# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_GR-MOF-2
_database_code_depnum_ccdc_archive 'CCDC 1836112'
_audit_update_record             
;
2018-04-10 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014


_chemical_name_systematic        
"poly{[(mu-azopyridine)-kN,N')bis(mu4-glutarato-kO:kO':kO'':kO''')dicopper(II)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H10 Cu N2 O4, 2(H2 O)'
_chemical_formula_sum            'C10 H14 Cu N2 O6'
_chemical_formula_weight         321.77

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   24.153(2)
_cell_length_b                   13.120(1)
_cell_length_c                   8.600(1)
_cell_angle_alpha                90
_cell_angle_beta                 92.537(1)
_cell_angle_gamma                90
_cell_volume                     2722.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43628
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.73

# SQUEEZE RESULTS (Version = 160617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 -0.018 362 -1 ' '
2 0.000 0.500 -0.025 362 -1 ' '
# Missing Reflections Below sin(th)/lambda = 0.25

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
4 0 0 3.377
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelx     C 2/c        R = 0.04
CELL   24.1530   13.1197    8.5999     90.00     92.54     90.00
SPGR C2/c
# Solvent Accessible Volume =       718
# Electrons Found in S.A.V. =         0
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.523 0.249 0.071 !       0.65 eA-3
Q102 0.486 0.456 0.495 !       0.63 eA-3
Q103 0.585 0.465 0.160 !       0.58 eA-3
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.627
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            43628
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         28.036
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3080
_reflns_number_gt                2446
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;The crystal structure contains large voids filled with disordered
water molecules. Given the impossibility to refine them, their 
electron density was subtracted with the SQUEEZE routine as implemented
in PLATON.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0452P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3080
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0906
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.29478(2) 0.29677(2) 0.05598(3) 0.02728(11) Uani 1 1 d . . . . .
N1A N 0.36282(9) 0.37267(15) 0.1843(2) 0.0349(5) Uani 1 1 d . . . . .
C2A C 0.40250(13) 0.3193(2) 0.2575(3) 0.0462(7) Uani 1 1 d . . . . .
H2A H 0.4033 0.2492 0.2418 0.055 Uiso 1 1 calc R U . . .
C3A C 0.44307(12) 0.3626(2) 0.3566(3) 0.0505(7) Uani 1 1 d . . . . .
H3A H 0.4701 0.3228 0.4075 0.061 Uiso 1 1 calc R U . . .
C4A C 0.44175(12) 0.4667(2) 0.3764(3) 0.0441(7) Uani 1 1 d . . . . .
C5A C 0.40093(13) 0.5229(2) 0.3036(4) 0.0537(8) Uani 1 1 d . . . . .
H5A H 0.3994 0.5932 0.3168 0.064 Uiso 1 1 calc R U . . .
C6A C 0.36205(12) 0.4730(2) 0.2099(3) 0.0449(7) Uani 1 1 d . . . . .
H6A H 0.3337 0.5112 0.1619 0.054 Uiso 1 1 calc R U . . .
N7A N 0.48285(11) 0.5264(2) 0.4705(3) 0.0572(7) Uani 1 1 d . . . . .
O1B O 0.32161(8) 0.15738(12) 0.1016(2) 0.0395(4) Uani 1 1 d . . . . .
O2B O 0.24532(8) 0.07834(12) 0.0102(2) 0.0406(4) Uani 1 1 d . . . . .
C3B C 0.29340(11) 0.07987(18) 0.0728(2) 0.0289(5) Uani 1 1 d . . . . .
C4B C 0.31814(12) -0.02183(17) 0.1262(3) 0.0397(6) Uani 1 1 d . . . . .
H4B1 H 0.3580 -0.0141 0.1382 0.048 Uiso 1 1 calc R U . . .
H4B2 H 0.3046 -0.0377 0.2278 0.048 Uiso 1 1 calc R U . . .
C5B C 0.30563(12) -0.11166(18) 0.0187(3) 0.0365(6) Uani 1 1 d . . . . .
H5B1 H 0.3242 -0.1017 -0.0778 0.044 Uiso 1 1 calc R U . . .
H5B2 H 0.2661 -0.1144 -0.0059 0.044 Uiso 1 1 calc R U . . .
C6B C 0.32436(12) -0.21255(17) 0.0917(3) 0.0351(6) Uani 1 1 d . . . . .
H6B1 H 0.3161 -0.2672 0.0183 0.042 Uiso 1 1 calc R U . . .
H6B2 H 0.3642 -0.2108 0.1116 0.042 Uiso 1 1 calc R U . . .
C7B C 0.29674(11) -0.23515(17) 0.2420(3) 0.0307(5) Uani 1 1 d . . . . .
O8B O 0.24765(8) -0.20573(12) 0.25327(19) 0.0365(4) Uani 1 1 d . . . . .
O9B O 0.32467(8) -0.28146(13) 0.34794(19) 0.0423(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O9B 1.9690(16) 6 ?
Cu1 O8B 1.9726(16) 4 ?
Cu1 O1B 1.9737(16) . ?
Cu1 O2B 1.9742(17) 7 ?
Cu1 N1A 2.179(2) . ?
Cu1 Cu1 2.6319(6) 7 ?
N1A C2A 1.323(3) . ?
N1A C6A 1.335(3) . ?
C2A C3A 1.391(4) . ?
C3A C4A 1.376(4) . ?
C4A C5A 1.362(4) . ?
C4A N7A 1.477(4) . ?
C5A C6A 1.376(4) . ?
N7A N7A 1.177(5) 5_666 ?
O1B C3B 1.243(3) . ?
O2B C3B 1.258(3) . ?
O2B Cu1 1.9742(17) 7 ?
C3B C4B 1.524(3) . ?
C4B C5B 1.520(3) . ?
C5B C6B 1.525(3) . ?
C6B C7B 1.511(3) . ?
C7B O8B 1.255(3) . ?
C7B O9B 1.265(3) . ?
O8B Cu1 1.9726(16) 4_545 ?
O9B Cu1 1.9690(16) 6_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
O9B Cu1 O8B 168.19(7) 6 4 ?
O9B Cu1 O1B 87.46(8) 6 . ?
O8B Cu1 O1B 89.85(7) 4 . ?
O9B Cu1 O2B 91.01(8) 6 7 ?
O8B Cu1 O2B 89.27(7) 4 7 ?
O1B Cu1 O2B 168.19(7) . 7 ?
O9B Cu1 N1A 102.00(7) 6 . ?
O8B Cu1 N1A 89.69(7) 4 . ?
O1B Cu1 N1A 95.11(7) . . ?
O2B Cu1 N1A 96.66(7) 7 . ?
O9B Cu1 Cu1 87.05(5) 6 7 ?
O8B Cu1 Cu1 81.24(5) 4 7 ?
O1B Cu1 Cu1 84.15(5) . 7 ?
O2B Cu1 Cu1 84.08(5) 7 7 ?
N1A Cu1 Cu1 170.89(5) . 7 ?
C2A N1A C6A 117.3(2) . . ?
C2A N1A Cu1 120.88(17) . . ?
C6A N1A Cu1 121.23(18) . . ?
N1A C2A C3A 123.5(3) . . ?
C4A C3A C2A 117.5(3) . . ?
C5A C4A C3A 120.0(3) . . ?
C5A C4A N7A 114.8(2) . . ?
C3A C4A N7A 125.1(3) . . ?
C4A C5A C6A 118.2(3) . . ?
N1A C6A C5A 123.5(3) . . ?
N7A N7A C4A 111.5(3) 5_666 . ?
C3B O1B Cu1 123.11(17) . . ?
C3B O2B Cu1 122.80(15) . 7 ?
O1B C3B O2B 125.8(2) . . ?
O1B C3B C4B 116.9(2) . . ?
O2B C3B C4B 117.2(2) . . ?
C5B C4B C3B 115.5(2) . . ?
C4B C5B C6B 112.1(2) . . ?
C7B C6B C5B 112.9(2) . . ?
O8B C7B O9B 124.6(2) . . ?
O8B C7B C6B 117.4(2) . . ?
O9B C7B C6B 118.0(2) . . ?
C7B O8B Cu1 126.63(15) . 4_545 ?
C7B O9B Cu1 119.86(17) . 6_556 ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.070

_shelxl_version_number           2014-3




# start Validation Reply Form
_vrf_CHEMW03_GR-MOF-2            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This compound contains two crystallization water molecules per
formula unit that could not be resolved since they are highly disordered.
;
_vrf_PLAT230_GR-MOF-2            
;
PROBLEM: Hirshfeld Test Diff for    N7A    --  C4A     ..       11.0 s.u.  
RESPONSE: This atoms seem to be affected by the absence of crystallization
water molecules in the final model.
;
# end Validation Reply Form
_exptl_crystal_preparation       'adsorption properties'
####################################################################### 
# 
# 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_GR-MOF-4
_database_code_depnum_ccdc_archive 'CCDC 1836114'
_audit_update_record             
;
2018-04-10 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014


_chemical_name_systematic        
"poly-{[(mu-1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene)-kN,N')bis(mu4-2,2'-dimethylglutarato-kO:kO':kO'':kO''')dicopper(II)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H15 Cu N2 O4, 2(H2 O)'
_chemical_formula_sum            'C13 H19 Cu N2 O6'
_chemical_formula_weight         362.84

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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   27.253(1)
_cell_length_b                   13.608(1)
_cell_length_c                   9.146(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.81(3)
_cell_angle_gamma                90
_cell_volume                     3387.8(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25819
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.338

# SQUEEZE RESULTS (Version = 160617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.030 435 18 ' '
2 0.500 0.500 -0.023 435 18 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
2 0 0 1.496
1 1 0 1.673
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelx     C 2/c        R = 0.05
CELL   27.2530   13.6080    9.1460     90.00     92.81     90.00
SPGR C2/c
# Solvent Accessible Volume =       860
# Electrons Found in S.A.V. =        34
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.885 0.114 0.222 !       0.58 eA-3
Q102 0.796 0.096-0.003 !       0.56 eA-3
Q103 0.784 0.502 0.464 !       0.54 eA-3
Q104 0.773 0.191 0.368 !       0.53 eA-3
Q105 0.298 0.315 0.476 !       0.52 eA-3
Q106 0.188 0.401 0.031 !       0.52 eA-3
Q107 0.263 0.179 0.374 !       0.51 eA-3
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.317
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            25819
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.698
_diffrn_reflns_theta_max         23.291
_diffrn_reflns_theta_full        23.300
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2432
_reflns_number_gt                1703
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;The crystal structure contains large voids filled with disordered
water molecules. Given the impossibility to refine them, their 
electron density was subtracted with the SQUEEZE routine as implemented
in PLATON.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0577P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2432
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1097
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.71242(2) 0.20010(4) 0.04187(6) 0.0211(2) Uani 1 1 d . . . . .
C2A C 0.65990(16) 0.0306(3) 0.1891(5) 0.0236(12) Uani 1 1 d . . . . .
H2A H 0.6882 -0.0027 0.1647 0.028 Uiso 1 1 calc R U . . .
C3A C 0.62693(17) -0.0170(3) 0.2734(5) 0.0249(12) Uani 1 1 d . . . . .
H3A H 0.6327 -0.0814 0.3034 0.030 Uiso 1 1 calc R U . . .
C3B C 0.79904(19) 0.2129(3) 0.2363(5) 0.0266(12) Uani 1 1 d . . . . .
C4A C 0.58510(16) 0.0320(3) 0.3132(4) 0.0196(11) Uani 1 1 d . . . . .
C4B C 0.8281(2) 0.1814(4) 0.3742(6) 0.0448(15) Uani 1 1 d . . . . .
C5A C 0.57808(16) 0.1272(3) 0.2628(5) 0.0266(12) Uani 1 1 d . . . . .
H5A H 0.5504 0.1626 0.2866 0.032 Uiso 1 1 calc R U . . .
C5B C 0.8070(2) 0.0857(3) 0.4362(5) 0.0366(14) Uani 1 1 d . . . . .
H5B1 H 0.8257 0.0691 0.5258 0.044 Uiso 1 1 calc R U . . .
H5B2 H 0.7734 0.0978 0.4614 0.044 Uiso 1 1 calc R U . . .
C6A C 0.61239(17) 0.1684(3) 0.1779(5) 0.0250(11) Uani 1 1 d . . . . .
H6A H 0.6071 0.2321 0.1438 0.030 Uiso 1 1 calc R U . . .
C6B C 0.80744(19) -0.0022(3) 0.3341(5) 0.0383(14) Uani 1 1 d . . . . .
H6B1 H 0.7891 0.0141 0.2438 0.046 Uiso 1 1 calc R U . . .
H6B2 H 0.8411 -0.0157 0.3102 0.046 Uiso 1 1 calc R U . . .
C7A C 0.54989(17) -0.0160(3) 0.4041(5) 0.0255(12) Uani 1 1 d . . . . .
H7A H 0.5532 -0.0828 0.4238 0.031 Uiso 1 1 calc R U . . .
C7B C 0.78561(18) -0.0937(3) 0.3990(5) 0.0242(11) Uani 1 1 d . . . . .
O8B O 0.80938(12) -0.1714(2) 0.3875(3) 0.0312(9) Uani 1 1 d . . . . .
O9B O 0.74467(12) -0.0859(2) 0.4565(4) 0.0349(9) Uani 1 1 d . . . . .
C41B C 0.8232(3) 0.2624(4) 0.4872(6) 0.088(3) Uani 1 1 d . . . . .
H41A H 0.8398 0.3204 0.4556 0.132 Uiso 1 1 calc R U . . .
H41B H 0.8378 0.2411 0.5795 0.132 Uiso 1 1 calc R U . . .
H41C H 0.7891 0.2768 0.4977 0.132 Uiso 1 1 calc R U . . .
C42B C 0.8823(2) 0.1678(5) 0.3407(8) 0.092(3) Uani 1 1 d . . . . .
H42A H 0.8848 0.1213 0.2624 0.137 Uiso 1 1 calc R U . . .
H42B H 0.9002 0.1439 0.4264 0.137 Uiso 1 1 calc R U . . .
H42C H 0.8958 0.2297 0.3121 0.137 Uiso 1 1 calc R U . . .
N1A N 0.65332(13) 0.1215(2) 0.1412(4) 0.0192(9) Uani 1 1 d . . . . .
N8A N 0.51474(14) 0.0312(3) 0.4574(4) 0.0311(10) Uani 1 1 d . . . . .
O1B O 0.75537(12) 0.1837(2) 0.2179(3) 0.0318(8) Uani 1 1 d . . . . .
O2B O 0.82032(12) 0.2673(2) 0.1490(3) 0.0342(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1B 1.956(3) . ?
Cu1 O9B 1.966(3) 6 ?
Cu1 O8B 1.966(3) 4_655 ?
Cu1 O2B 1.972(3) 7_655 ?
Cu1 N1A 2.169(3) . ?
Cu1 Cu1 2.6040(11) 7_655 ?
C2A N1A 1.322(5) . ?
C2A C3A 1.374(6) . ?
C3A C4A 1.385(6) . ?
C3B O2B 1.252(5) . ?
C3B O1B 1.258(5) . ?
C3B C4B 1.518(7) . ?
C4A C5A 1.385(6) . ?
C4A C7A 1.455(6) . ?
C4B C41B 1.521(7) . ?
C4B C42B 1.534(8) . ?
C4B C5B 1.543(6) . ?
C5A C6A 1.365(6) . ?
C5B C6B 1.517(6) . ?
C6A N1A 1.342(5) . ?
C6B C7B 1.515(6) . ?
C7A N8A 1.270(5) . ?
C7B O8B 1.246(5) . ?
C7B O9B 1.261(5) . ?
O8B Cu1 1.966(3) 4_645 ?
O9B Cu1 1.966(3) 6_556 ?
N8A N8A 1.428(7) 5_656 ?
O2B Cu1 1.972(3) 7_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
O1B Cu1 O9B 88.59(14) . 6 ?
O1B Cu1 O8B 90.52(13) . 4_655 ?
O9B Cu1 O8B 169.03(12) 6 4_655 ?
O1B Cu1 O2B 168.75(12) . 7_655 ?
O9B Cu1 O2B 91.05(14) 6 7_655 ?
O8B Cu1 O2B 87.69(14) 4_655 7_655 ?
O1B Cu1 N1A 91.48(13) . . ?
O9B Cu1 N1A 97.60(12) 6 . ?
O8B Cu1 N1A 93.35(12) 4_655 . ?
O2B Cu1 N1A 99.71(13) 7_655 . ?
O1B Cu1 Cu1 81.59(9) . 7_655 ?
O9B Cu1 Cu1 85.53(9) 6 7_655 ?
O8B Cu1 Cu1 83.53(9) 4_655 7_655 ?
O2B Cu1 Cu1 87.17(9) 7_655 7_655 ?
N1A Cu1 Cu1 172.35(10) . 7_655 ?
N1A C2A C3A 123.0(4) . . ?
C2A C3A C4A 119.4(4) . . ?
O2B C3B O1B 124.5(4) . . ?
O2B C3B C4B 117.2(4) . . ?
O1B C3B C4B 118.3(4) . . ?
C3A C4A C5A 117.7(4) . . ?
C3A C4A C7A 120.6(4) . . ?
C5A C4A C7A 121.7(4) . . ?
C3B C4B C41B 107.5(5) . . ?
C3B C4B C42B 109.7(5) . . ?
C41B C4B C42B 109.9(5) . . ?
C3B C4B C5B 110.8(4) . . ?
C41B C4B C5B 108.4(4) . . ?
C42B C4B C5B 110.6(5) . . ?
C6A C5A C4A 119.1(4) . . ?
C6B C5B C4B 115.1(4) . . ?
N1A C6A C5A 123.3(4) . . ?
C7B C6B C5B 113.1(4) . . ?
N8A C7A C4A 121.5(4) . . ?
O8B C7B O9B 125.5(4) . . ?
O8B C7B C6B 116.7(4) . . ?
O9B C7B C6B 117.8(4) . . ?
C7B O8B Cu1 124.0(3) . 4_645 ?
C7B O9B Cu1 121.4(3) . 6_556 ?
C2A N1A C6A 117.6(4) . . ?
C2A N1A Cu1 120.6(3) . . ?
C6A N1A Cu1 120.9(3) . . ?
C7A N8A N8A 111.3(4) . 5_656 ?
C3B O1B Cu1 126.7(3) . . ?
C3B O2B Cu1 119.6(3) . 7_655 ?

_refine_diff_density_max         0.478
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.082

_shelxl_version_number           2014-3





# start Validation Reply Form
_vrf_CHEMW03_GR-MOF-4            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Two crystallization water molecules could not be found in the 
voids of the structure, so SQUEEZE routine has been applied for the
final refinement of the structure.
;
_vrf_THETM01_GR-MOF-4            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Crystal structure contains a large void volume in which disordered
water molecules are placed. Therefore, these crystal diffract only up to 
not too high 2theta angles.
;
_vrf_PLAT043_GR-MOF-4            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      36.02 Check 
RESPONSE: Two crystallization water molecules could not be found in the 
voids of the structure, so SQUEEZE routine has been applied for the
final refinement of the structure.
;
_vrf_PLAT601_GR-MOF-4            
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        430 Ang3  
RESPONSE: Two crystallization water molecules could not be found in the 
voids of the structure, so SQUEEZE routine has been applied for the
final refinement of the structure.
;
# end Validation Reply Form
_exptl_crystal_preparation       adsorption
####################################################################### 
# 
# 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_GR-MOF-3
_database_code_depnum_ccdc_archive 'CCDC 1836113'
_audit_update_record             
;
2018-04-10 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014


_chemical_name_systematic        
"poly-{[(mu-1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene)-kN,N')bis(mu4-2-methylglutarato-kO:kO':kO'':kO''')dicopper(II)] pentahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 Cu2 N4 O8, 5(H2 O)'
_chemical_formula_sum            'C24 H36 Cu2 N4 O13'
_chemical_formula_weight         715.64

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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   27.019(9)
_cell_length_b                   13.506(5)
_cell_length_c                   8.921(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.792(6)
_cell_angle_gamma                90
_cell_volume                     3244(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25819
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.338

# SQUEEZE RESULTS (Version = 160617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.088 0.531 -0.045 26 3 ' '
2 0.412 0.969 0.045 26 3 ' '
3 0.588 0.031 -0.045 26 3 ' '
4 0.912 0.469 0.045 26 3 ' '
5 0.088 0.469 0.455 26 3 ' '
6 0.588 0.969 0.455 26 3 ' '
7 0.412 0.031 0.545 26 3 ' '
8 0.912 0.531 0.545 26 3 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
2 0 0 1.513
1 1 0 1.687
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelx     C 2/c        R = 0.05
CELL   27.0190   13.5060    8.9210     90.00     94.79     90.00
SPGR C2/c
# Solvent Accessible Volume =       216
# Electrons Found in S.A.V. =        23
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
Q101 0.131 0.502 0.112 !       1.45 eA-3
Q102 0.907 0.406 0.059 !       0.83 eA-3
Q103 0.538 0.096 0.034 !       0.82 eA-3
Q104 0.952 0.437-0.003 !       0.79 eA-3
Q105 0.445 0.096 0.130 !       0.69 eA-3
Q106 0.450 0.043 0.282 !       0.54 eA-3
Q107 0.431 0.037 0.256 !       0.53 eA-3
Q108 0.023 0.230 0.075 !       0.51 eA-3
Q109 0.578 0.235 0.840 !       0.50 eA-3
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.376
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            25819
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.725
_diffrn_reflns_theta_max         23.338
_diffrn_reflns_theta_full        23.350
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2337
_reflns_number_gt                1893
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;Single crystals are twinned so the twin law specified in the manuscript, that is,
(0  1  2  0 -1  0  1  0  0) has been employed in the refinement.
Moreover, the crystal structure contains large voids filled with disordered
water molecules. Given the impossibility to refine them, their 
electron density was subtracted with the SQUEEZE routine as implemented
in PLATON.,Twin,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0877P)²+20.5172P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2337
_refine_ls_number_parameters     185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1568
_refine_ls_wR_factor_gt          0.1440
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.21014(2) -0.20389(4) 0.03595(7) 0.0222(3) Uani 1 1 d . . . . .
C1A C 0.1114(2) -0.1754(4) 0.1776(7) 0.0340(14) Uani 1 1 d . . . . .
H1A H 0.1070 -0.2413 0.1495 0.041 Uiso 1 1 calc R U . . .
C3B C 0.2863(2) -0.0879(4) -0.0794(6) 0.0304(13) Uani 1 1 d . . . . .
C2A C 0.0774(2) -0.1328(4) 0.2642(7) 0.0352(14) Uani 1 1 d . . . . .
H2A H 0.0508 -0.1694 0.2939 0.042 Uiso 1 1 calc R U . . .
C4B C 0.3078(2) 0.0095(4) -0.1327(8) 0.0435(17) Uani 1 1 d . . . . .
H4B1 H 0.2929 0.0243 -0.2328 0.052 Uiso 1 1 calc R U . . .
H4B2 H 0.3432 0.0015 -0.1391 0.052 Uiso 1 1 calc R U . . .
C3A C 0.08348(18) -0.0346(4) 0.3065(6) 0.0217(12) Uani 1 1 d . . . . .
C5B C 0.2991(3) 0.0972(4) -0.0290(7) 0.0426(17) Uani 1 1 d . . . . .
H5B1 H 0.2637 0.1040 -0.0193 0.051 Uiso 1 1 calc R U . . .
H5B2 H 0.3152 0.0841 0.0702 0.051 Uiso 1 1 calc R U . . .
C4A C 0.12346(19) 0.0164(4) 0.2585(6) 0.0252(12) Uani 1 1 d . . . . .
H4A H 0.1284 0.0827 0.2839 0.030 Uiso 1 1 calc R U . . .
C6B C 0.3189(3) 0.1935(5) -0.0883(8) 0.058(2) Uani 1 1 d . . . . .
C61B C 0.3290(6) 0.2659(12) 0.0010(18) 0.064(4) Uiso 0.5 1 d . . P A 1
H61A H 0.3417 0.3201 -0.0537 0.096 Uiso 0.5 1 calc R U P A 1
H61B H 0.3534 0.2456 0.0793 0.096 Uiso 0.5 1 calc R U P A 1
H61C H 0.2994 0.2864 0.0448 0.096 Uiso 0.5 1 calc R U P A 1
C62B C 0.3682(8) 0.2028(14) -0.077(2) 0.088(6) Uiso 0.5 1 d . . P A 2
H62A H 0.3821 0.1570 -0.1444 0.132 Uiso 0.5 1 calc R U P A 2
H62B H 0.3811 0.1889 0.0243 0.132 Uiso 0.5 1 calc R U P A 2
H62C H 0.3769 0.2691 -0.1031 0.132 Uiso 0.5 1 calc R U P A 2
C5A C 0.15581(19) -0.0314(4) 0.1733(6) 0.0246(12) Uani 1 1 d . . . . .
H5A H 0.1828 0.0036 0.1426 0.030 Uiso 1 1 calc R U . . .
C7B C 0.2937(2) 0.2210(4) -0.2418(6) 0.0319(14) Uani 1 1 d . . . . .
C6A C 0.04800(19) 0.0162(4) 0.3976(6) 0.0268(13) Uani 1 1 d . . . . .
H6A H 0.0498 0.0846 0.4091 0.032 Uiso 1 1 calc R U . . .
N1A N 0.15023(16) -0.1268(3) 0.1319(5) 0.0244(10) Uani 1 1 d . . . . .
N2A N 0.01519(16) -0.0316(3) 0.4602(5) 0.0272(11) Uani 1 1 d . . . . .
O1B O 0.24404(15) -0.0850(3) -0.0323(5) 0.0382(11) Uani 1 1 d . . . . .
O2B O 0.31191(14) -0.1629(3) -0.0897(5) 0.0361(10) Uani 1 1 d . . . . .
O8B O 0.25005(15) 0.1947(3) -0.2694(4) 0.0359(10) Uani 1 1 d . . . . .
O9B O 0.31891(16) 0.2687(3) -0.3300(5) 0.0431(11) Uani 1 1 d . . . . .
O1W O 0.0715(5) 0.2753(10) 0.3310(14) 0.190(5) Uiso 1 1 d . . . . .
O2W O 0.0200(7) -0.2546(15) 0.561(2) 0.289(8) Uiso 1 1 d . . . . .
H11W H 0.1019 0.2434 0.3178 0.433 Uiso 1 1 d . U . . .
H12W H 0.0548 0.2518 0.2534 0.433 Uiso 1 1 d . U . . .
H21W H -0.0139 -0.2681 0.5326 0.433 Uiso 1 1 d . U . . .
H22W H 0.0217 -0.2017 0.6089 0.433 Uiso 1 1 d . U . . .
O3W O 0.0136(19) -0.389(3) 0.327(5) 0.37(3) Uiso 0.5 1 d . . P B -3


_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
Cu1 O2B 1.967(4) 7_545 ?
Cu1 O1B 1.970(4) . ?
Cu1 O8B 1.970(4) 6_556 ?
Cu1 O9B 1.972(4) 4_544 ?
Cu1 N1A 2.161(4) . ?
Cu1 Cu1 2.6139(13) 7_545 ?
C1A N1A 1.330(7) . ?
C1A C2A 1.374(8) . ?
C1A H1A 0.9300 . ?
C3B O2B 1.234(7) . ?
C3B O1B 1.250(7) . ?
C3B C4B 1.530(8) . ?
C2A C3A 1.385(8) . ?
C2A H2A 0.9300 . ?
C4B C5B 1.533(9) . ?
C4B H4B1 0.9700 . ?
C4B H4B2 0.9700 . ?
C3A C4A 1.379(7) . ?
C3A C6A 1.477(7) . ?
C5B C6B 1.519(8) . ?
C5B H5B1 0.9700 . ?
C5B H5B2 0.9700 . ?
C4A C5A 1.368(7) . ?
C4A H4A 0.9300 . ?
C6B C61B 1.276(17) . ?
C6B C62B 1.33(2) . ?
C6B C7B 1.523(8) . ?
C61B H61A 0.9600 . ?
C61B H61B 0.9600 . ?
C61B H61C 0.9600 . ?
C62B H62A 0.9600 . ?
C62B H62B 0.9600 . ?
C62B H62C 0.9600 . ?
C5A N1A 1.346(7) . ?
C5A H5A 0.9300 . ?
C7B O8B 1.238(7) . ?
C7B O9B 1.259(7) . ?
C6A N2A 1.264(7) . ?
C6A H6A 0.9300 . ?
N2A N2A 1.417(8) 5_556 ?
O2B Cu1 1.967(4) 7_545 ?
O8B Cu1 1.970(4) 6 ?
O9B Cu1 1.972(4) 4_554 ?
O1W H11W 0.9429 . ?
O1W H12W 0.8554 . ?
O2W H21W 0.9461 . ?
O2W H22W 0.8325 . ?

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
O2B Cu1 O1B 168.21(15) 7_545 . ?
O2B Cu1 O8B 89.85(18) 7_545 6_556 ?
O1B Cu1 O8B 89.23(18) . 6_556 ?
O2B Cu1 O9B 87.17(19) 7_545 4_544 ?
O1B Cu1 O9B 91.38(19) . 4_544 ?
O8B Cu1 O9B 168.30(16) 6_556 4_544 ?
O2B Cu1 N1A 95.25(16) 7_545 . ?
O1B Cu1 N1A 96.49(15) . . ?
O8B Cu1 N1A 89.61(16) 6_556 . ?
O9B Cu1 N1A 101.93(17) 4_544 . ?
O2B Cu1 Cu1 84.07(11) 7_545 7_545 ?
O1B Cu1 Cu1 84.17(11) . 7_545 ?
O8B Cu1 Cu1 81.08(12) 6_556 7_545 ?
O9B Cu1 Cu1 87.36(12) 4_544 7_545 ?
N1A Cu1 Cu1 170.66(12) . 7_545 ?
N1A C1A C2A 123.2(5) . . ?
N1A C1A H1A 118.4 . . ?
C2A C1A H1A 118.4 . . ?
O2B C3B O1B 125.8(5) . . ?
O2B C3B C4B 117.0(5) . . ?
O1B C3B C4B 117.3(5) . . ?
C1A C2A C3A 119.0(5) . . ?
C1A C2A H2A 120.5 . . ?
C3A C2A H2A 120.5 . . ?
C3B C4B C5B 113.4(5) . . ?
C3B C4B H4B1 108.9 . . ?
C5B C4B H4B1 108.9 . . ?
C3B C4B H4B2 108.9 . . ?
C5B C4B H4B2 108.9 . . ?
H4B1 C4B H4B2 107.7 . . ?
C4A C3A C2A 118.1(5) . . ?
C4A C3A C6A 120.0(5) . . ?
C2A C3A C6A 121.9(5) . . ?
C6B C5B C4B 112.1(6) . . ?
C6B C5B H5B1 109.2 . . ?
C4B C5B H5B1 109.2 . . ?
C6B C5B H5B2 109.2 . . ?
C4B C5B H5B2 109.2 . . ?
H5B1 C5B H5B2 107.9 . . ?
C5A C4A C3A 119.3(5) . . ?
C5A C4A H4A 120.3 . . ?
C3A C4A H4A 120.3 . . ?
C61B C6B C5B 120.1(10) . . ?
C62B C6B C5B 115.7(10) . . ?
C61B C6B C7B 115.5(9) . . ?
C62B C6B C7B 114.4(11) . . ?
C5B C6B C7B 112.2(5) . . ?
C6B C61B H61A 109.5 . . ?
C6B C61B H61B 109.5 . . ?
H61A C61B H61B 109.5 . . ?
C6B C61B H61C 109.5 . . ?
H61A C61B H61C 109.5 . . ?
H61B C61B H61C 109.5 . . ?
C6B C62B H62A 109.5 . . ?
C6B C62B H62B 109.5 . . ?
H62A C62B H62B 109.5 . . ?
C6B C62B H62C 109.5 . . ?
H62A C62B H62C 109.5 . . ?
H62B C62B H62C 109.5 . . ?
N1A C5A C4A 122.9(5) . . ?
N1A C5A H5A 118.6 . . ?
C4A C5A H5A 118.6 . . ?
O8B C7B O9B 125.4(5) . . ?
O8B C7B C6B 117.1(5) . . ?
O9B C7B C6B 117.5(6) . . ?
N2A C6A C3A 121.1(5) . . ?
N2A C6A H6A 119.4 . . ?
C3A C6A H6A 119.4 . . ?
C1A N1A C5A 117.5(4) . . ?
C1A N1A Cu1 121.4(3) . . ?
C5A N1A Cu1 120.0(3) . . ?
C6A N2A N2A 111.7(6) . 5_556 ?
C3B O1B Cu1 122.7(3) . . ?
C3B O2B Cu1 123.3(4) . 7_545 ?
C7B O8B Cu1 126.8(4) . 6 ?
C7B O9B Cu1 119.0(4) . 4_554 ?
H11W O1W H12W 97.7 . . ?
H21W O2W H22W 108.2 . . ?

_refine_diff_density_max         1.318
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.121

_shelxl_version_number           2014-3






# start Validation Reply Form
_vrf_THETM01_GR-MOF-3            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Crystal structure contains a large void volume in which disordered
water molecules are placed. Therefore, these crystal diffract only up to 
not too high 2theta angles.
;
_vrf_PLAT417_GR-MOF-3            
;
PROBLEM: Short Inter D-H..H-D       H12W   ..  H22W    ..       1.65 Ang.  
RESPONSE: Though the disorder corresponding to the lattice water molecules could
be solved, one of these molecules is disordered into two symmetry related positions,
so their hydrogen atoms could not be found. This, in turn, makes hydrogen atoms 
belonging to neighbouring water molecules to be somewhat close to each other so that
they point out through optimal hydrogen bonds.
;
_vrf_PLAT415_GR-MOF-3            
;
PROBLEM: Short Inter D-H..H-X       H11W   ..  H42C    ..       2.02 Ang.  
RESPONSE: Hydrogen atoms belonging to lattice water molecules have been refined 
in order to maximize the angle according to the hydrogen bonding interactions in which they
take part. On the contrary, methyl hydrogen atoms have been geometrically refined following
an idealised electron density.
;
_vrf_PLAT420_GR-MOF-3            
;
PROBLEM: D-H Without Acceptor       O2W    --  H22W   ...     Please Check 
RESPONSE: Though the disorder corresponding to the lattice water molecules could
be solved, one of these molecules is disordered into two symmetry related positions,
so their hydrogen atoms could not be found. This, in turn, makes hydrogen atoms 
belonging to neighbouring water molecules to be somewhat close to each other so that
they point out through optimal hydrogen bonds.
;
# end Validation Reply Form
_exptl_crystal_preparation       adsorption
####################################################################### 
# 
# 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_GR-MOF-5
_database_code_depnum_ccdc_archive 'CCDC 1836115'
_audit_update_record             
;
2018-04-10 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014


_chemical_name_systematic        
"poly-{[(mu-2,5-bis(4-pyridyl)-1,3,4-oxadiazole)-kN,N')bis(mu4-glutarato-kO:kO':kO'':kO''')dicopper(II)] tetrahydrate}"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Cu2 N4 O7, 4(H2 O)'
_chemical_formula_sum            'C22 H28 Cu2 N4 O13'
_chemical_formula_weight         683.56

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   26.9173(1)
_cell_length_b                   12.987(1)
_cell_length_c                   8.574(1)
_cell_angle_alpha                90
_cell_angle_beta                 104.82(1)
_cell_angle_gamma                90
_cell_volume                     2897.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    34817
_cell_measurement_theta_min      2.824
_cell_measurement_theta_max      28.767

# SQUEEZE RESULTS (Version = 160617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 -0.026 402 68 ' '
2 0.500 0.000 0.067 402 68 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
2 0 0 1.565
1 1 0 1.752
3 1 0 2.824
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelx     C 2/c        R = 0.05
CELL   26.9173   12.9871    8.5739     90.00    104.82     90.00
SPGR C2/c
# Solvent Accessible Volume =       804
# Electrons Found in S.A.V. =       134
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.046 0.411 0.839 !       1.03 eA-3
C102 1.001 0.498 0.163 !       0.91 eA-3
C103 0.525 0.048 0.344 !       0.86 eA-3
C104 0.984 0.466 0.716 !       0.84 eA-3
C105 0.538 0.015 0.880 !       0.83 eA-3
C106 0.986 0.451 0.409 !       0.80 eA-3
C107 0.953 0.420 0.154 !       0.80 eA-3
C108 0.525 0.076 0.907 !       0.79 eA-3
C109 0.448 0.078 0.475 !       0.78 eA-3
C110 0.468 0.118 0.429 !       0.78 eA-3
C111 0.405 0.097 0.975 !       0.77 eA-3
C112 0.513 0.064-0.010 !       0.76 eA-3
Q113 0.868 0.221 0.119 !       0.76 eA-3
C114 0.011 0.327 0.215 !       0.75 eA-3
C115 0.017 0.333 0.749 !       0.75 eA-3
C116 0.509 0.062 0.066 !       0.74 eA-3
C117 0.961 0.500 0.535 !       0.74 eA-3
C118 0.477 0.112 0.065 !       0.74 eA-3
C119 0.524 0.034 0.063 !       0.73 eA-3
C120 0.436 0.079 0.752 !       0.73 eA-3
Q121 0.758 0.365 0.814 !       0.73 eA-3
Q122 0.704 0.220 0.500 !       0.73 eA-3
C123 0.445 0.172 0.186 !       0.73 eA-3
C124 0.511 0.091 0.343 !       0.72 eA-3
C125 0.954 0.444 0.843 !       0.72 eA-3
C126 0.436 0.091 0.566 !       0.72 eA-3
Q127 0.352 0.338 0.688 !       0.71 eA-3
C128 0.981 0.618 0.247 !       0.71 eA-3
Q129 0.884 0.084 0.716 !       0.71 eA-3
C130 0.477 0.064-0.005 !       0.71 eA-3
C131 0.059 0.410 0.035 !       0.70 eA-3
C132 0.514 0.118 0.820 !       0.70 eA-3
C133 0.492 0.128 0.867 !       0.70 eA-3
C134 0.032 0.334 0.881 !       0.70 eA-3
C135 0.462 0.108 0.907 !       0.70 eA-3
Q136 0.772 0.484 0.783 !       0.69 eA-3
C137 0.930 0.342 0.606 !       0.69 eA-3
Q138 0.430 0.422 0.410 !       0.69 eA-3
C139 0.011 0.455 0.285 !       0.69 eA-3
C140 0.025 0.326 0.153 !       0.69 eA-3
Q141 0.414 0.424 0.165 !       0.69 eA-3
Q142 0.960 0.203 0.937 !       0.69 eA-3
C143 0.078 0.386 0.367 !       0.68 eA-3
C144 0.954 0.449 0.740 !       0.68 eA-3
C145 0.497 0.122-0.001 !       0.67 eA-3
C146 0.953 0.391 0.277 !       0.67 eA-3
Q147 0.142 0.253 0.064 !       0.67 eA-3
C148 0.530 0.124 0.179 !       0.66 eA-3
Q149 0.749 0.441 0.028 !       0.66 eA-3
Q150 0.368 0.078 0.221 !       0.65 eA-3
Q151 0.516 0.439 0.412 !       0.65 eA-3
Q152 0.907 0.345 0.882 !       0.65 eA-3
Q153 0.680 0.078 0.878 !       0.65 eA-3
Q154 0.711 0.184 0.431 !       0.65 eA-3
Q155 0.884 0.122 0.463 !       0.65 eA-3
Q156 0.726 0.484-0.006 !       0.65 eA-3
C157 0.586 0.079 0.147 !       0.65 eA-3
Q158 0.149 0.285 0.343 !       0.65 eA-3
Q159 0.752 0.296 0.843 !       0.64 eA-3
Q160 0.219 0.357 0.878 !       0.64 eA-3
Q161 0.843 0.271 0.253 !       0.64 eA-3
Q162 0.242 0.014 0.407 !       0.64 eA-3
Q163 0.734 0.061 0.030 !       0.64 eA-3
Q164 0.210 0.471 0.125 !       0.63 eA-3
Q165 0.649 0.343 0.689 !       0.63 eA-3
Q166 0.525 0.332 0.269 !       0.63 eA-3
Q167 0.757 0.183 0.276 !       0.63 eA-3
Q168 0.610 0.171 0.224 !       0.63 eA-3
Q169 0.711 0.107 0.064 !       0.63 eA-3
Q170 0.639 0.264 0.667 !       0.63 eA-3
C171 0.569 0.030 0.001 !       0.62 eA-3
Q172 0.842 0.311 0.037 !       0.62 eA-3
Q173 0.507 0.450 0.587 !       0.62 eA-3
C174 0.938 0.504 0.811 !       0.62 eA-3
Q175 0.758 0.441 0.658 !       0.62 eA-3
Q176 0.736 0.326 0.373 !       0.61 eA-3
Q177 0.602 0.061 0.432 !       0.61 eA-3
Q178 0.132 0.422 0.501 !       0.61 eA-3
C179 0.564 0.092 0.249 !       0.61 eA-3
C180 0.469 0.032 0.341 !       0.61 eA-3
Q181 0.150 0.097 0.248 !       0.61 eA-3
Q182 0.195 0.468 0.750 !       0.60 eA-3
Q183 0.986 0.155 0.277 !       0.60 eA-3
C184 0.094 0.433 0.471 !       0.60 eA-3
Q185 0.874 0.502 0.035 !       0.60 eA-3
Q186 0.766 0.065 0.874 !       0.60 eA-3
C187 0.430 0.070 0.061 !       0.60 eA-3
C188 0.464 0.173 0.032 !       0.60 eA-3
Q189 0.064 0.166 0.399 !       0.60 eA-3
Q190 0.212 0.035 0.896 !       0.59 eA-3
Q191 0.852 0.645 0.659 !       0.59 eA-3
Q192 0.352 0.145 0.659 !       0.59 eA-3
Q193 0.608 0.107 0.716 !       0.59 eA-3
Q194 0.378 0.358 0.276 !       0.59 eA-3
C195 0.437 0.014 0.417 !       0.59 eA-3
C196 0.008 0.510 0.478 !       0.59 eA-3
Q197 0.025 0.297 0.318 !       0.59 eA-3
Q198 0.406 0.139 0.566 !       0.59 eA-3
Q199 0.788 0.084 0.381 !       0.59 eA-3
;

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.537
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            34809
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.851
_diffrn_reflns_theta_max         28.767
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3755
_reflns_number_gt                2743
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;The crystal structure contains large voids filled with disordered
water molecules. Given the impossibility to refine them, their 
electron density was subtracted with the SQUEEZE routine as implemented
in PLATON.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²+0.6035P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3755
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.79112(2) 0.20256(2) 0.58488(3) 0.01656(11) Uani 1 1 d . . . . .
C1A C 0.88869(10) 0.1888(2) 0.8603(3) 0.0237(6) Uani 1 1 d . . . . .
H1A H 0.8874 0.2595 0.8420 0.028 Uiso 1 1 calc R U . . .
C3B C 0.78969(11) 0.42373(19) 0.5971(3) 0.0205(6) Uani 1 1 d . . . . .
C2A C 0.92626(10) 0.1518(2) 0.9878(3) 0.0235(6) Uani 1 1 d . . . . .
H2A H 0.9498 0.1961 1.0535 0.028 Uiso 1 1 calc R U . . .
C4B C 0.81370(12) 0.5239(2) 0.6647(3) 0.0285(6) Uani 1 1 d . . . . .
H4B1 H 0.8507 0.5146 0.6982 0.034 Uiso 1 1 calc R U . . .
H4B2 H 0.8023 0.5399 0.7604 0.034 Uiso 1 1 calc R U . . .
C3A C 0.92818(9) 0.0464(2) 1.0158(3) 0.0185(5) Uani 1 1 d . . . . .
C5B C 0.80203(11) 0.6159(2) 0.5510(3) 0.0255(6) Uani 1 1 d . . . . .
H5B1 H 0.7653 0.6189 0.5021 0.031 Uiso 1 1 calc R U . . .
H5B2 H 0.8192 0.6067 0.4652 0.031 Uiso 1 1 calc R U . . .
C4A C 0.89193(10) -0.0167(2) 0.9157(3) 0.0211(6) Uani 1 1 d . . . . .
H4A H 0.8922 -0.0875 0.9319 0.025 Uiso 1 1 calc R U . . .
C6B C 0.81947(12) 0.7173(2) 0.6374(3) 0.0266(6) Uani 1 1 d . . . . .
H6B1 H 0.8564 0.7154 0.6817 0.032 Uiso 1 1 calc R U . . .
H6B2 H 0.8117 0.7731 0.5598 0.032 Uiso 1 1 calc R U . . .
C5A C 0.85553(10) 0.0285(2) 0.7915(3) 0.0200(6) Uani 1 1 d . . . . .
H5A H 0.8308 -0.0134 0.7256 0.024 Uiso 1 1 calc R U . . .
C7B C 0.79413(10) 0.73861(19) 0.7714(3) 0.0187(5) Uani 1 1 d . . . . .
C6A C 0.96813(9) 0.00201(19) 1.1476(3) 0.0170(5) Uani 1 1 d . . . . .
N1A N 0.85400(8) 0.13007(16) 0.7610(2) 0.0187(5) Uani 1 1 d . . . . .
N2A N 0.97887(8) -0.09340(17) 1.1815(2) 0.0218(5) Uani 1 1 d . . . . .
O1A O 1.0000 0.06746(19) 1.2500 0.0201(6) Uani 1 2 d S T P . .
O1B O 0.81573(7) 0.34393(14) 0.6437(2) 0.0266(4) Uani 1 1 d . . . . .
O2B O 0.74531(8) 0.42483(13) 0.5025(2) 0.0274(4) Uani 1 1 d . . . . .
O8B O 0.81980(7) 0.78511(15) 0.8955(2) 0.0291(5) Uani 1 1 d . . . . .
O9B O 0.74895(7) 0.70765(14) 0.7515(2) 0.0251(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2B 1.9708(18) 7_656 ?
Cu1 O1B 1.9730(18) . ?
Cu1 O8B 1.9744(18) 6_565 ?
Cu1 O9B 1.9771(18) 4_646 ?
Cu1 N1A 2.174(2) . ?
Cu1 Cu1 2.6244(6) 7_656 ?
C1A N1A 1.331(3) . ?
C1A C2A 1.372(4) . ?
C3B O1B 1.258(3) . ?
C3B O2B 1.261(3) . ?
C3B C4B 1.501(4) . ?
C2A C3A 1.389(4) . ?
C4B C5B 1.524(4) . ?
C3A C4A 1.390(3) . ?
C3A C6A 1.464(3) . ?
C5B C6B 1.524(4) . ?
C4A C5A 1.380(3) . ?
C6B C7B 1.504(4) . ?
C5A N1A 1.343(3) . ?
C7B O9B 1.250(3) . ?
C7B O8B 1.265(3) . ?
C6A N2A 1.289(3) . ?
C6A O1A 1.358(3) . ?
N2A N2A 1.411(4) 2_757 ?
O1A C6A 1.358(3) 2_757 ?
O2B Cu1 1.9708(18) 7_656 ?
O8B Cu1 1.9743(18) 6_566 ?
O9B Cu1 1.9771(18) 4_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
O2B Cu1 O1B 168.57(8) 7_656 . ?
O2B Cu1 O8B 90.96(8) 7_656 6_565 ?
O1B Cu1 O8B 87.60(8) . 6_565 ?
O2B Cu1 O9B 89.38(8) 7_656 4_646 ?
O1B Cu1 O9B 89.78(8) . 4_646 ?
O8B Cu1 O9B 168.41(7) 6_565 4_646 ?
O2B Cu1 N1A 97.11(8) 7_656 . ?
O1B Cu1 N1A 94.28(8) . . ?
O8B Cu1 N1A 101.98(8) 6_565 . ?
O9B Cu1 N1A 89.47(8) 4_646 . ?
O2B Cu1 Cu1 85.20(5) 7_656 7_656 ?
O1B Cu1 Cu1 83.41(5) . 7_656 ?
O8B Cu1 Cu1 87.57(6) 6_565 7_656 ?
O9B Cu1 Cu1 80.91(5) 4_646 7_656 ?
N1A Cu1 Cu1 170.10(6) . 7_656 ?
N1A C1A C2A 124.2(2) . . ?
O1B C3B O2B 125.0(2) . . ?
O1B C3B C4B 116.2(2) . . ?
O2B C3B C4B 118.8(2) . . ?
C1A C2A C3A 118.0(2) . . ?
C3B C4B C5B 115.8(2) . . ?
C2A C3A C4A 119.0(2) . . ?
C2A C3A C6A 120.6(2) . . ?
C4A C3A C6A 120.4(2) . . ?
C4B C5B C6B 112.3(2) . . ?
C5A C4A C3A 118.2(2) . . ?
C7B C6B C5B 112.8(2) . . ?
N1A C5A C4A 123.2(2) . . ?
O9B C7B O8B 124.8(2) . . ?
O9B C7B C6B 116.9(2) . . ?
O8B C7B C6B 118.3(2) . . ?
N2A C6A O1A 112.8(2) . . ?
N2A C6A C3A 129.1(2) . . ?
O1A C6A C3A 118.1(2) . . ?
C1A N1A C5A 117.2(2) . . ?
C1A N1A Cu1 119.36(17) . . ?
C5A N1A Cu1 122.68(17) . . ?
C6A N2A N2A 105.92(14) . 2_757 ?
C6A O1A C6A 102.5(3) . 2_757 ?
C3B O1B Cu1 124.21(17) . . ?
C3B O2B Cu1 122.17(16) . 7_656 ?
C7B O8B Cu1 119.11(17) . 6_566 ?
C7B O9B Cu1 127.02(17) . 4_656 ?

_refine_diff_density_max         0.388
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.088

_shelxl_version_number           2014-3





# start Validation Reply Form
_vrf_CHEMW03_GR-MOF-5            
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Crystal structure contains lattice water molecules at the voids 
that could not be located, so their electronic density was subtracted 
by means of SQUEEZE routine.
;
_vrf_PLAT043_GR-MOF-5            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     146.18 Check 
RESPONSE: Crystal structure contains lattice water molecules at the voids 
that could not be located, so their electronic density was subtracted 
by means of SQUEEZE routine.
;
_vrf_PLAT602_GR-MOF-5            
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: Crystal structure contains lattice water molecules at the voids 
that could not be located, so their electronic density was subtracted 
by means of SQUEEZE routine.
;
# end Validation Reply Form
_exptl_crystal_preparation       adsorption
