#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/20/2202073.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_2202073
loop_
_publ_author_name
'Mohamed, Ajax K.'
'Auner, Norbert'
'Bolte, Michael'
_publ_section_title
;
 Tris(N,N-diethyldithiocarbamato-κ²S,S')nickel(II)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m188
_journal_page_last               m189
_journal_paper_doi               10.1107/S1600536803006044
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C5 H10 N1 S2)3]'
_chemical_formula_moiety         'C15 H30 N3 Ni S6'
_chemical_formula_sum            'C15 H30 N3 Ni S6'
_chemical_formula_weight         503.49
_chemical_name_systematic
;
Tris(N,N-diethyldithiocarbamato-κ²S,S')nickel(II)
;
_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                 109.630(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0208(9)
_cell_length_b                   10.2305(7)
_cell_length_c                   16.9031(11)
_cell_measurement_reflns_used    15127
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      3.7
_cell_volume                     2283.7(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe IPDS-II two-circle'
_diffrn_measurement_method       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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16440
_diffrn_reflns_theta_full        29.73
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         3.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.403
_exptl_absorpt_correction_T_max  0.8724
_exptl_absorpt_correction_T_min  0.7666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 1990; Blessing, 1995)'
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.804
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0409P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                2635
_reflns_number_total             3232
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na6214.cif
_cod_data_source_block           I
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202073
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, y+1, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, -y, z-1/2'
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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 0.5000 0.25100(2) 0.7500 0.02044(7) Uani d S 1 . . Ni
C1 0.5000 -0.01879(19) 0.7500 0.0230(4) Uani d S 1 . . C
C2 0.40977(15) -0.22287(16) 0.74875(11) 0.0387(4) Uani d . 1 . . C
H2A 0.4056 -0.3036 0.7154 0.046 Uiso calc R 1 . . H
H2B 0.3487 -0.1699 0.7204 0.046 Uiso calc R 1 . . H
C3 0.4101(2) -0.2595(2) 0.83540(14) 0.0556(6) Uani d . 1 . . C
H3A 0.3482 -0.3083 0.8307 0.083 Uiso calc R 1 . . H
H3B 0.4128 -0.1800 0.8684 0.083 Uiso calc R 1 . . H
H3C 0.4693 -0.3140 0.8633 0.083 Uiso calc R 1 . . H
C4 0.35964(10) 0.38592(13) 0.62047(8) 0.0201(2) Uani d . 1 . . C
C5 0.29340(12) 0.43897(15) 0.47172(8) 0.0272(3) Uani d . 1 . . C
H5A 0.2229 0.4316 0.4326 0.033 Uiso calc R 1 . . H
H5B 0.3299 0.3582 0.4667 0.033 Uiso calc R 1 . . H
C6 0.22847(12) 0.55200(16) 0.57631(10) 0.0329(3) Uani d . 1 . . C
H6A 0.2637 0.6371 0.5816 0.040 Uiso calc R 1 . . H
H6B 0.2203 0.5325 0.6310 0.040 Uiso calc R 1 . . H
C7 0.34366(16) 0.5549(2) 0.44681(12) 0.0429(4) Uani d . 1 . . C
H7A 0.3419 0.5440 0.3887 0.064 Uiso calc R 1 . . H
H7B 0.4142 0.5608 0.4842 0.064 Uiso calc R 1 . . H
H7C 0.3075 0.6350 0.4514 0.064 Uiso calc R 1 . . H
C8 0.12560(12) 0.5640(2) 0.51083(13) 0.0439(4) Uani d . 1 . . C
H8A 0.0874 0.6331 0.5271 0.066 Uiso calc R 1 . . H
H8B 0.0894 0.4808 0.5059 0.066 Uiso calc R 1 . . H
H8C 0.1328 0.5861 0.4567 0.066 Uiso calc R 1 . . H
N1 0.5000 -0.14880(17) 0.7500 0.0293(4) Uani d S 1 . . N
N2 0.29225(9) 0.45005(12) 0.55808(7) 0.0245(2) Uani d . 1 . . N
S1 0.37317(3) 0.39993(3) 0.72495(2) 0.02400(8) Uani d . 1 . . S
S2 0.39946(2) 0.07687(3) 0.75000(2) 0.02308(8) Uani d . 1 . . S
S3 0.44642(2) 0.27616(3) 0.608522(19) 0.02077(8) Uani d . 1 . . S
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'
Ni Ni 0.3393 1.1124 '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'
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
S3 Ni1 S3 4_546 . 166.97(2)
S3 Ni1 S1 4_546 . 94.687(13)
S3 Ni1 S1 . . 76.466(12)
S3 Ni1 S1 4_546 4_546 76.466(13)
S3 Ni1 S1 . 4_546 94.687(13)
S1 Ni1 S1 . 4_546 95.72(2)
S3 Ni1 S2 4_546 . 94.285(13)
S3 Ni1 S2 . . 95.929(13)
S1 Ni1 S2 . . 94.538(14)
S1 Ni1 S2 4_546 . 166.699(14)
S3 Ni1 S2 4_546 4_546 95.931(13)
S3 Ni1 S2 . 4_546 94.283(13)
S1 Ni1 S2 . 4_546 166.698(14)
S1 Ni1 S2 4_546 4_546 94.536(14)
S2 Ni1 S2 . 4_546 76.71(2)
N1 C1 S2 . . 124.77(5)
N1 C1 S2 . 4_546 124.77(5)
S2 C1 S2 . 4_546 110.46(11)
N1 C2 C3 . . 113.11(15)
N1 C2 H2A . . 109.0
C3 C2 H2A . . 109.0
N1 C2 H2B . . 109.0
C3 C2 H2B . . 109.0
H2A C2 H2B . . 107.8
C2 C3 H3A . . 109.5
C2 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
C2 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
N2 C4 S3 . . 124.94(10)
N2 C4 S1 . . 125.32(10)
S3 C4 S1 . . 109.74(7)
N2 C5 C7 . . 112.23(13)
N2 C5 H5A . . 109.2
C7 C5 H5A . . 109.2
N2 C5 H5B . . 109.2
C7 C5 H5B . . 109.2
H5A C5 H5B . . 107.9
N2 C6 C8 . . 113.89(14)
N2 C6 H6A . . 108.8
C8 C6 H6A . . 108.8
N2 C6 H6B . . 108.8
C8 C6 H6B . . 108.8
H6A C6 H6B . . 107.7
C5 C7 H7A . . 109.5
C5 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
C5 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
C6 C8 H8A . . 109.5
C6 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C6 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
C1 N1 C2 . . 121.06(10)
C1 N1 C2 . 4_546 121.06(10)
C2 N1 C2 . 4_546 117.9(2)
C4 N2 C5 . . 120.53(12)
C4 N2 C6 . . 120.24(11)
C5 N2 C6 . . 118.20(11)
C4 S1 Ni1 . . 86.83(5)
C1 S2 Ni1 . . 86.42(5)
C4 S3 Ni1 . . 86.96(4)
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 S3 4_546 2.2676(3) ?
Ni1 S3 . 2.2677(4) y
Ni1 S1 . 2.2709(4) y
Ni1 S1 4_546 2.2709(4) ?
Ni1 S2 . 2.2717(4) y
Ni1 S2 4_546 2.2717(4) ?
C1 N1 . 1.330(2) ?
C1 S2 . 1.7161(11) y
C1 S2 4_546 1.7161(11) ?
C2 N1 . 1.469(2) ?
C2 C3 . 1.510(3) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 N2 . 1.3289(17) ?
C4 S3 . 1.7166(13) y
C4 S1 . 1.7178(13) y
C5 N2 . 1.4696(18) ?
C5 C7 . 1.510(2) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 N2 . 1.4723(19) ?
C6 C8 . 1.499(2) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 H8A . 0.9800 ?
C8 H8B . 0.9800 ?
C8 H8C . 0.9800 ?
N1 C2 4_546 1.469(2) ?
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_4
_geom_torsion
S2 C1 N1 C2 . . 0.91(8)
S2 C1 N1 C2 4_546 . -179.09(8)
S2 C1 N1 C2 . 4_546 -179.10(8)
S2 C1 N1 C2 4_546 4_546 0.91(8)
C3 C2 N1 C1 . . -93.33(17)
C3 C2 N1 C2 . 4_546 86.67(17)
S3 C4 N2 C5 . . -5.43(19)
S1 C4 N2 C5 . . 174.64(11)
S3 C4 N2 C6 . . -173.66(12)
S1 C4 N2 C6 . . 6.4(2)
C7 C5 N2 C4 . . -100.31(17)
C7 C5 N2 C6 . . 68.15(19)
C8 C6 N2 C4 . . -148.52(16)
C8 C6 N2 C5 . . 43.0(2)
N2 C4 S1 Ni1 . . 179.76(12)
S3 C4 S1 Ni1 . . -0.18(6)
S3 Ni1 S1 C4 4_546 . 170.43(5)
S3 Ni1 S1 C4 . . 0.13(5)
S1 Ni1 S1 C4 4_546 . 93.59(5)
S2 Ni1 S1 C4 . . -94.89(5)
S2 Ni1 S1 C4 4_546 . -46.69(8)
N1 C1 S2 Ni1 . . 180.0
S2 C1 S2 Ni1 4_546 . -0.0020(10)
S3 Ni1 S2 C1 4_546 . -95.091(15)
S3 Ni1 S2 C1 . . 93.018(14)
S1 Ni1 S2 C1 . . 169.852(13)
S1 Ni1 S2 C1 4_546 . -49.76(6)
S2 Ni1 S2 C1 4_546 . 0.0
N2 C4 S3 Ni1 . . -179.76(12)
S1 C4 S3 Ni1 . . 0.18(6)
S3 Ni1 S3 C4 4_546 . -48.29(5)
S1 Ni1 S3 C4 . . -0.13(5)
S1 Ni1 S3 C4 4_546 . -94.90(5)
S2 Ni1 S3 C4 . . 93.12(5)
S2 Ni1 S3 C4 4_546 . 170.18(5)
