Lewis Acid Enhanced Axial Ligation of [Mo2]4+ Complexes
Brian S. Dolinar; John F. Berry; Inorganic Chemistry 52 (2013) 4658–4667; doi:10.1021/ic400275x

data_4334524
_publ_contact_author_address
;
1101 University Avenue
Madison, WI 53706
USA
;
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John Berry'
_publ_section_title
;
 Lewis Acid Enhanced Axial Ligation of [Mo2]4+ Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4658
_journal_page_last               4667
_journal_paper_doi               10.1021/ic400275x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '(C5 H6 S N O)4 Mo2;(C2 H4 Cl2)1.5'
_chemical_formula_sum            'C23 H30 Cl3 Mo2 N4 O4 S4'
_chemical_formula_weight         852.98
_chemical_name_systematic
; 
 ? 
;
_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                 106.1590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6871(3)
_cell_length_b                   19.8411(6)
_cell_length_c                   15.3151(5)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3731
_cell_measurement_theta_min      2.7174
_cell_volume                     3119.17(16)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'microfocus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11157
_diffrn_reflns_theta_full        32.47
_diffrn_reflns_theta_max         32.47
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.9311
_exptl_absorpt_correction_T_min  0.8445
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         11157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+3.5148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                9515
_reflns_number_total             11157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400275x_si_001_3.cif
_cod_data_source_block           compound1b(100K)
_cod_database_code               4334524