Mechanism of Pyridine-Ligand Exchanges at the Different Labile Sites of 3d Heterometallic and Mixed Valence μ3-oxo Trinuclear Clusters
Ghenadie Novitchi; Fabrice Riblet; Rosario Scopelliti; Lothar Helm; Aurelian Gulea; André E. Merbach; Inorganic Chemistry 47 (2008) 10587–10599; doi:10.1021/ic801206m

data_4306363
_publ_contact_author_address
;Ecole polytechnique f\'ed\'erale de Lausanne
Institut des sciences et ing\'enierie chimiques
EPFL SB ISIC LCIB
BCH 3108 (B\^at. BCH)
CH-1015 Lausanne
Switzerland
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_publ_contact_author_email       lothar.helm@epfl.ch
_publ_contact_author_fax         '+41 21 693 98 71'
_publ_contact_author_name        'Lothar Helm'
_publ_contact_author_phone       '+41 21 693 98 75'
_publ_section_title
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Mechanism of Pyridine-Ligand Exchanges at the Different Labile Sites of
3d Heterometallic and Mixed Valence \m3-oxo Trinuclear Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10587
_journal_page_last               10599
_journal_paper_doi               10.1021/ic801206m
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C45 H45 Fe2 N3 Ni O13, 5(C2 H3 N)'
_chemical_formula_sum            'C55 H60 Fe2 N8 Ni O13'
_chemical_formula_weight         1211.52
_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           SHELXL-97
_cell_angle_alpha                105.040(8)
_cell_angle_beta                 96.423(10)
_cell_angle_gamma                92.983(9)
_cell_formula_units_Z            2
_cell_length_a                   11.3576(15)
_cell_length_b                   16.5028(16)
_cell_length_c                   16.6957(16)
_cell_measurement_reflns_used    5201
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.1357
_cell_measurement_theta_min      2.09175
_cell_volume                     2992.4(6)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Oxford Diffraction KM4/Sapphire CCD'
_diffrn_measurement_method       'phi and omega 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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17871
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            amber
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       iregular
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.284
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.0088(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         9253
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1696P)^2^+2.1998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2594
_reflns_number_gt                6350
_reflns_number_total             9253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801206m_si_002_5.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4306363