#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/11/7011149.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_7011149
loop_
_publ_author_name
'Michael M. Bishop'
'Leonard F. Lindoy'
'Brian W. Skelton'
'Allan H. White'
_publ_section_title
;
 Modification of supramolecular motifs: some effects of incorporation
 of metal complexes into supramolecular arrays
;
_journal_issue                   3
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              377
_journal_page_last               382
_journal_paper_doi               10.1039/b108070a
_journal_year                    2002
_chemical_formula_sum            'C20 H20 N10 Ni O2 S4'
_chemical_formula_weight         619.4
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             01-06-27
_audit_creation_method           Xtal3.6
_cell_angle_alpha                91.773(2)
_cell_angle_beta                 107.638(2)
_cell_angle_gamma                113.737(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5020(10)
_cell_length_b                   7.6810(10)
_cell_length_c                   12.061(2)
_cell_measurement_reflns_used    4093
_cell_measurement_temperature    153
_cell_measurement_theta_max      23.1
_cell_measurement_theta_min      2.8
_cell_volume                     596.90(15)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .029
_diffrn_reflns_av_sigmaI/netI    .027
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7043
_diffrn_reflns_theta_max         29.34
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  .93
_exptl_absorpt_correction_T_min  .59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       prism
_exptl_crystal_F_000             318
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .21
_exptl_crystal_size_min          .17
_refine_diff_density_max         .789
_refine_diff_density_min         -.629
_refine_ls_goodness_of_fit_all   1.194
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2607
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .04
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          .021
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .044
_refine_ls_wR_factor_ref         .042
_reflns_d_resolution_high        .725
_reflns_d_resolution_low         11.291
_reflns_Friedel_coverage         0
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              -10
_reflns_limit_l_max              15
_reflns_limit_l_min              -16
_reflns_number_gt                2607
_reflns_number_total             2943
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b108070a.txt
_cod_data_source_block           ii20mb
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_original_formula_sum        'C20 H20 N10 Ni1 O2 S4'
_cod_database_code               7011149
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni .00000 .00000 .00000 .01764(15) Uani ? ? 1.00000 ? ?
S1 .10256(8) -.07603(7) .17173(4) .0223(2) Uani ? ? 1.00000 ? ?
C2 .2799(3) .1172(3) .28440(18) .0179(7) Uani ? ? 1.00000 ? ?
N21 .2900(3) .0758(3) .39179(16) .0222(6) Uani ? ? 1.00000 ? ?
N3 .4137(3) .2954(2) .28082(15) .0179(6) Uani ? ? 1.00000 ? ?
C4 .4247(3) .3682(3) .18263(18) .0191(7) Uani ? ? 1.00000 ? ?
N41 .5789(3) .5435(3) .19819(17) .0242(7) Uani ? ? 1.00000 ? ?
S5 .26597(8) .27632(8) .03635(5) .0244(2) Uani ? ? 1.00000 ? ?
C11 .7623(3) .4516(3) .61188(18) .0204(7) Uani ? ? 1.00000 ? ?
N11 .6224(3) .2987(3) .62311(18) .0241(7) Uani ? ? 1.00000 ? ?
N12 .7464(3) .5109(3) .50247(16) .0218(6) Uani ? ? 1.00000 ? ?
C13 .9130(3) .6794(3) .5083(2) .0216(7) Uani ? ? 1.00000 ? ?
O13 .9364(3) .7566(2) .42286(14) .0280(6) Uani ? ? 1.00000 ? ?
C13a 1.0508(3) .7399(3) .6343(2) .0219(7) Uani ? ? 1.00000 ? ?
C14 1.2348(4) .9030(3) .6897(2) .0282(9) Uani ? ? 1.00000 ? ?
C15 1.3275(4) .9217(4) .8108(2) .0327(9) Uani ? ? 1.00000 ? ?
C16 1.2394(4) .7821(4) .8731(2) .0330(9) Uani ? ? 1.00000 ? ?
C17 1.0541(4) .6188(4) .8170(2) .0274(8) Uani ? ? 1.00000 ? ?
C17a .9609(3) .6008(3) .6963(2) .0216(7) Uani ? ? 1.00000 ? ?
H21a .388(5) .153(4) .450(3) .035(8) Uiso ? ? 1.00000 ? ?
H21b .201(4) -.031(4) .399(2) .025(7) Uiso ? ? 1.00000 ? ?
H41a .681(5) .594(4) .267(3) .029(7) Uiso ? ? 1.00000 ? ?
H41b .591(5) .592(4) .135(3) .035(8) Uiso ? ? 1.00000 ? ?
H11 .657(5) .280(5) .687(3) .044(9) Uiso ? ? 1.00000 ? ?
H12 .644(5) .447(5) .436(3) .049(9) Uiso ? ? 1.00000 ? ?
H14 1.291(4) 1.000(4) .646(2) .024(7) Uiso ? ? 1.00000 ? ?
H15 1.454(6) 1.034(5) .844(3) .058(10) Uiso ? ? 1.00000 ? ?
H16 1.295(6) .795(5) .956(3) .055(10) Uiso ? ? 1.00000 ? ?
H17 .992(4) .521(4) .861(2) .021(6) Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 20 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 20 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 10 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Ni ? 0 1 .285 1.113 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
S ? 0 4 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Ni S5 . . . 95.72(2) ?
S1 Ni S1 . . 2 180.0000 ?
S1 Ni S5 . . 2 84.28(2) ?
S5 Ni S1 . . 2 84.28(2) ?
S5 Ni S5 . . 2 180.0000 ?
S1 Ni S5 2 . 2 95.72(2) ?
Ni S1 C2 . . . 115.23(8) ?
S1 C2 N21 . . . 113.34(14) ?
S1 C2 N3 . . . 130.82(17) ?
N21 C2 N3 . . . 115.74(16) ?
C2 N21 H21a . . . 119(2) ?
C2 N21 H21b . . . 119.4(17) ?
H21a N21 H21b . . . 122(3) ?
C2 N3 C4 . . . 125.40(15) ?
N3 C4 N41 . . . 115.83(16) ?
N3 C4 S5 . . . 130.68(13) ?
N41 C4 S5 . . . 113.46(17) ?
C4 N41 H41a . . . 120(2) ?
C4 N41 H41b . . . 117.3(16) ?
H41a N41 H41b . . . 121(3) ?
Ni S5 C4 . . . 117.20(7) ?
N11 C11 N12 . . . 121.26(16) ?
N11 C11 C17a . . . 133.3(2) ?
N12 C11 C17a . . . 105.45(17) ?
C11 N11 H11 . . . 110(2) ?
C11 N12 C13 . . . 112.56(15) ?
C11 N12 H12 . . . 124(2) ?
C13 N12 H12 . . . 123(2) ?
N12 C13 O13 . . . 124.37(17) ?
N12 C13 C13a . . . 106.21(19) ?
O13 C13 C13a . . . 129.41(17) ?
C13 C13a C14 . . . 130.3(2) ?
C13 C13a C17a . . . 107.71(16) ?
C14 C13a C17a . . . 121.9(2) ?
C13a C14 C15 . . . 117.1(2) ?
C13a C14 H14 . . . 120.6(13) ?
C15 C14 H14 . . . 122.3(13) ?
C14 C15 C16 . . . 121.3(2) ?
C14 C15 H15 . . . 114(2) ?
C16 C15 H15 . . . 125(2) ?
C15 C16 C17 . . . 121.5(2) ?
C15 C16 H16 . . . 123(2) ?
C17 C16 H16 . . . 116(2) ?
C16 C17 C17a . . . 117.3(2) ?
C16 C17 H17 . . . 121.2(13) ?
C17a C17 H17 . . . 121.5(13) ?
C11 C17a C13a . . . 108.03(18) ?
C11 C17a C17 . . . 130.9(2) ?
C13a C17a C17 . . . 121.02(17) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni S1 . . 2.1665(6) ?
Ni S5 . . 2.1636(5) ?
Ni S1 . 2 2.1665(6) ?
Ni S5 . 2 2.1636(5) ?
S1 C2 . . 1.7349(17) ?
C2 N21 . . 1.330(3) ?
C2 N3 . . 1.344(2) ?
N21 H21a . . .84(2) ?
N21 H21b . . .85(3) ?
N3 C4 . . 1.336(3) ?
C4 N41 . . 1.336(2) ?
C4 S5 . . 1.733(2) ?
N41 H41a . . .88(3) ?
N41 H41b . . .87(3) ?
C11 N11 . . 1.266(3) ?
C11 N12 . . 1.396(3) ?
C11 C17a . . 1.484(2) ?
N11 H11 . . .77(4) ?
N12 C13 . . 1.371(3) ?
N12 H12 . . .88(3) ?
C13 O13 . . 1.228(3) ?
C13 C13a . . 1.486(3) ?
C13a C14 . . 1.385(3) ?
C13a C17a . . 1.390(3) ?
C14 C15 . . 1.388(3) ?
C14 H14 . . .96(3) ?
C15 C16 . . 1.390(4) ?
C15 H15 . . .94(3) ?
C16 C17 . . 1.392(3) ?
C16 H16 . . .94(4) ?
C17 C17a . . 1.386(3) ?
C17 H17 . . .98(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
