Synthetic Tuning of Redox, Spectroscopic, and Photophysical Properties of {Mo6I8}(4+) Core Cluster Complexes by Terminal Carboxylate Ligands.
Mikhailov, Maxim A.; Brylev, Konstantin A.; Abramov, Pavel A.; Sakuda, Eri; Akagi, Soichiro; Ito, Akitaka; Kitamura, Noboru; Sokolov, Maxim N.; Inorganic chemistry 55 (2016) 8437–8445; doi:10.1021/acs.inorgchem.6b01042

data_4348160
_publ_section_title
;
 Synthetic Tuning of Redox, Spectroscopic, and Photophysical Properties of
 {Mo6I8}(4+) Core Cluster Complexes by Terminal Carboxylate Ligands.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8437
_journal_page_last               8445
_journal_paper_doi               10.1021/acs.inorgchem.6b01042
_journal_volume                  55
_journal_year                    2016
_chemical_formula_structural     ((C4H9)4N)2[Mo6I8(O2CC2F5)6]
_chemical_formula_sum            'C50 H72 F30 I8 Mo6 N2 O12'
_chemical_formula_weight         3053.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.9590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5244(5)
_cell_length_b                   21.0853(8)
_cell_length_c                   16.6103(5)
_cell_measurement_reflns_used    9402
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.65
_cell_volume                     4217.4(3)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         1.817
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.909
_exptl_absorpt_correction_T_max  0.651
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    2.405
_exptl_crystal_description       brown
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.726
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9699
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+30.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8254
_reflns_number_total             9699
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b01042_si_001.cif
_cod_data_source_block           814n
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4348160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.480
_shelx_estimated_absorpt_t_max   0.651
_shelx_res_checksum              10307
_shelx_hkl_checksum              5095