#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/60/2006064.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_2006064
loop_
_publ_author_name
'Blake, A. J.'
'Danks, J. P.'
'Parsons, S.'
'Schröder, M.'
_publ_section_title
;
 Bis[bis(2-aminoethyl-N)sulfide-S]nickel(II)
 Bis(hexafluorophosphate)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              411
_journal_page_last               413
_journal_paper_doi               10.1107/S0108270196013297
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Ni (C4 H12 N2 S)2] [P F6]2'
_chemical_formula_moiety         'C8 H24 N4 Ni S2 2+ , 2P F6 -'
_chemical_formula_sum            'C8 H24 F12 N4 Ni P2 S2'
_chemical_formula_weight         589.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.88(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.582(12)
_cell_length_b                   9.451(8)
_cell_length_c                   24.558(17)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      26
_cell_volume                     4032(5)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device
;
Stoe Stadi-4 four circle diffractometer with Oxford Cryosystems open-flow
cryostat (Cosier & Glazer, 1986)
;
_diffrn_measurement_method       ω-2θ
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8991
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   'calculated from \DF (Walker & Stuart, 1983)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_meas      ?
_exptl_crystal_description       columnar
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         '1.47 (0.96\%A from Ni)'
_refine_diff_density_min         '-1.81 (1.03\%A from Ni)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   0.856
_refine_ls_hydrogen_treatment    'H atoms introduced at calculated positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      0.856
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_obs          0.0647
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.231P)²+13.02P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3020
_refine_ls_wR_factor_obs         0.2062
_reflns_number_observed          2840
_reflns_number_total             3514
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1164.cif
_cod_data_source_block           nis3n2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (18
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15
times).

'_geom_torsion_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.231P)^2^+13.02P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.231P)^2^+13.02P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               2006064
_cod_database_fobs_code          2006064
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Ni 1 0.58827(4) 0.24704(7) -0.12065(3) 0.0154(4) Uani d . Ni
N1 1 0.4715(3) 0.2248(6) -0.1563(2) 0.0189(12) Uani d . N
H1A 1 0.4598(3) 0.2921(6) -0.1833(2) 0.023 Uiso calc R H
H1B 1 0.4645(3) 0.1373(6) -0.1727(2) 0.023 Uiso calc R H
C2 1 0.4176(4) 0.2397(7) -0.1157(3) 0.0209(14) Uani d . C
H2A 1 0.4216(4) 0.1557(7) -0.0914(3) 0.025 Uiso calc R H
H2B 1 0.3641(4) 0.2454(7) -0.1353(3) 0.025 Uiso calc R H
C3 1 0.4366(4) 0.3730(7) -0.0810(3) 0.0218(14) Uani d . C
H3A 1 0.4031(4) 0.3764(7) -0.0520(3) 0.026 Uiso calc R H
H3B 1 0.4249(4) 0.4572(7) -0.1048(3) 0.026 Uiso calc R H
S4 1 0.53614(9) 0.3807(2) -0.04866(7) 0.0216(5) Uani d . S
C5 1 0.5366(5) 0.2377(8) 0.0023(3) 0.030(2) Uani d . C
H5A 1 0.5506(5) 0.2769(8) 0.0399(3) 0.036 Uiso calc R H
H5B 1 0.4844(5) 0.1964(8) -0.0006(3) 0.036 Uiso calc R H
C6 1 0.5932(4) 0.1234(8) -0.0069(3) 0.030(2) Uani d . C
H6A 1 0.6462(4) 0.1595(8) 0.0041(3) 0.036 Uiso calc R H
H6B 1 0.5862(4) 0.0415(8) 0.0170(3) 0.036 Uiso calc R H
N7 1 0.5841(3) 0.0763(6) -0.0639(2) 0.0201(12) Uani d . N
H7A 1 0.5376(3) 0.0303(6) -0.0724(2) 0.024 Uiso calc R H
H7B 1 0.6224(3) 0.0126(6) -0.0678(2) 0.024 Uiso calc R H
N11 1 0.6314(3) 0.1186(5) -0.1788(2) 0.0192(11) Uani d . N
H11A 1 0.6271(3) 0.0254(5) -0.1690(2) 0.023 Uiso calc R H
H11B 1 0.6015(3) 0.1314(5) -0.2126(2) 0.023 Uiso calc R H
C21 1 0.7127(4) 0.1482(7) -0.1840(3) 0.0231(14) Uani d . C
H21A 1 0.7163(4) 0.2400(7) -0.2028(3) 0.028 Uiso calc R H
H21B 1 0.7323(4) 0.0735(7) -0.2064(3) 0.028 Uiso calc R H
C31 1 0.7603(4) 0.1527(8) -0.1280(3) 0.030(2) Uani d . C
H31A 1 0.8141(4) 0.1759(8) -0.1319(3) 0.036 Uiso calc R H
H31B 1 0.7602(4) 0.0579(8) -0.1109(3) 0.036 Uiso calc R H
S41 1 0.72506(9) 0.2832(2) -0.08248(7) 0.0214(5) Uani d . S
C51 1 0.7385(4) 0.4504(7) -0.1165(4) 0.031(2) Uani d . C
H51A 1 0.7758(4) 0.5096(7) -0.0922(4) 0.038 Uiso calc R H
H51B 1 0.7598(4) 0.4322(7) -0.1509(4) 0.038 Uiso calc R H
C61 1 0.6626(4) 0.5290(7) -0.1301(3) 0.0263(15) Uani d . C
H61A 1 0.6444(4) 0.5574(7) -0.0955(3) 0.032 Uiso calc R H
H61B 1 0.6703(4) 0.6159(7) -0.1511(3) 0.032 Uiso calc R H
N71 1 0.6040(3) 0.4384(6) -0.1630(2) 0.0223(12) Uani d . N
H71A 1 0.6193(3) 0.4179(6) -0.1963(2) 0.027 Uiso calc R H
H71B 1 0.5580(3) 0.4865(6) -0.1699(2) 0.027 Uiso calc R H
P1 1 1.02317(9) -0.2005(2) 0.17829(7) 0.0218(5) Uani d . P
F11 1 1.1097(3) -0.2160(5) 0.2088(2) 0.0401(12) Uani d . F
F12 1 0.9368(2) -0.1786(5) 0.1486(2) 0.0382(11) Uani d . F
F13 1 0.9941(3) -0.3046(5) 0.2227(2) 0.0401(12) Uani d . F
F14 1 1.0523(2) -0.0957(5) 0.1343(2) 0.0358(11) Uani d . F
F15 1 1.0329(4) -0.3314(5) 0.1397(2) 0.056(2) Uani d . F
F16 1 1.0120(3) -0.0678(5) 0.2168(2) 0.0439(12) Uani d . F
P2 1 0.2500 0.2500 0.2500 0.0263(7) Uani d S P
F21 1 0.3198(3) 0.3605(5) 0.2536(2) 0.0389(11) Uani d . F
F22 1 0.2677(3) 0.1955(5) 0.1914(2) 0.0363(11) Uani d . F
F23 1 0.1928(3) 0.3673(5) 0.2196(2) 0.0408(11) Uani d . F
P3 1 0.7500 0.7967(3) 0.0000 0.0233(6) Uani d S P
F31 1 0.7500 0.6278(6) 0.0000 0.044(2) Uani d S F
F32 1 0.7500 0.9682(6) 0.0000 0.041(2) Uani d S F
F33 1 0.7470(4) 0.7962(6) 0.0640(2) 0.060(2) Uani d . F
F34 1 0.8414(3) 0.7965(6) 0.0133(3) 0.058(2) Uani d . F
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni S4 . . 84.4(2) yes
N1 Ni N7 . . 93.8(2) yes
N1 Ni N11 . . 95.2(2) yes
N1 Ni S41 . . 177.0(2) yes
N1 Ni N71 . . 94.2(2) yes
S4 Ni N7 . . 82.2(2) yes
S4 Ni N11 . . 175.6(2) yes
S4 Ni S41 . . 96.04(8) yes
S4 Ni N71 . . 90.3(2) yes
N7 Ni N11 . . 93.4(2) yes
N7 Ni S41 . . 89.2(2) yes
N7 Ni N71 . . 168.5(2) yes
N11 Ni S41 . . 84.6(2) yes
N11 Ni N71 . . 94.1(2) yes
S41 Ni N71 . . 82.8(2) yes
C2 N1 Ni . . 113.1(4) ?
N1 C2 C3 . . 110.3(5) ?
C2 C3 S4 . . 113.0(5) ?
C3 S4 C5 . . 99.9(4) ?
C3 S4 Ni . . 96.1(2) ?
C5 S4 Ni . . 98.5(3) ?
C6 C5 S4 . . 111.0(5) ?
N7 C6 C5 . . 112.7(6) ?
C6 N7 Ni . . 112.8(4) ?
C21 N11 Ni . . 113.8(4) ?
N11 C21 C31 . . 109.7(6) ?
C21 C31 S41 . . 112.7(5) ?
C51 S41 C31 . . 102.9(4) ?
C51 S41 Ni . . 97.7(2) ?
C31 S41 Ni . . 94.4(2) ?
C61 C51 S41 . . 110.7(5) ?
N71 C61 C51 . . 110.5(6) ?
C61 N71 Ni . . 110.9(4) ?
F15 P1 F12 . . 90.6(3) ?
F15 P1 F11 . . 91.5(3) ?
F12 P1 F11 . . 177.7(3) ?
F15 P1 F16 . . 179.1(3) ?
F12 P1 F16 . . 88.5(3) ?
F11 P1 F16 . . 89.4(3) ?
F15 P1 F14 . . 90.2(3) ?
F12 P1 F14 . . 89.6(2) ?
F11 P1 F14 . . 89.6(2) ?
F16 P1 F14 . . 89.7(3) ?
F15 P1 F13 . . 90.2(3) ?
F12 P1 F13 . . 90.5(3) ?
F11 P1 F13 . . 90.3(3) ?
F16 P1 F13 . . 89.8(3) ?
F14 P1 F13 . . 179.6(3) ?
F23 P2 F23 . 7 180.0000(10) ?
F23 P2 F21 . 7 90.3(3) ?
F23 P2 F21 7 7 89.7(3) ?
F23 P2 F21 . . 89.7(3) ?
F23 P2 F21 7 . 90.3(3) ?
F21 P2 F21 7 . 180.0 ?
F23 P2 F22 . . 90.0(2) ?
F23 P2 F22 7 . 90.0(2) ?
F21 P2 F22 7 . 89.6(2) ?
F21 P2 F22 . . 90.4(2) ?
F23 P2 F22 . 7 90.0(2) ?
F23 P2 F22 7 7 90.0(2) ?
F21 P2 F22 7 7 90.4(2) ?
F21 P2 F22 . 7 89.6(2) ?
F22 P2 F22 . 7 180.0 ?
F33 P3 F33 2_655 . 179.6(5) ?
F33 P3 F34 2_655 2_655 89.0(4) ?
F33 P3 F34 . 2_655 91.0(4) ?
F33 P3 F34 2_655 . 91.0(4) ?
F33 P3 F34 . . 89.0(4) ?
F34 P3 F34 2_655 . 179.9(4) ?
F33 P3 F31 2_655 . 89.8(2) ?
F33 P3 F31 . . 89.8(2) ?
F34 P3 F31 2_655 . 89.9(2) ?
F34 P3 F31 . . 89.9(2) ?
F33 P3 F32 2_655 . 90.2(2) ?
F33 P3 F32 . . 90.2(2) ?
F34 P3 F32 2_655 . 90.1(2) ?
F34 P3 F32 . . 90.1(2) ?
F31 P3 F32 . . 180.0000(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N1 . 2.115(6) yes
Ni S4 . 2.462(2) yes
Ni N7 . 2.141(5) yes
Ni N11 . 2.102(5) yes
Ni S41 . 2.467(3) yes
Ni N71 . 2.126(5) yes
N1 C2 . 1.482(9) yes
C2 C3 . 1.529(9) yes
C3 S4 . 1.809(7) yes
S4 C5 . 1.841(8) yes
C5 C6 . 1.509(10) yes
C6 N7 . 1.455(9) yes
N11 C21 . 1.482(8) yes
C21 C31 . 1.495(10) yes
C31 S41 . 1.836(8) yes
S41 C51 . 1.820(7) yes
C51 C61 . 1.518(9) yes
C61 N71 . 1.480(9) yes
P1 F15 . 1.584(5) ?
P1 F12 . 1.594(4) ?
P1 F11 . 1.595(5) ?
P1 F16 . 1.602(5) ?
P1 F14 . 1.606(5) ?
P1 F13 . 1.610(5) ?
P2 F23 . 1.601(4) ?
P2 F23 7 1.601(4) ?
P2 F21 7 1.603(4) ?
P2 F21 . 1.603(4) ?
P2 F22 . 1.604(5) ?
P2 F22 7 1.604(5) ?
P3 F33 2_655 1.580(5) ?
P3 F33 . 1.580(5) ?
P3 F34 2_655 1.589(5) ?
P3 F34 . 1.589(5) ?
P3 F31 . 1.597(6) ?
P3 F32 . 1.621(6) ?
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
_geom_torsion_publ_flag
N1 C2 C3 S4 -53.6(7) yes
C2 C3 S4 C5 -69.7(5) yes
C3 S4 C5 C6 120.0(6) yes
S4 C5 C6 N7 -49.8(8) yes
N11 C21 C31 S41 -56.7(6) yes
C21 C31 S41 C51 -64.3(5) yes
C31 S41 C51 C61 122.1(6) yes
S41 C51 C61 N71 -54.9(7) yes
