#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309110.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_4309110
loop_
_publ_author_name
'Louise Natrajan'
'Jacques Pécaut'
'Marinella Mazzanti'
'Colette LeBrun'
_publ_section_title
;
Controlled Hydrolysis of Lanthanide Complexes of the N-Donor Tripod
Tris(2-pyridylmethyl)amine versus Bisligand Complex Formation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4756
_journal_page_last               4765
_journal_paper_doi               10.1021/ic0502224
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H38 Eu2 F12 N8 O14 S4'
_chemical_formula_weight         1514.94
_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-97
_cell_angle_alpha                101.038(3)
_cell_angle_beta                 101.996(3)
_cell_angle_gamma                106.494(3)
_cell_formula_units_Z            1
_cell_length_a                   10.168(2)
_cell_length_b                   10.759(2)
_cell_length_c                   13.117(3)
_cell_measurement_temperature    223(2)
_cell_volume                     1297.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5777
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    2.671
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         3709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0204
_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)+(0.0380P)²+0.9934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                3624
_reflns_number_total             3709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0502224si20050211_013138_8.cif
_cod_data_source_block           struc_[Eu(tpa)(?-OH)(OTf)2]2,8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        1296.9(4)
_cod_database_code               4309110
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu Eu 0.986193(13) 0.461719(13) 0.353145(10) 0.01684(8) Uani 1 1 d . . .
O1 O 1.1083(2) 0.4586(2) 0.51414(17) 0.0230(5) Uani 1 1 d . . .
H1O H 1.168(5) 0.435(4) 0.532(3) 0.038(13) Uiso 1 1 d . . .
N1 N 0.9778(3) 0.4088(3) 0.1512(2) 0.0221(6) Uani 1 1 d . . .
N2 N 1.1343(3) 0.7144(3) 0.3944(2) 0.0249(6) Uani 1 1 d . . .
N3 N 1.0607(3) 0.2403(3) 0.2910(2) 0.0242(6) Uani 1 1 d . . .
N4 N 1.2401(3) 0.5126(3) 0.3180(2) 0.0203(5) Uani 1 1 d . . .
C1 C 1.2348(3) 0.5216(4) 0.2056(3) 0.0251(7) Uani 1 1 d . . .
H1A H 1.239(4) 0.614(4) 0.207(3) 0.023(8) Uiso 1 1 d . . .
H1B H 1.312(4) 0.506(3) 0.188(3) 0.028(9) Uiso 1 1 d . . .
C2 C 1.0991(3) 0.4299(3) 0.1219(2) 0.0219(7) Uani 1 1 d . . .
C3 C 1.0988(4) 0.3785(4) 0.0166(3) 0.0291(8) Uani 1 1 d . . .
H3 H 1.180(4) 0.389(4) -0.001(3) 0.034(10) Uiso 1 1 d . . .
C4 C 0.9731(4) 0.3043(4) -0.0601(3) 0.0328(8) Uani 1 1 d . . .
H4 H 0.977(5) 0.271(4) -0.131(4) 0.051(12) Uiso 1 1 d . . .
C5 C 0.8476(4) 0.2822(3) -0.0301(3) 0.0312(8) Uani 1 1 d . . .
H5 H 0.762(4) 0.233(4) -0.079(3) 0.037(10) Uiso 1 1 d . . .
C6 C 0.8541(4) 0.3360(3) 0.0754(3) 0.0276(7) Uani 1 1 d . . .
H6 H 0.773(4) 0.325(4) 0.094(3) 0.034(10) Uiso 1 1 d . . .
C7 C 1.3380(3) 0.6422(3) 0.3939(3) 0.0254(7) Uani 1 1 d . . .
H7A H 1.353(3) 0.632(3) 0.463(3) 0.021(8) Uiso 1 1 d . . .
H7B H 1.434(4) 0.671(4) 0.378(3) 0.035(10) Uiso 1 1 d . . .
C8 C 1.2725(3) 0.7499(3) 0.3924(2) 0.0244(7) Uani 1 1 d . . .
C9 C 1.3491(4) 0.8798(4) 0.3932(3) 0.0329(8) Uani 1 1 d . . .
H9 H 1.443(5) 0.898(4) 0.390(3) 0.055(13) Uiso 1 1 d . . .
C10 C 1.2860(4) 0.9771(4) 0.4014(3) 0.0394(9) Uani 1 1 d . . .
H10 H 1.332(5) 1.066(4) 0.403(3) 0.047(11) Uiso 1 1 d . . .
C11 C 1.1474(4) 0.9435(4) 0.4089(3) 0.0364(8) Uani 1 1 d . . .
H11 H 1.105(4) 1.011(4) 0.417(3) 0.046(11) Uiso 1 1 d . . .
C12 C 1.0760(4) 0.8118(4) 0.4047(3) 0.0316(8) Uani 1 1 d . . .
H12 H 0.981(4) 0.787(4) 0.405(3) 0.032(10) Uiso 1 1 d . . .
C13 C 1.2965(3) 0.4035(3) 0.3389(3) 0.0254(7) Uani 1 1 d . . .
H13A H 1.309(4) 0.404(3) 0.415(3) 0.023(8) Uiso 1 1 d . . .
H13B H 1.382(4) 0.420(3) 0.322(3) 0.024(8) Uiso 1 1 d . . .
C14 C 1.1916(3) 0.2694(3) 0.2742(2) 0.0233(7) Uani 1 1 d . . .
C15 C 1.2254(4) 0.1825(4) 0.1999(3) 0.0305(8) Uani 1 1 d . . .
H15 H 1.317(4) 0.210(4) 0.191(3) 0.033(10) Uiso 1 1 d . . .
C16 C 1.1242(4) 0.0602(4) 0.1420(3) 0.0348(8) Uani 1 1 d . . .
H16 H 1.142(5) 0.002(4) 0.094(4) 0.045(12) Uiso 1 1 d . . .
C17 C 0.9927(4) 0.0261(4) 0.1624(3) 0.0351(8) Uani 1 1 d . . .
H17 H 0.926(4) -0.057(4) 0.123(3) 0.041(11) Uiso 1 1 d . . .
C18 C 0.9655(4) 0.1181(3) 0.2365(3) 0.0295(8) Uani 1 1 d . . .
H18 H 0.879(4) 0.100(4) 0.252(3) 0.034(10) Uiso 1 1 d . . .
S1 S 0.67421(8) 0.56831(8) 0.25875(7) 0.02560(18) Uani 1 1 d . . .
F1S1 F 0.6917(4) 0.7106(3) 0.1178(2) 0.0794(10) Uani 1 1 d . . .
F2S1 F 0.7791(3) 0.8279(3) 0.2816(3) 0.0763(9) Uani 1 1 d . . .
F3S1 F 0.5527(2) 0.7416(2) 0.21278(19) 0.0449(5) Uani 1 1 d . . .
O1S1 O 0.8144(2) 0.5597(2) 0.25649(18) 0.0264(5) Uani 1 1 d . . .
O2S1 O 0.5564(3) 0.4649(3) 0.1801(2) 0.0478(7) Uani 1 1 d . . .
O3S1 O 0.6592(3) 0.6014(3) 0.3660(2) 0.0425(7) Uani 1 1 d . . .
C1S C 0.6744(4) 0.7190(4) 0.2150(3) 0.0366(9) Uani 1 1 d . . .
S2 S 0.64355(8) 0.17790(8) 0.30371(6) 0.02336(18) Uani 1 1 d . . .
F1S2 F 0.5143(2) 0.1663(2) 0.10492(16) 0.0439(5) Uani 1 1 d . . .
F2S2 F 0.6292(2) 0.0279(3) 0.11602(18) 0.0520(6) Uani 1 1 d . . .
F3S2 F 0.4299(2) -0.0093(2) 0.1565(2) 0.0517(6) Uani 1 1 d . . .
O1S2 O 0.7671(2) 0.2778(2) 0.29201(18) 0.0267(5) Uani 1 1 d . . .
O2S2 O 0.5450(2) 0.2337(3) 0.34181(19) 0.0340(6) Uani 1 1 d . . .
O3S2 O 0.6785(3) 0.0776(3) 0.3499(2) 0.0392(6) Uani 1 1 d . . .
C2S C 0.5495(4) 0.0866(4) 0.1628(3) 0.0311(8) Uani 1 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 O1 69.64(10) . 2_766 ?
O1 Eu O1S2 109.11(8) . . ?
O1 Eu O1S2 84.89(8) 2_766 . ?
O1 Eu O1S1 144.84(8) . . ?
O1 Eu O1S1 76.85(8) 2_766 . ?
O1S2 Eu O1S1 77.43(8) . . ?
O1 Eu N1 142.33(8) . . ?
O1 Eu N1 148.01(8) 2_766 . ?
O1S2 Eu N1 83.44(8) . . ?
O1S1 Eu N1 71.58(7) . . ?
O1 Eu N2 89.19(8) . . ?
O1 Eu N2 82.57(8) 2_766 . ?
O1S2 Eu N2 152.55(8) . . ?
O1S1 Eu N2 75.98(8) . . ?
N1 Eu N2 94.51(8) . . ?
O1 Eu N4 82.12(8) . . ?
O1 Eu N4 136.86(8) 2_766 . ?
O1S2 Eu N4 136.28(8) . . ?
O1S1 Eu N4 117.75(8) . . ?
N1 Eu N4 66.07(8) . . ?
N2 Eu N4 64.60(8) . . ?
O1 Eu N3 80.72(8) . . ?
O1 Eu N3 136.28(8) 2_766 . ?
O1S2 Eu N3 75.08(8) . . ?
O1S1 Eu N3 133.07(8) . . ?
N1 Eu N3 68.13(8) . . ?
N2 Eu N3 129.50(8) . . ?
N4 Eu N3 65.03(8) . . ?
O1 Eu Eu 35.44(6) . 2_766 ?
O1 Eu Eu 34.21(6) 2_766 2_766 ?
O1S2 Eu Eu 98.12(5) . 2_766 ?
O1S1 Eu Eu 110.46(5) . 2_766 ?
N1 Eu Eu 177.64(6) . 2_766 ?
N2 Eu Eu 84.93(6) . 2_766 ?
N4 Eu Eu 111.66(5) . 2_766 ?
N3 Eu Eu 110.50(5) . 2_766 ?
Eu O1 Eu 110.36(10) . 2_766 ?
C2 N1 C6 118.2(3) . . ?
C2 N1 Eu 120.2(2) . . ?
C6 N1 Eu 120.3(2) . . ?
C12 N2 C8 117.5(3) . . ?
C12 N2 Eu 122.8(2) . . ?
C8 N2 Eu 119.2(2) . . ?
C18 N3 C14 116.7(3) . . ?
C18 N3 Eu 123.6(2) . . ?
C14 N3 Eu 113.7(2) . . ?
C7 N4 C1 108.6(3) . . ?
C7 N4 C13 108.8(2) . . ?
C1 N4 C13 109.5(2) . . ?
C7 N4 Eu 109.04(17) . . ?
C1 N4 Eu 112.16(18) . . ?
C13 N4 Eu 108.66(18) . . ?
N4 C1 C2 114.5(3) . . ?
N1 C2 C3 121.5(3) . . ?
N1 C2 C1 117.3(3) . . ?
C3 C2 C1 121.0(3) . . ?
C4 C3 C2 120.1(3) . . ?
C3 C4 C5 118.6(3) . . ?
C6 C5 C4 118.9(3) . . ?
N1 C6 C5 122.7(3) . . ?
N4 C7 C8 111.1(3) . . ?
N2 C8 C9 121.8(3) . . ?
N2 C8 C7 115.6(3) . . ?
C9 C8 C7 122.6(3) . . ?
C10 C9 C8 119.5(3) . . ?
C9 C10 C11 119.1(3) . . ?
C12 C11 C10 118.4(4) . . ?
N2 C12 C11 123.5(3) . . ?
N4 C13 C14 110.5(3) . . ?
N3 C14 C15 122.5(3) . . ?
N3 C14 C13 115.5(3) . . ?
C15 C14 C13 122.0(3) . . ?
C16 C15 C14 119.5(3) . . ?
C15 C16 C17 118.6(3) . . ?
C18 C17 C16 118.8(4) . . ?
N3 C18 C17 123.6(3) . . ?
O2S1 S1 O3S1 116.28(18) . . ?
O2S1 S1 O1S1 115.08(15) . . ?
O3S1 S1 O1S1 113.39(14) . . ?
O2S1 S1 C1S 103.54(18) . . ?
O3S1 S1 C1S 102.74(17) . . ?
O1S1 S1 C1S 103.43(14) . . ?
S1 O1S1 Eu 136.34(13) . . ?
F1S1 C1S F3S1 107.2(3) . . ?
F1S1 C1S F2S1 107.0(3) . . ?
F3S1 C1S F2S1 107.2(3) . . ?
F1S1 C1S S1 112.4(3) . . ?
F3S1 C1S S1 111.1(2) . . ?
F2S1 C1S S1 111.6(3) . . ?
O3S2 S2 O2S2 117.56(16) . . ?
O3S2 S2 O1S2 113.57(15) . . ?
O2S2 S2 O1S2 113.89(14) . . ?
O3S2 S2 C2S 103.42(17) . . ?
O2S2 S2 C2S 104.43(15) . . ?
O1S2 S2 C2S 101.41(14) . . ?
S2 O1S2 Eu 155.78(14) . . ?
F1S2 C2S F3S2 107.5(3) . . ?
F1S2 C2S F2S2 107.7(3) . . ?
F3S2 C2S F2S2 107.7(3) . . ?
F1S2 C2S S2 112.1(2) . . ?
F3S2 C2S S2 110.4(2) . . ?
F2S2 C2S S2 111.3(2) . . ?
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 2.228(2) . ?
Eu O1 2.298(2) 2_766 ?
Eu O1S2 2.381(2) . ?
Eu O1S1 2.531(2) . ?
Eu N1 2.578(3) . ?
Eu N2 2.593(3) . ?
Eu N4 2.639(2) . ?
Eu N3 2.730(3) . ?
Eu Eu 3.7153(8) 2_766 ?
O1 Eu 2.298(2) 2_766 ?
N1 C2 1.339(4) . ?
N1 C6 1.344(4) . ?
N2 C12 1.341(5) . ?
N2 C8 1.355(4) . ?
N3 C18 1.344(4) . ?
N3 C14 1.353(4) . ?
N4 C7 1.482(4) . ?
N4 C1 1.487(4) . ?
N4 C13 1.490(4) . ?
C1 C2 1.505(5) . ?
C2 C3 1.385(5) . ?
C3 C4 1.364(5) . ?
C4 C5 1.382(5) . ?
C5 C6 1.375(5) . ?
C7 C8 1.492(5) . ?
C8 C9 1.391(5) . ?
C9 C10 1.373(6) . ?
C10 C11 1.382(6) . ?
C11 C12 1.381(5) . ?
C13 C14 1.490(5) . ?
C14 C15 1.383(5) . ?
C15 C16 1.375(5) . ?
C16 C17 1.379(5) . ?
C17 C18 1.378(5) . ?
S1 O2S1 1.423(3) . ?
S1 O3S1 1.434(3) . ?
S1 O1S1 1.460(2) . ?
S1 C1S 1.820(4) . ?
F1S1 C1S 1.313(5) . ?
F2S1 C1S 1.335(5) . ?
F3S1 C1S 1.323(4) . ?
S2 O3S2 1.427(3) . ?
S2 O2S2 1.432(2) . ?
S2 O1S2 1.461(2) . ?
S2 C2S 1.826(3) . ?
F1S2 C2S 1.324(4) . ?
F2S2 C2S 1.334(4) . ?
F3S2 C2S 1.327(4) . ?
