#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179379 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/76/4327642.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_4327642
loop_
_publ_author_name
'Chandrika P. Kulatilleke'
'Scott N. Goldie'
'Mary Jane Heeg'
'L. A. Ochrymowycz'
'D. B. Rorabacher'
_publ_section_title
;
 Formation and Dissociation Kinetics and Crystal Structures of
 Nickel(II)-Macrocyclic Tetrathiaether Complexes in Acetonitrile.
 Comparison to Nickel(II)-Macrocyclic Tetramines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1444
_journal_page_last               1453
_journal_paper_doi               10.1021/ic991019+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H32 Cl2 Ni O8 S4'
_chemical_formula_weight         634.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                83.428(2)
_cell_angle_beta                 76.6390(10)
_cell_angle_gamma                87.6770(10)
_cell_formula_units_Z            1
_cell_length_a                   7.3849(6)
_cell_length_b                   8.8365(7)
_cell_length_c                   9.7503(8)
_cell_measurement_reflns_used    2722
_cell_measurement_temperature    295(2)
_cell_volume                     614.92(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.016
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4350
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0000(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.971
_refine_ls_goodness_of_fit_obs   1.032
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_restrained_S_obs      1.032
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_obs          0.0310
_refine_ls_shift/esd_max         -1.546
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0555P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0823
_refine_ls_wR_factor_obs         0.0773
_reflns_number_observed          2226
_reflns_number_total             2763
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9910192B_3.cif
_cod_data_source_block           pler
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4327642
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.5000 0.5000 0.0000 0.02618(13) Uani 1 d S
S1 S 0.78324(7) 0.52097(6) -0.12980(6) 0.02773(14) Uani 1 d .
S2 S 0.40301(7) 0.66619(6) -0.15252(6) 0.02892(14) Uani 1 d .
C1 C 0.7513(3) 0.6141(2) -0.3021(2) 0.0306(5) Uani 1 d .
C2 C 0.9397(3) 0.6661(3) -0.3974(3) 0.0367(5) Uani 1 d .
C3 C 1.0204(3) 0.7965(3) -0.3426(3) 0.0390(5) Uani 1 d .
C4 C 0.8808(4) 0.9271(3) -0.3179(3) 0.0442(6) Uani 1 d .
C5 C 0.7017(3) 0.8755(3) -0.2131(3) 0.0352(5) Uani 1 d .
C6 C 0.6166(3) 0.7489(2) -0.2700(2) 0.0307(5) Uani 1 d .
C7 C 0.2927(3) 0.8228(3) -0.0555(3) 0.0350(5) Uani 1 d .
C8 C 0.1114(3) 0.7713(3) 0.0448(3) 0.0359(5) Uani 1 d .
C9 C 0.1339(4) 0.6680(3) 0.1759(3) 0.0351(5) Uani 1 d .
Cl1 Cl 0.39686(8) 0.24863(6) -0.30607(6) 0.0379(2) Uani 1 d .
O1 O 0.5804(3) 0.2299(3) -0.3858(3) 0.0852(8) Uani 1 d .
O2 O 0.2815(4) 0.1289(3) -0.3183(3) 0.0821(8) Uani 1 d .
O3 O 0.3211(4) 0.3892(3) -0.3563(3) 0.0751(7) Uani 1 d .
O4 O 0.4023(4) 0.2494(3) -0.1604(2) 0.0792(7) Uani 1 d .
H1 H 0.6989(33) 0.5426(28) -0.3406(25) 0.029(6) Uiso 1 d .
H2A H 0.9175(35) 0.6994(28) -0.4909(27) 0.037(6) Uiso 1 d .
H2B H 1.0242(34) 0.5785(29) -0.4058(26) 0.036(6) Uiso 1 d .
H3A H 1.1278(42) 0.8255(32) -0.4038(31) 0.048(8) Uiso 1 d .
H3B H 1.0570(32) 0.7624(26) -0.2504(26) 0.029(6) Uiso 1 d .
H4A H 0.8426(35) 0.9642(29) -0.4080(30) 0.043(7) Uiso 1 d .
H4B H 0.9299(38) 1.0026(32) -0.2815(29) 0.044(7) Uiso 1 d .
H5A H 0.7271(38) 0.8404(30) -0.1235(30) 0.044(7) Uiso 1 d .
H5B H 0.6114(42) 0.9540(34) -0.2009(31) 0.052(8) Uiso 1 d .
H6 H 0.5803(34) 0.7849(27) -0.3548(26) 0.033(6) Uiso 1 d .
H7A H 0.2714(39) 0.8952(32) -0.1288(31) 0.048(8) Uiso 1 d .
H7B H 0.3704(36) 0.8528(28) -0.0032(27) 0.037(7) Uiso 1 d .
H8A H 0.0576(36) 0.8599(32) 0.0755(27) 0.041(7) Uiso 1 d .
H8B H 0.0399(43) 0.7281(36) -0.0082(32) 0.060(9) Uiso 1 d .
H9A H 0.2223(38) 0.7058(30) 0.2257(29) 0.043(7) Uiso 1 d .
H9B H 0.0283(46) 0.6499(34) 0.2372(33) 0.056(9) Uiso 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
S1 Ni1 S1 180.0 . 2_665
S1 Ni1 S2 90.26(2) . 2_665
S1 Ni1 S2 89.74(2) 2_665 2_665
S1 Ni1 S2 89.74(2) . .
S1 Ni1 S2 90.26(2) 2_665 .
S2 Ni1 S2 180.0 2_665 .
C9 S1 C1 101.32(10) 2_665 .
C9 S1 Ni1 108.13(9) 2_665 .
C1 S1 Ni1 103.71(7) . .
C7 S2 C6 104.37(11) . .
C7 S2 Ni1 107.02(9) . .
C6 S2 Ni1 105.08(7) . .
C6 C1 C2 111.7(2) . .
C6 C1 S1 106.73(15) . .
C2 C1 S1 110.4(2) . .
C3 C2 C1 112.3(2) . .
C4 C3 C2 111.1(2) . .
C3 C4 C5 111.5(2) . .
C6 C5 C4 109.3(2) . .
C5 C6 C1 112.7(2) . .
C5 C6 S2 115.3(2) . .
C1 C6 S2 105.6(2) . .
C8 C7 S2 110.2(2) . .
C7 C8 C9 114.7(2) . .
C8 C9 S1 110.8(2) . 2_665
O1 Cl1 O2 111.3(2) . .
O1 Cl1 O3 109.3(2) . .
O2 Cl1 O3 108.6(2) . .
O1 Cl1 O4 108.5(2) . .
O2 Cl1 O4 109.2(2) . .
O3 Cl1 O4 109.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S1 2.1830(5) .
Ni1 S1 2.1830(5) 2_665
Ni1 S2 2.1882(5) 2_665
Ni1 S2 2.1882(5) .
S1 C9 1.824(2) 2_665
S1 C1 1.845(2) .
S2 C7 1.824(2) .
S2 C6 1.844(2) .
C1 C6 1.533(3) .
C1 C2 1.539(3) .
C2 C3 1.521(3) .
C3 C4 1.518(3) .
C4 C5 1.522(3) .
C5 C6 1.521(3) .
C7 C8 1.516(3) .
C8 C9 1.521(3) .
C9 S1 1.824(2) 2_665
Cl1 O1 1.412(2) .
Cl1 O2 1.417(2) .
Cl1 O3 1.424(2) .
Cl1 O4 1.431(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
S1 Ni1 S1 C9 67.3(149) 2_665 2_665
S2 Ni1 S1 C9 56.93(9) 2_665 2_665
S2 Ni1 S1 C9 -123.07(9) . 2_665
S1 Ni1 S1 C1 174.3(149) 2_665 .
S2 Ni1 S1 C1 163.94(7) 2_665 .
S2 Ni1 S1 C1 -16.06(7) . .
S1 Ni1 S2 C7 -122.11(9) . .
S1 Ni1 S2 C7 57.89(9) 2_665 .
S2 Ni1 S2 C7 78.2(100) 2_665 .
S1 Ni1 S2 C6 -11.54(7) . .
S1 Ni1 S2 C6 168.46(7) 2_665 .
S2 Ni1 S2 C6 -171.2(100) 2_665 .
C9 S1 C1 C6 159.3(2) 2_665 .
Ni1 S1 C1 C6 47.3(2) . .
C9 S1 C1 C2 -79.1(2) 2_665 .
Ni1 S1 C1 C2 168.87(13) . .
C6 C1 C2 C3 49.9(3) . .
S1 C1 C2 C3 -68.7(2) . .
C1 C2 C3 C4 -53.0(3) . .
C2 C3 C4 C5 58.1(3) . .
C3 C4 C5 C6 -58.9(3) . .
C4 C5 C6 C1 56.0(3) . .
C4 C5 C6 S2 177.4(2) . .
C2 C1 C6 C5 -52.0(3) . .
S1 C1 C6 C5 68.8(2) . .
C2 C1 C6 S2 -178.70(15) . .
S1 C1 C6 S2 -58.0(2) . .
C7 S2 C6 C5 30.4(2) . .
Ni1 S2 C6 C5 -82.1(2) . .
C7 S2 C6 C1 155.5(2) . .
Ni1 S2 C6 C1 43.1(2) . .
C6 S2 C7 C8 179.1(2) . .
Ni1 S2 C7 C8 -69.8(2) . .
S2 C7 C8 C9 74.0(2) . .
C7 C8 C9 S1 -72.3(2) . 2_665
