# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CYCU-5as

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H12 O7.50 S Zn1.50'
_chemical_formula_weight         442.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   14.0847(4)
_cell_length_b                   5.9953(2)
_cell_length_c                   19.3347(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.729(2)
_cell_angle_gamma                90.00
_cell_volume                     1629.20(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9975
_cell_measurement_theta_min      2.8986
_cell_measurement_theta_max      28.3001

_exptl_crystal_description       lamellar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             892
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_T_max  0.7958
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            26234
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         28.32
_reflns_number_total             4029
_reflns_number_gt                3608
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL


_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0266P)²+12.5581P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4029
_refine_ls_number_parameters     226
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1146
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.5000 0.5000 0.00869(14) Uani 1 2 d S . .
Zn2 Zn 0.39977(3) 0.98594(7) 0.47761(2) 0.00981(12) Uani 1 1 d . . .
S1 S 0.03455(6) 0.39971(16) 0.76716(5) 0.00885(18) Uani 1 1 d . . .
O1 O 0.30348(19) 0.8638(5) 0.53307(14) 0.0140(6) Uani 1 1 d . . .
O2 O 0.59764(19) 0.4087(5) 0.42893(14) 0.0126(5) Uani 1 1 d . . .
O3 O 0.3789(2) 0.4830(5) 0.42477(14) 0.0144(6) Uani 1 1 d . . .
O4 O 0.3390(2) 1.1295(5) 0.39846(15) 0.0144(6) Uani 1 1 d . . .
O5 O 0.04005(19) 0.1605(5) 0.77269(15) 0.0139(6) Uani 1 1 d . . .
O6 O 0.04869(19) 0.5353(5) 0.82893(14) 0.0139(6) Uani 1 1 d . . .
O7 O 0.51537(18) 0.8135(5) 0.46303(13) 0.0093(5) Uani 1 1 d . . .
H7 H 0.5264 0.8187 0.4185 0.011 Uiso 1 1 d . . .
C1 C 0.3265(3) 0.6966(6) 0.57166(19) 0.0102(7) Uani 1 1 d . . .
C2 C 0.2538(3) 0.6246(6) 0.62062(19) 0.0099(7) Uani 1 1 d . . .
C3 C 0.2613(3) 0.4149(7) 0.6517(2) 0.0139(7) Uani 1 1 d . . .
H3A H 0.3122 0.3221 0.6433 0.017 Uiso 1 1 calc R . .
C4 C 0.1925(3) 0.3453(7) 0.6952(2) 0.0136(7) Uani 1 1 d . . .
H4A H 0.1957 0.2039 0.7150 0.016 Uiso 1 1 calc R . .
C5 C 0.1188(3) 0.4888(6) 0.70885(19) 0.0102(7) Uani 1 1 d . . .
C6 C 0.1126(3) 0.7010(7) 0.6804(2) 0.0139(8) Uani 1 1 d . . .
H6A H 0.0642 0.7976 0.6914 0.017 Uiso 1 1 calc R . .
C7 C 0.1797(3) 0.7669(7) 0.6351(2) 0.0144(8) Uani 1 1 d . . .
H7A H 0.1752 0.9067 0.6143 0.017 Uiso 1 1 calc R . .
C8 C -0.0767(3) 0.4712(6) 0.72544(18) 0.0092(7) Uani 1 1 d . . .
C9 C -0.1175(3) 0.6760(7) 0.73834(19) 0.0103(7) Uani 1 1 d . . .
H9A H -0.0899 0.7720 0.7717 0.012 Uiso 1 1 calc R . .
C10 C -0.2011(3) 0.7344(7) 0.69996(19) 0.0116(7) Uani 1 1 d . . .
H10A H -0.2290 0.8726 0.7068 0.014 Uiso 1 1 calc R . .
C11 C -0.2431(3) 0.5870(7) 0.65145(19) 0.0104(7) Uani 1 1 d . . .
C12 C -0.2032(3) 0.3777(7) 0.6416(2) 0.0128(7) Uani 1 1 d . . .
H12A H -0.2331 0.2771 0.6107 0.015 Uiso 1 1 calc R . .
C13 C -0.1185(3) 0.3198(7) 0.6782(2) 0.0128(7) Uani 1 1 d . . .
H13A H -0.0902 0.1821 0.6711 0.015 Uiso 1 1 calc R . .
C14 C 0.3283(3) 1.3400(7) 0.39426(19) 0.0103(7) Uani 1 1 d . . .
C2S C 0.1141(13) 0.011(3) 0.4704(10) 0.074(5) Uiso 0.50 1 d PD . .
H2SA H 0.1809 0.0193 0.4636 0.110 Uiso 0.50 1 calc PR . .
H2SB H 0.0806 -0.0408 0.4286 0.110 Uiso 0.50 1 calc PR . .
H2SC H 0.1038 -0.0912 0.5075 0.110 Uiso 0.50 1 calc PR . .
C1S C 0.078(2) 0.238(4) 0.4885(19) 0.163(13) Uiso 0.50 1 d PD . .
H1SA H 0.1336 0.2847 0.5171 0.195 Uiso 0.50 1 calc PR . .
H1SB H 0.0868 0.3080 0.4442 0.195 Uiso 0.50 1 calc PR . .
O1S O 0.013(2) 0.398(5) 0.5133(16) 0.214(13) Uiso 0.50 1 d PD . .
H1SC H 0.0454 0.5309 0.5119 0.321 Uiso 0.50 1 d P . .


_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
Zn1 O7 2.027(3) 3_666 ?
Zn1 O7 2.027(3) . ?
Zn1 O2 2.080(3) . ?
Zn1 O2 2.080(3) 3_666 ?
Zn1 O3 2.170(3) . ?
Zn1 O3 2.170(3) 3_666 ?
Zn2 O4 1.909(3) . ?
Zn2 O1 1.927(3) . ?
Zn2 O7 1.965(3) . ?
Zn2 O7 2.003(3) 3_676 ?
Zn2 Zn2 2.9038(8) 3_676 ?
S1 O5 1.440(3) . ?
S1 O6 1.448(3) . ?
S1 C8 1.768(4) . ?
S1 C5 1.771(4) . ?
O1 C1 1.279(5) . ?
O2 C1 1.242(5) 3_666 ?
O3 C14 1.240(5) 1_545 ?
O4 C14 1.273(5) . ?
O7 Zn2 2.003(3) 3_676 ?
O7 H7 0.8853 . ?
C1 O2 1.242(5) 3_666 ?
C1 C2 1.502(5) . ?
C2 C3 1.394(5) . ?
C2 C7 1.390(5) . ?
C3 C4 1.389(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.386(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.387(5) . ?
C6 C7 1.388(5) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.385(5) . ?
C8 C13 1.391(5) . ?
C9 C10 1.396(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.392(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.393(5) . ?
C11 C14 1.508(5) 3_576 ?
C12 C13 1.391(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 O3 1.240(5) 1_565 ?
C14 C11 1.508(5) 3_576 ?
C2S C1S 1.500(3) . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9600 . ?
C2S H2SC 0.9600 . ?
C1S O1S 1.430(3) . ?
C1S H1SA 0.9700 . ?
C1S H1SB 0.9700 . ?
O1S O1S 1.37(5) 3_566 ?
O1S H1SC 0.9211 . ?

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
O7 Zn1 O7 179.998(1) 3_666 . ?
O7 Zn1 O2 94.55(11) 3_666 . ?
O7 Zn1 O2 85.45(11) . . ?
O7 Zn1 O2 85.45(11) 3_666 3_666 ?
O7 Zn1 O2 94.55(11) . 3_666 ?
O2 Zn1 O2 179.999(1) . 3_666 ?
O7 Zn1 O3 95.48(11) 3_666 . ?
O7 Zn1 O3 84.52(11) . . ?
O2 Zn1 O3 93.97(11) . . ?
O2 Zn1 O3 86.03(11) 3_666 . ?
O7 Zn1 O3 84.52(11) 3_666 3_666 ?
O7 Zn1 O3 95.48(11) . 3_666 ?
O2 Zn1 O3 86.03(11) . 3_666 ?
O2 Zn1 O3 93.97(11) 3_666 3_666 ?
O3 Zn1 O3 179.999(1) . 3_666 ?
O4 Zn2 O1 108.78(12) . . ?
O4 Zn2 O7 117.07(12) . . ?
O1 Zn2 O7 119.97(12) . . ?
O4 Zn2 O7 114.11(12) . 3_676 ?
O1 Zn2 O7 108.93(11) . 3_676 ?
O7 Zn2 O7 85.93(11) . 3_676 ?
O4 Zn2 Zn2 126.13(9) . 3_676 ?
O1 Zn2 Zn2 124.18(9) . 3_676 ?
O7 Zn2 Zn2 43.49(8) . 3_676 ?
O7 Zn2 Zn2 42.44(8) 3_676 3_676 ?
O5 S1 O6 119.63(18) . . ?
O5 S1 C8 108.48(18) . . ?
O6 S1 C8 108.10(17) . . ?
O5 S1 C5 108.20(18) . . ?
O6 S1 C5 107.09(17) . . ?
C8 S1 C5 104.30(17) . . ?
C1 O1 Zn2 117.5(2) . . ?
C1 O2 Zn1 138.3(3) 3_666 . ?
C14 O3 Zn1 138.9(3) 1_545 . ?
C14 O4 Zn2 122.9(3) . . ?
Zn2 O7 Zn2 94.07(11) . 3_676 ?
Zn2 O7 Zn1 109.20(12) . . ?
Zn2 O7 Zn1 115.33(12) 3_676 . ?
Zn2 O7 H7 108.7 . . ?
Zn2 O7 H7 113.6 3_676 . ?
Zn1 O7 H7 113.9 . . ?
O2 C1 O1 125.3(3) 3_666 . ?
O2 C1 C2 118.8(3) 3_666 . ?
O1 C1 C2 115.8(3) . . ?
C3 C2 C7 120.2(3) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.1(3) . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C5 C4 C3 119.3(4) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C4 C5 C6 121.5(3) . . ?
C4 C5 S1 118.4(3) . . ?
C6 C5 S1 120.1(3) . . ?
C7 C6 C5 118.9(4) . . ?
C7 C6 H6A 120.5 . . ?
C5 C6 H6A 120.5 . . ?
C6 C7 C2 120.2(4) . . ?
C6 C7 H7A 119.9 . . ?
C2 C7 H7A 119.9 . . ?
C9 C8 C13 122.3(3) . . ?
C9 C8 S1 119.9(3) . . ?
C13 C8 S1 117.8(3) . . ?
C10 C9 C8 118.2(3) . . ?
C10 C9 H9A 120.9 . . ?
C8 C9 H9A 120.9 . . ?
C9 C10 C11 120.4(4) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C12 C11 C10 120.4(4) . . ?
C12 C11 C14 119.6(3) . 3_576 ?
C10 C11 C14 119.8(3) . 3_576 ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
C12 C13 C8 118.9(4) . . ?
C12 C13 H13A 120.5 . . ?
C8 C13 H13A 120.5 . . ?
O3 C14 O4 126.4(4) 1_565 . ?
O3 C14 C11 119.3(3) 1_565 3_576 ?
O4 C14 C11 114.3(3) . 3_576 ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
O1S C1S C2S 157(3) . . ?
O1S C1S H1SA 97.1 . . ?
C2S C1S H1SA 97.1 . . ?
O1S C1S H1SB 97.2 . . ?
C2S C1S H1SB 97.1 . . ?
H1SA C1S H1SB 103.5 . . ?
O1S O1S C1S 130(3) 3_566 . ?
O1S O1S H1SC 48.2 3_566 . ?
C1S O1S H1SC 104.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7 O6 0.89 1.98 2.815(4) 155.8 4_675

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.146
_database_code_depnum_ccdc_archive 'CCDC 943771'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CYCU-5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H18 O14 S2 Zn3'
_chemical_formula_sum            'C28 H18 O14 S2 Zn3'
_chemical_formula_weight         838.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   14.1168(2)
_cell_length_b                   6.05310(10)
_cell_length_c                   19.3678(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6270(10)
_cell_angle_gamma                90.00
_cell_volume                     1651.67(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7156
_cell_measurement_theta_min      2.8917
_cell_measurement_theta_max      28.2922

_exptl_crystal_description       acicular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    2.353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6504
_exptl_absorpt_correction_T_max  0.7987
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            15157
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.30
_reflns_number_total             4098
_reflns_number_gt                3128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0308P)²+0.4854P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4098
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.5000 0.5000 0.02104(9) Uani 1 2 d S . .
Zn2 Zn 0.399647(16) 0.98820(4) 0.479454(13) 0.02453(8) Uani 1 1 d . . .
S1 S 0.03266(3) 0.40487(11) 0.76635(3) 0.02525(14) Uani 1 1 d . . .
O1 O 0.30593(10) 0.8640(3) 0.53561(8) 0.0336(4) Uani 1 1 d . . .
O2 O 0.59981(10) 0.4159(3) 0.42994(8) 0.0317(4) Uani 1 1 d . . .
O3 O 0.37996(11) 0.4769(3) 0.42382(9) 0.0338(4) Uani 1 1 d . . .
O4 O 0.33725(11) 1.1274(3) 0.40097(8) 0.0363(4) Uani 1 1 d . . .
O5 O 0.03773(10) 0.1690(3) 0.77228(9) 0.0364(4) Uani 1 1 d . . .
O6 O 0.04648(11) 0.5396(3) 0.82728(8) 0.0370(4) Uani 1 1 d . . .
O7 O 0.51365(9) 0.8122(2) 0.46343(7) 0.0217(3) Uani 1 1 d . . .
H7 H 0.5264 0.8187 0.4185 0.026 Uiso 1 1 d . . .
C1 C 0.32612(14) 0.6940(4) 0.57155(11) 0.0252(5) Uani 1 1 d . . .
C2 C 0.25302(13) 0.6217(4) 0.62014(11) 0.0245(5) Uani 1 1 d . . .
C3 C 0.25893(15) 0.4169(4) 0.65111(12) 0.0331(6) Uani 1 1 d . . .
H3A H 0.3093 0.3237 0.6428 0.040 Uiso 1 1 calc R . .
C4 C 0.19058(15) 0.3490(4) 0.69447(12) 0.0320(6) Uani 1 1 d . . .
H4A H 0.1940 0.2092 0.7144 0.038 Uiso 1 1 calc R . .
C5 C 0.11737(14) 0.4896(4) 0.70790(11) 0.0235(5) Uani 1 1 d . . .
C6 C 0.11192(16) 0.6984(4) 0.67874(13) 0.0384(6) Uani 1 1 d . . .
H6A H 0.0634 0.7944 0.6891 0.046 Uiso 1 1 calc R . .
C7 C 0.17945(16) 0.7626(4) 0.63412(13) 0.0367(6) Uani 1 1 d . . .
H7A H 0.1754 0.9011 0.6134 0.044 Uiso 1 1 calc R . .
C8 C -0.07774(13) 0.4760(4) 0.72397(11) 0.0225(5) Uani 1 1 d . . .
C9 C -0.11864(14) 0.6784(4) 0.73653(11) 0.0274(5) Uani 1 1 d . . .
H9A H -0.0914 0.7734 0.7699 0.033 Uiso 1 1 calc R . .
C10 C -0.20113(14) 0.7368(4) 0.69825(11) 0.0263(5) Uani 1 1 d . . .
H10A H -0.2288 0.8739 0.7052 0.032 Uiso 1 1 calc R . .
C11 C -0.24281(13) 0.5921(4) 0.64966(10) 0.0228(5) Uani 1 1 d . . .
C12 C -0.20278(15) 0.3872(4) 0.63994(12) 0.0316(5) Uani 1 1 d . . .
H12A H -0.2321 0.2881 0.6087 0.038 Uiso 1 1 calc R . .
C13 C -0.11910(15) 0.3289(4) 0.67661(12) 0.0305(5) Uani 1 1 d . . .
H13A H -0.0911 0.1924 0.6694 0.037 Uiso 1 1 calc R . .
C14 C 0.32805(14) 1.3350(4) 0.39524(10) 0.0249(5) 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
Zn1 O7 2.0316(14) . ?
Zn1 O7 2.0317(14) 3_666 ?
Zn1 O2 2.0802(14) 3_666 ?
Zn1 O2 2.0802(14) . ?
Zn1 O3 2.1799(15) . ?
Zn1 O3 2.1799(15) 3_666 ?
Zn2 O4 1.9045(16) . ?
Zn2 O1 1.9184(15) . ?
Zn2 O7 1.9710(13) . ?
Zn2 O7 2.0025(14) 3_676 ?
Zn2 Zn2 2.8977(5) 3_676 ?
S1 O5 1.4336(18) . ?
S1 O6 1.4376(17) . ?
S1 C8 1.768(2) . ?
S1 C5 1.774(2) . ?
O1 C1 1.265(3) . ?
O2 C1 1.241(3) 3_666 ?
O3 C14 1.237(3) 1_545 ?
O4 C14 1.268(3) . ?
O7 Zn2 2.0025(14) 3_676 ?
O7 H7 0.9005 . ?
C1 O2 1.241(3) 3_666 ?
C1 C2 1.505(3) . ?
C2 C3 1.378(3) . ?
C2 C7 1.383(3) . ?
C3 C4 1.381(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.377(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.384(3) . ?
C6 C7 1.382(3) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.381(3) . ?
C8 C9 1.383(3) . ?
C9 C10 1.386(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.389(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.381(3) . ?
C11 C14 1.506(3) 3_576 ?
C12 C13 1.385(3) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 O3 1.237(3) 1_565 ?
C14 C11 1.506(3) 3_576 ?

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
O7 Zn1 O7 180.00(7) . 3_666 ?
O7 Zn1 O2 94.76(6) . 3_666 ?
O7 Zn1 O2 85.24(6) 3_666 3_666 ?
O7 Zn1 O2 85.24(6) . . ?
O7 Zn1 O2 94.76(6) 3_666 . ?
O2 Zn1 O2 180.00(10) 3_666 . ?
O7 Zn1 O3 84.87(6) . . ?
O7 Zn1 O3 95.13(6) 3_666 . ?
O2 Zn1 O3 85.85(6) 3_666 . ?
O2 Zn1 O3 94.15(6) . . ?
O7 Zn1 O3 95.13(6) . 3_666 ?
O7 Zn1 O3 84.87(6) 3_666 3_666 ?
O2 Zn1 O3 94.15(6) 3_666 3_666 ?
O2 Zn1 O3 85.85(6) . 3_666 ?
O3 Zn1 O3 179.999(1) . 3_666 ?
O4 Zn2 O1 108.97(7) . . ?
O4 Zn2 O7 117.03(7) . . ?
O1 Zn2 O7 118.47(6) . . ?
O4 Zn2 O7 114.19(7) . 3_676 ?
O1 Zn2 O7 110.03(6) . 3_676 ?
O7 Zn2 O7 86.36(6) . 3_676 ?
O4 Zn2 Zn2 126.32(5) . 3_676 ?
O1 Zn2 Zn2 124.13(5) . 3_676 ?
O7 Zn2 Zn2 43.61(4) . 3_676 ?
O7 Zn2 Zn2 42.75(4) 3_676 3_676 ?
O5 S1 O6 119.71(11) . . ?
O5 S1 C8 108.52(10) . . ?
O6 S1 C8 108.24(10) . . ?
O5 S1 C5 107.87(10) . . ?
O6 S1 C5 107.33(10) . . ?
C8 S1 C5 104.09(10) . . ?
C1 O1 Zn2 119.43(13) . . ?
C1 O2 Zn1 138.83(15) 3_666 . ?
C14 O3 Zn1 139.52(15) 1_545 . ?
C14 O4 Zn2 123.24(15) . . ?
Zn2 O7 Zn2 93.64(6) . 3_676 ?
Zn2 O7 Zn1 110.57(6) . . ?
Zn2 O7 Zn1 115.89(7) 3_676 . ?
Zn2 O7 H7 110.1 . . ?
Zn2 O7 H7 110.8 3_676 . ?
Zn1 O7 H7 114.0 . . ?
O2 C1 O1 125.73(19) 3_666 . ?
O2 C1 C2 118.1(2) 3_666 . ?
O1 C1 C2 116.17(19) . . ?
C3 C2 C7 119.66(19) . . ?
C3 C2 C1 120.58(19) . . ?
C7 C2 C1 119.8(2) . . ?
C2 C3 C4 120.5(2) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 119.5(2) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C4 C5 C6 120.7(2) . . ?
C4 C5 S1 119.09(18) . . ?
C6 C5 S1 120.14(16) . . ?
C7 C6 C5 119.3(2) . . ?
C7 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
C6 C7 C2 120.3(2) . . ?
C6 C7 H7A 119.8 . . ?
C2 C7 H7A 119.8 . . ?
C13 C8 C9 121.62(19) . . ?
C13 C8 S1 118.35(17) . . ?
C9 C8 S1 119.98(17) . . ?
C8 C9 C10 118.5(2) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
C9 C10 C11 120.5(2) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C12 C11 C10 119.96(19) . . ?
C12 C11 C14 120.2(2) . 3_576 ?
C10 C11 C14 119.7(2) . 3_576 ?
C11 C12 C13 120.1(2) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C8 C13 C12 119.2(2) . . ?
C8 C13 H13A 120.4 . . ?
C12 C13 H13A 120.4 . . ?
O3 C14 O4 126.5(2) 1_565 . ?
O3 C14 C11 119.0(2) 1_565 3_576 ?
O4 C14 C11 114.5(2) . 3_576 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7 O6 0.90 2.00 2.851(2) 157.0 4_675

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.073


_database_code_depnum_ccdc_archive 'CCDC 943772'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H74 Mg6 O43 S4'
_chemical_formula_weight         1757.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c
_symmetry_space_group_name_hall  '-P 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   28.1637(9)
_cell_length_b                   6.4411(2)
_cell_length_c                   24.8679(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.445(2)
_cell_angle_gamma                90.00
_cell_volume                     4073.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9986
_cell_measurement_theta_min      2.4025
_cell_measurement_theta_max      28.2676

_exptl_crystal_description       columnar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1828
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9455
_exptl_absorpt_correction_T_max  0.9624
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            45162
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         28.40
_reflns_number_total             10210
_reflns_number_gt                5338
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0688P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10210
_refine_ls_number_parameters     510
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1468
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.42411(3) 0.42022(14) 0.39919(3) 0.0330(2) Uani 1 1 d . . .
S2 S 1.09333(3) 0.34684(14) 0.62768(3) 0.0331(2) Uani 1 1 d . . .
Mg1 Mg 0.77774(3) -0.12110(15) 0.43822(4) 0.0205(2) Uani 1 1 d . . .
Mg2 Mg 0.75701(3) 0.37763(14) 0.48502(4) 0.0183(2) Uani 1 1 d . . .
Mg3 Mg 0.73607(3) -0.12183(15) 0.53295(4) 0.0214(2) Uani 1 1 d . . .
O1 O 0.77832(7) 0.0727(3) 0.50411(8) 0.0193(4) Uani 1 1 d . . .
H1 H 0.8080 0.1001 0.5327 0.023 Uiso 1 1 d R . .
O2 O 0.73521(7) -0.3162(3) 0.46690(8) 0.0200(4) Uani 1 1 d . . .
H2 H 0.7011 -0.3366 0.4420 0.024 Uiso 1 1 d R . .
O3 O 0.77491(8) -0.3294(3) 0.37116(8) 0.0302(5) Uani 1 1 d . . .
H3B H 0.8060 -0.3574 0.3759 0.045 Uiso 1 1 d R . .
H3C H 0.7594 -0.4403 0.3733 0.045 Uiso 1 1 d R . .
O4 O 0.85126(7) -0.2411(3) 0.49582(9) 0.0287(5) Uani 1 1 d . . .
O5 O 0.70953(8) 0.0034(3) 0.37211(9) 0.0291(5) Uani 1 1 d . . .
O6 O 0.82269(8) 0.0845(3) 0.41144(10) 0.0370(6) Uani 1 1 d . . .
H6B H 0.8516 0.0274 0.4170 0.056 Uiso 1 1 d R . .
H6C H 0.8286 0.1956 0.4317 0.056 Uiso 1 1 d R . .
O7 O 0.79085(7) 0.4133(3) 0.57837(8) 0.0281(5) Uani 1 1 d . . .
O8 O 0.83192(7) 0.4206(3) 0.48873(8) 0.0261(5) Uani 1 1 d . . .
O9 O 0.72324(7) 0.3400(3) 0.39288(8) 0.0282(5) Uani 1 1 d . . .
O10 O 0.68278(7) 0.3374(3) 0.48434(9) 0.0289(5) Uani 1 1 d . . .
O11 O 0.80514(8) -0.2487(3) 0.59780(9) 0.0302(5) Uani 1 1 d . . .
O12 O 0.66260(7) 0.0009(3) 0.47927(10) 0.0327(5) Uani 1 1 d . . .
O13 O 0.69354(8) -0.3344(3) 0.55992(9) 0.0344(5) Uani 1 1 d . . .
H13B H 0.6644 -0.2807 0.5552 0.052 Uiso 1 1 d R . .
H13C H 0.6879 -0.4442 0.5391 0.052 Uiso 1 1 d R . .
O14 O 0.74205(9) 0.0845(3) 0.60195(9) 0.0371(6) Uani 1 1 d . . .
H14A H 0.7695 0.1595 0.6157 0.056 Uiso 1 1 d R . .
O15 O 0.42114(8) 0.6411(4) 0.40289(10) 0.0469(7) Uani 1 1 d . . .
O16 O 0.40429(8) 0.2906(4) 0.43209(9) 0.0466(7) Uani 1 1 d . . .
O17 O 1.09685(8) 0.1245(4) 0.62387(10) 0.0470(7) Uani 1 1 d . . .
O18 O 1.12041(8) 0.4771(4) 0.60281(9) 0.0445(7) Uani 1 1 d . . .
C1 C 0.65081(10) 0.1896(5) 0.47380(12) 0.0244(7) Uani 1 1 d . . .
C1S C 0.70737(18) 0.1159(7) 0.6283(2) 0.0737(13) Uani 1 1 d . . .
H1SA H 0.6981 -0.0189 0.6384 0.088 Uiso 1 1 calc R . .
H1SB H 0.6754 0.1776 0.5987 0.088 Uiso 1 1 calc R . .
C2 C 0.59389(10) 0.2453(5) 0.45395(12) 0.0255(7) Uani 1 1 d . . .
C2S C 0.72572(19) 0.2432(9) 0.6807(2) 0.0948(17) Uani 1 1 d . . .
H2SA H 0.6989 0.2529 0.6947 0.142 Uiso 1 1 calc R . .
H2SB H 0.7338 0.3795 0.6714 0.142 Uiso 1 1 calc R . .
H2SC H 0.7568 0.1824 0.7111 0.142 Uiso 1 1 calc R . .
C3 C 0.55886(11) 0.1000(5) 0.45668(14) 0.0329(8) Uani 1 1 d . . .
H3A H 0.5704 -0.0340 0.4697 0.040 Uiso 1 1 calc R . .
C4 C 0.50685(11) 0.1521(5) 0.44021(14) 0.0352(8) Uani 1 1 d . . .
H4A H 0.4834 0.0548 0.4425 0.042 Uiso 1 1 calc R . .
C5 C 0.49045(10) 0.3498(5) 0.42051(12) 0.0275(7) Uani 1 1 d . . .
C6 C 0.52445(12) 0.4973(5) 0.41739(15) 0.0399(9) Uani 1 1 d . . .
H6A H 0.5127 0.6309 0.4042 0.048 Uiso 1 1 calc R . .
C7 C 0.57652(12) 0.4436(5) 0.43421(15) 0.0385(9) Uani 1 1 d . . .
H7A H 0.5999 0.5417 0.4322 0.046 Uiso 1 1 calc R . .
C8 C 0.39055(10) 0.3473(5) 0.32322(12) 0.0277(7) Uani 1 1 d . . .
C9 C 0.37327(12) 0.1469(5) 0.30861(13) 0.0358(8) Uani 1 1 d . . .
H9A H 0.3808 0.0469 0.3381 0.043 Uiso 1 1 calc R . .
C10 C 0.65539(12) 0.0965(5) 0.25046(13) 0.0348(8) Uani 1 1 d . . .
H10A H 0.6668 -0.0393 0.2610 0.042 Uiso 1 1 calc R . .
C11 C 0.66726(11) 0.2453(5) 0.29417(12) 0.0257(7) Uani 1 1 d . . .
C12 C 0.64831(13) 0.4422(5) 0.27897(14) 0.0396(9) Uani 1 1 d . . .
H12A H 0.6554 0.5414 0.3086 0.048 Uiso 1 1 calc R . .
C13 C 0.38142(13) 0.4961(6) 0.28027(14) 0.0409(9) Uani 1 1 d . . .
H13A H 0.3948 0.6296 0.2906 0.049 Uiso 1 1 calc R . .
C14 C 0.70246(10) 0.1910(5) 0.35806(12) 0.0236(7) Uani 1 1 d . . .
C15 C 0.86343(10) 0.5712(5) 0.50497(11) 0.0230(7) Uani 1 1 d . . .
C16 C 0.92144(10) 0.5186(5) 0.53769(12) 0.0236(7) Uani 1 1 d . . .
C17 C 0.95920(11) 0.6655(5) 0.54453(13) 0.0314(8) Uani 1 1 d . . .
H17B H 0.9490 0.7995 0.5303 0.038 Uiso 1 1 calc R . .
C18 C 1.01197(11) 0.6159(5) 0.57234(14) 0.0353(8) Uani 1 1 d . . .
H18B H 1.0374 0.7145 0.5764 0.042 Uiso 1 1 calc R . .
C19 C 1.02627(10) 0.4160(5) 0.59406(12) 0.0290(8) Uani 1 1 d . . .
C20 C 0.98903(12) 0.2683(6) 0.58857(16) 0.0452(10) Uani 1 1 d . . .
H20A H 0.9990 0.1355 0.6040 0.054 Uiso 1 1 calc R . .
C21 C 0.93647(12) 0.3217(6) 0.55960(15) 0.0423(9) Uani 1 1 d . . .
H21A H 0.9109 0.2228 0.5549 0.051 Uiso 1 1 calc R . .
C22 C 1.11678(11) 0.4153(5) 0.70337(12) 0.0292(8) Uani 1 1 d . . .
C23 C 1.13858(13) 0.6097(5) 0.72103(14) 0.0411(9) Uani 1 1 d . . .
H23A H 1.1389 0.7055 0.6932 0.049 Uiso 1 1 calc R . .
C24 C 0.84005(13) 0.6593(5) 0.71914(13) 0.0400(9) Uani 1 1 d . . .
H24A H 0.8259 0.7906 0.7066 0.048 Uiso 1 1 calc R . .
C25 C 0.83958(11) 0.5149(5) 0.67764(12) 0.0261(7) Uani 1 1 d . . .
C26 C 0.86230(13) 0.3229(6) 0.69625(14) 0.0402(9) Uani 1 1 d . . .
H26A H 0.8625 0.2268 0.6684 0.048 Uiso 1 1 calc R . .
C27 C 0.88491(13) 0.2723(6) 0.75629(14) 0.0417(9) Uani 1 1 d . . .
H27A H 0.9009 0.1440 0.7691 0.050 Uiso 1 1 calc R . .
C28 C 0.81028(10) 0.5655(5) 0.61260(12) 0.0244(7) Uani 1 1 d . . .
O1W O 0.9031(4) -0.0742(12) 0.6304(5) 0.384(5) Uani 1 1 d . . .
H1WA H 0.8796 -0.0795 0.6433 0.576 Uiso 1 1 d R . .
H1WB H 0.9304 -0.1334 0.6561 0.576 Uiso 1 1 d R . .
O2W O 0.6120(5) -0.1831(16) 0.3613(5) 0.411(6) Uani 1 1 d . . .
H2WA H 0.6119 -0.1815 0.3955 0.616 Uiso 1 1 d R . .
H2WB H 0.5836 -0.1273 0.3367 0.616 Uiso 1 1 d R . .
O3W O 1.0000 0.790(4) 0.7500 0.519(14) Uani 1 2 d S . .
H3WA H 1.0155 0.7092 0.7358 0.778 Uiso 1 1 d R . .
O4W O 0.5041(11) 0.008(3) 0.2774(6) 0.713(18) Uani 1 1 d . . .
H4WA H 0.4802 -0.0774 0.2750 1.070 Uiso 1 1 d R . .
H4WB H 0.4964 0.1257 0.2868 1.070 Uiso 1 1 d R . .


_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
S1 O15 1.431(2) . ?
S1 O16 1.439(3) . ?
S1 C5 1.768(3) . ?
S1 C8 1.774(3) . ?
S2 O18 1.440(2) . ?
S2 O17 1.442(3) . ?
S2 C22 1.762(3) . ?
S2 C19 1.763(3) . ?
Mg1 O1 2.054(2) . ?
Mg1 O2 2.063(2) . ?
Mg1 O5 2.079(2) . ?
Mg1 O4 2.095(2) . ?
Mg1 O3 2.115(2) . ?
Mg1 O6 2.127(2) . ?
Mg2 O1 2.049(2) . ?
Mg2 O2 2.057(2) 1_565 ?
Mg2 O9 2.083(2) . ?
Mg2 O8 2.090(2) . ?
Mg2 O10 2.099(2) . ?
Mg2 O7 2.109(2) . ?
Mg2 H1 2.2805 . ?
Mg3 O2 2.057(2) . ?
Mg3 O1 2.058(2) . ?
Mg3 O12 2.077(2) . ?
Mg3 O11 2.087(2) . ?
Mg3 O13 2.109(2) . ?
Mg3 O14 2.119(2) . ?
O1 H1 0.8512 . ?
O2 Mg2 2.057(2) 1_545 ?
O2 H2 0.9013 . ?
O3 H3B 0.8500 . ?
O3 H3C 0.8501 . ?
O4 C15 1.251(3) 1_545 ?
O5 C14 1.250(3) . ?
O6 H6B 0.8496 . ?
O6 H6C 0.8501 . ?
O7 C28 1.259(3) . ?
O8 C15 1.259(3) . ?
O9 C14 1.257(3) . ?
O10 C1 1.258(3) . ?
O11 C28 1.242(4) 1_545 ?
O12 C1 1.252(3) . ?
O13 H13B 0.8501 . ?
O13 H13C 0.8502 . ?
O14 C1S 1.405(5) . ?
O14 H14A 0.8501 . ?
C1 C2 1.504(4) . ?
C1S C2S 1.434(6) . ?
C1S H1SA 0.9700 . ?
C1S H1SB 0.9700 . ?
C2 C7 1.380(4) . ?
C2 C3 1.383(4) . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9600 . ?
C2S H2SC 0.9600 . ?
C3 C4 1.382(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.371(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.374(4) . ?
C6 C7 1.385(4) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.372(4) . ?
C8 C13 1.374(4) . ?
C9 C10 1.377(4) 2_655 ?
C9 H9A 0.9300 . ?
C10 C9 1.377(4) 2_655 ?
C10 C11 1.378(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.365(4) . ?
C11 C14 1.509(4) . ?
C12 C13 1.390(4) 2_655 ?
C12 H12A 0.9300 . ?
C13 C12 1.390(4) 2_655 ?
C13 H13A 0.9300 . ?
C15 O4 1.251(3) 1_565 ?
C15 C16 1.518(4) . ?
C16 C21 1.374(4) . ?
C16 C17 1.378(4) . ?
C17 C18 1.381(4) . ?
C17 H17B 0.9300 . ?
C18 C19 1.387(4) . ?
C18 H18B 0.9300 . ?
C19 C20 1.379(5) . ?
C20 C21 1.383(4) . ?
C20 H20A 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C27 1.378(5) 2_756 ?
C22 C23 1.381(4) . ?
C23 C24 1.382(4) 2_756 ?
C23 H23A 0.9300 . ?
C24 C23 1.381(4) 2_756 ?
C24 C25 1.385(4) . ?
C24 H24A 0.9300 . ?
C25 C26 1.378(4) . ?
C25 C28 1.502(4) . ?
C26 C27 1.387(4) . ?
C26 H26A 0.9300 . ?
C27 C22 1.378(5) 2_756 ?
C27 H27A 0.9300 . ?
C28 O11 1.242(4) 1_565 ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8500 . ?
O3W H3WA 0.8500 . ?
O4W O4W 1.28(3) 2_655 ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8500 . ?

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
O15 S1 O16 119.53(16) . . ?
O15 S1 C5 108.62(15) . . ?
O16 S1 C5 107.38(14) . . ?
O15 S1 C8 108.21(14) . . ?
O16 S1 C8 107.01(14) . . ?
C5 S1 C8 105.20(14) . . ?
O18 S2 O17 119.11(15) . . ?
O18 S2 C22 106.77(15) . . ?
O17 S2 C22 108.30(15) . . ?
O18 S2 C19 107.84(14) . . ?
O17 S2 C19 108.05(15) . . ?
C22 S2 C19 106.07(14) . . ?
O1 Mg1 O2 84.34(8) . . ?
O1 Mg1 O5 94.84(8) . . ?
O2 Mg1 O5 91.82(8) . . ?
O1 Mg1 O4 90.69(8) . . ?
O2 Mg1 O4 95.11(8) . . ?
O5 Mg1 O4 171.53(10) . . ?
O1 Mg1 O3 177.49(9) . . ?
O2 Mg1 O3 93.17(8) . . ?
O5 Mg1 O3 84.96(8) . . ?
O4 Mg1 O3 89.80(8) . . ?
O1 Mg1 O6 93.99(9) . . ?
O2 Mg1 O6 178.15(9) . . ?
O5 Mg1 O6 89.11(9) . . ?
O4 Mg1 O6 84.10(9) . . ?
O3 Mg1 O6 88.51(9) . . ?
O1 Mg1 Mg3 42.16(6) . . ?
O2 Mg1 Mg3 42.17(6) . . ?
O5 Mg1 Mg3 94.58(7) . . ?
O4 Mg1 Mg3 93.82(7) . . ?
O3 Mg1 Mg3 135.34(7) . . ?
O6 Mg1 Mg3 136.15(7) . . ?
O1 Mg1 Mg2 30.07(5) . . ?
O2 Mg1 Mg2 103.66(6) . . ?
O5 Mg1 Mg2 71.58(6) . . ?
O4 Mg1 Mg2 111.29(7) . . ?
O3 Mg1 Mg2 151.27(7) . . ?
O6 Mg1 Mg2 75.12(7) . . ?
Mg3 Mg1 Mg2 64.92(3) . . ?
O1 Mg1 Mg2 103.67(6) . 1_545 ?
O2 Mg1 Mg2 30.06(5) . 1_545 ?
O5 Mg1 Mg2 112.47(7) . 1_545 ?
O4 Mg1 Mg2 72.24(6) . 1_545 ?
O3 Mg1 Mg2 74.14(6) . 1_545 ?
O6 Mg1 Mg2 150.37(7) . 1_545 ?
Mg3 Mg1 Mg2 64.85(3) . 1_545 ?
Mg2 Mg1 Mg2 129.77(4) . 1_545 ?
O1 Mg2 O2 179.09(9) . 1_565 ?
O1 Mg2 O9 95.35(8) . . ?
O2 Mg2 O9 85.31(8) 1_565 . ?
O1 Mg2 O8 85.82(8) . . ?
O2 Mg2 O8 94.79(8) 1_565 . ?
O9 Mg2 O8 92.24(8) . . ?
O1 Mg2 O10 94.30(8) . . ?
O2 Mg2 O10 85.08(8) 1_565 . ?
O9 Mg2 O10 89.67(8) . . ?
O8 Mg2 O10 178.06(9) . . ?
O1 Mg2 O7 84.29(8) . . ?
O2 Mg2 O7 95.04(8) 1_565 . ?
O9 Mg2 O7 179.49(10) . . ?
O8 Mg2 O7 88.10(8) . . ?
O10 Mg2 O7 89.99(8) . . ?
O1 Mg2 Mg1 30.16(5) . . ?
O2 Mg2 Mg1 150.64(6) 1_565 . ?
O9 Mg2 Mg1 66.16(6) . . ?
O8 Mg2 Mg1 80.16(6) . . ?
O10 Mg2 Mg1 100.90(7) . . ?
O7 Mg2 Mg1 113.53(7) . . ?
O1 Mg2 Mg1 150.60(7) . 1_565 ?
O2 Mg2 Mg1 30.16(5) 1_565 1_565 ?
O9 Mg2 Mg1 78.91(6) . 1_565 ?
O8 Mg2 Mg1 65.84(6) . 1_565 ?
O10 Mg2 Mg1 114.30(7) . 1_565 ?
O7 Mg2 Mg1 101.59(7) . 1_565 ?
Mg1 Mg2 Mg1 129.77(4) . 1_565 ?
O1 Mg2 Mg3 29.78(5) . . ?
O2 Mg2 Mg3 149.45(7) 1_565 . ?
O9 Mg2 Mg3 101.53(7) . . ?
O8 Mg2 Mg3 114.41(7) . . ?
O10 Mg2 Mg3 65.43(6) . . ?
O7 Mg2 Mg3 77.98(6) . . ?
Mg1 Mg2 Mg3 50.76(2) . . ?
Mg1 Mg2 Mg3 179.47(4) 1_565 . ?
O1 Mg2 Mg3 149.49(6) . 1_565 ?
O2 Mg2 Mg3 29.71(5) 1_565 1_565 ?
O9 Mg2 Mg3 114.14(7) . 1_565 ?
O8 Mg2 Mg3 100.02(7) . 1_565 ?
O10 Mg2 Mg3 78.91(6) . 1_565 ?
O7 Mg2 Mg3 66.17(6) . 1_565 ?
Mg1 Mg2 Mg3 179.62(4) . 1_565 ?
Mg1 Mg2 Mg3 50.60(2) 1_565 1_565 ?
Mg3 Mg2 Mg3 128.88(4) . 1_565 ?
O1 Mg2 H1 21.8 . . ?
O2 Mg2 H1 158.0 1_565 . ?
O9 Mg2 H1 111.6 . . ?
O8 Mg2 H1 71.5 . . ?
O10 Mg2 H1 108.0 . . ?
O7 Mg2 H1 68.1 . . ?
Mg1 Mg2 H1 46.0 . . ?
Mg1 Mg2 H1 136.5 1_565 . ?
Mg3 Mg2 H1 43.7 . . ?
Mg3 Mg2 H1 133.7 1_565 . ?
O2 Mg3 O1 84.41(8) . . ?
O2 Mg3 O12 92.96(8) . . ?
O1 Mg3 O12 96.31(9) . . ?
O2 Mg3 O11 93.78(8) . . ?
O1 Mg3 O11 91.22(8) . . ?
O12 Mg3 O11 170.35(10) . . ?
O2 Mg3 O13 92.60(9) . . ?
O1 Mg3 O13 176.90(9) . . ?
O12 Mg3 O13 84.63(9) . . ?
O11 Mg3 O13 88.18(9) . . ?
O2 Mg3 O14 176.20(9) . . ?
O1 Mg3 O14 92.50(9) . . ?
O12 Mg3 O14 89.57(9) . . ?
O11 Mg3 O14 84.06(9) . . ?
O13 Mg3 O14 90.46(9) . . ?
O2 Mg3 Mg1 42.32(6) . . ?
O1 Mg3 Mg1 42.08(6) . . ?
O12 Mg3 Mg1 96.35(7) . . ?
O11 Mg3 Mg1 93.28(7) . . ?
O13 Mg3 Mg1 134.92(7) . . ?
O14 Mg3 Mg1 134.54(7) . . ?
O2 Mg3 Mg2 103.24(6) . . ?
O1 Mg3 Mg2 29.63(5) . . ?
O12 Mg3 Mg2 72.79(7) . . ?
O11 Mg3 Mg2 112.23(7) . . ?
O13 Mg3 Mg2 152.84(7) . . ?
O14 Mg3 Mg2 74.81(7) . . ?
Mg1 Mg3 Mg2 64.33(3) . . ?
O2 Mg3 Mg2 29.72(5) . 1_545 ?
O1 Mg3 Mg2 103.31(6) . 1_545 ?
O12 Mg3 Mg2 112.99(7) . 1_545 ?
O11 Mg3 Mg2 70.84(6) . 1_545 ?
O13 Mg3 Mg2 73.62(6) . 1_545 ?
O14 Mg3 Mg2 150.33(7) . 1_545 ?
Mg1 Mg3 Mg2 64.55(3) . 1_545 ?
Mg2 Mg3 Mg2 128.88(4) . 1_545 ?
Mg2 O1 Mg1 119.77(9) . . ?
Mg2 O1 Mg3 120.59(9) . . ?
Mg1 O1 Mg3 95.75(8) . . ?
Mg2 O1 H1 94.6 . . ?
Mg1 O1 H1 117.4 . . ?
Mg3 O1 H1 110.0 . . ?
Mg2 O2 Mg3 120.57(9) 1_545 . ?
Mg2 O2 Mg1 119.78(9) 1_545 . ?
Mg3 O2 Mg1 95.50(8) . . ?
Mg2 O2 H2 98.1 1_545 . ?
Mg3 O2 H2 106.3 . . ?
Mg1 O2 H2 117.2 . . ?
Mg1 O3 H3B 109.7 . . ?
Mg1 O3 H3C 109.3 . . ?
H3B O3 H3C 109.8 . . ?
C15 O4 Mg1 126.45(18) 1_545 . ?
C14 O5 Mg1 125.17(18) . . ?
Mg1 O6 H6B 109.8 . . ?
Mg1 O6 H6C 109.2 . . ?
H6B O6 H6C 109.8 . . ?
C28 O7 Mg2 133.52(19) . . ?
C15 O8 Mg2 132.49(19) . . ?
C14 O9 Mg2 134.75(19) . . ?
C1 O10 Mg2 135.75(19) . . ?
C28 O11 Mg3 123.88(18) 1_545 . ?
C1 O12 Mg3 125.71(18) . . ?
Mg3 O13 H13B 109.7 . . ?
Mg3 O13 H13C 109.2 . . ?
H13B O13 H13C 109.8 . . ?
C1S O14 Mg3 129.7(2) . . ?
C1S O14 H14A 115.2 . . ?
Mg3 O14 H14A 115.1 . . ?
O12 C1 O10 125.4(3) . . ?
O12 C1 C2 117.6(3) . . ?
O10 C1 C2 117.0(3) . . ?
O14 C1S C2S 117.0(4) . . ?
O14 C1S H1SA 108.0 . . ?
C2S C1S H1SA 108.0 . . ?
O14 C1S H1SB 108.0 . . ?
C2S C1S H1SB 108.0 . . ?
H1SA C1S H1SB 107.3 . . ?
C7 C2 C3 119.5(3) . . ?
C7 C2 C1 120.2(3) . . ?
C3 C2 C1 120.3(3) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.6 . . ?
C4 C5 C6 121.7(3) . . ?
C4 C5 S1 119.7(2) . . ?
C6 C5 S1 118.5(2) . . ?
C5 C6 C7 118.9(3) . . ?
C5 C6 H6A 120.5 . . ?
C7 C6 H6A 120.5 . . ?
C2 C7 C6 120.4(3) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C9 C8 C13 121.6(3) . . ?
C9 C8 S1 119.8(2) . . ?
C13 C8 S1 118.6(2) . . ?
C8 C9 C10 118.9(3) . 2_655 ?
C8 C9 H9A 120.6 . . ?
C10 C9 H9A 120.6 2_655 . ?
C9 C10 C11 120.6(3) 2_655 . ?
C9 C10 H10A 119.7 2_655 . ?
C11 C10 H10A 119.7 . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 C14 120.6(3) . . ?
C10 C11 C14 119.7(3) . . ?
C11 C12 C13 120.8(3) . 2_655 ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 2_655 . ?
C8 C13 C12 118.4(3) . 2_655 ?
C8 C13 H13A 120.8 . . ?
C12 C13 H13A 120.8 2_655 . ?
O5 C14 O9 125.1(3) . . ?
O5 C14 C11 118.2(3) . . ?
O9 C14 C11 116.7(3) . . ?
O4 C15 O8 125.9(2) 1_565 . ?
O4 C15 C16 117.5(3) 1_565 . ?
O8 C15 C16 116.6(3) . . ?
C21 C16 C17 119.7(3) . . ?
C21 C16 C15 119.7(3) . . ?
C17 C16 C15 120.6(3) . . ?
C16 C17 C18 120.7(3) . . ?
C16 C17 H17B 119.7 . . ?
C18 C17 H17B 119.7 . . ?
C17 C18 C19 118.7(3) . . ?
C17 C18 H18B 120.7 . . ?
C19 C18 H18B 120.7 . . ?
C20 C19 C18 121.4(3) . . ?
C20 C19 S2 119.1(3) . . ?
C18 C19 S2 119.5(2) . . ?
C19 C20 C21 118.6(3) . . ?
C19 C20 H20A 120.7 . . ?
C21 C20 H20A 120.7 . . ?
C16 C21 C20 121.0(3) . . ?
C16 C21 H21A 119.5 . . ?
C20 C21 H21A 119.5 . . ?
C27 C22 C23 121.6(3) 2_756 . ?
C27 C22 S2 119.8(3) 2_756 . ?
C23 C22 S2 118.6(2) . . ?
C22 C23 C24 118.7(3) . 2_756 ?
C22 C23 H23A 120.6 . . ?
C24 C23 H23A 120.6 2_756 . ?
C23 C24 C25 120.5(3) 2_756 . ?
C23 C24 H24A 119.8 2_756 . ?
C25 C24 H24A 119.8 . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 C28 121.1(3) . . ?
C24 C25 C28 118.8(3) . . ?
C25 C26 C27 120.3(3) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C22 C27 C26 118.9(3) 2_756 . ?
C22 C27 H27A 120.5 2_756 . ?
C26 C27 H27A 120.5 . . ?
O11 C28 O7 126.0(3) 1_565 . ?
O11 C28 C25 117.9(3) 1_565 . ?
O7 C28 C25 115.9(3) . . ?
H1WA O1W H1WB 107.4 . . ?
H2WA O2W H2WB 108.1 . . ?
O4W O4W H4WA 98.7 2_655 . ?
O4W O4W H4WB 110.1 2_655 . ?
H4WA O4W H4WB 108.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3B O18 0.85 2.06 2.894(3) 168.1 3_756
O3 H3C O9 0.85 1.92 2.760(3) 167.1 1_545
O6 H6B O17 0.85 2.32 3.070(3) 148.1 3_756
O6 H6C O8 0.85 2.00 2.832(3) 165.5 .
O13 H13B O16 0.85 2.09 2.860(3) 150.1 3_656
O13 H13C O10 0.85 1.92 2.758(3) 168.3 1_545
O14 H14A O7 0.85 2.09 2.722(3) 130.6 .
O1W H1WA O11 0.85 2.20 2.758(9) 123.5 .
O1W H1WB O3W 0.85 2.37 3.175(13) 158.8 1_545
O2W H2WA O12 0.85 2.28 2.906(11) 130.5 .
O2W H2WB O4W 0.85 2.26 3.11(2) 173.8 .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.40
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 805748'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H13 Mn O7 S'
_chemical_formula_sum            'C16 H13 Mn O7 S'
_chemical_formula_weight         404.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   10.1610(5)
_cell_length_b                   7.3197(3)
_cell_length_c                   22.3295(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6990(10)
_cell_angle_gamma                90.00
_cell_volume                     1657.31(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.2597
_cell_measurement_theta_max      28.2721

_exptl_crystal_description       lamellar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            14612
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         28.27
_reflns_number_total             4090
_reflns_number_gt                3714
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0517P)²+8.3258P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4090
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1573
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.70056(5) 0.29595(7) 0.24471(2) 0.01028(16) Uani 1 1 d . . .
S2 S 1.25038(9) 0.75112(12) 0.51793(4) 0.01101(19) Uani 1 1 d . . .
C1 C 0.8639(3) 0.4406(5) 0.32900(16) 0.0108(6) Uani 1 1 d . . .
C2 C 0.9556(4) 0.5120(5) 0.37861(16) 0.0121(7) Uani 1 1 d . . .
C3 C 1.0653(4) 0.4090(5) 0.39939(17) 0.0160(7) Uani 1 1 d . . .
H3A H 1.0788 0.2934 0.3836 0.019 Uiso 1 1 calc R . .
C4 C 1.1539(4) 0.4789(5) 0.44347(18) 0.0156(7) Uani 1 1 d . . .
H4A H 1.2280 0.4122 0.4569 0.019 Uiso 1 1 calc R . .
C5 C 1.1298(3) 0.6515(5) 0.46727(15) 0.0107(7) Uani 1 1 d . . .
C6 C 1.0193(4) 0.7520(5) 0.44875(16) 0.0132(7) Uani 1 1 d . . .
H6A H 1.0042 0.8653 0.4658 0.016 Uiso 1 1 calc R . .
C7 C 0.9312(4) 0.6819(5) 0.40443(17) 0.0130(7) Uani 1 1 d . . .
H7A H 0.8561 0.7477 0.3919 0.016 Uiso 1 1 calc R . .
C8 C 1.3600(3) 0.8407(5) 0.46701(16) 0.0116(7) Uani 1 1 d . . .
C9 C 1.4570(4) 0.7272(5) 0.44662(17) 0.0151(7) Uani 1 1 d . . .
H9A H 1.4684 0.6099 0.4621 0.018 Uiso 1 1 calc R . .
C10 C 1.5368(4) 0.7907(5) 0.40294(18) 0.0156(7) Uani 1 1 d . . .
H10A H 1.6024 0.7162 0.3890 0.019 Uiso 1 1 calc R . .
C11 C 1.5179(3) 0.9674(5) 0.37997(16) 0.0106(7) Uani 1 1 d . . .
C12 C 1.4215(4) 1.0804(5) 0.40153(17) 0.0146(7) Uani 1 1 d . . .
H12A H 1.4103 1.1983 0.3866 0.017 Uiso 1 1 calc R . .
C13 C 1.3419(4) 1.0172(5) 0.44531(17) 0.0145(7) Uani 1 1 d . . .
H13A H 1.2773 1.0920 0.4599 0.017 Uiso 1 1 calc R . .
C14 C 0.8967(4) 0.5305(5) 0.16829(16) 0.0122(7) Uani 1 1 d . . .
O1 O 0.7740(3) 0.5452(3) 0.30574(11) 0.0122(5) Uani 1 1 d . . .
O2 O 0.8770(3) 0.2804(3) 0.30994(12) 0.0160(6) Uani 1 1 d . . .
O3 O 0.8001(3) 0.4309(3) 0.17893(12) 0.0145(5) Uani 1 1 d . . .
O4 O 0.9274(3) 0.6773(4) 0.19554(13) 0.0168(6) Uani 1 1 d . . .
O5 O 1.1903(3) 0.9004(4) 0.54813(12) 0.0154(5) Uani 1 1 d . . .
O6 O 1.3171(3) 0.6078(4) 0.55204(12) 0.0162(6) Uani 1 1 d . . .
O1S O 0.5309(3) 0.4400(4) 0.20444(13) 0.0176(6) Uani 1 1 d . . .
C1S C 0.3949(5) 0.4273(7) 0.2173(3) 0.0407(14) Uani 1 1 d . . .
H1SA H 0.3735 0.3009 0.2254 0.049 Uiso 1 1 calc R . .
H1SB H 0.3401 0.4668 0.1825 0.049 Uiso 1 1 calc R . .
C2S C 0.3653(9) 0.5428(10) 0.2705(5) 0.090(3) Uani 1 1 d . . .
H2SA H 0.2743 0.5286 0.2786 0.135 Uiso 1 1 calc R . .
H2SB H 0.3827 0.6687 0.2619 0.135 Uiso 1 1 calc R . .
H2SC H 0.4201 0.5047 0.3049 0.135 Uiso 1 1 calc R . .


_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 O3 2.085(3) . ?
Mn1 O4 2.109(3) 2_645 ?
Mn1 O1S 2.166(3) . ?
Mn1 O1 2.178(2) 2_645 ?
Mn1 O2 2.239(3) . ?
Mn1 O1 2.369(3) . ?
S2 O6 1.440(3) . ?
S2 O5 1.441(3) . ?
S2 C8 1.769(4) . ?
S2 C5 1.770(3) . ?
C1 O2 1.258(4) . ?
C1 O1 1.276(4) . ?
C1 C2 1.495(5) . ?
C2 C3 1.399(5) . ?
C2 C7 1.399(5) . ?
C3 C4 1.389(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.398(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.383(5) . ?
C6 C7 1.389(5) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.388(5) . ?
C8 C13 1.388(5) . ?
C9 C10 1.388(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.401(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.392(5) . ?
C11 C14 1.499(5) 2_755 ?
C12 C13 1.388(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 O3 1.258(4) . ?
C14 O4 1.264(4) . ?
C14 C11 1.499(5) 2_745 ?
O1 Mn1 2.178(2) 2_655 ?
O4 Mn1 2.109(3) 2_655 ?
O1S C1S 1.432(5) . ?
C1S C2S 1.503(10) . ?
C1S H1SA 0.9700 . ?
C1S H1SB 0.9700 . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9600 . ?
C2S H2SC 0.9600 . ?

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
O3 Mn1 O4 170.93(11) . 2_645 ?
O3 Mn1 O1S 83.47(11) . . ?
O4 Mn1 O1S 87.50(11) 2_645 . ?
O3 Mn1 O1 87.46(10) . 2_645 ?
O4 Mn1 O1 94.52(10) 2_645 2_645 ?
O1S Mn1 O1 108.27(10) . 2_645 ?
O3 Mn1 O2 94.46(11) . . ?
O4 Mn1 O2 93.90(11) 2_645 . ?
O1S Mn1 O2 151.31(10) . . ?
O1 Mn1 O2 100.19(10) 2_645 . ?
O3 Mn1 O1 83.76(10) . . ?
O4 Mn1 O1 97.90(10) 2_645 . ?
O1S Mn1 O1 94.39(10) . . ?
O1 Mn1 O1 154.58(4) 2_645 . ?
O2 Mn1 O1 57.01(9) . . ?
O6 S2 O5 120.29(17) . . ?
O6 S2 C8 108.39(17) . . ?
O5 S2 C8 108.86(17) . . ?
O6 S2 C5 108.69(16) . . ?
O5 S2 C5 108.37(17) . . ?
C8 S2 C5 100.41(17) . . ?
O2 C1 O1 120.7(3) . . ?
O2 C1 C2 120.1(3) . . ?
O1 C1 C2 119.2(3) . . ?
C3 C2 C7 120.0(3) . . ?
C3 C2 C1 120.2(3) . . ?
C7 C2 C1 119.8(3) . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 118.7(3) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 S2 119.1(3) . . ?
C4 C5 S2 119.0(3) . . ?
C5 C6 C7 119.4(3) . . ?
C5 C6 H6A 120.3 . . ?
C7 C6 H6A 120.3 . . ?
C6 C7 C2 119.9(3) . . ?
C6 C7 H7A 120.0 . . ?
C2 C7 H7A 120.0 . . ?
C9 C8 C13 121.6(3) . . ?
C9 C8 S2 118.6(3) . . ?
C13 C8 S2 119.6(3) . . ?
C10 C9 C8 119.3(3) . . ?
C10 C9 H9A 120.3 . . ?
C8 C9 H9A 120.3 . . ?
C9 C10 C11 119.6(3) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 C14 121.2(3) . 2_755 ?
C10 C11 C14 118.4(3) . 2_755 ?
C13 C12 C11 120.1(3) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C8 C13 C12 119.1(3) . . ?
C8 C13 H13A 120.5 . . ?
C12 C13 H13A 120.5 . . ?
O3 C14 O4 125.0(4) . . ?
O3 C14 C11 116.9(3) . 2_745 ?
O4 C14 C11 118.2(3) . 2_745 ?
C1 O1 Mn1 127.6(2) . 2_655 ?
C1 O1 Mn1 87.9(2) . . ?
Mn1 O1 Mn1 113.27(11) 2_655 . ?
C1 O2 Mn1 94.3(2) . . ?
C14 O3 Mn1 145.9(2) . . ?
C14 O4 Mn1 120.8(2) . 2_655 ?
C1S O1S Mn1 129.6(3) . . ?
O1S C1S C2S 111.5(5) . . ?
O1S C1S H1SA 109.3 . . ?
C2S C1S H1SA 109.3 . . ?
O1S C1S H1SB 109.3 . . ?
C2S C1S H1SB 109.3 . . ?
H1SA C1S H1SB 108.0 . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.113
_database_code_depnum_ccdc_archive 'CCDC 998723'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H10 Mn O7 S'
_chemical_formula_sum            'C14 H10 Mn O7 S'
_chemical_formula_weight         377.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.9980(2)
_cell_length_b                   11.8959(4)
_cell_length_c                   13.0287(7)
_cell_angle_alpha                112.118(3)
_cell_angle_beta                 102.502(3)
_cell_angle_gamma                99.816(2)
_cell_volume                     807.49(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7926
_cell_measurement_theta_min      3.1280
_cell_measurement_theta_max      28.2539

_exptl_crystal_description       lamellar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             382
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            13815
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         28.30
_reflns_number_total             3960
_reflns_number_gt                3240
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0419P)²+2.0381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3960
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1282
_refine_ls_wR_factor_gt          0.1241
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.73607(8) 0.43540(5) 0.01787(4) 0.01917(14) Uani 1 1 d . . .
S2 S 0.59850(15) 0.74855(8) 0.72547(7) 0.02349(19) Uani 1 1 d . . .
O1S O 0.8198(5) 0.3085(3) 0.0978(2) 0.0375(6) Uani 1 1 d . . .
H1SA H 0.7458 0.3119 0.1473 0.056 Uiso 1 1 d . . .
H1SB H 0.9695 0.3303 0.1320 0.056 Uiso 1 1 d . . .
O1 O 0.3792(5) 0.5978(3) 0.1599(2) 0.0397(7) Uani 1 1 d . . .
O2 O 0.7150(5) 0.5395(3) 0.1902(2) 0.0333(6) Uani 1 1 d . . .
O3 O 1.0484(4) 1.3820(2) 0.9568(2) 0.0274(5) Uani 1 1 d . . .
O4 O 1.3782(4) 1.3196(2) 0.9732(2) 0.0340(6) Uani 1 1 d . . .
O5 O 0.7336(5) 0.6820(2) 0.7748(2) 0.0327(6) Uani 1 1 d . . .
O6 O 0.3605(4) 0.7426(2) 0.7324(2) 0.0336(6) Uani 1 1 d . . .
C1 C 0.5527(6) 0.5822(3) 0.2214(3) 0.0269(7) Uani 1 1 d . . .
C2 C 0.5619(6) 0.6210(3) 0.3477(3) 0.0262(7) Uani 1 1 d . . .
C3 C 0.3882(7) 0.6703(4) 0.3871(3) 0.0345(8) Uani 1 1 d . . .
H3A H 0.2641 0.6780 0.3357 0.041 Uiso 1 1 calc R . .
C4 C 0.3976(7) 0.7084(4) 0.5031(3) 0.0337(8) Uani 1 1 d . . .
H4A H 0.2810 0.7419 0.5299 0.040 Uiso 1 1 calc R . .
C5 C 0.5825(6) 0.6959(3) 0.5778(3) 0.0231(7) Uani 1 1 d . . .
C6 C 0.7575(6) 0.6447(4) 0.5392(3) 0.0299(8) Uani 1 1 d . . .
H6B H 0.8809 0.6363 0.5904 0.036 Uiso 1 1 calc R . .
C7 C 0.7437(6) 0.6066(4) 0.4230(3) 0.0304(8) Uani 1 1 d . . .
H7A H 0.8578 0.5711 0.3955 0.036 Uiso 1 1 calc R . .
C8 C 0.7625(6) 0.9101(3) 0.7911(3) 0.0224(6) Uani 1 1 d . . .
C9 C 0.6453(6) 0.9988(3) 0.7826(3) 0.0332(8) Uani 1 1 d . . .
H9A H 0.4832 0.9741 0.7439 0.040 Uiso 1 1 calc R . .
C10 C 0.7739(6) 1.1247(3) 0.8329(3) 0.0328(8) Uani 1 1 d . . .
H10A H 0.6976 1.1851 0.8278 0.039 Uiso 1 1 calc R . .
C11 C 1.0145(6) 1.1614(3) 0.8905(3) 0.0235(7) Uani 1 1 d . . .
C12 C 1.1289(6) 1.0711(3) 0.8963(3) 0.0322(8) Uani 1 1 d . . .
H12A H 1.2914 1.0958 0.9341 0.039 Uiso 1 1 calc R . .
C13 C 1.0038(6) 0.9444(3) 0.8462(3) 0.0335(8) Uani 1 1 d . . .
H13A H 1.0809 0.8838 0.8497 0.040 Uiso 1 1 calc R . .
C14 C 1.1585(6) 1.2976(3) 0.9449(3) 0.0228(7) 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
Mn1 O1 2.126(2) 2_665 ?
Mn1 O2 2.162(2) . ?
Mn1 O4 2.166(2) 1_444 ?
Mn1 O3 2.195(2) 2_776 ?
Mn1 O1S 2.198(3) . ?
Mn1 O3 2.284(2) 1_544 ?
S2 O5 1.440(3) . ?
S2 O6 1.441(3) . ?
S2 C5 1.760(3) . ?
S2 C8 1.773(3) . ?
O1S H1SA 0.8509 . ?
O1S H1SB 0.8556 . ?
O1 C1 1.256(4) . ?
O1 Mn1 2.126(2) 2_665 ?
O2 C1 1.247(4) . ?
O3 C14 1.273(4) . ?
O3 Mn1 2.195(2) 2_776 ?
O3 Mn1 2.284(2) 1_566 ?
O4 C14 1.241(4) . ?
O4 Mn1 2.166(2) 1_666 ?
C1 C2 1.518(4) . ?
C2 C7 1.381(5) . ?
C2 C3 1.381(5) . ?
C3 C4 1.389(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.378(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.393(5) . ?
C6 C7 1.386(5) . ?
C6 H6B 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C13 1.380(5) . ?
C8 C9 1.389(5) . ?
C9 C10 1.384(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.381(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.386(5) . ?
C11 C14 1.505(4) . ?
C12 C13 1.387(5) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?

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
O1 Mn1 O2 145.25(11) 2_665 . ?
O1 Mn1 O4 82.29(11) 2_665 1_444 ?
O2 Mn1 O4 88.21(10) . 1_444 ?
O1 Mn1 O3 84.25(11) 2_665 2_776 ?
O2 Mn1 O3 84.78(10) . 2_776 ?
O4 Mn1 O3 145.07(10) 1_444 2_776 ?
O1 Mn1 O1S 130.91(11) 2_665 . ?
O2 Mn1 O1S 79.80(10) . . ?
O4 Mn1 O1S 81.33(10) 1_444 . ?
O3 Mn1 O1S 130.47(10) 2_776 . ?
O1 Mn1 O3 78.16(10) 2_665 1_544 ?
O2 Mn1 O3 131.07(10) . 1_544 ?
O4 Mn1 O3 129.72(9) 1_444 1_544 ?
O3 Mn1 O3 77.99(9) 2_776 1_544 ?
O1S Mn1 O3 77.70(9) . 1_544 ?
O5 S2 O6 118.78(16) . . ?
O5 S2 C5 108.76(16) . . ?
O6 S2 C5 107.64(15) . . ?
O5 S2 C8 108.37(16) . . ?
O6 S2 C8 107.82(16) . . ?
C5 S2 C8 104.57(15) . . ?
Mn1 O1S H1SA 110.4 . . ?
Mn1 O1S H1SB 109.7 . . ?
H1SA O1S H1SB 109.2 . . ?
C1 O1 Mn1 134.0(2) . 2_665 ?
C1 O2 Mn1 130.4(2) . . ?
C14 O3 Mn1 114.38(19) . 2_776 ?
C14 O3 Mn1 140.1(2) . 1_566 ?
Mn1 O3 Mn1 102.01(9) 2_776 1_566 ?
C14 O4 Mn1 153.9(2) . 1_666 ?
O2 C1 O1 127.3(3) . . ?
O2 C1 C2 117.6(3) . . ?
O1 C1 C2 115.1(3) . . ?
C7 C2 C3 120.1(3) . . ?
C7 C2 C1 120.0(3) . . ?
C3 C2 C1 119.9(3) . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.6 . . ?
C4 C5 C6 121.5(3) . . ?
C4 C5 S2 118.7(3) . . ?
C6 C5 S2 119.8(3) . . ?
C7 C6 C5 118.6(3) . . ?
C7 C6 H6B 120.7 . . ?
C5 C6 H6B 120.7 . . ?
C2 C7 C6 120.5(3) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C13 C8 C9 121.5(3) . . ?
C13 C8 S2 119.6(3) . . ?
C9 C8 S2 118.9(3) . . ?
C10 C9 C8 118.8(3) . . ?
C10 C9 H9A 120.6 . . ?
C8 C9 H9A 120.6 . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 C14 121.5(3) . . ?
C12 C11 C14 118.8(3) . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C8 C13 C12 118.6(3) . . ?
C8 C13 H13A 120.7 . . ?
C12 C13 H13A 120.7 . . ?
O4 C14 O3 124.4(3) . . ?
O4 C14 C11 117.3(3) . . ?
O3 C14 C11 118.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.095
_database_code_depnum_ccdc_archive 'CCDC 998724'
