# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_compound_II
_database_code_depnum_ccdc_archive 'CCDC 1504134'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Two-dimensional Magnesium Sulfate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H14 Mg3 N2 O16 S3'
_chemical_formula_weight         467.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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           Orthorhombic
_symmetry_space_group_name_H-M   Cmc21

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

_cell_length_a                   18.2294(13)
_cell_length_b                   7.5534(5)
_cell_length_c                   9.8334(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1354.00(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3156
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      40.2

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_process_details   'SADABS Bruker, 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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 SMART APEX CCD diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12786
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         40.16
_reflns_number_total             3156
_reflns_number_gt                2858
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       'SMART, SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_publication_material  'SHELXTLCIF-97 (Sheldrick, 2008)'

_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)+(0.0378P)²+0.2465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_number_reflns         3156
_refine_ls_number_parameters     148
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.083
_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
Mg1 Mg 0.5000 0.79950(8) 0.61012(8) 0.01065(11) Uani 1 2 d S . .
Mg2 Mg 0.58404(3) 0.46502(6) 0.38942(6) 0.01155(9) Uani 1 1 d . . .
S1 S 0.671239(17) 0.69422(4) 0.61894(4) 0.01066(6) Uani 1 1 d . . .
S2 S 0.5000 0.81497(6) 0.28920(4) 0.01018(8) Uani 1 2 d S . .
O1 O 0.5000 0.68770(18) 0.80372(16) 0.0120(2) Uani 1 2 d SD . .
O2 O 0.5000 0.54793(18) 0.52245(15) 0.0118(2) Uani 1 2 d SD . .
O3 O 0.61381(6) 0.83261(13) 0.61235(15) 0.01678(18) Uani 1 1 d . . .
O4 O 0.5000 0.9301(2) 0.16792(16) 0.0152(3) Uani 1 2 d S . .
O5 O 0.5000 0.9232(2) 0.41338(16) 0.0183(3) Uani 1 2 d S . .
O6 O 0.65850(8) 0.58081(18) 0.73801(13) 0.0193(2) Uani 1 1 d . . .
O7 O 0.66917(7) 0.58830(17) 0.49283(13) 0.0179(2) Uani 1 1 d . . .
O8 O 0.56570(7) 0.70150(15) 0.28407(14) 0.0192(2) Uani 1 1 d . . .
O9 O 0.61912(7) 0.23870(17) 0.50131(12) 0.0194(2) Uani 1 1 d D . .
O10 O 0.74312(6) 0.77894(17) 0.63081(15) 0.0213(2) Uani 1 1 d . . .
N1 N 0.80638(11) 0.5421(2) 0.8481(2) 0.0257(3) Uani 1 1 d D . .
H1 H 0.8356(16) 0.493(5) 0.904(4) 0.061(11) Uiso 1 1 d D . .
H2 H 0.771(2) 0.544(5) 0.898(5) 0.062(11) Uiso 1 1 d . . .
H3 H 0.814(2) 0.498(8) 0.768(5) 0.077(13) Uiso 1 1 d . . .
H4 H 0.802(2) 0.654(3) 0.834(6) 0.098(18) Uiso 1 1 d D . .
H5 H 0.5000 0.493(4) 0.591(2) 0.013(7) Uiso 1 2 d SD . .
H6 H 0.5000 0.787(3) 0.839(4) 0.035(11) Uiso 1 2 d SD . .
H10A H 0.5880(12) 0.198(3) 0.553(2) 0.021(6) Uiso 1 1 d D . .
H10B H 0.6503(15) 0.267(5) 0.554(3) 0.062(12) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mg1 0.0132(3) 0.0095(2) 0.0092(3) -0.0001(2) 0.000 0.000
Mg2 0.0126(2) 0.0122(2) 0.00984(18) -0.00093(15) -0.00029(17) 0.00110(15)
S1 0.01062(11) 0.01233(11) 0.00903(10) -0.00021(11) 0.00034(11) -0.00133(9)
S2 0.01361(19) 0.00930(16) 0.00762(15) 0.00111(13) 0.000 0.000
O1 0.0145(6) 0.0109(5) 0.0105(5) 0.0015(4) 0.000 0.000
O2 0.0154(6) 0.0111(5) 0.0090(5) -0.0005(4) 0.000 0.000
O3 0.0152(4) 0.0137(4) 0.0214(5) 0.0010(4) 0.0012(5) 0.0020(3)
O4 0.0235(7) 0.0116(6) 0.0104(6) 0.0038(5) 0.000 0.000
O5 0.0317(9) 0.0134(6) 0.0099(6) -0.0015(4) 0.000 0.000
O6 0.0191(5) 0.0235(5) 0.0154(5) 0.0081(4) 0.0058(4) 0.0036(4)
O7 0.0173(5) 0.0234(6) 0.0131(4) -0.0070(4) -0.0018(4) 0.0006(4)
O8 0.0199(5) 0.0178(5) 0.0198(5) 0.0070(4) 0.0048(4) 0.0072(4)
O9 0.0223(6) 0.0193(5) 0.0167(5) 0.0047(4) -0.0007(4) 0.0005(4)
O10 0.0134(4) 0.0244(5) 0.0262(6) -0.0027(5) 0.0004(5) -0.0068(4)
N1 0.0287(8) 0.0242(7) 0.0243(7) -0.0037(5) -0.0060(6) 0.0045(6)

_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
Mg1 O1 2.0826(17) . ?
Mg1 O2 2.0867(15) . ?
Mg1 O3 2.0897(11) 4_655 ?
Mg1 O3 2.0897(11) . ?
Mg1 O4 2.1202(17) 2_675 ?
Mg1 O5 2.1484(18) . ?
Mg1 Mg2 3.6660(8) 4_655 ?
Mg1 Mg2 3.6660(8) . ?
Mg1 H5 2.33(3) . ?
Mg1 H6 2.26(4) . ?
Mg2 O6 2.0443(13) 3_564 ?
Mg2 O7 2.0759(13) . ?
Mg2 O8 2.0918(12) . ?
Mg2 O1 2.0947(11) 2_664 ?
Mg2 O2 2.1095(11) . ?
Mg2 O9 2.1311(13) . ?
Mg2 Mg2 3.0639(10) 4_655 ?
S1 O10 1.4630(12) . ?
S1 O6 1.4693(12) . ?
S1 O7 1.4762(13) . ?
S1 O3 1.4809(11) . ?
S2 O5 1.4695(16) . ?
S2 O8 1.4737(12) 4_655 ?
S2 O8 1.4737(12) . ?
S2 O4 1.4759(16) . ?
O1 Mg2 2.0947(11) 2_665 ?
O1 Mg2 2.0947(11) 3_565 ?
O1 H6 0.832(19) . ?
O2 Mg2 2.1095(11) 4_655 ?
O2 H5 0.789(18) . ?
O4 Mg1 2.1202(17) 2_674 ?
O6 Mg2 2.0443(13) 3_565 ?
O9 H10A 0.825(17) . ?
O9 H10B 0.796(18) . ?
N1 H1 0.850(19) . ?
N1 H2 0.81(4) . ?
N1 H3 0.86(5) . ?
N1 H4 0.860(19) . ?

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 Mg1 O2 90.48(6) . . ?
O1 Mg1 O3 92.23(4) . 4_655 ?
O2 Mg1 O3 96.51(4) . 4_655 ?
O1 Mg1 O3 92.23(4) . . ?
O2 Mg1 O3 96.51(4) . . ?
O3 Mg1 O3 166.20(7) 4_655 . ?
O1 Mg1 O4 98.37(7) . 2_675 ?
O2 Mg1 O4 171.15(7) . 2_675 ?
O3 Mg1 O4 83.22(3) 4_655 2_675 ?
O3 Mg1 O4 83.22(3) . 2_675 ?
O1 Mg1 O5 178.14(7) . . ?
O2 Mg1 O5 91.38(7) . . ?
O3 Mg1 O5 87.56(4) 4_655 . ?
O3 Mg1 O5 87.56(4) . . ?
O4 Mg1 O5 79.77(7) 2_675 . ?
O1 Mg1 Mg2 105.17(4) . 4_655 ?
O2 Mg1 Mg2 29.29(2) . 4_655 ?
O3 Mg1 Mg2 70.96(4) 4_655 4_655 ?
O3 Mg1 Mg2 120.23(4) . 4_655 ?
O4 Mg1 Mg2 145.35(4) 2_675 4_655 ?
O5 Mg1 Mg2 76.51(4) . 4_655 ?
O1 Mg1 Mg2 105.17(4) . . ?
O2 Mg1 Mg2 29.29(2) . . ?
O3 Mg1 Mg2 120.23(4) 4_655 . ?
O3 Mg1 Mg2 70.96(4) . . ?
O4 Mg1 Mg2 145.35(4) 2_675 . ?
O5 Mg1 Mg2 76.51(4) . . ?
Mg2 Mg1 Mg2 49.401(19) 4_655 . ?
O1 Mg1 H5 70.8(6) . . ?
O2 Mg1 H5 19.7(6) . . ?
O3 Mg1 H5 96.90(3) 4_655 . ?
O3 Mg1 H5 96.90(3) . . ?
O4 Mg1 H5 169.2(6) 2_675 . ?
O5 Mg1 H5 111.0(6) . . ?
Mg2 Mg1 H5 42.6(4) 4_655 . ?
Mg2 Mg1 H5 42.6(4) . . ?
O1 Mg1 H6 21.6(6) . . ?
O2 Mg1 H6 112.1(6) . . ?
O3 Mg1 H6 89.68(9) 4_655 . ?
O3 Mg1 H6 89.68(9) . . ?
O4 Mg1 H6 76.8(6) 2_675 . ?
O5 Mg1 H6 156.5(6) . . ?
Mg2 Mg1 H6 124.3(5) 4_655 . ?
Mg2 Mg1 H6 124.3(5) . . ?
H5 Mg1 H6 92.4(8) . . ?
O6 Mg2 O7 86.35(5) 3_564 . ?
O6 Mg2 O8 83.68(6) 3_564 . ?
O7 Mg2 O8 88.80(6) . . ?
O6 Mg2 O1 95.70(6) 3_564 2_664 ?
O7 Mg2 O1 172.23(6) . 2_664 ?
O8 Mg2 O1 98.87(6) . 2_664 ?
O6 Mg2 O2 169.76(6) 3_564 . ?
O7 Mg2 O2 96.08(5) . . ?
O8 Mg2 O2 86.42(6) . . ?
O1 Mg2 O2 83.22(5) 2_664 . ?
O6 Mg2 O9 92.34(6) 3_564 . ?
O7 Mg2 O9 83.26(6) . . ?
O8 Mg2 O9 171.34(6) . . ?
O1 Mg2 O9 89.16(6) 2_664 . ?
O2 Mg2 O9 97.81(6) . . ?
O6 Mg2 Mg2 131.61(4) 3_564 4_655 ?
O7 Mg2 Mg2 138.38(4) . 4_655 ?
O8 Mg2 Mg2 80.81(4) . 4_655 ?
O1 Mg2 Mg2 43.00(3) 2_664 4_655 ?
O2 Mg2 Mg2 43.43(3) . 4_655 ?
O9 Mg2 Mg2 107.46(4) . 4_655 ?
O6 Mg2 Mg1 145.62(4) 3_564 . ?
O7 Mg2 Mg1 73.34(4) . . ?
O8 Mg2 Mg1 68.77(4) . . ?
O1 Mg2 Mg1 108.19(3) 2_664 . ?
O2 Mg2 Mg1 28.94(3) . . ?
O9 Mg2 Mg1 111.87(4) . . ?
Mg2 Mg2 Mg1 65.299(9) 4_655 . ?
O10 S1 O6 109.45(8) . . ?
O10 S1 O7 109.09(8) . . ?
O6 S1 O7 110.45(7) . . ?
O10 S1 O3 109.15(7) . . ?
O6 S1 O3 109.55(8) . . ?
O7 S1 O3 109.13(7) . . ?
O5 S2 O8 110.61(7) . 4_655 ?
O5 S2 O8 110.61(7) . . ?
O8 S2 O8 108.73(10) 4_655 . ?
O5 S2 O4 110.10(9) . . ?
O8 S2 O4 108.36(6) 4_655 . ?
O8 S2 O4 108.36(6) . . ?
Mg1 O1 Mg2 126.23(5) . 2_665 ?
Mg1 O1 Mg2 126.23(5) . 3_565 ?
Mg2 O1 Mg2 94.00(6) 2_665 3_565 ?
Mg1 O1 H6 91(3) . . ?
Mg2 O1 H6 109(2) 2_665 . ?
Mg2 O1 H6 109(2) 3_565 . ?
Mg1 O2 Mg2 121.77(5) . 4_655 ?
Mg1 O2 Mg2 121.77(5) . . ?
Mg2 O2 Mg2 93.14(6) 4_655 . ?
Mg1 O2 H5 98(2) . . ?
Mg2 O2 H5 111.7(16) 4_655 . ?
Mg2 O2 H5 111.7(15) . . ?
S1 O3 Mg1 128.16(6) . . ?
S2 O4 Mg1 141.64(10) . 2_674 ?
S2 O5 Mg1 120.42(10) . . ?
S1 O6 Mg2 141.64(9) . 3_565 ?
S1 O7 Mg2 132.35(8) . . ?
S2 O8 Mg2 127.55(8) . . ?
Mg2 O9 H10A 114.6(18) . . ?
Mg2 O9 H10B 110(3) . . ?
H10A O9 H10B 101(3) . . ?
H1 N1 H2 96(4) . . ?
H1 N1 H3 109(5) . . ?
H2 N1 H3 134(4) . . ?
H1 N1 H4 126(4) . . ?
H2 N1 H4 90(4) . . ?
H3 N1 H4 104(5) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        40.16
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.093
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound_I
_database_code_depnum_ccdc_archive 'CCDC 1406154'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            'Two-dimensional Cobalt Sulfate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H16 Co3 F2 N2 O14 S3'
_chemical_formula_weight         627.16

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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   10.0475(2)
_cell_length_b                   22.0781(4)
_cell_length_c                   7.26340(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1611.24(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2537
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      30.6

_exptl_crystal_description       Block
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1252
_exptl_absorpt_coefficient_mu    3.545
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4983
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS Bruker, 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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 SMART APEX CCD diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29917
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         30.56
_reflns_number_total             2537
_reflns_number_gt                2363
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       'SMART, SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_publication_material  'SHELXTLCIF-97 (Sheldrick, 2008)'

_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)+(0.0286P)²+0.8291P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2537
_refine_ls_number_parameters     144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0508
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
Co1 Co 0.823559(17) 0.323151(8) 0.21226(2) 0.01337(6) Uani 1 1 d . . .
Co2 Co 0.60226(2) 0.2500 0.53809(3) 0.01269(6) Uani 1 2 d S . .
S1 S 0.58726(3) 0.392783(14) 0.44128(4) 0.01362(7) Uani 1 1 d . . .
S2 S 0.92042(4) 0.2500 0.56554(6) 0.01366(9) Uani 1 2 d S . .
F1 F 0.42104(11) 0.2500 0.40791(16) 0.0161(2) Uani 1 2 d S . .
F2 F 0.69799(11) 0.2500 0.28468(15) 0.0156(2) Uani 1 2 d S . .
O1 O 0.70074(13) 0.38917(5) 0.31190(18) 0.0303(3) Uani 1 1 d . . .
O2 O 0.92719(11) 0.30542(5) 0.45212(14) 0.0211(2) Uani 1 1 d . . .
O3 O 0.46311(12) 0.39178(5) 0.33107(17) 0.0272(2) Uani 1 1 d . . .
O4 O 0.73042(15) 0.33515(6) -0.04402(18) 0.0275(3) Uani 1 1 d . . .
O5 O 0.58910(12) 0.34052(5) 0.56857(15) 0.0241(2) Uani 1 1 d . . .
O6 O 1.03702(14) 0.2500 0.6869(2) 0.0234(3) Uani 1 2 d S . .
O7 O 0.79576(14) 0.2500 0.6740(2) 0.0194(3) Uani 1 2 d S . .
O8 O 0.59669(11) 0.44794(5) 0.54751(15) 0.0233(2) Uani 1 1 d . . .
N1 N 0.46390(14) 0.56014(6) 0.0580(2) 0.0263(3) Uani 1 1 d . . .
H2 H 0.4755 0.5814 -0.0464 0.032 Uiso 1 1 calc R . .
H1 H 0.4360 0.5859 0.1461 0.032 Uiso 1 1 calc R . .
C1 C 0.59318(15) 0.53252(8) 0.1146(2) 0.0265(3) Uani 1 1 d . . .
H6 H 0.5825 0.5122 0.2321 0.032 Uiso 1 1 calc R . .
H5 H 0.6595 0.5641 0.1294 0.032 Uiso 1 1 calc R . .
C2 C 0.36008(16) 0.51232(8) 0.0274(2) 0.0279(3) Uani 1 1 d . . .
H4 H 0.2781 0.5311 -0.0137 0.033 Uiso 1 1 calc R . .
H3 H 0.3422 0.4915 0.1423 0.033 Uiso 1 1 calc R . .
H8 H 0.667(5) 0.3202(19) -0.039(6) 0.108(17) Uiso 1 1 d . . .
H7 H 0.777(3) 0.3201(14) -0.133(5) 0.067(9) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01400(9) 0.01328(9) 0.01283(10) 0.00002(6) 0.00119(6) -0.00021(6)
Co2 0.01144(11) 0.01596(12) 0.01068(12) 0.000 0.00035(8) 0.000
S1 0.01411(14) 0.01306(14) 0.01368(14) -0.00196(10) -0.00004(10) -0.00005(10)
S2 0.01146(18) 0.0193(2) 0.01023(19) 0.000 -0.00175(14) 0.000
F1 0.0144(5) 0.0174(5) 0.0165(5) 0.000 -0.0037(4) 0.000
F2 0.0135(5) 0.0181(5) 0.0153(5) 0.000 0.0020(4) 0.000
O1 0.0322(6) 0.0209(5) 0.0377(7) -0.0007(5) 0.0200(5) 0.0046(4)
O2 0.0256(5) 0.0215(5) 0.0162(5) 0.0039(4) -0.0049(4) -0.0055(4)
O3 0.0263(5) 0.0205(5) 0.0347(6) 0.0038(4) -0.0158(5) -0.0059(4)
O4 0.0352(7) 0.0255(6) 0.0219(6) -0.0047(4) -0.0104(5) 0.0048(5)
O5 0.0360(6) 0.0181(5) 0.0182(5) 0.0032(4) -0.0029(4) 0.0010(4)
O6 0.0157(6) 0.0399(9) 0.0147(7) 0.000 -0.0067(5) 0.000
O7 0.0142(6) 0.0294(8) 0.0146(6) 0.000 0.0019(5) 0.000
O8 0.0269(5) 0.0179(5) 0.0250(6) -0.0091(4) -0.0009(4) -0.0003(4)
N1 0.0269(6) 0.0252(6) 0.0267(7) 0.0010(5) 0.0013(5) 0.0006(5)
C1 0.0201(6) 0.0351(9) 0.0242(7) -0.0004(6) -0.0001(5) -0.0043(6)
C2 0.0194(6) 0.0345(8) 0.0297(8) 0.0003(6) 0.0031(6) -0.0020(6)

_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
Co1 O1 2.0423(11) . ?
Co1 O2 2.0671(10) . ?
Co1 F1 2.0807(7) 6_656 ?
Co1 O3 2.0882(11) 6_656 ?
Co1 O4 2.1002(12) . ?
Co1 F2 2.1159(7) . ?
Co2 O5 2.0150(12) 7_565 ?
Co2 O5 2.0150(12) . ?
Co2 F1 2.0518(11) . ?
Co2 F2 2.0768(11) . ?
Co2 O6 2.1022(14) 6_557 ?
Co2 O7 2.1804(14) . ?
S1 O8 1.4447(11) . ?
S1 O5 1.4787(11) . ?
S1 O1 1.4797(11) . ?
S1 O3 1.4823(11) . ?
S2 O6 1.4662(14) . ?
S2 O2 1.4766(11) 7_565 ?
S2 O2 1.4766(11) . ?
S2 O7 1.4796(14) . ?
F1 Co1 2.0807(7) 4_455 ?
F1 Co1 2.0807(7) 6_556 ?
F2 Co1 2.1159(7) 7_565 ?
O3 Co1 2.0882(11) 6_556 ?
O6 Co2 2.1022(14) 6_657 ?
N1 C1 1.493(2) . ?
N1 C2 1.501(2) . ?
C1 C2 1.505(2) 5_665 ?
C2 C1 1.505(2) 5_665 ?

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 Co1 O2 98.10(5) . . ?
O1 Co1 F1 170.76(5) . 6_656 ?
O2 Co1 F1 88.25(5) . 6_656 ?
O1 Co1 O3 86.63(5) . 6_656 ?
O2 Co1 O3 85.77(5) . 6_656 ?
F1 Co1 O3 100.60(4) 6_656 6_656 ?
O1 Co1 O4 87.41(5) . . ?
O2 Co1 O4 174.48(5) . . ?
F1 Co1 O4 86.32(5) 6_656 . ?
O3 Co1 O4 94.25(6) 6_656 . ?
O1 Co1 F2 95.53(4) . . ?
O2 Co1 F2 86.92(4) . . ?
F1 Co1 F2 78.02(3) 6_656 . ?
O3 Co1 F2 172.60(5) 6_656 . ?
O4 Co1 F2 92.92(5) . . ?
O5 Co2 O5 165.30(7) 7_565 . ?
O5 Co2 F1 89.56(3) 7_565 . ?
O5 Co2 F1 89.56(3) . . ?
O5 Co2 F2 97.34(3) 7_565 . ?
O5 Co2 F2 97.34(3) . . ?
F1 Co2 F2 90.15(5) . . ?
O5 Co2 O6 82.83(3) 7_565 6_557 ?
O5 Co2 O6 82.83(3) . 6_557 ?
F1 Co2 O6 99.27(5) . 6_557 ?
F2 Co2 O6 170.58(5) . 6_557 ?
O5 Co2 O7 90.50(3) 7_565 . ?
O5 Co2 O7 90.50(3) . . ?
F1 Co2 O7 179.48(5) . . ?
F2 Co2 O7 89.33(5) . . ?
O6 Co2 O7 81.25(6) 6_557 . ?
O8 S1 O5 108.85(7) . . ?
O8 S1 O1 109.52(7) . . ?
O5 S1 O1 110.21(7) . . ?
O8 S1 O3 110.87(7) . . ?
O5 S1 O3 109.66(7) . . ?
O1 S1 O3 107.74(8) . . ?
O6 S2 O2 107.38(5) . 7_565 ?
O6 S2 O2 107.38(5) . . ?
O2 S2 O2 111.91(9) 7_565 . ?
O6 S2 O7 110.87(9) . . ?
O2 S2 O7 109.64(5) 7_565 . ?
O2 S2 O7 109.64(5) . . ?
Co2 F1 Co1 127.67(3) . 4_455 ?
Co2 F1 Co1 127.67(3) . 6_556 ?
Co1 F1 Co1 101.83(5) 4_455 6_556 ?
Co2 F2 Co1 119.77(4) . 7_565 ?
Co2 F2 Co1 119.77(4) . . ?
Co1 F2 Co1 99.51(5) 7_565 . ?
S1 O1 Co1 136.81(8) . . ?
S2 O2 Co1 127.16(7) . . ?
S1 O3 Co1 131.09(7) . 6_556 ?
S1 O5 Co2 134.92(7) . . ?
S2 O6 Co2 145.13(10) . 6_657 ?
S2 O7 Co2 120.92(8) . . ?
C1 N1 C2 111.00(13) . . ?
N1 C1 C2 110.59(13) . 5_665 ?
N1 C2 C1 110.33(13) . 5_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.56
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.085
