Metal-Controlled Diastereoselective Self-Assembly and Circularly Polarized Luminescence of a Chiral Heptanuclear Europium Wheel
Gülay Bozoklu; Christelle Gateau; Daniel Imbert; Jacques Pécaut; Koen Robeyns; Yaroslav Filinchuk; Farah Memon; Gilles Muller; Marinella Mazzanti; Journal of the American Chemical Society 134 (2012) 8372–8375; doi:10.1021/ja3020814

data_4117961
_publ_section_title
;
 Metal-Controlled Diastereoselective Self-Assembly and Circularly
 Polarized Luminescence of a Chiral Heptanuclear Europium Wheel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8372
_journal_page_last               8375
_journal_paper_doi               10.1021/ja3020814
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C42.88 H35.5 Eu F3 N6 O10.88 S'
_chemical_formula_weight         1049.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   17.3261(2)
_cell_length_b                   32.2069(3)
_cell_length_c                   32.3667(3)
_cell_measurement_reflns_used    35255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      40.7376
_cell_measurement_theta_min      3.3529
_cell_volume                     18061.3(3)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -27.00   -1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9375   77.0000  -60.0000 26

  2 omega   14.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9375   77.0000  -60.0000 32

  3 omega   44.00  106.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       44.8283   77.0000  -90.0000 62

  4 omega   33.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       44.8283   77.0000  -30.0000 72

  5 omega  -74.00    7.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -46.7033   77.0000  120.0000 81

  6 omega  -72.00  -27.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -46.7033   77.0000 -180.0000 45

  7 omega   -5.00   21.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -46.7033   77.0000  -60.0000 26

  8 omega  -77.00  -49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9375  179.0000   90.0000 28

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w 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  0.0695
_diffrn_reflns_av_sigmaI/netI    0.1774
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            146014
_diffrn_reflns_theta_full        30.45
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    1.512
_exptl_absorpt_correction_T_max  0.8288
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             8444
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.776
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2380
_refine_ls_number_reflns         54983
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.779
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                29466
_reflns_number_total             54983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3020814_si_002.cif
_cod_data_source_block           gbi88_2
_cod_original_cell_volume        18061.2(3)
_cod_original_formula_sum        'C42.88 H35.50 Eu F3 N6 O10.88 S'
_cod_database_code               4117961