#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:22:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179324 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/21/4322163.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_4322163
loop_
_publ_author_name
'Raphaël Wietzke'
'Marinella Mazzanti'
'Jean-Marc Latour'
'Jacques Pécaut'
_publ_section_title
;
 Crystal Structure and Solution Fluxionality of Lanthanide Complexes of
 2,4,6,-Tris-2-pyridyl-1,3,5-triazine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3581
_journal_page_last               3585
_journal_paper_doi               10.1021/ic990122w
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C22 H28 Cl3 Eu N6 O4'
_chemical_formula_weight         698.81
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                96.3090(10)
_cell_angle_beta                 100.4130(10)
_cell_angle_gamma                99.3150(10)
_cell_formula_units_Z            2
_cell_length_a                   7.1306(5)
_cell_length_b                   13.8850(9)
_cell_length_c                   13.9400(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1325.71(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6197
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_F_000             696
_refine_diff_density_max         2.287
_refine_diff_density_min         -3.243
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_obs          0.0622
_refine_ls_shift/esd_max         -0.062
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1105P)²+6.2314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1681
_refine_ls_wR_factor_obs         0.1664
_reflns_number_observed          4152
_reflns_number_total             4422
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990122w_1.cif
_cod_data_source_block           struc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+6.2314P] 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^)+(0.1105P)^2^+6.2314P] 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        1325.7(2)
_cod_database_code               4322163
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Eu Eu 0.79513(3) 0.18679(2) 0.31269(2) 0.01528(7) Uani 1 d . .
Cl1 Cl 0.9878(2) 0.13953(10) 0.17073(9) 0.0222(3) Uani 1 d . .
Cl2 Cl 0.6576(2) -0.00040(10) 0.33479(11) 0.0284(3) Uani 1 d . .
Cl3 Cl 0.5059(2) 0.28119(10) 0.35633(9) 0.0202(3) Uani 1 d . .
O1 O 0.8378(6) 0.1994(3) 0.4947(3) 0.0237(10) Uani 1 d . .
H1 H 0.9639(6) 0.2233(3) 0.5295(3) 0.028 Uiso 1 calc R .
O2 O 1.1201(5) 0.1604(3) 0.3934(3) 0.0219(9) Uani 1 d . .
H2 H 1.2154(5) 0.2150(3) 0.4223(3) 0.026 Uiso 1 calc R .
O3 O 0.1766(10) 0.1935(5) 0.6259(4) 0.064(2) Uani 1 d . .
O4 O 0.1330(10) 0.6994(4) 0.1950(3) 0.052(2) Uani 1 d . .
N1 N 0.7688(6) 0.3144(3) 0.1945(3) 0.0159(10) Uani 1 d . .
N2 N 0.6554(7) 0.3496(3) 0.0343(3) 0.0174(10) Uani 1 d . .
N3 N 0.8675(7) 0.4738(3) 0.1537(3) 0.0200(11) Uani 1 d . .
N4 N 1.0157(7) 0.3609(3) 0.3701(3) 0.0188(11) Uani 1 d . .
N5 N 0.5246(7) 0.1359(3) 0.1498(3) 0.0202(11) Uani 1 d . .
N6 N 0.8516(7) 0.6028(3) 0.0178(3) 0.0221(11) Uani 1 d . .
C1 C 0.8715(8) 0.4067(4) 0.2151(4) 0.0185(12) Uani 1 d . .
C2 C 0.6585(8) 0.2905(4) 0.1034(4) 0.0179(12) Uani 1 d . .
C3 C 0.7596(7) 0.4411(4) 0.0633(4) 0.0159(12) Uani 1 d . .
C4 C 1.0010(8) 0.4348(4) 0.3135(4) 0.0184(12) Uani 1 d . .
C5 C 1.1035(8) 0.5301(4) 0.3435(4) 0.0215(13) Uani 1 d . .
H5 H 1.0903(8) 0.5784(4) 0.3028(4) 0.026 Uiso 1 calc R .
C6 C 1.2266(8) 0.5521(4) 0.4356(4) 0.0213(13) Uani 1 d . .
H6 H 1.2959(8) 0.6157(4) 0.4584(4) 0.026 Uiso 1 calc R .
C7 C 1.2440(8) 0.4763(4) 0.4932(4) 0.0219(13) Uani 1 d . .
H7 H 1.3270(8) 0.4883(4) 0.5546(4) 0.026 Uiso 1 calc R .
C8 C 1.1357(8) 0.3836(4) 0.4571(4) 0.0209(13) Uani 1 d . .
H8 H 1.1476(8) 0.3340(4) 0.4963(4) 0.025 Uiso 1 calc R .
C9 C 0.5316(8) 0.1926(4) 0.0778(4) 0.0183(12) Uani 1 d . .
C10 C 0.4146(8) 0.1643(4) -0.0161(4) 0.0213(13) Uani 1 d . .
H10 H 0.4222(8) 0.2051(4) -0.0645(4) 0.026 Uiso 1 calc R .
C11 C 0.2880(8) 0.0752(4) -0.0362(4) 0.0234(14) Uani 1 d . .
H11 H 0.2114(8) 0.0538(4) -0.0988(4) 0.028 Uiso 1 calc R .
C12 C 0.2772(8) 0.0183(4) 0.0386(4) 0.0204(13) Uani 1 d . .
H12 H 0.1904(8) -0.0413(4) 0.0280(4) 0.025 Uiso 1 calc R .
C13 C 0.3975(8) 0.0516(4) 0.1296(4) 0.0220(13) Uani 1 d . .
H13 H 0.3891(8) 0.0128(4) 0.1795(4) 0.026 Uiso 1 calc R .
C14 C 0.7521(7) 0.5102(4) -0.0111(4) 0.0170(12) Uani 1 d . .
C15 C 0.6431(8) 0.4768(4) -0.1058(4) 0.0210(13) Uani 1 d . .
H15 H 0.5784(8) 0.4117(4) -0.1234(4) 0.025 Uiso 1 calc R .
C16 C 0.6337(9) 0.5437(4) -0.1735(4) 0.0250(14) Uani 1 d . .
H16 H 0.5594(9) 0.5245(4) -0.2368(4) 0.030 Uiso 1 calc R .
C17 C 0.7361(8) 0.6386(4) -0.1450(4) 0.0249(13) Uani 1 d . .
H17 H 0.7341(8) 0.6841(4) -0.1893(4) 0.030 Uiso 1 calc R .
C18 C 0.8417(8) 0.6651(4) -0.0500(4) 0.0230(13) Uani 1 d . .
H18 H 0.9098(8) 0.7295(4) -0.0316(4) 0.028 Uiso 1 calc R .
C21 C 0.6989(9) 0.1756(5) 0.5534(4) 0.031(2) Uani 1 d . .
H21A H 0.7614(9) 0.1888(5) 0.6218(4) 0.046 Uiso 1 calc R .
H21B H 0.6410(9) 0.1070(5) 0.5366(4) 0.046 Uiso 1 calc R .
H21C H 0.6001(9) 0.2148(5) 0.5417(4) 0.046 Uiso 1 calc R .
C22 C 1.1649(9) 0.0640(5) 0.3967(5) 0.035(2) Uani 1 d . .
H22A H 1.2966(9) 0.0693(5) 0.4308(5) 0.052 Uiso 1 calc R .
H22B H 1.1493(9) 0.0310(5) 0.3307(5) 0.052 Uiso 1 calc R .
H22C H 1.0790(9) 0.0270(5) 0.4307(5) 0.052 Uiso 1 calc R .
C23 C 0.2819(14) 0.2663(7) 0.7020(7) 0.061(3) Uani 1 d . .
C24 C 0.1744(12) 0.7933(5) 0.1678(5) 0.044(2) Uani 1 d . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 Eu O2 67.12(14) . . ?
O1 Eu N1 132.61(13) . . ?
O2 Eu N1 119.90(13) . . ?
O1 Eu N4 78.34(13) . . ?
O2 Eu N4 72.80(13) . . ?
N1 Eu N4 62.67(13) . . ?
O1 Eu N5 141.36(14) . . ?
O2 Eu N5 143.28(14) . . ?
N1 Eu N5 63.21(13) . . ?
N4 Eu N5 125.64(14) . . ?
O1 Eu Cl1 138.84(10) . . ?
O2 Eu Cl1 71.92(10) . . ?
N1 Eu Cl1 72.76(10) . . ?
N4 Eu Cl1 93.54(11) . . ?
N5 Eu Cl1 75.21(11) . . ?
O1 Eu Cl2 78.49(10) . . ?
O2 Eu Cl2 87.04(9) . . ?
N1 Eu Cl2 143.51(9) . . ?
N4 Eu Cl2 153.82(10) . . ?
N5 Eu Cl2 80.45(10) . . ?
Cl1 Eu Cl2 95.92(5) . . ?
O1 Eu Cl3 75.74(10) . . ?
O2 Eu Cl3 139.26(10) . . ?
N1 Eu Cl3 74.55(10) . . ?
N4 Eu Cl3 84.12(11) . . ?
N5 Eu Cl3 77.35(11) . . ?
Cl1 Eu Cl3 144.20(4) . . ?
Cl2 Eu Cl3 101.76(5) . . ?
C21 O1 Eu 129.7(3) . . ?
C22 O2 Eu 122.0(3) . . ?
C1 N1 C2 115.1(5) . . ?
C1 N1 Eu 123.5(3) . . ?
C2 N1 Eu 121.2(3) . . ?
C2 N2 C3 115.6(4) . . ?
C1 N3 C3 114.9(4) . . ?
C8 N4 C4 117.0(4) . . ?
C8 N4 Eu 122.2(4) . . ?
C4 N4 Eu 120.6(3) . . ?
C13 N5 C9 117.5(4) . . ?
C13 N5 Eu 123.9(4) . . ?
C9 N5 Eu 118.0(3) . . ?
C14 N6 C18 116.8(5) . . ?
N3 C1 N1 125.1(5) . . ?
N3 C1 C4 118.0(4) . . ?
N1 C1 C4 116.8(5) . . ?
N2 C2 N1 124.3(5) . . ?
N2 C2 C9 117.5(4) . . ?
N1 C2 C9 118.1(5) . . ?
N3 C3 N2 124.7(5) . . ?
N3 C3 C14 118.5(5) . . ?
N2 C3 C14 116.8(4) . . ?
N4 C4 C5 123.1(5) . . ?
N4 C4 C1 116.0(4) . . ?
C5 C4 C1 120.8(5) . . ?
C4 C5 C6 118.6(5) . . ?
C5 C6 C7 118.5(5) . . ?
C8 C7 C6 118.7(5) . . ?
N4 C8 C7 124.1(5) . . ?
N5 C9 C10 122.3(5) . . ?
N5 C9 C2 117.4(4) . . ?
C10 C9 C2 120.2(5) . . ?
C11 C10 C9 119.1(5) . . ?
C10 C11 C12 118.5(5) . . ?
C13 C12 C11 118.8(5) . . ?
N5 C13 C12 123.7(5) . . ?
N6 C14 C15 123.5(5) . . ?
N6 C14 C3 117.4(4) . . ?
C15 C14 C3 119.1(4) . . ?
C14 C15 C16 118.1(5) . . ?
C17 C16 C15 119.0(5) . . ?
C16 C17 C18 119.0(5) . . ?
N6 C18 C17 123.6(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu O1 2.483(4) . ?
Eu O2 2.488(4) . ?
Eu N1 2.555(4) . ?
Eu N4 2.617(4) . ?
Eu N5 2.646(4) . ?
Eu Cl1 2.6874(14) . ?
Eu Cl2 2.6967(14) . ?
Eu Cl3 2.7378(14) . ?
O1 C21 1.417(8) . ?
O2 C22 1.429(8) . ?
O3 C23 1.394(10) . ?
O4 C24 1.399(9) . ?
N1 C1 1.342(7) . ?
N1 C2 1.343(6) . ?
N2 C2 1.331(7) . ?
N2 C3 1.342(7) . ?
N3 C1 1.333(7) . ?
N3 C3 1.342(6) . ?
N4 C8 1.326(7) . ?
N4 C4 1.367(7) . ?
N5 C13 1.328(7) . ?
N5 C9 1.344(7) . ?
N6 C14 1.344(7) . ?
N6 C18 1.350(8) . ?
C1 C4 1.482(7) . ?
C2 C9 1.474(7) . ?
C3 C14 1.488(8) . ?
C4 C5 1.384(7) . ?
C5 C6 1.390(7) . ?
C6 C7 1.400(8) . ?
C7 C8 1.378(8) . ?
C9 C10 1.397(7) . ?
C10 C11 1.376(8) . ?
C11 C12 1.382(9) . ?
C12 C13 1.381(7) . ?
C14 C15 1.392(7) . ?
C15 C16 1.396(8) . ?
C16 C17 1.376(8) . ?
C17 C18 1.379(8) . ?
