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_1565032
_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         'C38 H47 Cd N5, 2(Cl O4)'
_chemical_formula_sum            'C38 H47 Cd Cl2 N5 O8'
_chemical_formula_weight         885.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 101.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8274(3)
_cell_length_b                   13.1823(3)
_cell_length_c                   23.1202(5)
_cell_measurement_reflns_used    9620
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.40
_cell_measurement_theta_min      3.67
_cell_volume                     3833.37(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      99.99
_diffrn_detector                 'Bruker CMOS area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_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  0.0649
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76294
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.463
_diffrn_reflns_theta_min         3.669
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.336
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1305 before and 0.0783 after correction. The Ratio of minimum to maximum transmission is 0.6769. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_preparation       100
_exptl_crystal_recrystallization_method 100
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7557
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0535P)^2^+11.2799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6966
_reflns_number_total             7557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-506-119544.cif
_cod_data_source_block           rh144
_cod_database_code               1565032
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.281
_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. Restrained distances
 Cl1_2-O4_2 \\sim Cl1_1-O4_1 \\sim Cl1_3-O4_3 \\sim Cl1_2-O2_2 \\sim Cl1_1-O2_1
\\sim Cl1_3-O2_3 ~
 Cl1_2-O1_2 \\sim Cl1_1-O1_1 \\sim Cl1_3-O1_3 \\sim Cl1_3-O3_3 \\sim Cl1_1-O3_1
\\sim Cl1_2-O3_2
 with sigma of 0.02
 O1_3-O2_3 \\sim O1_1-O2_1 \\sim O1_2-O2_2 \\sim O2_3-O3_3 \\sim O2_1-O3_1
\\sim O2_2-O3_2 \\sim O1_3-
 O3_3 \\sim O1_1-O3_1 \\sim O1_2-O3_2 \\sim O2_3-O4_3 \\sim O2_1-O4_1 \\sim
O2_2-O4_2 \\sim O3_3-O4_3 ~
 O3_1-O4_1 \\sim O3_2-O4_2 \\sim O1_3-O4_3 \\sim O1_1-O4_1 \\sim O1_2-O4_2
 with sigma of 0.02
3. Rigid bond restraints
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
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)
6.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)
6.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)
6.c Idealised Me refined as rotating group:
 C2AC(H2AA,H2AB,H2AC)
;