#------------------------------------------------------------------------------
#$Date: 2016-03-05 12:10:03 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177847 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/79/7037920.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7037920
loop_
_publ_author_name
'Di Pietro, Sebastiano'
'Gautier, Nicholas'
'Imbert, Daniel'
'Pécaut, Jacques'
'Mazzanti, Marinella'
_publ_section_title
;
 Versatile pyridine-2,6-bis-tetrazolate scaffolds for the formation of
 highly luminescent lanthanide complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3429
_journal_page_last               3442
_journal_paper_doi               10.1039/c5dt04811g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C48 H27 Eu N27 O3'
_chemical_formula_weight         1181.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-11-12 deposited with the CCDC.
2016-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   32.8261(3)
_cell_length_b                   32.8261(3)
_cell_length_c                   32.8261(3)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.9555
_cell_measurement_theta_min      3.3938
_cell_volume                     35371.9(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   35.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7812  179.0000 -180.0000 27

  2 omega   24.00  111.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       44.6562 -125.0000 -150.0000 87

  3 omega  -80.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7812  -77.0000  -90.0000 80

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43756
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9294
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9456
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
4347 electrons per cell is equivalent to 272 electrons per complexe. They corresponds to 3 triethylamonium (3 x 47 = 141 electrons) and 13 water molecules (13 x 10 = 130 electrons)
;
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.017(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         9005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0614P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                4794
_reflns_number_total             9005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04811g2.cif
_cod_data_source_block           EuL5
_cod_depositor_comments          'Adding full bibliography for 7037920.cif.'
_cod_database_code               7037920
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y+1/4, -x+3/4, -z+1/4'
'x, -y, -z+1/2'
'z, x, y'
'-x, -y+1/2, z'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'-z+1/4, y+1/4, -x+3/4'
'x+1/4, -z+3/4, -y+1/4'
'-z+1/2, x, -y'
'z, -x, -y+1/2'
'y, z, x'
'-y+3/4, x+3/4, -z+1/4'
'-x, y+1/2, -z+1/2'
'-z, -x+1/2, y'
'z+1/4, y+1/4, x+1/4'
'x+1/4, z+1/4, y+1/4'
'-z+1/4, -y+3/4, x+3/4'
'-x+1/4, -z+3/4, y+3/4'
'z+1/4, -y+3/4, -x+1/4'
'-y, -z+1/2, x'
'y, -z, -x+1/2'
'-y+1/2, z, -x'
'-x+3/4, z+3/4, -y+1/4'
'x+1/2, y+1/2, z+1/2'
'y+3/4, -x+5/4, -z+3/4'
'x+1/2, -y+1/2, -z+1'
'z+1/2, x+1/2, y+1/2'
'-x+1/2, -y+1, z+1/2'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'-z+3/4, y+3/4, -x+5/4'
'x+3/4, -z+5/4, -y+3/4'
'-z+1, x+1/2, -y+1/2'
'z+1/2, -x+1/2, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+5/4, x+5/4, -z+3/4'
'-x+1/2, y+1, -z+1'
'-z+1/2, -x+1, y+1/2'
'z+3/4, y+3/4, x+3/4'
'x+3/4, z+3/4, y+3/4'
'-z+3/4, -y+5/4, x+5/4'
'-x+3/4, -z+5/4, y+5/4'
'z+3/4, -y+5/4, -x+3/4'
'-y+1/2, -z+1, x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+1, z+1/2, -x+1/2'
'-x+5/4, z+5/4, -y+3/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Eu1 Eu 0.054174(6) 0.445826(6) 0.554174(6) 0.05003(11) Uani 1 3 d S
O1 O 0.39026(11) 0.61569(10) 0.38554(13) 0.0893(12) Uani 1 1 d .
N1 N 0.11388(10) 0.39946(10) 0.54044(10) 0.0518(8) Uani 1 1 d .
N2 N 0.12175(11) 0.36017(11) 0.54745(11) 0.0608(10) Uani 1 1 d .
N3 N 0.15899(13) 0.35254(12) 0.53629(13) 0.0670(10) Uani 1 1 d .
N4 N 0.17668(12) 0.38678(11) 0.52130(12) 0.0642(10) Uani 1 1 d .
N5 N 0.11768(10) 0.48003(9) 0.52264(9) 0.0445(7) Uani 1 1 d .
N6 N 0.05074(12) 0.52195(10) 0.54470(11) 0.0610(9) Uani 1 1 d .
N7 N 0.02156(13) 0.55072(14) 0.55131(15) 0.0806(13) Uani 1 1 d .
N8 N 0.03533(16) 0.58531(14) 0.53645(18) 0.0964(17) Uani 1 1 d .
N9 N 0.07264(14) 0.57980(12) 0.51907(17) 0.0826(14) Uani 1 1 d .
C1 C 0.14809(13) 0.41521(13) 0.52416(12) 0.0491(10) Uani 1 1 d .
C2 C 0.15125(13) 0.45722(13) 0.51255(13) 0.0529(10) Uani 1 1 d .
C3 C 0.18322(13) 0.47371(14) 0.49264(13) 0.0545(11) Uani 1 1 d .
H3A H 0.2062 0.4573 0.4863 0.065 Uiso 1 1 calc R
C4 C 0.18287(13) 0.51545(14) 0.48103(13) 0.0561(11) Uani 1 1 d .
C5 C 0.14832(14) 0.53856(14) 0.49156(13) 0.0585(11) Uani 1 1 d .
H5A H 0.1465 0.5666 0.4847 0.070 Uiso 1 1 calc R
C6 C 0.11727(13) 0.51932(13) 0.51202(14) 0.0556(11) Uani 1 1 d .
C7 C 0.08095(14) 0.54101(13) 0.52468(13) 0.0519(10) Uani 1 1 d .
C8 C 0.21671(14) 0.53270(14) 0.45999(13) 0.0605(11) Uani 1 1 d .
C9 C 0.24603(14) 0.54766(13) 0.44554(13) 0.0580(10) Uani 1 1 d .
C10 C 0.28333(14) 0.56470(12) 0.42887(13) 0.0562(11) Uani 1 1 d .
C11 C 0.29292(15) 0.60564(14) 0.43400(15) 0.0662(12) Uani 1 1 d .
H11A H 0.2739 0.6229 0.4474 0.079 Uiso 1 1 calc R
C12 C 0.32798(16) 0.62166(15) 0.42068(17) 0.0734(14) Uani 1 1 d .
H12A H 0.3341 0.6495 0.4258 0.088 Uiso 1 1 calc R
C13 C 0.35562(16) 0.59722(16) 0.39923(18) 0.0767(14) Uani 1 1 d .
C14 C 0.34832(16) 0.55604(17) 0.39422(18) 0.0800(15) Uani 1 1 d .
H14A H 0.3678 0.5388 0.3814 0.096 Uiso 1 1 calc R
C15 C 0.31124(16) 0.54057(14) 0.40864(16) 0.0734(14) Uani 1 1 d .
H15A H 0.3051 0.5126 0.4044 0.088 Uiso 1 1 calc R
C16 C 0.42031(18) 0.5915(2) 0.3638(2) 0.107(2) Uani 1 1 d .
H16A H 0.4433 0.6088 0.3560 0.161 Uiso 1 1 calc R
H16B H 0.4079 0.5799 0.3392 0.161 Uiso 1 1 calc R
H16C H 0.4300 0.5694 0.3814 0.161 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N6 Eu1 N6 80.08(14) 35_455 .
N6 Eu1 N6 80.08(14) 35_455 45
N6 Eu1 N6 80.08(14) . 45
N6 Eu1 N1 146.81(11) 35_455 45
N6 Eu1 N1 86.89(12) . 45
N6 Eu1 N1 127.66(11) 45 45
N6 Eu1 N1 127.66(11) 35_455 35_455
N6 Eu1 N1 146.81(11) . 35_455
N6 Eu1 N1 86.89(12) 45 35_455
N1 Eu1 N1 77.16(12) 45 35_455
N6 Eu1 N1 86.89(12) 35_455 .
N6 Eu1 N1 127.66(11) . .
N6 Eu1 N1 146.81(11) 45 .
N1 Eu1 N1 77.16(12) 45 .
N1 Eu1 N1 77.16(12) 35_455 .
N6 Eu1 N5 63.64(11) 35_455 35_455
N6 Eu1 N5 136.74(12) . 35_455
N6 Eu1 N5 71.52(11) 45 35_455
N1 Eu1 N5 136.35(10) 45 35_455
N1 Eu1 N5 64.13(10) 35_455 35_455
N1 Eu1 N5 75.33(10) . 35_455
N6 Eu1 N5 71.52(11) 35_455 .
N6 Eu1 N5 63.64(11) . .
N6 Eu1 N5 136.74(12) 45 .
N1 Eu1 N5 75.33(11) 45 .
N1 Eu1 N5 136.35(10) 35_455 .
N1 Eu1 N5 64.13(10) . .
N5 Eu1 N5 119.974(4) 35_455 .
N6 Eu1 N5 136.74(12) 35_455 45
N6 Eu1 N5 71.52(11) . 45
N6 Eu1 N5 63.64(11) 45 45
N1 Eu1 N5 64.13(10) 45 45
N1 Eu1 N5 75.33(10) 35_455 45
N1 Eu1 N5 136.35(10) . 45
N5 Eu1 N5 119.973(4) 35_455 45
N5 Eu1 N5 119.974(4) . 45
C13 O1 C16 118.9(4) . .
N2 N1 C1 106.1(3) . .
N2 N1 Eu1 134.6(3) . .
C1 N1 Eu1 119.2(3) . .
N3 N2 N1 108.6(3) . .
N2 N3 N4 110.2(4) . .
C1 N4 N3 104.7(4) . .
C6 N5 C2 118.2(4) . .
C6 N5 Eu1 121.0(3) . .
C2 N5 Eu1 120.5(2) . .
C7 N6 N7 105.9(4) . .
C7 N6 Eu1 119.3(3) . .
N7 N6 Eu1 134.3(3) . .
N8 N7 N6 107.3(4) . .
N7 N8 N9 110.4(4) . .
C7 N9 N8 104.9(4) . .
N4 C1 N1 110.3(4) . .
N4 C1 C2 127.3(4) . .
N1 C1 C2 122.3(4) . .
C3 C2 N5 121.5(4) . .
C3 C2 C1 124.8(4) . .
N5 C2 C1 113.7(4) . .
C2 C3 C4 120.7(4) . .
C5 C4 C3 117.4(4) . .
C5 C4 C8 122.2(4) . .
C3 C4 C8 120.4(4) . .
C6 C5 C4 118.0(4) . .
N5 C6 C5 124.3(4) . .
N5 C6 C7 114.1(4) . .
C5 C6 C7 121.6(4) . .
N9 C7 N6 111.5(4) . .
N9 C7 C6 127.3(4) . .
N6 C7 C6 121.2(4) . .
C9 C8 C4 174.7(5) . .
C8 C9 C10 177.2(5) . .
C15 C10 C11 117.5(4) . .
C15 C10 C9 121.3(4) . .
C11 C10 C9 121.1(4) . .
C12 C11 C10 122.3(5) . .
C11 C12 C13 119.7(5) . .
O1 C13 C14 122.7(5) . .
O1 C13 C12 116.8(5) . .
C14 C13 C12 120.5(5) . .
C13 C14 C15 117.7(5) . .
C10 C15 C14 122.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu1 N6 2.521(3) 35_455
Eu1 N6 2.521(3) .
Eu1 N6 2.521(3) 45
Eu1 N1 2.522(3) 45
Eu1 N1 2.522(3) 35_455
Eu1 N1 2.522(3) .
Eu1 N5 2.584(3) 35_455
Eu1 N5 2.584(3) .
Eu1 N5 2.584(3) 45
O1 C13 1.365(6) .
O1 C16 1.454(7) .
N1 N2 1.335(5) .
N1 C1 1.347(5) .
N2 N3 1.300(5) .
N3 N4 1.357(5) .
N4 C1 1.327(5) .
N5 C6 1.336(5) .
N5 C2 1.373(5) .
N6 C7 1.344(5) .
N6 N7 1.363(5) .
N7 N8 1.316(6) .
N8 N9 1.363(6) .
N9 C7 1.315(6) .
C1 C2 1.434(6) .
C2 C3 1.350(6) .
C3 C4 1.422(6) .
C4 C5 1.408(6) .
C4 C8 1.425(6) .
C5 C6 1.375(6) .
C6 C7 1.449(6) .
C8 C9 1.180(6) .
C9 C10 1.453(6) .
C10 C15 1.381(6) .
C10 C11 1.391(6) .
C11 C12 1.338(7) .
C12 C13 1.401(7) .
C13 C14 1.383(7) .
C14 C15 1.401(7) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.173 0.003 0.016 18733 4347 ' '
