Visible Circularly Polarized Luminescence of Octanuclear Circular Eu(III) Helicate.
Tan, Yan Bing; Okayasu, Yoshinori; Katao, Shohei; Nishikawa, Yoshiko; Asanoma, Fumio; Yamada, Mihoko; Yuasa, Junpei; Kawai, Tsuyoshi; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c08229

data_4135264
_publ_section_title
;
 Visible Circularly Polarized Luminescence of Octanuclear Circular Eu(III)
 Helicate.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c08229
_journal_year                    2020
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C356 H208 F168 N24 O64 Tb8'
_chemical_formula_sum            'C356 H208 F168 N24 O64 Tb8'
_chemical_formula_weight         10308.82
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   30.7532(12)
_cell_length_b                   30.7532(12)
_cell_length_c                   23.0554(4)
_cell_measurement_reflns_used    101440
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      1.73
_cell_volume                     21804.9(13)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0797
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            150304
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.546
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.415
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10112.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.98
_refine_ls_abs_structure_details
;
 Flack x determined using 6507 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.068(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         19914
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0453P)^2^+89.3069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                16120
_reflns_number_total             19914
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja0c08229_si_003.cif
_cod_data_source_block           expt269_2
_cod_original_cell_volume        21804.9(12)
_cod_database_code               4135264
_shelx_res_checksum              29409
_shelx_hkl_checksum              28336
_shelx_fab_checksum
'5260 RESPONSE: The alerts (Level B) are due to the disordering on the iPr units.'