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_4334522
_publ_contact_author_address
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1101 University Avenue
Madison, WI 53706
USA
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_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John Berry'
_publ_section_title
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 Lewis Acid Enhanced Axial Ligation of [Mo2]4+ Complexes
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_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         'C32 H32 Cl2 Li2 Mo4 N8 O8 S8, 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H36 Cl6 Li2 Mo4 N8 O8 S8'
_chemical_formula_weight         1551.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 108.07(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.704(3)
_cell_length_b                   22.530(8)
_cell_length_c                   13.543(5)
_cell_measurement_reflns_used    7157
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.136
_cell_measurement_theta_min      2.402
_cell_volume                     2524.8(16)
_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
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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.
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_computing_publication_material
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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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52146
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.486
_diffrn_reflns_theta_min         1.808
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.676
_exptl_absorpt_correction_T_max  0.9734
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0767 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.8968.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+3.1785P]
 where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4997
_reflns_number_total             6403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400275x_si_001_1.cif
_cod_data_source_block           compound2-dim
_cod_original_cell_volume        2525.1(17)
_cod_database_code               4334522
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H1SA,H1SB} of C1S, {H2A,H2B} of C2, {H3A,H3B} of C3, {H6A,H6B} of C6,
  {H10A,H10B} of C10, {H11A,H11B} of C11, {H15A,H15B} of C15, {H14A,H14B} of
  C14, {H7A,H7B} of C7
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,
 H10B), C11(H11A,H11B), C14(H14A,H14B), C15(H15A,H15B)
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