Studying anion-dependent paradoxically fluorescent Cu(II) complexes bearing a pyridine-decorated tetradentate half-salamo-like ligand
Han, Xiu-Juan; Li, Ruo-Yu; Yue, Yong-Ning; Zhang, Yang; Dong, Wen-Kui; Inorganica Chimica Acta 529 (2022) 120634–; doi:10.1016/j.ica.2021.120634

data_1566010
_publ_section_title
;
 Studying anion-dependent paradoxically fluorescent Cu(II) complexes
 bearing a pyridine-decorated tetradentate half-salamo-like ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120634
_journal_paper_doi               10.1016/j.ica.2021.120634
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C15 H13 Cu N5 O8'
_chemical_formula_sum            'C15 H13 Cu N5 O8'
_chemical_formula_weight         454.84
_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                 106.2220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2783(4)
_cell_length_b                   11.8570(3)
_cell_length_c                   17.5045(3)
_cell_measurement_reflns_used    6909
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.60
_cell_volume                     3443.35(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43403
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.741
_diffrn_reflns_theta_min         2.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7299
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0302P)^2^+3.9793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5525
_reflns_number_total             7299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120634.cif
_cod_data_source_block           3
_cod_database_code               1566010
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O15-N10 \\sim O15A-N10 \\sim O16-N10
 with sigma of 0.02
 O16-O14 \\sim O14-O15
 with sigma of 0.02
3. Restrained planarity
 O14, N10, O16, O15
 with sigma of 0.1
 O14, N10A, O15A, O16A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N10, O15, O16, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O16A, O15A, N10A, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O16A)=Sof(O15A)=Sof(N10A)=1-FVAR(1)
 Sof(N10)=Sof(O15)=Sof(O16)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C22(H22A,H22B), C23(H23A,H23B)
7.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C9(H9), C15(H15), C24(H24), C28(H28), C12(H12), C13(H13), C27(H27),
 C1(H1), C6(H6), C2(H2), C21(H21), C4(H4), C16(H16), C3(H3), C18(H18), C19(H19),
  C17(H17)
;
_shelx_res_checksum              63346
_shelx_hkl_checksum              45373