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_1565703
_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 H48 N2 O13 Pb, 2(Cl O4), 3.5(H2 O1)'
_chemical_formula_sum            'C36 H55 Cl2 N2 O24.5 Pb'
_chemical_formula_weight         1185.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.537(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3715(7)
_cell_length_b                   14.3081(6)
_cell_length_c                   21.6132(9)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      2.27
_cell_volume                     4687.8(4)
_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      296.15
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52390
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.699
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.800
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0828 before and 0.0578 after correction.
The Ratio of minimum to maximum transmission is 0.8329.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       plate
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+7.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4993
_reflns_number_total             5486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-499-119181.cif
_cod_data_source_block           rh132
_cod_original_formula_sum        'C36 H55 Cl2 N2 O24.50 Pb'
_cod_database_code               1565703
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.548
_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, All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) O2W(0.3333) H2WA(0.3333) H2WB(0.3333)
 O3W(0.16666) H3WA(0.16666) H3WB(0.16666) O4W(0.25) H4WA(0.25) H4WB(0.25)
 O5W(0.5) H5WA(0.5) H5WB(0.5) O11(0.5) H11A(0.5) H11B(0.5)
3.a Riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
3.b Free rotating group:
 O5W(H5WA,H5WB), O11(H11A,H11B)
3.c Rotating group:
 O1W(H1WA,H1WB)
3.d Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B)
3.e Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C16(H16)
3.f Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;