#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007326.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_7007326
loop_
_publ_author_name
'Fritz, Thorsten'
'Steinfeld, Gunther'
'Käss, Steffen'
'Kersting, Berthold'
_publ_section_title
;
 Preparation and characterization of mononuclear Co, Ni, and Zn
 complexes of dinucleating macrocyclic hexaaza-dithiophenolate ligands
 and their open-chain derivatives.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3812
_journal_page_last               3821
_journal_paper_doi               10.1039/b603740b
_journal_year                    2006
_chemical_compound_source
;
Crystals were taken from the mother liquor.
;
_chemical_formula_structural
;
[Ni(L4)]
;
_chemical_formula_sum            'C18 H23 N3 Ni S2'
_chemical_formula_weight         404.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.799(2)
_cell_length_b                   13.289(3)
_cell_length_c                   12.474(2)
_cell_measurement_reflns_used    180
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      8
_cell_volume                     1778.0(6)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 (FARRUGIA)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'BRUKER AXS'
_diffrn_measurement_method       hemisphere
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.1199
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11219
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, SHELDRICK, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0507
_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)+(0.0373P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                2125
_reflns_number_total             4239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603740b.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7007326
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.19173(5) 0.21236(4) 0.26382(4) 0.02139(16) Uani 1 1 d . . .
S1 S 0.33123(11) 0.20625(10) 0.13867(9) 0.0335(3) Uani 1 1 d . . .
S2 S 0.08636(11) 0.33046(8) 0.35892(9) 0.0242(3) Uani 1 1 d . . .
N1 N 0.3305(3) 0.1959(3) 0.3957(3) 0.0241(8) Uani 1 1 d . . .
H1 H 0.3099 0.2398 0.4468 0.029 Uiso 1 1 calc R . .
N2 N 0.1331(3) 0.0762(3) 0.3130(3) 0.0238(9) Uani 1 1 d . . .
H2 H 0.1669 0.0266 0.2753 0.029 Uiso 1 1 calc R . .
N3 N 0.0397(3) 0.1945(3) 0.1420(3) 0.0232(8) Uani 1 1 d . . .
H3 H 0.0736 0.1797 0.0804 0.028 Uiso 1 1 calc R . .
C1 C 0.4643(4) 0.1413(3) 0.1936(3) 0.0231(10) Uani 1 1 d . . .
C2 C 0.5265(4) 0.0780(3) 0.1258(4) 0.0295(11) Uani 1 1 d . . .
H2A H 0.4982 0.0748 0.0526 0.035 Uiso 1 1 calc R . .
C3 C 0.6278(4) 0.0214(4) 0.1659(4) 0.0338(12) Uani 1 1 d . . .
H3A H 0.6662 -0.0204 0.1198 0.041 Uiso 1 1 calc R . .
C4 C 0.6730(4) 0.0260(4) 0.2738(4) 0.0347(12) Uani 1 1 d . . .
H4 H 0.7404 -0.0136 0.3010 0.042 Uiso 1 1 calc R . .
C5 C 0.6170(4) 0.0903(3) 0.3412(4) 0.0303(11) Uani 1 1 d . . .
H5 H 0.6487 0.0945 0.4136 0.036 Uiso 1 1 calc R . .
C6 C 0.5148(4) 0.1485(3) 0.3031(3) 0.0243(10) Uani 1 1 d . . .
C7 C 0.4598(4) 0.2203(3) 0.3790(3) 0.0249(10) Uani 1 1 d . . .
H7A H 0.5110 0.2193 0.4482 0.030 Uiso 1 1 calc R . .
H7B H 0.4622 0.2880 0.3502 0.030 Uiso 1 1 calc R . .
C8 C 0.3169(4) 0.0939(3) 0.4418(4) 0.0270(11) Uani 1 1 d . . .
H8A H 0.3491 0.0935 0.5177 0.032 Uiso 1 1 calc R . .
H8B H 0.3636 0.0453 0.4046 0.032 Uiso 1 1 calc R . .
C9 C 0.1793(4) 0.0665(3) 0.4281(3) 0.0248(10) Uani 1 1 d . . .
H9A H 0.1681 -0.0020 0.4522 0.030 Uiso 1 1 calc R . .
H9B H 0.1336 0.1113 0.4706 0.030 Uiso 1 1 calc R . .
C10 C -0.0035(4) 0.0759(3) 0.2860(3) 0.0272(11) Uani 1 1 d . . .
H10A H -0.0413 0.1243 0.3306 0.033 Uiso 1 1 calc R . .
H10B H -0.0368 0.0098 0.2990 0.033 Uiso 1 1 calc R . .
C11 C -0.0323(4) 0.1037(3) 0.1673(4) 0.0278(11) Uani 1 1 d . . .
H11A H -0.0111 0.0478 0.1229 0.033 Uiso 1 1 calc R . .
H11B H -0.1209 0.1169 0.1509 0.033 Uiso 1 1 calc R . .
C12 C -0.0375(4) 0.2857(3) 0.1176(3) 0.0255(10) Uani 1 1 d . . .
H12A H -0.0887 0.2756 0.0493 0.031 Uiso 1 1 calc R . .
H12B H 0.0175 0.3420 0.1087 0.031 Uiso 1 1 calc R . .
C13 C -0.1216(4) 0.3137(3) 0.2015(3) 0.0208(10) Uani 1 1 d . . .
C14 C -0.2485(4) 0.3217(3) 0.1698(4) 0.0298(11) Uani 1 1 d . . .
H14 H -0.2801 0.3009 0.1008 0.036 Uiso 1 1 calc R . .
C15 C -0.3293(4) 0.3597(3) 0.2376(4) 0.0328(12) Uani 1 1 d . . .
H15 H -0.4137 0.3671 0.2139 0.039 Uiso 1 1 calc R . .
C16 C -0.2822(4) 0.3866(3) 0.3419(4) 0.0316(12) Uani 1 1 d . . .
H16 H -0.3354 0.4122 0.3887 0.038 Uiso 1 1 calc R . .
C17 C -0.1577(4) 0.3756(3) 0.3763(4) 0.0268(11) Uani 1 1 d . . .
H17 H -0.1283 0.3931 0.4469 0.032 Uiso 1 1 calc R . .
C18 C -0.0723(4) 0.3385(3) 0.3076(3) 0.0196(9) 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni N1 83.68(14) . . ?
N2 Ni N3 82.79(13) . . ?
N1 Ni N3 166.44(13) . . ?
N2 Ni S1 115.19(10) . . ?
N1 Ni S1 93.68(10) . . ?
N3 Ni S1 91.32(10) . . ?
N2 Ni S2 104.89(10) . . ?
N1 Ni S2 91.00(10) . . ?
N3 Ni S2 93.28(10) . . ?
S1 Ni S2 139.92(5) . . ?
C1 S1 Ni 109.03(15) . . ?
C18 S2 Ni 111.46(14) . . ?
C7 N1 C8 113.2(3) . . ?
C7 N1 Ni 117.9(3) . . ?
C8 N1 Ni 107.7(3) . . ?
C9 N2 C10 116.1(3) . . ?
C9 N2 Ni 106.9(3) . . ?
C10 N2 Ni 105.7(3) . . ?
C12 N3 C11 114.2(3) . . ?
C12 N3 Ni 115.2(3) . . ?
C11 N3 Ni 108.6(3) . . ?
C6 C1 C2 117.4(4) . . ?
C6 C1 S1 123.5(3) . . ?
C2 C1 S1 119.0(3) . . ?
C3 C2 C1 121.5(4) . . ?
C2 C3 C4 120.5(4) . . ?
C3 C4 C5 119.3(5) . . ?
C6 C5 C4 121.5(4) . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 C7 119.5(4) . . ?
C1 C6 C7 120.8(4) . . ?
N1 C7 C6 113.4(3) . . ?
N1 C8 C9 108.3(3) . . ?
N2 C9 C8 107.8(3) . . ?
N2 C10 C11 107.9(3) . . ?
N3 C11 C10 110.5(4) . . ?
N3 C12 C13 115.4(3) . . ?
C14 C13 C18 120.3(4) . . ?
C14 C13 C12 118.4(4) . . ?
C18 C13 C12 121.1(4) . . ?
C15 C14 C13 121.8(4) . . ?
C14 C15 C16 118.7(4) . . ?
C17 C16 C15 120.4(4) . . ?
C16 C17 C18 122.0(4) . . ?
C13 C18 C17 116.6(4) . . ?
C13 C18 S2 125.0(3) . . ?
C17 C18 S2 118.3(3) . . ?
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 N2 2.036(3) . ?
Ni N1 2.104(4) . ?
Ni N3 2.117(4) . ?
Ni S1 2.2936(13) . ?
Ni S2 2.3407(13) . ?
S1 C1 1.747(4) . ?
S2 C18 1.762(4) . ?
N1 C7 1.472(5) . ?
N1 C8 1.486(5) . ?
N2 C9 1.469(5) . ?
N2 C10 1.475(5) . ?
N3 C12 1.483(5) . ?
N3 C11 1.490(5) . ?
C1 C6 1.414(6) . ?
C1 C2 1.416(6) . ?
C2 C3 1.373(6) . ?
C3 C4 1.379(6) . ?
C4 C5 1.387(6) . ?
C5 C6 1.386(6) . ?
C6 C7 1.513(6) . ?
C8 C9 1.521(6) . ?
C10 C11 1.523(6) . ?
C12 C13 1.510(5) . ?
C13 C14 1.385(6) . ?
C13 C18 1.406(6) . ?
C14 C15 1.379(6) . ?
C15 C16 1.387(6) . ?
C16 C17 1.370(6) . ?
C17 C18 1.419(5) . ?
