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

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

data_mo_BA7_0m
_database_code_depnum_ccdc_archive 'CCDC 1923048'
loop_
_audit_author_name
_audit_author_address
'Philip Netzsch'
;Universitaet Augsburg
Germany
;
_audit_update_record             
;
2019-08-02 deposited with the CCDC.	2019-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H O8 S2 Tb'
_chemical_formula_weight         352.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   6.6503(5)
_cell_length_b                   6.5941(5)
_cell_length_c                   6.8024(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.640(2)
_cell_angle_gamma                90
_cell_volume                     288.62(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    7319
_cell_measurement_theta_min      3.095
_cell_measurement_theta_max      31.166

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.051
_exptl_crystal_F_000             324
_exptl_transmission_factor_min   0.6057
_exptl_transmission_factor_max   0.7462
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    12.975
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
 multi-scan absorption correction using SADABS 
(G. M. Sheldrick, (1996). SADABS. Program for Empirical 
Absorption Correction. University of Göttingen, Germany.)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(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  'Bruker D8 Venture'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7319
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.095
_diffrn_reflns_theta_max         31.166
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1877
_reflns_number_gt                1748
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0076(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.032(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1877
_refine_ls_number_parameters     105
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0367
_refine_ls_wR_factor_gt          0.0358
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      0.926
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.35019(4) 0.74999(7) 0.63157(4) 0.00544(8) Uani 1 1 d . . . . .
S1 S 0.7801(2) 0.70420(19) 0.4304(2) 0.0062(3) Uani 1 1 d . . . . .
S2 S 0.2397(2) 0.5805(2) 0.1047(2) 0.0067(3) Uani 1 1 d . . . . .
O11 O 0.9876(6) 0.7299(13) 0.5621(7) 0.0106(11) Uani 1 1 d . . . . .
O12 O 0.6845(8) 0.9008(7) 0.3640(8) 0.0140(11) Uani 1 1 d . . . . .
O13 O 0.7803(7) 0.5722(7) 0.2560(7) 0.0094(9) Uani 1 1 d . . . . .
O14 O 0.6455(7) 0.5907(7) 0.5396(7) 0.0092(9) Uani 1 1 d . . . . .
O21 O 0.2410(7) 0.7037(6) 0.2819(7) 0.0116(11) Uani 1 1 d . . . . .
O22 O 0.3178(8) 0.6908(7) -0.0441(7) 0.0134(11) Uani 1 1 d . . . . .
O23 O 0.3500(8) 0.3905(7) 0.1617(7) 0.0132(10) Uani 1 1 d . . . . .
O24 O 0.0144(13) 0.5299(9) -0.0008(14) 0.0107(13) Uani 1 1 d D . . . .
H1 H -0.055(12) 0.542(12) 0.102(11) 0.016 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O22 2.304(5) 1_556 ?
Tb1 O12 2.315(5) 2_646 ?
Tb1 O23 2.323(5) 2_656 ?
Tb1 O21 2.325(5) . ?
Tb1 O11 2.340(4) 1_455 ?
Tb1 O14 2.444(5) . ?
Tb1 O13 2.487(5) 2_656 ?
Tb1 O14 2.534(5) 2_656 ?
Tb1 S1 3.1168(14) 2_656 ?
S1 O11 1.453(5) . ?
S1 O12 1.464(5) . ?
S1 O13 1.472(5) . ?
S1 O14 1.500(5) . ?
S1 Tb1 3.1168(14) 2_646 ?
S2 O22 1.445(5) . ?
S2 O21 1.452(5) . ?
S2 O23 1.454(5) . ?
S2 O24 1.525(8) . ?
O11 Tb1 2.340(4) 1_655 ?
O12 Tb1 2.315(5) 2_656 ?
O13 Tb1 2.487(5) 2_646 ?
O14 Tb1 2.534(5) 2_646 ?
O22 Tb1 2.304(5) 1_554 ?
O23 Tb1 2.323(5) 2_646 ?
O24 H1 0.93(5) . ?

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
O22 Tb1 O12 77.61(17) 1_556 2_646 ?
O22 Tb1 O23 76.19(17) 1_556 2_656 ?
O12 Tb1 O23 117.52(18) 2_646 2_656 ?
O22 Tb1 O21 151.29(17) 1_556 . ?
O12 Tb1 O21 82.90(16) 2_646 . ?
O23 Tb1 O21 132.08(17) 2_656 . ?
O22 Tb1 O11 80.97(17) 1_556 1_455 ?
O12 Tb1 O11 81.1(2) 2_646 1_455 ?
O23 Tb1 O11 145.9(2) 2_656 1_455 ?
O21 Tb1 O11 75.32(16) . 1_455 ?
O22 Tb1 O14 116.62(17) 1_556 . ?
O12 Tb1 O14 70.42(16) 2_646 . ?
O23 Tb1 O14 72.80(17) 2_656 . ?
O21 Tb1 O14 75.22(16) . . ?
O11 Tb1 O14 141.0(2) 1_455 . ?
O22 Tb1 O13 74.09(16) 1_556 2_656 ?
O12 Tb1 O13 143.32(18) 2_646 2_656 ?
O23 Tb1 O13 77.63(17) 2_656 2_656 ?
O21 Tb1 O13 112.56(15) . 2_656 ?
O11 Tb1 O13 71.9(2) 1_455 2_656 ?
O14 Tb1 O13 144.21(16) . 2_656 ?
O22 Tb1 O14 127.22(16) 1_556 2_656 ?
O12 Tb1 O14 154.23(18) 2_646 2_656 ?
O23 Tb1 O14 79.44(16) 2_656 2_656 ?
O21 Tb1 O14 71.53(15) . 2_656 ?
O11 Tb1 O14 95.0(2) 1_455 2_656 ?
O14 Tb1 O14 99.22(9) . 2_656 ?
O13 Tb1 O14 55.20(16) 2_656 2_656 ?
O22 Tb1 S1 101.67(12) 1_556 2_656 ?
O12 Tb1 S1 158.80(13) 2_646 2_656 ?
O23 Tb1 S1 82.26(13) 2_656 2_656 ?
O21 Tb1 S1 89.06(11) . 2_656 ?
O11 Tb1 S1 77.9(2) 1_455 2_656 ?
O14 Tb1 S1 126.33(11) . 2_656 ?
O13 Tb1 S1 27.64(11) 2_656 2_656 ?
O14 Tb1 S1 28.47(11) 2_656 2_656 ?
O11 S1 O12 111.0(4) . . ?
O11 S1 O13 111.9(3) . . ?
O12 S1 O13 111.4(3) . . ?
O11 S1 O14 110.2(3) . . ?
O12 S1 O14 109.1(3) . . ?
O13 S1 O14 103.1(3) . . ?
O11 S1 Tb1 112.6(3) . 2_646 ?
O12 S1 Tb1 136.5(2) . 2_646 ?
O13 S1 Tb1 51.63(19) . 2_646 ?
O14 S1 Tb1 53.63(18) . 2_646 ?
O22 S2 O21 111.8(3) . . ?
O22 S2 O23 111.9(3) . . ?
O21 S2 O23 111.4(3) . . ?
O22 S2 O24 105.4(4) . . ?
O21 S2 O24 108.2(4) . . ?
O23 S2 O24 107.9(3) . . ?
S1 O11 Tb1 154.2(3) . 1_655 ?
S1 O12 Tb1 156.0(3) . 2_656 ?
S1 O13 Tb1 100.7(2) . 2_646 ?
S1 O14 Tb1 122.1(3) . . ?
S1 O14 Tb1 97.9(2) . 2_646 ?
Tb1 O14 Tb1 127.00(19) . 2_646 ?
S2 O21 Tb1 149.0(3) . . ?
S2 O22 Tb1 153.2(3) . 1_554 ?
S2 O23 Tb1 143.5(3) . 2_646 ?
S2 O24 H1 104(5) . . ?

_refine_diff_density_max         0.925
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.187

