
data_mo_PN163_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 Sm2'
_chemical_formula_weight         898.68

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'
Sm Sm -0.1638 3.4418 '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                   13.636(3)
_cell_length_b                   11.492(3)
_cell_length_c                   11.112(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.567(6)
_cell_angle_gamma                90
_cell_volume                     1738.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    19598
_cell_measurement_theta_min      2.320
_cell_measurement_theta_max      29.998

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.435
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   0.6730
_exptl_transmission_factor_max   0.7479
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    7.546
_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      298(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            19598
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.320
_diffrn_reflns_theta_max         29.998
_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             2543
_reflns_number_gt                2305
_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)+(0.0196P)²+3.7024P] 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       0.00014(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2543
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0163
_refine_ls_wR_factor_ref         0.0381
_refine_ls_wR_factor_gt          0.0370
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Sm1 Sm 0.31220(2) 0.04808(2) 0.84446(2) 0.00698(4) Uani 1 1 d . . . . .
B1 B 0.49931(19) 0.3302(2) 1.0279(2) 0.0089(5) Uani 1 1 d . . . . .
S1 S 0.36252(4) -0.20180(5) 0.63874(5) 0.00699(10) Uani 1 1 d . . . . .
S2 S 0.57790(4) 0.15012(5) 0.91951(5) 0.00772(10) Uani 1 1 d . . . . .
S3 S 0.62776(4) 0.51277(5) 1.07689(5) 0.00805(10) Uani 1 1 d . . . . .
O11 O 0.37945(13) -0.11089(15) 0.72738(16) 0.0141(3) Uani 1 1 d . . . . .
O12 O 0.19439(13) 0.20242(16) 0.81718(16) 0.0144(4) Uani 1 1 d . . . . .
O13 O 0.32060(13) 0.15768(15) 1.02438(15) 0.0119(3) Uani 1 1 d . . . . .
O14 O 0.46549(12) -0.24972(15) 0.61754(15) 0.0109(3) Uani 1 1 d . . . . .
O21 O 0.61540(16) 0.08454(19) 1.02236(18) 0.0241(4) Uani 1 1 d . . . . .
O22 O 0.48015(13) 0.11498(18) 0.87874(17) 0.0200(4) Uani 1 1 d . . . . .
O23 O 0.64650(13) 0.15141(17) 0.82538(16) 0.0162(4) Uani 1 1 d . . . . .
O24 O 0.57472(13) 0.27777(15) 0.95930(17) 0.0142(4) Uani 1 1 d . . . . .
O31 O 0.18648(13) -0.01826(16) 0.68784(17) 0.0148(4) Uani 1 1 d . . . . .
O32 O 0.17622(13) -0.01901(16) 0.97074(16) 0.0147(4) Uani 1 1 d . . . . .
O33 O 0.58123(13) 0.63215(15) 1.06006(16) 0.0126(3) Uani 1 1 d . . . . .
O34 O 0.54196(12) 0.43139(14) 1.09604(15) 0.0100(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
Sm1 O21 2.3033(19) 5_657 ?
Sm1 O23 2.3284(18) 2_656 ?
Sm1 O13 2.3597(17) . ?
Sm1 O12 2.3997(18) . ?
Sm1 O22 2.4234(19) . ?
Sm1 O11 2.4534(17) . ?
Sm1 O31 2.4856(18) . ?
Sm1 O32 2.5151(18) . ?
B1 O24 1.448(3) . ?
B1 O14 1.455(3) 6_556 ?
B1 O34 1.487(3) . ?
B1 O33 1.488(3) 5_667 ?
S1 O11 1.4445(18) . ?
S1 O12 1.4494(18) 4_546 ?
S1 O13 1.4521(17) 6 ?
S1 O14 1.5400(17) . ?
S2 O21 1.436(2) . ?
S2 O22 1.4386(19) . ?
S2 O23 1.4461(18) . ?
S2 O24 1.5335(18) . ?
S3 O31 1.4292(19) 8_556 ?
S3 O32 1.4346(18) 3 ?
S3 O33 1.5182(18) . ?
S3 O34 1.5231(17) . ?
O12 S1 1.4494(18) 4_556 ?
O13 S1 1.4521(17) 6_556 ?
O14 B1 1.455(3) 6 ?
O21 Sm1 2.3034(19) 5_657 ?
O23 Sm1 2.3284(18) 2_656 ?
O31 S3 1.4291(19) 8_455 ?
O32 S3 1.4346(18) 3_445 ?
O33 B1 1.488(3) 5_667 ?

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
O21 Sm1 O23 137.95(7) 5_657 2_656 ?
O21 Sm1 O13 79.20(7) 5_657 . ?
O23 Sm1 O13 114.40(7) 2_656 . ?
O21 Sm1 O12 145.80(7) 5_657 . ?
O23 Sm1 O12 73.41(6) 2_656 . ?
O13 Sm1 O12 73.10(6) . . ?
O21 Sm1 O22 75.28(8) 5_657 . ?
O23 Sm1 O22 72.05(7) 2_656 . ?
O13 Sm1 O22 72.66(6) . . ?
O12 Sm1 O22 113.83(7) . . ?
O21 Sm1 O11 71.86(7) 5_657 . ?
O23 Sm1 O11 80.37(7) 2_656 . ?
O13 Sm1 O11 147.86(6) . . ?
O12 Sm1 O11 138.83(6) . . ?
O22 Sm1 O11 86.49(6) . . ?
O21 Sm1 O31 119.76(7) 5_657 . ?
O23 Sm1 O31 77.29(7) 2_656 . ?
O13 Sm1 O31 138.76(6) . . ?
O12 Sm1 O31 73.21(6) . . ?
O22 Sm1 O31 144.22(6) . . ?
O11 Sm1 O31 70.40(6) . . ?
O21 Sm1 O32 74.94(7) 5_657 . ?
O23 Sm1 O32 146.35(6) 2_656 . ?
O13 Sm1 O32 71.91(6) . . ?
O12 Sm1 O32 77.64(6) . . ?
O22 Sm1 O32 137.05(6) . . ?
O11 Sm1 O32 112.36(6) . . ?
O31 Sm1 O32 78.25(6) . . ?
O24 B1 O14 111.2(2) . 6_556 ?
O24 B1 O34 108.99(19) . . ?
O14 B1 O34 106.19(19) 6_556 . ?
O24 B1 O33 107.14(19) . 5_667 ?
O14 B1 O33 112.46(19) 6_556 5_667 ?
O34 B1 O33 110.87(19) . 5_667 ?
O11 S1 O12 112.65(11) . 4_546 ?
O11 S1 O13 112.44(11) . 6 ?
O12 S1 O13 111.78(10) 4_546 6 ?
O11 S1 O14 104.74(10) . . ?
O12 S1 O14 107.01(10) 4_546 . ?
O13 S1 O14 107.70(10) 6 . ?
O21 S2 O22 112.35(13) . . ?
O21 S2 O23 111.51(12) . . ?
O22 S2 O23 113.80(11) . . ?
O21 S2 O24 106.71(12) . . ?
O22 S2 O24 108.48(11) . . ?
O23 S2 O24 103.29(11) . . ?
O31 S3 O32 117.29(12) 8_556 3 ?
O31 S3 O33 105.89(11) 8_556 . ?
O32 S3 O33 109.82(11) 3 . ?
O31 S3 O34 107.49(10) 8_556 . ?
O32 S3 O34 110.84(10) 3 . ?
O33 S3 O34 104.67(10) . . ?
S1 O11 Sm1 148.32(11) . . ?
S1 O12 Sm1 152.49(11) 4_556 . ?
S1 O13 Sm1 157.46(11) 6_556 . ?
B1 O14 S1 131.51(16) 6 . ?
S2 O21 Sm1 167.31(14) . 5_657 ?
S2 O22 Sm1 170.59(13) . . ?
S2 O23 Sm1 141.35(11) . 2_656 ?
B1 O24 S2 125.67(16) . . ?
S3 O31 Sm1 156.28(12) 8_455 . ?
S3 O32 Sm1 140.71(11) 3_445 . ?
B1 O33 S3 129.01(15) 5_667 . ?
B1 O34 S3 133.53(16) . . ?

_refine_diff_density_max         0.589
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.123



