#------------------------------------------------------------------------------
#$Date: 2019-11-23 00:06:13 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231620 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/61/4346109.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_4346109
loop_
_publ_author_name
'Li, Jia'
'Fu, Hong-Ru'
'Zhang, Jian'
'Zheng, Lan-Sun'
'Tao, Jun'
_publ_section_title
;
 Anionic metal-organic framework for adsorption and separation of light
 hydrocarbons.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3093
_journal_page_last               3095
_journal_paper_doi               10.1021/acs.inorgchem.5b00316
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '0.17(C204 H132 N24 Ni18 O84 S12)'
_chemical_formula_sum            'C34 H22 N4 Ni3 O14 S2'
_chemical_formula_weight         950.81
_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   26.7674(5)
_cell_length_b                   26.7674(5)
_cell_length_c                   26.7674(5)
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.8490
_cell_measurement_theta_min      3.9670
_cell_volume                     19178.7(6)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1240
_diffrn_reflns_av_unetI/netI     0.1265
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8128
_diffrn_reflns_theta_full        73.99
_diffrn_reflns_theta_max         73.99
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.017
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_platon_squeeze_details
;
;
_refine_diff_density_max         2.384
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.321
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.1055
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.2833
_reflns_number_gt                2159
_reflns_number_total             3390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00316_si_002.cif
_cod_data_source_block           p
_cod_database_code               4346109
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: S2(0.25) H9a(0.5) H9b(0.5)
3.a Riding coordinates:
 C9(H9a,H9b,H9c)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C3(H3)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z'
3 '-x, y, -z'
4 'x, -y, -z'
5 'z, x, y'
6 'z, -x, -y'
7 '-z, -x, y'
8 '-z, x, -y'
9 'y, z, x'
10 '-y, z, -x'
11 'y, -z, -x'
12 '-y, -z, x'
13 'x+1/2, y+1/2, z+1/2'
14 '-x+1/2, -y+1/2, z+1/2'
15 '-x+1/2, y+1/2, -z+1/2'
16 'x+1/2, -y+1/2, -z+1/2'
17 'z+1/2, x+1/2, y+1/2'
18 'z+1/2, -x+1/2, -y+1/2'
19 '-z+1/2, -x+1/2, y+1/2'
20 '-z+1/2, x+1/2, -y+1/2'
21 'y+1/2, z+1/2, x+1/2'
22 '-y+1/2, z+1/2, -x+1/2'
23 'y+1/2, -z+1/2, -x+1/2'
24 '-y+1/2, -z+1/2, x+1/2'
25 '-x, -y, -z'
26 'x, y, -z'
27 'x, -y, z'
28 '-x, y, z'
29 '-z, -x, -y'
30 '-z, x, y'
31 'z, x, -y'
32 'z, -x, y'
33 '-y, -z, -x'
34 'y, -z, x'
35 '-y, z, x'
36 'y, z, -x'
37 '-x+1/2, -y+1/2, -z+1/2'
38 'x+1/2, y+1/2, -z+1/2'
39 'x+1/2, -y+1/2, z+1/2'
40 '-x+1/2, y+1/2, z+1/2'
41 '-z+1/2, -x+1/2, -y+1/2'
42 '-z+1/2, x+1/2, y+1/2'
43 'z+1/2, x+1/2, -y+1/2'
44 'z+1/2, -x+1/2, y+1/2'
45 '-y+1/2, -z+1/2, -x+1/2'
46 'y+1/2, -z+1/2, x+1/2'
47 '-y+1/2, z+1/2, x+1/2'
48 '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
Ni2 Ni 0.0000 0.5000 0.15889(6) 0.0363(4) Uani 1 4 d S
Ni1 Ni 0.06659(5) 0.5000 0.05458(4) 0.0394(4) Uani 1 2 d S
S1 S 0.0000 0.41511(11) 0.0000 0.0518(7) Uani 1 4 d S
O2 O 0.05253(16) 0.44587(15) 0.16749(14) 0.0496(9) Uani 1 1 d .
O5 O 0.0447(2) 0.4479(2) 0.0000 0.0454(11) Uani 1 2 d S
O1 O 0.09691(16) 0.44640(16) 0.09493(15) 0.0525(10) Uani 1 1 d .
O6 O 0.1275(3) 0.5000 0.0000 0.0452(16) Uani 1 4 d S
C2 C 0.1124(2) 0.3840(2) 0.1554(2) 0.0522(14) Uani 1 1 d .
C1 C 0.0846(2) 0.4293(2) 0.1385(2) 0.0447(11) Uani 1 1 d .
O4 O 0.0000 0.3850(3) 0.0453(3) 0.073(2) Uani 1 2 d S
N1 N 0.1728(2) 0.2295(3) 0.2402(2) 0.0716(19) Uani 1 1 d .
O3 O 0.0000 0.5000 0.0858(3) 0.064(2) Uani 1 4 d S
C8 C 0.1896(3) 0.2540(3) 0.1998(3) 0.068(2) Uani 1 1 d .
C5 C 0.1616(3) 0.2985(3) 0.1840(3) 0.066(2) Uani 1 1 d .
C4 C 0.1767(3) 0.3238(3) 0.1406(3) 0.074(2) Uani 1 1 d .
H4 H 0.2036 0.3123 0.1219 0.088 Uiso 1 1 calc R
C6 C 0.1231(3) 0.3172(3) 0.2134(3) 0.072(2) Uani 1 1 d .
H6 H 0.1144 0.3015 0.2431 0.086 Uiso 1 1 calc R
C7 C 0.0979(3) 0.3596(3) 0.1976(3) 0.068(2) Uani 1 1 d .
H7 H 0.0710 0.3715 0.2161 0.082 Uiso 1 1 calc R
C3 C 0.1513(3) 0.3658(3) 0.1264(3) 0.070(2) Uani 1 1 d .
H3 H 0.1602 0.3822 0.0971 0.084 Uiso 1 1 calc R
S2 S 0.17029(16) 0.46812(16) 0.0000 0.0549(10) Uani 0.50 2 d SP
C9 C 0.2080(5) 0.5000 0.0511(6) 0.124(6) Uani 1 2 d S
H9A H 0.2389 0.4824 0.0559 0.186 Uiso 0.50 1 d PR
H9B H 0.2150 0.5339 0.0417 0.186 Uiso 0.50 1 d PR
H9C H 0.1891 0.5000 0.0816 0.186 Uiso 1 2 d SR
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'
Ni Ni -3.0029 0.5091 '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'
S S 0.3331 0.5567 '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
O2 Ni2 O2 167.0(2) 2_565 .
O2 Ni2 O2 167.0(2) 27_565 28
O2 Ni2 O2 91.0(3) 2_565 28
O2 Ni2 O2 87.6(3) . 28
O2 Ni2 O2 91.0(3) 27_565 .
O2 Ni2 O2 87.6(3) 27_565 2_565
O3 Ni2 O2 96.51(11) . 27_565
O3 Ni2 O2 96.51(11) . 2_565
O3 Ni2 O2 96.51(11) . 28
O3 Ni2 O2 96.51(11) . .
O5 Ni1 Ni1 45.99(10) . 26
O5 Ni1 Ni1 45.99(10) 27_565 26
O5 Ni1 O5 83.1(2) . 27_565
O5 Ni1 O6 75.16(17) . .
O5 Ni1 O6 75.16(17) 27_565 .
O1 Ni1 Ni1 123.24(12) . 26
O1 Ni1 Ni1 123.24(12) 27_565 26
O1 Ni1 O5 168.03(18) . 27_565
O1 Ni1 O5 168.03(18) 27_565 .
O1 Ni1 O5 90.74(19) . .
O1 Ni1 O5 90.74(19) 27_565 27_565
O1 Ni1 O1 93.4(3) 27_565 .
O1 Ni1 O6 93.39(15) 27_565 .
O1 Ni1 O6 93.39(15) . .
O6 Ni1 Ni1 48.13(13) . 26
O3 Ni1 Ni1 115.1(2) . 26
O3 Ni1 O5 92.5(2) . 27_565
O3 Ni1 O5 92.5(2) . .
O3 Ni1 O1 98.0(2) . 27_565
O3 Ni1 O1 98.0(2) . .
O3 Ni1 O6 163.3(3) . .
O5 S1 O5 107.5(5) 3 .
O4 S1 O5 109.1(2) 26 .
O4 S1 O5 109.1(2) . .
O4 S1 O5 109.1(2) . 3
O4 S1 O5 109.1(2) 26 3
O4 S1 O4 112.7(7) . 26
C1 O2 Ni2 131.6(4) . .
Ni1 O5 Ni1 88.0(2) . 26
S1 O5 Ni1 128.1(2) . 26
S1 O5 Ni1 128.1(2) . .
C1 O1 Ni1 130.2(4) . .
Ni1 O6 Ni1 83.7(3) 26 .
S2 O6 Ni1 126.67(10) 27_565 .
S2 O6 Ni1 126.67(10) . .
S2 O6 Ni1 126.67(10) . 26
S2 O6 Ni1 126.67(10) 27_565 26
S2 O6 S2 73.4(5) 27_565 .
C7 C2 C1 120.0(5) . .
C7 C2 C3 120.5(6) . .
C3 C2 C1 119.4(5) . .
O2 C1 O1 127.8(5) . .
O2 C1 C2 116.5(5) . .
O1 C1 C2 115.7(5) . .
C8 N1 C8 115.5(6) 5 .
Ni2 O3 Ni1 115.1(2) . .
Ni2 O3 Ni1 115.1(2) . 2_565
Ni1 O3 Ni1 129.7(4) 2_565 .
N1 C8 N1 124.5(6) 9 .
N1 C8 C5 117.2(5) . .
N1 C8 C5 118.3(5) 9 .
C4 C5 C8 118.9(6) . .
C6 C5 C8 120.4(6) . .
C6 C5 C4 120.5(5) . .
C3 C4 C5 118.9(6) . .
C7 C6 C5 118.9(6) . .
C2 C7 C6 120.5(6) . .
C4 C3 C2 120.5(6) . .
O6 S2 S2 53.3(2) . 27_565
O6 S2 C9 99.1(4) . .
O6 S2 C9 99.1(4) . 26
S2 S2 C9 63.3(2) 27_565 26
S2 S2 C9 63.3(2) 27_565 .
C9 S2 C9 91.9(10) . 26
S2 C9 S2 53.3(4) . 27_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni2 O2 2.032(4) 28
Ni2 O2 2.032(4) .
Ni2 O2 2.032(4) 2_565
Ni2 O2 2.032(4) 27_565
Ni2 O3 1.956(8) .
Ni1 Ni1 2.922(2) 26
Ni1 O5 2.103(4) 27_565
Ni1 O5 2.103(4) .
Ni1 O1 1.971(4) .
Ni1 O1 1.971(4) 27_565
Ni1 O6 2.189(5) .
Ni1 O3 1.969(4) .
S1 O5 1.484(6) 3
S1 O5 1.484(6) .
S1 O4 1.457(7) .
S1 O4 1.457(7) 26
O2 C1 1.239(7) .
O5 Ni1 2.103(4) 26
O1 C1 1.296(7) .
O6 Ni1 2.189(5) 26
O6 S2 1.428(7) 27_565
O6 S2 1.428(7) .
C2 C1 1.491(7) .
C2 C7 1.362(9) .
C2 C3 1.389(8) .
N1 C8 1.344(8) .
N1 C8 1.339(8) 5
O3 Ni1 1.969(4) 2_565
C8 N1 1.339(8) 9
C8 C5 1.469(7) .
C5 C4 1.404(9) .
C5 C6 1.390(9) .
C4 C3 1.367(9) .
C6 C7 1.388(9) .
S2 S2 1.707(9) 27_565
S2 C9 1.902(11) 26
S2 C9 1.902(11) .
C9 S2 1.902(11) 27_565
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 0.000 0.000 0.000 4998 1874 ' '
2 0.500 0.500 0.500 4998 1874 ' '
