Synthesis and Isolation of [Fe@Ge10]3-: A Pentagonal Prismatic Zintl Ion Cage Encapsulating an Interstitial Iron Atom
Binbin Zhou; Mark S. Denning; Deborah L. Kays; Jose M. Goicoechea; Journal of the American Chemical Society 131 (2009) 2802–2803; doi:10.1021/ja900055j

data_4103993
_publ_contact_author             'Jose M. Goicoechea'
_publ_contact_author_address
;    
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford OX1 3TA. UK.
;
_publ_contact_author_email       jose.goicoechea@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 275961'
_publ_section_title
;
 Synthesis and Isolation of [Fe@Ge10]3-: A Pentagonal Prismatic Zintl Ion
 Cage Encapsulating an Interstitial Iron Atom
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2802
_journal_page_last               2803
_journal_paper_doi               10.1021/ja900055j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         '3(C18 H36 K N2 O6), Fe Ge10, 2(C2 H6 N2)'
_chemical_formula_sum            'C58 H124 Fe Ge10 K3 N10 O18'
_chemical_formula_weight         2148.72
_chemical_name_systematic
;
[K-(2,2,2-crypt)]3[Fe@Ge10]*2en
;
_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
_cell_angle_alpha                93.2587(3)
_cell_angle_beta                 100.4043(3)
_cell_angle_gamma                107.2794(4)
_cell_formula_units_Z            2
_cell_length_a                   14.4014(1)
_cell_length_b                   15.7227(1)
_cell_length_c                   21.6608(2)
_cell_measurement_reflns_used    148030
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     4574.28(6)
_computing_cell_refinement
;
KappaCCD software "DENZO" (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software "Collect" (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software "DENZO" (Otwinowski & Minor, 1996)
;
_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_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega 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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30663
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    3.584
_exptl_absorpt_correction_T_max  0.7625
_exptl_absorpt_correction_T_min  0.3429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black-green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2178
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         15928
_refine_ls_number_restraints     243
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+5.4415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                12709
_reflns_number_total             15928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900055j_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4574.29(6)
_cod_database_code               4103993