#------------------------------------------------------------------------------
#$Date: 2019-11-24 08:25:00 +0100 (dom 24 de nov de 2019) $
#$Revision: 237454 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/71/7237150.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7237150
loop_
_publ_author_name
'Cepeda, Javier'
'Pérez-Mendoza, Manuel'
'Calahorro, Antonio J.'
'Casati, Nicola'
'Seco, José Manuel'
'Aragones-Anglada, Marta'
'Moghadam, Peyman Z.'
'Fairen-Jimenez, David'
'Rodríguez-Diéguez, Antonio'
_publ_section_title
;
 Modulation of pore shape and adsorption selectivity by ligand
 functionalization in a series of “rob”-like flexible
 metal--organic frameworks
;
_journal_issue                   36
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              17409
_journal_paper_doi               10.1039/C8TA04316G
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C10 H10 Cu N2 O4, 2(H2 O)'
_chemical_formula_sum            'C10 H14 Cu N2 O6'
_chemical_formula_weight         321.77
_chemical_name_systematic
'poly{[(mu-azopyridine)-kN,N')bis(mu4-glutarato-kO:kO':kO'':kO''')dicopper(II)] tetrahydrate}'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-04-10 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.537(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.153(2)
_cell_length_b                   13.120(1)
_cell_length_c                   8.600(1)
_cell_measurement_reflns_used    43628
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.34
_cell_volume                     2722.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_number            43628
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.036
_diffrn_reflns_theta_min         1.688
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   numerical
_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_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1320
_exptl_crystal_preparation       'adsorption properties'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_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
;
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0369
_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)+(0.0452P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2446
_reflns_number_total             3080
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ta04316g2.cif
_cod_data_source_block           GR-MOF-2
_cod_original_cell_volume        2722.4(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7237150
_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.
;
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
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'
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
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 . .
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'
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
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
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_
_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 ' '
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
