A highly emissive inorganic hexamolybdenum cluster complex as a handy precursor for the preparation of new luminescent materials.
Efremova, O. A.; Shestopalov, M. A.; Chirtsova, N. A.; Smolentsev, A. I.; Mironov, Y. V.; Kitamura, N.; Brylev, K. A.; Sutherland, A. J.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 6021–6025; doi:10.1039/c3dt53126k

data_7029510
_publ_section_title
;
 A highly emissive inorganic hexamolybdenum cluster complex as a handy
 precursor for the preparation of new luminescent materials.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6021
_journal_page_last               6025
_journal_paper_doi               10.1039/c3dt53126k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'I8 Mo6 N6 O18, 2(C16 H36 N), 3(C3 H6 O)'
_chemical_formula_sum            'C41 H90 I8 Mo6 N8 O21'
_chemical_formula_weight         2622.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.8350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5949(4)
_cell_length_b                   11.4521(3)
_cell_length_c                   22.3086(5)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.27
_cell_volume                     3709.39(16)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18245
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.378
_exptl_absorpt_correction_T_max  0.8108
_exptl_absorpt_correction_T_min  0.3534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The solvent acetone molecules appeared to be highly disordered and it 
was difficult to model their positions reliably. Therefore, the structure 
was treated via PLATON/SQUEEZE (van der Sluis & Spek, 1990; Spek, 2003) 
procedure to remove the contribution of the electron density in the solvent 
regions from the intensity data, and the solvent-free model was employed from 
the final refinement. The total potential solvent accessible void volume was 
estimated to be 582 Ang**3 and the electron count per unit cell was 277, 
which were assigned to 6 acetone molecules per unit cell or 3 acetone 
molecules per formula unit.
;
_refine_diff_density_max         1.644
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0791P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                4994
_reflns_number_total             8462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53126k.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7029510