# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

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

data_fq36-sw-1
_database_code_depnum_ccdc_archive 'CCDC 1437010'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 1'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H20 O29 Tb2'
_chemical_formula_weight         982.15

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6093(4)
_cell_length_b                   9.1855(4)
_cell_length_c                   9.5881(4)
_cell_angle_alpha                94.5500(10)
_cell_angle_beta                 94.0690(10)
_cell_angle_gamma                96.6840(10)
_cell_volume                     748.24(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             472
_exptl_absorpt_coefficient_mu    4.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_T_max  0.619
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10469
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         28.35
_reflns_number_total             3716
_reflns_number_gt                3629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.3274P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3716
_refine_ls_number_parameters     252
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.1439
_refine_ls_wR_factor_gt          0.1430
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_restrained_S_all      1.353
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.32739(2) 0.23233(2) 0.27942(2) 0.01941(14) Uani 1 1 d . . 3
C1 C 0.1024(7) 0.5189(6) 0.3510(6) 0.0202(10) Uani 1 1 d . A 3
C2 C 0.1260(7) 0.6797(5) 0.3727(6) 0.0201(10) Uani 1 1 d . A 3
C3 C -0.0260(6) 0.7297(6) 0.3370(6) 0.0254(11) Uani 1 1 d . A 3
C4 C -0.1408(7) 0.5998(6) 0.3030(6) 0.0263(11) Uani 1 1 d . A 3
C5 C -0.0605(6) 0.4691(6) 0.3127(6) 0.0217(10) Uani 1 1 d . A 3
C6 C 0.2014(12) -0.1229(7) 0.0832(10) 0.054(5) Uani 0.50 1 d PG B 3
C7 C 0.0563(11) -0.1142(7) 0.0249(10) 0.044(4) Uani 0.50 1 d PGD B 3
C8 C -0.0112(9) -0.2517(10) -0.0170(9) 0.037(3) Uani 0.50 1 d PG . 3
C9 C 0.0921(11) -0.3454(9) 0.0154(8) 0.031(3) Uani 0.50 1 d PG . 3
C10 C 0.2235(12) -0.2658(10) 0.0773(8) 0.031(3) Uani 0.50 1 d PG B 3
O1 O 0.2120(5) 0.4375(5) 0.3681(5) 0.0283(9) Uani 1 1 d . A 3
O2 O 0.2515(6) 0.7557(5) 0.4113(6) 0.0365(11) Uani 1 1 d . A 3
O3 O -0.0557(8) 0.8583(6) 0.3313(9) 0.0477(16) Uani 1 1 d . A 3
O4 O -0.2816(7) 0.6016(7) 0.2684(9) 0.0447(16) Uani 1 1 d . A 3
O5 O -0.1237(5) 0.3382(4) 0.2903(5) 0.0305(9) Uani 1 1 d . A 3
O6 O 0.2975(6) 0.0024(6) 0.1394(7) 0.0424(13) Uani 0.50 1 d P B 3
O6W O 0.2975(6) 0.0024(6) 0.1394(7) 0.0424(13) Uani 0.50 1 d P B 3
O7 O 0.0000 0.0000 0.0000 0.065(3) Uani 1 2 d SDU . 3
O8 O -0.1564(18) -0.2854(18) -0.0882(17) 0.027(3) Uani 0.50 1 d PU . 3
O8W O 0.1886(18) 0.2665(17) 0.0650(16) 0.033(3) Uani 0.50 1 d P . 3
O9 O 0.0608(14) -0.4820(11) 0.0007(12) 0.036(2) Uani 0.50 1 d PU . 3
O10 O 0.3485(14) -0.3086(14) 0.1121(12) 0.039(2) Uani 0.50 1 d PU B 3
O11 O 0.4571(6) 0.4290(6) 0.1690(6) 0.0393(11) Uani 1 1 d . C 3
H11A H 0.5472 0.4686 0.1899 0.059 Uiso 1 1 d R C 3
H11B H 0.4064 0.4903 0.1356 0.059 Uiso 1 1 d R C 3
O12 O 0.4838(6) 0.3453(5) 0.4854(6) 0.0351(10) Uani 1 1 d . D 3
H12A H 0.5785 0.3553 0.5103 0.053 Uiso 1 1 d R D 3
H12B H 0.4392 0.3752 0.5530 0.053 Uiso 1 1 d R D 3
O13 O 0.5845(6) 0.1744(6) 0.2422(7) 0.0447(12) Uani 1 1 d . E 3
H13A H 0.6544 0.2409 0.2288 0.067 Uiso 1 1 d R E 3
H13B H 0.6304 0.1015 0.2609 0.067 Uiso 1 1 d R E 3
O14 O 0.3530(7) 0.0488(6) 0.4415(7) 0.0408(13) Uani 1 1 d . F 3
H14A H 0.3650 0.0570 0.5276 0.061 Uiso 1 1 d R F 3
H14B H 0.2928 -0.0276 0.4178 0.061 Uiso 1 1 d R F 3
O15 O 0.0748(5) 0.1373(5) 0.3283(6) 0.0366(11) Uani 1 1 d . G 3
H15A H 0.0226 0.2062 0.3111 0.055 Uiso 1 1 d R G 3
H15B H 0.0235 0.0619 0.2890 0.055 Uiso 1 1 d R G 3
O16A O 0.3797(13) 0.1032(11) 0.7397(14) 0.060(4) Uani 0.68(3) 1 d PU H 1
O16B O 0.380(3) 0.112(2) 0.838(3) 0.051(7) Uani 0.32(3) 1 d PU H 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 O15 2.340(5) . ?
Tb1 O1 2.359(4) . ?
Tb1 O8W 2.366(13) . ?
Tb1 O11 2.373(5) . ?
Tb1 O13 2.381(5) . ?
Tb1 O8 2.386(17) 2 ?
Tb1 O6 2.389(5) . ?
Tb1 O14 2.399(6) . ?
Tb1 O12 2.401(5) . ?
C1 O1 1.279(7) . ?
C1 C5 1.435(8) . ?
C1 C2 1.463(7) . ?
C2 O2 1.233(7) . ?
C2 C3 1.463(8) . ?
C3 O3 1.242(8) . ?
C3 C4 1.458(8) . ?
C4 O4 1.236(9) . ?
C4 C5 1.460(8) . ?
C5 O5 1.256(7) . ?
C6 C7 1.346(6) . ?
C6 C10 1.346(6) . ?
C6 O6 1.384(9) . ?
C7 O7 1.238(5) . ?
C7 C8 1.346(6) . ?
C8 C9 1.346(6) . ?
C8 O8 1.371(18) . ?
C8 O8W 1.550(16) 2 ?
C9 O9 1.247(13) . ?
C9 C10 1.346(6) . ?
C9 O9 1.928(14) 2_545 ?
C10 O10 1.221(15) . ?
O7 C7 1.238(14) 2 ?
O8 O8W 0.41(2) 2 ?
O8 Tb1 2.386(17) 2 ?
O8W O8 0.41(2) 2 ?
O8W C8 1.55(3) 2 ?
O9 O9 1.06(2) 2_545 ?
O9 C9 1.93(2) 2_545 ?
O11 H11A 0.8216 . ?
O11 H11B 0.8215 . ?
O12 H12A 0.8256 . ?
O12 H12B 0.8215 . ?
O13 H13A 0.8308 . ?
O13 H13B 0.8409 . ?
O14 H14A 0.8216 . ?
O14 H14B 0.8281 . ?
O15 H15A 0.8373 . ?
O15 H15B 0.8250 . ?

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
O15 Tb1 O1 74.84(16) . . ?
O15 Tb1 O8W 80.8(4) . . ?
O1 Tb1 O8W 84.4(4) . . ?
O15 Tb1 O11 140.24(17) . . ?
O1 Tb1 O11 77.06(17) . . ?
O8W Tb1 O11 69.0(4) . . ?
O15 Tb1 O13 144.93(18) . . ?
O1 Tb1 O13 137.24(16) . . ?
O8W Tb1 O13 111.0(4) . . ?
O11 Tb1 O13 72.6(2) . . ?
O15 Tb1 O8 74.3(4) . 2 ?
O1 Tb1 O8 75.6(4) . 2 ?
O8W Tb1 O8 9.9(5) . 2 ?
O11 Tb1 O8 71.9(4) . 2 ?
O13 Tb1 O8 120.6(4) . 2 ?
O15 Tb1 O6 79.69(19) . . ?
O1 Tb1 O6 148.25(16) . . ?
O8W Tb1 O6 72.9(4) . . ?
O11 Tb1 O6 113.4(2) . . ?
O13 Tb1 O6 73.13(18) . . ?
O8 Tb1 O6 79.5(4) 2 . ?
O15 Tb1 O14 72.2(2) . . ?
O1 Tb1 O14 114.4(2) . . ?
O8W Tb1 O14 140.5(4) . . ?
O11 Tb1 O14 146.38(19) . . ?
O13 Tb1 O14 79.3(2) . . ?
O8 Tb1 O14 140.4(4) 2 . ?
O6 Tb1 O14 74.3(2) . . ?
O15 Tb1 O12 112.53(19) . . ?
O1 Tb1 O12 71.31(16) . . ?
O8W Tb1 O12 147.0(4) . . ?
O11 Tb1 O12 83.76(18) . . ?
O13 Tb1 O12 76.06(18) . . ?
O8 Tb1 O12 142.4(4) 2 . ?
O6 Tb1 O12 137.42(17) . . ?
O14 Tb1 O12 71.69(18) . . ?
O1 C1 C5 126.3(5) . . ?
O1 C1 C2 123.9(5) . . ?
C5 C1 C2 109.7(5) . . ?
O2 C2 C3 127.8(5) . . ?
O2 C2 C1 125.6(5) . . ?
C3 C2 C1 106.6(5) . . ?
O3 C3 C4 124.4(6) . . ?
O3 C3 C2 127.8(6) . . ?
C4 C3 C2 107.8(5) . . ?
O4 C4 C3 125.2(6) . . ?
O4 C4 C5 126.3(6) . . ?
C3 C4 C5 108.5(5) . . ?
O5 C5 C1 127.1(5) . . ?
O5 C5 C4 125.7(5) . . ?
C1 C5 C4 107.2(5) . . ?
C7 C6 C10 108.0 . . ?
C7 C6 O6 120.8(7) . . ?
C10 C6 O6 131.1(7) . . ?
O7 C7 C6 126.4(7) . . ?
O7 C7 C8 125.2(7) . . ?
C6 C7 C8 108.0 . . ?
C9 C8 C7 108.0 . . ?
C9 C8 O8 127.4(9) . . ?
C7 C8 O8 124.5(9) . . ?
C9 C8 O8W 135.5(9) . 2 ?
C7 C8 O8W 115.5(9) . 2 ?
O9 C9 C8 123.9(9) . . ?
O9 C9 C10 127.8(9) . . ?
C8 C9 C10 108.0 . . ?
C8 C9 O9 95.4(7) . 2_545 ?
C10 C9 O9 150.9(6) . 2_545 ?
O10 C10 C9 128.2(9) . . ?
O10 C10 C6 123.5(9) . . ?
C9 C10 C6 108.0 . . ?
C1 O1 Tb1 146.6(4) . . ?
C6 O6 Tb1 148.8(5) . . ?
C7 O7 C7 180.0(11) . 2 ?
O8W O8 C8 108(4) 2 . ?
O8W O8 Tb1 82(4) 2 2 ?
C8 O8 Tb1 145.8(11) . 2 ?
O8 O8W C8 57(4) 2 2 ?
O8 O8W Tb1 88(4) 2 . ?
C8 O8W Tb1 132.8(15) 2 . ?
O9 O9 C9 113.2(16) 2_545 . ?
C9 O9 C9 149.7(10) . 2_545 ?
Tb1 O11 H11A 125.9 . . ?
Tb1 O11 H11B 119.9 . . ?
H11A O11 H11B 107.8 . . ?
Tb1 O12 H12A 134.2 . . ?
Tb1 O12 H12B 118.7 . . ?
H12A O12 H12B 106.8 . . ?
Tb1 O13 H13A 119.7 . . ?
Tb1 O13 H13B 131.7 . . ?
H13A O13 H13B 106.3 . . ?
Tb1 O14 H14A 130.3 . . ?
Tb1 O14 H14B 112.2 . . ?
H14A O14 H14B 107.2 . . ?
Tb1 O15 H15A 102.3 . . ?
Tb1 O15 H15B 125.7 . . ?
H15A O15 H15B 105.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 -1.1(10) . . . . ?
C5 C1 C2 O2 177.2(6) . . . . ?
O1 C1 C2 C3 177.8(5) . . . . ?
C5 C1 C2 C3 -3.9(6) . . . . ?
O2 C2 C3 O3 4.4(12) . . . . ?
C1 C2 C3 O3 -174.5(7) . . . . ?
O2 C2 C3 C4 -177.6(6) . . . . ?
C1 C2 C3 C4 3.5(6) . . . . ?
O3 C3 C4 O4 -2.1(12) . . . . ?
C2 C3 C4 O4 179.8(7) . . . . ?
O3 C3 C4 C5 176.2(7) . . . . ?
C2 C3 C4 C5 -1.9(7) . . . . ?
O1 C1 C5 O5 0.5(10) . . . . ?
C2 C1 C5 O5 -177.8(5) . . . . ?
O1 C1 C5 C4 -179.0(5) . . . . ?
C2 C1 C5 C4 2.8(6) . . . . ?
O4 C4 C5 O5 -1.8(11) . . . . ?
C3 C4 C5 O5 180.0(6) . . . . ?
O4 C4 C5 C1 177.7(7) . . . . ?
C3 C4 C5 C1 -0.5(6) . . . . ?
C10 C6 C7 O7 -172.9(10) . . . . ?
O6 C6 C7 O7 8.8(10) . . . . ?
C10 C6 C7 C8 0.0 . . . . ?
O6 C6 C7 C8 -178.4(9) . . . . ?
O7 C7 C8 C9 173.0(10) . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
O7 C7 C8 O8 -3.2(13) . . . . ?
C6 C7 C8 O8 -176.2(12) . . . . ?
O7 C7 C8 O8W -16.6(12) . . . 2 ?
C6 C7 C8 O8W 170.4(10) . . . 2 ?
C7 C8 C9 O9 173.9(11) . . . . ?
O8 C8 C9 O9 -10.1(14) . . . . ?
O8W C8 C9 O9 6.2(15) 2 . . . ?
C7 C8 C9 C10 0.0 . . . . ?
O8 C8 C9 C10 176.1(12) . . . . ?
O8W C8 C9 C10 -167.7(13) 2 . . . ?
C7 C8 C9 O9 162.6(7) . . . 2_545 ?
O8 C8 C9 O9 -21.3(11) . . . 2_545 ?
O8W C8 C9 O9 -5.1(12) 2 . . 2_545 ?
O9 C9 C10 O10 12.8(14) . . . . ?
C8 C9 C10 O10 -173.7(11) . . . . ?
O9 C9 C10 O10 44.2(17) 2_545 . . . ?
O9 C9 C10 C6 -173.6(12) . . . . ?
C8 C9 C10 C6 0.0 . . . . ?
O9 C9 C10 C6 -142.1(15) 2_545 . . . ?
C7 C6 C10 O10 174.1(11) . . . . ?
O6 C6 C10 O10 -7.8(13) . . . . ?
C7 C6 C10 C9 0.0 . . . . ?
O6 C6 C10 C9 178.1(11) . . . . ?
C5 C1 O1 Tb1 45.3(10) . . . . ?
C2 C1 O1 Tb1 -136.7(6) . . . . ?
O15 Tb1 O1 C1 -62.7(7) . . . . ?
O8W Tb1 O1 C1 19.2(8) . . . . ?
O11 Tb1 O1 C1 88.9(7) . . . . ?
O13 Tb1 O1 C1 134.3(7) . . . . ?
O8 Tb1 O1 C1 14.6(8) 2 . . . ?
O6 Tb1 O1 C1 -24.9(9) . . . . ?
O14 Tb1 O1 C1 -124.6(7) . . . . ?
O12 Tb1 O1 C1 176.6(8) . . . . ?
C7 C6 O6 Tb1 44.2(14) . . . . ?
C10 C6 O6 Tb1 -133.7(9) . . . . ?
O15 Tb1 O6 C6 9.2(10) . . . . ?
O1 Tb1 O6 C6 -27.8(13) . . . . ?
O8W Tb1 O6 C6 -74.2(12) . . . . ?
O11 Tb1 O6 C6 -131.4(11) . . . . ?
O13 Tb1 O6 C6 166.8(11) . . . . ?
O8 Tb1 O6 C6 -66.5(11) 2 . . . ?
O14 Tb1 O6 C6 83.5(11) . . . . ?
O12 Tb1 O6 C6 121.4(10) . . . . ?
C9 C8 O8 O8W 129(4) . . . 2 ?
C7 C8 O8 O8W -56(5) . . . 2 ?
C9 C8 O8 Tb1 -127.6(15) . . . 2 ?
C7 C8 O8 Tb1 48(2) . . . 2 ?
O8W C8 O8 Tb1 104(5) 2 . . 2 ?
O15 Tb1 O8W O8 49(4) . . . 2 ?
O1 Tb1 O8W O8 -27(4) . . . 2 ?
O11 Tb1 O8W O8 -105(4) . . . 2 ?
O13 Tb1 O8W O8 -166(4) . . . 2 ?
O6 Tb1 O8W O8 131(4) . . . 2 ?
O14 Tb1 O8W O8 95(4) . . . 2 ?
O12 Tb1 O8W O8 -69(4) . . . 2 ?
O15 Tb1 O8W C8 9.5(14) . . . 2 ?
O1 Tb1 O8W C8 -66.1(15) . . . 2 ?
O11 Tb1 O8W C8 -144.3(16) . . . 2 ?
O13 Tb1 O8W C8 155.1(14) . . . 2 ?
O8 Tb1 O8W C8 -39(4) 2 . . 2 ?
O6 Tb1 O8W C8 91.4(15) . . . 2 ?
O14 Tb1 O8W C8 56.3(17) . . . 2 ?
O12 Tb1 O8W C8 -108.1(15) . . . 2 ?
C8 C9 O9 O9 -23(2) . . . 2_545 ?
C10 C9 O9 O9 149.9(13) . . . 2_545 ?
C8 C9 O9 C9 -23(2) . . . 2_545 ?
C10 C9 O9 C9 150(2) . . . 2_545 ?
O9 C9 O9 C9 0.0(12) 2_545 . . 2_545 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11A O4 0.82 1.87 2.667(8) 161.9 1_655
O11 H11B O10 0.82 1.99 2.765(13) 155.8 1_565
O12 H12A O2 0.83 2.01 2.711(7) 141.7 2_666
O12 H12A O1 0.83 2.60 3.260(6) 137.3 2_666
O12 H12B O4 0.82 2.27 3.073(10) 165.1 2_566
O13 H13A O5 0.83 2.04 2.763(6) 145.4 1_655
O15 H15A O5 0.84 1.86 2.685(6) 168.8 .
O15 H15B O3 0.82 2.00 2.679(8) 139.5 1_545

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         3.894
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.198
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fy97-1_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1437011'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 2'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H12 K O16 Tb'
_chemical_formula_weight         586.22

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   20.232(4)
_cell_length_b                   9.0720(18)
_cell_length_c                   16.015(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.84(3)
_cell_angle_gamma                90.00
_cell_volume                     2622.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'synchrotron, 3W1A at BSRF'
_diffrn_radiation_monochromator  'double crystal monochromator'
_diffrn_measurement_device_type  mar555
_diffrn_measurement_method       'oscillation mode'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4257
_diffrn_reflns_av_R_equivalents  0.0124
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.04
_reflns_number_total             2281
_reflns_number_gt                2232
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1522P)²+41.2818P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0126(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2281
_refine_ls_number_parameters     133
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1771
_refine_ls_wR_factor_gt          0.1724
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.015
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.0000 1.04667(4) 0.2500 0.0088(4) Uani 1 2 d S . .
K1 K 0.1143(3) 0.6821(6) 0.4368(4) 0.0505(12) Uani 0.50 1 d P . .
C1 C 0.0741(4) 0.7488(8) 0.1860(5) 0.0106(15) Uani 1 1 d . . .
C2 C 0.0771(4) 0.7806(8) 0.0990(5) 0.0110(14) Uani 1 1 d . . .
C3 C 0.0840(4) 0.6389(8) 0.0595(5) 0.0130(15) Uani 1 1 d . . .
C4 C 0.0855(5) 0.5211(10) 0.1227(6) 0.0118(16) Uani 1 1 d . . .
C5 C 0.0816(4) 0.5902(9) 0.2032(5) 0.0111(14) Uani 1 1 d . . .
O1 O 0.0690(3) 0.8412(5) 0.2417(4) 0.0152(11) Uani 1 1 d . . .
O2 O 0.0754(3) 0.9047(6) 0.0643(4) 0.0163(11) Uani 1 1 d . . .
O3 O 0.0900(4) 0.6181(6) -0.0137(4) 0.0234(13) Uani 1 1 d . . .
O4 O 0.0906(4) 0.3882(7) 0.1080(5) 0.0223(13) Uani 1 1 d . . .
O5 O 0.0858(4) 0.5262(6) 0.2743(5) 0.0165(13) Uani 1 1 d . . .
O6 O 0.0766(4) 0.9689(5) 0.4072(4) 0.0143(12) Uani 1 1 d . . .
H6A H 0.1092 1.0115 0.4526 0.021 Uiso 1 1 d R . .
H6B H 0.0381 0.9745 0.4138 0.021 Uiso 1 1 d R . .
O7 O -0.0663(3) 1.1289(6) 0.3310(4) 0.0186(13) Uani 1 1 d U . .
H7A H -0.0495 1.0883 0.3832 0.028 Uiso 1 1 d R . .
H7B H -0.0721 1.2163 0.3408 0.028 Uiso 1 1 d R . .
O8 O 0.0746(3) 1.2500(5) 0.3322(4) 0.0184(12) Uani 1 1 d . . .
H8A H 0.0796 1.2924 0.3821 0.028 Uiso 1 1 d R . .
H8B H 0.0609 1.3272 0.3008 0.028 Uiso 1 1 d R . .


_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 O7 2.368(5) . ?
Tb1 O7 2.368(5) 2 ?
Tb1 O1 2.369(5) 2 ?
Tb1 O1 2.369(5) . ?
Tb1 O8 2.370(5) 2 ?
Tb1 O8 2.370(5) . ?
Tb1 O6 2.391(6) . ?
Tb1 O6 2.391(6) 2 ?
Tb1 K1 4.357(5) 2 ?
Tb1 H6B 2.4650 . ?
K1 O6 2.693(7) . ?
K1 O5 2.783(9) . ?
K1 O3 2.940(8) 6_566 ?
K1 O4 3.057(8) 6_566 ?
K1 O1 3.178(7) . ?
K1 C1 3.463(9) 2 ?
K1 H6A 3.0050 . ?
K1 H6B 3.0065 . ?
C1 O1 1.262(9) . ?
C1 C2 1.452(11) . ?
C1 C5 1.459(11) . ?
C1 K1 3.463(9) 2 ?
C2 O2 1.250(10) . ?
C2 C3 1.466(10) . ?
C3 O3 1.245(10) . ?
C3 C4 1.463(11) . ?
C4 O4 1.242(12) . ?
C4 C5 1.468(12) . ?
C5 O5 1.246(10) . ?
O3 K1 2.940(8) 6_565 ?
O4 K1 3.057(8) 6_565 ?
O6 H6A 0.8247 . ?
O6 H6B 0.8323 . ?
O7 H7A 0.8320 . ?
O7 H7B 0.8269 . ?
O8 H8A 0.8503 . ?
O8 H8B 0.8342 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Tb1 O7 143.3(3) . 2 ?
O7 Tb1 O1 73.93(18) . 2 ?
O7 Tb1 O1 140.59(18) 2 2 ?
O7 Tb1 O1 140.59(18) . . ?
O7 Tb1 O1 73.92(18) 2 . ?
O1 Tb1 O1 76.2(3) 2 . ?
O7 Tb1 O8 71.54(19) . 2 ?
O7 Tb1 O8 80.0(2) 2 2 ?
O1 Tb1 O8 113.56(19) 2 2 ?
O1 Tb1 O8 145.57(18) . 2 ?
O7 Tb1 O8 80.0(2) . . ?
O7 Tb1 O8 71.54(19) 2 . ?
O1 Tb1 O8 145.57(18) 2 . ?
O1 Tb1 O8 113.56(19) . . ?
O8 Tb1 O8 77.8(3) 2 . ?
O7 Tb1 O6 76.9(2) . . ?
O7 Tb1 O6 114.3(2) 2 . ?
O1 Tb1 O6 80.03(19) 2 . ?
O1 Tb1 O6 73.07(19) . . ?
O8 Tb1 O6 139.64(18) 2 . ?
O8 Tb1 O6 72.38(18) . . ?
O7 Tb1 O6 114.3(2) . 2 ?
O7 Tb1 O6 76.9(2) 2 2 ?
O1 Tb1 O6 73.07(19) 2 2 ?
O1 Tb1 O6 80.02(19) . 2 ?
O8 Tb1 O6 72.38(18) 2 2 ?
O8 Tb1 O6 139.64(18) . 2 ?
O6 Tb1 O6 145.7(2) . 2 ?
O7 Tb1 K1 111.04(17) . 2 ?
O7 Tb1 K1 96.85(16) 2 2 ?
O1 Tb1 K1 45.37(14) 2 2 ?
O1 Tb1 K1 60.51(15) . 2 ?
O8 Tb1 K1 101.64(15) 2 2 ?
O8 Tb1 K1 168.34(15) . 2 ?
O6 Tb1 K1 112.93(15) . 2 ?
O6 Tb1 K1 33.11(14) 2 2 ?
O7 Tb1 H6B 58.9 . . ?
O7 Tb1 H6B 133.2 2 . ?
O1 Tb1 H6B 68.9 2 . ?
O1 Tb1 H6B 86.7 . . ?
O8 Tb1 H6B 127.8 2 . ?
O8 Tb1 H6B 78.5 . . ?
O6 Tb1 H6B 19.7 . . ?
O6 Tb1 H6B 141.7 2 . ?
K1 Tb1 H6B 110.1 2 . ?
O6 K1 O5 113.8(3) . . ?
O6 K1 O3 150.9(3) . 6_566 ?
O5 K1 O3 78.0(2) . 6_566 ?
O6 K1 O4 102.2(2) . 6_566 ?
O5 K1 O4 133.1(3) . 6_566 ?
O3 K1 O4 56.74(19) 6_566 6_566 ?
O6 K1 O1 57.00(19) . . ?
O5 K1 O1 57.70(18) . . ?
O3 K1 O1 132.6(2) 6_566 . ?
O4 K1 O1 152.2(2) 6_566 . ?
O6 K1 C1 65.1(2) . 2 ?
O5 K1 C1 81.3(2) . 2 ?
O3 K1 C1 92.3(2) 6_566 2 ?
O4 K1 C1 88.1(2) 6_566 2 ?
O1 K1 C1 66.91(19) . 2 ?
O6 K1 H6A 15.4 . . ?
O5 K1 H6A 125.7 . . ?
O3 K1 H6A 151.9 6_566 . ?
O4 K1 H6A 96.1 6_566 . ?
O1 K1 H6A 68.0 . . ?
C1 K1 H6A 78.7 2 . ?
O6 K1 H6B 15.6 . . ?
O5 K1 H6B 117.1 . . ?
O3 K1 H6B 135.4 6_566 . ?
O4 K1 H6B 90.8 6_566 . ?
O1 K1 H6B 64.8 . . ?
C1 K1 H6B 53.4 2 . ?
H6A K1 H6B 25.5 . . ?
O1 C1 C2 126.8(7) . . ?
O1 C1 C5 123.8(7) . . ?
C2 C1 C5 109.3(6) . . ?
O1 C1 K1 95.6(4) . 2 ?
C2 C1 K1 90.1(4) . 2 ?
C5 C1 K1 85.9(4) . 2 ?
O2 C2 C1 127.0(7) . . ?
O2 C2 C3 126.0(6) . . ?
C1 C2 C3 107.1(6) . . ?
O3 C3 C4 124.1(7) . . ?
O3 C3 C2 127.4(7) . . ?
C4 C3 C2 108.5(6) . . ?
O4 C4 C3 123.8(7) . . ?
O4 C4 C5 128.5(8) . . ?
C3 C4 C5 107.7(7) . . ?
O5 C5 C1 126.1(7) . . ?
O5 C5 C4 126.5(7) . . ?
C1 C5 C4 107.3(7) . . ?
C1 O1 Tb1 143.2(5) . . ?
C1 O1 K1 108.3(4) . . ?
Tb1 O1 K1 102.6(2) . . ?
C3 O3 K1 119.6(5) . 6_565 ?
C4 O4 K1 115.6(6) . 6_565 ?
C5 O5 K1 121.2(5) . . ?
Tb1 O6 K1 117.9(3) . . ?
Tb1 O6 H6A 132.1 . . ?
K1 O6 H6A 104.3 . . ?
Tb1 O6 H6B 85.2 . . ?
K1 O6 H6B 104.1 . . ?
H6A O6 H6B 106.4 . . ?
Tb1 O7 H7A 109.6 . . ?
Tb1 O7 H7B 124.8 . . ?
H7A O7 H7B 105.2 . . ?
Tb1 O8 H8A 130.5 . . ?
Tb1 O8 H8B 111.3 . . ?
H8A O8 H8B 93.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 0.1(12) . . . . ?
C5 C1 C2 O2 -177.0(7) . . . . ?
K1 C1 C2 O2 97.2(7) 2 . . . ?
O1 C1 C2 C3 179.1(7) . . . . ?
C5 C1 C2 C3 2.0(8) . . . . ?
K1 C1 C2 C3 -83.8(5) 2 . . . ?
O2 C2 C3 O3 0.7(13) . . . . ?
C1 C2 C3 O3 -178.3(8) . . . . ?
O2 C2 C3 C4 178.8(7) . . . . ?
C1 C2 C3 C4 -0.2(8) . . . . ?
O3 C3 C4 O4 -2.2(13) . . . . ?
C2 C3 C4 O4 179.6(7) . . . . ?
O3 C3 C4 C5 176.6(7) . . . . ?
C2 C3 C4 C5 -1.6(8) . . . . ?
O1 C1 C5 O5 -1.8(12) . . . . ?
C2 C1 C5 O5 175.4(7) . . . . ?
K1 C1 C5 O5 -95.9(7) 2 . . . ?
O1 C1 C5 C4 179.8(7) . . . . ?
C2 C1 C5 C4 -3.0(8) . . . . ?
K1 C1 C5 C4 85.7(5) 2 . . . ?
O4 C4 C5 O5 3.1(13) . . . . ?
C3 C4 C5 O5 -175.6(7) . . . . ?
O4 C4 C5 C1 -178.5(8) . . . . ?
C3 C4 C5 C1 2.8(8) . . . . ?
C2 C1 O1 Tb1 51.2(12) . . . . ?
C5 C1 O1 Tb1 -132.0(7) . . . . ?
K1 C1 O1 Tb1 -43.2(8) 2 . . . ?
C2 C1 O1 K1 -163.2(6) . . . . ?
C5 C1 O1 K1 13.5(8) . . . . ?
K1 C1 O1 K1 102.4(3) 2 . . . ?
O7 Tb1 O1 C1 126.2(7) . . . . ?
O7 Tb1 O1 C1 -69.3(8) 2 . . . ?
O1 Tb1 O1 C1 84.6(8) 2 . . . ?
O8 Tb1 O1 C1 -27.1(10) 2 . . . ?
O8 Tb1 O1 C1 -130.3(8) . . . . ?
O6 Tb1 O1 C1 168.2(8) . . . . ?
O6 Tb1 O1 C1 9.8(8) 2 . . . ?
K1 Tb1 O1 C1 38.4(8) 2 . . . ?
O7 Tb1 O1 K1 -20.4(4) . . . . ?
O7 Tb1 O1 K1 144.0(2) 2 . . . ?
O1 Tb1 O1 K1 -61.98(18) 2 . . . ?
O8 Tb1 O1 K1 -173.7(3) 2 . . . ?
O8 Tb1 O1 K1 83.1(2) . . . . ?
O6 Tb1 O1 K1 21.6(2) . . . . ?
O6 Tb1 O1 K1 -136.8(2) 2 . . . ?
K1 Tb1 O1 K1 -108.2(2) 2 . . . ?
O6 K1 O1 C1 178.4(5) . . . . ?
O5 K1 O1 C1 -12.9(4) . . . . ?
O3 K1 O1 C1 -36.7(6) 6_566 . . . ?
O4 K1 O1 C1 -135.1(6) 6_566 . . . ?
C1 K1 O1 C1 -107.2(5) 2 . . . ?
O6 K1 O1 Tb1 -21.9(2) . . . . ?
O5 K1 O1 Tb1 146.8(3) . . . . ?
O3 K1 O1 Tb1 123.0(3) 6_566 . . . ?
O4 K1 O1 Tb1 24.6(6) 6_566 . . . ?
C1 K1 O1 Tb1 52.5(2) 2 . . . ?
C4 C3 O3 K1 -2.5(10) . . . 6_565 ?
C2 C3 O3 K1 175.3(6) . . . 6_565 ?
C3 C4 O4 K1 5.3(9) . . . 6_565 ?
C5 C4 O4 K1 -173.2(7) . . . 6_565 ?
C1 C5 O5 K1 -14.4(10) . . . . ?
C4 C5 O5 K1 163.7(6) . . . . ?
O6 K1 O5 C5 23.7(7) . . . . ?
O3 K1 O5 C5 175.7(6) 6_566 . . . ?
O4 K1 O5 C5 160.6(5) 6_566 . . . ?
O1 K1 O5 C5 13.4(5) . . . . ?
C1 K1 O5 C5 81.5(6) 2 . . . ?
O7 Tb1 O6 K1 125.5(3) . . . . ?
O7 Tb1 O6 K1 -91.6(3) 2 . . . ?
O1 Tb1 O6 K1 49.8(3) 2 . . . ?
O1 Tb1 O6 K1 -28.7(3) . . . . ?
O8 Tb1 O6 K1 164.6(3) 2 . . . ?
O8 Tb1 O6 K1 -151.0(4) . . . . ?
O6 Tb1 O6 K1 11.3(2) 2 . . . ?
K1 Tb1 O6 K1 17.9(4) 2 . . . ?
O5 K1 O6 Tb1 13.6(4) . . . . ?
O3 K1 O6 Tb1 -95.5(6) 6_566 . . . ?
O4 K1 O6 Tb1 -135.6(3) 6_566 . . . ?
O1 K1 O6 Tb1 24.1(2) . . . . ?
C1 K1 O6 Tb1 -53.5(3) 2 . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O2 0.83 2.04 2.695(8) 135.4 2
O7 H7B O4 0.83 1.88 2.676(8) 162.5 2_565
O8 H8A O3 0.85 1.78 2.631(8) 179.8 6_576
O8 H8B O5 0.83 1.97 2.718(7) 148.4 1_565
O6 H6A O2 0.82 2.31 2.774(8) 115.9 6_576

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         2.086
_refine_diff_density_min         -2.321
_refine_diff_density_rms         0.534
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 -0.081 0.099 360 224 ' '
2 0.750 0.051 0.109 360 224 ' '
_platon_squeeze_details          ?
_exptl_crystal_recrystallization_method 'Vapour Deposition'
####################################################################### 
# 
# 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_fq59-1
_database_code_depnum_ccdc_archive 'CCDC 1437012'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 3'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 N O15 Tb'
_chemical_formula_weight         573.18

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Cc
_symmetry_space_group_name_Hall  'C -2yc'

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

_cell_length_a                   9.4830(19)
_cell_length_b                   13.725(3)
_cell_length_c                   14.272(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.18(3)
_cell_angle_gamma                90.00
_cell_volume                     1792.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    4.028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3778
_exptl_absorpt_correction_T_max  0.6888
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'synchrotron, 3W1A at BSRF'
_diffrn_radiation_monochromator  'double crystal monochromator'
_diffrn_measurement_device_type  mar555
_diffrn_measurement_method       'oscillation mode'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4852
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         30.54
_reflns_number_total             4047
_reflns_number_gt                4010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0872P)²+1.2574P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0067(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(17)
_refine_ls_number_reflns         4047
_refine_ls_number_parameters     273
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1060
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 1.10731(5) 0.143056(10) 0.03725(4) 0.01182(11) Uani 1 1 d . . .
C1 C 0.8562(6) 0.1653(4) 0.1810(4) 0.0122(8) Uani 1 1 d . . .
C2 C 0.6989(6) 0.1778(3) 0.1670(4) 0.0133(9) Uani 1 1 d . . .
C3 C 0.6647(7) 0.1566(4) 0.2609(5) 0.0135(10) Uani 1 1 d . . .
C4 C 0.8058(10) 0.1377(3) 0.3320(5) 0.0141(13) Uani 1 1 d . . .
C5 C 0.9210(9) 0.1396(3) 0.2814(5) 0.0143(12) Uani 1 1 d . . .
C6 C 0.9070(6) 0.1099(3) -0.1957(4) 0.0139(9) Uani 1 1 d . . .
C7 C 0.7971(7) 0.1003(4) -0.2824(4) 0.0158(9) Uani 1 1 d . . .
H7 H 0.8200 0.0995 -0.3419 0.019 Uiso 1 1 calc R . .
C8 C 0.6534(7) 0.0922(4) -0.2778(4) 0.0182(11) Uani 1 1 d . . .
H8 H 0.5776 0.0879 -0.3342 0.022 Uiso 1 1 calc R . .
C9 C 0.6250(7) 0.0905(4) -0.1865(4) 0.0150(9) Uani 1 1 d . . .
C10 C 0.7411(6) 0.0998(4) -0.1037(4) 0.0145(9) Uani 1 1 d . . .
H10 H 0.7215 0.0976 -0.0432 0.017 Uiso 1 1 calc R . .
C11 C 1.0650(6) 0.1215(4) -0.1952(4) 0.0135(9) Uani 1 1 d . . .
C12 C 0.4722(7) 0.0771(3) -0.1768(4) 0.0151(9) Uani 1 1 d . . .
N1 N 0.8796(5) 0.1118(3) -0.1073(3) 0.0152(8) Uani 1 1 d . . .
O1 O 0.9217(5) 0.1773(3) 0.1154(3) 0.0169(7) Uani 1 1 d . . .
O2 O 0.6109(5) 0.2007(3) 0.0897(3) 0.0200(8) Uani 1 1 d . . .
O3 O 0.5435(6) 0.1548(3) 0.2775(4) 0.0164(9) Uani 1 1 d . . .
O4 O 0.8215(5) 0.1214(3) 0.4202(3) 0.0166(8) Uani 1 1 d . . .
O5 O 1.0545(6) 0.1228(4) 0.3199(4) 0.0203(8) Uani 1 1 d . . .
O6 O 1.1513(7) 0.1456(2) -0.1151(4) 0.0165(10) Uani 1 1 d . . .
O7 O 1.1022(5) 0.1070(3) -0.2718(3) 0.0165(8) Uani 1 1 d . . .
O8 O 0.4485(5) 0.0422(4) -0.1051(4) 0.0248(9) Uani 1 1 d . . .
O9 O 0.3766(6) 0.1086(4) -0.2544(4) 0.0208(9) Uani 1 1 d . . .
H9 H 0.2939 0.0970 -0.2498 0.031 Uiso 1 1 calc R . .
O10 O 1.3058(6) 0.0331(3) 0.0406(3) 0.0192(9) Uani 1 1 d . . .
H10A H 1.2759 -0.0306 0.0291 0.029 Uiso 1 1 d R . .
H10B H 1.3939 0.0357 0.0411 0.029 Uiso 1 1 d R . .
O11 O 1.2320(7) 0.1305(3) 0.2023(4) 0.0209(10) Uani 1 1 d . . .
H11A H 1.3211 0.1160 0.2078 0.031 Uiso 1 1 d R . .
H11B H 1.1927 0.0861 0.2287 0.031 Uiso 1 1 d R . .
O12 O 1.0139(5) -0.0133(3) 0.0574(3) 0.0193(8) Uani 1 1 d . . .
H12A H 1.0730 -0.0431 0.1043 0.029 Uiso 1 1 d R . .
H12B H 1.0037 -0.0464 0.0053 0.029 Uiso 1 1 d R . .
O13 O 1.0238(5) 0.3038(3) -0.0171(3) 0.0171(7) Uani 1 1 d . . .
H13A H 0.9276 0.3088 -0.0276 0.026 Uiso 1 1 d R . .
H13B H 1.0458 0.3184 -0.0722 0.026 Uiso 1 1 d R . .
O14 O 1.3191(6) 0.2417(3) 0.0573(3) 0.0180(8) Uani 1 1 d . . .
H14A H 1.3133 0.2745 0.0054 0.027 Uiso 1 1 d R . .
H14B H 1.3952 0.2055 0.0686 0.027 Uiso 1 1 d R . .
O15 O 0.7477(6) 0.3399(3) 0.9917(4) 0.0178(8) Uani 1 1 d G . .
H15A H 0.6791 0.3526 0.9415 0.027 Uiso 1 1 d G . .
H15B H 0.7209 0.2946 1.0238 0.027 Uiso 1 1 d G . .


_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 O6 2.318(6) . ?
Tb1 O11 2.350(6) . ?
Tb1 O1 2.365(5) . ?
Tb1 O12 2.368(4) . ?
Tb1 O14 2.377(5) . ?
Tb1 O13 2.403(4) . ?
Tb1 O10 2.404(5) . ?
Tb1 N1 2.602(5) . ?
C1 O1 1.263(7) . ?
C1 C5 1.447(9) . ?
C1 C2 1.462(7) . ?
C2 O2 1.237(6) . ?
C2 C3 1.487(8) . ?
C3 O3 1.234(9) . ?
C3 C4 1.475(10) . ?
C4 O4 1.249(9) . ?
C4 C5 1.459(12) . ?
C5 O5 1.262(9) . ?
C6 N1 1.353(7) . ?
C6 C7 1.399(7) . ?
C6 C11 1.505(8) . ?
C7 C8 1.385(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.394(7) . ?
C9 C12 1.503(9) . ?
C10 N1 1.338(7) . ?
C10 H10 0.9300 . ?
C11 O7 1.250(7) . ?
C11 O6 1.263(8) . ?
C12 O8 1.203(8) . ?
C12 O9 1.308(7) . ?
O9 H9 0.8200 . ?
O10 H10A 0.9204 . ?
O10 H10B 0.8347 . ?
O11 H11A 0.8509 . ?
O11 H11B 0.8509 . ?
O12 H12A 0.8560 . ?
O12 H12B 0.8558 . ?
O13 H13A 0.8874 . ?
O13 H13B 0.8870 . ?
O14 H14A 0.8559 . ?
O14 H14B 0.8559 . ?
O15 H15A 0.8501 . ?
O15 H15B 0.8500 . ?

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
O6 Tb1 O11 140.8(2) . . ?
O6 Tb1 O1 141.09(18) . . ?
O11 Tb1 O1 77.47(19) . . ?
O6 Tb1 O12 107.00(14) . . ?
O11 Tb1 O12 85.26(15) . . ?
O1 Tb1 O12 76.98(15) . . ?
O6 Tb1 O14 75.56(17) . . ?
O11 Tb1 O14 74.55(18) . . ?
O1 Tb1 O14 122.67(16) . . ?
O12 Tb1 O14 146.40(16) . . ?
O6 Tb1 O13 78.98(14) . . ?
O11 Tb1 O13 115.34(15) . . ?
O1 Tb1 O13 75.31(14) . . ?
O12 Tb1 O13 140.29(16) . . ?
O14 Tb1 O13 73.29(15) . . ?
O6 Tb1 O10 72.28(17) . . ?
O11 Tb1 O10 75.41(18) . . ?
O1 Tb1 O10 142.32(15) . . ?
O12 Tb1 O10 75.18(16) . . ?
O14 Tb1 O10 73.91(18) . . ?
O13 Tb1 O10 140.64(16) . . ?
O6 Tb1 N1 64.82(18) . . ?
O11 Tb1 N1 151.44(19) . . ?
O1 Tb1 N1 80.86(15) . . ?
O12 Tb1 N1 71.82(14) . . ?
O14 Tb1 N1 133.55(15) . . ?
O13 Tb1 N1 76.15(15) . . ?
O10 Tb1 N1 113.26(16) . . ?
O1 C1 C5 127.1(5) . . ?
O1 C1 C2 124.4(5) . . ?
C5 C1 C2 108.5(5) . . ?
O2 C2 C1 125.3(5) . . ?
O2 C2 C3 126.7(5) . . ?
C1 C2 C3 108.0(4) . . ?
O3 C3 C4 126.0(6) . . ?
O3 C3 C2 127.7(6) . . ?
C4 C3 C2 106.3(6) . . ?
O4 C4 C5 126.5(7) . . ?
O4 C4 C3 124.9(8) . . ?
C5 C4 C3 108.6(6) . . ?
O5 C5 C1 126.4(7) . . ?
O5 C5 C4 125.3(7) . . ?
C1 C5 C4 108.4(6) . . ?
N1 C6 C7 123.1(5) . . ?
N1 C6 C11 115.3(5) . . ?
C7 C6 C11 121.6(5) . . ?
C8 C7 C6 118.7(5) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 118.4(5) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
C10 C9 C8 119.1(6) . . ?
C10 C9 C12 120.0(5) . . ?
C8 C9 C12 120.9(5) . . ?
N1 C10 C9 122.9(5) . . ?
N1 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
O7 C11 O6 124.7(6) . . ?
O7 C11 C6 119.2(5) . . ?
O6 C11 C6 116.1(6) . . ?
O8 C12 O9 127.5(6) . . ?
O8 C12 C9 121.8(5) . . ?
O9 C12 C9 110.7(5) . . ?
C10 N1 C6 117.6(5) . . ?
C10 N1 Tb1 127.5(4) . . ?
C6 N1 Tb1 114.9(4) . . ?
C1 O1 Tb1 153.5(4) . . ?
C11 O6 Tb1 127.7(5) . . ?
C12 O9 H9 109.5 . . ?
Tb1 O10 H10A 112.9 . . ?
Tb1 O10 H10B 138.6 . . ?
H10A O10 H10B 107.7 . . ?
Tb1 O11 H11A 109.6 . . ?
Tb1 O11 H11B 109.4 . . ?
H11A O11 H11B 109.4 . . ?
Tb1 O12 H12A 109.9 . . ?
Tb1 O12 H12B 109.7 . . ?
H12A O12 H12B 109.2 . . ?
Tb1 O13 H13A 111.3 . . ?
Tb1 O13 H13B 111.0 . . ?
H13A O13 H13B 107.6 . . ?
Tb1 O14 H14A 109.6 . . ?
Tb1 O14 H14B 109.6 . . ?
H14A O14 H14B 109.2 . . ?
H15A O15 H15B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 0.7(8) . . . . ?
C5 C1 C2 O2 179.3(5) . . . . ?
O1 C1 C2 C3 179.8(5) . . . . ?
C5 C1 C2 C3 -1.6(6) . . . . ?
O2 C2 C3 O3 2.8(9) . . . . ?
C1 C2 C3 O3 -176.3(5) . . . . ?
O2 C2 C3 C4 -177.3(5) . . . . ?
C1 C2 C3 C4 3.6(5) . . . . ?
O3 C3 C4 O4 -3.4(9) . . . . ?
C2 C3 C4 O4 176.7(5) . . . . ?
O3 C3 C4 C5 175.6(5) . . . . ?
C2 C3 C4 C5 -4.3(5) . . . . ?
O1 C1 C5 O5 -1.7(9) . . . . ?
C2 C1 C5 O5 179.7(5) . . . . ?
O1 C1 C5 C4 177.5(5) . . . . ?
C2 C1 C5 C4 -1.1(5) . . . . ?
O4 C4 C5 O5 1.6(8) . . . . ?
C3 C4 C5 O5 -177.3(5) . . . . ?
O4 C4 C5 C1 -177.6(5) . . . . ?
C3 C4 C5 C1 3.4(5) . . . . ?
N1 C6 C7 C8 -0.2(8) . . . . ?
C11 C6 C7 C8 -178.5(5) . . . . ?
C6 C7 C8 C9 -2.2(8) . . . . ?
C7 C8 C9 C10 1.8(8) . . . . ?
C7 C8 C9 C12 -177.1(5) . . . . ?
C8 C9 C10 N1 1.0(8) . . . . ?
C12 C9 C10 N1 179.9(5) . . . . ?
N1 C6 C11 O7 170.1(5) . . . . ?
C7 C6 C11 O7 -11.4(8) . . . . ?
N1 C6 C11 O6 -9.8(7) . . . . ?
C7 C6 C11 O6 168.6(5) . . . . ?
C10 C9 C12 O8 -25.3(8) . . . . ?
C8 C9 C12 O8 153.5(6) . . . . ?
C10 C9 C12 O9 154.3(5) . . . . ?
C8 C9 C12 O9 -26.9(7) . . . . ?
C9 C10 N1 C6 -3.3(7) . . . . ?
C9 C10 N1 Tb1 175.1(4) . . . . ?
C7 C6 N1 C10 2.9(7) . . . . ?
C11 C6 N1 C10 -178.7(5) . . . . ?
C7 C6 N1 Tb1 -175.7(4) . . . . ?
C11 C6 N1 Tb1 2.7(5) . . . . ?
O6 Tb1 N1 C10 -176.2(5) . . . . ?
O11 Tb1 N1 C10 26.0(6) . . . . ?
O1 Tb1 N1 C10 -15.0(4) . . . . ?
O12 Tb1 N1 C10 64.2(4) . . . . ?
O14 Tb1 N1 C10 -142.0(4) . . . . ?
O13 Tb1 N1 C10 -92.0(4) . . . . ?
O10 Tb1 N1 C10 128.4(4) . . . . ?
O6 Tb1 N1 C6 2.3(3) . . . . ?
O11 Tb1 N1 C6 -155.6(4) . . . . ?
O1 Tb1 N1 C6 163.4(4) . . . . ?
O12 Tb1 N1 C6 -117.4(4) . . . . ?
O14 Tb1 N1 C6 36.5(4) . . . . ?
O13 Tb1 N1 C6 86.4(4) . . . . ?
O10 Tb1 N1 C6 -53.1(4) . . . . ?
C5 C1 O1 Tb1 33.7(12) . . . . ?
C2 C1 O1 Tb1 -147.9(6) . . . . ?
O6 Tb1 O1 C1 151.0(8) . . . . ?
O11 Tb1 O1 C1 -38.0(8) . . . . ?
O12 Tb1 O1 C1 50.0(8) . . . . ?
O14 Tb1 O1 C1 -100.2(8) . . . . ?
O13 Tb1 O1 C1 -158.7(9) . . . . ?
O10 Tb1 O1 C1 6.8(9) . . . . ?
N1 Tb1 O1 C1 123.3(8) . . . . ?
O7 C11 O6 Tb1 -166.1(4) . . . . ?
C6 C11 O6 Tb1 13.9(7) . . . . ?
O11 Tb1 O6 C11 154.3(4) . . . . ?
O1 Tb1 O6 C11 -39.6(5) . . . . ?
O12 Tb1 O6 C11 50.6(5) . . . . ?
O14 Tb1 O6 C11 -164.2(5) . . . . ?
O13 Tb1 O6 C11 -88.9(4) . . . . ?
O10 Tb1 O6 C11 118.4(4) . . . . ?
N1 Tb1 O6 C11 -9.1(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15B O1 0.85 2.57 3.048(6) 116.4 1_556
O15 H15B O2 0.85 2.04 2.870(7) 166.8 1_556
O15 H15A O5 0.85 1.86 2.698(7) 169.7 4_455
O14 H14B O2 0.86 1.99 2.742(7) 146.2 1_655
O14 H14A O4 0.86 1.89 2.716(6) 161.7 4_554
O13 H13B O3 0.89 2.17 3.039(7) 165.9 4_554
O13 H13A O15 0.89 1.85 2.700(7) 160.2 1_554
O12 H12B O4 0.86 2.10 2.738(6) 130.7 2_554
O12 H12A O7 0.86 1.93 2.688(6) 147.4 2
O11 H11B O5 0.85 2.13 2.671(9) 120.7 .
O11 H11A O3 0.85 2.15 2.886(8) 144.5 1_655
O10 H10B O8 0.83 2.28 2.765(7) 117.4 1_655
O10 H10A O15 0.92 1.85 2.760(6) 167.4 3_544
O9 H9 O7 0.82 1.77 2.549(7) 158.7 1_455

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        30.54
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.918
_refine_diff_density_min         -3.120
_refine_diff_density_rms         0.220
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_fq38-sd-36
_database_code_depnum_ccdc_archive 'CCDC 1437013'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Complex 4'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H14 K O17 Tb'
_chemical_formula_weight         604.23

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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'

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

_cell_length_a                   16.031(3)
_cell_length_b                   12.505(3)
_cell_length_c                   8.4522(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1694.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    4.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.352
_exptl_absorpt_correction_T_max  0.405
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11426
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.37
_reflns_number_total             2191
_reflns_number_gt                2019
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0258P)²+0.0200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(14)
_refine_ls_number_reflns         2191
_refine_ls_number_parameters     143
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0489
_refine_ls_wR_factor_gt          0.0469
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_restrained_S_all      0.895
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.5000 0.817031(17) 0.67242(4) 0.01665(7) Uani 1 2 d S . .
K1 K 1.0000 0.98975(12) 0.51006(18) 0.0317(3) Uani 1 2 d S . .
C1 C 0.6968(3) 0.8752(4) 0.6144(6) 0.0186(11) Uani 1 1 d . . .
C2 C 0.6818(3) 0.8790(4) 0.7815(6) 0.0165(9) Uani 1 1 d . . .
C3 C 0.7617(3) 0.8846(3) 0.8640(5) 0.0197(8) Uani 1 1 d . . .
C4 C 0.8262(3) 0.8951(4) 0.7401(5) 0.0217(9) Uani 1 1 d . . .
C5 C 0.7866(3) 0.8838(3) 0.5825(5) 0.0223(9) Uani 1 1 d U . .
O1 O 0.6371(2) 0.8629(4) 0.5171(4) 0.0254(8) Uani 1 1 d . . .
O2 O 0.6101(2) 0.8735(3) 0.8405(4) 0.0238(8) Uani 1 1 d . . .
O3 O 0.77263(18) 0.8788(3) 1.0094(4) 0.0287(7) Uani 1 1 d . . .
O4 O 0.90157(17) 0.9086(3) 0.7646(4) 0.0327(7) Uani 1 1 d . . .
O5 O 0.8225(2) 0.8825(3) 0.4550(4) 0.0353(8) Uani 1 1 d . . .
O6 O 0.5000 0.7500(6) 0.4115(7) 0.0315(17) Uani 1 2 d S . .
H6A H 0.5428 0.7471 0.3590 0.047 Uiso 1 1 d R . .
O7 O 0.5000 0.7349(5) 0.9576(7) 0.0235(13) Uani 1 2 d SU . .
H7A H 0.4587 0.7540 1.0080 0.035 Uiso 1 1 d R . .
O8 O 0.59180(14) 0.66105(18) 0.6795(8) 0.0247(6) Uani 1 1 d . . .
H8A H 0.6330 0.6452 0.6164 0.037 Uiso 1 1 d R . .
H8B H 0.6092 0.6708 0.7814 0.037 Uiso 1 1 d R . .
O9 O 0.5000 0.9985(3) 0.6223(5) 0.0339(13) Uani 1 2 d S . .
H9A H 0.4599 1.0388 0.6312 0.051 Uiso 1 1 d R . .
O10 O 0.87555(18) 0.6439(3) 0.6900(6) 0.0341(8) Uani 1 1 d G . .
H10A H 0.8661 0.6347 0.7883 0.051 Uiso 1 1 d G . .
H10B H 0.8301 0.6356 0.6379 0.051 Uiso 1 1 d G . .


_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 O9 2.309(4) . ?
Tb1 O6 2.360(6) . ?
Tb1 O2 2.373(4) . ?
Tb1 O2 2.373(4) 3_655 ?
Tb1 O8 2.444(2) 3_655 ?
Tb1 O8 2.444(2) . ?
Tb1 O7 2.620(6) . ?
Tb1 O1 2.623(4) . ?
Tb1 O1 2.623(4) 3_655 ?
Tb1 K1 4.3164(18) 5_445 ?
K1 O7 2.844(6) 6_664 ?
K1 O4 2.854(3) 3_755 ?
K1 O4 2.855(3) . ?
K1 O4 2.900(4) 4_574 ?
K1 O4 2.900(4) 2_774 ?
K1 O8 2.967(4) 5 ?
K1 O8 2.967(4) 7_655 ?
K1 O5 3.180(4) 3_755 ?
K1 O5 3.180(4) . ?
K1 O6 3.359(7) 5 ?
K1 K1 4.2338(9) 2_775 ?
K1 K1 4.2339(9) 2_774 ?
C1 O1 1.271(5) . ?
C1 C2 1.434(7) . ?
C1 C5 1.468(7) . ?
C2 O2 1.254(6) . ?
C2 C3 1.460(6) . ?
C3 O3 1.244(5) . ?
C3 C4 1.478(6) . ?
C4 O4 1.238(5) . ?
C4 C5 1.482(6) . ?
C5 O5 1.221(5) . ?
O4 K1 2.900(4) 2_775 ?
O6 K1 3.359(7) 5_445 ?
O6 H6A 0.8176 . ?
O7 K1 2.844(6) 6_665 ?
O7 H7A 0.8227 . ?
O8 K1 2.967(4) 5_445 ?
O8 H8A 0.8717 . ?
O8 H8B 0.9133 . ?
O9 H9A 0.8202 . ?
O10 H10A 0.8527 . ?
O10 H10B 0.8569 . ?

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
O9 Tb1 O6 100.2(2) . . ?
O9 Tb1 O2 79.49(13) . . ?
O6 Tb1 O2 131.69(9) . . ?
O9 Tb1 O2 79.48(13) . 3_655 ?
O6 Tb1 O2 131.68(9) . 3_655 ?
O2 Tb1 O2 96.14(17) . 3_655 ?
O9 Tb1 O8 142.09(7) . 3_655 ?
O6 Tb1 O8 74.9(2) . 3_655 ?
O2 Tb1 O8 132.11(17) . 3_655 ?
O2 Tb1 O8 76.98(15) 3_655 3_655 ?
O9 Tb1 O8 142.09(7) . . ?
O6 Tb1 O8 74.9(2) . . ?
O2 Tb1 O8 76.97(15) . . ?
O2 Tb1 O8 132.11(17) 3_655 . ?
O8 Tb1 O8 74.04(11) 3_655 . ?
O9 Tb1 O7 123.65(18) . . ?
O6 Tb1 O7 136.10(14) . . ?
O2 Tb1 O7 64.28(12) . . ?
O2 Tb1 O7 64.28(12) 3_655 . ?
O8 Tb1 O7 70.40(19) 3_655 . ?
O8 Tb1 O7 70.40(19) . . ?
O9 Tb1 O1 72.14(11) . . ?
O6 Tb1 O1 67.05(11) . . ?
O2 Tb1 O1 67.12(11) . . ?
O2 Tb1 O1 149.06(11) 3_655 . ?
O8 Tb1 O1 133.73(16) 3_655 . ?
O8 Tb1 O1 71.48(14) . . ?
O7 Tb1 O1 123.09(8) . . ?
O9 Tb1 O1 72.14(11) . 3_655 ?
O6 Tb1 O1 67.05(11) . 3_655 ?
O2 Tb1 O1 149.06(10) . 3_655 ?
O2 Tb1 O1 67.12(11) 3_655 3_655 ?
O8 Tb1 O1 71.48(14) 3_655 3_655 ?
O8 Tb1 O1 133.73(16) . 3_655 ?
O7 Tb1 O1 123.09(8) . 3_655 ?
O1 Tb1 O1 113.81(16) . 3_655 ?
O9 Tb1 K1 150.89(12) . 5_445 ?
O6 Tb1 K1 50.64(18) . 5_445 ?
O2 Tb1 K1 118.17(10) . 5_445 ?
O2 Tb1 K1 118.17(10) 3_655 5_445 ?
O8 Tb1 K1 41.51(10) 3_655 5_445 ?
O8 Tb1 K1 41.51(10) . 5_445 ?
O7 Tb1 K1 85.46(14) . 5_445 ?
O1 Tb1 K1 92.77(10) . 5_445 ?
O1 Tb1 K1 92.76(10) 3_655 5_445 ?
O7 K1 O4 76.50(13) 6_664 3_755 ?
O7 K1 O4 76.50(13) 6_664 . ?
O4 K1 O4 67.12(13) 3_755 . ?
O7 K1 O4 108.74(13) 6_664 4_574 ?
O4 K1 O4 174.75(8) 3_755 4_574 ?
O4 K1 O4 113.21(10) . 4_574 ?
O7 K1 O4 108.74(13) 6_664 2_774 ?
O4 K1 O4 113.22(10) 3_755 2_774 ?
O4 K1 O4 174.75(8) . 2_774 ?
O4 K1 O4 65.93(12) 4_574 2_774 ?
O7 K1 O8 142.03(10) 6_664 5 ?
O4 K1 O8 67.58(12) 3_755 5 ?
O4 K1 O8 99.61(14) . 5 ?
O4 K1 O8 107.39(12) 4_574 5 ?
O4 K1 O8 76.06(14) 2_774 5 ?
O7 K1 O8 142.03(10) 6_664 7_655 ?
O4 K1 O8 99.61(14) 3_755 7_655 ?
O4 K1 O8 67.58(12) . 7_655 ?
O4 K1 O8 76.06(14) 4_574 7_655 ?
O4 K1 O8 107.39(12) 2_774 7_655 ?
O8 K1 O8 59.46(11) 5 7_655 ?
O7 K1 O5 63.95(7) 6_664 3_755 ?
O4 K1 O5 57.70(9) 3_755 3_755 ?
O4 K1 O5 117.07(10) . 3_755 ?
O4 K1 O5 124.55(10) 4_574 3_755 ?
O4 K1 O5 65.99(9) 2_774 3_755 ?
O8 K1 O5 86.04(8) 5 3_755 ?
O8 K1 O5 144.95(10) 7_655 3_755 ?
O7 K1 O5 63.95(7) 6_664 . ?
O4 K1 O5 117.07(10) 3_755 . ?
O4 K1 O5 57.70(9) . . ?
O4 K1 O5 65.99(9) 4_574 . ?
O4 K1 O5 124.55(10) 2_774 . ?
O8 K1 O5 144.95(10) 5 . ?
O8 K1 O5 86.04(8) 7_655 . ?
O5 K1 O5 127.00(13) 3_755 . ?
O7 K1 O6 156.7(2) 6_664 5 ?
O4 K1 O6 122.09(11) 3_755 5 ?
O4 K1 O6 122.09(11) . 5 ?
O4 K1 O6 52.99(10) 4_574 5 ?
O4 K1 O6 52.99(10) 2_774 5 ?
O8 K1 O6 54.58(13) 5 5 ?
O8 K1 O6 54.58(13) 7_655 5 ?
O5 K1 O6 111.84(7) 3_755 5 ?
O5 K1 O6 111.84(7) . 5 ?
O7 K1 K1 102.44(13) 6_664 2_775 ?
O4 K1 K1 43.04(7) 3_755 2_775 ?
O4 K1 K1 43.04(7) . 2_775 ?
O4 K1 K1 133.44(8) 4_574 2_775 ?
O4 K1 K1 133.44(8) 2_774 2_775 ?
O8 K1 K1 58.30(12) 5 2_775 ?
O8 K1 K1 58.30(12) 7_655 2_775 ?
O5 K1 K1 99.87(7) 3_755 2_775 ?
O5 K1 K1 99.87(7) . 2_775 ?
O6 K1 K1 100.89(11) 5 2_775 ?
O7 K1 K1 84.50(13) 6_664 2_774 ?
O4 K1 K1 140.70(7) 3_755 2_774 ?
O4 K1 K1 140.70(7) . 2_774 ?
O4 K1 K1 42.21(7) 4_574 2_774 ?
O4 K1 K1 42.21(7) 2_774 2_774 ?
O8 K1 K1 115.98(13) 5 2_774 ?
O8 K1 K1 115.98(13) 7_655 2_774 ?
O5 K1 K1 83.08(7) 3_755 2_774 ?
O5 K1 K1 83.08(7) . 2_774 ?
O6 K1 K1 72.17(11) 5 2_774 ?
K1 K1 K1 173.06(8) 2_775 2_774 ?
O1 C1 C2 120.9(5) . . ?
O1 C1 C5 129.0(4) . . ?
C2 C1 C5 110.1(4) . . ?
O2 C2 C1 123.0(5) . . ?
O2 C2 C3 128.0(4) . . ?
C1 C2 C3 108.9(4) . . ?
O3 C3 C2 126.4(4) . . ?
O3 C3 C4 127.4(4) . . ?
C2 C3 C4 106.2(4) . . ?
O4 C4 C3 125.2(4) . . ?
O4 C4 C5 125.6(4) . . ?
C3 C4 C5 109.2(3) . . ?
O5 C5 C1 128.5(4) . . ?
O5 C5 C4 126.3(4) . . ?
C1 C5 C4 105.2(4) . . ?
C1 O1 Tb1 109.5(3) . . ?
C2 O2 Tb1 117.4(3) . . ?
C4 O4 K1 117.5(3) . . ?
C4 O4 K1 135.3(3) . 2_775 ?
K1 O4 K1 94.74(9) . 2_775 ?
C5 O5 K1 106.7(3) . . ?
Tb1 O6 K1 96.5(2) . 5_445 ?
Tb1 O6 H6A 121.5 . . ?
K1 O6 H6A 95.3 5_445 . ?
Tb1 O7 K1 122.0(2) . 6_665 ?
Tb1 O7 H7A 111.3 . . ?
K1 O7 H7A 101.9 6_665 . ?
Tb1 O8 K1 105.40(13) . 5_445 ?
Tb1 O8 H8A 128.5 . . ?
K1 O8 H8A 85.2 5_445 . ?
Tb1 O8 H8B 95.8 . . ?
K1 O8 H8B 134.6 5_445 . ?
H8A O8 H8B 112.1 . . ?
Tb1 O9 H9A 125.9 . . ?
H10A O10 H10B 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 -1.9(10) . . . . ?
C5 C1 C2 O2 179.9(4) . . . . ?
O1 C1 C2 C3 175.3(4) . . . . ?
C5 C1 C2 C3 -2.9(7) . . . . ?
O2 C2 C3 O3 4.2(9) . . . . ?
C1 C2 C3 O3 -172.8(5) . . . . ?
O2 C2 C3 C4 -177.4(5) . . . . ?
C1 C2 C3 C4 5.6(6) . . . . ?
O3 C3 C4 O4 -6.3(8) . . . . ?
C2 C3 C4 O4 175.4(4) . . . . ?
O3 C3 C4 C5 172.1(5) . . . . ?
C2 C3 C4 C5 -6.3(5) . . . . ?
O1 C1 C5 O5 1.3(9) . . . . ?
C2 C1 C5 O5 179.3(5) . . . . ?
O1 C1 C5 C4 -179.0(6) . . . . ?
C2 C1 C5 C4 -1.0(6) . . . . ?
O4 C4 C5 O5 2.6(8) . . . . ?
C3 C4 C5 O5 -175.7(4) . . . . ?
O4 C4 C5 C1 -177.2(4) . . . . ?
C3 C4 C5 C1 4.5(5) . . . . ?
C2 C1 O1 Tb1 -9.0(7) . . . . ?
C5 C1 O1 Tb1 168.8(4) . . . . ?
O9 Tb1 O1 C1 96.5(4) . . . . ?
O6 Tb1 O1 C1 -153.6(4) . . . . ?
O2 Tb1 O1 C1 10.7(3) . . . . ?
O2 Tb1 O1 C1 72.1(4) 3_655 . . . ?
O8 Tb1 O1 C1 -116.5(4) 3_655 . . . ?
O8 Tb1 O1 C1 -72.6(4) . . . . ?
O7 Tb1 O1 C1 -22.5(4) . . . . ?
O1 Tb1 O1 C1 156.9(3) 3_655 . . . ?
K1 Tb1 O1 C1 -108.9(4) 5_445 . . . ?
C1 C2 O2 Tb1 13.5(7) . . . . ?
C3 C2 O2 Tb1 -163.1(4) . . . . ?
O9 Tb1 O2 C2 -87.1(4) . . . . ?
O6 Tb1 O2 C2 7.3(5) . . . . ?
O2 Tb1 O2 C2 -165.2(3) 3_655 . . . ?
O8 Tb1 O2 C2 116.8(4) 3_655 . . . ?
O8 Tb1 O2 C2 62.9(4) . . . . ?
O7 Tb1 O2 C2 137.2(4) . . . . ?
O1 Tb1 O2 C2 -12.2(3) . . . . ?
O1 Tb1 O2 C2 -110.7(4) 3_655 . . . ?
K1 Tb1 O2 C2 68.2(4) 5_445 . . . ?
C3 C4 O4 K1 -161.3(3) . . . . ?
C5 C4 O4 K1 20.6(6) . . . . ?
C3 C4 O4 K1 -30.1(7) . . . 2_775 ?
C5 C4 O4 K1 151.8(4) . . . 2_775 ?
O7 K1 O4 C4 -86.5(3) 6_664 . . . ?
O4 K1 O4 C4 -167.3(3) 3_755 . . . ?
O4 K1 O4 C4 18.4(3) 4_574 . . . ?
O8 K1 O4 C4 132.1(3) 5 . . . ?
O8 K1 O4 C4 81.0(3) 7_655 . . . ?
O5 K1 O4 C4 -137.4(3) 3_755 . . . ?
O5 K1 O4 C4 -19.0(3) . . . . ?
O6 K1 O4 C4 78.1(3) 5 . . . ?
K1 K1 O4 C4 147.9(4) 2_775 . . . ?
K1 K1 O4 C4 -23.2(4) 2_774 . . . ?
O7 K1 O4 K1 125.57(11) 6_664 . . 2_775 ?
O4 K1 O4 K1 44.74(11) 3_755 . . 2_775 ?
O4 K1 O4 K1 -129.56(14) 4_574 . . 2_775 ?
O8 K1 O4 K1 -15.83(10) 5 . . 2_775 ?
O8 K1 O4 K1 -66.98(12) 7_655 . . 2_775 ?
O5 K1 O4 K1 74.62(12) 3_755 . . 2_775 ?
O5 K1 O4 K1 -166.92(14) . . . 2_775 ?
O6 K1 O4 K1 -69.84(13) 5 . . 2_775 ?
K1 K1 O4 K1 -171.11(11) 2_774 . . 2_775 ?
C1 C5 O5 K1 159.6(4) . . . . ?
C4 C5 O5 K1 -20.1(6) . . . . ?
O7 K1 O5 C5 108.7(3) 6_664 . . . ?
O4 K1 O5 C5 51.5(3) 3_755 . . . ?
O4 K1 O5 C5 18.6(3) . . . . ?
O4 K1 O5 C5 -123.7(3) 4_574 . . . ?
O4 K1 O5 C5 -155.7(3) 2_774 . . . ?
O8 K1 O5 C5 -37.5(4) 5 . . . ?
O8 K1 O5 C5 -47.2(3) 7_655 . . . ?
O5 K1 O5 C5 120.1(3) 3_755 . . . ?
O6 K1 O5 C5 -96.4(3) 5 . . . ?
K1 K1 O5 C5 9.6(3) 2_775 . . . ?
K1 K1 O5 C5 -164.0(3) 2_774 . . . ?
O9 Tb1 O6 K1 180.0 . . . 5_445 ?
O2 Tb1 O6 K1 95.0(2) . . . 5_445 ?
O2 Tb1 O6 K1 -95.0(2) 3_655 . . 5_445 ?
O8 Tb1 O6 K1 -38.59(7) 3_655 . . 5_445 ?
O8 Tb1 O6 K1 38.59(7) . . . 5_445 ?
O7 Tb1 O6 K1 0.000(1) . . . 5_445 ?
O1 Tb1 O6 K1 114.52(12) . . . 5_445 ?
O1 Tb1 O6 K1 -114.52(12) 3_655 . . 5_445 ?
O9 Tb1 O7 K1 180.0 . . . 6_665 ?
O6 Tb1 O7 K1 0.000(2) . . . 6_665 ?
O2 Tb1 O7 K1 -124.33(12) . . . 6_665 ?
O2 Tb1 O7 K1 124.33(12) 3_655 . . 6_665 ?
O8 Tb1 O7 K1 39.73(8) 3_655 . . 6_665 ?
O8 Tb1 O7 K1 -39.73(8) . . . 6_665 ?
O1 Tb1 O7 K1 -90.35(14) . . . 6_665 ?
O1 Tb1 O7 K1 90.34(14) 3_655 . . 6_665 ?
K1 Tb1 O7 K1 0.0 5_445 . . 6_665 ?
O9 Tb1 O8 K1 -134.0(2) . . . 5_445 ?
O6 Tb1 O8 K1 -46.68(19) . . . 5_445 ?
O2 Tb1 O8 K1 173.0(2) . . . 5_445 ?
O2 Tb1 O8 K1 86.5(3) 3_655 . . 5_445 ?
O8 Tb1 O8 K1 31.6(3) 3_655 . . 5_445 ?
O7 Tb1 O8 K1 105.99(18) . . . 5_445 ?
O1 Tb1 O8 K1 -117.1(2) . . . 5_445 ?
O1 Tb1 O8 K1 -11.5(3) 3_655 . . 5_445 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H10B O3 0.86 1.98 2.838(5) 177.1 6_664
O10 H10A O1 0.85 1.94 2.774(6) 167.7 6_665
O9 H9A O2 0.82 2.92 3.370(5) 117.1 2_674
O9 H9A O10 0.82 1.95 2.759(4) 168.8 5_455
O8 H8B O7 0.91 2.43 2.923(8) 113.7 .
O8 H8B O5 0.91 1.95 2.759(7) 146.7 6_665
O8 H8A O3 0.87 1.79 2.653(5) 171.4 6_664
O7 H7A O5 0.82 2.81 3.203(5) 111.5 8_465
O7 H7A O10 0.82 2.40 3.183(6) 158.8 8_465
O6 H6A O4 0.82 2.29 2.822(6) 123.7 6_664
O6 H6A O10 0.82 2.37 3.041(7) 139.9 6_664

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.096
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_preparation       'Magnetic properties, Luminescent'
