Controlled Redox Conversion of New X-ray-Characterized Mono- and Dinuclear Heptacoordinated Mn(II) Complexes into Di-μ-oxo-dimanganese Core Complexes
Christelle Hureau; Sébastien Blanchard; Martine Nierlich; Guillaume Blain; Eric Rivière; Jean-Jacques Girerd; Elodie Anxolabéhère-Mallart; Geneviève Blondin; Inorganic Chemistry 43 (2004) 4415–4426; doi:10.1021/ic035332u

data_4311220
_publ_contact_author_address
;
CEA/Saclay, SCM
B\^at. 125
91191 Gif-sur-Yvette Cedex
France
;
_publ_contact_author_email       nierlich@drecam.cea.fr
_publ_contact_author_fax         '01 69 08 66 40'
_publ_contact_author_name        ' Nierlich Martine'
_publ_contact_author_phone       '01 69 08 32 22'
_publ_section_title
;
 Controlled Redox Conversion of New X-ray-Characterized Mono- and
 Dinuclear Heptacoordinated Mn(II) Complexes into Di-\m-oxo-dimanganese
 Core Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4415
_journal_page_last               4426
_journal_paper_doi               10.1021/ic035332u
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
;
C54 H59 N12 O14 Cl3 Mn2,0.5[(CH~3CH~2)O(CH~2CH~3)]
;
_chemical_formula_sum            'C56 H64 Cl3 Mn2 N12 O14.5'
_chemical_formula_weight         1353.42
_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                102.71(3)
_cell_angle_beta                 97.83(3)
_cell_angle_gamma                98.15(3)
_cell_formula_units_Z            2
_cell_length_a                   12.707(3)
_cell_length_b                   12.824(3)
_cell_length_c                   19.052(4)
_cell_measurement_reflns_used    18481
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2952.5(13)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 2\%steps'
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18841
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         2.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1402
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         9305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.791
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0491
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1914
_reflns_number_gt                7344
_reflns_number_total             9305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035332usi20031118_092653_3.cif
_cod_data_source_block           struc
_cod_original_cell_volume        2952.5(10)
_cod_original_formula_sum        'C56 H64 Cl3 Mn2 N12 O14.50'
_cod_database_code               4311220