Electrochemical, Spectroscopic, and Structural Evidence for the Mild Hydrolysis of Tetracyanoethylene, TCNE, To Form the 2,3,3-Tricyanoacrylamidate Ligand: Isolation of an Unexpected Quadruply-Bonded Polymeric Material [Mo2(O2CCMe3)3((NC)2CC(CN)CONH)]\ιnfty
Françoise Conan; Benoît Le Gall; Jean-Michel Kerbaol; Sylvie Le Stang; Jean Sala Pala; Yves Le Mest; John Bacsa; Xiang Ouyang; Kim R. Dunbar; Charles F. Campana; Inorganic Chemistry 43 (2004) 3673–3681; doi:10.1021/ic0351186

data_4311097
_publ_contact_author_address
; 
Department of Chemistry
Texas A&M University
PO Box 30012 
College Station 
Texas 77842-3012 
USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         (979)8457177
_publ_contact_author_name        'Kim R. Dunbar'
_publ_contact_author_phone       (979)8455235
_publ_section_title
;
 Electrochemical, Spectroscopic, and Structural Evidence for the Mild
 Hydrolysis of Tetracyanoethylene, TCNE, To Form the
 2,3,3-Tricyanoacrylamidate Ligand: Isolation of an Unexpected
 Quadruply-Bonded Polymeric Material
 [Mo2(O2CCMe3)3((NC)2CC(CN)CONH)]\\infty
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3673
_journal_page_last               3681
_journal_paper_doi               10.1021/ic0351186
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C93 H144 Cl60 Mo6 N12 O21'
_chemical_formula_weight         4468.84
_chemical_name_common            MSU4S
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXTL (Bruker, 2001)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   46.976(2)
_cell_length_b                   46.976(2)
_cell_length_c                   22.8013(11)
_cell_measurement_temperature    133(2)
_cell_volume                     43575(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  ' Bruker SMART CCD'
_diffrn_measurement_method       ' omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            113574
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         0.87
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.7308
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            'green, red'
_exptl_crystal_density_diffrn    2.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             26712
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.718
_refine_diff_density_min         -2.851
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.000625
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         26338
_refine_ls_number_restraints     3386
_refine_ls_restrained_S_all      3.185
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.1581
_refine_ls_shift/su_max          2.416
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3054
_refine_ls_wR_factor_ref         0.3150
_reflns_number_gt                20729
_reflns_number_total             26338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0351186si20040421_111949.cif
_cod_data_source_block           MSU4Z.CIF
_cod_original_cell_volume        43575(4)
_cod_database_code               4311097