The Extraordinary Ability of Guanidinate Derivatives to Stabilize Higher Oxidation Numbers in Dimetal Units by Modification of Redox Potentials: Structures of Mo25+ and Mo26+ Compounds
F. Albert Cotton; Lee M. Daniels; Carlos A. Murillo; Daren J. Timmons; Chad C. Wilkinson; Journal of the American Chemical Society 124 (2002) 9249–9256; doi:10.1021/ja0266464

data_4115010
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, P.O. Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 The Extraordinary Ability of Guanidinate Derivatives to Stabilize Higher
 Oxidation Numbers in Dimetal Units by Modification of Redox Potentials:
 Structures of Mo25+ and Mo26+ Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9249
_journal_page_last               9256
_journal_paper_doi               10.1021/ja0266464
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         Mo2(hpp)4Cl.2CH2Cl2
_chemical_formula_sum            'C30 H52 Cl5 Mo2 N12'
_chemical_formula_weight         949.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6912(8)
_cell_length_b                   13.6912(8)
_cell_length_c                   20.4755(12)
_cell_measurement_reflns_used    6054
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.895
_cell_volume                     3838.1(4)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART'
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0080
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21709
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.578664
_exptl_absorpt_correction_T_min  0.502988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00136(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2223
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+2.7795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                1936
_reflns_number_total             2223
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0266464_s2_3.cif
_cod_data_source_block           compound22CH2CL2
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               4115010