# 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_mo_ss1900_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1401089'
_audit_update_record             
;
2015-05-15 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Co Na2 O14, 2(H2O)'
_chemical_formula_sum            'C4 H12 Co Na2 O16'
_chemical_formula_weight         421.041

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.7969(6)
_cell_length_b                   6.9292(6)
_cell_length_c                   8.8126(8)
_cell_angle_alpha                86.786(3)
_cell_angle_beta                 67.652(3)
_cell_angle_gamma                89.192(3)
_cell_volume                     383.26(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.96

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             205
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_process_details   multi-scan

_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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1565
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         26.36
_reflns_number_total             1565
_reflns_number_gt                1556
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0639P)²+0.2764P] 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         1565
_refine_ls_number_parameters     114
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0997
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.109
_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
Co1 Co 1.0000 0.0000 0.0000 0.02285(17) Uani 1 2 d SU . .
O2 O 0.8301(3) 0.0482(2) 0.24556(18) 0.0280(4) Uani 1 1 d U . .
O3 O 0.7969(3) 0.2605(2) 0.43452(18) 0.0291(4) Uani 1 1 d U . .
O1 O 1.1358(3) 0.2596(2) 0.02096(18) 0.0291(4) Uani 1 1 d U . .
O4 O 1.1349(3) 0.4641(2) 0.2081(2) 0.0316(4) Uani 1 1 d U . .
O7 O 0.7575(3) 0.7338(2) 0.4785(2) 0.0338(4) Uani 1 1 d U . .
O5 O 1.2333(3) -0.1560(3) 0.0566(3) 0.0399(4) Uani 1 1 d U . .
H5 H 1.2548 -0.1051 0.1307 0.060 Uiso 1 1 calc R . .
C2 C 0.8807(3) 0.2012(3) 0.2947(2) 0.0218(4) Uani 1 1 d U . .
C1 C 1.0671(3) 0.3208(3) 0.1633(2) 0.0223(4) Uani 1 1 d U . .
O9 O 0.3793(3) 0.9932(3) 0.2795(3) 0.0421(4) Uani 1 1 d . . .
O10 O 0.4496(4) 0.4799(4) 0.7760(3) 0.0562(7) Uani 1 1 d U . .
Na1 Na 1.0000 0.5000 0.5000 0.0296(3) Uani 1 2 d SU . .
Na2 Na 0.5000 0.5000 0.5000 0.0299(3) Uani 1 2 d SU . .
H10W H 0.373(7) 0.439(6) 0.844(5) 0.061(12) 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 0.0291(2) 0.0203(2) 0.0165(2) -0.00380(15) -0.00514(17) -0.00581(15)
O2 0.0355(8) 0.0245(7) 0.0196(7) -0.0035(6) -0.0048(6) -0.0112(6)
O3 0.0333(8) 0.0309(8) 0.0193(7) -0.0071(6) -0.0049(6) -0.0040(6)
O1 0.0364(8) 0.0269(8) 0.0188(7) -0.0037(6) -0.0038(6) -0.0122(6)
O4 0.0410(9) 0.0264(8) 0.0262(8) -0.0049(6) -0.0103(7) -0.0128(7)
O7 0.0400(9) 0.0274(8) 0.0327(9) 0.0022(7) -0.0127(7) -0.0033(7)
O5 0.0512(11) 0.0322(9) 0.0469(11) -0.0075(8) -0.0298(9) 0.0024(8)
C2 0.0243(9) 0.0211(9) 0.0191(9) -0.0017(7) -0.0072(8) -0.0031(7)
C1 0.0255(9) 0.0208(9) 0.0200(9) -0.0008(7) -0.0078(8) -0.0041(7)
O9 0.0394(10) 0.0421(10) 0.0463(11) -0.0084(8) -0.0170(9) -0.0029(8)
O10 0.0503(12) 0.0854(18) 0.0288(10) 0.0185(10) -0.0123(9) -0.0297(12)
Na1 0.0342(7) 0.0306(7) 0.0280(6) -0.0104(5) -0.0151(5) 0.0012(5)
Na2 0.0290(6) 0.0333(7) 0.0262(6) 0.0001(5) -0.0092(5) -0.0044(5)

_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 O2 2.0731(15) 2_755 ?
Co1 O2 2.0731(15) . ?
Co1 O1 2.0824(15) 2_755 ?
Co1 O1 2.0824(15) . ?
Co1 O5 2.1030(18) 2_755 ?
Co1 O5 2.1030(18) . ?
O2 C2 1.267(3) . ?
O3 C2 1.236(3) . ?
O3 Na1 2.4020(16) . ?
O3 Na2 2.5074(17) . ?
O1 C1 1.257(3) . ?
O4 C1 1.244(3) . ?
O4 Na1 2.4068(16) . ?
O7 Na1 2.3464(17) . ?
O7 Na2 2.3486(17) . ?
C2 C1 1.562(3) . ?
O10 Na2 2.320(2) . ?
Na1 O7 2.3464(17) 2_766 ?
Na1 O3 2.4020(16) 2_766 ?
Na1 O4 2.4069(16) 2_766 ?
Na1 Na2 3.3984(3) 1_655 ?
Na1 Na2 3.3984(3) . ?
Na2 O10 2.320(2) 2_666 ?
Na2 O7 2.3486(17) 2_666 ?
Na2 O3 2.5074(17) 2_666 ?
Na2 Na1 3.3985(3) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O2 180.0 2_755 . ?
O2 Co1 O1 79.19(6) 2_755 2_755 ?
O2 Co1 O1 100.81(6) . 2_755 ?
O2 Co1 O1 100.80(6) 2_755 . ?
O2 Co1 O1 79.19(6) . . ?
O1 Co1 O1 180.0 2_755 . ?
O2 Co1 O5 91.64(7) 2_755 2_755 ?
O2 Co1 O5 88.36(7) . 2_755 ?
O1 Co1 O5 90.48(7) 2_755 2_755 ?
O1 Co1 O5 89.52(7) . 2_755 ?
O2 Co1 O5 88.36(7) 2_755 . ?
O2 Co1 O5 91.64(7) . . ?
O1 Co1 O5 89.52(7) 2_755 . ?
O1 Co1 O5 90.48(7) . . ?
O5 Co1 O5 180.0 2_755 . ?
C2 O2 Co1 114.93(13) . . ?
C2 O3 Na1 114.92(13) . . ?
C2 O3 Na2 120.52(14) . . ?
Na1 O3 Na2 87.59(5) . . ?
C1 O1 Co1 114.75(13) . . ?
C1 O4 Na1 115.51(14) . . ?
Na1 O7 Na2 92.75(6) . . ?
O3 C2 O2 125.84(19) . . ?
O3 C2 C1 118.86(18) . . ?
O2 C2 C1 115.30(17) . . ?
O4 C1 O1 126.30(19) . . ?
O4 C1 C2 118.07(18) . . ?
O1 C1 C2 115.63(17) . . ?
O7 Na1 O7 180.00(9) 2_766 . ?
O7 Na1 O3 88.68(6) 2_766 2_766 ?
O7 Na1 O3 91.32(6) . 2_766 ?
O7 Na1 O3 91.32(6) 2_766 . ?
O7 Na1 O3 88.68(6) . . ?
O3 Na1 O3 180.0 2_766 . ?
O7 Na1 O4 89.15(6) 2_766 . ?
O7 Na1 O4 90.85(6) . . ?
O3 Na1 O4 110.37(5) 2_766 . ?
O3 Na1 O4 69.63(5) . . ?
O7 Na1 O4 90.85(6) 2_766 2_766 ?
O7 Na1 O4 89.15(6) . 2_766 ?
O3 Na1 O4 69.63(5) 2_766 2_766 ?
O3 Na1 O4 110.37(5) . 2_766 ?
O4 Na1 O4 180.000(1) . 2_766 ?
O7 Na1 Na2 43.65(4) 2_766 1_655 ?
O7 Na1 Na2 136.35(4) . 1_655 ?
O3 Na1 Na2 47.49(4) 2_766 1_655 ?
O3 Na1 Na2 132.51(4) . 1_655 ?
O4 Na1 Na2 91.55(4) . 1_655 ?
O4 Na1 Na2 88.45(4) 2_766 1_655 ?
O7 Na1 Na2 136.35(4) 2_766 . ?
O7 Na1 Na2 43.65(4) . . ?
O3 Na1 Na2 132.51(4) 2_766 . ?
O3 Na1 Na2 47.49(4) . . ?
O4 Na1 Na2 88.45(4) . . ?
O4 Na1 Na2 91.55(4) 2_766 . ?
Na2 Na1 Na2 180.0 1_655 . ?
O10 Na2 O10 180.0 . 2_666 ?
O10 Na2 O7 84.02(7) . . ?
O10 Na2 O7 95.98(7) 2_666 . ?
O10 Na2 O7 95.98(7) . 2_666 ?
O10 Na2 O7 84.02(7) 2_666 2_666 ?
O7 Na2 O7 180.0 . 2_666 ?
O10 Na2 O3 91.37(8) . . ?
O10 Na2 O3 88.63(8) 2_666 . ?
O7 Na2 O3 86.16(6) . . ?
O7 Na2 O3 93.84(6) 2_666 . ?
O10 Na2 O3 88.63(8) . 2_666 ?
O10 Na2 O3 91.37(8) 2_666 2_666 ?
O7 Na2 O3 93.84(6) . 2_666 ?
O7 Na2 O3 86.16(6) 2_666 2_666 ?
O3 Na2 O3 180.00(6) . 2_666 ?
O10 Na2 Na1 104.49(6) . 1_455 ?
O10 Na2 Na1 75.51(6) 2_666 1_455 ?
O7 Na2 Na1 136.40(4) . 1_455 ?
O7 Na2 Na1 43.60(4) 2_666 1_455 ?
O3 Na2 Na1 135.08(4) . 1_455 ?
O3 Na2 Na1 44.92(4) 2_666 1_455 ?
O10 Na2 Na1 75.51(6) . . ?
O10 Na2 Na1 104.49(6) 2_666 . ?
O7 Na2 Na1 43.60(4) . . ?
O7 Na2 Na1 136.40(4) 2_666 . ?
O3 Na2 Na1 44.92(4) . . ?
O3 Na2 Na1 135.08(4) 2_666 . ?
Na1 Na2 Na1 180.0 1_455 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.123
