# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1499450'
_audit_update_record             
;
2017-04-24 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;
_chemical_name_systematic        '[Tb(BTC)(H2O)6]'
_chemical_name_common            '[Tb(BTC)(H2O)6]'
_chemical_formula_moiety         'C9 H15 O12 Tb'
_chemical_formula_sum            'C9 H15 O12 Tb'
_chemical_formula_iupac          ?
_chemical_formula_weight         474.13
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   11.324(3)
_cell_length_b                   17.756(4)
_cell_length_c                   7.1389(17)
_cell_angle_alpha                90
_cell_angle_beta                 118.871(2)
_cell_angle_gamma                90
_cell_volume                     1257.0(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    141
_cell_measurement_theta_min      3.1274
_cell_measurement_theta_max      24.7285
_cell_measurement_temperature    223.(2)

_exptl_crystal_description       rod
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.033
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920

_exptl_absorpt_coefficient_mu    5.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.83

_exptl_special_details           
;
;

_diffrn_ambient_temperature      223.(2)

_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'BrukerTourbo X-ray Source'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            6615
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_full        26.95
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9

_refine_special_details          
;
;

_reflns_number_total             2678
_reflns_number_gt                2467
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0591
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.992
_refine_ls_number_reflns         2678
_refine_ls_number_parameters     170
_refine_ls_number_restraints     14
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.759
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.044(13)

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'

_computing_data_collection       'Bruker SMART APEXII ULTRA'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V7.56A (Bruker AXS)'
_computing_structure_solution    'SHELXS (Bruker AXS 2013)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS, 2013)'
_computing_publication_material  'Generate Report (Bruker AXS)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.2530(14) 0.5110(8) 0.786(2) 0.0128(5) Uani d . . . 1 . .
C C2 0.1820(13) 0.5811(8) 0.701(2) 0.0128(5) Uani d . . . 1 . .
H H2 0.224 0.6278 0.7543 0.015 Uiso calc U . R 1 . .
C C3 0.0486(13) 0.5766(8) 0.5375(19) 0.0128(5) Uani d . . . 1 . .
C C4 -0.0150(14) 0.5103(8) 0.461(2) 0.0128(5) Uani d . . . 1 . .
H H4 -0.1047 0.5094 0.3498 0.015 Uiso calc U . R 1 . .
C C5 0.0537(13) 0.4427(9) 0.549(2) 0.0128(5) Uani d . . . 1 . .
C C6 0.1870(13) 0.4434(9) 0.708(2) 0.0128(5) Uani d . . . 1 . .
H H6 0.2326 0.3978 0.764 0.015 Uiso calc U . R 1 . .
C C7 0.3965(8) 0.5110(5) 0.9628(14) 0.0128(5) Uani d . . . 1 . .
C C8 0.4695(9) 0.8496(5) 0.9503(15) 0.0128(5) Uani d . . . 1 . .
C C9 -0.0166(9) 0.3671(5) 0.4753(15) 0.0128(5) Uani d . . . 1 . .
O O1 0.4532(7) 0.5734(4) 1.0338(12) 0.0249(16) Uani d . . . 1 . .
O O2 0.4526(7) 0.4481(4) 1.0314(12) 0.0257(17) Uani d . . . 1 . .
O O3 0.0540(6) 0.3085(4) 0.5491(10) 0.0164(14) Uani d . . . 1 . .
O O4 -0.1421(6) 0.3660(4) 0.3435(10) 0.0151(13) Uani d . . . 1 . .
O O5 0.5199(7) 0.7899(3) 1.0523(11) 0.0208(15) Uani d . . . 1 . .
O O6 0.8581(6) 0.6463(4) 1.2810(10) 0.0172(14) Uani d . . . 1 . .
O O7 0.7368(6) 0.7473(4) 1.4408(11) 0.0191(15) Uani d . . D 1 . .
H H7A 0.8191 0.7443 1.4839 0.029 Uiso calc U . DR 1 . .
H H7B 0.718(5) 0.786(4) 1.489(16) 0.029 Uiso d U . D 1 . .
O O8 0.4666(7) 0.6863(4) 1.2921(10) 0.0160(14) Uani d . . D 1 . .
H H8A 0.4981 0.7195 1.3854 0.024 Uiso calc U . DR 1 . .
H H8B 0.468(11) 0.6453(18) 1.354(8) 0.024 Uiso d U . D 1 . .
O O9 0.4491(8) 0.6798(4) 0.7527(13) 0.0329(19) Uani d . . D 1 . .
H H9A 0.434 0.6376 0.6954 0.049 Uiso calc U . DR 1 . .
H H9B 0.378(6) 0.706(3) 0.681(15) 0.049 Uiso d U . D 1 . .
O O10 0.6615(7) 0.5718(4) 0.9232(12) 0.0229(16) Uani d . . D 1 . .
H H10A 0.5928 0.5662 0.8056 0.034 Uiso calc U . DR 1 . .
H H10B 0.727(4) 0.583(7) 0.904(8) 0.034 Uiso d U . D 1 . .
O O11 0.7176(7) 0.7400(4) 0.9446(11) 0.0193(14) Uani d . . D 1 . .
H H11A 0.7443 0.7102 0.8834 0.029 Uiso calc U . DR 1 . .
H H11B 0.666(9) 0.771(4) 0.848(7) 0.029 Uiso d U . D 1 . .
O O12 0.6950(7) 0.5860(4) 1.4360(11) 0.0198(15) Uani d . . D 1 . .
H H12A 0.6762 0.5418 1.3944 0.03 Uiso calc U . DR 1 . .
H H12B 0.755(9) 0.587(3) 1.566(6) 0.03 Uiso d U . D 1 . .
Tb Tb1 0.61832(8) 0.66831(2) 1.13240(9) 0.01112(11) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.38(2) ?
C1 C2 . 1.446(19) ?
C1 C7 . 1.502(16) ?
C2 C3 . 1.396(10) ?
C2 H2 . 0.94 ?
C3 C4 . 1.349(18) ?
C3 C8 4_464 1.540(17) ?
C4 C5 . 1.40(2) ?
C4 H4 . 0.94 ?
C5 C6 . 1.384(9) ?
C5 C9 . 1.519(17) ?
C6 H6 . 0.94 ?
C7 O1 . 1.258(11) ?
C7 O2 . 1.261(11) ?
C8 O5 . 1.256(11) ?
C8 O6 4_464 1.259(11) ?
C8 C3 4_565 1.540(17) ?
C9 O3 . 1.263(11) ?
C9 O4 . 1.270(11) ?
O1 Tb1 . 2.358(7) ?
O5 Tb1 . 2.369(6) ?
O6 C8 4_565 1.259(11) ?
O6 Tb1 . 2.422(6) ?
O7 Tb1 . 2.401(6) ?
O7 H7A . 0.83 ?
O7 H7B . 0.843(15) ?
O8 Tb1 . 2.498(7) ?
O8 H8A . 0.83 ?
O8 H8B . 0.847(15) ?
O9 Tb1 . 2.459(8) ?
O9 H9A . 0.83 ?
O9 H9B . 0.855(15) ?
O10 Tb1 . 2.471(7) ?
O10 H10A . 0.83 ?
O10 H10B . 0.846(15) ?
O11 Tb1 . 2.477(7) ?
O11 H11A . 0.83 ?
O11 H11B . 0.853(15) ?
O12 Tb1 . 2.402(7) ?
O12 H12A . 0.83 ?
O12 H12B . 0.844(15) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C2 . . 119.7(13) ?
C6 C1 C7 . . 119.6(12) ?
C2 C1 C7 . . 120.6(11) ?
C3 C2 C1 . . 117.3(16) ?
C3 C2 H2 . . 121.3 ?
C1 C2 H2 . . 121.3 ?
C4 C3 C2 . . 122.6(16) ?
C4 C3 C8 . 4_464 119.1(11) ?
C2 C3 C8 . 4_464 118.2(14) ?
C3 C4 C5 . . 119.6(13) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
C6 C5 C4 . . 120.6(17) ?
C6 C5 C9 . . 118.2(16) ?
C4 C5 C9 . . 121.1(11) ?
C1 C6 C5 . . 120.2(18) ?
C1 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
O1 C7 O2 . . 124.1(8) ?
O1 C7 C1 . . 118.2(9) ?
O2 C7 C1 . . 117.7(9) ?
O5 C8 O6 . 4_464 124.8(8) ?
O5 C8 C3 . 4_565 118.1(8) ?
O6 C8 C3 4_464 4_565 117.1(8) ?
O3 C9 O4 . . 123.6(8) ?
O3 C9 C5 . . 117.7(9) ?
O4 C9 C5 . . 118.8(9) ?
C7 O1 Tb1 . . 157.9(6) ?
C8 O5 Tb1 . . 159.7(6) ?
C8 O6 Tb1 4_565 . 143.4(6) ?
Tb1 O7 H7A . . 109.5 ?
Tb1 O7 H7B . . 135.(5) ?
H7A O7 H7B . . 111.3 ?
Tb1 O8 H8A . . 109.5 ?
Tb1 O8 H8B . . 107.(7) ?
H8A O8 H8B . . 107.4 ?
Tb1 O9 H9A . . 109.5 ?
Tb1 O9 H9B . . 135.(6) ?
H9A O9 H9B . . 106.7 ?
Tb1 O10 H10A . . 109.5 ?
Tb1 O10 H10B . . 113.(7) ?
H10A O10 H10B . . 109.3 ?
Tb1 O11 H11A . . 109.5 ?
Tb1 O11 H11B . . 117.(7) ?
H11A O11 H11B . . 105.7 ?
Tb1 O12 H12A . . 109.5 ?
Tb1 O12 H12B . . 137.(5) ?
H12A O12 H12B . . 110.1 ?
O1 Tb1 O5 . . 111.5(2) ?
O1 Tb1 O7 . . 134.7(3) ?
O5 Tb1 O7 . . 71.3(2) ?
O1 Tb1 O12 . . 74.0(2) ?
O5 Tb1 O12 . . 134.0(2) ?
O7 Tb1 O12 . . 74.3(2) ?
O1 Tb1 O6 . . 125.1(2) ?
O5 Tb1 O6 . . 123.4(2) ?
O7 Tb1 O6 . . 71.4(2) ?
O12 Tb1 O6 . . 70.5(2) ?
O1 Tb1 O9 . . 69.3(3) ?
O5 Tb1 O9 . . 68.5(2) ?
O7 Tb1 O9 . . 139.1(2) ?
O12 Tb1 O9 . . 142.7(2) ?
O6 Tb1 O9 . . 127.5(3) ?
O1 Tb1 O10 . . 71.6(2) ?
O5 Tb1 O10 . . 133.9(2) ?
O7 Tb1 O10 . . 140.6(2) ?
O12 Tb1 O10 . . 91.9(2) ?
O6 Tb1 O10 . . 69.3(2) ?
O9 Tb1 O10 . . 70.6(2) ?
O1 Tb1 O11 . . 135.0(2) ?
O5 Tb1 O11 . . 71.6(2) ?
O7 Tb1 O11 . . 89.9(2) ?
O12 Tb1 O11 . . 137.7(3) ?
O6 Tb1 O11 . . 67.3(2) ?
O9 Tb1 O11 . . 71.1(3) ?
O10 Tb1 O11 . . 75.8(2) ?
O1 Tb1 O8 . . 66.9(2) ?
O5 Tb1 O8 . . 69.3(2) ?
O7 Tb1 O8 . . 73.1(2) ?
O12 Tb1 O8 . . 72.2(2) ?
O6 Tb1 O8 . . 133.9(2) ?
O9 Tb1 O8 . . 98.7(3) ?
O10 Tb1 O8 . . 138.1(2) ?
O11 Tb1 O8 . . 140.6(2) ?


_exptl_crystal_preparation       ', Luminescent'
