#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:36:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179148 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/09/4310913.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_4310913
loop_
_publ_author_name
'Craig A. Grapperhaus'
'Christopher S. Mullins'
'Pawel M. Kozlowski'
'Mark S. Mashuta'
_publ_contact_author_address
' Department of Chemistry, University of Louisville, Louisville, KY 40292, USA'
_publ_contact_author_email       craig.grapperhaus@louisville.edu
_publ_contact_author_fax         502-852-8149
_publ_contact_author_name        'Grapperhaus, Craig A.'
_publ_contact_author_phone       502-852-5932
_publ_section_title
;
 Synthesis and Oxygenation of a Nickel(II) and Zinc(II) Dithiolate: An
 Experimental and Theoretical Comparison
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2859
_journal_page_last               2866
_journal_paper_doi               10.1021/ic035205y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C12 H26 N2 Ni S2'
_chemical_formula_sum            'C12 H26 N2 Ni S2'
_chemical_formula_weight         321.18
_chemical_name_common            '[(bmmp-TASN)Ni]'
_chemical_name_systematic
; 
 [(bmmp-TASN)Ni] 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'November 25, 2001'
_audit_creation_method           SHELXL-97
_audit_update_record
;
  December_21_2001 text and data added by Mark S. Mashuta
  Oct_6_2003 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.562(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1621(10)
_cell_length_b                   20.7343(10)
_cell_length_c                   12.3340(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      15.0
_cell_volume                     1558.3(3)
_computing_cell_refinement       'Enraf-Nonius Diffractometer Control'
_computing_data_collection       'Enraf-Nonius Diffractometer Control'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'data from ω/2θ_scans'
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_source         'normal focus Philips Mo tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2873
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        'not applied (less than 0.5)'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0069(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0487
_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)+(0.0797P)²+1.1806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                2395
_reflns_number_total             2742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035205ysi20031021_120352_1.cif
_cod_data_source_block           1
_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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4310913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.64334(7) 0.223246(19) 0.92195(3) 0.0323(2) Uani 1 1 d . . .
S1 S 0.68408(19) 0.30984(4) 0.83155(8) 0.0484(3) Uani 1 1 d . . .
N1 N 0.5333(5) 0.27368(13) 1.0335(2) 0.0365(7) Uani 1 1 d . . .
C1 C 0.6369(6) 0.37275(17) 0.9318(3) 0.0407(8) Uani 1 1 d . . .
S2 S 0.7031(2) 0.15844(5) 0.79238(9) 0.0623(4) Uani 1 1 d . . .
N2 N 0.6548(5) 0.14925(14) 1.0202(2) 0.0363(6) Uani 1 1 d . . .
C2 C 0.6261(6) 0.33957(17) 1.0422(3) 0.0441(9) Uani 1 1 d . . .
H2A H 0.7732 0.3376 1.0830 0.053 Uiso 1 1 calc R . .
H2B H 0.5382 0.3660 1.0839 0.053 Uiso 1 1 calc R . .
C3 C 0.5852(7) 0.23851(19) 1.1384(3) 0.0476(9) Uani 1 1 d . . .
H3A H 0.4935 0.2539 1.1904 0.057 Uiso 1 1 calc R . .
H3B H 0.7376 0.2452 1.1694 0.057 Uiso 1 1 calc R . .
C4 C 0.5425(7) 0.16717(18) 1.1149(3) 0.0441(9) Uani 1 1 d . . .
H4A H 0.5996 0.1416 1.1786 0.053 Uiso 1 1 calc R . .
H4B H 0.3861 0.1593 1.0973 0.053 Uiso 1 1 calc R . .
C5 C 0.5470(7) 0.09357(17) 0.9594(3) 0.0443(9) Uani 1 1 d . . .
H5A H 0.3896 0.1006 0.9481 0.053 Uiso 1 1 calc R . .
H5B H 0.5761 0.0552 1.0043 0.053 Uiso 1 1 calc R . .
C6 C 0.6209(7) 0.08100(17) 0.8474(3) 0.0463(9) Uani 1 1 d . . .
C7 C 0.4369(7) 0.4130(2) 0.8876(4) 0.0579(11) Uani 1 1 d . . .
H7A H 0.4139 0.4453 0.9405 0.087 Uiso 1 1 calc R . .
H7B H 0.3102 0.3857 0.8739 0.087 Uiso 1 1 calc R . .
H7C H 0.4605 0.4335 0.8205 0.087 Uiso 1 1 calc R . .
C8 C 0.8337(7) 0.41860(19) 0.9476(4) 0.0585(11) Uani 1 1 d . . .
H8A H 0.8108 0.4514 0.9996 0.088 Uiso 1 1 calc R . .
H8B H 0.8494 0.4383 0.8788 0.088 Uiso 1 1 calc R . .
H8C H 0.9644 0.3948 0.9744 0.088 Uiso 1 1 calc R . .
C9 C 0.2883(7) 0.2771(2) 1.0019(4) 0.0539(10) Uani 1 1 d . . .
H9A H 0.2264 0.3019 1.0554 0.081 Uiso 1 1 calc R . .
H9B H 0.2281 0.2344 0.9986 0.081 Uiso 1 1 calc R . .
H9C H 0.2539 0.2973 0.9313 0.081 Uiso 1 1 calc R . .
C10 C 0.8883(6) 0.1344(2) 1.0611(3) 0.0544(10) Uani 1 1 d . . .
H10A H 0.8965 0.0980 1.1097 0.082 Uiso 1 1 calc R . .
H10B H 0.9563 0.1711 1.0998 0.082 Uiso 1 1 calc R . .
H10C H 0.9632 0.1245 1.0002 0.082 Uiso 1 1 calc R . .
C11 C 0.4222(9) 0.0544(2) 0.7713(4) 0.0733(14) Uani 1 1 d . . .
H11A H 0.3783 0.0141 0.7996 0.110 Uiso 1 1 calc R . .
H11B H 0.4605 0.0478 0.6994 0.110 Uiso 1 1 calc R . .
H11C H 0.3031 0.0846 0.7670 0.110 Uiso 1 1 calc R . .
C12 C 0.8059(8) 0.0322(2) 0.8526(4) 0.0682(13) Uani 1 1 d . . .
H12A H 0.7608 -0.0077 0.8817 0.102 Uiso 1 1 calc R . .
H12B H 0.9330 0.0483 0.8991 0.102 Uiso 1 1 calc R . .
H12C H 0.8408 0.0251 0.7802 0.102 Uiso 1 1 calc 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'
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
_geom_angle_publ_flag
N1 Ni N2 88.11(12) . . no
N1 Ni S1 89.87(9) . . no
N2 Ni S1 169.79(9) . . no
N1 Ni S2 168.75(10) . . no
N2 Ni S2 88.63(9) . . no
S1 Ni S2 95.16(4) . . no
C1 S1 Ni 101.57(12) . . no
C3 N1 C2 111.2(3) . . no
C3 N1 C9 109.2(3) . . no
C2 N1 C9 109.7(3) . . no
C3 N1 Ni 107.7(2) . . no
C2 N1 Ni 112.3(2) . . no
C9 N1 Ni 106.6(2) . . no
C7 C1 C8 106.8(3) . . no
C7 C1 C2 115.1(3) . . no
C8 C1 C2 107.6(3) . . no
C7 C1 S1 110.3(3) . . no
C8 C1 S1 108.9(3) . . no
C2 C1 S1 108.0(2) . . no
C6 S2 Ni 100.54(12) . . no
C5 N2 C10 110.5(3) . . no
C5 N2 C4 111.5(3) . . no
C10 N2 C4 109.0(3) . . no
C5 N2 Ni 109.1(2) . . no
C10 N2 Ni 108.5(2) . . no
C4 N2 Ni 108.2(2) . . no
N1 C2 C1 114.7(3) . . no
N1 C2 H2A 108.6 . . no
C1 C2 H2A 108.6 . . no
N1 C2 H2B 108.6 . . no
C1 C2 H2B 108.6 . . no
H2A C2 H2B 107.6 . . no
N1 C3 C4 107.7(3) . . no
N1 C3 H3A 110.2 . . no
C4 C3 H3A 110.2 . . no
N1 C3 H3B 110.2 . . no
C4 C3 H3B 110.2 . . no
H3A C3 H3B 108.5 . . no
N2 C4 C3 107.7(3) . . no
N2 C4 H4A 110.2 . . no
C3 C4 H4A 110.2 . . no
N2 C4 H4B 110.2 . . no
C3 C4 H4B 110.2 . . no
H4A C4 H4B 108.5 . . no
N2 C5 C6 114.6(3) . . no
N2 C5 H5A 108.6 . . no
C6 C5 H5A 108.6 . . no
N2 C5 H5B 108.6 . . no
C6 C5 H5B 108.6 . . no
H5A C5 H5B 107.6 . . no
C12 C6 C11 108.2(4) . . no
C12 C6 C5 113.3(3) . . no
C11 C6 C5 107.2(4) . . no
C12 C6 S2 110.5(3) . . no
C11 C6 S2 109.1(3) . . no
C5 C6 S2 108.5(2) . . no
C1 C7 H7A 109.5 . . no
C1 C7 H7B 109.5 . . no
H7A C7 H7B 109.5 . . no
C1 C7 H7C 109.5 . . no
H7A C7 H7C 109.5 . . no
H7B C7 H7C 109.5 . . no
C1 C8 H8A 109.5 . . no
C1 C8 H8B 109.5 . . no
H8A C8 H8B 109.5 . . no
C1 C8 H8C 109.5 . . no
H8A C8 H8C 109.5 . . no
H8B C8 H8C 109.5 . . no
N1 C9 H9A 109.5 . . no
N1 C9 H9B 109.5 . . no
H9A C9 H9B 109.5 . . no
N1 C9 H9C 109.5 . . no
H9A C9 H9C 109.5 . . no
H9B C9 H9C 109.5 . . no
N2 C10 H10A 109.5 . . no
N2 C10 H10B 109.5 . . no
H10A C10 H10B 109.5 . . no
N2 C10 H10C 109.5 . . no
H10A C10 H10C 109.5 . . no
H10B C10 H10C 109.5 . . no
C6 C11 H11A 109.5 . . no
C6 C11 H11B 109.5 . . no
H11A C11 H11B 109.5 . . no
C6 C11 H11C 109.5 . . no
H11A C11 H11C 109.5 . . no
H11B C11 H11C 109.5 . . no
C6 C12 H12A 109.5 . . no
C6 C12 H12B 109.5 . . no
H12A C12 H12B 109.5 . . no
C6 C12 H12C 109.5 . . no
H12A C12 H12C 109.5 . . no
H12B C12 H12C 109.5 . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N1 1.930(3) . no
Ni N2 1.950(3) . no
Ni S1 2.1479(10) . no
Ni S2 2.1612(10) . no
S1 C1 1.849(4) . no
N1 C3 1.478(4) . no
N1 C2 1.479(4) . no
N1 C9 1.504(5) . no
C1 C7 1.521(5) . no
C1 C8 1.530(5) . no
C1 C2 1.536(5) . no
S2 C6 1.843(4) . no
N2 C5 1.479(4) . no
N2 C10 1.485(5) . no
N2 C4 1.490(4) . no
C2 H2A 0.9700 . no
C2 H2B 0.9700 . no
C3 C4 1.523(5) . no
C3 H3A 0.9700 . no
C3 H3B 0.9700 . no
C4 H4A 0.9700 . no
C4 H4B 0.9700 . no
C5 C6 1.540(5) . no
C5 H5A 0.9700 . no
C5 H5B 0.9700 . no
C6 C12 1.519(6) . no
C6 C11 1.531(6) . no
C7 H7A 0.9600 . no
C7 H7B 0.9600 . no
C7 H7C 0.9600 . no
C8 H8A 0.9600 . no
C8 H8B 0.9600 . no
C8 H8C 0.9600 . no
C9 H9A 0.9600 . no
C9 H9B 0.9600 . no
C9 H9C 0.9600 . no
C10 H10A 0.9600 . no
C10 H10B 0.9600 . no
C10 H10C 0.9600 . no
C11 H11A 0.9600 . no
C11 H11B 0.9600 . no
C11 H11C 0.9600 . no
C12 H12A 0.9600 . no
C12 H12B 0.9600 . no
C12 H12C 0.9600 . no
