Molybdenum(VI) Dioxo Complexes with Tridentate Phenolate Ligands
Martina E. Judmaier; Andreas Wallner; Gregor N. Stipicic; Karl Kirchner; Judith Baumgartner; Ferdinand Belaj; Nadia C. Mösch-Zanetti; Inorganic Chemistry 48 (2009) 10211–10221; doi:10.1021/ic901201s

data_4303469
_publ_contact_author_address
; Institut f\"ur Chemie, Bereich Anorganische Chemie,
  Karl-Franzens Universit\"at 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
;
Molybdenum(VI) Dioxo Complexes with Tridentate Phenolate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10211
_journal_page_last               10221
_journal_paper_doi               10.1021/ic901201s
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C80 H140 K4 N8 O4'
_chemical_formula_sum            'C80 H140 K4 N8 O4'
_chemical_formula_weight         1434.40
_chemical_name_systematic
; Potassium 2-[[[2-(dimethylamino)ethyl]methylamino]methyl]-4,6-bis(1,1-di-
methylethyl)-phenolate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90.00
_cell_angle_beta                 110.818(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.046(3)
_cell_length_b                   18.085(3)
_cell_length_c                   13.499(2)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      20.10
_cell_measurement_theta_min      19.56
_cell_volume                     4346.1(12)
_computing_cell_refinement       'local software'
_computing_data_collection       'local software'
_computing_data_reduction        'local software'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Stoe
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            10238
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0.78
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Parkin, S., Moezzi, B. and Hope H. (1995) J. Appl. Cryst. 28, 53-56'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0359P)^2^+1.5718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                6859
_reflns_number_total             8508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901201s_si_002_2.cif
_cod_data_source_block           KLNMe2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303469