A Binuclear MnIII Complex of a Scorpiand-Like Ligand Displaying a Single Unsupported MnIII-O-MnIII Bridge
Salvador Blasco; Joan Cano; M. Paz Clares; Santiago García-Granda; Antonio Doménech; Hermas R. Jiménez; Begoña Verdejo; Francesc Lloret; Enrique García-España; Inorganic Chemistry 51 (2012) 11698–11706; doi:10.1021/ic3016063

data_4330887
_publ_contact_author_address
;
Instituto de Ciencia Molecular, 
Departamento de Qu\'imica Inorg\'anica, 
Universidad de Valencia, 
C/ Catedr\'atico Jos\'e Beltr\'an Mart\'inez, 2, 
46980, Paterna, Valencia, Spain. 
;
_publ_contact_author_email       Enrique.Garcia-Es@uv.es
_publ_contact_author_name        'Enrique Garc\'ia-Espa\~na'
_publ_section_title
;
 A Binuclear MnIII Complex of a Scorpiand-Like Ligand Displaying a Single
 Unsupported MnIII-O-MnIII Bridge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11698
_journal_page_last               11706
_journal_paper_doi               10.1021/ic3016063
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C26 H46 Mn2 N10 O, 3(H2O), 4(Br)'
_chemical_formula_sum            'C26 H52 Br4 Mn2 N10 O4'
_chemical_formula_weight         998.26
_chemical_name_common            'Mn(II)(pytren) Br2'
_space_group_IT_number           178
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61 2 (0 0 5)'
_symmetry_space_group_name_H-M   'P 61 2 2'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.6892(1)
_cell_length_b                   10.6892(1)
_cell_length_c                   55.4479(8)
_cell_measurement_reflns_used    24773
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1472
_cell_measurement_theta_min      3.3006
_cell_volume                     5486.64(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2673
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            90361
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    5.107
_exptl_absorpt_correction_T_max  0.7227
_exptl_absorpt_correction_T_min  0.5267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       'hexagonal well-shaped'
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.1443
_exptl_crystal_size_mid          0.1366
_exptl_crystal_size_min          0.0681
_refine_diff_density_max         1.732
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+2.4780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                3311
_reflns_number_total             4190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3016063_si_002.cif
_cod_data_source_block           mnpytren
_cod_original_cell_volume        5486.6(1)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               4330887