Alkynyl Complexes of High-Valence Clusters. Synthesis and Luminescence Properties of [Mo6I8(C\τbCC(O)OMe)6]2-, the First Complex with Exclusively Organometallic Outer Ligands in the Family of Octahedral {M6X8} Clusters
Maxim N. Sokolov; Maxim A. Mikhailov; Konstantin A. Brylev; Alexander V. Virovets; Cristian Vicent; Nikolay B. Kompankov; Noboru Kitamura; Vladimir P. Fedin; Inorganic Chemistry 52 (2013) 12477–12481; doi:10.1021/ic401377g

data_4336548
_publ_section_title
;
 Alkynyl Complexes of High-Valence Clusters. Synthesis and Luminescence
 Properties of [Mo6I8(C\\tbCC(O)OMe)6]2-, the First Complex with
 Exclusively Organometallic Outer Ligands in the Family of Octahedral
 {M6X8} Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12477
_journal_page_last               12481
_journal_paper_doi               10.1021/ic401377g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_structural     (PPh4)2[Mo6I8(C3O2Me)6]
_chemical_formula_sum            'C72 H58 I8 Mo6 O12 P2'
_chemical_formula_weight         2767.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.947(2)
_cell_angle_beta                 88.8800(10)
_cell_angle_gamma                76.016(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5340(7)
_cell_length_b                   13.0467(9)
_cell_length_c                   13.4417(8)
_cell_measurement_reflns_used    4310
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      38.5935
_cell_measurement_theta_min      2.1755
_cell_volume                     1961.4(2)
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_device_type  'Bruker X8Apex CCD detector'
_diffrn_measurement_method       'combined omega- and phi-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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24981
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         40.52
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    4.176
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6060
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.343
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.315
_refine_diff_density_min         -1.553
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         20237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                11904
_reflns_number_total             20237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401377g_si_001.cif
_cod_data_source_block           m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4336548