#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/16/2201625.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2201625
loop_
_publ_author_name
'Soh, Shu Fang'
'Lai, Chian Sing'
'Tiekink, Edward R. T.'
_publ_section_title
(4,7-Dimethyl-1,10-phenanthroline)bis(O-isopropropyldithiocarbonato)zinc(II)
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m641
_journal_page_last               m643
_journal_paper_doi               10.1107/S1600536802018433
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Zn (C4 H7 O S2)2 (C14 H12 N2)]'
_chemical_formula_moiety         'C22 H26 N2 O2 S4 Zn'
_chemical_formula_sum            'C22 H26 N2 O2 S4 Zn'
_chemical_formula_weight         544.06
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 103.4030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6834(10)
_cell_length_b                   9.8097(5)
_cell_length_c                   12.8171(7)
_cell_measurement_reflns_used    6953
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.3
_cell_volume                     2407.4(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9944
_diffrn_reflns_theta_full        30.1
_diffrn_reflns_theta_max         30.1
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996; Blessing, 1995)'
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.028
_refine_ls_R_factor_gt           0.027
_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)+(0.046P)²+1.2962P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.075
_refine_ls_wR_factor_ref         0.076
_reflns_number_gt                3322
_reflns_number_total             3524
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su6001.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201625
_cod_database_fobs_code          2201625
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn 0.0000 0.102897(18) 0.2500 0.02037(7) Uani d S 1 . . Zn
S1 0.061715(18) -0.00653(3) 0.14366(3) 0.02762(9) Uani d . 1 . . S
S2 0.140616(18) -0.04670(3) 0.37112(3) 0.02729(8) Uani d . 1 . . S
O1 0.17104(5) -0.14665(10) 0.19463(8) 0.02657(19) Uani d . 1 . . O
N1 -0.04180(5) 0.26879(10) 0.15207(8) 0.01855(18) Uani d . 1 . . N
C1 0.12892(6) -0.07212(12) 0.24034(10) 0.0222(2) Uani d . 1 . . C
C2 0.23644(7) -0.20082(14) 0.25903(12) 0.0288(3) Uani d . 1 . . C
H2 0.2565 -0.1355 0.3180 0.035 Uiso calc R 1 . . H
C3 0.22396(9) -0.33684(17) 0.30623(14) 0.0380(3) Uani d . 1 . . C
H3a 0.1933 -0.3246 0.3557 0.057 Uiso calc R 1 . . H
H3b 0.2686 -0.3752 0.3451 0.057 Uiso calc R 1 . . H
H3c 0.2019 -0.3991 0.2485 0.057 Uiso calc R 1 . . H
C4 0.28419(8) -0.21151(17) 0.18341(15) 0.0406(4) Uani d . 1 . . C
H4a 0.2910 -0.1209 0.1552 0.061 Uiso calc R 1 . . H
H4b 0.2634 -0.2723 0.1239 0.061 Uiso calc R 1 . . H
H4c 0.3294 -0.2483 0.2217 0.061 Uiso calc R 1 . . H
C5 -0.07949(6) 0.26590(13) 0.05194(10) 0.0229(2) Uani d . 1 . . C
H5 -0.0942 0.1802 0.0200 0.027 Uiso calc R 1 . . H
C6 -0.09833(7) 0.38402(13) -0.00826(10) 0.0245(2) Uani d . 1 . . C
H6 -0.1242 0.3769 -0.0805 0.029 Uiso calc R 1 . . H
C7 -0.08012(6) 0.51050(13) 0.03514(10) 0.0212(2) Uani d . 1 . . C
C8 -0.04060(6) 0.51597(12) 0.14295(9) 0.0184(2) Uani d . 1 . . C
C9 -0.02164(6) 0.39207(11) 0.19632(9) 0.0164(2) Uani d . 1 . . C
C10 -0.10042(7) 0.63789(15) -0.02900(11) 0.0288(3) Uani d . 1 . . C
H10a -0.1187 0.6141 -0.1046 0.043 Uiso calc R 1 . . H
H10b -0.0594 0.6967 -0.0223 0.043 Uiso calc R 1 . . H
H10c -0.1365 0.6862 -0.0021 0.043 Uiso calc R 1 . . H
C11 -0.01905(6) 0.64070(12) 0.19857(10) 0.0227(2) Uani d . 1 . . C
H11 -0.0316 0.7250 0.1629 0.027 Uiso calc R 1 . . H
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'
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'
Zn Zn 0.2839 1.4301 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Zn N1 . . 101.27(3) y
S1 Zn S1 . 2 124.15(2) y
S1 Zn N1 . 2 121.97(3) y
N1 Zn N1 . 2 78.59(5) y
Zn S1 C1 . . 99.93(4) y
C1 O1 C2 . . 120.42(10) y
C5 N1 C9 . . 117.91(10) ?
C5 N1 Zn . . 127.96(8) ?
C9 N1 Zn . . 113.86(7) ?
O1 C1 S2 . . 124.77(10) ?
O1 C1 S1 . . 109.95(9) ?
S2 C1 S1 . . 125.28(7) ?
O1 C2 C3 . . 110.17(11) ?
O1 C2 C4 . . 105.21(12) ?
C3 C2 C4 . . 112.42(12) ?
O1 C2 H2 . . 109.6 ?
C3 C2 H2 . . 109.6 ?
C4 C2 H2 . . 109.6 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C2 C4 H4A . . 109.5 ?
C2 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C2 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N1 C5 C6 . . 122.39(11) ?
N1 C5 H5 . . 118.8 ?
C6 C5 H5 . . 118.8 ?
C7 C6 C5 . . 121.07(12) ?
C7 C6 H6 . . 119.5 ?
C5 C6 H6 . . 119.5 ?
C6 C7 C8 . . 117.44(11) ?
C6 C7 C10 . . 121.34(11) ?
C8 C7 C10 . . 121.22(11) ?
C9 C8 C7 . . 117.74(10) ?
C9 C8 C11 . . 118.93(10) ?
C7 C8 C11 . . 123.32(10) ?
N1 C9 C8 . . 123.38(10) ?
N1 C9 C9 . 2 116.78(6) ?
C8 C9 C9 . 2 119.84(6) ?
C7 C10 H10A . . 109.5 ?
C7 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C7 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C11 C11 C8 2 . 121.17(7) ?
C11 C11 H11 2 . 119.4 ?
C8 C11 H11 . . 119.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn S1 . 2.2920(3) y
Zn N1 . 2.1028(10) y
S1 C1 . 1.7145(13) y
S2 C1 . 1.6571(13) y
C1 O1 . 1.3380(15) y
O1 C2 . 1.4588(16) y
N1 C5 . 1.3254(15) ?
N1 C9 . 1.3555(14) ?
C2 C3 . 1.508(2) ?
C2 C4 . 1.502(2) ?
C2 H2 . 1.0000 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
C4 H4A . 0.9800 ?
C4 H4B . 0.9800 ?
C4 H4C . 0.9800 ?
C5 C6 . 1.3939(18) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.3729(18) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.4210(16) ?
C7 C10 . 1.4982(17) ?
C8 C9 . 1.4023(15) ?
C8 C11 . 1.4301(16) ?
C9 C9 2 1.441(2) ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 C11 2 1.357(2) ?
C11 H11 . 0.9500 ?
