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_4346611
_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 Br0.04 N4.96 O9.88 Zn'
_chemical_formula_sum            'C24 H23 Br0.04 N4.96 O9.88 Zn'
_chemical_formula_weight         607.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.20 svn.r3092 for OlexSys, GUI svn.r4949)
;
_cell_angle_alpha                81.422(2)
_cell_angle_beta                 87.890(2)
_cell_angle_gamma                75.316(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8979(3)
_cell_length_b                   8.4500(4)
_cell_length_c                   19.2843(8)
_cell_measurement_reflns_used    5401
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.590
_cell_volume                     1231.02(9)
_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      110.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX2 area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_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  0.1299
_diffrn_reflns_av_unetI/netI     0.1111
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29341
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         2.136
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0852 before and 0.0713 after correction. The Ratio of minimum to maximum transmission is 0.9034. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0112(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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.7247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3471
_reflns_number_total             5621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01766_si_003.cif
_cod_data_source_block           rh118
_cod_database_code               4346611
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.807
_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. Rigid body (RIGU) restrains
 N4, O5, O6, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Br1)=1-FVAR(1)
 Sof(N4)=Sof(O5)=Sof(O6)=Sof(O7)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
4.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)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              11223
_shelx_hkl_checksum              97033
_olex2_submission_special_instructions 'No special instructions were received'