#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:18:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180132 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/30/7103030.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_7103030
loop_
_publ_author_name
'Wada, Atsushi'
'Watanabe, Masayuki'
'Yamanoi, Yoshinori'
'Nishihara, Hiroshi'
_publ_section_title
;
 Modification of the luminescence spectra of
 chloro(tetrapyridylcyclotetramine)europium complexes by fine tuning of
 the Eu-Cl distance with outer-sphere counterions in the solid state,
 in a polymer matrix and in solution.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1671
_journal_page_last               1673
_journal_paper_doi               10.1039/b716987f
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_sum            'C34 H40 Cl Eu F6 N8 O6 S2'
_chemical_formula_weight         1022.27
_space_group_IT_number           18
_symmetry_space_group_name_Hall  'P 2bc 2'
_symmetry_space_group_name_H-M   'P 2 21 21'
_audit_creation_date             2006-07-31T20:21:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.346(2)
_cell_length_b                   11.116(3)
_cell_length_c                   21.206(5)
_cell_measurement_temperature    113(2)
_cell_volume                     1967.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15578
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.852
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.353
_refine_diff_density_min         -0.977
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.467
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0581P)²+14.5198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                4302
_reflns_number_total             4455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716987f.txt
_cod_data_source_block           11
_cod_database_code               7103030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Eu01 Eu 0.39925(5) 0 0 0.01540(13) Uani 1 d S . .
Cl1 Cl 0.7258(2) 0 0 0.0214(4) Uani 1 d S . .
S1 S 0.9481(2) -0.0166(2) 0.32447(9) 0.0311(5) Uani 1 d . . .
O2 O 1.0986(6) 0.0005(8) 0.2944(3) 0.0410(12) Uani 1 d . . .
F3 F 0.8051(8) 0.0490(5) 0.2208(3) 0.0478(15) Uani 1 d . . .
F2 F 0.8671(8) 0.1944(5) 0.2814(3) 0.0519(16) Uani 1 d . . .
C2 C 0.6829(15) -0.2844(9) -0.1337(5) 0.027(2) Uani 1 d . . .
H4 H 0.7704 -0.2783 -0.1607 0.032 Uiso 1 calc R . .
N2 N 0.4955(8) -0.1291(6) 0.0947(3) 0.0256(14) Uani 1 d . . .
N1 N 0.4951(8) -0.1881(6) -0.0647(3) 0.0214(13) Uani 1 d . . .
N5 N 0.2084(8) 0.0102(14) 0.0984(3) 0.050(2) Uani 1 d . . .
O3 O 0.9377(11) 0.0265(10) 0.3874(3) 0.071(3) Uani 1 d . . .
C7 C 0.6137(17) -0.2079(8) 0.0912(5) 0.031(2) Uani 1 d . . .
H1 H 0.6512 -0.2294 0.0515 0.038 Uiso 1 calc R . .
F1 F 0.6679(8) 0.0817(7) 0.3053(4) 0.071(2) Uani 1 d . . .
N4 N 0.2026(8) -0.1873(5) 0.0045(8) 0.053(3) Uani 1 d . . .
O1 O 0.8793(10) -0.1334(6) 0.3145(4) 0.058(2) Uani 1 d . . .
C6 C 0.2952(8) -0.3014(5) -0.0035(7) 0.0288(16) Uani 1 d . . .
H01A H 0.2209 -0.3647 -0.0153 0.035 Uiso 1 calc R . .
H01B H 0.3412 -0.3232 0.0369 0.035 Uiso 1 calc R . .
C12 C 0.3081(10) -0.0084(12) 0.1563(3) 0.0368(18) Uani 1 d . . .
H01C H 0.2371 -0.0318 0.1904 0.044 Uiso 1 calc R . .
H01D H 0.355 0.0684 0.1678 0.044 Uiso 1 calc R . .
C1 C 0.6193(15) -0.1854(8) -0.1060(4) 0.025(2) Uani 1 d . . .
H020 H 0.6636 -0.111 -0.1159 0.03 Uiso 1 calc R . .
C4 C 0.4825(11) -0.4016(7) -0.0793(4) 0.0289(17) Uani 1 d . . .
H021 H 0.4329 -0.4745 -0.0704 0.035 Uiso 1 calc R . .
C11 C 0.4409(10) -0.0995(7) 0.1527(4) 0.0274(17) Uani 1 d . . .
C5 C 0.4299(9) -0.2978(6) -0.0525(3) 0.0209(15) Uani 1 d . . .
C9 C 0.6350(13) -0.2267(9) 0.2021(5) 0.047(3) Uani 1 d . . .
H026 H 0.6835 -0.2573 0.2382 0.057 Uiso 1 calc R . .
C10 C 0.5094(13) -0.1452(8) 0.2069(4) 0.040(2) Uani 1 d . . .
H028 H 0.4718 -0.1216 0.2463 0.048 Uiso 1 calc R . .
C33 C 0.8159(11) 0.0814(8) 0.2809(4) 0.0335(19) Uani 1 d . . .
C8 C 0.6859(17) -0.2610(10) 0.1442(6) 0.040(3) Uani 1 d . . .
H034 H 0.7664 -0.3181 0.1396 0.048 Uiso 1 calc R . .
C3 C 0.6131(11) -0.3959(7) -0.1207(4) 0.0298(17) Uani 1 d . . .
H5 H 0.653 -0.4656 -0.1393 0.036 Uiso 1 calc R . .
C27 C 0.1285(19) 0.145(2) 0.0943(7) 0.098(7) Uani 1 d . . .
H8A H 0.0414 0.1495 0.1246 0.117 Uiso 1 calc R . .
H8B H 0.2088 0.2034 0.1075 0.117 Uiso 1 calc R . .
C25 C 0.131(2) -0.1790(14) 0.0813(11) 0.106(9) Uani 1 d . . .
H7A H 0.0478 -0.2387 0.0865 0.128 Uiso 1 calc R . .
H7B H 0.218 -0.1998 0.1098 0.128 Uiso 1 calc R . .
C26 C 0.0715(13) -0.0688(11) 0.0987(5) 0.047(3) Uani 1 d . . .
H9A H 0.0239 -0.0726 0.1404 0.056 Uiso 1 calc R . .
H9B H -0.0089 -0.0416 0.0689 0.056 Uiso 1 calc R . .
C32 C 0.0713(13) -0.1802(9) -0.0378(6) 0.053(3) Uani 1 d . . .
H10A H 0.0195 -0.258 -0.0413 0.063 Uiso 1 calc R . .
H10B H -0.0067 -0.1224 -0.0225 0.063 Uiso 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 0 '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 0.006 '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'
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
N2 Eu01 N2 143.9(3) . 3 ?
N2 Eu01 N1 82.5(2) . . ?
N2 Eu01 N1 86.7(2) 3 . ?
N2 Eu01 N1 86.7(2) . 3 ?
N2 Eu01 N1 82.5(2) 3 3 ?
N1 Eu01 N1 144.5(3) . 3 ?
N2 Eu01 N5 141.1(4) . 3 ?
N2 Eu01 N5 66.2(3) 3 3 ?
N1 Eu01 N5 74.6(3) . 3 ?
N1 Eu01 N5 129.4(4) 3 3 ?
N2 Eu01 N5 66.2(3) . . ?
N2 Eu01 N5 141.1(4) 3 . ?
N1 Eu01 N5 129.4(4) . . ?
N1 Eu01 N5 74.6(3) 3 . ?
N5 Eu01 N5 105.4(3) 3 . ?
N2 Eu01 N4 74.3(3) . . ?
N2 Eu01 N4 130.8(4) 3 . ?
N1 Eu01 N4 65.3(3) . . ?
N1 Eu01 N4 142.6(4) 3 . ?
N5 Eu01 N4 67.7(4) 3 . ?
N5 Eu01 N4 68.3(5) . . ?
N2 Eu01 N4 130.8(4) . 3 ?
N2 Eu01 N4 74.3(3) 3 3 ?
N1 Eu01 N4 142.6(4) . 3 ?
N1 Eu01 N4 65.3(3) 3 3 ?
N5 Eu01 N4 68.3(5) 3 3 ?
N5 Eu01 N4 67.7(4) . 3 ?
N4 Eu01 N4 103.6(3) . 3 ?
N2 Eu01 Cl1 71.97(15) . . ?
N2 Eu01 Cl1 71.97(15) 3 . ?
N1 Eu01 Cl1 72.26(14) . . ?
N1 Eu01 Cl1 72.26(14) 3 . ?
N5 Eu01 Cl1 127.31(16) 3 . ?
N5 Eu01 Cl1 127.31(16) . . ?
N4 Eu01 Cl1 128.22(14) . . ?
N4 Eu01 Cl1 128.22(14) 3 . ?
O2 S1 O3 115.5(5) . . ?
O2 S1 O1 114.1(5) . . ?
O3 S1 O1 114.8(6) . . ?
O2 S1 C33 103.3(4) . . ?
O3 S1 C33 103.9(5) . . ?
O1 S1 C33 103.1(5) . . ?
C1 C2 C3 118.1(10) . . ?
C7 N2 C11 117.7(8) . . ?
C7 N2 Eu01 123.7(6) . . ?
C11 N2 Eu01 117.7(5) . . ?
C1 N1 C5 116.7(7) . . ?
C1 N1 Eu01 123.5(5) . . ?
C5 N1 Eu01 119.5(5) . . ?
C26 N5 C12 110.6(9) . . ?
C26 N5 C27 103.6(10) . . ?
C12 N5 C27 113.2(10) . . ?
C26 N5 Eu01 117.3(7) . . ?
C12 N5 Eu01 108.0(5) . . ?
C27 N5 Eu01 104.1(7) . . ?
N2 C7 C8 123.6(11) . . ?
C32 N4 C6 111.9(10) . . ?
C32 N4 C25 109.0(10) . . ?
C6 N4 C25 109.2(10) . . ?
C32 N4 Eu01 114.3(7) . . ?
C6 N4 Eu01 110.0(4) . . ?
C25 N4 Eu01 101.8(7) . . ?
N4 C6 C5 115.8(8) . . ?
N5 C12 C11 117.4(8) . . ?
C2 C1 N1 124.1(9) . . ?
C5 C4 C3 118.4(8) . . ?
N2 C11 C10 121.8(8) . . ?
N2 C11 C12 117.3(7) . . ?
C10 C11 C12 120.7(8) . . ?
C4 C5 N1 123.5(7) . . ?
C4 C5 C6 119.9(7) . . ?
N1 C5 C6 116.6(6) . . ?
C8 C9 C10 119.1(9) . . ?
C11 C10 C9 119.5(9) . . ?
F2 C33 F3 106.6(7) . . ?
F2 C33 F1 106.9(8) . . ?
F3 C33 F1 108.0(8) . . ?
F2 C33 S1 111.7(7) . . ?
F3 C33 S1 111.7(6) . . ?
F1 C33 S1 111.6(6) . . ?
C9 C8 C7 118.2(12) . . ?
C2 C3 C4 119.2(8) . . ?
C32 C27 N5 116.8(9) 3 . ?
C26 C25 N4 115.1(10) . . ?
C25 C26 N5 104.7(11) . . ?
C27 C32 N4 107.8(12) 3 . ?
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
Eu01 N2 2.596(6) . ?
Eu01 N2 2.596(6) 3 ?
Eu01 N1 2.626(6) . ?
Eu01 N1 2.626(6) 3 ?
Eu01 N5 2.627(6) 3 ?
Eu01 N5 2.627(6) . ?
Eu01 N4 2.652(6) . ?
Eu01 N4 2.652(6) 3 ?
Eu01 Cl1 2.725(2) . ?
S1 O2 1.422(6) . ?
S1 O3 1.422(8) . ?
S1 O1 1.436(7) . ?
S1 C33 1.804(9) . ?
F3 C33 1.329(11) . ?
F2 C33 1.327(11) . ?
C2 C1 1.355(13) . ?
C2 C3 1.397(13) . ?
N2 C7 1.321(14) . ?
N2 C11 1.353(11) . ?
N1 C1 1.357(12) . ?
N1 C5 1.360(10) . ?
N5 C26 1.442(15) . ?
N5 C12 1.498(10) . ?
N5 C27 1.65(2) . ?
C7 C8 1.405(15) . ?
F1 C33 1.339(11) . ?
N4 C32 1.418(14) . ?
N4 C6 1.496(9) . ?
N4 C25 1.74(3) . ?
C6 C5 1.531(12) . ?
C12 C11 1.503(14) . ?
C4 C5 1.359(10) . ?
C4 C3 1.401(12) . ?
C11 C10 1.380(11) . ?
C9 C8 1.354(17) . ?
C9 C10 1.389(16) . ?
C27 C32 1.35(2) 3 ?
C25 C26 1.37(2) . ?
C32 C27 1.35(2) 3 ?
