Unusual Nonoctahedral Geometry with Molybdenum Oxoimido Complexes Containing η2-Pyrazolate Ligands
T. Arumuganathan; Manuel Volpe; Bastian Harum; Dietmar Wurm; Ferdinand Belaj; Nadia C. Mösch-Zanetti; Inorganic Chemistry 51 (2012) 150–156; doi:10.1021/ic201308g

data_4327734
_publ_contact_author_address
; Institute of Chemistry,
  Karl-Franzens University Graz,
  Schubertstr. 1,
  A-8010 Graz,
  Austria
;
_publ_contact_author_email       ferdinand.belaj@uni-graz.at
_publ_contact_author_fax         43(316)3809835
_publ_contact_author_name        'Ferdinand Belaj'
_publ_contact_author_phone       43(316)3805288
_publ_section_title
;
 Unusual Nonoctahedral Geometry with Molybdenum Oxoimido Complexes
 Containing \h2-Pyrazolate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              150
_journal_page_last               156
_journal_paper_doi               10.1021/ic201308g
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C26 H45 Br2 Mo N5 O'
_chemical_formula_sum            'C26 H45 Br2 Mo N5 O'
_chemical_formula_weight         699.43
_chemical_name_systematic
; Bis[4-bromo-3,5-di(tert-butyl)-1H-pyrazolato-kappa-N1,kappa-N2][tert-bu-
tyl-imido]-oxo-molybdenum(VI)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                104.523(2)
_cell_angle_beta                 90.810(2)
_cell_angle_gamma                100.914(3)
_cell_formula_units_Z            4
_cell_length_a                   11.7782(6)
_cell_length_b                   15.5201(8)
_cell_length_c                   17.9310(9)
_cell_measurement_reflns_used    9372
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      2.18
_cell_volume                     3109.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26100
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.413
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         12055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+10.4708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                9133
_reflns_number_total             12055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201308g_si_002_3.cif
_cod_data_source_block           MO173C
_cod_database_code               4327734