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_1517980
_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         'C19 H16 N2 O3'
_chemical_formula_sum            'C19 H16 N2 O3'
_chemical_formula_weight         320.34
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.840(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8507(4)
_cell_length_b                   26.7770(17)
_cell_length_c                   8.4103(5)
_cell_measurement_reflns_used    9553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.969
_cell_measurement_theta_min      2.422
_cell_volume                     1542.63(16)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47256
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.038
_diffrn_reflns_theta_min         1.521
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker, 2012)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 4782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.31(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10624
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.1720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                10218
_reflns_number_total             10624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc02474e2.cif
_cod_data_source_block           1S
_cod_depositor_comments
'Adding full bibliography for 1517979--1517983.cif.'
_cod_database_code               1517980
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2013-4
_shelx_res_checksum              61955