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_4326560
_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_sum            'C47 H58 Cl Fe3 N3 O21.5'
_chemical_formula_weight         1211.96
_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                90.535(12)
_cell_angle_beta                 92.815(11)
_cell_angle_gamma                102.893(12)
_cell_formula_units_Z            2
_cell_length_a                   7.6728(10)
_cell_length_b                   13.847(2)
_cell_length_c                   26.316(3)
_cell_measurement_reflns_used    13226
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      1.51
_cell_volume                     2721.6(6)
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_molecular_graphics    'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.12 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16169
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.12 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.547
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2287
_reflns_number_gt                6641
_reflns_number_total             10066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201484q_si_001_1.cif
_cod_data_source_block           novc7a
_cod_original_cell_volume        2721.6(7)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_formula_sum        'C47 H58 Cl Fe3 N3 O21.50'
_cod_database_code               4326560