A Strongly Luminescent Organic-Solvent-Soluble Salt of the Tris(dipicolinato)europium(III) Trianion
Brayshaw, P. A.; Harrowfield, J. M.; Sobolev, A. N.; Acta Crystallographica Section C 51 (1995) 1799–1802; doi:10.1107/S0108270195002897

data_2003931
_publ_section_title
;
 A Strongly Luminescent Organic-Solvent-Soluble Salt of the
 Tris(dipicolinato)europium(III) Trianion
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1799
_journal_page_last               1802
_journal_paper_doi               10.1107/S0108270195002897
_journal_volume                  51
_journal_year                    1995
_chemical_formula_analytical     'C45 H77 Eu1 N6 O16'
_chemical_formula_moiety         '(C8 H20 N)3,C21 H9 Eu1 N3 O12,4(H2 O1)'
_chemical_formula_structural     '[N(C2H5)4]3.[Eu(dipicolinate)3].4H2O'
_chemical_formula_sum            'C45 H77 Eu N6 O16'
_chemical_formula_weight         1110.09
_chemical_name_common
'The tetraethylammonium salt of the Eu(dipic)3'
_chemical_name_systematic
;
tris(tetraethylammonium)tris(dipicolinato)europium(III) tetrahydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 98.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.096(5)
_cell_length_b                   10.692(2)
_cell_length_c                   20.188(4)
_cell_measurement_reflns_used    6
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      18.6
_cell_volume                     5145.9(18)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1983)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       2\q/\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9031
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  0.7726
_exptl_absorpt_correction_T_min  0.7311
_exptl_absorpt_correction_type   'SHELX76 gaussian (Sheldrick, 1976)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       'Pseudo-hexagonal rod'
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         .884
_refine_diff_density_min         -.588
_refine_ls_extinction_coef       0.00022(8)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment    'H atoms were located but not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         9031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_obs          0.0417
_refine_ls_shift/esd_max         -0.129
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0362P)^2^ + 4.4863P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0975
_refine_ls_wR_factor_obs         0.0860
_reflns_number_observed          6645
_reflns_number_total             9031
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            na1151.cif
_cod_data_source_block           EUDIPIC
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5146(2)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C45 H77 Eu1 N6 O16'
_cod_database_code               2003931
_cod_database_fobs_code          2003931