# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_296
_database_code_depnum_ccdc_archive 'CCDC 1552190'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_296                 
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.55 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_RINTA01_296                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_296                 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.225 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT026_296                 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         38 %
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2794(13)
_cell_length_b                   15.2794(13)
_cell_length_c                   18.9886(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4433.1(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1507
_cell_measurement_temperature    296
_cell_measurement_theta_max      57.78
_cell_measurement_theta_min      5.712
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.854
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2246
_diffrn_reflns_av_unetI/netI     0.1628
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11395
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.890
_diffrn_reflns_theta_min         2.856
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                568
_reflns_number_total             1507
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1507
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1726
_refine_ls_R_factor_gt           0.0830
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0870P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2375
_refine_special_details          ', SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-Co1
 2.09 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq, Uanis(C4B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C4B(0.5) C4A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.57126(6) 0.0445(6) Uani 1 4 d DS T P A .
O1 O 0.3905(3) 0.5714(3) 0.55800(19) 0.0795(15) Uani 1 1 d . . . . .
C1 C 0.3604(6) 0.5936(6) 0.5000 0.068(3) Uani 1 2 d S T P . .
C2 C 0.2866(6) 0.6541(7) 0.5000 0.077(3) Uani 1 2 d S T P . .
C3 C 0.2534(5) 0.6904(5) 0.5647(3) 0.114(3) Uani 1 1 d . . . . .
H3 H 0.2755 0.6704 0.6074 0.136 Uiso 1 1 calc R . . . .
N1 N 0.5000 0.5000 0.6828(3) 0.043(2) Uani 1 4 d DS T P . .
C4B C 0.4052(9) 0.4810(11) 0.7104(7) 0.067(4) Uani 0.5 1 d . U . A 1
C4A C 0.4527(11) 0.4191(9) 0.7104(7) 0.070(4) Uani 0.5 1 d . U . A 2


_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 Co1 2.706(2) 17_666 ?
Co1 O1 2.013(4) 4_565 ?
Co1 O1 2.013(4) 2_655 ?
Co1 O1 2.013(4) 3_665 ?
Co1 O1 2.013(4) . ?
Co1 N1 2.118(6) . ?
O1 C1 1.241(5) . ?
C1 O1 1.241(5) 19_556 ?
C1 C2 1.458(12) . ?
C2 C3 1.440(7) . ?
C2 C3 1.440(7) 19_556 ?
C3 C3 1.361(13) 32_455 ?
N1 C4B 1.567(14) . ?
N1 C4B 1.567(14) 2_655 ?
N1 C4B 1.567(14) 4_565 ?
N1 C4B 1.567(14) 3_665 ?
N1 C4A 1.525(13) . ?
N1 C4A 1.525(13) 4_565 ?
N1 C4A 1.525(13) 3_665 ?
N1 C4A 1.525(13) 2_655 ?
C4B C4B 1.61(3) 5_566 ?
C4A C4A 2.026(18) 4_565 ?
C4A C4A 2.026(18) 2_655 ?
C4A C4A 1.67(3) 7_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 82.82(11) 2_655 17_666 ?
O1 Co1 Co1 82.81(11) . 17_666 ?
O1 Co1 Co1 82.82(11) 4_565 17_666 ?
O1 Co1 Co1 82.82(11) 3_665 17_666 ?
O1 Co1 O1 89.10(3) 4_565 . ?
O1 Co1 O1 89.11(3) 2_655 . ?
O1 Co1 O1 89.10(3) 4_565 3_665 ?
O1 Co1 O1 165.6(2) 3_665 . ?
O1 Co1 O1 165.6(2) 2_655 4_565 ?
O1 Co1 O1 89.10(3) 2_655 3_665 ?
O1 Co1 N1 97.18(11) 2_655 . ?
O1 Co1 N1 97.18(11) 4_565 . ?
O1 Co1 N1 97.18(11) 3_665 . ?
O1 Co1 N1 97.19(11) . . ?
N1 Co1 Co1 180.0 . 17_666 ?
C1 O1 Co1 124.6(5) . . ?
O1 C1 O1 125.1(9) . 19_556 ?
O1 C1 C2 117.4(4) 19_556 . ?
O1 C1 C2 117.4(4) . . ?
C3 C2 C1 121.1(4) . . ?
C3 C2 C1 121.1(4) 19_556 . ?
C3 C2 C3 117.1(9) 19_556 . ?
C3 C3 C2 121.4(4) 32_455 . ?
C4B N1 Co1 109.6(6) 3_665 . ?
C4B N1 Co1 109.6(6) . . ?
C4B N1 Co1 109.6(6) 4_565 . ?
C4B N1 Co1 109.6(6) 2_655 . ?
C4B N1 C4B 140.9(11) 4_565 2_655 ?
C4B N1 C4B 83.6(4) 3_665 4_565 ?
C4B N1 C4B 83.6(4) 3_665 2_655 ?
C4B N1 C4B 83.6(4) . 4_565 ?
C4B N1 C4B 140.9(11) . 3_665 ?
C4B N1 C4B 83.6(4) . 2_655 ?
C4A N1 Co1 110.1(6) . . ?
C4A N1 Co1 110.1(6) 4_565 . ?
C4A N1 Co1 110.1(6) 3_665 . ?
C4A N1 Co1 110.1(6) 2_655 . ?
C4A N1 C4A 83.2(4) 3_665 2_655 ?
C4A N1 C4A 83.2(4) 3_665 4_565 ?
C4A N1 C4A 139.8(11) . 3_665 ?
C4A N1 C4A 83.2(4) . 4_565 ?
C4A N1 C4A 139.8(11) 2_655 4_565 ?
C4A N1 C4A 83.2(4) . 2_655 ?
N1 C4B C4B 104.2(7) . 5_566 ?
N1 C4A C4A 48.39(19) . 2_655 ?
N1 C4A C4A 101.9(8) . 7_556 ?
N1 C4A C4A 48.39(19) . 4_565 ?
C4A C4A C4A 102.7(3) 7_556 2_655 ?
C4A C4A C4A 90.001(7) 4_565 2_655 ?
C4A C4A C4A 68.0(12) 7_556 4_565 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.408 -0.658 -0.257 2676.1 624.1 4DMF.H2O


_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_exptl_crystal_preparation       ', piezochromic'
####################################################################### 
# 
# 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_273
_database_code_depnum_ccdc_archive 'CCDC 1552191'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_273                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_273                 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.232 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT026_273                 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         37 %
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT084_273                 
;
PROBLEM: High wR2 Value (i.e. &gt; 0.25) ...................       0.38 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT341_273                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01525 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT430_273                 
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.60 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2735(15)
_cell_length_b                   15.2735(15)
_cell_length_c                   18.9723(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4425.8(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1505
_cell_measurement_temperature    273
_cell_measurement_theta_max      58.828
_cell_measurement_theta_min      5.716
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.856
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2320
_diffrn_reflns_av_unetI/netI     0.1634
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11401
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.914
_diffrn_reflns_theta_min         2.858
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                561
_reflns_number_total             1505
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1505
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.2434
_refine_ls_R_factor_gt           0.1134
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3037
_refine_ls_wR_factor_ref         0.3818
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C4B, C4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4B \\sim C4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C4B(0.5) C4A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.57123(8) 0.0446(8) Uani 1 4 d S T P A .
O1 O 0.3896(4) 0.5711(5) 0.5587(3) 0.080(2) Uani 1 1 d . . . . .
C1 C 0.3578(8) 0.5933(9) 0.5000 0.063(4) Uani 1 2 d S T P . .
C2 C 0.2848(9) 0.6541(10) 0.5000 0.074(4) Uani 1 2 d S T P . .
C3 C 0.2542(9) 0.6880(8) 0.5618(4) 0.108(5) Uani 1 1 d . . . . .
H3 H 0.2767 0.6678 0.6044 0.129 Uiso 1 1 calc R . . . .
N1 N 0.5000 0.5000 0.6815(5) 0.042(3) Uani 1 4 d S T P . .
C4B C 0.4224(14) 0.4502(15) 0.7064(12) 0.081(6) Uani 0.5 1 d . U . A 1
C4A C 0.4832(14) 0.4019(12) 0.7076(11) 0.067(5) Uani 0.5 1 d . U . A 2


_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 Co1 2.703(3) 17_666 ?
Co1 O1 2.020(7) 4_565 ?
Co1 O1 2.020(7) 2_655 ?
Co1 O1 2.020(7) 3_665 ?
Co1 O1 2.020(7) . ?
Co1 N1 2.091(10) . ?
O1 C1 1.261(8) . ?
C1 O1 1.261(8) 19_556 ?
C1 C2 1.451(16) . ?
C2 C3 1.364(11) 19_556 ?
C2 C3 1.364(11) . ?
C3 C3 1.43(2) 32_455 ?
N1 C4B 1.48(2) . ?
N1 C4B 1.48(2) 4_565 ?
N1 C4B 1.48(2) 3_665 ?
N1 C4B 1.48(2) 2_655 ?
N1 C4A 1.599(19) 3_665 ?
N1 C4A 1.599(19) . ?
N1 C4A 1.599(19) 4_565 ?
N1 C4A 1.599(19) 2_655 ?
C4B C4B 1.76(5) 7_556 ?
C4B C4B 1.99(3) 4_565 ?
C4B C4B 1.99(3) 2_655 ?
C4A C4A 1.69(4) 6_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 83.23(17) 2_655 17_666 ?
O1 Co1 Co1 83.23(17) . 17_666 ?
O1 Co1 Co1 83.23(17) 4_565 17_666 ?
O1 Co1 Co1 83.23(17) 3_665 17_666 ?
O1 Co1 O1 89.20(4) 4_565 . ?
O1 Co1 O1 89.20(4) 2_655 . ?
O1 Co1 O1 89.20(4) 4_565 3_665 ?
O1 Co1 O1 166.5(3) 3_665 . ?
O1 Co1 O1 166.5(3) 2_655 4_565 ?
O1 Co1 O1 89.20(4) 2_655 3_665 ?
O1 Co1 N1 96.77(17) 2_655 . ?
O1 Co1 N1 96.77(17) 4_565 . ?
O1 Co1 N1 96.77(17) 3_665 . ?
O1 Co1 N1 96.77(17) . . ?
N1 Co1 Co1 180.0 . 17_666 ?
C1 O1 Co1 124.7(7) . . ?
O1 C1 O1 124.0(12) 19_556 . ?
O1 C1 C2 117.9(6) . . ?
O1 C1 C2 117.9(6) 19_556 . ?
C3 C2 C1 120.4(7) 19_556 . ?
C3 C2 C1 120.4(7) . . ?
C3 C2 C3 118.6(13) . 19_556 ?
C2 C3 C3 120.7(6) . 32_455 ?
C4B N1 Co1 108.6(9) 3_665 . ?
C4B N1 Co1 108.6(9) . . ?
C4B N1 Co1 108.6(9) 4_565 . ?
C4B N1 Co1 108.6(9) 2_655 . ?
C4B N1 C4B 142.9(19) 4_565 2_655 ?
C4B N1 C4B 84.2(6) . 2_655 ?
C4B N1 C4B 84.2(6) 3_665 2_655 ?
C4B N1 C4B 84.2(6) 3_665 4_565 ?
C4B N1 C4B 142.9(19) . 3_665 ?
C4B N1 C4B 84.2(6) . 4_565 ?
C4A N1 Co1 108.0(8) 3_665 . ?
C4A N1 Co1 108.0(8) . . ?
C4A N1 Co1 108.0(8) 2_655 . ?
C4A N1 Co1 108.0(8) 4_565 . ?
C4A N1 C4A 84.5(5) 3_665 4_565 ?
C4A N1 C4A 84.5(5) 3_665 2_655 ?
C4A N1 C4A 143.9(16) 3_665 . ?
C4A N1 C4A 143.9(16) 2_655 4_565 ?
C4A N1 C4A 84.5(5) 2_655 . ?
C4A N1 C4A 84.5(5) 4_565 . ?
N1 C4B C4B 47.9(3) . 2_655 ?
N1 C4B C4B 47.9(3) . 4_565 ?
N1 C4B C4B 103.3(11) . 7_556 ?
C4B C4B C4B 73.3(15) 7_556 2_655 ?
C4B C4B C4B 90.000(10) 2_655 4_565 ?
C4B C4B C4B 100.6(6) 7_556 4_565 ?
N1 C4A C4A 104.3(9) . 6_656 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.874 -0.160 -0.526 2786.0 255.0 4DMF.H2O


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_220
_database_code_depnum_ccdc_archive 'CCDC 1552193'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_220                 
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.59 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_RINTA01_220                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_220                 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.230 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT026_220                 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         39 %
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT097_220                 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.77 eA-3
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2554(15)
_cell_length_b                   15.2554(15)
_cell_length_c                   18.9276(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4405.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1490
_cell_measurement_temperature    220
_cell_measurement_theta_max      57.962
_cell_measurement_theta_min      6.86
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.854
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2304
_diffrn_reflns_av_unetI/netI     0.1623
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11215
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.981
_diffrn_reflns_theta_min         3.430
_diffrn_ambient_temperature      220
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                574
_reflns_number_total             1490
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.771
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1696
_refine_ls_R_factor_gt           0.0872
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2113
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C4A, C4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4A \\sim C4B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4A) \\sim Ueq, Uanis(C4B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.57077(5) 0.0436(6) Uani 1 4 d S T P . .
O1 O 0.3890(3) 0.5695(3) 0.55897(17) 0.087(3) Uani 1 1 d . . . . .
C1 C 0.3569(6) 0.5918(6) 0.5000 0.078(5) Uani 1 2 d S T P . .
C2 C 0.2821(6) 0.6531(6) 0.5000 0.099(5) Uani 1 2 d S T P . .
C3 C 0.2505(5) 0.6854(5) 0.5628(3) 0.092(4) Uani 1 1 d . . . . .
H3 H 0.2723 0.6642 0.6054 0.111 Uiso 1 1 calc R . . . .
N1 N 0.5000 0.5000 0.6816(3) 0.044(3) Uani 1 4 d S T P . .
C4B C 0.4834(9) 0.5936(8) 0.7084(6) 0.049(3) Uani 0.5 1 d . U . . .
C4A C 0.4187(9) 0.5497(10) 0.7078(7) 0.055(4) Uani 0.5 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.679(2) 17_666 ?
Co1 O1 2.010(4) 4_565 ?
Co1 O1 2.010(4) . ?
Co1 O1 2.010(4) 2_655 ?
Co1 O1 2.010(4) 3_665 ?
Co1 N1 2.098(6) . ?
O1 C1 1.265(5) . ?
C1 O1 1.265(5) 19_556 ?
C1 C2 1.476(11) . ?
C2 C3 1.375(7) 19_556 ?
C2 C3 1.375(7) . ?
C3 C3 1.404(12) 32_455 ?
N1 C4B 1.536(12) . ?
N1 C4B 1.536(12) 3_665 ?
N1 C4B 1.536(12) 2_655 ?
N1 C4B 1.536(12) 4_565 ?
N1 C4A 1.536(13) . ?
N1 C4A 1.536(13) 2_655 ?
N1 C4A 1.536(13) 4_565 ?
N1 C4A 1.536(13) 3_665 ?
C4B C4B 1.65(2) 6_656 ?
C4B C4A 1.675(16) 8_666 ?
C4B C4A 1.029(14) 4_565 ?
C4B C4A 1.193(14) . ?
C4A C4B 1.029(14) 2_655 ?
C4A C4B 1.675(16) 8_666 ?
C4A C4A 1.74(3) 8_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 83.62(10) 3_665 17_666 ?
O1 Co1 Co1 83.62(10) 4_565 17_666 ?
O1 Co1 Co1 83.62(10) 2_655 17_666 ?
O1 Co1 Co1 83.62(10) . 17_666 ?
O1 Co1 O1 89.29(2) . 4_565 ?
O1 Co1 O1 89.29(2) . 2_655 ?
O1 Co1 O1 167.2(2) 2_655 4_565 ?
O1 Co1 O1 167.2(2) . 3_665 ?
O1 Co1 O1 89.29(2) 2_655 3_665 ?
O1 Co1 O1 89.29(2) 4_565 3_665 ?
O1 Co1 N1 96.38(10) 3_665 . ?
O1 Co1 N1 96.38(10) 4_565 . ?
O1 Co1 N1 96.38(10) . . ?
O1 Co1 N1 96.38(10) 2_655 . ?
N1 Co1 Co1 180.0 . 17_666 ?
C1 O1 Co1 124.4(5) . . ?
O1 C1 O1 123.8(8) 19_556 . ?
O1 C1 C2 118.0(4) . . ?
O1 C1 C2 118.0(4) 19_556 . ?
C3 C2 C1 119.9(4) 19_556 . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 C3 119.8(9) . 19_556 ?
C2 C3 C3 120.1(4) . 32_455 ?
C4B N1 Co1 109.3(5) 4_565 . ?
C4B N1 Co1 109.3(5) . . ?
C4B N1 Co1 109.3(5) 2_655 . ?
C4B N1 Co1 109.3(5) 3_665 . ?
C4B N1 C4B 83.7(3) 4_565 3_665 ?
C4B N1 C4B 141.5(10) . 3_665 ?
C4B N1 C4B 141.5(10) 4_565 2_655 ?
C4B N1 C4B 83.7(3) 2_655 3_665 ?
C4B N1 C4B 83.7(3) . 2_655 ?
C4B N1 C4B 83.7(3) . 4_565 ?
C4B N1 C4A 39.1(5) . 4_565 ?
C4B N1 C4A 39.1(5) 4_565 3_665 ?
C4B N1 C4A 124.3(6) 4_565 . ?
C4B N1 C4A 45.7(5) 4_565 4_565 ?
C4B N1 C4A 45.7(5) 3_665 3_665 ?
C4B N1 C4A 119.1(6) 2_655 4_565 ?
C4B N1 C4A 119.1(6) 3_665 . ?
C4B N1 C4A 124.3(6) 3_665 4_565 ?
C4B N1 C4A 124.3(6) 2_655 3_665 ?
C4B N1 C4A 124.3(6) . 2_655 ?
C4B N1 C4A 45.7(5) . . ?
C4B N1 C4A 45.7(5) 2_655 2_655 ?
C4B N1 C4A 39.1(5) 2_655 . ?
C4B N1 C4A 39.1(5) 3_665 2_655 ?
C4B N1 C4A 119.1(6) . 3_665 ?
C4B N1 C4A 119.1(6) 4_565 2_655 ?
C4A N1 Co1 108.8(5) . . ?
C4A N1 Co1 108.8(5) 3_665 . ?
C4A N1 Co1 108.8(5) 4_565 . ?
C4A N1 Co1 108.8(5) 2_655 . ?
C4A N1 C4A 142.4(10) 4_565 2_655 ?
C4A N1 C4A 142.4(10) . 3_665 ?
C4A N1 C4A 84.0(3) . 2_655 ?
C4A N1 C4A 84.0(3) 4_565 3_665 ?
C4A N1 C4A 84.0(3) 2_655 3_665 ?
C4A N1 C4A 84.0(3) . 4_565 ?
N1 C4B C4B 105.3(6) . 6_656 ?
N1 C4B C4A 105.0(10) . 8_666 ?
C4B C4B C4A 36.0(6) 6_656 8_666 ?
C4A C4B N1 67.1(9) . . ?
C4A C4B N1 70.4(11) 4_565 . ?
C4A C4B C4B 73.2(13) 4_565 6_656 ?
C4A C4B C4B 105.3(13) . 6_656 ?
C4A C4B C4A 72.4(13) . 8_666 ?
C4A C4B C4A 106.7(14) 4_565 8_666 ?
C4A C4B C4A 135(2) 4_565 . ?
N1 C4A C4B 104.2(10) . 8_666 ?
N1 C4A C4A 102.1(7) . 8_666 ?
C4B C4A N1 70.5(11) 2_655 . ?
C4B C4A N1 67.2(9) . . ?
C4B C4A C4B 135(2) 2_655 . ?
C4B C4A C4B 104.6(13) . 8_666 ?
C4B C4A C4B 70.8(14) 2_655 8_666 ?
C4B C4A C4A 66.8(12) . 8_666 ?
C4B C4A C4A 108.2(15) 2_655 8_666 ?
C4B C4A C4A 40.9(6) 8_666 8_666 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.659 0.100 -0.684 2674.5 1006.5 ?


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_250
_database_code_depnum_ccdc_archive 'CCDC 1552192'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_250                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_250                 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.229 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT026_250                 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         38 %
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT430_250                 
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.60 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2626(16)
_cell_length_b                   15.2626(16)
_cell_length_c                   18.9551(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4415.5(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1500
_cell_measurement_temperature    250
_cell_measurement_theta_max      57.884
_cell_measurement_theta_min      5.72
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2291
_diffrn_reflns_av_unetI/netI     0.1677
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11321
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.942
_diffrn_reflns_theta_min         2.860
_diffrn_ambient_temperature      250
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                572
_reflns_number_total             1500
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1500
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1870
_refine_ls_R_factor_gt           0.0972
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0951P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2540
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq, Uanis(C4B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: C4A(0.5) C4B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.57103(6) 0.0430(6) Uani 1 4 d S T P . .
O1 O 0.3893(3) 0.5702(3) 0.5589(2) 0.0633(19) Uani 1 1 d . . . . .
C1 C 0.3575(7) 0.5916(7) 0.5000 0.077(5) Uani 1 2 d S T P . .
C2 C 0.2820(7) 0.6534(7) 0.5000 0.082(5) Uani 1 2 d S T P . .
C3 C 0.2494(5) 0.6870(6) 0.5623(3) 0.080(3) Uani 1 1 d . . . . .
H3 H 0.2709 0.6662 0.6051 0.097 Uiso 1 1 calc R . . . .
N1 N 0.5000 0.5000 0.6813(4) 0.044(3) Uani 1 4 d S T P . .
C4A C 0.4048(9) 0.5178(10) 0.7097(7) 0.047(3) Uani 0.5 1 d . U . . .
C4B C 0.4237(11) 0.4498(12) 0.7080(8) 0.066(4) Uani 0.5 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.693(2) 17_666 ?
Co1 O1 2.013(5) . ?
Co1 O1 2.013(5) 3_665 ?
Co1 O1 2.013(5) 2_655 ?
Co1 O1 2.013(5) 4_565 ?
Co1 N1 2.090(7) . ?
O1 C1 1.261(6) . ?
C1 O1 1.261(6) 19_556 ?
C1 C2 1.490(13) . ?
C2 C3 1.381(8) 19_556 ?
C2 C3 1.381(8) . ?
C3 C3 1.345(14) 32_455 ?
N1 C4A 1.572(14) 4_565 ?
N1 C4A 1.573(14) . ?
N1 C4A 1.572(14) 3_665 ?
N1 C4A 1.572(14) 2_655 ?
N1 C4B 1.482(15) 3_665 ?
N1 C4B 1.482(15) . ?
N1 C4B 1.482(15) 4_565 ?
N1 C4B 1.482(15) 2_655 ?
C4A C4A 1.62(3) 5_566 ?
C4A C4B 1.077(16) . ?
C4A C4B 1.127(17) 4_565 ?
C4A C4B 1.66(2) 5_566 ?
C4B C4A 1.66(2) 5_566 ?
C4B C4A 1.127(17) 2_655 ?
C4B C4B 1.97(2) 4_565 ?
C4B C4B 1.97(2) 2_655 ?
C4B C4B 1.69(3) 7_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 83.45(12) 2_655 17_666 ?
O1 Co1 Co1 83.45(12) 4_565 17_666 ?
O1 Co1 Co1 83.45(12) . 17_666 ?
O1 Co1 Co1 83.45(12) 3_665 17_666 ?
O1 Co1 O1 89.25(3) 2_655 . ?
O1 Co1 O1 166.9(2) 3_665 . ?
O1 Co1 O1 89.25(3) 4_565 3_665 ?
O1 Co1 O1 89.25(3) 2_655 3_665 ?
O1 Co1 O1 89.25(3) 4_565 . ?
O1 Co1 O1 166.9(2) 2_655 4_565 ?
O1 Co1 N1 96.55(12) 4_565 . ?
O1 Co1 N1 96.55(12) 3_665 . ?
O1 Co1 N1 96.55(12) . . ?
O1 Co1 N1 96.55(12) 2_655 . ?
N1 Co1 Co1 180.0 . 17_666 ?
C1 O1 Co1 124.2(5) . . ?
O1 C1 O1 124.7(9) 19_556 . ?
O1 C1 C2 117.5(5) . . ?
O1 C1 C2 117.5(5) 19_556 . ?
C3 C2 C1 121.0(5) 19_556 . ?
C3 C2 C1 121.0(5) . . ?
C3 C2 C3 117.6(10) 19_556 . ?
C3 C3 C2 121.2(5) 32_455 . ?
C4A N1 Co1 110.0(6) . . ?
C4A N1 Co1 110.0(6) 4_565 . ?
C4A N1 Co1 110.0(6) 3_665 . ?
C4A N1 Co1 110.0(6) 2_655 . ?
C4A N1 C4A 83.3(4) 4_565 3_665 ?
C4A N1 C4A 83.3(4) 3_665 2_655 ?
C4A N1 C4A 140.0(11) 4_565 2_655 ?
C4A N1 C4A 83.3(4) 2_655 . ?
C4A N1 C4A 140.0(11) 3_665 . ?
C4A N1 C4A 83.3(4) 4_565 . ?
C4B N1 Co1 110.0(7) 4_565 . ?
C4B N1 Co1 110.0(7) 2_655 . ?
C4B N1 Co1 110.0(7) 3_665 . ?
C4B N1 Co1 110.0(7) . . ?
C4B N1 C4A 41.2(6) . . ?
C4B N1 C4A 119.7(7) 2_655 . ?
C4B N1 C4A 121.3(7) 4_565 2_655 ?
C4B N1 C4A 43.2(6) 4_565 . ?
C4B N1 C4A 41.2(6) 2_655 2_655 ?
C4B N1 C4A 121.3(7) 3_665 . ?
C4B N1 C4A 119.7(7) 4_565 3_665 ?
C4B N1 C4A 43.2(6) 3_665 4_565 ?
C4B N1 C4A 119.7(7) 3_665 2_655 ?
C4B N1 C4A 121.3(7) . 3_665 ?
C4B N1 C4A 119.7(7) . 4_565 ?
C4B N1 C4A 41.2(6) 4_565 4_565 ?
C4B N1 C4A 121.3(7) 2_655 4_565 ?
C4B N1 C4A 43.2(6) 2_655 3_665 ?
C4B N1 C4A 41.2(6) 3_665 3_665 ?
C4B N1 C4A 43.2(6) . 2_655 ?
C4B N1 C4B 83.3(4) 4_565 . ?
C4B N1 C4B 83.3(4) 3_665 4_565 ?
C4B N1 C4B 83.3(4) 2_655 . ?
C4B N1 C4B 140.1(13) 4_565 2_655 ?
C4B N1 C4B 83.3(4) 3_665 2_655 ?
C4B N1 C4B 140.1(13) 3_665 . ?
N1 C4A C4A 105.3(7) . 5_566 ?
N1 C4A C4B 102.2(11) . 5_566 ?
C4A C4A C4B 38.2(7) 5_566 5_566 ?
C4B C4A N1 64.1(11) 4_565 . ?
C4B C4A N1 64.9(12) . . ?
C4B C4A C4A 106.9(16) 4_565 5_566 ?
C4B C4A C4A 72.9(15) . 5_566 ?
C4B C4A C4B 127(2) . 4_565 ?
C4B C4A C4B 71.7(16) 4_565 5_566 ?
C4B C4A C4B 105.5(16) . 5_566 ?
N1 C4B C4A 107.7(13) . 5_566 ?
N1 C4B C4B 105.0(8) . 7_556 ?
N1 C4B C4B 48.3(2) . 2_655 ?
N1 C4B C4B 48.3(2) . 4_565 ?
C4A C4B N1 73.9(12) . . ?
C4A C4B N1 72.7(11) 2_655 . ?
C4A C4B C4A 143(2) . 2_655 ?
C4A C4B C4A 107.0(16) 2_655 5_566 ?
C4A C4B C4A 68.9(16) . 5_566 ?
C4A C4B C4B 69.1(15) 2_655 7_556 ?
C4A C4B C4B 103.3(8) 5_566 2_655 ?
C4A C4B C4B 26.0(11) 2_655 2_655 ?
C4A C4B C4B 75.2(11) 5_566 4_565 ?
C4A C4B C4B 105.2(18) . 7_556 ?
C4A C4B C4B 115.9(11) 2_655 4_565 ?
C4A C4B C4B 39.3(8) 5_566 7_556 ?
C4A C4B C4B 117.2(12) . 2_655 ?
C4A C4B C4B 27.3(12) . 4_565 ?
C4B C4B C4B 100.6(5) 7_556 4_565 ?
C4B C4B C4B 73.8(12) 7_556 2_655 ?
C4B C4B C4B 89.999(8) 4_565 2_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.005 -0.398 -0.510 2675.8 690.0 4DMF.H2O


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_180
_database_code_depnum_ccdc_archive 'CCDC 1552194'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_180                 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_180                 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.256 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT026_180                 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         38 %
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT201_180                 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT242_180                 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         N1 Check
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT430_180                 
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.62 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2439(18)
_cell_length_b                   15.2439(18)
_cell_length_c                   18.9075(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4393.7(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1482
_cell_measurement_temperature    180
_cell_measurement_theta_max      58.026
_cell_measurement_theta_min      6.352
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.856
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2562
_diffrn_reflns_av_unetI/netI     0.1828
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11163
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.013
_diffrn_reflns_theta_min         3.176
_diffrn_ambient_temperature      180
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                563
_reflns_number_total             1482
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.858
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         1482
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1877
_refine_ls_R_factor_gt           0.0963
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0920P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2444
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.57051(6) 0.0413(7) Uani 1 4 d S T P . .
O1 O 0.3884(3) 0.5679(3) 0.55919(19) 0.081(3) Uani 1 1 d . . . . .
C1 C 0.3563(7) 0.5918(7) 0.5000 0.063(5) Uani 1 2 d S T P . .
C2 C 0.2822(7) 0.6511(7) 0.5000 0.062(5) Uani 1 2 d S T P . .
C3 C 0.2487(6) 0.6843(5) 0.5633(3) 0.066(3) Uani 1) 1 d . . . . .
H3 H 0.2699 0.6630 0.6061 0.080 Uiso 0.49(16) 1 calc R . . . .
C4B C 0.4001(9) 0.5141(15) 0.7083(8) 0.109(5) Uani 0.5 1 d . U . . .
C4A C 0.5716(12) 0.5470(15) 0.7067(8) 0.120(5) Uani 0.5 1 d . U . . .
N1 N 0.5000 0.5000 0.6808(4) 0.0096(18) Uiso 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.666(2) 17_666 ?
Co1 O1 2.003(5) 2_655 ?
Co1 O1 2.003(5) . ?
Co1 O1 2.003(5) 3_665 ?
Co1 O1 2.003(5) 4_565 ?
Co1 N1 2.086(8) . ?
O1 C1 1.274(6) . ?
C1 O1 1.274(6) 19_556 ?
C1 C2 1.446(13) . ?
C2 C3 1.396(8) 19_556 ?
C2 C3 1.396(8) . ?
C3 C3 1.389(14) 32_455 ?
C4B C4B 1.64(3) 5_566 ?
C4B C4A 1.192(19) 2_655 ?
C4B C4A 1.026(17) 3_665 ?
C4B C4A 1.74(2) 6_656 ?
C4B N1 1.623(14) . ?
C4A C4B 1.192(18) 4_565 ?
C4A C4B 1.026(17) 3_665 ?
C4A C4B 1.74(2) 6_656 ?
C4A C4A 1.847(17) 4_565 ?
C4A C4A 1.72(3) 7_556 ?
C4A C4A 1.847(17) 2_655 ?
C4A N1 1.395(12) . ?
N1 C4B 1.623(14) 4_565 ?
N1 C4B 1.623(14) 2_655 ?
N1 C4B 1.623(15) 3_665 ?
N1 C4A 1.395(12) 3_665 ?
N1 C4A 1.395(12) 4_565 ?
N1 C4A 1.395(12) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 83.87(11) . 17_666 ?
O1 Co1 Co1 83.86(11) 4_565 17_666 ?
O1 Co1 Co1 83.86(11) 3_665 17_666 ?
O1 Co1 Co1 83.86(11) 2_655 17_666 ?
O1 Co1 O1 167.7(2) 3_665 . ?
O1 Co1 O1 89.34(2) 2_655 . ?
O1 Co1 O1 89.35(2) 4_565 . ?
O1 Co1 O1 167.7(2) 2_655 4_565 ?
O1 Co1 O1 89.35(2) 2_655 3_665 ?
O1 Co1 O1 89.35(2) 4_565 3_665 ?
O1 Co1 N1 96.14(11) 4_565 . ?
O1 Co1 N1 96.13(11) . . ?
O1 Co1 N1 96.14(11) 2_655 . ?
O1 Co1 N1 96.14(11) 3_665 . ?
N1 Co1 Co1 180.0 . 17_666 ?
C1 O1 Co1 124.6(5) . . ?
O1 C1 O1 122.8(10) 19_556 . ?
O1 C1 C2 118.6(5) . . ?
O1 C1 C2 118.6(5) 19_556 . ?
C3 C2 C1 120.8(5) 19_556 . ?
C3 C2 C1 120.8(5) . . ?
C3 C2 C3 117.9(10) 19_556 . ?
C3 C3 C2 121.0(5) 32_455 . ?
C4B C4B C4A 35.3(7) 5_566 6_656 ?
C4A C4B C4B 77.8(19) 3_665 5_566 ?
C4A C4B C4B 102.5(16) 2_655 5_566 ?
C4A C4B C4A 112(2) 3_665 2_655 ?
C4A C4B C4A 69.0(18) 2_655 6_656 ?
C4A C4B C4A 100.6(18) 3_665 6_656 ?
C4A C4B N1 58.5(11) 3_665 . ?
C4A C4B N1 56.9(9) 2_655 . ?
N1 C4B C4B 105.9(8) . 5_566 ?
N1 C4B C4A 95.8(11) . 6_656 ?
C4B C4A C4B 110.8(18) 4_565 6_656 ?
C4B C4A C4B 67(2) 3_665 6_656 ?
C4B C4A C4B 157(2) 3_665 4_565 ?
C4B C4A C4A 105(2) 3_665 7_556 ?
C4B C4A C4A 36.6(12) 3_665 4_565 ?
C4B C4A C4A 120.9(11) 4_565 4_565 ?
C4B C4A C4A 126.6(13) 3_665 2_655 ?
C4B C4A C4A 76.6(16) 6_656 4_565 ?
C4B C4A C4A 70.6(19) 4_565 7_556 ?
C4B C4A C4A 107.6(8) 6_656 2_655 ?
C4B C4A C4A 30.9(11) 4_565 2_655 ?
C4B C4A N1 77.3(11) 4_565 . ?
C4B C4A N1 82.7(12) 3_665 . ?
C4A C4A C4B 40.3(8) 7_556 6_656 ?
C4A C4A C4A 75.0(17) 7_556 2_655 ?
C4A C4A C4A 99.8(6) 7_556 4_565 ?
C4A C4A C4A 90.002(11) 4_565 2_655 ?
N1 C4A C4B 111.8(14) . 6_656 ?
N1 C4A C4A 106.0(11) . 7_556 ?
N1 C4A C4A 48.5(2) . 2_655 ?
N1 C4A C4A 48.5(2) . 4_565 ?
C4B N1 Co1 108.6(6) 2_655 . ?
C4B N1 Co1 108.6(6) 3_665 . ?
C4B N1 Co1 108.6(6) 4_565 . ?
C4B N1 Co1 108.6(6) . . ?
C4B N1 C4B 84.1(4) 4_565 3_665 ?
C4B N1 C4B 84.1(4) . 4_565 ?
C4B N1 C4B 84.1(4) . 2_655 ?
C4B N1 C4B 142.7(12) . 3_665 ?
C4B N1 C4B 84.1(4) 3_665 2_655 ?
C4B N1 C4B 142.7(12) 4_565 2_655 ?
C4A N1 Co1 110.6(7) . . ?
C4A N1 Co1 110.6(7) 2_655 . ?
C4A N1 Co1 110.6(7) 3_665 . ?
C4A N1 Co1 110.6(7) 4_565 . ?
C4A N1 C4B 118.2(8) 2_655 3_665 ?
C4A N1 C4B 118.2(8) 4_565 . ?
C4A N1 C4B 38.8(7) 4_565 2_655 ?
C4A N1 C4B 38.8(7) 3_665 . ?
C4A N1 C4B 123.7(8) 2_655 2_655 ?
C4A N1 C4B 123.7(8) . . ?
C4A N1 C4B 38.8(7) 2_655 4_565 ?
C4A N1 C4B 118.2(8) . 2_655 ?
C4A N1 C4B 45.8(7) 3_665 2_655 ?
C4A N1 C4B 118.2(8) 3_665 4_565 ?
C4A N1 C4B 45.8(7) 2_655 . ?
C4A N1 C4B 45.8(7) 4_565 3_665 ?
C4A N1 C4B 38.8(7) . 3_665 ?
C4A N1 C4B 123.7(8) 3_665 3_665 ?
C4A N1 C4B 123.7(8) 4_565 4_565 ?
C4A N1 C4B 45.8(7) . 4_565 ?
C4A N1 C4A 138.9(14) . 3_665 ?
C4A N1 C4A 138.9(14) 2_655 4_565 ?
C4A N1 C4A 82.9(5) . 2_655 ?
C4A N1 C4A 82.9(5) 3_665 4_565 ?
C4A N1 C4A 82.9(5) 3_665 2_655 ?
C4A N1 C4A 82.9(5) . 4_565 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.060 -0.257 -0.609 2672.8 543.3 4DMF.H2O


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_100k
_database_code_depnum_ccdc_archive 'CCDC 1552196'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_100k                
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_100k                
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.255 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT430_100k                
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.59 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2236(19)
_cell_length_b                   15.2236(19)
_cell_length_c                   18.8603(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4371.1(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1295
_cell_measurement_temperature    100
_cell_measurement_theta_max      53.964
_cell_measurement_theta_min      5.744
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.860
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2553
_diffrn_reflns_av_unetI/netI     0.1345
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10750
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.982
_diffrn_reflns_theta_min         2.872
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                531
_reflns_number_total             1295
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.702
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1295
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1785
_refine_ls_R_factor_gt           0.0931
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0976P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2296
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.0002
3. Others
 Fixed Sof: C4B(0.5) C4A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 0.07022(6) 0.0397(7) Uani 1 4 d S T P . .
O1 O 0.0673(3) 0.1130(3) 0.05931(19) 0.072(3) Uani 1 1 d . . . . .
C1 C 0.0897(7) 0.1444(7) 0.0000 0.076(5) Uani 1 2 d S T P . .
C2 C 0.1489(7) 0.2191(7) 0.0000 0.078(5) Uani 1 2 d S T P . .
C3 C 0.1852(5) 0.2513(6) 0.0633(3) 0.080(4) Uani 1 1 d . . . . .
H3 H 0.1656 0.2289 0.1064 0.096 Uiso 1 1 calc R . . . .
N1 N 0.0000 0.0000 0.1813(4) 0.037(3) Uani 1 4 d S T P . .
C4B C 0.0498(11) 0.0807(10) 0.2084(8) 0.044(4) Uani 0.5 1 d . U . . .
C4A C -0.0160(11) 0.0953(10) 0.2089(8) 0.044(4) Uani 0.5 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.649(2) 17 ?
Co1 O1 2.012(5) 3 ?
Co1 O1 2.012(5) . ?
Co1 O1 2.012(5) 2 ?
Co1 O1 2.012(5) 4 ?
Co1 N1 2.094(7) . ?
O1 C1 1.264(6) . ?
C1 O1 1.264(6) 19 ?
C1 C2 1.451(13) . ?
C2 C3 1.405(8) 19 ?
C2 C3 1.405(8) . ?
C3 C3 1.366(15) 31 ?
N1 C4B 1.532(14) 3 ?
N1 C4B 1.532(14) 4 ?
N1 C4B 1.532(14) 2 ?
N1 C4B 1.532(14) . ?
N1 C4A 1.561(15) . ?
N1 C4A 1.561(15) 4 ?
N1 C4A 1.561(15) 2 ?
N1 C4A 1.561(15) 3 ?
C4B C4B 1.70(3) 7 ?
C4B C4A 1.204(16) 4 ?
C4B C4A 1.658(19) 6 ?
C4B C4A 1.027(16) . ?
C4A C4B 1.204(16) 2 ?
C4A C4B 1.658(19) 6 ?
C4A C4A 1.63(3) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 84.13(11) . 17 ?
O1 Co1 Co1 84.13(11) 4 17 ?
O1 Co1 Co1 84.13(11) 2 17 ?
O1 Co1 Co1 84.13(11) 3 17 ?
O1 Co1 O1 89.40(2) 2 . ?
O1 Co1 O1 168.3(2) 3 . ?
O1 Co1 O1 89.40(2) 4 . ?
O1 Co1 O1 89.40(2) 3 4 ?
O1 Co1 O1 89.40(2) 3 2 ?
O1 Co1 O1 168.3(2) 4 2 ?
O1 Co1 N1 95.87(11) . . ?
O1 Co1 N1 95.87(11) 4 . ?
O1 Co1 N1 95.87(11) 2 . ?
O1 Co1 N1 95.87(11) 3 . ?
N1 Co1 Co1 180.0 . 17 ?
C1 O1 Co1 123.5(6) . . ?
O1 C1 O1 124.6(10) . 19 ?
O1 C1 C2 117.7(5) 19 . ?
O1 C1 C2 117.7(5) . . ?
C3 C2 C1 121.2(5) 19 . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 C3 116.5(10) 19 . ?
C3 C3 C2 121.7(5) 31 . ?
C4B N1 Co1 109.5(6) . . ?
C4B N1 Co1 109.5(6) 2 . ?
C4B N1 Co1 109.5(6) 3 . ?
C4B N1 Co1 109.5(6) 4 . ?
C4B N1 C4B 83.6(4) 4 . ?
C4B N1 C4B 83.6(4) 3 2 ?
C4B N1 C4B 83.6(4) 2 . ?
C4B N1 C4B 141.0(12) 3 . ?
C4B N1 C4B 141.0(12) 4 2 ?
C4B N1 C4B 83.6(4) 3 4 ?
C4B N1 C4A 45.8(6) . 4 ?
C4B N1 C4A 123.9(7) 4 2 ?
C4B N1 C4A 118.3(7) . 2 ?
C4B N1 C4A 45.8(6) 3 2 ?
C4B N1 C4A 123.9(7) 2 4 ?
C4B N1 C4A 38.8(6) 2 2 ?
C4B N1 C4A 118.3(7) 2 3 ?
C4B N1 C4A 118.3(7) 3 4 ?
C4B N1 C4A 123.9(7) 3 . ?
C4B N1 C4A 45.8(6) 4 3 ?
C4B N1 C4A 45.8(6) 2 . ?
C4B N1 C4A 118.3(7) 4 . ?
C4B N1 C4A 38.8(6) 3 3 ?
C4B N1 C4A 38.8(6) 4 4 ?
C4B N1 C4A 123.9(7) . 3 ?
C4B N1 C4A 38.8(6) . . ?
C4A N1 Co1 109.5(6) 4 . ?
C4A N1 Co1 109.5(6) 3 . ?
C4A N1 Co1 109.5(6) . . ?
C4A N1 Co1 109.5(6) 2 . ?
C4A N1 C4A 141.1(12) 4 2 ?
C4A N1 C4A 83.6(4) . 4 ?
C4A N1 C4A 141.1(12) . 3 ?
C4A N1 C4A 83.6(4) 4 3 ?
C4A N1 C4A 83.6(4) 2 3 ?
C4A N1 C4A 83.6(4) . 2 ?
N1 C4B C4B 102.9(7) . 7 ?
N1 C4B C4A 105.5(12) . 6 ?
C4A C4B N1 72.1(13) . . ?
C4A C4B N1 68.3(10) 4 . ?
C4A C4B C4B 108.7(17) . 7 ?
C4A C4B C4B 41.9(7) 6 7 ?
C4A C4B C4B 67.0(13) 4 7 ?
C4A C4B C4A 70.1(16) . 6 ?
C4A C4B C4A 138(2) . 4 ?
C4A C4B C4A 106.3(14) 4 6 ?
N1 C4A C4B 103.7(11) . 6 ?
N1 C4A C4A 105.7(7) . 6 ?
C4B C4A N1 69.1(12) . . ?
C4B C4A N1 65.8(11) 2 . ?
C4B C4A C4B 71.1(14) 2 6 ?
C4B C4A C4B 132(2) . 2 ?
C4B C4A C4B 106.4(16) . 6 ?
C4B C4A C4A 73.5(15) . 6 ?
C4B C4A C4A 104.6(15) 2 6 ?
C4A C4A C4B 36.4(7) 6 6 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.553 -0.540 -0.488 2641.9 645.7 4DMF.H2O


_olex2_submission_special_instructions 'No special instructions were received'

#===END



####################################################################### 
# 
# 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_150
_database_code_depnum_ccdc_archive 'CCDC 1552195'
_audit_update_record             
;
2017-05-24 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_150                 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT020_150                 
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.250 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT026_150                 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         38 %
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT084_150                 
;
PROBLEM: High wR2 Value (i.e. &gt; 0.25) ...................       0.45 Report
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT341_150                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0175 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
_vrf_PLAT430_150                 
;
PROBLEM: Short Inter D...A Contact  N1     ..  N1      ..       2.62 Ang.
RESPONSE: The single crystal was of a good quality, however its low air stability resulted in its deterioration during the measurement. Voids content with disordered DMF and water molecules was removed by 'squeeze' procedure as it significantly destabilized refinement. However, as guest-free and guest-filled structures differ in symmetry it should not confuse readers. Dabco molecules are symmetry-disordered, thus a correct refinement of atoms' positions within a molecule is difficult.
;
# Added during the CSD deposition process: Wednesday 24 May 2017 01:40 PM
# end Validation Reply Form

_audit_creation_date             2017-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Co2Bdc2Dabco*4DMF*H2O
_chemical_name_systematic        
'catena-(bis(m4-1,4-Benzenedicarboxylato)-(m2-1,4-diazabicyclo(2.2.0)octane)-di-cobalt dimethylformamide solvate monohydrate)'
_chemical_formula_moiety         '0.25(C96 H32 Co8 N8 O32)'
_chemical_formula_sum            'C24 H8 Co2 N2 O8'
_chemical_formula_weight         570.18
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   15.2363(17)
_cell_length_b                   15.2363(17)
_cell_length_c                   18.8931(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4386.0(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1488
_cell_measurement_temperature    150
_cell_measurement_theta_max      58.072
_cell_measurement_theta_min      6.356
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Data were collected and reduced by program CrysAlisPro, 
and SCALE3 ABSPACK was used for absorption correction
;
_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2498
_diffrn_reflns_av_unetI/netI     0.1762
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11161
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.036
_diffrn_reflns_theta_min         3.178
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                564
_reflns_number_total             1488
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1488
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.2862
_refine_ls_R_factor_gt           0.1395
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3433
_refine_ls_wR_factor_ref         0.4481
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C4A, C4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4A \\sim C4B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C4A) \\sim Ueq, Uanis(C4B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: C1(0.25) C2(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.5000 0.57035(10) 0.0386(10) Uani 1 4 d S T P . .
O1 O 0.3873(5) 0.5683(6) 0.5594(3) 0.075(4) Uani 1 1 d . . . . .
C1 C 0.3563(10) 0.5901(11) 0.5000 0.063(6) Uani 1 2 d S T P . .
C2 C 0.2823(12) 0.6504(12) 0.5000 0.073(7) Uani 1 2 d S T P . .
C3 C 0.2479(11) 0.6826(10) 0.5624(5) 0.066(6) Uani 1 1 d . . . . .
H3 H 0.2683 0.6607 0.6053 0.079 Uiso 1 1 calc R . . . .
N1 N 0.5000 0.5000 0.6806(6) 0.032(5) Uani 1 4 d S T P . .
C4B C 0.5172(15) 0.5956(14) 0.7073(13) 0.051(7) Uani 0.5 1 d . U . . .
C4A C 0.4516(18) 0.5810(17) 0.7075(15) 0.048(8) Uani 0.5 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Co1 2.658(4) 17_666 ?
Co1 O1 2.018(8) 2_655 ?
Co1 O1 2.018(8) . ?
Co1 O1 2.018(8) 4_565 ?
Co1 O1 2.018(8) 3_665 ?
Co1 N1 2.084(12) . ?
O1 C1 1.261(9) . ?
C1 O1 1.261(9) 19_556 ?
C1 C2 1.45(2) . ?
C2 C3 1.381(13) . ?
C2 C3 1.381(13) 19_556 ?
C3 C3 1.41(3) 32_455 ?
N1 C4B 1.56(2) 4_565 ?
N1 C4B 1.56(2) 3_665 ?
N1 C4B 1.56(2) 2_655 ?
N1 C4B 1.56(2) . ?
N1 C4A 1.52(3) . ?
N1 C4A 1.52(3) 4_565 ?
N1 C4A 1.52(3) 3_665 ?
N1 C4A 1.52(3) 2_655 ?
C4B C4B 1.70(5) 6_656 ?
C4B C4A 1.02(3) . ?
C4B C4A 1.21(3) 4_565 ?
C4B C4A 1.69(4) 6_656 ?
C4A C4B 1.69(4) 6_656 ?
C4A C4B 1.21(3) 2_655 ?
C4A C4A 1.75(6) 8_666 ?
C4A C4A 2.03(4) 2_655 ?
C4A C4A 2.03(4) 4_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Co1 84.09(19) 2_655 17_666 ?
O1 Co1 Co1 84.10(19) . 17_666 ?
O1 Co1 Co1 84.09(19) 4_565 17_666 ?
O1 Co1 Co1 84.09(19) 3_665 17_666 ?
O1 Co1 O1 89.40(4) 4_565 . ?
O1 Co1 O1 89.39(4) 2_655 3_665 ?
O1 Co1 O1 168.2(4) 2_655 4_565 ?
O1 Co1 O1 168.2(4) 3_665 . ?
O1 Co1 O1 89.39(4) 4_565 3_665 ?
O1 Co1 O1 89.39(4) 2_655 . ?
O1 Co1 N1 95.91(19) 4_565 . ?
O1 Co1 N1 95.90(19) . . ?
O1 Co1 N1 95.91(19) 2_655 . ?
O1 Co1 N1 95.91(19) 3_665 . ?
N1 Co1 Co1 180.0 . 17_666 ?
C1 O1 Co1 123.1(8) . . ?
O1 C1 O1 125.5(15) 19_556 . ?
O1 C1 C2 117.2(7) . . ?
O1 C1 C2 117.2(7) 19_556 . ?
C3 C2 C1 121.2(8) . . ?
C3 C2 C1 121.2(8) 19_556 . ?
C3 C2 C3 117.4(16) 19_556 . ?
C2 C3 C3 121.3(8) . 32_455 ?
C4B N1 Co1 108.8(10) 3_665 . ?
C4B N1 Co1 108.8(10) 4_565 . ?
C4B N1 Co1 108.8(10) 2_655 . ?
C4B N1 Co1 108.8(10) . . ?
C4B N1 C4B 84.0(6) 4_565 3_665 ?
C4B N1 C4B 84.0(6) 2_655 . ?
C4B N1 C4B 142.4(19) 3_665 . ?
C4B N1 C4B 142.4(19) 4_565 2_655 ?
C4B N1 C4B 84.0(6) 4_565 . ?
C4B N1 C4B 84.0(6) 3_665 2_655 ?
C4A N1 Co1 109.4(11) 4_565 . ?
C4A N1 Co1 109.4(11) . . ?
C4A N1 Co1 109.4(11) 2_655 . ?
C4A N1 Co1 109.4(11) 3_665 . ?
C4A N1 C4B 38.7(10) 4_565 4_565 ?
C4A N1 C4B 46.1(10) 2_655 3_665 ?
C4A N1 C4B 124.5(13) . 3_665 ?
C4A N1 C4B 118.6(12) . 4_565 ?
C4A N1 C4B 38.7(10) 3_665 3_665 ?
C4A N1 C4B 38.7(10) 2_655 2_655 ?
C4A N1 C4B 124.5(13) 4_565 2_655 ?
C4A N1 C4B 118.6(12) 3_665 2_655 ?
C4A N1 C4B 118.6(12) 4_565 3_665 ?
C4A N1 C4B 118.6(12) 2_655 . ?
C4A N1 C4B 46.1(10) . 2_655 ?
C4A N1 C4B 124.5(13) 3_665 . ?
C4A N1 C4B 46.1(10) 3_665 4_565 ?
C4A N1 C4B 46.1(10) 4_565 . ?
C4A N1 C4B 124.5(13) 2_655 4_565 ?
C4A N1 C4B 38.7(10) . . ?
C4A N1 C4A 83.7(7) 4_565 3_665 ?
C4A N1 C4A 141(2) 4_565 2_655 ?
C4A N1 C4A 141(2) . 3_665 ?
C4A N1 C4A 83.7(7) 2_655 3_665 ?
C4A N1 C4A 83.7(7) . 4_565 ?
C4A N1 C4A 83.7(7) . 2_655 ?
N1 C4B C4B 104.8(10) . 6_656 ?
N1 C4B C4A 103.3(16) . 6_656 ?
C4A C4B N1 65.2(17) 4_565 . ?
C4A C4B N1 69(2) . . ?
C4A C4B C4B 72(2) . 6_656 ?
C4A C4B C4B 104(2) 4_565 6_656 ?
C4A C4B C4B 35.2(12) 6_656 6_656 ?
C4A C4B C4A 131(4) . 4_565 ?
C4A C4B C4A 72(2) 4_565 6_656 ?
C4A C4B C4A 104(3) . 6_656 ?
N1 C4A C4B 106.7(19) . 6_656 ?
N1 C4A C4A 48.2(4) . 4_565 ?
N1 C4A C4A 48.2(4) . 2_655 ?
N1 C4A C4A 102.2(13) . 8_666 ?
C4B C4A N1 73(2) . . ?
C4B C4A N1 68.7(17) 2_655 . ?
C4B C4A C4B 139(4) . 2_655 ?
C4B C4A C4B 106(2) 2_655 6_656 ?
C4B C4A C4B 73(2) . 6_656 ?
C4B C4A C4A 41.1(13) 6_656 8_666 ?
C4B C4A C4A 117(2) . 2_655 ?
C4B C4A C4A 110(3) . 8_666 ?
C4B C4A C4A 27(2) . 4_565 ?
C4B C4A C4A 22.4(17) 2_655 2_655 ?
C4B C4A C4A 101.3(11) 6_656 2_655 ?
C4B C4A C4A 67(2) 2_655 8_666 ?
C4B C4A C4A 112.4(17) 2_655 4_565 ?
C4B C4A C4A 76.1(15) 6_656 4_565 ?
C4A C4A C4A 101.9(5) 8_666 4_565 ?
C4A C4A C4A 90.002(3) 4_565 2_655 ?
C4A C4A C4A 69.9(17) 8_666 2_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.353 -0.089 -0.225 2674.1 0.0 4DMF.H2O


_olex2_submission_special_instructions 'No special instructions were received'
