Reductive Nitrosylation and Proton-Assisted Bridge Splitting of a (μ-Oxo)dimanganese(III) Complex Derived from a Polypyridine Ligand with One Carboxamide Group
Kaushik Ghosh; Aura A. Eroy-Reveles; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 44 (2005) 8469–8475; doi:10.1021/ic0503535

data_4309924
_publ_section_title
;
Reductive Nitrosylation and Proton-Assisted Bridge Splitting of a
(\m-Oxo)dimanganese(III) Complex Derived from a Polypyridine Ligand with
One Carboxamide Group
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8469
_journal_page_last               8475
_journal_paper_doi               10.1021/ic0503535
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C27 H5 Mn N5 O3, Cl O4, C H2 Cl2'
_chemical_formula_sum            'C28 H27 Cl3 Mn N5 O7'
_chemical_formula_weight         706.84
_chemical_name_common            '[Mn(PaPy3)(OOC6H5)](ClO4).CH2Cl2'
_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                110.209(4)
_cell_angle_beta                 105.526(2)
_cell_angle_gamma                102.543(3)
_cell_formula_units_Z            4
_cell_length_a                   11.2904(9)
_cell_length_b                   17.3599(13)
_cell_length_c                   17.8750(13)
_cell_measurement_reflns_used    953
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2976.3(4)
_computing_cell_refinement       'SMART 5.628 (Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.35A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       \w
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29727
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         13569
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                8647
_reflns_number_total             13569
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0503535si20050307_025819.cif
_cod_data_source_block           mn1513
_cod_database_code               4309924