Effect of Protonation and Zn(II) Coordination on the Fluorescence Emission of a Phenanthroline-Containing Macrocycle. An Unusual Case of "Nonemissive" Zn(II) Complex
Carla Bazzicalupi; Andrea Bencini; Antonio Bianchi; Claudia Giorgi; Vieri Fusi; Barbara Valtancoli; M. Alexandra Bernardo; Fernando Pina; Inorganic Chemistry 38 (1999) 3806–3813; doi:10.1021/ic981374k

data_4322199
_publ_section_title
;
 Effect of Protonation and Zn(II) Coordination on the Fluorescence
 Emission of a Phenanthroline-Containing Macrocycle. An Unusual Case of
 "Nonemissive" Zn(II) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3806
_journal_page_last               3813
_journal_paper_doi               10.1021/ic981374k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety
;
(C18 H24 N5 3+), (Br -)3, H2 O
;
_chemical_formula_structural
;
(C18 H24 N5) (Br)3 (H2 O)
;
_chemical_formula_sum            'C18 H26 Br3 N5 O'
_chemical_formula_weight         568.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.750(6)
_cell_length_b                   7.875(9)
_cell_length_c                   20.487(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      10
_cell_measurement_theta_min      6
_cell_volume                     2218(3)
_computing_cell_refinement       'ENRAF NONIUS CAD4'
_computing_data_collection       'ENRAF NONIUS CAD4'
_computing_data_reduction        'ENRAF NONIUS CAD4'
_computing_molecular_graphics    'ORTEP (Johson, 1971)'
_computing_publication_material
;
SHELXL-93 (Sheldrick, 1993), PARST93 (Nardelli, 1993)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altamore,1993)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'ENRAF NONIUS CAD4'
_diffrn_measurement_method       "'\q/2\q"
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3964
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.473
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_obs          0.0655
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+8.1333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1840
_refine_ls_wR_factor_obs         0.1363
_reflns_number_observed          1987
_reflns_number_total             3844
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981374k_1.cif
_cod_data_source_block           '[H3L]Br3.H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+8.1333P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+8.1333P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2218.3(27)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4322199