#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/73/4107382.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_4107382
loop_
_publ_author_name
'Amy J. Cairns'
'Jason A. Perman'
'Lukasz Wojtas'
'Victor Ch. Kravtsov'
'Mohamed H. Alkordi'
'Mohamed Eddaoudi'
'Michael J. Zaworotko'
_publ_section_title
;
 Supermolecular Building Blocks (SBBs) and Crystal Design: 12-Connected
 Open Frameworks Based on a Molecular Cubohemioctahedron
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1560
_journal_page_last               1561
_journal_paper_doi               10.1021/ja078060t
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C6 H2.25 N0.75 Ni0.75 O3.9'
_chemical_formula_weight         191.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           202
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 2 2 3'
_symmetry_space_group_name_H-M   'F m -3'
_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            64
_cell_length_a                   31.3400(7)
_cell_length_b                   31.3400(7)
_cell_length_c                   31.3400(7)
_cell_measurement_temperature    100(2)
_cell_volume                     30782.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_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  0.1212
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19812
_diffrn_reflns_theta_full        19.98
_diffrn_reflns_theta_max         19.98
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.9631
_exptl_crystal_density_diffrn    0.660
_exptl_crystal_F_000             6125
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1153
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.999
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.1432
_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)+(0.1981P)²+875.6840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3462
_refine_ls_wR_factor_ref         0.3575
_reflns_number_gt                929
_reflns_number_total             1153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja078060t-file001.cif
_cod_data_source_block           squeezed
_cod_original_formula_sum        'C6 H2.25 N0.75 Ni0.75 O3.90'
_cod_database_code               4107382
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'y, z, x'
'-y, -z, x'
'y, -z, -x'
'-y, z, -x'
'z, x, y'
'-z, x, -y'
'-z, -x, y'
'z, -x, -y'
'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'
'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'
'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+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'
'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'
'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, 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'
'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'
'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, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-y, -z, -x'
'y, z, -x'
'-y, z, x'
'y, -z, x'
'-z, -x, -y'
'z, -x, y'
'z, x, -y'
'-z, x, y'
'-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'
'-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'
'-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+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'
'-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'
'-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, -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'
'-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'
'-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'
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 0.32147(13) 0.0000 0.0000 0.026(2) Uani 1 4 d S
O1 O 0.3255(9) 0.0644(8) 0.0000 0.097(9) Uani 1 2 d S
O2 O 0.3227(6) 0.0000 -0.0677(5) 0.030(5) Uani 1 2 d S
O4 O 0.2559(12) 0.0000 -0.0916(8) 0.101(10) Uani 1 2 d S
C1 C 0.3148 0.0000 -0.1414 0.001 Uiso 1 2 d SD
C2 C 0.3576 0.0000 -0.1532 0.061 Uani 1 2 d SD
H2 H 0.3792 0.0000 -0.1320 0.073 Uiso 1 2 calc SR
C3 C 0.3687 0.0000 -0.1962 0.161 Uani 1 2 d S
C4 C 0.3371 0.0000 -0.2273 0.201 Uani 1 2 d S
H4 H 0.3447 0.0000 -0.2566 0.241 Uiso 1 2 calc SR
C5 C 0.2943 0.0000 -0.2155 0.044 Uani 1 2 d SD
C6 C 0.2832 0.0000 -0.1725 0.069 Uani 1 2 d SD
H6 H 0.2540 0.0000 -0.1644 0.082 Uiso 1 2 calc SR
C8 C 0.2964(17) 0.0000 -0.0966(12) 0.16(3) Uani 1 2 d SD
C9 C 0.2857(12) 0.0849(15) 0.0000 0.19(4) Uani 1 2 d SD
O10 O 0.2550(11) 0.0000 0.0000 0.13(2) Uani 1 4 d SD
O11 O 0.3852(13) 0.0000 0.0000 0.105(14) Uani 1 4 d S
N1 N 0.2687(9) 0.0000 -0.2561(8) 0.085(10) Uani 1 2 d SD
Ni2 Ni 0.2161(18) 0.0360(17) 0.0342(17) 0.300 Uiso 0.25 1 d PD
O3 O 0.2526(9) 0.0598(7) 0.0000 0.075(8) Uani 1 2 d SD
O102 O 0.171(12) 0.032(9) 0.047(11) 0.16(11) Uiso 0.10 1 d P
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'
Ni Ni 0.3393 1.1124 '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
O11 Ni1 O1 86.4(8) . 3
O11 Ni1 O1 86.4(8) . .
O1 Ni1 O1 172.9(16) 3 .
O11 Ni1 O10 180.0 . .
O1 Ni1 O10 93.6(8) 3 .
O1 Ni1 O10 93.6(8) . .
O11 Ni1 O2 88.9(5) . 50
O1 Ni1 O2 89.93(3) 3 50
O1 Ni1 O2 89.93(3) . 50
O10 Ni1 O2 91.1(5) . 50
O11 Ni1 O2 88.9(5) . .
O1 Ni1 O2 89.93(3) 3 .
O1 Ni1 O2 89.93(3) . .
O10 Ni1 O2 91.1(5) . .
O2 Ni1 O2 177.9(10) 50 .
C9 O1 Ni1 114(2) . .
C8 O2 Ni1 137(2) . .
C2 C1 C6 120.0 . .
C2 C1 C8 128(2) . .
C6 C1 C8 112(2) . .
C1 C2 C3 120.0 . .
C2 C3 C4 120.0 . .
C2 C3 C9 125.9(17) . 30_554
C4 C3 C9 114.1(17) . 30_554
C5 C4 C3 120.0 . .
C6 C5 C4 120.0 . .
C6 C5 N1 133.2(12) . .
C4 C5 N1 106.8(12) . .
C5 C6 C1 120.0 . .
O2 C8 O4 125(3) . .
O2 C8 C1 115(4) . .
O4 C8 C1 119(4) . .
O3 C9 O1 116(4) . .
O3 C9 C3 148(4) . 94
O1 C9 C3 96(2) . 94
Ni2 O10 Ni2 66(3) 52 3
Ni2 O10 Ni2 70(4) 52 .
Ni2 O10 Ni2 104(4) 3 .
Ni2 O10 Ni2 104(4) 52 50
Ni2 O10 Ni2 70(4) 3 50
Ni2 O10 Ni2 66(3) . 50
Ni2 O10 Ni1 128(2) 52 .
Ni2 O10 Ni1 128(2) 3 .
Ni2 O10 Ni1 128(2) . .
Ni2 O10 Ni1 128(2) 50 .
N1 N1 C5 104(3) 73_554 .
O102 Ni2 O3 147(10) . .
O102 Ni2 O10 134(10) . .
O3 Ni2 O10 60.3(14) . .
O102 Ni2 Ni2 106(10) . 50
O3 Ni2 Ni2 52(2) . 50
O10 Ni2 Ni2 57.2(17) . 50
O102 Ni2 Ni2 86(10) . 52
O3 Ni2 Ni2 115.5(16) . 52
O10 Ni2 Ni2 55.2(19) . 52
Ni2 Ni2 Ni2 90.000(5) 50 52
C9 O3 Ni2 142(2) . 50
C9 O3 Ni2 142(2) . .
Ni2 O3 Ni2 76(4) 50 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O11 2.00(4) .
Ni1 O1 2.02(3) 3
Ni1 O1 2.02(3) .
Ni1 O10 2.08(3) .
Ni1 O2 2.122(16) 50
Ni1 O2 2.122(16) .
O1 C9 1.40(6) .
O2 C8 1.22(5) .
O4 C8 1.28(6) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C1 C8 1.52(3) .
C2 C3 1.3900 .
C3 C4 1.3900 .
C3 C9 1.56(4) 30_554
C4 C5 1.3900 .
C5 C6 1.3900 .
C5 N1 1.50(2) .
C9 O3 1.3001(19) .
C9 C3 1.56(4) 94
O10 Ni2 1.98(3) 52
O10 Ni2 1.98(3) 3
O10 Ni2 1.98(3) .
O10 Ni2 1.98(3) 50
N1 N1 1.23(6) 73_554
Ni2 O102 1.5(4) .
Ni2 O3 1.74(6) .
Ni2 Ni2 2.14(11) 50
Ni2 Ni2 2.26(11) 52
O3 Ni2 1.74(6) 50
