#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:26:17 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179060 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/22/4302244.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_4302244
loop_
_publ_author_name
'Fabrice Pointillart'
'Yann Le Gal'
'Stéphane Golhen'
'Olivier Cador'
'Lahcène Ouahab'
_publ_contact_author_address
;Organométalliques et Matériaux Moléculaires
UMR 6226 CNRS-UR1 Sciences Chimiques de Rennes
Université de Rennes 1
35042 Rennes cedex
FRANCE
;
_publ_contact_author_email       lahcene.ouahab@univ-rennes1.fr
_publ_contact_author_fax         '+33 2 23 23 68 40'
_publ_contact_author_name        'Lahcène Ouahab'
_publ_contact_author_phone       '+33 2 23 23 56 59'
_publ_section_title
;
4f Gadolinium(III) Complex Involving
Tetrathiafulvalene-amido-2-pyrimidine-1-oxide as a Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4631
_journal_page_last               4633
_journal_paper_doi               10.1021/ic9003966
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'[Gd(C5 O2 F6 H)3(C11 N3 O2 S4 H7)3] (CH2Cl2) 0.5(C6H14)'
_chemical_formula_sum            'C52 H33 Cl2 F18 Gd N9 O12 S12'
_chemical_formula_weight         1930.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.297(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.066(5)
_cell_length_b                   14.879(5)
_cell_length_c                   26.377(5)
_cell_measurement_reflns_used    24793
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      0.998
_cell_volume                     7519(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare al, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.1411
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48390
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         15951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.2021
_refine_ls_R_factor_gt           0.0981
_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)+(0.0848P)²+28.2440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2505
_reflns_number_gt                7673
_reflns_number_total             15951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9003966_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302244
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2948(7) 0.1204(10) -0.0173(6) 0.097(4) Uani 1 1 d . . .
H1 H 0.2864 0.1685 -0.0408 0.116 Uiso 1 1 calc R . .
C2 C 0.2612(8) 0.1115(11) 0.0173(6) 0.102(5) Uani 1 1 d . . .
H2 H 0.2275 0.1532 0.0192 0.123 Uiso 1 1 calc R . .
C3 C 0.3511(6) -0.0171(9) 0.0385(5) 0.073(3) Uani 1 1 d . . .
C4 C 0.3972(7) -0.0789(9) 0.0649(4) 0.074(3) Uani 1 1 d . . .
C5 C 0.4828(6) -0.1595(8) 0.1416(5) 0.071(3) Uani 1 1 d . . .
H5 H 0.5062 -0.1801 0.1755 0.085 Uiso 1 1 calc R . .
C6 C 0.5150(6) -0.1546(7) 0.1045(4) 0.063(3) Uani 1 1 d . . .
C7 C 0.5866(7) -0.1889(7) 0.1098(6) 0.071(3) Uani 1 1 d . . .
C8 C 0.6958(7) -0.2190(8) 0.1771(5) 0.068(3) Uani 1 1 d . . .
C9 C 0.7824(9) -0.3138(9) 0.1737(7) 0.094(4) Uani 1 1 d . . .
H9 H 0.7995 -0.3573 0.1555 0.112 Uiso 1 1 calc R . .
C10 C 0.8240(7) -0.2857(9) 0.2215(7) 0.088(4) Uani 1 1 d . . .
H10 H 0.8680 -0.3104 0.2364 0.105 Uiso 1 1 calc R . .
C11 C 0.7995(6) -0.2209(8) 0.2467(6) 0.078(4) Uani 1 1 d . . .
H11 H 0.8271 -0.1993 0.2792 0.093 Uiso 1 1 calc R . .
C12 C 0.9089(9) -0.5451(10) 0.2450(8) 0.113(5) Uani 1 1 d . . .
H12 H 0.9525 -0.5600 0.2419 0.135 Uiso 1 1 calc R . .
C13 C 0.8523(10) -0.5584(11) 0.2056(9) 0.128(6) Uani 1 1 d . . .
H13 H 0.8545 -0.5778 0.1726 0.153 Uiso 1 1 calc R . .
C14 C 0.8110(6) -0.4849(8) 0.2776(6) 0.080(4) Uani 1 1 d . . .
C15 C 0.7749(6) -0.4294(8) 0.3029(5) 0.077(4) Uani 1 1 d . . .
C16 C 0.6880(6) -0.3100(8) 0.3102(5) 0.073(3) Uani 1 1 d . . .
H16 H 0.6496 -0.2719 0.3028 0.087 Uiso 1 1 calc R . .
C17 C 0.7477(6) -0.2900(8) 0.3494(5) 0.069(3) Uani 1 1 d . . .
C18 C 0.7613(6) -0.2147(9) 0.3855(6) 0.074(3) Uani 1 1 d . . .
C19 C 0.7213(6) -0.0590(9) 0.3922(5) 0.072(3) Uani 1 1 d . . .
C20 C 0.7338(8) 0.0289(12) 0.4649(6) 0.096(4) Uani 1 1 d . . .
H20 H 0.7497 0.0357 0.5016 0.116 Uiso 1 1 calc R . .
C21 C 0.7059(7) 0.0993(10) 0.4362(5) 0.081(4) Uani 1 1 d . . .
H21 H 0.7004 0.1531 0.4525 0.098 Uiso 1 1 calc R . .
C22 C 0.6856(6) 0.0923(9) 0.3834(5) 0.075(3) Uani 1 1 d . . .
H22 H 0.6665 0.1418 0.3627 0.091 Uiso 1 1 calc R . .
C23 C 0.6361(7) 0.0637(10) 0.5777(5) 0.092(4) Uani 1 1 d . . .
H23 H 0.6568 0.0993 0.6071 0.110 Uiso 1 1 calc R . .
C24 C 0.6453(7) -0.0239(11) 0.5799(5) 0.096(5) Uani 1 1 d . . .
H24 H 0.6719 -0.0520 0.6107 0.115 Uiso 1 1 calc R . .
C25 C 0.5744(6) 0.0116(7) 0.4834(4) 0.065(3) Uani 1 1 d . . .
C26 C 0.5462(6) 0.0053(7) 0.4317(4) 0.059(3) Uani 1 1 d . . .
C27 C 0.5305(6) -0.0473(7) 0.3359(4) 0.061(3) Uani 1 1 d . . .
H27 H 0.5330 -0.0805 0.3067 0.073 Uiso 1 1 calc R . .
C28 C 0.5173(5) 0.0430(7) 0.3322(4) 0.056(2) Uani 1 1 d . . .
C29 C 0.5006(5) 0.0960(7) 0.2832(4) 0.055(3) Uani 1 1 d . . .
C30 C 0.5161(5) 0.0870(7) 0.1947(4) 0.050(2) Uani 1 1 d . . .
C31 C 0.4537(6) 0.1573(7) 0.1179(4) 0.062(3) Uani 1 1 d . . .
H31 H 0.4146 0.1904 0.0996 0.074 Uiso 1 1 calc R . .
C32 C 0.4991(6) 0.1338(8) 0.0920(4) 0.065(3) Uani 1 1 d . . .
H32 H 0.4931 0.1526 0.0573 0.078 Uiso 1 1 calc R . .
C33 C 0.5550(6) 0.0811(8) 0.1183(4) 0.062(3) Uani 1 1 d . . .
H33 H 0.5873 0.0625 0.1014 0.074 Uiso 1 1 calc R . .
C34 C 0.7311(9) 0.1940(11) 0.0898(6) 0.093(4) Uani 1 1 d . . .
C35 C 0.7501(7) 0.1165(8) 0.1274(5) 0.071(3) Uani 1 1 d . . .
C36 C 0.8026(7) 0.0584(8) 0.1226(5) 0.075(3) Uani 1 1 d . . .
H36 H 0.8272 0.0714 0.0987 0.090 Uiso 1 1 calc R . .
C37 C 0.8182(6) -0.0194(8) 0.1539(5) 0.075(3) Uani 1 1 d . . .
C38 C 0.8748(10) -0.0805(11) 0.1480(8) 0.107(5) Uani 1 1 d . . .
C39 C 0.9468(10) 0.1862(14) 0.2535(13) 0.107(6) Uani 1 1 d . . .
C40 C 0.9015(7) 0.1135(8) 0.2695(6) 0.079(4) Uani 1 1 d . . .
C41 C 0.9325(6) 0.0559(9) 0.3095(6) 0.093(5) Uani 1 1 d . . .
H41 H 0.9799 0.0626 0.3268 0.111 Uiso 1 1 calc R . .
C42 C 0.8973(6) -0.0111(10) 0.3254(6) 0.097(5) Uani 1 1 d . . .
C43 C 0.9436(18) -0.090(4) 0.3554(18) 0.35(4) Uani 1 1 d . . .
C44 C 0.8345(11) 0.273(3) 0.3797(7) 0.201(16) Uani 1 1 d . . .
C45 C 0.7782(7) 0.2199(10) 0.3314(5) 0.079(4) Uani 1 1 d . . .
C46 C 0.7279(6) 0.2792(8) 0.3012(5) 0.072(3) Uani 1 1 d . . .
H46 H 0.7304 0.3400 0.3099 0.086 Uiso 1 1 calc R . .
C47 C 0.6754(6) 0.2491(8) 0.2592(4) 0.059(3) Uani 1 1 d . . .
C48 C 0.6193(6) 0.3128(7) 0.2313(5) 0.069(3) Uani 1 1 d . . .
C49 C 0.135(4) 0.132(3) 0.4623(14) 0.70(8) Uani 1 1 d . . .
H490 H 0.1758 0.1710 0.4712 0.838 Uiso 1 1 calc R . .
H491 H 0.1362 0.0968 0.4935 0.838 Uiso 1 1 calc R . .
C50 C 0.960(3) 0.172(5) 0.052(2) 0.45(4) Uani 1 1 d . . .
H500 H 0.9775 0.2278 0.0432 0.678 Uiso 1 1 calc R . .
H501 H 0.9801 0.1603 0.0894 0.678 Uiso 1 1 calc R . .
H502 H 0.9098 0.1765 0.0446 0.678 Uiso 1 1 calc R . .
C51 C 0.976(5) 0.103(4) 0.023(3) 0.50(7) Uani 1 1 d . . .
H510 H 0.9277 0.0901 0.0030 0.599 Uiso 1 1 calc R . .
H511 H 0.9914 0.1421 -0.0007 0.599 Uiso 1 1 calc R . .
C52 C 0.999(4) 0.036(2) 0.011(3) 0.38(5) Uani 1 1 d . . .
H520 H 1.0232 0.0164 0.0467 0.461 Uiso 1 1 calc R . .
H521 H 1.0359 0.0648 -0.0005 0.461 Uiso 1 1 calc R . .
N1 N 0.6306(5) -0.1830(6) 0.1596(4) 0.066(2) Uani 1 1 d . . .
H1N H 0.6160 -0.1539 0.1824 0.079 Uiso 1 1 calc R . .
N2 N 0.7193(6) -0.2829(7) 0.1520(5) 0.087(3) Uani 1 1 d . . .
N3 N 0.7354(5) -0.1875(6) 0.2250(4) 0.062(2) Uani 1 1 d . . .
N4 N 0.7245(5) -0.1362(7) 0.3646(4) 0.068(2) Uani 1 1 d . . .
H4N H 0.7019 -0.1365 0.3313 0.081 Uiso 1 1 calc R . .
N5 N 0.7410(6) -0.0541(8) 0.4441(4) 0.091(3) Uani 1 1 d . . .
N6 N 0.6925(4) 0.0137(7) 0.3598(4) 0.062(2) Uani 1 1 d . . .
N7 N 0.5288(4) 0.0598(5) 0.2455(3) 0.055(2) Uani 1 1 d . . .
H7N H 0.5571 0.0155 0.2556 0.066 Uiso 1 1 calc R . .
N8 N 0.4609(4) 0.1361(6) 0.1690(3) 0.059(2) Uani 1 1 d . . .
N9 N 0.5624(4) 0.0564(5) 0.1693(3) 0.051(2) Uani 1 1 d . . .
O1 O 0.6000(5) -0.2175(6) 0.0704(3) 0.090(3) Uani 1 1 d . . .
O2 O 0.7071(3) -0.1242(5) 0.2483(3) 0.0588(18) Uani 1 1 d . . .
O3 O 0.8010(5) -0.2193(6) 0.4301(4) 0.102(3) Uani 1 1 d . . .
O4 O 0.6722(3) 0.0025(5) 0.3078(3) 0.0620(18) Uani 1 1 d . . .
O5 O 0.4662(4) 0.1648(5) 0.2774(3) 0.0656(19) Uani 1 1 d . . .
O6 O 0.6136(3) 0.0034(5) 0.1962(3) 0.0594(18) Uani 1 1 d . . .
O7 O 0.7144(4) 0.1107(6) 0.1583(3) 0.075(2) Uani 1 1 d . . .
O8 O 0.7918(4) -0.0438(5) 0.1891(3) 0.074(2) Uani 1 1 d . . .
O9 O 0.8384(4) 0.1199(5) 0.2442(3) 0.074(2) Uani 1 1 d . . .
O10 O 0.8332(4) -0.0302(5) 0.3081(3) 0.083(2) Uani 1 1 d . . .
O11 O 0.7835(4) 0.1382(7) 0.3246(3) 0.083(2) Uani 1 1 d . . .
O12 O 0.6665(4) 0.1715(5) 0.2409(3) 0.067(2) Uani 1 1 d . . .
F1 F 0.7520(6) 0.2690(6) 0.1145(4) 0.152(4) Uani 1 1 d . . .
F2 F 0.7553(7) 0.1894(8) 0.0492(5) 0.169(5) Uani 1 1 d . . .
F3 F 0.6623(6) 0.2009(7) 0.0681(4) 0.146(4) Uani 1 1 d . . .
F4 F 0.9088(7) -0.0530(8) 0.1172(7) 0.222(8) Uani 1 1 d . . .
F5 F 0.8479(6) -0.1588(7) 0.1278(5) 0.155(4) Uani 1 1 d . . .
F6 F 0.9191(5) -0.1055(9) 0.1923(5) 0.163(5) Uani 1 1 d . . .
F7 F 0.979(2) 0.144(2) 0.219(2) 0.23(2) Uani 0.64(5) 1 d P . .
F7A F 0.934(3) 0.200(5) 0.2106(18) 0.13(2) Uani 0.36(5) 1 d P . .
F8 F 0.993(3) 0.207(6) 0.281(3) 0.38(5) Uani 0.64(5) 1 d P . .
F8A F 1.0178(18) 0.181(3) 0.287(2) 0.134(18) Uani 0.36(5) 1 d P . .
F9 F 0.9154(17) 0.245(2) 0.223(3) 0.22(3) Uani 0.64(5) 1 d P . .
F9A F 0.941(3) 0.262(2) 0.286(2) 0.14(2) Uani 0.36(5) 1 d P . .
F10 F 0.9262(18) -0.060(2) 0.4067(10) 0.344(17) Uani 1 1 d . . .
F11 F 1.0031(6) -0.0707(13) 0.3810(10) 0.297(13) Uani 1 1 d . . .
F12 F 0.9157(9) -0.1515(11) 0.3666(11) 0.270(12) Uani 1 1 d . . .
F13 F 0.8456(13) 0.2072(13) 0.4184(6) 0.281(14) Uani 1 1 d . . .
F14 F 0.8904(8) 0.2630(18) 0.3759(7) 0.276(11) Uani 1 1 d . . .
F15 F 0.8175(12) 0.328(2) 0.3989(12) 0.41(2) Uani 1 1 d . . .
F16 F 0.6293(5) 0.3969(5) 0.2462(4) 0.131(3) Uani 1 1 d . . .
F17 F 0.5597(4) 0.2916(5) 0.2403(4) 0.115(3) Uani 1 1 d . . .
F18 F 0.6059(6) 0.3106(7) 0.1810(4) 0.146(4) Uani 1 1 d . . .
S1 S 0.3571(2) 0.0379(3) -0.01824(13) 0.0936(11) Uani 1 1 d . . .
S2 S 0.2807(2) 0.0194(3) 0.06025(16) 0.0998(12) Uani 1 1 d . . .
S3 S 0.39624(19) -0.1266(3) 0.12529(14) 0.0920(11) Uani 1 1 d . . .
S4 S 0.4650(2) -0.1171(3) 0.04172(13) 0.0905(11) Uani 1 1 d . . .
S5 S 0.90116(19) -0.4992(3) 0.3033(2) 0.1074(13) Uani 1 1 d . . .
S6 S 0.7732(2) -0.5384(3) 0.21727(17) 0.0969(11) Uani 1 1 d . . .
S7 S 0.68524(17) -0.4072(2) 0.27462(16) 0.0848(10) Uani 1 1 d . . .
S8 S 0.81530(17) -0.3704(2) 0.36069(15) 0.0857(10) Uani 1 1 d . . .
S9 S 0.58573(19) 0.1112(2) 0.51994(12) 0.0774(9) Uani 1 1 d . . .
S10 S 0.60552(19) -0.0847(2) 0.52270(13) 0.0827(10) Uani 1 1 d . . .
S11 S 0.54244(18) -0.0968(2) 0.39690(12) 0.0742(9) Uani 1 1 d . . .
S12 S 0.51161(17) 0.09726(19) 0.38977(11) 0.0662(8) Uani 1 1 d . . .
Gd1 Gd 0.73580(3) 0.03920(4) 0.24503(2) 0.05724(19) Uani 1 1 d . . .
Cl1 Cl 0.1362(6) 0.0700(10) 0.4163(4) 0.315(7) Uani 1 1 d . . .
Cl2 Cl 0.0612(11) 0.1947(18) 0.4435(7) 0.563(17) 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'
Gd Gd -0.1653 3.9035 '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'
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
C2 C1 S1 117.5(13) . . ?
C1 C2 S2 118.4(13) . . ?
C4 C3 S1 123.7(9) . . ?
C4 C3 S2 122.5(10) . . ?
S1 C3 S2 113.8(8) . . ?
C3 C4 S4 122.0(9) . . ?
C3 C4 S3 124.0(9) . . ?
S4 C4 S3 114.0(8) . . ?
C6 C5 S3 118.3(9) . . ?
C5 C6 C7 125.3(11) . . ?
C5 C6 S4 116.6(10) . . ?
C7 C6 S4 117.6(9) . . ?
O1 C7 N1 127.1(12) . . ?
O1 C7 C6 119.2(12) . . ?
N1 C7 C6 113.7(11) . . ?
N2 C8 N3 121.0(12) . . ?
N2 C8 N1 124.2(13) . . ?
N3 C8 N1 114.7(10) . . ?
N2 C9 C10 123.1(13) . . ?
C11 C10 C9 117.9(12) . . ?
N3 C11 C10 120.1(14) . . ?
C13 C12 S5 118.7(14) . . ?
C12 C13 S6 117.3(17) . . ?
C15 C14 S6 124.2(10) . . ?
C15 C14 S5 120.8(11) . . ?
S6 C14 S5 114.9(8) . . ?
C14 C15 S8 123.2(10) . . ?
C14 C15 S7 121.3(10) . . ?
S8 C15 S7 115.3(8) . . ?
C17 C16 S7 118.5(10) . . ?
C16 C17 C18 128.5(11) . . ?
C16 C17 S8 115.9(10) . . ?
C18 C17 S8 115.5(9) . . ?
O3 C18 N4 123.1(13) . . ?
O3 C18 C17 122.5(12) . . ?
N4 C18 C17 114.3(11) . . ?
N5 C19 N4 123.8(13) . . ?
N5 C19 N6 122.6(12) . . ?
N4 C19 N6 113.6(10) . . ?
C21 C20 N5 124.2(13) . . ?
C20 C21 C22 119.0(14) . . ?
C21 C22 N6 120.5(13) . . ?
C24 C23 S9 119.1(11) . . ?
C23 C24 S10 117.2(11) . . ?
C26 C25 S9 125.3(9) . . ?
C26 C25 S10 121.2(9) . . ?
S9 C25 S10 113.5(6) . . ?
C25 C26 S12 124.2(8) . . ?
C25 C26 S11 122.6(9) . . ?
S12 C26 S11 113.1(6) . . ?
C28 C27 S11 117.3(8) . . ?
C27 C28 C29 125.6(10) . . ?
C27 C28 S12 116.8(8) . . ?
C29 C28 S12 117.4(8) . . ?
O5 C29 N7 124.7(10) . . ?
O5 C29 C28 122.4(10) . . ?
N7 C29 C28 112.8(10) . . ?
N8 C30 N7 123.5(9) . . ?
N8 C30 N9 120.9(9) . . ?
N7 C30 N9 115.5(8) . . ?
C32 C31 N8 124.2(10) . . ?
C31 C32 C33 117.9(10) . . ?
N9 C33 C32 119.1(10) . . ?
F1 C34 F2 108.4(14) . . ?
F1 C34 F3 106.8(14) . . ?
F2 C34 F3 104.0(14) . . ?
F1 C34 C35 110.5(13) . . ?
F2 C34 C35 115.0(13) . . ?
F3 C34 C35 111.8(13) . . ?
O7 C35 C36 127.9(11) . . ?
O7 C35 C34 114.2(12) . . ?
C36 C35 C34 117.8(12) . . ?
C35 C36 C37 120.0(11) . . ?
O8 C37 C36 127.4(11) . . ?
O8 C37 C38 113.8(12) . . ?
C36 C37 C38 118.8(11) . . ?
F4 C38 F6 108.3(17) . . ?
F4 C38 F5 104.9(16) . . ?
F6 C38 F5 101.3(13) . . ?
F4 C38 C37 116.1(13) . . ?
F6 C38 C37 114.7(15) . . ?
F5 C38 C37 110.1(15) . . ?
F8 C39 F7A 124(5) . . ?
F8 C39 F9 115(5) . . ?
F7A C39 F9 44(3) . . ?
F8 C39 F7 95(5) . . ?
F7A C39 F7 56(4) . . ?
F9 C39 F7 98(4) . . ?
F8 C39 F8A 22(7) . . ?
F7A C39 F8A 122(4) . . ?
F9 C39 F8A 132(3) . . ?
F7 C39 F8A 79(3) . . ?
F8 C39 F9A 65(5) . . ?
F7A C39 F9A 115(4) . . ?
F9 C39 F9A 73(3) . . ?
F7 C39 F9A 150(2) . . ?
F8A C39 F9A 86(4) . . ?
F8 C39 C40 119(4) . . ?
F7A C39 C40 116(3) . . ?
F9 C39 C40 117(2) . . ?
F7 C39 C40 107(2) . . ?
F8A C39 C40 110(2) . . ?
F9A C39 C40 103(2) . . ?
O9 C40 C41 128.4(11) . . ?
O9 C40 C39 112.6(14) . . ?
C41 C40 C39 118.8(14) . . ?
C40 C41 C42 122.9(11) . . ?
O10 C42 C41 128.3(12) . . ?
O10 C42 C43 113.9(14) . . ?
C41 C42 C43 114.9(16) . . ?
F12 C43 F11 121(2) . . ?
F12 C43 C42 118(3) . . ?
F11 C43 C42 116(3) . . ?
F12 C43 F10 76(4) . . ?
F11 C43 F10 84(4) . . ?
C42 C43 F10 88(4) . . ?
F15 C44 F14 126(5) . . ?
F15 C44 F13 101(3) . . ?
F14 C44 F13 92(3) . . ?
F15 C44 C45 120(2) . . ?
F14 C44 C45 109.5(19) . . ?
F13 C44 C45 99(3) . . ?
O11 C45 C46 128.0(12) . . ?
O11 C45 C44 121.1(19) . . ?
C46 C45 C44 110.9(18) . . ?
C47 C46 C45 120.7(11) . . ?
O12 C47 C46 127.6(11) . . ?
O12 C47 C48 113.5(10) . . ?
C46 C47 C48 118.9(11) . . ?
F18 C48 F16 107.6(11) . . ?
F18 C48 F17 105.0(12) . . ?
F16 C48 F17 104.0(10) . . ?
F18 C48 C47 113.2(10) . . ?
F16 C48 C47 115.8(11) . . ?
F17 C48 C47 110.5(10) . . ?
Cl1 C49 Cl2 108(2) . . ?
C52 C51 C50 163(9) . . ?
C51 C52 C52 159(10) . 3_755 ?
C7 N1 C8 126.0(11) . . ?
C9 N2 C8 118.5(13) . . ?
C11 N3 O2 123.4(11) . . ?
C11 N3 C8 119.4(11) . . ?
O2 N3 C8 117.2(9) . . ?
C19 N4 C18 126.1(10) . . ?
C19 N5 C20 115.6(12) . . ?
O4 N6 C22 123.1(10) . . ?
O4 N6 C19 118.8(9) . . ?
C22 N6 C19 118.0(10) . . ?
C30 N7 C29 126.7(9) . . ?
C30 N8 C31 117.5(9) . . ?
O6 N9 C33 122.1(8) . . ?
O6 N9 C30 117.8(8) . . ?
C33 N9 C30 120.1(9) . . ?
N3 O2 Gd1 122.3(5) . . ?
N6 O4 Gd1 128.0(6) . . ?
N9 O6 Gd1 130.2(6) . . ?
C35 O7 Gd1 132.3(7) . . ?
C37 O8 Gd1 132.4(8) . . ?
C40 O9 Gd1 134.2(8) . . ?
C42 O10 Gd1 133.5(8) . . ?
C45 O11 Gd1 132.0(8) . . ?
C47 O12 Gd1 136.9(7) . . ?
F7A F7 C39 49(2) . . ?
F9 F7A C39 76(5) . . ?
F9 F7A F7 147(9) . . ?
C39 F7A F7 75(5) . . ?
F8A F8 C39 118(10) . . ?
F8A F8 F9A 162(10) . . ?
C39 F8 F9A 72(4) . . ?
F8 F8A C39 40(10) . . ?
F7A F9 C39 60(4) . . ?
F7A F9 F9A 118(7) . . ?
C39 F9 F9A 60(3) . . ?
F8 F9A C39 44(3) . . ?
F8 F9A F9 81(4) . . ?
C39 F9A F9 47(2) . . ?
C43 F10 F12 41.4(14) . . ?
C43 F12 F10 63(4) . . ?
C3 S1 C1 94.8(7) . . ?
C2 S2 C3 94.4(7) . . ?
C5 S3 C4 93.4(6) . . ?
C4 S4 C6 93.4(6) . . ?
C12 S5 C14 93.4(8) . . ?
C13 S6 C14 93.9(9) . . ?
C16 S7 C15 93.7(6) . . ?
C15 S8 C17 93.5(6) . . ?
C23 S9 C25 95.0(6) . . ?
C24 S10 C25 94.4(7) . . ?
C27 S11 C26 95.2(5) . . ?
C28 S12 C26 94.1(5) . . ?
O9 Gd1 O10 72.2(3) . . ?
O9 Gd1 O12 94.4(3) . . ?
O10 Gd1 O12 136.9(3) . . ?
O9 Gd1 O4 138.3(3) . . ?
O10 Gd1 O4 85.2(3) . . ?
O12 Gd1 O4 78.5(3) . . ?
O9 Gd1 O8 72.3(3) . . ?
O10 Gd1 O8 76.9(3) . . ?
O12 Gd1 O8 139.0(3) . . ?
O4 Gd1 O8 136.6(3) . . ?
O9 Gd1 O7 71.6(3) . . ?
O10 Gd1 O7 136.0(3) . . ?
O12 Gd1 O7 70.2(3) . . ?
O4 Gd1 O7 138.9(2) . . ?
O8 Gd1 O7 68.8(3) . . ?
O9 Gd1 O6 146.1(3) . . ?
O10 Gd1 O6 138.6(3) . . ?
O12 Gd1 O6 71.3(2) . . ?
O4 Gd1 O6 70.5(2) . . ?
O8 Gd1 O6 98.0(2) . . ?
O7 Gd1 O6 74.6(3) . . ?
O9 Gd1 O2 134.1(2) . . ?
O10 Gd1 O2 72.9(2) . . ?
O12 Gd1 O2 131.5(2) . . ?
O4 Gd1 O2 65.6(2) . . ?
O8 Gd1 O2 71.4(2) . . ?
O7 Gd1 O2 118.5(3) . . ?
O6 Gd1 O2 66.8(2) . . ?
O9 Gd1 O11 66.2(3) . . ?
O10 Gd1 O11 69.0(3) . . ?
O12 Gd1 O11 68.1(3) . . ?
O4 Gd1 O11 73.1(3) . . ?
O8 Gd1 O11 132.3(3) . . ?
O7 Gd1 O11 116.4(3) . . ?
O6 Gd1 O11 129.6(2) . . ?
O2 Gd1 O11 125.1(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
C1 C2 1.292(18) . ?
C1 S1 1.758(14) . ?
C2 S2 1.748(17) . ?
C3 C4 1.342(17) . ?
C3 S1 1.740(13) . ?
C3 S2 1.762(12) . ?
C4 S4 1.744(12) . ?
C4 S3 1.749(12) . ?
C5 C6 1.325(15) . ?
C5 S3 1.732(12) . ?
C6 C7 1.493(16) . ?
C6 S4 1.752(12) . ?
C7 O1 1.224(14) . ?
C7 N1 1.350(15) . ?
C8 N2 1.323(14) . ?
C8 N3 1.360(15) . ?
C8 N1 1.362(14) . ?
C9 N2 1.309(17) . ?
C9 C10 1.354(19) . ?
C10 C11 1.343(17) . ?
C11 N3 1.337(13) . ?
C12 C13 1.31(2) . ?
C12 S5 1.730(18) . ?
C13 S6 1.729(18) . ?
C14 C15 1.393(18) . ?
C14 S6 1.738(15) . ?
C14 S5 1.745(12) . ?
C15 S8 1.736(14) . ?
C15 S7 1.763(13) . ?
C16 C17 1.364(16) . ?
C16 S7 1.716(13) . ?
C17 C18 1.442(17) . ?
C17 S8 1.767(11) . ?
C18 O3 1.210(14) . ?
C18 N4 1.404(15) . ?
C19 N5 1.309(14) . ?
C19 N4 1.372(15) . ?
C19 N6 1.395(15) . ?
C20 C21 1.316(19) . ?
C20 N5 1.377(18) . ?
C21 C22 1.334(16) . ?
C22 N6 1.350(15) . ?
C23 C24 1.315(19) . ?
C23 S9 1.711(14) . ?
C24 S10 1.737(15) . ?
C25 C26 1.315(14) . ?
C25 S9 1.745(11) . ?
C25 S10 1.771(11) . ?
C26 S12 1.766(11) . ?
C26 S11 1.766(11) . ?
C27 C28 1.367(14) . ?
C27 S11 1.720(10) . ?
C28 C29 1.464(14) . ?
C28 S12 1.753(10) . ?
C29 O5 1.220(12) . ?
C29 N7 1.391(12) . ?
C30 N8 1.333(12) . ?
C30 N7 1.350(12) . ?
C30 N9 1.375(12) . ?
C31 C32 1.340(15) . ?
C31 N8 1.348(13) . ?
C32 C33 1.375(15) . ?
C33 N9 1.360(12) . ?
C34 F1 1.296(17) . ?
C34 F2 1.302(16) . ?
C34 F3 1.333(17) . ?
C34 C35 1.495(17) . ?
C35 O7 1.238(13) . ?
C35 C36 1.397(16) . ?
C36 C37 1.404(16) . ?
C37 O8 1.251(13) . ?
C37 C38 1.498(18) . ?
C38 F4 1.275(16) . ?
C38 F6 1.294(19) . ?
C38 F5 1.33(2) . ?
C39 F8 1.05(5) . ?
C39 F7A 1.10(4) . ?
C39 F9 1.23(4) . ?
C39 F7 1.41(4) . ?
C39 F8A 1.44(5) . ?
C39 F9A 1.44(5) . ?
C39 C40 1.55(2) . ?
C40 O9 1.246(14) . ?
C40 C41 1.358(18) . ?
C41 C42 1.358(18) . ?
C42 O10 1.262(13) . ?
C42 C43 1.56(4) . ?
C43 F12 1.16(3) . ?
C43 F11 1.22(2) . ?
C43 F10 1.56(7) . ?
C44 F15 1.07(3) . ?
C44 F14 1.16(2) . ?
C44 F13 1.38(4) . ?
C44 C45 1.63(3) . ?
C45 O11 1.238(15) . ?
C45 C46 1.399(18) . ?
C46 C47 1.356(15) . ?
C47 O12 1.245(12) . ?
C47 C48 1.488(16) . ?
C48 F18 1.275(13) . ?
C48 F16 1.308(12) . ?
C48 F17 1.325(13) . ?
C49 Cl1 1.53(3) . ?
C49 Cl2 1.70(5) . ?
C50 C51 1.38(8) . ?
C51 C52 1.19(7) . ?
C52 C52 1.23(11) 3_755 ?
N3 O2 1.341(11) . ?
N6 O4 1.320(10) . ?
N9 O6 1.322(10) . ?
O2 Gd1 2.505(7) . ?
O4 Gd1 2.435(7) . ?
O6 Gd1 2.465(7) . ?
O7 Gd1 2.441(8) . ?
O8 Gd1 2.439(8) . ?
O9 Gd1 2.389(8) . ?
O10 Gd1 2.392(8) . ?
O11 Gd1 2.510(9) . ?
O12 Gd1 2.394(7) . ?
F7 F7A 1.20(7) . ?
F7A F9 0.88(6) . ?
F8 F8A 0.61(9) . ?
F8 F9A 1.37(8) . ?
F9 F9A 1.59(5) . ?
F10 F12 1.70(3) . ?
