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_4334525
_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_absolute_configuration ad
_chemical_formula_moiety         'C21 H21 Cl Li Mo2 N5 O4 S4, C5 H5 N'
_chemical_formula_sum            'C26 H26 Cl Li Mo2 N6 O4 S4'
_chemical_formula_weight         849.04
_chemical_name_systematic
;
 ?
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6895(3)
_cell_length_b                   13.7221(5)
_cell_length_c                   26.1281(9)
_cell_measurement_reflns_used    9687
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.77
_cell_volume                     3115.47(19)
_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 v7.68A (Bruker, 2009)'
_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.
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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
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            84886
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.514
_diffrn_reflns_theta_min         1.559
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.8254
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.8450.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
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_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+1.7044P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                9128
_reflns_number_total             9429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400275x_si_001_4.cif
_cod_data_source_block           compound2py
_cod_database_code               4334525
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H2A,H2B} of C2, {H3A,H3B} of C3, {H6A,H6B} of C6, {H7A,H7B} of C7, {H10A,
  H10B} of C10, {H11A,H11B} of C11, {H14A,H14B} of C14, {H15A,H15B} of C15, H1S
  of C1S, H2S of C2S, H3S of C3S, H4S of C4S, H5S of C5S, H17 of C17, H18 of
  C18, H19 of C19, H1A of C1A, H1B of C1B
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C17(H17), C18(H18),
 C19(H19), C1A(H1A), C1B(H1B)
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