# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1553050'
_audit_update_record             
;
2017-05-30 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Nickel 5-sulphoisophthalate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H19 Na Ni3 O21 S2'
_chemical_formula_weight         810.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0133 0.0073 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Na Na 0.0434 0.0300 'Calculated using XDISP in WinGX (Farrugia, 1999)'
S S 0.1434 0.1473 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ni Ni 0.3222 1.3014 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8590(11)
_cell_length_b                   11.0355(13)
_cell_length_c                   12.5671(14)
_cell_angle_alpha                104.782(2)
_cell_angle_beta                 89.974(2)
_cell_angle_gamma                109.954(2)
_cell_volume                     1237.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    4714
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      30.75

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_F_000             820
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.009
_exptl_absorpt_coefficient_mu    3.119
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5594
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'sadabs (G.M. Sheldrick)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Ligth Source, station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            13217
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.224
_diffrn_reflns_theta_max         30.809
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5909
_reflns_number_gt                4050
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          .
_vrf_PLAT430_shelx               
;           
PROBLEM: Short Inter D...A Contact  O2WA   ..  O5W     ..  
         2.50 Ang.  
RESPONSE: The water molecules (O2WA and B) are disordered and not 
          fully occupied. - - For the short O5W - O14 distance, 
          it does look like a hydrogen bond would form here but 
          the hydrogens were not modelled.
;
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ
         Please Check
RESPONSE: Hydrogens attached to disordered water molecules 
          were not included in the model but were included in the 
          SumFormula
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: O5W is a bound water molecule whose Hydrogens have not 
          been modelled.
;
_vrf_PLAT906_shelx               
;
PROBLEM: Large K value in the Analysis of Variance ......      3.379 Check 
RESPONSE: The most common place for a high value of K is in the 
          lowest-intensity bin in the table. Almost all area detector 
          integration programs end up slightly underestimating the 
          background, resulting in overestimated values of Fo, thus 
          the high value of Fo/Fc. This is most obvious in the weakest 
          intensities, since the small addition to Fo becomes 
          insignificant in the ratio when Fo is large.
;
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Residual Density  0.98A From     O4W       0.69 eA-3  
RESPONSE: O4W does not have it's hydrogen's modelled, this residual
          denisty is from them.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+0.0921P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5909
_refine_ls_number_parameters     398
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1172
_refine_ls_wR_factor_gt          0.1037
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.013
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1816(5) 0.5446(4) 0.0032(4) 0.0161(9) Uani 1 1 d . . . . .
C2 C 0.1956(5) -0.3259(5) 0.0609(4) 0.0165(9) Uani 1 1 d . . . . .
H2 H 0.2187 -0.2971 0.1371 0.020 Uiso 1 1 calc R U . . .
C3 C 0.1751(5) -0.2389(4) 0.0046(4) 0.0160(9) Uani 1 1 d . . . . .
C4 C 0.1457(5) -0.2809(4) -0.1096(4) 0.0167(10) Uani 1 1 d . . . . .
H4 H 0.1322 -0.2231 -0.1476 0.020 Uiso 1 1 calc R U . . .
C5 C -0.1365(5) 0.4092(4) 0.1671(4) 0.0150(9) Uani 1 1 d . . . . .
C6 C 0.1531(5) 0.5028(4) -0.1106(4) 0.0160(9) Uani 1 1 d . . . . .
H6 H 0.1451 0.4163 -0.1492 0.019 Uiso 1 1 calc R U . . .
C7 C 0.1859(5) 0.4420(4) 0.0635(4) 0.0164(10) Uani 1 1 d . . . . .
C8 C 0.1804(5) -0.1008(4) 0.0618(4) 0.0153(9) Uani 1 1 d . . . . .
C9 C 0.5764(5) 0.5963(5) 0.2713(4) 0.0184(10) Uani 1 1 d . . . . .
C10 C 0.3890(5) 0.3818(5) 0.6175(4) 0.0185(10) Uani 1 1 d . . . . .
H10 H 0.4194 0.4532 0.5861 0.022 Uiso 1 1 calc R U . . .
C11 C 0.3102(5) 0.2557(4) 0.5523(4) 0.0167(10) Uani 1 1 d . . . . .
C12 C 0.2664(5) 0.1481(5) 0.5990(4) 0.0206(10) Uani 1 1 d . . . . .
H12 H 0.2175 0.0616 0.5552 0.025 Uiso 1 1 calc R U . . .
C13 C 0.2965(5) 0.1719(4) -0.2895(4) 0.0173(10) Uani 1 1 d . . . . .
C14 C 0.6259(5) 0.7003(5) 0.2225(4) 0.0197(10) Uani 1 1 d . . . . .
H14 H 0.6080 0.6854 0.1467 0.024 Uiso 1 1 calc R U . . .
C15 C 0.4923(5) 0.4569(4) 0.2028(4) 0.0171(10) Uani 1 1 d . . . . .
C16 C 0.2716(5) 0.2382(4) 0.4324(4) 0.0181(10) Uani 1 1 d . . . . .
Na1 Na -0.0568(3) 0.2590(2) 0.4692(2) 0.0422(6) Uani 1 1 d . . . . .
Ni1 Ni 0.12779(6) 0.14294(5) 0.01822(5) 0.01358(14) Uani 1 1 d . . . . .
Ni2 Ni 0.33378(6) 0.16889(6) 0.20345(5) 0.01467(14) Uani 1 1 d . . . . .
Ni3 Ni 0.20159(6) 0.38479(6) 0.28372(5) 0.01506(15) Uani 1 1 d . . . . .
O1 O 0.1592(4) 0.3254(3) 0.0030(3) 0.0194(7) Uani 1 1 d . . . . .
O2 O 0.2085(4) 0.4818(3) 0.1673(3) 0.0211(8) Uani 1 1 d . . . . .
O3 O 0.0980(3) -0.0562(3) 0.0155(3) 0.0149(7) Uani 1 1 d . . . . .
O4 O 0.2663(4) -0.0342(3) 0.1451(3) 0.0210(8) Uani 1 1 d . . . . .
O5 O 0.4116(3) 0.3767(3) 0.2548(3) 0.0150(7) Uani 1 1 d . . . . .
O6 O 0.5058(4) 0.4269(3) 0.1024(3) 0.0255(8) Uani 1 1 d . . . . .
O7 O 0.3132(4) 0.1595(3) 0.3612(3) 0.0226(8) Uani 1 1 d . . . . .
O8 O 0.2012(4) 0.3072(3) 0.4153(3) 0.0214(7) Uani 1 1 d . . . . .
O9 O 0.1246(4) 0.0764(3) -0.1533(3) 0.0237(8) Uani 1 1 d . . . . .
O10 O 0.3502(4) 0.0331(4) -0.1666(3) 0.0280(8) Uani 1 1 d . . . . .
O11 O 0.1541(5) -0.0810(3) -0.3143(3) 0.0370(11) Uani 1 1 d . . . . .
O12 O -0.0027(4) 0.3848(3) 0.3318(3) 0.0209(7) Uani 1 1 d . . . . .
O13 O -0.2386(4) 0.3966(4) 0.3566(3) 0.0257(8) Uani 1 1 d . . . . .
O14 O 0.0376(4) 0.4028(3) 0.6488(3) 0.0281(9) Uani 1 1 d . . . . .
O15 O 0.1395(3) 0.1948(3) 0.1826(3) 0.0144(7) Uani 1 1 d . . . . .
H15 H 0.0606 0.1322 0.2104 0.017 Uiso 1 1 calc R U . . .
O1W O 0.3498(4) 0.1850(3) 0.0406(3) 0.0180(7) Uani 1 1 d D . . . .
O2WB O -0.3401(17) 0.1751(14) 0.4973(13) 0.070 Uiso 0.431(10) 1 d . U P . .
O2WA O -0.2675(13) 0.1860(10) 0.5509(10) 0.070 Uiso 0.569(10) 1 d . U P . .
O3W O 0.5418(4) 0.1747(4) 0.2191(4) 0.0322(9) Uani 1 1 d D . . . .
O4W O 0.2880(4) 0.5634(4) 0.4067(3) 0.0311(9) Uani 1 1 d . . . . .
O5W O -0.0840(9) 0.1202(8) 0.6366(8) 0.141(4) Uani 1 1 d . . . . .
OSA O 0.434(2) -0.041(2) 0.343(2) 0.050 Uiso 0.231(13) 1 d . U . A 1
OSB O 0.4789(14) 0.0139(14) 0.3974(12) 0.050 Uiso 0.424(12) 1 d . U . B 2
S1 S 0.22667(14) 0.03928(11) -0.22742(10) 0.0188(3) Uani 1 1 d . . . . .
S2 S -0.10099(13) 0.45292(11) 0.31197(10) 0.0171(2) Uani 1 1 d . . . . .
H1A H 0.401(5) 0.2724(13) 0.051(4) 0.020 Uiso 1 1 d D U . . .
H1B H 0.370(5) 0.137(3) -0.023(2) 0.020 Uiso 1 1 d D U . . .
H3A H 0.572(5) 0.105(3) 0.204(4) 0.020 Uiso 1 1 d D U . . .
H3B H 0.608(4) 0.245(3) 0.268(3) 0.020 Uiso 1 1 d D U . . .


_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
C1 C6 1.384(7) . ?
C1 C2 1.387(6) 1_565 ?
C1 C7 1.526(6) . ?
C2 C1 1.387(6) 1_545 ?
C2 C3 1.394(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(6) . ?
C3 C8 1.493(6) . ?
C4 C5 1.387(6) 2 ?
C4 H4 0.9300 . ?
C5 C4 1.387(6) 2 ?
C5 C6 1.390(6) 2_565 ?
C5 S2 1.763(5) . ?
C6 C5 1.390(6) 2_565 ?
C6 H6 0.9300 . ?
C7 O1 1.253(5) . ?
C7 O2 1.259(6) . ?
C8 O4 1.240(5) . ?
C8 O3 1.288(5) . ?
C9 C10 1.378(7) 2_666 ?
C9 C14 1.382(6) . ?
C9 C15 1.500(6) . ?
C10 C11 1.375(6) . ?
C10 C9 1.378(7) 2_666 ?
C10 H10 0.9300 . ?
C11 C12 1.396(6) . ?
C11 C16 1.501(7) . ?
C12 C13 1.371(7) 1_556 ?
C12 H12 0.9300 . ?
C13 C12 1.372(7) 1_554 ?
C13 C14 1.393(6) 2_665 ?
C13 S1 1.766(4) . ?
C14 C13 1.393(6) 2_665 ?
C14 H14 0.9300 . ?
C15 O6 1.239(6) . ?
C15 O5 1.288(5) . ?
C16 O8 1.247(6) . ?
C16 O7 1.253(6) . ?
Na1 O2WA 2.301(11) . ?
Na1 O11 2.309(4) 2 ?
Na1 O14 2.376(4) . ?
Na1 O12 2.431(4) . ?
Na1 O8 2.544(4) . ?
Na1 O2WB 2.681(15) . ?
Na1 O5W 2.864(10) . ?
Na1 S2 3.387(3) . ?
Ni1 O1 1.990(3) . ?
Ni1 O15 1.990(3) . ?
Ni1 O1W 2.080(3) . ?
Ni1 O9 2.089(4) . ?
Ni1 O3 2.095(3) 2 ?
Ni1 O3 2.106(3) . ?
Ni1 Ni2 2.9820(9) . ?
Ni2 O7 2.018(3) . ?
Ni2 O4 2.037(3) . ?
Ni2 O3W 2.038(4) . ?
Ni2 O15 2.058(3) . ?
Ni2 O5 2.076(3) . ?
Ni2 O1W 2.100(3) . ?
Ni3 O2 2.010(3) . ?
Ni3 O15 2.037(3) . ?
Ni3 O8 2.046(3) . ?
Ni3 O4W 2.074(4) . ?
Ni3 O12 2.103(3) . ?
Ni3 O5 2.129(3) . ?
O3 Ni1 2.095(3) 2 ?
O9 S1 1.460(4) . ?
O10 S1 1.468(4) . ?
O11 S1 1.442(4) . ?
O11 Na1 2.309(4) 2 ?
O12 S2 1.470(3) . ?
O13 S2 1.464(4) . ?
O14 S2 1.445(3) 2_566 ?
O15 H15 0.9800 . ?
O1W H1A 0.898(10) . ?
O1W H1B 0.898(10) . ?
O2WB O2WA 0.939(15) . ?
O3W H3A 0.895(10) . ?
O3W H3B 0.901(10) . ?
S2 O14 1.445(3) 2_566 ?

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
C6 C1 C2 120.3(4) . 1_565 ?
C6 C1 C7 118.3(4) . . ?
C2 C1 C7 121.3(4) 1_565 . ?
C1 C2 C3 120.0(4) 1_545 . ?
C1 C2 H2 120.0 1_545 . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 C8 117.3(4) . . ?
C2 C3 C8 123.0(4) . . ?
C5 C4 C3 119.9(4) 2 . ?
C5 C4 H4 120.0 2 . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.3(4) 2 2_565 ?
C4 C5 S2 116.7(4) 2 . ?
C6 C5 S2 123.0(4) 2_565 . ?
C1 C6 C5 119.7(4) . 2_565 ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 2_565 . ?
O1 C7 O2 127.7(4) . . ?
O1 C7 C1 115.3(4) . . ?
O2 C7 C1 117.0(4) . . ?
O4 C8 O3 124.2(4) . . ?
O4 C8 C3 119.8(4) . . ?
O3 C8 C3 115.9(4) . . ?
C10 C9 C14 120.2(4) 2_666 . ?
C10 C9 C15 119.3(4) 2_666 . ?
C14 C9 C15 120.4(4) . . ?
C11 C10 C9 121.0(4) . 2_666 ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 2_666 . ?
C10 C11 C12 119.6(4) . . ?
C10 C11 C16 118.8(4) . . ?
C12 C11 C16 121.7(4) . . ?
C13 C12 C11 119.0(4) 1_556 . ?
C13 C12 H12 120.5 1_556 . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 121.8(4) 1_554 2_665 ?
C12 C13 S1 119.3(3) 1_554 . ?
C14 C13 S1 118.9(4) 2_665 . ?
C9 C14 C13 118.4(4) . 2_665 ?
C9 C14 H14 120.8 . . ?
C13 C14 H14 120.8 2_665 . ?
O6 C15 O5 125.1(4) . . ?
O6 C15 C9 118.8(4) . . ?
O5 C15 C9 116.1(4) . . ?
O8 C16 O7 127.0(5) . . ?
O8 C16 C11 114.5(4) . . ?
O7 C16 C11 118.5(4) . . ?
O2WA Na1 O11 89.6(3) . 2 ?
O2WA Na1 O14 84.4(3) . . ?
O11 Na1 O14 166.87(18) 2 . ?
O2WA Na1 O12 129.8(3) . . ?
O11 Na1 O12 82.23(14) 2 . ?
O14 Na1 O12 110.54(15) . . ?
O2WA Na1 O8 163.4(3) . . ?
O11 Na1 O8 93.55(16) 2 . ?
O14 Na1 O8 89.00(14) . . ?
O12 Na1 O8 66.80(13) . . ?
O2WA Na1 O2WB 19.9(3) . . ?
O11 Na1 O2WB 77.4(3) 2 . ?
O14 Na1 O2WB 99.7(4) . . ?
O12 Na1 O2WB 111.8(4) . . ?
O8 Na1 O2WB 170.9(3) . . ?
O2WA Na1 O5W 56.7(4) . . ?
O11 Na1 O5W 100.6(2) 2 . ?
O14 Na1 O5W 66.4(2) . . ?
O12 Na1 O5W 173.2(2) . . ?
O8 Na1 O5W 106.7(2) . . ?
O2WB Na1 O5W 74.9(4) . . ?
O2WA Na1 S2 108.0(3) . . ?
O11 Na1 S2 86.02(12) 2 . ?
O14 Na1 S2 106.94(12) . . ?
O12 Na1 S2 22.43(9) . . ?
O8 Na1 S2 88.48(10) . . ?
O2WB Na1 S2 91.4(3) . . ?
O5W Na1 S2 162.8(2) . . ?
O1 Ni1 O15 95.49(13) . . ?
O1 Ni1 O1W 91.60(13) . . ?
O15 Ni1 O1W 84.88(13) . . ?
O1 Ni1 O9 88.70(14) . . ?
O15 Ni1 O9 174.87(14) . . ?
O1W Ni1 O9 92.06(13) . . ?
O1 Ni1 O3 100.15(13) . 2 ?
O15 Ni1 O3 98.86(12) . 2 ?
O1W Ni1 O3 167.22(12) . 2 ?
O9 Ni1 O3 83.26(13) . 2 ?
O1 Ni1 O3 173.61(13) . . ?
O15 Ni1 O3 90.78(12) . . ?
O1W Ni1 O3 87.69(12) . . ?
O9 Ni1 O3 84.98(13) . . ?
O3 Ni1 O3 80.07(13) 2 . ?
O1 Ni1 Ni2 108.13(10) . . ?
O15 Ni1 Ni2 43.43(9) . . ?
O1W Ni1 Ni2 44.77(9) . . ?
O9 Ni1 Ni2 132.24(10) . . ?
O3 Ni1 Ni2 133.53(9) 2 . ?
O3 Ni1 Ni2 75.69(9) . . ?
O7 Ni2 O4 92.08(14) . . ?
O7 Ni2 O3W 89.75(16) . . ?
O4 Ni2 O3W 89.23(14) . . ?
O7 Ni2 O15 94.99(14) . . ?
O4 Ni2 O15 99.22(13) . . ?
O3W Ni2 O15 170.13(14) . . ?
O7 Ni2 O5 90.97(13) . . ?
O4 Ni2 O5 176.28(14) . . ?
O3W Ni2 O5 88.66(14) . . ?
O15 Ni2 O5 82.62(12) . . ?
O7 Ni2 O1W 177.29(14) . . ?
O4 Ni2 O1W 89.73(13) . . ?
O3W Ni2 O1W 92.29(16) . . ?
O15 Ni2 O1W 82.72(13) . . ?
O5 Ni2 O1W 87.29(12) . . ?
O7 Ni2 Ni1 134.04(11) . . ?
O4 Ni2 Ni1 83.41(10) . . ?
O3W Ni2 Ni1 135.65(13) . . ?
O15 Ni2 Ni1 41.69(9) . . ?
O5 Ni2 Ni1 95.98(9) . . ?
O1W Ni2 Ni1 44.22(9) . . ?
O2 Ni3 O15 98.27(13) . . ?
O2 Ni3 O8 173.39(14) . . ?
O15 Ni3 O8 88.34(13) . . ?
O2 Ni3 O4W 91.90(15) . . ?
O15 Ni3 O4W 167.98(15) . . ?
O8 Ni3 O4W 81.55(15) . . ?
O2 Ni3 O12 96.11(14) . . ?
O15 Ni3 O12 98.74(13) . . ?
O8 Ni3 O12 82.66(14) . . ?
O4W Ni3 O12 86.46(14) . . ?
O2 Ni3 O5 91.51(13) . . ?
O15 Ni3 O5 81.81(12) . . ?
O8 Ni3 O5 89.58(13) . . ?
O4W Ni3 O5 91.58(14) . . ?
O12 Ni3 O5 172.19(13) . . ?
C7 O1 Ni1 139.0(3) . . ?
C7 O2 Ni3 132.4(3) . . ?
C8 O3 Ni1 126.5(3) . 2 ?
C8 O3 Ni1 128.9(3) . . ?
Ni1 O3 Ni1 99.93(13) 2 . ?
C8 O4 Ni2 124.4(3) . . ?
C15 O5 Ni2 126.8(3) . . ?
C15 O5 Ni3 117.6(3) . . ?
Ni2 O5 Ni3 92.85(11) . . ?
C16 O7 Ni2 123.5(3) . . ?
C16 O8 Ni3 128.2(3) . . ?
C16 O8 Na1 120.0(3) . . ?
Ni3 O8 Na1 103.48(15) . . ?
S1 O9 Ni1 134.1(2) . . ?
S1 O11 Na1 172.3(3) . 2 ?
S2 O12 Ni3 135.4(2) . . ?
S2 O12 Na1 118.4(2) . . ?
Ni3 O12 Na1 105.61(15) . . ?
S2 O14 Na1 131.2(2) 2_566 . ?
Ni1 O15 Ni3 126.37(16) . . ?
Ni1 O15 Ni2 94.88(13) . . ?
Ni3 O15 Ni2 96.18(12) . . ?
Ni1 O15 H15 111.9 . . ?
Ni3 O15 H15 111.9 . . ?
Ni2 O15 H15 111.9 . . ?
Ni1 O1W Ni2 91.01(13) . . ?
Ni1 O1W H1A 112(3) . . ?
Ni2 O1W H1A 103(3) . . ?
Ni1 O1W H1B 104(3) . . ?
Ni2 O1W H1B 135(3) . . ?
H1A O1W H1B 110(2) . . ?
O2WA O2WB Na1 56.6(11) . . ?
O2WB O2WA Na1 103.5(13) . . ?
Ni2 O3W H3A 127(3) . . ?
Ni2 O3W H3B 120(3) . . ?
H3A O3W H3B 109(2) . . ?
O11 S1 O9 111.3(2) . . ?
O11 S1 O10 113.5(2) . . ?
O9 S1 O10 111.8(2) . . ?
O11 S1 C13 107.6(2) . . ?
O9 S1 C13 105.3(2) . . ?
O10 S1 C13 106.8(2) . . ?
O14 S2 O13 113.4(2) 2_566 . ?
O14 S2 O12 113.3(2) 2_566 . ?
O13 S2 O12 109.1(2) . . ?
O14 S2 C5 108.1(2) 2_566 . ?
O13 S2 C5 107.2(2) . . ?
O12 S2 C5 105.2(2) . . ?
O14 S2 Na1 120.35(17) 2_566 . ?
O13 S2 Na1 71.58(16) . . ?
O12 S2 Na1 39.13(14) . . ?
C5 S2 Na1 127.73(16) . . ?

_refine_diff_density_max         0.913
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1553053'
_audit_update_record             
;
2017-05-30 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'CO loaded Nickel 5-sulphoisophthalate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16.30 H11 Na Ni3 O17.30 S2'
_chemical_formula_weight         746.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0130 0.0070 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Na Na 0.0430 0.0300 'Calculated using XDISP in WinGX (Farrugia, 1999)'
S S 0.1430 0.1470 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ni Ni 0.3220 1.3010 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8418(16)
_cell_length_b                   10.9891(18)
_cell_length_c                   12.587(2)
_cell_angle_alpha                104.340(3)
_cell_angle_beta                 91.715(3)
_cell_angle_gamma                110.678(3)
_cell_volume                     1223.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    3832
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      29.90

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_F_000             748
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.009
_exptl_absorpt_coefficient_mu    3.133
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5578
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'sadabs (G.M. Sheldrick)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Ligth Source, station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            12300
_diffrn_reflns_av_unetI/netI     0.1173
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.247
_diffrn_reflns_theta_max         29.919
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5431
_reflns_number_gt                3447
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          .
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact  O12    ..  O13     ..       2.41 Ang.  
RESPONSE: Both oxygens are coming from the same sulphonte group.
;
_vrf_PLAT601_shelx               
;
PROBLEM:Structure Contains Solvent Accessible VOIDS of .        140 Ang3 
RESPONSE:This is a Metal organic framework at 400K under a CO atmosphere,
         these voids will be filled with CO gas.
;
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Some water bound hydrogen atoms were mot modelled but 
          included in the sumFormula.
;
_vrf_PLAT906_shelx               
;
PROBLEM: Large K value in the Analysis of Variance ......      4.484 Check 
RESPONSE: The most common place for a high value of K is in the
          lowest-intensity bin in the table. Almost all area detector
          integration programs end up slightly underestimating the 
          background, resulting in overestimated values of Fo, thus the 
          high value of Fo/Fc. This is most obvious in the weakest 
          intensities, since the small addition to Fo becomes
          insignificant in the ratio when Fo is large.
;
_vrf_PLAT976_shelx               
;
PROBLEM: Check Calcd Residual Density  0.71A From     O3W      -0.48 eA-3  
RESPONSE: hydrogen atoms were not modelled on water O3W, this is the 
          residual density.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0258P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5431
_refine_ls_number_parameters     369
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1G C 0.306(3) 0.583(3) 0.393(2) 0.060(10) Uiso 0.31(2) 1 d . . . . .
C1 C 0.1801(6) 0.5379(5) -0.0036(4) 0.0194(11) Uani 1 1 d . . . . .
C2 C 0.1977(6) -0.3315(5) 0.0546(5) 0.0205(12) Uani 1 1 d . . . . .
H2 H 0.2268 -0.3015 0.1305 0.025 Uiso 1 1 calc R U . . .
C3 C 0.1716(5) -0.2450(5) -0.0008(4) 0.0187(11) Uani 1 1 d . . . . .
C4 C 0.1318(6) -0.2911(5) -0.1144(5) 0.0227(12) Uani 1 1 d . . . . .
H4 H 0.1132 -0.2347 -0.1522 0.027 Uiso 1 1 calc R U . . .
C5 C 0.1197(6) -0.4188(5) -0.1715(4) 0.0184(11) Uani 1 1 d . . . . .
C6 C 0.1400(5) -0.5063(5) -0.1169(4) 0.0203(12) Uani 1 1 d . . . . .
H6 H 0.1269 -0.5943 -0.1558 0.024 Uiso 1 1 calc R U . . .
C7 C 0.1928(6) 0.4373(5) 0.0554(5) 0.0204(12) Uani 1 1 d . . . . .
C8 C 0.1814(6) -0.1051(5) 0.0577(4) 0.0188(11) Uani 1 1 d . . . . .
C9 C 0.5881(6) 0.5959(5) 0.2702(5) 0.0224(12) Uani 1 1 d . . . . .
C10 C 0.3865(6) 0.3843(6) 0.6173(4) 0.0250(13) Uani 1 1 d . . . . .
H10 H 0.4194 0.4581 0.5882 0.030 Uiso 1 1 calc R U . . .
C11 C 0.3133(6) 0.2568(5) 0.5475(5) 0.0222(12) Uani 1 1 d . . . . .
C12 C 0.2645(6) 0.1469(5) 0.5913(5) 0.0237(13) Uani 1 1 d . . . . .
H12 H 0.2197 0.0597 0.5446 0.028 Uiso 1 1 calc R U . . .
C13 C 0.2828(6) 0.1677(5) -0.2966(4) 0.0233(12) Uani 1 1 d . . . . .
C14 C 0.6419(6) 0.7036(6) 0.2263(5) 0.0247(13) Uani 1 1 d . . . . .
H14 H 0.6281 0.6906 0.1503 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5055(6) 0.4560(5) 0.1980(5) 0.0222(12) Uani 1 1 d . . . . .
C16 C 0.2863(6) 0.2427(6) 0.4266(4) 0.0203(12) Uani 1 1 d . . . . .
O2 O 0.2211(4) 0.4769(4) 0.1592(3) 0.0271(9) Uani 1 1 d . . . . .
O1 O 0.1667(4) 0.3202(4) -0.0049(3) 0.0249(9) Uani 1 1 d . . . . .
O1W O 0.3562(4) 0.1783(4) 0.0330(3) 0.0214(8) Uani 1 1 d D . . . .
O3 O 0.0962(4) -0.0612(3) 0.0125(3) 0.0194(8) Uani 1 1 d . . . . .
O4 O 0.2750(4) -0.0379(4) 0.1383(3) 0.0263(9) Uani 1 1 d . . . . .
O3W O 0.5532(4) 0.1756(4) 0.2201(4) 0.0394(12) Uani 1 1 d D . . . .
O5 O 0.4218(4) 0.3735(3) 0.2470(3) 0.0203(8) Uani 1 1 d . . . . .
O6 O 0.5191(4) 0.4270(4) 0.0996(3) 0.0328(10) Uani 1 1 d . . . . .
O7 O 0.3236(5) 0.1623(4) 0.3593(3) 0.0283(9) Uani 1 1 d . . . . .
O8 O 0.2280(4) 0.3212(4) 0.4058(3) 0.0295(10) Uani 1 1 d . . . . .
O9 O 0.1141(4) 0.0650(4) -0.1637(3) 0.0260(9) Uani 1 1 d . . . . .
O10 O 0.3388(5) 0.0255(4) -0.1776(3) 0.0330(10) Uani 1 1 d . . . . .
O11 O -0.1386(5) 0.0873(4) 0.3272(3) 0.0423(12) Uani 1 1 d . . . . .
O12 O 0.0452(5) 0.4177(5) 0.3328(3) 0.0385(11) Uani 1 1 d . . . . .
O13 O 0.0258(5) 0.3899(4) 0.6447(3) 0.0420(12) Uani 1 1 d . . . . .
O14 O 0.1975(5) -0.3935(5) -0.3620(4) 0.0458(12) Uani 1 1 d . . . . .
O15 O 0.1498(4) 0.1862(3) 0.1741(3) 0.0201(8) Uani 1 1 d . . . . .
H15 H 0.0696 0.1239 0.2014 0.024 Uiso 1 1 calc R U . . .
Na1 Na -0.0195(3) 0.2865(3) 0.4580(2) 0.0444(7) Uani 1 1 d . . . . .
S1 S 0.21413(16) 0.03166(14) -0.23806(11) 0.0243(3) Uani 1 1 d . . . . .
S2 S 0.07209(16) -0.46632(15) -0.31537(12) 0.0254(3) Uani 1 1 d . . . . .
Ni1 Ni 0.13209(7) 0.13732(7) 0.01033(6) 0.01752(17) Uani 1 1 d . . . . .
Ni2 Ni 0.34471(8) 0.16386(7) 0.20066(6) 0.01917(17) Uani 1 1 d . . . . .
Ni3 Ni 0.21535(8) 0.37564(7) 0.26816(6) 0.02091(18) Uani 1 1 d . . . . .
H1WA H 0.384(6) 0.132(4) -0.026(3) 0.031 Uiso 1 1 d D U . . .
H1WB H 0.410(5) 0.2669(14) 0.047(4) 0.031 Uiso 1 1 d D U . . .
H3WA H 0.620(4) 0.249(3) 0.267(4) 0.031 Uiso 1 1 d D U . . .
H3WB H 0.577(5) 0.103(3) 0.214(5) 0.031 Uiso 1 1 d D U . . .


_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
C1G Ni3 2.27(3) . ?
C1 C6 1.384(7) 1_565 ?
C1 C2 1.387(7) 1_565 ?
C1 C7 1.512(7) . ?
C2 C1 1.387(7) 1_545 ?
C2 C3 1.394(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(7) . ?
C3 C8 1.499(7) . ?
C4 C5 1.370(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(7) . ?
C5 S2 1.755(5) . ?
C6 C1 1.384(7) 1_545 ?
C6 H6 0.9300 . ?
C7 O1 1.253(6) . ?
C7 O2 1.259(6) . ?
C8 O4 1.231(6) . ?
C8 O3 1.286(6) . ?
C9 C14 1.373(7) . ?
C9 C10 1.380(7) 2_666 ?
C9 C15 1.494(7) . ?
C10 C11 1.376(7) . ?
C10 C9 1.380(7) 2_666 ?
C10 H10 0.9300 . ?
C11 C12 1.389(7) . ?
C11 C16 1.496(7) . ?
C12 C13 1.368(7) 1_556 ?
C12 H12 0.9300 . ?
C13 C12 1.368(7) 1_554 ?
C13 C14 1.390(7) 2_665 ?
C13 S1 1.760(5) . ?
C14 C13 1.390(7) 2_665 ?
C14 H14 0.9300 . ?
C15 O6 1.224(6) . ?
C15 O5 1.288(6) . ?
C16 O7 1.229(6) . ?
C16 O8 1.263(6) . ?
O2 Ni3 1.959(4) . ?
O1 Ni1 1.976(4) . ?
O1W Ni1 2.085(4) . ?
O1W Ni2 2.159(4) . ?
O1W H1WA 0.899(10) . ?
O1W H1WB 0.898(10) . ?
O3 Ni1 2.084(4) 2 ?
O3 Ni1 2.090(3) . ?
O4 Ni2 2.008(4) . ?
O3W Ni2 2.013(4) . ?
O3W H3WA 0.893(10) . ?
O3W H3WB 0.897(10) . ?
O5 Ni3 2.065(4) . ?
O5 Ni2 2.072(4) . ?
O7 Ni2 2.018(4) . ?
O8 Ni3 1.982(4) . ?
O8 Na1 2.465(5) . ?
O9 S1 1.456(4) . ?
O9 Ni1 2.116(4) . ?
O10 S1 1.455(4) . ?
O11 S1 1.434(4) 2 ?
O11 Na1 2.273(5) . ?
O12 S2 1.464(4) 2 ?
O12 Ni3 2.030(4) . ?
O12 Na1 2.347(5) . ?
O13 S2 1.429(4) 1_566 ?
O13 Na1 2.295(5) . ?
O14 S2 1.445(4) . ?
O14 Na1 2.818(6) 2 ?
O15 Ni1 1.983(4) . ?
O15 Ni3 1.984(3) . ?
O15 Ni2 2.046(4) . ?
O15 H15 0.9800 . ?
Na1 O14 2.818(6) 2 ?
Na1 S2 3.134(3) 2 ?
Na1 S2 3.257(3) 1_566 ?
Na1 Ni3 3.450(3) . ?
S1 O11 1.434(4) 2 ?
S2 O13 1.429(4) 1_544 ?
S2 O12 1.464(4) 2 ?
S2 Na1 3.134(3) 2 ?
S2 Na1 3.257(3) 1_544 ?
Ni1 O3 2.084(4) 2 ?
Ni2 Ni3 2.9894(11) . ?

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
C6 C1 C2 120.3(5) 1_565 1_565 ?
C6 C1 C7 118.3(5) 1_565 . ?
C2 C1 C7 121.2(5) 1_565 . ?
C1 C2 C3 120.0(5) 1_545 . ?
C1 C2 H2 120.0 1_545 . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 118.8(5) . . ?
C4 C3 C8 118.4(5) . . ?
C2 C3 C8 122.7(5) . . ?
C5 C4 C3 120.7(5) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 S2 117.1(4) . . ?
C6 C5 S2 122.0(4) . . ?
C5 C6 C1 119.3(5) . 1_545 ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 1_545 . ?
O1 C7 O2 126.7(5) . . ?
O1 C7 C1 115.7(5) . . ?
O2 C7 C1 117.5(5) . . ?
O4 C8 O3 125.0(5) . . ?
O4 C8 C3 119.2(5) . . ?
O3 C8 C3 115.5(4) . . ?
C14 C9 C10 119.8(5) . 2_666 ?
C14 C9 C15 121.3(5) . . ?
C10 C9 C15 118.9(5) 2_666 . ?
C11 C10 C9 120.8(5) . 2_666 ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 2_666 . ?
C10 C11 C12 119.4(5) . . ?
C10 C11 C16 118.2(5) . . ?
C12 C11 C16 122.4(5) . . ?
C13 C12 C11 119.6(5) 1_556 . ?
C13 C12 H12 120.2 1_556 . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 120.9(5) 1_554 2_665 ?
C12 C13 S1 120.8(4) 1_554 . ?
C14 C13 S1 118.4(4) 2_665 . ?
C9 C14 C13 119.4(5) . 2_665 ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 2_665 . ?
O6 C15 O5 124.7(5) . . ?
O6 C15 C9 120.1(5) . . ?
O5 C15 C9 115.2(5) . . ?
O7 C16 O8 126.8(5) . . ?
O7 C16 C11 119.7(5) . . ?
O8 C16 C11 113.5(5) . . ?
C7 O2 Ni3 130.8(4) . . ?
C7 O1 Ni1 139.0(4) . . ?
Ni1 O1W Ni2 90.75(14) . . ?
Ni1 O1W H1WA 111(4) . . ?
Ni2 O1W H1WA 132(4) . . ?
Ni1 O1W H1WB 113(4) . . ?
Ni2 O1W H1WB 99(3) . . ?
H1WA O1W H1WB 109(2) . . ?
C8 O3 Ni1 128.0(3) . 2 ?
C8 O3 Ni1 128.5(3) . . ?
Ni1 O3 Ni1 98.25(15) 2 . ?
C8 O4 Ni2 125.1(3) . . ?
Ni2 O3W H3WA 119(3) . . ?
Ni2 O3W H3WB 123(3) . . ?
H3WA O3W H3WB 111(2) . . ?
C15 O5 Ni3 118.6(3) . . ?
C15 O5 Ni2 128.5(3) . . ?
Ni3 O5 Ni2 92.53(14) . . ?
C16 O7 Ni2 124.6(4) . . ?
C16 O8 Ni3 129.2(4) . . ?
C16 O8 Na1 116.5(3) . . ?
Ni3 O8 Na1 101.22(17) . . ?
S1 O9 Ni1 132.9(2) . . ?
S1 O11 Na1 175.0(3) 2 . ?
S2 O12 Ni3 145.2(3) 2 . ?
S2 O12 Na1 108.4(2) 2 . ?
Ni3 O12 Na1 103.80(19) . . ?
S2 O13 Na1 120.2(3) 1_566 . ?
S2 O14 Na1 88.5(2) . 2 ?
Ni1 O15 Ni3 123.20(18) . . ?
Ni1 O15 Ni2 97.11(15) . . ?
Ni3 O15 Ni2 95.75(15) . . ?
Ni1 O15 H15 112.6 . . ?
Ni3 O15 H15 112.6 . . ?
Ni2 O15 H15 112.6 . . ?
O11 Na1 O13 144.04(19) . . ?
O11 Na1 O12 95.48(18) . . ?
O13 Na1 O12 119.88(19) . . ?
O11 Na1 O8 96.88(18) . . ?
O13 Na1 O8 102.90(18) . . ?
O12 Na1 O8 66.34(15) . . ?
O11 Na1 O14 87.34(18) . 2 ?
O13 Na1 O14 107.74(18) . 2 ?
O12 Na1 O14 53.39(15) . 2 ?
O8 Na1 O14 119.69(16) . 2 ?
O11 Na1 S2 94.85(14) . 2 ?
O13 Na1 S2 113.70(15) . 2 ?
O12 Na1 S2 26.31(11) . 2 ?
O8 Na1 S2 92.56(12) . 2 ?
O14 Na1 S2 27.44(9) 2 2 ?
O11 Na1 S2 163.05(16) . 1_566 ?
O13 Na1 S2 22.29(11) . 1_566 ?
O12 Na1 S2 97.86(14) . 1_566 ?
O8 Na1 S2 98.02(13) . 1_566 ?
O14 Na1 S2 92.25(13) 2 1_566 ?
S2 Na1 S2 92.51(8) 2 1_566 ?
O11 Na1 Ni3 87.04(13) . . ?
O13 Na1 Ni3 125.35(15) . . ?
O12 Na1 Ni3 34.86(11) . . ?
O8 Na1 Ni3 34.29(9) . . ?
O14 Na1 Ni3 86.56(11) 2 . ?
S2 Na1 Ni3 60.72(6) 2 . ?
S2 Na1 Ni3 109.86(8) 1_566 . ?
O11 S1 O10 113.8(3) 2 . ?
O11 S1 O9 111.5(3) 2 . ?
O10 S1 O9 111.3(2) . . ?
O11 S1 C13 107.1(3) 2 . ?
O10 S1 C13 107.0(3) . . ?
O9 S1 C13 105.7(3) . . ?
O13 S2 O14 113.8(3) 1_544 . ?
O13 S2 O12 112.7(3) 1_544 2 ?
O14 S2 O12 108.3(3) . 2 ?
O13 S2 C5 108.5(3) 1_544 . ?
O14 S2 C5 107.7(3) . . ?
O12 S2 C5 105.3(3) 2 . ?
O13 S2 Na1 123.08(19) 1_544 2 ?
O14 S2 Na1 64.0(2) . 2 ?
O12 S2 Na1 45.28(19) 2 2 ?
C5 S2 Na1 126.81(19) . 2 ?
O13 S2 Na1 37.53(18) 1_544 1_544 ?
O14 S2 Na1 88.9(2) . 1_544 ?
O12 S2 Na1 97.20(19) 2 1_544 ?
C5 S2 Na1 145.56(19) . 1_544 ?
Na1 S2 Na1 87.49(8) 2 1_544 ?
O1 Ni1 O15 96.81(15) . . ?
O1 Ni1 O3 98.43(15) . 2 ?
O15 Ni1 O3 94.85(14) . 2 ?
O1 Ni1 O1W 91.77(15) . . ?
O15 Ni1 O1W 84.98(15) . . ?
O3 Ni1 O1W 169.73(14) 2 . ?
O1 Ni1 O3 175.30(15) . . ?
O15 Ni1 O3 87.85(14) . . ?
O3 Ni1 O3 81.75(15) 2 . ?
O1W Ni1 O3 87.98(14) . . ?
O1 Ni1 O9 89.21(15) . . ?
O15 Ni1 O9 173.85(15) . . ?
O3 Ni1 O9 85.46(14) 2 . ?
O1W Ni1 O9 93.62(15) . . ?
O3 Ni1 O9 86.12(15) . . ?
O4 Ni2 O3W 90.52(17) . . ?
O4 Ni2 O7 95.99(16) . . ?
O3W Ni2 O7 91.42(19) . . ?
O4 Ni2 O15 98.34(15) . . ?
O3W Ni2 O15 169.15(17) . . ?
O7 Ni2 O15 93.85(15) . . ?
O4 Ni2 O5 173.46(15) . . ?
O3W Ni2 O5 88.70(16) . . ?
O7 Ni2 O5 90.53(15) . . ?
O15 Ni2 O5 81.79(14) . . ?
O4 Ni2 O1W 87.57(15) . . ?
O3W Ni2 O1W 92.60(18) . . ?
O7 Ni2 O1W 174.61(15) . . ?
O15 Ni2 O1W 81.59(14) . . ?
O5 Ni2 O1W 85.98(14) . . ?
O4 Ni2 Ni3 138.25(12) . . ?
O3W Ni2 Ni3 130.91(13) . . ?
O7 Ni2 Ni3 80.29(11) . . ?
O15 Ni2 Ni3 41.32(10) . . ?
O5 Ni2 Ni3 43.64(10) . . ?
O1W Ni2 Ni3 94.35(10) . . ?
O2 Ni3 O8 164.97(17) . . ?
O2 Ni3 O15 102.49(15) . . ?
O8 Ni3 O15 92.54(16) . . ?
O2 Ni3 O12 92.64(17) . . ?
O8 Ni3 O12 82.08(17) . . ?
O15 Ni3 O12 111.23(17) . . ?
O2 Ni3 O5 92.76(16) . . ?
O8 Ni3 O5 88.56(16) . . ?
O15 Ni3 O5 83.49(14) . . ?
O12 Ni3 O5 162.77(16) . . ?
O2 Ni3 C1G 84.6(7) . . ?
O8 Ni3 C1G 80.4(7) . . ?
O15 Ni3 C1G 172.1(7) . . ?
O12 Ni3 C1G 71.5(7) . . ?
O5 Ni3 C1G 92.7(7) . . ?
O2 Ni3 Ni2 113.23(12) . . ?
O8 Ni3 Ni2 77.71(12) . . ?
O15 Ni3 Ni2 42.93(10) . . ?
O12 Ni3 Ni2 145.32(14) . . ?
O5 Ni3 Ni2 43.83(10) . . ?
C1G Ni3 Ni2 131.0(7) . . ?
O2 Ni3 Na1 133.58(13) . . ?
O8 Ni3 Na1 44.49(13) . . ?
O15 Ni3 Na1 92.60(11) . . ?
O12 Ni3 Na1 41.35(13) . . ?
O5 Ni3 Na1 132.80(11) . . ?
C1G Ni3 Na1 84.9(7) . . ?
Ni2 Ni3 Na1 107.67(5) . . ?

_refine_diff_density_max         0.681
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.147

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1553051'
_audit_update_record             
;
2017-05-30 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'NO loaded Nickel 5-sulphoisophthalate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H11 N0.40 Na Ni3 O17.40 S2'
_chemical_formula_weight         750.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
N N 0.0080 0.0040 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0130 0.0070 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Na Na 0.0430 0.0300 'Calculated using XDISP in WinGX (Farrugia, 1999)'
S S 0.1430 0.1470 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ni Ni 0.3220 1.3010 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8979(17)
_cell_length_b                   10.9915(18)
_cell_length_c                   12.589(2)
_cell_angle_alpha                104.603(3)
_cell_angle_beta                 91.331(3)
_cell_angle_gamma                110.658(3)
_cell_volume                     1230.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    3412
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      26.83

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.009
_exptl_absorpt_coefficient_mu    3.117
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5469
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'sadabs (G.M. Sheldrick)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Ligth Source, station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            9285
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.248
_diffrn_reflns_theta_max         26.877
_diffrn_reflns_theta_full        26.877
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             3997
_reflns_number_gt                2652
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          .
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact  O12    ..  OgB     ..       2.89 Ang.  
RESPONSE: Short D...A distances have been noted, but no 
          hydrogen bonds exist, at least one of the 
          oxygens (typically OgB) is disordered in each 
          case.
;
_vrf_PLAT601_shelx               
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .      121 Ang3
RESPONSE: This is a metal organic framework structure that has
          been gas loaded with NO, any residual density in the 
          pores will be NO or H2O.
;
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: This data was collected at 400 K inside a gas cell, these
          are of course not ideal circumstances for collection, 
          hence the lower than expected sine(theta_max)/wavelength.
;
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: water bound hydrogen atoms were taken into account for the 
          sumFormula but could not be seen in the model. 
;
_vrf_PLAT906_shelx               
;
PROBLEM: Large K value in the Analysis of Variance ......      4.423 Check 
RESPONSE: The most common place for a high value of K is 
          in the lowest-intensity bin in the table. Almost 
          all area detector integration programs end up slightly 
          underestimating the background, resulting in overestimated 
          values of Fo, thus the high value of Fo/Fc. This is most 
          obvious in the weakest intensities, since the small addition 
          to Fo becomes insignificant in the ratio when Fo is large.
;
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Residual Density  0.81A From     O3W       0.61 eA-3  
RESPONSE: The hydrogen atoms on water O3W were not modelled.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0389P)²+2.8306P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3997
_refine_ls_number_parameters     370
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1324(8) -0.2903(7) -0.1130(6) 0.0204(18) Uani 1 1 d . . . . .
H1 H 0.1139 -0.2340 -0.1506 0.025 Uiso 1 1 calc R U . . .
C2 C 0.1707(8) -0.2435(7) -0.0001(6) 0.0181(17) Uani 1 1 d . . . . .
C3 C 0.1953(8) -0.3300(7) 0.0543(6) 0.0187(17) Uani 1 1 d . . . . .
H3 H 0.2226 -0.3000 0.1304 0.022 Uiso 1 1 calc R U . . .
C4 C 0.1799(8) 0.5386(7) -0.0031(6) 0.0192(17) Uani 1 1 d . . . . .
C5 C 0.1413(8) -0.5051(7) -0.1169(6) 0.0199(18) Uani 1 1 d . . . . .
H5 H 0.1295 -0.5929 -0.1560 0.024 Uiso 1 1 calc R U . . .
C6 C 0.1207(9) -0.4184(7) -0.1717(6) 0.0201(18) Uani 1 1 d . . . . .
C7 C 0.1794(9) -0.1053(7) 0.0569(6) 0.0212(19) Uani 1 1 d . . . . .
C8 C 0.1919(8) 0.4376(7) 0.0562(6) 0.0172(17) Uani 1 1 d . . . . .
C9 C 0.6168(9) 0.6157(8) 0.3820(7) 0.028(2) Uani 1 1 d . . . . .
H9 H 0.5850 0.5421 0.4112 0.034 Uiso 1 1 calc R U . . .
C10 C 0.5891(8) 0.5943(7) 0.2693(6) 0.0211(18) Uani 1 1 d . . . . .
C11 C 0.6427(9) 0.7034(8) 0.2263(7) 0.0236(19) Uani 1 1 d . . . . .
H11 H 0.6299 0.6905 0.1503 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2848(8) 0.1685(8) -0.2961(6) 0.0210(18) Uani 1 1 d . . . . .
C13 C 0.2623(9) 0.1475(8) -0.4082(7) 0.027(2) Uani 1 1 d . . . . .
H13 H 0.2154 0.0606 -0.4549 0.032 Uiso 1 1 calc R U . . .
C14 C 0.3110(8) 0.2589(7) 0.5489(6) 0.0192(18) Uani 1 1 d . . . . .
C15 C 0.2835(9) 0.2442(8) 0.4275(7) 0.0231(19) Uani 1 1 d . . . . .
C16 C 0.5052(8) 0.4574(8) 0.1981(7) 0.0208(18) Uani 1 1 d . . . . .
NG N 0.3128(17) 0.5799(17) 0.3874(14) 0.023(4) Uiso 0.4 1 d D . P . .
O3 O 0.0948(5) -0.0603(5) 0.0133(4) 0.0186(12) Uani 1 1 d . . . . .
O4 O 0.2720(6) -0.0375(5) 0.1390(4) 0.0225(13) Uani 1 1 d . . . . .
O3W O 0.5514(6) 0.1744(6) 0.2207(5) 0.0370(16) Uani 1 1 d . . . . .
O2 O 0.2205(6) 0.4793(5) 0.1600(4) 0.0261(13) Uani 1 1 d . . . . .
O1W O 0.3545(6) 0.1784(5) 0.0331(4) 0.0223(13) Uani 1 1 d D . . . .
O1 O 0.1661(6) 0.3207(5) -0.0043(4) 0.0222(13) Uani 1 1 d . . . . .
O7 O 0.3213(6) 0.1635(5) 0.3597(4) 0.0280(14) Uani 1 1 d . . . . .
O8 O 0.2252(6) 0.3224(6) 0.4073(4) 0.0294(14) Uani 1 1 d . . . . .
O5 O 0.4214(5) 0.3747(5) 0.2473(4) 0.0203(12) Uani 1 1 d . . . . .
O6 O 0.5187(6) 0.4256(5) 0.0982(4) 0.0320(15) Uani 1 1 d . . . . .
O9 O 0.1155(6) 0.0643(5) -0.1628(5) 0.0292(14) Uani 1 1 d . . . . .
O10 O 0.3397(6) 0.0261(6) -0.1786(5) 0.0336(15) Uani 1 1 d . . . . .
O11 O 0.1413(7) -0.0876(6) -0.3277(5) 0.0444(18) Uani 1 1 d . . . . .
O12 O 0.0374(6) 0.4114(6) 0.3319(5) 0.0357(15) Uani 1 1 d . . . . .
O13 O 0.2024(7) -0.3938(6) -0.3622(5) 0.0427(17) Uani 1 1 d . . . . .
O14 O 0.0260(7) -0.6090(6) -0.3556(5) 0.0388(16) Uani 1 1 d . . . . .
O15 O 0.1488(5) 0.1890(5) 0.1756(4) 0.0178(12) Uani 1 1 d . . . . .
H15 H 0.0690 0.1274 0.2034 0.021 Uiso 1 1 calc R U . . .
OGA O 0.305(3) 0.669(3) 0.365(3) 0.080 Uiso 0.268(16) 1 d D U . . .
OGB O 0.260(8) 0.642(7) 0.445(6) 0.080 Uiso 0.106(15) 1 d D U . . .
Na1 Na -0.0223(4) 0.2841(4) 0.4583(3) 0.0445(10) Uani 1 1 d . . . . .
S1 S 0.2158(2) 0.03167(19) -0.23785(17) 0.0243(5) Uani 1 1 d . . . . .
S2 S 0.0762(2) -0.4641(2) -0.31523(17) 0.0248(5) Uani 1 1 d . . . . .
Ni1 Ni 0.13166(10) 0.13789(9) 0.01133(8) 0.0169(3) Uani 1 1 d . . . . .
Ni2 Ni 0.34226(11) 0.16494(10) 0.20100(8) 0.0183(3) Uani 1 1 d . . . . .
Ni3 Ni 0.21659(11) 0.38091(10) 0.27095(8) 0.0212(3) Uani 1 1 d . . . . .
H2WA H 0.400(7) 0.2672(15) 0.042(5) 0.032 Uiso 1 1 d D U . . .
H2WB H 0.375(8) 0.130(5) -0.028(4) 0.032 Uiso 1 1 d D U . . .


_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
C1 C2 1.377(10) . ?
C1 C6 1.378(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(10) . ?
C2 C7 1.478(10) . ?
C3 C4 1.394(10) 1_545 ?
C3 H3 0.9300 . ?
C4 C5 1.389(10) 1_565 ?
C4 C3 1.394(10) 1_565 ?
C4 C8 1.520(10) . ?
C5 C6 1.374(10) . ?
C5 C4 1.389(10) 1_545 ?
C5 H5 0.9300 . ?
C6 S2 1.749(8) . ?
C7 O4 1.245(8) . ?
C7 O3 1.286(9) . ?
C8 O1 1.250(9) . ?
C8 O2 1.260(9) . ?
C9 C14 1.356(11) 2_666 ?
C9 C10 1.382(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.379(10) . ?
C10 C16 1.471(10) . ?
C11 C12 1.380(11) 2_665 ?
C11 H11 0.9300 . ?
C12 C13 1.371(10) . ?
C12 C11 1.380(11) 2_665 ?
C12 S1 1.766(7) . ?
C13 C14 1.397(10) 1_554 ?
C13 H13 0.9300 . ?
C14 C9 1.356(11) 2_666 ?
C14 C13 1.397(10) 1_556 ?
C14 C15 1.504(11) . ?
C15 O7 1.234(9) . ?
C15 O8 1.261(9) . ?
C16 O6 1.241(9) . ?
C16 O5 1.293(9) . ?
NG OGA 1.111(18) . ?
NG OGB 1.13(2) . ?
NG Ni3 2.166(16) . ?
O3 Ni1 2.082(5) 2 ?
O3 Ni1 2.085(5) . ?
O4 Ni2 2.013(5) . ?
O3W Ni2 2.042(6) . ?
O2 Ni3 1.963(5) . ?
O1W Ni1 2.087(6) . ?
O1W Ni2 2.158(5) . ?
O1W H2WA 0.896(10) . ?
O1W H2WB 0.896(10) . ?
O1 Ni1 1.978(5) . ?
O7 Ni2 2.017(5) . ?
O8 Ni3 1.988(6) . ?
O8 Na1 2.465(7) . ?
O5 Ni2 2.072(5) . ?
O5 Ni3 2.079(5) . ?
O9 S1 1.460(6) . ?
O9 Ni1 2.118(6) . ?
O10 S1 1.448(6) . ?
O11 S1 1.439(6) . ?
O11 Na1 2.255(6) 2 ?
O12 S2 1.468(6) 2 ?
O12 Ni3 2.049(6) . ?
O12 Na1 2.328(7) . ?
O13 S2 1.446(6) . ?
O13 Na1 2.872(8) 2 ?
O14 S2 1.436(6) . ?
O14 Na1 2.293(7) 1_544 ?
O15 Ni1 1.988(5) . ?
O15 Ni3 2.007(5) . ?
O15 Ni2 2.051(5) . ?
O15 H15 0.9800 . ?
OGA OGB 1.17(7) . ?
OGB Na1 2.95(4) 2_566 ?
Na1 O11 2.255(6) 2 ?
Na1 O14 2.293(7) 1_566 ?
Na1 O13 2.872(8) 2 ?
Na1 OGB 2.95(4) 2_566 ?
Na1 S2 3.153(4) 2 ?
Na1 S2 3.275(4) 1_566 ?
Na1 Ni3 3.469(4) . ?
S2 O12 1.468(6) 2 ?
S2 Na1 3.153(4) 2 ?
S2 Na1 3.275(4) 1_544 ?
Ni1 O3 2.082(5) 2 ?

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
C2 C1 C6 121.7(7) . . ?
C2 C1 H1 119.1 . . ?
C6 C1 H1 119.1 . . ?
C1 C2 C3 118.1(7) . . ?
C1 C2 C7 118.4(7) . . ?
C3 C2 C7 123.5(7) . . ?
C2 C3 C4 121.1(7) . 1_545 ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 1_545 . ?
C5 C4 C3 119.2(7) 1_565 1_565 ?
C5 C4 C8 118.6(7) 1_565 . ?
C3 C4 C8 122.0(7) 1_565 . ?
C6 C5 C4 119.9(7) . 1_545 ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 1_545 . ?
C5 C6 C1 119.9(7) . . ?
C5 C6 S2 122.7(6) . . ?
C1 C6 S2 117.3(6) . . ?
O4 C7 O3 124.2(7) . . ?
O4 C7 C2 118.9(7) . . ?
O3 C7 C2 116.8(7) . . ?
O1 C8 O2 127.7(7) . . ?
O1 C8 C4 115.5(7) . . ?
O2 C8 C4 116.8(6) . . ?
C14 C9 C10 121.8(8) 2_666 . ?
C14 C9 H9 119.1 2_666 . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 118.6(7) . . ?
C11 C10 C16 121.5(7) . . ?
C9 C10 C16 119.9(7) . . ?
C10 C11 C12 120.0(7) . 2_665 ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 2_665 . ?
C13 C12 C11 121.0(7) . 2_665 ?
C13 C12 S1 120.3(6) . . ?
C11 C12 S1 118.7(6) 2_665 . ?
C12 C13 C14 118.9(7) . 1_554 ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 1_554 . ?
C9 C14 C13 119.6(7) 2_666 1_556 ?
C9 C14 C15 118.6(7) 2_666 . ?
C13 C14 C15 121.7(7) 1_556 . ?
O7 C15 O8 127.0(8) . . ?
O7 C15 C14 119.5(7) . . ?
O8 C15 C14 113.5(7) . . ?
O6 C16 O5 123.7(7) . . ?
O6 C16 C10 120.7(7) . . ?
O5 C16 C10 115.5(7) . . ?
OGA NG OGB 63(4) . . ?
OGA NG Ni3 119(2) . . ?
OGB NG Ni3 130(4) . . ?
C7 O3 Ni1 128.0(4) . 2 ?
C7 O3 Ni1 128.7(4) . . ?
Ni1 O3 Ni1 98.9(2) 2 . ?
C7 O4 Ni2 125.1(5) . . ?
C8 O2 Ni3 130.9(5) . . ?
Ni1 O1W Ni2 90.6(2) . . ?
Ni1 O1W H2WA 107(5) . . ?
Ni2 O1W H2WA 103(4) . . ?
Ni1 O1W H2WB 107(5) . . ?
Ni2 O1W H2WB 134(5) . . ?
H2WA O1W H2WB 111(3) . . ?
C8 O1 Ni1 138.7(5) . . ?
C15 O7 Ni2 124.5(5) . . ?
C15 O8 Ni3 129.2(5) . . ?
C15 O8 Na1 116.2(5) . . ?
Ni3 O8 Na1 101.8(2) . . ?
C16 O5 Ni2 129.0(5) . . ?
C16 O5 Ni3 118.0(5) . . ?
Ni2 O5 Ni3 92.82(19) . . ?
S1 O9 Ni1 133.3(4) . . ?
S1 O11 Na1 175.4(4) . 2 ?
S2 O12 Ni3 144.2(4) 2 . ?
S2 O12 Na1 110.2(3) 2 . ?
Ni3 O12 Na1 104.7(3) . . ?
S2 O13 Na1 87.3(3) . 2 ?
S2 O14 Na1 121.1(4) . 1_544 ?
Ni1 O15 Ni3 123.7(2) . . ?
Ni1 O15 Ni2 96.7(2) . . ?
Ni3 O15 Ni2 95.6(2) . . ?
Ni1 O15 H15 112.5 . . ?
Ni3 O15 H15 112.5 . . ?
Ni2 O15 H15 112.5 . . ?
NG OGA OGB 59(2) . . ?
NG OGB OGA 58(2) . . ?
NG OGB Na1 157(6) . 2_566 ?
OGA OGB Na1 123(5) . 2_566 ?
O11 Na1 O14 145.4(3) 2 1_566 ?
O11 Na1 O12 94.1(2) 2 . ?
O14 Na1 O12 119.8(3) 1_566 . ?
O11 Na1 O8 98.2(2) 2 . ?
O14 Na1 O8 101.3(2) 1_566 . ?
O12 Na1 O8 66.8(2) . . ?
O11 Na1 O13 86.7(2) 2 2 ?
O14 Na1 O13 107.5(2) 1_566 2 ?
O12 Na1 O13 52.7(2) . 2 ?
O8 Na1 O13 119.6(2) . 2 ?
O11 Na1 OGB 103.1(15) 2 2_566 ?
O14 Na1 OGB 65.5(16) 1_566 2_566 ?
O12 Na1 OGB 101.9(17) . 2_566 ?
O8 Na1 OGB 156.7(16) . 2_566 ?
O13 Na1 OGB 53.2(17) 2 2_566 ?
O11 Na1 S2 94.0(2) 2 2 ?
O14 Na1 S2 113.21(19) 1_566 2 ?
O12 Na1 S2 25.90(15) . 2 ?
O8 Na1 S2 92.51(17) . 2 ?
O13 Na1 S2 27.27(13) 2 2 ?
OGB Na1 S2 76.7(17) 2_566 2 ?
O11 Na1 S2 164.3(2) 2 1_566 ?
O14 Na1 S2 22.06(15) 1_566 1_566 ?
O12 Na1 S2 97.89(19) . 1_566 ?
O8 Na1 S2 95.82(17) . 1_566 ?
O13 Na1 S2 92.47(17) 2 1_566 ?
OGB Na1 S2 64.5(15) 2_566 1_566 ?
S2 Na1 S2 92.39(11) 2 1_566 ?
O11 Na1 Ni3 88.36(19) 2 . ?
O14 Na1 Ni3 123.0(2) 1_566 . ?
O12 Na1 Ni3 34.85(15) . . ?
O8 Na1 Ni3 34.12(14) . . ?
O13 Na1 Ni3 86.57(15) 2 . ?
OGB Na1 Ni3 136.6(17) 2_566 . ?
S2 Na1 Ni3 60.59(8) 2 . ?
S2 Na1 Ni3 107.27(11) 1_566 . ?
O11 S1 O10 113.9(4) . . ?
O11 S1 O9 111.4(4) . . ?
O10 S1 O9 111.5(3) . . ?
O11 S1 C12 107.1(4) . . ?
O10 S1 C12 106.4(4) . . ?
O9 S1 C12 106.1(4) . . ?
O14 S2 O13 114.0(4) . . ?
O14 S2 O12 112.7(4) . 2 ?
O13 S2 O12 108.2(4) . 2 ?
O14 S2 C6 108.2(4) . . ?
O13 S2 C6 108.3(4) . . ?
O12 S2 C6 105.0(4) 2 . ?
O14 S2 Na1 122.3(3) . 2 ?
O13 S2 Na1 65.5(3) . 2 ?
O12 S2 Na1 43.9(3) 2 2 ?
C6 S2 Na1 127.3(3) . 2 ?
O14 S2 Na1 36.8(2) . 1_544 ?
O13 S2 Na1 89.7(3) . 1_544 ?
O12 S2 Na1 97.4(3) 2 1_544 ?
C6 S2 Na1 144.7(3) . 1_544 ?
Na1 S2 Na1 87.61(11) 2 1_544 ?
O1 Ni1 O15 96.5(2) . . ?
O1 Ni1 O3 98.6(2) . 2 ?
O15 Ni1 O3 95.7(2) . 2 ?
O1 Ni1 O3 175.1(2) . . ?
O15 Ni1 O3 88.4(2) . . ?
O3 Ni1 O3 81.1(2) 2 . ?
O1 Ni1 O1W 91.9(2) . . ?
O15 Ni1 O1W 85.1(2) . . ?
O3 Ni1 O1W 169.29(19) 2 . ?
O3 Ni1 O1W 88.2(2) . . ?
O1 Ni1 O9 89.3(2) . . ?
O15 Ni1 O9 174.0(2) . . ?
O3 Ni1 O9 84.9(2) 2 . ?
O3 Ni1 O9 85.8(2) . . ?
O1W Ni1 O9 93.2(2) . . ?
O4 Ni2 O7 95.7(2) . . ?
O4 Ni2 O3W 90.2(2) . . ?
O7 Ni2 O3W 90.9(2) . . ?
O4 Ni2 O15 98.5(2) . . ?
O7 Ni2 O15 93.9(2) . . ?
O3W Ni2 O15 169.6(2) . . ?
O4 Ni2 O5 173.5(2) . . ?
O7 Ni2 O5 90.7(2) . . ?
O3W Ni2 O5 88.6(2) . . ?
O15 Ni2 O5 82.09(19) . . ?
O4 Ni2 O1W 87.6(2) . . ?
O7 Ni2 O1W 175.0(2) . . ?
O3W Ni2 O1W 92.9(2) . . ?
O15 Ni2 O1W 81.8(2) . . ?
O5 Ni2 O1W 86.1(2) . . ?
O2 Ni3 O8 167.1(2) . . ?
O2 Ni3 O15 101.4(2) . . ?
O8 Ni3 O15 91.5(2) . . ?
O2 Ni3 O12 93.7(2) . . ?
O8 Ni3 O12 81.7(2) . . ?
O15 Ni3 O12 107.1(2) . . ?
O2 Ni3 O5 93.2(2) . . ?
O8 Ni3 O5 89.0(2) . . ?
O15 Ni3 O5 83.00(19) . . ?
O12 Ni3 O5 166.4(2) . . ?
O2 Ni3 NG 85.1(5) . . ?
O8 Ni3 NG 82.1(5) . . ?
O15 Ni3 NG 171.2(5) . . ?
O12 Ni3 NG 78.0(5) . . ?
O5 Ni3 NG 90.9(5) . . ?
O2 Ni3 Na1 133.82(18) . . ?
O8 Ni3 Na1 44.05(18) . . ?
O15 Ni3 Na1 90.91(16) . . ?
O12 Ni3 Na1 40.48(18) . . ?
O5 Ni3 Na1 132.66(16) . . ?
NG Ni3 Na1 88.6(4) . . ?

_refine_diff_density_max         0.652
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.149

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1553052'
_audit_update_record             
;
2017-05-30 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
'Partially Dehydrated Nickel 5-sulphoisophthalate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H11 Na Ni3 O17 S2'
_chemical_formula_weight         738.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0130 0.0070 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Na Na 0.0430 0.0300 'Calculated using XDISP in WinGX (Farrugia, 1999)'
S S 0.1430 0.1470 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ni Ni 0.3220 1.3010 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8415(13)
_cell_length_b                   11.0066(15)
_cell_length_c                   12.6355(17)
_cell_angle_alpha                104.131(3)
_cell_angle_beta                 92.127(3)
_cell_angle_gamma                110.798(3)
_cell_volume                     1229.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    3674
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      29.04

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_F_000             740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.009
_exptl_absorpt_coefficient_mu    3.117
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5578
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'sadabs (G.M. Sheldrick)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Ligth Source, station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            11818
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.245
_diffrn_reflns_theta_max         29.082
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5052
_reflns_number_gt                3430
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          .
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ
         Please Check
RESPONSE: Some hydrogens attached to water molecules 
          were not included in the model but were included in the 
          SumFormula
;
_vrf_PLAT601_shelx               
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        183 Ang3
RESPONSE: This is a dehydrated metal organic framework at 400 K, the voids
          will have minimal residual disordered water molecules in that 
          have not been driven off by the vacuum.          
;
_vrf_PLAT906_shelx               
;
PROBLEM: Large K value in the Analysis of Variance ......      3.499 Check 
RESPONSE: The most common place for a high value of K is in the 
          lowest-intensity bin in the table. Almost all area detector 
          integration programs end up slightly underestimating the 
          background, resulting in overestimated values of Fo, thus 
          the high value of Fo/Fc. This is most obvious in the weakest 
          intensities, since the small addition to Fo becomes insignificant
          in the ratio when Fo is large.
;
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Residual Density  0.96A From     O1W       0.56 eA-3  
RESPONSE: Hydrogen atoms were not modelled on water O1W, this residual
          density is from those hydrogens.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5052
_refine_ls_number_parameters     358
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1003
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.975
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1805(5) 0.5380(5) -0.0032(4) 0.0180(10) Uani 1 1 d . . . . .
C2 C 0.1994(5) -0.3318(5) 0.0546(4) 0.0184(10) Uani 1 1 d . . . . .
H2 H 0.2307 -0.3012 0.1301 0.022 Uiso 1 1 calc R U . . .
C3 C 0.1709(5) -0.2461(5) -0.0015(4) 0.0182(10) Uani 1 1 d . . . . .
C4 C 0.1308(5) 0.7089(5) 0.8858(4) 0.0204(11) Uani 1 1 d . . . . .
H4 H 0.1128 0.7658 0.8484 0.025 Uiso 1 1 calc R U . . .
C5 C 0.1169(5) 0.5799(5) 0.8279(4) 0.0191(10) Uani 1 1 d . . . . .
C6 C 0.1392(5) 0.4940(5) -0.1164(4) 0.0177(10) Uani 1 1 d . . . . .
H6 H 0.1266 0.4063 -0.1549 0.021 Uiso 1 1 calc R U . . .
C7 C 0.1940(5) 0.4374(5) 0.0551(4) 0.0215(11) Uani 1 1 d . . . . .
C8 C 0.1813(5) -0.1065(4) 0.0568(4) 0.0182(10) Uani 1 1 d . . . . .
C9 C 0.5886(5) 0.5961(5) 0.2705(4) 0.0214(11) Uani 1 1 d . . . . .
C10 C 0.6126(5) 0.6166(5) 0.3832(4) 0.0237(12) Uani 1 1 d . . . . .
H10 H 0.5788 0.5430 0.4124 0.028 Uiso 1 1 calc R U . . .
C11 C 0.3146(5) 0.2564(5) 0.5474(4) 0.0199(11) Uani 1 1 d . . . . .
C12 C 0.2642(5) 0.1456(5) 0.5906(4) 0.0239(12) Uani 1 1 d . . . . .
H12 H 0.2194 0.0585 0.5440 0.029 Uiso 1 1 calc R U . . .
C13 C 0.7185(5) 0.8331(5) 0.2976(4) 0.0207(11) Uani 1 1 d . . . . .
C14 C 0.6446(5) 0.7045(5) 0.2265(4) 0.0229(11) Uani 1 1 d . . . . .
H14 H 0.6330 0.6917 0.1507 0.027 Uiso 1 1 calc R U . . .
C15 C 0.5067(5) 0.4559(5) 0.1982(4) 0.0201(11) Uani 1 1 d . . . . .
C16 C 0.2882(5) 0.2429(5) 0.4260(4) 0.0202(11) Uani 1 1 d . . . . .
O1 O 0.1684(4) 0.3205(3) -0.0047(3) 0.0227(8) Uani 1 1 d . . . . .
O2 O 0.2238(4) 0.4769(3) 0.1588(3) 0.0245(8) Uani 1 1 d . . . . .
O1W O 0.3592(3) 0.1790(3) 0.0321(3) 0.0207(7) Uani 1 1 d . . . . .
O3 O 0.0964(3) -0.0613(3) 0.0121(3) 0.0180(7) Uani 1 1 d . . . . .
O4 O 0.2760(4) -0.0390(3) 0.1378(3) 0.0253(8) Uani 1 1 d . . . . .
O3W O 0.5554(4) 0.1762(4) 0.2211(4) 0.0384(10) Uani 1 1 d D . . . .
O5 O 0.4232(3) 0.3725(3) 0.2469(3) 0.0205(7) Uani 1 1 d . . . . .
O6 O 0.5215(4) 0.4275(3) 0.1003(3) 0.0313(9) Uani 1 1 d . . . . .
O7 O 0.3250(4) 0.1617(3) 0.3591(3) 0.0279(9) Uani 1 1 d . . . . .
O8 O 0.2300(4) 0.3217(4) 0.4050(3) 0.0275(8) Uani 1 1 d . . . . .
O9 O -0.1123(4) -0.0653(3) 0.1639(3) 0.0253(8) Uani 1 1 d . . . . .
O10 O -0.3371(4) -0.0250(4) 0.1781(3) 0.0316(9) Uani 1 1 d . . . . .
O11 O -0.1354(5) 0.0881(4) 0.3276(3) 0.0408(11) Uani 1 1 d . . . . .
O12 O 0.0541(4) 0.4258(4) 0.3338(3) 0.0348(9) Uani 1 1 d . . . . .
O13 O -0.1920(4) 0.3914(4) 0.3617(3) 0.0418(11) Uani 1 1 d . . . . .
O14 O 0.0264(5) 0.3884(4) 0.6450(3) 0.0408(11) Uani 1 1 d . . . . .
O15 O 0.1508(3) 0.1848(3) 0.1732(3) 0.0178(7) Uani 1 1 d . . . . .
H15 H 0.0705 0.1224 0.2001 0.021 Uiso 1 1 calc R U . . .
Na1 Na -0.0175(3) 0.2896(2) 0.45712(18) 0.0398(6) Uani 1 1 d . . . . .
S1 S -0.21175(15) -0.03114(12) 0.23847(10) 0.0228(3) Uani 1 1 d . . . . .
S2 S 0.06823(14) 0.53171(13) 0.68477(10) 0.0234(3) Uani 1 1 d . . . . .
Ni1 Ni 0.13279(7) 0.13672(6) 0.00976(5) 0.01665(15) Uani 1 1 d . . . . .
Ni2 Ni 0.34666(7) 0.16310(6) 0.20069(5) 0.01840(16) Uani 1 1 d . . . . .
Ni3 Ni 0.21656(7) 0.37336(6) 0.26624(5) 0.01883(16) Uani 1 1 d . . . . .
H3WA H 0.626(3) 0.246(3) 0.269(3) 0.023 Uiso 1 1 d D U . . .
H3WB H 0.581(4) 0.105(3) 0.202(4) 0.023 Uiso 1 1 d D U . . .


_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
C1 C2 1.383(6) 1_565 ?
C1 C6 1.388(6) . ?
C1 C7 1.511(6) . ?
C2 C1 1.383(6) 1_545 ?
C2 C3 1.404(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(7) 1_544 ?
C3 C8 1.498(6) . ?
C4 C3 1.379(7) 1_566 ?
C4 C5 1.385(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(6) 1_556 ?
C5 S2 1.751(5) . ?
C6 C5 1.377(6) 1_554 ?
C6 H6 0.9300 . ?
C7 O1 1.253(6) . ?
C7 O2 1.263(6) . ?
C8 O4 1.239(5) . ?
C8 O3 1.289(5) . ?
C9 C10 1.383(7) . ?
C9 C14 1.385(7) . ?
C9 C15 1.496(6) . ?
C10 C11 1.372(7) 2_666 ?
C10 H10 0.9300 . ?
C11 C10 1.372(7) 2_666 ?
C11 C12 1.395(6) . ?
C11 C16 1.508(6) . ?
C12 C13 1.369(7) 2_666 ?
C12 H12 0.9300 . ?
C13 C12 1.369(7) 2_666 ?
C13 C14 1.392(6) . ?
C13 S1 1.765(5) 1_665 ?
C14 H14 0.9300 . ?
C15 O6 1.227(6) . ?
C15 O5 1.294(5) . ?
C16 O7 1.236(6) . ?
C16 O8 1.267(6) . ?
O1 Ni1 1.983(3) . ?
O2 Ni3 1.962(3) . ?
O1W Ni1 2.100(3) . ?
O1W Ni2 2.184(3) . ?
O3 Ni1 2.088(3) . ?
O3 Ni1 2.090(3) 2 ?
O4 Ni2 2.015(3) . ?
O3W Ni2 2.010(4) . ?
O3W H3WA 0.894(10) . ?
O3W H3WB 0.889(10) . ?
O5 Ni3 2.060(3) . ?
O5 Ni2 2.073(3) . ?
O7 Ni2 2.024(3) . ?
O8 Ni3 1.984(3) . ?
O8 Na1 2.473(4) . ?
O9 S1 1.464(4) . ?
O9 Ni1 2.118(3) 2 ?
O10 S1 1.457(4) . ?
O11 S1 1.439(4) . ?
O11 Na1 2.281(4) . ?
O12 S2 1.469(4) 2_566 ?
O12 Ni3 2.033(4) . ?
O12 Na1 2.375(4) . ?
O13 S2 1.452(4) 2_566 ?
O13 Na1 2.744(5) . ?
O14 S2 1.431(4) . ?
O14 Na1 2.309(4) . ?
O15 Ni3 1.976(3) . ?
O15 Ni1 1.988(3) . ?
O15 Ni2 2.052(3) . ?
O15 H15 0.9800 . ?
Na1 S2 3.112(3) 2_566 ?
Na1 S2 3.251(2) . ?
Na1 Ni3 3.459(2) . ?
S1 C13 1.765(5) 1_445 ?
S2 O13 1.452(4) 2_566 ?
S2 O12 1.469(4) 2_566 ?
S2 Na1 3.112(3) 2_566 ?
Ni1 O3 2.090(3) 2 ?
Ni1 O9 2.118(3) 2 ?
Ni2 Ni3 2.9880(9) . ?

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
C2 C1 C6 120.3(4) 1_565 . ?
C2 C1 C7 121.4(4) 1_565 . ?
C6 C1 C7 118.2(4) . . ?
C1 C2 C3 119.5(4) 1_545 . ?
C1 C2 H2 120.3 1_545 . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 119.5(4) 1_544 . ?
C4 C3 C8 118.2(4) 1_544 . ?
C2 C3 C8 122.3(4) . . ?
C3 C4 C5 120.8(5) 1_566 . ?
C3 C4 H4 119.6 1_566 . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.7(4) 1_556 . ?
C6 C5 S2 122.5(4) 1_556 . ?
C4 C5 S2 117.8(4) . . ?
C5 C6 C1 120.2(4) 1_554 . ?
C5 C6 H6 119.9 1_554 . ?
C1 C6 H6 119.9 . . ?
O1 C7 O2 126.4(5) . . ?
O1 C7 C1 116.1(4) . . ?
O2 C7 C1 117.5(4) . . ?
O4 C8 O3 124.4(4) . . ?
O4 C8 C3 119.3(4) . . ?
O3 C8 C3 116.1(4) . . ?
C10 C9 C14 119.6(4) . . ?
C10 C9 C15 119.2(4) . . ?
C14 C9 C15 121.2(4) . . ?
C11 C10 C9 121.0(4) 2_666 . ?
C11 C10 H10 119.5 2_666 . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.8(5) 2_666 . ?
C10 C11 C16 117.9(4) 2_666 . ?
C12 C11 C16 122.3(4) . . ?
C13 C12 C11 119.1(4) 2_666 . ?
C13 C12 H12 120.5 2_666 . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 121.4(4) 2_666 . ?
C12 C13 S1 120.9(4) 2_666 1_665 ?
C14 C13 S1 117.7(4) . 1_665 ?
C9 C14 C13 118.9(4) . . ?
C9 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
O6 C15 O5 124.9(4) . . ?
O6 C15 C9 120.0(4) . . ?
O5 C15 C9 115.1(4) . . ?
O7 C16 O8 127.1(5) . . ?
O7 C16 C11 119.5(4) . . ?
O8 C16 C11 113.3(4) . . ?
C7 O1 Ni1 139.4(3) . . ?
C7 O2 Ni3 130.2(3) . . ?
Ni1 O1W Ni2 89.99(12) . . ?
C8 O3 Ni1 129.1(3) . . ?
C8 O3 Ni1 127.6(3) . 2 ?
Ni1 O3 Ni1 98.10(13) . 2 ?
C8 O4 Ni2 125.2(3) . . ?
Ni2 O3W H3WA 123(3) . . ?
Ni2 O3W H3WB 123(3) . . ?
H3WA O3W H3WB 111(2) . . ?
C15 O5 Ni3 118.2(3) . . ?
C15 O5 Ni2 128.6(3) . . ?
Ni3 O5 Ni2 92.60(13) . . ?
C16 O7 Ni2 124.6(3) . . ?
C16 O8 Ni3 128.4(3) . . ?
C16 O8 Na1 117.0(3) . . ?
Ni3 O8 Na1 101.24(15) . . ?
S1 O9 Ni1 132.7(2) . 2 ?
S1 O11 Na1 174.1(3) . . ?
S2 O12 Ni3 145.7(2) 2_566 . ?
S2 O12 Na1 105.7(2) 2_566 . ?
Ni3 O12 Na1 103.10(16) . . ?
S2 O13 Na1 90.3(2) 2_566 . ?
S2 O14 Na1 118.8(2) . . ?
Ni3 O15 Ni1 122.89(16) . . ?
Ni3 O15 Ni2 95.75(13) . . ?
Ni1 O15 Ni2 97.19(14) . . ?
Ni3 O15 H15 112.7 . . ?
Ni1 O15 H15 112.7 . . ?
Ni2 O15 H15 112.7 . . ?
O11 Na1 O14 142.16(17) . . ?
O11 Na1 O12 97.31(15) . . ?
O14 Na1 O12 120.20(16) . . ?
O11 Na1 O8 95.73(16) . . ?
O14 Na1 O8 103.75(16) . . ?
O12 Na1 O8 65.65(13) . . ?
O11 Na1 O13 87.90(16) . . ?
O14 Na1 O13 108.92(16) . . ?
O12 Na1 O13 54.56(13) . . ?
O8 Na1 O13 120.03(14) . . ?
O11 Na1 S2 95.86(13) . 2_566 ?
O14 Na1 S2 114.98(13) . 2_566 ?
O12 Na1 S2 27.03(9) . 2_566 ?
O8 Na1 S2 92.67(11) . 2_566 ?
O13 Na1 S2 27.82(8) . 2_566 ?
O11 Na1 S2 161.62(14) . . ?
O14 Na1 S2 22.68(10) . . ?
O12 Na1 S2 98.01(12) . . ?
O8 Na1 S2 99.81(11) . . ?
O13 Na1 S2 92.74(11) . . ?
S2 Na1 S2 93.18(7) 2_566 . ?
O11 Na1 Ni3 86.21(12) . . ?
O14 Na1 Ni3 127.10(14) . . ?
O12 Na1 Ni3 34.93(9) . . ?
O8 Na1 Ni3 34.24(8) . . ?
O13 Na1 Ni3 86.91(10) . . ?
S2 Na1 Ni3 61.04(5) 2_566 . ?
S2 Na1 Ni3 112.17(7) . . ?
O11 S1 O10 113.7(2) . . ?
O11 S1 O9 111.9(2) . . ?
O10 S1 O9 111.2(2) . . ?
O11 S1 C13 106.9(2) . 1_445 ?
O10 S1 C13 106.6(2) . 1_445 ?
O9 S1 C13 106.0(2) . 1_445 ?
O14 S2 O13 114.0(3) . 2_566 ?
O14 S2 O12 112.1(3) . 2_566 ?
O13 S2 O12 108.4(2) 2_566 2_566 ?
O14 S2 C5 108.6(2) . . ?
O13 S2 C5 107.6(2) 2_566 . ?
O12 S2 C5 105.7(2) 2_566 . ?
O14 S2 Na1 123.73(17) . 2_566 ?
O13 S2 Na1 61.86(18) 2_566 2_566 ?
O12 S2 Na1 47.29(16) 2_566 2_566 ?
C5 S2 Na1 126.60(17) . 2_566 ?
O14 S2 Na1 38.48(16) . . ?
O13 S2 Na1 88.37(17) 2_566 . ?
O12 S2 Na1 96.18(16) 2_566 . ?
C5 S2 Na1 146.55(18) . . ?
Na1 S2 Na1 86.82(7) 2_566 . ?
O1 Ni1 O15 96.69(13) . . ?
O1 Ni1 O3 175.61(13) . . ?
O15 Ni1 O3 87.64(12) . . ?
O1 Ni1 O3 98.43(13) . 2 ?
O15 Ni1 O3 94.21(13) . 2 ?
O3 Ni1 O3 81.90(13) . 2 ?
O1 Ni1 O1W 91.30(14) . . ?
O15 Ni1 O1W 85.43(13) . . ?
O3 Ni1 O1W 88.34(13) . . ?
O3 Ni1 O1W 170.24(12) 2 . ?
O1 Ni1 O9 89.19(13) . 2 ?
O15 Ni1 O9 174.07(13) . 2 ?
O3 Ni1 O9 86.46(13) . 2 ?
O3 Ni1 O9 85.59(13) 2 2 ?
O1W Ni1 O9 93.75(13) . 2 ?
O3W Ni2 O4 90.85(15) . . ?
O3W Ni2 O7 91.70(17) . . ?
O4 Ni2 O7 96.34(14) . . ?
O3W Ni2 O15 169.00(15) . . ?
O4 Ni2 O15 98.16(13) . . ?
O7 Ni2 O15 93.56(14) . . ?
O3W Ni2 O5 88.74(14) . . ?
O4 Ni2 O5 173.33(14) . . ?
O7 Ni2 O5 90.33(14) . . ?
O15 Ni2 O5 81.57(12) . . ?
O3W Ni2 O1W 92.38(16) . . ?
O4 Ni2 O1W 87.63(13) . . ?
O7 Ni2 O1W 174.27(13) . . ?
O15 Ni2 O1W 81.76(12) . . ?
O5 Ni2 O1W 85.74(12) . . ?
O3W Ni2 Ni3 130.90(11) . . ?
O4 Ni2 Ni3 137.97(10) . . ?
O7 Ni2 Ni3 80.12(10) . . ?
O15 Ni2 Ni3 41.15(8) . . ?
O5 Ni2 Ni3 43.53(9) . . ?
O1W Ni2 Ni3 94.16(9) . . ?
O2 Ni3 O15 103.29(14) . . ?
O2 Ni3 O8 163.40(15) . . ?
O15 Ni3 O8 93.30(14) . . ?
O2 Ni3 O12 91.61(15) . . ?
O15 Ni3 O12 114.46(15) . . ?
O8 Ni3 O12 81.75(15) . . ?
O2 Ni3 O5 92.68(14) . . ?
O15 Ni3 O5 83.74(13) . . ?
O8 Ni3 O5 88.65(14) . . ?
O12 Ni3 O5 159.75(14) . . ?
O2 Ni3 Ni2 113.64(11) . . ?
O15 Ni3 Ni2 43.10(9) . . ?
O8 Ni3 Ni2 78.35(10) . . ?
O12 Ni3 Ni2 148.07(12) . . ?
O5 Ni3 Ni2 43.87(9) . . ?
O2 Ni3 Na1 133.02(11) . . ?
O15 Ni3 Na1 93.57(10) . . ?
O8 Ni3 Na1 44.53(11) . . ?
O12 Ni3 Na1 41.97(11) . . ?
O5 Ni3 Na1 133.00(10) . . ?
Ni2 Ni3 Na1 108.61(4) . . ?

_refine_diff_density_max         0.654
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.127

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1553467'
_audit_update_record             
;
2017-06-01 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Cobalt 5-sulphoisophthalate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H19 Co3 Na O21 S2'
_chemical_formula_weight         811.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0434 0.0300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1434 0.1473 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3499 1.1396 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.972(4)
_cell_length_b                   11.192(5)
_cell_length_c                   12.679(5)
_cell_angle_alpha                104.544(9)
_cell_angle_beta                 90.078(9)
_cell_angle_gamma                110.086(9)
_cell_volume                     1280.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    7659
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      35.97

_exptl_crystal_description       rod
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_F_000             814
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.017
_exptl_absorpt_coefficient_mu    2.682
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6163
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'sadabs (G.M. Sheldrick)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'Advanced Ligth Source, station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            19997
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.193
_diffrn_reflns_theta_max         36.045
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9248
_reflns_number_gt                6872
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          .
_vrf_PLAT430_shelx               
;           
PROBLEM: Short Inter D...A Contact  O5W   ..  O2WC     ..  
         2.79 Ang.  
RESPONSE: If the oxygens in question are O?W or Os? then they 
disordered, not fully occupied and often without modelled
 hydrogens and therefore difficult to assign hydrogen bonds.
If both oxygens are framework bound such as O5W to O14, then
they are bound to the same Cobalt and so there is no chance
 of a hydrogen bond.
;
_vrf_PLAT041_shelx               
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ
         Please Check
RESPONSE: Hydrogens attached to disordered water molecules 
          were not included in the model but were included in the 
          SumFormula
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: O5W is a bound water molecule whose Hydrogens have not 
          been modelled.
;
_vrf_PLAT906_shelx               
;
PROBLEM: Large K value in the Analysis of Variance ......      3.379 Check 
RESPONSE: The most common place for a high value of K is in the 
          lowest-intensity bin in the table. Almost all area detector 
          integration programs end up slightly underestimating the 
          background, resulting in overestimated values of Fo, thus 
          the high value of Fo/Fc. This is most obvious in the weakest 
          intensities, since the small addition to Fo becomes 
          insignificant in the ratio when Fo is large.
;
_vrf_PLAT043_shelx               
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       5.93 Check 
RESPONSE: Disordered water molecules' hydrogen atoms have not been 
modelled but have been taken into account in the formula sum.
;
_vrf_PLAT241_shelx               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        Na1 Check 
RESPONSE: Na1 has many disordered or low occupancy water molecules 
attached, hence it is expected that their thermals are much higher than 
that of sodium.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600          7 Report
RESPONSE: This collection was carried out inside an in-situ gas-cell. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0565P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9248
_refine_ls_number_parameters     407
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1038
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co2 Co 0.66205(4) 0.33137(3) 0.79515(3) 0.01354(8) Uani 1 1 d . . . . .
Co1 Co 0.87105(4) 0.35496(3) 0.98282(3) 0.01227(8) Uani 1 1 d . . . . .
Co3 Co 0.79771(4) 0.11374(3) 0.71658(3) 0.01356(8) Uani 1 1 d . . . . .
S2 S 1.10036(7) 0.04608(6) 0.68765(5) 0.01423(12) Uani 1 1 d . . . . .
S1 S 0.77231(7) 0.46208(6) 1.22764(5) 0.01658(13) Uani 1 1 d . . . . .
Na1 Na 1.05898(18) 0.24218(14) 0.53001(12) 0.0396(4) Uani 1 1 d . . . . .
O16 O 0.85727(18) 0.30465(17) 0.81721(15) 0.0131(3) Uani 1 1 d . . . . .
H16 H 0.9356 0.3666 0.7899 0.016 Uiso 1 1 calc R U . . .
O5 O 0.58330(19) 0.12058(17) 0.74531(16) 0.0155(3) Uani 1 1 d . . . . .
O3 O 0.89919(18) 0.55623(16) 0.98381(15) 0.0135(3) Uani 1 1 d . . . . .
O1 O 0.8369(2) 0.17128(18) 0.99717(17) 0.0205(4) Uani 1 1 d . . . . .
O1W O 0.6422(2) 0.31172(19) 0.95971(16) 0.0171(4) Uani 1 1 d D . . . .
O12 O 1.0041(2) 0.1138(2) 0.66593(16) 0.0193(4) Uani 1 1 d . . . . .
O2 O 0.7897(2) 0.01618(19) 0.83450(16) 0.0192(4) Uani 1 1 d . . . . .
O4 O 0.7307(2) 0.53715(18) 0.85629(17) 0.0213(4) Uani 1 1 d . . . . .
O9 O 0.8745(2) 0.4268(2) 1.15376(17) 0.0218(4) Uani 1 1 d . . . . .
O13 O 1.2381(2) 0.1009(2) 0.64415(17) 0.0247(4) Uani 1 1 d . . . . .
O8 O 0.8035(2) 0.1974(2) 0.58437(17) 0.0224(4) Uani 1 1 d . . . . .
O7 O 0.6934(3) 0.3445(2) 0.63677(17) 0.0254(4) Uani 1 1 d . . . . .
O10 O 0.6491(2) 0.4671(2) 1.16731(19) 0.0259(4) Uani 1 1 d . . . . .
O6 O 0.4904(2) 0.0696(2) 0.89666(17) 0.0254(5) Uani 1 1 d . . . . .
O3W O 0.4550(2) 0.3254(2) 0.7750(2) 0.0334(6) Uani 1 1 d D . . . .
O4W O 0.7089(3) -0.0596(2) 0.5891(2) 0.0311(5) Uani 1 1 d D . . . .
O14 O 0.9641(2) 0.0974(2) 0.35073(18) 0.0262(5) Uani 1 1 d . . . . .
O11 O 0.8438(3) 0.5818(2) 1.31441(19) 0.0351(6) Uani 1 1 d . . . . .
C6 C 0.8485(3) -0.0030(2) 1.1124(2) 0.0144(4) Uani 1 1 d . . . . .
H6 H 0.8578 0.0825 1.1506 0.017 Uiso 1 1 calc R U . . .
C4 C 0.8557(3) 0.7817(2) 1.1105(2) 0.0139(4) Uani 1 1 d . . . . .
H4 H 0.8705 0.7251 1.1480 0.017 Uiso 1 1 calc R U . . .
C3 C 0.8240(3) 0.7396(2) 0.9969(2) 0.0131(4) Uani 1 1 d . . . . .
C1 C 0.8176(3) -0.0452(2) 0.9978(2) 0.0136(4) Uani 1 1 d . . . . .
C7 C 0.8127(3) 0.0547(2) 0.9373(2) 0.0147(4) Uani 1 1 d . . . . .
C14 C 0.3723(3) -0.2029(2) 0.7775(2) 0.0168(5) Uani 1 1 d . . . . .
H14 H 0.3904 -0.1884 0.8525 0.020 Uiso 1 1 calc R U . . .
C8 C 0.8173(3) 0.6016(2) 0.9399(2) 0.0129(4) Uani 1 1 d . . . . .
C11 C 0.6928(3) 0.2473(2) 0.4472(2) 0.0145(4) Uani 1 1 d . . . . .
C2 C 0.8026(3) 0.8254(2) 0.9407(2) 0.0141(4) Uani 1 1 d . . . . .
H2 H 0.7784 0.7966 0.8654 0.017 Uiso 1 1 calc R U . . .
C9 C 0.4211(3) -0.0981(2) 0.7289(2) 0.0140(4) Uani 1 1 d . . . . .
C12 C 0.7356(3) 0.3538(3) 0.4008(2) 0.0175(5) Uani 1 1 d . . . . .
H12 H 0.7840 0.4392 0.4439 0.021 Uiso 1 1 calc R U . . .
C5 C 1.1349(3) 0.0906(2) 0.8321(2) 0.0136(4) Uani 1 1 d . . . . .
C15 C 0.5034(3) 0.0403(2) 0.7977(2) 0.0147(4) Uani 1 1 d . . . . .
C10 C 0.6142(3) 0.1198(2) 0.3822(2) 0.0149(5) Uani 1 1 d . . . . .
H10 H 0.5856 0.0494 0.4136 0.018 Uiso 1 1 calc R U . . .
C16 C 0.7323(3) 0.2651(2) 0.5652(2) 0.0155(5) Uani 1 1 d . . . . .
C13 C 0.7042(3) 0.3297(2) 1.2889(2) 0.0155(5) Uani 1 1 d . . . . .
O5W O 1.0825(6) 0.3787(5) 0.3718(5) 0.119(2) Uani 1 1 d . . . . .
OSA O 0.5759(8) 0.5477(8) 0.6587(7) 0.050 Uiso 0.437(6) 1 d . U P A 1
OSB O 0.5255(6) 0.4885(6) 0.6035(5) 0.050 Uiso 0.563(6) 1 d . U P A 2
O2WA O 0.6943(14) -0.3138(7) 0.5170(10) 0.050 Uiso 0.490(12) 1 d . U . . .
O2WB O 0.634(2) -0.3273(13) 0.4872(12) 0.050 Uiso 0.264(12) 1 d . U . . .
O2WC O 0.7362(17) -0.3103(13) 0.5603(16) 0.050 Uiso 0.253(12) 1 d . U . . .
H4A H 0.694(5) -0.141(2) 0.595(3) 0.060 Uiso 1 1 d D U . . .
H4B H 0.740(5) -0.054(4) 0.5232(19) 0.060 Uiso 1 1 d D U . . .
H3B H 0.429(4) 0.396(3) 0.793(4) 0.060 Uiso 1 1 d D U . . .
H3A H 0.398(4) 0.261(3) 0.720(3) 0.060 Uiso 1 1 d D U . . .
H1A H 0.592(4) 0.2250(12) 0.948(4) 0.060 Uiso 1 1 d D U . . .
H1B H 0.596(4) 0.356(3) 1.005(3) 0.060 Uiso 1 1 d D U . . .


_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
Co2 O3W 2.057(2) . ?
Co2 O7 2.066(2) . ?
Co2 O4 2.096(2) . ?
Co2 O16 2.097(2) . ?
Co2 O5 2.135(2) . ?
Co2 O1W 2.155(2) . ?
Co1 O1 2.020(2) . ?
Co1 O16 2.024(2) . ?
Co1 O9 2.110(2) . ?
Co1 O3 2.154(2) 2_767 ?
Co1 O1W 2.168(2) . ?
Co1 O3 2.169(2) . ?
Co3 O2 2.048(2) . ?
Co3 O16 2.0744(19) . ?
Co3 O4W 2.098(2) . ?
Co3 O8 2.107(2) . ?
Co3 O12 2.156(2) . ?
Co3 O5 2.193(2) . ?
S2 O14 1.458(2) 2_756 ?
S2 O13 1.470(2) . ?
S2 O12 1.475(2) . ?
S2 C5 1.773(3) . ?
S1 O11 1.454(2) . ?
S1 O10 1.471(2) . ?
S1 O9 1.472(2) . ?
S1 C13 1.774(3) . ?
Na1 O2WC 2.332(13) 2_756 ?
Na1 O11 2.333(3) 2_767 ?
Na1 O14 2.404(3) . ?
Na1 O2WA 2.438(10) 2_756 ?
Na1 O12 2.458(3) . ?
Na1 O8 2.553(3) . ?
Na1 O5W 2.777(6) . ?
Na1 O2WB 2.907(17) 2_756 ?
O16 H16 0.9800 . ?
O5 C15 1.301(3) . ?
O3 C8 1.288(3) . ?
O3 Co1 2.154(2) 2_767 ?
O1 C7 1.274(3) . ?
O1W H1A 0.899(10) . ?
O1W H1B 0.898(10) . ?
O2 C7 1.260(3) . ?
O4 C8 1.256(3) . ?
O8 C16 1.265(3) . ?
O7 C16 1.264(3) . ?
O6 C15 1.234(3) . ?
O3W H3B 0.890(10) . ?
O3W H3A 0.890(10) . ?
O4W H4A 0.897(10) . ?
O4W H4B 0.901(10) . ?
O14 S2 1.458(2) 2_756 ?
O11 Na1 2.333(3) 2_767 ?
C6 C5 1.394(4) 2_757 ?
C6 C1 1.408(4) . ?
C6 H6 0.9300 . ?
C4 C3 1.398(4) . ?
C4 C5 1.402(3) 2_767 ?
C4 H4 0.9300 . ?
C3 C2 1.400(4) . ?
C3 C8 1.510(3) . ?
C1 C2 1.403(3) 1_545 ?
C1 C7 1.519(3) . ?
C14 C13 1.400(3) 2_657 ?
C14 C9 1.402(3) . ?
C14 H14 0.9300 . ?
C11 C12 1.398(3) . ?
C11 C10 1.403(3) . ?
C11 C16 1.493(4) . ?
C2 C1 1.403(3) 1_565 ?
C2 H2 0.9300 . ?
C9 C10 1.391(4) 2_656 ?
C9 C15 1.510(3) . ?
C12 C13 1.389(4) 1_554 ?
C12 H12 0.9300 . ?
C5 C6 1.394(4) 2_757 ?
C5 C4 1.402(3) 2_767 ?
C10 C9 1.391(4) 2_656 ?
C10 H10 0.9300 . ?
C13 C12 1.389(4) 1_556 ?
C13 C14 1.400(3) 2_657 ?
O2WA O2WB 0.663(15) . ?
O2WA O2WC 0.674(16) . ?
O2WA Na1 2.438(10) 2_756 ?
O2WB O2WC 1.31(2) . ?
O2WB Na1 2.907(17) 2_756 ?
O2WC Na1 2.332(13) 2_756 ?

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
O3W Co2 O7 90.81(11) . . ?
O3W Co2 O4 89.36(9) . . ?
O7 Co2 O4 92.01(9) . . ?
O3W Co2 O16 170.38(9) . . ?
O7 Co2 O16 92.91(8) . . ?
O4 Co2 O16 99.37(8) . . ?
O3W Co2 O5 88.89(8) . . ?
O7 Co2 O5 92.58(8) . . ?
O4 Co2 O5 175.11(8) . . ?
O16 Co2 O5 82.08(7) . . ?
O3W Co2 O1W 93.13(10) . . ?
O7 Co2 O1W 175.69(8) . . ?
O4 Co2 O1W 89.77(8) . . ?
O16 Co2 O1W 82.93(7) . . ?
O5 Co2 O1W 85.77(8) . . ?
O1 Co1 O16 95.61(8) . . ?
O1 Co1 O9 90.91(9) . . ?
O16 Co1 O9 172.42(8) . . ?
O1 Co1 O3 101.13(8) . 2_767 ?
O16 Co1 O3 99.01(7) . 2_767 ?
O9 Co1 O3 83.45(8) . 2_767 ?
O1 Co1 O1W 91.02(8) . . ?
O16 Co1 O1W 84.32(7) . . ?
O9 Co1 O1W 91.73(8) . . ?
O3 Co1 O1W 166.96(7) 2_767 . ?
O1 Co1 O3 174.06(8) . . ?
O16 Co1 O3 89.77(7) . . ?
O9 Co1 O3 83.56(8) . . ?
O3 Co1 O3 80.44(8) 2_767 . ?
O1W Co1 O3 87.00(7) . . ?
O2 Co3 O16 98.73(8) . . ?
O2 Co3 O4W 94.37(10) . . ?
O16 Co3 O4W 164.61(9) . . ?
O2 Co3 O8 174.66(8) . . ?
O16 Co3 O8 86.55(8) . . ?
O4W Co3 O8 80.52(10) . . ?
O2 Co3 O12 96.94(8) . . ?
O16 Co3 O12 99.84(8) . . ?
O4W Co3 O12 86.48(9) . . ?
O8 Co3 O12 81.26(8) . . ?
O2 Co3 O5 91.18(8) . . ?
O16 Co3 O5 81.21(7) . . ?
O4W Co3 O5 90.52(9) . . ?
O8 Co3 O5 90.43(8) . . ?
O12 Co3 O5 171.53(7) . . ?
O14 S2 O13 113.48(13) 2_756 . ?
O14 S2 O12 113.20(13) 2_756 . ?
O13 S2 O12 109.10(13) . . ?
O14 S2 C5 108.31(12) 2_756 . ?
O13 S2 C5 106.86(12) . . ?
O12 S2 C5 105.39(12) . . ?
O11 S1 O10 113.31(15) . . ?
O11 S1 O9 111.42(15) . . ?
O10 S1 O9 111.91(13) . . ?
O11 S1 C13 107.83(13) . . ?
O10 S1 C13 106.71(13) . . ?
O9 S1 C13 105.12(13) . . ?
O2WC Na1 O11 92.4(4) 2_756 2_767 ?
O2WC Na1 O14 81.9(5) 2_756 . ?
O11 Na1 O14 167.75(11) 2_767 . ?
O2WC Na1 O2WA 16.1(4) 2_756 2_756 ?
O11 Na1 O2WA 82.4(3) 2_767 2_756 ?
O14 Na1 O2WA 94.1(3) . 2_756 ?
O2WC Na1 O12 131.3(5) 2_756 . ?
O11 Na1 O12 82.54(9) 2_767 . ?
O14 Na1 O12 109.38(9) . . ?
O2WA Na1 O12 117.1(3) 2_756 . ?
O2WC Na1 O8 161.2(5) 2_756 . ?
O11 Na1 O8 92.83(10) 2_767 . ?
O14 Na1 O8 89.41(9) . . ?
O2WA Na1 O8 172.8(2) 2_756 . ?
O12 Na1 O8 67.27(8) . . ?
O2WC Na1 O5W 55.8(5) 2_756 . ?
O11 Na1 O5W 100.22(13) 2_767 . ?
O14 Na1 O5W 67.60(13) . . ?
O2WA Na1 O5W 70.3(3) 2_756 . ?
O12 Na1 O5W 172.49(14) . . ?
O8 Na1 O5W 105.49(14) . . ?
O2WC Na1 O2WB 26.1(6) 2_756 2_756 ?
O11 Na1 O2WB 75.9(3) 2_767 2_756 ?
O14 Na1 O2WB 102.1(3) . 2_756 ?
O2WA Na1 O2WB 10.1(4) 2_756 2_756 ?
O12 Na1 O2WB 108.2(3) . 2_756 ?
O8 Na1 O2WB 168.5(3) . 2_756 ?
O5W Na1 O2WB 79.3(3) . 2_756 ?
Co1 O16 Co3 125.51(9) . . ?
Co1 O16 Co2 95.91(8) . . ?
Co3 O16 Co2 97.28(7) . . ?
Co1 O16 H16 111.7 . . ?
Co3 O16 H16 111.7 . . ?
Co2 O16 H16 111.7 . . ?
C15 O5 Co2 127.42(17) . . ?
C15 O5 Co3 117.34(17) . . ?
Co2 O5 Co3 92.66(7) . . ?
C8 O3 Co1 126.12(15) . 2_767 ?
C8 O3 Co1 130.20(15) . . ?
Co1 O3 Co1 99.56(7) 2_767 . ?
C7 O1 Co1 140.00(18) . . ?
Co2 O1W Co1 90.17(7) . . ?
Co2 O1W H1A 102(3) . . ?
Co1 O1W H1A 112(3) . . ?
Co2 O1W H1B 119(3) . . ?
Co1 O1W H1B 123(3) . . ?
H1A O1W H1B 108(2) . . ?
S2 O12 Co3 134.05(12) . . ?
S2 O12 Na1 119.66(12) . . ?
Co3 O12 Na1 105.95(9) . . ?
C7 O2 Co3 132.82(17) . . ?
C8 O4 Co2 123.82(17) . . ?
S1 O9 Co1 134.80(13) . . ?
C16 O8 Co3 128.62(18) . . ?
C16 O8 Na1 120.54(17) . . ?
Co3 O8 Na1 104.22(9) . . ?
C16 O7 Co2 124.40(18) . . ?
Co2 O3W H3B 125(3) . . ?
Co2 O3W H3A 116(3) . . ?
H3B O3W H3A 113(2) . . ?
Co3 O4W H4A 124(3) . . ?
Co3 O4W H4B 115(3) . . ?
H4A O4W H4B 109(2) . . ?
S2 O14 Na1 131.44(14) 2_756 . ?
S1 O11 Na1 172.13(15) . 2_767 ?
C5 C6 C1 119.4(2) 2_757 . ?
C5 C6 H6 120.3 2_757 . ?
C1 C6 H6 120.3 . . ?
C3 C4 C5 120.0(2) . 2_767 ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 2_767 . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 C8 117.3(2) . . ?
C2 C3 C8 123.0(2) . . ?
C2 C1 C6 120.0(2) 1_545 . ?
C2 C1 C7 121.0(2) 1_545 . ?
C6 C1 C7 118.7(2) . . ?
O2 C7 O1 126.6(2) . . ?
O2 C7 C1 117.8(2) . . ?
O1 C7 C1 115.5(2) . . ?
C13 C14 C9 118.7(2) 2_657 . ?
C13 C14 H14 120.6 2_657 . ?
C9 C14 H14 120.6 . . ?
O4 C8 O3 124.3(2) . . ?
O4 C8 C3 119.0(2) . . ?
O3 C8 C3 116.7(2) . . ?
C12 C11 C10 120.1(2) . . ?
C12 C11 C16 121.3(2) . . ?
C10 C11 C16 118.5(2) . . ?
C3 C2 C1 120.1(2) . 1_565 ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 1_565 . ?
C10 C9 C14 119.9(2) 2_656 . ?
C10 C9 C15 119.5(2) 2_656 . ?
C14 C9 C15 120.4(2) . . ?
C13 C12 C11 118.7(2) 1_554 . ?
C13 C12 H12 120.7 1_554 . ?
C11 C12 H12 120.7 . . ?
C6 C5 C4 120.6(2) 2_757 2_767 ?
C6 C5 S2 121.96(19) 2_757 . ?
C4 C5 S2 117.42(19) 2_767 . ?
O6 C15 O5 125.1(2) . . ?
O6 C15 C9 119.3(2) . . ?
O5 C15 C9 115.6(2) . . ?
C9 C10 C11 120.4(2) 2_656 . ?
C9 C10 H10 119.8 2_656 . ?
C11 C10 H10 119.8 . . ?
O7 C16 O8 125.5(3) . . ?
O7 C16 C11 118.8(2) . . ?
O8 C16 C11 115.7(2) . . ?
C12 C13 C14 121.9(2) 1_556 2_657 ?
C12 C13 S1 118.81(19) 1_556 . ?
C14 C13 S1 119.2(2) 2_657 . ?
O2WB O2WA O2WC 157(3) . . ?
O2WB O2WA Na1 129.8(17) . 2_756 ?
O2WC O2WA Na1 73.1(16) . 2_756 ?
O2WA O2WB O2WC 11.6(13) . . ?
O2WA O2WB Na1 40.1(14) . 2_756 ?
O2WC O2WB Na1 51.6(9) . 2_756 ?
O2WA O2WC O2WB 11.4(12) . . ?
O2WA O2WC Na1 90.9(17) . 2_756 ?
O2WB O2WC Na1 102.2(11) . 2_756 ?

_refine_diff_density_max         0.829
_refine_diff_density_min         -1.946
_refine_diff_density_rms         0.132

