NMR Study of Ligand Exchange and Electron Self-Exchange between Oxo-Centered Trinuclear Clusters [Fe3(μ3-O)(μ-O2CR)6(4-R'py)3]+/0
Ghenadie Novitchi; Lothar Helm; Christopher E. Anson; Annie K. Powell; André E. Merbach; Inorganic Chemistry 50 (2011) 10402–10416; doi:10.1021/ic201484q

data_4326561
_publ_contact_author
; 
'Lother Helm'
;
_publ_contact_author_email       lothar.helm@epfl.ch
_publ_contact_author_phone       '+41 21 693 98 76'
_publ_section_title
;
 NMR Study of Ligand Exchange and Electron Self-Exchange between
 Oxo-Centered Trinuclear Clusters [Fe3(\m3-O)(\m-O2CR)6(4-R'py)3]+/0
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10402
_journal_page_last               10416
_journal_paper_doi               10.1021/ic201484q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '(C84 H111 Fe3 N3 O13), (N O3), 3.5(C7 H8)'
_chemical_formula_sum            'C108.5 H139 Fe3 N4 O16'
_chemical_formula_weight         1922.79
_chemical_name_systematic
; 
 ? 
;
_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                100.128(1)
_cell_angle_beta                 92.063(1)
_cell_angle_gamma                109.350(1)
_cell_formula_units_Z            2
_cell_length_a                   12.8294(4)
_cell_length_b                   15.2913(4)
_cell_length_c                   27.2934(8)
_cell_measurement_reflns_used    13594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.29
_cell_volume                     4947.5(3)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34427
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         21413
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+2.9425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                16741
_reflns_number_total             21413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201484q_si_001_2.cif
_cod_data_source_block           nov64b
_cod_original_cell_volume        4947.5(2)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4326561