
data_mo_pn38_2_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 Pr2 S6'
_chemical_formula_weight         879.80

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'
Pr Pr -0.2180 2.8214 '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                   13.7141(11)
_cell_length_b                   11.5305(9)
_cell_length_c                   11.2643(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.638(2)
_cell_angle_gamma                90
_cell_volume                     1777.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    2565
_cell_measurement_theta_min      2.310
_cell_measurement_theta_max      30.555

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.287
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   0.6174
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    6.252
_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            24061
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.310
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2719
_reflns_number_gt                2565
_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)+(0.0162P)²+3.7272P] 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       0.00090(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2719
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0140
_refine_ls_wR_factor_ref         0.0343
_refine_ls_wR_factor_gt          0.0337
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
Pr01 Pr 0.31256(2) 0.45204(2) 0.34302(2) 0.00552(4) Uani 1 1 d . . . . .
S1 S 0.63584(3) 0.70243(4) 0.36238(4) 0.00535(8) Uani 1 1 d . . . . .
S2 S 0.62690(3) 0.98672(4) 0.57578(4) 0.00614(8) Uani 1 1 d . . . . .
S3 S 0.42194(3) 0.65239(4) 0.57949(4) 0.00650(8) Uani 1 1 d . . . . .
O11 O 0.61843(10) 0.61129(12) 0.27541(13) 0.0132(3) Uani 1 1 d . . . . .
O12 O 0.69251(10) 0.79722(12) 0.31739(13) 0.0139(3) Uani 1 1 d . . . . .
O13 O 0.67807(10) 0.65908(12) 0.47522(12) 0.0111(3) Uani 1 1 d . . . . .
O14 O 0.53353(9) 0.75083(11) 0.38327(12) 0.0093(2) Uani 1 1 d . . . . .
O21 O 0.68530(10) 0.98015(12) 0.68547(13) 0.0130(3) Uani 1 1 d . . . . .
O22 O 0.67560(10) 1.01881(12) 0.47151(13) 0.0139(3) Uani 1 1 d . . . . .
O23 O 0.58034(10) 0.86820(11) 0.55876(12) 0.0107(3) Uani 1 1 d . . . . .
O24 O 0.45805(9) 0.93196(11) 0.40466(12) 0.0080(2) Uani 1 1 d . . . . .
O31 O 0.51888(10) 0.61873(14) 0.62233(14) 0.0179(3) Uani 1 1 d . . . . .
O32 O 0.38654(13) 0.58525(14) 0.47799(14) 0.0225(3) Uani 1 1 d . . . . .
O33 O 0.35265(10) 0.65378(13) 0.67128(13) 0.0149(3) Uani 1 1 d . . . . .
O34 O 0.42461(10) 0.77906(11) 0.53887(13) 0.0122(3) Uani 1 1 d . . . . .
B1 B 0.49995(14) 0.83078(17) 0.47162(18) 0.0067(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
Pr01 O32 2.3461(15) . ?
Pr01 O33 2.3808(14) 6_565 ?
Pr01 O13 2.4118(13) 5_666 ?
Pr01 O12 2.4332(14) 3_445 ?
Pr01 O31 2.4592(14) 5_666 ?
Pr01 O11 2.4915(13) 2_655 ?
Pr01 O21 2.5326(14) 8_465 ?
Pr01 O22 2.5614(13) 3_445 ?
S1 O11 1.4462(14) . ?
S1 O12 1.4510(14) . ?
S1 O13 1.4516(14) . ?
S1 O14 1.5419(13) . ?
S2 O21 1.4311(15) . ?
S2 O22 1.4360(14) . ?
S2 O23 1.5154(13) . ?
S2 O24 1.5224(13) 5_676 ?
S3 O31 1.4386(15) . ?
S3 O32 1.4394(16) . ?
S3 O33 1.4480(14) . ?
S3 O34 1.5317(13) . ?
O11 Pr01 2.4914(13) 2_655 ?
O12 Pr01 2.4332(14) 3 ?
O13 Pr01 2.4118(13) 5_666 ?
O14 B1 1.453(2) . ?
O21 Pr01 2.5325(14) 8_566 ?
O22 Pr01 2.5615(13) 3 ?
O23 B1 1.493(2) . ?
O24 B1 1.485(2) . ?
O24 S2 1.5224(13) 5_676 ?
O31 Pr01 2.4592(14) 5_666 ?
O33 Pr01 2.3809(14) 6_566 ?
O34 B1 1.448(2) . ?

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 Pr01 O33 138.54(5) . 6_565 ?
O32 Pr01 O13 78.47(5) . 5_666 ?
O33 Pr01 O13 114.51(5) 6_565 5_666 ?
O32 Pr01 O12 144.96(5) . 3_445 ?
O33 Pr01 O12 73.56(5) 6_565 3_445 ?
O13 Pr01 O12 73.15(5) 5_666 3_445 ?
O32 Pr01 O31 75.58(6) . 5_666 ?
O33 Pr01 O31 72.28(5) 6_565 5_666 ?
O13 Pr01 O31 71.95(5) 5_666 5_666 ?
O12 Pr01 O31 113.43(5) 3_445 5_666 ?
O32 Pr01 O11 72.61(5) . 2_655 ?
O33 Pr01 O11 80.07(5) 6_565 2_655 ?
O13 Pr01 O11 147.62(5) 5_666 2_655 ?
O12 Pr01 O11 138.97(5) 3_445 2_655 ?
O31 Pr01 O11 86.81(5) 5_666 2_655 ?
O32 Pr01 O21 120.16(5) . 8_465 ?
O33 Pr01 O21 76.89(5) 6_565 8_465 ?
O13 Pr01 O21 139.12(5) 5_666 8_465 ?
O12 Pr01 O21 73.28(5) 3_445 8_465 ?
O31 Pr01 O21 144.36(5) 5_666 8_465 ?
O11 Pr01 O21 70.46(5) 2_655 8_465 ?
O32 Pr01 O22 74.90(5) . 3_445 ?
O33 Pr01 O22 145.95(5) 6_565 3_445 ?
O13 Pr01 O22 71.43(5) 5_666 3_445 ?
O12 Pr01 O22 76.86(5) 3_445 3_445 ?
O31 Pr01 O22 136.53(5) 5_666 3_445 ?
O11 Pr01 O22 113.46(5) 2_655 3_445 ?
O21 Pr01 O22 78.80(5) 8_465 3_445 ?
O11 S1 O12 112.32(9) . . ?
O11 S1 O13 112.49(8) . . ?
O12 S1 O13 111.86(8) . . ?
O11 S1 O14 104.69(8) . . ?
O12 S1 O14 107.06(8) . . ?
O13 S1 O14 107.90(8) . . ?
O21 S2 O22 117.13(9) . . ?
O21 S2 O23 105.65(8) . . ?
O22 S2 O23 110.06(8) . . ?
O21 S2 O24 107.41(8) . 5_676 ?
O22 S2 O24 111.07(8) . 5_676 ?
O23 S2 O24 104.68(8) . 5_676 ?
O31 S3 O32 112.29(10) . . ?
O31 S3 O33 113.44(9) . . ?
O32 S3 O33 111.69(10) . . ?
O31 S3 O34 108.56(9) . . ?
O32 S3 O34 106.78(9) . . ?
O33 S3 O34 103.41(8) . . ?
S1 O11 Pr01 147.81(8) . 2_655 ?
S1 O12 Pr01 152.20(9) . 3 ?
S1 O13 Pr01 157.37(9) . 5_666 ?
B1 O14 S1 131.70(12) . . ?
S2 O21 Pr01 155.74(9) . 8_566 ?
S2 O22 Pr01 141.31(8) . 3 ?
B1 O23 S2 129.17(12) . . ?
B1 O24 S2 133.27(12) . 5_676 ?
S3 O31 Pr01 169.16(10) . 5_666 ?
S3 O32 Pr01 167.70(11) . . ?
S3 O33 Pr01 140.38(9) . 6_566 ?
B1 O34 S3 125.49(12) . . ?
O34 B1 O14 111.39(15) . . ?
O34 B1 O24 108.87(14) . . ?
O14 B1 O24 106.25(14) . . ?
O34 B1 O23 107.27(15) . . ?
O14 B1 O23 112.39(15) . . ?
O24 B1 O23 110.66(14) . . ?

_refine_diff_density_max         0.582
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.127



