Syntheses, X-ray Structures, Solid State High-Field Electron Paramagnetic Resonance, and Density-Functional Theory Investigations on Chloro and Aqua MnII Mononuclear Complexes with Amino-Pyridine Pentadentate Ligands
Christelle Hureau; Sihem Groni; Régis Guillot; Geneviève Blondin; Carole Duboc; Elodie Anxolabéhère-Mallart; Inorganic Chemistry 47 (2008) 9238–9247; doi:10.1021/ic800551u

data_4305570
_publ_contact_author_address
;
"Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay,
 Univ Paris-Sud, UMR 8182 CNRS, Orsay, F- 91405"
;
_publ_contact_author_email       eanxolab@icmo.u-psud.fr
_publ_contact_author_name        'Elodie Anxolab\'eh\`ere-Mallart'
_publ_contact_author_phone       '33 1 69 15 76 40'
_publ_section_title
;
Syntheses, X-ray Structures, Solid State High-Field Electron Paramagnetic
Resonance, and Density-Functional Theory Investigations on Chloro and Aqua
MnII Mononuclear Complexes with Amino-Pyridine Pentadentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9238
_journal_page_last               9247
_journal_paper_doi               10.1021/ic800551u
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '2(C22 H27 Cl Mn N5), 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C46 H57 Cl2 F12 Mn2 N11 P2'
_chemical_formula_weight         1234.75
_chemical_name_systematic
;
[N-methyl-N,N',N'-tris(2-pyridylmethylpropane-1,3-diamine) Mn Cl] (PF6)2
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6295(3)
_cell_length_b                   17.0758(4)
_cell_length_c                   18.9529(4)
_cell_measurement_reflns_used    8233
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      36.11
_cell_measurement_theta_min      2.39
_cell_volume                     5381.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            109804
_diffrn_reflns_theta_full        36.17
_diffrn_reflns_theta_max         36.17
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'X8 APEX II Bruker ICMMO'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.409(8)
_refine_ls_extinction_coef       0.00000(10)
_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   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         23697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          5.893
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.9191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                20393
_reflns_number_total             23697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800551u_si_002_4.cif
_cod_data_source_block           519GuillotICMMO
_cod_database_code               4305570