Heptacoordinated Molybdenum(VI) Complexes of Phenylenediamine Bis(phenolate): A Stable Molybdenum Amidophenoxide Radical
Mikko M. Hänninen; Petriina Paturi; Heikki M. Tuononen; Reijo Sillanpää; Ari Lehtonen; Inorganic Chemistry 52 (2013) 5714–5721; doi:10.1021/ic302355b

data_4334804
_publ_section_title
;
 Heptacoordinated Molybdenum(VI) Complexes of Phenylenediamine
 Bis(phenolate): A Stable Molybdenum Amidophenoxide Radical
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5714
_journal_page_last               5721
_journal_paper_doi               10.1021/ic302355b
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C68 H89 Mo N4 O4'
_chemical_formula_sum            'C68 H89 Mo N4 O4'
_chemical_formula_weight         1122.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2010-12-15T13:10:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.2260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.4051(3)
_cell_length_b                   18.9197(2)
_cell_length_c                   45.7404(5)
_cell_measurement_reflns_used    9534
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     25505.5(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.709
_diffrn_measured_fraction_theta_max 0.709
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.055
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            21562
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Greenish Black'
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             9584
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1393
_refine_ls_number_reflns         15921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+113.3826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                11787
_reflns_number_total             15921
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302355b_si_003.cif
_cod_data_source_block           molyx3
_cod_database_code               4334804