#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:44:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180194 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/90/7109015.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_7109015
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            'C60 H52 N6 Ni S2'
_chemical_formula_weight         979.91
_chemical_name_common            ml108
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.6737(9)
_cell_length_b                   10.2287(2)
_cell_length_c                   22.9715(4)
_cell_measurement_temperature    100(2)
_cell_volume                     10261.9(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.858
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17282
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         34.55
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9513
_exptl_absorpt_correction_T_min  0.8633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2002'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.375(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0463P)²+3.7190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                7131
_reflns_number_total             8191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40521d.txt
_cod_data_source_block           C:1tolI.CIF
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7109015
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
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 0.0000 0.0000 0.107450(13) 0.01360(6) Uani 1 2 d S . .
S1 S 0.074254(13) -0.34937(5) 0.11264(3) 0.03448(13) Uani 1 1 d . . .
N1 N 0.02785(3) -0.16165(14) 0.10861(7) 0.0185(3) Uani 1 1 d . . .
C1 C 0.04719(4) -0.23925(15) 0.11015(8) 0.0177(3) Uani 1 1 d . . .
N1A N 0.03950(3) 0.12069(13) 0.10837(7) 0.0158(3) Uani 1 1 d . . .
C1A C 0.06566(4) 0.08899(17) 0.08098(8) 0.0180(3) Uani 1 1 d . . .
H1A H 0.0662 0.0105 0.0589 0.022 Uiso 1 1 calc R . .
C2A C 0.09187(4) 0.16534(18) 0.08333(8) 0.0187(3) Uani 1 1 d . . .
H2A H 0.1098 0.1392 0.0631 0.022 Uiso 1 1 calc R . .
C3A C 0.09164(4) 0.28113(17) 0.11572(7) 0.0165(3) Uani 1 1 d . . .
C4A C 0.06446(4) 0.31387(18) 0.14438(8) 0.0197(3) Uani 1 1 d . . .
H4A H 0.0633 0.3913 0.1671 0.024 Uiso 1 1 calc R . .
C5A C 0.03930(4) 0.23221(17) 0.13927(8) 0.0187(3) Uani 1 1 d . . .
H5A H 0.0209 0.2563 0.1586 0.022 Uiso 1 1 calc R . .
C6A C 0.11909(4) 0.36563(16) 0.11943(7) 0.0182(3) Uani 1 1 d . . .
C7A C 0.12857(4) 0.41652(19) 0.17290(8) 0.0214(3) Uani 1 1 d . . .
H7A H 0.1170 0.3984 0.2070 0.026 Uiso 1 1 calc R . .
C8A C 0.15459(5) 0.4928(2) 0.17692(9) 0.0244(4) Uani 1 1 d . . .
H8A H 0.1610 0.5253 0.2137 0.029 Uiso 1 1 calc R . .
C9A C 0.17132(5) 0.5220(2) 0.12699(9) 0.0254(4) Uani 1 1 d . . .
H9A H 0.1892 0.5744 0.1297 0.030 Uiso 1 1 calc R . .
C10A C 0.16189(5) 0.4748(2) 0.07351(9) 0.0245(4) Uani 1 1 d . . .
H10A H 0.1730 0.4964 0.0393 0.029 Uiso 1 1 calc R . .
C11A C 0.13603(5) 0.39558(19) 0.06989(8) 0.0218(4) Uani 1 1 d . . .
H11A H 0.1299 0.3616 0.0332 0.026 Uiso 1 1 calc R . .
N1B N 0.0000 0.0000 0.01643(10) 0.0157(4) Uani 1 2 d S . .
C1B C -0.00083(4) -0.11231(17) -0.01405(7) 0.0180(3) Uani 1 1 d . . .
H1B H -0.0015 -0.1925 0.0068 0.022 Uiso 1 1 calc R . .
C2B C -0.00082(4) -0.11683(18) -0.07439(7) 0.0183(3) Uani 1 1 d . . .
H2B H -0.0014 -0.1984 -0.0941 0.022 Uiso 1 1 calc R . .
C3B C 0.0000 0.0000 -0.10587(11) 0.0162(5) Uani 1 2 d S . .
C4B C 0.0000 0.0000 -0.17028(12) 0.0170(5) Uani 1 2 d S . .
C5B C 0.01384(5) 0.10129(19) -0.20148(8) 0.0209(3) Uani 1 1 d . . .
H5B H 0.0231 0.1717 -0.1811 0.025 Uiso 1 1 calc R . .
C6B C 0.01419(5) 0.1001(2) -0.26209(8) 0.0255(4) Uani 1 1 d . . .
H6B H 0.0242 0.1683 -0.2827 0.031 Uiso 1 1 calc R . .
C7B C 0.0000 0.0000 -0.29258(12) 0.0249(6) Uani 1 2 d S . .
H7B H 0.0000 0.0000 -0.3339 0.030 Uiso 1 2 calc SR . .
N1C N 0.0000 0.0000 0.19968(10) 0.0163(4) Uani 1 2 d S . .
C1C C 0.02604(4) -0.01506(18) 0.23034(7) 0.0178(3) Uani 1 1 d . . .
H1C H 0.0447 -0.0269 0.2096 0.021 Uiso 1 1 calc R . .
C2C C 0.02702(4) -0.01418(17) 0.29043(8) 0.0183(3) Uani 1 1 d . . .
H2C H 0.0461 -0.0232 0.3099 0.022 Uiso 1 1 calc R . .
C3C C 0.0000 0.0000 0.32273(12) 0.0159(5) Uani 1 2 d S . .
C4C C 0.0000 0.0000 0.38690(12) 0.0198(6) Uani 1 2 d S . .
C5C C 0.02539(5) 0.0456(2) 0.41808(9) 0.0248(4) Uani 1 1 d . . .
H5C H 0.0428 0.0773 0.3976 0.030 Uiso 1 1 calc R . .
C6C C 0.02547(6) 0.0449(2) 0.47862(9) 0.0346(5) Uani 1 1 d . . .
H6C H 0.0429 0.0752 0.4994 0.042 Uiso 1 1 calc R . .
C7C C 0.0000 0.0000 0.50835(14) 0.0391(9) Uani 1 2 d S . .
H7C H 0.0000 0.0000 0.5497 0.047 Uiso 1 2 calc SR . .
C1D C 0.12353(11) 0.1212(4) 0.45137(18) 0.0419(12) Uani 0.600(8) 1 d P A 2
H1D1 H 0.1419 0.1717 0.4613 0.063 Uiso 0.600(8) 1 calc PR A 2
H1D2 H 0.1296 0.0342 0.4377 0.063 Uiso 0.600(8) 1 calc PR A 2
H1D3 H 0.1105 0.1125 0.4859 0.063 Uiso 0.600(8) 1 calc PR A 2
C2D C 0.10618(18) 0.1903(8) 0.4043(3) 0.0286(12) Uani 0.600(8) 1 d P A 2
C3D C 0.0912(2) 0.3058(9) 0.4156(4) 0.0270(14) Uani 0.600(8) 1 d P A 2
H3D H 0.0917 0.3416 0.4538 0.032 Uiso 0.600(8) 1 calc PR A 2
C4D C 0.0757(4) 0.3698(15) 0.3723(7) 0.032(2) Uani 0.600(8) 1 d P A 2
H4D H 0.0662 0.4510 0.3808 0.039 Uiso 0.600(8) 1 calc PR A 2
C5D C 0.0736(4) 0.3208(15) 0.3177(4) 0.033(2) Uani 0.600(8) 1 d P A 2
H5D H 0.0619 0.3651 0.2890 0.039 Uiso 0.600(8) 1 calc PR A 2
C6D C 0.0886(3) 0.2058(12) 0.3041(4) 0.0333(18) Uani 0.600(8) 1 d P A 2
H6D H 0.0877 0.1716 0.2657 0.040 Uiso 0.600(8) 1 calc PR A 2
C7D C 0.10539(19) 0.1393(8) 0.3479(3) 0.0273(12) Uani 0.600(8) 1 d P A 2
H7D H 0.1160 0.0608 0.3390 0.033 Uiso 0.600(8) 1 calc PR A 2
C1E C 0.09168(19) 0.3213(7) 0.4658(3) 0.046(2) Uani 0.400(8) 1 d P A 3
H1E1 H 0.0947 0.2456 0.4913 0.069 Uiso 0.400(8) 1 calc PR A 3
H1E2 H 0.0725 0.3651 0.4760 0.069 Uiso 0.400(8) 1 calc PR A 3
H1E3 H 0.1088 0.3824 0.4707 0.069 Uiso 0.400(8) 1 calc PR A 3
C2E C 0.0904(4) 0.2758(13) 0.4028(5) 0.027(2) Uani 0.400(8) 1 d P A 3
C3E C 0.0736(6) 0.349(2) 0.3596(9) 0.029(3) Uani 0.400(8) 1 d P A 3
H3E H 0.0624 0.4255 0.3701 0.035 Uiso 0.400(8) 1 calc PR A 3
C4E C 0.0743(5) 0.307(2) 0.3031(6) 0.022(2) Uani 0.400(8) 1 d P A 3
H4E H 0.0638 0.3546 0.2738 0.027 Uiso 0.400(8) 1 calc PR A 3
C5E C 0.0904(4) 0.1921(16) 0.2880(6) 0.026(2) Uani 0.400(8) 1 d P A 3
H5E H 0.0901 0.1623 0.2488 0.031 Uiso 0.400(8) 1 calc PR A 3
C6E C 0.1061(3) 0.1250(12) 0.3277(5) 0.032(2) Uani 0.400(8) 1 d P A 3
H6E H 0.1169 0.0485 0.3164 0.039 Uiso 0.400(8) 1 calc PR A 3
C7E C 0.1069(2) 0.1648(11) 0.3849(5) 0.031(2) Uani 0.400(8) 1 d P A 3
H7E H 0.1187 0.1172 0.4125 0.037 Uiso 0.400(8) 1 calc PR A 3
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 178.51(9) 2 .
N1 Ni1 N1B 90.74(4) 2 .
N1 Ni1 N1B 90.74(4) . .
N1 Ni1 N1C 89.26(4) 2 .
N1 Ni1 N1C 89.26(4) . .
N1B Ni1 N1C 180.0 . .
N1 Ni1 N1A 90.74(6) 2 .
N1 Ni1 N1A 89.24(6) . .
N1B Ni1 N1A 90.57(4) . .
N1C Ni1 N1A 89.43(4) . .
N1 Ni1 N1A 89.24(6) 2 2
N1 Ni1 N1A 90.74(6) . 2
N1B Ni1 N1A 90.57(4) . 2
N1C Ni1 N1A 89.43(4) . 2
N1A Ni1 N1A 178.86(8) . 2
C1 N1 Ni1 169.50(14) . .
N1 C1 S1 179.52(18) . .
C5A N1A C1A 117.24(15) . .
C5A N1A Ni1 119.61(12) . .
C1A N1A Ni1 123.11(11) . .
N1A C1A C2A 123.20(16) . .
C1A C2A C3A 119.44(16) . .
C2A C3A C4A 117.36(16) . .
C2A C3A C6A 121.27(16) . .
C4A C3A C6A 121.37(15) . .
C5A C4A C3A 119.27(16) . .
N1A C5A C4A 123.48(16) . .
C11A C6A C7A 118.66(16) . .
C11A C6A C3A 120.79(15) . .
C7A C6A C3A 120.55(15) . .
C8A C7A C6A 120.86(17) . .
C7A C8A C9A 119.86(18) . .
C10A C9A C8A 120.03(19) . .
C9A C10A C11A 119.87(18) . .
C6A C11A C10A 120.69(17) . .
C1B N1B C1B 117.3(2) . 2
C1B N1B Ni1 121.35(11) . .
C1B N1B Ni1 121.35(11) 2 .
N1B C1B C2B 123.26(17) . .
C1B C2B C3B 119.25(17) . .
C2B C3B C2B 117.7(2) 2 .
C2B C3B C4B 121.16(11) 2 .
C2B C3B C4B 121.16(11) . .
C5B C4B C5B 118.3(2) 2 .
C5B C4B C3B 120.85(12) 2 .
C5B C4B C3B 120.85(12) . .
C6B C5B C4B 120.7(2) . .
C7B C6B C5B 120.4(2) . .
C6B C7B C6B 119.3(3) 2 .
C1C N1C C1C 116.9(2) 2 .
C1C N1C Ni1 121.54(11) 2 .
C1C N1C Ni1 121.54(11) . .
N1C C1C C2C 123.26(18) . .
C1C C2C C3C 120.23(18) . .
C2C C3C C2C 116.1(2) . 2
C2C C3C C4C 121.96(12) . .
C2C C3C C4C 121.96(12) 2 .
C5C C4C C5C 118.5(3) 2 .
C5C C4C C3C 120.77(13) 2 .
C5C C4C C3C 120.77(14) . .
C6C C5C C4C 120.8(2) . .
C7C C6C C5C 119.5(2) . .
C6C C7C C6C 120.8(3) . 2
C3D C2D C7D 118.9(7) . .
C3D C2D C1D 120.6(6) . .
C7D C2D C1D 120.4(6) . .
C4D C3D C2D 120.5(9) . .
C5D C4D C3D 122.0(13) . .
C4D C5D C6D 119.4(12) . .
C5D C6D C7D 119.5(8) . .
C2D C7D C6D 119.5(7) . .
C7E C2E C3E 118.7(11) . .
C7E C2E C1E 120.3(12) . .
C3E C2E C1E 120.9(12) . .
C4E C3E C2E 118.3(17) . .
C3E C4E C5E 120.6(17) . .
C6E C5E C4E 121.0(11) . .
C5E C6E C7E 121.1(11) . .
C6E C7E C2E 120.2(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.0527(14) 2
Ni1 N1 2.0527(14) .
Ni1 N1B 2.091(2) .
Ni1 N1C 2.119(2) .
Ni1 N1A 2.1215(14) .
Ni1 N1A 2.1215(14) 2
S1 C1 1.6336(18) .
N1 C1 1.160(2) .
N1A C5A 1.344(2) .
N1A C1A 1.344(2) .
C1A C2A 1.387(3) .
C2A C3A 1.399(2) .
C3A C4A 1.398(2) .
C3A C6A 1.481(2) .
C4A C5A 1.385(3) .
C6A C11A 1.391(2) .
C6A C7A 1.397(2) .
C7A C8A 1.381(3) .
C8A C9A 1.392(3) .
C9A C10A 1.383(3) .
C10A C11A 1.392(3) .
N1B C1B 1.346(2) .
N1B C1B 1.346(2) 2
C1B C2B 1.387(2) .
C2B C3B 1.397(2) .
C3B C2B 1.397(2) 2
C3B C4B 1.480(4) .
C4B C5B 1.397(2) 2
C4B C5B 1.397(2) .
C5B C6B 1.393(2) .
C6B C7B 1.387(3) .
C7B C6B 1.387(3) 2
N1C C1C 1.347(2) 2
N1C C1C 1.347(2) .
C1C C2C 1.381(2) .
C2C C3C 1.402(2) .
C3C C2C 1.402(2) 2
C3C C4C 1.474(4) .
C4C C5C 1.400(2) 2
C4C C5C 1.400(2) .
C5C C6C 1.391(3) .
C6C C7C 1.384(3) .
C7C C6C 1.384(3) 2
C1D C2D 1.497(9) .
C2D C3D 1.375(10) .
C2D C7D 1.397(6) .
C3D C4D 1.371(19) .
C4D C5D 1.353(14) .
C5D C6D 1.383(18) .
C6D C7D 1.419(14) .
C1E C2E 1.521(12) .
C2E C7E 1.407(17) .
C2E C3E 1.44(3) .
C3E C4E 1.37(2) .
C4E C5E 1.41(2) .
C5E C6E 1.33(2) .
C6E C7E 1.376(10) .
