
data_mo_PN82_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 Ho2 O24 S6'
_chemical_formula_weight         927.84

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'
Ho Ho -0.2175 4.6783 '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'

_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                   13.5053(14)
_cell_length_b                   11.4095(11)
_cell_length_c                   10.9210(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.453(3)
_cell_angle_gamma                90
_cell_volume                     1679.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    5956
_cell_measurement_theta_min      2.339
_cell_measurement_theta_max      45.656

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.669
_exptl_crystal_F_000             1728
_exptl_transmission_factor_min   0.6038
_exptl_transmission_factor_max   0.7490
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    10.236
_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      200(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            19064
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_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         2.339
_diffrn_reflns_theta_max         29.994
_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             2456
_reflns_number_gt                2325
_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)+(0.0133P)²+6.9233P] 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       0.00077(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2456
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0124
_refine_ls_wR_factor_ref         0.0293
_refine_ls_wR_factor_gt          0.0287
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_restrained_S_all      0.952
_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
Ho01 Ho 0.68815(2) 0.54878(2) 0.65444(2) 0.00436(4) Uani 1 1 d . . . . .
S002 S 0.36074(3) 0.29903(4) 0.63982(4) 0.00441(8) Uani 1 1 d . . . . .
S003 S 0.37128(4) 0.01267(4) 0.42209(4) 0.00490(9) Uani 1 1 d . . . . .
S004 S 0.57794(3) 0.35226(4) 0.41873(4) 0.00501(8) Uani 1 1 d . . . . .
O005 O 0.47862(11) 0.38711(14) 0.37847(15) 0.0134(3) Uani 1 1 d . . . . .
O006 O 0.46533(11) 0.25224(12) 0.61855(13) 0.0069(3) Uani 1 1 d . . . . .
O007 O 0.54184(11) 0.06911(12) 0.59722(13) 0.0063(3) Uani 1 1 d . . . . .
O008 O 0.30368(11) 0.20154(13) 0.68448(14) 0.0095(3) Uani 1 1 d . . . . .
O009 O 0.37709(11) 0.39100(13) 0.73018(14) 0.0090(3) Uani 1 1 d . . . . .
O00A O 0.31217(11) 0.01774(13) 0.30886(14) 0.0088(3) Uani 1 1 d . . . . .
O00B O 0.57610(11) 0.22345(12) 0.45856(14) 0.0091(3) Uani 1 1 d . . . . .
O00C O 0.31834(11) 0.34298(12) 0.52313(13) 0.0077(3) Uani 1 1 d . . . . .
O00D O 0.32240(12) -0.01933(13) 0.53067(14) 0.0098(3) Uani 1 1 d . . . . .
O00E O 0.61674(13) 0.41873(15) 0.52308(15) 0.0160(3) Uani 1 1 d . . . . .
O00F O 0.64687(11) 0.35129(13) 0.32222(14) 0.0102(3) Uani 1 1 d . . . . .
O00G O 0.41809(11) 0.13316(12) 0.43822(13) 0.0079(3) Uani 1 1 d . . . . .
B00H B 0.49975(16) 0.17121(18) 0.5279(2) 0.0053(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
Ho01 O00E 2.2412(16) . ?
Ho01 O00F 2.2564(15) 6_566 ?
Ho01 O00C 2.2963(14) 5_666 ?
Ho01 O008 2.3491(15) 3 ?
Ho01 O005 2.3747(15) 5_666 ?
Ho01 O009 2.3955(14) 2_656 ?
Ho01 O00A 2.4260(15) 8_556 ?
Ho01 O00D 2.4522(15) 3 ?
S002 O009 1.4483(14) . ?
S002 O00C 1.4545(14) . ?
S002 O008 1.4540(15) . ?
S002 O006 1.5406(15) . ?
S003 O00A 1.4321(15) . ?
S003 O00D 1.4386(16) . ?
S003 O00G 1.5189(14) . ?
S003 O007 1.5237(15) 5_656 ?
S004 O00E 1.4410(16) . ?
S004 O005 1.4422(16) . ?
S004 O00F 1.4477(15) . ?
S004 O00B 1.5333(14) . ?
O005 Ho01 2.3747(15) 5_666 ?
O006 B00H 1.452(3) . ?
O007 B00H 1.484(2) . ?
O007 S003 1.5237(15) 5_656 ?
O008 Ho01 2.3491(14) 3_445 ?
O009 Ho01 2.3955(14) 2_656 ?
O00A Ho01 2.4260(15) 8_455 ?
O00B B00H 1.444(3) . ?
O00C Ho01 2.2963(14) 5_666 ?
O00D Ho01 2.4521(15) 3_445 ?
O00F Ho01 2.2565(15) 6_565 ?
O00G B00H 1.494(3) . ?

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
O00E Ho01 O00F 137.43(6) . 6_566 ?
O00E Ho01 O00C 79.77(6) . 5_666 ?
O00F Ho01 O00C 114.54(6) 6_566 5_666 ?
O00E Ho01 O008 146.85(6) . 3 ?
O00F Ho01 O008 72.91(5) 6_566 3 ?
O00C Ho01 O008 73.15(5) 5_666 3 ?
O00E Ho01 O005 74.90(6) . 5_666 ?
O00F Ho01 O005 71.87(6) 6_566 5_666 ?
O00C Ho01 O005 73.68(5) 5_666 5_666 ?
O008 Ho01 O005 114.11(6) 3 5_666 ?
O00E Ho01 O009 71.42(6) . 2_656 ?
O00F Ho01 O009 80.55(5) 6_566 2_656 ?
O00C Ho01 O009 148.41(5) 5_666 2_656 ?
O008 Ho01 O009 138.27(5) 3 2_656 ?
O005 Ho01 O009 86.30(5) 5_666 2_656 ?
O00E Ho01 O00A 119.36(6) . 8_556 ?
O00F Ho01 O00A 77.73(5) 6_566 8_556 ?
O00C Ho01 O00A 138.16(5) 5_666 8_556 ?
O008 Ho01 O00A 73.15(5) 3 8_556 ?
O005 Ho01 O00A 144.13(5) 5_666 8_556 ?
O009 Ho01 O00A 70.10(5) 2_656 8_556 ?
O00E Ho01 O00D 75.01(6) . 3 ?
O00F Ho01 O00D 146.59(5) 6_566 3 ?
O00C Ho01 O00D 72.35(5) 5_666 3 ?
O008 Ho01 O00D 78.77(5) 3 3 ?
O005 Ho01 O00D 137.75(5) 5_666 3 ?
O009 Ho01 O00D 111.06(5) 2_656 3 ?
O00A Ho01 O00D 77.39(5) 8_556 3 ?
O009 S002 O00C 112.52(9) . . ?
O009 S002 O008 112.82(9) . . ?
O00C S002 O008 111.65(9) . . ?
O009 S002 O006 104.50(8) . . ?
O00C S002 O006 107.67(9) . . ?
O008 S002 O006 107.14(9) . . ?
O00A S003 O00D 117.54(9) . . ?
O00A S003 O00G 105.66(9) . . ?
O00D S003 O00G 110.03(9) . . ?
O00A S003 O007 107.40(9) . 5_656 ?
O00D S003 O007 110.74(8) . 5_656 ?
O00G S003 O007 104.58(8) . 5_656 ?
O00E S004 O005 112.54(10) . . ?
O00E S004 O00F 111.14(10) . . ?
O005 S004 O00F 114.03(9) . . ?
O00E S004 O00B 106.94(9) . . ?
O005 S004 O00B 108.66(9) . . ?
O00F S004 O00B 102.79(9) . . ?
S004 O005 Ho01 170.87(11) . 5_666 ?
B00H O006 S002 131.13(13) . . ?
B00H O007 S003 133.20(13) . 5_656 ?
S002 O008 Ho01 151.85(9) . 3_445 ?
S002 O009 Ho01 149.00(9) . 2_656 ?
S003 O00A Ho01 155.96(10) . 8_455 ?
B00H O00B S004 124.65(13) . . ?
S002 O00C Ho01 156.68(9) . 5_666 ?
S003 O00D Ho01 139.92(9) . 3_445 ?
S004 O00E Ho01 167.58(11) . . ?
S004 O00F Ho01 142.05(9) . 6_565 ?
B00H O00G S003 128.64(13) . . ?
O00B B00H O006 111.28(16) . . ?
O00B B00H O007 109.14(16) . . ?
O006 B00H O007 106.28(16) . . ?
O00B B00H O00G 107.37(16) . . ?
O006 B00H O00G 112.21(16) . . ?
O007 B00H O00G 110.56(15) . . ?

_refine_diff_density_max         0.678
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.110



