#------------------------------------------------------------------------------
#$Date: 2023-12-04 14:50:57 +0200 (Mon, 04 Dec 2023) $
#$Revision: 287984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501458.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_1501458
loop_
_publ_author_name
'Theivanayagam C. Deivaraj'
'Wei Hoon Lye'
'Jagadese J. Vittal'
_publ_contact_author_address
; Department of Chemistry
  National University of Singapore
  Kent Ridge
  Singapore 117543 
;
_publ_contact_author_email       chmjjv@nus.edu.sg
_publ_contact_author_fax         '(65) 874 2975'
_publ_contact_author_name        'Jagadese J. Vittal'
_publ_contact_author_phone       '(65) 779 1691'
_publ_section_title
;
 New Metalloligands [M(SC{O}Ph)4]-: Synthesis and Characterization of
 Polymeric [A(MeCN)x{M(SC{O}Ph)4}] Compounds (A = Li, Na and K; M = Ga and
 In; x= 0-2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3755
_journal_page_last               3760
_journal_paper_doi               10.1021/ic025533i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H26 K N2 O4 S4'
_chemical_formula_weight         784.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.356(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.307(3)
_cell_length_b                   13.672(3)
_cell_length_c                   20.575(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     3459.0(13)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_method       'ω 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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21042
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.7079
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plates, cut'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0288P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                5896
_reflns_number_total             7870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025533i_s1_1.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3458.8(12)
_cod_original_formula_sum        'C32 H26  K N2 O4 S4'
_cod_database_code               1501458
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
In1 In 0.554999(14) 0.228321(13) 0.220503(9) 0.03393(6) Uani 1 1 d . . .
K1 K 0.75709(4) 0.47198(4) 0.30440(3) 0.03944(14) Uani 1 1 d . . .
S1 S 0.68113(5) 0.22993(5) 0.13123(3) 0.04275(17) Uani 1 1 d . . .
S2 S 0.39488(5) 0.33901(5) 0.19808(3) 0.04127(17) Uani 1 1 d . . .
S3 S 0.46139(5) 0.06536(5) 0.21631(3) 0.04133(17) Uani 1 1 d . . .
S4 S 0.59837(6) 0.25250(5) 0.33851(3) 0.04109(17) Uani 1 1 d . . .
O1 O 0.79291(13) 0.32028(13) 0.22456(9) 0.0433(4) Uani 1 1 d . . .
O2 O 0.57948(12) 0.42502(12) 0.22223(8) 0.0409(4) Uani 1 1 d . . .
O3 O 0.45247(15) 0.14298(14) 0.09998(9) 0.0539(5) Uani 1 1 d . . .
O4 O 0.70482(13) 0.10651(13) 0.29055(8) 0.0411(4) Uani 1 1 d . . .
C1 C 0.78835(19) 0.29932(18) 0.16709(13) 0.0347(6) Uani 1 1 d . . .
C2 C 0.48168(19) 0.43835(18) 0.20965(11) 0.0327(6) Uani 1 1 d . . .
C3 C 0.4163(2) 0.07934(19) 0.13443(13) 0.0376(6) Uani 1 1 d . . .
C4 C 0.68960(19) 0.15381(18) 0.34000(12) 0.0344(6) Uani 1 1 d . . .
N1 N 0.9055(2) 0.38477(19) 0.39508(13) 0.0578(7) Uani 1 1 d . . .
C5 C 0.9664(2) 0.3353(2) 0.42105(14) 0.0485(7) Uani 1 1 d . . .
C6 C 1.0443(3) 0.2711(2) 0.45536(16) 0.0656(9) Uani 1 1 d . . .
H6A H 1.1176 0.2885 0.4440 0.098 Uiso 1 1 calc R . .
H6B H 1.0298 0.2037 0.4430 0.098 Uiso 1 1 calc R . .
H6C H 1.0374 0.2783 0.5019 0.098 Uiso 1 1 calc R . .
C7 C 0.5040(3) 0.5975(2) 0.37778(15) 0.0537(8) Uani 1 1 d . . .
N2 N 0.5790(2) 0.5524(2) 0.36986(13) 0.0626(7) Uani 1 1 d . . .
C8 C 0.4084(2) 0.6569(2) 0.38706(19) 0.0750(11) Uani 1 1 d . . .
H8A H 0.3588 0.6507 0.3494 0.112 Uiso 1 1 calc R . .
H8B H 0.4298 0.7248 0.3924 0.112 Uiso 1 1 calc R . .
H8C H 0.3725 0.6350 0.4256 0.112 Uiso 1 1 calc R . .
C1A C 0.87272(19) 0.33515(17) 0.12229(13) 0.0356(6) Uani 1 1 d . . .
C2A C 0.9550(2) 0.39439(19) 0.14820(15) 0.0479(7) Uani 1 1 d . . .
H2A H 0.9567 0.4105 0.1926 0.058 Uiso 1 1 calc R . .
C3A C 1.0345(2) 0.4299(2) 0.10896(19) 0.0609(9) Uani 1 1 d . . .
H3A H 1.0897 0.4703 0.1269 0.073 Uiso 1 1 calc R . .
C4A C 1.0336(2) 0.4068(2) 0.04426(19) 0.0605(9) Uani 1 1 d . . .
H4A H 1.0885 0.4306 0.0181 0.073 Uiso 1 1 calc R . .
C5A C 0.9526(3) 0.3488(2) 0.01766(16) 0.0582(8) Uani 1 1 d . . .
H5A H 0.9516 0.3334 -0.0269 0.070 Uiso 1 1 calc R . .
C6A C 0.8716(2) 0.3126(2) 0.05655(14) 0.0463(7) Uani 1 1 d . . .
H6A1 H 0.8162 0.2728 0.0382 0.056 Uiso 1 1 calc R . .
C1B C 0.43702(19) 0.53978(18) 0.20492(12) 0.0334(6) Uani 1 1 d . . .
C2B C 0.5080(2) 0.61799(19) 0.21433(12) 0.0414(6) Uani 1 1 d . . .
H2B H 0.5830 0.6064 0.2201 0.050 Uiso 1 1 calc R . .
C3B C 0.4693(3) 0.7122(2) 0.21520(14) 0.0522(8) Uani 1 1 d . . .
H3B H 0.5178 0.7648 0.2216 0.063 Uiso 1 1 calc R . .
C4B C 0.3600(3) 0.7295(2) 0.20670(16) 0.0630(9) Uani 1 1 d . . .
H4B H 0.3336 0.7939 0.2084 0.076 Uiso 1 1 calc R . .
C5B C 0.2887(2) 0.6532(2) 0.19563(16) 0.0598(9) Uani 1 1 d . . .
H5B H 0.2140 0.6657 0.1886 0.072 Uiso 1 1 calc R . .
C6B C 0.3270(2) 0.5580(2) 0.19479(14) 0.0458(7) Uani 1 1 d . . .
H6B1 H 0.2784 0.5057 0.1874 0.055 Uiso 1 1 calc R . .
C1C C 0.32943(19) 0.01217(18) 0.10830(12) 0.0355(6) Uani 1 1 d . . .
C2C C 0.2618(2) -0.03948(18) 0.14786(13) 0.0390(6) Uani 1 1 d . . .
H2C H 0.2739 -0.0374 0.1933 0.047 Uiso 1 1 calc R . .
C3C C 0.1768(2) -0.09400(19) 0.12138(15) 0.0471(7) Uani 1 1 d . . .
H3C H 0.1307 -0.1283 0.1487 0.057 Uiso 1 1 calc R . .
C4C C 0.1596(2) -0.0981(2) 0.05504(16) 0.0581(8) Uani 1 1 d . . .
H4C H 0.1006 -0.1340 0.0370 0.070 Uiso 1 1 calc R . .
C5C C 0.2285(3) -0.0496(2) 0.01493(16) 0.0658(9) Uani 1 1 d . . .
H5C H 0.2182 -0.0545 -0.0305 0.079 Uiso 1 1 calc R . .
C6C C 0.3124(2) 0.0061(2) 0.04147(14) 0.0541(8) Uani 1 1 d . . .
H6C1 H 0.3584 0.0402 0.0140 0.065 Uiso 1 1 calc R . .
C1D C 0.74630(18) 0.12916(18) 0.40320(12) 0.0334(6) Uani 1 1 d . . .
C2D C 0.7977(2) 0.03900(19) 0.40867(13) 0.0436(7) Uani 1 1 d . . .
H2D H 0.7973 -0.0035 0.3728 0.052 Uiso 1 1 calc R . .
C3D C 0.8497(2) 0.0114(2) 0.46677(15) 0.0539(8) Uani 1 1 d . . .
H3D H 0.8827 -0.0504 0.4707 0.065 Uiso 1 1 calc R . .
C4D C 0.8526(2) 0.0749(3) 0.51864(14) 0.0582(9) Uani 1 1 d . . .
H4D H 0.8881 0.0562 0.5580 0.070 Uiso 1 1 calc R . .
C5D C 0.8044(2) 0.1651(2) 0.51355(14) 0.0540(8) Uani 1 1 d . . .
H5D H 0.8083 0.2085 0.5490 0.065 Uiso 1 1 calc R . .
C6D C 0.7499(2) 0.1924(2) 0.45612(12) 0.0410(6) Uani 1 1 d . . .
H6D H 0.7154 0.2536 0.4530 0.049 Uiso 1 1 calc R . .
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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
S1 In1 S4 127.80(3) . . ?
S1 In1 S3 106.62(2) . . ?
S4 In1 S3 103.39(2) . . ?
S1 In1 S2 111.88(3) . . ?
S4 In1 S2 103.56(2) . . ?
S3 In1 S2 99.97(3) . . ?
O1 K1 O4 92.58(6) . 2_655 ?
O1 K1 O2 66.17(5) . . ?
O4 K1 O2 82.80(5) 2_655 . ?
O1 K1 N1 87.72(7) . . ?
O4 K1 N1 129.11(6) 2_655 . ?
O2 K1 N1 140.83(7) . . ?
O1 K1 N2 137.39(7) . . ?
O4 K1 N2 103.68(7) 2_655 . ?
O2 K1 N2 77.01(7) . . ?
N1 K1 N2 109.95(8) . . ?
O1 K1 S4 65.67(4) . . ?
O4 K1 S4 142.67(4) 2_655 . ?
O2 K1 S4 61.04(4) . . ?
N1 K1 S4 82.12(5) . . ?
N2 K1 S4 78.36(6) . . ?
O1 K1 S3 91.02(4) . 2_655 ?
O4 K1 S3 60.12(4) 2_655 2_655 ?
O2 K1 S3 135.97(4) . 2_655 ?
N1 K1 S3 68.99(5) . 2_655 ?
N2 K1 S3 131.27(6) . 2_655 ?
S4 K1 S3 143.76(2) . 2_655 ?
C1 S1 In1 100.21(9) . . ?
C2 S2 In1 88.43(8) . . ?
C3 S3 In1 93.59(9) . . ?
C3 S3 K1 100.68(9) . 2_645 ?
In1 S3 K1 83.14(2) . 2_645 ?
C4 S4 In1 91.51(9) . . ?
C4 S4 K1 106.69(8) . . ?
In1 S4 K1 90.95(2) . . ?
C1 O1 K1 140.59(17) . . ?
C2 O2 K1 145.92(16) . . ?
C4 O4 K1 169.34(17) . 2_645 ?
O1 C1 C1A 121.0(2) . . ?
O1 C1 S1 122.5(2) . . ?
C1A C1 S1 116.37(19) . . ?
O2 C2 C1B 120.3(2) . . ?
O2 C2 S2 120.12(19) . . ?
C1B C2 S2 119.62(18) . . ?
O3 C3 C1C 120.2(2) . . ?
O3 C3 S3 121.7(2) . . ?
C1C C3 S3 118.05(19) . . ?
O4 C4 C1D 121.5(2) . . ?
O4 C4 S4 120.69(19) . . ?
C1D C4 S4 117.76(19) . . ?
C5 N1 K1 165.1(2) . . ?
N1 C5 C6 179.3(3) . . ?
N2 C7 C8 178.9(4) . . ?
C7 N2 K1 158.8(3) . . ?
C2A C1A C6A 118.9(3) . . ?
C2A C1A C1 117.9(2) . . ?
C6A C1A C1 123.2(2) . . ?
C3A C2A C1A 120.3(3) . . ?
C4A C3A C2A 120.7(3) . . ?
C3A C4A C5A 119.9(3) . . ?
C4A C5A C6A 120.1(3) . . ?
C1A C6A C5A 120.1(3) . . ?
C6B C1B C2B 119.2(2) . . ?
C6B C1B C2 122.1(2) . . ?
C2B C1B C2 118.6(2) . . ?
C3B C2B C1B 120.5(3) . . ?
C4B C3B C2B 119.9(3) . . ?
C3B C4B C5B 120.5(3) . . ?
C4B C5B C6B 119.9(3) . . ?
C1B C6B C5B 119.9(3) . . ?
C2C C1C C6C 118.9(2) . . ?
C2C C1C C3 122.8(2) . . ?
C6C C1C C3 118.1(2) . . ?
C3C C2C C1C 120.6(3) . . ?
C4C C3C C2C 119.9(3) . . ?
C3C C4C C5C 120.2(3) . . ?
C4C C5C C6C 119.9(3) . . ?
C5C C6C C1C 120.5(3) . . ?
C2D C1D C6D 119.3(2) . . ?
C2D C1D C4 117.9(2) . . ?
C6D C1D C4 122.9(2) . . ?
C3D C2D C1D 120.3(3) . . ?
C4D C3D C2D 119.6(3) . . ?
C5D C4D C3D 120.8(3) . . ?
C4D C5D C6D 120.0(3) . . ?
C5D C6D C1D 120.0(3) . . ?
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
In1 S1 2.4532(8) . ?
In1 S4 2.4865(8) . ?
In1 S3 2.5080(8) . ?
In1 S2 2.5122(8) . ?
K1 O1 2.6932(19) . ?
K1 O4 2.7376(19) 2_655 ?
K1 O2 2.7829(18) . ?
K1 N1 2.821(3) . ?
K1 N2 2.841(3) . ?
K1 S4 3.6640(11) . ?
K1 S3 3.7331(11) 2_655 ?
S1 C1 1.762(3) . ?
S2 C2 1.738(2) . ?
S3 C3 1.762(3) . ?
S3 K1 3.7331(11) 2_645 ?
S4 C4 1.755(3) . ?
O1 C1 1.216(3) . ?
O2 C2 1.234(3) . ?
O3 C3 1.218(3) . ?
O4 C4 1.226(3) . ?
O4 K1 2.7376(19) 2_645 ?
C1 C1A 1.499(3) . ?
C2 C1B 1.493(3) . ?
C3 C1C 1.493(3) . ?
C4 C1D 1.489(3) . ?
N1 C5 1.127(3) . ?
C5 C6 1.462(4) . ?
C7 N2 1.128(4) . ?
C7 C8 1.449(4) . ?
C1A C2A 1.386(3) . ?
C1A C6A 1.387(4) . ?
C2A C3A 1.382(4) . ?
C3A C4A 1.368(4) . ?
C4A C5A 1.370(4) . ?
C5A C6A 1.394(4) . ?
C1B C6B 1.383(3) . ?
C1B C2B 1.389(3) . ?
C2B C3B 1.373(4) . ?
C3B C4B 1.370(4) . ?
C4B C5B 1.376(4) . ?
C5B C6B 1.386(4) . ?
C1C C2C 1.382(3) . ?
C1C C6C 1.385(4) . ?
C2C C3C 1.379(3) . ?
C3C C4C 1.374(4) . ?
C4C C5C 1.377(4) . ?
C5C C6C 1.378(4) . ?
C1D C2D 1.388(3) . ?
C1D C6D 1.389(3) . ?
C2D C3D 1.385(4) . ?
C3D C4D 1.375(4) . ?
C4D C5D 1.371(4) . ?
C5D C6D 1.385(4) . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2023-12-04T14:50:13+02:00
;
 Changed the atom site label from '1' to 'In1' in multiple data loops for
 consistency and readability.
;
