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_4305714
_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        'see text'
_chemical_formula_moiety         'C32 H45 Mo N O8 Rh, 2(C4 H8 O)'
_chemical_formula_structural     'C40 H61 Mo N O10 Rh'
_chemical_formula_sum            'C40 H61 Mo N O10 Rh'
_chemical_formula_weight         914.75
_chemical_name_systematic        ?
_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
_cell_angle_alpha                76.179(2)
_cell_angle_beta                 85.032(2)
_cell_angle_gamma                70.937(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1232(2)
_cell_length_b                   12.4414(3)
_cell_length_c                   18.7882(3)
_cell_measurement_reflns_used    15093
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      32.6685
_cell_measurement_theta_min      3.0673
_cell_volume                     2171.69(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123.0(2)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
  1 omega   -4.00   54.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441  -77.0000   90.0000    0.0000    0.0000 58

  2 omega   43.00   96.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441   45.0000    0.0000    0.0000    0.0000 53

  3 omega   43.00   96.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441   45.0000   60.0000    0.0000    0.0000 53

  4 omega   43.00   96.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441   45.0000  300.0000    0.0000    0.0000 53

  5 omega  -51.00   -1.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441  -45.0000  180.0000    0.0000    0.0000 50

  6 omega  -13.00   39.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441   77.0000   30.0000    0.0000    0.0000 52

  7 omega  -51.00   -7.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441  -45.0000  120.0000    0.0000    0.0000 44

  8 omega  -13.00   85.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       20.8441   77.0000  240.0000    0.0000    0.0000 98

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24498
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         12684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+4.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                9482
_reflns_number_total             12684
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800693r_si_009.cif
_cod_data_source_block           FD206
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2171.70(8)
_cod_database_code               4305714