#------------------------------------------------------------------------------
#$Date: 2023-12-04 14:50:57 +0200 (Mon, 04 Dec 2023) $
#$Revision: 287984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/14/1501460.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_1501460
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            'C30 H23 N Na O4 S4'
_chemical_formula_weight         727.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.121(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5774(7)
_cell_length_b                   21.9723(15)
_cell_length_c                   14.4196(10)
_cell_measurement_reflns_used    5980
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     3146.7(4)
_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 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20502
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_T_max  0.8068
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism, cut'
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.00016(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0250
_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)+(0.0201P)²+1.2767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0557
_reflns_number_gt                6342
_reflns_number_total             7782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025533i_s1_3.cif
_cod_data_source_block           compound4
_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_formula_sum        'C30 H23  N Na O4 S4'
_cod_database_code               1501460
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.204943(13) 0.310613(6) -0.044119(9) 0.04027(5) Uani 1 1 d . . .
S1 S 0.15335(6) 0.22189(2) -0.15805(4) 0.05586(14) Uani 1 1 d . . .
S2 S 0.01712(5) 0.38346(3) -0.08219(4) 0.05221(13) Uani 1 1 d . . .
S3 S 0.33478(5) 0.26649(2) 0.11977(4) 0.04699(11) Uani 1 1 d . . .
S4 S 0.39075(5) 0.36106(2) -0.08348(4) 0.04872(12) Uani 1 1 d . . .
O1 O 0.06217(16) 0.18533(7) -0.02062(11) 0.0562(4) Uani 1 1 d . . .
O2 O 0.00962(16) 0.31163(7) 0.05865(12) 0.0604(4) Uani 1 1 d . . .
O3 O 0.31154(17) 0.38423(7) 0.12021(11) 0.0630(4) Uani 1 1 d . . .
O4 O 0.19804(13) 0.34962(6) -0.25453(10) 0.0467(3) Uani 1 1 d . . .
Na1 Na 0.06694(8) 0.21913(3) 0.13083(5) 0.04408(17) Uani 1 1 d . . .
N1 N -0.1310(2) 0.19694(12) 0.16724(17) 0.0756(6) Uani 1 1 d . . .
C5 C -0.1934(3) 0.20815(13) 0.2134(2) 0.0714(7) Uani 1 1 d . . .
C6 C -0.2728(4) 0.2243(2) 0.2749(3) 0.1306(15) Uani 1 1 d . . .
H6A H -0.2264 0.2557 0.3214 0.196 Uiso 1 1 calc R . .
H6B H -0.2844 0.1886 0.3108 0.196 Uiso 1 1 calc R . .
H6C H -0.3602 0.2393 0.2334 0.196 Uiso 1 1 calc R . .
C1 C 0.08487(18) 0.17121(8) -0.09520(13) 0.0401(4) Uani 1 1 d . . .
C2 C -0.03614(19) 0.35800(8) 0.01285(13) 0.0422(4) Uani 1 1 d . . .
C3 C 0.3640(2) 0.34007(9) 0.16983(14) 0.0450(4) Uani 1 1 d . . .
C4 C 0.31350(19) 0.36701(8) -0.21097(14) 0.0396(4) Uani 1 1 d . . .
C11 C 0.0555(2) 0.10852(8) -0.13676(13) 0.0425(4) Uani 1 1 d . . .
C12 C 0.1005(2) 0.08686(10) -0.21004(15) 0.0518(5) Uani 1 1 d . . .
H12 H 0.1521 0.1120 -0.2359 0.062 Uiso 1 1 calc R . .
C13 C 0.0692(3) 0.02788(11) -0.24536(18) 0.0655(6) Uani 1 1 d . . .
H13 H 0.1000 0.0133 -0.2951 0.079 Uiso 1 1 calc R . .
C14 C -0.0050(3) -0.00875(12) -0.2088(2) 0.0851(9) Uani 1 1 d . . .
H14 H -0.0253 -0.0486 -0.2329 0.102 Uiso 1 1 calc R . .
C15 C -0.0504(4) 0.01221(13) -0.1368(2) 0.1033(12) Uani 1 1 d . . .
H15 H -0.1021 -0.0133 -0.1116 0.124 Uiso 1 1 calc R . .
C16 C -0.0207(3) 0.07086(12) -0.1007(2) 0.0784(8) Uani 1 1 d . . .
H16 H -0.0528 0.0850 -0.0513 0.094 Uiso 1 1 calc R . .
C21 C -0.14081(18) 0.39421(8) 0.03557(13) 0.0396(4) Uani 1 1 d . . .
C22 C -0.2011(2) 0.36879(10) 0.09805(17) 0.0572(5) Uani 1 1 d . . .
H22 H -0.1771 0.3294 0.1234 0.069 Uiso 1 1 calc R . .
C23 C -0.2961(3) 0.40127(12) 0.1230(2) 0.0696(7) Uani 1 1 d . . .
H23 H -0.3371 0.3839 0.1650 0.084 Uiso 1 1 calc R . .
C24 C -0.3311(2) 0.45915(12) 0.08650(19) 0.0664(6) Uani 1 1 d . . .
H24 H -0.3960 0.4811 0.1039 0.080 Uiso 1 1 calc R . .
C25 C -0.2722(2) 0.48491(10) 0.02513(17) 0.0572(5) Uani 1 1 d . . .
H25 H -0.2965 0.5244 0.0003 0.069 Uiso 1 1 calc R . .
C26 C -0.1767(2) 0.45265(9) -0.00031(14) 0.0464(4) Uani 1 1 d . . .
H26 H -0.1358 0.4704 -0.0422 0.056 Uiso 1 1 calc R . .
C31 C 0.4605(2) 0.34686(9) 0.27232(14) 0.0453(4) Uani 1 1 d . . .
C32 C 0.4940(2) 0.29926(11) 0.33908(15) 0.0572(5) Uani 1 1 d . . .
H32 H 0.4512 0.2613 0.3217 0.069 Uiso 1 1 calc R . .
C33 C 0.5911(3) 0.30758(14) 0.43201(18) 0.0795(8) Uani 1 1 d . . .
H33 H 0.6136 0.2755 0.4779 0.095 Uiso 1 1 calc R . .
C34 C 0.6540(3) 0.36294(16) 0.4563(2) 0.0911(9) Uani 1 1 d . . .
H34 H 0.7218 0.3682 0.5182 0.109 Uiso 1 1 calc R . .
C35 C 0.6193(3) 0.41017(14) 0.3920(2) 0.0831(8) Uani 1 1 d . . .
H35 H 0.6621 0.4480 0.4099 0.100 Uiso 1 1 calc R . .
C36 C 0.5214(2) 0.40293(11) 0.30018(17) 0.0605(6) Uani 1 1 d . . .
H36 H 0.4962 0.4361 0.2565 0.073 Uiso 1 1 calc R . .
C41 C 0.3957(2) 0.39449(8) -0.26642(15) 0.0454(4) Uani 1 1 d . . .
C42 C 0.3417(2) 0.39760(10) -0.36817(16) 0.0557(5) Uani 1 1 d . . .
H42 H 0.2535 0.3838 -0.4011 0.067 Uiso 1 1 calc R . .
C43 C 0.4168(3) 0.42097(12) -0.4220(2) 0.0771(8) Uani 1 1 d . . .
H43 H 0.3798 0.4229 -0.4913 0.093 Uiso 1 1 calc R . .
C44 C 0.5459(3) 0.44140(14) -0.3736(2) 0.0863(9) Uani 1 1 d . . .
H44 H 0.5972 0.4571 -0.4100 0.104 Uiso 1 1 calc R . .
C45 C 0.5995(3) 0.43888(15) -0.2732(2) 0.0917(10) Uani 1 1 d . . .
H45 H 0.6873 0.4533 -0.2406 0.110 Uiso 1 1 calc R . .
C46 C 0.5254(2) 0.41515(12) -0.21864(19) 0.0678(7) Uani 1 1 d . . .
H46 H 0.5633 0.4131 -0.1494 0.081 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'
Na Na 0.0362 0.0249 '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'
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
S2 In1 S3 127.245(18) . . ?
S2 In1 S1 112.68(2) . . ?
S3 In1 S1 104.262(19) . . ?
S2 In1 S4 107.45(2) . . ?
S3 In1 S4 99.750(18) . . ?
S1 In1 S4 102.115(18) . . ?
C1 S1 In1 101.16(6) . . ?
C1 S1 Na1 137.14(7) . 4_565 ?
In1 S1 Na1 103.98(2) . 4_565 ?
C2 S2 In1 94.03(6) . . ?
C3 S3 In1 89.62(7) . . ?
C3 S3 Na1 109.03(7) . . ?
In1 S3 Na1 87.92(2) . . ?
C4 S4 In1 98.85(6) . . ?
C1 O1 Na1 167.54(14) . . ?
C2 O2 Na1 171.91(16) . . ?
C4 O4 Na1 144.61(12) . 4_565 ?
O2 Na1 O1 86.46(6) . . ?
O2 Na1 O4 155.77(7) . 4_566 ?
O1 Na1 O4 106.29(6) . 4_566 ?
O2 Na1 N1 99.69(8) . . ?
O1 Na1 N1 114.31(8) . . ?
O4 Na1 N1 93.74(7) 4_566 . ?
O2 Na1 S3 77.20(5) . . ?
O1 Na1 S3 77.21(4) . . ?
O4 Na1 S3 85.50(4) 4_566 . ?
N1 Na1 S3 168.06(7) . . ?
O2 Na1 S1 91.02(5) . 4_566 ?
O1 Na1 S1 164.00(5) . 4_566 ?
O4 Na1 S1 70.98(4) 4_566 4_566 ?
N1 Na1 S1 81.68(6) . 4_566 ?
S3 Na1 S1 86.82(3) . 4_566 ?
C5 N1 Na1 146.5(2) . . ?
N1 C5 C6 178.4(4) . . ?
O1 C1 C11 120.80(17) . . ?
O1 C1 S1 122.61(15) . . ?
C11 C1 S1 116.59(13) . . ?
O2 C2 C21 120.92(17) . . ?
O2 C2 S2 121.21(15) . . ?
C21 C2 S2 117.86(13) . . ?
O3 C3 C31 121.43(19) . . ?
O3 C3 S3 120.76(16) . . ?
C31 C3 S3 117.72(15) . . ?
O4 C4 C41 120.76(17) . . ?
O4 C4 S4 122.71(14) . . ?
C41 C4 S4 116.53(14) . . ?
C16 C11 C12 118.81(19) . . ?
C16 C11 C1 118.13(18) . . ?
C12 C11 C1 123.07(18) . . ?
C11 C12 C13 120.0(2) . . ?
C14 C13 C12 120.6(2) . . ?
C13 C14 C15 120.0(2) . . ?
C14 C15 C16 120.4(3) . . ?
C11 C16 C15 120.2(2) . . ?
C26 C21 C22 119.11(18) . . ?
C26 C21 C2 122.78(17) . . ?
C22 C21 C2 118.07(17) . . ?
C23 C22 C21 120.0(2) . . ?
C22 C23 C24 120.2(2) . . ?
C25 C24 C23 120.4(2) . . ?
C24 C25 C26 119.8(2) . . ?
C25 C26 C21 120.44(19) . . ?
C32 C31 C36 119.3(2) . . ?
C32 C31 C3 122.70(19) . . ?
C36 C31 C3 118.01(19) . . ?
C31 C32 C33 119.9(2) . . ?
C34 C33 C32 119.7(3) . . ?
C35 C34 C33 120.6(3) . . ?
C34 C35 C36 120.4(3) . . ?
C35 C36 C31 120.1(2) . . ?
C42 C41 C46 119.34(19) . . ?
C42 C41 C4 118.94(18) . . ?
C46 C41 C4 121.70(19) . . ?
C41 C42 C43 120.4(2) . . ?
C44 C43 C42 119.8(3) . . ?
C45 C44 C43 120.2(2) . . ?
C44 C45 C46 120.5(3) . . ?
C41 C46 C45 119.8(2) . . ?
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 S2 2.4617(5) . ?
In1 S3 2.4856(5) . ?
In1 S1 2.4859(5) . ?
In1 S4 2.4861(5) . ?
S1 C1 1.7429(19) . ?
S1 Na1 3.1413(9) 4_565 ?
S2 C2 1.7434(19) . ?
S3 C3 1.754(2) . ?
S3 Na1 3.0733(9) . ?
S4 C4 1.7409(19) . ?
O1 C1 1.220(2) . ?
O1 Na1 2.2908(15) . ?
O2 C2 1.220(2) . ?
O2 Na1 2.2688(15) . ?
O3 C3 1.220(2) . ?
O4 C4 1.226(2) . ?
O4 Na1 2.3152(14) 4_565 ?
Na1 O4 2.3152(14) 4_566 ?
Na1 N1 2.377(2) . ?
Na1 S1 3.1413(9) 4_566 ?
N1 C5 1.114(3) . ?
C5 C6 1.459(4) . ?
C1 C11 1.492(3) . ?
C2 C21 1.488(3) . ?
C3 C31 1.487(3) . ?
C4 C41 1.496(3) . ?
C11 C16 1.376(3) . ?
C11 C12 1.384(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.352(4) . ?
C14 C15 1.365(4) . ?
C15 C16 1.385(4) . ?
C21 C26 1.388(3) . ?
C21 C22 1.388(3) . ?
C22 C23 1.377(3) . ?
C23 C24 1.377(3) . ?
C24 C25 1.368(3) . ?
C25 C26 1.383(3) . ?
C31 C32 1.383(3) . ?
C31 C36 1.384(3) . ?
C32 C33 1.392(3) . ?
C33 C34 1.373(4) . ?
C34 C35 1.356(4) . ?
C35 C36 1.380(3) . ?
C41 C42 1.381(3) . ?
C41 C46 1.383(3) . ?
C42 C43 1.386(3) . ?
C43 C44 1.377(4) . ?
C44 C45 1.363(4) . ?
C45 C46 1.389(3) . ?
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.
;
