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#$Date: 2016-03-25 12:22:40 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179813 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010920.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_7010920
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            'C30 H28 N10 Ni O2 S2'
_chemical_formula_weight         683.45
_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                 96.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.737(4)
_cell_length_b                   11.527(2)
_cell_length_c                   17.120(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3476.7(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8676
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.720
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3921
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.507
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0681P)²+7.1246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                2476
_reflns_number_total             3921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105299n.txt
_cod_data_source_block           c:\ethc2c\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               7010920
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 0.25851(5) 0.2500 0.0185(2) Uani 1 2 d S . .
S1 S 0.70182(6) 0.24167(9) 0.08414(6) 0.0338(3) Uani 1 1 d . . .
N1 N 0.58048(17) 0.2591(2) 0.17439(16) 0.0231(7) Uani 1 1 d . . .
C1 C 0.6303(2) 0.2526(3) 0.13650(19) 0.0206(7) Uani 1 1 d . . .
N3 N 0.43725(16) 0.1276(2) 0.18228(16) 0.0227(7) Uani 1 1 d . . .
N2 N 0.44013(16) 0.3880(2) 0.18016(15) 0.0213(7) Uani 1 1 d . . .
C4 C 0.3712(2) 0.5652(3) 0.0863(2) 0.0368(10) Uani 1 1 d . . .
H10 H 0.3485 0.6244 0.0550 0.044 Uiso 1 1 calc R . .
C10 C 0.3554(3) -0.0423(4) 0.0935(2) 0.0423(11) Uani 1 1 d . . .
H2 H 0.3282 -0.0990 0.0636 0.051 Uiso 1 1 calc R . .
C2 C 0.43678(19) 0.3840(3) 0.10169(19) 0.0224(8) Uani 1 1 d . . .
H3 H 0.4582 0.3208 0.0786 0.027 Uiso 1 1 calc R . .
C3 C 0.4028(2) 0.4701(3) 0.0536(2) 0.0254(8) Uani 1 1 d . . .
C7 C 0.4000(2) 0.4581(3) -0.0306(2) 0.0319(9) Uani 1 1 d . . .
C8 C 0.4724(2) 0.0459(3) 0.14449(19) 0.0252(8) Uani 1 1 d . . .
H6 H 0.5252 0.0463 0.1486 0.030 Uiso 1 1 calc R . .
C9 C 0.4333(2) -0.0391(3) 0.0996(2) 0.0304(9) Uani 1 1 d . . .
C6 C 0.4083(2) 0.4804(3) 0.2116(2) 0.0295(9) Uani 1 1 d . . .
H8 H 0.4092 0.4839 0.2660 0.035 Uiso 1 1 calc R . .
C12 C 0.3611(2) 0.1239(4) 0.1757(2) 0.0341(9) Uani 1 1 d . . .
H9 H 0.3359 0.1804 0.2014 0.041 Uiso 1 1 calc R . .
C5 C 0.3746(3) 0.5694(3) 0.1677(2) 0.0392(11) Uani 1 1 d . . .
H12 H 0.3541 0.6321 0.1922 0.047 Uiso 1 1 calc R . .
C13 C 0.4749(3) -0.1235(4) 0.0582(2) 0.0389(10) Uani 1 1 d . . .
C11 C 0.3184(3) 0.0411(4) 0.1330(3) 0.0482(12) Uani 1 1 d . . .
H15 H 0.2657 0.0412 0.1307 0.058 Uiso 1 1 calc R . .
N4 N 0.3970(2) 0.4465(3) -0.0970(2) 0.0490(10) Uani 1 1 d . . .
N5 N 0.5068(2) -0.1882(4) 0.0251(2) 0.0578(11) Uani 1 1 d . . .
O1A O 0.2013(5) 0.3606(10) 0.0932(6) 0.169(5) Uiso 0.633(10) 1 d PD . .
C14 C 0.1903(4) 0.3766(3) 0.1739(6) 0.208(4) Uiso 1 1 d D . .
C15 C 0.1883(9) 0.2515(6) 0.2034(8) 0.208(4) Uiso 1 1 d D . .
O1B O 0.1535(5) 0.4817(6) 0.1463(6) 0.073(4) Uiso 0.367(10) 1 d PD . .
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'
O O 0.0106 0.0060 '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 179.64(16) . 2_655 ?
N1 Ni1 N2 90.80(11) . 2_655 ?
N1 Ni1 N2 88.94(11) 2_655 2_655 ?
N1 Ni1 N2 88.94(11) . . ?
N1 Ni1 N2 90.80(11) 2_655 . ?
N2 Ni1 N2 90.45(15) 2_655 . ?
N1 Ni1 N3 90.96(11) . . ?
N1 Ni1 N3 89.29(11) 2_655 . ?
N2 Ni1 N3 178.22(10) 2_655 . ?
N2 Ni1 N3 89.76(11) . . ?
N1 Ni1 N3 89.29(11) . 2_655 ?
N1 Ni1 N3 90.96(11) 2_655 2_655 ?
N2 Ni1 N3 89.76(11) 2_655 2_655 ?
N2 Ni1 N3 178.22(10) . 2_655 ?
N3 Ni1 N3 90.09(16) . 2_655 ?
C1 N1 Ni1 173.5(3) . . ?
N1 C1 S1 178.8(3) . . ?
C8 N3 C12 117.2(3) . . ?
C8 N3 Ni1 121.2(2) . . ?
C12 N3 Ni1 121.6(2) . . ?
C2 N2 C6 117.2(3) . . ?
C2 N2 Ni1 120.2(2) . . ?
C6 N2 Ni1 122.5(2) . . ?
C3 C4 C5 117.5(3) . . ?
C9 C10 C11 118.3(4) . . ?
N2 C2 C3 122.6(3) . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 C7 120.8(3) . . ?
C2 C3 C7 119.3(3) . . ?
N4 C7 C3 178.5(5) . . ?
N3 C8 C9 122.4(4) . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 C13 120.5(4) . . ?
C8 C9 C13 119.7(4) . . ?
N2 C6 C5 123.4(3) . . ?
N3 C12 C11 123.7(4) . . ?
C6 C5 C4 119.4(3) . . ?
N5 C13 C9 179.0(5) . . ?
C12 C11 C10 118.5(4) . . ?
O1A C14 O1B 84.1(8) . . ?
O1A C14 C15 102.0(8) . . ?
O1B C14 C15 151.7(9) . . ?
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 2.035(3) . ?
Ni1 N1 2.035(3) 2_655 ?
Ni1 N2 2.119(3) 2_655 ?
Ni1 N2 2.119(3) . ?
Ni1 N3 2.136(3) . ?
Ni1 N3 2.136(3) 2_655 ?
S1 C1 1.641(3) . ?
N1 C1 1.158(5) . ?
N3 C8 1.337(4) . ?
N3 C12 1.342(5) . ?
N2 C2 1.339(4) . ?
N2 C6 1.347(4) . ?
C4 C3 1.380(5) . ?
C4 C5 1.390(5) . ?
C10 C9 1.375(6) . ?
C10 C11 1.383(6) . ?
C2 C3 1.382(5) . ?
C3 C7 1.442(5) . ?
C7 N4 1.139(5) . ?
C8 C9 1.381(5) . ?
C9 C13 1.454(5) . ?
C6 C5 1.367(5) . ?
C12 C11 1.375(6) . ?
C13 N5 1.129(5) . ?
O1A C14 1.4300(3) . ?
C14 O1B 1.4299(3) . ?
C14 C15 1.5300(3) . ?
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 126(2) 2_655 . . . ?
N2 Ni1 N1 C1 81(2) 2_655 . . . ?
N2 Ni1 N1 C1 171(2) . . . . ?
N3 Ni1 N1 C1 -99(2) . . . . ?
N3 Ni1 N1 C1 -9(2) 2_655 . . . ?
Ni1 N1 C1 S1 2(19) . . . . ?
N1 Ni1 N3 C8 33.3(3) . . . . ?
N1 Ni1 N3 C8 -146.9(3) 2_655 . . . ?
N2 Ni1 N3 C8 -141(3) 2_655 . . . ?
N2 Ni1 N3 C8 122.3(3) . . . . ?
N3 Ni1 N3 C8 -56.0(2) 2_655 . . . ?
N1 Ni1 N3 C12 -146.6(3) . . . . ?
N1 Ni1 N3 C12 33.2(3) 2_655 . . . ?
N2 Ni1 N3 C12 39(4) 2_655 . . . ?
N2 Ni1 N3 C12 -57.6(3) . . . . ?
N3 Ni1 N3 C12 124.1(3) 2_655 . . . ?
N1 Ni1 N2 C2 38.5(3) . . . . ?
N1 Ni1 N2 C2 -141.7(3) 2_655 . . . ?
N2 Ni1 N2 C2 129.3(3) 2_655 . . . ?
N3 Ni1 N2 C2 -52.4(3) . . . . ?
N3 Ni1 N2 C2 33(4) 2_655 . . . ?
N1 Ni1 N2 C6 -137.3(3) . . . . ?
N1 Ni1 N2 C6 42.5(3) 2_655 . . . ?
N2 Ni1 N2 C6 -46.5(2) 2_655 . . . ?
N3 Ni1 N2 C6 131.8(3) . . . . ?
N3 Ni1 N2 C6 -143(3) 2_655 . . . ?
C6 N2 C2 C3 0.3(5) . . . . ?
Ni1 N2 C2 C3 -175.7(3) . . . . ?
C5 C4 C3 C2 -0.6(6) . . . . ?
C5 C4 C3 C7 178.6(4) . . . . ?
N2 C2 C3 C4 0.5(6) . . . . ?
N2 C2 C3 C7 -178.6(3) . . . . ?
C4 C3 C7 N4 -120(19) . . . . ?
C2 C3 C7 N4 59(19) . . . . ?
C12 N3 C8 C9 0.6(5) . . . . ?
Ni1 N3 C8 C9 -179.3(3) . . . . ?
C11 C10 C9 C8 0.1(6) . . . . ?
C11 C10 C9 C13 -178.9(4) . . . . ?
N3 C8 C9 C10 -0.8(5) . . . . ?
N3 C8 C9 C13 178.2(3) . . . . ?
C2 N2 C6 C5 -1.2(6) . . . . ?
Ni1 N2 C6 C5 174.7(3) . . . . ?
C8 N3 C12 C11 0.3(6) . . . . ?
Ni1 N3 C12 C11 -179.8(3) . . . . ?
N2 C6 C5 C4 1.2(7) . . . . ?
C3 C4 C5 C6 -0.2(6) . . . . ?
C10 C9 C13 N5 75(30) . . . . ?
C8 C9 C13 N5 -104(29) . . . . ?
N3 C12 C11 C10 -1.0(7) . . . . ?
C9 C10 C11 C12 0.7(7) . . . . ?
