
data_mo_PN83Yb_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 Yb2'
_chemical_formula_weight         944.06

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'
Yb Yb -0.3850 5.5486 '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                   13.4949(11)
_cell_length_b                   11.3452(9)
_cell_length_c                   10.7961(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.390(2)
_cell_angle_gamma                90
_cell_volume                     1650.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    2238
_cell_measurement_theta_min      2.347
_cell_measurement_theta_max      29.999

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.800
_exptl_crystal_F_000             1752
_exptl_transmission_factor_min   0.6527
_exptl_transmission_factor_max   0.7490
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    12.166
_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            19093
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_av_R_equivalents  0.0289
_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         2.347
_diffrn_reflns_theta_max         29.999
_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             2409
_reflns_number_gt                2238
_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)+(0.0103P)²+4.7218P] 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       0.00030(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2409
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0128
_refine_ls_wR_factor_ref         0.0281
_refine_ls_wR_factor_gt          0.0277
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.003
_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
Yb1 Yb 0.68867(2) 0.54833(2) 0.65352(2) 0.00607(3) Uani 1 1 d . . . . .
S1 S 0.35964(4) 0.29936(4) 0.64008(5) 0.00541(9) Uani 1 1 d . . . . .
S2 S 0.37114(4) 0.01185(5) 0.42229(5) 0.00639(10) Uani 1 1 d . . . . .
S3 S 0.57865(4) 0.35437(5) 0.41806(5) 0.00638(9) Uani 1 1 d . . . . .
O13 O 0.31786(12) 0.34369(14) 0.52217(14) 0.0096(3) Uani 1 1 d . . . . .
O24 O 0.54241(12) 0.07035(13) 0.59749(15) 0.0086(3) Uani 1 1 d . . . . .
O14 O 0.46442(12) 0.25293(14) 0.61894(14) 0.0087(3) Uani 1 1 d . . . . .
O33 O 0.64466(13) 0.35162(15) 0.31715(16) 0.0141(3) Uani 1 1 d . . . . .
O31 O 0.48013(13) 0.39418(18) 0.38330(17) 0.0187(4) Uani 1 1 d . . . . .
O12 O 0.30239(13) 0.20163(15) 0.68436(15) 0.0125(3) Uani 1 1 d . . . . .
O23 O 0.41794(12) 0.13288(14) 0.43657(15) 0.0103(3) Uani 1 1 d . . . . .
O11 O 0.37572(13) 0.39145(14) 0.73144(16) 0.0123(3) Uani 1 1 d . . . . .
O34 O 0.57492(13) 0.22475(14) 0.45638(16) 0.0125(3) Uani 1 1 d . . . . .
O22 O 0.32367(13) -0.01905(15) 0.53326(16) 0.0132(3) Uani 1 1 d . . . . .
O21 O 0.31084(12) 0.01580(15) 0.30866(16) 0.0122(3) Uani 1 1 d . . . . .
O32 O 0.62317(15) 0.41710(17) 0.52239(18) 0.0213(4) Uani 1 1 d . . . . .
B1 B 0.49892(18) 0.1718(2) 0.5269(2) 0.0069(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
Yb1 O32 2.2031(18) . ?
Yb1 O33 2.2104(16) 6_566 ?
Yb1 O13 2.2553(16) 5_666 ?
Yb1 O12 2.3304(16) 3 ?
Yb1 O11 2.3649(16) 2_656 ?
Yb1 O31 2.3802(18) 5_666 ?
Yb1 O21 2.3930(17) 8_556 ?
Yb1 O22 2.4226(16) 3 ?
S1 O11 1.4445(16) . ?
S1 O12 1.4486(16) . ?
S1 O13 1.4513(16) . ?
S1 O14 1.5384(16) . ?
S2 O21 1.4321(17) . ?
S2 O22 1.4350(17) . ?
S2 O23 1.5154(16) . ?
S2 O24 1.5185(16) 5_656 ?
S3 O31 1.4329(18) . ?
S3 O32 1.4340(19) . ?
S3 O33 1.4479(16) . ?
S3 O34 1.5293(16) . ?
O13 Yb1 2.2553(15) 5_666 ?
O24 B1 1.482(3) . ?
O24 S2 1.5185(16) 5_656 ?
O14 B1 1.451(3) . ?
O33 Yb1 2.2104(16) 6_565 ?
O31 Yb1 2.3802(18) 5_666 ?
O12 Yb1 2.3304(16) 3_445 ?
O23 B1 1.488(3) . ?
O11 Yb1 2.3649(16) 2_656 ?
O34 B1 1.444(3) . ?
O22 Yb1 2.4226(16) 3_445 ?
O21 Yb1 2.3930(17) 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
O32 Yb1 O33 138.08(7) . 6_566 ?
O32 Yb1 O13 80.36(7) . 5_666 ?
O33 Yb1 O13 113.22(6) 6_566 5_666 ?
O32 Yb1 O12 146.30(6) . 3 ?
O33 Yb1 O12 73.04(6) 6_566 3 ?
O13 Yb1 O12 72.98(6) 5_666 3 ?
O32 Yb1 O11 71.52(7) . 2_656 ?
O33 Yb1 O11 80.93(6) 6_566 2_656 ?
O13 Yb1 O11 148.56(6) 5_666 2_656 ?
O12 Yb1 O11 138.24(6) 3 2_656 ?
O32 Yb1 O31 74.59(7) . 5_666 ?
O33 Yb1 O31 72.13(7) 6_566 5_666 ?
O13 Yb1 O31 73.82(6) 5_666 5_666 ?
O12 Yb1 O31 115.78(7) 3 5_666 ?
O11 Yb1 O31 85.20(6) 2_656 5_666 ?
O32 Yb1 O21 118.55(7) . 8_556 ?
O33 Yb1 O21 78.65(6) 6_566 8_556 ?
O13 Yb1 O21 138.14(6) 5_666 8_556 ?
O12 Yb1 O21 72.92(6) 3 8_556 ?
O11 Yb1 O21 70.30(6) 2_656 8_556 ?
O31 Yb1 O21 144.41(6) 5_666 8_556 ?
O32 Yb1 O22 74.23(7) . 3 ?
O33 Yb1 O22 146.76(6) 6_566 3 ?
O13 Yb1 O22 73.38(6) 5_666 3 ?
O12 Yb1 O22 78.60(6) 3 3 ?
O11 Yb1 O22 110.81(6) 2_656 3 ?
O31 Yb1 O22 137.70(6) 5_666 3 ?
O21 Yb1 O22 76.72(6) 8_556 3 ?
O11 S1 O12 112.94(10) . . ?
O11 S1 O13 112.53(10) . . ?
O12 S1 O13 111.57(10) . . ?
O11 S1 O14 104.28(9) . . ?
O12 S1 O14 107.44(10) . . ?
O13 S1 O14 107.54(9) . . ?
O21 S2 O22 117.63(11) . . ?
O21 S2 O23 105.73(10) . . ?
O22 S2 O23 109.90(10) . . ?
O21 S2 O24 107.52(10) . 5_656 ?
O22 S2 O24 110.61(9) . 5_656 ?
O23 S2 O24 104.58(9) . 5_656 ?
O31 S3 O32 112.86(12) . . ?
O31 S3 O33 114.36(11) . . ?
O32 S3 O33 110.72(11) . . ?
O31 S3 O34 109.21(11) . . ?
O32 S3 O34 106.48(11) . . ?
O33 S3 O34 102.38(10) . . ?
S1 O13 Yb1 156.88(10) . 5_666 ?
B1 O24 S2 133.53(14) . 5_656 ?
B1 O14 S1 130.81(15) . . ?
S3 O33 Yb1 142.81(11) . 6_565 ?
S3 O31 Yb1 173.76(11) . 5_666 ?
S1 O12 Yb1 152.09(11) . 3_445 ?
B1 O23 S2 128.40(14) . . ?
S1 O11 Yb1 149.09(11) . 2_656 ?
B1 O34 S3 125.34(15) . . ?
S2 O22 Yb1 139.23(10) . 3_445 ?
S2 O21 Yb1 157.38(11) . 8_455 ?
S3 O32 Yb1 166.82(14) . . ?
O34 B1 O14 111.34(18) . . ?
O34 B1 O24 108.79(18) . . ?
O14 B1 O24 105.89(17) . . ?
O34 B1 O23 107.16(18) . . ?
O14 B1 O23 112.59(18) . . ?
O24 B1 O23 111.07(18) . . ?

_refine_diff_density_max         0.535
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.114



