#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:50:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179396 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/93/4329360.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_4329360
loop_
_publ_author_name
'Jia Li'
'Jun Tao'
'Rong-Bin Huang'
'Lan-Sun Zheng'
_publ_contact_author_address
;
Department of Chemistry
Xiamen University
Xiamen 361005
P. R. China
;
_publ_contact_author_email       taojun@xmu.edu.cn
_publ_contact_author_name        'Prof. Jun Tao'
_publ_contact_author_phone       86-592-2188138
_publ_section_title
;
 Magnetic Nanosized {MII24}-Wheel-Based (M = Co, Ni) Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5988
_journal_page_last               5990
_journal_paper_doi               10.1021/ic300487a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C16 H81.3 Ni4 O23.3 S5'
_chemical_formula_weight         1001.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.907(2)
_cell_length_b                   26.907(2)
_cell_length_c                   28.712(4)
_cell_measurement_temperature    153(2)
_cell_volume                     18002(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1813
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10982
_diffrn_reflns_theta_full        62.08
_diffrn_reflns_theta_max         62.08
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    5.244
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             9276
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.0900
_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)+(0.1193P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2900
_reflns_number_gt                3051
_reflns_number_total             6195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300487a_si_002_1.cif
_cod_data_source_block           2guests
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4329360
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.04888(7) 0.42780(7) 0.20472(6) 0.0329(4) Uani 1 1 d .
Ni2 Ni 0.08808(7) 0.39119(7) 0.11680(6) 0.0308(4) Uani 1 1 d .
Ni3 Ni 0.17342(7) 0.43923(7) 0.19680(6) 0.0337(5) Uani 1 1 d .
Ni4 Ni 0.15576(7) 0.31321(7) 0.13841(6) 0.0321(5) Uani 1 1 d .
O1 O 0.1808(3) 0.2580(3) 0.1116(3) 0.0417(18) Uani 1 1 d .
O2 O 0.2679(3) 0.3220(3) 0.0818(2) 0.0375(17) Uani 1 1 d .
O3 O 0.3248(3) 0.2747(3) -0.0732(2) 0.0365(16) Uani 1 1 d .
O4 O 0.2785(3) 0.1812(3) -0.0890(3) 0.048(2) Uani 1 1 d .
C1 C 0.2218(5) 0.2744(5) 0.0793(4) 0.047(3) Uani 1 1 d .
C2 C 0.2847(4) 0.2248(4) -0.0658(3) 0.031(2) Uani 1 1 d .
C3 C 0.2088(4) 0.2345(4) 0.0430(3) 0.0226(19) Uani 1 1 d .
C4 C 0.2519(4) 0.2491(4) 0.0061(4) 0.034(2) Uani 1 1 d .
H4A H 0.2879 0.2836 0.0082 0.040 Uiso 1 1 calc R
C5 C 0.2402(4) 0.2127(4) -0.0320(4) 0.040(3) Uani 1 1 d .
C6 C 0.1867(5) 0.1621(6) -0.0356(4) 0.050(3) Uani 1 1 d .
H6A H 0.1797 0.1361 -0.0605 0.060 Uiso 1 1 calc R
C7 C 0.1419(5) 0.1492(5) -0.0012(4) 0.050(3) Uani 1 1 d .
H7A H 0.1043 0.1173 -0.0050 0.060 Uiso 1 1 calc R
C8 C 0.1561(5) 0.1853(4) 0.0371(4) 0.044(3) Uani 1 1 d .
H8A H 0.1280 0.1755 0.0607 0.053 Uiso 1 1 calc R
O5 O 0.1194(3) 0.4581(3) 0.16367(18) 0.0252(14) Uani 1 1 d .
H5 H 0.1355 0.4978 0.1509 0.030 Uiso 1 1 calc R
O6 O 0.1265(3) 0.3637(3) 0.1618(2) 0.0312(15) Uani 1 1 d .
H6 H 0.0953 0.3388 0.1841 0.037 Uiso 1 1 calc R
O1W O 0.2175(3) 0.5150(3) 0.2303(2) 0.0402(18) Uani 1 1 d .
O2W O 0.1030(4) 0.2515(3) 0.1850(3) 0.053(2) Uani 1 1 d .
S1 S 0.21934(10) 0.44400(11) 0.09577(9) 0.0327(6) Uani 1 1 d .
O7 O 0.1620(3) 0.4316(3) 0.0785(2) 0.0298(15) Uani 1 1 d .
O8 O 0.2314(3) 0.4715(3) 0.1435(3) 0.0395(17) Uani 1 1 d .
O9 O 0.2201(3) 0.3892(3) 0.0997(2) 0.0341(16) Uani 1 1 d .
O10 O 0.2645(3) 0.4823(3) 0.0635(3) 0.0468(19) Uani 1 1 d .
S2 S 0.22931(10) 0.36359(11) 0.23164(9) 0.0351(6) Uani 1 1 d .
O11 O 0.2237(3) 0.3411(3) 0.1833(3) 0.0407(18) Uani 1 1 d .
O12 O 0.2258(3) 0.4165(3) 0.2313(2) 0.0375(17) Uani 1 1 d .
O13 O 0.1810(3) 0.3184(3) 0.2599(2) 0.0408(17) Uani 1 1 d .
O14 O 0.2858(3) 0.3766(3) 0.2498(2) 0.0366(16) Uani 1 1 d .
S3 S -0.04432(13) 0.30582(13) 0.16628(13) 0.0547(8) Uani 1 1 d .
O15 O 0.0197(2) 0.3522(3) 0.16663(19) 0.0240(14) Uani 1 1 d .
C9 C -0.0688(5) 0.3136(6) 0.1096(6) 0.076(5) Uani 1 1 d .
H9A H -0.0700 0.3495 0.1086 0.115 Uiso 1 1 calc R
H9B H -0.1073 0.2811 0.1038 0.115 Uiso 1 1 calc R
H9C H -0.0424 0.3146 0.0856 0.115 Uiso 1 1 calc R
C10 C -0.0428(6) 0.2402(6) 0.1609(6) 0.079(5) Uani 1 1 d .
H10A H -0.0284 0.2328 0.1899 0.118 Uiso 1 1 calc R
H10B H -0.0176 0.2434 0.1350 0.118 Uiso 1 1 calc R
H10C H -0.0817 0.2085 0.1548 0.118 Uiso 1 1 calc R
S4 S 0.09149(14) 0.40106(14) 0.29884(12) 0.0548(8) Uani 1 1 d .
O16 O 0.1047(3) 0.4149(3) 0.2448(2) 0.0409(17) Uani 1 1 d .
C11 C 0.1571(11) 0.4216(11) 0.3218(12) 0.27(2) Uani 1 1 d .
H11A H 0.1804 0.4636 0.3216 0.410 Uiso 1 1 calc R
H11B H 0.1762 0.4055 0.3032 0.410 Uiso 1 1 calc R
H11C H 0.1527 0.4076 0.3539 0.410 Uiso 1 1 calc R
C12 C 0.0673(6) 0.3267(5) 0.3031(3) 0.050(3) Uani 1 1 d .
H12A H 0.0276 0.3048 0.2920 0.075 Uiso 1 1 calc R
H12B H 0.0691 0.3168 0.3356 0.075 Uiso 1 1 calc R
H12C H 0.0917 0.3175 0.2840 0.075 Uiso 1 1 calc R
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'
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'
Ni Ni -3.0029 0.5091 '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 Ni1 O5 165.7(3) 14_455 .
O2 Ni1 O16 89.6(3) 14_455 .
O5 Ni1 O16 77.1(3) . .
O2 Ni1 O15 90.9(3) 14_455 .
O5 Ni1 O15 84.7(2) . .
O16 Ni1 O15 94.5(3) . .
O2 Ni1 O9 84.9(3) 14_455 14_455
O5 Ni1 O9 103.2(3) . 14_455
O16 Ni1 O9 102.6(3) . 14_455
O15 Ni1 O9 162.3(3) . 14_455
O2 Ni1 O11 104.8(3) 14_455 14_455
O5 Ni1 O11 88.4(2) . 14_455
O16 Ni1 O11 165.6(3) . 14_455
O15 Ni1 O11 84.4(3) . 14_455
O9 Ni1 O11 80.1(3) 14_455 14_455
O3 Ni2 O6 101.6(3) 12 .
O3 Ni2 O7 93.7(3) 12 .
O6 Ni2 O7 90.0(3) . .
O3 Ni2 O14 87.0(3) 12 14_455
O6 Ni2 O14 167.7(3) . 14_455
O7 Ni2 O14 98.3(3) . 14_455
O3 Ni2 O5 174.4(3) 12 .
O6 Ni2 O5 80.8(2) . .
O7 Ni2 O5 91.3(2) . .
O14 Ni2 O5 89.9(3) 14_455 .
O3 Ni2 O15 93.0(3) 12 .
O6 Ni2 O15 82.2(3) . .
O7 Ni2 O15 170.6(2) . .
O14 Ni2 O15 88.6(3) 14_455 .
O5 Ni2 O15 82.4(2) . .
O5 Ni3 O1W 96.1(3) . .
O5 Ni3 O6 81.5(3) . .
O1W Ni3 O6 177.5(3) . .
O5 Ni3 O8 91.9(3) . .
O1W Ni3 O8 89.4(3) . .
O6 Ni3 O8 90.9(3) . .
O5 Ni3 O12 177.6(3) . .
O1W Ni3 O12 85.8(3) . .
O6 Ni3 O12 96.7(3) . .
O8 Ni3 O12 89.7(3) . .
O5 Ni3 O16 76.0(3) . .
O1W Ni3 O16 89.1(3) . .
O6 Ni3 O16 90.1(3) . .
O8 Ni3 O16 167.6(3) . .
O12 Ni3 O16 102.5(3) . .
O4 Ni4 O6 94.1(3) 12 .
O4 Ni4 O11 168.7(3) 12 .
O6 Ni4 O11 97.0(3) . .
O4 Ni4 O2W 91.2(4) 12 .
O6 Ni4 O2W 89.0(3) . .
O11 Ni4 O2W 90.9(3) . .
O4 Ni4 O1 82.0(3) 12 .
O6 Ni4 O1 176.0(3) . .
O11 Ni4 O1 87.0(3) . .
O2W Ni4 O1 90.2(3) . .
O4 Ni4 O9 98.4(3) 12 .
O6 Ni4 O9 86.2(3) . .
O11 Ni4 O9 80.5(3) . .
O2W Ni4 O9 169.5(3) . .
O1 Ni4 O9 95.3(3) . .
C1 O1 Ni4 122.3(7) . .
C1 O2 Ni1 127.0(7) . 15
C2 O3 Ni2 130.2(7) . 11
C2 O4 Ni4 143.3(6) . 11
O2 C1 O1 121.7(11) . .
O2 C1 C3 124.0(10) . .
O1 C1 C3 114.3(10) . .
O3 C2 O4 122.7(9) . .
O3 C2 C5 121.9(9) . .
O4 C2 C5 115.3(9) . .
C8 C3 C1 124.4(9) . .
C8 C3 C4 117.4(8) . .
C1 C3 C4 117.8(9) . .
C5 C4 C3 120.3(9) . .
C4 C5 C6 120.1(10) . .
C4 C5 C2 119.7(9) . .
C6 C5 C2 120.0(9) . .
C5 C6 C7 120.3(10) . .
C8 C7 C6 117.6(10) . .
C3 C8 C7 124.0(10) . .
Ni3 O5 Ni1 105.9(3) . .
Ni3 O5 Ni2 96.9(3) . .
Ni1 O5 Ni2 97.9(3) . .
Ni4 O6 Ni2 118.9(3) . .
Ni4 O6 Ni3 125.8(3) . .
Ni2 O6 Ni3 97.2(3) . .
O10 S1 O9 109.0(4) . .
O10 S1 O7 110.4(4) . .
O9 S1 O7 109.2(4) . .
O10 S1 O8 109.3(4) . .
O9 S1 O8 108.0(4) . .
O7 S1 O8 110.8(4) . .
S1 O7 Ni2 124.2(4) . .
S1 O8 Ni3 122.7(4) . .
S1 O9 Ni1 124.2(4) . 15
S1 O9 Ni4 124.2(4) . .
Ni1 O9 Ni4 91.8(3) 15 .
O14 S2 O12 109.2(4) . .
O14 S2 O11 108.0(4) . .
O12 S2 O11 110.0(4) . .
O14 S2 O13 112.0(4) . .
O12 S2 O13 109.9(5) . .
O11 S2 O13 107.7(4) . .
S2 O11 Ni4 128.7(5) . .
S2 O11 Ni1 124.8(4) . 15
Ni4 O11 Ni1 93.8(3) . 15
S2 O12 Ni3 132.7(4) . .
S2 O14 Ni2 127.0(4) . 15
O15 S3 C10 103.4(6) . .
O15 S3 C9 103.7(5) . .
C10 S3 C9 103.1(8) . .
S3 O15 Ni1 121.1(4) . .
S3 O15 Ni2 136.9(4) . .
Ni1 O15 Ni2 93.5(2) . .
O16 S4 C11 103.2(9) . .
O16 S4 C12 104.1(5) . .
C11 S4 C12 94.4(9) . .
S4 O16 Ni1 119.2(4) . .
S4 O16 Ni3 139.5(4) . .
Ni1 O16 Ni3 100.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 1.961(7) 14_455
Ni1 O5 2.026(6) .
Ni1 O16 2.056(7) .
Ni1 O15 2.086(6) .
Ni1 O9 2.093(6) 14_455
Ni1 O11 2.181(8) 14_455
Ni2 O3 1.993(6) 12
Ni2 O6 2.012(6) .
Ni2 O7 2.046(7) .
Ni2 O14 2.055(7) 14_455
Ni2 O5 2.060(6) .
Ni2 O15 2.145(6) .
Ni3 O5 2.004(6) .
Ni3 O1W 2.017(7) .
Ni3 O6 2.042(6) .
Ni3 O8 2.042(8) .
Ni3 O12 2.050(6) .
Ni3 O16 2.130(7) .
Ni4 O4 1.971(7) 12
Ni4 O6 1.997(7) .
Ni4 O11 2.048(7) .
Ni4 O2W 2.051(7) .
Ni4 O1 2.063(7) .
Ni4 O9 2.207(7) .
O1 C1 1.336(13) .
O2 C1 1.263(13) .
O2 Ni1 1.961(7) 15
O3 C2 1.250(12) .
O3 Ni2 1.993(6) 11
O4 C2 1.286(12) .
O4 Ni4 1.971(7) 11
C1 C3 1.408(15) .
C2 C5 1.449(14) .
C3 C8 1.384(14) .
C3 C4 1.473(13) .
C4 C5 1.394(14) .
C5 C6 1.406(15) .
C6 C7 1.458(14) .
C7 C8 1.389(15) .
S1 O10 1.464(8) .
S1 O9 1.490(7) .
S1 O7 1.491(7) .
S1 O8 1.514(7) .
O9 Ni1 2.092(6) 15
S2 O14 1.473(7) .
S2 O12 1.473(7) .
S2 O11 1.490(8) .
S2 O13 1.500(7) .
O11 Ni1 2.181(8) 15
O14 Ni2 2.055(7) 15
S3 O15 1.541(6) .
S3 C10 1.793(13) .
S3 C9 1.807(15) .
S4 O16 1.593(7) .
S4 C11 1.70(3) .
S4 C12 1.771(12) .
