Strategies for a fluorescent sensor with receptor and fluorophore designed for the recognition of heavy metal ions
Deems, Justin C.; Reibenspies, Joseph H.; Lee, Hee-Seung; Hancock, Robert D.; Inorganica Chimica Acta 499 (2020) 119181–; doi:10.1016/j.ica.2019.119181

data_1565704
_publ_section_title
;
 Strategies for a fluorescent sensor with receptor and fluorophore
 designed for the recognition of heavy metal ions
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119181
_journal_paper_doi               10.1016/j.ica.2019.119181
_journal_volume                  499
_journal_year                    2020
_chemical_formula_moiety         'C36 H46 Ag N2 O12, Cl O4'
_chemical_formula_sum            'C36 H46 Ag Cl N2 O16'
_chemical_formula_weight         906.07
_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
_cell_angle_alpha                90
_cell_angle_beta                 105.2530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4875(6)
_cell_length_b                   25.2151(12)
_cell_length_c                   24.4961(12)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.55
_cell_volume                     8037.4(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.04
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            266026
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.219
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1353 before and 0.0480 after correction.
The Ratio of minimum to maximum transmission is 0.9151.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.763
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00047(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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1110
_refine_ls_number_reflns         19738
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0432P)^2^+18.3280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17367
_reflns_number_total             19738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119181.cif
_cod_data_source_block           rh133_sq
_cod_database_code               1565704
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.641
_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 bond restraints
 Cl1_1, O1_1, O2_1, O3_1, O4_1
 Cl1_2, O1_2, O2_2, O3_2, O4_2
 Cl1_3, O1_3, O2_3, O3_3, O4_3
 Cl1_4, O1_4, O2_4, O3_4, O4_4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Cl1_1 \\sim O1_1 \\sim O2_1 \\sim O3_1 \\sim O4_1 \\sim Cl1_2 \\sim O1_2 \\sim
O2_2 \\sim O3_2 \\sim O4_2 \\sim Cl1_3 \\sim O1_3 \\sim O2_3 \\sim O3_3 \\sim
O4_3 \\sim Cl1_4 \\sim O1_4 \\sim O2_4 \\sim O3_4 \\sim O4_4: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
4. Same fragment restrains
{Cl1_2, O1_2, O2_2, O3_2, O4_2}
{Cl1_3, O1_3, O2_3, O3_3, O4_3}
{Cl1_4, O1_4, O2_4, O3_4, O4_4}
as
{Cl1_1, O1_1, O2_1, O3_1, O4_1} sigma for 1-2: 0.005 1-3: 0.04
5. Others
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=1-FVAR(1)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(1)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=1-FVAR(2)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,
 H5AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB),
 C10A(H10A,H10B), C11A(H11A,H11B), C12A(H12A,H12B), C13A(H13A,H13B), C25A(H25A,
 H25B), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3B(H3BA,H3BB), C4B(H4BA,H4BB),
 C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C9B(H9BA,H9BB),
  C10B(H10C,H10D), C11B(H11C,H11D), C12B(H12C,H12D), C13B(H13C,H13D), C25B(H25C,
 H25D)
6.b Aromatic/amide H refined with riding coordinates:
 C15A(H15A), C18A(H18A), C21A(H21A), C27A(H27A), C30A(H30A), C33A(H33A),
 C15B(H15B), C18B(H18B), C21B(H21B), C27B(H27B), C30B(H30B), C33B(H33B)
6.c Idealised Me refined as rotating group:
 C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C35A(H35A,H35B,H35C), C36A(H36A,
 H36B,H36C), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F), C35B(H35D,H35E,H35F),
 C36B(H36D,H36E,H36F)
;