#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:43:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/92/2209233.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_2209233
loop_
_publ_author_name
'Nair, Sreekumari P.'
'Mirkovic, Tihana'
'Scholes, Gregory D.'
'Lough, Alan J.'
_publ_section_title
;Poly[(μ₃-O-ethyl
 dithiocarbonato-κ⁵O,S:S,S':S')[(1,10-phenanthroline-κ²N,N')potassium(I)]]
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1317
_journal_page_last               m1319
_journal_paper_doi               10.1107/S1600536806017636
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[K (C3 H5 O S2) (C12 H8 N2)]'
_chemical_formula_moiety         'C15 H13 K N2 O S2'
_chemical_formula_sum            'C15 H13 K N2 O S2'
_chemical_formula_weight         340.49
_chemical_name_systematic
;
Poly[(O-ethyl
 dithiocarbonate-κ3S,S',O)(1,10-phenanthroline-κ2N,N')potassium(I)]
;
_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
_cell_angle_alpha                64.580(3)
_cell_angle_beta                 89.405(4)
_cell_angle_gamma                80.336(5)
_cell_formula_units_Z            2
_cell_length_a                   6.7148(5)
_cell_length_b                   10.5307(7)
_cell_length_c                   12.2614(9)
_cell_measurement_reflns_used    6420
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.1
_cell_volume                     770.12(10)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXTL/PC (Sheldrick, 2001)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0790
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8041
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         4.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SORTAV (Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.530
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0545
_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)+(0.0804P)²+0.0809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                2371
_reflns_number_total             3442
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kj2005.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2209233
_cod_database_fobs_code          2209233
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
K K1 0.30484(10) 0.05784(7) 0.84773(5) 0.0293(2) Uani d . 1
S S1 0.30209(14) 0.22110(9) 1.02625(7) 0.0381(3) Uani d . 1
S S2 0.19758(12) -0.07014(8) 1.15529(7) 0.0322(2) Uani d . 1
O O1 -0.0621(4) 0.1586(2) 1.0921(2) 0.0435(6) Uani d . 1
N N1 0.2568(4) 0.1077(3) 0.6022(2) 0.0292(6) Uani d . 1
N N2 0.2642(4) 0.3366(3) 0.6532(2) 0.0263(6) Uani d . 1
C C1 0.2500(5) -0.0017(3) 0.5752(3) 0.0330(7) Uani d . 1
H H1A 0.2467 -0.0927 0.6399 0.040 Uiso calc R 1
C C2 0.2476(5) 0.0098(4) 0.4573(3) 0.0373(8) Uani d . 1
H H2A 0.2397 -0.0710 0.4428 0.045 Uiso calc R 1
C C3 0.2567(5) 0.1388(3) 0.3635(3) 0.0336(7) Uani d . 1
H H3A 0.2601 0.1483 0.2829 0.040 Uiso calc R 1
C C4 0.2610(4) 0.2575(3) 0.3870(3) 0.0280(7) Uani d . 1
C C5 0.2604(5) 0.3980(3) 0.2914(3) 0.0328(7) Uani d . 1
H H5A 0.2669 0.4106 0.2100 0.039 Uiso calc R 1
C C6 0.2506(5) 0.5123(3) 0.3159(3) 0.0309(7) Uani d . 1
H H6A 0.2435 0.6048 0.2512 0.037 Uiso calc R 1
C C7 0.2508(4) 0.4959(3) 0.4384(3) 0.0278(7) Uani d . 1
C C8 0.2389(5) 0.6133(3) 0.4658(3) 0.0297(7) Uani d . 1
H H8A 0.2293 0.7073 0.4028 0.036 Uiso calc R 1
C C9 0.2411(5) 0.5906(3) 0.5848(3) 0.0307(7) Uani d . 1
H H9A 0.2328 0.6685 0.6054 0.037 Uiso calc R 1
C C10 0.2559(5) 0.4510(3) 0.6751(3) 0.0291(7) Uani d . 1
H H10A 0.2603 0.4367 0.7571 0.035 Uiso calc R 1
C C11 0.2589(4) 0.3596(3) 0.5350(2) 0.0243(6) Uani d . 1
C C12 0.2622(4) 0.2369(3) 0.5088(2) 0.0252(6) Uani d . 1
C C13 0.1384(5) 0.1085(3) 1.0897(2) 0.0285(7) Uani d . 1
C C14 -0.1523(7) 0.3072(4) 1.0281(4) 0.0627(12) Uani d . 1
H H14A -0.2604 0.3186 0.9687 0.075 Uiso calc R 1
H H14B -0.0484 0.3625 0.9834 0.075 Uiso calc R 1
C C15 -0.2372(8) 0.3624(4) 1.1119(4) 0.0647(12) Uani d . 1
H H15A -0.2968 0.4638 1.0669 0.097 Uiso calc R 1
H H15B -0.1299 0.3516 1.1704 0.097 Uiso calc R 1
H H15C -0.3421 0.3091 1.1548 0.097 Uiso calc R 1
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
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 K1 N2 . . 57.77(7) y
N1 K1 O1 . 2_557 88.23(7) y
N2 K1 O1 . 2_557 131.57(7) y
N1 K1 S1 . . 143.08(6) y
N2 K1 S1 . . 85.51(5) y
O1 K1 S1 2_557 . 117.50(5) y
N1 K1 S2 . 2_557 84.61(5) y
N2 K1 S2 . 2_557 92.25(5) y
O1 K1 S2 2_557 2_557 47.47(5) y
S1 K1 S2 . 2_557 93.88(3) y
N1 K1 S2 . 2_657 95.36(6) y
N2 K1 S2 . 2_657 84.39(5) y
O1 K1 S2 2_557 2_657 136.51(5) y
S1 K1 S2 . 2_657 83.74(2) y
S2 K1 S2 2_557 2_657 176.02(3) y
N1 K1 S1 . 2_657 105.62(6) y
N2 K1 S1 . 2_657 133.82(5) y
O1 K1 S1 2_557 2_657 84.81(5) y
S1 K1 S1 . 2_657 102.86(2) y
S2 K1 S1 2_557 2_657 131.39(3) y
S2 K1 S1 2_657 2_657 52.44(2) y
N1 K1 S2 . . 156.96(6) ?
N2 K1 S2 . . 133.38(5) ?
O1 K1 S2 2_557 . 69.80(5) ?
S1 K1 S2 . . 51.69(2) ?
S2 K1 S2 2_557 . 75.51(2) ?
S2 K1 S2 2_657 . 105.28(2) ?
C13 K1 S2 . . 27.92(5) ?
S1 K1 S2 2_657 . 80.00(2) ?
C13 S1 K1 . . 77.65(10) ?
C13 S1 K1 . 2_657 89.63(11) ?
K1 S1 K1 . 2_657 77.14(3) ?
C13 S2 K1 . 2_557 84.95(11) ?
C13 S2 K1 . 2_657 91.13(11) ?
K1 S2 K1 2_557 2_657 176.02(3) ?
C13 S2 K1 . . 71.04(10) ?
K1 S2 K1 2_557 . 104.49(2) ?
K1 S2 K1 2_657 . 74.72(2) ?
C13 O1 C14 . . 122.8(3) ?
C13 O1 K1 . 2_557 112.75(17) ?
C14 O1 K1 . 2_557 120.4(2) ?
C1 N1 C12 . . 117.4(3) ?
C1 N1 K1 . . 119.8(2) ?
C12 N1 K1 . . 122.42(17) ?
C10 N2 C11 . . 117.0(3) ?
C10 N2 K1 . . 120.61(18) ?
C11 N2 K1 . . 122.35(18) ?
N1 C1 C2 . . 123.9(3) ?
N1 C1 H1A . . 118.1 ?
C2 C1 H1A . . 118.1 ?
C3 C2 C1 . . 118.9(3) ?
C3 C2 H2A . . 120.6 ?
C1 C2 H2A . . 120.6 ?
C2 C3 C4 . . 119.4(3) ?
C2 C3 H3A . . 120.3 ?
C4 C3 H3A . . 120.3 ?
C3 C4 C12 . . 118.1(3) ?
C3 C4 C5 . . 122.0(3) ?
C12 C4 C5 . . 119.8(3) ?
C6 C5 C4 . . 120.8(3) ?
C6 C5 H5A . . 119.6 ?
C4 C5 H5A . . 119.6 ?
C5 C6 C7 . . 121.0(3) ?
C5 C6 H6A . . 119.5 ?
C7 C6 H6A . . 119.5 ?
C8 C7 C11 . . 118.1(3) ?
C8 C7 C6 . . 121.9(3) ?
C11 C7 C6 . . 120.0(3) ?
C9 C8 C7 . . 119.1(3) ?
C9 C8 H8A . . 120.4 ?
C7 C8 H8A . . 120.4 ?
C8 C9 C10 . . 118.9(3) ?
C8 C9 H9A . . 120.5 ?
C10 C9 H9A . . 120.5 ?
N2 C10 C9 . . 124.0(3) ?
N2 C10 H10A . . 118.0 ?
C9 C10 H10A . . 118.0 ?
N2 C11 C7 . . 122.8(3) ?
N2 C11 C12 . . 118.0(3) ?
C7 C11 C12 . . 119.2(2) ?
N1 C12 C4 . . 122.3(3) ?
N1 C12 C11 . . 118.6(2) ?
C4 C12 C11 . . 119.1(3) ?
O1 C13 S2 . . 113.1(2) ?
O1 C13 S1 . . 121.3(2) ?
S2 C13 S1 . . 125.6(2) ?
O1 C13 K1 . . 119.78(18) ?
S2 C13 K1 . . 81.04(10) ?
S1 C13 K1 . . 73.16(10) ?
O1 C14 C15 . . 110.5(3) ?
O1 C14 H14A . . 109.5 ?
C15 C14 H14A . . 109.5 ?
O1 C14 H14B . . 109.5 ?
C15 C14 H14B . . 109.5 ?
H14A C14 H14B . . 108.1 ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
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
K1 N1 . 2.837(2) y
K1 N2 . 2.849(2) y
K1 O1 2_557 2.860(2) y
K1 S1 . 3.3116(10) y
K1 S2 2_557 3.3543(10) y
K1 S2 2_657 3.3645(10) y
K1 S1 2_657 3.4011(12) y
S1 C13 . 1.687(3) ?
S2 C13 . 1.673(3) ?
O1 C13 . 1.366(4) ?
O1 C14 . 1.438(4) ?
N1 C1 . 1.336(4) ?
N1 C12 . 1.357(4) ?
N2 C10 . 1.334(4) ?
N2 C11 . 1.364(3) ?
C1 C2 . 1.399(5) ?
C1 H1A . 0.9500 ?
C2 C3 . 1.362(4) ?
C2 H2A . 0.9500 ?
C3 C4 . 1.403(4) ?
C3 H3A . 0.9500 ?
C4 C12 . 1.414(4) ?
C4 C5 . 1.439(4) ?
C5 C6 . 1.352(4) ?
C5 H5A . 0.9500 ?
C6 C7 . 1.436(4) ?
C6 H6A . 0.9500 ?
C7 C8 . 1.404(4) ?
C7 C11 . 1.408(4) ?
C8 C9 . 1.374(4) ?
C8 H8A . 0.9500 ?
C9 C10 . 1.397(4) ?
C9 H9A . 0.9500 ?
C10 H10A . 0.9500 ?
C11 C12 . 1.455(4) ?
C14 C15 . 1.451(5) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 H15A . 0.9800 ?
C15 H15B . 0.9800 ?
C15 H15C . 0.9800 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168308977
