#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:14:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179886 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/82/7018247.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_7018247
loop_
_publ_author_name
'Crouse, Heather F.'
'Potoma, Julianne'
'Nejrabi, Farhat'
'Snyder, Deanna L.'
'Chohan, Balwant S.'
'Basu, Swarna'
_publ_section_title
;
 Quenching of tryptophan fluorescence in various proteins by a series of
 small nickel complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2720
_journal_page_last               2731
_journal_paper_doi               10.1039/c2dt12169g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C11 H24 N2 Ni S2'
_chemical_formula_sum            'C11 H24 N2 Ni S2'
_chemical_formula_weight         307.15
_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_method           SHELXL-97
_audit_update_record
;
2011-06-13 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.126(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5547(10)
_cell_length_b                   12.3943(11)
_cell_length_c                   11.5831(11)
_cell_measurement_reflns_used    6246
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      38.38
_cell_measurement_theta_min      2.64
_cell_volume                     1413.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0866
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39600
_diffrn_reflns_theta_full        43.94
_diffrn_reflns_theta_max         43.94
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
PSISCANS: North, A. C. T.; Phillips, D. C.; Mathews, F. S. Acta.
Crystallogr. Sect A, 1968, 24, 351-359.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.049
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         10794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0565P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                6550
_reflns_number_total             10794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12169g.txt
_cod_data_source_block           bsc1a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7018247
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
Ni1 Ni 0.102265(12) 0.632338(11) 0.170112(12) 0.01997(4) Uani 1 1 d .
C1 C 0.48535(14) 0.60576(13) 0.11640(15) 0.0417(3) Uani 1 1 d .
H1A H 0.5183 0.6508 0.0636 0.063 Uiso 1 1 calc R
H1B H 0.5180 0.5317 0.1169 0.063 Uiso 1 1 calc R
H1C H 0.5192 0.6345 0.2009 0.063 Uiso 1 1 calc R
C2 C 0.33148(12) 0.60634(11) 0.06668(12) 0.0305(2) Uani 1 1 d .
H2 H 0.2977 0.5759 -0.0191 0.037 Uiso 1 1 calc R
C3 C 0.27848(12) 0.72081(10) 0.06252(12) 0.0310(2) Uani 1 1 d .
H3A H 0.3283 0.7572 0.1421 0.037 Uiso 1 1 calc R
H3B H 0.2958 0.7613 -0.0040 0.037 Uiso 1 1 calc R
C4 C 0.05466(14) 0.67869(12) -0.08558(12) 0.0360(3) Uani 1 1 d .
H4A H -0.0431 0.6857 -0.1037 0.054 Uiso 1 1 calc R
H4B H 0.0777 0.6024 -0.0883 0.054 Uiso 1 1 calc R
H4C H 0.0792 0.7189 -0.1473 0.054 Uiso 1 1 calc R
C5 C 0.09423(14) 0.83808(10) 0.04625(14) 0.0361(3) Uani 1 1 d .
H5A H 0.1210 0.8796 -0.0144 0.043 Uiso 1 1 calc R
H5B H 0.1479 0.8660 0.1297 0.043 Uiso 1 1 calc R
C6 C -0.05633(16) 0.85888(11) 0.02083(17) 0.0430(3) Uani 1 1 d .
H6A H -0.0641 0.9273 0.0619 0.052 Uiso 1 1 calc R
H6B H -0.1029 0.8695 -0.0694 0.052 Uiso 1 1 calc R
C7 C -0.13219(12) 0.77123(11) 0.06280(13) 0.0332(2) Uani 1 1 d .
H7A H -0.2141 0.8037 0.0712 0.040 Uiso 1 1 calc R
H7B H -0.1630 0.7154 -0.0026 0.040 Uiso 1 1 calc R
C8 C -0.00536(13) 0.79833(10) 0.28281(13) 0.0353(3) Uani 1 1 d .
H8A H 0.0513 0.8527 0.2632 0.053 Uiso 1 1 calc R
H8B H 0.0477 0.7620 0.3604 0.053 Uiso 1 1 calc R
H8C H -0.0844 0.8335 0.2919 0.053 Uiso 1 1 calc R
C9 C -0.14408(11) 0.63949(9) 0.20917(12) 0.0284(2) Uani 1 1 d .
H9A H -0.1822 0.5898 0.1381 0.034 Uiso 1 1 calc R
H9B H -0.2205 0.6792 0.2198 0.034 Uiso 1 1 calc R
C10 C -0.07211(12) 0.57450(11) 0.32447(11) 0.0294(2) Uani 1 1 d .
H10 H -0.0543 0.6221 0.3984 0.035 Uiso 1 1 calc R
C11 C -0.15993(14) 0.48007(13) 0.33426(14) 0.0392(3) Uani 1 1 d .
H11A H -0.2446 0.5074 0.3398 0.059 Uiso 1 1 calc R
H11B H -0.1109 0.4378 0.4084 0.059 Uiso 1 1 calc R
H11C H -0.1808 0.4342 0.2608 0.059 Uiso 1 1 calc R
N1 N 0.13076(9) 0.72282(7) 0.03975(9) 0.02349(16) Uani 1 1 d .
N2 N -0.05170(9) 0.71792(8) 0.18150(9) 0.02488(17) Uani 1 1 d .
S1 S 0.26219(4) 0.52684(3) 0.16286(4) 0.03682(8) Uani 1 1 d .
S2 S 0.08999(3) 0.53050(3) 0.31803(3) 0.02927(7) Uani 1 1 d .
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
N2 Ni1 N1 95.77(4)
N2 Ni1 S1 174.90(3)
N1 Ni1 S1 88.72(3)
N2 Ni1 S2 88.57(3)
N1 Ni1 S2 175.00(3)
S1 Ni1 S2 87.044(14)
C1 C2 C3 110.39(12)
C1 C2 S1 112.07(10)
C3 C2 S1 107.42(8)
N1 C3 C2 111.86(10)
N1 C5 C6 114.96(11)
C7 C6 C5 116.46(11)
N2 C7 C6 114.83(11)
N2 C9 C10 112.25(9)
C9 C10 C11 110.52(10)
C9 C10 S2 107.69(8)
C11 C10 S2 112.25(10)
C3 N1 C4 109.29(9)
C3 N1 C5 106.36(9)
C4 N1 C5 110.10(10)
C3 N1 Ni1 106.99(7)
C4 N1 Ni1 110.95(8)
C5 N1 Ni1 112.95(8)
C8 N2 C7 110.44(10)
C8 N2 C9 108.84(9)
C7 N2 C9 106.79(9)
C8 N2 Ni1 111.57(7)
C7 N2 Ni1 112.65(8)
C9 N2 Ni1 106.28(7)
C2 S1 Ni1 100.81(4)
C10 S2 Ni1 100.51(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 N2 1.9844(9)
Ni1 N1 1.9888(9)
Ni1 S1 2.1605(3)
Ni1 S2 2.1692(3)
C1 C2 1.5149(18)
C2 C3 1.5194(18)
C2 S1 1.8260(13)
C3 N1 1.4848(15)
C4 N1 1.4871(16)
C5 N1 1.4886(16)
C5 C6 1.530(2)
C6 C7 1.529(2)
C7 N2 1.4855(16)
C8 N2 1.4819(15)
C9 N2 1.4911(15)
C9 C10 1.5093(18)
C10 C11 1.5223(18)
C10 S2 1.8228(12)
