A Highly Distorted Open-Shell Endohedral Zintl Cluster: [Mn@Pb12]3-
Binbin Zhou; Tobias Krämer; Amber L. Thompson; John E. McGrady; José M. Goicoechea; Inorganic Chemistry 50 (2011) 8028–8037; doi:10.1021/ic200329m

data_4326009
_publ_contact_author             'Jos\'e M. Goicoechea'
_publ_contact_author_email       jose.goicoechea@chem.ox.ac.uk
_publ_section_title
;
 A Highly Distorted Open-Shell Endohedral Zintl Cluster: [Mn@Pb12]3-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8028
_journal_page_last               8037
_journal_paper_doi               10.1021/ic200329m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '3(C18 H36 K N2 O6), Mn Pb12, 1.5(C2 H8 N2)'
_chemical_formula_sum            'C57 H120 K3 Mn N9 O18 Pb12'
_chemical_formula_weight         3878.14
_chemical_name_systematic
;
 [K(2,2,2-crypt)]2[Mn@Pb12]*1.5en
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 109.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.373(3)
_cell_length_b                   23.275(5)
_cell_length_c                   50.436(12)
_cell_measurement_reflns_used    50361
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.6465
_cell_measurement_theta_min      1.1876
_cell_volume                     19186(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1212
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            105799
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.19
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    21.285
_exptl_absorpt_correction_T_max  0.4158
_exptl_absorpt_correction_T_min  0.1003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            metallic_dark_grey
_exptl_crystal_density_diffrn    2.685
_exptl_crystal_description       needle
_exptl_crystal_F_000             13880
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.005
_refine_diff_density_min         -3.588
_refine_diff_density_rms         0.408
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1905
_refine_ls_number_reflns         34956
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+25.8983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2175
_reflns_number_gt                26740
_reflns_number_total             34956
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200329m_si_004_1.cif
_cod_data_source_block           1b
_cod_original_cell_volume        19186(7)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4326009