On chirality induction in the crystalline solid-containing sandwich-type [Ln(α-PW11O39)2]11−polyoxotungstate and proline
Iijima, Jun; Naruke, Haruo; Sanji, Takanobu; RSC Adv. 6 (2016) 91494–; doi:10.1039/C6RA22278A

data_7226620
_publ_section_title
;
 On chirality induction in the crystalline solid-containing sandwich-type
 [Ln(\a-PW11O39)2]11&#x2212;polyoxotungstate and proline
;
_journal_issue                   94
_journal_name_full               'RSC Adv.'
_journal_page_first              91494
_journal_paper_doi               10.1039/C6RA22278A
_journal_volume                  6
_journal_year                    2016
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety
'C41.5 H109.2 Er K1.3 N8.3 Na3.2 O108.6 P2 W22'
_chemical_formula_sum
'C41.5 H109.2 Er K1.3 N8.3 Na3.2 O108.6 P2 W22'
_chemical_formula_weight         6860.61
_chemical_properties_physical    ', Photo-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 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
_audit_update_record
;
2016-09-01 deposited with the CCDC.
2016-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                103.5786(9)
_cell_angle_beta                 93.9442(8)
_cell_angle_gamma                97.6353(9)
_cell_formula_units_Z            1
_cell_length_a                   12.8410(4)
_cell_length_b                   13.2876(4)
_cell_length_c                   19.8313(6)
_cell_measurement_reflns_used    26238
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.11
_cell_volume                     3242.39(17)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS Version 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_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            52590
_diffrn_reflns_point_group_measured_fraction_full 0.883
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.275
_exptl_absorpt_correction_T_max  0.210
_exptl_absorpt_correction_T_min  0.008
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            light
_exptl_crystal_density_diffrn    3.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3071.00
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.79
_refine_diff_density_min         -1.99
_refine_ls_abs_structure_details
;
 No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.028(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     781
_refine_ls_number_reflns         25584
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.768
_reflns_Friedel_fraction_max     0.727
_reflns_number_gt                24202
_reflns_number_total             25584
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6ra22278a3.cif
_cod_data_source_block           110127
_cod_original_cell_volume        3242.38(17)
_cod_database_code               7226620
_shelxl_version_number           2014/6
_shelx_res_checksum              98677
_shelx_fab_checksum              94287
_platon_squeeze_void_probe_radius 1.20