#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/78/2007880.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007880
loop_
_publ_author_name
'James, Michael'
'Kawaguchi, Hiroyuki'
'Tatsumi, Kazuyuki'
'Hambley, Trevor W.'
_publ_section_title
;
 Bis[bis(ethylenediamine-N,N')(μN,{ıt
 S}-thiocyanato)nickel(II)] Bis(hexafluorophosphate)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1809
_journal_page_last               1811
_journal_paper_doi               10.1107/S0108270198008841
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[Ni2 (N C S)2 (C2 H8 N2)4] (P F6)2'
_chemical_formula_moiety         'C10 H32 N10 Ni2 S2 2+, 2(P F6 1-)'
_chemical_formula_sum            'C10 H32 F12 N10 Ni2 P2 S2'
_chemical_formula_weight         763.87
_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'
_cell_angle_alpha                90
_cell_angle_beta                 124.72(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.865(3)
_cell_length_b                   16.781(3)
_cell_length_c                   12.691(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2777.1(12)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1994)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1997)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et. al. 1993)'
_diffrn_ambient_temperature      273.2
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 four-circle'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3981
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        2.4
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.73
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.49
_refine_ls_goodness_of_fit_ref   1.49
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.0003|Fo|²]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.047
_refine_ls_wR_factor_ref         0.047
_reflns_number_gt                2615
_reflns_number_total             3483
_reflns_threshold_expression     I>2.50σ(I)
_cod_data_source_file            bk1401.cif
_cod_data_source_block           nienncspf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2777.0(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C10 H32 F12 N10 Ni2 P2 S2 '
_cod_database_code               2007880
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+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_refinement_flags
_atom_site_occupancy
Ni1 0.80354(2) 0.17584(2) 0.23253(3) 0.03089(7) Uani d ? . 1.000
S1 0.86936(5) 0.12724(4) 0.09688(6) 0.0423(2) Uani d ? . 1.000
P1 1.0000 0.13401(6) 0.7500 0.0400(2) Uani d ? ST 1.000
P2 0.5000 0.00078(8) 0.2500 0.0541(3) Uani d ? ST 1.000
F1 1.0000 0.2263(2) 0.7500 0.135(2) Uani d ? ST 1.000
F2 1.0000 0.0412(2) 0.7500 0.1100(10) Uani d ? ST 1.000
F3 1.1098(2) 0.1333(2) 0.8799(2) 0.1019(9) Uani d ? . 1.000
F4 1.0477(2) 0.1339(2) 0.6703(2) 0.0922(8) Uani d ? . 1.000
F5 0.5856(2) 0.0659(2) 0.3016(3) 0.1210(10) Uani d ? . 1.000
F6 0.4144(2) -0.0651(2) 0.1956(3) 0.1280(10) Uani d ? . 1.000
F7 0.4928(2) 0.0004(3) 0.1224(3) 0.1350(10) Uani d ? . 1.000
N1 0.7100(2) 0.25920(10) 0.0965(2) 0.0461(6) Uani d ? . 1.000
N2 0.6910(2) 0.0883(2) 0.1453(2) 0.0456(6) Uani d ? . 1.000
N3 0.8913(2) 0.08230(10) 0.3605(2) 0.0405(5) Uani d ? . 1.000
N4 0.9201(2) 0.26080(10) 0.3243(2) 0.0426(6) Uani d ? . 1.000
N5 0.7662(2) 0.2222(2) 0.3561(2) 0.0418(6) Uani d ? . 1.000
C1 0.6779(2) 0.30630(10) 0.0168(2) 0.0305(5) Uani d ? . 1.000
C2 0.7386(3) 0.0100(2) 0.1980(4) 0.0564(8) Uani d ? . 1.000
C3 0.8178(2) 0.0189(2) 0.3396(3) 0.0550(8) Uani d ? . 1.000
C4 0.9242(3) 0.2936(2) 0.4346(3) 0.0550(8) Uani d ? . 1.000
C5 0.8170(3) 0.2995(2) 0.4017(3) 0.0539(8) Uani d ? . 1.000
H1 0.934(2) 0.065(2) 0.349(3) 0.048(9) Uiso d ? . 1.000
H2 0.925(2) 0.094(2) 0.433(3) 0.060(10) Uiso d ? . 1.000
H3 0.784(2) 0.037(2) 0.383(3) 0.037(7) Uiso d ? . 1.000
H4 0.861(2) -0.029(2) 0.381(3) 0.060(10) Uiso d ? . 1.000
H5 0.684(3) -0.028(2) 0.174(3) 0.070(10) Uiso d ? . 1.000
H6 0.773(2) -0.005(2) 0.158(3) 0.053(9) Uiso d ? . 1.000
H7 0.639(2) 0.097(2) 0.160(3) 0.060(10) Uiso d ? . 1.000
H8 0.656(2) 0.087(2) 0.060(3) 0.070(10) Uiso d ? . 1.000
H9 0.983(2) 0.244(2) 0.352(3) 0.060(10) Uiso d ? . 1.000
H10 0.910(2) 0.297(2) 0.272(3) 0.048(9) Uiso d ? . 1.000
H11 0.964(3) 0.258(2) 0.506(4) 0.070(10) Uiso d ? . 1.000
H12 0.955(3) 0.339(2) 0.454(3) 0.060(10) Uiso d ? . 1.000
H13 0.817(3) 0.317(2) 0.485(4) 0.070(10) Uiso d ? . 1.000
H14 0.784(2) 0.333(2) 0.343(3) 0.048(9) Uiso d ? . 1.000
H15 0.704(2) 0.225(2) 0.323(3) 0.052(9) Uiso d ? . 1.000
H16 0.778(2) 0.191(2) 0.421(3) 0.060(10) Uiso d ? . 1.000
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni 0.285 1.113
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S 0.110 0.124
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
P 0.090 0.095
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F 0.014 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_3
_geom_angle
_geom_angle_publ_flag
S1 Ni1 N1 . . 91.56(7) yes
S1 Ni1 N2 . . 88.44(8) yes
S1 Ni1 N3 . . 86.50(7) yes
S1 Ni1 N4 . . 91.23(7) yes
S1 Ni1 N5 . . 173.47(7) yes
N1 Ni1 N2 . . 92.50(10) yes
N1 Ni1 N3 . . 174.90(10) yes
N1 Ni1 N4 . . 89.40(10) yes
N1 Ni1 N5 . . 89.97(9) yes
N2 Ni1 N3 . . 82.80(10) yes
N2 Ni1 N4 . . 178.06(9) yes
N2 Ni1 N5 . . 97.80(10) yes
N3 Ni1 N4 . . 95.29(9) yes
N3 Ni1 N5 . . 92.50(10) yes
N4 Ni1 N5 . . 82.40(10) yes
Ni1 S1 C1 . 7_655 102.43(9) yes
F1 P1 F2 . . 180.00(10) no
F1 P1 F3 . . 90.40(10) no
F1 P1 F3 . 2_756 90.40(10) no
F1 P1 F4 . . 90.10(10) no
F1 P1 F4 . 2_756 90.10(10) no
F2 P1 F3 . . 89.60(10) no
F2 P1 F3 . 2_756 89.60(10) no
F2 P1 F4 . . 89.90(10) no
F2 P1 F4 . 2_756 89.90(10) no
F3 P1 F3 . 2_756 179.2(3) no
F3 P1 F4 . . 91.30(10) no
F3 P1 F4 . 2_756 88.70(10) no
F3 P1 F4 2_756 . 88.70(10) no
F3 P1 F4 2_756 2_756 91.30(10) no
F4 P1 F4 . 2_756 179.9(2) no
F5 P2 F5 . 2_655 91.5(2) no
F5 P2 F6 . . 178.7(2) no
F5 P2 F6 . 2_655 88.9(2) no
F5 P2 F7 . . 88.3(2) no
F5 P2 F7 . 2_655 92.0(2) no
F5 P2 F6 2_655 . 88.9(2) no
F5 P2 F6 2_655 2_655 178.7(2) no
F5 P2 F7 2_655 . 92.0(2) no
F5 P2 F7 2_655 2_655 88.3(2) no
F6 P2 F6 . 2_655 90.8(3) no
F6 P2 F7 . . 90.4(2) no
F6 P2 F7 . 2_655 89.3(2) no
F6 P2 F7 2_655 . 89.3(2) no
F6 P2 F7 2_655 2_655 90.4(2) no
F7 P2 F7 . 2_655 179.6(3) no
Ni1 N1 C1 . . 162.5(2) yes
Ni1 N2 C2 . . 109.0(2) yes
Ni1 N2 H7 . . 111(2) no
Ni1 N2 H8 . . 114(2) no
C2 N2 H7 . . 109(2) no
C2 N2 H8 . . 110(2) no
H7 N2 H8 . . 103(3) no
Ni1 N3 C3 . . 106.7(2) yes
Ni1 N3 H1 . . 112(2) no
Ni1 N3 H2 . . 115(3) no
C3 N3 H1 . . 111(2) no
C3 N3 H2 . . 110(3) no
H1 N3 H2 . . 102(3) no
Ni1 N4 C4 . . 109.4(2) yes
Ni1 N4 H9 . . 116(2) no
Ni1 N4 H10 . . 110(2) no
C4 N4 H9 . . 108(2) no
C4 N4 H10 . . 111(2) no
H9 N4 H10 . . 102(3) no
Ni1 N5 C5 . . 107.2(2) yes
Ni1 N5 H15 . . 114(2) no
Ni1 N5 H16 . . 118(2) no
C5 N5 H15 . . 112(2) no
C5 N5 H16 . . 112(2) no
H15 N5 H16 . . 94(3) no
S1 C1 N1 7_655 . 179.1(2) yes
N2 C2 C3 . . 108.5(3) yes
N2 C2 H5 . . 108(2) no
N2 C2 H6 . . 107(2) no
C3 C2 H5 . . 115(2) no
C3 C2 H6 . . 109(2) no
H5 C2 H6 . . 110(3) no
N3 C3 C2 . . 108.7(3) yes
N3 C3 H3 . . 107(2) no
N3 C3 H4 . . 105(2) no
C2 C3 H3 . . 110.0(10) no
C2 C3 H4 . . 114(2) no
H3 C3 H4 . . 111(3) no
N4 C4 C5 . . 109.3(3) yes
N4 C4 H11 . . 108(2) no
N4 C4 H12 . . 108(3) no
C5 C4 H11 . . 109(2) no
C5 C4 H12 . . 113(2) no
H11 C4 H12 . . 109(3) no
N5 C5 C4 . . 109.4(3) yes
N5 C5 H13 . . 109(2) no
N5 C5 H14 . . 108(2) no
C4 C5 H13 . . 111(2) no
C4 C5 H14 . . 109(2) no
H13 C5 H14 . . 110(3) no
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
Ni1 S1 . . 2.6014(8) yes
Ni1 N1 . . 2.055(2) yes
Ni1 N2 . . 2.078(2) yes
Ni1 N3 . . 2.113(2) yes
Ni1 N4 . . 2.087(2) yes
Ni1 N5 . . 2.115(2) yes
S1 C1 . 7_655 1.630(2) yes
P1 F1 . . 1.549(4) no
P1 F2 . . 1.557(3) no
P1 F3 . . 1.575(2) no
P1 F3 . 2_756 1.575(2) no
P1 F4 . . 1.571(2) no
P1 F4 . 2_756 1.571(2) no
P2 F5 . . 1.566(3) no
P2 F5 . 2_655 1.566(3) no
P2 F6 . . 1.573(3) no
P2 F6 . 2_655 1.573(3) no
P2 F7 . . 1.558(3) no
P2 F7 . 2_655 1.558(3) no
N1 C1 . . 1.148(3) yes
N2 C2 . . 1.473(4) yes
N2 H7 . . 0.95(3) no
N2 H8 . . 0.90(4) no
N3 C3 . . 1.486(4) yes
N3 H1 . . 0.83(3) no
N3 H2 . . 0.78(3) no
N4 C4 . . 1.471(4) yes
N4 H9 . . 0.89(3) no
N4 H10 . . 0.85(3) no
N5 C5 . . 1.462(4) yes
N5 H15 . . 0.82(3) no
N5 H16 . . 0.90(3) no
C2 C3 . . 1.503(5) yes
C2 H5 . . 0.98(4) no
C2 H6 . . 0.97(3) no
C3 H3 . . 1.02(3) no
C3 H4 . . 0.99(3) no
C4 C5 . . 1.506(5) yes
C4 H11 . . 0.97(4) no
C4 H12 . . 0.87(3) no
C5 H13 . . 1.10(4) no
C5 H14 . . 0.83(3) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
S1 F2 3.387(3) 3_756 no
S1 N3 3.598(2) 2_755 no
F2 N3 3.463(3) 3_756 no
F2 N3 3.463(3) 4 no
F3 N5 3.132(3) 2_756 no
F3 C5 3.334(4) 8 no
F3 N3 3.413(4) 2_756 no
F4 N3 3.355(3) . no
F4 C3 3.385(4) 3_756 no
F5 N2 3.265(4) . no
F5 C2 3.485(5) . no
F5 C3 3.521(4) . no
F6 N4 3.324(4) 5_445 no
F7 F7 3.242(6) 3_655 no
F7 N2 3.313(4) 3_655 no
F7 N2 3.332(4) . no
F7 C2 3.448(5) . no
N4 C1 3.547(3) 8 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N2 H7 F5 . 2.45(4) y
N2 H7 F7 . 2.65(3) y
N2 H8 F6 3_655 2.79(4) y
N2 H8 F7 3_655 2.62(3) y
N3 H1 F2 4_555 2.70(3) y
N3 H2 F3 2_756 2.81(4) y
N3 H2 F4 . 2.58(3) y
N4 H10 F6 5_445 2.52(3) y
N5 H15 F1 8_454 2.93(3) y
N5 H16 F3 2_756 2.32(3) y
' ' H1 S1 2_755 2.97(3) y
' ' H9 S1 2_755 2.83(3) y
