New Mixed-Valent Mn Clusters from the Use of N,N,N',N'-Tetrakis(2-hydroxyethyl)ethylenediamine (edteH4): Mn3, Mn4, Mn6, and Mn10
Arpita Saha; Khalil A. Abboud; George Christou; Inorganic Chemistry 50 (2011) 12774–12784; doi:10.1021/ic201916d

data_4327168
_publ_section_title
;
 New Mixed-Valent Mn Clusters from the Use of
 N,N,N',N'-Tetrakis(2-hydroxyethyl)ethylenediamine (edteH4): Mn3, Mn4,
 Mn6, and Mn10
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12774
_journal_page_last               12784
_journal_paper_doi               10.1021/ic201916d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C25 H47 Mn3 N5 O11'
_chemical_formula_weight         758.50
_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
_audit_update_record
;
2010-05-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.264(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.5084(17)
_cell_length_b                   14.4661(11)
_cell_length_c                   20.2570(15)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     6676.5(9)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_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  0.2884
_diffrn_reflns_av_sigmaI/netI    0.1407
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53924
_diffrn_reflns_theta_full        66.54
_diffrn_reflns_theta_max         66.54
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    9.620
_exptl_absorpt_correction_T_max  0.7054
_exptl_absorpt_correction_T_min  0.3610
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plates
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.000090(14)
_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   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0501P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                2883
_reflns_number_total             5862
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201916d_si_002_3.cif
_cod_data_source_block           saha71
_cod_database_code               4327168