#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:17:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180472 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/41/7214109.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_7214109
loop_
_publ_author_name
'Lusi, Matteo'
'Barbour, Leonard J.'
_publ_section_title
;
 Temperature-dependent guest reorientation: a reversible order--disorder
 transformation in a single crystal
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              36
_journal_paper_doi               10.1039/c3ce41572d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C61.99 H55.99 N6 Ni S2'
_chemical_formula_weight         1007.82
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.649(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6221(7)
_cell_length_b                   23.1917(16)
_cell_length_c                   23.0275(15)
_cell_measurement_temperature    313(2)
_cell_volume                     5592.4(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      313(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.913
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27880
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.462
_diffrn_reflns_theta_min         1.756
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.9771
_exptl_absorpt_correction_T_min  0.8731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            lilac
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0755P)²+3.4730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3831
_reflns_number_total             7766
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3ce41572d.txt
_cod_data_source_block           C:1_313d3
_cod_database_code               7214109
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.29386(2) 0.2500 0.05366(18) Uani 1 2 d S T P . .
S1 S 0.90789(10) 0.28006(6) 0.37384(5) 0.1100(4) Uani 1 1 d . . . . .
N1 N 0.6857(2) 0.29095(10) 0.29412(10) 0.0606(6) Uani 1 1 d . . . . .
C1 C 0.7773(3) 0.28703(11) 0.32666(12) 0.0545(6) Uani 1 1 d . . . . .
N1A N 0.4323(2) 0.29925(10) 0.33313(10) 0.0588(6) Uani 1 1 d . . . . .
C1A C 0.3163(3) 0.28437(15) 0.34101(14) 0.0747(9) Uani 1 1 d . . . . .
H1A H 0.2642 0.2657 0.3102 0.090 Uiso 1 1 calc R U . . .
C2A C 0.2675(3) 0.29466(16) 0.39146(14) 0.0801(10) Uani 1 1 d . . . . .
H2A H 0.1850 0.2827 0.3939 0.096 Uiso 1 1 calc R U . . .
C3A C 0.3387(3) 0.32226(13) 0.43845(12) 0.0609(7) Uani 1 1 d . . . . .
C4A C 0.4592(3) 0.33897(17) 0.42974(14) 0.0808(10) Uani 1 1 d . . . . .
H4A H 0.5121 0.3587 0.4595 0.097 Uiso 1 1 calc R U . . .
C5A C 0.5017(3) 0.32702(16) 0.37834(14) 0.0797(10) Uani 1 1 d . . . . .
H5A H 0.5836 0.3389 0.3746 0.096 Uiso 1 1 calc R U . . .
C6A C 0.2920(3) 0.33619(14) 0.49415(13) 0.0662(8) Uani 1 1 d . . . . .
C7A C 0.3758(3) 0.34170(17) 0.54653(14) 0.0834(10) Uani 1 1 d . . . . .
H7A H 0.4623 0.3349 0.5470 0.100 Uiso 1 1 calc R U . . .
C8A C 0.3350(4) 0.3569(2) 0.59786(15) 0.1020(13) Uani 1 1 d . . . . .
H8A H 0.3941 0.3608 0.6323 0.122 Uiso 1 1 calc R U . . .
C9A C 0.2107(4) 0.3661(2) 0.59877(18) 0.1085(14) Uani 1 1 d . . . . .
H9A H 0.1829 0.3764 0.6336 0.130 Uiso 1 1 calc R U . . .
C10A C 0.1265(4) 0.3602(3) 0.54808(19) 0.133(2) Uani 1 1 d . . . . .
H10A H 0.0401 0.3664 0.5484 0.160 Uiso 1 1 calc R U . . .
C11A C 0.1658(3) 0.3452(2) 0.49615(17) 0.1096(15) Uani 1 1 d . . . . .
H11A H 0.1057 0.3412 0.4620 0.131 Uiso 1 1 calc R U . . .
N1B N 0.5000 0.38542(14) 0.2500 0.0585(8) Uani 1 2 d S T P . .
C1B C 0.6079(3) 0.41612(14) 0.25769(15) 0.0698(8) Uani 1 1 d . . . . .
H1B H 0.6851 0.3963 0.2628 0.084 Uiso 1 1 calc R U . . .
C2B C 0.6111(3) 0.47492(14) 0.25840(15) 0.0711(8) Uani 1 1 d . . . . .
H2B H 0.6895 0.4937 0.2647 0.085 Uiso 1 1 calc R U . . .
C3B C 0.5000 0.50718(17) 0.2500 0.0552(9) Uani 1 2 d S T P . .
C4B C 0.5000 0.57047(17) 0.2500 0.0546(9) Uani 1 2 d S T P . .
C5B C 0.3948(3) 0.60158(14) 0.26125(13) 0.0667(8) Uani 1 1 d . . . . .
H5B H 0.3229 0.5819 0.2687 0.080 Uiso 1 1 calc R U . . .
C6B C 0.3951(4) 0.66128(15) 0.26150(15) 0.0790(9) Uani 1 1 d . . . . .
H6B H 0.3242 0.6814 0.2695 0.095 Uiso 1 1 calc R U . . .
C7B C 0.5000 0.6905(2) 0.2500 0.0799(14) Uani 1 2 d S T P . .
H7B H 0.5000 0.7306 0.2500 0.096 Uiso 1 2 calc R U P . .
N1C N 0.5000 0.20250(14) 0.2500 0.0574(8) Uani 1 2 d S T P . .
C1C C 0.5442(3) 0.17161(13) 0.29815(13) 0.0657(8) Uani 1 1 d . . . . .
H1C H 0.5759 0.1915 0.3326 0.079 Uiso 1 1 calc R U . . .
C2C C 0.5457(3) 0.11261(14) 0.29991(14) 0.0684(8) Uani 1 1 d . . . . .
H2C H 0.5776 0.0938 0.3350 0.082 Uiso 1 1 calc R U . . .
C3C C 0.5000 0.08068(18) 0.2500 0.0617(10) Uani 1 2 d S T P . .
C4C C 0.5000 0.0166(2) 0.2500 0.0808(14) Uani 1 2 d S T P . .
C5C C 0.4854(6) -0.0144(2) 0.2000(3) 0.145(2) Uani 1 1 d . . . . .
H5C H 0.4752 0.0049 0.1641 0.174 Uiso 1 1 calc R U . . .
C6C C 0.4852(8) -0.0742(2) 0.2003(3) 0.181(3) Uani 1 1 d . . . . .
H6C H 0.4744 -0.0943 0.1648 0.217 Uiso 1 1 calc R U . . .
C7C C 0.5000 -0.1028(4) 0.2500 0.157(4) Uani 1 2 d S T P . .
H7C H 0.5000 -0.1429 0.2500 0.188 Uiso 1 2 calc R U P . .
C1D C 0.6856(10) 0.4636(5) 0.5589(4) 0.123(4) Uiso 0.701(8) 1 d . . P A 1
C2D C 0.7340(12) 0.4791(4) 0.5098(5) 0.139(4) Uiso 0.701(8) 1 d . . P A 1
H2D H 0.7332 0.5178 0.4995 0.167 Uiso 0.701(8) 1 calc R U P A 1
C3D C 0.7804(9) 0.4426(5) 0.4774(4) 0.122(3) Uiso 0.701(8) 1 d . . P A 1
C4D C 0.7900(8) 0.3838(4) 0.4924(5) 0.110(2) Uiso 0.701(8) 1 d . . P A 1
H4D H 0.8260 0.3578 0.4692 0.131 Uiso 0.701(8) 1 calc R U P A 1
C5D C 0.7450(8) 0.3652(3) 0.5424(4) 0.102(2) Uiso 0.701(8) 1 d . . P A 1
H5D H 0.7517 0.3267 0.5536 0.123 Uiso 0.701(8) 1 calc R U P A 1
C6D C 0.6886(8) 0.4062(4) 0.5762(3) 0.104(2) Uiso 0.701(8) 1 d . . P A 1
H6D H 0.6546 0.3948 0.6090 0.124 Uiso 0.701(8) 1 calc R U P A 1
C7D C 0.6374(13) 0.5064(6) 0.5973(6) 0.201(6) Uiso 0.701(8) 1 d . . P A 1
H7D1 H 0.6986 0.5369 0.6062 0.302 Uiso 0.701(8) 1 calc R U P A 1
H7D2 H 0.6242 0.4881 0.6331 0.302 Uiso 0.701(8) 1 calc R U P A 1
H7D3 H 0.5580 0.5220 0.5774 0.302 Uiso 0.701(8) 1 calc R U P A 1
C8D C 0.8331(12) 0.4632(5) 0.4256(5) 0.213(5) Uiso 0.701(8) 1 d . . P A 1
H8D1 H 0.7710 0.4869 0.4015 0.319 Uiso 0.701(8) 1 calc R U P A 1
H8D2 H 0.8537 0.4307 0.4031 0.319 Uiso 0.701(8) 1 calc R U P A 1
H8D3 H 0.9089 0.4854 0.4386 0.319 Uiso 0.701(8) 1 calc R U P A 1
C1F C 0.6747(17) 0.4466(9) 0.5633(7) 0.112(9) Uiso 0.298(8) 1 d G . P B 3
C2F C 0.7124(13) 0.3892(7) 0.5632(5) 0.084(4) Uiso 0.298(8) 1 d G . P B 3
H2F H 0.6978 0.3647 0.5933 0.101 Uiso 0.298(8) 1 calc R U P B 3
C3F C 0.7717(13) 0.3685(5) 0.5180(8) 0.081(4) Uiso 0.298(8) 1 d G . P B 3
C4F C 0.7934(13) 0.4052(10) 0.4729(5) 0.095(5) Uiso 0.298(8) 1 d G . P B 3
H4F H 0.8332 0.3913 0.4427 0.114 Uiso 0.298(8) 1 calc R U P B 3
C5F C 0.756(2) 0.4626(9) 0.4731(7) 0.38(5) Uiso 0.298(8) 1 d G . P B 3
H5F H 0.7704 0.4871 0.4429 0.454 Uiso 0.298(8) 1 calc R U P B 3
C6F C 0.696(2) 0.4833(5) 0.5183(10) 0.191(18) Uiso 0.298(8) 1 d G . P B 3
H6F H 0.6713 0.5217 0.5184 0.229 Uiso 0.298(8) 1 calc R U P B 3
C7F C 0.577(2) 0.4864(11) 0.5950(11) 0.158(9) Uiso 0.298(8) 1 d . . P B 3
H7F1 H 0.4933 0.4695 0.5880 0.236 Uiso 0.298(8) 1 calc R U P B 3
H7F2 H 0.5731 0.5246 0.5787 0.236 Uiso 0.298(8) 1 calc R U P B 3
H7F3 H 0.6076 0.4882 0.6366 0.236 Uiso 0.298(8) 1 calc R U P B 3
C8F C 0.7836(18) 0.3073(8) 0.5309(8) 0.136(7) Uiso 0.298(8) 1 d . . P B 3
H8F1 H 0.7077 0.2939 0.5440 0.204 Uiso 0.298(8) 1 calc R U P B 3
H8F2 H 0.8561 0.3009 0.5612 0.204 Uiso 0.298(8) 1 calc R U P B 3
H8F3 H 0.7950 0.2867 0.4960 0.204 Uiso 0.298(8) 1 calc R U P B 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 176.25(13) . 2_655
N1 Ni1 N1C 88.12(7) . .
N1 Ni1 N1C 88.12(7) 2_655 .
N1 Ni1 N1B 91.88(7) . .
N1 Ni1 N1B 91.88(7) 2_655 .
N1C Ni1 N1B 180.0 . .
N1 Ni1 N1A 89.90(9) . .
N1 Ni1 N1A 90.32(9) 2_655 .
N1C Ni1 N1A 93.32(6) . .
N1B Ni1 N1A 86.68(6) . .
N1 Ni1 N1A 90.32(9) . 2_655
N1 Ni1 N1A 89.90(9) 2_655 2_655
N1C Ni1 N1A 93.32(6) . 2_655
N1B Ni1 N1A 86.68(6) . 2_655
N1A Ni1 N1A 173.36(12) . 2_655
C1 N1 Ni1 167.7(2) . .
N1 C1 S1 178.7(3) . .
C1A N1A C5A 115.1(3) . .
C1A N1A Ni1 124.32(19) . .
C5A N1A Ni1 119.8(2) . .
N1A C1A C2A 124.4(3) . .
C3A C2A C1A 120.9(3) . .
C2A C3A C4A 114.7(3) . .
C2A C3A C6A 124.3(3) . .
C4A C3A C6A 121.0(3) . .
C5A C4A C3A 121.2(3) . .
N1A C5A C4A 123.6(3) . .
C11A C6A C7A 116.7(3) . .
C11A C6A C3A 122.3(3) . .
C7A C6A C3A 121.0(3) . .
C8A C7A C6A 121.8(3) . .
C9A C8A C7A 120.6(4) . .
C8A C9A C10A 118.7(4) . .
C9A C10A C11A 121.5(4) . .
C6A C11A C10A 120.7(3) . .
C1B N1B C1B 115.6(4) . 2_655
C1B N1B Ni1 122.21(18) . .
C1B N1B Ni1 122.21(18) 2_655 .
N1B C1B C2B 123.6(3) . .
C1B C2B C3B 121.4(3) . .
C2B C3B C2B 114.5(4) 2_655 .
C2B C3B C4B 122.75(19) 2_655 .
C2B C3B C4B 122.75(19) . .
C5B C4B C5B 117.5(4) . 2_655
C5B C4B C3B 121.26(19) . .
C5B C4B C3B 121.26(19) 2_655 .
C6B C5B C4B 121.2(3) . .
C7B C6B C5B 119.7(4) . .
C6B C7B C6B 120.5(5) . 2_655
C1C N1C C1C 115.2(4) 2_655 .
C1C N1C Ni1 122.40(18) 2_655 .
C1C N1C Ni1 122.40(18) . .
N1C C1C C2C 124.1(3) . .
C1C C2C C3C 120.6(3) . .
C2C C3C C2C 115.3(4) 2_655 .
C2C C3C C4C 122.3(2) 2_655 .
C2C C3C C4C 122.3(2) . .
C5C C4C C5C 115.4(6) 2_655 .
C5C C4C C3C 122.3(3) 2_655 .
C5C C4C C3C 122.3(3) . .
C4C C5C C6C 122.0(6) . .
C7C C6C C5C 120.7(7) . .
C6C C7C C6C 119.2(9) 2_655 .
C2D C1D C6D 119.6(9) . .
C2D C1D C7D 122.4(12) . .
C6D C1D C7D 117.8(10) . .
C3D C2D C1D 123.0(10) . .
C2D C3D C4D 121.1(9) . .
C2D C3D C8D 119.5(11) . .
C4D C3D C8D 119.3(12) . .
C5D C4D C3D 119.0(8) . .
C4D C5D C6D 118.7(6) . .
C1D C6D C5D 118.4(7) . .
C2F C1F C6F 120.0 . .
C2F C1F C7F 137.7(18) . .
C6F C1F C7F 100.6(17) . .
C3F C2F C1F 120.0 . .
C2F C3F C4F 120.0 . .
C2F C3F C8F 102.7(17) . .
C4F C3F C8F 137.0(16) . .
C3F C4F C5F 120.0 . .
C6F C5F C4F 120.0 . .
C5F C6F C1F 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 2.063(2) .
Ni1 N1 2.063(2) 2_655
Ni1 N1C 2.119(3) .
Ni1 N1B 2.123(3) .
Ni1 N1A 2.158(2) .
Ni1 N1A 2.158(2) 2_655
S1 C1 1.620(3) .
N1 C1 1.128(3) .
N1A C1A 1.321(4) .
N1A C5A 1.336(4) .
C1A C2A 1.370(4) .
C2A C3A 1.370(4) .
C3A C4A 1.383(4) .
C3A C6A 1.486(4) .
C4A C5A 1.364(4) .
C6A C11A 1.366(4) .
C6A C7A 1.380(4) .
C7A C8A 1.371(5) .
C8A C9A 1.342(5) .
C9A C10A 1.353(5) .
C10A C11A 1.375(5) .
N1B C1B 1.336(3) .
N1B C1B 1.336(3) 2_655
C1B C2B 1.364(4) .
C2B C3B 1.383(4) .
C3B C2B 1.383(4) 2_655
C3B C4B 1.468(5) .
C4B C5B 1.391(4) .
C4B C5B 1.391(4) 2_655
C5B C6B 1.384(4) .
C6B C7B 1.368(4) .
C7B C6B 1.368(4) 2_655
N1C C1C 1.337(3) 2_655
N1C C1C 1.337(3) .
C1C C2C 1.369(4) .
C2C C3C 1.385(4) .
C3C C2C 1.385(4) 2_655
C3C C4C 1.486(6) .
C4C C5C 1.344(5) 2_655
C4C C5C 1.344(5) .
C5C C6C 1.389(7) .
C6C C7C 1.309(7) .
C7C C6C 1.309(7) 2_655
C1D C2D 1.365(14) .
C1D C6D 1.388(13) .
C1D C7D 1.475(14) .
C2D C3D 1.280(16) .
C3D C4D 1.405(12) .
C3D C8D 1.480(13) .
C4D C5D 1.387(12) .
C5D C6D 1.422(11) .
C1F C2F 1.3900 .
C1F C6F 1.3900 .
C1F C7F 1.65(3) .
C2F C3F 1.3900 .
C3F C4F 1.3900 .
C3F C8F 1.45(2) .
C4F C5F 1.3900 .
C5F C6F 1.3900 .
