Modulation of photocatalytic properties through counter-ion substitution: tuning the bandgaps of aromatic sulfonium octamolybdates for efficient photo-degradation of rhodamine B.
Singh, Mahender; Pradeep, Chullikkattil P.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 3122–3136; doi:10.1039/d1dt03609b

data_7709341
_publ_section_title
;
 Modulation of photocatalytic properties through counter-ion substitution:
 tuning the bandgaps of aromatic sulfonium octamolybdates for efficient
 photo-degradation of rhodamine B.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3122
_journal_page_last               3136
_journal_paper_doi               10.1039/d1dt03609b
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'Mo8 O26, 4(C8 H10 Cl S), 2(H2 O)'
_chemical_formula_sum            'C32 H44 Cl4 Mo8 O28 S4'
_chemical_formula_weight         1914.214
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-09-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-09-14 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.704(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7572(4)
_cell_length_b                   19.9652(6)
_cell_length_c                   10.5884(3)
_cell_measurement_reflns_used    3621
_cell_measurement_temperature    150.01(11)
_cell_measurement_theta_max      28.0980
_cell_measurement_theta_min      2.2610
_cell_volume                     2754.67(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9897
_diffrn_measured_fraction_theta_max 0.8625
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     48.00 114.00   1.00    6.39    --   26.84 178.00 150.00   66
  2  \w    -13.00  94.00   1.00    6.39    --   26.84  37.00-150.00  107
  3  \w     58.00 109.00   1.00    6.39    --   26.84 178.00   0.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0446489000
_diffrn_orient_matrix_UB_12      0.0198649000
_diffrn_orient_matrix_UB_13      -0.0102757000
_diffrn_orient_matrix_UB_21      -0.0311921000
_diffrn_orient_matrix_UB_22      -0.0283614000
_diffrn_orient_matrix_UB_23      -0.0251671000
_diffrn_orient_matrix_UB_31      -0.0001474000
_diffrn_orient_matrix_UB_32      -0.0078249000
_diffrn_orient_matrix_UB_33      0.0652931000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.9897
_diffrn_reflns_Laue_measured_fraction_max 0.8625
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9379
_diffrn_reflns_point_group_measured_fraction_full 0.9897
_diffrn_reflns_point_group_measured_fraction_max 0.8625
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.87
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1831.427
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.9086
_refine_diff_density_min         -1.0599
_refine_diff_density_rms         0.2398
_refine_ls_d_res_high            0.7478
_refine_ls_d_res_low             10.9122
_refine_ls_goodness_of_fit_ref   1.0409
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0409
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -18
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                4434
_reflns_number_total             5955
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03609b2.cif
_cod_data_source_block           Mo8_Cl_Lt_Mo
_cod_depositor_comments          'Adding full bibliography for 7709341.cif.'
_cod_original_cell_volume        2754.68(15)
_cod_database_code               7709341
_chemical_oxdiff_formula         'C64  H88  Cl8  Mo16  O56  S8  '
_reflns_odcompleteness_completeness 98.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O14(H14a,H14b)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C7(H7), C4(H4), C16(H16), C5(H5), C15(H15), C13(H13)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C9(H9a,H9b,H9c), C2(H2a,H2b,H2c), C10(H10a,H10b,H10c)
;
_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 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.647