Metal-Metal Quadruple Bonds Supported by 5-Ethynylthiophene-2-carboxylato Ligands: Preparation, Molecular and Electronic Structures, Photoexcited State Dynamics, and Application as Molecular Synthons
Samantha E. Brown-Xu; Malcolm H. Chisholm; Christopher B. Durr; Thomas F. Spilker; Journal of the American Chemical Society 135 (2013) 8254–8259; doi:10.1021/ja400508u

data_4119823
_publ_contact_author_address
;Department of Chemistry and Biochemistry
The Ohio State University 
100 West 18th Avenue
Columbus, OH  43210
;
_publ_contact_author_email       chisholm@chemistry.ohio-state.edu
_publ_contact_author_fax         '(+1) 614 292-0368'
_publ_contact_author_name        'Malcolm H. Chisholm'
_publ_contact_author_phone       '(+1) 614 282-7216'
_publ_section_title
;
 Metal-Metal Quadruple Bonds Supported by 5-Ethynylthiophene-2-carboxylato
 Ligands: Preparation, Molecular and Electronic Structures, Photoexcited
 State Dynamics, and Application as Molecular Synthons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8254
_journal_page_last               8259
_journal_paper_doi               10.1021/ja400508u
_journal_volume                  135
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C64 H74 Mo2 N2 O10 S2'
_chemical_formula_sum            'C64 H74 Mo2 N2 O10 S2'
_chemical_formula_weight         1287.25
_chemical_name_common            chisholm1925
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-11-27T16:16:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.0010(10)
_cell_angle_beta                 73.1240(10)
_cell_angle_gamma                84.2920(10)
_cell_formula_units_Z            1
_cell_length_a                   10.04830(10)
_cell_length_b                   11.27560(10)
_cell_length_c                   14.6132(2)
_cell_measurement_reflns_used    7053
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     1553.57(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0991348
_diffrn_orient_matrix_UB_12      -0.0085734
_diffrn_orient_matrix_UB_13      -0.0391505
_diffrn_orient_matrix_UB_21      -0.000516
_diffrn_orient_matrix_UB_22      -0.0893167
_diffrn_orient_matrix_UB_23      0.0234442
_diffrn_orient_matrix_UB_31      -0.0318041
_diffrn_orient_matrix_UB_32      -0.0113819
_diffrn_orient_matrix_UB_33      -0.0564244
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13835
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       'triangular block'
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                5660
_reflns_number_total             7098
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja400508u_si_002_1.cif
_cod_data_source_block           cbd034
_cod_database_code               4119823