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_4305567
_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_absolute_configuration unk
_chemical_formula_moiety         '4(C21 H25 Mn N5 O), 8(C24 H20 B)'
_chemical_formula_sum            'C69 H65 B2 Mn N5 O'
_chemical_formula_weight         4227.43
_chemical_name_systematic
;
[N-methyl-N,N',N'-tris(2-pyridylmethylethane-1,2-diamine  Mn H2O] ](BPh4)2 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                61.958(3)
_cell_angle_beta                 84.894(3)
_cell_angle_gamma                85.547(3)
_cell_formula_units_Z            4
_cell_length_a                   11.887(3)
_cell_length_b                   23.689(6)
_cell_length_c                   23.812(7)
_cell_measurement_reflns_used    15031
_cell_measurement_temperature    0
_cell_measurement_theta_max      24
_cell_measurement_theta_min      1
_cell_volume                     5890(3)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SHELXS 86 (Sheldrick, 1986) 
;
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30649
_diffrn_reflns_theta_full        24.376
_diffrn_reflns_theta_max         24.376
_diffrn_reflns_theta_min         1.005
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' none '
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0730
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_reflns         10632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.000022
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
 
 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1883
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1394
_reflns_limit_h_max              13
_reflns_limit_h_min              -11
_reflns_limit_k_max              27
_reflns_limit_k_min              -27
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                10632
_reflns_number_total             0
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic800551u_si_002_1.cif
_cod_data_source_block           GuillotICMMO
_cod_database_code               4305567