
data_mo_MH061_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 Lu2 O24 S6'
_chemical_formula_weight         947.92

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'
Lu Lu -0.4720 5.8584 '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                   13.469(3)
_cell_length_b                   11.364(3)
_cell_length_c                   10.799(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.369(8)
_cell_angle_gamma                90
_cell_volume                     1650.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3251
_cell_measurement_theta_min      2.347
_cell_measurement_theta_max      33.550

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.816
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   0.4652
_exptl_transmission_factor_max   0.7466
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    12.795
_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      300(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            29911
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.347
_diffrn_reflns_theta_max         33.550
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3251
_reflns_number_gt                2789
_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)+(0.0215P)²+0.9933P] 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       0.00060(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3251
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0522
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.31139(2) 0.04838(2) 0.84664(2) 0.00592(5) Uani 1 1 d . . . . .
B1 B 0.4992(3) 0.3279(3) 1.0268(3) 0.0061(6) Uani 1 1 d . . . . .
S1 S 0.57854(6) 0.14531(6) 0.91790(7) 0.00629(13) Uani 1 1 d . . . . .
S2 S 0.35951(6) -0.20058(6) 0.64019(7) 0.00547(13) Uani 1 1 d . . . . .
S3 S 0.12920(6) -0.01166(7) 0.57781(7) 0.00610(13) Uani 1 1 d . . . . .
O11 O 0.57443(18) 0.27482(19) 0.9560(2) 0.0121(5) Uani 1 1 d . . . . .
O12 O 0.6234(2) 0.0828(2) 1.0227(3) 0.0205(6) Uani 1 1 d . . . . .
O13 O 0.4795(2) 0.1051(2) 0.8835(3) 0.0181(5) Uani 1 1 d . . . . .
O14 O 0.35597(19) 0.1476(2) 0.6833(2) 0.0136(5) Uani 1 1 d . . . . .
O21 O 0.37503(19) -0.1086(2) 0.7315(2) 0.0124(5) Uani 1 1 d . . . . .
O22 O 0.19767(18) 0.2017(2) 0.8148(2) 0.0120(5) Uani 1 1 d . . . . .
O23 O 0.31759(18) 0.1561(2) 1.0220(2) 0.0103(4) Uani 1 1 d . . . . .
O24 O 0.46448(17) -0.2471(2) 0.6189(2) 0.0088(4) Uani 1 1 d . . . . .
O31 O 0.18948(18) -0.0151(2) 0.6916(2) 0.0108(4) Uani 1 1 d . . . . .
O32 O 0.17667(19) -0.0191(2) 0.9667(2) 0.0130(5) Uani 1 1 d . . . . .
O33 O -0.08239(18) 0.1322(2) 0.4367(2) 0.0106(4) Uani 1 1 d . . . . .
O34 O 0.04234(17) 0.0706(2) 0.5973(2) 0.0085(4) 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
Lu1 O12 2.200(3) 5_657 ?
Lu1 O14 2.206(2) . ?
Lu1 O23 2.252(2) . ?
Lu1 O22 2.332(2) . ?
Lu1 O21 2.364(2) . ?
Lu1 O13 2.366(3) . ?
Lu1 O31 2.386(3) . ?
Lu1 O32 2.416(2) . ?
B1 O11 1.438(4) . ?
B1 O24 1.451(4) 6_556 ?
B1 O34 1.482(4) 8_556 ?
B1 O33 1.494(4) 8_556 ?
S1 O13 1.438(3) . ?
S1 O12 1.438(3) . ?
S1 O14 1.444(3) 2_656 ?
S1 O11 1.530(2) . ?
S2 O21 1.444(2) . ?
S2 O22 1.451(2) 4_546 ?
S2 O23 1.456(2) 6 ?
S2 O24 1.539(2) . ?
S3 O31 1.433(3) . ?
S3 O32 1.436(3) 6 ?
S3 O33 1.512(2) 5_556 ?
S3 O34 1.522(2) . ?
O12 Lu1 2.200(3) 5_657 ?
O14 S1 1.444(2) 2_656 ?
O22 S2 1.451(2) 4_556 ?
O23 S2 1.456(2) 6_556 ?
O24 B1 1.451(4) 6 ?
O32 S3 1.436(3) 6_556 ?
O33 B1 1.494(4) 8_455 ?
O33 S3 1.512(2) 5_556 ?
O34 B1 1.482(4) 8_455 ?

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
O12 Lu1 O14 137.89(10) 5_657 . ?
O12 Lu1 O23 80.52(10) 5_657 . ?
O14 Lu1 O23 113.34(10) . . ?
O12 Lu1 O22 146.61(10) 5_657 . ?
O14 Lu1 O22 73.00(9) . . ?
O23 Lu1 O22 73.11(9) . . ?
O12 Lu1 O21 71.50(10) 5_657 . ?
O14 Lu1 O21 80.84(9) . . ?
O23 Lu1 O21 148.84(9) . . ?
O22 Lu1 O21 137.87(9) . . ?
O12 Lu1 O13 74.59(11) 5_657 . ?
O14 Lu1 O13 72.10(10) . . ?
O23 Lu1 O13 73.89(9) . . ?
O22 Lu1 O13 115.79(10) . . ?
O21 Lu1 O13 85.48(9) . . ?
O12 Lu1 O31 118.53(10) 5_657 . ?
O14 Lu1 O31 78.58(10) . . ?
O23 Lu1 O31 138.07(8) . . ?
O22 Lu1 O31 72.76(9) . . ?
O21 Lu1 O31 70.05(9) . . ?
O13 Lu1 O31 144.38(9) . . ?
O12 Lu1 O32 74.04(10) 5_657 . ?
O14 Lu1 O32 147.08(9) . . ?
O23 Lu1 O32 73.33(9) . . ?
O22 Lu1 O32 78.97(9) . . ?
O21 Lu1 O32 110.47(9) . . ?
O13 Lu1 O32 137.54(10) . . ?
O31 Lu1 O32 76.88(9) . . ?
O11 B1 O24 111.3(3) . 6_556 ?
O11 B1 O34 109.4(3) . 8_556 ?
O24 B1 O34 105.8(3) 6_556 8_556 ?
O11 B1 O33 107.2(3) . 8_556 ?
O24 B1 O33 112.6(3) 6_556 8_556 ?
O34 B1 O33 110.5(3) 8_556 8_556 ?
O13 S1 O12 112.72(18) . . ?
O13 S1 O14 114.13(16) . 2_656 ?
O12 S1 O14 110.93(17) . 2_656 ?
O13 S1 O11 109.12(16) . . ?
O12 S1 O11 106.47(17) . . ?
O14 S1 O11 102.70(14) 2_656 . ?
O21 S2 O22 112.56(15) . 4_546 ?
O21 S2 O23 112.36(15) . 6 ?
O22 S2 O23 111.92(15) 4_546 6 ?
O21 S2 O24 104.69(14) . . ?
O22 S2 O24 107.30(14) 4_546 . ?
O23 S2 O24 107.49(14) 6 . ?
O31 S3 O32 117.76(16) . 6 ?
O31 S3 O33 106.02(14) . 5_556 ?
O32 S3 O33 109.70(15) 6 5_556 ?
O31 S3 O34 107.40(14) . . ?
O32 S3 O34 110.49(14) 6 . ?
O33 S3 O34 104.58(14) 5_556 . ?
B1 O11 S1 125.8(2) . . ?
S1 O12 Lu1 166.5(2) . 5_657 ?
S1 O13 Lu1 173.90(18) . . ?
S1 O14 Lu1 143.41(16) 2_656 . ?
S2 O21 Lu1 149.68(16) . . ?
S2 O22 Lu1 151.54(16) 4_556 . ?
S2 O23 Lu1 156.83(16) 6_556 . ?
B1 O24 S2 130.9(2) 6 . ?
S3 O31 Lu1 157.67(17) . . ?
S3 O32 Lu1 139.18(15) 6_556 . ?
B1 O33 S3 128.9(2) 8_455 5_556 ?
B1 O34 S3 133.5(2) 8_455 . ?

_refine_diff_density_max         1.831
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.239



