#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:45:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179934 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/29/7022962.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7022962
loop_
_publ_author_name
'Ben Yahia, Hamdi'
'Shikano, Masahiro'
'Kobayashi, Hironori'
_publ_section_title
;
 Single crystal growth of the novel Mn2(OH)2SO3, Mn2F(OH)SO3, and
 Mn5(OH)4(H2O)2[SO3]2[SO4] compounds using a hydrothermal method.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7158
_journal_page_last               7166
_journal_paper_doi               10.1039/c3dt50415h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'H8 Mn5 O16 S3'
_chemical_formula_sum            'H8 Mn5 O16 S3'
_chemical_formula_weight         634.9
_chemical_name_systematic        ' ?'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.6005(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6117(7)
_cell_length_b                   8.5326(7)
_cell_length_c                   10.9273(9)
_cell_measurement_reflns_used    5936
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      1.9
_cell_volume                     695.21(10)
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Smart Apex'
_diffrn_measurement_method       Multi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.12
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5936
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         1.9
_exptl_absorpt_coefficient_mu    4.954
_exptl_absorpt_correction_T_max  0.6556
_exptl_absorpt_correction_T_min  0.1805
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'Jana2006  (Petricek, Dusek & Palatinus, 2000)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    3.0321
_exptl_crystal_description       needle
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.14
_refine_ls_goodness_of_fit_ref   1.15
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_constraints    0
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1559
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.0009I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                1500
_reflns_number_total             1559
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            c3dt50415h_3.cif
_cod_data_source_block           I
_cod_database_code               7022962
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
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
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
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'
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_3
_geom_angle
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
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_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
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)
