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_4305569
_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         'C22 H27 Mn N5 O, 2(C24 H20 B)'
_chemical_formula_sum            'C70 H69 B2 Mn N5 O'
_chemical_formula_weight         1070.85
_chemical_name_systematic
;
[N-methyl-N,N',N'-tris(2-pyridylmethylpropane-1,3-diamine) Mn H2O] (BPh4)2 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.665(3)
_cell_length_b                   17.325(4)
_cell_length_c                   21.128(4)
_cell_measurement_reflns_used    15829
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     5726(2)
_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 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device       '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  0.1270
_diffrn_reflns_av_sigmaI/netI    0.2083
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15829
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        ?0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(7)
_refine_ls_extinction_coef       0.0028(5)
_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   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         8068
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.3006
_refine_ls_R_factor_gt           0.1154
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.3456
_reflns_number_gt                2683
_reflns_number_total             8068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800551u_si_002_3.cif
_cod_data_source_block           166SG
_cod_database_code               4305569