.495(3) . ?
C1 C2 1.506(3) . ?
C3 C4 1.511(3) . ?
C5 C6 1.509(3) . ?
C7 C11 1.529(2) . ?
C8 C9 1.523(3) . ?
C10 C13 1.532(3) . ?
C12 C14 1.530(2) . ?
C50 N52 1.324(3) . ?
C50 N53 1.329(3) . ?
C50 N51 1.339(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
O3 Gd O9 93.11(5) . . ?
O3 Gd O5 76.43(5) . . ?
O9 Gd O5 70.43(6) . . ?
O3 Gd O7 129.89(5) . . ?
O9 Gd O7 74.29(5) . . ?
O5 Gd O7 136.94(6) . . ?
O3 Gd OW1 79.54(6) . . ?
O9 Gd OW1 140.62(6) . . ?
O5 Gd OW1 70.24(6) . . ?
O7 Gd OW1 138.49(5) . . ?
O3 Gd O1 79.13(5) . . ?
O9 Gd O1 147.08(5) . . ?
O5 Gd O1 136.11(5) . . ?
O7 Gd O1 86.25(5) . . ?
OW1 Gd O1 69.85(5) . . ?
O3 Gd O2 140.36(6) . . ?
O9 Gd O2 126.41(5) . . ?
O5 Gd O2 116.44(5) . . ?
O7 Gd O2 67.79(5) . . ?
OW1 Gd O2 71.51(5) . . ?
O1 Gd O2 65.93(5) . . ?
O3 Gd N1 142.91(6) . . ?
O9 Gd N1 69.30(5) . . ?
O5 Gd N1 67.03(5) . . ?
O7 Gd N1 78.02(5) . . ?
OW1 Gd N1 93.58(5) . . ?
O1 Gd N1 132.81(5) . . ?
O2 Gd N1 66.92(5) . . ?
O3 Gd N2 65.94(5) . . ?
O9 Gd N2 77.99(5) . . ?
O5 Gd N2 128.76(5) . . ?
O7 Gd N2 64.02(5) . . ?
OW1 Gd N2 130.47(5) . . ?
O1 Gd N2 69.60(5) . . ?
O2 Gd N2 114.75(5) . . ?
N1 Gd N2 135.25(5) . . ?
C1 O1 C5 112.72(16) . . ?
C1 O1 Gd 115.66(12) . . ?
C5 O1 Gd 113.50(12) . . ?
C2 O2 C3 114.12(14) . . ?
C2 O2 Gd 116.20(11) . . ?
C3 O2 Gd 115.60(12) . . ?
C9 O3 Gd 126.36(13) . . ?
C13 O5 Gd 124.71(12) . . ?
C11 O7 Gd 122.29(11) . . ?
C12 O9 Gd 122.68(11) . . ?
C14 N1 C10 110.58(16) . . ?
C14 N1 C4 109.84(14) . . ?
C10 N1 C4 109.46(14) . . ?
C14 N1 Gd 107.04(10) . . ?
C10 N1 Gd 108.45(11) . . ?
C4 N1 Gd 111.45(12) . . ?
C7 N2 C8 111.30(15) . . ?
C7 N2 C6 108.37(16) . . ?
C8 N2 C6 111.36(15) . . ?
C7 N2 Gd 108.00(11) . . ?
C8 N2 Gd 110.31(11) . . ?
C6 N2 Gd 107.35(10) . . ?
O1 C1 C2 108.72(17) . . ?
O2 C2 C1 107.03(15) . . ?
O2 C3 C4 106.29(15) . . ?
N1 C4 C3 111.55(15) . . ?
O1 C5 C6 109.92(16) . . ?
N2 C6 C5 112.26(16) . . ?
N2 C7 C11 111.12(14) . . ?
N2 C8 C9 112.93(15) . . ?
O4 C9 O3 124.67(18) . . ?
O4 C9 C8 117.44(16) . . ?
O3 C9 C8 117.87(16) . . ?
N1 C10 C13 113.77(14) . . ?
O8 C11 O7 125.01(17) . . ?
O8 C11 C7 117.39(16) . . ?
O7 C11 C7 117.57(16) . . ?
O10 C12 O9 124.43(16) . . ?
O10 C12 C14 117.05(17) . . ?
O9 C12 C14 118.39(17) . . ?
O6 C13 O5 125.29(17) . . ?
O6 C13 C10 118.18(17) . . ?
O5 C13 C10 116.45(17) . . ?
N1 C14 C12 115.27(15) . . ?
N52 C50 N53 119.52(19) . . ?
N52 C50 N51 120.0(2) . . ?
N53 C50 N51 120.5(2) . . ?

_refine_diff_density_max         1.757
_refine_diff_density_min         -3.239
_refine_diff_density_rms         0.218

####################################################################### 
# 
# 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_lucdtaa
_database_code_depnum_ccdc_archive 'CCDC 1882456'
_audit_update_record             
;
2019-01-26 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H67 Lu2 N10 O24'
_chemical_formula_weight         1301.87

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.392(2)
_cell_length_b                   16.491(4)
_cell_length_c                   16.752(4)
_cell_angle_alpha                88.53(2)
_cell_angle_beta                 83.24(2)
_cell_angle_gamma                83.52(2)
_cell_volume                     2287.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12069
_cell_measurement_theta_min      2.4439
_cell_measurement_theta_max      36.5814

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_F_000             1302
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.079
_exptl_absorpt_coefficient_mu    4.386
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.335
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.8b (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16242
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.871
_diffrn_reflns_theta_max         36.649
_diffrn_reflns_theta_full        26.3154
_diffrn_measured_fraction_theta_max 0.440
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.440
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.440
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             9993
_reflns_number_gt                8915
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    
'G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122.'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
DIAMOND-Visual Crystal Structure Information System, 	CRYSTALIMPACT, Postfach 1251, 53002 Bonn, Germany
;
_computing_publication_material  cifpub
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0874P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9993
_refine_ls_number_parameters     659
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.85057(2) 0.41031(2) 0.27160(2) 0.00900(8) Uani 1 1 d . . . . .
O1 O 0.7693(4) 0.4393(2) 0.4031(2) 0.0140(7) Uani 1 1 d . . . . .
O2 O 0.6945(5) 0.5370(2) 0.4935(2) 0.0168(8) Uani 1 1 d . . . . .
O3 O 0.6421(4) 0.35579(19) 0.2282(2) 0.0130(7) Uani 1 1 d . . . . .
O4 O 0.3783(4) 0.3507(2) 0.2291(2) 0.0182(7) Uani 1 1 d . . . . .
O5 O 0.9370(4) 0.5358(2) 0.2705(2) 0.0130(7) Uani 1 1 d . . . . .
O6 O 0.9776(5) 0.6539(2) 0.2079(2) 0.0194(8) Uani 1 1 d . . . . .
O7 O 1.0044(4) 0.34934(19) 0.1645(2) 0.0134(7) Uani 1 1 d . . . . .
O8 O 1.0635(5) 0.32972(19) 0.0327(2) 0.0175(7) Uani 1 1 d . . . . .
OW11 O 1.0999(4) 0.3868(2) 0.3181(2) 0.0158(7) Uani 1 1 d D . . . .
H111 H 1.192(5) 0.369(5) 0.287(3) 0.07(3) Uiso 1 1 d D . . . .
H112 H 1.115(8) 0.367(4) 0.3677(16) 0.07(3) Uiso 1 1 d D . . . .
OW12 O 0.8493(4) 0.2832(2) 0.3334(2) 0.0153(7) Uani 1 1 d D . . . .
H121 H 0.749(2) 0.269(3) 0.343(4) 0.032(19) Uiso 1 1 d D . . . .
H122 H 0.914(5) 0.2358(16) 0.330(5) 0.04(2) Uiso 1 1 d D . . . .
N1 N 0.5935(5) 0.5096(2) 0.2917(2) 0.0091(8) Uani 1 1 d . . . . .
N2 N 0.8008(5) 0.4846(2) 0.1418(2) 0.0115(8) Uani 1 1 d . . . . .
C1 C 0.6921(6) 0.5079(3) 0.4270(3) 0.0115(9) Uani 1 1 d . . . . .
C2 C 0.5973(6) 0.5565(3) 0.3663(3) 0.0123(10) Uani 1 1 d . . . . .
H2A H 0.487590 0.571510 0.390630 0.015 Uiso 1 1 calc R U . . .
H2B H 0.645819 0.606371 0.352262 0.015 Uiso 1 1 calc R U . . .
C3 C 0.4674(6) 0.4534(3) 0.3064(3) 0.0124(9) Uani 1 1 d . . . . .
H3A H 0.363247 0.483338 0.299817 0.015 Uiso 1 1 calc R U . . .
H3B H 0.463638 0.433418 0.361420 0.015 Uiso 1 1 calc R U . . .
C4 C 0.4962(6) 0.3816(3) 0.2503(3) 0.0143(10) Uani 1 1 d . . . . .
C5 C 0.5713(6) 0.5681(3) 0.2221(3) 0.0141(9) Uani 1 1 d . . . . .
H5 H 0.639298 0.611662 0.227682 0.017 Uiso 1 1 calc R U . . .
C6 C 0.3979(6) 0.6091(3) 0.2223(3) 0.0177(10) Uani 1 1 d . . . . .
H61 H 0.363730 0.636367 0.273105 0.021 Uiso 1 1 calc R U . . .
H62 H 0.326010 0.567989 0.216807 0.021 Uiso 1 1 calc R U . . .
C7 C 0.3875(7) 0.6715(3) 0.1530(3) 0.0210(11) Uani 1 1 d . . . . .
H71 H 0.277972 0.697983 0.154398 0.025 Uiso 1 1 calc R U . . .
H72 H 0.458519 0.712946 0.158549 0.025 Uiso 1 1 calc R U . . .
C8 C 0.4365(6) 0.6280(3) 0.0736(3) 0.0209(11) Uani 1 1 d . . . . .
H81 H 0.427916 0.666717 0.029399 0.025 Uiso 1 1 calc R U . . .
H82 H 0.365240 0.586614 0.067964 0.025 Uiso 1 1 calc R U . . .
C9 C 0.6111(6) 0.5881(3) 0.0716(3) 0.0195(11) Uani 1 1 d . . . . .
H91 H 0.681956 0.630258 0.074533 0.023 Uiso 1 1 calc R U . . .
H92 H 0.642415 0.560223 0.020955 0.023 Uiso 1 1 calc R U . . .
C10 C 0.6327(6) 0.5269(3) 0.1411(3) 0.0129(9) Uani 1 1 d . . . . .
H10 H 0.562690 0.484305 0.134844 0.015 Uiso 1 1 calc R U . . .
C11 C 0.9274(6) 0.5421(3) 0.1305(3) 0.0122(9) Uani 1 1 d . . . . .
H11A H 0.898235 0.583669 0.091155 0.015 Uiso 1 1 calc R U . . .
H11B H 1.029467 0.512338 0.109456 0.015 Uiso 1 1 calc R U . . .
C12 C 0.9479(6) 0.5826(3) 0.2077(3) 0.0132(10) Uani 1 1 d . . . . .
C13 C 0.8367(6) 0.4249(3) 0.0763(3) 0.0133(10) Uani 1 1 d . . . . .
H13A H 0.861072 0.453398 0.025657 0.016 Uiso 1 1 calc R U . . .
H13B H 0.742622 0.396720 0.072430 0.016 Uiso 1 1 calc R U . . .
C14 C 0.9796(6) 0.3630(3) 0.0910(3) 0.0140(10) Uani 1 1 d . . . . .
Lu2 Lu 1.20302(2) 0.08703(2) 0.23585(2) 0.00951(8) Uani 1 1 d . . . . .
O9 O 1.0784(4) 0.15210(19) 0.3493(2) 0.0137(7) Uani 1 1 d . . . . .
O10 O 1.0715(5) 0.1773(2) 0.4804(2) 0.0170(8) Uani 1 1 d . . . . .
O11 O 0.9891(5) -0.1371(2) 0.2990(2) 0.0201(8) Uani 1 1 d . . . . .
O12 O 1.0739(4) -0.0264(2) 0.2364(2) 0.0135(7) Uani 1 1 d . . . . .
O13 O 1.4316(4) 0.1215(2) 0.2769(2) 0.0152(7) Uani 1 1 d . . . . .
O14 O 1.6914(4) 0.0896(2) 0.2907(2) 0.0218(8) Uani 1 1 d . . . . .
O15 O 1.2671(4) 0.0618(2) 0.1026(2) 0.0143(7) Uani 1 1 d . . . . .
O16 O 1.3211(4) -0.0298(2) 0.0047(2) 0.0166(8) Uani 1 1 d . . . . .
OW21 O 0.9554(4) 0.1276(2) 0.1947(2) 0.0187(8) Uani 1 1 d D . . . .
H211 H 0.874(5) 0.110(3) 0.228(3) 0.04(2) Uiso 1 1 d D . . . .
H212 H 0.910(6) 0.171(3) 0.168(4) 0.07(3) Uiso 1 1 d D . . . .
OW22 O 1.2325(4) 0.2182(2) 0.1829(2) 0.0155(7) Uani 1 1 d D . . . .
H221 H 1.316(5) 0.242(3) 0.198(4) 0.05(2) Uiso 1 1 d D . . . .
H222 H 1.159(4) 0.2604(19) 0.173(4) 0.023(17) Uiso 1 1 d D . . . .
N3 N 1.2387(5) 0.0023(2) 0.3634(2) 0.0126(8) Uani 1 1 d . . . . .
N4 N 1.4263(5) -0.0286(2) 0.2086(2) 0.0127(8) Uani 1 1 d . . . . .
C15 C 1.1198(6) 0.1361(3) 0.4196(3) 0.0125(9) Uani 1 1 d . . . . .
C16 C 1.2375(6) 0.0607(3) 0.4295(3) 0.0139(10) Uani 1 1 d . . . . .
H16A H 1.345123 0.076651 0.430058 0.017 Uiso 1 1 calc R U . . .
H16B H 1.207453 0.034188 0.480574 0.017 Uiso 1 1 calc R U . . .
C17 C 1.0880(6) -0.0381(3) 0.3766(3) 0.0146(10) Uani 1 1 d . . . . .
H17A H 0.999629 0.000942 0.398536 0.018 Uiso 1 1 calc R U . . .
H17B H 1.101171 -0.082220 0.415544 0.018 Uiso 1 1 calc R U . . .
C18 C 1.0464(6) -0.0721(3) 0.2990(3) 0.0139(10) Uani 1 1 d . . . . .
C19 C 1.3900(6) -0.0559(3) 0.3571(3) 0.0149(10) Uani 1 1 d . . . . .
H19 H 1.478447 -0.023981 0.365081 0.018 Uiso 1 1 calc R U . . .
C20 C 1.3903(7) -0.1243(3) 0.4214(3) 0.0195(11) Uani 1 1 d . . . . .
H20A H 1.370625 -0.100158 0.474333 0.023 Uiso 1 1 calc R U . . .
H20B H 1.303400 -0.157015 0.415650 0.023 Uiso 1 1 calc R U . . .
C21 C 1.5515(7) -0.1795(3) 0.4143(3) 0.0263(13) Uani 1 1 d . . . . .
H21A H 1.638485 -0.147604 0.422318 0.032 Uiso 1 1 calc R U . . .
H21B H 1.547558 -0.222011 0.455304 0.032 Uiso 1 1 calc R U . . .
C22 C 1.5826(7) -0.2175(3) 0.3319(3) 0.0215(11) Uani 1 1 d . . . . .
H22A H 1.496917 -0.250337 0.324217 0.026 Uiso 1 1 calc R U . . .
H22B H 1.683929 -0.252641 0.327187 0.026 Uiso 1 1 calc R U . . .
C23 C 1.5897(6) -0.1500(3) 0.2680(3) 0.0149(10) Uani 1 1 d . . . . .
H23A H 1.611126 -0.174128 0.215119 0.018 Uiso 1 1 calc R U . . .
H23B H 1.677487 -0.118260 0.275114 0.018 Uiso 1 1 calc R U . . .
C24 C 1.4296(6) -0.0933(2) 0.2736(3) 0.0111(9) Uani 1 1 d . . . . .
H24 H 1.344139 -0.127401 0.266538 0.013 Uiso 1 1 calc R U . . .
C25 C 1.4086(7) -0.0672(3) 0.1316(3) 0.0160(10) Uani 1 1 d . . . . .
H25A H 1.345040 -0.112652 0.142473 0.019 Uiso 1 1 calc R U . . .
H25B H 1.514433 -0.088537 0.106290 0.019 Uiso 1 1 calc R U . . .
C26 C 1.3277(6) -0.0076(3) 0.0738(3) 0.0128(10) Uani 1 1 d . . . . .
C27 C 1.5732(6) 0.0144(3) 0.1974(3) 0.0143(10) Uani 1 1 d . . . . .
H27A H 1.582720 0.039481 0.144255 0.017 Uiso 1 1 calc R U . . .
H27B H 1.667460 -0.024813 0.200716 0.017 Uiso 1 1 calc R U . . .
C28 C 1.5688(6) 0.0790(3) 0.2595(3) 0.0160(10) Uani 1 1 d . . . . .
OW1 O 1.4787(5) -0.1834(2) -0.0377(2) 0.0232(8) Uani 1 1 d D . . . .
HW11 H 1.579(4) -0.186(4) -0.064(5) 0.08(3) Uiso 1 1 d D . . . .
HW12 H 1.455(8) -0.1308(13) -0.023(4) 0.07(3) Uiso 1 1 d D . . . .
OW2 O 0.7601(4) 0.2331(2) 0.1195(2) 0.0181(7) Uani 1 1 d D . . . .
HW21 H 0.704(5) 0.269(4) 0.155(4) 0.10(4) Uiso 1 1 d D . . . .
HW22 H 0.685(4) 0.212(3) 0.095(3) 0.010(13) Uiso 1 1 d D . . . .
OW3 O 1.2498(5) 0.3178(2) 0.4435(2) 0.0202(8) Uani 1 1 d D . . . .
HW31 H 1.265(8) 0.356(2) 0.479(2) 0.036(19) Uiso 1 1 d D . . . .
HW32 H 1.231(11) 0.273(2) 0.474(3) 0.10(3) Uiso 1 1 d D . . . .
OW4 O 0.5623(6) 0.2335(3) 0.3882(3) 0.0345(11) Uani 1 1 d D . . . .
HW41 H 0.541(7) 0.196(3) 0.354(3) 0.05(2) Uiso 1 1 d D . . . .
HW42 H 0.467(4) 0.263(3) 0.402(4) 0.06(3) Uiso 1 1 d D . . . .
N5 N 0.8500(5) 0.3199(2) 0.5202(3) 0.0157(9) Uani 1 1 d . . . . .
H5A H 0.797654 0.352613 0.489197 0.019 Uiso 1 1 calc R U . . .
H5B H 0.864476 0.268410 0.510723 0.019 Uiso 1 1 calc R U . . .
N6 N 0.8860(5) 0.4284(2) 0.5970(3) 0.0147(8) Uani 1 1 d . . . . .
H6A H 0.833576 0.461080 0.566019 0.018 Uiso 1 1 calc R U . . .
H6B H 0.923833 0.447168 0.637462 0.018 Uiso 1 1 calc R U . . .
N7 N 0.9890(5) 0.2985(3) 0.6314(3) 0.0180(9) Uani 1 1 d . . . . .
H7A H 1.003406 0.246896 0.622599 0.022 Uiso 1 1 calc R U . . .
H7B H 1.026512 0.317778 0.671708 0.022 Uiso 1 1 calc R U . . .
C29 C 0.9084(6) 0.3487(3) 0.5824(3) 0.0134(9) Uani 1 1 d . . . . .
N8 N 0.8834(6) -0.1643(3) 0.0134(3) 0.0221(10) Uani 1 1 d . . . . .
H8A H 0.842811 -0.130398 -0.020622 0.027 Uiso 1 1 calc R U . . .
H8B H 0.888994 -0.215969 0.005564 0.027 Uiso 1 1 calc R U . . .
N9 N 0.9290(5) -0.0571(2) 0.0899(3) 0.0156(9) Uani 1 1 d . . . . .
H9A H 0.961940 -0.039159 0.132066 0.019 Uiso 1 1 calc R U . . .
H9B H 0.890190 -0.023367 0.055190 0.019 Uiso 1 1 calc R U . . .
N10 N 0.9982(5) -0.1886(3) 0.1323(3) 0.0187(9) Uani 1 1 d . . . . .
H10A H 1.030980 -0.170260 0.174406 0.022 Uiso 1 1 calc R U . . .
H10B H 1.004369 -0.240392 0.125155 0.022 Uiso 1 1 calc R U . . .
C30 C 0.9379(6) -0.1368(3) 0.0782(3) 0.0146(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O3 2.255(3) . ?
Lu1 O5 2.267(3) . ?
Lu1 O7 2.270(3) . ?
Lu1 O1 2.275(4) . ?
Lu1 OW11 2.307(3) . ?
Lu1 OW12 2.314(3) . ?
Lu1 N2 2.523(4) . ?
Lu1 N1 2.552(4) . ?
O1 C1 1.287(6) . ?
O2 C1 1.226(6) . ?
O3 C4 1.265(6) . ?
O4 C4 1.254(6) . ?
O5 C12 1.289(6) . ?
O6 C12 1.229(6) . ?
O7 C14 1.283(6) . ?
O8 C14 1.235(6) . ?
N1 C3 1.480(6) . ?
N1 C2 1.490(6) . ?
N1 C5 1.508(6) . ?
N2 C13 1.474(6) . ?
N2 C11 1.495(6) . ?
N2 C10 1.502(6) . ?
C1 C2 1.521(6) . ?
C3 C4 1.510(7) . ?
C5 C6 1.533(7) . ?
C5 C10 1.541(7) . ?
C6 C7 1.535(7) . ?
C7 C8 1.518(7) . ?
C8 C9 1.533(7) . ?
C9 C10 1.535(6) . ?
C11 C12 1.508(7) . ?
C13 C14 1.524(7) . ?
Lu2 O13 2.248(3) . ?
Lu2 O12 2.264(3) . ?
Lu2 O15 2.271(4) . ?
Lu2 O9 2.289(3) . ?
Lu2 OW21 2.289(4) . ?
Lu2 OW22 2.344(3) . ?
Lu2 N4 2.529(4) . ?
Lu2 N3 2.551(4) . ?
O9 C15 1.280(6) . ?
O10 C15 1.240(6) . ?
O11 C18 1.223(6) . ?
O12 C18 1.289(6) . ?
O13 C28 1.285(6) . ?
O14 C28 1.239(6) . ?
O15 C26 1.281(6) . ?
O16 C26 1.232(6) . ?
N3 C16 1.484(6) . ?
N3 C17 1.487(6) . ?
N3 C19 1.498(6) . ?
N4 C27 1.481(6) . ?
N4 C25 1.483(6) . ?
N4 C24 1.505(6) . ?
C15 C16 1.517(6) . ?
C17 C18 1.521(7) . ?
C19 C24 1.529(7) . ?
C19 C20 1.539(6) . ?
C20 C21 1.537(7) . ?
C21 C22 1.512(7) . ?
C22 C23 1.525(6) . ?
C23 C24 1.543(6) . ?
C25 C26 1.522(7) . ?
C27 C28 1.503(7) . ?
N5 C29 1.324(6) . ?
N6 C29 1.330(6) . ?
N7 C29 1.337(6) . ?
N8 C30 1.335(7) . ?
N9 C30 1.327(6) . ?
N10 C30 1.334(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Lu1 O5 136.26(12) . . ?
O3 Lu1 O7 86.26(12) . . ?
O5 Lu1 O7 102.82(13) . . ?
O3 Lu1 O1 104.89(13) . . ?
O5 Lu1 O1 82.87(12) . . ?
O7 Lu1 O1 157.42(12) . . ?
O3 Lu1 OW11 147.02(12) . . ?
O5 Lu1 OW11 76.07(12) . . ?
O7 Lu1 OW11 78.17(13) . . ?
O1 Lu1 OW11 82.16(13) . . ?
O3 Lu1 OW12 74.78(12) . . ?
O5 Lu1 OW12 146.87(13) . . ?
O7 Lu1 OW12 88.24(12) . . ?
O1 Lu1 OW12 76.22(12) . . ?
OW11 Lu1 OW12 75.85(13) . . ?
O3 Lu1 N2 74.50(13) . . ?
O5 Lu1 N2 69.82(13) . . ?
O7 Lu1 N2 68.33(12) . . ?
O1 Lu1 N2 133.20(12) . . ?
OW11 Lu1 N2 124.13(13) . . ?
OW12 Lu1 N2 142.21(13) . . ?
O3 Lu1 N1 69.35(12) . . ?
O5 Lu1 N1 74.97(12) . . ?
O7 Lu1 N1 135.51(12) . . ?
O1 Lu1 N1 67.03(12) . . ?
OW11 Lu1 N1 139.73(13) . . ?
OW12 Lu1 N1 118.20(12) . . ?
N2 Lu1 N1 69.51(13) . . ?
C1 O1 Lu1 123.4(3) . . ?
C4 O3 Lu1 122.7(3) . . ?
C12 O5 Lu1 123.7(3) . . ?
C14 O7 Lu1 124.5(3) . . ?
C3 N1 C2 109.0(4) . . ?
C3 N1 C5 113.9(4) . . ?
C2 N1 C5 109.6(3) . . ?
C3 N1 Lu1 101.9(2) . . ?
C2 N1 Lu1 108.1(3) . . ?
C5 N1 Lu1 114.0(3) . . ?
C13 N2 C11 107.3(4) . . ?
C13 N2 C10 109.9(4) . . ?
C11 N2 C10 112.9(3) . . ?
C13 N2 Lu1 107.9(3) . . ?
C11 N2 Lu1 104.0(3) . . ?
C10 N2 Lu1 114.4(3) . . ?
O2 C1 O1 124.5(4) . . ?
O2 C1 C2 118.9(4) . . ?
O1 C1 C2 116.5(4) . . ?
N1 C2 C1 112.3(4) . . ?
N1 C3 C4 112.8(4) . . ?
O4 C4 O3 123.9(4) . . ?
O4 C4 C3 119.8(4) . . ?
O3 C4 C3 116.4(4) . . ?
N1 C5 C6 113.6(4) . . ?
N1 C5 C10 111.4(4) . . ?
C6 C5 C10 111.2(4) . . ?
C5 C6 C7 110.5(4) . . ?
C8 C7 C6 109.3(4) . . ?
C7 C8 C9 109.1(4) . . ?
C8 C9 C10 112.2(4) . . ?
N2 C10 C9 114.9(4) . . ?
N2 C10 C5 111.2(4) . . ?
C9 C10 C5 110.2(4) . . ?
N2 C11 C12 112.3(4) . . ?
O6 C12 O5 124.6(5) . . ?
O6 C12 C11 120.9(4) . . ?
O5 C12 C11 114.5(4) . . ?
N2 C13 C14 111.0(4) . . ?
O8 C14 O7 124.4(5) . . ?
O8 C14 C13 119.0(4) . . ?
O7 C14 C13 116.6(4) . . ?
O13 Lu2 O12 137.08(12) . . ?
O13 Lu2 O15 104.70(13) . . ?
O12 Lu2 O15 84.39(12) . . ?
O13 Lu2 O9 84.78(13) . . ?
O12 Lu2 O9 102.27(13) . . ?
O15 Lu2 O9 158.07(12) . . ?
O13 Lu2 OW21 148.58(13) . . ?
O12 Lu2 OW21 73.53(13) . . ?
O15 Lu2 OW21 81.67(13) . . ?
O9 Lu2 OW21 80.31(14) . . ?
O13 Lu2 OW22 74.34(13) . . ?
O12 Lu2 OW22 147.62(13) . . ?
O15 Lu2 OW22 78.11(12) . . ?
O9 Lu2 OW22 85.75(12) . . ?
OW21 Lu2 OW22 77.10(13) . . ?
O13 Lu2 N4 70.34(13) . . ?
O12 Lu2 N4 75.31(13) . . ?
O15 Lu2 N4 67.36(13) . . ?
O9 Lu2 N4 134.44(12) . . ?
OW21 Lu2 N4 137.67(14) . . ?
OW22 Lu2 N4 120.88(13) . . ?
O13 Lu2 N3 75.04(14) . . ?
O12 Lu2 N3 69.30(13) . . ?
O15 Lu2 N3 133.82(12) . . ?
O9 Lu2 N3 67.40(12) . . ?
OW21 Lu2 N3 122.81(14) . . ?
OW22 Lu2 N3 140.67(13) . . ?
N4 Lu2 N3 69.54(13) . . ?
C15 O9 Lu2 123.5(3) . . ?
C18 O12 Lu2 123.9(3) . . ?
C28 O13 Lu2 122.3(3) . . ?
C26 O15 Lu2 124.3(3) . . ?
C16 N3 C17 108.5(4) . . ?
C16 N3 C19 110.5(4) . . ?
C17 N3 C19 113.9(4) . . ?
C16 N3 Lu2 107.0(3) . . ?
C17 N3 Lu2 102.9(3) . . ?
C19 N3 Lu2 113.6(3) . . ?
C27 N4 C25 108.5(4) . . ?
C27 N4 C24 113.5(4) . . ?
C25 N4 C24 108.9(4) . . ?
C27 N4 Lu2 102.6(3) . . ?
C25 N4 Lu2 108.9(3) . . ?
C24 N4 Lu2 114.1(3) . . ?
O10 C15 O9 125.3(4) . . ?
O10 C15 C16 117.3(4) . . ?
O9 C15 C16 117.4(4) . . ?
N3 C16 C15 111.3(4) . . ?
N3 C17 C18 111.7(4) . . ?
O11 C18 O12 124.8(5) . . ?
O11 C18 C17 120.7(4) . . ?
O12 C18 C17 114.5(4) . . ?
N3 C19 C24 112.1(4) . . ?
N3 C19 C20 114.3(4) . . ?
C24 C19 C20 109.5(4) . . ?
C21 C20 C19 111.8(4) . . ?
C22 C21 C20 109.5(5) . . ?
C21 C22 C23 109.2(4) . . ?
C22 C23 C24 111.1(4) . . ?
N4 C24 C19 111.4(3) . . ?
N4 C24 C23 113.2(4) . . ?
C19 C24 C23 110.8(4) . . ?
N4 C25 C26 112.4(4) . . ?
O16 C26 O15 125.1(4) . . ?
O16 C26 C25 118.7(4) . . ?
O15 C26 C25 116.2(4) . . ?
N4 C27 C28 111.8(4) . . ?
O14 C28 O13 123.4(5) . . ?
O14 C28 C27 121.0(5) . . ?
O13 C28 C27 115.6(4) . . ?
N5 C29 N6 120.0(4) . . ?
N5 C29 N7 120.6(4) . . ?
N6 C29 N7 119.4(5) . . ?
N9 C30 N10 119.5(5) . . ?
N9 C30 N8 119.7(4) . . ?
N10 C30 N8 120.8(4) . . ?

_refine_diff_density_max         1.282
_refine_diff_density_min         -2.063
_refine_diff_density_rms         0.241

