#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:22:40 +0100 (vie 25 de mar de 2016) $
#$Revision: 179813 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010921.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_7010921
loop_
_publ_author_name
'Kilkenny, Mairi L.'
'Nassimbeni, Luigi R.'
_publ_section_title
;
 Tetrakis(3-cyanopyridine)diisothiocyanatonickel(ii) and its clathrates
 with EtOH and CH2Cl2: structures, thermal stabilities and enthalpies
 of guest releaseWerner clathrates. Part 15.10 Electronic supplementary
 information (ESI) available: XRPD traces for 1â€“3 and
 for the product obtained on exposure of 1 to CH2Cl2 vapour; graphical
 representation of the Clausiusâ€“Clapeyron equation
 for the thermal decomposition of 2 and 3; rotatable 3-D crystal
 structure diagrams in CHIME format. See
 http://www.rsc.org/suppdata/dt/b1/b105299n/
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3065
_journal_paper_doi               10.1039/b105299n
_journal_year                    2001
_chemical_formula_sum            'C28 H20 Cl4 N10 Ni S2'
_chemical_formula_weight         761.16
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 97.668(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8126(7)
_cell_length_b                   11.5532(4)
_cell_length_c                   17.1122(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3490.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6867
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.017
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1544
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.0765P)²+12.2913P] where 
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                2789
_reflns_number_total             3598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105299n.txt
_cod_data_source_block           c:\dcmc2c\NidiEt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010921
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.5000 0.25691(4) 0.2500 0.01908(18) Uani 1 2 d S . .
S1 S 0.70124(5) 0.23820(9) 0.08746(6) 0.0408(3) Uani 1 1 d . . .
N1 N 0.57960(16) 0.2562(2) 0.17472(15) 0.0233(6) Uani 1 1 d . . .
N2 N 0.43974(15) 0.3854(2) 0.17924(14) 0.0233(6) Uani 1 1 d . . .
N3 N 0.43624(15) 0.1256(2) 0.18165(15) 0.0238(6) Uani 1 1 d . . .
C1 C 0.62971(18) 0.2497(3) 0.13813(18) 0.0234(7) Uani 1 1 d . . .
C4 C 0.3691(2) 0.5613(4) 0.0847(2) 0.0432(10) Uani 1 1 d . . .
H2 H 0.3459 0.6202 0.0532 0.052 Uiso 1 1 calc R . .
C2 C 0.43680(17) 0.3819(3) 0.10076(17) 0.0244(7) Uani 1 1 d . . .
H1 H 0.4592 0.3199 0.0780 0.029 Uiso 1 1 calc R . .
C10 C 0.3531(2) -0.0435(4) 0.0925(2) 0.0452(10) Uani 1 1 d . . .
H6 H 0.3254 -0.1004 0.0628 0.054 Uiso 1 1 calc R . .
C3 C 0.40153(19) 0.4675(3) 0.05190(19) 0.0303(7) Uani 1 1 d . . .
C7 C 0.3991(2) 0.4560(3) -0.0323(2) 0.0356(8) Uani 1 1 d . . .
C9 C 0.4309(2) -0.0388(3) 0.0970(2) 0.0347(8) Uani 1 1 d . . .
C6 C 0.4072(2) 0.4763(3) 0.21060(19) 0.0331(8) Uani 1 1 d . . .
H4 H 0.4085 0.4794 0.2651 0.040 Uiso 1 1 calc R . .
C8 C 0.47073(19) 0.0464(3) 0.14259(18) 0.0274(7) Uani 1 1 d . . .
H5 H 0.5233 0.0481 0.1459 0.033 Uiso 1 1 calc R . .
C12 C 0.3605(2) 0.1208(3) 0.1763(2) 0.0363(8) Uani 1 1 d . . .
H8 H 0.3358 0.1758 0.2033 0.044 Uiso 1 1 calc R . .
C13 C 0.4724(2) -0.1206(3) 0.0555(2) 0.0426(9) Uani 1 1 d . . .
C5 C 0.3721(3) 0.5650(4) 0.1660(2) 0.0499(11) Uani 1 1 d . . .
H3 H 0.3507 0.6266 0.1902 0.060 Uiso 1 1 calc R . .
C11 C 0.3174(2) 0.0382(4) 0.1329(3) 0.0493(11) Uani 1 1 d . . .
H7 H 0.2650 0.0377 0.1310 0.059 Uiso 1 1 calc R . .
N4 N 0.3958(2) 0.4462(4) -0.09915(19) 0.0524(9) Uani 1 1 d . . .
N5 N 0.5064(2) -0.1827(3) 0.0221(2) 0.0566(10) Uani 1 1 d . . .
Cl2B Cl 0.23414(17) 0.3050(3) 0.0424(2) 0.0823(12) Uani 0.423(3) 1 d PD . 2
Cl1B Cl 0.2122(2) 0.3443(4) 0.2094(3) 0.0947(14) Uani 0.423(3) 1 d PD . 2
C14B C 0.1784(6) 0.3748(11) 0.1082(3) 0.134(10) Uani 0.423(3) 1 d PD . 2
H10B H 0.1794 0.4578 0.0998 0.161 Uiso 0.423(3) 1 calc PR . 2
H9B H 0.1262 0.3492 0.0965 0.161 Uiso 0.423(3) 1 calc PR . 2
Cl1A Cl 0.0827(2) 0.3159(5) 0.2306(3) 0.155(3) Uani 0.423(3) 1 d PD . 1
Cl2A Cl 0.1812(3) 0.4398(7) 0.1443(6) 0.172(3) Uani 0.423(3) 1 d PD . 1
C14A C 0.1679(6) 0.3008(10) 0.1866(10) 0.139(9) Uani 0.423(3) 1 d PD . 1
H10A H 0.2103 0.2813 0.2260 0.167 Uiso 0.423(3) 1 calc PR . 1
H9A H 0.1623 0.2412 0.1464 0.167 Uiso 0.423(3) 1 calc PR . 1
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 Ni1 N1 179.55(14) . 2_655 ?
N1 Ni1 N2 91.25(10) . 2_655 ?
N1 Ni1 N2 89.06(10) 2_655 2_655 ?
N1 Ni1 N2 89.06(10) . . ?
N1 Ni1 N2 91.25(10) 2_655 . ?
N2 Ni1 N2 90.86(14) 2_655 . ?
N1 Ni1 N3 90.86(10) . . ?
N1 Ni1 N3 88.83(10) 2_655 . ?
N2 Ni1 N3 177.84(9) 2_655 . ?
N2 Ni1 N3 89.60(11) . . ?
N1 Ni1 N3 88.83(10) . 2_655 ?
N1 Ni1 N3 90.86(10) 2_655 2_655 ?
N2 Ni1 N3 89.60(11) 2_655 2_655 ?
N2 Ni1 N3 177.84(9) . 2_655 ?
N3 Ni1 N3 90.01(14) . 2_655 ?
C1 N1 Ni1 172.8(2) . . ?
C2 N2 C6 117.6(3) . . ?
C2 N2 Ni1 120.1(2) . . ?
C6 N2 Ni1 122.2(2) . . ?
C8 N3 C12 117.7(3) . . ?
C8 N3 Ni1 120.9(2) . . ?
C12 N3 Ni1 121.4(2) . . ?
N1 C1 S1 178.9(3) . . ?
C3 C4 C5 118.0(3) . . ?
N2 C2 C3 122.4(3) . . ?
C11 C10 C9 118.2(3) . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 C7 121.3(3) . . ?
C2 C3 C7 119.1(3) . . ?
N4 C7 C3 178.7(4) . . ?
C10 C9 C8 119.6(3) . . ?
C10 C9 C13 121.5(3) . . ?
C8 C9 C13 118.9(3) . . ?
N2 C6 C5 123.2(3) . . ?
N3 C8 C9 122.2(3) . . ?
N3 C12 C11 123.2(3) . . ?
N5 C13 C9 178.0(5) . . ?
C6 C5 C4 119.1(3) . . ?
C10 C11 C12 119.1(4) . . ?
C14B Cl2B Cl2B 161.2(5) . 7 ?
Cl1B C14B Cl2B 112.1(3) . . ?
Cl2A C14A Cl1A 104.4(5) . . ?
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 N1 2.039(3) . ?
Ni1 N1 2.039(3) 2_655 ?
Ni1 N2 2.116(3) 2_655 ?
Ni1 N2 2.116(3) . ?
Ni1 N3 2.146(3) . ?
Ni1 N3 2.146(3) 2_655 ?
S1 C1 1.640(3) . ?
N1 C1 1.159(4) . ?
N2 C2 1.338(4) . ?
N2 C6 1.345(4) . ?
N3 C8 1.331(4) . ?
N3 C12 1.341(4) . ?
C4 C3 1.382(5) . ?
C4 C5 1.386(5) . ?
C2 C3 1.390(5) . ?
C10 C11 1.374(6) . ?
C10 C9 1.380(5) . ?
C3 C7 1.442(5) . ?
C7 N4 1.143(5) . ?
C9 C8 1.390(5) . ?
C9 C13 1.444(5) . ?
C6 C5 1.376(5) . ?
C12 C11 1.378(5) . ?
C13 N5 1.140(5) . ?
Cl2B C14B 1.78999(12) . ?
Cl2B Cl2B 2.065(9) 7 ?
Cl1B C14B 1.79000(13) . ?
Cl1A C14A 1.79000(13) . ?
Cl2A C14A 1.79000(12) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 N1 C1 -61(2) 2_655 . . . ?
N2 Ni1 N1 C1 74(2) 2_655 . . . ?
N2 Ni1 N1 C1 165(2) . . . . ?
N3 Ni1 N1 C1 -106(2) . . . . ?
N3 Ni1 N1 C1 -16(2) 2_655 . . . ?
N1 Ni1 N2 C2 37.2(2) . . . . ?
N1 Ni1 N2 C2 -142.5(2) 2_655 . . . ?
N2 Ni1 N2 C2 128.4(3) 2_655 . . . ?
N3 Ni1 N2 C2 -53.7(2) . . . . ?
N3 Ni1 N2 C2 26(3) 2_655 . . . ?
N1 Ni1 N2 C6 -138.8(3) . . . . ?
N1 Ni1 N2 C6 41.5(3) 2_655 . . . ?
N2 Ni1 N2 C6 -47.5(2) 2_655 . . . ?
N3 Ni1 N2 C6 130.4(3) . . . . ?
N3 Ni1 N2 C6 -150(3) 2_655 . . . ?
N1 Ni1 N3 C8 31.1(2) . . . . ?
N1 Ni1 N3 C8 -148.6(2) 2_655 . . . ?
N2 Ni1 N3 C8 -137(3) 2_655 . . . ?
N2 Ni1 N3 C8 120.2(2) . . . . ?
N3 Ni1 N3 C8 -57.7(2) 2_655 . . . ?
N1 Ni1 N3 C12 -148.4(3) . . . . ?
N1 Ni1 N3 C12 31.9(3) 2_655 . . . ?
N2 Ni1 N3 C12 43(3) 2_655 . . . ?
N2 Ni1 N3 C12 -59.4(3) . . . . ?
N3 Ni1 N3 C12 122.8(3) 2_655 . . . ?
Ni1 N1 C1 S1 23(18) . . . . ?
C6 N2 C2 C3 -0.3(5) . . . . ?
Ni1 N2 C2 C3 -176.4(2) . . . . ?
C5 C4 C3 C2 -1.1(6) . . . . ?
C5 C4 C3 C7 178.5(4) . . . . ?
N2 C2 C3 C4 1.1(5) . . . . ?
N2 C2 C3 C7 -178.5(3) . . . . ?
C4 C3 C7 N4 -79(20) . . . . ?
C2 C3 C7 N4 100(20) . . . . ?
C11 C10 C9 C8 0.8(6) . . . . ?
C11 C10 C9 C13 -179.3(4) . . . . ?
C2 N2 C6 C5 -0.6(6) . . . . ?
Ni1 N2 C6 C5 175.5(3) . . . . ?
C12 N3 C8 C9 0.4(5) . . . . ?
Ni1 N3 C8 C9 -179.1(2) . . . . ?
C10 C9 C8 N3 -0.9(5) . . . . ?
C13 C9 C8 N3 179.1(3) . . . . ?
C8 N3 C12 C11 0.2(5) . . . . ?
Ni1 N3 C12 C11 179.8(3) . . . . ?
C10 C9 C13 N5 139(13) . . . . ?
C8 C9 C13 N5 -41(14) . . . . ?
N2 C6 C5 C4 0.5(7) . . . . ?
C3 C4 C5 C6 0.3(7) . . . . ?
C9 C10 C11 C12 -0.2(7) . . . . ?
N3 C12 C11 C10 -0.3(7) . . . . ?
Cl2B Cl2B C14B Cl1B 112.6(10) 7 . . . ?
