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_4327170
_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            'C58 H117.5 Mn10 N27.5 O25.5'
_chemical_formula_weight         2157.70
_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
_audit_update_record
;
2010-05-26 # Formatted by publCIF
;
_cell_angle_alpha                82.451(4)
_cell_angle_beta                 82.488(7)
_cell_angle_gamma                66.784(7)
_cell_formula_units_Z            2
_cell_length_a                   13.058(3)
_cell_length_b                   16.551(3)
_cell_length_c                   22.339(5)
_cell_measurement_reflns_used    323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     4382.0(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w & \f 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59631
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  0.9259
_exptl_absorpt_correction_T_min  0.7451
_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    1.635
_exptl_crystal_description       plates
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         20088
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0372P)^2^+5.6669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                14604
_reflns_number_total             20088
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201916d_si_002_5.cif
_cod_data_source_block           saha75
_cod_original_cell_volume        4382.3(16)
_cod_original_formula_sum        'C58 H117.50 Mn10 N27.50 O25.50'
_cod_database_code               4327170