# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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
_database_code_depnum_ccdc_archive 'CCDC 1574413'
_audit_update_record             
;
2017-09-14 deposited with the CCDC.
2017-11-07 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            'C24 H23 Eu O7'
_chemical_formula_weight         575.38

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   7.8984(12)
_cell_length_b                   20.324(3)
_cell_length_c                   13.907(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2232.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    9452
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      27.52

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    2.852
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5624
_exptl_absorpt_correction_T_max  0.7456
_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            40918
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.966
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2021
_reflns_number_gt                1851
_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)+(0.0239P)²+3.2622P] 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         2021
_refine_ls_number_parameters     163
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0469
_refine_ls_wR_factor_gt          0.0448
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
Eu1 Eu 0.55641(2) 0.750000 0.21387(2) 0.01539(8) Uani 1 2 d S T P . .
C1 C 0.2614(3) 0.63345(14) 0.3130(2) 0.0243(6) Uani 1 1 d . . . . .
O1 O 0.3239(2) 0.68313(9) 0.26905(14) 0.0251(4) Uani 1 1 d . . . . .
O3 O 0.5891(3) 0.750000 0.3892(2) 0.0300(7) Uani 1 2 d S T P . .
C3 C 0.2878(4) 0.51826(15) 0.3801(2) 0.0354(8) Uani 1 1 d . . . . .
O2 O 0.1097(3) 0.63306(11) 0.33486(18) 0.0400(6) Uani 1 1 d . . . . .
C2 C 0.3773(4) 0.57698(16) 0.3381(3) 0.0420(9) Uani 1 1 d . . . . .
H2A H 0.436945 0.563288 0.280518 0.050 Uiso 1 1 calc R U . . .
H2B H 0.461135 0.592360 0.383884 0.050 Uiso 1 1 calc R U . . .
O4 O 0.8685(3) 0.750000 0.41589(19) 0.0279(6) Uani 1 2 d S T P . .
C4 C 0.2077(5) 0.47368(18) 0.3216(3) 0.0491(9) Uani 1 1 d . . . . .
H4 H 0.213811 0.478743 0.255210 0.059 Uiso 1 1 calc R U . . .
C8 C 0.2791(5) 0.50886(19) 0.4785(3) 0.0500(9) Uani 1 1 d . . . . .
H8 H 0.333307 0.538113 0.519675 0.060 Uiso 1 1 calc R U . . .
C7 C 0.1890(6) 0.4556(2) 0.5163(3) 0.0621(12) Uani 1 1 d . . . . .
H7 H 0.184418 0.449431 0.582556 0.074 Uiso 1 1 calc R U . . .
C6 C 0.1084(5) 0.4128(2) 0.4570(4) 0.0625(12) Uani 1 1 d . . . . .
H6 H 0.046889 0.377923 0.482492 0.075 Uiso 1 1 calc R U . . .
C5 C 0.1181(6) 0.42137(19) 0.3596(4) 0.0620(11) Uani 1 1 d . . . . .
H5 H 0.064042 0.391833 0.318795 0.074 Uiso 1 1 calc R U . . .
O5 O 0.7240(4) 0.750000 0.0644(2) 0.0475(9) Uani 1 2 d DS T P . .
H5B H 0.692(7) 0.750000 0.0073(19) 0.057 Uiso 1 2 d DS U P . .
H5A H 0.831(3) 0.750000 0.069(4) 0.057 Uiso 1 2 d DS U P . .
C9 C 0.7180(5) 0.750000 0.4433(3) 0.0214(8) Uani 1 2 d S T P . .
C10 C 0.6987(5) 0.750000 0.5524(3) 0.0333(10) Uani 1 2 d S T P . .
H10A H 0.757222 0.711599 0.577144 0.040 Uiso 0.5 1 calc R U P . .
H10B H 0.757222 0.788401 0.577144 0.040 Uiso 0.5 1 calc R U P . .
C11 C 0.5237(5) 0.750000 0.5932(3) 0.0297(10) Uani 1 2 d S T P B .
C12 C 0.4432(5) 0.6922(2) 0.6150(3) 0.0638(13) Uani 1 1 d . . . . .
H12 H 0.483412 0.650247 0.600997 0.077 Uiso 1 1 calc R U . A 1
C13A C 0.2686(12) 0.7085(6) 0.6685(7) 0.039(3) Uiso 0.479(18) 1 d . . P B 1
C14A C 0.2050(18) 0.741(2) 0.6753(9) 0.030(6) Uiso 0.240(9) 1 d . . P B 1
C13B C 0.2920(9) 0.6776(5) 0.6443(6) 0.043(3) Uiso 0.521(18) 1 d . . P B 2
H13B H 0.252881 0.634407 0.642432 0.051 Uiso 0.521(18) 1 calc R U P B 2
C14B C 0.202(3) 0.7780(10) 0.6744(13) 0.038(7) Uiso 0.260(9) 1 d . . P B 2
H14B H 0.107475 0.794506 0.706118 0.046 Uiso 0.260(9) 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4 2.336(3) 6_556 ?
Eu1 O1 2.4098(18) 7_575 ?
Eu1 O1 2.4098(18) . ?
Eu1 O3 2.452(3) . ?
Eu1 O5 2.465(3) . ?
Eu1 O2 2.507(2) 6_656 ?
Eu1 O2 2.507(2) 4_565 ?
Eu1 O1 2.5235(18) 4_565 ?
Eu1 O1 2.5235(18) 6_656 ?
Eu1 C1 2.893(3) 4_565 ?
Eu1 C1 2.893(3) 6_656 ?
Eu1 Eu1 4.0750(6) 6_656 ?
C1 O2 1.236(3) . ?
C1 O1 1.279(3) . ?
C1 C2 1.509(4) . ?
O3 C9 1.266(5) . ?
C3 C4 1.373(5) . ?
C3 C8 1.383(5) . ?
C3 C2 1.505(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O4 C9 1.249(5) . ?
C4 C5 1.383(5) . ?
C4 H4 0.9300 . ?
C8 C7 1.398(5) . ?
C8 H8 0.9300 . ?
C7 C6 1.357(6) . ?
C7 H7 0.9300 . ?
C6 C5 1.368(6) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
O5 H5B 0.83(2) . ?
O5 H5A 0.85(2) . ?
C9 C10 1.525(5) . ?
C10 C11 1.495(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.370(5) 7_575 ?
C11 C12 1.370(5) . ?
C12 C13B 1.297(8) . ?
C12 C13A 1.602(12) . ?
C12 H12 0.9300 . ?
C13A C14A 0.83(4) . ?
C13A C14A 1.15(4) 7_575 ?
C13A C13A 1.69(3) 7_575 ?
C14A C14A 0.38(8) 7_575 ?
C13B C14B 1.22(2) 7_575 ?
C13B H13B 0.9300 . ?
C14B C14B 1.14(4) 7_575 ?
C14B H14B 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
O4 Eu1 O1 76.23(7) 6_556 7_575 ?
O4 Eu1 O1 76.23(7) 6_556 . ?
O1 Eu1 O1 68.66(9) 7_575 . ?
O4 Eu1 O3 146.61(9) 6_556 . ?
O1 Eu1 O3 76.32(7) 7_575 . ?
O1 Eu1 O3 76.32(7) . . ?
O4 Eu1 O5 71.91(10) 6_556 . ?
O1 Eu1 O5 132.67(7) 7_575 . ?
O1 Eu1 O5 132.67(7) . . ?
O3 Eu1 O5 141.49(10) . . ?
O4 Eu1 O2 84.14(6) 6_556 6_656 ?
O1 Eu1 O2 138.48(6) 7_575 6_656 ?
O1 Eu1 O2 71.30(7) . 6_656 ?
O3 Eu1 O2 104.54(6) . 6_656 ?
O5 Eu1 O2 71.44(6) . 6_656 ?
O4 Eu1 O2 84.14(6) 6_556 4_565 ?
O1 Eu1 O2 71.31(7) 7_575 4_565 ?
O1 Eu1 O2 138.48(6) . 4_565 ?
O3 Eu1 O2 104.54(6) . 4_565 ?
O5 Eu1 O2 71.44(6) . 4_565 ?
O2 Eu1 O2 142.88(12) 6_656 4_565 ?
O4 Eu1 O1 127.20(6) 6_556 4_565 ?
O1 Eu1 O1 107.72(6) 7_575 4_565 ?
O1 Eu1 O1 155.75(2) . 4_565 ?
O3 Eu1 O1 79.53(7) . 4_565 ?
O5 Eu1 O1 68.27(8) . 4_565 ?
O2 Eu1 O1 113.28(6) 6_656 4_565 ?
O2 Eu1 O1 51.26(6) 4_565 4_565 ?
O4 Eu1 O1 127.20(6) 6_556 6_656 ?
O1 Eu1 O1 155.75(2) 7_575 6_656 ?
O1 Eu1 O1 107.72(7) . 6_656 ?
O3 Eu1 O1 79.53(7) . 6_656 ?
O5 Eu1 O1 68.27(8) . 6_656 ?
O2 Eu1 O1 51.26(6) 6_656 6_656 ?
O2 Eu1 O1 113.28(6) 4_565 6_656 ?
O1 Eu1 O1 65.16(8) 4_565 6_656 ?
O4 Eu1 C1 104.82(7) 6_556 4_565 ?
O1 Eu1 C1 90.33(7) 7_575 4_565 ?
O1 Eu1 C1 158.30(7) . 4_565 ?
O3 Eu1 C1 93.97(7) . 4_565 ?
O5 Eu1 C1 65.84(7) . 4_565 ?
O2 Eu1 C1 130.33(7) 6_656 4_565 ?
O2 Eu1 C1 25.18(7) 4_565 4_565 ?
O1 Eu1 C1 26.19(7) 4_565 4_565 ?
O1 Eu1 C1 89.11(7) 6_656 4_565 ?
O4 Eu1 C1 104.82(7) 6_556 6_656 ?
O1 Eu1 C1 158.30(7) 7_575 6_656 ?
O1 Eu1 C1 90.33(7) . 6_656 ?
O3 Eu1 C1 93.97(7) . 6_656 ?
O5 Eu1 C1 65.84(7) . 6_656 ?
O2 Eu1 C1 25.18(7) 6_656 6_656 ?
O2 Eu1 C1 130.33(7) 4_565 6_656 ?
O1 Eu1 C1 89.11(7) 4_565 6_656 ?
O1 Eu1 C1 26.19(7) 6_656 6_656 ?
C1 Eu1 C1 109.91(11) 4_565 6_656 ?
O4 Eu1 Eu1 143.71(7) 6_556 6_656 ?
O1 Eu1 Eu1 131.29(5) 7_575 6_656 ?
O1 Eu1 Eu1 131.29(5) . 6_656 ?
O3 Eu1 Eu1 69.68(6) . 6_656 ?
O5 Eu1 Eu1 71.80(8) . 6_656 ?
O2 Eu1 Eu1 84.48(5) 6_656 6_656 ?
O2 Eu1 Eu1 84.48(5) 4_565 6_656 ?
O1 Eu1 Eu1 33.42(4) 4_565 6_656 ?
O1 Eu1 Eu1 33.42(4) 6_656 6_656 ?
C1 Eu1 Eu1 59.30(5) 4_565 6_656 ?
C1 Eu1 Eu1 59.30(6) 6_656 6_656 ?
O2 C1 O1 119.8(3) . . ?
O2 C1 C2 121.7(3) . . ?
O1 C1 C2 118.5(2) . . ?
O2 C1 Eu1 59.64(15) . 6_556 ?
O1 C1 Eu1 60.55(14) . 6_556 ?
C2 C1 Eu1 172.7(2) . 6_556 ?
C1 O1 Eu1 153.04(18) . . ?
C1 O1 Eu1 93.26(16) . 6_556 ?
Eu1 O1 Eu1 111.36(7) . 6_556 ?
C9 O3 Eu1 132.5(2) . . ?
C4 C3 C8 118.2(3) . . ?
C4 C3 C2 120.6(3) . . ?
C8 C3 C2 121.1(3) . . ?
C1 O2 Eu1 95.18(17) . 6_556 ?
C3 C2 C1 114.1(3) . . ?
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 . . ?
C9 O4 Eu1 147.2(3) . 6_656 ?
C3 C4 C5 121.1(4) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C3 C8 C7 120.3(4) . . ?
C3 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C6 C7 C8 120.4(4) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C6 C5 119.6(4) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
Eu1 O5 H5B 130(4) . . ?
Eu1 O5 H5A 118(4) . . ?
H5B O5 H5A 112(6) . . ?
O4 C9 O3 125.8(3) . . ?
O4 C9 C10 113.5(3) . . ?
O3 C9 C10 120.7(3) . . ?
C11 C10 C9 118.1(3) . . ?
C11 C10 H10A 107.8 . . ?
C9 C10 H10A 107.8 . . ?
C11 C10 H10B 107.8 . . ?
C9 C10 H10B 107.8 . . ?
H10A C10 H10B 107.1 . . ?
C12 C11 C12 118.2(5) 7_575 . ?
C12 C11 C10 120.9(3) 7_575 . ?
C12 C11 C10 120.9(2) . . ?
C13B C12 C11 133.9(7) . . ?
C11 C12 C13A 108.9(6) . . ?
C11 C12 H12 125.5 . . ?
C13A C12 H12 125.5 . . ?
C14A C13A C14A 12(3) . 7_575 ?
C14A C13A C12 137.6(18) . . ?
C14A C13A C12 126.7(15) 7_575 . ?
C14A C13A C13A 38.2(19) . 7_575 ?
C14A C13A C13A 26.3(14) 7_575 7_575 ?
C12 C13A C13A 102.0(5) . 7_575 ?
C14A C14A C13A 141.8(19) 7_575 . ?
C14A C14A C13A 26.3(14) 7_575 7_575 ?
C13A C14A C13A 116(2) . 7_575 ?
C14B C13B C12 118.2(14) 7_575 . ?
C14B C13B H13B 120.9 7_575 . ?
C12 C13B H13B 120.9 . . ?
C14B C14B H14B 111.2 7_575 . ?
C13B C14B H14B 111.2 7_575 . ?

_refine_diff_density_max         0.366
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.078

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1574414'
_audit_update_record             
;
2017-09-14 deposited with the CCDC.
2017-11-07 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            'C24 H23 Gd O7'
_chemical_formula_weight         580.67

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   7.8711(2)
_cell_length_b                   20.3008(6)
_cell_length_c                   13.8754(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2217.15(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      27.52

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    3.034
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5649
_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            31702
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.140
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2006
_reflns_number_gt                1727
_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)+(0.0218P)²+3.8214P] 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     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0039(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2006
_refine_ls_number_parameters     164
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0493
_refine_ls_wR_factor_gt          0.0454
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 -0.05682(2) 0.250000 0.71388(2) 0.01760(10) Uani 1 2 d S T P . .
C1 C 0.2380(4) 0.36607(16) 0.8130(2) 0.0262(8) Uani 1 1 d . . . . .
O1 O 0.1761(3) 0.31659(10) 0.76848(16) 0.0268(5) Uani 1 1 d . . . . .
O3 O 0.1295(4) 0.250000 0.5842(2) 0.0300(8) Uani 1 2 d S T P . .
C3 C 0.2108(5) 0.48149(18) 0.8798(3) 0.0368(9) Uani 1 1 d . . . . .
O2 O 0.3903(3) 0.36623(13) 0.8350(2) 0.0417(7) Uani 1 1 d . . . . .
C2 C 0.1222(5) 0.42267(19) 0.8380(3) 0.0431(10) Uani 1 1 d . . . . .
H2A H 0.062439 0.436240 0.780196 0.052 Uiso 1 1 calc R U . . .
H2B H 0.037984 0.407342 0.883861 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3108(7) 0.5440(3) 1.0160(4) 0.0634(14) Uani 1 1 d . . . . .
H5 H 0.315865 0.550038 1.082393 0.076 Uiso 1 1 calc R U . . .
O5 O -0.2231(5) 0.250000 0.5654(3) 0.0482(11) Uani 1 2 d DS T P . .
H5B H -0.329(3) 0.250000 0.562(5) 0.058 Uiso 1 2 d DS U P . .
H5A H -0.169(7) 0.250000 0.514(3) 0.058 Uiso 1 2 d DS U P . .
O4 O 0.4117(4) 0.250000 0.6126(2) 0.0304(8) Uani 1 2 d S T P . .
C4 C 0.2209(6) 0.4910(2) 0.9783(3) 0.0530(12) Uani 1 1 d . . . . .
H4 H 0.166889 0.461720 1.019669 0.064 Uiso 1 1 calc R U . . .
C8 C 0.2912(6) 0.5262(2) 0.8210(3) 0.0512(12) Uani 1 1 d . . . . .
H8 H 0.284986 0.521288 0.754452 0.061 Uiso 1 1 calc R U . . .
C7 C 0.3811(7) 0.5784(2) 0.8595(4) 0.0644(14) Uani 1 1 d . . . . .
H7 H 0.435014 0.608081 0.818597 0.077 Uiso 1 1 calc R U . . .
C6 C 0.3918(6) 0.5870(2) 0.9563(4) 0.0646(15) Uani 1 1 d . . . . .
H6 H 0.453768 0.621906 0.981598 0.078 Uiso 1 1 calc R U . . .
C9 C 0.2821(6) 0.250000 0.5569(3) 0.0229(10) Uani 1 2 d S T P . .
C10 C 0.3014(6) 0.250000 0.4486(3) 0.0350(13) Uani 1 2 d S T P . .
H10A H 0.242483 0.211571 0.423855 0.042 Uiso 0.5 1 calc R U P . .
H10B H 0.242483 0.288429 0.423855 0.042 Uiso 0.5 1 calc R U P . .
C11 C 0.4765(6) 0.250000 0.4068(3) 0.0297(11) Uani 1 2 d S T P B .
C12 C 0.5591(6) 0.3082(3) 0.3858(4) 0.0645(15) Uani 1 1 d . . . . .
H12 H 0.489156 0.344600 0.394593 0.077 Uiso 1 1 calc R U . A 1
C13A C 0.7094(11) 0.3248(6) 0.3568(7) 0.044(3) Uiso 0.51(2) 1 d . . P B 1
C14A C 0.794(2) 0.260(2) 0.3262(11) 0.034(7) Uiso 0.255(11) 1 d . . P B 1
C13B C 0.7323(13) 0.2928(7) 0.3329(7) 0.039(4) Uiso 0.49(2) 1 d . . P B 2
C14B C 0.804(4) 0.2227(15) 0.3262(17) 0.039(9) Uiso 0.245(11) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.322(3) . ?
Gd1 O1 2.400(2) . ?
Gd1 O1 2.400(2) 7_565 ?
Gd1 O4 2.421(3) 6_557 ?
Gd1 O5 2.441(4) . ?
Gd1 O2 2.490(2) 4_456 ?
Gd1 O2 2.490(2) 6_557 ?
Gd1 O1 2.512(2) 4_456 ?
Gd1 O1 2.512(2) 6_557 ?
Gd1 C1 2.881(3) 4_456 ?
Gd1 C1 2.881(3) 6_557 ?
Gd1 Gd1 4.06119(14) 6_657 ?
C1 O2 1.237(4) . ?
C1 O1 1.276(4) . ?
C1 C2 1.507(5) . ?
O3 C9 1.259(6) . ?
C3 C8 1.376(6) . ?
C3 C4 1.382(6) . ?
C3 C2 1.500(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 C6 1.362(7) . ?
C5 C4 1.389(6) . ?
C5 H5 0.9300 . ?
O5 H5B 0.83(2) . ?
O5 H5A 0.83(2) . ?
O4 C9 1.279(5) . ?
C4 H4 0.9300 . ?
C8 C7 1.382(6) . ?
C8 H8 0.9300 . ?
C7 C6 1.356(8) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C9 C10 1.512(7) . ?
C10 C11 1.495(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.379(5) . ?
C11 C12 1.379(5) 7_565 ?
C12 C13A 1.295(9) . ?
C12 C13B 1.580(13) . ?
C12 H12 0.9300 . ?
C13A C14A 1.53(4) . ?
C13A C14A 1.90(4) 7_565 ?
C14A C14A 0.42(9) 7_565 ?
C13B C14B 0.65(3) 7_565 ?
C13B C14B 1.53(2) . ?
C13B C13B 1.74(3) 7_565 ?
C14B C14B 1.11(6) 7_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Gd1 O1 76.25(9) . . ?
O3 Gd1 O1 76.25(9) . 7_565 ?
O1 Gd1 O1 68.55(10) . 7_565 ?
O3 Gd1 O4 146.70(11) . 6_557 ?
O1 Gd1 O4 76.36(8) . 6_557 ?
O1 Gd1 O4 76.36(8) 7_565 6_557 ?
O3 Gd1 O5 71.60(12) . . ?
O1 Gd1 O5 132.53(8) . . ?
O1 Gd1 O5 132.53(8) 7_565 . ?
O4 Gd1 O5 141.70(12) 6_557 . ?
O3 Gd1 O2 83.94(7) . 4_456 ?
O1 Gd1 O2 138.36(8) . 4_456 ?
O1 Gd1 O2 71.34(8) 7_565 4_456 ?
O4 Gd1 O2 104.71(7) 6_557 4_456 ?
O5 Gd1 O2 71.36(7) . 4_456 ?
O3 Gd1 O2 83.94(7) . 6_557 ?
O1 Gd1 O2 71.34(8) . 6_557 ?
O1 Gd1 O2 138.36(8) 7_565 6_557 ?
O4 Gd1 O2 104.71(7) 6_557 6_557 ?
O5 Gd1 O2 71.36(7) . 6_557 ?
O2 Gd1 O2 142.71(14) 4_456 6_557 ?
O3 Gd1 O1 127.18(8) . 4_456 ?
O1 Gd1 O1 155.74(2) . 4_456 ?
O1 Gd1 O1 107.78(7) 7_565 4_456 ?
O4 Gd1 O1 79.48(8) 6_557 4_456 ?
O5 Gd1 O1 68.49(9) . 4_456 ?
O2 Gd1 O1 51.43(8) 4_456 4_456 ?
O2 Gd1 O1 113.36(7) 6_557 4_456 ?
O3 Gd1 O1 127.18(8) . 6_557 ?
O1 Gd1 O1 107.78(7) . 6_557 ?
O1 Gd1 O1 155.74(2) 7_565 6_557 ?
O4 Gd1 O1 79.48(8) 6_557 6_557 ?
O5 Gd1 O1 68.49(9) . 6_557 ?
O2 Gd1 O1 113.36(7) 4_456 6_557 ?
O2 Gd1 O1 51.43(7) 6_557 6_557 ?
O1 Gd1 O1 65.13(10) 4_456 6_557 ?
O3 Gd1 C1 104.70(8) . 4_456 ?
O1 Gd1 C1 158.38(8) . 4_456 ?
O1 Gd1 C1 90.48(8) 7_565 4_456 ?
O4 Gd1 C1 94.10(8) 6_557 4_456 ?
O5 Gd1 C1 65.79(8) . 4_456 ?
O2 Gd1 C1 25.31(9) 4_456 4_456 ?
O2 Gd1 C1 130.23(9) 6_557 4_456 ?
O1 Gd1 C1 26.24(8) 4_456 4_456 ?
O1 Gd1 C1 89.05(8) 6_557 4_456 ?
O3 Gd1 C1 104.70(8) . 6_557 ?
O1 Gd1 C1 90.49(8) . 6_557 ?
O1 Gd1 C1 158.38(9) 7_565 6_557 ?
O4 Gd1 C1 94.10(8) 6_557 6_557 ?
O5 Gd1 C1 65.79(8) . 6_557 ?
O2 Gd1 C1 130.23(9) 4_456 6_557 ?
O2 Gd1 C1 25.31(9) 6_557 6_557 ?
O1 Gd1 C1 89.05(8) 4_456 6_557 ?
O1 Gd1 C1 26.24(8) 6_557 6_557 ?
C1 Gd1 C1 109.74(13) 4_456 6_557 ?
O3 Gd1 Gd1 65.11(8) . 6_657 ?
O1 Gd1 Gd1 35.12(5) . 6_657 ?
O1 Gd1 Gd1 35.12(5) 7_565 6_657 ?
O4 Gd1 Gd1 81.58(7) 6_557 6_657 ?
O5 Gd1 Gd1 136.72(9) . 6_657 ?
O2 Gd1 Gd1 103.25(6) 4_456 6_657 ?
O2 Gd1 Gd1 103.25(6) 6_557 6_657 ?
O1 Gd1 Gd1 141.92(5) 4_456 6_657 ?
O1 Gd1 Gd1 141.92(5) 6_557 6_657 ?
C1 Gd1 Gd1 125.12(7) 4_456 6_657 ?
C1 Gd1 Gd1 125.12(7) 6_557 6_657 ?
O2 C1 O1 119.4(3) . . ?
O2 C1 C2 121.8(3) . . ?
O1 C1 C2 118.7(3) . . ?
O2 C1 Gd1 59.39(18) . 6_657 ?
O1 C1 Gd1 60.50(16) . 6_657 ?
C2 C1 Gd1 173.0(3) . 6_657 ?
C1 O1 Gd1 152.6(2) . . ?
C1 O1 Gd1 93.26(19) . 6_657 ?
Gd1 O1 Gd1 111.53(8) . 6_657 ?
C9 O3 Gd1 146.6(3) . . ?
C8 C3 C4 117.9(4) . . ?
C8 C3 C2 120.7(4) . . ?
C4 C3 C2 121.4(4) . . ?
C1 O2 Gd1 95.3(2) . 6_657 ?
C3 C2 C1 114.5(3) . . ?
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 . . ?
C6 C5 C4 120.3(5) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
Gd1 O5 H5B 126(5) . . ?
Gd1 O5 H5A 117(5) . . ?
H5B O5 H5A 117(7) . . ?
C9 O4 Gd1 133.0(3) . 6_657 ?
C3 C4 C5 120.7(5) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C3 C8 C7 120.8(4) . . ?
C3 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C6 C7 C8 120.8(5) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C6 C5 119.5(4) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
O3 C9 O4 125.4(4) . . ?
O3 C9 C10 113.2(4) . . ?
O4 C9 C10 121.4(4) . . ?
C11 C10 C9 118.5(4) . . ?
C11 C10 H10A 107.7 . . ?
C9 C10 H10A 107.7 . . ?
C11 C10 H10B 107.7 . . ?
C9 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
C12 C11 C12 117.8(6) . 7_565 ?
C12 C11 C10 121.1(3) . . ?
C12 C11 C10 121.1(3) 7_565 . ?
C13A C12 C11 136.1(8) . . ?
C11 C12 C13B 109.6(7) . . ?
C13A C12 H12 112.0 . . ?
C11 C12 H12 112.0 . . ?
C12 C13A C14A 105.0(13) . . ?
C12 C13A C14A 98.7(11) . 7_565 ?
C14A C13A C14A 6.5(14) . 7_565 ?
C14A C14A C13A 149.0(10) 7_565 . ?
C14A C14A C13A 24.5(8) 7_565 7_565 ?
C13A C14A C13A 124.5(12) . 7_565 ?
C14B C13B C14B 39(3) 7_565 . ?
C14B C13B C12 155(3) 7_565 . ?
C14B C13B C12 121.8(12) . . ?
C12 C13B C13B 101.4(5) . 7_565 ?
C13B C14B C14B 119(3) 7_565 7_565 ?
C13B C14B C13B 97(4) 7_565 . ?
C14B C14B C13B 21.8(10) 7_565 . ?

_refine_diff_density_max         0.627
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.088

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1574416'
_audit_update_record             
;
2017-09-14 deposited with the CCDC.
2017-11-07 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            'C24 H23 Dy O7'
_chemical_formula_weight         585.92

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   7.8673(3)
_cell_length_b                   20.3050(9)
_cell_length_c                   13.8787(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2217.06(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9582
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      27.52

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_F_000             1156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.413
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5059
_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            40795
_diffrn_reflns_av_unetI/netI     0.0082
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.976
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1989
_reflns_number_gt                1889
_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)+(0.0410P)²+7.9846P] 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     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0104(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1989
_refine_ls_number_parameters     164
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0684
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_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
Dy1 Dy 0.94313(3) 0.750000 0.28614(2) 0.01497(15) Uani 1 2 d S T P . .
C1 C 0.7379(5) 0.63401(18) 0.3130(3) 0.0224(7) Uani 1 1 d . . . . .
O1 O 0.8903(3) 0.63358(14) 0.3352(2) 0.0353(7) Uani 1 1 d . . . . .
O2 O 0.6755(3) 0.68354(12) 0.26855(19) 0.0225(5) Uani 1 1 d . . . . .
C2 C 0.6219(5) 0.5773(2) 0.3382(4) 0.0388(11) Uani 1 1 d . . . . .
H2A H 0.537916 0.592605 0.384196 0.047 Uiso 1 1 calc R U . . .
H2B H 0.561871 0.563683 0.280517 0.047 Uiso 1 1 calc R U . . .
O3 O 0.9126(5) 0.750000 0.1130(3) 0.0256(8) Uani 1 2 d S T P . .
C3 C 0.7114(5) 0.51854(19) 0.3799(3) 0.0336(9) Uani 1 1 d . . . . .
O5 O 0.7766(5) 0.750000 0.4349(3) 0.0421(11) Uani 1 2 d DS T P . .
H5B H 0.670(3) 0.750000 0.424(5) 0.051 Uiso 1 2 d DS U P . .
H5A H 0.802(10) 0.750000 0.494(2) 0.051 Uiso 1 2 d DS U P . .
C5 C 0.8811(8) 0.4212(2) 0.3594(5) 0.0572(14) Uani 1 1 d . . . . .
H5 H 0.935171 0.391679 0.318320 0.069 Uiso 1 1 calc R U . . .
O4 O 0.6307(4) 0.750000 0.0839(2) 0.0240(8) Uani 1 2 d S T P . .
C4 C 0.7906(7) 0.4736(2) 0.3217(4) 0.0458(11) Uani 1 1 d . . . . .
H4 H 0.783291 0.478377 0.255209 0.055 Uiso 1 1 calc R U . . .
C8 C 0.7210(6) 0.5092(2) 0.4783(4) 0.0452(11) Uani 1 1 d . . . . .
H8 H 0.666851 0.538613 0.519572 0.054 Uiso 1 1 calc R U . . .
C7 C 0.8112(7) 0.4561(3) 0.5162(4) 0.0584(15) Uani 1 1 d . . . . .
H7 H 0.816820 0.450163 0.582598 0.070 Uiso 1 1 calc R U . . .
C6 C 0.8912(7) 0.4128(2) 0.4565(5) 0.0570(15) Uani 1 1 d . . . . .
H6 H 0.952487 0.377740 0.481967 0.068 Uiso 1 1 calc R U . . .
C9 C 0.7816(6) 0.750000 0.0571(3) 0.0179(10) Uani 1 2 d S T P . .
C10 C 0.8021(7) 0.750000 -0.0520(4) 0.0307(13) Uani 1 2 d S T P . .
H10A H 0.743455 0.711578 -0.076939 0.037 Uiso 0.5 1 calc R U P . .
H10B H 0.743455 0.788422 -0.076939 0.037 Uiso 0.5 1 calc R U P . .
C11 C 0.9764(7) 0.750000 -0.0928(4) 0.0272(12) Uani 1 2 d S T P B .
C12 C 1.0582(6) 0.8080(3) -0.1144(4) 0.0591(17) Uani 1 1 d . . . . .
H12 H 0.988840 0.844575 -0.105986 0.071 Uiso 1 1 calc R U . A 1
C13A C 1.2088(12) 0.8235(6) -0.1437(7) 0.042(3) Uiso 0.53(2) 1 d . . P B 1
C14A C 1.2958(19) 0.7380(14) -0.1750(10) 0.021(6) Uiso 0.266(12) 1 d . . P B 1
C13B C 1.2302(15) 0.7927(7) -0.1674(8) 0.032(4) Uiso 0.47(2) 1 d . . P B 2
C14B C 1.301(4) 0.7206(16) -0.1745(19) 0.037(10) Uiso 0.234(12) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O4 2.330(3) 6_656 ?
Dy1 O2 2.396(2) 4_565 ?
Dy1 O2 2.396(2) 6_656 ?
Dy1 O3 2.415(4) . ?
Dy1 O5 2.445(4) . ?
Dy1 O1 2.495(3) . ?
Dy1 O1 2.495(3) 7_575 ?
Dy1 O2 2.512(2) . ?
Dy1 O2 2.512(2) 7_575 ?
Dy1 C1 2.879(4) 7_575 ?
Dy1 C1 2.880(4) . ?
C1 O1 1.238(5) . ?
C1 O2 1.277(4) . ?
C1 C2 1.510(5) . ?
C2 C3 1.502(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O3 C9 1.290(6) . ?
C3 C4 1.369(7) . ?
C3 C8 1.380(7) . ?
O5 H5B 0.85(2) . ?
O5 H5A 0.84(2) . ?
C5 C6 1.361(8) . ?
C5 C4 1.382(7) . ?
C5 H5 0.9300 . ?
O4 C9 1.244(6) . ?
C4 H4 0.9300 . ?
C8 C7 1.395(7) . ?
C8 H8 0.9300 . ?
C7 C6 1.362(9) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C9 C10 1.523(7) . ?
C10 C11 1.484(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.374(6) . ?
C11 C12 1.374(6) 7_575 ?
C12 C13A 1.292(11) . ?
C12 C13B 1.570(14) . ?
C12 H12 0.9300 . ?
C13A C14A 1.49(3) 7_575 ?
C13A C14A 1.92(3) . ?
C14A C14A 0.49(6) 7_575 ?
C13B C14B 0.63(3) 7_575 ?
C13B C14B 1.57(3) . ?
C13B C13B 1.73(3) 7_575 ?
C14B C14B 1.19(6) 7_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Dy1 O2 76.22(10) 6_656 4_565 ?
O4 Dy1 O2 76.22(10) 6_656 6_656 ?
O2 Dy1 O2 68.56(12) 4_565 6_656 ?
O4 Dy1 O3 146.41(12) 6_656 . ?
O2 Dy1 O3 76.15(10) 4_565 . ?
O2 Dy1 O3 76.15(10) 6_656 . ?
O4 Dy1 O5 71.69(13) 6_656 . ?
O2 Dy1 O5 132.56(9) 4_565 . ?
O2 Dy1 O5 132.56(9) 6_656 . ?
O3 Dy1 O5 141.90(13) . . ?
O4 Dy1 O1 83.94(8) 6_656 . ?
O2 Dy1 O1 138.36(9) 4_565 . ?
O2 Dy1 O1 71.34(9) 6_656 . ?
O3 Dy1 O1 104.77(8) . . ?
O5 Dy1 O1 71.35(8) . . ?
O4 Dy1 O1 83.94(8) 6_656 7_575 ?
O2 Dy1 O1 71.34(9) 4_565 7_575 ?
O2 Dy1 O1 138.36(9) 6_656 7_575 ?
O3 Dy1 O1 104.77(8) . 7_575 ?
O5 Dy1 O1 71.35(8) . 7_575 ?
O1 Dy1 O1 142.70(15) . 7_575 ?
O4 Dy1 O2 127.29(8) 6_656 . ?
O2 Dy1 O2 155.67(3) 4_565 . ?
O2 Dy1 O2 107.83(9) 6_656 . ?
O3 Dy1 O2 79.63(9) . . ?
O5 Dy1 O2 68.48(10) . . ?
O1 Dy1 O2 51.54(8) . . ?
O1 Dy1 O2 113.31(9) 7_575 . ?
O4 Dy1 O2 127.29(8) 6_656 7_575 ?
O2 Dy1 O2 107.83(9) 4_565 7_575 ?
O2 Dy1 O2 155.67(3) 6_656 7_575 ?
O3 Dy1 O2 79.63(9) . 7_575 ?
O5 Dy1 O2 68.48(10) . 7_575 ?
O1 Dy1 O2 113.32(9) . 7_575 ?
O1 Dy1 O2 51.53(8) 7_575 7_575 ?
O2 Dy1 O2 64.97(11) . 7_575 ?
O4 Dy1 C1 104.78(9) 6_656 7_575 ?
O2 Dy1 C1 90.47(9) 4_565 7_575 ?
O2 Dy1 C1 158.36(10) 6_656 7_575 ?
O3 Dy1 C1 94.18(9) . 7_575 ?
O5 Dy1 C1 65.83(9) . 7_575 ?
O1 Dy1 C1 130.26(10) . 7_575 ?
O1 Dy1 C1 25.36(10) 7_575 7_575 ?
O2 Dy1 C1 88.97(9) . 7_575 ?
O2 Dy1 C1 26.29(9) 7_575 7_575 ?
O4 Dy1 C1 104.78(9) 6_656 . ?
O2 Dy1 C1 158.36(10) 4_565 . ?
O2 Dy1 C1 90.47(9) 6_656 . ?
O3 Dy1 C1 94.18(9) . . ?
O5 Dy1 C1 65.83(9) . . ?
O1 Dy1 C1 25.36(10) . . ?
O1 Dy1 C1 130.26(10) 7_575 . ?
O2 Dy1 C1 26.29(9) . . ?
O2 Dy1 C1 88.97(9) 7_575 . ?
C1 Dy1 C1 109.74(15) 7_575 . ?
O1 C1 O2 119.9(3) . . ?
O1 C1 C2 121.4(3) . . ?
O2 C1 C2 118.7(3) . . ?
O1 C1 Dy1 59.68(19) . . ?
O2 C1 Dy1 60.60(18) . . ?
C2 C1 Dy1 172.9(3) . . ?
C1 O1 Dy1 95.0(2) . . ?
C1 O2 Dy1 152.8(2) . 6_556 ?
C1 O2 Dy1 93.1(2) . . ?
Dy1 O2 Dy1 111.58(9) 6_556 . ?
C3 C2 C1 114.3(3) . . ?
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 . . ?
C9 O3 Dy1 132.7(3) . . ?
C4 C3 C8 117.9(4) . . ?
C4 C3 C2 121.0(4) . . ?
C8 C3 C2 121.0(4) . . ?
Dy1 O5 H5B 112(5) . . ?
Dy1 O5 H5A 134(5) . . ?
H5B O5 H5A 114(8) . . ?
C6 C5 C4 120.0(5) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C9 O4 Dy1 146.7(3) . 6_556 ?
C3 C4 C5 121.6(5) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C3 C8 C7 120.4(5) . . ?
C3 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C6 C7 C8 120.3(5) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C5 C6 C7 119.7(5) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
O4 C9 O3 125.6(4) . . ?
O4 C9 C10 113.5(4) . . ?
O3 C9 C10 120.9(4) . . ?
C11 C10 C9 118.5(4) . . ?
C11 C10 H10A 107.7 . . ?
C9 C10 H10A 107.7 . . ?
C11 C10 H10B 107.7 . . ?
C9 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
C12 C11 C12 117.8(7) . 7_575 ?
C12 C11 C10 121.1(3) . . ?
C12 C11 C10 121.1(3) 7_575 . ?
C13A C12 C11 135.1(8) . . ?
C11 C12 C13B 109.7(7) . . ?
C13A C12 H12 112.5 . . ?
C11 C12 H12 112.5 . . ?
C12 C13A C14A 107.9(12) . 7_575 ?
C12 C13A C14A 100.2(9) . . ?
C14A C13A C14A 7.9(10) 7_575 . ?
C14A C14A C13A 147.1(8) 7_575 7_575 ?
C14A C14A C13A 25.0(6) 7_575 . ?
C13A C14A C13A 122.0(11) 7_575 . ?
C14B C13B C14B 43(4) 7_575 . ?
C14B C13B C12 158(3) 7_575 . ?
C14B C13B C12 121.3(12) . . ?
C12 C13B C13B 101.4(5) . 7_575 ?
C13B C14B C14B 116(4) 7_575 7_575 ?
C13B C14B C13B 94(4) 7_575 . ?
C14B C14B C13B 21.1(11) 7_575 . ?

_refine_diff_density_max         0.951
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.096

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1574415'
_audit_update_record             
;
2017-09-14 deposited with the CCDC.
2017-11-07 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            'C24 H23 O7 Tb'
_chemical_formula_weight         582.34

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   7.8370(3)
_cell_length_b                   20.3107(8)
_cell_length_c                   13.8607(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2206.28(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.54

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    3.249
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5570
_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            29086
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.986
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1994
_reflns_number_gt                1794
_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)+(0.0349P)²+5.5897P] 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         1994
_refine_ls_number_parameters     163
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0639
_refine_ls_wR_factor_gt          0.0605
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
Tb1 Tb 1.05705(3) 0.750000 0.71389(2) 0.01494(10) Uani 1 2 d S T P . .
C1 C 0.7617(5) 0.6345(2) 0.8131(3) 0.0233(9) Uani 1 1 d . . . . .
O1 O 0.8240(3) 0.68419(13) 0.76826(19) 0.0245(6) Uani 1 1 d . . . . .
O2 O 0.6090(4) 0.63438(15) 0.8350(3) 0.0394(8) Uani 1 1 d . . . . .
C2 C 0.8784(6) 0.5779(2) 0.8377(4) 0.0401(12) Uani 1 1 d . . . . .
H2A H 0.937637 0.564229 0.779596 0.048 Uiso 1 1 calc R U . . .
H2B H 0.963503 0.593122 0.883288 0.048 Uiso 1 1 calc R U . . .
O4 O 0.5886(5) 0.750000 0.6129(3) 0.0297(10) Uani 1 2 d S T P . .
C4 C 0.7797(7) 0.5095(3) 0.9786(4) 0.0484(13) Uani 1 1 d . . . . .
H4 H 0.833566 0.538868 1.020038 0.058 Uiso 1 1 calc R U . . .
O3 O 0.8719(5) 0.750000 0.5848(3) 0.0269(9) Uani 1 2 d S T P . .
C3 C 0.7892(5) 0.5192(2) 0.8799(4) 0.0339(11) Uani 1 1 d . . . . .
C7 C 0.6201(8) 0.4215(3) 0.8596(5) 0.0591(15) Uani 1 1 d . . . . .
H7 H 0.566827 0.391680 0.818577 0.071 Uiso 1 1 calc R U . . .
C6 C 0.6089(8) 0.4131(3) 0.9565(5) 0.0586(16) Uani 1 1 d . . . . .
H6 H 0.546469 0.378215 0.981895 0.070 Uiso 1 1 calc R U . . .
O5 O 1.2237(6) 0.750000 0.5662(3) 0.0471(13) Uani 1 2 d DS T P . .
H5B H 1.331(3) 0.750000 0.563(6) 0.056 Uiso 1 2 d DS U P . .
H5A H 1.180(10) 0.750000 0.511(3) 0.056 Uiso 1 2 d DS U P . .
C5 C 0.6904(8) 0.4563(3) 1.0163(4) 0.0604(17) Uani 1 1 d . . . . .
H5 H 0.686073 0.450024 1.082742 0.072 Uiso 1 1 calc R U . . .
C9 C 0.7196(7) 0.750000 0.5576(4) 0.0189(11) Uani 1 2 d S T P . .
C8 C 0.7101(7) 0.4743(3) 0.8208(4) 0.0482(13) Uani 1 1 d . . . . .
H8 H 0.716763 0.479177 0.754246 0.058 Uiso 1 1 calc R U . . .
C10 C 0.6978(7) 0.750000 0.4487(4) 0.0334(15) Uani 1 2 d S T P . .
H10A H 0.756786 0.788384 0.423756 0.040 Uiso 0.5 1 calc R U P . .
H10B H 0.756785 0.711616 0.423756 0.040 Uiso 0.5 1 calc R U P . .
C11 C 0.5240(7) 0.750000 0.4071(4) 0.0281(14) Uani 1 2 d S T P B .
C12 C 0.4419(7) 0.6923(3) 0.3861(5) 0.0610(17) Uani 1 1 d . . . . .
H12 H 0.482357 0.650451 0.400638 0.073 Uiso 1 1 calc R U . A 1
C13A C 0.2674(16) 0.7078(7) 0.3332(8) 0.044(3) Uiso 0.538(9) 1 d . . P B 1
C14A C 0.193(5) 0.7789(17) 0.324(2) 0.064(15) Uiso 0.269(4) 1 d . . P B 1
C13B C 0.2912(13) 0.6760(6) 0.3564(8) 0.046(3) Uiso 0.538(9) 1 d . . P B 2
C14B C 0.202(2) 0.7374(14) 0.3258(12) 0.020(6) Uiso 0.269(4) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O3 2.304(4) . ?
Tb1 O1 2.386(3) 7_575 ?
Tb1 O1 2.386(3) . ?
Tb1 O4 2.414(4) 6_657 ?
Tb1 O5 2.428(4) . ?
Tb1 O2 2.478(3) 6_657 ?
Tb1 O2 2.478(3) 4_566 ?
Tb1 O1 2.495(3) 4_566 ?
Tb1 O1 2.495(3) 6_657 ?
Tb1 C1 2.867(4) 4_566 ?
Tb1 C1 2.867(4) 6_657 ?
C1 O2 1.235(5) . ?
C1 O1 1.282(5) . ?
C1 C2 1.508(6) . ?
C2 C3 1.500(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
O4 C9 1.281(7) . ?
C4 C3 1.384(7) . ?
C4 C5 1.390(8) . ?
C4 H4 0.9300 . ?
O3 C9 1.251(7) . ?
C3 C8 1.374(7) . ?
C7 C6 1.357(9) . ?
C7 C8 1.390(7) . ?
C7 H7 0.9300 . ?
C6 C5 1.365(9) . ?
C6 H6 0.9300 . ?
O5 H5B 0.84(2) . ?
O5 H5A 0.84(2) . ?
C5 H5 0.9300 . ?
C9 C10 1.519(8) . ?
C8 H8 0.9300 . ?
C10 C11 1.479(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.368(6) . ?
C11 C12 1.368(6) 7_575 ?
C12 C13B 1.294(11) . ?
C12 C13A 1.583(14) . ?
C12 H12 0.9300 . ?
C13A C14A 0.66(4) 7_575 ?
C13A C14A 1.56(3) . ?
C13A C13A 1.72(3) 7_575 ?
C14A C14A 1.17(7) 7_575 ?
C13B C14B 1.49(3) . ?
C13B C14B 1.94(3) 7_575 ?
C14B C14B 0.51(6) 7_575 ?

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 Tb1 O1 76.30(10) . 7_575 ?
O3 Tb1 O1 76.30(10) . . ?
O1 Tb1 O1 68.15(13) 7_575 . ?
O3 Tb1 O4 146.84(13) . 6_657 ?
O1 Tb1 O4 76.36(10) 7_575 6_657 ?
O1 Tb1 O4 76.36(10) . 6_657 ?
O3 Tb1 O5 71.57(15) . . ?
O1 Tb1 O5 132.70(10) 7_575 . ?
O1 Tb1 O5 132.70(10) . . ?
O4 Tb1 O5 141.58(15) 6_657 . ?
O3 Tb1 O2 83.74(8) . 6_657 ?
O1 Tb1 O2 138.01(10) 7_575 6_657 ?
O1 Tb1 O2 71.42(10) . 6_657 ?
O4 Tb1 O2 104.80(9) 6_657 6_657 ?
O5 Tb1 O2 71.39(8) . 6_657 ?
O3 Tb1 O2 83.74(8) . 4_566 ?
O1 Tb1 O2 71.42(10) 7_575 4_566 ?
O1 Tb1 O2 138.01(10) . 4_566 ?
O4 Tb1 O2 104.80(9) 6_657 4_566 ?
O5 Tb1 O2 71.39(8) . 4_566 ?
O2 Tb1 O2 142.77(17) 6_657 4_566 ?
O3 Tb1 O1 127.24(9) . 4_566 ?
O1 Tb1 O1 108.09(9) 7_575 4_566 ?
O1 Tb1 O1 155.63(3) . 4_566 ?
O4 Tb1 O1 79.37(10) 6_657 4_566 ?
O5 Tb1 O1 68.45(11) . 4_566 ?
O2 Tb1 O1 113.39(9) 6_657 4_566 ?
O2 Tb1 O1 51.80(9) 4_566 4_566 ?
O3 Tb1 O1 127.24(9) . 6_657 ?
O1 Tb1 O1 155.63(3) 7_575 6_657 ?
O1 Tb1 O1 108.09(9) . 6_657 ?
O4 Tb1 O1 79.37(10) 6_657 6_657 ?
O5 Tb1 O1 68.45(11) . 6_657 ?
O2 Tb1 O1 51.80(9) 6_657 6_657 ?
O2 Tb1 O1 113.39(9) 4_566 6_657 ?
O1 Tb1 O1 64.79(12) 4_566 6_657 ?
O3 Tb1 C1 104.53(10) . 4_566 ?
O1 Tb1 C1 90.64(10) 7_575 4_566 ?
O1 Tb1 C1 158.16(10) . 4_566 ?
O4 Tb1 C1 94.16(10) 6_657 4_566 ?
O5 Tb1 C1 65.73(10) . 4_566 ?
O2 Tb1 C1 130.39(11) 6_657 4_566 ?
O2 Tb1 C1 25.40(11) 4_566 4_566 ?
O1 Tb1 C1 26.53(10) 4_566 4_566 ?
O1 Tb1 C1 88.99(10) 6_657 4_566 ?
O3 Tb1 C1 104.53(10) . 6_657 ?
O1 Tb1 C1 158.16(10) 7_575 6_657 ?
O1 Tb1 C1 90.64(10) . 6_657 ?
O4 Tb1 C1 94.16(10) 6_657 6_657 ?
O5 Tb1 C1 65.73(9) . 6_657 ?
O2 Tb1 C1 25.40(11) 6_657 6_657 ?
O2 Tb1 C1 130.39(11) 4_566 6_657 ?
O1 Tb1 C1 88.99(10) 4_566 6_657 ?
O1 Tb1 C1 26.53(10) 6_657 6_657 ?
C1 Tb1 C1 109.87(16) 4_566 6_657 ?
O2 C1 O1 119.3(4) . . ?
O2 C1 C2 122.0(4) . . ?
O1 C1 C2 118.6(4) . . ?
O2 C1 Tb1 59.4(2) . 6_557 ?
O1 C1 Tb1 60.3(2) . 6_557 ?
C2 C1 Tb1 173.1(3) . 6_557 ?
C1 O1 Tb1 152.3(3) . . ?
C1 O1 Tb1 93.1(2) . 6_557 ?
Tb1 O1 Tb1 111.91(10) . 6_557 ?
C1 O2 Tb1 95.2(2) . 6_557 ?
C3 C2 C1 114.3(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 . . ?
C9 O4 Tb1 132.6(3) . 6_557 ?
C3 C4 C5 120.7(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C9 O3 Tb1 146.6(4) . . ?
C8 C3 C4 118.0(5) . . ?
C8 C3 C2 120.4(5) . . ?
C4 C3 C2 121.6(5) . . ?
C6 C7 C8 120.8(6) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C6 C5 119.3(5) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
Tb1 O5 H5B 125(6) . . ?
Tb1 O5 H5A 123(6) . . ?
H5B O5 H5A 111(8) . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
O3 C9 O4 125.8(5) . . ?
O3 C9 C10 114.0(5) . . ?
O4 C9 C10 120.2(5) . . ?
C3 C8 C7 120.7(5) . . ?
C3 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C11 C10 C9 119.4(5) . . ?
C11 C10 H10A 107.5 . . ?
C9 C10 H10A 107.5 . . ?
C11 C10 H10B 107.5 . . ?
C9 C10 H10B 107.5 . . ?
H10A C10 H10B 107.0 . . ?
C12 C11 C12 117.8(7) . 7_575 ?
C12 C11 C10 121.1(4) . . ?
C12 C11 C10 121.1(4) 7_575 . ?
C13B C12 C11 135.8(8) . . ?
C11 C12 C13A 109.6(7) . . ?
C11 C12 H12 125.2 . . ?
C13A C12 H12 125.2 . . ?
C14A C13A C14A 43(4) 7_575 . ?
C14A C13A C12 160(4) 7_575 . ?
C14A C13A C12 123.0(16) . . ?
C14A C13A C13A 66(4) 7_575 7_575 ?
C14A C13A C13A 22.5(14) . 7_575 ?
C12 C13A C13A 101.4(5) . 7_575 ?
C13A C14A C14A 114(4) 7_575 7_575 ?
C13A C14A C13A 92(4) 7_575 . ?
C14A C14A C13A 22.5(14) 7_575 . ?
C12 C13B C14B 107.6(12) . . ?
C12 C13B C14B 99.5(10) . 7_575 ?
C14B C13B C14B 8.3(10) . 7_575 ?
C14B C14B C13B 146.8(9) 7_575 . ?

_refine_diff_density_max         0.468
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.101

