# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

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

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1532662'
_audit_update_record             
;
2017-02-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 Cu Dy2 O24'
_chemical_formula_weight         1044.99

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   6.9551(8)
_cell_length_b                   10.5490(11)
_cell_length_c                   11.4502(12)
_cell_angle_alpha                109.409(4)
_cell_angle_beta                 99.928(4)
_cell_angle_gamma                98.943(4)
_cell_volume                     759.75(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    9725
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      28.34

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_F_000             505
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    5.661
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21325
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.055
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2667
_reflns_number_gt                2547
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+2.8483P] 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         2667
_refine_ls_number_parameters     238
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0566
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.047
_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
Dy1 Dy 0.64039(3) 0.70704(2) 0.09877(2) 0.01472(8) Uani 1 1 d . . . . .
Cu1 Cu 1.000000 1.000000 0.500000 0.02034(17) Uani 1 2 d S . P . .
O1 O 0.7306(5) 0.7452(3) 0.3182(3) 0.0281(7) Uani 1 1 d . . . . .
C1 C 0.6882(6) 0.7742(5) 0.4243(4) 0.0189(9) Uani 1 1 d . . . . .
O2 O 0.7810(5) 0.8792(3) 0.5200(3) 0.0283(7) Uani 1 1 d . . . . .
C2 C 0.5235(7) 0.6779(5) 0.4449(4) 0.0263(10) Uani 1 1 d . . . . .
H2A H 0.429757 0.624194 0.363448 0.032 Uiso 1 1 calc R U . . .
H2B H 0.582266 0.614143 0.475989 0.032 Uiso 1 1 calc R U . . .
O3 O 0.2346(5) 0.8080(4) 0.3724(3) 0.0345(8) Uani 1 1 d . . . . .
C3 C 0.4099(7) 0.7498(5) 0.5372(4) 0.0251(10) Uani 1 1 d . . . . .
O4 O 0.1890(5) 0.9041(3) 0.5664(3) 0.0268(7) Uani 1 1 d . . . . .
C4 C 0.2693(6) 0.8262(5) 0.4875(4) 0.0226(9) Uani 1 1 d . . . . .
O5 O 0.6393(5) 0.2626(3) 0.0559(3) 0.0243(7) Uani 1 1 d . . . . .
C5 C 0.4169(11) 0.7362(8) 0.6471(7) 0.0645(19) Uani 1 1 d . . . . .
H5A H 0.494331 0.680294 0.670679 0.077 Uiso 1 1 calc R U . . .
H5B H 0.344420 0.782341 0.701712 0.077 Uiso 1 1 calc R U . . .
O6 O 0.6130(4) 0.4753(3) 0.0940(3) 0.0201(6) Uani 1 1 d . . . . .
C6 C 0.7088(6) 0.3882(4) 0.1159(4) 0.0164(8) Uani 1 1 d . . . . .
O7 O 1.1374(5) 0.3994(3) 0.0331(3) 0.0264(7) Uani 1 1 d . . . . .
C7 C 0.9053(7) 0.4400(5) 0.2159(4) 0.0253(10) Uani 1 1 d . . . . .
H7A H 0.978209 0.524284 0.212237 0.030 Uiso 1 1 calc R U . . .
H7B H 0.877549 0.462156 0.299673 0.030 Uiso 1 1 calc R U . . .
O8 O 1.2320(5) 0.2225(3) 0.0625(3) 0.0253(7) Uani 1 1 d . . . . .
C8 C 1.0352(6) 0.3362(5) 0.1985(4) 0.0252(10) Uani 1 1 d . . . . .
O9 O 0.9688(5) 0.8544(4) 0.1965(3) 0.0283(7) Uani 1 1 d D . . . .
C9 C 1.1396(6) 0.3176(4) 0.0920(4) 0.0185(9) Uani 1 1 d . . . . .
H9A H 1.043(6) 0.887(5) 0.158(4) 0.022 Uiso 1 1 d D U . . .
H9B H 1.049(6) 0.845(5) 0.255(4) 0.022 Uiso 1 1 d D U . . .
O10 O 0.6011(5) 0.9334(4) 0.1844(3) 0.0362(9) Uani 1 1 d D . . . .
C10 C 1.0609(9) 0.2670(7) 0.2728(6) 0.0513(17) Uani 1 1 d . . . . .
H10A H 1.144457 0.205458 0.260018 0.062 Uiso 1 1 calc R U . . .
H10B H 0.995649 0.279105 0.338805 0.062 Uiso 1 1 calc R U . . .
H10C H 0.498(7) 0.963(7) 0.165(7) 0.062 Uiso 1 1 d D U . . .
H10D H 0.667(9) 0.985(6) 0.259(3) 0.062 Uiso 1 1 d D U . . .
O11 O 0.3331(5) 0.6683(3) 0.1563(3) 0.0264(7) Uani 1 1 d D . . . .
H11A H 0.247(6) 0.594(3) 0.127(5) 0.032 Uiso 1 1 d D U . . .
H11B H 0.308(8) 0.705(5) 0.227(3) 0.032 Uiso 1 1 d D U . . .
O12 O 0.2385(5) 0.9706(4) 0.0832(3) 0.0317(8) Uani 1 1 d D . . . .
H12A H 0.235(9) 1.042(4) 0.066(5) 0.038 Uiso 1 1 d D U . . .
H12B H 0.250(9) 0.923(5) 0.009(3) 0.038 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
Dy1 O10 2.340(3) . ?
Dy1 O11 2.358(3) . ?
Dy1 O1 2.361(3) . ?
Dy1 O9 2.397(3) . ?
Dy1 O6 2.404(3) . ?
Dy1 O8 2.454(3) 2_765 ?
Dy1 O7 2.480(3) 2_765 ?
Dy1 O5 2.531(3) 2_665 ?
Dy1 O6 2.542(3) 2_665 ?
Dy1 C9 2.843(4) 2_765 ?
Dy1 C6 2.914(4) 2_665 ?
Cu1 O2 1.925(3) . ?
Cu1 O2 1.925(3) 2_776 ?
Cu1 O4 1.977(3) 2_676 ?
Cu1 O4 1.977(3) 1_655 ?
O1 C1 1.249(5) . ?
C1 O2 1.254(6) . ?
C1 C2 1.513(6) . ?
C2 C3 1.503(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O3 C4 1.240(5) . ?
C3 C5 1.307(8) . ?
C3 C4 1.513(6) . ?
O4 C4 1.276(5) . ?
O5 C6 1.242(5) . ?
C5 H5A 0.9300 . ?
C5 H5B 0.9300 . ?
O6 C6 1.279(5) . ?
C6 C7 1.513(6) . ?
O7 C9 1.260(5) . ?
C7 C8 1.510(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
O8 C9 1.258(5) . ?
C8 C10 1.300(7) . ?
C8 C9 1.498(6) . ?
O9 H9A 0.84(2) . ?
O9 H9B 0.84(2) . ?
O10 H10C 0.85(2) . ?
O10 H10D 0.84(2) . ?
C10 H10A 0.9300 . ?
C10 H10B 0.9300 . ?
O11 H11A 0.83(2) . ?
O11 H11B 0.83(2) . ?
O12 H12A 0.84(2) . ?
O12 H12B 0.86(2) . ?

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
O10 Dy1 O11 79.22(13) . . ?
O10 Dy1 O1 80.38(13) . . ?
O11 Dy1 O1 75.10(11) . . ?
O10 Dy1 O9 72.63(12) . . ?
O11 Dy1 O9 137.29(11) . . ?
O1 Dy1 O9 69.10(11) . . ?
O10 Dy1 O6 152.77(13) . . ?
O11 Dy1 O6 79.05(11) . . ?
O1 Dy1 O6 78.33(11) . . ?
O9 Dy1 O6 114.46(11) . . ?
O10 Dy1 O8 85.91(13) . 2_765 ?
O11 Dy1 O8 138.12(11) . 2_765 ?
O1 Dy1 O8 140.50(11) . 2_765 ?
O9 Dy1 O8 71.46(11) . 2_765 ?
O6 Dy1 O8 121.30(10) . 2_765 ?
O10 Dy1 O7 133.23(13) . 2_765 ?
O11 Dy1 O7 145.25(11) . 2_765 ?
O1 Dy1 O7 116.70(11) . 2_765 ?
O9 Dy1 O7 74.25(11) . 2_765 ?
O6 Dy1 O7 72.37(10) . 2_765 ?
O8 Dy1 O7 52.44(10) 2_765 2_765 ?
O10 Dy1 O5 71.88(11) . 2_665 ?
O11 Dy1 O5 69.42(11) . 2_665 ?
O1 Dy1 O5 138.10(11) . 2_665 ?
O9 Dy1 O5 127.62(11) . 2_665 ?
O6 Dy1 O5 114.84(10) . 2_665 ?
O8 Dy1 O5 68.77(10) 2_765 2_665 ?
O7 Dy1 O5 105.16(11) 2_765 2_665 ?
O10 Dy1 O6 121.75(10) . 2_665 ?
O11 Dy1 O6 71.98(10) . 2_665 ?
O1 Dy1 O6 134.75(10) . 2_665 ?
O9 Dy1 O6 150.68(11) . 2_665 ?
O6 Dy1 O6 65.72(11) . 2_665 ?
O8 Dy1 O6 83.61(10) 2_765 2_665 ?
O7 Dy1 O6 78.42(10) 2_765 2_665 ?
O5 Dy1 O6 50.95(9) 2_665 2_665 ?
O10 Dy1 C9 110.25(14) . 2_765 ?
O11 Dy1 C9 150.10(11) . 2_765 ?
O1 Dy1 C9 133.51(11) . 2_765 ?
O9 Dy1 C9 71.52(11) . 2_765 ?
O6 Dy1 C9 96.73(11) . 2_765 ?
O8 Dy1 C9 26.18(11) 2_765 2_765 ?
O7 Dy1 C9 26.27(11) 2_765 2_765 ?
O5 Dy1 C9 86.26(11) 2_665 2_765 ?
O6 Dy1 C9 79.29(10) 2_665 2_765 ?
O10 Dy1 C6 96.00(12) . 2_665 ?
O11 Dy1 C6 66.41(11) . 2_665 ?
O1 Dy1 C6 141.28(11) . 2_665 ?
O9 Dy1 C6 146.69(11) . 2_665 ?
O6 Dy1 C6 90.16(11) . 2_665 ?
O8 Dy1 C6 76.66(11) 2_765 2_665 ?
O7 Dy1 C6 93.93(11) 2_765 2_665 ?
O5 Dy1 C6 25.12(11) 2_665 2_665 ?
O6 Dy1 C6 25.99(10) 2_665 2_665 ?
C9 Dy1 C6 84.14(11) 2_765 2_665 ?
O2 Cu1 O2 180.0 . 2_776 ?
O2 Cu1 O4 90.43(14) . 2_676 ?
O2 Cu1 O4 89.57(14) 2_776 2_676 ?
O2 Cu1 O4 89.57(14) . 1_655 ?
O2 Cu1 O4 90.43(14) 2_776 1_655 ?
O4 Cu1 O4 180.0 2_676 1_655 ?
C1 O1 Dy1 150.1(3) . . ?
O1 C1 O2 123.4(4) . . ?
O1 C1 C2 120.5(4) . . ?
O2 C1 C2 116.0(4) . . ?
C1 O2 Cu1 117.4(3) . . ?
C3 C2 C1 114.2(4) . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C5 C3 C2 122.5(5) . . ?
C5 C3 C4 122.3(5) . . ?
C2 C3 C4 114.9(4) . . ?
C4 O4 Cu1 117.6(3) . 1_455 ?
O3 C4 O4 123.4(4) . . ?
O3 C4 C3 118.8(4) . . ?
O4 C4 C3 117.8(4) . . ?
C6 O5 Dy1 95.0(2) . 2_665 ?
C3 C5 H5A 120.0 . . ?
C3 C5 H5B 120.0 . . ?
H5A C5 H5B 120.0 . . ?
C6 O6 Dy1 145.4(3) . . ?
C6 O6 Dy1 93.5(2) . 2_665 ?
Dy1 O6 Dy1 114.28(11) . 2_665 ?
O5 C6 O6 119.9(4) . . ?
O5 C6 C7 120.8(4) . . ?
O6 C6 C7 119.3(4) . . ?
O5 C6 Dy1 59.9(2) . 2_665 ?
O6 C6 Dy1 60.5(2) . 2_665 ?
C7 C6 Dy1 172.9(3) . 2_665 ?
C9 O7 Dy1 93.2(2) . 2_765 ?
C8 C7 C6 112.8(4) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C9 O8 Dy1 94.4(2) . 2_765 ?
C10 C8 C9 120.4(5) . . ?
C10 C8 C7 122.7(5) . . ?
C9 C8 C7 116.9(4) . . ?
Dy1 O9 H9A 125(3) . . ?
Dy1 O9 H9B 123(3) . . ?
H9A O9 H9B 104(5) . . ?
O8 C9 O7 119.9(4) . . ?
O8 C9 C8 120.5(4) . . ?
O7 C9 C8 119.5(4) . . ?
O8 C9 Dy1 59.4(2) . 2_765 ?
O7 C9 Dy1 60.6(2) . 2_765 ?
C8 C9 Dy1 176.4(3) . 2_765 ?
Dy1 O10 H10C 127(5) . . ?
Dy1 O10 H10D 119(5) . . ?
H10C O10 H10D 109(7) . . ?
C8 C10 H10A 120.0 . . ?
C8 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
Dy1 O11 H11A 126(4) . . ?
Dy1 O11 H11B 128(4) . . ?
H11A O11 H11B 101(5) . . ?
H12A O12 H12B 94(5) . . ?

_refine_diff_density_max         3.000
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.124

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

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1532661'
_audit_update_record             
;
2017-02-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 Cu La2 O24'
_chemical_formula_weight         997.81

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   7.0117(5)
_cell_length_b                   10.8073(9)
_cell_length_c                   11.6598(9)
_cell_angle_alpha                108.747(2)
_cell_angle_beta                 100.358(2)
_cell_angle_gamma                99.018(2)
_cell_volume                     800.92(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9940
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_F_000             487
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.372
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5786
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17757
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.035
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2825
_reflns_number_gt                2700
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²+0.9261P] 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         2825
_refine_ls_number_parameters     254
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0188
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0513
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.040
_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
La1 La 0.35318(2) 0.29090(2) 0.89576(2) 0.01627(7) Uani 1 1 d . . . . .
Cu1 Cu 0.000000 0.000000 0.500000 0.02199(12) Uani 1 2 d S . P . .
O1 O 0.3751(3) 0.5296(2) 0.90421(19) 0.0239(4) Uani 1 1 d . . . . .
C1 C 0.2860(4) 0.6182(3) 0.8856(3) 0.0182(6) Uani 1 1 d . . . . .
O2 O 0.3548(3) 0.7394(2) 0.9484(2) 0.0278(5) Uani 1 1 d . . . . .
C2 C 0.0964(4) 0.5733(3) 0.7825(3) 0.0278(7) Uani 1 1 d . . . . .
H2A H 0.130980 0.558739 0.702994 0.033 Uiso 1 1 calc R U . . .
H2B H 0.020927 0.488351 0.779095 0.033 Uiso 1 1 calc R U . . .
C3 C -0.0325(4) 0.6741(3) 0.8009(3) 0.0262(7) Uani 1 1 d . . . . .
O3 O -0.1235(4) 0.6082(2) 0.9633(2) 0.0322(5) Uani 1 1 d . . . . .
O4 O -0.2248(3) 0.7807(2) 0.9366(2) 0.0311(5) Uani 1 1 d . . . . .
C4 C -0.1314(4) 0.6892(3) 0.9065(3) 0.0217(6) Uani 1 1 d . . . . .
C5 C -0.0607(7) 0.7425(5) 0.7292(4) 0.0583(12) Uani 1 1 d . . . . .
H5A H -0.143525 0.802289 0.742795 0.070 Uiso 1 1 calc R U . . .
H5B H 0.001924 0.731969 0.663907 0.070 Uiso 1 1 calc R U . . .
O5 O 0.2636(3) 0.2501(2) 0.66951(19) 0.0316(5) Uani 1 1 d . . . . .
C6 C 0.3080(4) 0.2180(3) 0.5659(3) 0.0204(6) Uani 1 1 d . . . . .
O6 O 0.2185(3) 0.1131(2) 0.4748(2) 0.0301(5) Uani 1 1 d . . . . .
C7 C 0.4727(4) 0.3098(3) 0.5450(3) 0.0272(7) Uani 1 1 d . . . . .
O7 O 0.7619(4) 0.1894(3) 0.6241(2) 0.0381(6) Uani 1 1 d . . . . .
O8 O 0.8136(3) 0.0957(2) 0.43646(19) 0.0284(5) Uani 1 1 d . . . . .
C8 C 0.5887(5) 0.2417(3) 0.4569(3) 0.0285(7) Uani 1 1 d . . . . .
C9 C 0.7304(4) 0.1703(3) 0.5109(3) 0.0243(6) Uani 1 1 d . . . . .
O9 O 0.0126(3) 0.1339(2) 0.7951(2) 0.0320(5) Uani 1 1 d D . . . .
H9B H -0.066(5) 0.147(4) 0.740(3) 0.038 Uiso 1 1 d D U . . .
H9A H -0.057(5) 0.103(4) 0.836(3) 0.038 Uiso 1 1 d D U . . .
O10 O 0.3980(4) 0.0580(3) 0.8086(3) 0.0498(8) Uani 1 1 d D . . . .
H10D H 0.328(5) 0.008(4) 0.738(2) 0.060 Uiso 1 1 d D U . . .
H10C H 0.499(4) 0.030(4) 0.831(4) 0.060 Uiso 1 1 d D U . . .
C10B C 0.5265(12) 0.4295(8) 0.6090(8) 0.042(2) Uani 0.517(10) 1 d . . P A 1
H10F H 0.621(13) 0.488(9) 0.599(8) 0.050 Uiso 0.517(10) 1 d . U P A 1
H10E H 0.443(12) 0.465(8) 0.667(8) 0.050 Uiso 0.517(10) 1 d . U P A 1
C10A C 0.5855(10) 0.2556(7) 0.3492(6) 0.028(2) Uani 0.483(10) 1 d . . P A 2
H10A H 0.508991 0.309521 0.324159 0.034 Uiso 0.483(10) 1 calc R U P A 2
H10B H 0.659772 0.211439 0.297754 0.034 Uiso 0.483(10) 1 calc R U P A 2
O11 O 0.6794(3) 0.3393(2) 0.8385(2) 0.0331(5) Uani 1 1 d D . . . .
H11A H 0.772(5) 0.408(3) 0.875(3) 0.040 Uiso 1 1 d D U . . .
H11B H 0.708(6) 0.303(4) 0.772(2) 0.040 Uiso 1 1 d D U . . .
O12 O 0.7557(4) 0.0242(2) 0.9148(2) 0.0355(5) Uani 1 1 d D . . . .
H12A H 0.740(6) 0.074(4) 0.983(2) 0.043 Uiso 1 1 d D U . . .
H12B H 0.758(6) -0.052(3) 0.920(4) 0.043 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
La1 O5 2.473(2) . ?
La1 O10 2.487(2) . ?
La1 O11 2.520(2) . ?
La1 O1 2.529(2) . ?
La1 O9 2.530(2) . ?
La1 O4 2.573(2) 2_567 ?
La1 O3 2.614(2) 2_567 ?
La1 O2 2.619(2) 2_667 ?
La1 O1 2.677(2) 2_667 ?
La1 C4 2.976(3) 2_567 ?
La1 C1 3.026(3) 2_667 ?
Cu1 O6 1.932(2) . ?
Cu1 O6 1.932(2) 2_556 ?
Cu1 O8 1.974(2) 2_656 ?
Cu1 O8 1.974(2) 1_455 ?
O1 C1 1.275(3) . ?
C1 O2 1.243(4) . ?
C1 C2 1.516(4) . ?
C2 C3 1.510(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.292(5) . ?
C3 C4 1.495(4) . ?
O3 C4 1.258(4) . ?
O4 C4 1.263(4) . ?
C5 H5A 0.9300 . ?
C5 H5B 0.9300 . ?
O5 C6 1.256(4) . ?
C6 O6 1.254(4) . ?
C6 C7 1.508(4) . ?
C7 C10B 1.224(8) . ?
C7 C8 1.503(4) . ?
O7 C9 1.240(4) . ?
O8 C9 1.274(4) . ?
C8 C10A 1.308(7) . ?
C8 C9 1.519(4) . ?
O9 H9B 0.836(19) . ?
O9 H9A 0.841(19) . ?
O10 H10D 0.829(18) . ?
O10 H10C 0.840(18) . ?
C10B H10F 0.89(9) . ?
C10B H10E 1.00(9) . ?
C10A H10A 0.9300 . ?
C10A H10B 0.9300 . ?
O11 H11A 0.839(19) . ?
O11 H11B 0.826(19) . ?
O12 H12A 0.840(19) . ?
O12 H12B 0.846(19) . ?

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
O5 La1 O10 79.47(9) . . ?
O5 La1 O11 74.52(7) . . ?
O10 La1 O11 80.41(10) . . ?
O5 La1 O1 80.29(7) . . ?
O10 La1 O1 154.29(10) . . ?
O11 La1 O1 79.04(8) . . ?
O5 La1 O9 69.97(7) . . ?
O10 La1 O9 71.66(9) . . ?
O11 La1 O9 137.92(8) . . ?
O1 La1 O9 115.46(7) . . ?
O5 La1 O4 141.42(8) . 2_567 ?
O10 La1 O4 86.27(10) . 2_567 ?
O11 La1 O4 138.10(8) . 2_567 ?
O1 La1 O4 119.41(7) . 2_567 ?
O9 La1 O4 71.53(8) . 2_567 ?
O5 La1 O3 119.96(7) . 2_567 ?
O10 La1 O3 131.54(10) . 2_567 ?
O11 La1 O3 144.79(8) . 2_567 ?
O1 La1 O3 72.95(7) . 2_567 ?
O9 La1 O3 74.92(8) . 2_567 ?
O4 La1 O3 49.90(7) 2_567 2_567 ?
O5 La1 O2 136.14(7) . 2_667 ?
O10 La1 O2 71.37(7) . 2_667 ?
O11 La1 O2 68.95(8) . 2_667 ?
O1 La1 O2 114.58(7) . 2_667 ?
O9 La1 O2 126.77(7) . 2_667 ?
O4 La1 O2 69.14(7) 2_567 2_667 ?
O3 La1 O2 103.90(7) 2_567 2_667 ?
O5 La1 O1 135.71(7) . 2_667 ?
O10 La1 O1 119.32(7) . 2_667 ?
O11 La1 O1 70.46(7) . 2_667 ?
O1 La1 O1 67.27(7) . 2_667 ?
O9 La1 O1 151.26(7) . 2_667 ?
O4 La1 O1 82.36(7) 2_567 2_667 ?
O3 La1 O1 79.19(7) 2_567 2_667 ?
O2 La1 O1 48.88(6) 2_667 2_667 ?
O5 La1 C4 135.55(8) . 2_567 ?
O10 La1 C4 109.55(10) . 2_567 ?
O11 La1 C4 148.75(8) . 2_567 ?
O1 La1 C4 96.00(7) . 2_567 ?
O9 La1 C4 72.13(8) . 2_567 ?
O4 La1 C4 24.98(8) 2_567 2_567 ?
O3 La1 C4 24.94(8) 2_567 2_567 ?
O2 La1 C4 85.86(7) 2_667 2_567 ?
O1 La1 C4 79.13(7) 2_667 2_567 ?
O5 La1 C1 140.72(7) . 2_667 ?
O10 La1 C1 94.71(8) . 2_667 ?
O11 La1 C1 66.21(7) . 2_667 ?
O1 La1 C1 90.99(7) . 2_667 ?
O9 La1 C1 145.01(7) . 2_667 ?
O4 La1 C1 75.64(7) 2_567 2_667 ?
O3 La1 C1 93.05(7) 2_567 2_667 ?
O2 La1 C1 24.07(7) 2_667 2_667 ?
O1 La1 C1 24.88(7) 2_667 2_667 ?
C4 La1 C1 83.19(7) 2_567 2_667 ?
O6 Cu1 O6 180.0 . 2_556 ?
O6 Cu1 O8 90.10(9) . 2_656 ?
O6 Cu1 O8 89.90(9) 2_556 2_656 ?
O6 Cu1 O8 89.90(9) . 1_455 ?
O6 Cu1 O8 90.10(9) 2_556 1_455 ?
O8 Cu1 O8 180.00(12) 2_656 1_455 ?
C1 O1 La1 148.47(19) . . ?
C1 O1 La1 93.04(16) . 2_667 ?
La1 O1 La1 112.73(7) . 2_667 ?
O2 C1 O1 121.1(3) . . ?
O2 C1 C2 120.2(3) . . ?
O1 C1 C2 118.7(3) . . ?
O2 C1 La1 59.27(15) . 2_667 ?
O1 C1 La1 62.08(14) . 2_667 ?
C2 C1 La1 176.06(19) . 2_667 ?
C1 O2 La1 96.66(17) . 2_667 ?
C3 C2 C1 112.7(3) . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C5 C3 C4 121.1(3) . . ?
C5 C3 C2 122.8(3) . . ?
C4 C3 C2 116.2(3) . . ?
C4 O3 La1 93.85(18) . 2_567 ?
C4 O4 La1 95.66(18) . 2_567 ?
O3 C4 O4 120.5(3) . . ?
O3 C4 C3 119.3(3) . . ?
O4 C4 C3 120.2(3) . . ?
O3 C4 La1 61.21(15) . 2_567 ?
O4 C4 La1 59.37(15) . 2_567 ?
C3 C4 La1 176.2(2) . 2_567 ?
C3 C5 H5A 120.0 . . ?
C3 C5 H5B 120.0 . . ?
H5A C5 H5B 120.0 . . ?
C6 O5 La1 149.6(2) . . ?
O6 C6 O5 123.4(3) . . ?
O6 C6 C7 116.6(3) . . ?
O5 C6 C7 120.0(3) . . ?
C6 O6 Cu1 116.31(19) . . ?
C10B C7 C8 121.8(5) . . ?
C10B C7 C6 121.7(4) . . ?
C8 C7 C6 115.8(3) . . ?
C9 O8 Cu1 119.61(19) . 1_655 ?
C10A C8 C7 123.0(4) . . ?
C10A C8 C9 122.6(4) . . ?
C7 C8 C9 114.0(3) . . ?
O7 C9 O8 123.8(3) . . ?
O7 C9 C8 118.9(3) . . ?
O8 C9 C8 117.3(3) . . ?
La1 O9 H9B 120(3) . . ?
La1 O9 H9A 123(3) . . ?
H9B O9 H9A 107(4) . . ?
La1 O10 H10D 118(3) . . ?
La1 O10 H10C 126(3) . . ?
H10D O10 H10C 113(3) . . ?
C7 C10B H10F 125(5) . . ?
C7 C10B H10E 116(5) . . ?
H10F C10B H10E 119(7) . . ?
C8 C10A H10A 120.0 . . ?
C8 C10A H10B 120.0 . . ?
H10A C10A H10B 120.0 . . ?
La1 O11 H11A 126(3) . . ?
La1 O11 H11B 128(3) . . ?
H11A O11 H11B 104(4) . . ?
H12A O12 H12B 107(4) . . ?

_refine_diff_density_max         1.088
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.113

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

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1532660'
_audit_update_record             
;
2017-02-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 Cu Gd2 O24'
_chemical_formula_weight         1034.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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                   6.9675(8)
_cell_length_b                   10.6078(12)
_cell_length_c                   11.4879(13)
_cell_angle_alpha                109.198(3)
_cell_angle_beta                 100.025(3)
_cell_angle_gamma                98.983(3)
_cell_volume                     768.54(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9988
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      28.38

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.235
_exptl_crystal_F_000             501
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    5.050
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4590
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9686
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.050
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2699
_reflns_number_gt                2634
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+3.0116P] 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         2699
_refine_ls_number_parameters     246
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0622
_refine_ls_wR_factor_gt          0.0618
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.061
_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
Gd1 Gd 0.64118(3) 0.70737(2) 0.09979(2) 0.01398(9) Uani 1 1 d . . . . .
Cu1 Cu 1.000000 1.000000 0.500000 0.02071(17) Uani 1 2 d S . P . .
O1 O 0.7315(5) 0.7457(4) 0.3209(3) 0.0289(7) Uani 1 1 d . . . . .
C1 C 0.6887(6) 0.7757(4) 0.4261(4) 0.0190(9) Uani 1 1 d . . . . .
O2 O 0.7808(5) 0.8809(3) 0.5213(3) 0.0278(7) Uani 1 1 d . . . . .
C2 C 0.5241(7) 0.6804(5) 0.4474(4) 0.0262(10) Uani 1 1 d . . . . .
H2A H 0.430559 0.626660 0.366342 0.031 Uiso 1 1 calc R U . . .
H2B H 0.582985 0.617342 0.478969 0.031 Uiso 1 1 calc R U . . .
O3 O 0.2357(5) 0.8085(4) 0.3733(3) 0.0347(8) Uani 1 1 d . . . . .
C3 C 0.4101(7) 0.7516(5) 0.5388(4) 0.0268(10) Uani 1 1 d . U . . .
O4 O 0.1884(5) 0.9040(3) 0.5660(3) 0.0274(7) Uani 1 1 d . . . . .
C4 C 0.2694(6) 0.8265(5) 0.4877(4) 0.0219(9) Uani 1 1 d . . . . .
O5 O 0.6151(4) 0.4742(3) 0.0942(3) 0.0204(6) Uani 1 1 d . . . . .
C5 C 0.4166(12) 0.7380(9) 0.6484(8) 0.067(2) Uani 1 1 d . U . . .
H5A H 0.493781 0.682474 0.672286 0.080 Uiso 1 1 calc R U . . .
H5B H 0.343913 0.783699 0.702412 0.080 Uiso 1 1 calc R U . . .
O6 O 0.6405(5) 0.2623(3) 0.0547(3) 0.0245(7) Uani 1 1 d . . . . .
C6 C 0.7098(6) 0.3871(4) 0.1155(4) 0.0168(8) Uani 1 1 d . . . . .
O7 O 1.1345(5) 0.3977(3) 0.0336(3) 0.0265(7) Uani 1 1 d . . . . .
C7 C 0.9050(7) 0.4373(5) 0.2162(4) 0.0266(10) Uani 1 1 d . . . . .
H7A H 0.978666 0.521603 0.213938 0.032 Uiso 1 1 calc R U . . .
H7B H 0.875983 0.457782 0.299158 0.032 Uiso 1 1 calc R U . . .
C8 C 1.0347(6) 0.3339(5) 0.1986(4) 0.0261(10) Uani 1 1 d . . . . .
O8 O 1.2305(5) 0.2215(3) 0.0626(3) 0.0260(7) Uani 1 1 d . . . . .
C9 C 1.1379(6) 0.3162(4) 0.0923(4) 0.0200(9) Uani 1 1 d . . . . .
H9B H 1.050(7) 0.887(6) 0.160(5) 0.041(17) Uiso 1 1 d D . . . .
H9A H 1.055(6) 0.848(5) 0.258(4) 0.028(14) Uiso 1 1 d D . . . .
O9 O 0.9720(5) 0.8564(4) 0.1986(3) 0.0282(7) Uani 1 1 d D . . . .
C10 C 1.0613(10) 0.2647(8) 0.2728(6) 0.0540(17) Uani 1 1 d . . . . .
H10A H 1.145058 0.203799 0.259865 0.065 Uiso 1 1 calc R U . . .
H10B H 0.996680 0.276315 0.338587 0.065 Uiso 1 1 calc R U . . .
H10C H 0.493(7) 0.960(7) 0.165(6) 0.08(3) Uiso 1 1 d D . . . .
H10D H 0.660(8) 0.986(5) 0.262(3) 0.045(17) Uiso 1 1 d D . . . .
O10 O 0.6006(6) 0.9349(3) 0.1859(4) 0.0385(9) Uani 1 1 d D . . . .
O11 O 0.3305(5) 0.6663(3) 0.1576(3) 0.0273(7) Uani 1 1 d D . . . .
H11A H 0.238(8) 0.596(4) 0.124(6) 0.06(2) Uiso 1 1 d D . . . .
H11B H 0.312(9) 0.707(6) 0.229(3) 0.041(17) Uiso 1 1 d D . . . .
O12 O 1.2394(5) -0.0283(4) 0.0836(4) 0.0324(8) Uani 1 1 d D . . . .
H12B H 1.220(10) 0.039(5) 0.063(6) 0.05(2) Uiso 1 1 d D . . . .
H12A H 1.242(11) -0.074(7) 0.007(3) 0.06(2) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O10 2.372(3) . ?
Gd1 O1 2.387(3) . ?
Gd1 O11 2.390(3) . ?
Gd1 O9 2.423(3) . ?
Gd1 O5 2.431(3) . ?
Gd1 O8 2.479(3) 2_765 ?
Gd1 O7 2.508(3) 2_765 ?
Gd1 O6 2.543(3) 2_665 ?
Gd1 O5 2.566(3) 2_665 ?
Gd1 C9 2.871(4) 2_765 ?
Gd1 C6 2.933(4) 2_665 ?
Cu1 O2 1.929(3) . ?
Cu1 O2 1.929(3) 2_776 ?
Cu1 O4 1.978(3) 2_676 ?
Cu1 O4 1.978(3) 1_655 ?
O1 C1 1.246(5) . ?
C1 O2 1.258(5) . ?
C1 C2 1.515(6) . ?
C2 C3 1.503(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O3 C4 1.238(6) . ?
C3 C5 1.308(9) . ?
C3 C4 1.512(6) . ?
O4 C4 1.281(5) . ?
O5 C6 1.278(5) . ?
C5 H5A 0.9300 . ?
C5 H5B 0.9300 . ?
O6 C6 1.244(5) . ?
C6 C7 1.514(6) . ?
O7 C9 1.260(6) . ?
C7 C8 1.512(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C10 1.303(8) . ?
C8 C9 1.497(6) . ?
O8 C9 1.264(5) . ?
O9 H9B 0.85(2) . ?
O9 H9A 0.85(2) . ?
C10 H10A 0.9300 . ?
C10 H10B 0.9300 . ?
O10 H10C 0.85(2) . ?
O10 H10D 0.85(2) . ?
O11 H11A 0.84(2) . ?
O11 H11B 0.83(2) . ?
O12 H12B 0.84(2) . ?
O12 H12A 0.86(2) . ?

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
O10 Gd1 O1 80.18(13) . . ?
O10 Gd1 O11 79.50(13) . . ?
O1 Gd1 O11 74.89(11) . . ?
O10 Gd1 O9 72.46(13) . . ?
O1 Gd1 O9 69.13(11) . . ?
O11 Gd1 O9 137.27(11) . . ?
O10 Gd1 O5 153.08(13) . . ?
O1 Gd1 O5 78.72(11) . . ?
O11 Gd1 O5 78.99(11) . . ?
O9 Gd1 O5 114.56(11) . . ?
O10 Gd1 O8 86.01(13) . 2_765 ?
O1 Gd1 O8 140.60(11) . 2_765 ?
O11 Gd1 O8 138.32(11) . 2_765 ?
O9 Gd1 O8 71.54(11) . 2_765 ?
O5 Gd1 O8 120.90(10) . 2_765 ?
O10 Gd1 O7 132.95(13) . 2_765 ?
O1 Gd1 O7 117.22(11) . 2_765 ?
O11 Gd1 O7 145.17(11) . 2_765 ?
O9 Gd1 O7 74.39(12) . 2_765 ?
O5 Gd1 O7 72.40(10) . 2_765 ?
O8 Gd1 O7 51.99(10) 2_765 2_765 ?
O10 Gd1 O6 71.80(11) . 2_665 ?
O1 Gd1 O6 137.70(11) . 2_665 ?
O11 Gd1 O6 69.41(11) . 2_665 ?
O9 Gd1 O6 127.61(11) . 2_665 ?
O5 Gd1 O6 114.77(10) . 2_665 ?
O8 Gd1 O6 68.96(10) 2_765 2_665 ?
O7 Gd1 O6 105.05(11) 2_765 2_665 ?
O10 Gd1 O5 121.38(11) . 2_665 ?
O1 Gd1 O5 134.93(10) . 2_665 ?
O11 Gd1 O5 71.76(10) . 2_665 ?
O9 Gd1 O5 150.90(11) . 2_665 ?
O5 Gd1 O5 65.93(11) . 2_665 ?
O8 Gd1 O5 83.44(10) 2_765 2_665 ?
O7 Gd1 O5 78.59(10) 2_765 2_665 ?
O6 Gd1 O5 50.62(9) 2_665 2_665 ?
O10 Gd1 C9 110.23(14) . 2_765 ?
O1 Gd1 C9 133.83(11) . 2_765 ?
O11 Gd1 C9 149.96(11) . 2_765 ?
O9 Gd1 C9 71.74(12) . 2_765 ?
O5 Gd1 C9 96.46(11) . 2_765 ?
O8 Gd1 C9 26.03(11) 2_765 2_765 ?
O7 Gd1 C9 25.98(11) 2_765 2_765 ?
O6 Gd1 C9 86.31(11) 2_665 2_765 ?
O5 Gd1 C9 79.24(10) 2_665 2_765 ?
O10 Gd1 C6 95.85(12) . 2_665 ?
O1 Gd1 C6 141.20(11) . 2_665 ?
O11 Gd1 C6 66.49(11) . 2_665 ?
O9 Gd1 C6 146.55(11) . 2_665 ?
O5 Gd1 C6 90.25(11) . 2_665 ?
O8 Gd1 C6 76.55(11) 2_765 2_665 ?
O7 Gd1 C6 93.80(11) 2_765 2_665 ?
O6 Gd1 C6 24.98(11) 2_665 2_665 ?
O5 Gd1 C6 25.78(10) 2_665 2_665 ?
C9 Gd1 C6 83.98(11) 2_765 2_665 ?
O2 Cu1 O2 180.0 . 2_776 ?
O2 Cu1 O4 90.41(14) . 2_676 ?
O2 Cu1 O4 89.59(14) 2_776 2_676 ?
O2 Cu1 O4 89.59(14) . 1_655 ?
O2 Cu1 O4 90.41(14) 2_776 1_655 ?
O4 Cu1 O4 180.0 2_676 1_655 ?
C1 O1 Gd1 149.8(3) . . ?
O1 C1 O2 123.7(4) . . ?
O1 C1 C2 120.4(4) . . ?
O2 C1 C2 115.8(4) . . ?
C1 O2 Cu1 117.0(3) . . ?
C3 C2 C1 114.5(4) . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C5 C3 C2 122.5(5) . . ?
C5 C3 C4 122.5(5) . . ?
C2 C3 C4 114.6(4) . . ?
C4 O4 Cu1 118.0(3) . 1_455 ?
O3 C4 O4 123.5(4) . . ?
O3 C4 C3 119.0(4) . . ?
O4 C4 C3 117.5(4) . . ?
C6 O5 Gd1 146.0(3) . . ?
C6 O5 Gd1 93.4(2) . 2_665 ?
Gd1 O5 Gd1 114.06(11) . 2_665 ?
C3 C5 H5A 120.0 . . ?
C3 C5 H5B 120.0 . . ?
H5A C5 H5B 120.0 . . ?
C6 O6 Gd1 95.3(2) . 2_665 ?
O6 C6 O5 120.0(4) . . ?
O6 C6 C7 120.6(4) . . ?
O5 C6 C7 119.3(4) . . ?
O6 C6 Gd1 59.7(2) . 2_665 ?
O5 C6 Gd1 60.8(2) . 2_665 ?
C7 C6 Gd1 173.5(3) . 2_665 ?
C9 O7 Gd1 93.3(3) . 2_765 ?
C8 C7 C6 112.8(4) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C10 C8 C9 120.5(5) . . ?
C10 C8 C7 122.8(5) . . ?
C9 C8 C7 116.7(4) . . ?
C9 O8 Gd1 94.6(3) . 2_765 ?
O7 C9 O8 120.0(4) . . ?
O7 C9 C8 119.6(4) . . ?
O8 C9 C8 120.3(4) . . ?
O7 C9 Gd1 60.7(2) . 2_765 ?
O8 C9 Gd1 59.4(2) . 2_765 ?
C8 C9 Gd1 176.4(3) . 2_765 ?
Gd1 O9 H9B 125(4) . . ?
Gd1 O9 H9A 124(4) . . ?
H9B O9 H9A 101(5) . . ?
C8 C10 H10A 120.0 . . ?
C8 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
Gd1 O10 H10C 124(4) . . ?
Gd1 O10 H10D 120(4) . . ?
H10C O10 H10D 109(3) . . ?
Gd1 O11 H11A 128(5) . . ?
Gd1 O11 H11B 124(4) . . ?
H11A O11 H11B 105(6) . . ?
H12B O12 H12A 90(6) . . ?

_refine_diff_density_max         3.060
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.131

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

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1532663'
_audit_update_record             
;
2017-02-14 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H32 Cu O24 Tb2'
_chemical_formula_weight         1037.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   6.9630(4)
_cell_length_b                   10.5852(5)
_cell_length_c                   11.4644(6)
_cell_angle_alpha                109.296(2)
_cell_angle_beta                 99.958(2)
_cell_angle_gamma                98.927(2)
_cell_volume                     764.74(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      28.38

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_F_000             503
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    5.363
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4517
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      299(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26211
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.051
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2689
_reflns_number_gt                2607
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+3.5799P] 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         2689
_refine_ls_number_parameters     238
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0622
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.048
_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
Tb1 Tb 0.64102(3) 0.70710(2) 0.09937(2) 0.01415(9) Uani 1 1 d . . . . .
Cu1 Cu 1.000000 1.000000 0.500000 0.01979(17) Uani 1 2 d S . P . .
O1 O 0.7313(5) 0.7455(4) 0.3197(3) 0.0276(7) Uani 1 1 d . . . . .
O2 O 0.7808(5) 0.8799(4) 0.5205(3) 0.0285(7) Uani 1 1 d . . . . .
O3 O 0.2351(6) 0.8082(4) 0.3730(3) 0.0343(8) Uani 1 1 d . . . . .
O4 O 0.1885(5) 0.9043(4) 0.5662(3) 0.0271(7) Uani 1 1 d . . . . .
O5 O 0.6138(4) 0.4746(3) 0.0939(3) 0.0199(6) Uani 1 1 d . . . . .
O6 O 0.6402(5) 0.2626(3) 0.0554(3) 0.0237(7) Uani 1 1 d . . . . .
O7 O 1.1359(5) 0.3989(3) 0.0336(3) 0.0262(7) Uani 1 1 d . . . . .
O8 O 1.2312(5) 0.2222(3) 0.0625(3) 0.0253(7) Uani 1 1 d . . . . .
O9 O 0.9712(5) 0.8553(4) 0.1976(3) 0.0273(7) Uani 1 1 d D . . . .
H9B H 1.044(7) 0.888(6) 0.157(5) 0.033 Uiso 1 1 d D U . . .
H9A H 1.054(7) 0.845(6) 0.255(4) 0.033 Uiso 1 1 d D U . . .
O10 O 0.6009(6) 0.9340(4) 0.1851(4) 0.0373(9) Uani 1 1 d D . . . .
H10D H 0.495(6) 0.960(6) 0.166(5) 0.045 Uiso 1 1 d D U . . .
H10C H 0.657(8) 0.979(6) 0.263(2) 0.045 Uiso 1 1 d D U . . .
O11 O 0.3326(5) 0.6671(3) 0.1571(3) 0.0258(7) Uani 1 1 d D . . . .
H11A H 0.303(8) 0.708(5) 0.226(3) 0.031 Uiso 1 1 d D U . . .
H11B H 0.246(7) 0.593(4) 0.125(5) 0.031 Uiso 1 1 d D U . . .
O12 O 0.2387(5) 0.9711(4) 0.0833(4) 0.0321(8) Uani 1 1 d D . . . .
H12B H 0.251(9) 0.926(6) 0.009(3) 0.038 Uiso 1 1 d D U . . .
H12A H 0.228(9) 1.038(4) 0.060(6) 0.038 Uiso 1 1 d D U . . .
C1 C 0.6884(6) 0.7751(5) 0.4251(4) 0.0180(8) Uani 1 1 d . . . . .
C2 C 0.5247(7) 0.6796(5) 0.4466(4) 0.0245(10) Uani 1 1 d . . . . .
H2A H 0.431144 0.625508 0.365408 0.029 Uiso 1 1 calc R U . . .
H2B H 0.583933 0.616605 0.478267 0.029 Uiso 1 1 calc R U . . .
C3 C 0.4099(7) 0.7514(5) 0.5387(5) 0.0256(10) Uani 1 1 d . . . . .
C4 C 0.2687(6) 0.8262(5) 0.4877(4) 0.0216(9) Uani 1 1 d . . . . .
C5 C 0.4170(12) 0.7371(9) 0.6480(8) 0.066(2) Uani 1 1 d . . . . .
H5A H 0.494518 0.681323 0.671363 0.080 Uiso 1 1 calc R U . . .
H5B H 0.344536 0.782741 0.702639 0.080 Uiso 1 1 calc R U . . .
C6 C 0.7094(6) 0.3874(4) 0.1156(4) 0.0161(8) Uani 1 1 d . . . . .
C7 C 0.9049(7) 0.4384(5) 0.2161(4) 0.0257(10) Uani 1 1 d . . . . .
H7A H 0.977978 0.522718 0.213258 0.031 Uiso 1 1 calc R U . . .
H7B H 0.876257 0.459507 0.299425 0.031 Uiso 1 1 calc R U . . .
C8 C 1.0346(7) 0.3355(5) 0.1988(4) 0.0264(10) Uani 1 1 d . . . . .
C9 C 1.1388(6) 0.3166(4) 0.0920(4) 0.0185(8) Uani 1 1 d . . . . .
C10 C 1.0616(9) 0.2659(8) 0.2729(6) 0.0507(17) Uani 1 1 d . . . . .
H10A H 1.145264 0.204657 0.259633 0.061 Uiso 1 1 calc R U . . .
H10B H 0.997172 0.277470 0.339092 0.061 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
Tb1 O10 2.357(3) . ?
Tb1 O11 2.372(3) . ?
Tb1 O1 2.373(3) . ?
Tb1 O9 2.415(3) . ?
Tb1 O5 2.418(3) . ?
Tb1 O8 2.466(3) 2_765 ?
Tb1 O7 2.495(3) 2_765 ?
Tb1 O6 2.541(3) 2_665 ?
Tb1 O5 2.554(3) 2_665 ?
Tb1 C9 2.854(4) 2_765 ?
Tb1 C6 2.926(4) 2_665 ?
Cu1 O2 1.929(3) 2_776 ?
Cu1 O2 1.929(3) . ?
Cu1 O4 1.975(3) 2_676 ?
Cu1 O4 1.975(3) 1_655 ?
O1 C1 1.246(5) . ?
O2 C1 1.255(6) . ?
O3 C4 1.238(6) . ?
O4 C4 1.277(6) . ?
O5 C6 1.281(5) . ?
O6 C6 1.241(5) . ?
O7 C9 1.263(5) . ?
O8 C9 1.257(5) . ?
O9 H9B 0.85(2) . ?
O9 H9A 0.84(2) . ?
O10 H10D 0.847(19) . ?
O10 H10C 0.85(2) . ?
O11 H11A 0.84(2) . ?
O11 H11B 0.84(2) . ?
O12 H12B 0.86(2) . ?
O12 H12A 0.85(2) . ?
C1 C2 1.511(6) . ?
C2 C3 1.510(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.305(9) . ?
C3 C4 1.512(6) . ?
C5 H5A 0.9300 . ?
C5 H5B 0.9300 . ?
C6 C7 1.513(6) . ?
C7 C8 1.506(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C10 1.305(8) . ?
C8 C9 1.501(6) . ?
C10 H10A 0.9300 . ?
C10 H10B 0.9300 . ?

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
O10 Tb1 O11 79.45(14) . . ?
O10 Tb1 O1 80.28(13) . . ?
O11 Tb1 O1 74.99(11) . . ?
O10 Tb1 O9 72.58(13) . . ?
O11 Tb1 O9 137.35(11) . . ?
O1 Tb1 O9 69.12(11) . . ?
O10 Tb1 O5 153.00(13) . . ?
O11 Tb1 O5 78.91(11) . . ?
O1 Tb1 O5 78.67(11) . . ?
O9 Tb1 O5 114.61(11) . . ?
O10 Tb1 O8 85.89(13) . 2_765 ?
O11 Tb1 O8 138.25(11) . 2_765 ?
O1 Tb1 O8 140.51(11) . 2_765 ?
O9 Tb1 O8 71.46(11) . 2_765 ?
O5 Tb1 O8 121.09(10) . 2_765 ?
O10 Tb1 O7 133.08(13) . 2_765 ?
O11 Tb1 O7 145.11(11) . 2_765 ?
O1 Tb1 O7 117.03(11) . 2_765 ?
O9 Tb1 O7 74.33(12) . 2_765 ?
O5 Tb1 O7 72.38(10) . 2_765 ?
O8 Tb1 O7 52.23(10) 2_765 2_765 ?
O10 Tb1 O6 71.81(11) . 2_665 ?
O11 Tb1 O6 69.40(11) . 2_665 ?
O1 Tb1 O6 137.84(11) . 2_665 ?
O9 Tb1 O6 127.65(11) . 2_665 ?
O5 Tb1 O6 114.66(10) . 2_665 ?
O8 Tb1 O6 68.90(10) 2_765 2_665 ?
O7 Tb1 O6 105.10(11) 2_765 2_665 ?
O10 Tb1 O5 121.50(11) . 2_665 ?
O11 Tb1 O5 71.80(10) . 2_665 ?
O1 Tb1 O5 134.87(10) . 2_665 ?
O9 Tb1 O5 150.79(11) . 2_665 ?
O5 Tb1 O5 65.73(11) . 2_665 ?
O8 Tb1 O5 83.55(10) 2_765 2_665 ?
O7 Tb1 O5 78.49(10) 2_765 2_665 ?
O6 Tb1 O5 50.74(9) 2_665 2_665 ?
O10 Tb1 C9 110.10(14) . 2_765 ?
O11 Tb1 C9 150.04(11) . 2_765 ?
O1 Tb1 C9 133.69(11) . 2_765 ?
O9 Tb1 C9 71.56(12) . 2_765 ?
O5 Tb1 C9 96.68(11) . 2_765 ?
O8 Tb1 C9 26.03(11) 2_765 2_765 ?
O7 Tb1 C9 26.21(12) 2_765 2_765 ?
O6 Tb1 C9 86.28(11) 2_665 2_765 ?
O5 Tb1 C9 79.34(11) 2_665 2_765 ?
O10 Tb1 C6 95.83(12) . 2_665 ?
O11 Tb1 C6 66.43(11) . 2_665 ?
O1 Tb1 C6 141.23(11) . 2_665 ?
O9 Tb1 C6 146.59(11) . 2_665 ?
O5 Tb1 C6 90.13(11) . 2_665 ?
O8 Tb1 C6 76.61(11) 2_765 2_665 ?
O7 Tb1 C6 93.86(11) 2_765 2_665 ?
O6 Tb1 C6 24.98(11) 2_665 2_665 ?
O5 Tb1 C6 25.91(11) 2_665 2_665 ?
C9 Tb1 C6 84.09(11) 2_765 2_665 ?
O2 Cu1 O2 180.0 2_776 . ?
O2 Cu1 O4 89.62(14) 2_776 2_676 ?
O2 Cu1 O4 90.38(14) . 2_676 ?
O2 Cu1 O4 90.38(14) 2_776 1_655 ?
O2 Cu1 O4 89.62(14) . 1_655 ?
O4 Cu1 O4 180.0 2_676 1_655 ?
C1 O1 Tb1 149.8(3) . . ?
C1 O2 Cu1 117.3(3) . . ?
C4 O4 Cu1 117.9(3) . 1_455 ?
C6 O5 Tb1 145.6(3) . . ?
C6 O5 Tb1 93.5(2) . 2_665 ?
Tb1 O5 Tb1 114.27(11) . 2_665 ?
C6 O6 Tb1 95.2(2) . 2_665 ?
C9 O7 Tb1 93.0(3) . 2_765 ?
C9 O8 Tb1 94.5(2) . 2_765 ?
Tb1 O9 H9B 124(4) . . ?
Tb1 O9 H9A 123(4) . . ?
H9B O9 H9A 104(6) . . ?
Tb1 O10 H10D 125(4) . . ?
Tb1 O10 H10C 117(4) . . ?
H10D O10 H10C 109(3) . . ?
Tb1 O11 H11A 129(4) . . ?
Tb1 O11 H11B 125(4) . . ?
H11A O11 H11B 103(6) . . ?
H12B O12 H12A 89(6) . . ?
O1 C1 O2 123.5(4) . . ?
O1 C1 C2 120.6(4) . . ?
O2 C1 C2 115.8(4) . . ?
C3 C2 C1 114.5(4) . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C5 C3 C2 122.1(5) . . ?
C5 C3 C4 122.8(5) . . ?
C2 C3 C4 114.7(4) . . ?
O3 C4 O4 123.4(4) . . ?
O3 C4 C3 119.0(4) . . ?
O4 C4 C3 117.6(4) . . ?
C3 C5 H5A 120.0 . . ?
C3 C5 H5B 120.0 . . ?
H5A C5 H5B 120.0 . . ?
O6 C6 O5 119.9(4) . . ?
O6 C6 C7 120.7(4) . . ?
O5 C6 C7 119.3(4) . . ?
O6 C6 Tb1 59.9(2) . 2_665 ?
O5 C6 Tb1 60.6(2) . 2_665 ?
C7 C6 Tb1 173.3(3) . 2_665 ?
C8 C7 C6 112.8(4) . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C10 C8 C9 119.9(5) . . ?
C10 C8 C7 123.0(5) . . ?
C9 C8 C7 117.1(4) . . ?
O8 C9 O7 120.2(4) . . ?
O8 C9 C8 120.7(4) . . ?
O7 C9 C8 119.0(4) . . ?
O8 C9 Tb1 59.5(2) . 2_765 ?
O7 C9 Tb1 60.8(2) . 2_765 ?
C8 C9 Tb1 176.3(3) . 2_765 ?
C8 C10 H10A 120.0 . . ?
C8 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?

_refine_diff_density_max         3.264
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.136

