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_7226617
_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 H133.2 Gd K1.3 N8.3 Na3.2 O120.6 P2 W22'
_chemical_formula_sum
'C41.5 H133.2 Gd K1.3 N8.3 Na3.2 O120.6 P2 W22'
_chemical_formula_weight         7066.78
_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                103.6870(13)
_cell_angle_beta                 93.1594(11)
_cell_angle_gamma                97.5260(13)
_cell_formula_units_Z            1
_cell_length_a                   12.8744(6)
_cell_length_b                   13.3048(7)
_cell_length_c                   19.7946(9)
_cell_measurement_reflns_used    38446
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.10
_cell_volume                     3252.9(3)
_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  0.0824
_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       -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            52614
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         3.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.089
_exptl_absorpt_correction_T_max  0.300
_exptl_absorpt_correction_T_min  0.025
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3187.00
_exptl_crystal_size_max          0.780
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.00
_refine_diff_density_min         -2.96
_refine_ls_abs_structure_details
;
 Flack x determined using 6616 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     785
_refine_ls_number_reflns         25658
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0814P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.770
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                20530
_reflns_number_total             25658
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6ra22278a3.cif
_cod_data_source_block           110221
_cod_database_code               7226617
_shelxl_version_number           2014/6
_shelx_res_checksum              43280
_shelx_fab_checksum              13832
_platon_squeeze_void_probe_radius 1.20