# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_MOF6
_database_code_depnum_ccdc_archive 'CCDC 1032694'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C22 H15 In N3 O9'
_chemical_formula_sum            'C22 H15 In N3 O9'
_chemical_formula_weight         580.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '

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

_cell_length_a                   17.303(4)
_cell_length_b                   9.925(2)
_cell_length_c                   22.410(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3848.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4575
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            35646
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         27.44
_reflns_number_total             4575
_reflns_number_gt                3520
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1704P)²+3.6706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4575
_refine_ls_number_parameters     142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0700
_refine_ls_wR_factor_ref         0.2692
_refine_ls_wR_factor_gt          0.2562
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.10587(3) -0.2500 0.82992(2) 0.0486(3) Uani 1 2 d S . .
O1 O 0.2220(3) -0.2500 0.5196(2) 0.0639(15) Uani 1 2 d S . .
O2 O 0.1207(3) -0.2500 0.7286(3) 0.0668(16) Uani 1 2 d S . .
O3 O 0.2228(4) -0.2500 0.7855(3) 0.0714(18) Uani 1 2 d S . .
O4 O 0.4844(3) -0.2500 0.6962(3) 0.0681(16) Uani 1 2 d S . .
O5 O 0.4993(4) -0.2500 0.6002(3) 0.099(3) Uani 1 2 d S . .
O6 O 0.3434(3) 0.1096(4) 0.3957(2) 0.0768(13) Uani 1 1 d . . .
O7 O 0.3975(3) 0.0096(6) 0.3197(2) 0.0773(15) Uani 1 1 d . . .
C1 C 0.2583(4) -0.2500 0.5739(3) 0.0520(17) Uani 1 2 d S . .
C2 C 0.2105(4) -0.2500 0.6246(3) 0.0512(17) Uani 1 2 d S . .
H2 H 0.1570 -0.2500 0.6204 0.080 Uiso 1 2 calc S . .
C3 C 0.2430(5) -0.2500 0.6802(3) 0.0547(18) Uani 1 2 d S . .
C4 C 0.3238(5) -0.2500 0.6873(4) 0.0550(18) Uani 1 2 d S . .
H4 H 0.3456 -0.2500 0.7252 0.080 Uiso 1 2 calc S . .
C5 C 0.3702(5) -0.2500 0.6376(4) 0.0560(18) Uani 1 2 d S . .
C6 C 0.3387(5) -0.2500 0.5798(4) 0.0562(18) Uani 1 2 d S . .
H6 H 0.3705 -0.2500 0.5464 0.080 Uiso 1 2 calc S . .
C7 C 0.1927(5) -0.2500 0.7340(4) 0.0577(19) Uani 1 2 d S . .
C8 C 0.4557(5) -0.2500 0.6444(4) 0.061(2) Uani 1 2 d S . .
C9 C 0.2689(4) -0.2500 0.4688(3) 0.0539(18) Uani 1 2 d S . .
C10 C 0.2908(3) -0.1278(6) 0.4437(3) 0.0570(13) Uani 1 1 d . . .
H10 H 0.2747 -0.0468 0.4605 0.080 Uiso 1 1 calc . . .
C11 C 0.3371(3) -0.1290(5) 0.3931(2) 0.0524(12) Uani 1 1 d . . .
C12 C 0.3596(5) -0.2500 0.3677(3) 0.0531(17) Uani 1 2 d S . .
H12 H 0.3899 -0.2500 0.3334 0.080 Uiso 1 2 calc S . .
C13 C 0.3612(4) 0.0022(7) 0.3670(3) 0.0650(15) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 O4 2.182(6) 6_557 ?
In1 O6 2.210(5) 2 ?
In1 O6 2.210(5) 8_656 ?
In1 O3 2.255(6) . ?
In1 O2 2.285(6) . ?
In1 O7 2.398(7) 8_656 ?
In1 O7 2.398(7) 2 ?
In1 O5 2.419(7) 6_557 ?
In1 C7 2.622(8) . ?
In1 C13 2.658(7) 2 ?
In1 C13 2.658(7) 8_656 ?
In1 C8 2.662(8) 6_557 ?
O1 C1 1.371(9) . ?
O1 C9 1.398(9) . ?
O2 C7 1.251(10) . ?
O3 C7 1.267(10) . ?
O4 C8 1.262(11) . ?
O4 In1 2.182(6) 6_657 ?
O5 C8 1.246(10) . ?
O5 In1 2.419(7) 6_657 ?
O6 C13 1.282(8) . ?
O6 In1 2.210(5) 2_554 ?
O7 C13 1.234(8) . ?
O7 In1 2.398(7) 2_554 ?
C1 C6 1.397(11) . ?
C1 C2 1.406(10) . ?
C2 C3 1.367(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.407(12) . ?
C3 C7 1.489(11) . ?
C4 C5 1.372(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.405(11) . ?
C5 C8 1.486(11) . ?
C6 H6 0.9300 . ?
C8 In1 2.662(8) 6_657 ?
C9 C10 1.389(7) . ?
C9 C10 1.389(7) 7 ?
C10 C11 1.389(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.385(6) . ?
C11 C13 1.486(8) . ?
C12 C11 1.385(6) 7 ?
C12 H12 0.9300 . ?
C13 In1 2.658(7) 2_554 ?

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
O4 In1 O6 124.16(17) 6_557 2 ?
O4 In1 O6 124.16(17) 6_557 8_656 ?
O6 In1 O6 78.2(3) 2 8_656 ?
O4 In1 O3 138.3(2) 6_557 . ?
O6 In1 O3 86.42(18) 2 . ?
O6 In1 O3 86.42(18) 8_656 . ?
O4 In1 O2 80.9(2) 6_557 . ?
O6 In1 O2 128.17(15) 2 . ?
O6 In1 O2 128.17(15) 8_656 . ?
O3 In1 O2 57.4(2) . . ?
O4 In1 O7 87.21(11) 6_557 8_656 ?
O6 In1 O7 134.47(18) 2 8_656 ?
O6 In1 O7 56.34(17) 8_656 8_656 ?
O3 In1 O7 88.83(13) . 8_656 ?
O2 In1 O7 84.72(13) . 8_656 ?
O4 In1 O7 87.21(11) 6_557 2 ?
O6 In1 O7 56.34(17) 2 2 ?
O6 In1 O7 134.47(18) 8_656 2 ?
O3 In1 O7 88.83(13) . 2 ?
O2 In1 O7 84.72(13) . 2 ?
O7 In1 O7 168.7(3) 8_656 2 ?
O4 In1 O5 55.9(2) 6_557 6_557 ?
O6 In1 O5 82.59(17) 2 6_557 ?
O6 In1 O5 82.59(17) 8_656 6_557 ?
O3 In1 O5 165.8(2) . 6_557 ?
O2 In1 O5 136.8(2) . 6_557 ?
O7 In1 O5 92.48(13) 8_656 6_557 ?
O7 In1 O5 92.48(13) 2 6_557 ?
O4 In1 C7 109.4(2) 6_557 . ?
O6 In1 C7 108.60(19) 2 . ?
O6 In1 C7 108.60(19) 8_656 . ?
O3 In1 C7 28.9(2) . . ?
O2 In1 C7 28.5(2) . . ?
O7 In1 C7 86.31(14) 8_656 . ?
O7 In1 C7 86.31(14) 2 . ?
O5 In1 C7 165.3(2) 6_557 . ?
O4 In1 C13 106.89(15) 6_557 2 ?
O6 In1 C13 28.69(18) 2 2 ?
O6 In1 C13 106.8(2) 8_656 2 ?
O3 In1 C13 86.87(14) . 2 ?
O2 In1 C13 106.67(14) . 2 ?
O7 In1 C13 162.9(2) 8_656 2 ?
O7 In1 C13 27.65(18) 2 2 ?
O5 In1 C13 87.76(14) 6_557 2 ?
C7 In1 C13 97.67(15) . 2 ?
O4 In1 C13 106.89(15) 6_557 8_656 ?
O6 In1 C13 106.8(2) 2 8_656 ?
O6 In1 C13 28.69(18) 8_656 8_656 ?
O3 In1 C13 86.87(14) . 8_656 ?
O2 In1 C13 106.67(14) . 8_656 ?
O7 In1 C13 27.65(18) 8_656 8_656 ?
O7 In1 C13 162.9(2) 2 8_656 ?
O5 In1 C13 87.76(14) 6_557 8_656 ?
C7 In1 C13 97.67(15) . 8_656 ?
C13 In1 C13 135.4(3) 2 8_656 ?
O4 In1 C8 28.0(3) 6_557 6_557 ?
O6 In1 C8 104.1(2) 2 6_557 ?
O6 In1 C8 104.1(2) 8_656 6_557 ?
O3 In1 C8 166.3(2) . 6_557 ?
O2 In1 C8 108.9(2) . 6_557 ?
O7 In1 C8 89.83(12) 8_656 6_557 ?
O7 In1 C8 89.83(12) 2 6_557 ?
O5 In1 C8 27.9(2) 6_557 6_557 ?
C7 In1 C8 137.4(3) . 6_557 ?
C13 In1 C8 98.15(15) 2 6_557 ?
C13 In1 C8 98.15(15) 8_656 6_557 ?
C1 O1 C9 117.2(6) . . ?
C7 O2 In1 90.9(5) . . ?
C7 O3 In1 91.8(5) . . ?
C8 O4 In1 97.6(5) . 6_657 ?
C8 O5 In1 87.0(5) . 6_657 ?
C13 O6 In1 95.4(4) . 2_554 ?
C13 O7 In1 88.0(5) . 2_554 ?
O1 C1 C6 122.7(7) . . ?
O1 C1 C2 116.6(7) . . ?
C6 C1 C2 120.6(7) . . ?
C3 C2 C1 119.6(7) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 120.8(7) . . ?
C2 C3 C7 119.8(8) . . ?
C4 C3 C7 119.4(7) . . ?
C5 C4 C3 119.3(8) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.3(8) . . ?
C4 C5 C8 119.9(7) . . ?
C6 C5 C8 118.8(7) . . ?
C1 C6 C5 118.3(7) . . ?
C1 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
O2 C7 O3 119.9(7) . . ?
O2 C7 C3 120.2(8) . . ?
O3 C7 C3 119.8(7) . . ?
O2 C7 In1 60.6(4) . . ?
O3 C7 In1 59.3(4) . . ?
C3 C7 In1 179.1(6) . . ?
O5 C8 O4 119.5(8) . . ?
O5 C8 C5 121.4(8) . . ?
O4 C8 C5 119.1(7) . . ?
O5 C8 In1 65.2(5) . 6_657 ?
O4 C8 In1 54.3(4) . 6_657 ?
C5 C8 In1 173.4(6) . 6_657 ?
C10 C9 C10 121.6(7) . 7 ?
C10 C9 O1 119.2(4) . . ?
C10 C9 O1 119.2(4) 7 . ?
C9 C10 C11 118.7(5) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 120.3(5) . . ?
C12 C11 C13 121.3(5) . . ?
C10 C11 C13 118.4(5) . . ?
C11 C12 C11 120.3(7) 7 . ?
C11 C12 H12 119.9 7 . ?
C11 C12 H12 119.9 . . ?
O7 C13 O6 120.2(6) . . ?
O7 C13 C11 122.1(6) . . ?
O6 C13 C11 117.7(6) . . ?
O7 C13 In1 64.4(4) . 2_554 ?
O6 C13 In1 55.9(3) . 2_554 ?
C11 C13 In1 173.4(5) . 2_554 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.170

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.007 -0.015 0.010 2636 260 ' '
_platon_squeeze_details          
;
three molcules of disordeded acetonitrile
;
####################################################################### 
# 
# 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_MOF4
_database_code_depnum_ccdc_archive 'CCDC 1032695'
_audit_update_record             
;
2015-02-10 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C28 H36 N4 O14 Zn2'
_chemical_formula_sum            'C28 H40 N4 O16 Zn2'
_chemical_formula_weight         819.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   10.289(2)
_cell_length_b                   15.763(3)
_cell_length_c                   24.796(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.65(3)
_cell_angle_gamma                90.00
_cell_volume                     3711.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9245
_cell_measurement_theta_min      1.57
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_T_max  0.693
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27099
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         28.35
_reflns_number_total             9245
_reflns_number_gt                6163
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger, For the disordered of DMF
 molecule , we use some restraints about the C and N atoms from DMF in the
 refinement,
eqiv $1 x+1, y, z,
htab O14 O13_$1,
eadp o10 n1 c17 c18 c19,
eadp o11 n2 c20 c21 c22,
eadp o12 n3 c23 c24 c25,
dfix 0.90  0.01 o14 h14a,
dfix 0.90  0.01 o14 h14b,
dfix 1.40  0.01 h14a h14b.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1184P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9245
_refine_ls_number_parameters     371
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0670
_refine_ls_wR_factor_ref         0.2101
_refine_ls_wR_factor_gt          0.1959
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.74215(5) -0.14623(3) -0.26493(2) 0.03075(16) Uani 1 1 d . . .
Zn2 Zn 0.70840(5) -0.01794(3) -0.144514(18) 0.02419(15) Uani 1 1 d . . .
O1 O 0.6184(4) -0.1763(2) -0.21589(17) 0.0539(10) Uani 1 1 d . . .
O2 O 0.5973(4) -0.1154(2) -0.13961(16) 0.0477(9) Uani 1 1 d . . .
O3 O 0.3800(4) -0.4496(2) -0.28605(14) 0.0396(8) Uani 1 1 d . . .
O4 O 0.2796(4) -0.5168(2) -0.23379(16) 0.0439(9) Uani 1 1 d . . .
O5 O -0.0794(4) -0.1550(2) -0.19071(14) 0.0412(8) Uani 1 1 d . . .
O6 O -0.1023(4) -0.0590(2) -0.12908(14) 0.0441(8) Uani 1 1 d . . .
O7 O 0.2325(4) -0.0473(2) 0.07295(14) 0.0404(8) Uani 1 1 d . . .
O8 O 0.4300(4) -0.1212(3) 0.09971(16) 0.0638(12) Uani 1 1 d . . .
O9 O 0.3424(3) -0.32707(18) -0.06549(12) 0.0299(6) Uani 1 1 d . . .
C1 C 0.3829(4) -0.3220(2) -0.11286(17) 0.0253(8) Uani 1 1 d . . .
C2 C 0.4578(5) -0.2532(3) -0.11957(18) 0.0281(8) Uani 1 1 d . . .
H2 H 0.4806 -0.2087 -0.0929 0.080 Uiso 1 1 calc . . .
C3 C 0.4987(4) -0.2512(3) -0.16673(18) 0.0280(8) Uani 1 1 d . . .
C4 C 0.4661(4) -0.3182(3) -0.20592(18) 0.0286(8) Uani 1 1 d . . .
H4 H 0.4947 -0.3168 -0.2372 0.080 Uiso 1 1 calc . . .
C5 C 0.3911(4) -0.3872(2) -0.19879(17) 0.0254(8) Uani 1 1 d . . .
C6 C 0.3495(4) -0.3893(2) -0.15137(17) 0.0257(8) Uani 1 1 d . . .
H6 H 0.2999 -0.4356 -0.1458 0.080 Uiso 1 1 calc . . .
C7 C 0.5790(5) -0.1756(3) -0.17505(19) 0.0326(9) Uani 1 1 d . . .
C8 C 0.3476(4) -0.4577(3) -0.24197(18) 0.0288(8) Uani 1 1 d . . .
C9 C 0.2724(4) -0.2553(2) -0.05782(17) 0.0246(8) Uani 1 1 d . . .
C10 C 0.1577(5) -0.2241(3) -0.10323(17) 0.0283(8) Uani 1 1 d . . .
H10 H 0.1280 -0.2494 -0.1399 0.080 Uiso 1 1 calc . . .
C11 C 0.0860(4) -0.1541(2) -0.09400(18) 0.0260(8) Uani 1 1 d . . .
C12 C 0.1340(4) -0.1166(3) -0.03865(18) 0.0283(8) Uani 1 1 d . . .
H12 H 0.0861 -0.0703 -0.0320 0.080 Uiso 1 1 calc . . .
C13 C 0.2529(4) -0.1477(3) 0.00669(18) 0.0277(8) Uani 1 1 d . . .
C14 C 0.3225(4) -0.2184(3) -0.00240(18) 0.0285(8) Uani 1 1 d . . .
H14 H 0.4007 -0.2407 0.0277 0.080 Uiso 1 1 calc . . .
C15 C -0.0423(4) -0.1209(3) -0.14241(18) 0.0283(8) Uani 1 1 d . . .
C16 C 0.3124(5) -0.1032(3) 0.06531(18) 0.0319(9) Uani 1 1 d . . .
O10 O 0.7524(7) -0.2758(4) -0.2787(3) 0.0982(11) Uani 1 1 d . . .
N1 N 0.8355(9) -0.3979(5) -0.2921(3) 0.0982(11) Uani 1 1 d D . .
C17 C 0.8290(11) -0.3116(7) -0.2786(4) 0.0982(11) Uani 1 1 d . . .
H17 H 0.9150 -0.2836 -0.2673 0.100 Uiso 1 1 calc . . .
C18 C 0.9680(11) -0.4219(6) -0.2883(4) 0.0982(11) Uani 1 1 d . . .
H18A H 1.0283 -0.3731 -0.2798 0.100 Uiso 1 1 calc . . .
H18B H 0.9612 -0.4463 -0.3248 0.100 Uiso 1 1 calc . . .
H18C H 1.0063 -0.4630 -0.2577 0.100 Uiso 1 1 calc . . .
C19 C 0.7257(10) -0.4547(6) -0.3033(4) 0.0982(11) Uani 1 1 d D . .
H19A H 0.7349 -0.4997 -0.3276 0.080 Uiso 1 1 calc R . .
H19B H 0.6378 -0.4259 -0.3229 0.080 Uiso 1 1 calc R . .
H19C H 0.7282 -0.4779 -0.2671 0.080 Uiso 1 1 calc R . .
O11 O 0.5469(6) -0.1481(4) -0.3365(3) 0.0909(10) Uani 1 1 d . . .
N2 N 0.3204(7) -0.1730(5) -0.3467(3) 0.0909(10) Uani 1 1 d . . .
C20 C 0.4493(9) -0.1922(6) -0.3403(4) 0.0909(10) Uani 1 1 d . . .
H20 H 0.4682 -0.2500 -0.3383 0.100 Uiso 1 1 calc . . .
C21 C 0.2912(8) -0.0834(6) -0.3475(4) 0.0909(10) Uani 1 1 d . . .
H21A H 0.1974 -0.0753 -0.3490 0.100 Uiso 1 1 calc . . .
H21B H 0.2994 -0.0579 -0.3812 0.100 Uiso 1 1 calc . . .
H21C H 0.3574 -0.0575 -0.3127 0.100 Uiso 1 1 calc . . .
C22 C 0.2141(9) -0.2303(6) -0.3523(4) 0.0909(10) Uani 1 1 d . . .
H22A H 0.1303 -0.2001 -0.3557 0.100 Uiso 1 1 calc . . .
H22B H 0.2428 -0.2663 -0.3185 0.100 Uiso 1 1 calc . . .
H22C H 0.1954 -0.2643 -0.3866 0.100 Uiso 1 1 calc . . .
O12 O 0.0301(7) -0.4803(4) -0.1479(3) 0.0991(11) Uani 1 1 d . . .
N3 N -0.0383(9) -0.4027(5) -0.0895(4) 0.0991(11) Uani 1 1 d . . .
C23 C 0.0426(11) -0.4560(6) -0.1038(5) 0.0991(11) Uani 1 1 d . . .
H23 H 0.1210 -0.4761 -0.0727 0.100 Uiso 1 1 calc . . .
C24 C -0.1593(11) -0.3653(6) -0.1304(5) 0.0991(11) Uani 1 1 d . . .
H24A H -0.2005 -0.3281 -0.1106 0.100 Uiso 1 1 calc . . .
H24B H -0.2258 -0.4086 -0.1505 0.100 Uiso 1 1 calc . . .
H24C H -0.1347 -0.3333 -0.1580 0.100 Uiso 1 1 calc . . .
C25 C 0.0046(11) -0.3770(6) -0.0294(5) 0.0991(11) Uani 1 1 d . . .
H25A H -0.0626 -0.3375 -0.0258 0.100 Uiso 1 1 calc . . .
H25B H 0.0956 -0.3506 -0.0167 0.100 Uiso 1 1 calc . . .
H25C H 0.0096 -0.4259 -0.0056 0.100 Uiso 1 1 calc . . .
O13 O -0.1601(7) -0.2342(4) -0.4057(3) 0.0989(19) Uani 1 1 d . . .
N4 N -0.2503(6) -0.3515(3) -0.4616(2) 0.0578(13) Uani 1 1 d . . .
C26 C -0.2500(8) -0.2918(5) -0.4246(3) 0.0662(18) Uani 1 1 d . . .
H26 H -0.3231 -0.2924 -0.4113 0.080 Uiso 1 1 calc . . .
C27 C -0.3538(7) -0.4179(4) -0.4794(3) 0.0704(19) Uani 1 1 d . . .
H27A H -0.4226 -0.4081 -0.4627 0.080 Uiso 1 1 calc R . .
H27B H -0.3087 -0.4715 -0.4661 0.080 Uiso 1 1 calc R . .
H27C H -0.3993 -0.4184 -0.5212 0.080 Uiso 1 1 calc R . .
C28 C -0.1376(11) -0.3565(6) -0.4833(4) 0.102(3) Uani 1 1 d . . .
H28A H -0.1518 -0.4053 -0.5080 0.080 Uiso 1 1 calc . . .
H28B H -0.0487 -0.3613 -0.4509 0.080 Uiso 1 1 calc . . .
H28C H -0.1381 -0.3062 -0.5052 0.080 Uiso 1 1 calc . . .
O14 O 0.8550(5) -0.1271(3) -0.31849(19) 0.0573(11) Uani 1 1 d D . .
H14B H 0.829(9) -0.167(3) -0.347(2) 0.12(3) Uiso 1 1 d D . .
H14A H 0.857(9) -0.080(2) -0.339(3) 0.11(3) Uiso 1 1 d D . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O5 2.043(3) 1_655 ?
Zn1 O4 2.051(3) 2_654 ?
Zn1 O10 2.080(6) . ?
Zn1 O14 2.095(4) . ?
Zn1 O11 2.107(6) . ?
Zn1 O1 2.126(3) . ?
Zn2 O7 1.935(3) 3_655 ?
Zn2 O3 1.936(3) 2_654 ?
Zn2 O6 1.946(3) 1_655 ?
Zn2 O2 1.946(3) . ?
O1 C7 1.227(5) . ?
O2 C7 1.257(5) . ?
O3 C8 1.266(5) . ?
O3 Zn2 1.936(3) 2_644 ?
O4 C8 1.229(5) . ?
O4 Zn1 2.051(3) 2_644 ?
O5 C15 1.231(5) . ?
O5 Zn1 2.043(3) 1_455 ?
O6 C15 1.265(5) . ?
O6 Zn2 1.946(3) 1_455 ?
O7 C16 1.269(5) . ?
O7 Zn2 1.935(3) 3_655 ?
O8 C16 1.215(6) . ?
O9 C1 1.391(4) . ?
O9 C9 1.393(4) . ?
C1 C2 1.377(6) . ?
C1 C6 1.380(5) . ?
C2 C3 1.388(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(6) . ?
C3 C7 1.509(6) . ?
C4 C5 1.383(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(5) . ?
C5 C8 1.488(5) . ?
C6 H6 0.9300 . ?
C9 C10 1.370(6) . ?
C9 C14 1.395(5) . ?
C10 C11 1.394(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.399(5) . ?
C11 C15 1.495(6) . ?
C12 C13 1.394(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(6) . ?
C13 C16 1.515(5) . ?
C14 H14 0.9300 . ?
O10 C17 0.968(9) . ?
N1 C18 1.382(11) . ?
N1 C19 1.384(10) . ?
N1 C17 1.409(12) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9601 . ?
C18 H18C 0.9601 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
O11 C20 1.195(9) . ?
N2 C20 1.308(10) . ?
N2 C22 1.384(10) . ?
N2 C21 1.442(11) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9599 . ?
C21 H21B 0.9601 . ?
C21 H21C 0.9601 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
O12 C23 1.118(10) . ?
N3 C23 1.323(11) . ?
N3 C24 1.397(12) . ?
N3 C25 1.441(12) . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9599 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O13 C26 1.252(9) . ?
N4 C26 1.313(8) . ?
N4 C27 1.436(8) . ?
N4 C28 1.455(9) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O14 H14B 0.899(10) . ?
O14 H14A 0.900(10) . ?

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
O5 Zn1 O4 97.81(15) 1_655 2_654 ?
O5 Zn1 O10 89.8(2) 1_655 . ?
O4 Zn1 O10 170.42(19) 2_654 . ?
O5 Zn1 O14 93.18(17) 1_655 . ?
O4 Zn1 O14 86.02(15) 2_654 . ?
O10 Zn1 O14 87.8(2) . . ?
O5 Zn1 O11 172.86(19) 1_655 . ?
O4 Zn1 O11 86.43(19) 2_654 . ?
O10 Zn1 O11 86.6(2) . . ?
O14 Zn1 O11 92.8(2) . . ?
O5 Zn1 O1 89.91(16) 1_655 . ?
O4 Zn1 O1 98.32(14) 2_654 . ?
O10 Zn1 O1 87.4(2) . . ?
O14 Zn1 O1 174.30(15) . . ?
O11 Zn1 O1 83.8(2) . . ?
O7 Zn2 O3 113.19(15) 3_655 2_654 ?
O7 Zn2 O6 93.38(14) 3_655 1_655 ?
O3 Zn2 O6 116.85(15) 2_654 1_655 ?
O7 Zn2 O2 110.30(15) 3_655 . ?
O3 Zn2 O2 114.16(17) 2_654 . ?
O6 Zn2 O2 107.02(16) 1_655 . ?
C7 O1 Zn1 158.6(3) . . ?
C7 O2 Zn2 119.1(3) . . ?
C8 O3 Zn2 121.5(3) . 2_644 ?
C8 O4 Zn1 144.8(3) . 2_644 ?
C15 O5 Zn1 132.9(3) . 1_455 ?
C15 O6 Zn2 139.2(3) . 1_455 ?
C16 O7 Zn2 120.9(3) . 3_655 ?
C1 O9 C9 114.0(3) . . ?
C2 C1 C6 121.6(3) . . ?
C2 C1 O9 120.7(3) . . ?
C6 C1 O9 117.7(3) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 C7 120.3(4) . . ?
C2 C3 C7 119.5(4) . . ?
C5 C4 C3 120.4(4) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 C8 121.6(3) . . ?
C6 C5 C8 118.9(4) . . ?
C1 C6 C5 119.2(4) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
O1 C7 O2 125.1(4) . . ?
O1 C7 C3 118.5(4) . . ?
O2 C7 C3 116.3(4) . . ?
O4 C8 O3 125.1(4) . . ?
O4 C8 C5 118.7(4) . . ?
O3 C8 C5 116.1(4) . . ?
C10 C9 O9 120.4(3) . . ?
C10 C9 C14 122.3(4) . . ?
O9 C9 C14 117.3(4) . . ?
C9 C10 C11 119.4(4) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C12 119.1(4) . . ?
C10 C11 C15 120.3(4) . . ?
C12 C11 C15 120.6(4) . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 C16 119.0(4) . . ?
C12 C13 C16 121.0(4) . . ?
C13 C14 C9 118.4(4) . . ?
C13 C14 H14 120.8 . . ?
C9 C14 H14 120.8 . . ?
O5 C15 O6 126.2(4) . . ?
O5 C15 C11 118.4(4) . . ?
O6 C15 C11 115.4(4) . . ?
O8 C16 O7 125.8(4) . . ?
O8 C16 C13 119.4(4) . . ?
O7 C16 C13 114.8(4) . . ?
C17 O10 Zn1 131.7(10) . . ?
C18 N1 C19 123.0(8) . . ?
C18 N1 C17 112.6(9) . . ?
C19 N1 C17 124.2(8) . . ?
O10 C17 N1 132.5(12) . . ?
O10 C17 H17 113.7 . . ?
N1 C17 H17 113.7 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 O11 Zn1 125.0(6) . . ?
C20 N2 C22 125.9(8) . . ?
C20 N2 C21 115.1(8) . . ?
C22 N2 C21 119.0(7) . . ?
O11 C20 N2 131.0(9) . . ?
O11 C20 H20 114.5 . . ?
N2 C20 H20 114.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 N3 C24 123.5(9) . . ?
C23 N3 C25 118.7(9) . . ?
C24 N3 C25 117.7(8) . . ?
O12 C23 N3 129.1(11) . . ?
O12 C23 H23 115.5 . . ?
N3 C23 H23 115.5 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 N4 C27 122.6(6) . . ?
C26 N4 C28 120.6(6) . . ?
C27 N4 C28 116.7(5) . . ?
O13 C26 N4 125.7(6) . . ?
O13 C26 H26 117.1 . . ?
N4 C26 H26 117.1 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N4 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Zn1 O14 H14B 108(5) . . ?
Zn1 O14 H14A 128(5) . . ?
H14B O14 H14A 102.1(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O14 H14B O13 0.899(10) 1.85(3) 2.700(6) 157(7) 1_655

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.661
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.121

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 175 41 ' '
2 0.000 0.500 0.000 175 41 ' '
3 0.134 0.578 0.587 10 0 ' '
4 0.134 0.922 0.087 10 0 ' '
5 0.338 0.690 0.738 33 2 ' '
6 0.337 0.810 0.238 33 2 ' '
7 0.662 0.190 0.761 33 2 ' '
8 0.662 0.310 0.261 33 2 ' '
9 0.865 0.078 0.913 10 0 ' '
10 0.865 0.422 0.413 10 0 ' '
_platon_squeeze_details          
;
 two molcules of disordeded water
;
####################################################################### 
# 
# 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_MOF5
_database_code_depnum_ccdc_archive 'CCDC 1032696'
_audit_update_record             
;
2015-02-10 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H6 O10 Zn2'
_chemical_formula_sum            'C16 H6 O10 Zn2'
_chemical_formula_weight         488.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

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

_cell_length_a                   19.005(4)
_cell_length_b                   13.683(3)
_cell_length_c                   14.521(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.11(3)
_cell_angle_gamma                90.00
_cell_volume                     3299.2(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3771
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15946
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3771
_reflns_number_gt                3299
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0376P)²+8.3138P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3771
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0809
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn -0.192510(18) 1.14234(2) -0.75831(2) 0.02045(9) Uani 1 1 d . . .
Zn2 Zn -0.207620(17) 1.146176(19) -0.11898(2) 0.01869(9) Uani 1 1 d . . .
O1 O -0.15472(13) 1.04657(13) -0.64049(14) 0.0286(4) Uani 1 1 d . . .
O2 O -0.16070(12) 0.96092(12) -0.51603(14) 0.0269(4) Uani 1 1 d . . .
O3 O -0.18632(17) 1.15514(15) -0.2362(2) 0.0461(6) Uani 1 1 d . . .
O4 O -0.21997(13) 1.31066(15) -0.28062(17) 0.0335(5) Uani 1 1 d . . .
O5 O 0.17992(11) 1.60910(15) -0.18563(16) 0.0318(5) Uani 1 1 d . . .
O6 O 0.12353(12) 1.74313(14) -0.28115(17) 0.0366(5) Uani 1 1 d . . .
O7 O -0.16443(13) 1.74123(14) -0.52771(16) 0.0357(5) Uani 1 1 d . . .
O8 O -0.22388(11) 1.59996(15) -0.60233(15) 0.0314(5) Uani 1 1 d . . .
O9 O -0.00774(11) 1.34627(12) -0.41170(16) 0.0243(4) Uani 1 1 d . . .
O10 O -0.10758(16) 1.0723(2) -0.7963(2) 0.0651(9) Uani 1 1 d . . .
C1 C -0.06709(15) 1.28301(17) -0.41962(19) 0.0199(5) Uani 1 1 d . . .
C2 C -0.08186(16) 1.20149(18) -0.4832(2) 0.0222(5) Uani 1 1 d . . .
H2A H -0.0570 1.1948 -0.5245 0.080 Uiso 1 1 calc R . .
C3 C -0.13432(17) 1.12971(17) -0.4845(2) 0.0219(5) Uani 1 1 d . . .
C4 C -0.17009(17) 1.13879(18) -0.4211(2) 0.0230(5) Uani 1 1 d . . .
H4A H -0.2031 1.0894 -0.4196 0.080 Uiso 1 1 calc R . .
C5 C -0.15612(16) 1.22251(18) -0.3598(2) 0.0214(5) Uani 1 1 d . . .
C6 C -0.10545(16) 1.29570(18) -0.3602(2) 0.0225(5) Uani 1 1 d . . .
H6A H -0.0974 1.3524 -0.3210 0.080 Uiso 1 1 calc R . .
C7 C -0.15131(15) 1.04164(18) -0.5525(2) 0.0215(5) Uani 1 1 d . . .
C8 C -0.19108(16) 1.23124(19) -0.2871(2) 0.0244(5) Uani 1 1 d . . .
C9 C -0.01708(15) 1.44603(17) -0.40211(19) 0.0181(5) Uani 1 1 d . . .
C10 C 0.05169(15) 1.49699(17) -0.33376(19) 0.0188(5) Uani 1 1 d . . .
H10B H 0.0997 1.4640 -0.2922 0.080 Uiso 1 1 calc R . .
C11 C 0.04798(15) 1.59838(17) -0.32815(19) 0.0179(5) Uani 1 1 d . . .
C12 C -0.02357(15) 1.64728(17) -0.3908(2) 0.0204(5) Uani 1 1 d . . .
H12A H -0.0257 1.7149 -0.3866 0.080 Uiso 1 1 calc R . .
C13 C -0.09187(15) 1.59589(17) -0.45951(19) 0.0185(5) Uani 1 1 d . . .
C14 C -0.08904(15) 1.49393(18) -0.46483(19) 0.0197(5) Uani 1 1 d . . .
H14A H -0.1349 1.4588 -0.5099 0.080 Uiso 1 1 calc R . .
C15 C 0.12305(16) 1.65443(18) -0.2592(2) 0.0220(5) Uani 1 1 d . . .
C16 C -0.16607(16) 1.64955(18) -0.5352(2) 0.0224(5) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O6 1.9421(19) 5_584 ?
Zn1 O8 1.956(2) 4_443 ?
Zn1 O1 1.9912(19) . ?
Zn1 O4 2.101(2) 7_474 ?
Zn1 O10 2.166(3) . ?
Zn2 O7 1.9353(19) 6_586 ?
Zn2 O3 1.936(2) . ?
Zn2 O5 1.936(2) 3_445 ?
Zn2 O2 1.9699(18) 6_576 ?
O1 C7 1.249(3) . ?
O2 C7 1.275(3) . ?
O2 Zn2 1.9699(18) 6_575 ?
O3 C8 1.255(3) . ?
O4 C8 1.242(3) . ?
O4 Zn1 2.101(2) 7_474 ?
O5 C15 1.254(3) . ?
O5 Zn2 1.936(2) 3 ?
O6 C15 1.256(3) . ?
O6 Zn1 1.9421(19) 5_584 ?
O7 C16 1.258(3) . ?
O7 Zn2 1.9353(19) 6_585 ?
O8 C16 1.255(3) . ?
O8 Zn1 1.956(2) 4_453 ?
O9 C1 1.381(3) . ?
O9 C9 1.392(3) . ?
C1 C6 1.385(4) . ?
C1 C2 1.387(3) . ?
C2 C3 1.393(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.391(4) . ?
C3 C7 1.490(3) . ?
C4 C5 1.395(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.391(4) . ?
C5 C8 1.501(3) . ?
C6 H6A 0.9300 . ?
C9 C10 1.385(3) . ?
C9 C14 1.385(3) . ?
C10 C11 1.394(3) . ?
C10 H10B 0.9300 . ?
C11 C12 1.386(4) . ?
C11 C15 1.495(3) . ?
C12 C13 1.384(3) . ?
C12 H12A 0.9300 . ?
C13 C14 1.400(3) . ?
C13 C16 1.492(3) . ?
C14 H14A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Zn1 O8 129.52(9) 5_584 4_443 ?
O6 Zn1 O1 111.59(9) 5_584 . ?
O8 Zn1 O1 117.75(9) 4_443 . ?
O6 Zn1 O4 100.53(9) 5_584 7_474 ?
O8 Zn1 O4 91.04(9) 4_443 7_474 ?
O1 Zn1 O4 88.40(9) . 7_474 ?
O6 Zn1 O10 87.27(11) 5_584 . ?
O8 Zn1 O10 86.36(9) 4_443 . ?
O1 Zn1 O10 85.74(11) . . ?
O4 Zn1 O10 171.58(11) 7_474 . ?
O7 Zn2 O3 110.57(10) 6_586 . ?
O7 Zn2 O5 123.24(10) 6_586 3_445 ?
O3 Zn2 O5 103.25(11) . 3_445 ?
O7 Zn2 O2 100.82(9) 6_586 6_576 ?
O3 Zn2 O2 120.23(9) . 6_576 ?
O5 Zn2 O2 99.58(9) 3_445 6_576 ?
C7 O1 Zn1 137.05(17) . . ?
C7 O2 Zn2 115.61(16) . 6_575 ?
C8 O3 Zn2 125.79(19) . . ?
C8 O4 Zn1 136.52(19) . 7_474 ?
C15 O5 Zn2 125.50(18) . 3 ?
C15 O6 Zn1 142.38(19) . 5_584 ?
C16 O7 Zn2 138.60(19) . 6_585 ?
C16 O8 Zn1 127.35(17) . 4_453 ?
C1 O9 C9 118.94(19) . . ?
O9 C1 C6 121.7(2) . . ?
O9 C1 C2 116.9(2) . . ?
C6 C1 C2 121.2(2) . . ?
C1 C2 C3 119.2(2) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C4 C3 C2 120.3(2) . . ?
C4 C3 C7 119.5(2) . . ?
C2 C3 C7 120.1(2) . . ?
C3 C4 C5 119.5(2) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C6 C5 C4 120.4(2) . . ?
C6 C5 C8 119.3(2) . . ?
C4 C5 C8 120.1(2) . . ?
C1 C6 C5 119.1(2) . . ?
C1 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
O1 C7 O2 121.6(2) . . ?
O1 C7 C3 121.4(2) . . ?
O2 C7 C3 117.0(2) . . ?
O4 C8 O3 126.1(3) . . ?
O4 C8 C5 119.1(2) . . ?
O3 C8 C5 114.8(2) . . ?
C10 C9 C14 121.3(2) . . ?
C10 C9 O9 116.3(2) . . ?
C14 C9 O9 122.1(2) . . ?
C9 C10 C11 119.1(2) . . ?
C9 C10 H10B 120.5 . . ?
C11 C10 H10B 120.5 . . ?
C12 C11 C10 120.2(2) . . ?
C12 C11 C15 120.2(2) . . ?
C10 C11 C15 119.4(2) . . ?
C13 C12 C11 120.3(2) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
C12 C13 C14 119.9(2) . . ?
C12 C13 C16 120.0(2) . . ?
C14 C13 C16 119.8(2) . . ?
C9 C14 C13 119.2(2) . . ?
C9 C14 H14A 120.4 . . ?
C13 C14 H14A 120.4 . . ?
O5 C15 O6 125.8(2) . . ?
O5 C15 C11 117.6(2) . . ?
O6 C15 C11 116.6(2) . . ?
O8 C16 O7 125.6(2) . . ?
O8 C16 C13 117.5(2) . . ?
O7 C16 C13 116.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.083
####################################################################### 
# 
# 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_MOF1
_database_code_depnum_ccdc_archive 'CCDC 1032697'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C30 H34 Co2 N2 O15 S2'
_chemical_formula_sum            'C30 H34 Co2 N2 O15 S2'
_chemical_formula_weight         844.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P3(1)21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   19.851(3)
_cell_length_b                   19.851(3)
_cell_length_c                   9.876(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3370.6(10)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5117
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.44

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1302
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31398
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         27.44
_reflns_number_total             5117
_reflns_number_gt                4095
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even largerFor the vibration of DMSO 
molecule , we use some restraints about the oxygen atoms from DMSO in the 
refinement.
 dfix 1.75 0.005 S1' C14',
dfix 1.75 0.005 S1' C15',
dfix 2.90 0.005 C14' C15',
eadp c14 c14',eadp c15 c15',isor 0.01 0.001 c14 c14' c15 c15',
DFIX 2.8 0.05 C14' C15'.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1325P)²+13.9736P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_number_reflns         5117
_refine_ls_number_parameters     233
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0951
_refine_ls_wR_factor_ref         0.2646
_refine_ls_wR_factor_gt          0.2540
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.48192(6) 0.91078(5) 0.23747(10) 0.0283(3) Uani 1 1 d . . .
S1' S 0.6443(3) 0.9252(4) 0.0984(6) 0.0607(14) Uani 0.50 1 d PD . .
S1 S 0.5439(14) 0.9614(5) -0.0767(8) 0.268(14) Uani 0.50 1 d P . .
O1 O 0.6025(5) 0.8908(4) 0.4457(10) 0.076(3) Uani 1 1 d . . .
O2 O 0.5097(3) 0.8283(3) 0.2899(7) 0.0387(14) Uani 1 1 d . . .
O3 O 0.4783(4) 0.5860(4) 0.0765(7) 0.0471(16) Uani 1 1 d . . .
O4 O 0.5454(5) 0.5336(4) 0.1683(10) 0.075(3) Uani 1 1 d . . .
O5 O 0.7295(4) 0.7295(4) 0.5000 0.0340(18) Uani 1 2 d S . .
O6 O 0.5583(7) 0.9305(6) 0.0627(9) 0.093(3) Uani 1 1 d . . .
O7 O 0.5841(3) 1.0000 0.3333 0.0313(17) Uani 1 2 d S . .
N1 N 0.3875(5) 0.8218(4) 0.1242(9) 0.053(2) Uani 1 1 d . . .
C1 C 0.5848(5) 0.7708(4) 0.3569(8) 0.0319(17) Uani 1 1 d . . .
C2 C 0.5438(5) 0.7078(5) 0.2668(8) 0.0330(17) Uani 1 1 d . . .
H2 H 0.5031 0.7038 0.2143 0.080 Uiso 1 1 calc . . .
C3 C 0.5662(5) 0.6532(5) 0.2597(9) 0.0320(17) Uani 1 1 d . . .
C4 C 0.6278(5) 0.6586(5) 0.3377(9) 0.0386(19) Uani 1 1 d . . .
H4 H 0.6432 0.6216 0.3298 0.080 Uiso 1 1 calc . . .
C5 C 0.6649(5) 0.7200(4) 0.4259(7) 0.0306(15) Uani 1 1 d . . .
C6 C 0.6448(5) 0.7761(4) 0.4354(9) 0.0338(17) Uani 1 1 d . . .
H6 H 0.6713 0.8178 0.4944 0.080 Uiso 1 1 calc . . .
C7 C 0.5643(5) 0.8361(5) 0.3665(9) 0.0396(19) Uani 1 1 d . . .
C8 C 0.5261(6) 0.5854(6) 0.1619(11) 0.050(3) Uani 1 1 d . . .
C9 C 0.3954(7) 0.7676(6) 0.0527(11) 0.057(3) Uani 1 1 d . . .
H9 H 0.4435 0.7703 0.0548 0.080 Uiso 1 1 calc . . .
C10 C 0.3393(10) 0.7110(8) -0.0199(13) 0.087(5) Uani 1 1 d . . .
H10 H 0.3468 0.6733 -0.0617 0.080 Uiso 1 1 calc . . .
C11 C 0.2708(10) 0.7099(8) -0.0310(15) 0.087(5) Uani 1 1 d . . .
H11 H 0.2311 0.6718 -0.0834 0.080 Uiso 1 1 calc . . .
C12 C 0.2596(8) 0.7638(9) 0.0334(17) 0.085(4) Uani 1 1 d . . .
H12 H 0.2133 0.7643 0.0242 0.080 Uiso 1 1 calc . . .
C13 C 0.3189(7) 0.8175(6) 0.1127(15) 0.072(4) Uani 1 1 d . . .
H13 H 0.3106 0.8529 0.1610 0.080 Uiso 1 1 calc . . .
C14' C 0.7235(16) 1.0091(9) 0.028(3) 0.120(9) Uani 0.50 1 d PDU . .
C15' C 0.6266(14) 0.8423(9) 0.005(2) 0.074(5) Uani 0.50 1 d PDU . .
C14 C 0.548(3) 1.063(2) -0.161(5) 0.120(9) Uani 0.50 1 d PU . .
C15 C 0.5219(17) 0.9340(18) -0.237(3) 0.074(5) Uani 0.50 1 d PU . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O4 2.000(7) 6_665 ?
Co1 O2 2.038(5) . ?
Co1 O3 2.087(6) 2_665 ?
Co1 O7 2.135(4) . ?
Co1 N1 2.139(8) . ?
Co1 O6 2.199(10) . ?
S1' C15' 1.761(5) . ?
S1' C14' 1.762(5) . ?
S1' O6 1.797(13) . ?
S1 C14 1.39(5) 5_674 ?
S1 O6 1.591(15) . ?
S1 C15 1.66(3) . ?
S1 C15 1.82(3) 5_674 ?
S1 C14 2.14(5) . ?
S1 S1 2.217(16) 5_674 ?
O1 C7 1.242(11) . ?
O2 C7 1.267(10) . ?
O3 C8 1.275(11) . ?
O3 Co1 2.087(6) 3_564 ?
O4 C8 1.266(10) . ?
O4 Co1 2.000(7) 6_655 ?
O5 C5 1.404(8) . ?
O5 C5 1.404(8) 4_556 ?
O7 Co1 2.135(4) 5_675 ?
N1 C13 1.325(15) . ?
N1 C9 1.360(13) . ?
C1 C6 1.379(11) . ?
C1 C2 1.414(11) . ?
C1 C7 1.544(10) . ?
C2 C3 1.364(11) . ?
C3 C4 1.404(11) . ?
C3 C8 1.519(11) . ?
C4 C5 1.374(11) . ?
C5 C6 1.363(10) . ?
C9 C10 1.329(17) . ?
C10 C11 1.35(2) . ?
C11 C12 1.36(2) . ?
C12 C13 1.372(17) . ?
C14 C15 0.99(5) 5_674 ?
C14 S1 1.39(5) 5_674 ?
C15 C14 0.99(5) 5_674 ?
C15 S1 1.82(3) 5_674 ?

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
O4 Co1 O2 173.7(3) 6_665 . ?
O4 Co1 O3 91.5(4) 6_665 2_665 ?
O2 Co1 O3 93.6(3) . 2_665 ?
O4 Co1 O7 91.8(2) 6_665 . ?
O2 Co1 O7 91.6(2) . . ?
O3 Co1 O7 92.7(2) 2_665 . ?
O4 Co1 N1 89.1(3) 6_665 . ?
O2 Co1 N1 87.0(3) . . ?
O3 Co1 N1 93.4(3) 2_665 . ?
O7 Co1 N1 173.8(3) . . ?
O4 Co1 O6 90.6(4) 6_665 . ?
O2 Co1 O6 84.4(4) . . ?
O3 Co1 O6 177.0(4) 2_665 . ?
O7 Co1 O6 85.2(3) . . ?
N1 Co1 O6 88.8(4) . . ?
C15' S1' C14' 110.2(4) . . ?
C15' S1' O6 101.5(10) . . ?
C14' S1' O6 107.0(14) . . ?
C14 S1 O6 138(2) 5_674 . ?
C14 S1 C15 36.7(19) 5_674 . ?
O6 S1 C15 140.2(15) . . ?
C14 S1 C15 99(2) 5_674 5_674 ?
O6 S1 C15 117.2(12) . 5_674 ?
C15 S1 C15 99.8(14) . 5_674 ?
C14 S1 C14 72(3) 5_674 . ?
O6 S1 C14 140.2(14) . . ?
C15 S1 C14 79.5(18) . . ?
C15 S1 C14 27.5(13) 5_674 . ?
C14 S1 S1 68.6(19) 5_674 5_674 ?
O6 S1 S1 153.3(9) . 5_674 ?
C15 S1 S1 53.5(11) . 5_674 ?
C15 S1 S1 47.3(9) 5_674 5_674 ?
C14 S1 S1 37.1(12) . 5_674 ?
C7 O2 Co1 127.8(5) . . ?
C8 O3 Co1 130.2(5) . 3_564 ?
C8 O4 Co1 142.3(6) . 6_655 ?
C5 O5 C5 116.9(8) . 4_556 ?
S1 O6 S1' 123.5(11) . . ?
S1 O6 Co1 120.5(12) . . ?
S1' O6 Co1 115.3(5) . . ?
Co1 O7 Co1 115.2(3) . 5_675 ?
C13 N1 C9 115.2(10) . . ?
C13 N1 Co1 123.1(8) . . ?
C9 N1 Co1 121.7(8) . . ?
C6 C1 C2 121.0(7) . . ?
C6 C1 C7 118.7(7) . . ?
C2 C1 C7 120.2(7) . . ?
C3 C2 C1 117.5(7) . . ?
C2 C3 C4 121.9(7) . . ?
C2 C3 C8 120.2(7) . . ?
C4 C3 C8 117.9(7) . . ?
C5 C4 C3 118.5(7) . . ?
C6 C5 C4 121.5(7) . . ?
C6 C5 O5 118.4(7) . . ?
C4 C5 O5 119.9(6) . . ?
C5 C6 C1 119.5(7) . . ?
O1 C7 O2 126.4(7) . . ?
O1 C7 C1 118.0(7) . . ?
O2 C7 C1 115.5(7) . . ?
O4 C8 O3 124.8(8) . . ?
O4 C8 C3 116.8(8) . . ?
O3 C8 C3 118.3(7) . . ?
C10 C9 N1 124.7(13) . . ?
C9 C10 C11 117.9(14) . . ?
C10 C11 C12 120.6(12) . . ?
C11 C12 C13 117.8(14) . . ?
N1 C13 C12 123.6(13) . . ?
C15 C14 S1 87(4) 5_674 5_674 ?
C15 C14 S1 58(3) 5_674 . ?
S1 C14 S1 74(2) 5_674 . ?
C14 C15 S1 57(3) 5_674 . ?
C14 C15 S1 95(4) 5_674 5_674 ?
S1 C15 S1 79.2(13) . 5_674 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.210
_refine_diff_density_min         -1.518
_refine_diff_density_rms         0.141

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.024 857 102 ' '
_platon_squeeze_details          
;
 three molcules of disordeded water
;
####################################################################### 
# 
# 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_MOF2
_database_code_depnum_ccdc_archive 'CCDC 1032698'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C32 H44 Co2 N4 O14'
_chemical_formula_sum            'C32 H44 Co2 N4 O14'
_chemical_formula_weight         826.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '

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

_cell_length_a                   10.1170(11)
_cell_length_b                   16.767(2)
_cell_length_c                   22.415(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3802.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9416
_cell_measurement_theta_min      1.52
_cell_measurement_theta_max      28.58

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            27558
_diffrn_reflns_av_R_equivalents  0.1570
_diffrn_reflns_av_sigmaI/netI    0.2911
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         28.58
_reflns_number_total             9416
_reflns_number_gt                3511
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
isor 0.02 0.02  C11 C15 C22 C10 O6 C21,
isor 0.002 0.001 N2 C1 C9 c7 C12 O7,
dfix 1.45 0.05 c21 c22,
dfix 1.45 0.05 C21 N2,
dfix 2.3 0.05 C21 C24,
dfix 2.3 0.05 N2 C22,
dfix 1.45 0.05 N2 C23.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0380P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_number_reflns         9416
_refine_ls_number_parameters     361
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.1759
_refine_ls_R_factor_gt           0.0779
_refine_ls_wR_factor_ref         0.1700
_refine_ls_wR_factor_gt          0.1567
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.98150(9) 0.88472(7) 0.63937(5) 0.0281(3) Uani 1 1 d . . .
Co2 Co 0.76740(9) 0.83612(7) 0.75616(5) 0.0318(3) Uani 1 1 d . . .
N1 N 0.8884(14) 0.7058(8) 0.9157(5) 0.122(5) Uani 1 1 d . . .
N2 N 0.502(2) 0.9865(11) 0.8306(8) 0.201(8) Uani 1 1 d DU . .
O1 O 1.0013(5) 0.9776(3) 0.9508(2) 0.0345(14) Uani 1 1 d . . .
O2 O 0.9503(4) 0.8925(3) 0.7368(3) 0.0337(15) Uani 1 1 d . . .
O3 O 1.0155(6) 0.9944(4) 0.6873(2) 0.0453(17) Uani 1 1 d . . .
O4 O 1.1565(6) 1.2387(4) 0.7863(2) 0.0385(16) Uani 1 1 d . . .
O5 O 1.0500(5) 1.2699(3) 0.8711(3) 0.0397(17) Uani 1 1 d . . .
O6 O 1.3898(5) 1.0790(4) 1.0692(3) 0.0407(18) Uani 1 1 d U . .
O7 O 1.3047(5) 1.1335(3) 1.1491(2) 0.0351(15) Uani 1 1 d U . .
O8 O 0.6910(5) 1.0774(4) 1.1040(2) 0.0381(17) Uani 1 1 d . . .
O9 O 0.8180(5) 1.1180(4) 1.1811(3) 0.0447(17) Uani 1 1 d . . .
O10 O 0.5829(6) 0.7792(4) 0.7658(3) 0.066(2) Uani 1 1 d . . .
O11 O 0.8379(6) 0.7859(4) 0.8377(3) 0.0494(19) Uani 1 1 d . . .
O12 O 0.6946(6) 0.9325(4) 0.8037(3) 0.061(2) Uani 1 1 d . . .
C1 C 1.0150(7) 1.0188(4) 0.8982(3) 0.0151(16) Uani 1 1 d U . .
C2 C 0.9970(7) 0.9761(4) 0.8471(3) 0.0264(19) Uani 1 1 d U . .
H2A H 0.9720 0.9229 0.8502 0.032 Uiso 1 1 calc R . .
C3 C 1.0135(8) 1.0074(5) 0.7932(3) 0.026(2) Uani 1 1 d . . .
C4 C 1.0517(7) 1.0865(5) 0.7888(4) 0.031(2) Uani 1 1 d . . .
H4A H 1.0678 1.1086 0.7515 0.038 Uiso 1 1 calc R . .
C5 C 1.0663(7) 1.1332(5) 0.8400(4) 0.023(2) Uani 1 1 d . . .
C6 C 1.0430(7) 1.0986(5) 0.8946(4) 0.032(2) Uani 1 1 d . . .
H6A H 1.0462 1.1294 0.9290 0.039 Uiso 1 1 calc R . .
C7 C 1.0170(9) 1.0192(5) 1.0028(4) 0.032(2) Uani 1 1 d U . .
C8 C 0.9077(8) 1.0388(5) 1.0379(3) 0.030(2) Uani 1 1 d . . .
H8A H 0.8237 1.0276 1.0233 0.036 Uiso 1 1 calc R . .
C9 C 0.9182(7) 1.0728(5) 1.0913(3) 0.0193(19) Uani 1 1 d U . .
C10 C 1.0450(6) 1.0941(5) 1.1130(3) 0.030(2) Uani 1 1 d U . .
H10A H 1.0544 1.1192 1.1498 0.035 Uiso 1 1 calc R . .
C11 C 1.1566(7) 1.0761(5) 1.0777(4) 0.026(2) Uani 1 1 d U . .
C12 C 1.1436(7) 1.0383(4) 1.0257(3) 0.0208(19) Uani 1 1 d U . .
H12A H 1.2187 1.0243 1.0041 0.025 Uiso 1 1 calc R . .
C13 C 0.9902(7) 0.9638(5) 0.7359(4) 0.0261(19) Uani 1 1 d U . .
C14 C 1.0926(7) 1.2207(6) 0.8323(4) 0.026(2) Uani 1 1 d . . .
C15 C 0.8015(7) 1.0916(5) 1.1315(4) 0.025(2) Uani 1 1 d U . .
C16 C 1.2929(7) 1.0978(5) 1.1017(4) 0.039(3) Uani 1 1 d U . .
C17 C 0.8293(11) 0.7219(7) 0.8628(6) 0.063(3) Uani 1 1 d . . .
C18 C 0.7536(10) 0.6574(7) 0.8408(4) 0.074(3) Uani 1 1 d . . .
H18A H 0.7598 0.6132 0.8679 0.100 Uiso 1 1 calc . . .
H18B H 0.7867 0.6417 0.8024 0.100 Uiso 1 1 calc . . .
H18C H 0.6629 0.6734 0.8371 0.100 Uiso 1 1 calc . . .
C19 C 0.9711(17) 0.7768(10) 0.9403(5) 0.140(7) Uani 1 1 d . . .
H19A H 1.0090 0.7623 0.9780 0.100 Uiso 1 1 calc . . .
H19B H 0.9150 0.8224 0.9454 0.100 Uiso 1 1 calc . . .
H19C H 1.0404 0.7894 0.9126 0.100 Uiso 1 1 calc . . .
C20 C 0.894(2) 0.6356(8) 0.9525(8) 0.175(9) Uani 1 1 d . . .
H20A H 0.9496 0.6457 0.9864 0.100 Uiso 1 1 calc . . .
H20B H 0.9297 0.5921 0.9298 0.100 Uiso 1 1 calc . . .
H20C H 0.8067 0.6222 0.9658 0.100 Uiso 1 1 calc . . .
C21 C 0.6009(17) 0.9532(10) 0.8435(8) 0.115(5) Uani 1 1 d DU . .
C22 C 0.6144(14) 0.9341(10) 0.9079(7) 0.139(6) Uani 1 1 d DU . .
H22A H 0.7001 0.9115 0.9152 0.100 Uiso 1 1 calc . . .
H22B H 0.5474 0.8965 0.9192 0.100 Uiso 1 1 calc . . .
H22C H 0.6044 0.9820 0.9309 0.100 Uiso 1 1 calc . . .
C23 C 0.3940(12) 1.0001(9) 0.8792(7) 0.128(6) Uani 1 1 d D . .
H23A H 0.3186 1.0256 0.8614 0.100 Uiso 1 1 calc . . .
H23B H 0.4289 1.0334 0.9102 0.100 Uiso 1 1 calc . . .
H23C H 0.3679 0.9497 0.8957 0.100 Uiso 1 1 calc . . .
C24 C 0.4907(15) 1.0015(7) 0.7668(7) 0.119(5) Uani 1 1 d D . .
H24A H 0.4069 1.0260 0.7586 0.100 Uiso 1 1 calc . . .
H24B H 0.4969 0.9520 0.7455 0.100 Uiso 1 1 calc . . .
H24C H 0.5606 1.0364 0.7543 0.100 Uiso 1 1 calc . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O5 1.966(6) 3_746 ?
Co1 O8 2.019(5) 2_674 ?
Co1 O6 2.131(6) 2_774 ?
Co1 O3 2.157(6) . ?
Co1 O7 2.195(5) 2_774 ?
Co1 O2 2.211(6) . ?
Co1 C16 2.451(8) 2_774 ?
Co2 O4 2.041(6) 3_746 ?
Co2 O9 2.042(6) 2_674 ?
Co2 O12 2.071(7) . ?
Co2 O10 2.108(6) . ?
Co2 O2 2.123(5) . ?
Co2 O11 2.134(7) . ?
N1 C17 1.355(14) . ?
N1 C20 1.439(15) . ?
N1 C19 1.556(16) . ?
N2 C21 1.18(2) . ?
N2 C24 1.456(18) . ?
N2 C23 1.562(19) . ?
O1 C7 1.368(8) . ?
O1 C1 1.374(8) . ?
O2 C13 1.261(8) . ?
O3 C13 1.232(9) . ?
O4 C14 1.254(9) . ?
O4 Co2 2.041(6) 3_756 ?
O5 C14 1.273(9) . ?
O5 Co1 1.966(6) 3_756 ?
O6 C16 1.262(8) . ?
O6 Co1 2.131(6) 2_775 ?
O7 C16 1.224(8) . ?
O7 Co1 2.195(5) 2_775 ?
O8 C15 1.299(9) . ?
O8 Co1 2.019(5) 2_675 ?
O9 C15 1.208(9) . ?
O9 Co2 2.042(6) 2_675 ?
O11 C17 1.215(11) . ?
O12 C21 1.348(16) . ?
C1 C2 1.362(9) . ?
C1 C6 1.369(10) . ?
C2 C3 1.328(9) . ?
C3 C4 1.384(10) . ?
C3 C13 1.497(10) . ?
C4 C5 1.396(10) . ?
C5 C6 1.375(10) . ?
C5 C14 1.502(11) . ?
C7 C8 1.396(10) . ?
C7 C12 1.416(10) . ?
C8 C9 1.330(10) . ?
C9 C10 1.417(9) . ?
C9 C15 1.519(10) . ?
C10 C11 1.412(10) . ?
C11 C12 1.334(10) . ?
C11 C16 1.525(10) . ?
C16 Co1 2.451(8) 2_775 ?
C17 C18 1.414(14) . ?
C21 C22 1.483(18) . ?

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
O5 Co1 O8 96.9(2) 3_746 2_674 ?
O5 Co1 O6 106.9(2) 3_746 2_774 ?
O8 Co1 O6 98.5(2) 2_674 2_774 ?
O5 Co1 O3 157.0(2) 3_746 . ?
O8 Co1 O3 93.7(2) 2_674 . ?
O6 Co1 O3 91.5(2) 2_774 . ?
O5 Co1 O7 92.0(2) 3_746 2_774 ?
O8 Co1 O7 159.1(2) 2_674 2_774 ?
O6 Co1 O7 60.7(2) 2_774 2_774 ?
O3 Co1 O7 85.0(2) . 2_774 ?
O5 Co1 O2 98.8(2) 3_746 . ?
O8 Co1 O2 104.24(19) 2_674 . ?
O6 Co1 O2 143.1(2) 2_774 . ?
O3 Co1 O2 58.69(19) . . ?
O7 Co1 O2 92.94(18) 2_774 . ?
O5 Co1 C16 103.1(3) 3_746 2_774 ?
O8 Co1 C16 129.2(2) 2_674 2_774 ?
O6 Co1 C16 31.0(2) 2_774 2_774 ?
O3 Co1 C16 85.5(3) . 2_774 ?
O7 Co1 C16 29.9(2) 2_774 2_774 ?
O2 Co1 C16 117.8(2) . 2_774 ?
O4 Co2 O9 94.4(2) 3_746 2_674 ?
O4 Co2 O12 176.7(3) 3_746 . ?
O9 Co2 O12 88.8(3) 2_674 . ?
O4 Co2 O10 91.1(3) 3_746 . ?
O9 Co2 O10 83.1(2) 2_674 . ?
O12 Co2 O10 89.2(3) . . ?
O4 Co2 O2 86.2(2) 3_746 . ?
O9 Co2 O2 91.9(2) 2_674 . ?
O12 Co2 O2 93.9(2) . . ?
O10 Co2 O2 174.1(3) . . ?
O4 Co2 O11 87.6(2) 3_746 . ?
O9 Co2 O11 174.5(2) 2_674 . ?
O12 Co2 O11 89.2(3) . . ?
O10 Co2 O11 91.7(3) . . ?
O2 Co2 O11 93.4(2) . . ?
C17 N1 C20 133.0(13) . . ?
C17 N1 C19 113.3(11) . . ?
C20 N1 C19 113.6(11) . . ?
C21 N2 C24 113(2) . . ?
C21 N2 C23 119.4(18) . . ?
C24 N2 C23 127.1(18) . . ?
C7 O1 C1 117.6(6) . . ?
C13 O2 Co2 134.8(5) . . ?
C13 O2 Co1 89.7(5) . . ?
Co2 O2 Co1 107.4(2) . . ?
C13 O3 Co1 93.0(5) . . ?
C14 O4 Co2 140.3(6) . 3_756 ?
C14 O5 Co1 127.4(6) . 3_756 ?
C16 O6 Co1 88.6(5) . 2_775 ?
C16 O7 Co1 86.7(5) . 2_775 ?
C15 O8 Co1 120.0(5) . 2_675 ?
C15 O9 Co2 146.9(5) . 2_675 ?
C17 O11 Co2 136.1(8) . . ?
C21 O12 Co2 142.4(9) . . ?
C2 C1 C6 119.4(7) . . ?
C2 C1 O1 116.3(6) . . ?
C6 C1 O1 124.3(7) . . ?
C3 C2 C1 122.7(8) . . ?
C2 C3 C4 118.6(8) . . ?
C2 C3 C13 124.6(8) . . ?
C4 C3 C13 116.8(7) . . ?
C3 C4 C5 120.5(8) . . ?
C6 C5 C4 118.4(8) . . ?
C6 C5 C14 123.0(8) . . ?
C4 C5 C14 118.2(8) . . ?
C1 C6 C5 120.1(7) . . ?
O1 C7 C8 120.5(8) . . ?
O1 C7 C12 121.9(8) . . ?
C8 C7 C12 117.4(7) . . ?
C9 C8 C7 123.0(8) . . ?
C8 C9 C10 119.3(7) . . ?
C8 C9 C15 124.1(7) . . ?
C10 C9 C15 116.6(7) . . ?
C11 C10 C9 118.5(7) . . ?
C12 C11 C10 120.9(7) . . ?
C12 C11 C16 120.7(7) . . ?
C10 C11 C16 118.3(7) . . ?
C11 C12 C7 120.8(7) . . ?
O3 C13 O2 118.3(8) . . ?
O3 C13 C3 121.5(7) . . ?
O2 C13 C3 120.0(8) . . ?
O4 C14 O5 125.5(8) . . ?
O4 C14 C5 114.8(8) . . ?
O5 C14 C5 119.7(8) . . ?
O9 C15 O8 128.5(7) . . ?
O9 C15 C9 121.0(7) . . ?
O8 C15 C9 110.4(7) . . ?
O7 C16 O6 123.2(7) . . ?
O7 C16 C11 120.7(7) . . ?
O6 C16 C11 116.0(7) . . ?
O7 C16 Co1 63.4(4) . 2_775 ?
O6 C16 Co1 60.4(4) . 2_775 ?
C11 C16 Co1 173.0(6) . 2_775 ?
O11 C17 N1 123.3(12) . . ?
O11 C17 C18 123.6(12) . . ?
N1 C17 C18 113.1(12) . . ?
N2 C21 O12 123.6(18) . . ?
N2 C21 C22 114.8(18) . . ?
O12 C21 C22 121.6(15) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        28.58
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.801
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.122



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.040 0.250 0.000 676 230 ' '
2 0.026 0.750 0.500 676 230 ' '
_platon_squeeze_details          
; 
two molcules of disordeded DMA
;
####################################################################### 
# 
# 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_MOF3
_database_code_depnum_ccdc_archive 'CCDC 1032699'
_audit_update_record             
;
2015-02-13 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C46 H62 Co4 O29 S7'
_chemical_formula_sum            'C46 H62 Co4 O29 S7'
_chemical_formula_weight         1539.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   21.818(4)
_cell_length_b                   14.704(3)
_cell_length_c                   26.282(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.84(3)
_cell_angle_gamma                90.00
_cell_volume                     6748(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11196
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3160
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7357
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            46716
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11196
_reflns_number_gt                9314
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1683P)²+54.6367P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11196
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.1127
_refine_ls_wR_factor_ref         0.2943
_refine_ls_wR_factor_gt          0.2865
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.35252(5) 0.35684(7) 0.85780(4) 0.0235(3) Uani 1 1 d . . .
Co4 Co 0.44070(6) 0.34273(7) 0.78265(5) 0.0245(3) Uani 1 1 d . . .
Co2 Co -0.07371(6) 0.31097(7) 0.65916(5) 0.0290(3) Uani 1 1 d . . .
Co3 Co -0.17963(6) 0.32545(7) 0.49178(5) 0.0303(3) Uani 1 1 d . . .
O1 O 0.3870(3) 0.4877(4) 0.8553(3) 0.0353(13) Uani 1 1 d . . .
O2 O 0.4191(4) 0.4733(4) 0.7887(3) 0.0460(16) Uani 1 1 d . . .
O3 O 0.5217(4) 0.7253(4) 0.7420(3) 0.0398(14) Uani 1 1 d . . .
O4 O 0.5269(4) 0.8608(4) 0.7776(3) 0.0370(13) Uani 1 1 d . . .
O5 O 0.5502(3) 0.7013(4) 1.1332(3) 0.0347(13) Uani 1 1 d . . .
O6 O 0.4486(3) 0.6659(5) 1.1274(3) 0.0421(15) Uani 1 1 d . . .
O7 O 0.1850(3) 0.7739(4) 0.9354(3) 0.0345(12) Uani 1 1 d . . .
O8 O 0.1772(3) 0.8114(5) 0.8510(3) 0.0445(15) Uani 1 1 d . . .
O9 O 0.4423(4) 0.8272(4) 0.9147(3) 0.0353(13) Uani 1 1 d . . .
O10 O 0.3330(3) 0.3015(5) 0.7156(3) 0.0434(15) Uani 1 1 d . . .
O11 O 0.2758(3) 0.3366(5) 0.7603(3) 0.0398(14) Uani 1 1 d . . .
O12 O 0.0006(3) 0.2758(6) 0.6402(3) 0.0533(18) Uani 1 1 d . . .
O13 O -0.0709(3) 0.2732(6) 0.5347(3) 0.0500(17) Uani 1 1 d . . .
O14 O -0.0018(4) 0.1684(4) 0.2593(3) 0.0414(15) Uani 1 1 d . . .
O15 O -0.0401(4) 0.3049(4) 0.2222(3) 0.0418(14) Uani 1 1 d . . .
O16 O 0.0821(5) 0.5583(5) 0.3652(3) 0.060(2) Uani 1 1 d . . .
O17 O 0.1357(4) 0.5476(4) 0.4686(3) 0.0449(15) Uani 1 1 d . . .
O18 O 0.1242(3) 0.2029(4) 0.4949(3) 0.0346(12) Uani 1 1 d . . .
C1 C 0.4461(4) 0.7663(5) 0.8777(4) 0.0292(16) Uani 1 1 d . . .
C2 C 0.4264(4) 0.6735(5) 0.8725(4) 0.0277(15) Uani 1 1 d . . .
H2 H 0.4083 0.6505 0.8942 0.100 Uiso 1 1 calc . . .
C3 C 0.4344(4) 0.6176(5) 0.8347(4) 0.0263(15) Uani 1 1 d . . .
C4 C 0.4634(5) 0.6504(6) 0.8035(4) 0.0347(18) Uani 1 1 d . . .
H4 H 0.4696 0.6113 0.7791 0.100 Uiso 1 1 calc . . .
C5 C 0.4827(4) 0.7392(5) 0.8086(4) 0.0297(16) Uani 1 1 d . . .
C6 C 0.4752(4) 0.7979(5) 0.8470(4) 0.0300(16) Uani 1 1 d . . .
H6 H 0.4901 0.8584 0.8516 0.100 Uiso 1 1 calc . . .
C7 C 0.4126(5) 0.5171(5) 0.8260(4) 0.0304(16) Uani 1 1 d . . .
C8 C 0.5129(5) 0.7765(6) 0.7743(4) 0.0340(18) Uani 1 1 d . . .
C9 C 0.4114(5) 0.7961(5) 0.9457(4) 0.0299(16) Uani 1 1 d . . .
C10 C 0.4598(5) 0.7661(5) 1.0074(4) 0.0311(17) Uani 1 1 d . . .
H10 H 0.5125 0.7657 1.0286 0.100 Uiso 1 1 calc . . .
C11 C 0.4290(4) 0.7367(5) 1.0378(4) 0.0281(15) Uani 1 1 d . . .
C12 C 0.3477(4) 0.7442(6) 1.0053(3) 0.0289(16) Uani 1 1 d . . .
H12 H 0.3261 0.7252 1.0251 0.100 Uiso 1 1 calc . . .
C13 C 0.3022(4) 0.7793(5) 0.9452(3) 0.0277(15) Uani 1 1 d . . .
C14 C 0.3337(5) 0.8054(6) 0.9144(4) 0.0356(18) Uani 1 1 d . . .
H14 H 0.3028 0.8287 0.8733 0.100 Uiso 1 1 calc . . .
C15 C 0.4768(4) 0.6996(6) 1.1011(3) 0.0292(16) Uani 1 1 d . . .
C16 C 0.2161(4) 0.7885(5) 0.9079(4) 0.0312(17) Uani 1 1 d . . .
C17 C 0.1263(4) 0.2357(5) 0.5455(3) 0.0286(16) Uani 1 1 d . . .
C18 C 0.1980(5) 0.2576(6) 0.6025(4) 0.0360(18) Uani 1 1 d . . .
H18 H 0.2427 0.2546 0.6056 0.100 Uiso 1 1 calc . . .
C19 C 0.1992(4) 0.2843(6) 0.6545(4) 0.0336(17) Uani 1 1 d . . .
C20 C 0.1343(4) 0.2883(6) 0.6501(3) 0.0314(17) Uani 1 1 d . . .
H20 H 0.1368 0.3067 0.6852 0.100 Uiso 1 1 calc . . .
C21 C 0.0640(5) 0.2652(6) 0.5941(4) 0.0327(17) Uani 1 1 d . . .
C22 C 0.0594(4) 0.2424(6) 0.5408(3) 0.0367(19) Uani 1 1 d . . .
H22 H 0.0120 0.2316 0.5022 0.100 Uiso 1 1 calc . . .
C23 C 0.2754(5) 0.3111(6) 0.7153(4) 0.038(2) Uani 1 1 d . . .
C24 C -0.0085(4) 0.2739(6) 0.5900(4) 0.0346(18) Uani 1 1 d . . .
C25 C 0.1001(4) 0.2639(6) 0.4465(3) 0.0282(16) Uani 1 1 d . . .
C26 C 0.0624(5) 0.2298(6) 0.3852(4) 0.0359(18) Uani 1 1 d . . .
H26 H 0.0539 0.1675 0.3781 0.100 Uiso 1 1 calc . . .
C27 C 0.0375(4) 0.2876(6) 0.3344(3) 0.0299(16) Uani 1 1 d . . .
C28 C 0.0493(5) 0.3797(6) 0.3443(3) 0.0340(18) Uani 1 1 d . . .
H28 H 0.0319 0.4183 0.3101 0.100 Uiso 1 1 calc . . .
C29 C 0.0872(4) 0.4158(5) 0.4052(4) 0.0282(15) Uani 1 1 d . . .
C30 C 0.1122(4) 0.3575(6) 0.4575(3) 0.0286(16) Uani 1 1 d . . .
H30 H 0.1361 0.3811 0.4981 0.100 Uiso 1 1 calc . . .
C31 C -0.0045(5) 0.2530(7) 0.2675(4) 0.0367(19) Uani 1 1 d . . .
C32 C 0.1028(5) 0.5177(6) 0.4138(4) 0.0382(19) Uani 1 1 d . . .
O19 O 0.2596(4) 0.4171(5) 0.8519(4) 0.0703(8) Uani 1 1 d . . .
S1 S 0.20933(18) 0.4885(2) 0.80462(17) 0.0703(8) Uani 1 1 d . . .
C33 C 0.2260(7) 0.5929(8) 0.8392(7) 0.0703(8) Uani 1 1 d . . .
H33A H 0.2776 0.6113 0.8578 0.100 Uiso 1 1 calc . . .
H33B H 0.2186 0.5897 0.8717 0.100 Uiso 1 1 calc . . .
H33C H 0.1910 0.6364 0.8076 0.100 Uiso 1 1 calc . . .
C34 C 0.1207(7) 0.4582(8) 0.7733(7) 0.0703(8) Uani 1 1 d . . .
H34A H 0.1103 0.4001 0.7529 0.100 Uiso 1 1 calc . . .
H34B H 0.0860 0.5027 0.7425 0.100 Uiso 1 1 calc . . .
H34C H 0.1140 0.4542 0.8061 0.100 Uiso 1 1 calc . . .
O20 O -0.2884(5) 0.3828(7) 0.4457(5) 0.0831(10) Uani 1 1 d . . .
S2 S -0.3356(2) 0.4275(3) 0.38407(18) 0.0831(10) Uani 1 1 d . . .
C35 C -0.4246(8) 0.4413(11) 0.3657(7) 0.0831(10) Uani 1 1 d . . .
H35A H -0.4489 0.3830 0.3569 0.100 Uiso 1 1 calc . . .
H35B H -0.4548 0.4795 0.3289 0.100 Uiso 1 1 calc . . .
H35C H -0.4200 0.4690 0.4009 0.100 Uiso 1 1 calc . . .
C36 C -0.3054(8) 0.5384(11) 0.3992(7) 0.0831(10) Uani 1 1 d . . .
H36A H -0.2547 0.5419 0.4106 0.100 Uiso 1 1 calc . . .
H36B H -0.3051 0.5611 0.4336 0.100 Uiso 1 1 calc . . .
H36C H -0.3396 0.5745 0.3619 0.100 Uiso 1 1 calc . . .
O21 O 0.4067(4) 0.3637(5) 0.9574(3) 0.0415(15) Uani 1 1 d . . .
O22 O 0.3312(4) 0.2223(4) 0.8689(4) 0.0488(16) Uani 1 1 d . . .
O23 O -0.1789(4) 0.3706(6) 0.4153(3) 0.0555(18) Uani 1 1 d . . .
O24 O -0.2307(5) 0.2029(5) 0.4420(4) 0.068(2) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O11 2.078(6) . ?
Co1 O1 2.081(6) . ?
Co1 O22 2.092(6) . ?
Co1 O19 2.131(8) . ?
Co1 O21 2.134(6) . ?
Co1 O5 2.164(5) 3_667 ?
Co4 O2 2.005(6) . ?
Co4 O10 2.007(6) . ?
Co4 O4 2.101(5) 2_646 ?
Co4 O6 2.143(6) 3_667 ?
Co4 O3 2.170(6) 2_646 ?
Co4 O5 2.197(6) 3_667 ?
Co4 C8 2.457(7) 2_646 ?
Co2 O16 1.999(7) 3_566 ?
Co2 O12 2.028(6) . ?
Co2 O8 2.109(6) 2_546 ?
Co2 O14 2.127(6) 4_566 ?
Co2 O15 2.174(6) 4_566 ?
Co2 O7 2.265(6) 2_546 ?
Co2 C31 2.474(8) 4_566 ?
Co2 C16 2.511(8) 2_546 ?
Co3 O13 2.069(6) . ?
Co3 O17 2.072(6) 3_566 ?
Co3 O20 2.089(9) . ?
Co3 O24 2.109(8) . ?
Co3 O23 2.125(6) . ?
Co3 O7 2.126(6) 2_546 ?
O1 C7 1.267(9) . ?
O2 C7 1.251(10) . ?
O3 C8 1.233(10) . ?
O3 Co4 2.170(6) 2_656 ?
O4 C8 1.268(11) . ?
O4 Co4 2.101(5) 2_656 ?
O5 C15 1.287(10) . ?
O5 Co1 2.164(5) 3_667 ?
O5 Co4 2.197(6) 3_667 ?
O6 C15 1.268(9) . ?
O6 Co4 2.143(6) 3_667 ?
O7 C16 1.272(10) . ?
O7 Co3 2.126(6) 2_556 ?
O7 Co2 2.265(6) 2_556 ?
O8 C16 1.244(10) . ?
O8 Co2 2.109(6) 2_556 ?
O9 C1 1.361(9) . ?
O9 C9 1.409(9) . ?
O10 C23 1.260(11) . ?
O11 C23 1.234(10) . ?
O12 C24 1.211(11) . ?
O13 C24 1.263(10) . ?
O14 C31 1.269(11) . ?
O14 Co2 2.127(6) 4_565 ?
O15 C31 1.224(11) . ?
O15 Co2 2.174(6) 4_565 ?
O16 C32 1.226(11) . ?
O16 Co2 1.999(7) 3_566 ?
O17 C32 1.241(10) . ?
O17 Co3 2.072(6) 3_566 ?
O18 C25 1.377(9) . ?
O18 C17 1.388(9) . ?
C1 C6 1.372(11) . ?
C1 C2 1.412(11) . ?
C2 C3 1.378(11) . ?
C3 C4 1.389(10) . ?
C3 C7 1.528(10) . ?
C4 C5 1.353(12) . ?
C5 C6 1.411(11) . ?
C5 C8 1.502(10) . ?
C8 Co4 2.457(7) 2_656 ?
C9 C10 1.374(12) . ?
C9 C14 1.377(12) . ?
C10 C11 1.386(11) . ?
C11 C15 1.439(11) . ?
C11 C12 1.440(10) . ?
C12 C13 1.367(11) . ?
C13 C14 1.394(12) . ?
C13 C16 1.516(10) . ?
C16 Co2 2.510(8) 2_556 ?
C17 C22 1.394(12) . ?
C17 C18 1.409(11) . ?
C18 C19 1.406(11) . ?
C19 C20 1.352(12) . ?
C19 C23 1.512(11) . ?
C20 C21 1.389(11) . ?
C21 C22 1.383(11) . ?
C21 C24 1.526(11) . ?
C25 C26 1.393(10) . ?
C25 C30 1.398(12) . ?
C26 C27 1.389(12) . ?
C27 C28 1.374(12) . ?
C27 C31 1.501(10) . ?
C28 C29 1.393(11) . ?
C29 C30 1.422(11) . ?
C29 C32 1.523(12) . ?
C31 Co2 2.474(8) 4_565 ?
O19 S1 1.487(8) . ?
S1 C34 1.646(13) . ?
S1 C33 1.710(13) . ?
O20 S2 1.455(9) . ?
S2 C35 1.708(14) . ?
S2 C36 1.714(17) . ?

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
O11 Co1 O1 97.6(3) . . ?
O11 Co1 O22 87.4(3) . . ?
O1 Co1 O22 173.3(3) . . ?
O11 Co1 O19 86.7(3) . . ?
O1 Co1 O19 87.7(3) . . ?
O22 Co1 O19 97.0(3) . . ?
O11 Co1 O21 164.7(3) . . ?
O1 Co1 O21 92.9(2) . . ?
O22 Co1 O21 83.1(3) . . ?
O19 Co1 O21 82.7(3) . . ?
O11 Co1 O5 95.2(2) . 3_667 ?
O1 Co1 O5 91.1(2) . 3_667 ?
O22 Co1 O5 84.1(2) . 3_667 ?
O19 Co1 O5 177.9(3) . 3_667 ?
O21 Co1 O5 95.7(2) . 3_667 ?
O2 Co4 O10 98.7(3) . . ?
O2 Co4 O4 98.0(2) . 2_646 ?
O10 Co4 O4 97.0(3) . 2_646 ?
O2 Co4 O6 97.6(3) . 3_667 ?
O10 Co4 O6 154.5(3) . 3_667 ?
O4 Co4 O6 100.0(2) 2_646 3_667 ?
O2 Co4 O3 159.0(2) . 2_646 ?
O10 Co4 O3 87.2(3) . 2_646 ?
O4 Co4 O3 61.2(2) 2_646 2_646 ?
O6 Co4 O3 84.5(3) 3_667 2_646 ?
O2 Co4 O5 94.9(2) . 3_667 ?
O10 Co4 O5 98.4(2) . 3_667 ?
O4 Co4 O5 158.1(2) 2_646 3_667 ?
O6 Co4 O5 60.6(2) 3_667 3_667 ?
O3 Co4 O5 104.1(2) 2_646 3_667 ?
O2 Co4 C8 129.0(3) . 2_646 ?
O10 Co4 C8 92.2(3) . 2_646 ?
O4 Co4 C8 31.1(3) 2_646 2_646 ?
O6 Co4 C8 92.6(3) 3_667 2_646 ?
O3 Co4 C8 30.1(3) 2_646 2_646 ?
O5 Co4 C8 132.5(2) 3_667 2_646 ?
O16 Co2 O12 95.8(3) 3_566 . ?
O16 Co2 O8 94.1(3) 3_566 2_546 ?
O12 Co2 O8 157.4(3) . 2_546 ?
O16 Co2 O14 96.7(2) 3_566 4_566 ?
O12 Co2 O14 103.5(3) . 4_566 ?
O8 Co2 O14 95.5(3) 2_546 4_566 ?
O16 Co2 O15 157.1(2) 3_566 4_566 ?
O12 Co2 O15 91.9(3) . 4_566 ?
O8 Co2 O15 86.9(3) 2_546 4_566 ?
O14 Co2 O15 60.5(2) 4_566 4_566 ?
O16 Co2 O7 92.8(3) 3_566 2_546 ?
O12 Co2 O7 99.1(2) . 2_546 ?
O8 Co2 O7 60.0(2) 2_546 2_546 ?
O14 Co2 O7 154.4(2) 4_566 2_546 ?
O15 Co2 O7 107.3(2) 4_566 2_546 ?
O16 Co2 C31 127.5(3) 3_566 4_566 ?
O12 Co2 C31 99.2(3) . 4_566 ?
O8 Co2 C31 90.9(3) 2_546 4_566 ?
O14 Co2 C31 30.9(3) 4_566 4_566 ?
O15 Co2 C31 29.7(3) 4_566 4_566 ?
O7 Co2 C31 133.2(3) 2_546 4_566 ?
O16 Co2 C16 93.7(3) 3_566 2_546 ?
O12 Co2 C16 129.0(3) . 2_546 ?
O8 Co2 C16 29.6(3) 2_546 2_546 ?
O14 Co2 C16 124.8(3) 4_566 2_546 ?
O15 Co2 C16 98.2(3) 4_566 2_546 ?
O7 Co2 C16 30.4(2) 2_546 2_546 ?
C31 Co2 C16 113.7(3) 4_566 2_546 ?
O13 Co3 O17 91.6(3) . 3_566 ?
O13 Co3 O20 177.0(3) . . ?
O17 Co3 O20 87.1(4) 3_566 . ?
O13 Co3 O24 91.6(3) . . ?
O17 Co3 O24 174.0(3) 3_566 . ?
O20 Co3 O24 89.5(4) . . ?
O13 Co3 O23 88.6(3) . . ?
O17 Co3 O23 86.0(3) 3_566 . ?
O20 Co3 O23 88.6(3) . . ?
O24 Co3 O23 88.9(3) . . ?
O13 Co3 O7 92.3(2) . 2_546 ?
O17 Co3 O7 97.3(2) 3_566 2_546 ?
O20 Co3 O7 90.5(3) . 2_546 ?
O24 Co3 O7 87.7(3) . 2_546 ?
O23 Co3 O7 176.5(3) . 2_546 ?
C7 O1 Co1 129.3(5) . . ?
C7 O2 Co4 134.2(6) . . ?
C8 O3 Co4 87.9(5) . 2_656 ?
C8 O4 Co4 90.1(4) . 2_656 ?
C15 O5 Co1 144.9(5) . 3_667 ?
C15 O5 Co4 88.8(4) . 3_667 ?
Co1 O5 Co4 106.4(2) 3_667 3_667 ?
C15 O6 Co4 91.7(5) . 3_667 ?
C16 O7 Co3 141.9(5) . 2_556 ?
C16 O7 Co2 85.5(4) . 2_556 ?
Co3 O7 Co2 107.5(2) 2_556 2_556 ?
C16 O8 Co2 93.4(5) . 2_556 ?
C1 O9 C9 117.1(6) . . ?
C23 O10 Co4 127.6(5) . . ?
C23 O11 Co1 139.7(6) . . ?
C24 O12 Co2 129.7(6) . . ?
C24 O13 Co3 135.8(6) . . ?
C31 O14 Co2 89.8(5) . 4_565 ?
C31 O15 Co2 88.9(5) . 4_565 ?
C32 O16 Co2 135.0(7) . 3_566 ?
C32 O17 Co3 132.3(6) . 3_566 ?
C25 O18 C17 115.7(6) . . ?
O9 C1 C6 116.5(7) . . ?
O9 C1 C2 124.0(7) . . ?
C6 C1 C2 119.4(7) . . ?
C3 C2 C1 118.9(7) . . ?
C2 C3 C4 121.2(7) . . ?
C2 C3 C7 121.6(6) . . ?
C4 C3 C7 117.3(7) . . ?
C5 C4 C3 120.2(8) . . ?
C4 C5 C6 119.8(7) . . ?
C4 C5 C8 121.0(7) . . ?
C6 C5 C8 119.2(7) . . ?
C1 C6 C5 120.5(7) . . ?
O2 C7 O1 126.8(7) . . ?
O2 C7 C3 116.4(6) . . ?
O1 C7 C3 116.7(6) . . ?
O3 C8 O4 120.8(7) . . ?
O3 C8 C5 119.8(8) . . ?
O4 C8 C5 119.4(7) . . ?
O3 C8 Co4 62.0(4) . 2_656 ?
O4 C8 Co4 58.8(4) . 2_656 ?
C5 C8 Co4 177.8(7) . 2_656 ?
C10 C9 C14 122.5(7) . . ?
C10 C9 O9 119.4(7) . . ?
C14 C9 O9 117.8(7) . . ?
C9 C10 C11 119.1(7) . . ?
C10 C11 C15 121.2(7) . . ?
C10 C11 C12 119.0(7) . . ?
C15 C11 C12 119.8(7) . . ?
C13 C12 C11 119.8(7) . . ?
C12 C13 C14 120.4(7) . . ?
C12 C13 C16 122.7(7) . . ?
C14 C13 C16 116.8(7) . . ?
C9 C14 C13 119.0(8) . . ?
O6 C15 O5 118.1(7) . . ?
O6 C15 C11 121.6(7) . . ?
O5 C15 C11 120.3(7) . . ?
O8 C16 O7 121.1(7) . . ?
O8 C16 C13 119.3(7) . . ?
O7 C16 C13 119.6(7) . . ?
O8 C16 Co2 57.0(4) . 2_556 ?
O7 C16 Co2 64.1(4) . 2_556 ?
C13 C16 Co2 176.0(6) . 2_556 ?
O18 C17 C22 120.6(7) . . ?
O18 C17 C18 118.5(7) . . ?
C22 C17 C18 120.9(7) . . ?
C19 C18 C17 117.4(7) . . ?
C20 C19 C18 121.4(7) . . ?
C20 C19 C23 120.7(7) . . ?
C18 C19 C23 117.9(7) . . ?
C19 C20 C21 121.0(7) . . ?
C22 C21 C20 119.7(7) . . ?
C22 C21 C24 120.5(7) . . ?
C20 C21 C24 119.6(7) . . ?
C21 C22 C17 119.5(7) . . ?
O11 C23 O10 126.4(8) . . ?
O11 C23 C19 117.6(8) . . ?
O10 C23 C19 115.9(7) . . ?
O12 C24 O13 128.0(8) . . ?
O12 C24 C21 116.0(7) . . ?
O13 C24 C21 115.9(8) . . ?
O18 C25 C26 117.9(7) . . ?
O18 C25 C30 122.0(6) . . ?
C26 C25 C30 120.1(7) . . ?
C27 C26 C25 120.7(8) . . ?
C28 C27 C26 120.0(7) . . ?
C28 C27 C31 118.0(7) . . ?
C26 C27 C31 122.0(8) . . ?
C27 C28 C29 120.5(7) . . ?
C28 C29 C30 120.0(7) . . ?
C28 C29 C32 118.1(7) . . ?
C30 C29 C32 121.8(7) . . ?
C25 C30 C29 118.6(7) . . ?
O15 C31 O14 120.8(7) . . ?
O15 C31 C27 120.9(8) . . ?
O14 C31 C27 118.3(8) . . ?
O15 C31 Co2 61.5(4) . 4_565 ?
O14 C31 Co2 59.3(4) . 4_565 ?
C27 C31 Co2 177.4(7) . 4_565 ?
O16 C32 O17 129.3(9) . . ?
O16 C32 C29 114.5(8) . . ?
O17 C32 C29 116.2(7) . . ?
S1 O19 Co1 123.2(6) . . ?
O19 S1 C34 106.5(6) . . ?
O19 S1 C33 112.0(6) . . ?
C34 S1 C33 108.6(6) . . ?
S2 O20 Co3 128.9(6) . . ?
O20 S2 C35 107.1(6) . . ?
O20 S2 C36 104.8(7) . . ?
C35 S2 C36 99.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         2.796
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.169


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.001 -0.033 0.012 3281 1031 ' '
_platon_squeeze_details          
;
five molcules of disordeded DMSO
;
