
#=======================================================================
data_I
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic
; ?
;
_chemical_name_common                    ?
_chemical_formula_moiety                 'H8 Mn5 O16 S3'
_chemical_formula_structural             ?
_chemical_formula_analytical             ?
_chemical_formula_iupac                  ?
_chemical_formula_sum                    'H8 Mn5 O16 S3'
_chemical_formula_weight                 634.9
_chemical_melting_point                  ?
_chemical_compound_source                ?
_chemical_absolute_configuration         .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting                   monoclinic
_symmetry_space_group_name_H-M           'P 1 21/m 1'
_symmetry_space_group_name_Hall          '-P 2yb'
_symmetry_Int_Tables_number              11
loop_
 _symmetry_equiv_pos_site_id
 _symmetry_equiv_pos_as_xyz
 1   x,y,z
 2   -x,y+1/2,-z
 3   -x,-y,-z
 4   x,-y+1/2,z
_cell_length_a                           7.6117(7)
_cell_length_b                           8.5326(7)
_cell_length_c                           10.9273(9)
_cell_angle_alpha                        90
_cell_angle_beta                         101.6005(13)
_cell_angle_gamma                        90
_cell_volume                             695.21(10)

loop_
 _jana_cell_twin_matrix_id
 _jana_cell_twin_volume_fraction
 _jana_cell_twin_matrix_1_1
 _jana_cell_twin_matrix_1_2
 _jana_cell_twin_matrix_1_3
 _jana_cell_twin_matrix_2_1
 _jana_cell_twin_matrix_2_2
 _jana_cell_twin_matrix_2_3
 _jana_cell_twin_matrix_3_1
 _jana_cell_twin_matrix_3_2
 _jana_cell_twin_matrix_3_3
 ? ? ? ? ? ? ? ? ? ? ?
_cell_formula_units_Z                    2

_cell_measurement_reflns_used            5936
_cell_measurement_theta_min              1.9
_cell_measurement_theta_max              27.83
_cell_measurement_temperature            293
_cell_special_details
; ?
;

_exptl_crystal_density_diffrn            3.0321
_exptl_crystal_density_meas              ?
_exptl_crystal_density_method            ?
_exptl_crystal_F_000                     618

_exptl_absorpt_coefficient_mu            4.954
_exptl_crystal_description               needle
_exptl_crystal_size_max                  0.8
_exptl_crystal_size_mid                  0.180
_exptl_crystal_size_min                  0.085
_exptl_crystal_size_rad                  ?
_exptl_crystal_colour                    pink
_exptl_absorpt_correction_type           gaussian
_exptl_absorpt_process_details
 'Jana2006  (Petricek, Dusek & Palatinus, 2000)'
_exptl_absorpt_correction_T_min          0.1805
_exptl_absorpt_correction_T_max          0.6556

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details                   ?

_diffrn_ambient_temperature              293
_diffrn_source                           ?
_diffrn_source_power                     ?
_diffrn_source_voltage                   ?
_diffrn_source_current                   ?
_diffrn_radiation_type                   'Mo K\a'
_diffrn_radiation_source                 'X-ray tube'
_diffrn_radiation_wavelength             0.71073
_diffrn_radiation_monochromator          graphite
_diffrn_measurement_device               'four-cycle diffractometer'
_diffrn_measurement_device_type          'Smart Apex'
_diffrn_detector                         ?
_diffrn_detector_area_resol_mean         ?
_diffrn_measurement_method               'Multi-scan'
_diffrn_measurement_specimen_support     ?

_diffrn_reflns_number                    5936
_diffrn_reflns_theta_min                 1.9
_diffrn_reflns_theta_max                 27.83
_diffrn_reflns_theta_full                27.71
_diffrn_measured_fraction_theta_max      0.96
_diffrn_measured_fraction_theta_full     0.98
_diffrn_reflns_av_R_equivalents          0.12
_diffrn_reflns_av_sigmaI/netI            0.0778
_diffrn_reflns_limit_h_min               -10
_diffrn_reflns_limit_h_max               9
_diffrn_reflns_limit_k_min               -10
_diffrn_reflns_limit_k_max               11
_diffrn_reflns_limit_l_min               -14
_diffrn_reflns_limit_l_max               13
_diffrn_reflns_reduction_process         ?

_diffrn_standards_number                 ?
_diffrn_standards_interval_count         ?
_diffrn_standards_interval_time          ?
_diffrn_standards_decay_%                ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
  ? ? ?

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details
; ?
;

_reflns_number_total                     1559
_reflns_number_gt                        1500
_reflns_threshold_expression             'I>3σ(I)'

_refine_ls_structure_factor_coef         Fsqd
_refine_ls_R_factor_gt                   0.0347
_refine_ls_wR_factor_gt                  0.0802
_refine_ls_R_factor_all                  0.0360
_refine_ls_wR_factor_ref                 0.0824
_refine_ls_goodness_of_fit_ref           1.15
_refine_ls_goodness_of_fit_gt            1.14
_refine_ls_restrained_S_gt               ?
_refine_ls_restrained_S_all              ?
_refine_ls_number_reflns                 1559
_refine_ls_number_parameters             138
_refine_ls_number_restraints             5
_refine_ls_number_constraints            0
_refine_ls_weighting_scheme              sigma
_refine_ls_weighting_details             'w=1/(σ²(I)+0.0009I²)'
_refine_ls_hydrogen_treatment            'refall'
_refine_ls_shift/su_max                  0.0010
_refine_ls_shift/su_mean                 0.0000
_refine_diff_density_max                 0.50
_refine_diff_density_min                 -0.36
_refine_ls_extinction_method             'none'
_refine_ls_extinction_coef               ?
_refine_ls_abs_structure_details         ?
_refine_ls_abs_structure_Flack           ?
_refine_ls_abs_structure_Rogers          ?

loop_
 _atom_type_symbol
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 H   0.0000  0.0000
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 Mn  0.3368  0.7283
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 O   0.0106  0.0060
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 S   0.1246  0.1234
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection               ?
_computing_cell_refinement               ?
_computing_data_reduction                ?
_computing_structure_solution            ?
_computing_structure_refinement          ?
_computing_molecular_graphics            ?
_computing_publication_material          ?

#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_adp_type
 _atom_site_U_iso_or_equiv
 _atom_site_symmetry_multiplicity
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
  Mn1 Mn 0.55560(6) 0.75 0.11212(4) Uani 0.01563(15) 2 1 d . . .
  Mn2 Mn 0.19383(4) 0.44908(3) 0.10437(4) Uani 0.01655(13) 4 1 d . . .
  Mn3 Mn 0.55407(5) 0.55063(3) 0.35978(3) Uani 0.01738(13) 4 1 d . . .
  S1 S 0.16879(9) 0.75 0.88712(7) Uani 0.01419(19) 2 1 d . . .
  S2 S 0.26613(9) 0.25 0.38573(7) Uani 0.01481(19) 2 1 d . . .
  S3 S 0.15163(9) 0.75 0.30391(7) Uani 0.0165(2) 2 1 d . . .
  O1 O 0.3708(3) 0.75 0.9343(2) Uani 0.0182(6) 2 1 d . . .
  O2 O 0.0994(2) 0.60803(16) 0.94841(17) Uani 0.0215(4) 4 1 d . . .
  O3 O 0.3840(2) 0.39190(17) 0.43255(16) Uani 0.0227(5) 4 1 d . . .
  O4 O 0.2504(3) 0.25 0.2445(2) Uani 0.0200(6) 2 1 d . . .
  O5 O 0.0715(4) 0.75 0.4135(3) Uani 0.0336(8) 2 1 d . . .
  O6 O 0.3521(3) 0.75 0.3394(3) Uani 0.0228(7) 2 1 d . . .
  O7 O 0.0920(3) 0.8921(3) 0.2312(2) Uani 0.0411(6) 4 1 d . . .
  O8 O 0.8144(3) 0.4351(3) 0.3818(3) Uani 0.0427(8) 4 1 d . . .
  O9 O 0.4653(2) 0.52180(17) 0.15930(16) Uani 0.0168(4) 4 1 d . . .
  O10 O 0.6877(3) 0.75 0.3069(2) Uani 0.0157(5) 2 1 d . . .
  O11 O 0.7663(3) 0.75 0.0154(2) Uani 0.0165(5) 2 1 d . . .
  H8a H 0.855(7) 0.471(5) 0.325(4) Uiso 0.054(6) 4 1 d . . .
  H8b H 0.859(6) 0.386(5) 0.441(3) Uiso 0.054(6) 4 1 d . . .
  H9 H 0.538(6) 0.444(4) 0.146(5) Uiso 0.054(6) 4 1 d . . .
  H10 H 0.800(4) 0.75 0.327(6) Uiso 0.054(6) 2 1 d . . .
  H11 H 0.851(6) 0.75 0.078(4) Uiso 0.054(6) 2 1 d . . .



#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_1
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
  Mn1 O1 . 1_554 2.157(2) ?
  Mn1 O9 . . 2.1614(16) ?
  Mn1 O9 . 4_565 2.1614(16) ?
  Mn1 O10 . . 2.164(2) ?
  Mn1 O11 . . 2.091(3) ?
  Mn1 H11 . . 2.35(5) ?
  Mn2 O2 . 1_554 2.1834(16) ?
  Mn2 O2 . 3_566 2.2440(16) ?
  Mn2 O4 . . 2.2692(15) ?
  Mn2 O7 . 4_565 2.189(3) ?
  Mn2 O9 . . 2.1253(16) ?
  Mn2 O11 . 2_645 2.2022(17) ?
  Mn3 O3 . . 2.1345(18) ?
  Mn3 O3 . 3_666 2.2764(17) ?
  Mn3 O6 . . 2.2735(16) ?
  Mn3 O8 . . 2.183(2) ?
  Mn3 O9 . . 2.1728(17) ?
  Mn3 O10 . . 2.1208(14) ?
  Mn3 H8a . . 2.49(5) ?
  Mn3 H9 . . 2.49(5) ?
  S1 O1 . . 1.520(2) ?
  S1 O2 . . 1.5286(17) ?
  S1 O2 . 4_565 1.5286(17) ?
  S2 O3 . . 1.5325(16) ?
  S2 O3 . 4_555 1.5325(16) ?
  S2 O4 . . 1.524(2) ?
  S3 O5 . . 1.449(3) ?
  S3 O6 . . 1.497(2) ?
  S3 O7 . . 1.471(2) ?
  S3 O7 . 4_565 1.471(2) ?
  O1 O2 . . 2.426(2) ?
  O1 O2 . 4_565 2.426(2) ?
  O1 H9 . 2_656 2.06(4) ?
  O1 H9 . 3_666 2.06(4) ?
  O2 O2 . 4_565 2.423(2) ?
  O3 O3 . 4_555 2.422(2) ?
  O3 O4 . . 2.426(2) ?
  O5 O6 . . 2.432(4) ?
  O5 O7 . . 2.364(4) ?
  O5 O7 . 4_565 2.364(4) ?
  O5 H8b . 2_656 1.95(4) ?
  O5 H8b . 3_666 1.95(4) ?
  O5 H10 . 1_455 2.09(3) ?
  O6 O7 . . 2.418(3) ?
  O6 O7 . 4_565 2.418(3) ?
  O7 O7 . 4_565 2.425(3) ?
  O8 H8a . . 0.81(5) ?
  O8 H8b . . 0.79(4) ?
  O9 H9 . . 0.90(4) ?
  O10 H10 . . 0.84(3) ?
  O11 H11 . . 0.84(4) ?
  H8a H8b . . 1.46(6) ?
  H8a H10 . . 2.41(4) ?
  H8b H8b . 4_555 2.32(6) ?

loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_2
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
  O1 S1 O2 . . . 105.43(8) ?
  O1 S1 O2 . . 4_565 105.43(8) ?
  O2 S1 O2 . . 4_565 104.83(10) ?
  O3 S2 O3 . . 4_555 104.39(9) ?
  O3 S2 O4 . . . 105.06(9) ?
  O3 S2 O4 4_555 . . 105.06(9) ?
  O5 S3 O6 . . . 111.27(16) ?
  O5 S3 O7 . . . 108.11(12) ?
  O5 S3 O7 . . 4_565 108.11(12) ?
  O6 S3 O7 . . . 109.13(10) ?
  O6 S3 O7 . . 4_565 109.13(10) ?
  O7 S3 O7 . . 4_565 111.08(13) ?

loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion
 _geom_torsion_publ_flag
 ? ? ? ? ? ? ? ? ? ?

loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_D
 _geom_hbond_site_symmetry_H
 _geom_hbond_site_symmetry_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_publ_flag
  O8 H8b O5 . . 2_646   0.79(4)   1.95(4)   2.734(4)   171(4) ?
  O9 H9 O1 . . 2_646   0.90(4)   2.06(4)   2.914(2)   160(4) ?
  O10 H10 O5 . . 1_655   0.84(3)   2.09(3)   2.919(3)   169(7) ?


#=======================================================================

# 11. STRUCTURE-FACTOR LIST


