Controlling the Fluorescence Response of PET Sensors via the Metal-Ion π-Contacting Ability of the Fluorophore: Coumarin, a Weaker π Contacter.
Nugent, Joseph W.; Reibenspies, Joseph H.; Hancock, Robert D.; Inorganic chemistry 54 (2015) 9976–9988; doi:10.1021/acs.inorgchem.5b01766

data_4346613
_publ_section_title
;
 Controlling the Fluorescence Response of PET Sensors via the Metal-Ion
 \p-Contacting Ability of the Fluorophore: Coumarin, a Weaker \p
 Contacter.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9976
_journal_page_last               9988
_journal_paper_doi               10.1021/acs.inorgchem.5b01766
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C24 H23 N5 O10 Pb'
_chemical_formula_sum            'C24 H23 N5 O10 Pb'
_chemical_formula_weight         748.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.20 svn.r3092 for OlexSys, GUI svn.r4949)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9460(3)
_cell_length_b                   28.8405(7)
_cell_length_c                   8.7430(2)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.57
_cell_volume                     2606.36(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEXII (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX2 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            43701
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         2.093
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.540
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1504 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.4227.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.643
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.529
_refine_diff_density_min         -2.553
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.00022(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0050P)^2^+14.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5503
_reflns_number_total             6024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01766_si_002.cif
_cod_data_source_block           rh117
_cod_database_code               4346613
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.102
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C18(H18), C21(H21)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'