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_7230395
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00  71.00   1.00   35.00    --   26.84 178.00  30.00   36
  2  \w      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       '\w 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/[\s^2^(Fo^2^)+(0.0291P)^2^+433.7857P] where P=(Fo^2^+2Fc^2^)/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