Synthesis and Electrochemical Reactivity of Molybdenum Dicarbonyl Supported by a Redox-Active α-Diimine Ligand
Isaac R. Corn; Pablo D. Astudillo-Sánchez; Michael J. Zdilla; Phillip E. Fanwick; Michael J. Shaw; Jeffrey T. Miller; Dennis H. Evans; Mahdi M. Abu-Omar; Inorganic Chemistry 52 (2013) 5457–5463; doi:10.1021/ic400348j

data_4334732
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Fanwick, Phillip E.'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Synthesis and Electrochemical Reactivity of Molybdenum Dicarbonyl
 Supported by a Redox-Active \a-Diimine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5457
_journal_page_last               5463
_journal_paper_doi               10.1021/ic400348j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H56 Mo1 N4 O2'
_chemical_formula_sum            'C46 H56 Mo N4 O2'
_chemical_formula_weight         792.92
_chemical_name_systematic        ' ?'
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.030(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4335(11)
_cell_length_b                   8.9648(7)
_cell_length_c                   16.7602(13)
_cell_measurement_reflns_used    22246
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     2317.5(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150.00(2)
_diffrn_measured_fraction_theta_full 0.8600
_diffrn_measured_fraction_theta_max 0.8600
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22246
_diffrn_reflns_theta_full        60.0
_diffrn_reflns_theta_max         76.73
_diffrn_reflns_theta_min         3.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.595
_exptl_absorpt_correction_T_max  0.9251
_exptl_absorpt_correction_T_min  0.9251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_platon_squeeze_details
'                                                                       '
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.075
_refine_ls_R_factor_gt           0.069
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.1023P)^2^+3.3840P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.186
_refine_ls_wR_factor_ref         0.192
_reflns_number_gt                3727
_reflns_number_total             4204
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic400348j_si_002_2.cif
_cod_data_source_block           IRC078
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_formula_sum        'C46 H56 Mo1 N4 O2'
_cod_database_code               4334732