
data_mo_pn22_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 Eu2 O24 S6'
_chemical_formula_weight         901.90

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'
Eu Eu -0.1578 3.6682 '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'

loop_
_symmetry_equiv_pos_as_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                   13.602(6)
_cell_length_b                   11.470(5)
_cell_length_c                   11.050(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.465(9)
_cell_angle_gamma                90.00
_cell_volume                     1720.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    1541
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    8.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5053
_exptl_absorpt_correction_T_max  0.7459
_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_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6047
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1968
_reflns_number_gt                1541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0334P)²+6.7381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1968
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.18779(3) 0.95165(3) 0.15554(3) 0.00581(11) Uani 1 1 d . . .
S1 S 0.13794(14) 1.20181(16) 0.36121(16) 0.0063(4) Uani 1 1 d . . .
S2 S 0.12790(14) 0.51284(16) 0.07698(16) 0.0065(4) Uani 1 1 d . . .
S3 S -0.07760(14) 0.85044(16) 0.08057(16) 0.0071(4) Uani 1 1 d . . .
O11 O 0.1798(4) 1.1576(4) 0.4756(4) 0.0111(8) Uani 1 1 d . . .
O12 O 0.1211(4) 1.1105(4) 0.2720(5) 0.0111(8) Uani 1 1 d . . .
O13 O 0.1959(4) 1.2983(5) 0.3169(5) 0.0124(12) Uani 1 1 d . . .
O14 O 0.0339(4) 1.2495(5) 0.3825(4) 0.0085(11) Uani 1 1 d . . .
O21 O 0.1765(4) 0.4812(4) -0.0292(5) 0.0125(12) Uani 1 1 d . . .
O22 O 0.1865(4) 0.5179(4) 0.1887(5) 0.0109(12) Uani 1 1 d . . .
O23 O 0.0813(4) 0.6321(4) 0.0607(5) 0.0125(12) Uani 1 1 d . . .
O24 O 0.0419(4) 0.4311(4) 0.0961(5) 0.0094(12) Uani 1 1 d . . .
O31 O 0.0202(4) 0.8850(5) 0.1210(5) 0.0182(13) Uani 1 1 d . . .
O32 O 0.1154(5) 1.0840(5) 0.0233(5) 0.0212(14) Uani 1 1 d . . .
O33 O -0.1471(4) 0.8491(5) 0.1743(5) 0.0132(12) Uani 1 1 d . . .
O34 O -0.0748(4) 0.7228(4) 0.0404(5) 0.0120(12) Uani 1 1 d . . .
B1 B 0.0006(7) 0.6700(7) -0.0271(7) 0.0081(18) 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
Eu1 O32 2.288(5) . ?
Eu1 O33 2.314(5) 2 ?
Eu1 O11 2.348(5) 6_575 ?
Eu1 O13 2.373(5) 4_545 ?
Eu1 O31 2.413(6) . ?
Eu1 O12 2.438(5) . ?
Eu1 O22 2.472(5) 4 ?
Eu1 O21 2.503(5) 7_565 ?
S1 O12 1.447(5) . ?
S1 O11 1.446(5) . ?
S1 O13 1.460(5) . ?
S1 O14 1.549(6) . ?
S2 O21 1.427(6) . ?
S2 O22 1.429(5) . ?
S2 O23 1.514(5) . ?
S2 O24 1.524(5) . ?
S3 O31 1.434(6) . ?
S3 O32 1.441(6) 5_575 ?
S3 O33 1.444(5) . ?
S3 O34 1.531(5) . ?
O11 Eu1 2.348(5) 6_576 ?
O13 Eu1 2.373(5) 4 ?
O14 B1 1.453(10) 6_576 ?
O21 Eu1 2.503(5) 7_565 ?
O22 Eu1 2.472(5) 4_545 ?
O23 B1 1.485(10) . ?
O24 B1 1.485(9) 5_565 ?
O32 S3 1.441(6) 5_575 ?
O33 Eu1 2.314(5) 2 ?
O34 B1 1.437(10) . ?
B1 O14 1.453(10) 6_575 ?
B1 O24 1.485(9) 5_565 ?

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 Eu1 O33 137.9(2) . 2 ?
O32 Eu1 O11 79.4(2) . 6_575 ?
O33 Eu1 O11 114.57(19) 2 6_575 ?
O32 Eu1 O13 146.25(19) . 4_545 ?
O33 Eu1 O13 73.10(19) 2 4_545 ?
O11 Eu1 O13 73.11(18) 6_575 4_545 ?
O32 Eu1 O31 75.1(2) . . ?
O33 Eu1 O31 72.36(19) 2 . ?
O11 Eu1 O31 72.65(18) 6_575 . ?
O13 Eu1 O31 113.7(2) 4_545 . ?
O32 Eu1 O12 71.45(19) . . ?
O33 Eu1 O12 80.56(18) 2 . ?
O11 Eu1 O12 147.85(18) 6_575 . ?
O13 Eu1 O12 138.85(17) 4_545 . ?
O31 Eu1 O12 86.68(19) . . ?
O32 Eu1 O22 119.6(2) . 4 ?
O33 Eu1 O22 77.29(19) 2 4 ?
O11 Eu1 O22 138.49(18) 6_575 4 ?
O13 Eu1 O22 73.19(17) 4_545 4 ?
O31 Eu1 O22 144.57(18) . 4 ?
O12 Eu1 O22 70.52(18) . 4 ?
O32 Eu1 O21 75.1(2) . 7_565 ?
O33 Eu1 O21 146.19(18) 2 7_565 ?
O11 Eu1 O21 71.93(17) 6_575 7_565 ?
O13 Eu1 O21 77.94(18) 4_545 7_565 ?
O31 Eu1 O21 136.99(18) . 7_565 ?
O12 Eu1 O21 112.04(17) . 7_565 ?
O22 Eu1 O21 77.94(18) 4 7_565 ?
O12 S1 O11 112.3(3) . . ?
O12 S1 O13 112.7(3) . . ?
O11 S1 O13 111.5(3) . . ?
O12 S1 O14 104.5(3) . . ?
O11 S1 O14 107.8(3) . . ?
O13 S1 O14 107.5(3) . . ?
O21 S2 O22 117.3(3) . . ?
O21 S2 O23 110.1(3) . . ?
O22 S2 O23 105.9(3) . . ?
O21 S2 O24 110.8(3) . . ?
O22 S2 O24 107.3(3) . . ?
O23 S2 O24 104.6(3) . . ?
O31 S3 O32 112.6(4) . 5_575 ?
O31 S3 O33 114.5(3) . . ?
O32 S3 O33 111.1(4) 5_575 . ?
O31 S3 O34 108.4(3) . . ?
O32 S3 O34 106.4(3) 5_575 . ?
O33 S3 O34 103.1(3) . . ?
S1 O11 Eu1 157.4(4) . 6_576 ?
S1 O12 Eu1 148.4(3) . . ?
S1 O13 Eu1 152.6(3) . 4 ?
B1 O14 S1 130.9(5) 6_576 . ?
S2 O21 Eu1 140.7(3) . 7_565 ?
S2 O22 Eu1 156.2(3) . 4_545 ?
B1 O23 S2 129.1(5) . . ?
B1 O24 S2 133.4(5) 5_565 . ?
S3 O31 Eu1 170.8(4) . . ?
S3 O32 Eu1 167.0(4) 5_575 . ?
S3 O33 Eu1 141.0(3) . 2 ?
B1 O34 S3 125.7(5) . . ?
O34 B1 O14 110.5(6) . 6_575 ?
O34 B1 O24 109.1(7) . 5_565 ?
O14 B1 O24 105.7(6) 6_575 5_565 ?
O34 B1 O23 107.9(6) . . ?
O14 B1 O23 112.7(7) 6_575 . ?
O24 B1 O23 110.8(6) 5_565 . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.642
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.287
