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_7103895
_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(DAniF)2]2Cl4,2(CH2Cl2)'
_chemical_formula_sum            'C62 H64 Cl8 Mo4 N8 O8'
_chemical_formula_weight         1716.57
_chemical_name_common            (Mo2(DAniF)2)2Cl4,2CH2Cl2
_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                 98.7730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7836(7)
_cell_length_b                   12.3312(7)
_cell_length_c                   23.8669(14)
_cell_measurement_reflns_used    17925
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5225
_cell_measurement_theta_min      2.3895
_cell_volume                     3427.4(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SAMRT
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18908
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.8654
_exptl_absorpt_correction_T_min  0.7895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.934
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.076
_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     382
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0384P)^2^+7.3468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                5405
_reflns_number_total             6023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306822f.txt
_cod_data_source_block           cmpd1
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7103895