#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/51/1515146.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_1515146
loop_
_publ_author_name
'Brozek, Carl K.'
'Dincă, Mircea'
_publ_section_title
;
 Lattice-imposed geometry in metal--organic frameworks: lacunary Zn4O
 clusters in MOF-5 serve as tripodal chelating ligands for Ni2+
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2110
_journal_paper_doi               10.1039/c2sc20306e
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C6 H3 N4 Ni0.1 O3.25 Zn'
_chemical_formula_weight         247.91
_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            32
_cell_length_a                   25.8380(16)
_cell_length_b                   25.8380(16)
_cell_length_c                   25.8380(16)
_cell_measurement_reflns_used    80165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      1.37
_cell_volume                     17249.5(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0104
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            80165
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.7925
_exptl_absorpt_correction_T_min  0.7925
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3930.2
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.047
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.00006(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.571
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.571
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2759
_refine_ls_wR_factor_ref         0.3424
_reflns_number_gt                780
_reflns_number_total             991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc20306e.txt
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      f_m_-3_m
_cod_original_formula_sum        'C6 H3 N4 Ni0.10 O3.25 Zn'
_cod_database_code               1515146
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
Ni1 Ni 0.20654(2) 0.20654(2) 0.20654(2) 0.0324(7) Uani 0.09 6 d SP
Zn1 Zn 0.20654(2) 0.20654(2) 0.20654(2) 0.0324(7) Uani 0.91 6 d SP
O2 O 0.2500 0.2500 0.2500 0.038(3) Uani 1 24 d S
O1 O 0.21893(12) 0.21893(12) 0.13338(15) 0.0517(12) Uani 1 2 d S
C1 C 0.2500 0.2500 0.1108(2) 0.0454(18) Uani 1 4 d S
C2 C 0.2500 0.2500 0.0532(3) 0.050(2) Uani 1 4 d S
C3 C 0.21749(17) 0.21749(17) 0.0271(3) 0.061(2) Uani 1 2 d S
H3 H 0.1950 0.1950 0.0455 0.073 Uiso 1 2 calc SR
N4 N 0.3446(13) 0.1554(13) 0.1554(13) 0.26(2) Uani 1 6 d S
N3 N 0.0783(10) 0.2567(10) 0.0783(10) 0.42(3) Uani 1 2 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 O1 107.05(14) . 9
O1 Ni1 O1 107.05(14) . 5
O1 Ni1 O1 107.05(14) 9 5
O1 Ni1 O2 111.80(13) . .
O1 Ni1 O2 111.80(13) 9 .
O1 Ni1 O2 111.80(13) 5 .
Zn1 O2 Ni1 0.00(9) 74 74
Zn1 O2 Zn1 109.5 74 28
Ni1 O2 Zn1 109.5 74 28
Zn1 O2 Zn1 109.5 74 51
Ni1 O2 Zn1 109.5 74 51
Zn1 O2 Zn1 109.5 28 51
Zn1 O2 Ni1 109.5 74 51
Ni1 O2 Ni1 109.5 74 51
Zn1 O2 Ni1 109.5 28 51
Zn1 O2 Ni1 0.00(6) 51 51
Zn1 O2 Ni1 109.5 74 28
Ni1 O2 Ni1 109.5 74 28
Zn1 O2 Ni1 0.00(6) 28 28
Zn1 O2 Ni1 109.5 51 28
Ni1 O2 Ni1 109.5 51 28
Zn1 O2 Ni1 109.5 74 .
Ni1 O2 Ni1 109.5 74 .
Zn1 O2 Ni1 109.5 28 .
Zn1 O2 Ni1 109.5 51 .
Ni1 O2 Ni1 109.5 51 .
Ni1 O2 Ni1 109.5 28 .
C1 O1 Ni1 130.6(4) . .
O1 C1 O1 125.6(6) 74 .
O1 C1 C2 117.2(3) 74 .
O1 C1 C2 117.2(3) . .
C3 C2 C3 120.7(7) 74 .
C3 C2 C1 119.7(4) 74 .
C3 C2 C1 119.7(4) . .
C2 C3 C3 119.7(4) . 98
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 1.944(4) .
Ni1 O1 1.944(4) 9
Ni1 O1 1.944(4) 5
Ni1 O2 1.9449(10) .
O2 Zn1 1.9448(10) 74
O2 Ni1 1.9448(10) 74
O2 Zn1 1.9448(10) 28
O2 Zn1 1.9448(10) 51
O2 Ni1 1.9448(10) 51
O2 Ni1 1.9448(10) 28
O1 C1 1.276(5) .
C1 O1 1.276(5) 74
C1 C2 1.488(10) .
C2 C3 1.367(8) 74
C2 C3 1.367(8) .
C3 C3 1.398(13) 98
