#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:58:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179164 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/25/4312501.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_4312501
loop_
_publ_author_name
'Jana A. Lewis'
'David T. Puerta'
'Seth M. Cohen'
_publ_section_title
;
 Metal Complexes of the trans-Influencing Ligand Thiomaltol
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7455
_journal_page_last               7459
_journal_paper_doi               10.1021/ic0347135
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H14 Ni O6 S2'
_chemical_formula_weight         377.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.9288(15)
_cell_length_b                   6.6926(4)
_cell_length_c                   18.8132(13)
_cell_measurement_temperature    100(2)
_cell_volume                     2886.9(3)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23027
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.004
_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          0.0812
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2628
_reflns_number_total             3309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347135si20030922_123727_3.cif
_cod_data_source_block           nitm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312501
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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_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
C1 C 0.64794(7) 0.7294(2) 0.24804(9) 0.0170(3) Uani 1 1 d . . .
C2 C 0.67044(8) 0.7187(2) 0.31790(9) 0.0202(4) Uani 1 1 d . . .
H2 H 0.6449 0.7161 0.3576 0.024 Uiso 1 1 calc R . .
C3 C 0.72857(8) 0.7124(2) 0.32722(9) 0.0226(4) Uani 1 1 d . . .
H3 H 0.7436 0.7036 0.3742 0.027 Uiso 1 1 calc R . .
C4 C 0.74676(8) 0.7286(2) 0.20403(9) 0.0176(4) Uani 1 1 d . . .
C5 C 0.79373(7) 0.7336(2) 0.15012(10) 0.0221(4) Uani 1 1 d . . .
H5A H 0.7885 0.8504 0.1194 0.033 Uiso 1 1 calc R . .
H5B H 0.7921 0.6117 0.1213 0.033 Uiso 1 1 calc R . .
H5C H 0.8317 0.7419 0.1740 0.033 Uiso 1 1 calc R . .
C6 C 0.68764(7) 0.7331(2) 0.18971(9) 0.0163(3) Uani 1 1 d . . .
C7 C 0.49665(7) 0.75020(18) 0.00452(10) 0.0148(3) Uani 1 1 d . . .
C8 C 0.44764(8) 0.75093(19) -0.04095(10) 0.0182(4) Uani 1 1 d . . .
H8 H 0.4094 0.7487 -0.0216 0.022 Uiso 1 1 calc R . .
C9 C 0.45550(8) 0.75481(19) -0.11166(10) 0.0199(4) Uani 1 1 d . . .
H9 H 0.4222 0.7557 -0.1416 0.024 Uiso 1 1 calc R . .
C10 C 0.55712(8) 0.75736(19) -0.10019(10) 0.0153(3) Uani 1 1 d . . .
C11 C 0.61165(8) 0.7636(2) -0.14276(10) 0.0201(4) Uani 1 1 d . . .
H11A H 0.6102 0.6603 -0.1796 0.030 Uiso 1 1 calc R . .
H11B H 0.6452 0.7396 -0.1116 0.030 Uiso 1 1 calc R . .
H11C H 0.6155 0.8952 -0.1651 0.030 Uiso 1 1 calc R . .
C12 C 0.55298(7) 0.75310(18) -0.02734(9) 0.0140(3) Uani 1 1 d . . .
H12 H 0.7161(8) 0.468(3) 0.9877(9) 0.020(5) Uiso 1 1 d . . .
H13 H 0.6635(10) 0.518(5) 0.9966(12) 0.064(9) Uiso 1 1 d . . .
H14 H 0.6879(8) 0.123(3) 0.9831(10) 0.029(6) Uiso 1 1 d . . .
H15 H 0.6738(10) -0.047(4) 0.9956(12) 0.056(9) Uiso 1 1 d . . .
Ni1 Ni 0.586438(9) 0.74479(2) 0.113197(12) 0.01358(9) Uani 1 1 d . . .
O1 O 0.66783(5) 0.74081(13) 0.12408(6) 0.0164(3) Uani 1 1 d . . .
O2 O 0.76638(5) 0.71810(16) 0.27217(7) 0.0199(3) Uani 1 1 d . . .
O3 O 0.59997(5) 0.75171(13) 0.01415(6) 0.0150(3) Uani 1 1 d . . .
O4 O 0.50854(5) 0.75747(13) -0.14162(7) 0.0172(3) Uani 1 1 d . . .
O5 O 0.68326(6) 0.43259(19) 0.98336(7) 0.0234(3) Uani 1 1 d . . .
O6 O 0.69832(5) 0.0122(2) 0.97858(7) 0.0249(3) Uani 1 1 d . . .
S1 S 0.575614(19) 0.73646(6) 0.22695(2) 0.02014(12) Uani 1 1 d . . .
S2 S 0.493214(18) 0.74613(5) 0.09516(3) 0.01596(12) 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'
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'
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
C2 C1 C6 118.90(16) . . ?
C2 C1 S1 124.92(14) . . ?
C6 C1 S1 116.18(13) . . ?
C3 C2 C1 118.98(16) . . ?
C2 C3 O2 122.34(16) . . ?
O2 C4 C6 120.60(16) . . ?
O2 C4 C5 113.98(15) . . ?
C6 C4 C5 125.42(16) . . ?
O1 C6 C4 121.46(16) . . ?
O1 C6 C1 120.13(15) . . ?
C4 C6 C1 118.40(16) . . ?
C8 C7 C12 117.82(17) . . ?
C8 C7 S2 124.63(14) . . ?
C12 C7 S2 117.55(14) . . ?
C9 C8 C7 119.55(17) . . ?
O4 C9 C8 122.59(17) . . ?
O4 C10 C12 121.02(16) . . ?
O4 C10 C11 112.36(16) . . ?
C12 C10 C11 126.62(16) . . ?
O3 C12 C10 121.96(15) . . ?
O3 C12 C7 119.17(16) . . ?
C10 C12 C7 118.86(16) . . ?
O1 Ni1 O3 86.83(5) . . ?
O1 Ni1 S1 90.33(4) . . ?
O3 Ni1 S1 177.16(4) . . ?
O1 Ni1 S2 177.18(4) . . ?
O3 Ni1 S2 90.43(4) . . ?
S1 Ni1 S2 92.411(19) . . ?
C6 O1 Ni1 116.47(11) . . ?
C3 O2 C4 120.77(13) . . ?
C12 O3 Ni1 116.47(11) . . ?
C9 O4 C10 120.15(15) . . ?
C1 S1 Ni1 96.88(6) . . ?
C7 S2 Ni1 96.38(6) . . ?
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
C1 C2 1.414(2) . ?
C1 C6 1.426(2) . ?
C1 S1 1.7058(18) . ?
C2 C3 1.345(2) . ?
C3 O2 1.351(2) . ?
C4 O2 1.360(2) . ?
C4 C6 1.382(2) . ?
C4 C5 1.480(2) . ?
C6 O1 1.317(2) . ?
C7 C8 1.412(2) . ?
C7 C12 1.424(2) . ?
C7 S2 1.7072(19) . ?
C8 C9 1.343(3) . ?
C9 O4 1.341(2) . ?
C10 O4 1.360(2) . ?
C10 C12 1.374(3) . ?
C10 C11 1.485(2) . ?
C12 O3 1.330(2) . ?
Ni1 O1 1.8776(12) . ?
Ni1 O3 1.8896(12) . ?
Ni1 S1 2.1550(5) . ?
Ni1 S2 2.1643(5) . ?
