#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:29:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180396 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/65/7206595.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_7206595
loop_
_publ_author_name
'Ren, Guojian'
'Liu, Shuxia'
'Ma, Fengji'
'Wei, Feng'
'Tang, Qun'
'Yang, Yuan'
'Liang, Dadong'
'Li, Shujun'
'Chen, Yaguang'
_publ_section_title
;
 A 9-connected metal--organic framework with gas adsorption properties
;
_journal_issue                   40
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              15909
_journal_paper_doi               10.1039/c1jm12834e
_journal_volume                  21
_journal_year                    2011
_chemical_formula_sum            'C30 H18 N3 Ni3 O13'
_chemical_formula_weight         804.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           217
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 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            8
_cell_length_a                   21.6623(19)
_cell_length_b                   21.6623(19)
_cell_length_c                   21.6623(19)
_cell_measurement_reflns_used    1755
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      1.33
_cell_volume                     10165.1(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1512
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31197
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_density_meas      1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.192
_platon_squeeze_details
;
;
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0235P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                1849
_reflns_number_total             2340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1jm12834e.txt
_cod_data_source_block           p1
_cod_database_code               7206595
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y, -z'
'-y, -x, z'
'-x, y, -z'
'y, x, z'
'z, x, y'
'x, -z, -y'
'-z, -x, y'
'-x, z, -y'
'z, -x, -y'
'-x, -z, y'
'-z, x, -y'
'x, z, y'
'y, z, x'
'z, y, x'
'z, -y, -x'
'-z, -y, x'
'-z, y, -x'
'y, -z, -x'
'-y, -z, x'
'-y, z, -x'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'z+1/2, x+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+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
C1 C 0.70314(13) 0.70314(13) 0.91426(18) 0.0347(9) Uani 1 2 d S
C2 C 0.67137(14) 0.74796(14) 0.94634(13) 0.0483(10) Uani 1 1 d .
H2 H 0.6397 0.7699 0.9274 0.071(10) Uiso 1 1 calc R
C3 C 0.54525(12) 0.7529(2) 0.54525(12) 0.0556(15) Uani 1 2 d S
C4 C 0.68688(12) 0.75969(15) 1.00616(13) 0.0448(8) Uani 1 1 d .
H4 H 0.6639 0.7890 1.0274 0.19(2) Uiso 1 1 calc R
C5 C 0.56149(15) 0.7566(2) 0.48403(15) 0.1017(18) Uani 1 1 d .
H5 H 0.6029 0.7591 0.4730 0.066(10) Uiso 1 1 calc R
C6 C 0.69189(12) 0.69189(12) 0.84608(17) 0.0273(9) Uani 1 2 d S
C7 C 0.59479(12) 0.7453(2) 0.59479(12) 0.0437(12) Uani 1 2 d S
N1 N 0.73226(10) 0.73226(10) 1.03583(11) 0.0293(6) Uani 1 2 d S
Ni1 Ni 0.618802(18) 0.731960(14) 0.731960(14) 0.01851(10) Uani 1 2 d S
O1 O 0.65252(8) 0.72567(10) 0.82121(8) 0.0431(5) Uani 1 1 d .
O3 O 0.57662(9) 0.74112(12) 0.64816(9) 0.0658(8) Uani 1 1 d .
O2 O 0.69929(11) 0.69929(11) 0.69929(11) 0.0255(10) 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 0.0033 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'
Ni Ni 0.3393 1.1124 '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'
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
C2 C1 C2 116.7(4) 8 .
C2 C1 C6 121.61(18) 8 .
C2 C1 C6 121.61(18) . .
C4 C2 C1 119.2(3) . .
C5 C3 C5 119.4(4) 18 .
C5 C3 C7 120.3(2) 18 .
C5 C3 C7 120.3(2) . .
N1 C4 C2 124.4(3) . .
C3 C5 C5 120.08(19) . 21_656
O1 C6 O1 128.1(3) 8 .
O1 C6 C1 115.89(17) 8 .
O1 C6 C1 115.89(17) . .
O3 C7 O3 127.0(4) 18 .
O3 C7 C3 116.47(19) 18 .
O3 C7 C3 116.47(19) . .
C4 N1 C4 115.8(3) 8 .
C4 N1 Ni1 121.71(16) 8 44_665
C4 N1 Ni1 121.71(16) . 44_665
O2 Ni1 O3 96.28(10) . .
O2 Ni1 O3 96.28(10) . 16
O3 Ni1 O3 88.42(15) . 16
O2 Ni1 O1 89.98(10) . 16
O3 Ni1 O1 90.50(9) . 16
O3 Ni1 O1 173.73(8) 16 16
O2 Ni1 O1 89.98(10) . .
O3 Ni1 O1 173.73(8) . .
O3 Ni1 O1 90.50(9) 16 .
O1 Ni1 O1 89.91(12) 16 .
O2 Ni1 N1 178.48(15) . 37_466
O3 Ni1 N1 84.81(9) . 37_466
O3 Ni1 N1 84.81(9) 16 37_466
O1 Ni1 N1 88.95(7) 16 37_466
O1 Ni1 N1 88.95(7) . 37_466
O2 Ni1 Ni1 30.44(2) . 17
O3 Ni1 Ni1 71.81(6) . 17
O3 Ni1 Ni1 112.65(7) 16 17
O1 Ni1 Ni1 72.79(5) 16 17
O1 Ni1 Ni1 114.25(5) . 17
N1 Ni1 Ni1 149.772(9) 37_466 17
O2 Ni1 Ni1 30.44(2) . 8
O3 Ni1 Ni1 112.65(7) . 8
O3 Ni1 Ni1 71.81(6) 16 8
O1 Ni1 Ni1 114.25(5) 16 8
O1 Ni1 Ni1 72.79(5) . 8
N1 Ni1 Ni1 149.772(9) 37_466 8
Ni1 Ni1 Ni1 60.0 17 8
C6 O1 Ni1 133.1(2) . .
C7 O3 Ni1 134.6(2) . .
Ni1 O2 Ni1 119.12(4) 17 .
Ni1 O2 Ni1 119.12(4) 17 8
Ni1 O2 Ni1 119.12(4) . 8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.378(3) 8
C1 C2 1.378(3) .
C1 C6 1.516(5) .
C2 C4 1.362(4) .
C3 C5 1.374(4) 18
C3 C5 1.374(4) .
C3 C7 1.527(5) .
C4 N1 1.316(3) .
C5 C5 1.395(6) 21_656
C6 O1 1.246(2) 8
C6 O1 1.246(2) .
C7 O3 1.225(2) 18
C7 O3 1.225(2) .
N1 C4 1.316(3) 8
N1 Ni1 2.105(3) 44_665
Ni1 O2 2.0104(6) .
Ni1 O3 2.0419(18) .
Ni1 O3 2.0419(18) 16
Ni1 O1 2.0712(17) 16
Ni1 O1 2.0712(17) .
Ni1 N1 2.105(3) 37_466
Ni1 Ni1 3.4666(8) 17
Ni1 Ni1 3.4666(8) 8
O2 Ni1 2.0104(6) 17
O2 Ni1 2.0104(6) 8
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 -0.102 -0.043 -0.030 5271 1625 ' '
