#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:28:04 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179897 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/93/7019347.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_7019347
loop_
_publ_author_name
'Pei, Wen-Bo'
'Wu, Jian-Sheng'
'Ren, Xiao-Ming'
'Tian, Zheng-Fang'
'Xie, Jingli'
_publ_section_title
;
 Observation of divergent isotope effects as well as metal ion-modulated
 T(C) and spin-canting nature in isostructural supramolecular magnets.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7609
_journal_page_last               7619
_journal_paper_doi               10.1039/c2dt30215b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C8 N4 Ni S4, C5 H6 D N2'
_chemical_formula_sum            'C13 H6 D N6 Ni S4'
_chemical_formula_weight         435.22
_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                 93.780(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.406(5)
_cell_length_b                   6.4709(8)
_cell_length_c                   12.9791(16)
_cell_measurement_reflns_used    3724
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.97
_cell_volume                     3470.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0527P)²+0.1578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                2588
_reflns_number_total             2945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30215b.txt
_cod_data_source_block           786197
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7019347
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
Ni1 Ni 0.2500 0.2500 0.5000 0.03668(15) Uani 1 2 d S
Ni2 Ni 0.0000 0.5000 0.5000 0.04276(15) Uani 1 2 d S
S1 S 0.275704(17) -0.02254(9) 0.45826(6) 0.04767(19) Uani 1 1 d .
S2 S 0.264433(16) 0.41856(9) 0.36782(5) 0.04603(19) Uani 1 1 d .
S3 S -0.011627(18) 0.73408(10) 0.38636(5) 0.0494(2) Uani 1 1 d .
S4 S 0.030529(19) 0.36432(11) 0.39046(5) 0.0544(2) Uani 1 1 d .
C2 C 0.29276(6) 0.0501(3) 0.34699(19) 0.0385(5) Uani 1 1 d .
C1 C 0.31308(7) -0.0958(4) 0.2987(2) 0.0470(6) Uani 1 1 d .
C3 C 0.28768(6) 0.2432(3) 0.30674(19) 0.0388(6) Uani 1 1 d .
C4 C 0.30267(7) 0.3062(4) 0.2149(2) 0.0466(6) Uani 1 1 d .
C6 C -0.03783(6) 0.8915(4) 0.4468(2) 0.0424(6) Uani 1 1 d .
C5 C -0.05147(6) 1.0660(4) 0.3913(2) 0.0486(6) Uani 1 1 d .
C8 C 0.04595(6) 0.1516(4) 0.4557(2) 0.0428(6) Uani 1 1 d .
C7 C 0.06810(7) 0.0189(4) 0.4054(2) 0.0478(6) Uani 1 1 d .
C9 C 0.14729(6) 0.9197(4) 0.0392(2) 0.0505(7) Uani 1 1 d .
H9A H 0.15771(6) 1.0471(4) 0.0405(2) 0.061 Uiso 1 1 d R
C10 C 0.13020(6) 0.8638(4) 0.1193(2) 0.0444(6) Uani 1 1 d .
H10A H 0.12880(6) 0.9526(4) 0.1752(2) 0.053 Uiso 1 1 d R
C11 C 0.11436(6) 0.6701(4) 0.1186(2) 0.0411(6) Uani 1 1 d .
C12 C 0.11761(7) 0.5431(4) 0.0314(2) 0.0504(7) Uani 1 1 d .
H12A H 0.10772(7) 0.4140(4) 0.0276(2) 0.060 Uiso 1 1 d R
C13 C 0.13504(7) 0.6089(5) -0.0463(2) 0.0566(7) Uani 1 1 d .
H13A H 0.13705(7) 0.5244(5) -0.1035(2) 0.068 Uiso 1 1 d R
N1 N 0.32981(7) -0.2084(4) 0.2601(2) 0.0635(7) Uani 1 1 d .
N2 N 0.31520(7) 0.3560(4) 0.1439(2) 0.0677(7) Uani 1 1 d .
N3 N -0.06317(7) 1.2030(4) 0.3492(2) 0.0651(7) Uani 1 1 d .
N4 N 0.08564(7) -0.0880(4) 0.3678(2) 0.0661(7) Uani 1 1 d .
N5 N 0.14957(6) 0.7949(4) -0.04249(18) 0.0533(6) Uani 1 1 d .
D5A D 0.1605 0.8344 -0.0931 0.064 Uiso 1 1 d R
N6 N 0.09744(5) 0.6094(3) 0.19606(17) 0.0521(6) Uani 1 1 d .
H6A H 0.08815(5) 0.4905(3) 0.19398(17) 0.062 Uiso 1 1 d R
H6B H 0.09573(5) 0.6889(3) 0.24853(17) 0.062 Uiso 1 1 d R
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'
D D 0.0000 0.0000 '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
S1 Ni1 S1 180.00(5) . 7_556
S1 Ni1 S2 92.69(3) . .
S1 Ni1 S2 87.31(3) 7_556 .
S1 Ni1 S2 87.31(3) . 7_556
S1 Ni1 S2 92.69(3) 7_556 7_556
S2 Ni1 S2 180.00(3) . 7_556
S3 Ni2 S3 180.00(4) 5_566 .
S3 Ni2 S4 92.93(3) 5_566 .
S3 Ni2 S4 87.07(3) . .
S3 Ni2 S4 87.07(3) 5_566 5_566
S3 Ni2 S4 92.93(3) . 5_566
S4 Ni2 S4 180.00(3) . 5_566
C2 S1 Ni1 103.05(8) . .
C3 S2 Ni1 103.13(8) . .
C6 S3 Ni2 102.98(9) . .
C8 S4 Ni2 102.53(9) . .
C3 C2 C1 121.0(2) . .
C3 C2 S1 120.8(2) . .
C1 C2 S1 118.24(18) . .
N1 C1 C2 178.4(3) . .
C2 C3 C4 120.8(2) . .
C2 C3 S2 120.4(2) . .
C4 C3 S2 118.78(18) . .
N2 C4 C3 178.3(3) . .
C8 C6 C5 121.0(2) 5_566 .
C8 C6 S3 120.4(2) 5_566 .
C5 C6 S3 118.5(2) . .
N3 C5 C6 177.7(3) . .
C6 C8 C7 120.1(2) 5_566 .
C6 C8 S4 121.11(19) 5_566 .
C7 C8 S4 118.7(2) . .
N4 C7 C8 178.5(3) . .
H9A C9 N5 119.43(16) . .
H9A C9 C10 119.43(16) . .
N5 C9 C10 121.1(3) . .
H10A C10 C9 119.99(16) . .
H10A C10 C11 119.99(16) . .
C9 C10 C11 120.0(2) . .
N6 C11 C12 121.3(2) . .
N6 C11 C10 121.8(2) . .
C12 C11 C10 116.9(2) . .
H12A C12 C13 120.00(17) . .
H12A C12 C11 119.99(16) . .
C13 C12 C11 120.0(3) . .
H13A C13 N5 119.50(16) . .
H13A C13 C12 119.49(17) . .
N5 C13 C12 121.0(2) . .
C9 N5 C13 120.9(2) . .
C9 N5 D5A 119.5 . .
C13 N5 D5A 119.5 . .
H6B N6 H6A 120.0 . .
H6B N6 C11 120.00(15) . .
H6A N6 C11 120.00(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S1 2.1476(6) .
Ni1 S1 2.1476(6) 7_556
Ni1 S2 2.1506(7) .
Ni1 S2 2.1506(7) 7_556
Ni2 S3 2.1466(7) 5_566
Ni2 S3 2.1466(7) .
Ni2 S4 2.1511(7) .
Ni2 S4 2.1511(7) 5_566
S1 C2 1.715(3) .
S2 C3 1.716(2) .
S3 C6 1.716(2) .
S4 C8 1.717(3) .
C2 C3 1.365(3) .
C2 C1 1.436(4) .
C1 N1 1.144(3) .
C3 C4 1.439(4) .
C4 N2 1.133(3) .
C6 C8 1.359(4) 5_566
C6 C5 1.435(4) .
C5 N3 1.133(3) .
C8 C6 1.359(4) 5_566
C8 C7 1.443(4) .
C7 N4 1.136(3) .
C9 H9A 0.9300 .
C9 N5 1.341(3) .
C9 C10 1.345(4) .
C10 H10A 0.9300 .
C10 C11 1.415(4) .
C11 N6 1.323(3) .
C11 C12 1.412(4) .
C12 H12A 0.9300 .
C12 C13 1.348(4) .
C13 H13A 0.9300 .
C13 N5 1.345(4) .
N5 D5A 0.8600 .
N6 H6B 0.8600 .
N6 H6A 0.8600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 D5A N2 0.86 2.36 3.036(3) 136.2 7_565
N5 D5A N1 0.86 2.37 3.056(3) 136.4 7
N6 H6A N3 0.86 2.18 3.027(3) 166.9 2_545
N6 H6B N4 0.86 2.18 3.030(3) 171.5 1_565
