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_4334523
_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         'C16 H16 Mo2 N4 O4 S4'
_chemical_formula_sum            'C16 H16 Mo2 N4 O4 S4'
_chemical_formula_weight         648.45
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6032(7)
_cell_length_b                   12.5912(10)
_cell_length_c                   15.8418(15)
_cell_measurement_reflns_used    9457
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      71.602
_cell_measurement_theta_min      5.455
_cell_volume                     2115.0(3)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30667
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.03
_diffrn_reflns_theta_min         5.45
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.700
_exptl_absorpt_correction_T_max  0.4949
_exptl_absorpt_correction_T_min  0.0813
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.1008 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.1643.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'orange red'
_exptl_crystal_colour_modifier   orange
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0430P)^2^+3.0934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                1958
_reflns_number_total             2040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400275x_si_001_2.cif
_cod_data_source_block           compound1a
_cod_database_code               4334523