Dimolybdenum Bis-2,4,6-triisopropyl-benzoate Bis-4-isonicotinate: A Redox Active Analogue of 4,4'-Bipyridine with Ambivalent Properties
Malcolm H. Chisholm; Angela S. Dann; Fabian Dielmann; Judith C. Gallucci; Nathan J. Patmore; Ramkrishna Ramnauth; Manfred Scheer; Inorganic Chemistry 47 (2008) 9248–9255; doi:10.1021/ic800693r

data_4305713
_publ_section_title
;
Dimolybdenum Bis-2,4,6-triisopropyl-benzoate Bis-4-isonicotinate: A Redox
Active Analogue of 4,4'-Bipyridine with Ambivalent Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9248
_journal_page_last               9255
_journal_paper_doi               10.1021/ic800693r
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H66 Mo2 N2 O10 S2'
_chemical_formula_sum            'C48 H66 Mo2 N2 O10 S2'
_chemical_formula_weight         1087.03
_chemical_name_common            'Chisholm 1332'
_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     heavy
_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      2.3
_audit_creation_date             2008-03-04T16:43:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.240(8)
_cell_angle_beta                 84.046(9)
_cell_angle_gamma                62.388(6)
_cell_formula_units_Z            1
_cell_length_a                   10.2059(10)
_cell_length_b                   10.248(2)
_cell_length_c                   13.932(2)
_cell_measurement_reflns_used    5874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     1284.0(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.352104E-1
_diffrn_orient_matrix_UB_12      0.750737E-1
_diffrn_orient_matrix_UB_13      0.737297E-1
_diffrn_orient_matrix_UB_21      -0.763613E-1
_diffrn_orient_matrix_UB_22      -0.509167E-1
_diffrn_orient_matrix_UB_23      -0.608988E-1
_diffrn_orient_matrix_UB_31      0.9492E-3
_diffrn_orient_matrix_UB_32      -0.546727E-1
_diffrn_orient_matrix_UB_33      0.471142E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39225
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular rod'
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.036
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+2.7846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                4907
_reflns_number_total             5891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800693r_si_007.cif
_cod_data_source_block           Chisholm1332
_cod_database_code               4305713