Aromatic sulfonium polyoxomolybdates: tuning the photochromic properties through substitutions on the counter ion moiety
Kumar, Ashwani; Pradeep, Chullikkattil P.; CrystEngComm  (2018) –; doi:10.1039/C8CE00345A

data_7230396
_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 O S)'
_chemical_formula_sum            'C27 H39 Mo12 O43 P S3'
_chemical_formula_weight         2330.01
_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     direct
_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                   20.1657(6)
_cell_length_b                   20.1657(6)
_cell_length_c                   24.1757(8)
_cell_measurement_reflns_used    3614
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0800
_cell_measurement_theta_min      2.4470
_cell_volume                     8514.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122

Alert level B

PLAT097_ALERT_2_B Large Reported Max. (Positive) Residual Density 4.82 eA-3
PLAT213_ALERT_2_B Atom O8 has ADP max/min Ratio ..... 4.1 prolat

discussion: Due to the poor quality of diffraction data and small unresolved disorders, alerts like Large Reported Max. (Positive) Residual Density and high ADP max/min Ratio were generated in cluster.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9866
_diffrn_measured_fraction_theta_max 0.8736
_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    -53.00  69.00   1.00   72.50    --   26.84 -77.00-120.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004027000
_diffrn_orient_matrix_UB_12      -0.0102880000
_diffrn_orient_matrix_UB_13      -0.0280901000
_diffrn_orient_matrix_UB_21      0.0381004000
_diffrn_orient_matrix_UB_22      0.0305487000
_diffrn_orient_matrix_UB_23      -0.0027146000
_diffrn_orient_matrix_UB_31      0.0138827000
_diffrn_orient_matrix_UB_32      -0.0246244000
_diffrn_orient_matrix_UB_33      0.0081272000
_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  0.0209
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5396
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trigonal
_exptl_crystal_F_000             6672
_refine_diff_density_max         4.820
_refine_diff_density_min         -2.365
_refine_diff_density_rms         0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0860
_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/[\s^2^(Fo^2^)+(0.0000P)^2^+1506.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                3831
_reflns_number_total             4083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00345a2.cif
_cod_data_source_block           as_194
_cod_original_cell_volume        8514.0(4)
_cod_database_code               7230396
_chemical_oxdiff_formula         'c h o s Mo'
_reflns_odcompleteness_completeness 98.66
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.305
_oxdiff_exptl_absorpt_empirical_full_min 0.824