Synthesis and Comparison of Transition Metal Complexes of Abnormal and Normal Tetrazolylidenes: A Neglected Ligand Species
Lars-Arne Schaper; Xuhui Wei; Philipp J. Altmann; Karl Öfele; Alexander Pöthig; Markus Drees; János Mink; Eberhardt Herdtweck; Bettina Bechlars; Wolfgang A. Herrmann; Fritz E. Kühn; Inorganic Chemistry 52 (2013) 7031–7044; doi:10.1021/ic4005449

data_4335189
_publ_contact_author_address
;
Catalysis Research Center
Technische Universit/"at M/"unchen
Ernst-Otto-Fischer-Str. 1
85747 Garching bei M/"unchen
Germany
;
_publ_contact_author_email       alexander.poethig@tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
Dr. Alexander P\"othig
;
_publ_contact_author_phone       '+49(0)89 289 13133'
_publ_section_title
;
 Synthesis and Comparison of Transition Metal Complexes of Abnormal and
 Normal Tetrazolylidenes: A Neglected Ligand Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7031
_journal_page_last               7044
_journal_paper_doi               10.1021/ic4005449
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C10 H11 Cl Mo N4 O2'
_chemical_formula_sum            'C10 H11 Cl Mo N4 O2'
_chemical_formula_weight         350.62
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.9942(2)
_cell_length_b                   19.9942(2)
_cell_length_c                   7.4709(1)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.2120
_cell_measurement_theta_min      2.7264
_cell_volume                     2986.63(6)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focused sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            64066
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.190
_platon_squeeze_details
;
The unit cell contains 2 dichloromethane molecules which have been treated as 
a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.

PLATON OUTPUT:

N: No S.U.'s (esd) on observed/calculated parameters.
--------------------------------------------------------------------------------
N: Number of moved primary input atoms: ..................................   29
N: Number of Ignored Lines on INPUT ......................................    2
          of which blank in column 1 .....................................    2
N: Total Potential Solvent Accessible Void Vol ..................   381.6 Ang3
N: Electron Count / Cell =    100 - To be included in D(calc), F000 & Mol.Wght.
;
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+1.7406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                2428
_reflns_number_total             2736
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic4005449_si_002_1.cif
_cod_data_source_block           Compound_2e
_cod_original_cell_volume        2986.63(7)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4335189