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#$Date: 2016-03-22 11:32:17 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178903 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/32/4113289.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_4113289
loop_
_publ_author_name
'Ryo Sekiya'
'Shin-ichi Nishikiori'
'Katsuyuki Ogura'
_publ_contact_author_address
;
Department of Basic Science,
Graduate School of Arts and Sciences,
The University of Tokyo,
Komaba3-8-1, Meguro, Tokyo 153-8902, Japan
;
_publ_contact_author_email       csekiya@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5454-6569
_publ_contact_author_name        'Sekiya, Ryo'
_publ_contact_author_phone       +81-3-5454-6569
_publ_section_title
;
 Crystalline Inclusion Compounds Constructed through Self-Assembly of
 Isonicotinic Acid and Thiocyanato Coordination Bridges
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16587
_journal_page_last               16600
_journal_paper_doi               10.1021/ja0463280
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C19.98 H12.12 N4.46 Ni O4.46 S2'
_chemical_formula_sum            'C19.98 H12.12 N4.46 Ni O4.46 S2'
_chemical_formula_weight         508.85
_chemical_name_systematic
;
catena-bis(N-isonicotinic acid)nickel(II)
-bis(/m-thiocyanato-N,N',S,S')(9-fluorenone oxime)0.46
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Apr 19 12:58:11 2002'
_audit_creation_method           WinGX
_cell_angle_alpha                100.924(7)
_cell_angle_beta                 52.792(10)
_cell_angle_gamma                100.947(5)
_cell_formula_units_Z            2
_cell_length_a                   7.0736(12)
_cell_length_b                   11.0952(17)
_cell_length_c                   16.481(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.79
_cell_measurement_theta_min      1.56
_cell_volume                     1006.8(3)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       RAPID-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5399
_diffrn_reflns_theta_max         29.79
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8903
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       block
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.907
_refine_diff_density_min         -0.93
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_obs          0.102
_refine_ls_shift/esd_max         0.00
_refine_ls_shift/esd_mean        0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1897P)²+3.1870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3358
_refine_ls_wR_factor_obs         0.2954
_reflns_number_observed          3464
_reflns_number_total             5399
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0463280si20040622_120150.cif
_cod_data_source_block           9-fluorenoneoxime
_cod_database_code               4113289
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C -0.2896(13) 0.2316(6) 0.0780(5) 0.0362(14) Uani 1 1 d .
C2 C 0.2653(12) 0.2758(6) -0.0401(5) 0.0325(13) Uani 1 1 d .
C11 C 0.1351(15) 0.0022(9) 0.1425(6) 0.053(2) Uani 1 1 d .
H11 H 0.2735 -0.0237 0.081 0.064 Uiso 1 1 calc R
C12 C 0.1323(16) 0.0257(10) 0.2281(6) 0.059(2) Uani 1 1 d .
H12 H 0.2645 0.0155 0.2247 0.071 Uiso 1 1 calc R
C13 C -0.0733(15) 0.0651(8) 0.3197(6) 0.0473(18) Uani 1 1 d .
C14 C -0.2659(16) 0.0754(10) 0.3224(6) 0.061(2) Uani 1 1 d .
H14 H -0.4064 0.1001 0.3834 0.073 Uiso 1 1 calc R
C15 C -0.2492(16) 0.0483(9) 0.2328(7) 0.057(2) Uani 1 1 d .
H15 H -0.3821 0.0541 0.2353 0.068 Uiso 1 1 calc R
C16 C -0.0705(17) 0.1020(8) 0.4100(6) 0.054(2) Uani 1 1 d .
C21 C -0.1616(14) 0.4344(7) 0.8638(6) 0.0456(17) Uani 1 1 d .
H21 H -0.2777 0.4851 0.9155 0.055 Uiso 1 1 calc R
C22 C -0.1825(14) 0.3783(8) 0.7881(6) 0.0473(17) Uani 1 1 d .
H22 H -0.3112 0.3892 0.7892 0.057 Uiso 1 1 calc R
C23 C -0.0081(14) 0.3047(7) 0.7096(5) 0.0434(16) Uani 1 1 d .
C24 C 0.1840(16) 0.2944(8) 0.7096(6) 0.053(2) Uani 1 1 d .
H24 H 0.3094 0.2499 0.6559 0.064 Uiso 1 1 calc R
C25 C 0.1839(16) 0.3520(8) 0.7914(6) 0.053(2) Uani 1 1 d .
H25 H 0.309 0.3421 0.7932 0.063 Uiso 1 1 calc R
C26 C -0.0271(16) 0.2407(8) 0.6267(6) 0.052(2) Uani 1 1 d .
N1 N -0.2143(11) 0.1376(5) 0.0553(5) 0.0403(13) Uani 1 1 d .
N2 N 0.1968(11) 0.3702(5) -0.0243(5) 0.0383(12) Uani 1 1 d .
N11 N -0.0493(11) 0.0142(6) 0.1426(5) 0.0429(14) Uani 1 1 d .
N21 N 0.0144(11) 0.4209(6) 0.8678(4) 0.0393(13) Uani 1 1 d .
O11 O 0.1172(12) 0.0967(7) 0.4002(5) 0.071(2) Uani 1 1 d .
O12 O -0.2603(12) 0.1350(7) 0.4931(5) 0.071(2) Uani 1 1 d .
H212 H -0.239 0.1533 0.5378 0.107 Uiso 1 1 calc R
O21 O 0.1467(13) 0.1877(7) 0.5507(5) 0.072(2) Uani 1 1 d .
H221 H 0.1156 0.156 0.5104 0.108 Uiso 1 1 calc R
O22 O -0.2188(12) 0.2425(7) 0.6379(5) 0.0682(19) Uani 1 1 d .
S1 S -0.3907(4) 0.36682(16) 0.10950(16) 0.0459(5) Uani 1 1 d .
S2 S 0.3699(4) 0.14382(16) -0.06700(18) 0.0476(5) Uani 1 1 d .
Ni1 Ni 0 0 0 0.0335(3) Uani 1 2 d S
Ni2 Ni 0 0.5 0 0.0342(3) Uani 1 2 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 C1 S1 178.7(7) . .
N2 C2 S2 177.8(7) . .
N11 C11 C12 123.8(7) . .
C11 C12 C13 118.1(7) . .
C14 C13 C12 119.3(7) . .
C14 C13 C16 122.1(7) . .
C12 C13 C16 118.5(7) . .
C13 C14 C15 119.0(8) . .
N11 C15 C14 122.8(7) . .
O11 C16 O12 123.9(7) . .
O11 C16 C13 118.5(7) . .
O12 C16 C13 117.6(8) . .
N21 C21 C22 123.8(7) . .
C21 C22 C23 118.6(7) . .
C22 C23 C24 118.5(6) . .
C22 C23 C26 120.0(7) . .
C24 C23 C26 121.4(7) . .
C25 C24 C23 118.1(7) . .
N21 C25 C24 123.4(7) . .
O21 C26 O22 124.0(7) . .
O21 C26 C23 118.3(8) . .
O22 C26 C23 117.7(7) . .
C1 N1 Ni1 165.1(6) . .
C2 N2 Ni2 161.9(6) . .
C11 N11 C15 117.0(6) . .
C11 N11 Ni1 119.1(5) . .
C15 N11 Ni1 123.4(5) . .
C21 N21 C25 117.5(6) . .
C21 N21 Ni2 118.8(5) . 1_556
C25 N21 Ni2 123.6(5) . 1_556
C1 S1 Ni2 100.1(3) . .
C2 S2 Ni1 101.0(2) . .
N1 Ni1 N1 180.0(4) 2 .
N1 Ni1 N11 89.9(2) 2 2
N1 Ni1 N11 90.1(2) . 2
N1 Ni1 N11 90.1(2) 2 .
N1 Ni1 N11 89.9(2) . .
N11 Ni1 N11 180.00(6) 2 .
N1 Ni1 S2 86.18(18) 2 .
N1 Ni1 S2 93.82(18) . .
N11 Ni1 S2 90.47(19) 2 .
N11 Ni1 S2 89.53(19) . .
N1 Ni1 S2 93.82(18) 2 2
N1 Ni1 S2 86.18(18) . 2
N11 Ni1 S2 89.53(19) 2 2
N11 Ni1 S2 90.47(19) . 2
S2 Ni1 S2 180.00(7) . 2
N2 Ni2 N2 180.0000(10) . 2_565
N2 Ni2 N21 89.7(2) . 1_554
N2 Ni2 N21 90.3(2) 2_565 1_554
N2 Ni2 N21 90.3(2) . 2_566
N2 Ni2 N21 89.7(2) 2_565 2_566
N21 Ni2 N21 180.0000(10) 1_554 2_566
N2 Ni2 S1 87.33(18) . 2_565
N2 Ni2 S1 92.67(18) 2_565 2_565
N21 Ni2 S1 90.99(18) 1_554 2_565
N21 Ni2 S1 89.01(18) 2_566 2_565
N2 Ni2 S1 92.67(18) . .
N2 Ni2 S1 87.33(18) 2_565 .
N21 Ni2 S1 89.01(18) 1_554 .
N21 Ni2 S1 90.99(18) 2_566 .
S1 Ni2 S1 180 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.155(9) .
C1 S1 1.642(7) .
C2 N2 1.156(8) .
C2 S2 1.630(6) .
C11 N11 1.336(9) .
C11 C12 1.373(10) .
C12 C13 1.387(11) .
C13 C14 1.362(11) .
C13 C16 1.478(10) .
C14 C15 1.385(11) .
C15 N11 1.342(10) .
C16 O11 1.248(10) .
C16 O12 1.259(10) .
C21 N21 1.324(9) .
C21 C22 1.364(10) .
C22 C23 1.383(10) .
C23 C24 1.386(11) .
C23 C26 1.486(10) .
C24 C25 1.378(10) .
C25 N21 1.329(9) .
C26 O21 1.249(10) .
C26 O22 1.257(11) .
N1 Ni1 2.035(6) .
N2 Ni2 2.010(6) .
N11 Ni1 2.135(6) .
N21 Ni2 2.137(5) 1_556
S1 Ni2 2.551(2) .
S2 Ni1 2.490(2) .
Ni1 N1 2.035(6) 2
Ni1 N11 2.135(6) 2
Ni1 S2 2.490(2) 2
Ni2 N2 2.010(6) 2_565
Ni2 N21 2.137(5) 1_554
Ni2 N21 2.137(5) 2_566
Ni2 S1 2.551(2) 2_565
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O12 H212 O22 0.8200 1.8300 2.615(11) 161.00 1_555 yes
O21 H221 O11 0.8200 1.8000 2.610(11) 167.00 1_555 yes
