#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/46/2004607.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_2004607
loop_
_publ_author_name
'Kruger, P. E.'
'McKee, V.'
_publ_section_title
;
 Tetrakis(triethylammonium) Hexakis(isothiocyanato-N)nickel(II)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              617
_journal_page_last               619
_journal_paper_doi               10.1107/S0108270195013837
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(C6 H16 N1)4[Ni1 (N1 C1 S1)6]'
_chemical_formula_structural     '(C2 H5)3 N H)4 (Ni (N C S)6)'
_chemical_formula_sum            'C30 H64 N10 Ni S6'
_chemical_formula_weight         815.98
_chemical_name_systematic
;
Tetrakis(triethylammonium) hexakis(isothiocyanato)-nickel(II)
;
_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_method           SHELXL
_cell_angle_alpha                93.64
_cell_angle_beta                 93.23
_cell_angle_gamma                95.23
_cell_formula_units_Z            2
_cell_length_a                   12.575(2)
_cell_length_b                   13.4200(10)
_cell_length_c                   13.530(2)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8
_cell_volume                     2264.7(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990a)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990b)'
_diffrn_ambient_temperature      566(2)
_diffrn_measurement_device       'Siemens P4 four-circle'
_diffrn_measurement_method       '1.2° ω'
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7301
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   '\y scans (SHELXTL/PC; Sheldrick, 1990a)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.438
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_hydrogen_treatment
'H atoms riding, with N---H 0.91 and C---H 0.96--0.97\%A'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.047
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_obs          0.0552
_refine_ls_shift/esd_max         0.132
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0689P)^2^ + 2.8778P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1638
_refine_ls_wR_factor_obs         0.1355
_reflns_number_observed          4906
_reflns_number_total             6905
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1110.cif
_cod_data_source_block           pk167f
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2004607
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ni1 1 0 .5 0 .0488(2) Uani d S Ni
N11 1 .1649(3) .5140(3) .0293(3) .0640(10) Uani d . N
C11 1 .2538(4) .5188(4) .0502(3) .0644(12) Uani d . C
S11 1 .38257(12) .5276(2) .08151(14) .1144(7) Uani d . S
N12 1 -.0215(3) .4633(3) .1451(3) .0646(10) Uani d . N
C12 1 -.0368(4) .4240(3) .2160(3) .0599(11) Uani d . C
S12 1 -.06046(15) .36590(12) .31691(10) .0954(5) Uani d . S
N13 1 -.0041(3) .6524(3) .0433(3) .0655(10) Uani d . N
C13 1 -.0155(4) .7345(4) .0636(3) .0571(11) Uani d . C
S13 1 -.03591(13) .85189(10) .09447(11) .0826(4) Uani d . S
Ni2 1 .5 0 -0.5 .0588(2) Uani d S Ni
N21 1 .4868(4) .0339(3) -0.3491(3) .0755(12) Uani d . N
C21 1 .4738(4) .0533(4) -0.2686(4) .0666(12) Uani d . C
S21 1 .4575(2) .0817(2) -0.15210(12) .1125(6) Uani d . S
N22 1 .4365(3) .1339(3) -0.5318(3) .0756(12) Uani d . N
C22 1 .3941(4) .2009(3) -0.5529(3) .0585(11) Uani d . C
S22 1 .33085(13) .29737(10) -0.58343(11) .0873(5) Uani d . S
N23 1 .3470(3) -.0733(3) -0.5104(3) .0714(11) Uani d . N
C23 1 .2636(5) -0.1139(4) -0.5049(3) .0645(12) Uani d . C
S23 1 .14525(14) -0.17358(13) -0.49527(14) .1045(6) Uani d . S
N4 1 .2190(3) .1352(3) .2411(3) .0699(11) Uani d . N
H4 1 .2493(3) .1780(3) .2919(3) .084 Uiso calc R H
C41 1 .3094(5) .0995(5) .1882(5) .103(2) Uani d . C
H41A 1 .3487(5) .0586(5) .2312(5) .123 Uiso calc R H
H41B 1 .3575(5) .1569(5) .1745(5) .123 Uiso calc R H
C42 1 .2757(6) .0388(6) .0917(5) .125(3) Uani d . C
H42A 1 .3356(13) .007(4) .068(2) .188 Uiso calc R H
H42B 1 .251(4) .0823(9) .0434(13) .188 Uiso calc R H
H42C 1 .219(3) -.012(3) .1026(10) .188 Uiso calc R H
C43 1 .1624(7) .0484(5) .2900(5) .130(3) Uani d . C
H43A 1 .1189(7) .0064(5) .2392(5) .156 Uiso calc R H
H43B 1 .2161(7) .0083(5) .3169(5) .156 Uiso calc R H
C44 1 .0965(8) .0747(8) .3666(6) .167(4) Uani d . C
H44A 1 .073(5) .0157(13) .399(4) .251 Uiso calc R H
H44B 1 .036(3) .104(6) .3390(10) .251 Uiso calc R H
H44C 1 .136(2) .122(5) .414(3) .251 Uiso calc R H
C45 1 .1494(5) .1946(5) .1826(4) .097(2) Uani d . C
H45A 1 .1142(5) .1522(5) .1274(4) .116 Uiso calc R H
H45B 1 .0944(5) .2171(5) .2239(4) .116 Uiso calc R H
C46 1 .2076(7) .2822(5) .1440(5) .137(3) Uani d . C
H46A 1 .1574(7) .324(2) .116(4) .205 Uiso calc R H
H46B 1 .253(4) .2603(5) .094(3) .205 Uiso calc R H
H46C 1 .250(4) .320(3) .1972(10) .205 Uiso calc R H
N5 1 .1754(3) .2651(3) .7387(3) .0720(11) Uani d . N
H5 1 .1499(3) .2281(3) .7879(3) .086 Uiso calc R H
C51 1 .2416(6) .3575(5) .7907(6) .119(2) Uani d . C
H51A 1 .2801(6) .3932(5) .7415(6) .142 Uiso calc R H
H51B 1 .1933(6) .4021(5) .8194(6) .142 Uiso calc R H
C52 1 .3160(7) .3338(7) .8665(6) .147(3) Uani d . C
H52A 1 .348(4) .3946(7) .901(3) .220 Uiso calc R H
H52B 1 .370(3) .298(5) .8374(7) .220 Uiso calc R H
H52C 1 .2795(12) .293(4) .912(3) .220 Uiso calc R H
C53 1 .2412(5) .1999(5) .6805(5) .098(2) Uani d . C
H53A 1 .3045(5) .1880(5) .7208(5) .118 Uiso calc R H
H53B 1 .2644(5) .2335(5) .6230(5) .118 Uiso calc R H
C54 1 .1800(7) .1021(6) .6473(5) .134(3) Uani d . C
H54A 1 .161(4) .067(2) .7043(6) .202 Uiso calc R H
H54B 1 .2232(19) .0628(19) .607(4) .202 Uiso calc R H
H54C 1 .116(3) .1139(6) .610(4) .202 Uiso calc R H
C55 1 .0776(5) .2995(5) .6832(4) .091(2) Uani d . C
H55A 1 .0277(5) .2411(5) .6638(4) .109 Uiso calc R H
H55B 1 .0425(5) .3430(5) .7284(4) .109 Uiso calc R H
C56 1 .1003(6) .3532(6) .5940(5) .118(2) Uani d . C
H56A 1 .0346(7) .371(4) .563(2) .177 Uiso calc R H
H56B 1 .134(4) .3107(15) .5481(17) .177 Uiso calc R H
H56C 1 .147(3) .413(2) .6124(7) .177 Uiso calc R H
N6 1 .3012(4) -0.3704(4) -0.7129(4) .0953(15) Uani d . N
H6 1 .3326(4) -0.3900(4) -0.7689(4) .114 Uiso calc R H
C61 1 .2202(8) -0.2974(7) -0.7448(6) .148(3) Uani d . C
H61A 1 .1591(8) -0.3368(7) -0.7792(6) .177 Uiso calc R H
H61B 1 .1952(8) -0.2659(7) -0.6850(6) .177 Uiso calc R H
C62 1 .2523(7) -0.2242(6) -0.8029(6) .142(3) Uani d . C
H62A 1 .312(3) -0.183(3) -0.770(2) .213 Uiso calc R H
H62B 1 .1944(17) -0.184(3) -0.816(4) .213 Uiso calc R H
H62C 1 .274(5) -0.2534(6) -0.864(2) .213 Uiso calc R H
C63 1 .2412(6) -0.4611(5) -0.6813(5) .110(2) Uani d . C
H63A 1 .1816(6) -0.4794(5) -0.7296(5) .132 Uiso calc R H
H63B 1 .2877(6) -0.5149(5) -0.6850(5) .132 Uiso calc R H
C64 1 .1993(7) -0.4583(6) -0.5842(6) .137(3) Uani d . C
H64A 1 .154(4) -0.519(2) -0.5775(18) .205 Uiso calc R H
H64B 1 .158(4) -0.402(3) -0.5761(19) .205 Uiso calc R H
H64C 1 .2574(7) -0.452(5) -0.5344(6) .205 Uiso calc R H
C65 1 .3875(7) -0.3266(6) -0.6434(7) .142(3) Uani d . C
H65A 1 .3602(7) -0.3128(6) -0.5788(7) .170 Uiso calc R H
H65B 1 .4181(7) -0.2638(6) -0.6662(7) .170 Uiso calc R H
C66 1 .4719(6) -0.3983(7) -0.6353(6) .147(3) Uani d . C
H66A 1 .449(3) -0.450(3) -0.593(4) .221 Uiso calc R H
H66B 1 .5377(15) -0.3629(12) -0.608(5) .221 Uiso calc R H
H66C 1 .483(4) -0.428(4) -0.7000(8) .221 Uiso calc R H
N7 1 .7190(4) .2454(4) .2120(4) .0874(13) Uani d . N
H7 1 .7788(4) .2837(4) .2377(4) .105 Uiso calc R H
C71 1 .6859(7) .2927(6) .1239(5) .135(3) Uani d . C
H71A 1 .7420(7) .2913(6) .0775(5) .162 Uiso calc R H
H71B 1 .6766(7) .3624(6) .1416(5) .162 Uiso calc R H
C72 1 .5800(9) .2408(9) .0721(7) .210(5) Uani d . C
H72A 1 .575(4) .257(7) .004(2) .315 Uiso calc R H
H72B 1 .5204(9) .264(6) .105(5) .315 Uiso calc R H
H72C 1 .579(4) .1695(10) .076(7) .315 Uiso calc R H
C73 1 .6387(6) .2496(8) .2937(6) .137(3) Uani d . C
H73A 1 .5719(6) .2109(8) .2711(6) .164 Uiso calc R H
H73B 1 .6672(6) .2211(8) .3526(6) .164 Uiso calc R H
C74 1 .6191(9) .3591(10) .3182(8) .201(5) Uani d . C
H74A 1 .576(7) .3631(13) .374(5) .302 Uiso calc R H
H74B 1 .583(7) .384(3) .262(3) .302 Uiso calc R H
H74C 1 .6863(10) .3983(17) .334(7) .302 Uiso calc R H
C75 1 .7507(9) .1403(7) .2028(8) .167(4) Uani d . C
H75A 1 .7747(9) .1216(7) .2679(8) .200 Uiso calc R H
H75B 1 .6885(9) .0951(7) .1797(8) .200 Uiso calc R H
C76 1 .8374(7) .1280(8) .1333(7) .172(4) Uani d . C
H76A 1 .851(5) .0587(12) .126(5) .258 Uiso calc R H
H76B 1 .902(2) .168(5) .159(3) .258 Uiso calc R H
H76C 1 .816(3) .150(6) .070(2) .258 Uiso calc R H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 Ni1 N11 . 2_565 180.0 ?
N11 Ni1 N12 . . 90.1(2) y
N11 Ni1 N12 2_565 . 89.9(2) ?
N11 Ni1 N12 . 2_565 89.9(2) ?
N11 Ni1 N12 2_565 2_565 90.1(2) ?
N12 Ni1 N12 . 2_565 180.0 ?
N11 Ni1 N13 . . 90.0(2) y
N11 Ni1 N13 2_565 . 90.0(2) ?
N12 Ni1 N13 . . 90.25(15) y
N12 Ni1 N13 2_565 . 89.75(15) ?
N11 Ni1 N13 . 2_565 90.0(2) ?
N11 Ni1 N13 2_565 2_565 90.0(2) ?
N12 Ni1 N13 . 2_565 89.75(15) ?
N12 Ni1 N13 2_565 2_565 90.25(15) ?
N13 Ni1 N13 . 2_565 180.0 ?
C11 N11 Ni1 . . 176.1(4) ?
N11 C11 S11 . . 179.0(4) ?
C12 N12 Ni1 . . 166.2(4) ?
N12 C12 S12 . . 178.9(5) ?
C13 N13 Ni1 . . 173.9(4) ?
N13 C13 S13 . . 178.0(4) ?
N23 Ni2 N23 2_654 . 180.0 ?
N23 Ni2 N21 2_654 2_654 90.0(2) ?
N23 Ni2 N21 . 2_654 90.0(2) ?
N23 Ni2 N21 2_654 . 90.0(2) ?
N23 Ni2 N21 . . 90.0(2) y
N21 Ni2 N21 2_654 . 180.0 ?
N23 Ni2 N22 2_654 . 90.1(2) ?
N23 Ni2 N22 . . 89.9(2) y
N21 Ni2 N22 2_654 . 90.0(2) ?
N21 Ni2 N22 . . 90.0(2) y
N23 Ni2 N22 2_654 2_654 89.9(2) ?
N23 Ni2 N22 . 2_654 90.1(2) ?
N21 Ni2 N22 2_654 2_654 90.0(2) ?
N21 Ni2 N22 . 2_654 90.0(2) ?
N22 Ni2 N22 . 2_654 180.0 ?
C21 N21 Ni2 . . 176.1(4) ?
N21 C21 S21 . . 179.0(5) ?
C22 N22 Ni2 . . 173.6(4) ?
N22 C22 S22 . . 179.2(5) ?
C23 N23 Ni2 . . 172.4(4) ?
N23 C23 S23 . . 178.7(5) ?
C45 N4 C41 . . 114.7(4) ?
C45 N4 C43 . . 115.6(5) ?
C41 N4 C43 . . 109.2(5) ?
N4 C41 C42 . . 113.7(5) ?
C44 C43 N4 . . 115.9(7) ?
C46 C45 N4 . . 113.0(5) ?
C53 N5 C55 . . 116.3(4) ?
C53 N5 C51 . . 112.6(5) ?
C55 N5 C51 . . 108.7(5) ?
C52 C51 N5 . . 113.5(6) ?
N5 C53 C54 . . 111.2(6) ?
C56 C55 N5 . . 115.1(5) ?
C65 N6 C63 . . 114.9(6) ?
C65 N6 C61 . . 114.9(6) ?
C63 N6 C61 . . 108.2(6) ?
C62 C61 N6 . . 118.5(8) ?
C64 C63 N6 . . 118.9(6) ?
N6 C65 C66 . . 109.2(6) ?
C71 N7 C75 . . 119.5(6) ?
C71 N7 C73 . . 113.4(6) ?
C75 N7 C73 . . 107.2(7) ?
N7 C71 C72 . . 112.7(6) ?
C74 C73 N7 . . 108.9(6) ?
C76 C75 N7 . . 112.9(8) ?
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
Ni1 N11 . 2.078(4) y
Ni1 N11 2_565 2.078(4) ?
Ni1 N12 . 2.080(4) y
Ni1 N12 2_565 2.080(4) ?
Ni1 N13 . 2.097(4) y
Ni1 N13 2_565 2.097(4) ?
N11 C11 . 1.133(6) ?
C11 S11 . 1.642(6) ?
N12 C12 . 1.142(5) ?
C12 S12 . 1.643(5) ?
N13 C13 . 1.142(5) ?
C13 S13 . 1.651(5) ?
Ni2 N23 2_654 2.072(4) ?
Ni2 N23 . 2.072(4) y
Ni2 N21 2_654 2.083(5) ?
Ni2 N21 . 2.083(5) y
Ni2 N22 . 2.091(4) y
Ni2 N22 2_654 2.091(4) ?
N21 C21 . 1.127(6) ?
C21 S21 . 1.627(6) ?
N22 C22 . 1.131(5) ?
C22 S22 . 1.642(5) ?
N23 C23 . 1.146(6) ?
C23 S23 . 1.640(6) ?
N4 C45 . 1.468(7) ?
N4 C41 . 1.477(7) ?
N4 C43 . 1.518(8) ?
C41 C42 . 1.512(8) ?
C43 C44 . 1.411(10) ?
C45 C46 . 1.467(9) ?
N5 C53 . 1.479(6) ?
N5 C55 . 1.529(7) ?
N5 C51 . 1.537(7) ?
C51 C52 . 1.420(10) ?
C53 C54 . 1.489(9) ?
C55 C56 . 1.473(8) ?
N6 C65 . 1.452(8) ?
N6 C63 . 1.472(8) ?
N6 C61 . 1.539(8) ?
C61 C62 . 1.345(10) ?
C63 C64 . 1.442(9) ?
C65 C66 . 1.500(10) ?
N7 C71 . 1.444(8) ?
N7 C75 . 1.500(10) ?
N7 C73 . 1.541(9) ?
C71 C72 . 1.554(11) ?
C73 C74 . 1.530(12) ?
C75 C76 . 1.494(12) ?
