A mixed-valence compound with one unpaired electron delocalized over four molybdenum atoms in a cyclic tetranuclear ion
Cotton, F. Albert; Liu, Chun Y.; Murillo, Carlos A.; Wang, Xiaoping; Chemical Communications (Cambridge, United Kingdom)  (2003) 2190–2191; doi:10.1039/b306822f

data_7113845
_publ_section_title
;
 A mixed-valence compound with one unpaired electron delocalized over four
 molybdenum atoms in a cyclic tetranuclear ion
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   17
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2190
_journal_page_last               2191
_journal_paper_doi               10.1039/b306822f
_journal_year                    2003
_chemical_formula_moiety         '[Mo2(C15H15N2O2)2]2Cl4(PF6)'
_chemical_formula_sum            'C60 H60 Cl4 F6 Mo4 N8 O8 P'
_chemical_formula_weight         1691.69
_chemical_name_common            (Mo2(DAniF)2)2Cl4(PF6)
_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                69.1150(10)
_cell_angle_beta                 68.2310(10)
_cell_angle_gamma                67.4780(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8175(8)
_cell_length_b                   13.0151(10)
_cell_length_c                   14.2603(10)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.008
_cell_measurement_theta_min      2.1705
_cell_volume                     1667.7(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'BRUKER-SMART 1000'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9524
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             845
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.8572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                5660
_reflns_number_total             6432
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103896
_cod_data_source_file            b306822f.txt
_cod_data_source_block           cmpd2
_cod_database_code               7113845