Structure and Properties of New Mixed-Valent [MnIII2MnIV3LnIII5O5] Complexes (LnIII= TmIII, LuIII, and YbIII)
Kirstin Hallier; Małgorzata Hołyńska; Mathieu Rouzières; Rodolphe Clérac; Stefanie Dehnen; Inorganic Chemistry 51 (2012) 3929–3931; doi:10.1021/ic202443u

data_4328781
_publ_section_title
;
 Structure and Properties of New Mixed-Valent [MnIII2MnIV3LnIII5O5]
 Complexes (LnIII= TmIII, LuIII, and YbIII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3929
_journal_page_last               3931
_journal_paper_doi               10.1021/ic202443u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C80 H94 Mn5 N9 O32 Tm5, 2(C H4 O), 2(Cl)'
_chemical_formula_sum            'C82 H102 Cl2 Mn5 N9 O34 Tm5'
_chemical_formula_weight         2947.98
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 107.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.830(4)
_cell_length_b                   23.109(5)
_cell_length_c                   17.037(4)
_cell_measurement_reflns_used    13142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.30
_cell_volume                     5185(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  IPDS2t
_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  0.1264
_diffrn_reflns_av_sigmaI/netI    0.1379
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35185
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.81
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    4.947
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE, X-area ver. 1.54'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       block
_exptl_crystal_F_000             2866
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.08
_refine_diff_density_min         -3.61
_refine_diff_density_rms         0.65
_refine_ls_extinction_coef       0.0070(3)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11262
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0743
_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^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                5533
_reflns_number_total             11262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202443u_si_002.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4328781