Exciplex formation as an approach to selective Copper(II) fluorescent sensors
Correia, Bruna B.; Brown, Thomas R.; Reibenspies, Joseph H.; Lee, Hee-Seung; Hancock, Robert D.; Inorganica Chimica Acta 506 (2020) 119544–; doi:10.1016/j.ica.2020.119544

data_1565034
_publ_section_title
;
 Exciplex formation as an approach to selective Copper(II) fluorescent
 sensors
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119544
_journal_paper_doi               10.1016/j.ica.2020.119544
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C36 H44 N4 Pb, 2(Cl O4)'
_chemical_formula_sum            'C36 H44 Cl2 N4 O8 Pb'
_chemical_formula_weight         938.84
_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     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.106(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1622(4)
_cell_length_b                   18.9273(7)
_cell_length_c                   19.6809(7)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.30
_cell_measurement_theta_min      3.24
_cell_volume                     3784.8(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Micro-Source CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35484
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        65.418
_diffrn_reflns_theta_max         65.418
_diffrn_reflns_theta_min         3.240
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           50
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           .1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.428
_exptl_absorpt_correction_T_max  0.3165
_exptl_absorpt_correction_T_min  0.1928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1221 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.6092. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.039
_refine_diff_density_max         2.160
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0210P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5460
_reflns_number_total             6439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-119544.cif
_cod_data_source_block           rh147
_cod_database_code               1565034
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.393
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a 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), C8(H8A,H8B), C9(H9A,H9B), C16(H16A,H16B), C23(H23A,H23B),
 C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;