#------------------------------------------------------------------------------
#$Date: 2025-08-23 00:12:46 +0300 (Sat, 23 Aug 2025) $
#$Revision: 301866 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/03/7230395.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_7230395
loop_
_publ_author_name
'Kumar, Ashwani'
'Pradeep, Chullikkattil P.'
_publ_section_title
;
 Aromatic sulfonium polyoxomolybdates: tuning the photochromic properties
 through substitutions on the counter ion moiety
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00345A
_journal_year                    2018
_chemical_formula_moiety         'Mo12 O40 P1, 3(C9 H13 S)'
_chemical_formula_sum            'C27 H39 Mo12 O40 P S3'
_chemical_formula_weight         2282.01
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-02-23
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.3393(3)
_cell_length_b                   20.3393(3)
_cell_length_c                   23.9935(4)
_cell_measurement_reflns_used    3696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1180
_cell_measurement_theta_min      2.4460
_cell_volume                     8596.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122

Alert level B

PLAT430_ALERT_2_B Short Inter D...A Contact O14 ..O14 2.81 Ang

discussion: Short Inter D...A Contact might have arisen due to less intensely scattered oxygen atoms of cluster
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9852
_diffrn_measured_fraction_theta_max 0.8620
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  71.00   1.00   35.00    --   26.84 178.00  30.00   36
  2  ω      8.00  97.00   1.00   35.00    --   26.84  57.00 120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388350000
_diffrn_orient_matrix_UB_12      -0.0283529000
_diffrn_orient_matrix_UB_13      -0.0019554000
_diffrn_orient_matrix_UB_21      0.0090452000
_diffrn_orient_matrix_UB_22      -0.0277330000
_diffrn_orient_matrix_UB_23      0.0090457000
_diffrn_orient_matrix_UB_31      -0.0056048000
_diffrn_orient_matrix_UB_32      0.0069974000
_diffrn_orient_matrix_UB_33      0.0280761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            5544
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trigonal
_exptl_crystal_F_000             6528
_refine_diff_density_max         3.591
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0682
_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)+(0.0291P)²+433.7857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                3736
_reflns_number_total             4121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00345a2.cif
_cod_data_source_block           as_187_rt_mo
_cod_original_cell_volume        8596.0(3)
_cod_database_code               7230395
_chemical_oxdiff_formula         'c h o s p Mo'
_reflns_odcompleteness_completeness 98.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.087
_oxdiff_exptl_absorpt_empirical_full_min 0.875
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 'x+2/3, y+1/3, z+1/3'
5 '-y+2/3, x-y+1/3, z+1/3'
6 '-x+y+2/3, -x+1/3, z+1/3'
7 'x+1/3, y+2/3, z+2/3'
8 '-y+1/3, x-y+2/3, z+2/3'
9 '-x+y+1/3, -x+2/3, z+2/3'
10 '-x, -y, -z'
11 'y, -x+y, -z'
12 'x-y, x, -z'
13 '-x+2/3, -y+1/3, -z+1/3'
14 'y+2/3, -x+y+1/3, -z+1/3'
15 'x-y+2/3, x+1/3, -z+1/3'
16 '-x+1/3, -y+2/3, -z+2/3'
17 'y+1/3, -x+y+2/3, -z+2/3'
18 'x-y+1/3, x+2/3, -z+2/3'
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
Mo1 Mo 0.57155(5) 0.33972(6) 0.67137(3) 0.0408(2) Uani 1 1 d .
Mo6 Mo 0.46516(4) 0.23148(5) 0.54994(4) 0.0406(2) Uani 1 1 d .
Mo11 Mo 0.57021(5) 0.43826(5) 0.54512(4) 0.0363(2) Uani 1 1 d .
Mo19 Mo 0.67235(5) 0.43902(5) 0.42932(3) 0.0361(2) Uani 1 1 d .
P2 P 0.6667 0.3333 0.54907(13) 0.0193(6) Uani 1 3 d S
S4 S 0.66651(17) 0.72619(18) 0.61690(13) 0.0563(7) Uani 1 1 d .
O0AA O 0.5179(5) 0.3401(5) 0.7228(3) 0.066(2) Uani 1 1 d .
O4 O 0.4983(5) 0.2624(4) 0.6223(3) 0.055(2) Uani 1 1 d .
O7 O 0.5732(5) 0.4098(4) 0.6210(3) 0.056(2) Uani 1 1 d .
O13 O 0.5907(4) 0.2602(4) 0.6963(4) 0.0499(18) Uani 1 1 d .
O30 O 0.3714(4) 0.1919(5) 0.5524(3) 0.054(2) Uani 1 1 d .
O6 O 0.4986(5) 0.3349(4) 0.5332(3) 0.0519(19) Uani 1 1 d .
O8 O 0.4755(5) 0.1442(5) 0.5586(3) 0.060(2) Uani 1 1 d .
O11 O 0.7416(4) 0.4060(4) 0.4184(3) 0.0437(17) Uani 1 1 d .
O14 O 0.5173(5) 0.4790(5) 0.5514(3) 0.056(2) Uani 1 1 d .
O16 O 0.4756(5) 0.2200(5) 0.4695(3) 0.055(2) Uani 1 1 d .
O26 O 0.5949(4) 0.4509(4) 0.4687(3) 0.0496(19) Uani 1 1 d .
O31 O 0.6676(4) 0.4051(4) 0.5269(3) 0.0415(15) Uani 1 1 d .
C46 C 0.5744(7) 0.6610(7) 0.5897(5) 0.065(3) Uani 1 1 d .
H46A H 0.5695 0.6118 0.5856 0.097 Uiso 1 1 calc R
H46B H 0.5681 0.6786 0.5540 0.097 Uiso 1 1 calc R
H46C H 0.5362 0.6576 0.6148 0.097 Uiso 1 1 calc R
O2 O 0.6731(5) 0.4790(4) 0.3685(3) 0.0527(19) Uani 1 1 d .
O1 O 0.6667 0.3333 0.6118(5) 0.044(3) Uani 1 3 d S
C2 C 0.6685(6) 0.6790(6) 0.6785(4) 0.041(2) Uani 1 1 d .
C0AA C 0.6386(6) 0.6842(7) 0.7284(5) 0.051(3) Uani 1 1 d .
H0AA H 0.6189 0.7165 0.7329 0.062 Uiso 1 1 calc R
C1 C 0.6389(7) 0.6392(8) 0.7724(5) 0.061(3) Uani 1 1 d .
H1 H 0.6196 0.6420 0.8069 0.073 Uiso 1 1 calc R
C3 C 0.6990(9) 0.6329(9) 0.6723(5) 0.074(4) Uani 1 1 d .
H3 H 0.7209 0.6313 0.6386 0.088 Uiso 1 1 calc R
C4 C 0.6667(8) 0.5916(7) 0.7659(6) 0.066(4) Uani 1 1 d .
C5 C 0.6970(10) 0.5894(8) 0.7161(6) 0.079(5) Uani 1 1 d .
H5 H 0.7169 0.5573 0.7118 0.095 Uiso 1 1 calc R
C1AA C 0.6513(9) 0.8010(7) 0.6391(7) 0.082(5) Uani 1 1 d .
H1AA H 0.6516 0.8298 0.6073 0.123 Uiso 1 1 calc R
H1AB H 0.6909 0.8336 0.6643 0.123 Uiso 1 1 calc R
H1AC H 0.6031 0.7800 0.6576 0.123 Uiso 1 1 calc R
C2AA C 0.6629(12) 0.5393(10) 0.8133(8) 0.120(8) Uani 1 1 d .
H2AA H 0.6722 0.5657 0.8482 0.180 Uiso 1 1 calc R
H2AB H 0.7007 0.5249 0.8075 0.180 Uiso 1 1 calc R
H2AC H 0.6135 0.4947 0.8140 0.180 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'
Mo Mo -1.6832 0.6857 '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'
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
O0AA Mo1 O4 102.6(4) . .
O0AA Mo1 O7 103.9(4) . .
O0AA Mo1 O13 100.5(4) . .
O0AA Mo1 O13 102.3(4) . 3_665
O0AA Mo1 O1 166.9(4) . .
O4 Mo1 O13 84.5(3) . .
O4 Mo1 O1 84.8(3) . .
O7 Mo1 O4 86.5(3) . .
O7 Mo1 O13 155.3(4) . .
O7 Mo1 O13 91.4(3) . 3_665
O7 Mo1 O1 87.2(3) . .
O13 Mo1 O4 154.8(4) 3_665 .
O13 Mo1 O13 87.1(4) 3_665 .
O13 Mo1 O1 69.1(3) . .
O13 Mo1 O1 70.0(3) 3_665 .
O4 Mo6 O6 87.4(3) . .
O4 Mo6 O8 91.3(3) . .
O4 Mo6 O16 156.3(4) . .
O4 Mo6 O31 87.8(3) . 2_655
O30 Mo6 O4 105.4(4) . .
O30 Mo6 O6 103.5(4) . .
O30 Mo6 O8 100.3(4) . .
O30 Mo6 O16 98.3(4) . .
O30 Mo6 O31 164.1(3) . 2_655
O6 Mo6 O16 85.7(3) . .
O6 Mo6 O31 85.7(3) . 2_655
O8 Mo6 O6 155.6(4) . .
O8 Mo6 O16 85.8(3) . .
O8 Mo6 O31 69.9(3) . 2_655
O16 Mo6 O31 69.1(3) . 2_655
O7 Mo11 O31 86.2(3) . .
O6 Mo11 O7 86.0(3) . .
O6 Mo11 O8 156.3(4) . 3_665
O6 Mo11 O31 86.9(3) . .
O8 Mo11 O7 86.6(3) 3_665 .
O8 Mo11 O31 70.2(3) 3_665 .
O14 Mo11 O7 101.0(4) . .
O14 Mo11 O6 103.7(4) . .
O14 Mo11 O8 99.8(4) . 3_665
O14 Mo11 O26 102.4(4) . .
O14 Mo11 O31 167.4(3) . .
O26 Mo11 O7 156.5(4) . .
O26 Mo11 O6 90.5(3) . .
O26 Mo11 O8 87.3(3) . 3_665
O26 Mo11 O31 70.4(3) . .
O11 Mo19 O11 87.1(4) . 2_655
O11 Mo19 O16 91.4(3) . 3_665
O11 Mo19 O26 156.6(3) . .
O11 Mo19 O26 85.5(3) 2_655 .
O11 Mo19 O31 87.9(3) . .
O11 Mo19 O31 85.8(3) 2_655 .
O16 Mo19 O11 156.5(3) 3_665 2_655
O16 Mo19 O26 86.7(3) 3_665 .
O16 Mo19 O31 70.8(3) 3_665 .
O26 Mo19 O31 69.4(3) . .
O2 Mo19 O11 102.5(4) . 2_655
O2 Mo19 O11 103.3(4) . .
O2 Mo19 O16 100.7(4) . 3_665
O2 Mo19 O26 100.0(4) . .
O2 Mo19 O31 166.4(3) . .
O31 P2 O31 108.8(3) 3_665 2_655
O31 P2 O31 108.8(3) 3_665 .
O31 P2 O31 108.8(3) 2_655 .
O1 P2 O31 110.1(3) . .
O1 P2 O31 110.1(3) . 3_665
O1 P2 O31 110.1(3) . 2_655
C2 S4 C46 101.6(5) . .
C2 S4 C1AA 106.0(6) . .
C1AA S4 C46 100.2(7) . .
Mo6 O4 Mo1 148.0(4) . .
Mo1 O7 Mo11 149.0(5) . .
Mo1 O13 Mo1 131.0(4) 2_655 .
Mo11 O6 Mo6 148.2(4) . .
Mo6 O8 Mo11 129.7(5) . 2_655
Mo19 O11 Mo19 147.8(4) . 3_665
Mo19 O16 Mo6 129.2(4) 2_655 .
Mo11 O26 Mo19 129.0(4) . .
Mo11 O31 Mo6 90.2(2) . 3_665
Mo19 O31 Mo6 91.0(2) . 3_665
Mo19 O31 Mo11 91.0(2) . .
P2 O31 Mo6 123.8(4) . 3_665
P2 O31 Mo11 125.0(4) . .
P2 O31 Mo19 125.5(4) . .
Mo1 O1 Mo1 89.7(3) 3_665 .
Mo1 O1 Mo1 89.7(3) 2_655 .
Mo1 O1 Mo1 89.7(3) 2_655 3_665
P2 O1 Mo1 125.5(2) . 2_655
P2 O1 Mo1 125.5(2) . 3_665
P2 O1 Mo1 125.5(2) . .
C0AA C2 S4 123.6(8) . .
C3 C2 S4 115.0(9) . .
C3 C2 C0AA 121.3(10) . .
C2 C0AA C1 117.4(10) . .
C4 C1 C0AA 121.5(12) . .
C5 C3 C2 119.0(12) . .
C1 C4 C5 119.1(12) . .
C1 C4 C2AA 121.1(15) . .
C5 C4 C2AA 119.9(15) . .
C4 C5 C3 121.7(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O0AA 1.650(7) .
Mo1 O4 1.934(7) .
Mo1 O7 1.857(7) .
Mo1 O13 1.938(7) .
Mo1 O13 1.874(7) 3_665
Mo1 O1 2.460(7) .
Mo6 O4 1.854(7) .
Mo6 O30 1.659(7) .
Mo6 O6 1.902(7) .
Mo6 O8 1.900(8) .
Mo6 O16 1.968(7) .
Mo6 O31 2.450(7) 2_655
Mo11 O7 1.921(7) .
Mo11 O6 1.887(7) .
Mo11 O8 1.919(8) 3_665
Mo11 O14 1.661(7) .
Mo11 O26 1.885(7) .
Mo11 O31 2.430(7) .
Mo19 O11 1.919(6) 2_655
Mo19 O11 1.856(7) .
Mo19 O16 1.883(7) 3_665
Mo19 O26 1.953(7) .
Mo19 O31 2.429(7) .
Mo19 O2 1.667(7) .
P2 O31 1.545(7) 2_655
P2 O31 1.545(7) .
P2 O31 1.545(7) 3_665
P2 O1 1.506(12) .
S4 C46 1.792(12) .
S4 C2 1.773(10) .
S4 C1AA 1.779(14) .
O13 Mo1 1.874(7) 2_655
O8 Mo11 1.919(8) 2_655
O11 Mo19 1.920(6) 3_665
O16 Mo19 1.883(7) 2_655
O31 Mo6 2.450(7) 3_665
O1 Mo1 2.460(7) 3_665
O1 Mo1 2.460(7) 2_655
C2 C0AA 1.372(15) .
C2 C3 1.367(15) .
C0AA C1 1.400(17) .
C1 C4 1.352(18) .
C3 C5 1.362(18) .
C4 C5 1.35(2) .
C4 C2AA 1.534(19) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139204548
