#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:57:53 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179997 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/91/7029147.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_7029147
loop_
_publ_author_name
'Almáši, Miroslav'
'Zeleňák, Vladimír'
'Opanasenko, Maksym'
'Cejka, Jíří'
_publ_section_title
;
 A novel nickel metal-organic framework with fluorite-like structure: gas
 adsorption properties and catalytic activity in Knoevenagel condensation.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3730
_journal_page_last               3738
_journal_paper_doi               10.1039/c3dt52698d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C29 H16 Ni2 O12, 2(O)'
_chemical_formula_sum            'C29 H16 Ni2 O14'
_chemical_formula_weight         705.80
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n 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            4
_cell_length_a                   14.9927(17)
_cell_length_b                   17.2321(16)
_cell_length_c                   24.798(3)
_cell_measurement_reflns_used    2525
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.1328
_cell_measurement_theta_min      3.0462
_cell_volume                     6406.7(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Diamond (Crystal Impact, 2009)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '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  0.0837
_diffrn_reflns_av_sigmaI/netI    0.1523
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17541
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.5523
_exptl_crystal_size_mid          0.1435
_exptl_crystal_size_min          0.1245
_platon_squeeze_details
;
;
_refine_diff_density_max         1.297
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         6782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0863
_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)+(0.1350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2356
_refine_ls_wR_factor_ref         0.2556
_reflns_number_gt                3242
_reflns_number_total             6782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52698d.txt
_cod_data_source_block           shelxl
_cod_database_code               7029147
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x-1/2, y-1/2, z-1/2'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.30544(6) 0.21086(5) 0.0000 0.0297(3) Uani 1 2 d S
Ni2 Ni 0.39507(7) 0.02422(6) 0.0000 0.0387(3) Uani 1 2 d S
O7 O 0.1916(4) 0.2826(3) 0.0000 0.0526(15) Uani 1 2 d S
O5 O 0.3571(3) 0.2833(2) 0.05826(15) 0.0466(10) Uani 1 1 d .
O1 O 0.4207(3) 0.1406(3) 0.0000 0.0330(11) Uani 1 2 d S
C6 C 0.0000 0.0000 0.2459(3) 0.0308(16) Uani 1 2 d S
O3 O 0.3092(3) 0.0327(2) 0.06131(17) 0.0546(11) Uani 1 1 d .
O4 O 0.2465(3) 0.1485(2) 0.05876(17) 0.0617(12) Uani 1 1 d .
C5 C 0.0756(3) 0.0231(3) 0.20663(18) 0.0277(11) Uani 1 1 d .
C13 C 0.4761(3) 0.4332(3) 0.21496(18) 0.0306(11) Uani 1 1 d .
O2 O 0.5000 0.0000 0.0562(2) 0.0527(15) Uani 1 2 d S
C2 C 0.1932(4) 0.0622(3) 0.1229(2) 0.0410(13) Uani 1 1 d .
C4 C 0.1487(4) -0.0227(3) 0.1956(2) 0.0407(13) Uani 1 1 d .
H4 H 0.1592 -0.0666 0.2165 0.049 Uiso 1 1 calc R
C8 C 0.1235(4) 0.1087(3) 0.1350(2) 0.0435(14) Uani 1 1 d .
H8 H 0.1157 0.1548 0.1161 0.052 Uiso 1 1 calc R
C3 C 0.2069(4) -0.0047(3) 0.1539(2) 0.0466(15) Uani 1 1 d .
H3 H 0.2550 -0.0370 0.1466 0.056 Uiso 1 1 calc R
C7 C 0.0633(4) 0.0888(3) 0.1750(2) 0.0394(13) Uani 1 1 d .
H7 H 0.0137 0.1201 0.1809 0.047 Uiso 1 1 calc R
O6 O 0.4726(4) 0.2116(3) 0.0841(2) 0.095(2) Uani 1 1 d .
C12 C 0.3981(4) 0.4401(3) 0.1837(2) 0.0451(14) Uani 1 1 d .
H12 H 0.3579 0.4801 0.1904 0.054 Uiso 1 1 calc R
C11 C 0.3814(4) 0.3868(3) 0.1428(2) 0.0503(16) Uani 1 1 d .
H11 H 0.3301 0.3914 0.1219 0.060 Uiso 1 1 calc R
C1 C 0.2561(4) 0.0832(3) 0.0775(2) 0.0391(13) Uani 1 1 d .
C10 C 0.4406(4) 0.3272(3) 0.1330(2) 0.0449(14) Uani 1 1 d .
C14 C 0.5318(4) 0.3724(3) 0.2052(2) 0.0476(15) Uani 1 1 d .
H14 H 0.5826 0.3660 0.2263 0.057 Uiso 1 1 calc R
C15 C 0.5138(4) 0.3206(4) 0.1648(2) 0.0505(16) Uani 1 1 d .
H15 H 0.5530 0.2796 0.1590 0.061 Uiso 1 1 calc R
C9 C 0.4199(5) 0.2706(4) 0.0877(3) 0.0577(17) Uani 1 1 d .
O8 O 0.3743(4) -0.0956(3) 0.0000 0.071(2) Uani 1 2 d S
O1W O 0.5602(5) 0.1010(4) 0.1322(3) 0.151(3) 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'
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
O4 Ni1 O4 92.6(3) 6 .
O4 Ni1 O5 174.41(16) 6 .
O4 Ni1 O5 88.91(18) . .
O4 Ni1 O5 88.91(18) 6 6
O4 Ni1 O5 174.41(16) . 6
O5 Ni1 O5 89.1(2) . 6
O4 Ni1 O7 87.60(16) 6 .
O4 Ni1 O7 87.60(16) . .
O5 Ni1 O7 87.09(15) . .
O5 Ni1 O7 87.09(15) 6 .
O4 Ni1 O1 93.02(15) 6 .
O4 Ni1 O1 93.02(15) . .
O5 Ni1 O1 92.26(14) . .
O5 Ni1 O1 92.26(14) 6 .
O7 Ni1 O1 179.1(2) . .
O3 Ni2 O3 99.1(2) 6 .
O3 Ni2 O1 92.82(15) 6 .
O3 Ni2 O1 92.82(15) . .
O3 Ni2 O8 88.67(16) 6 .
O3 Ni2 O8 88.67(16) . .
O1 Ni2 O8 177.7(2) . .
O3 Ni2 O2 169.27(15) 6 .
O3 Ni2 O2 89.54(17) . .
O1 Ni2 O2 93.04(11) . .
O8 Ni2 O2 85.23(13) . .
O3 Ni2 O2 89.54(17) 6 5_655
O3 Ni2 O2 169.27(15) . 5_655
O1 Ni2 O2 93.04(11) . 5_655
O8 Ni2 O2 85.23(13) . 5_655
O2 Ni2 O2 81.2(2) . 5_655
C9 O5 Ni1 127.2(4) . .
Ni2 O1 Ni1 114.2(2) . .
C13 C6 C13 102.4(5) 3_455 4_545
C13 C6 C5 114.6(2) 3_455 2
C13 C6 C5 111.9(2) 4_545 2
C13 C6 C5 111.9(2) 3_455 .
C13 C6 C5 114.6(2) 4_545 .
C5 C6 C5 101.9(5) 2 .
C1 O3 Ni2 135.1(4) . .
C1 O4 Ni1 135.5(4) . .
C4 C5 C7 117.3(5) . .
C4 C5 C6 124.2(4) . .
C7 C5 C6 117.9(4) . .
C14 C13 C12 118.5(5) . .
C14 C13 C6 122.8(4) . 3
C12 C13 C6 118.3(4) . 3
Ni2 O2 Ni2 98.8(2) . 5_655
C8 C2 C3 118.7(5) . .
C8 C2 C1 120.3(5) . .
C3 C2 C1 121.0(5) . .
C5 C4 C3 121.4(5) . .
C5 C4 H4 119.3 . .
C3 C4 H4 119.3 . .
C2 C8 C7 121.0(5) . .
C2 C8 H8 119.5 . .
C7 C8 H8 119.5 . .
C4 C3 C2 120.1(5) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C8 C7 C5 121.4(5) . .
C8 C7 H7 119.3 . .
C5 C7 H7 119.3 . .
C11 C12 C13 119.7(5) . .
C11 C12 H12 120.2 . .
C13 C12 H12 120.2 . .
C10 C11 C12 120.3(5) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
O4 C1 O3 126.4(5) . .
O4 C1 C2 115.4(5) . .
O3 C1 C2 118.1(5) . .
C15 C10 C11 118.7(5) . .
C15 C10 C9 122.8(5) . .
C11 C10 C9 118.4(5) . .
C13 C14 C15 120.7(5) . .
C13 C14 H14 119.6 . .
C15 C14 H14 119.6 . .
C10 C15 C14 122.1(6) . .
C10 C15 H15 119.0 . .
C14 C15 H15 119.0 . .
O5 C9 O6 125.2(6) . .
O5 C9 C10 119.2(5) . .
O6 C9 C10 115.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O4 2.015(4) 6
Ni1 O4 2.015(4) .
Ni1 O5 2.060(4) .
Ni1 O5 2.060(4) 6
Ni1 O7 2.108(6) .
Ni1 O1 2.110(5) .
Ni2 O3 1.997(4) 6
Ni2 O3 1.997(4) .
Ni2 O1 2.042(5) .
Ni2 O8 2.088(6) .
Ni2 O2 2.143(4) .
Ni2 O2 2.143(4) 5_655
O5 C9 1.211(7) .
C6 C13 1.548(6) 3_455
C6 C13 1.548(6) 4_545
C6 C5 1.546(6) 2
C6 C5 1.546(6) .
O3 C1 1.246(6) .
O4 C1 1.225(6) .
C5 C4 1.378(7) .
C5 C7 1.391(7) .
C13 C14 1.361(7) .
C13 C12 1.409(7) .
C13 C6 1.548(6) 3
O2 Ni2 2.143(4) 5_655
C2 C8 1.352(7) .
C2 C3 1.400(8) .
C2 C1 1.513(7) .
C4 C3 1.387(7) .
C4 H4 0.9300 .
C8 C7 1.384(7) .
C8 H8 0.9300 .
C3 H3 0.9300 .
C7 H7 0.9300 .
O6 C9 1.290(7) .
C12 C11 1.391(8) .
C12 H12 0.9300 .
C11 C10 1.381(8) .
C11 H11 0.9300 .
C10 C15 1.357(8) .
C10 C9 1.520(8) .
C14 C15 1.368(7) .
C14 H14 0.9300 .
C15 H15 0.9300 .
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
O4 Ni1 O5 C9 76.9(5) . .
O5 Ni1 O5 C9 -108.3(5) 6 .
O7 Ni1 O5 C9 164.6(5) . .
O1 Ni1 O5 C9 -16.1(5) . .
O3 Ni2 O1 Ni1 49.66(12) 6 .
O3 Ni2 O1 Ni1 -49.66(12) . .
O2 Ni2 O1 Ni1 -139.34(11) . .
O2 Ni2 O1 Ni1 139.34(11) 5_655 .
O4 Ni1 O1 Ni2 -46.40(13) 6 .
O4 Ni1 O1 Ni2 46.40(13) . .
O5 Ni1 O1 Ni2 135.43(12) . .
O5 Ni1 O1 Ni2 -135.43(12) 6 .
O3 Ni2 O3 C1 -61.6(6) 6 .
O1 Ni2 O3 C1 31.7(6) . .
O8 Ni2 O3 C1 -150.1(6) . .
O2 Ni2 O3 C1 124.7(5) . .
O2 Ni2 O3 C1 154.7(6) 5_655 .
O4 Ni1 O4 C1 73.6(6) 6 .
O5 Ni1 O4 C1 -111.8(6) . .
O7 Ni1 O4 C1 161.1(6) . .
O1 Ni1 O4 C1 -19.6(6) . .
C13 C6 C5 C4 133.1(4) 3_455 .
C13 C6 C5 C4 17.1(6) 4_545 .
C5 C6 C5 C4 -103.9(5) 2 .
C13 C6 C5 C7 -56.0(5) 3_455 .
C13 C6 C5 C7 -172.0(4) 4_545 .
C5 C6 C5 C7 66.9(4) 2 .
O3 Ni2 O2 Ni2 30.4(8) 6 5_655
O3 Ni2 O2 Ni2 174.60(13) . 5_655
O1 Ni2 O2 Ni2 -92.61(9) . 5_655
O8 Ni2 O2 Ni2 85.90(11) . 5_655
O2 Ni2 O2 Ni2 0.0 5_655 5_655
C7 C5 C4 C3 -1.1(8) . .
C6 C5 C4 C3 169.7(5) . .
C3 C2 C8 C7 -3.7(9) . .
C1 C2 C8 C7 177.4(5) . .
C5 C4 C3 C2 1.5(9) . .
C8 C2 C3 C4 0.9(9) . .
C1 C2 C3 C4 179.7(5) . .
C2 C8 C7 C5 4.2(9) . .
C4 C5 C7 C8 -1.7(8) . .
C6 C5 C7 C8 -173.2(5) . .
C14 C13 C12 C11 -2.2(8) . .
C6 C13 C12 C11 170.8(5) 3 .
C13 C12 C11 C10 0.4(9) . .
Ni1 O4 C1 O3 -3.0(10) . .
Ni1 O4 C1 C2 -179.9(4) . .
Ni2 O3 C1 O4 -4.5(10) . .
Ni2 O3 C1 C2 172.3(4) . .
C8 C2 C1 O4 10.0(8) . .
C3 C2 C1 O4 -168.8(6) . .
C8 C2 C1 O3 -167.2(5) . .
C3 C2 C1 O3 14.0(8) . .
C12 C11 C10 C15 1.6(9) . .
C12 C11 C10 C9 -179.7(6) . .
C12 C13 C14 C15 2.1(8) . .
C6 C13 C14 C15 -170.6(5) 3 .
C11 C10 C15 C14 -1.8(10) . .
C9 C10 C15 C14 179.6(6) . .
C13 C14 C15 C10 -0.1(9) . .
Ni1 O5 C9 O6 7.7(10) . .
Ni1 O5 C9 C10 -172.3(4) . .
C15 C10 C9 O5 -174.4(6) . .
C11 C10 C9 O5 7.0(9) . .
C15 C10 C9 O6 5.6(10) . .
C11 C10 C9 O6 -173.0(6) . .
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 -0.013 0.002 -0.006 4085 991 ' '
