Enantioselective Resolutions and Circular Dichroism Studies of Lanthanide-Containing Keggin-Type [Ln(PW11O39)2]11- Polyoxometalates
Haruo Naruke; Jun Iijima; Takanobu Sanji; Inorganic Chemistry 50 (2011) 7535–7539; doi:10.1021/ic200401g

data_4325860
_publ_contact_author_address
; Chemical Resources Laboratory
Tokyo Institute of Technology
R1-23, 4259 Nagatsuta, Midori-ku, Yokohama 226-8503
Japan 
;
_publ_contact_author_email       ' hnaruke@res.titech.ac.jp'
_publ_contact_author_fax         ' +81-(0)45-924-5271 '
_publ_contact_author_name        ' Haruo Naruke'
_publ_contact_author_phone       ' +81-(0)45-924-5271 '
_publ_section_title
;
 Enantioselective Resolutions and Circular Dichroism Studies of
 Lanthanide-Containing Keggin-Type [Ln(PW11O39)2]11- Polyoxometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7535
_journal_page_last               7539
_journal_paper_doi               10.1021/ic200401g
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C41.50 H115.20 K1.30 N8.30 Na3.20 O111.60 P2 Pr W22'
_chemical_formula_sum
'C41.5 H115.2 K1.3 N8.3 Na3.2 O111.6 P2 Pr W22'
_chemical_formula_weight         6888.31
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                103.7136(12)
_cell_angle_beta                 92.5694(13)
_cell_angle_gamma                97.6599(12)
_cell_formula_units_Z            1
_cell_length_a                   12.8016(4)
_cell_length_b                   13.2173(5)
_cell_length_c                   19.7108(7)
_cell_measurement_reflns_used    19421
_cell_measurement_temperature    203
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.13
_cell_volume                     3201.0(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52075
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.265
_exptl_absorpt_correction_T_max  0.132
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.573
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3092.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.010
_refine_diff_density_min         -2.380
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  10861 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.032(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     751
_refine_ls_number_reflns         25513
_refine_ls_number_restraints     6
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0955P)^2^+14.6824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                24513
_reflns_number_total             25513
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic200401g_si_002_3.cif
_cod_data_source_block           D-Pr
_cod_original_cell_volume        3201.01(18)
_cod_original_formula_sum
'C41.50 H115.20 K1.30 N8.30 Na3.20 O111.60 P2 Pr W22'
_cod_database_code               4325860