Unusual Electronic Structure of First Row Transition Metal Complexes Featuring Redox-Active Dipyrromethane Ligands
Evan R. King; Theodore A. Betley; Journal of the American Chemical Society 131 (2009) 14374–14380; doi:10.1021/ja903997a

data_4105094
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
Mallinckrodt 306E
12 Oxford Street
Cambridge, MA 02139
;
_publ_contact_author_email       betley@chemistry.harvard.edu
_publ_contact_author_name        'Professor Theodore A. Betley'
_publ_contact_author_phone       617-496-9944
_publ_section_title
;
 Unusual Electronic Structure of First Row Transition Metal Complexes
 Featuring Redox-Active Dipyrromethane Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14374
_journal_page_last               14380
_journal_paper_doi               10.1021/ja903997a
_journal_volume                  131
_journal_year                    2009
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C38.61 H43.19 Mn N3.61 O0.40, C39 H42 Mn N4'
_chemical_formula_sum            'C77.61 H85.19 Mn2 N7.61 O0.4'
_chemical_formula_weight         1240.65
_chemical_name_common            (dmpm)Mn(py)2
_chemical_name_systematic
'bis-pyridine (1,9-dimesityl-5,5-dimethyldipyrromethanato)manganese(II)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                70.6500(10)
_cell_angle_beta                 87.1450(10)
_cell_angle_gamma                83.7300(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0232(2)
_cell_length_b                   15.6642(3)
_cell_length_c                   18.9630(3)
_cell_measurement_reflns_used    4593
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.63
_cell_measurement_theta_min      2.28
_cell_volume                     3349.13(10)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'SMART V5.625 (Bruker AXS, 2001a)'
_computing_data_reduction
; 
SAINT V7.34A (Bruker AXS, 2006), SADABS (Bruker AXS, 2004) 
;
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'phi and omega scans 0.5%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37811
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.70
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.9290
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       prism
_exptl_crystal_F_000             1314.4
_exptl_crystal_recrystallization_method 'tetrahydrofuran, diethyl ether'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         11844
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                7433
_reflns_number_total             11844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903997a_si_001_1.cif
_cod_data_source_block           compound3-erk007
_cod_original_formula_sum        'C77.61 H85.19 Mn2 N7.61 O0.40'
_cod_database_code               4105094