
data_mo_PN150_II_0m

_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            'B2 O24 S6 Tm2'
_chemical_formula_weight         935.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   13.4981(4)
_cell_length_b                   11.3617(3)
_cell_length_c                   10.8327(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.4500(9)
_cell_angle_gamma                90
_cell_volume                     1658.31(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    299(2)
_cell_measurement_reflns_used    2207
_cell_measurement_theta_min      2.345
_cell_measurement_theta_max      29.991

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.748
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   0.6035
_exptl_transmission_factor_max   0.7482
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    11.526
_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      299(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            18788
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.345
_diffrn_reflns_theta_max         29.991
_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             2419
_reflns_number_gt                2207
_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       ?
_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          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0117P)²+4.0159P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00036(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2419
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0142
_refine_ls_wR_factor_ref         0.0303
_refine_ls_wR_factor_gt          0.0297
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Tm1 Tm 0.18856(2) 0.04850(2) 0.15385(2) 0.00616(4) Uani 1 1 d . . . . .
B1 B 0.5008(2) 0.1717(2) 0.4732(2) 0.0075(5) Uani 1 1 d . . . . .
S1 S 0.07850(4) 0.14620(5) 0.41821(5) 0.00650(11) Uani 1 1 d . . . . .
S2 S 0.13996(4) -0.20071(5) 0.36004(5) 0.00547(10) Uani 1 1 d . . . . .
S3 S 0.37115(4) -0.01195(5) 0.42241(5) 0.00635(11) Uani 1 1 d . . . . .
O11 O 0.12163(16) 0.08277(18) 0.52256(19) 0.0216(4) Uani 1 1 d . . . . .
O12 O 0.02012(14) 0.10730(18) 0.11781(19) 0.0184(4) Uani 1 1 d . . . . .
O13 O 0.14496(13) 0.14833(16) 0.31855(17) 0.0138(4) Uani 1 1 d . . . . .
O14 O 0.42515(13) 0.22453(14) 0.54316(17) 0.0123(4) Uani 1 1 d . . . . .
O21 O 0.12386(13) -0.10890(15) 0.26898(17) 0.0117(4) Uani 1 1 d . . . . .
O22 O 0.30306(13) 0.20176(15) 0.18450(17) 0.0125(4) Uani 1 1 d . . . . .
O23 O 0.18197(13) 0.15643(15) -0.02238(16) 0.0098(3) Uani 1 1 d . . . . .
O24 O 0.03534(12) -0.24747(15) 0.38136(16) 0.0092(3) Uani 1 1 d . . . . .
O31 O 0.31110(13) -0.01621(16) 0.30887(17) 0.0117(4) Uani 1 1 d . . . . .
O32 O 0.32343(14) -0.01889(15) 0.03262(17) 0.0124(4) Uani 1 1 d . . . . .
O33 O 0.58234(13) 0.13287(14) 0.56317(17) 0.0104(3) Uani 1 1 d . . . . .
O34 O 0.45774(12) 0.07012(14) 0.40256(16) 0.0084(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O11 2.2155(19) 6 ?
Tm1 O13 2.2232(18) . ?
Tm1 O23 2.2662(17) . ?
Tm1 O22 2.3387(17) . ?
Tm1 O21 2.3764(17) . ?
Tm1 O12 2.3793(18) . ?
Tm1 O31 2.4005(17) . ?
Tm1 O32 2.4317(18) . ?
B1 O14 1.439(3) . ?
B1 O24 1.451(3) 3 ?
B1 O34 1.483(3) . ?
B1 O33 1.492(3) . ?
S1 O11 1.434(2) . ?
S1 O12 1.4342(19) 2 ?
S1 O13 1.4447(19) . ?
S1 O14 1.5288(17) 7_556 ?
S2 O21 1.4432(17) . ?
S2 O22 1.4480(18) 4_545 ?
S2 O23 1.4526(17) 6_556 ?
S2 O24 1.5391(17) . ?
S3 O31 1.4325(18) . ?
S3 O32 1.4337(19) 6_556 ?
S3 O33 1.5147(17) 5_656 ?
S3 O34 1.5205(17) . ?
O11 Tm1 2.2155(19) 6_556 ?
O12 S1 1.4342(19) 2 ?
O14 S1 1.5288(17) 7_556 ?
O22 S2 1.4481(18) 4 ?
O23 S2 1.4526(17) 6 ?
O24 B1 1.451(3) 3_445 ?
O32 S3 1.4337(19) 6 ?
O33 S3 1.5147(17) 5_656 ?

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
O11 Tm1 O13 137.84(7) 6 . ?
O11 Tm1 O23 80.20(7) 6 . ?
O13 Tm1 O23 113.65(7) . . ?
O11 Tm1 O22 146.39(7) 6 . ?
O13 Tm1 O22 73.19(7) . . ?
O23 Tm1 O22 73.07(6) . . ?
O11 Tm1 O21 71.44(7) 6 . ?
O13 Tm1 O21 80.76(7) . . ?
O23 Tm1 O21 148.46(6) . . ?
O22 Tm1 O21 138.28(6) . . ?
O11 Tm1 O12 74.64(8) 6 . ?
O13 Tm1 O12 72.06(7) . . ?
O23 Tm1 O12 73.81(6) . . ?
O22 Tm1 O12 115.53(7) . . ?
O21 Tm1 O12 85.40(6) . . ?
O11 Tm1 O31 118.69(7) 6 . ?
O13 Tm1 O31 78.43(7) . . ?
O23 Tm1 O31 138.20(6) . . ?
O22 Tm1 O31 72.97(6) . . ?
O21 Tm1 O31 70.24(6) . . ?
O12 Tm1 O31 144.31(7) . . ?
O11 Tm1 O32 74.39(7) 6 . ?
O13 Tm1 O32 146.83(6) . . ?
O23 Tm1 O32 73.03(6) . . ?
O22 Tm1 O32 78.54(6) . . ?
O21 Tm1 O32 110.93(6) . . ?
O12 Tm1 O32 137.64(7) . . ?
O31 Tm1 O32 76.97(6) . . ?
O14 B1 O24 111.4(2) . 3 ?
O14 B1 O34 109.14(19) . . ?
O24 B1 O34 105.74(19) 3 . ?
O14 B1 O33 107.3(2) . . ?
O24 B1 O33 112.3(2) 3 . ?
O34 B1 O33 110.96(19) . . ?
O11 S1 O12 112.69(13) . 2 ?
O11 S1 O13 110.88(12) . . ?
O12 S1 O13 114.19(11) 2 . ?
O11 S1 O14 106.57(12) . 7_556 ?
O12 S1 O14 109.01(11) 2 7_556 ?
O13 S1 O14 102.72(10) . 7_556 ?
O21 S2 O22 112.73(11) . 4_545 ?
O21 S2 O23 112.57(11) . 6_556 ?
O22 S2 O23 111.72(10) 4_545 6_556 ?
O21 S2 O24 104.50(10) . . ?
O22 S2 O24 107.24(10) 4_545 . ?
O23 S2 O24 107.53(10) 6_556 . ?
O31 S3 O32 117.64(11) . 6_556 ?
O31 S3 O33 105.51(10) . 5_656 ?
O32 S3 O33 109.88(11) 6_556 5_656 ?
O31 S3 O34 107.42(10) . . ?
O32 S3 O34 110.83(10) 6_556 . ?
O33 S3 O34 104.68(10) 5_656 . ?
S1 O11 Tm1 167.09(14) . 6_556 ?
S1 O12 Tm1 173.34(13) 2 . ?
S1 O13 Tm1 142.88(11) . . ?
B1 O14 S1 125.50(16) . 7_556 ?
S2 O21 Tm1 149.06(11) . . ?
S2 O22 Tm1 151.91(11) 4 . ?
S2 O23 Tm1 156.85(11) 6 . ?
B1 O24 S2 131.06(16) 3_445 . ?
S3 O31 Tm1 157.03(12) . . ?
S3 O32 Tm1 139.57(11) 6 . ?
B1 O33 S3 128.33(15) . 5_656 ?
B1 O34 S3 133.22(16) . . ?

_refine_diff_density_max         0.528
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.123



