# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p131206d1
_database_code_depnum_ccdc_archive 'CCDC 1016428'
_audit_update_record             
;
2014-07-28 deposited with the CCDC.
2015-02-20 downloaded from the CCDC.
;
_audit_creation_date             2014-07-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'H2 Mn1.5 Na O8 S1.5'
_chemical_formula_sum            'H2 Mn1.50 Na O8 S1.50'
_chemical_formula_weight         283.51
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1MN1
_chemical_oxdiff_usercomment     HHC-MNSO4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 '-x, y, z'
4 'x, -y, z+1/2'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z+1/2'
7 '-x+1/2, y+1/2, z'
8 'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   18.0718(6)
_cell_length_b                   7.8465(3)
_cell_length_c                   9.9048(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1404.51(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1254
_cell_measurement_temperature    128.55(10)
_cell_measurement_theta_max      28.6050
_cell_measurement_theta_min      3.5040
_exptl_absorpt_coefficient_mu    3.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1784
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.50
_diffrn_ambient_temperature      128.55(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -17.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   19.0000  -90.0000 104

#__ type_ start__ end____ width___ exp.time_
  2 omega  -43.00   -4.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   77.0000 -150.0000 39
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0358123000
_diffrn_orient_matrix_UB_12      0.0280155000
_diffrn_orient_matrix_UB_13      -0.0191061000
_diffrn_orient_matrix_UB_21      -0.0134620000
_diffrn_orient_matrix_UB_22      0.0845524000
_diffrn_orient_matrix_UB_23      -0.0063481000
_diffrn_orient_matrix_UB_31      0.0087110000
_diffrn_orient_matrix_UB_32      0.0157355000
_diffrn_orient_matrix_UB_33      0.0686975000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                1150
_reflns_number_total             1193
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1193
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0400P)²+3.0873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0858
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups
2. Restrained distances
 O10-H10A = O10-H10B
 0.85 with sigma of 0.02
 H10A-H10B
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.01
Uanis(Mn1) = Uanis(O5) = Uanis(Mn2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.08913(5) 0.47307(11) 0.48606(9) 0.0126(2) Uani 1 d . . 1 . . .
Mn2 Mn 0.0000 0.19545(18) 0.20627(12) 0.0126(2) Uani 1 d . . 2 S T P
S1 S 0.17836(8) 0.3039(2) 0.21609(15) 0.0124(3) Uani 1 d . . 1 . . .
S2 S 0.0000 0.8162(3) 0.3791(2) 0.0122(4) Uani 1 d . . 2 S T P
Na1 Na 0.30988(14) 0.4613(3) 0.4408(3) 0.0213(6) Uani 1 d . . 1 . . .
O2 O 0.1793(2) 0.3925(6) 0.0840(4) 0.0182(10) Uani 1 d . . 1 . . .
O1 O 0.0000 0.9214(9) 0.5009(7) 0.0288(16) Uani 1 d . . 2 S T P
O3 O 0.0000 0.9241(8) 0.2555(6) 0.0157(13) Uani 1 d . . 2 S T P
O4 O 0.1205(2) 0.1685(6) 0.2135(5) 0.0190(10) Uani 1 d . . 1 . . .
O6 O 0.1618(3) 0.4264(7) 0.3229(4) 0.0214(10) Uani 1 d . . 1 . . .
O7 O 0.2504(3) 0.2247(7) 0.2408(5) 0.0244(11) Uani 1 d . . 1 . . .
O8 O 0.0000 0.4500(8) 0.1194(6) 0.0156(14) Uani 1 d . . 2 S T P
O9 O 0.0662(3) 0.7081(7) 0.3760(5) 0.0276(12) Uani 1 d . . 1 . . .
O10 O 0.1226(3) 0.2388(7) 0.5924(4) 0.0198(10) Uani 1 d . . 1 D . .
O5 O 0.0000 0.3299(8) 0.3945(6) 0.0126(2) Uani 1 d . . 2 S TU P
H10A H 0.158(2) 0.230(10) 0.646(6) 0.03(2) Uiso 1 d . . 1 D . .
H10B H 0.089(3) 0.171(9) 0.618(7) 0.037 Uiso 1 d . . 1 DR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0124(3) 0.0138(4) 0.0115(3) -0.0003(4) 0.0000(3) 0.0014(3)
Mn2 0.0124(3) 0.0138(4) 0.0115(3) -0.0003(4) 0.0000(3) 0.0014(3)
S1 0.0121(6) 0.0130(8) 0.0121(6) 0.0007(7) -0.0003(5) 0.0013(6)
S2 0.0134(9) 0.0121(11) 0.0110(9) 0.0003(9) 0.000 0.000
Na1 0.0244(13) 0.0190(14) 0.0204(12) 0.0005(12) -0.0017(11) -0.0032(11)
O2 0.018(2) 0.023(3) 0.0128(19) 0.005(2) -0.0052(18) -0.001(2)
O1 0.049(4) 0.020(4) 0.017(3) 0.000(3) 0.000 0.000
O3 0.021(3) 0.015(3) 0.012(3) 0.001(3) 0.000 0.000
O4 0.0129(19) 0.019(3) 0.025(2) -0.001(2) -0.001(2) -0.0043(18)
O6 0.022(2) 0.022(3) 0.020(2) -0.007(2) 0.0072(19) -0.004(2)
O7 0.014(2) 0.028(3) 0.031(2) 0.003(2) -0.0044(18) 0.008(2)
O8 0.013(3) 0.013(3) 0.021(3) 0.005(3) 0.000 0.000
O9 0.026(2) 0.033(3) 0.024(2) 0.009(2) 0.007(2) 0.017(2)
O10 0.017(2) 0.022(3) 0.020(2) 0.008(2) 0.000(2) 0.000(2)
O5 0.0124(3) 0.0138(4) 0.0115(3) -0.0003(4) 0.0000(3) 0.0014(3)

_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
Mn1 Mn1 3.2215(16) 3 ?
Mn1 O2 2.170(4) 4_565 ?
Mn1 O6 2.115(4) . ?
Mn1 O8 2.168(4) 2_565 ?
Mn1 O9 2.182(5) . ?
Mn1 O10 2.203(5) . ?
Mn1 O5 2.163(4) . ?
Mn2 O1 2.231(7) 2_564 ?
Mn2 O3 2.184(6) 1_545 ?
Mn2 O4 2.188(4) . ?
Mn2 O4 2.188(4) 3 ?
Mn2 O8 2.175(6) . ?
Mn2 O5 2.142(6) . ?
S1 O2 1.482(4) . ?
S1 O4 1.492(4) . ?
S1 O6 1.460(5) . ?
S1 O7 1.462(5) . ?
S2 O1 1.462(7) . ?
S2 O3 1.488(6) . ?
S2 O9 1.467(5) 3 ?
S2 O9 1.467(5) . ?
Na1 O2 2.983(5) 4_565 ?
Na1 O6 2.932(5) . ?
Na1 O7 2.920(6) . ?
Na1 O10 2.913(6) 7 ?
O2 Mn1 2.170(4) 4_564 ?
O2 Na1 2.983(5) 4_564 ?
O1 Mn2 2.231(7) 2_565 ?
O3 Mn2 2.184(6) 1_565 ?
O8 Mn1 2.168(4) 2_564 ?
O8 Mn1 2.168(4) 4_564 ?
O10 Na1 2.913(6) 7_545 ?
O5 Mn1 2.163(4) 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
O2 Mn1 Mn1 138.67(12) 4_565 3 ?
O2 Mn1 O9 87.41(18) 4_565 . ?
O2 Mn1 O10 89.19(19) 4_565 . ?
O6 Mn1 Mn1 128.41(13) . 3 ?
O6 Mn1 O2 87.67(17) . 4_565 ?
O6 Mn1 O8 167.2(2) . 2_565 ?
O6 Mn1 O9 83.25(19) . . ?
O6 Mn1 O10 92.88(18) . . ?
O6 Mn1 O5 92.99(18) . . ?
O8 Mn1 Mn1 42.03(12) 2_565 3 ?
O8 Mn1 O2 98.65(17) 2_565 4_565 ?
O8 Mn1 O9 85.9(2) 2_565 . ?
O8 Mn1 O10 98.3(2) 2_565 . ?
O9 Mn1 Mn1 79.07(13) . 3 ?
O9 Mn1 O10 174.95(19) . . ?
O10 Mn1 Mn1 105.92(12) . 3 ?
O5 Mn1 Mn1 41.87(12) . 3 ?
O5 Mn1 O2 177.5(2) . 4_565 ?
O5 Mn1 O8 81.18(17) . 2_565 ?
O5 Mn1 O9 95.1(2) . . ?
O5 Mn1 O10 88.4(2) . . ?
O3 Mn2 O1 78.7(2) 1_545 2_564 ?
O3 Mn2 O4 84.17(13) 1_545 3 ?
O3 Mn2 O4 84.17(13) 1_545 . ?
O4 Mn2 O1 89.42(14) 3 2_564 ?
O4 Mn2 O1 89.42(14) . 2_564 ?
O4 Mn2 O4 168.3(3) 3 . ?
O8 Mn2 O1 90.9(2) . 2_564 ?
O8 Mn2 O3 169.6(2) . 1_545 ?
O8 Mn2 O4 95.84(13) . 3 ?
O8 Mn2 O4 95.84(13) . . ?
O5 Mn2 O1 174.7(3) . 2_564 ?
O5 Mn2 O3 106.6(2) . 1_545 ?
O5 Mn2 O4 91.11(14) . . ?
O5 Mn2 O4 91.11(14) . 3 ?
O5 Mn2 O8 83.8(2) . . ?
O2 S1 O4 109.1(3) . . ?
O6 S1 O2 109.4(3) . . ?
O6 S1 O4 109.8(3) . . ?
O6 S1 O7 109.9(3) . . ?
O7 S1 O2 109.7(3) . . ?
O7 S1 O4 109.0(3) . . ?
O1 S2 O3 111.0(4) . . ?
O1 S2 O9 110.1(3) . 3 ?
O1 S2 O9 110.1(3) . . ?
O9 S2 O3 108.2(2) . . ?
O9 S2 O3 108.2(2) 3 . ?
O9 S2 O9 109.3(4) 3 . ?
O6 Na1 O2 60.23(12) . 4_565 ?
O7 Na1 O2 106.00(14) . 4_565 ?
O7 Na1 O6 48.25(13) . . ?
O10 Na1 O2 78.41(13) 7 4_565 ?
O10 Na1 O6 131.12(17) 7 . ?
O10 Na1 O7 168.29(16) 7 . ?
Mn1 O2 Na1 101.23(16) 4_564 4_564 ?
S1 O2 Mn1 127.9(2) . 4_564 ?
S1 O2 Na1 127.5(2) . 4_564 ?
S2 O1 Mn2 121.4(4) . 2_565 ?
S2 O3 Mn2 137.6(4) . 1_565 ?
S1 O4 Mn2 129.0(3) . . ?
Mn1 O6 Na1 104.25(17) . . ?
S1 O6 Mn1 142.6(3) . . ?
S1 O6 Na1 99.4(2) . . ?
S1 O7 Na1 99.9(3) . . ?
Mn1 O8 Mn1 95.9(2) 2_564 4_564 ?
Mn1 O8 Mn2 119.8(2) 2_564 . ?
Mn1 O8 Mn2 119.8(2) 4_564 . ?
S2 O9 Mn1 129.3(3) . . ?
Mn1 O10 Na1 119.49(18) . 7_545 ?
Mn1 O5 Mn1 96.3(2) . 3 ?
Mn2 O5 Mn1 128.36(14) . 3 ?
Mn2 O5 Mn1 128.36(14) . . ?

