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_1517981
_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 ad
_chemical_formula_moiety         'C26 H22 N2 O3'
_chemical_formula_sum            'C26 H22 N2 O3'
_chemical_formula_weight         410.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.277(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.4249(2)
_cell_length_b                   16.5948(6)
_cell_length_c                   11.4170(4)
_cell_measurement_reflns_used    5363
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.817
_cell_measurement_theta_min      2.662
_cell_volume                     1017.11(6)
_computing_cell_refinement       'Bruker SAINT, (Bruker 2012)'
_computing_data_collection       'Bruker APEX2, (Bruker 2012)'
_computing_data_reduction        'Bruker SAINT, (Bruker 2012)'
_computing_molecular_graphics    'Bruker SHELXTL v. 2008/4, (Bruker 2008)'
_computing_publication_material  'Bruker APEX2, (Bruker 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5614
_diffrn_reflns_point_group_measured_fraction_full 0.653
_diffrn_reflns_point_group_measured_fraction_max 0.676
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.323
_diffrn_reflns_theta_min         3.912
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker, 2012)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       needle
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.11(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2414
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.1345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.355
_reflns_Friedel_fraction_full    0.356
_reflns_Friedel_fraction_max     0.368
_reflns_number_gt                2401
_reflns_number_total             2414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc02474e2.cif
_cod_data_source_block           6R
_cod_depositor_comments
'Adding full bibliography for 1517979--1517983.cif.'
_cod_database_code               1517981
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.871
_shelxl_version_number           2013-4
_shelx_res_checksum              10998