Lanthanide-Potassium Wheels
Michael T. Gamer; Peter W. Roesky; Inorganic Chemistry 44 (2005) 5963–5965; doi:10.1021/ic050557l

data_4309436
_publ_contact_author
;
      Prof. Dr. Peter Roesky
      Freie Universit\"at Berlin
      Fabeckstr. 34-36
      14195 Berlin
      Bundesrepublik Deutschland
;
_publ_contact_author_email       roesky@chemie.fu-berlin.de
_publ_contact_author_fax         +49/(0)3083852440
_publ_contact_author_phone       +49/(0)3083854004
_publ_section_title
;
Lanthanide-Potassium Wheels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5963
_journal_page_last               5965
_journal_paper_doi               10.1021/ic050557l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C53 H45 K N3 P2 Sm, C4 H8 O'
_chemical_formula_sum            'C57 H53 K N3 O P2 Sm'
_chemical_formula_weight         1047.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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                90.00
_cell_formula_units_Z            16
_cell_length_a                   29.512(5)
_cell_length_b                   29.512(5)
_cell_length_c                   23.318(7)
_cell_measurement_temperature    173(2)
_cell_volume                     20309(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    Diamond
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'phi and 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  0.1287
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68159
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.768399
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS - Bruker/Siemens'
_exptl_crystal_colour            golden-yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8560
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.935
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         7305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0849P)^2^+155.1827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                5163
_reflns_number_total             7305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050557lsi20050411_062317_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        20310(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4309436