#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/91/4109100.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_4109100
loop_
_publ_author_name
'Shengqian Ma'
'Daofeng Sun'
'Michael Ambrogio'
'Jacqueline A. Fillinger'
'Sean Parkin'
'Hong-Cai Zhou'
_publ_section_title
;
 Framework-Catenation Isomerism in Metal-Organic Frameworks and Its Impact
 on Hydrogen Uptake
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1858
_journal_page_last               1859
_journal_paper_doi               10.1021/ja067435s
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'Cu0.50 (C27H12N7O6)1/3 (H2O)0.50'
_chemical_formula_sum            'C9 H4 Cu0.5 N2.33 O2.5'
_chemical_formula_weight         216.58
_chemical_name_common            " MOF-HTB' "
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            96
_cell_length_a                   52.993(6)
_cell_length_b                   52.993(6)
_cell_length_c                   52.993(6)
_cell_measurement_temperature    295(2)
_cell_volume                     148818(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            81536
_diffrn_reflns_theta_full        55.95
_diffrn_reflns_theta_max         55.95
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9558
_exptl_absorpt_correction_T_min  0.9558
_exptl_crystal_density_diffrn    0.232
_exptl_crystal_F_000             10448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.042
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.009
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         4665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.277
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0578P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                3145
_reflns_number_total             4665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067435ssi20061017_071513.cif
_cod_data_source_block           x05154sq
_cod_original_cell_volume        148815(30)
_cod_original_formula_sum        'C9 H4 Cu0.50 N2.33 O2.50'
_cod_database_code               4109100
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.0000 0.267747(5) 0.232253(5) 0.0879(7) Uani 1 4 d S
O1 O -0.026017(18) 0.283394(19) 0.25379(2) 0.1075(7) Uani 1 1 d .
O2 O 0.0000 0.29671(3) 0.20329(3) 0.1327(10) Uani 1 4 d S
C1 C -0.03336(4) 0.27314(3) 0.27314(3) 0.0976(8) Uani 1 2 d S
C2 C -0.05451(4) 0.28750(3) 0.28750(3) 0.1060(9) Uani 1 2 d S
C3 C -0.06415(3) 0.30905(3) 0.27820(3) 0.1250(9) Uani 1 1 d .
H3 H -0.0571 0.3159 0.2637 0.150 Uiso 1 1 calc R
C4 C -0.08421(3) 0.32147(3) 0.28947(3) 0.1294(9) Uani 1 1 d .
H4 H -0.0908 0.3361 0.2824 0.155 Uiso 1 1 calc R
C5 C -0.09426(4) 0.31163(3) 0.31163(3) 0.1180(10) Uani 1 2 d S
C6 C -0.11502(4) 0.32397(3) 0.32397(3) 0.1206(10) Uani 1 2 d S
N1 N -0.12460(3) 0.31258(2) 0.34461(3) 0.1275(8) Uani 1 1 d .
C7 C -0.14469(3) 0.32307(4) 0.35531(3) 0.1190(10) Uani 1 2 d S
N2 N -0.15522(4) 0.34478(4) 0.34478(4) 0.1101(11) Uani 1 6 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
O1 Cu1 O1 167.15(6) 100 138
O1 Cu1 O1 88.69(6) 100 .
O1 Cu1 O1 89.88(6) 138 .
O1 Cu1 O1 89.88(6) 100 43
O1 Cu1 O1 88.69(6) 138 43
O1 Cu1 O1 167.15(6) . 43
O1 Cu1 O2 96.42(3) 100 .
O1 Cu1 O2 96.42(3) 138 .
O1 Cu1 O2 96.42(3) . .
O1 Cu1 O2 96.42(3) 43 .
O1 Cu1 Cu1 83.58(3) 100 121
O1 Cu1 Cu1 83.58(3) 138 121
O1 Cu1 Cu1 83.58(3) . 121
O1 Cu1 Cu1 83.58(3) 43 121
O2 Cu1 Cu1 180.00(5) . 121
C1 O1 Cu1 121.35(12) . .
O1 C1 O1 130.0(2) . 115
O1 C1 C2 114.97(10) . .
O1 C1 C2 114.97(10) 115 .
C3 C2 C3 118.6(2) 115 .
C3 C2 C1 120.70(10) 115 .
C3 C2 C1 120.70(10) . .
C2 C3 C4 122.47(16) . .
C2 C3 H3 118.8 . .
C4 C3 H3 118.8 . .
C3 C4 C5 118.66(16) . .
C3 C4 H4 120.7 . .
C5 C4 H4 120.7 . .
C4 C5 C4 119.1(2) . 115
C4 C5 C6 120.44(10) . .
C4 C5 C6 120.44(10) 115 .
N1 C6 N1 125.8(2) 115 .
N1 C6 C5 116.97(10) 115 .
N1 C6 C5 116.97(10) . .
C7 N1 C6 117.44(15) . .
N1 C7 N1 120.62(19) 168_455 .
N1 C7 N2 119.67(10) 168_455 .
N1 C7 N2 119.67(10) . .
C7 N2 C7 119.980(10) 57_455 .
C7 N2 C7 119.980(10) 57_455 77_455
C7 N2 C7 119.979(10) . 77_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9726(10) 100
Cu1 O1 1.9726(10) 138
Cu1 O1 1.9726(10) .
Cu1 O1 1.9726(10) 43
Cu1 O2 2.171(2) .
Cu1 Cu1 2.6600(8) 121
O1 C1 1.2240(12) .
C1 O1 1.2240(12) 115
C1 C2 1.554(3) .
C2 C3 1.3447(17) 115
C2 C3 1.3447(17) .
C3 C4 1.385(2) .
C3 H3 0.9300 .
C4 C5 1.3909(17) .
C4 H4 0.9300 .
C5 C4 1.3909(17) 115
C5 C6 1.437(3) .
C6 N1 1.3486(15) 115
C6 N1 1.3486(15) .
N1 C7 1.3282(15) .
C7 N1 1.3282(15) 168_455
C7 N2 1.395(2) .
N2 C7 1.395(2) 57_455
N2 C7 1.395(2) 77_455
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Cu1 O1 C1 -85.69(15) 100 .
O1 Cu1 O1 C1 81.54(15) 138 .
O1 Cu1 O1 C1 -2.00(14) 43 .
O2 Cu1 O1 C1 178.00(14) . .
Cu1 Cu1 O1 C1 -2.00(14) 121 .
Cu1 O1 C1 O1 4.7(3) . 115
Cu1 O1 C1 C2 -178.12(12) . .
O1 C1 C2 C3 -179.9(2) . 115
O1 C1 C2 C3 -2.3(3) 115 115
O1 C1 C2 C3 2.3(3) . .
O1 C1 C2 C3 179.9(2) 115 .
C3 C2 C3 C4 -2.5(4) 115 .
C1 C2 C3 C4 175.36(18) . .
C2 C3 C4 C5 1.8(3) . .
C3 C4 C5 C4 -1.1(4) . 115
C3 C4 C5 C6 179.8(2) . .
C4 C5 C6 N1 2.5(4) . 115
C4 C5 C6 N1 -176.6(2) 115 115
C4 C5 C6 N1 176.6(2) . .
C4 C5 C6 N1 -2.5(4) 115 .
N1 C6 N1 C7 -2.7(4) 115 .
C5 C6 N1 C7 -176.2(2) . .
C6 N1 C7 N1 178.69(19) . 168_455
C6 N1 C7 N2 1.1(4) . .
N1 C7 N2 C7 -0.2(5) 168_455 57_455
N1 C7 N2 C7 177.37(17) . 57_455
N1 C7 N2 C7 -177.37(17) 168_455 77_455
N1 C7 N2 C7 0.2(5) . 77_455
