#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:34:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179413 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/10/4331017.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_4331017
loop_
_publ_author_name
'Fabrice Pointillart'
'Kevin Bernot'
'Giordano Poneti'
'Roberta Sessoli'
_publ_section_title
;
 Crystal Packing Effects on the Magnetic Slow Relaxation of
 Tb(III)-Nitronyl Nitroxide Radical Cyclic Dinuclear Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12218
_journal_page_last               12229
_journal_paper_doi               10.1021/ic301394x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C64 H58 F36 N4 O22 P2 Tb2'
_chemical_formula_weight         2298.92
_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                102.9512(23)
_cell_angle_beta                 104.6762(22)
_cell_angle_gamma                105.1194(22)
_cell_formula_units_Z            2
_cell_length_a                   12.6405(8)
_cell_length_b                   18.8158(12)
_cell_length_c                   20.4054(13)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.17
_cell_volume                     4308.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66183
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.077
_refine_diff_density_min         -2.687
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         19387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0790P)²+22.7991P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                14163
_reflns_number_total             19387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301394x_si_002_3.cif
_cod_data_source_block           (2B)
_cod_database_code               4331017
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
C22 C 0.0444(9) 0.0815(6) 1.0922(5) 0.064(2) Uani 1 1 d . . .
C11 C 0.5264(5) 0.3863(3) 0.9010(3) 0.0277(12) Uani 1 1 d . . .
C18 C 0.3964(9) 0.0619(5) 1.0329(6) 0.060(2) Uani 1 1 d . . .
C3 C 0.5415(6) 0.6731(4) 0.7682(4) 0.0381(15) Uani 1 1 d . . .
C26 C 0.1830(5) 0.4240(3) 0.9997(3) 0.0278(12) Uani 1 1 d . . .
C8 C 0.5500(5) 0.5039(4) 0.8385(3) 0.0299(13) Uani 1 1 d . . .
C7 C 0.5499(5) 0.5608(4) 0.7993(3) 0.0304(13) Uani 1 1 d . . .
C27 C 0.1628(6) 0.4756(4) 0.9534(4) 0.0377(15) Uani 1 1 d . . .
C39 C 0.0942(5) 0.3767(4) 0.6637(3) 0.0313(13) Uani 1 1 d . . .
C59 C 0.5366(8) 0.9167(6) 0.7051(5) 0.064(3) Uani 1 1 d . . .
C53 C 0.2322(6) 0.5785(4) 0.4268(4) 0.0400(16) Uani 1 1 d . . .
C4 C 0.5035(6) 0.6043(4) 0.6989(4) 0.0379(15) Uani 1 1 d . . .
C48 C -0.0804(8) 0.7393(6) 0.5979(5) 0.061(2) Uani 1 1 d . . .
H48A H -0.1473 0.7013 0.5593 0.074 Uiso 1 1 calc R . .
H48B H -0.0293 0.7680 0.5773 0.074 Uiso 1 1 calc R . .
C16 C 0.6323(7) 0.2843(6) 1.0462(5) 0.059(2) Uani 1 1 d . . .
H16B H 0.6405 0.2368 1.0213 0.071 Uiso 1 1 calc R . .
H16A H 0.5654 0.2707 1.0618 0.071 Uiso 1 1 calc R . .
C28 C -0.1465(7) 0.2157(7) 0.9059(6) 0.072(3) Uani 1 1 d . . .
C51 C 0.2057(7) 0.6517(5) 0.3454(4) 0.0499(19) Uani 1 1 d . . .
C21 C 0.1417(7) 0.1164(4) 1.0627(4) 0.0480(18) Uani 1 1 d . . .
C42 C 0.0750(6) 0.5757(4) 0.7099(3) 0.0338(14) Uani 1 1 d . . .
H42 H 0.0703 0.6116 0.7477 0.041 Uiso 1 1 calc R . .
C43 C 0.0824(5) 0.5951(4) 0.6485(3) 0.0294(13) Uani 1 1 d . . .
C9 C 0.4846(5) 0.5004(4) 0.8848(3) 0.0326(13) Uani 1 1 d . . .
H9 H 0.4509 0.5380 0.8956 0.039 Uiso 1 1 calc R . .
C19 C 0.3172(7) 0.1081(4) 1.0372(5) 0.0473(18) Uani 1 1 d . . .
C45 C 0.0797(5) 0.4671(4) 0.5936(3) 0.0299(13) Uani 1 1 d . . .
H45 H 0.0778 0.4301 0.5542 0.036 Uiso 1 1 calc R . .
C32 C 0.0660(9) 0.0564(5) 0.7985(5) 0.060(2) Uani 1 1 d . . .
C36 C 0.1808(10) 0.2956(5) 0.7142(5) 0.076(3) Uani 1 1 d . . .
C54 C 0.2602(6) 0.5068(5) 0.4404(4) 0.0424(17) Uani 1 1 d . . .
C25 C 0.1305(5) 0.4266(4) 1.0528(3) 0.0303(13) Uani 1 1 d . . .
H25 H 0.0847 0.4577 1.0573 0.036 Uiso 1 1 calc R . .
C23 C 0.0960(6) 0.3911(4) 1.1596(4) 0.0372(15) Uani 1 1 d . . .
C24 C 0.1471(5) 0.3823(4) 1.0990(3) 0.0280(12) Uani 1 1 d . . .
C10 C 0.4708(5) 0.4410(4) 0.9138(3) 0.0297(13) Uani 1 1 d . . .
H10 H 0.4241 0.4369 0.9423 0.036 Uiso 1 1 calc R . .
C13 C 0.6061(6) 0.4502(4) 0.8255(4) 0.0372(15) Uani 1 1 d . . .
H13 H 0.6509 0.4534 0.7958 0.045 Uiso 1 1 calc R . .
C12 C 0.5948(6) 0.3926(4) 0.8569(4) 0.0344(14) Uani 1 1 d . . .
H12 H 0.6332 0.3573 0.8488 0.041 Uiso 1 1 calc R . .
C35 C 0.0939(6) 0.2471(4) 0.6396(4) 0.0380(15) Uani 1 1 d . . .
C40 C 0.0786(5) 0.4490(4) 0.6559(3) 0.0279(12) Uani 1 1 d . . .
C41 C 0.0748(6) 0.5037(4) 0.7145(4) 0.0351(14) Uani 1 1 d . . .
H41 H 0.0720 0.4913 0.7558 0.042 Uiso 1 1 calc R . .
C44 C 0.0835(5) 0.5402(4) 0.5906(3) 0.0295(13) Uani 1 1 d . . .
H44 H 0.0869 0.5529 0.5495 0.035 Uiso 1 1 calc R . .
C20 C 0.2226(8) 0.0777(5) 1.0592(5) 0.057(2) Uani 1 1 d . . .
H20 H 0.2137 0.0323 1.0715 0.068 Uiso 1 1 calc R . .
C29 C -0.0312(7) 0.2029(5) 0.9108(5) 0.055(2) Uani 1 1 d . . .
C31 C 0.0693(7) 0.1258(4) 0.8577(4) 0.0488(18) Uani 1 1 d . . .
C5 C 0.5611(8) 0.6177(5) 0.6443(4) 0.055(2) Uani 1 1 d . . .
H5B H 0.6437 0.6402 0.6673 0.083 Uiso 1 1 calc R . .
H5C H 0.5332 0.6522 0.6222 0.083 Uiso 1 1 calc R . .
H5A H 0.5431 0.5692 0.6088 0.083 Uiso 1 1 calc R . .
C6 C 0.3714(7) 0.5695(6) 0.6620(4) 0.060(2) Uani 1 1 d . . .
H6B H 0.3344 0.5611 0.6967 0.091 Uiso 1 1 calc R . .
H6A H 0.3525 0.5210 0.6262 0.091 Uiso 1 1 calc R . .
H6C H 0.3446 0.6046 0.6401 0.091 Uiso 1 1 calc R . .
C52 C 0.2348(7) 0.5903(5) 0.3622(4) 0.0501(19) Uani 1 1 d . . .
C1 C 0.4531(9) 0.7138(6) 0.7734(5) 0.063(2) Uani 1 1 d . . .
H1A H 0.3786 0.6761 0.7633 0.095 Uiso 1 1 calc R . .
H1C H 0.4478 0.7420 0.7395 0.095 Uiso 1 1 calc R . .
H1B H 0.4772 0.7491 0.8206 0.095 Uiso 1 1 calc R . .
C2 C 0.6611(7) 0.7325(5) 0.7835(5) 0.055(2) Uani 1 1 d . . .
H2B H 0.7160 0.7061 0.7797 0.082 Uiso 1 1 calc R . .
H2C H 0.6865 0.7680 0.8307 0.082 Uiso 1 1 calc R . .
H2A H 0.6558 0.7606 0.7495 0.082 Uiso 1 1 calc R . .
C17 C 0.7357(9) 0.3278(8) 1.1077(7) 0.097(4) Uani 1 1 d . . .
H17A H 0.7468 0.2968 1.1387 0.146 Uiso 1 1 calc R . .
H17C H 0.7269 0.3743 1.1329 0.146 Uiso 1 1 calc R . .
H17B H 0.8019 0.3409 1.0923 0.146 Uiso 1 1 calc R . .
C46 C 0.2238(10) 0.8246(5) 0.7458(5) 0.071(3) Uani 1 1 d . . .
H46A H 0.3020 0.8424 0.7441 0.086 Uiso 1 1 calc R . .
H46B H 0.1757 0.8430 0.7132 0.086 Uiso 1 1 calc R . .
C30 C -0.0342(8) 0.1366(5) 0.8590(5) 0.063(2) Uani 1 1 d . . .
H30 H -0.1046 0.1013 0.8268 0.076 Uiso 1 1 calc R . .
C14 C 0.4260(12) 0.1631(7) 0.8551(8) 0.118(6) Uani 1 1 d . . .
H14B H 0.3501 0.1616 0.8277 0.141 Uiso 1 1 calc R . .
H14A H 0.4174 0.1485 0.8966 0.141 Uiso 1 1 calc R . .
C33 C 0.1439(13) 0.2119(9) 0.5876(7) 0.114(5) Uani 1 1 d . . .
H33A H 0.0832 0.1830 0.5429 0.171 Uiso 1 1 calc R . .
H33B H 0.1798 0.1778 0.6054 0.171 Uiso 1 1 calc R . .
H33C H 0.2009 0.2520 0.5809 0.171 Uiso 1 1 calc R . .
C55 C 0.5776(14) 0.7581(14) 0.4788(14) 0.136(7) Uani 1 1 d . . .
C34 C -0.0106(9) 0.1861(7) 0.6403(8) 0.105(5) Uani 1 1 d . . .
H34C H -0.0426 0.2090 0.6740 0.157 Uiso 1 1 calc R . .
H34A H 0.0126 0.1453 0.6536 0.157 Uiso 1 1 calc R . .
H34B H -0.0681 0.1654 0.5936 0.157 Uiso 1 1 calc R . .
C47 C 0.2253(18) 0.8570(8) 0.8139(7) 0.150(8) Uani 1 1 d . . .
H47C H 0.2560 0.9124 0.8267 0.225 Uiso 1 1 calc R . .
H47A H 0.2733 0.8395 0.8467 0.225 Uiso 1 1 calc R . .
H47B H 0.1477 0.8416 0.8156 0.225 Uiso 1 1 calc R . .
C49 C -0.1175(14) 0.7915(10) 0.6429(9) 0.143(7) Uani 1 1 d . . .
H49B H -0.1578 0.8173 0.6152 0.214 Uiso 1 1 calc R . .
H49C H -0.0509 0.8292 0.6807 0.214 Uiso 1 1 calc R . .
H49A H -0.1684 0.7627 0.6628 0.214 Uiso 1 1 calc R . .
C37 C 0.1933(18) 0.2710(7) 0.7736(7) 0.157(9) Uani 1 1 d . . .
H37C H 0.2538 0.3107 0.8136 0.235 Uiso 1 1 calc R . .
H37A H 0.2132 0.2247 0.7648 0.235 Uiso 1 1 calc R . .
H37B H 0.1216 0.2605 0.7836 0.235 Uiso 1 1 calc R . .
C38 C 0.3140(10) 0.3155(8) 0.7071(8) 0.110(5) Uani 1 1 d . . .
H38C H 0.3136 0.3314 0.6655 0.165 Uiso 1 1 calc R . .
H38A H 0.3362 0.2700 0.7031 0.165 Uiso 1 1 calc R . .
H38B H 0.3685 0.3564 0.7487 0.165 Uiso 1 1 calc R . .
C15 C 0.4518(15) 0.1059(8) 0.8148(11) 0.173(10) Uani 1 1 d . . .
H15B H 0.3916 0.0571 0.8030 0.260 Uiso 1 1 calc R . .
H15C H 0.5245 0.1033 0.8413 0.260 Uiso 1 1 calc R . .
H15A H 0.4574 0.1169 0.7719 0.260 Uiso 1 1 calc R . .
C64 C 0.3429(19) 0.9565(15) 0.4203(14) 0.188(14) Uani 1 1 d . . .
C50 C 0.2026(10) 0.6605(6) 0.2714(5) 0.067(3) Uani 1 1 d . . .
N2 N 0.5358(5) 0.5440(3) 0.7281(3) 0.0372(13) Uani 1 1 d . . .
N1 N 0.5531(4) 0.6328(3) 0.8242(3) 0.0282(11) Uani 1 1 d . . .
N4 N 0.1659(5) 0.3725(3) 0.7237(3) 0.0425(14) Uani 1 1 d . . .
N3 N 0.0512(5) 0.3077(3) 0.6146(3) 0.0306(11) Uani 1 1 d . . .
O11 O 0.6140(5) 0.3285(4) 0.9991(4) 0.069(2) Uani 1 1 d . . .
O10 O 0.4948(7) 0.2366(3) 0.8786(4) 0.081(2) Uani 1 1 d . . .
O2 O 0.3952(4) 0.2959(2) 0.9571(2) 0.0327(10) Uani 1 1 d . . .
O6 O 0.2427(4) 0.3836(3) 0.9847(2) 0.0309(9) Uani 1 1 d . . .
O5 O 0.2042(4) 0.3373(2) 1.0995(2) 0.0300(9) Uani 1 1 d . . .
O7 O 0.0554(4) 0.2525(3) 0.9547(3) 0.0401(11) Uani 1 1 d . . .
O8 O 0.1723(4) 0.1660(3) 0.8978(2) 0.0376(10) Uani 1 1 d . . .
O4 O 0.1404(4) 0.1757(3) 1.0469(3) 0.0374(10) Uani 1 1 d . . .
O3 O 0.3428(4) 0.1696(3) 1.0227(3) 0.0358(10) Uani 1 1 d . . .
O1 O 0.5729(4) 0.6699(2) 0.8909(2) 0.0298(9) Uani 1 1 d . . .
O9 O 0.5292(6) 0.4793(3) 0.6882(3) 0.0579(15) Uani 1 1 d . . .
O20 O 0.2266(5) 0.4289(3) 0.7795(3) 0.0592(16) Uani 1 1 d . . .
O15 O 0.2138(4) 0.6184(3) 0.4787(2) 0.0359(10) Uani 1 1 d . . .
O14 O 0.1812(4) 0.7029(3) 0.3827(2) 0.0390(11) Uani 1 1 d . . .
O16 O 0.4002(5) 0.7459(4) 0.4958(3) 0.0552(15) Uani 1 1 d . . .
O18 O 0.1703(4) 0.8582(3) 0.5599(3) 0.0391(11) Uani 1 1 d . . .
O17 O 0.3726(4) 0.8224(3) 0.6170(3) 0.0427(11) Uani 1 1 d . . .
O19 O 0.2939(5) 0.8553(3) 0.4678(3) 0.0531(14) Uani 1 1 d . . .
O22 O -0.0207(6) 0.7014(4) 0.6398(5) 0.085(3) Uani 1 1 d . . .
O21 O 0.1813(7) 0.7421(3) 0.7218(3) 0.0690(19) Uani 1 1 d . . .
O12 O -0.0175(4) 0.2905(3) 0.5493(2) 0.0332(10) Uani 1 1 d . . .
O13 O 0.1432(4) 0.7069(3) 0.5883(2) 0.0344(10) Uani 1 1 d . . .
F13 F -0.1453(7) 0.2826(6) 0.9036(7) 0.155(4) Uani 1 1 d . . .
F14 F -0.2319(7) 0.1695(7) 0.8545(8) 0.227(8) Uani 1 1 d . . .
F15 F -0.1728(10) 0.2089(11) 0.9600(8) 0.239(8) Uani 1 1 d . . .
F27 F 0.6014(14) 0.7050(10) 0.4928(11) 0.230(8) Uani 1 1 d . A .
F9 F 0.0309(4) 0.4373(3) 1.1574(3) 0.0569(12) Uani 1 1 d . . .
F8 F 0.0301(4) 0.3235(3) 1.1586(3) 0.0601(13) Uani 1 1 d . . .
F23 F 0.2320(4) 0.4512(3) 0.3794(2) 0.0567(12) Uani 1 1 d . . .
F10 F 0.2543(4) 0.5015(3) 0.9335(3) 0.0534(12) Uani 1 1 d . . .
F12 F 0.1420(5) 0.5378(3) 0.9845(3) 0.0595(13) Uani 1 1 d . . .
F7 F 0.1808(4) 0.4219(3) 1.2222(2) 0.0601(13) Uani 1 1 d . . .
F22 F 0.2025(5) 0.4772(3) 0.4790(3) 0.0621(14) Uani 1 1 d . . .
F24 F 0.3733(5) 0.5250(4) 0.4730(3) 0.0773(17) Uani 1 1 d . . .
F11 F 0.0734(5) 0.4369(3) 0.8942(3) 0.0824(18) Uani 1 1 d . . .
F6 F -0.0530(6) 0.0925(4) 1.0599(4) 0.094(2) Uani 1 1 d . . .
F4 F 0.0741(7) 0.1250(4) 1.1603(3) 0.103(3) Uani 1 1 d . . .
F5 F 0.0238(6) 0.0096(3) 1.0851(4) 0.0852(19) Uani 1 1 d . . .
F2 F 0.5047(6) 0.1043(4) 1.0670(6) 0.138(4) Uani 1 1 d . . .
F3 F 0.3784(8) 0.0024(5) 1.0523(7) 0.150(4) Uani 1 1 d . . .
F1 F 0.3968(10) 0.0370(6) 0.9686(5) 0.152(4) Uani 1 1 d . . .
F16 F 0.1263(6) 0.0159(3) 0.8234(3) 0.0794(17) Uani 1 1 d . . .
F17 F 0.1119(7) 0.0819(3) 0.7529(3) 0.092(2) Uani 1 1 d . . .
F18 F -0.0403(7) 0.0077(4) 0.7624(4) 0.108(3) Uani 1 1 d . . .
F30 F 0.5266(7) 0.8916(5) 0.7582(3) 0.124(3) Uani 1 1 d . A .
F29 F 0.5352(18) 0.9804(7) 0.7169(5) 0.254(10) Uani 1 1 d . A .
F25 F 0.6728(10) 0.8166(9) 0.4957(9) 0.207(6) Uani 1 1 d . A .
F26 F 0.5416(12) 0.7421(18) 0.4156(9) 0.344(17) Uani 1 1 d . A .
F35 F 0.2703(11) 0.9217(9) 0.3557(7) 0.214(7) Uani 1 1 d . A .
F36 F 0.4399(14) 0.9595(12) 0.4090(12) 0.245(9) Uani 1 1 d . A .
F32 F 0.2173(12) 1.0533(4) 0.6296(5) 0.176(5) Uani 1 1 d . . .
F20 F 0.2754(11) 0.7152(7) 0.2734(4) 0.243(9) Uani 1 1 d . . .
F19 F 0.0940(9) 0.6641(8) 0.2394(4) 0.156(4) Uani 1 1 d . . .
F34 F 0.355(3) 1.0224(13) 0.4393(11) 0.330(14) Uani 1 1 d . A .
F21 F 0.1880(8) 0.5983(5) 0.2239(3) 0.112(3) Uani 1 1 d . . .
F28 F 0.6336(12) 0.9298(13) 0.7089(10) 0.278(10) Uani 1 1 d . A .
P1 P 0.50037(14) 0.30755(10) 0.93630(9) 0.0311(3) Uani 1 1 d . . .
P2 P 0.09778(16) 0.69083(10) 0.64496(9) 0.0333(4) Uani 1 1 d . A .
Tb1 Tb 0.25333(2) 0.266316(17) 1.008043(15) 0.02707(9) Uani 1 1 d . . .
Tb2 Tb 0.22006(3) 0.749786(18) 0.507380(15) 0.03136(9) Uani 1 1 d . . .
C58 C 0.4841(11) 0.8550(7) 0.6340(8) 0.046(3) Uani 0.587(10) 1 d P A 1
C62 C 0.2537(19) 0.9651(9) 0.5241(9) 0.080(6) Uani 0.587(10) 1 d P A 1
H62 H 0.2648 1.0171 0.5293 0.096 Uiso 0.587(10) 1 calc PR A 1
C57 C 0.5506(13) 0.8386(11) 0.5908(9) 0.070(5) Uani 0.587(10) 1 d P A 1
H57 H 0.6300 0.8656 0.6077 0.084 Uiso 0.587(10) 1 calc PR A 1
C63 C 0.2941(16) 0.9241(10) 0.4775(9) 0.074(6) Uani 0.587(10) 1 d P A 1
C56 C 0.5029(12) 0.7844(10) 0.5248(10) 0.061(4) Uani 0.587(10) 1 d P A 1
C61 C 0.1946(17) 0.9272(10) 0.5644(11) 0.052(4) Uani 0.587(10) 1 d P A 1
C61A C 0.358(3) 0.8652(14) 0.4322(15) 0.085(10) Uani 0.413(10) 1 d P A 2
C62A C 0.448(3) 0.828(5) 0.4334(19) 0.26(5) Uani 0.413(10) 1 d P A 2
H62A H 0.4955 0.8391 0.4065 0.311 Uiso 0.413(10) 1 calc PR A 2
C56A C 0.4104(14) 0.8939(11) 0.6474(9) 0.040(4) Uani 0.413(10) 1 d P A 2
C57A C 0.3573(18) 0.9496(10) 0.6367(9) 0.045(5) Uani 0.413(10) 1 d P A 2
H57A H 0.3996 1.0022 0.6571 0.054 Uiso 0.413(10) 1 calc PR A 2
C58A C 0.239(2) 0.9246(14) 0.5946(13) 0.046(5) Uani 0.413(10) 1 d P A 2
C63A C 0.465(3) 0.776(3) 0.4738(18) 0.118(16) Uani 0.413(10) 1 d P A 2
F31 F 0.1710(17) 0.9627(8) 0.6756(8) 0.133(6) Uani 0.578(14) 1 d P B 3
F33 F 0.054(2) 0.9686(12) 0.5879(10) 0.133(6) Uani 0.578(14) 1 d P B 3
C60A C 0.153(2) 0.9758(11) 0.6164(13) 0.066(5) Uani 0.578(14) 1 d P B 3
F33A F 0.148(2) 0.9889(11) 0.5245(11) 0.122(7) Uani 0.422(14) 1 d P B 4
F31A F 0.067(3) 0.9549(15) 0.6139(15) 0.122(7) Uani 0.422(14) 1 d P B 4
C60B C 0.180(3) 0.9869(16) 0.5897(18) 0.066(5) Uani 0.422(14) 1 d P B 4
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
F5 C22 F6 109.4(8) . .
F5 C22 F4 112.7(9) . .
F6 C22 F4 103.3(9) . .
F5 C22 C21 113.7(8) . .
F6 C22 C21 109.5(8) . .
F4 C22 C21 107.6(7) . .
C12 C11 C10 118.8(6) . .
C12 C11 P1 121.9(5) . .
C10 C11 P1 119.2(4) . .
F3 C18 F1 103.8(9) . .
F3 C18 F2 106.9(9) . .
F1 C18 F2 102.0(10) . .
F3 C18 C19 118.7(9) . .
F1 C18 C19 111.9(9) . .
F2 C18 C19 111.9(7) . .
N1 C3 C1 108.7(6) . .
N1 C3 C2 107.6(6) . .
C1 C3 C2 110.3(7) . .
N1 C3 C4 101.5(5) . .
C1 C3 C4 115.0(6) . .
C2 C3 C4 113.1(6) . .
O6 C26 C25 128.1(6) . .
O6 C26 C27 115.5(5) . .
C25 C26 C27 116.4(5) . .
C13 C8 C9 120.3(6) . .
C13 C8 C7 120.6(6) . .
C9 C8 C7 118.9(6) . .
N1 C7 N2 109.1(6) . .
N1 C7 C8 126.7(5) . .
N2 C7 C8 124.0(6) . .
F11 C27 F12 106.7(6) . .
F11 C27 F10 106.6(6) . .
F12 C27 F10 106.0(6) . .
F11 C27 C26 111.0(6) . .
F12 C27 C26 114.5(6) . .
F10 C27 C26 111.5(5) . .
N3 C39 N4 108.8(6) . .
N3 C39 C40 127.8(6) . .
N4 C39 C40 123.2(6) . .
F28 C59 F29 98.3(15) . .
F28 C59 F30 106.0(12) . .
F29 C59 F30 109.9(12) . .
F28 C59 C58 97.8(14) . .
F29 C59 C58 126.1(11) . .
F30 C59 C58 114.2(9) . .
F28 C59 C56A 140.5(13) . .
F29 C59 C56A 85.1(13) . .
F30 C59 C56A 109.7(9) . .
C58 C59 C56A 52.1(8) . .
O15 C53 C52 130.6(7) . .
O15 C53 C54 112.9(6) . .
C52 C53 C54 116.5(6) . .
N2 C4 C5 110.2(6) . .
N2 C4 C6 104.8(6) . .
C5 C4 C6 109.3(7) . .
N2 C4 C3 101.4(5) . .
C5 C4 C3 116.8(6) . .
C6 C4 C3 113.5(6) . .
O22 C48 C49 108.8(9) . .
O11 C16 C17 110.8(8) . .
F14 C28 F15 104.8(13) . .
F14 C28 F13 105.7(12) . .
F15 C28 F13 105.6(12) . .
F14 C28 C29 115.9(9) . .
F15 C28 C29 110.0(10) . .
F13 C28 C29 113.9(9) . .
O14 C51 C52 128.5(7) . .
O14 C51 C50 113.4(7) . .
C52 C51 C50 118.1(7) . .
O4 C21 C20 127.7(7) . .
O4 C21 C22 116.2(8) . .
C20 C21 C22 116.1(8) . .
C41 C42 C43 120.2(6) . .
C44 C43 C42 119.9(6) . .
C44 C43 P2 119.2(5) . .
C42 C43 P2 120.9(5) . .
C10 C9 C8 119.4(6) . .
O3 C19 C20 127.1(7) . .
O3 C19 C18 116.8(7) . .
C20 C19 C18 116.1(7) . .
C44 C45 C40 119.7(6) . .
F16 C32 F18 106.6(7) . .
F16 C32 F17 106.3(9) . .
F18 C32 F17 108.2(8) . .
F16 C32 C31 112.7(7) . .
F18 C32 C31 112.7(9) . .
F17 C32 C31 109.9(7) . .
C37 C36 N4 115.2(10) . .
C37 C36 C35 124.6(10) . .
N4 C36 C35 103.3(6) . .
C37 C36 C38 103.0(12) . .
N4 C36 C38 101.2(8) . .
C35 C36 C38 107.0(9) . .
F22 C54 F24 109.2(7) . .
F22 C54 F23 107.2(7) . .
F24 C54 F23 106.9(6) . .
F22 C54 C53 111.9(6) . .
F24 C54 C53 110.5(7) . .
F23 C54 C53 111.0(6) . .
C26 C25 C24 120.0(5) . .
F8 C23 F7 107.7(6) . .
F8 C23 F9 107.3(6) . .
F7 C23 F9 107.0(6) . .
F8 C23 C24 111.3(5) . .
F7 C23 C24 110.0(5) . .
F9 C23 C24 113.3(6) . .
O5 C24 C25 127.9(5) . .
O5 C24 C23 113.5(6) . .
C25 C24 C23 118.5(5) . .
C9 C10 C11 120.8(5) . .
C12 C13 C8 119.6(6) . .
C13 C12 C11 121.0(6) . .
C33 C35 C34 109.6(10) . .
C33 C35 N3 108.2(7) . .
C34 C35 N3 107.1(6) . .
C33 C35 C36 115.7(9) . .
C34 C35 C36 113.9(9) . .
N3 C35 C36 101.5(5) . .
C45 C40 C41 120.2(6) . .
C45 C40 C39 119.9(5) . .
C41 C40 C39 119.6(6) . .
C42 C41 C40 119.4(6) . .
C45 C44 C43 120.5(6) . .
C21 C20 C19 119.7(7) . .
O7 C29 C30 125.9(8) . .
O7 C29 C28 117.2(8) . .
C30 C29 C28 116.6(8) . .
O8 C31 C30 129.7(8) . .
O8 C31 C32 111.7(8) . .
C30 C31 C32 118.5(8) . .
C51 C52 C53 119.4(7) . .
C47 C46 O21 114.0(10) . .
C31 C30 C29 118.8(8) . .
O10 C14 C15 122.1(12) . .
F27 C55 F26 108(3) . .
F27 C55 F25 109.5(18) . .
F26 C55 F25 102(2) . .
F27 C55 C63A 128(2) . .
F26 C55 C63A 83(2) . .
F25 C55 C63A 117(3) . .
F27 C55 C56 109(2) . .
F26 C55 C56 120.0(19) . .
F25 C55 C56 107.6(18) . .
C63A C55 C56 36.9(13) . .
F34 C64 F36 100.6(17) . .
F34 C64 F35 112(2) . .
F36 C64 F35 100(3) . .
F34 C64 C63 103(3) . .
F36 C64 C63 128.5(19) . .
F35 C64 C63 111.4(12) . .
F34 C64 C61A 155(2) . .
F36 C64 C61A 79(2) . .
F35 C64 C61A 92(2) . .
C63 C64 C61A 61.0(11) . .
F20 C50 F21 114.4(11) . .
F20 C50 F19 109.7(13) . .
F21 C50 F19 94.3(9) . .
F20 C50 C51 114.3(9) . .
F21 C50 C51 115.0(9) . .
F19 C50 C51 106.9(8) . .
O9 N2 C7 124.9(6) . .
O9 N2 C4 122.4(5) . .
C7 N2 C4 111.5(5) . .
O1 N1 C7 125.8(5) . .
O1 N1 C3 121.0(5) . .
C7 N1 C3 113.0(5) . .
O20 N4 C39 125.5(6) . .
O20 N4 C36 121.3(6) . .
C39 N4 C36 112.6(6) . .
O12 N3 C39 126.1(5) . .
O12 N3 C35 120.5(5) . .
C39 N3 C35 113.4(5) . .
C16 O11 P1 124.7(5) . .
C14 O10 P1 132.0(7) . .
P1 O2 Tb1 166.8(3) . .
C26 O6 Tb1 130.8(4) . .
C24 O5 Tb1 131.2(4) . .
C29 O7 Tb1 137.5(5) . .
C31 O8 Tb1 133.9(5) . .
C21 O4 Tb1 138.5(5) . .
C19 O3 Tb1 136.0(5) . .
N1 O1 Tb1 133.0(3) . 2_667
C53 O15 Tb2 129.6(5) . .
C51 O14 Tb2 132.2(5) . .
C63A O16 C56 49.8(17) . .
C63A O16 Tb2 137(2) . .
C56 O16 Tb2 137.9(9) . .
C61 O18 C58A 35.0(11) . .
C61 O18 Tb2 137.8(9) . .
C58A O18 Tb2 126.0(13) . .
C56A O17 C58 64.9(10) . .
C56A O17 Tb2 128.7(9) . .
C58 O17 Tb2 133.8(7) . .
C61A O19 C63 90.3(15) . .
C61A O19 Tb2 132.2(14) . .
C63 O19 Tb2 137.3(8) . .
C48 O22 P2 129.2(6) . .
C46 O21 P2 124.7(6) . .
N3 O12 Tb2 135.4(4) . 2_566
P2 O13 Tb2 172.1(3) . .
C59 F29 F28 40.6(9) . .
C59 F29 C56A 57.0(10) . .
F28 F29 C56A 90.4(10) . .
C55 F26 C63A 56.6(16) . .
C60B F32 C60A 32.8(14) . .
C59 F28 F29 41.1(9) . .
O2 P1 O10 113.3(3) . .
O2 P1 O11 114.1(3) . .
O10 P1 O11 106.8(5) . .
O2 P1 C11 112.2(3) . .
O10 P1 C11 105.9(3) . .
O11 P1 C11 103.9(3) . .
O13 P2 O22 114.9(3) . .
O13 P2 O21 113.5(3) . .
O22 P2 O21 105.8(5) . .
O13 P2 C43 112.3(3) . .
O22 P2 C43 106.8(3) . .
O21 P2 C43 102.6(3) . .
O2 Tb1 O4 147.86(15) . .
O2 Tb1 O5 134.19(15) . .
O4 Tb1 O5 73.32(15) . .
O2 Tb1 O8 78.57(17) . .
O4 Tb1 O8 83.70(17) . .
O5 Tb1 O8 142.80(16) . .
O2 Tb1 O7 124.55(17) . .
O4 Tb1 O7 72.41(18) . .
O5 Tb1 O7 75.03(16) . .
O8 Tb1 O7 70.26(17) . .
O2 Tb1 O6 77.14(14) . .
O4 Tb1 O6 134.27(15) . .
O5 Tb1 O6 71.84(14) . .
O8 Tb1 O6 107.74(16) . .
O7 Tb1 O6 70.67(16) . .
O2 Tb1 O1 76.93(16) . 2_667
O4 Tb1 O1 102.84(16) . 2_667
O5 Tb1 O1 72.65(14) . 2_667
O8 Tb1 O1 142.39(15) . 2_667
O7 Tb1 O1 147.24(15) . 2_667
O6 Tb1 O1 94.08(15) . 2_667
O2 Tb1 O3 78.62(15) . .
O4 Tb1 O3 70.71(16) . .
O5 Tb1 O3 122.80(15) . .
O8 Tb1 O3 73.65(17) . .
O7 Tb1 O3 130.30(17) . .
O6 Tb1 O3 154.85(15) . .
O1 Tb1 O3 73.86(16) 2_667 .
O13 Tb2 O12 75.98(16) . 2_566
O13 Tb2 O19 147.69(18) . .
O12 Tb2 O19 103.74(19) 2_566 .
O13 Tb2 O16 124.7(2) . .
O12 Tb2 O16 146.33(17) 2_566 .
O19 Tb2 O16 73.1(2) . .
O13 Tb2 O14 135.35(17) . .
O12 Tb2 O14 72.02(16) 2_566 .
O19 Tb2 O14 71.41(18) . .
O16 Tb2 O14 75.41(18) . .
O13 Tb2 O17 78.32(17) . .
O12 Tb2 O17 143.61(16) 2_566 .
O19 Tb2 O17 84.97(19) . .
O16 Tb2 O17 70.05(18) . .
O14 Tb2 O17 142.57(17) . .
O13 Tb2 O15 77.82(15) . .
O12 Tb2 O15 90.57(16) 2_566 .
O19 Tb2 O15 134.15(18) . .
O16 Tb2 O15 71.39(19) . .
O14 Tb2 O15 72.27(16) . .
O17 Tb2 O15 108.69(17) . .
O13 Tb2 O18 78.72(16) . .
O12 Tb2 O18 76.87(16) 2_566 .
O19 Tb2 O18 70.00(19) . .
O16 Tb2 O18 129.30(19) . .
O14 Tb2 O18 121.80(17) . .
O17 Tb2 O18 73.16(17) . .
O15 Tb2 O18 155.47(16) . .
O17 C58 C57 125.3(13) . .
O17 C58 C59 112.8(11) . .
C57 C58 C59 121.9(12) . .
C63 C62 C61 119.6(15) . .
C56 C57 C58 122.4(13) . .
O19 C63 C62 128.1(14) . .
O19 C63 C64 108.1(18) . .
C62 C63 C64 124(2) . .
O16 C56 C57 125.7(14) . .
O16 C56 C55 110.8(15) . .
C57 C56 C55 123.3(14) . .
O18 C61 C62 126.2(16) . .
O19 C61A C62A 122(3) . .
O19 C61A C64 98(2) . .
C62A C61A C64 135(3) . .
C63A C62A C61A 124(3) . .
O17 C56A C57A 129.0(16) . .
O17 C56A C59 108.8(13) . .
C57A C56A C59 122.2(15) . .
O17 C56A F29 146.7(14) . .
C57A C56A F29 84.3(12) . .
C59 C56A F29 37.9(6) . .
C58A C57A C56A 119.2(17) . .
O18 C58A C57A 130(2) . .
O16 C63A C62A 125(3) . .
O16 C63A C55 121(4) . .
C62A C63A C55 114(3) . .
O16 C63A F26 133(4) . .
C62A C63A F26 87(3) . .
C55 C63A F26 40.3(12) . .
F33 C60A F31 114(3) . .
F33 C60A F32 106(2) . .
F31 C60A F32 107.4(19) . .
F32 C60B F33A 108(2) . .
F32 C60B F31A 98(2) . .
F33A C60B F31A 111(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C22 F5 1.277(11) .
C22 F6 1.333(13) .
C22 F4 1.345(11) .
C22 C21 1.561(11) .
C11 C12 1.399(8) .
C11 C10 1.404(9) .
C11 P1 1.780(6) .
C18 F3 1.254(11) .
C18 F1 1.293(12) .
C18 F2 1.301(12) .
C18 C19 1.493(11) .
C3 N1 1.504(8) .
C3 C1 1.522(10) .
C3 C2 1.535(11) .
C3 C4 1.556(10) .
C26 O6 1.248(7) .
C26 C25 1.405(8) .
C26 C27 1.521(9) .
C8 C13 1.394(9) .
C8 C9 1.406(8) .
C8 C7 1.472(9) .
C7 N1 1.321(8) .
C7 N2 1.370(8) .
C27 F11 1.324(9) .
C27 F12 1.325(8) .
C27 F10 1.332(8) .
C39 N3 1.327(8) .
C39 N4 1.359(8) .
C39 C40 1.460(9) .
C59 F28 1.163(14) .
C59 F29 1.176(13) .
C59 F30 1.295(11) .
C59 C58 1.499(17) .
C59 C56A 1.607(19) .
C53 O15 1.264(8) .
C53 C52 1.394(10) .
C53 C54 1.545(10) .
C4 N2 1.493(9) .
C4 C5 1.508(10) .
C4 C6 1.535(10) .
C48 O22 1.427(10) .
C48 C49 1.443(15) .
C16 O11 1.418(10) .
C16 C17 1.451(14) .
C28 F14 1.244(12) .
C28 F15 1.254(16) .
C28 F13 1.265(14) .
C28 C29 1.521(12) .
C51 O14 1.245(9) .
C51 C52 1.386(12) .
C51 C50 1.546(11) .
C21 O4 1.232(9) .
C21 C20 1.409(12) .
C42 C41 1.378(9) .
C42 C43 1.399(9) .
C43 C44 1.390(8) .
C43 P2 1.781(7) .
C9 C10 1.370(9) .
C19 O3 1.241(9) .
C19 C20 1.410(12) .
C45 C44 1.380(9) .
C45 C40 1.390(8) .
C32 F16 1.305(11) .
C32 F18 1.320(12) .
C32 F17 1.327(10) .
C32 C31 1.551(11) .
C36 C37 1.378(15) .
C36 N4 1.482(10) .
C36 C35 1.537(10) .
C36 C38 1.679(17) .
C54 F22 1.318(9) .
C54 F24 1.329(9) .
C54 F23 1.330(8) .
C25 C24 1.406(9) .
C23 F8 1.319(8) .
C23 F7 1.328(8) .
C23 F9 1.343(8) .
C23 C24 1.531(8) .
C24 O5 1.247(7) .
C13 C12 1.372(10) .
C35 C33 1.487(13) .
C35 C34 1.512(12) .
C35 N3 1.513(8) .
C40 C41 1.413(9) .
C29 O7 1.211(9) .
C29 C30 1.428(13) .
C31 O8 1.267(9) .
C31 C30 1.381(12) .
C46 C47 1.379(16) .
C46 O21 1.425(10) .
C14 O10 1.328(13) .
C14 C15 1.365(15) .
C55 F27 1.19(2) .
C55 F26 1.19(2) .
C55 F25 1.31(2) .
C55 C63A 1.54(4) .
C55 C56 1.58(2) .
C64 F34 1.17(4) .
C64 F36 1.29(4) .
C64 F35 1.30(2) .
C64 C63 1.61(2) .
C64 C61A 1.84(4) .
C50 F20 1.174(13) .
C50 F21 1.278(11) .
C50 F19 1.390(13) .
N2 O9 1.272(8) .
N1 O1 1.309(6) .
N4 O20 1.266(7) .
N3 O12 1.307(7) .
O11 P1 1.552(6) .
O10 P1 1.541(6) .
O2 P1 1.473(5) .
O2 Tb1 2.301(4) .
O6 Tb1 2.388(4) .
O5 Tb1 2.357(4) .
O7 Tb1 2.380(5) .
O8 Tb1 2.364(5) .
O4 Tb1 2.341(5) .
O3 Tb1 2.414(4) .
O1 Tb1 2.396(4) 2_667
O15 Tb2 2.385(5) .
O14 Tb2 2.373(4) .
O16 C63A 1.12(4) .
O16 C56 1.220(16) .
O16 Tb2 2.367(5) .
O18 C61 1.230(18) .
O18 C58A 1.24(2) .
O18 Tb2 2.395(4) .
O17 C56A 1.251(19) .
O17 C58 1.299(14) .
O17 Tb2 2.379(5) .
O19 C61A 1.22(2) .
O19 C63 1.26(2) .
O19 Tb2 2.365(5) .
O22 P2 1.542(6) .
O21 P2 1.568(6) .
O12 Tb2 2.358(4) 2_566
O13 P2 1.470(5) .
O13 Tb2 2.307(4) .
F29 F28 1.770(19) .
F29 C56A 1.91(2) .
F26 C63A 1.83(3) .
F32 C60B 1.22(3) .
F32 C60A 1.40(2) .
Tb1 O1 2.396(4) 2_667
Tb2 O12 2.358(4) 2_566
C58 C57 1.40(2) .
C62 C63 1.37(3) .
C62 C61 1.43(3) .
C57 C56 1.37(2) .
C61A C62A 1.48(7) .
C62A C63A 1.43(9) .
C56A C57A 1.41(3) .
C57A C58A 1.41(3) .
F31 C60A 1.26(3) .
F33 C60A 1.19(3) .
F33A C60B 1.30(4) .
F31A C60B 1.65(5) .
