#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:25:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179059 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302150.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_4302150
loop_
_publ_author_name
'Pierre Thuéry'
_publ_section_title
;
Lanthanide Complexes with Cucurbit[n]urils (n= 5, 6, 7) and Perrhenate
Ligands: New Examples of Encapsulation of Perrhenate Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4497
_journal_page_last               4513
_journal_paper_doi               10.1021/ic900328z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C72 H112 N52 O88 Re8 Sm4'
_chemical_formula_weight         5205.14
_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                 108.873(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.3634(8)
_cell_length_b                   23.9396(13)
_cell_length_c                   19.8421(6)
_cell_measurement_reflns_used    134858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.96
_cell_volume                     6456.0(6)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 2° steps (425 frames)'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            134858
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.392
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.532
_refine_diff_density_min         -3.197
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         12225
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0669
_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)+(0.0408P)²+11.2201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                10054
_reflns_number_total             12225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900328z_si_001_09.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302150
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
Sm1 Sm 0.55302(6) 1.08155(4) 0.12799(4) 0.02689(19) Uani 1 1 d . . .
Sm2 Sm 0.97197(6) 0.77650(4) 0.35091(5) 0.0320(2) Uani 1 1 d . . .
Re1 Re 0.75210(4) 0.87813(3) 0.22502(3) 0.02399(15) Uani 1 1 d . . .
Re2 Re 1.14299(5) 0.79034(3) 0.56063(4) 0.02881(17) Uani 1 1 d . . .
Re3 Re 0.69030(6) 0.12764(3) 0.56405(4) 0.02645(16) Uani 1 1 d . . .
Re4 Re 0.34380(8) 0.05555(5) 0.38345(6) 0.0435(3) Uani 1 1 d . . .
O1 O 0.5076(7) 1.0219(4) 0.2104(5) 0.023(2) Uani 1 1 d . . .
O2 O 0.7160(7) 0.8485(4) 0.4195(6) 0.026(2) Uani 1 1 d . . .
O3 O 0.7089(8) 1.0655(4) 0.2163(5) 0.024(2) Uani 1 1 d . . .
O4 O 0.9588(8) 0.9218(4) 0.4647(6) 0.031(3) Uani 1 1 d . . .
O5 O 0.8482(9) 1.0239(6) 0.0985(6) 0.045(3) Uani 1 1 d . . .
O6 O 1.0541(9) 0.8651(5) 0.3381(6) 0.033(3) Uani 1 1 d . . .
O7 O 0.7676(9) 0.9176(6) -0.0108(7) 0.047(3) Uani 1 1 d . . .
O8 O 0.9626(9) 0.7613(6) 0.2314(6) 0.044(3) Uani 1 1 d . . .
O9 O 0.5316(8) 0.8612(6) -0.0275(6) 0.043(3) Uani 1 1 d . . .
O10 O 0.7219(8) 0.6882(5) 0.2101(7) 0.040(3) Uani 1 1 d . . .
O11 O 0.4245(8) 0.9141(4) 0.0906(5) 0.027(2) Uani 1 1 d . . .
O12 O 0.6008(8) 0.7363(4) 0.3084(6) 0.029(2) Uani 1 1 d . . .
O13 O 0.5983(12) 1.1689(6) 0.2109(10) 0.070(5) Uani 1 1 d . . .
O14 O 0.6657(12) 1.1682(6) 0.1337(8) 0.061(4) Uani 1 1 d . . .
O15 O 0.7212(12) 1.2271(7) 0.2290(9) 0.064(4) Uani 1 1 d . . .
O16 O 0.4077(8) 1.0348(5) 0.0514(7) 0.044(3) Uani 1 1 d . . .
O17 O 0.6589(9) 1.0726(5) 0.0549(6) 0.036(3) Uani 1 1 d . . .
O18 O 0.4253(9) 1.1241(4) 0.1684(6) 0.035(3) Uani 1 1 d . . .
O19 O 0.5882(8) 0.9809(4) 0.1078(6) 0.033(3) Uani 1 1 d . . .
O20 O 0.8531(13) 0.8433(8) 0.2777(10) 0.086(5) Uani 1 1 d U . .
O21 O 0.7785(15) 0.8997(9) 0.1539(10) 0.096(6) Uani 1 1 d U . .
O22 O 0.6549(12) 0.8357(8) 0.2079(10) 0.084(5) Uani 1 1 d U . .
O23 O 0.7284(15) 0.9313(9) 0.2734(12) 0.097(6) Uani 1 1 d U . .
O24 O 1.0930(8) 0.7993(5) 0.4687(6) 0.036(3) Uani 1 1 d . . .
O25 O 1.0630(9) 0.8119(5) 0.6007(8) 0.052(4) Uani 1 1 d . . .
O26 O 1.1710(9) 0.7202(5) 0.5808(7) 0.045(3) Uani 1 1 d . . .
O27 O 1.2490(8) 0.8281(4) 0.5929(7) 0.037(3) Uani 1 1 d . . .
O28 O 0.9617(10) 0.6707(5) 0.3213(6) 0.042(2) Uani 1 1 d U . .
O29 O 0.9928(9) 0.6944(5) 0.4316(6) 0.0401(19) Uani 1 1 d . . .
O30 O 0.9665(10) 0.6084(5) 0.4001(7) 0.049(2) Uani 1 1 d U . .
O31 O 1.1355(8) 0.7441(5) 0.3583(7) 0.041(3) Uani 1 1 d . . .
O32 O 0.8978(8) 0.8172(5) 0.4332(7) 0.041(3) Uani 1 1 d . . .
O33 O 0.8089(9) 0.7377(7) 0.3329(7) 0.057(4) Uani 1 1 d . . .
O34 O 0.7208(8) 0.1133(5) 0.6537(6) 0.033(3) Uani 1 1 d . . .
O35 O 0.5661(8) 0.1165(5) 0.5229(6) 0.036(3) Uani 1 1 d . . .
O36 O 0.7103(8) 0.1985(4) 0.5535(6) 0.034(3) Uani 1 1 d . . .
O37 O 0.7606(8) 0.0872(4) 0.5253(6) 0.031(3) Uani 1 1 d . . .
O38 O 0.2643(15) 0.0269(10) 0.3024(11) 0.105(6) Uani 1 1 d U . .
O39 O 0.3121(17) 0.1081(9) 0.4335(12) 0.105(6) Uani 1 1 d U . .
O40 O 0.3804(10) -0.0007(5) 0.4396(6) 0.037(3) Uani 1 1 d . . .
O41 O 0.4383(9) 0.0820(5) 0.3609(7) 0.043(3) Uani 1 1 d . . .
O42 O 0.2594(18) 1.0769(10) 0.1787(13) 0.116(7) Uani 1 1 d U . .
O43 O 0.7913(15) 1.0210(9) -0.0846(11) 0.097(6) Uani 1 1 d U . .
O44 O 1.1879(16) 0.6158(9) 0.5180(12) 0.103(7) Uani 1 1 d U . .
N1 N 0.4758(8) 0.9513(5) 0.2782(6) 0.018(2) Uani 1 1 d . . .
N2 N 0.5893(9) 1.0139(5) 0.3301(6) 0.019(2) Uani 1 1 d . . .
N3 N 0.6783(9) 0.9433(5) 0.4131(6) 0.021(3) Uani 1 1 d . . .
N4 N 0.5593(8) 0.8811(4) 0.3646(6) 0.018(2) Uani 1 1 d . . .
N5 N 0.7441(8) 1.0560(5) 0.3364(6) 0.021(3) Uani 1 1 d . . .
N6 N 0.8659(9) 1.0531(5) 0.2927(7) 0.024(3) Uani 1 1 d . . .
N7 N 0.9664(9) 0.9966(6) 0.3930(7) 0.033(3) Uani 1 1 d . . .
N8 N 0.8358(9) 0.9886(5) 0.4282(7) 0.027(3) Uani 1 1 d . . .
N9 N 0.9539(10) 1.0212(6) 0.2145(7) 0.036(3) Uani 1 1 d . . .
N10 N 0.9844(10) 0.9670(6) 0.1337(7) 0.030(3) Uani 1 1 d . . .
N11 N 1.0599(9) 0.8992(6) 0.2298(7) 0.031(3) Uani 1 1 d . . .
N12 N 1.0476(9) 0.9593(6) 0.3126(7) 0.032(3) Uani 1 1 d . . .
N13 N 0.9202(9) 0.8863(6) 0.0584(7) 0.034(3) Uani 1 1 d . . .
N14 N 0.8001(9) 0.8250(7) 0.0156(7) 0.033(3) Uani 1 1 d . . .
N15 N 0.8786(9) 0.7610(6) 0.1122(7) 0.029(3) Uani 1 1 d . . .
N16 N 1.0027(9) 0.8211(6) 0.1538(7) 0.029(3) Uani 1 1 d . . .
N17 N 0.6382(10) 0.7852(6) 0.0000(7) 0.032(3) Uani 1 1 d . . .
N18 N 0.5065(9) 0.7833(6) 0.0348(7) 0.026(3) Uani 1 1 d . . .
N19 N 0.5785(9) 0.7120(5) 0.1246(7) 0.027(3) Uani 1 1 d . . .
N20 N 0.7181(10) 0.7255(6) 0.1033(7) 0.030(3) Uani 1 1 d . . .
N21 N 0.4143(9) 0.8193(5) 0.1088(7) 0.026(3) Uani 1 1 d . . .
N22 N 0.4072(9) 0.8769(5) 0.1929(6) 0.022(3) Uani 1 1 d . . .
N23 N 0.4871(9) 0.8071(5) 0.2823(6) 0.025(3) Uani 1 1 d . . .
N24 N 0.4863(9) 0.7469(5) 0.1983(7) 0.027(3) Uani 1 1 d . . .
N25 N 0.6638(14) 1.1899(7) 0.1947(9) 0.038(4) Uani 1 1 d . . .
N26 N 0.9754(10) 0.6561(6) 0.3832(7) 0.0306(19) Uani 1 1 d . . .
C1 C 0.5226(10) 0.9979(6) 0.2680(8) 0.021(3) Uani 1 1 d . . .
C2 C 0.5901(11) 0.9770(6) 0.3879(7) 0.020(3) Uani 1 1 d . . .
H2 H 0.5768 0.9971 0.4268 0.024 Uiso 1 1 calc R . .
C3 C 0.5081(11) 0.9345(5) 0.3521(7) 0.018(3) Uani 1 1 d . . .
H3 H 0.4545 0.9357 0.3726 0.022 Uiso 1 1 calc R . .
C4 C 0.6581(11) 0.8872(6) 0.4010(7) 0.021(3) Uani 1 1 d . . .
C5 C 0.6438(10) 1.0648(6) 0.3395(7) 0.020(3) Uani 1 1 d . . .
H5A H 0.6480 1.0810 0.3852 0.024 Uiso 1 1 calc R . .
H5B H 0.6092 1.0911 0.3027 0.024 Uiso 1 1 calc R . .
C6 C 0.7710(12) 0.9648(7) 0.4621(8) 0.031(4) Uani 1 1 d . . .
H6A H 0.7561 0.9929 0.4922 0.038 Uiso 1 1 calc R . .
H6B H 0.8050 0.9345 0.4927 0.038 Uiso 1 1 calc R . .
C7 C 0.7671(11) 1.0587(6) 0.2754(8) 0.022(3) Uani 1 1 d . . .
C8 C 0.9145(11) 1.0489(6) 0.3684(8) 0.023(3) Uani 1 1 d . . .
H8 H 0.9565 1.0813 0.3872 0.028 Uiso 1 1 calc R . .
C9 C 0.8277(10) 1.0452(5) 0.3988(8) 0.019(3) Uani 1 1 d . . .
H9 H 0.8336 1.0735 0.4357 0.023 Uiso 1 1 calc R . .
C10 C 0.9219(13) 0.9640(6) 0.4299(10) 0.034(4) Uani 1 1 d . . .
C11 C 0.9157(13) 1.0674(7) 0.2426(10) 0.035(4) Uani 1 1 d . . .
H11A H 0.8702 1.0876 0.2033 0.042 Uiso 1 1 calc R . .
H11B H 0.9696 1.0924 0.2658 0.042 Uiso 1 1 calc R . .
C12 C 1.0598(12) 0.9806(7) 0.3842(8) 0.034(4) Uani 1 1 d . . .
H12A H 1.0908 0.9520 0.4190 0.041 Uiso 1 1 calc R . .
H12B H 1.1032 1.0127 0.3935 0.041 Uiso 1 1 calc R . .
C13 C 0.9222(12) 1.0054(8) 0.1470(9) 0.038(4) Uani 1 1 d . . .
C14 C 1.0671(11) 0.9522(7) 0.2007(8) 0.032(4) Uani 1 1 d . . .
H14 H 1.1316 0.9576 0.1946 0.038 Uiso 1 1 calc R . .
C15 C 1.0498(11) 0.9950(6) 0.2546(9) 0.030(4) Uani 1 1 d . . .
H15 H 1.1028 1.0227 0.2697 0.036 Uiso 1 1 calc R . .
C16 C 1.0539(11) 0.9050(6) 0.2980(9) 0.026(3) Uani 1 1 d . . .
C17 C 0.9699(11) 0.9396(7) 0.0677(8) 0.029(4) Uani 1 1 d . . .
H17A H 1.0337 0.9341 0.0617 0.035 Uiso 1 1 calc R . .
H17B H 0.9324 0.9643 0.0298 0.035 Uiso 1 1 calc R . .
C18 C 1.0834(11) 0.8477(7) 0.2037(8) 0.031(4) Uani 1 1 d . . .
H18A H 1.1337 0.8543 0.1817 0.037 Uiso 1 1 calc R . .
H18B H 1.1109 0.8226 0.2436 0.037 Uiso 1 1 calc R . .
C19 C 0.8232(12) 0.8806(8) 0.0191(8) 0.032(4) Uani 1 1 d . . .
C20 C 0.8848(12) 0.7898(7) 0.0494(8) 0.029(4) Uani 1 1 d . . .
H20 H 0.8989 0.7641 0.0155 0.035 Uiso 1 1 calc R . .
C21 C 0.9668(11) 0.8329(7) 0.0782(7) 0.027(3) Uani 1 1 d . . .
H21 H 1.0190 0.8274 0.0570 0.032 Uiso 1 1 calc R . .
C22 C 0.9501(12) 0.7795(7) 0.1708(9) 0.032(4) Uani 1 1 d . . .
C23 C 0.7077(12) 0.8052(9) -0.0339(9) 0.041(5) Uani 1 1 d . . .
H23A H 0.7214 0.7752 -0.0622 0.049 Uiso 1 1 calc R . .
H23B H 0.6773 0.8354 -0.0662 0.049 Uiso 1 1 calc R . .
C24 C 0.8191(11) 0.7129(6) 0.1104(9) 0.032(4) Uani 1 1 d . . .
H24A H 0.8478 0.6917 0.1538 0.038 Uiso 1 1 calc R . .
H24B H 0.8202 0.6895 0.0708 0.038 Uiso 1 1 calc R . .
C25 C 0.5577(11) 0.8149(8) 0.0002(8) 0.033(4) Uani 1 1 d . . .
C26 C 0.5476(12) 0.7285(7) 0.0494(9) 0.034(4) Uani 1 1 d . . .
H26 H 0.5034 0.7006 0.0193 0.041 Uiso 1 1 calc R . .
C27 C 0.6434(13) 0.7312(7) 0.0339(9) 0.036(4) Uani 1 1 d . . .
H27 H 0.6481 0.7010 0.0019 0.043 Uiso 1 1 calc R . .
C28 C 0.6743(13) 0.7075(7) 0.1519(8) 0.030(4) Uani 1 1 d . . .
C29 C 0.4118(11) 0.8002(6) 0.0386(8) 0.026(3) Uani 1 1 d . . .
H29A H 0.3668 0.7688 0.0247 0.031 Uiso 1 1 calc R . .
H29B H 0.3862 0.8300 0.0045 0.031 Uiso 1 1 calc R . .
C30 C 0.5130(12) 0.6991(7) 0.1630(9) 0.030(4) Uani 1 1 d . . .
H30A H 0.5434 0.6710 0.1985 0.036 Uiso 1 1 calc R . .
H30B H 0.4535 0.6830 0.1303 0.036 Uiso 1 1 calc R . .
C31 C 0.4172(10) 0.8743(7) 0.1278(8) 0.026(3) Uani 1 1 d . . .
C32 C 0.3987(11) 0.8227(6) 0.2228(7) 0.022(3) Uani 1 1 d . . .
H32 H 0.3379 0.8186 0.2346 0.026 Uiso 1 1 calc R . .
C33 C 0.4039(10) 0.7828(6) 0.1633(7) 0.020(3) Uani 1 1 d . . .
H33 H 0.3432 0.7610 0.1454 0.024 Uiso 1 1 calc R . .
C34 C 0.5302(11) 0.7606(6) 0.2661(8) 0.024(3) Uani 1 1 d . . .
C35 C 0.3900(11) 0.9293(6) 0.2256(8) 0.024(3) Uani 1 1 d . . .
H35A H 0.3650 0.9570 0.1885 0.029 Uiso 1 1 calc R . .
H35B H 0.3397 0.9229 0.2476 0.029 Uiso 1 1 calc R . .
C36 C 0.5085(12) 0.8282(6) 0.3533(7) 0.024(3) Uani 1 1 d . . .
H36A H 0.5485 0.8010 0.3865 0.029 Uiso 1 1 calc R . .
H36B H 0.4473 0.8324 0.3636 0.029 Uiso 1 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 0.0000 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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
O3 Sm1 O9 143.5(4) . 3_675 ?
O3 Sm1 O1 78.6(3) . . ?
O9 Sm1 O1 136.5(4) 3_675 . ?
O3 Sm1 O16 143.1(4) . . ?
O9 Sm1 O16 69.0(4) 3_675 . ?
O1 Sm1 O16 77.6(4) . . ?
O3 Sm1 O17 78.7(4) . . ?
O9 Sm1 O17 78.5(4) 3_675 . ?
O1 Sm1 O17 135.4(4) . . ?
O16 Sm1 O17 99.4(4) . . ?
O3 Sm1 O18 116.8(4) . . ?
O9 Sm1 O18 78.6(4) 3_675 . ?
O1 Sm1 O18 68.2(3) . . ?
O16 Sm1 O18 79.2(4) . . ?
O17 Sm1 O18 155.9(4) . . ?
O3 Sm1 O19 76.9(4) . . ?
O9 Sm1 O19 119.2(4) 3_675 . ?
O1 Sm1 O19 69.8(3) . . ?
O16 Sm1 O19 68.6(4) . . ?
O17 Sm1 O19 67.9(4) . . ?
O18 Sm1 O19 131.3(4) . . ?
O3 Sm1 O13 71.5(4) . . ?
O9 Sm1 O13 91.2(5) 3_675 . ?
O1 Sm1 O13 96.5(4) . . ?
O16 Sm1 O13 139.0(4) . . ?
O17 Sm1 O13 111.8(5) . . ?
O18 Sm1 O13 61.3(5) . . ?
O19 Sm1 O13 147.6(5) . . ?
O3 Sm1 O14 71.0(4) . . ?
O9 Sm1 O14 73.9(4) 3_675 . ?
O1 Sm1 O14 137.7(4) . . ?
O16 Sm1 O14 142.3(5) . . ?
O17 Sm1 O14 66.2(4) . . ?
O18 Sm1 O14 100.1(4) . . ?
O19 Sm1 O14 127.8(4) . . ?
O13 Sm1 O14 46.5(5) . . ?
O8 Sm2 O32 147.6(4) . . ?
O8 Sm2 O31 75.6(4) . . ?
O32 Sm2 O31 135.6(4) . . ?
O8 Sm2 O33 93.1(4) . . ?
O32 Sm2 O33 69.0(4) . . ?
O31 Sm2 O33 138.7(5) . . ?
O8 Sm2 O20 72.7(6) . . ?
O32 Sm2 O20 76.2(5) . . ?
O31 Sm2 O20 136.0(5) . . ?
O33 Sm2 O20 73.1(6) . . ?
O8 Sm2 O6 84.4(4) . . ?
O32 Sm2 O6 93.0(4) . . ?
O31 Sm2 O6 78.2(4) . . ?
O33 Sm2 O6 141.0(5) . . ?
O20 Sm2 O6 69.1(5) . . ?
O8 Sm2 O24 140.9(4) . . ?
O32 Sm2 O24 66.6(4) . . ?
O31 Sm2 O24 69.2(4) . . ?
O33 Sm2 O24 124.7(4) . . ?
O20 Sm2 O24 123.8(6) . . ?
O6 Sm2 O24 72.3(4) . . ?
O8 Sm2 O29 118.7(4) . . ?
O32 Sm2 O29 82.6(4) . . ?
O31 Sm2 O29 78.3(4) . . ?
O33 Sm2 O29 72.8(5) . . ?
O20 Sm2 O29 144.4(5) . . ?
O6 Sm2 O29 141.1(4) . . ?
O24 Sm2 O29 70.5(4) . . ?
O8 Sm2 O28 69.0(4) . . ?
O32 Sm2 O28 122.7(4) . . ?
O31 Sm2 O28 71.7(4) . . ?
O33 Sm2 O28 67.2(5) . . ?
O20 Sm2 O28 121.8(6) . . ?
O6 Sm2 O28 143.7(4) . . ?
O24 Sm2 O28 113.6(4) . . ?
O29 Sm2 O28 50.3(4) . . ?
O21 Re1 O22 115.0(10) . . ?
O21 Re1 O23 113.0(11) . . ?
O22 Re1 O23 105.3(9) . . ?
O21 Re1 O20 106.9(10) . . ?
O22 Re1 O20 108.5(10) . . ?
O23 Re1 O20 107.8(10) . . ?
O25 Re2 O27 108.9(6) . . ?
O25 Re2 O26 109.3(6) . . ?
O27 Re2 O26 108.2(6) . . ?
O25 Re2 O24 110.2(6) . . ?
O27 Re2 O24 110.0(6) . . ?
O26 Re2 O24 110.2(6) . . ?
O34 Re3 O35 109.6(5) . . ?
O34 Re3 O36 108.7(6) . . ?
O35 Re3 O36 106.2(5) . . ?
O34 Re3 O37 110.7(5) . . ?
O35 Re3 O37 111.2(6) . . ?
O36 Re3 O37 110.2(5) . . ?
O41 Re4 O40 111.3(6) . . ?
O41 Re4 O39 105.0(8) . . ?
O40 Re4 O39 106.1(8) . . ?
O41 Re4 O38 104.0(8) . . ?
O40 Re4 O38 104.8(8) . . ?
O39 Re4 O38 125.4(11) . . ?
C1 O1 Sm1 153.9(9) . . ?
C7 O3 Sm1 157.3(9) . . ?
C16 O6 Sm2 145.2(10) . . ?
C22 O8 Sm2 150.1(12) . . ?
C25 O9 Sm1 151.4(12) . 3_675 ?
N25 O13 Sm1 103.0(13) . . ?
N25 O14 Sm1 98.9(11) . . ?
Re1 O20 Sm2 167.2(11) . . ?
Re2 O24 Sm2 152.2(6) . . ?
N26 O28 Sm2 94.2(9) . . ?
N26 O29 Sm2 97.4(8) . . ?
C1 N1 C35 123.2(12) . . ?
C1 N1 C3 111.6(11) . . ?
C35 N1 C3 123.7(12) . . ?
C1 N2 C5 123.9(12) . . ?
C1 N2 C2 111.9(12) . . ?
C5 N2 C2 123.7(12) . . ?
C4 N3 C2 111.8(12) . . ?
C4 N3 C6 123.5(12) . . ?
C2 N3 C6 122.7(12) . . ?
C4 N4 C36 123.9(11) . . ?
C4 N4 C3 112.0(11) . . ?
C36 N4 C3 122.9(11) . . ?
C7 N5 C9 113.5(12) . . ?
C7 N5 C5 123.7(12) . . ?
C9 N5 C5 122.8(11) . . ?
C7 N6 C11 121.1(13) . . ?
C7 N6 C8 112.6(12) . . ?
C11 N6 C8 123.7(13) . . ?
C10 N7 C8 113.2(13) . . ?
C10 N7 C12 121.5(14) . . ?
C8 N7 C12 125.1(14) . . ?
C10 N8 C6 122.7(13) . . ?
C10 N8 C9 111.4(13) . . ?
C6 N8 C9 125.1(12) . . ?
C13 N9 C11 124.6(15) . . ?
C13 N9 C15 112.2(13) . . ?
C11 N9 C15 121.6(14) . . ?
C13 N10 C17 125.4(14) . . ?
C13 N10 C14 111.4(13) . . ?
C17 N10 C14 122.9(12) . . ?
C16 N11 C14 110.1(13) . . ?
C16 N11 C18 122.6(13) . . ?
C14 N11 C18 125.1(13) . . ?
C16 N12 C15 112.5(13) . . ?
C16 N12 C12 123.4(14) . . ?
C15 N12 C12 122.7(14) . . ?
C19 N13 C21 111.4(14) . . ?
C19 N13 C17 122.1(14) . . ?
C21 N13 C17 125.7(12) . . ?
C19 N14 C23 120.4(15) . . ?
C19 N14 C20 112.8(13) . . ?
C23 N14 C20 124.7(15) . . ?
C22 N15 C24 124.6(14) . . ?
C22 N15 C20 110.0(14) . . ?
C24 N15 C20 124.3(13) . . ?
C22 N16 C18 123.6(14) . . ?
C22 N16 C21 111.2(13) . . ?
C18 N16 C21 125.2(14) . . ?
C25 N17 C27 112.4(14) . . ?
C25 N17 C23 122.8(16) . . ?
C27 N17 C23 124.7(15) . . ?
C25 N18 C26 110.6(13) . . ?
C25 N18 C29 122.3(14) . . ?
C26 N18 C29 125.5(13) . . ?
C28 N19 C30 123.3(14) . . ?
C28 N19 C26 112.0(13) . . ?
C30 N19 C26 124.6(13) . . ?
C28 N20 C24 122.5(14) . . ?
C28 N20 C27 109.1(13) . . ?
C24 N20 C27 121.5(13) . . ?
C31 N21 C33 112.3(12) . . ?
C31 N21 C29 123.8(13) . . ?
C33 N21 C29 123.6(12) . . ?
C31 N22 C32 113.6(12) . . ?
C31 N22 C35 123.3(12) . . ?
C32 N22 C35 122.4(11) . . ?
C34 N23 C36 123.4(13) . . ?
C34 N23 C32 110.9(12) . . ?
C36 N23 C32 123.5(12) . . ?
C34 N24 C33 112.7(12) . . ?
C34 N24 C30 124.6(13) . . ?
C33 N24 C30 122.6(12) . . ?
O13 N25 O15 126.0(17) . . ?
O13 N25 O14 109.3(18) . . ?
O15 N25 O14 124.7(17) . . ?
O30 N26 O28 123.2(14) . . ?
O30 N26 O29 118.5(13) . . ?
O28 N26 O29 118.0(13) . . ?
O1 C1 N2 125.1(13) . . ?
O1 C1 N1 125.1(13) . . ?
N2 C1 N1 109.8(12) . . ?
N2 C2 N3 113.3(11) . . ?
N2 C2 C3 103.2(11) . . ?
N3 C2 C3 104.1(11) . . ?
N2 C2 H2 111.9 . . ?
N3 C2 H2 111.9 . . ?
C3 C2 H2 111.9 . . ?
N1 C3 N4 113.3(11) . . ?
N1 C3 C2 103.3(11) . . ?
N4 C3 C2 103.5(11) . . ?
N1 C3 H3 112.0 . . ?
N4 C3 H3 112.0 . . ?
C2 C3 H3 112.0 . . ?
O2 C4 N4 124.3(13) . . ?
O2 C4 N3 127.1(14) . . ?
N4 C4 N3 108.5(12) . . ?
N2 C5 N5 112.0(11) . . ?
N2 C5 H5A 109.2 . . ?
N5 C5 H5A 109.2 . . ?
N2 C5 H5B 109.2 . . ?
N5 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N8 C6 N3 114.7(13) . . ?
N8 C6 H6A 108.6 . . ?
N3 C6 H6A 108.6 . . ?
N8 C6 H6B 108.6 . . ?
N3 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
O3 C7 N5 125.4(13) . . ?
O3 C7 N6 126.6(13) . . ?
N5 C7 N6 108.0(13) . . ?
N6 C8 N7 115.6(12) . . ?
N6 C8 C9 103.3(11) . . ?
N7 C8 C9 102.1(12) . . ?
N6 C8 H8 111.7 . . ?
N7 C8 H8 111.7 . . ?
C9 C8 H8 111.7 . . ?
N5 C9 N8 116.4(11) . . ?
N5 C9 C8 101.9(11) . . ?
N8 C9 C8 103.6(11) . . ?
N5 C9 H9 111.4 . . ?
N8 C9 H9 111.4 . . ?
C8 C9 H9 111.4 . . ?
O4 C10 N8 125.9(16) . . ?
O4 C10 N7 125.1(15) . . ?
N8 C10 N7 108.7(14) . . ?
N9 C11 N6 115.2(13) . . ?
N9 C11 H11A 108.5 . . ?
N6 C11 H11A 108.5 . . ?
N9 C11 H11B 108.5 . . ?
N6 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
N7 C12 N12 112.4(13) . . ?
N7 C12 H12A 109.1 . . ?
N12 C12 H12A 109.1 . . ?
N7 C12 H12B 109.1 . . ?
N12 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
O5 C13 N9 126.9(17) . . ?
O5 C13 N10 122.1(16) . . ?
N9 C13 N10 110.8(14) . . ?
N11 C14 N10 115.4(13) . . ?
N11 C14 C15 105.2(13) . . ?
N10 C14 C15 101.3(13) . . ?
N11 C14 H14 111.4 . . ?
N10 C14 H14 111.4 . . ?
C15 C14 H14 111.4 . . ?
N12 C15 N9 114.9(13) . . ?
N12 C15 C14 101.9(12) . . ?
N9 C15 C14 103.6(13) . . ?
N12 C15 H15 111.9 . . ?
N9 C15 H15 111.9 . . ?
C14 C15 H15 111.9 . . ?
O6 C16 N12 126.5(15) . . ?
O6 C16 N11 123.9(14) . . ?
N12 C16 N11 109.7(14) . . ?
N10 C17 N13 116.3(13) . . ?
N10 C17 H17A 108.2 . . ?
N13 C17 H17A 108.2 . . ?
N10 C17 H17B 108.2 . . ?
N13 C17 H17B 108.2 . . ?
H17A C17 H17B 107.4 . . ?
N16 C18 N11 114.3(12) . . ?
N16 C18 H18A 108.7 . . ?
N11 C18 H18A 108.7 . . ?
N16 C18 H18B 108.7 . . ?
N11 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
O7 C19 N13 126.5(18) . . ?
O7 C19 N14 125.2(16) . . ?
N13 C19 N14 108.2(14) . . ?
N14 C20 N15 113.3(12) . . ?
N14 C20 C21 102.2(13) . . ?
N15 C20 C21 104.6(12) . . ?
N14 C20 H20 112.0 . . ?
N15 C20 H20 112.0 . . ?
C21 C20 H20 112.0 . . ?
N13 C21 N16 115.8(12) . . ?
N13 C21 C20 105.2(12) . . ?
N16 C21 C20 103.3(13) . . ?
N13 C21 H21 110.7 . . ?
N16 C21 H21 110.7 . . ?
C20 C21 H21 110.7 . . ?
O8 C22 N15 123.5(16) . . ?
O8 C22 N16 125.7(16) . . ?
N15 C22 N16 110.8(14) . . ?
N14 C23 N17 114.1(13) . . ?
N14 C23 H23A 108.7 . . ?
N17 C23 H23A 108.7 . . ?
N14 C23 H23B 108.7 . . ?
N17 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N15 C24 N20 114.1(13) . . ?
N15 C24 H24A 108.7 . . ?
N20 C24 H24A 108.7 . . ?
N15 C24 H24B 108.7 . . ?
N20 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
O9 C25 N17 127.0(15) . . ?
O9 C25 N18 125.2(15) . . ?
N17 C25 N18 107.8(15) . . ?
N18 C26 N19 115.0(13) . . ?
N18 C26 C27 105.3(14) . . ?
N19 C26 C27 102.9(13) . . ?
N18 C26 H26 111.1 . . ?
N19 C26 H26 111.1 . . ?
C27 C26 H26 111.1 . . ?
N17 C27 N20 115.8(13) . . ?
N17 C27 C26 102.7(14) . . ?
N20 C27 C26 104.3(14) . . ?
N17 C27 H27 111.2 . . ?
N20 C27 H27 111.2 . . ?
C26 C27 H27 111.2 . . ?
O10 C28 N19 127.7(16) . . ?
O10 C28 N20 122.3(16) . . ?
N19 C28 N20 109.9(14) . . ?
N18 C29 N21 113.9(12) . . ?
N18 C29 H29A 108.8 . . ?
N21 C29 H29A 108.8 . . ?
N18 C29 H29B 108.8 . . ?
N21 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
N19 C30 N24 114.1(13) . . ?
N19 C30 H30A 108.7 . . ?
N24 C30 H30A 108.7 . . ?
N19 C30 H30B 108.7 . . ?
N24 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
O11 C31 N22 126.6(14) . . ?
O11 C31 N21 125.5(14) . . ?
N22 C31 N21 107.8(13) . . ?
N22 C32 N23 112.9(12) . . ?
N22 C32 C33 102.1(11) . . ?
N23 C32 C33 102.4(11) . . ?
N22 C32 H32 112.8 . . ?
N23 C32 H32 112.8 . . ?
C33 C32 H32 112.8 . . ?
N21 C33 N24 117.1(12) . . ?
N21 C33 C32 104.1(11) . . ?
N24 C33 C32 103.6(11) . . ?
N21 C33 H33 110.5 . . ?
N24 C33 H33 110.5 . . ?
C32 C33 H33 110.5 . . ?
O12 C34 N24 126.1(14) . . ?
O12 C34 N23 124.2(14) . . ?
N24 C34 N23 109.7(13) . . ?
N1 C35 N22 114.0(12) . . ?
N1 C35 H35A 108.7 . . ?
N22 C35 H35A 108.7 . . ?
N1 C35 H35B 108.7 . . ?
N22 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
N23 C36 N4 113.4(12) . . ?
N23 C36 H36A 108.9 . . ?
N4 C36 H36A 108.9 . . ?
N23 C36 H36B 108.9 . . ?
N4 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
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
Sm1 O3 2.386(10) . ?
Sm1 O9 2.402(11) 3_675 ?
Sm1 O1 2.415(10) . ?
Sm1 O16 2.422(12) . ?
Sm1 O17 2.427(11) . ?
Sm1 O18 2.449(12) . ?
Sm1 O19 2.522(11) . ?
Sm1 O13 2.609(16) . ?
Sm1 O14 2.611(15) . ?
Sm2 O8 2.359(12) . ?
Sm2 O32 2.424(13) . ?
Sm2 O31 2.433(12) . ?
Sm2 O33 2.436(13) . ?
Sm2 O20 2.445(17) . ?
Sm2 O6 2.479(12) . ?
Sm2 O24 2.481(12) . ?
Sm2 O29 2.491(12) . ?
Sm2 O28 2.593(12) . ?
Re1 O21 1.658(19) . ?
Re1 O22 1.670(17) . ?
Re1 O23 1.695(19) . ?
Re1 O20 1.707(17) . ?
Re2 O25 1.676(15) . ?
Re2 O27 1.708(11) . ?
Re2 O26 1.742(12) . ?
Re2 O24 1.744(11) . ?
Re3 O34 1.724(11) . ?
Re3 O35 1.726(11) . ?
Re3 O36 1.744(11) . ?
Re3 O37 1.747(10) . ?
Re4 O41 1.685(12) . ?
Re4 O40 1.718(11) . ?
Re4 O39 1.75(2) . ?
Re4 O38 1.78(2) . ?
O1 C1 1.234(17) . ?
O2 C4 1.219(17) . ?
O3 C7 1.212(18) . ?
O4 C10 1.240(19) . ?
O5 C13 1.26(2) . ?
O6 C16 1.242(19) . ?
O7 C19 1.21(2) . ?
O8 C22 1.236(19) . ?
O9 C25 1.24(2) . ?
O9 Sm1 2.402(11) 3_675 ?
O10 C28 1.227(19) . ?
O11 C31 1.230(18) . ?
O12 C34 1.234(18) . ?
O13 N25 1.20(2) . ?
O14 N25 1.32(2) . ?
O15 N25 1.25(2) . ?
O28 N26 1.231(17) . ?
O29 N26 1.292(17) . ?
O30 N26 1.208(17) . ?
N1 C1 1.352(18) . ?
N1 C35 1.433(19) . ?
N1 C3 1.445(17) . ?
N2 C1 1.348(18) . ?
N2 C5 1.428(17) . ?
N2 C2 1.444(18) . ?
N3 C4 1.379(18) . ?
N3 C2 1.449(18) . ?
N3 C6 1.464(19) . ?
N4 C4 1.377(19) . ?
N4 C36 1.443(18) . ?
N4 C3 1.456(16) . ?
N5 C7 1.354(19) . ?
N5 C9 1.443(19) . ?
N5 C5 1.477(18) . ?
N6 C7 1.354(18) . ?
N6 C11 1.440(19) . ?
N6 C8 1.442(19) . ?
N7 C10 1.36(2) . ?
N7 C8 1.458(19) . ?
N7 C12 1.46(2) . ?
N8 C10 1.36(2) . ?
N8 C6 1.43(2) . ?
N8 C9 1.467(18) . ?
N9 C13 1.32(2) . ?
N9 C11 1.43(2) . ?
N9 C15 1.49(2) . ?
N10 C13 1.36(2) . ?
N10 C17 1.42(2) . ?
N10 C14 1.51(2) . ?
N11 C16 1.39(2) . ?
N11 C14 1.41(2) . ?
N11 C18 1.42(2) . ?
N12 C16 1.34(2) . ?
N12 C15 1.44(2) . ?
N12 C12 1.47(2) . ?
N13 C19 1.37(2) . ?
N13 C21 1.44(2) . ?
N13 C17 1.45(2) . ?
N14 C19 1.37(2) . ?
N14 C23 1.45(2) . ?
N14 C20 1.45(2) . ?
N15 C22 1.35(2) . ?
N15 C24 1.43(2) . ?
N15 C20 1.45(2) . ?
N16 C22 1.36(2) . ?
N16 C18 1.41(2) . ?
N16 C21 1.446(19) . ?
N17 C25 1.36(2) . ?
N17 C27 1.45(2) . ?
N17 C23 1.45(2) . ?
N18 C25 1.38(2) . ?
N18 C26 1.43(2) . ?
N18 C29 1.444(19) . ?
N19 C28 1.31(2) . ?
N19 C30 1.42(2) . ?
N19 C26 1.47(2) . ?
N20 C28 1.38(2) . ?
N20 C24 1.44(2) . ?
N20 C27 1.45(2) . ?
N21 C31 1.37(2) . ?
N21 C33 1.434(19) . ?
N21 C29 1.456(19) . ?
N22 C31 1.347(19) . ?
N22 C32 1.448(18) . ?
N22 C35 1.468(18) . ?
N23 C34 1.362(19) . ?
N23 C36 1.433(18) . ?
N23 C32 1.474(18) . ?
N24 C34 1.33(2) . ?
N24 C33 1.445(18) . ?
N24 C30 1.458(19) . ?
C2 C3 1.54(2) . ?
C2 H2 0.9800 . ?
C3 H3 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C8 C9 1.55(2) . ?
C8 H8 0.9800 . ?
C9 H9 0.9800 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 C15 1.56(2) . ?
C14 H14 0.9800 . ?
C15 H15 0.9800 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C20 C21 1.53(2) . ?
C20 H20 0.9800 . ?
C21 H21 0.9800 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C26 C27 1.51(2) . ?
C26 H26 0.9800 . ?
C27 H27 0.9800 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C32 C33 1.540(19) . ?
C32 H32 0.9800 . ?
C33 H33 0.9800 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
