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_4309925
_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
'C40 H40 MN2 N10 O3, 2(Cl O4), 2.7(C H2 Cl2), 0.5(C2 H3 N)'
_chemical_formula_sum            'C43.7 H48.4 Cl7.4 Mn2 N10.5 O11'
_chemical_formula_weight         1268.94
_chemical_name_common
'[(Mn(PaPy3))2(mu-O)](ClO4)2 . 2.7CH2Cl2 . 0.5CH3CN'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.344(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.112(3)
_cell_length_b                   13.682(3)
_cell_length_c                   22.511(5)
_cell_measurement_reflns_used    811
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.5
_cell_volume                     5057.4(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19973
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.460
_refine_diff_density_min         -3.154
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0654P)^2^+82.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1791
_reflns_number_gt                3497
_reflns_number_total             4635
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0503535si20050307_025834.cif
_cod_data_source_block           mn1609
_cod_original_cell_volume        5057.5(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C43.70 H48.40 Cl7.40 Mn2 N10.50 O11'
_cod_database_code               4309925