
data_mo_MH065_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 Ce2 O24 S6'
_chemical_formula_weight         878.22

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'
Ce Ce -0.2486 2.6331 '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                   13.7400(5)
_cell_length_b                   11.5371(4)
_cell_length_c                   11.3057(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.6606(12)
_cell_angle_gamma                90
_cell_volume                     1788.52(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2039
_cell_measurement_theta_min      2.307
_cell_measurement_theta_max      27.444

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.262
_exptl_crystal_F_000             1656
_exptl_transmission_factor_min   0.6730
_exptl_transmission_factor_max   0.7455
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    5.856
_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            16577
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0630
_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         2.307
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2039
_reflns_number_gt                1745
_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)+(0.0178P)²+2.7211P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2039
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0431
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_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
Ce1 Ce 0.18748(2) 0.45210(2) 0.15748(2) 0.00719(6) Uani 1 1 d . . . . .
S1 S 0.13505(6) 0.70251(7) 0.36287(7) 0.00689(17) Uani 1 1 d . . . . .
O11 O 0.03312(17) 0.2488(2) -0.1159(2) 0.0109(5) Uani 1 1 d . . . . .
O12 O 0.17733(18) 0.6595(2) 0.4752(2) 0.0108(5) Uani 1 1 d . . . . .
O13 O 0.11740(19) 0.6117(2) 0.2766(2) 0.0142(6) Uani 1 1 d . . . . .
O14 O 0.19196(19) 0.7972(2) 0.3180(2) 0.0155(6) Uani 1 1 d . . . . .
S2 S -0.07816(6) 0.34703(7) 0.07929(7) 0.00835(18) Uani 1 1 d . . . . .
O21 O -0.07504(18) 0.2205(2) 0.0386(2) 0.0130(5) Uani 1 1 d . . . . .
O22 O 0.01844(19) 0.3809(2) 0.1221(2) 0.0187(6) Uani 1 1 d . . . . .
O23 O -0.14730(18) 0.3456(2) 0.1703(2) 0.0162(6) Uani 1 1 d . . . . .
O24 O -0.1133(2) 0.4142(2) -0.0210(2) 0.0237(7) Uani 1 1 d . . . . .
S3 S 0.37337(6) 0.51337(7) 0.42462(7) 0.00775(17) Uani 1 1 d . . . . .
O31 O 0.42017(18) 0.6317(2) 0.4414(2) 0.0114(5) Uani 1 1 d . . . . .
O32 O 0.45789(17) 0.4318(2) 0.4052(2) 0.0089(5) Uani 1 1 d . . . . .
O33 O 0.32514(19) 0.4815(2) 0.5283(2) 0.0148(6) Uani 1 1 d . . . . .
O34 O 0.31473(19) 0.5201(2) 0.3156(2) 0.0155(6) Uani 1 1 d . . . . .
B1 B -0.0003(3) 0.1690(3) -0.0279(3) 0.0086(8) 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
Ce1 O24 2.366(3) 5_565 ?
Ce1 O23 2.397(2) 2 ?
Ce1 O12 2.426(2) 6_565 ?
Ce1 O14 2.440(3) 4_545 ?
Ce1 O22 2.472(3) . ?
Ce1 O13 2.510(2) . ?
Ce1 O34 2.543(3) . ?
Ce1 O33 2.579(2) 6_565 ?
S1 O13 1.441(2) . ?
S1 O12 1.450(2) . ?
S1 O14 1.454(3) . ?
S1 O11 1.542(2) 6_566 ?
O11 B1 1.452(4) . ?
O11 S1 1.542(2) 6_565 ?
O12 Ce1 2.426(2) 6_566 ?
O14 Ce1 2.440(3) 4 ?
S2 O24 1.431(3) . ?
S2 O22 1.437(3) . ?
S2 O23 1.444(3) . ?
S2 O21 1.532(2) . ?
O21 B1 1.439(5) . ?
O23 Ce1 2.397(2) 2 ?
O24 Ce1 2.367(3) 5_565 ?
S3 O33 1.431(3) . ?
S3 O34 1.431(3) . ?
S3 O31 1.516(2) . ?
S3 O32 1.522(2) . ?
O31 B1 1.488(5) 4 ?
O32 B1 1.484(4) 8_556 ?
O33 Ce1 2.579(2) 6_566 ?
B1 O32 1.484(4) 8_455 ?
B1 O31 1.488(4) 4_545 ?

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
O24 Ce1 O23 138.77(9) 5_565 2 ?
O24 Ce1 O12 78.05(9) 5_565 6_565 ?
O23 Ce1 O12 114.49(9) 2 6_565 ?
O24 Ce1 O14 144.35(9) 5_565 4_545 ?
O23 Ce1 O14 73.87(8) 2 4_545 ?
O12 Ce1 O14 73.14(8) 6_565 4_545 ?
O24 Ce1 O22 75.53(10) 5_565 . ?
O23 Ce1 O22 72.44(9) 2 . ?
O12 Ce1 O22 71.56(8) 6_565 . ?
O14 Ce1 O22 113.51(9) 4_545 . ?
O24 Ce1 O13 72.99(9) 5_565 . ?
O23 Ce1 O13 79.85(9) 2 . ?
O12 Ce1 O13 147.35(8) 6_565 . ?
O14 Ce1 O13 139.22(8) 4_545 . ?
O22 Ce1 O13 86.68(9) . . ?
O24 Ce1 O34 120.36(9) 5_565 . ?
O23 Ce1 O34 76.74(9) 2 . ?
O12 Ce1 O34 139.49(8) 6_565 . ?
O14 Ce1 O34 73.42(8) 4_545 . ?
O22 Ce1 O34 144.38(8) . . ?
O13 Ce1 O34 70.52(8) . . ?
O24 Ce1 O33 74.81(9) 5_565 6_565 ?
O23 Ce1 O33 145.88(9) 2 6_565 ?
O12 Ce1 O33 71.40(8) 6_565 6_565 ?
O14 Ce1 O33 76.40(8) 4_545 6_565 ?
O22 Ce1 O33 136.27(8) . 6_565 ?
O13 Ce1 O33 113.98(8) . 6_565 ?
O34 Ce1 O33 79.06(8) . 6_565 ?
O13 S1 O12 112.58(15) . . ?
O13 S1 O14 112.43(15) . . ?
O12 S1 O14 111.63(15) . . ?
O13 S1 O11 104.74(14) . 6_566 ?
O12 S1 O11 107.81(14) . 6_566 ?
O14 S1 O11 107.15(15) . 6_566 ?
B1 O11 S1 131.9(2) . 6_565 ?
S1 O12 Ce1 157.48(15) . 6_566 ?
S1 O13 Ce1 147.44(16) . . ?
S1 O14 Ce1 152.51(16) . 4 ?
O24 S2 O22 112.15(18) . . ?
O24 S2 O23 111.52(17) . . ?
O22 S2 O23 113.50(16) . . ?
O24 S2 O21 106.97(16) . . ?
O22 S2 O21 108.48(16) . . ?
O23 S2 O21 103.61(15) . . ?
B1 O21 S2 125.8(2) . . ?
S2 O22 Ce1 169.28(17) . . ?
S2 O23 Ce1 140.25(16) . 2 ?
S2 O24 Ce1 168.17(19) . 5_565 ?
O33 S3 O34 117.04(16) . . ?
O33 S3 O31 110.10(15) . . ?
O34 S3 O31 105.69(15) . . ?
O33 S3 O32 110.92(14) . . ?
O34 S3 O32 107.56(15) . . ?
O31 S3 O32 104.70(14) . . ?
B1 O31 S3 129.3(2) 4 . ?
B1 O32 S3 133.3(2) 8_556 . ?
S3 O33 Ce1 141.47(15) . 6_566 ?
S3 O34 Ce1 155.91(16) . . ?
O21 B1 O11 111.3(3) . . ?
O21 B1 O32 108.9(3) . 8_455 ?
O11 B1 O32 106.0(3) . 8_455 ?
O21 B1 O31 107.4(3) . 4_545 ?
O11 B1 O31 112.4(3) . 4_545 ?
O32 B1 O31 110.8(3) 8_455 4_545 ?

_refine_diff_density_max         0.623
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.142



