#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/46/2204608.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_2204608
loop_
_publ_author_name
'Tao Li'
'Zhi-Hua Li'
'Shao-Wu Du'
_publ_section_title
;catena-Poly[[bis(O,O'-diethyl
 dithiophosphato-κ²S,S')cadmium(II)]-μ-4,4'-bipyridine-N:N']
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1912
_journal_page_last               m1914
_journal_paper_doi               10.1107/S1600536804029721
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Cd (C4 H10 O2 P S2)2 (C10 H8 N2)]'
_chemical_formula_moiety         'C18 H28 Cd N2 O4 P2 S4'
_chemical_formula_sum            'C18 H28 Cd N2 O4 P2 S4'
_chemical_formula_weight         639.00
_chemical_name_systematic
'catena-Poly[[bis(O,O'-diethyl dithiophosphato-κ²S,S')cadmium(II)]-μ-4,4'-bipyridine-N:N']'
_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-97
_cell_angle_alpha                98.71(3)
_cell_angle_beta                 103.96(4)
_cell_angle_gamma                118.818(16)
_cell_formula_units_Z            1
_cell_length_a                   8.819(6)
_cell_length_b                   8.852(5)
_cell_length_c                   10.404(6)
_cell_measurement_reflns_used    2089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.1258
_cell_volume                     655.5(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130.1500
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD-profile-fitting
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5084
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         2.365
_refine_diff_density_min         -0.845
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0563
_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)+(0.0768P)²+2.5033P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                2687
_reflns_number_total             2975
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br6169.cif
_cod_data_source_block           I
_cod_database_code               2204608
_cod_database_fobs_code          2204608
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cd1 -0.5000 0.5000 0.5000 0.02289(16) Uani d S 1 . . Cd
S1 -0.27271(18) 0.52579(18) 0.35980(12) 0.0348(3) Uani d . 1 . . S
S2 -0.65652(16) 0.15207(16) 0.34613(12) 0.0313(3) Uani d . 1 . . S
O1 -0.3372(6) 0.1586(7) 0.2966(5) 0.0541(11) Uani d . 1 . . O
O2 -0.5137(6) 0.2105(7) 0.1143(4) 0.0573(13) Uani d . 1 . . O
C1 -0.2486(11) 0.1610(12) 0.4308(8) 0.066(2) Uani d . 1 . . C
H1A -0.3381 0.1103 0.4755 0.079 Uiso calc R 1 . . H
H1B -0.1525 0.2849 0.4887 0.079 Uiso calc R 1 . . H
C2 -0.1640(13) 0.0487(14) 0.4131(12) 0.087(3) Uani d . 1 . . C
H2A -0.1028 0.0486 0.5029 0.131 Uiso calc R 1 . . H
H2B -0.0755 0.1001 0.3689 0.131 Uiso calc R 1 . . H
H2C -0.2602 -0.0738 0.3562 0.131 Uiso calc R 1 . . H
C3 -0.6890(10) 0.0658(10) 0.0144(6) 0.0615(19) Uani d . 1 . . C
H3A -0.7540 -0.0195 0.0596 0.074 Uiso calc R 1 . . H
H3B -0.6697 0.0021 -0.0580 0.074 Uiso calc R 1 . . H
C4 -0.8040(15) 0.130(2) -0.0493(11) 0.118(4) Uani d . 1 . . C
H4A -0.9208 0.0284 -0.1156 0.177 Uiso calc R 1 . . H
H4B -0.7415 0.2125 -0.0960 0.177 Uiso calc R 1 . . H
H4C -0.8254 0.1915 0.0218 0.177 Uiso calc R 1 . . H
C11 -0.355(3) 0.457(4) 0.8119(17) 0.037(5) Uani d P 0.53(6) A 1 C
C12 -0.244(2) 0.461(3) 0.9329(14) 0.032(4) Uani d P 0.53(6) A 1 C
C11A -0.364(3) 0.379(5) 0.767(4) 0.067(13) Uani d P 0.47(6) A 2 C
C12A -0.247(2) 0.379(5) 0.885(4) 0.061(12) Uani d P 0.47(6) A 2 C
C13 -0.0657(7) 0.4935(7) 0.9359(5) 0.0348(11) Uani d . 1 . . C
C14 -0.0001(9) 0.5655(11) 0.8376(6) 0.0539(17) Uani d . 1 A . C
H14A 0.1254 0.6232 0.8509 0.065 Uiso calc R 1 . . H
C15 -0.1267(9) 0.5493(11) 0.7185(6) 0.0567(19) Uani d . 1 . . C
H15A -0.0828 0.5923 0.6507 0.068 Uiso calc R 1 A . H
P1 -0.44795(17) 0.25775(18) 0.27804(11) 0.0298(3) Uani d . 1 . . P
N1 -0.3062(6) 0.4767(5) 0.6948(4) 0.0309(9) Uani d . 1 A . N
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'
P P 0.1023 0.0942 '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'
Cd Cd -0.8075 1.2024 '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
N1 Cd1 N1 2_466 . 180.0000(10) no
N1 Cd1 S1 2_466 2_466 90.52(12) no
N1 Cd1 S1 . 2_466 89.48(12) no
N1 Cd1 S1 2_466 . 89.48(12) yes
N1 Cd1 S1 . . 90.52(12) yes
S1 Cd1 S1 2_466 . 180.0 no
N1 Cd1 S2 2_466 . 87.03(11) yes
N1 Cd1 S2 . . 92.97(11) yes
S1 Cd1 S2 2_466 . 103.14(5) no
S1 Cd1 S2 . . 76.86(5) yes
N1 Cd1 S2 2_466 2_466 92.97(11) no
N1 Cd1 S2 . 2_466 87.03(11) no
S1 Cd1 S2 2_466 2_466 76.86(5) no
S1 Cd1 S2 . 2_466 103.14(5) no
S2 Cd1 S2 . 2_466 180.0000(10) no
P1 S1 Cd1 . . 83.97(7) no
P1 S2 Cd1 . . 83.97(6) no
C1 O1 P1 . . 120.7(4) no
C3 O2 P1 . . 127.1(5) no
O1 C1 C2 . . 108.1(7) no
O1 C1 H1A . . 110.1 no
C2 C1 H1A . . 110.1 no
O1 C1 H1B . . 110.1 no
C2 C1 H1B . . 110.1 no
H1A C1 H1B . . 108.4 no
C1 C2 H2A . . 109.5 no
C1 C2 H2B . . 109.5 no
H2A C2 H2B . . 109.5 no
C1 C2 H2C . . 109.5 no
H2A C2 H2C . . 109.5 no
H2B C2 H2C . . 109.5 no
O2 C3 C4 . . 112.2(8) no
O2 C3 H3A . . 109.2 no
C4 C3 H3A . . 109.2 no
O2 C3 H3B . . 109.2 no
C4 C3 H3B . . 109.2 no
H3A C3 H3B . . 107.9 no
C3 C4 H4A . . 109.5 no
C3 C4 H4B . . 109.5 no
H4A C4 H4B . . 109.5 no
C3 C4 H4C . . 109.5 no
H4A C4 H4C . . 109.5 no
H4B C4 H4C . . 109.5 no
C12 C11 N1 . . 123.8(12) no
C11 C12 C13 . . 116.3(10) no
N1 C11A C12A . . 123.6(16) no
C13 C12A C11A . . 122.9(13) no
C12A C13 C14 . . 112.1(13) no
C12A C13 C12 . . 33.0(18) no
C14 C13 C12 . . 117.5(6) no
C12A C13 C13 . 2_567 125.7(9) no
C14 C13 C13 . 2_567 119.7(6) no
C12 C13 C13 . 2_567 120.0(7) no
C13 C14 C15 . . 118.2(6) no
C13 C14 H14A . . 120.9 no
C15 C14 H14A . . 120.9 no
N1 C15 C14 . . 124.6(5) no
N1 C15 H15A . . 117.7 no
C14 C15 H15A . . 117.7 no
O2 P1 O1 . . 98.3(2) no
O2 P1 S2 . . 113.27(18) no
O1 P1 S2 . . 111.0(2) no
O2 P1 S1 . . 107.5(2) no
O1 P1 S1 . . 110.3(2) no
S1 P1 S2 . . 115.20(8) yes
C11A N1 C15 . . 113.4(14) no
C11A N1 C11 . . 31.5(19) no
C15 N1 C11 . . 114.7(9) no
C11A N1 Cd1 . . 125.2(10) no
C15 N1 Cd1 . . 120.6(3) no
C11 N1 Cd1 . . 119.7(6) no
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
Cd1 N1 2_466 2.422(4) no
Cd1 N1 . 2.422(4) yes
Cd1 S1 2_466 2.696(2) no
Cd1 S1 . 2.696(2) yes
Cd1 S2 . 2.701(2) yes
Cd1 S2 2_466 2.701(2) no
P1 S1 . 1.990(2) yes
P1 S2 . 1.983(2) yes
O1 C1 . 1.417(8) no
O1 P1 . 1.596(4) no
O2 C3 . 1.422(7) no
O2 P1 . 1.578(4) no
C1 C2 . 1.518(10) no
C1 H1A . 0.9700 no
C1 H1B . 0.9700 no
C2 H2A . 0.9600 no
C2 H2B . 0.9600 no
C2 H2C . 0.9600 no
C3 C4 . 1.462(12) no
C3 H3A . 0.9700 no
C3 H3B . 0.9700 no
C4 H4A . 0.9600 no
C4 H4B . 0.9600 no
C4 H4C . 0.9600 no
C11 C12 . 1.382(18) no
C11 N1 . 1.393(15) no
C12 C13 . 1.444(12) no
C11A N1 . 1.24(2) no
C11A C12A . 1.39(2) no
C12A C13 . 1.318(15) no
C13 C14 . 1.384(8) no
C13 C13 2_567 1.488(8) no
C14 C15 . 1.388(7) no
C14 H14A . 0.9300 no
C15 N1 . 1.327(7) no
C15 H15A . 0.9300 no
