#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011998.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_7011998
loop_
_publ_author_name
'Vujovic, Dejana'
'Raubenheimer, Helgard G.'
'Nassimbeni, Luigi R.'
_publ_section_title
;
 New self-assembled one-dimensional nickel coordination polymers and
 hydrogen-bonded networks
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              631
_journal_paper_doi               10.1039/b206638f
_journal_year                    2003
_chemical_formula_moiety         Ni(NCS)2(C7H6N2)2.(C7H6N2)
_chemical_formula_sum            'C23 H18 N8 Ni S2'
_chemical_formula_weight         529.28
_chemical_melting_point          'DSC onset temperature = 230.7oC'
_chemical_name_common            none
_chemical_name_systematic
; 
catena-(bis(?2-4-aminobenzonitrile-N,N)-bis(thiocyanato-N)) nickel(II) 
4-aminobenzonitrile clathrate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 95.9030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.37110(10)
_cell_length_b                   13.2066(2)
_cell_length_c                   19.5217(3)
_cell_measurement_reflns_used    5476
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.32
_cell_volume                     2403.20(6)
_computing_cell_refinement       'Collect (Nonius, 2000)'
_computing_data_collection       'Collect (Nonius, 2000)'
_computing_data_reduction        'Collect (Nonius, 2000)'
_computing_molecular_graphics
'XSEED a graphical interface to SHELXL (1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'combination of phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5476
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rectangular plates'
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.305
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0283P)²+1.0889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                4387
_reflns_number_total             5476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206638f.txt
_cod_data_source_block           COMPOUND_4
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011998
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.65129(2) 0.455589(15) 0.177213(11) 0.01906(7) Uani 1 1 d . . .
S3C S 0.36097(5) 0.29407(4) -0.00072(2) 0.03602(13) Uani 1 1 d . . .
S3D S 0.93890(5) 0.61613(3) 0.35694(2) 0.03134(12) Uani 1 1 d . . .
N7G N 1.1727(2) 0.52709(16) 0.50643(10) 0.0394(4) Uani 1 1 d . . .
N7A N 0.76181(14) 0.31590(11) 0.20944(9) 0.0219(3) Uani 1 1 d . . .
N9A N 0.47332(14) 0.39353(11) 0.21765(7) 0.0240(3) Uani 1 1 d . . .
N7B N 0.54084(14) 0.59647(11) 0.14684(9) 0.0219(3) Uani 1 1 d . . .
N9B N 0.82930(15) 0.51484(11) 0.13608(8) 0.0268(3) Uani 1 1 d . . .
N1C N 0.57470(16) 0.38853(11) 0.08761(8) 0.0266(3) Uani 1 1 d . . .
N1D N 0.72544(16) 0.52342(11) 0.26739(8) 0.0284(3) Uani 1 1 d . . .
N9G N 1.67531(19) 0.27500(13) 0.35123(8) 0.0392(4) Uani 1 1 d . . .
C1A C -0.08612(16) 0.31688(12) 0.21501(9) 0.0195(3) Uani 1 1 d . . .
C2A C -0.01346(17) 0.29068(13) 0.15882(9) 0.0231(4) Uani 1 1 d . . .
H2A H -0.0637 0.2638 0.1194 0.028 Uiso 1 1 calc R . .
C3A C 0.13337(17) 0.30458(13) 0.16147(9) 0.0236(4) Uani 1 1 d . . .
H3A H 0.1820 0.2878 0.1238 0.028 Uiso 1 1 calc R . .
C4A C 0.20784(16) 0.34405(12) 0.22112(9) 0.0206(3) Uani 1 1 d . . .
C5A C 0.13663(17) 0.36613(12) 0.27875(9) 0.0220(4) Uani 1 1 d . . .
H5A H 0.1875 0.3901 0.3189 0.026 Uiso 1 1 calc R . .
C6A C -0.00993(17) 0.35201(12) 0.27561(9) 0.0209(3) Uani 1 1 d . . .
H6A H -0.0580 0.3659 0.3139 0.025 Uiso 1 1 calc R . .
C8A C 0.35706(17) 0.36907(12) 0.22082(9) 0.0221(4) Uani 1 1 d . . .
C1B C 1.38846(16) 0.59267(12) 0.14094(9) 0.0196(3) Uani 1 1 d . . .
C2B C 1.31374(17) 0.55950(12) 0.07964(9) 0.0226(4) Uani 1 1 d . . .
H2B H 1.3621 0.5479 0.0411 0.027 Uiso 1 1 calc R . .
C3B C 1.16751(17) 0.54399(13) 0.07648(9) 0.0241(4) Uani 1 1 d . . .
H3B H 1.1175 0.5199 0.0361 0.029 Uiso 1 1 calc R . .
C4B C 1.09475(17) 0.56445(12) 0.13364(9) 0.0225(4) Uani 1 1 d . . .
C5B C 1.16836(18) 0.60140(13) 0.19414(9) 0.0244(4) Uani 1 1 d . . .
H5B H 1.1192 0.6170 0.2318 0.029 Uiso 1 1 calc R . .
C6B C 1.31542(18) 0.61457(12) 0.19764(9) 0.0232(4) Uani 1 1 d . . .
H6B H 1.3656 0.6382 0.2381 0.028 Uiso 1 1 calc R . .
C8B C 0.94520(18) 0.53939(12) 0.13341(9) 0.0239(4) Uani 1 1 d . . .
C2C C 0.48617(19) 0.34748(13) 0.05164(9) 0.0248(4) Uani 1 1 d . . .
C2D C 0.81390(19) 0.56192(12) 0.30461(9) 0.0239(4) Uani 1 1 d . . .
C1G C 1.27024(19) 0.47612(14) 0.47315(9) 0.0288(4) Uani 1 1 d . . .
C2G C 1.3558(2) 0.52622(14) 0.42909(10) 0.0326(4) Uani 1 1 d . . .
H2G H 1.3426 0.5952 0.4210 0.039 Uiso 1 1 calc R . .
C3G C 1.4589(2) 0.47530(15) 0.39760(10) 0.0321(4) Uani 1 1 d . . .
H3G H 1.5157 0.5101 0.3691 0.038 Uiso 1 1 calc R . .
C4G C 1.4787(2) 0.37098(14) 0.40820(9) 0.0300(4) Uani 1 1 d . . .
C5G C 1.3909(2) 0.32042(14) 0.45050(10) 0.0354(5) Uani 1 1 d . . .
H5G H 1.4023 0.2511 0.4574 0.042 Uiso 1 1 calc R . .
C6G C 1.2881(2) 0.37099(14) 0.48212(10) 0.0351(4) Uani 1 1 d . . .
H6G H 1.2299 0.3357 0.5096 0.042 Uiso 1 1 calc R . .
C8G C 1.5882(2) 0.31805(15) 0.37651(10) 0.0319(4) Uani 1 1 d . . .
H7A1 H 0.725(2) 0.2711(15) 0.1788(10) 0.028(5) Uiso 1 1 d . . .
H7A2 H 0.7320(19) 0.3034(14) 0.2483(10) 0.022(5) Uiso 1 1 d . . .
H7B1 H 0.575(2) 0.6389(15) 0.1784(10) 0.027(5) Uiso 1 1 d . . .
H7B2 H 0.572(2) 0.6145(15) 0.1082(11) 0.031(6) Uiso 1 1 d . . .
H7G1 H 1.162(3) 0.588(2) 0.4990(12) 0.054(8) Uiso 1 1 d . . .
H7G2 H 1.130(3) 0.497(2) 0.5368(14) 0.055(8) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
N1C Ni1 N1D 179.23(6) . . ?
N1C Ni1 N9B 93.34(6) . . ?
N1D Ni1 N9B 87.26(6) . . ?
N1C Ni1 N9A 85.92(6) . . ?
N1D Ni1 N9A 93.49(6) . . ?
N9B Ni1 N9A 178.93(6) . . ?
N1C Ni1 N7A 89.70(6) . . ?
N1D Ni1 N7A 90.75(6) . . ?
N9B Ni1 N7A 93.09(6) . . ?
N9A Ni1 N7A 86.15(5) . . ?
N1C Ni1 N7B 91.26(6) . . ?
N1D Ni1 N7B 88.28(6) . . ?
N9B Ni1 N7B 87.20(6) . . ?
N9A Ni1 N7B 93.58(5) . . ?
N7A Ni1 N7B 178.97(7) . . ?
C1A N7A Ni1 117.32(10) 1_655 . ?
C8A N9A Ni1 159.18(14) . . ?
C1B N7B Ni1 115.88(10) 1_455 . ?
C8B N9B Ni1 158.70(15) . . ?
C2C N1C Ni1 153.11(14) . . ?
C2D N1D Ni1 153.22(15) . . ?
C2A C1A C6A 120.06(14) . . ?
C2A C1A N7A 120.41(15) . 1_455 ?
C6A C1A N7A 119.35(15) . 1_455 ?
C3A C2A C1A 120.16(15) . . ?
C2A C3A C4A 119.39(16) . . ?
C3A C4A C5A 120.72(15) . . ?
C3A C4A C8A 119.06(15) . . ?
C5A C4A C8A 120.06(15) . . ?
C6A C5A C4A 119.44(15) . . ?
C5A C6A C1A 120.12(16) . . ?
N9A C8A C4A 175.77(18) . . ?
C6B C1B C2B 120.27(15) . . ?
C6B C1B N7B 120.06(15) . 1_655 ?
C2B C1B N7B 119.50(15) . 1_655 ?
C3B C2B C1B 119.58(16) . . ?
C2B C3B C4B 120.06(16) . . ?
C3B C4B C5B 120.44(15) . . ?
C3B C4B C8B 120.64(16) . . ?
C5B C4B C8B 118.69(16) . . ?
C6B C5B C4B 119.31(16) . . ?
C5B C6B C1B 120.26(16) . . ?
N9B C8B C4B 175.72(18) . . ?
N1C C2C S3C 177.66(16) . . ?
N1D C2D S3D 179.9(2) . . ?
N7G C1G C2G 121.15(18) . . ?
N7G C1G C6G 120.56(19) . . ?
C2G C1G C6G 118.29(18) . . ?
C3G C2G C1G 121.13(17) . . ?
C2G C3G C4G 120.26(18) . . ?
C5G C4G C3G 118.69(18) . . ?
C5G C4G C8G 120.94(17) . . ?
C3G C4G C8G 120.36(18) . . ?
C6G C5G C4G 121.23(18) . . ?
C5G C6G C1G 120.33(18) . . ?
N9G C8G C4G 179.5(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1C 2.0252(15) . ?
Ni1 N1D 2.0329(15) . ?
Ni1 N9B 2.0773(14) . ?
Ni1 N9A 2.0849(14) . ?
Ni1 N7A 2.1766(14) . ?
Ni1 N7B 2.1814(14) . ?
S3C C2C 1.6347(18) . ?
S3D C2D 1.6377(18) . ?
N7G C1G 1.354(3) . ?
N7A C1A 1.418(2) 1_655 ?
N9A C8A 1.144(2) . ?
N7B C1B 1.422(2) 1_455 ?
N9B C8B 1.140(2) . ?
N1C C2C 1.164(2) . ?
N1D C2D 1.162(2) . ?
N9G C8G 1.148(2) . ?
C1A C2A 1.393(2) . ?
C1A C6A 1.397(2) . ?
C1A N7A 1.418(2) 1_455 ?
C2A C3A 1.384(2) . ?
C3A C4A 1.396(2) . ?
C4A C5A 1.397(2) . ?
C4A C8A 1.437(2) . ?
C5A C6A 1.381(2) . ?
C1B C6B 1.390(2) . ?
C1B C2B 1.394(2) . ?
C1B N7B 1.422(2) 1_655 ?
C2B C3B 1.381(2) . ?
C3B C4B 1.393(3) . ?
C4B C5B 1.393(2) . ?
C4B C8B 1.440(2) . ?
C5B C6B 1.384(2) . ?
C1G C2G 1.401(3) . ?
C1G C6G 1.407(3) . ?
C2G C3G 1.373(3) . ?
C3G C4G 1.403(3) . ?
C4G C5G 1.395(3) . ?
C4G C8G 1.433(3) . ?
C5G C6G 1.370(3) . ?
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
N7A H7A2 N9G 0.85(2) 2.16(2) 3.012(2) 174.8(16) 1_455
N7B H7B2 S3C 0.87(2) 2.56(2) 3.4078(17) 167.1(18) 3_665
N7G H7G1 S3C 0.83(3) 2.73(3) 3.541(2) 169(2) 2_655
N7G H7G2 S3D 0.85(3) 2.69(3) 3.516(2) 166(2) 3_766
