
data_mo_MH362_1_0m

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'beta-Copper(II) Borosulfate'
_chemical_name_common            beta-Cupperborosulfate
_chemical_melting_point          ?
_chemical_formula_moiety         'B2 Cu O16 S4'
_chemical_formula_sum            'B2 Cu O16 S4'
_chemical_formula_weight         469.40

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.712(3)
_cell_length_b                   8.149(3)
_cell_length_c                   9.092(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.220(11)
_cell_angle_gamma                90
_cell_volume                     532.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    3829
_cell_measurement_theta_min      2.979
_cell_measurement_theta_max      42.499

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.927
_exptl_crystal_F_000             462
_exptl_transmission_factor_min   0.6364
_exptl_transmission_factor_max   0.7503
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.944
_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      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'D8 Venture Bruker'
_diffrn_measurement_method       'generic phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31258
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.979
_diffrn_reflns_theta_max         42.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3829
_reflns_number_gt                3531
_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)+(0.0268P)²+0.1674P] 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         3829
_refine_ls_number_parameters     106
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0535
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_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
Cu1 Cu 0.0000 0.0000 0.0000 0.00933(3) Uani 1 2 d S . P . .
S1 S -0.70341(2) 0.07666(2) 0.35248(2) 0.00709(3) Uani 1 1 d . . . . .
S2 S -0.28560(2) -0.15743(2) 0.14444(2) 0.00769(3) Uani 1 1 d . . . . .
O11 O -0.55574(8) -0.00837(6) 0.30328(7) 0.00964(7) Uani 1 1 d . . . . .
O12 O -0.87397(8) 0.07810(8) 0.21722(6) 0.01422(9) Uani 1 1 d . . . . .
O13 O -0.64004(8) 0.23123(7) 0.42539(7) 0.01207(8) Uani 1 1 d . . . . .
O14 O -0.26687(8) 0.04582(7) 0.53142(6) 0.01043(8) Uani 1 1 d . . . . .
O21 O -0.25352(8) -0.07600(8) 0.30280(7) 0.01397(9) Uani 1 1 d . . . . .
O22 O -0.46910(8) -0.21490(8) 0.06918(8) 0.01697(10) Uani 1 1 d . . . . .
O23 O -0.35696(8) 0.20538(7) 0.29376(7) 0.01285(9) Uani 1 1 d . . . . .
O24 O -0.21969(9) -0.04854(9) 0.04967(8) 0.01643(10) Uani 1 1 d . . . . .
B1 B -0.35882(10) 0.04137(9) 0.35692(8) 0.00835(10) 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
Cu1 O24 1.9455(9) . ?
Cu1 O24 1.9455(9) 3 ?
Cu1 O12 1.9649(8) 1_655 ?
Cu1 O12 1.9649(8) 3_455 ?
Cu1 O13 2.4277(10) 2_445 ?
Cu1 O13 2.4277(10) 4_665 ?
S1 O13 1.4250(7) . ?
S1 O12 1.4393(7) . ?
S1 O14 1.5292(7) 3_456 ?
S1 O11 1.5317(7) . ?
S2 O22 1.4105(8) . ?
S2 O24 1.4509(7) . ?
S2 O21 1.5221(7) . ?
S2 O23 1.5255(7) 2_445 ?
O11 B1 1.4739(11) . ?
O12 Cu1 1.9649(8) 1_455 ?
O13 Cu1 2.4277(10) 2_455 ?
O14 B1 1.4855(10) . ?
O14 S1 1.5291(7) 3_456 ?
O21 B1 1.4512(9) . ?
O23 B1 1.4568(10) . ?
O23 S2 1.5255(7) 2_455 ?

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 Cu1 O24 180.0 . 3 ?
O24 Cu1 O12 89.32(3) . 1_655 ?
O24 Cu1 O12 90.68(4) 3 1_655 ?
O24 Cu1 O12 90.68(3) . 3_455 ?
O24 Cu1 O12 89.32(4) 3 3_455 ?
O12 Cu1 O12 180.000(19) 1_655 3_455 ?
O24 Cu1 O13 95.07(3) . 2_445 ?
O24 Cu1 O13 84.93(3) 3 2_445 ?
O12 Cu1 O13 90.18(3) 1_655 2_445 ?
O12 Cu1 O13 89.82(3) 3_455 2_445 ?
O24 Cu1 O13 84.93(3) . 4_665 ?
O24 Cu1 O13 95.07(3) 3 4_665 ?
O12 Cu1 O13 89.82(3) 1_655 4_665 ?
O12 Cu1 O13 90.18(3) 3_455 4_665 ?
O13 Cu1 O13 180.00(3) 2_445 4_665 ?
O13 S1 O12 116.34(4) . . ?
O13 S1 O14 111.58(4) . 3_456 ?
O12 S1 O14 106.03(4) . 3_456 ?
O13 S1 O11 111.70(4) . . ?
O12 S1 O11 107.48(4) . . ?
O14 S1 O11 102.67(4) 3_456 . ?
O22 S2 O24 114.88(4) . . ?
O22 S2 O21 113.25(4) . . ?
O24 S2 O21 108.85(5) . . ?
O22 S2 O23 113.46(4) . 2_445 ?
O24 S2 O23 107.84(4) . 2_445 ?
O21 S2 O23 97.03(4) . 2_445 ?
B1 O11 S1 124.40(5) . . ?
S1 O12 Cu1 145.36(4) . 1_455 ?
S1 O13 Cu1 166.05(4) . 2_455 ?
B1 O14 S1 126.05(5) . 3_456 ?
B1 O21 S2 133.54(5) . . ?
B1 O23 S2 129.48(5) . 2_455 ?
S2 O24 Cu1 141.62(4) . . ?
O21 B1 O23 112.61(6) . . ?
O21 B1 O11 110.03(6) . . ?
O23 B1 O11 106.13(6) . . ?
O21 B1 O14 105.59(6) . . ?
O23 B1 O14 109.25(6) . . ?
O11 B1 O14 113.36(6) . . ?

_refine_diff_density_max         0.643
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.102



