The application of chiroptical spectroscopy (circular dichroism) in quantifying binding events in lanthanide directed synthesis of chiral luminescent self-assembly structures
Kotova, Oxana; Blasco, Salvador; Twamley, Brendan; O'Brien, John; Peacock, Robert D.; Kitchen, Jonathan A.; Martínez-Calvo, Miguel; Gunnlaugsson, Thorfinnur; Chem. Sci. 6 (2015) 457–; doi:10.1039/C4SC02474E

data_1517983
_publ_section_title
;
 The application of chiroptical spectroscopy (circular dichroism) in
 quantifying binding events in lanthanide directed synthesis of chiral
 luminescent self-assembly structures
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              457
_journal_paper_doi               10.1039/C4SC02474E
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C57 H42 Eu N6 O9, 2.5(H2 O)'
_chemical_formula_sum            'C57 H49.5 Eu N6 O11.5'
_chemical_formula_weight         1154.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 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                   26.0015(12)
_cell_length_b                   26.4029(11)
_cell_length_c                   30.8305(11)
_cell_measurement_reflns_used    9422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.88
_cell_measurement_theta_min      2.78
_cell_volume                     21165.6(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.1200
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36491
_diffrn_reflns_theta_full        50.55
_diffrn_reflns_theta_max         50.55
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    9.048
_exptl_absorpt_correction_T_max  0.7249
_exptl_absorpt_correction_T_min  0.1846
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'APEX2 default values. r=0.2'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             9416
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(8)
_refine_ls_extinction_coef       0.000104(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         9417
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2618
_reflns_number_gt                5646
_reflns_number_total             9417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02474e2.cif
_cod_data_source_block           sal24
_cod_depositor_comments
'Adding full bibliography for 1517979--1517983.cif.'
_cod_original_sg_symbol_H-M      C222(1)
_cod_original_formula_sum        'C57 H49.50 Eu N6 O11.50'
_cod_database_code               1517983