#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/90/7109016.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_7109016
loop_
_publ_author_name
'Matteo Lusi'
'Leonard J. Barbour'
_publ_section_title
;
 Solid-vapour reactions as a post-synthetic modification tool for
 molecular crystals: the enclathration of benzene and toluene by Werner
 complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              2634
_journal_paper_doi               10.1039/c3cc40521d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C30 H26 N3 Ni0.5 S'
_chemical_formula_weight         489.95
_chemical_name_common            work
_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                 99.406(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.620(6)
_cell_length_b                   23.084(12)
_cell_length_c                   22.693(12)
_cell_measurement_temperature    293(2)
_cell_volume                     5488(5)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour,2001;Atwood&Barbour,2003)'
_computing_publication_material  'X-Seed (Barbour,2001;Atwood&Barbour,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11777
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.9632
_exptl_absorpt_correction_T_min  0.9456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2002'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1734P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2769
_reflns_number_gt                2447
_reflns_number_total             3936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40521d.txt
_cod_data_source_block           C:\1tolII.CIF
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C30 H26 N3 Ni0.50 S'
_cod_database_code               7109016
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 0.20891(4) 0.2500 0.0540(4) Uani 1 2 d S . .
S1 S 0.1038(2) 0.22520(12) 0.11770(11) 0.1217(10) Uani 1 1 d . . .
N1 N 0.3156(5) 0.21119(19) 0.2045(2) 0.0597(12) Uani 1 1 d . . .
C1 C 0.2271(6) 0.2164(2) 0.1694(3) 0.0611(15) Uani 1 1 d . . .
N1A N 0.5713(5) 0.2029(2) 0.1666(2) 0.0598(13) Uani 1 1 d . . .
C2A C 0.6869(6) 0.2167(3) 0.1599(3) 0.077(2) Uani 1 1 d . . .
H2A H 0.7395 0.2344 0.1915 0.092 Uiso 1 1 calc R . .
C3A C 0.7349(7) 0.2061(3) 0.1082(3) 0.082(2) Uani 1 1 d . . .
H3A H 0.8172 0.2184 0.1057 0.098 Uiso 1 1 calc R . .
C4A C 0.6674(6) 0.1786(3) 0.0611(3) 0.0636(16) Uani 1 1 d . . .
C5A C 0.5477(7) 0.1616(4) 0.0693(3) 0.099(3) Uani 1 1 d . . .
H5A H 0.4957 0.1416 0.0391 0.119 Uiso 1 1 calc R . .
C6A C 0.5029(7) 0.1739(4) 0.1226(3) 0.094(2) Uani 1 1 d . . .
H6A H 0.4220 0.1611 0.1271 0.113 Uiso 1 1 calc R . .
C7A C 0.7159(6) 0.1645(3) 0.0047(3) 0.0640(16) Uani 1 1 d . . .
C8A C 0.6345(7) 0.1565(3) -0.0471(3) 0.083(2) Uani 1 1 d . . .
H8A H 0.5479 0.1628 -0.0473 0.100 Uiso 1 1 calc R . .
C9A C 0.6731(8) 0.1397(4) -0.0990(3) 0.106(3) Uani 1 1 d . . .
H9A H 0.6133 0.1324 -0.1329 0.128 Uiso 1 1 calc R . .
C10A C 0.7985(9) 0.1338(4) -0.1006(4) 0.104(3) Uani 1 1 d . . .
H10A H 0.8264 0.1236 -0.1359 0.124 Uiso 1 1 calc R . .
C11A C 0.8825(9) 0.1427(5) -0.0508(4) 0.132(4) Uani 1 1 d . . .
H11A H 0.9692 0.1380 -0.0517 0.158 Uiso 1 1 calc R . .
C12A C 0.8423(8) 0.1589(4) 0.0025(3) 0.105(3) Uani 1 1 d . . .
H12A H 0.9022 0.1659 0.0364 0.126 Uiso 1 1 calc R . .
N1B N 0.5000 0.3012(3) 0.2500 0.0582(17) Uani 1 2 d S . .
C2B C 0.4524(6) 0.3323(3) 0.2013(3) 0.0651(16) Uani 1 1 d . . .
H2B H 0.4170 0.3125 0.1669 0.078 Uiso 1 1 calc R . .
C3B C 0.4532(6) 0.3913(3) 0.1996(3) 0.0695(17) Uani 1 1 d . . .
H3B H 0.4219 0.4104 0.1642 0.083 Uiso 1 1 calc R . .
C4B C 0.5000 0.4228(4) 0.2500 0.062(2) Uani 1 2 d S . .
C5B C 0.5000 0.4884(5) 0.2500 0.089(3) Uani 1 2 d S . .
C6B C 0.4961(12) 0.5189(4) 0.1974(5) 0.148(4) Uani 1 1 d . . .
H6B H 0.4923 0.4991 0.1614 0.177 Uiso 1 1 calc R . .
C7B C 0.4978(13) 0.5785(5) 0.1981(7) 0.164(5) Uani 1 1 d . . .
H7B H 0.4973 0.5987 0.1626 0.197 Uiso 1 1 calc R . .
C8B C 0.5000 0.6080(7) 0.2500 0.161(8) Uani 1 2 d S . .
H8B H 0.5000 0.6483 0.2500 0.193 Uiso 1 2 calc SR . .
N1C N 0.5000 0.1173(3) 0.2500 0.0619(18) Uani 1 2 d S . .
C2C C 0.3930(6) 0.0862(3) 0.2439(3) 0.0719(18) Uani 1 1 d . . .
H2C H 0.3160 0.1061 0.2402 0.086 Uiso 1 1 calc R . .
C3C C 0.3881(6) 0.0268(3) 0.2428(3) 0.0709(17) Uani 1 1 d . . .
H3C H 0.3095 0.0081 0.2371 0.085 Uiso 1 1 calc R . .
C4C C 0.5000 -0.0056(3) 0.2500 0.060(2) Uani 1 2 d S . .
C5C C 0.5000 -0.0694(3) 0.2500 0.057(2) Uani 1 2 d S . .
C6C C 0.6026(6) -0.1001(3) 0.2374(3) 0.0684(17) Uani 1 1 d . . .
H6C H 0.6733 -0.0799 0.2288 0.082 Uiso 1 1 calc R . .
C7C C 0.6048(8) -0.1599(3) 0.2369(3) 0.080(2) Uani 1 1 d . . .
H7C H 0.6755 -0.1797 0.2278 0.096 Uiso 1 1 calc R . .
C8C C 0.5000 -0.1897(4) 0.2500 0.083(3) Uani 1 2 d S . .
H8C H 0.5000 -0.2300 0.2500 0.099 Uiso 1 2 calc SR . .
C1E C 0.210(2) 0.0533(12) 0.0097(10) 0.162(12) Uiso 0.436(19) 1 d PG A 2
C2E C 0.236(2) 0.1057(9) -0.0160(10) 0.137(9) Uiso 0.436(19) 1 d PG A 2
H2E H 0.2110 0.1403 -0.0006 0.165 Uiso 0.436(19) 1 calc PR A 2
C3E C 0.301(2) 0.1063(9) -0.0647(10) 0.154(17) Uiso 0.436(19) 1 d PG A 2
H3E H 0.3183 0.1414 -0.0818 0.185 Uiso 0.436(19) 1 calc PR A 2
C4E C 0.339(2) 0.0546(11) -0.0876(9) 0.149(11) Uiso 0.436(19) 1 d PG A 2
H4E H 0.3818 0.0550 -0.1202 0.178 Uiso 0.436(19) 1 calc PR A 2
C5E C 0.313(3) 0.0022(9) -0.0620(12) 0.33(4) Uiso 0.436(19) 1 d PG A 2
H5E H 0.3380 -0.0325 -0.0774 0.391 Uiso 0.436(19) 1 calc PR A 2
C6E C 0.248(3) 0.0016(9) -0.0133(13) 0.192(15) Uiso 0.436(19) 1 d PG A 2
H6E H 0.2307 -0.0335 0.0039 0.230 Uiso 0.436(19) 1 calc PR A 2
C7E C 0.138(5) 0.0462(18) 0.0721(19) 0.25(2) Uiso 0.436(19) 1 d P A 2
H7E1 H 0.2007 0.0524 0.1073 0.377 Uiso 0.436(19) 1 calc PR A 2
H7E2 H 0.1033 0.0080 0.0731 0.377 Uiso 0.436(19) 1 calc PR A 2
H7E3 H 0.0715 0.0744 0.0707 0.377 Uiso 0.436(19) 1 calc PR A 2
C1D C 0.241(2) 0.0562(9) 0.0380(7) 0.212(13) Uiso 0.564(19) 1 d PG A 1
H1D H 0.2197 0.0439 0.0741 0.254 Uiso 0.564(19) 1 calc PR A 1
C2D C 0.2191(15) 0.1133(8) 0.0196(7) 0.138(8) Uiso 0.564(19) 1 d PG A 1
H2D H 0.1832 0.1392 0.0435 0.166 Uiso 0.564(19) 1 calc PR A 1
C3D C 0.2509(18) 0.1317(7) -0.0344(8) 0.157(9) Uiso 0.564(19) 1 d PG A 1
H3D H 0.2363 0.1699 -0.0466 0.188 Uiso 0.564(19) 1 calc PR A 1
C4D C 0.3046(18) 0.0929(10) -0.0701(6) 0.147(12) Uiso 0.564(19) 1 d PG A 1
H4D H 0.3259 0.1052 -0.1062 0.176 Uiso 0.564(19) 1 calc PR A 1
C5D C 0.3265(18) 0.0358(9) -0.0518(8) 0.158(9) Uiso 0.564(19) 1 d PG A 1
C6D C 0.295(2) 0.0175(7) 0.0023(10) 0.26(2) Uiso 0.564(19) 1 d PG A 1
H6D H 0.3094 -0.0207 0.0145 0.313 Uiso 0.564(19) 1 calc PR A 1
C7D C 0.375(3) -0.0015(15) -0.0923(16) 0.250(16) Uiso 0.564(19) 1 d P A 1
H7D1 H 0.3502 0.0127 -0.1323 0.375 Uiso 0.564(19) 1 calc PR A 1
H7D2 H 0.3410 -0.0397 -0.0893 0.375 Uiso 0.564(19) 1 calc PR A 1
H7D3 H 0.4663 -0.0028 -0.0828 0.375 Uiso 0.564(19) 1 calc PR A 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'
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 Ni1 N1 177.1(3) . 2_655
N1 Ni1 N1C 91.47(13) . .
N1 Ni1 N1C 91.47(13) 2_655 .
N1 Ni1 N1B 88.53(13) . .
N1 Ni1 N1B 88.53(13) 2_655 .
N1C Ni1 N1B 180.000(1) . .
N1 Ni1 N1A 90.02(19) . 2_655
N1 Ni1 N1A 90.17(19) 2_655 2_655
N1C Ni1 N1A 86.34(12) . 2_655
N1B Ni1 N1A 93.66(12) . 2_655
N1 Ni1 N1A 90.17(19) . .
N1 Ni1 N1A 90.02(19) 2_655 .
N1C Ni1 N1A 86.34(12) . .
N1B Ni1 N1A 93.66(12) . .
N1A Ni1 N1A 172.7(2) 2_655 .
C1 N1 Ni1 164.9(5) . .
N1 C1 S1 177.8(6) . .
C2A N1A C6A 116.7(5) . .
C2A N1A Ni1 124.1(4) . .
C6A N1A Ni1 118.0(4) . .
N1A C2A C3A 123.0(6) . .
C4A C3A C2A 122.5(6) . .
C3A C4A C5A 114.3(6) . .
C3A C4A C7A 124.8(6) . .
C5A C4A C7A 120.8(6) . .
C4A C5A C6A 120.9(6) . .
N1A C6A C5A 122.3(6) . .
C8A C7A C12A 116.7(6) . .
C8A C7A C4A 120.9(6) . .
C12A C7A C4A 122.4(6) . .
C7A C8A C9A 123.3(7) . .
C10A C9A C8A 119.3(7) . .
C11A C10A C9A 119.3(7) . .
C10A C11A C12A 121.0(8) . .
C7A C12A C11A 120.1(7) . .
C2B N1B C2B 115.4(7) . 2_655
C2B N1B Ni1 122.3(4) . .
C2B N1B Ni1 122.3(4) 2_655 .
N1B C2B C3B 123.6(6) . .
C2B C3B C4B 120.5(6) . .
C3B C4B C3B 116.3(8) . 2_655
C3B C4B C5B 121.9(4) . .
C3B C4B C5B 121.9(4) 2_655 .
C6B C5B C6B 118.8(12) . 2_655
C6B C5B C4B 120.6(6) . .
C6B C5B C4B 120.6(6) 2_655 .
C7B C6B C5B 120.1(11) . .
C8B C7B C6B 120.7(14) . .
C7B C8B C7B 119.7(16) . 2_655
C2C N1C C2C 114.8(7) 2_655 .
C2C N1C Ni1 122.6(4) 2_655 .
C2C N1C Ni1 122.6(4) . .
N1C C2C C3C 124.7(6) . .
C2C C3C C4C 120.4(6) . .
C3C C4C C3C 114.9(8) 2_655 .
C3C C4C C5C 122.6(4) 2_655 .
C3C C4C C5C 122.6(4) . .
C6C C5C C6C 117.7(8) 2_655 .
C6C C5C C4C 121.1(4) 2_655 .
C6C C5C C4C 121.1(4) . .
C5C C6C C7C 122.3(7) . .
C6C C7C C8C 118.8(7) . .
C7C C8C C7C 120.2(9) . 2_655
C2E C1E C6E 120.0 . .
C2E C1E C7E 125(2) . .
C6E C1E C7E 115(2) . .
C3E C2E C1E 120.0 . .
C2E C3E C4E 120.0 . .
C5E C4E C3E 120.0 . .
C4E C5E C6E 120.0 . .
C5E C6E C1E 120.0 . .
C2D C1D C6D 120.0 . .
C3D C2D C1D 120.0 . .
C4D C3D C2D 120.0 . .
C3D C4D C5D 120.0 . .
C6D C5D C4D 120.0 . .
C6D C5D C7D 124(2) . .
C4D C5D C7D 116(2) . .
C5D C6D C1D 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.060(5) .
Ni1 N1 2.060(5) 2_655
Ni1 N1C 2.116(7) .
Ni1 N1B 2.130(6) .
Ni1 N1A 2.155(5) 2_655
Ni1 N1A 2.155(5) .
S1 C1 1.623(7) .
N1 C1 1.134(8) .
N1A C2A 1.300(8) .
N1A C6A 1.319(8) .
C2A C3A 1.376(9) .
C3A C4A 1.345(8) .
C4A C5A 1.372(9) .
C4A C7A 1.490(8) .
C5A C6A 1.397(9) .
C7A C8A 1.353(9) .
C7A C12A 1.357(10) .
C8A C9A 1.366(9) .
C9A C10A 1.345(11) .
C10A C11A 1.335(12) .
C11A C12A 1.399(11) .
N1B C2B 1.346(7) .
N1B C2B 1.346(7) 2_655
C2B C3B 1.361(9) .
C3B C4B 1.377(8) .
C4B C3B 1.377(8) 2_655
C4B C5B 1.515(13) .
C5B C6B 1.380(10) .
C5B C6B 1.380(10) 2_655
C6B C7B 1.376(14) .
C7B C8B 1.358(13) .
C8B C7B 1.358(13) 2_655
N1C C2C 1.333(7) 2_655
N1C C2C 1.333(7) .
C2C C3C 1.372(8) .
C3C C4C 1.391(7) .
C4C C3C 1.391(7) 2_655
C4C C5C 1.472(11) .
C5C C6C 1.369(7) 2_655
C5C C6C 1.369(7) .
C6C C7C 1.381(9) .
C7C C8C 1.383(8) .
C8C C7C 1.383(8) 2_655
C1E C2E 1.3900 .
C1E C6E 1.3900 .
C1E C7E 1.72(5) .
C2E C3E 1.3900 .
C3E C4E 1.3900 .
C4E C5E 1.3900 .
C5E C6E 1.3900 .
C1D C2D 1.3900 .
C1D C6D 1.3900 .
C2D C3D 1.3900 .
C3D C4D 1.3900 .
C4D C5D 1.3900 .
C5D C6D 1.3900 .
C5D C7D 1.42(4) .
