#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/57/2215735.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2215735
loop_
_publ_author_name
'Xia, Hai-Tao'
'Liu, Yu-Fen'
'Wang, Da-Qi'
'Yang, Shu-Ping'
_publ_section_title
;Tetrakis(μ-naphthalene-1-acetato)bis(naphthalene-1-acetato)bis(1,10-phenanthroline)samarium(III)terbium(III)
 N,N-dimethylformamide disolvate
;
_journal_coeditor_code           AT2428
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2797
_journal_page_last               m2798
_journal_paper_doi               10.1107/S1600536807051720
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Sm Tb (C12 H9 O2)6 (C12 H8 N2)2], 2C3 H7 N O'
_chemical_formula_moiety         'C96 H70 N4 O12 Sm Tb, 2(C3 H7 N O)'
_chemical_formula_sum            'C102 H84 N6 O14 Sm Tb'
_chemical_formula_weight         1927.02
_chemical_name_systematic
;
Tetrakis(μ-naphthalene-1-acetato)bis(naphthalene-1-acetato)bis(1,10-
phenanthroline)samarium(III)terbium(III) N,N-dimethylformamide
disolvate
;
_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                 103.723(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4985(14)
_cell_length_b                   15.1320(17)
_cell_length_c                   22.181(2)
_cell_measurement_reflns_used    9128
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.922
_cell_measurement_theta_min      2.411
_cell_volume                     4401.3(8)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21723
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  0.8876
_exptl_absorpt_correction_T_min  0.4661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1954
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.983
_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     559
_refine_ls_number_reflns         7724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0529
_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)+(0.0325P)²+19.4345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                6069
_reflns_number_total             7724
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2428.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215735
_cod_database_fobs_code          2215735
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Sm Sm1 0.11747(2) 0.92966(2) 0.488418(14) 0.03101(10) Uani d P 0.50
Tb Tb1 0.11747(2) 0.92966(2) 0.488418(14) 0.03101(10) Uani d P 0.50
N N1 0.2709(4) 0.9436(4) 0.4349(3) 0.0448(14) Uani d . 1
N N2 0.2877(4) 0.8639(4) 0.5467(3) 0.0477(14) Uani d . 1
N N3 0.1323(7) 0.6639(6) 0.7473(4) 0.079(2) Uani d . 1
O O1 0.0591(3) 1.0802(3) 0.52069(18) 0.0362(10) Uani d . 1
O O2 0.2232(3) 1.0558(3) 0.5387(2) 0.0414(11) Uani d . 1
O O3 0.0870(4) 0.7727(3) 0.5111(2) 0.0542(13) Uani d . 1
O O4 0.0964(4) 0.8041(3) 0.4168(2) 0.0545(13) Uani d . 1
O O5 0.0958(3) 0.9248(3) 0.59139(19) 0.0404(10) Uani d . 1
O O6 -0.0489(3) 0.9875(3) 0.60333(19) 0.0417(11) Uani d . 1
O O7 0.2663(7) 0.7560(6) 0.7635(4) 0.128(3) Uani d . 1
C C1 0.1508(5) 1.0983(4) 0.5481(3) 0.0383(15) Uani d . 1
C C2 0.1653(5) 1.1738(5) 0.5945(3) 0.0510(18) Uani d . 1
H H2A 0.1407 1.2278 0.5723 0.061 Uiso calc R 1
H H2B 0.1232 1.1626 0.6235 0.061 Uiso calc R 1
C C3 0.2738(6) 1.1889(5) 0.6310(3) 0.0522(19) Uani d . 1
C C4 0.3228(6) 1.2634(6) 0.6203(4) 0.060(2) Uani d . 1
H H4 0.2889 1.3031 0.5904 0.073 Uiso calc R 1
C C5 0.4233(6) 1.2825(6) 0.6531(4) 0.070(2) Uani d . 1
H H5 0.4551 1.3342 0.6450 0.083 Uiso calc R 1
C C6 0.4723(7) 1.2256(6) 0.6957(4) 0.069(2) Uani d . 1
H H6 0.5393 1.2377 0.7164 0.083 Uiso calc R 1
C C7 0.4257(6) 1.1480(6) 0.7103(4) 0.066(2) Uani d . 1
C C8 0.3244(6) 1.1286(6) 0.6772(4) 0.057(2) Uani d . 1
C C9 0.2783(7) 1.0505(6) 0.6913(4) 0.066(2) Uani d . 1
H H9 0.2118 1.0373 0.6701 0.079 Uiso calc R 1
C C10 0.3300(8) 0.9937(7) 0.7359(4) 0.085(3) Uani d . 1
H H10 0.3001 0.9414 0.7446 0.102 Uiso calc R 1
C C11 0.4284(8) 1.0164(7) 0.7678(5) 0.089(3) Uani d . 1
H H11 0.4629 0.9783 0.7986 0.107 Uiso calc R 1
C C12 0.4762(8) 1.0900(7) 0.7566(4) 0.078(3) Uani d . 1
H H12 0.5420 1.1024 0.7792 0.094 Uiso calc R 1
C C13 0.0899(6) 0.7492(5) 0.4577(4) 0.0522(18) Uani d . 1
C C14 0.0862(7) 0.6504(5) 0.4447(4) 0.067(2) Uani d . 1
H H14A 0.0198 0.6279 0.4467 0.081 Uiso calc R 1
H H14B 0.0943 0.6406 0.4029 0.081 Uiso calc R 1
C C15 0.1661(8) 0.6001(6) 0.4889(4) 0.071(2) Uani d . 1
C C16 0.1407(8) 0.5477(6) 0.5335(5) 0.079(3) Uani d . 1
H H16 0.0729 0.5405 0.5351 0.095 Uiso calc R 1
C C17 0.2207(9) 0.5042(7) 0.5778(5) 0.089(3) Uani d . 1
H H17 0.2038 0.4668 0.6071 0.107 Uiso calc R 1
C C18 0.3174(10) 0.5160(7) 0.5779(5) 0.093(3) Uani d . 1
H H18 0.3671 0.4886 0.6085 0.112 Uiso calc R 1
C C19 0.3474(9) 0.5673(7) 0.5344(5) 0.087(3) Uani d . 1
C C20 0.2703(8) 0.6108(6) 0.4886(5) 0.073(3) Uani d . 1
C C21 0.3011(7) 0.6630(6) 0.4440(5) 0.076(3) Uani d . 1
H H21 0.2524 0.6906 0.4130 0.091 Uiso calc R 1
C C22 0.4044(7) 0.6739(6) 0.4459(5) 0.080(3) Uani d . 1
H H22 0.4254 0.7087 0.4166 0.096 Uiso calc R 1
C C23 0.4738(8) 0.6322(7) 0.4916(6) 0.090(3) Uani d . 1
H H23 0.5425 0.6398 0.4927 0.108 Uiso calc R 1
C C24 0.4501(9) 0.5820(7) 0.5342(6) 0.093(3) Uani d . 1
H H24 0.5014 0.5560 0.5645 0.112 Uiso calc R 1
C C25 0.0266(5) 0.9363(5) 0.6194(3) 0.0419(15) Uani d . 1
C C26 0.0374(6) 0.8860(5) 0.6796(3) 0.056(2) Uani d . 1
H H26A 0.0863 0.8388 0.6804 0.067 Uiso calc R 1
H H26B 0.0661 0.9258 0.7135 0.067 Uiso calc R 1
C C27 -0.0580(6) 0.8464(6) 0.6917(4) 0.057(2) Uani d . 1
C C28 -0.0902(6) 0.8723(6) 0.7435(4) 0.064(2) Uani d . 1
H H28 -0.0536 0.9153 0.7695 0.077 Uiso calc R 1
C C29 -0.1778(7) 0.8347(7) 0.7580(4) 0.073(3) Uani d . 1
H H29 -0.1986 0.8536 0.7929 0.087 Uiso calc R 1
C C30 -0.2306(7) 0.7720(7) 0.7216(4) 0.071(3) Uani d . 1
H H30 -0.2886 0.7486 0.7312 0.086 Uiso calc R 1
C C31 -0.2004(7) 0.7410(6) 0.6692(4) 0.067(2) Uani d . 1
C C32 -0.1133(6) 0.7798(6) 0.6537(4) 0.060(2) Uani d . 1
C C33 -0.0837(6) 0.7479(6) 0.6008(4) 0.062(2) Uani d . 1
H H33 -0.0280 0.7728 0.5891 0.074 Uiso calc R 1
C C34 -0.1366(7) 0.6807(7) 0.5667(4) 0.076(3) Uani d . 1
H H34 -0.1165 0.6609 0.5317 0.091 Uiso calc R 1
C C35 -0.2201(8) 0.6407(7) 0.5826(5) 0.084(3) Uani d . 1
H H35 -0.2535 0.5939 0.5591 0.100 Uiso calc R 1
C C36 -0.2519(7) 0.6702(7) 0.6321(5) 0.078(3) Uani d . 1
H H36 -0.3081 0.6440 0.6423 0.093 Uiso calc R 1
C C37 0.2630(6) 0.9833(5) 0.3812(4) 0.0524(19) Uani d . 1
H H37 0.2000 1.0060 0.3606 0.063 Uiso calc R 1
C C38 0.3471(6) 0.9927(6) 0.3535(4) 0.060(2) Uani d . 1
H H38 0.3393 1.0205 0.3152 0.072 Uiso calc R 1
C C39 0.4385(6) 0.9605(5) 0.3837(4) 0.057(2) Uani d . 1
H H39 0.4942 0.9658 0.3661 0.069 Uiso calc R 1
C C40 0.4503(5) 0.9200(5) 0.4406(4) 0.0533(19) Uani d . 1
C C41 0.3636(5) 0.9114(5) 0.4656(4) 0.0484(18) Uani d . 1
C C42 0.3729(5) 0.8697(5) 0.5247(4) 0.0524(19) Uani d . 1
C C43 0.4692(6) 0.8393(5) 0.5574(4) 0.060(2) Uani d . 1
C C44 0.4731(6) 0.8002(6) 0.6138(4) 0.071(2) Uani d . 1
H H44 0.5354 0.7797 0.6371 0.085 Uiso calc R 1
C C45 0.3878(6) 0.7907(6) 0.6366(4) 0.071(2) Uani d . 1
H H45 0.3908 0.7631 0.6745 0.086 Uiso calc R 1
C C46 0.2965(6) 0.8239(5) 0.6008(4) 0.060(2) Uani d . 1
H H46 0.2382 0.8177 0.6158 0.072 Uiso calc R 1
C C47 0.5460(6) 0.8855(5) 0.4757(4) 0.060(2) Uani d . 1
H H47 0.6033 0.8900 0.4595 0.072 Uiso calc R 1
C C48 0.5544(6) 0.8476(6) 0.5301(4) 0.064(2) Uani d . 1
H H48 0.6175 0.8258 0.5513 0.077 Uiso calc R 1
C C49 0.1896(9) 0.7236(9) 0.7785(5) 0.094(3) Uani d . 1
H H49 0.1736 0.7443 0.8145 0.113 Uiso calc R 1
C C50 0.0425(8) 0.6327(7) 0.7665(5) 0.094(3) Uani d . 1
H H50A 0.0334 0.6670 0.8012 0.141 Uiso calc R 1
H H50B 0.0512 0.5716 0.7782 0.141 Uiso calc R 1
H H50C -0.0165 0.6390 0.7327 0.141 Uiso calc R 1
C C51 0.1574(10) 0.6248(8) 0.6943(6) 0.117(4) Uani d . 1
H H51A 0.2183 0.6515 0.6876 0.176 Uiso calc R 1
H H51B 0.1023 0.6340 0.6585 0.176 Uiso calc R 1
H H51C 0.1683 0.5626 0.7012 0.176 Uiso calc R 1
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Sm1 O5 3_576 . 74.13(14)
O1 Sm1 O6 3_576 3_576 77.25(14)
O5 Sm1 O6 . 3_576 136.64(15)
O1 Sm1 O4 3_576 . 86.30(16)
O5 Sm1 O4 . . 125.39(17)
O6 Sm1 O4 3_576 . 83.81(17)
O1 Sm1 O3 3_576 . 75.12(15)
O5 Sm1 O3 . . 73.24(17)
O6 Sm1 O3 3_576 . 128.83(17)
O4 Sm1 O3 . . 52.40(17)
O1 Sm1 O2 3_576 . 123.42(14)
O5 Sm1 O2 . . 77.30(15)
O6 Sm1 O2 3_576 . 92.55(15)
O4 Sm1 O2 . . 148.57(15)
O3 Sm1 O2 . . 138.56(16)
O1 Sm1 N2 3_576 . 142.27(17)
O5 Sm1 N2 . . 78.59(16)
O6 Sm1 N2 3_576 . 139.25(17)
O4 Sm1 N2 . . 88.76(18)
O3 Sm1 N2 . . 72.36(18)
O2 Sm1 N2 . . 73.76(17)
O1 Sm1 O1 3_576 . 73.04(16)
O5 Sm1 O1 . . 69.07(14)
O6 Sm1 O1 3_576 . 71.84(14)
O4 Sm1 O1 . . 150.80(15)
O3 Sm1 O1 . . 135.76(15)
O2 Sm1 O1 . . 51.27(13)
N2 Sm1 O1 . . 120.20(16)
O1 Sm1 N1 3_576 . 149.18(16)
O5 Sm1 N1 . . 136.67(16)
O6 Sm1 N1 3_576 . 76.13(16)
O4 Sm1 N1 . . 75.67(17)
O3 Sm1 N1 . . 110.76(17)
O2 Sm1 N1 . . 73.16(15)
N2 Sm1 N1 . . 63.22(18)
O1 Sm1 N1 . . 112.40(15)
O1 Sm1 Tb1 3_576 3_576 38.40(11)
O5 Sm1 Tb1 . 3_576 66.76(10)
O6 Sm1 Tb1 3_576 3_576 70.52(10)
O4 Sm1 Tb1 . 3_576 121.91(12)
O3 Sm1 Tb1 . 3_576 108.21(11)
O2 Sm1 Tb1 . 3_576 85.47(10)
N2 Sm1 Tb1 . 3_576 142.82(13)
O1 Sm1 Tb1 . 3_576 34.64(9)
N1 Sm1 Tb1 . 3_576 139.27(13)
O1 Sm1 Sm1 3_576 3_576 38.40(11)
O5 Sm1 Sm1 . 3_576 66.76(10)
O6 Sm1 Sm1 3_576 3_576 70.52(10)
O4 Sm1 Sm1 . 3_576 121.91(12)
O3 Sm1 Sm1 . 3_576 108.21(11)
O2 Sm1 Sm1 . 3_576 85.47(10)
N2 Sm1 Sm1 . 3_576 142.82(13)
O1 Sm1 Sm1 . 3_576 34.64(9)
N1 Sm1 Sm1 . 3_576 139.27(13)
Tb1 Sm1 Sm1 3_576 3_576 0.000(8)
C37 N1 C41 . . 118.8(6)
C37 N1 Sm1 . . 122.8(4)
C41 N1 Sm1 . . 118.3(4)
C46 N2 C42 . . 117.1(6)
C46 N2 Sm1 . . 120.9(5)
C42 N2 Sm1 . . 122.0(5)
C49 N3 C51 . . 120.5(10)
C49 N3 C50 . . 120.6(10)
C51 N3 C50 . . 118.9(10)
C1 O1 Tb1 . 3_576 155.1(4)
C1 O1 Sm1 . 3_576 155.1(4)
C1 O1 Sm1 . . 89.8(4)
Tb1 O1 Sm1 3_576 . 106.96(16)
Sm1 O1 Sm1 3_576 . 106.96(16)
C1 O2 Sm1 . . 94.8(4)
C13 O3 Sm1 . . 92.1(5)
C13 O4 Sm1 . . 93.6(4)
C25 O5 Sm1 . . 138.7(4)
C25 O6 Tb1 . 3_576 133.5(4)
C25 O6 Sm1 . 3_576 133.5(4)
O2 C1 O1 . . 122.0(6)
O2 C1 C2 . . 122.0(6)
O1 C1 C2 . . 116.1(6)
C3 C2 C1 . . 115.4(6)
C3 C2 H2A . . 108.4
C1 C2 H2A . . 108.4
C3 C2 H2B . . 108.4
C1 C2 H2B . . 108.4
H2A C2 H2B . . 107.5
C4 C3 C8 . . 119.3(7)
C4 C3 C2 . . 118.8(7)
C8 C3 C2 . . 121.9(7)
C3 C4 C5 . . 122.0(8)
C3 C4 H4 . . 119.0
C5 C4 H4 . . 119.0
C6 C5 C4 . . 119.3(9)
C6 C5 H5 . . 120.4
C4 C5 H5 . . 120.4
C5 C6 C7 . . 121.9(8)
C5 C6 H6 . . 119.0
C7 C6 H6 . . 119.0
C12 C7 C6 . . 121.7(8)
C12 C7 C8 . . 119.5(9)
C6 C7 C8 . . 118.8(8)
C9 C8 C3 . . 122.6(7)
C9 C8 C7 . . 118.8(8)
C3 C8 C7 . . 118.6(8)
C10 C9 C8 . . 120.8(8)
C10 C9 H9 . . 119.6
C8 C9 H9 . . 119.6
C9 C10 C11 . . 118.3(10)
C9 C10 H10 . . 120.9
C11 C10 H10 . . 120.9
C12 C11 C10 . . 123.7(10)
C12 C11 H11 . . 118.2
C10 C11 H11 . . 118.2
C11 C12 C7 . . 119.0(9)
C11 C12 H12 . . 120.5
C7 C12 H12 . . 120.5
O3 C13 O4 . . 121.6(7)
O3 C13 C14 . . 117.0(8)
O4 C13 C14 . . 121.4(7)
C15 C14 C13 . . 113.1(7)
C15 C14 H14A . . 109.0
C13 C14 H14A . . 109.0
C15 C14 H14B . . 109.0
C13 C14 H14B . . 109.0
H14A C14 H14B . . 107.8
C16 C15 C20 . . 119.1(9)
C16 C15 C14 . . 120.4(9)
C20 C15 C14 . . 120.4(9)
C15 C16 C17 . . 118.8(10)
C15 C16 H16 . . 120.6
C17 C16 H16 . . 120.6
C18 C17 C16 . . 121.7(11)
C18 C17 H17 . . 119.2
C16 C17 H17 . . 119.2
C17 C18 C19 . . 122.1(11)
C17 C18 H18 . . 118.9
C19 C18 H18 . . 118.9
C18 C19 C24 . . 123.2(11)
C18 C19 C20 . . 118.3(11)
C24 C19 C20 . . 118.5(11)
C21 C20 C15 . . 121.8(9)
C21 C20 C19 . . 118.2(10)
C15 C20 C19 . . 120.0(10)
C22 C21 C20 . . 120.4(10)
C22 C21 H21 . . 119.8
C20 C21 H21 . . 119.8
C23 C22 C21 . . 118.3(11)
C23 C22 H22 . . 120.9
C21 C22 H22 . . 120.9
C24 C23 C22 . . 124.3(12)
C24 C23 H23 . . 117.8
C22 C23 H23 . . 117.8
C23 C24 C19 . . 120.3(11)
C23 C24 H24 . . 119.9
C19 C24 H24 . . 119.9
O5 C25 O6 . . 126.3(6)
O5 C25 C26 . . 116.2(6)
O6 C25 C26 . . 117.4(6)
C27 C26 C25 . . 116.8(6)
C27 C26 H26A . . 108.1
C25 C26 H26A . . 108.1
C27 C26 H26B . . 108.1
C25 C26 H26B . . 108.1
H26A C26 H26B . . 107.3
C28 C27 C32 . . 118.3(7)
C28 C27 C26 . . 119.3(8)
C32 C27 C26 . . 122.3(7)
C27 C28 C29 . . 121.3(9)
C27 C28 H28 . . 119.3
C29 C28 H28 . . 119.3
C30 C29 C28 . . 120.2(9)
C30 C29 H29 . . 119.9
C28 C29 H29 . . 119.9
C29 C30 C31 . . 121.4(9)
C29 C30 H30 . . 119.3
C31 C30 H30 . . 119.3
C30 C31 C32 . . 118.7(9)
C30 C31 C36 . . 122.2(9)
C32 C31 C36 . . 119.0(9)
C27 C32 C33 . . 121.8(7)
C27 C32 C31 . . 120.0(8)
C33 C32 C31 . . 118.2(8)
C34 C33 C32 . . 120.0(8)
C34 C33 H33 . . 120.0
C32 C33 H33 . . 120.0
C33 C34 C35 . . 122.1(10)
C33 C34 H34 . . 118.9
C35 C34 H34 . . 118.9
C36 C35 C34 . . 119.7(10)
C36 C35 H35 . . 120.2
C34 C35 H35 . . 120.2
C35 C36 C31 . . 120.9(9)
C35 C36 H36 . . 119.6
C31 C36 H36 . . 119.6
N1 C37 C38 . . 122.4(7)
N1 C37 H37 . . 118.8
C38 C37 H37 . . 118.8
C39 C38 C37 . . 118.6(8)
C39 C38 H38 . . 120.7
C37 C38 H38 . . 120.7
C38 C39 C40 . . 120.7(7)
C38 C39 H39 . . 119.6
C40 C39 H39 . . 119.6
C39 C40 C41 . . 118.2(7)
C39 C40 C47 . . 123.5(7)
C41 C40 C47 . . 118.3(8)
N1 C41 C40 . . 121.2(7)
N1 C41 C42 . . 118.9(6)
C40 C41 C42 . . 119.9(7)
N2 C42 C43 . . 123.5(7)
N2 C42 C41 . . 117.5(6)
C43 C42 C41 . . 119.0(7)
C44 C43 C42 . . 116.2(8)
C44 C43 C48 . . 124.4(8)
C42 C43 C48 . . 119.4(8)
C45 C44 C43 . . 121.9(8)
C45 C44 H44 . . 119.0
C43 C44 H44 . . 119.0
C44 C45 C46 . . 117.2(8)
C44 C45 H45 . . 121.4
C46 C45 H45 . . 121.4
N2 C46 C45 . . 124.1(8)
N2 C46 H46 . . 118.0
C45 C46 H46 . . 118.0
C48 C47 C40 . . 121.7(7)
C48 C47 H47 . . 119.1
C40 C47 H47 . . 119.1
C47 C48 C43 . . 121.7(8)
C47 C48 H48 . . 119.2
C43 C48 H48 . . 119.2
O7 C49 N3 . . 124.1(12)
O7 C49 H49 . . 117.9
N3 C49 H49 . . 117.9
N3 C50 H50A . . 109.5
N3 C50 H50B . . 109.5
H50A C50 H50B . . 109.5
N3 C50 H50C . . 109.5
H50A C50 H50C . . 109.5
H50B C50 H50C . . 109.5
N3 C51 H51A . . 109.5
N3 C51 H51B . . 109.5
H51A C51 H51B . . 109.5
N3 C51 H51C . . 109.5
H51A C51 H51C . . 109.5
H51B C51 H51C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sm1 O1 3_576 2.349(4)
Sm1 O5 . 2.371(4)
Sm1 O6 3_576 2.382(4)
Sm1 O4 . 2.449(5)
Sm1 O3 . 2.482(5)
Sm1 O2 . 2.483(4)
Sm1 N2 . 2.556(5)
Sm1 O1 . 2.567(4)
Sm1 N1 . 2.628(5)
Sm1 Tb1 3_576 3.9531(6)
Sm1 Sm1 3_576 3.9531(6)
N1 C37 . 1.316(9)
N1 C41 . 1.364(9)
N2 C46 . 1.323(9)
N2 C42 . 1.355(9)
N3 C49 . 1.280(13)
N3 C51 . 1.426(13)
N3 C50 . 1.456(12)
O1 C1 . 1.272(7)
O1 Tb1 3_576 2.349(4)
O1 Sm1 3_576 2.349(4)
O2 C1 . 1.228(7)
O3 C13 . 1.245(9)
O4 C13 . 1.249(9)
O5 C25 . 1.251(7)
O6 C25 . 1.262(8)
O6 Tb1 3_576 2.382(4)
O6 Sm1 3_576 2.382(4)
O7 C49 . 1.259(13)
C1 C2 . 1.520(9)
C2 C3 . 1.514(9)
C2 H2A . 0.9700
C2 H2B . 0.9700
C3 C4 . 1.355(11)
C3 C8 . 1.419(11)
C4 C5 . 1.409(11)
C4 H4 . 0.9300
C5 C6 . 1.332(12)
C5 H5 . 0.9300
C6 C7 . 1.406(12)
C6 H6 . 0.9300
C7 C12 . 1.399(12)
C7 C8 . 1.421(11)
C8 C9 . 1.405(11)
C9 C10 . 1.370(12)
C9 H9 . 0.9300
C10 C11 . 1.392(13)
C10 H10 . 0.9300
C11 C12 . 1.341(14)
C11 H11 . 0.9300
C12 H12 . 0.9300
C13 C14 . 1.521(10)
C14 C15 . 1.483(12)
C14 H14A . 0.9700
C14 H14B . 0.9700
C15 C16 . 1.375(13)
C15 C20 . 1.417(13)
C16 C17 . 1.435(13)
C16 H16 . 0.9300
C17 C18 . 1.317(14)
C17 H17 . 0.9300
C18 C19 . 1.372(15)
C18 H18 . 0.9300
C19 C24 . 1.405(15)
C19 C20 . 1.430(13)
C20 C21 . 1.405(13)
C21 C22 . 1.394(12)
C21 H21 . 0.9300
C22 C23 . 1.362(13)
C22 H22 . 0.9300
C23 C24 . 1.310(15)
C23 H23 . 0.9300
C24 H24 . 0.9300
C25 C26 . 1.513(9)
C26 C27 . 1.501(10)
C26 H26A . 0.9700
C26 H26B . 0.9700
C27 C28 . 1.379(11)
C27 C32 . 1.409(11)
C28 C29 . 1.415(11)
C28 H28 . 0.9300
C29 C30 . 1.336(12)
C29 H29 . 0.9300
C30 C31 . 1.399(12)
C30 H30 . 0.9300
C31 C32 . 1.427(11)
C31 C36 . 1.428(13)
C32 C33 . 1.412(11)
C33 C34 . 1.364(12)
C33 H33 . 0.9300
C34 C35 . 1.395(13)
C34 H34 . 0.9300
C35 C36 . 1.346(13)
C35 H35 . 0.9300
C36 H36 . 0.9300
C37 C38 . 1.421(10)
C37 H37 . 0.9300
C38 C39 . 1.348(11)
C38 H38 . 0.9300
C39 C40 . 1.377(11)
C39 H39 . 0.9300
C40 C41 . 1.416(9)
C40 C47 . 1.438(11)
C41 C42 . 1.433(10)
C42 C43 . 1.408(10)
C43 C44 . 1.373(12)
C43 C48 . 1.426(11)
C44 C45 . 1.372(12)
C44 H44 . 0.9300
C45 C46 . 1.392(10)
C45 H45 . 0.9300
C46 H46 . 0.9300
C47 C48 . 1.316(11)
C47 H47 . 0.9300
C48 H48 . 0.9300
C49 H49 . 0.9300
C50 H50A . 0.9600
C50 H50B . 0.9600
C50 H50C . 0.9600
C51 H51A . 0.9600
C51 H51B . 0.9600
C51 H51C . 0.9600
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C6 H6 O7 2_656 0.93 2.57 3.459(13) 160.0
C33 H33 O3 . 0.93 2.59 3.404(10) 147.0
C37 H37 O6 3_576 0.93 2.36 3.023(8) 127.7
C46 H46 O5 . 0.93 2.47 3.074(9) 122.3
C47 H47 O2 3_676 0.93 2.47 3.328(9) 152.9
C50 H50A O4 4_576 0.96 2.54 3.376(12) 145.8
C51 H51A O7 . 0.96 2.29 2.718(16) 106.2
C39 H39 CG1 3_676 0.93 2.98 3.853(15) 157.0
C30 H30 CG2 2_546 0.93 2.89 3.663(17) 141.8
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O1 Sm1 N1 C37 3_576 . 28.8(7)
O5 Sm1 N1 C37 . . -148.2(5)
O6 Sm1 N1 C37 3_576 . -2.1(5)
O4 Sm1 N1 C37 . . 84.9(6)
O3 Sm1 N1 C37 . . 124.5(5)
O2 Sm1 N1 C37 . . -99.2(6)
N2 Sm1 N1 C37 . . -179.1(6)
O1 Sm1 N1 C37 . . -65.4(6)
Tb1 Sm1 N1 C37 3_576 . -37.7(6)
Sm1 Sm1 N1 C37 3_576 . -37.7(6)
O1 Sm1 N1 C41 3_576 . -153.8(4)
O5 Sm1 N1 C41 . . 29.1(6)
O6 Sm1 N1 C41 3_576 . 175.2(5)
O4 Sm1 N1 C41 . . -97.8(5)
O3 Sm1 N1 C41 . . -58.2(5)
O2 Sm1 N1 C41 . . 78.1(5)
N2 Sm1 N1 C41 . . -1.8(5)
O1 Sm1 N1 C41 . . 111.9(5)
Tb1 Sm1 N1 C41 3_576 . 139.6(4)
Sm1 Sm1 N1 C41 3_576 . 139.6(4)
O1 Sm1 N2 C46 3_576 . -22.3(7)
O5 Sm1 N2 C46 . . 21.9(6)
O6 Sm1 N2 C46 3_576 . 176.3(5)
O4 Sm1 N2 C46 . . -104.6(6)
O3 Sm1 N2 C46 . . -53.9(6)
O2 Sm1 N2 C46 . . 101.8(6)
O1 Sm1 N2 C46 . . 79.3(6)
N1 Sm1 N2 C46 . . -179.2(6)
Tb1 Sm1 N2 C46 3_576 . 43.2(7)
Sm1 Sm1 N2 C46 3_576 . 43.2(7)
O1 Sm1 N2 C42 3_576 . 159.1(5)
O5 Sm1 N2 C42 . . -156.7(6)
O6 Sm1 N2 C42 3_576 . -2.3(7)
O4 Sm1 N2 C42 . . 76.7(6)
O3 Sm1 N2 C42 . . 127.4(6)
O2 Sm1 N2 C42 . . -76.8(5)
O1 Sm1 N2 C42 . . -99.4(5)
N1 Sm1 N2 C42 . . 2.2(5)
Tb1 Sm1 N2 C42 3_576 . -135.5(5)
Sm1 Sm1 N2 C42 3_576 . -135.5(5)
O1 Sm1 O1 C1 3_576 . 161.3(4)
O5 Sm1 O1 C1 . . 82.2(4)
O6 Sm1 O1 C1 3_576 . -116.9(4)
O4 Sm1 O1 C1 . . -151.9(4)
O3 Sm1 O1 C1 . . 115.6(4)
O2 Sm1 O1 C1 . . -8.1(3)
N2 Sm1 O1 C1 . . 20.1(4)
N1 Sm1 O1 C1 . . -51.0(4)
Tb1 Sm1 O1 C1 3_576 . 161.3(4)
Sm1 Sm1 O1 C1 3_576 . 161.3(4)
O1 Sm1 O1 Tb1 3_576 3_576 0.0
O5 Sm1 O1 Tb1 . 3_576 -79.08(17)
O6 Sm1 O1 Tb1 3_576 3_576 81.79(17)
O4 Sm1 O1 Tb1 . 3_576 46.8(4)
O3 Sm1 O1 Tb1 . 3_576 -45.7(3)
O2 Sm1 O1 Tb1 . 3_576 -169.4(2)
N2 Sm1 O1 Tb1 . 3_576 -141.19(18)
N1 Sm1 O1 Tb1 . 3_576 147.71(17)
Sm1 Sm1 O1 Tb1 3_576 3_576 0.0
O1 Sm1 O1 Sm1 3_576 3_576 0.0
O5 Sm1 O1 Sm1 . 3_576 -79.08(17)
O6 Sm1 O1 Sm1 3_576 3_576 81.79(17)
O4 Sm1 O1 Sm1 . 3_576 46.8(4)
O3 Sm1 O1 Sm1 . 3_576 -45.7(3)
O2 Sm1 O1 Sm1 . 3_576 -169.4(2)
N2 Sm1 O1 Sm1 . 3_576 -141.19(18)
N1 Sm1 O1 Sm1 . 3_576 147.71(17)
Tb1 Sm1 O1 Sm1 3_576 3_576 0.0
O1 Sm1 O2 C1 3_576 . -3.8(4)
O5 Sm1 O2 C1 . . -64.8(4)
O6 Sm1 O2 C1 3_576 . 72.6(4)
O4 Sm1 O2 C1 . . 154.9(4)
O3 Sm1 O2 C1 . . -110.2(4)
N2 Sm1 O2 C1 . . -146.5(4)
O1 Sm1 O2 C1 . . 8.4(4)
N1 Sm1 O2 C1 . . 147.3(4)
Tb1 Sm1 O2 C1 3_576 . 2.4(4)
Sm1 Sm1 O2 C1 3_576 . 2.4(4)
O1 Sm1 O3 C13 3_576 . 100.1(4)
O5 Sm1 O3 C13 . . 177.7(5)
O6 Sm1 O3 C13 3_576 . 40.6(5)
O4 Sm1 O3 C13 . . 3.2(4)
O2 Sm1 O3 C13 . . -135.8(4)
N2 Sm1 O3 C13 . . -99.3(5)
O1 Sm1 O3 C13 . . 145.2(4)
N1 Sm1 O3 C13 . . -48.0(5)
Tb1 Sm1 O3 C13 3_576 . 119.9(4)
Sm1 Sm1 O3 C13 3_576 . 119.9(4)
O1 Sm1 O4 C13 3_576 . -77.2(4)
O5 Sm1 O4 C13 . . -9.7(5)
O6 Sm1 O4 C13 3_576 . -154.8(4)
O3 Sm1 O4 C13 . . -3.2(4)
O2 Sm1 O4 C13 . . 120.5(5)
N2 Sm1 O4 C13 . . 65.3(4)
O1 Sm1 O4 C13 . . -121.6(5)
N1 Sm1 O4 C13 . . 128.0(5)
Tb1 Sm1 O4 C13 3_576 . -92.4(4)
Sm1 Sm1 O4 C13 3_576 . -92.4(4)
O1 Sm1 O5 C25 3_576 . -17.5(7)
O6 Sm1 O5 C25 3_576 . 33.1(8)
O4 Sm1 O5 C25 . . -91.0(7)
O3 Sm1 O5 C25 . . -96.3(7)
O2 Sm1 O5 C25 . . 113.2(7)
N2 Sm1 O5 C25 . . -171.1(7)
O1 Sm1 O5 C25 . . 60.1(7)
N1 Sm1 O5 C25 . . 161.0(6)
Tb1 Sm1 O5 C25 3_576 . 22.7(7)
Sm1 Sm1 O5 C25 3_576 . 22.7(7)
Sm1 O2 C1 O1 . . -15.7(7)
Sm1 O2 C1 C2 . . 162.4(6)
Tb1 O1 C1 O2 3_576 . 148.3(7)
Sm1 O1 C1 O2 3_576 . 148.3(7)
Sm1 O1 C1 O2 . . 15.1(6)
Tb1 O1 C1 C2 3_576 . -29.9(13)
Sm1 O1 C1 C2 3_576 . -29.9(13)
Sm1 O1 C1 C2 . . -163.1(5)
O2 C1 C2 C3 . . -3.8(10)
O1 C1 C2 C3 . . 174.5(6)
C1 C2 C3 C4 . . 111.5(8)
C1 C2 C3 C8 . . -70.3(9)
C8 C3 C4 C5 . . 0.9(12)
C2 C3 C4 C5 . . 179.2(7)
C3 C4 C5 C6 . . 0.3(13)
C4 C5 C6 C7 . . -1.8(13)
C5 C6 C7 C12 . . -177.8(8)
C5 C6 C7 C8 . . 1.9(13)
C4 C3 C8 C9 . . 179.4(7)
C2 C3 C8 C9 . . 1.2(11)
C4 C3 C8 C7 . . -0.8(11)
C2 C3 C8 C7 . . -179.0(7)
C12 C7 C8 C9 . . -1.1(12)
C6 C7 C8 C9 . . 179.3(8)
C12 C7 C8 C3 . . 179.1(7)
C6 C7 C8 C3 . . -0.6(11)
C3 C8 C9 C10 . . 179.5(8)
C7 C8 C9 C10 . . -0.3(12)
C8 C9 C10 C11 . . 1.5(14)
C9 C10 C11 C12 . . -1.3(17)
C10 C11 C12 C7 . . -0.2(16)
C6 C7 C12 C11 . . -179.0(9)
C8 C7 C12 C11 . . 1.3(14)
Sm1 O3 C13 O4 . . -5.8(8)
Sm1 O3 C13 C14 . . 173.6(6)
Sm1 O4 C13 O3 . . 5.9(8)
Sm1 O4 C13 C14 . . -173.5(7)
O3 C13 C14 C15 . . -54.3(11)
O4 C13 C14 C15 . . 125.1(9)
C13 C14 C15 C16 . . 107.2(10)
C13 C14 C15 C20 . . -67.9(11)
C20 C15 C16 C17 . . -1.1(13)
C14 C15 C16 C17 . . -176.3(8)
C15 C16 C17 C18 . . 2.5(15)
C16 C17 C18 C19 . . -2.7(17)
C17 C18 C19 C24 . . 178.9(10)
C17 C18 C19 C20 . . 1.6(16)
C16 C15 C20 C21 . . 179.6(8)
C14 C15 C20 C21 . . -5.2(13)
C16 C15 C20 C19 . . 0.0(13)
C14 C15 C20 C19 . . 175.2(8)
C18 C19 C20 C21 . . -179.8(9)
C24 C19 C20 C21 . . 2.8(13)
C18 C19 C20 C15 . . -0.2(14)
C24 C19 C20 C15 . . -177.6(9)
C15 C20 C21 C22 . . 178.5(8)
C19 C20 C21 C22 . . -1.9(13)
C20 C21 C22 C23 . . 0.4(14)
C21 C22 C23 C24 . . 0.2(16)
C22 C23 C24 C19 . . 0.7(17)
C18 C19 C24 C23 . . -179.5(10)
C20 C19 C24 C23 . . -2.2(15)
Sm1 O5 C25 O6 . . -29.9(12)
Sm1 O5 C25 C26 . . 152.5(5)
Tb1 O6 C25 O5 3_576 . 10.3(11)
Sm1 O6 C25 O5 3_576 . 10.3(11)
Tb1 O6 C25 C26 3_576 . -172.1(5)
Sm1 O6 C25 C26 3_576 . -172.1(5)
O5 C25 C26 C27 . . -139.4(7)
O6 C25 C26 C27 . . 42.8(10)
C25 C26 C27 C28 . . -119.9(8)
C25 C26 C27 C32 . . 63.6(10)
C32 C27 C28 C29 . . -1.3(12)
C26 C27 C28 C29 . . -177.9(7)
C27 C28 C29 C30 . . 0.8(13)
C28 C29 C30 C31 . . 1.0(14)
C29 C30 C31 C32 . . -2.2(13)
C29 C30 C31 C36 . . 175.8(8)
C28 C27 C32 C33 . . -178.3(8)
C26 C27 C32 C33 . . -1.8(12)
C28 C27 C32 C31 . . 0.1(11)
C26 C27 C32 C31 . . 176.6(7)
C30 C31 C32 C27 . . 1.6(12)
C36 C31 C32 C27 . . -176.5(8)
C30 C31 C32 C33 . . -180.0(8)
C36 C31 C32 C33 . . 2.0(12)
C27 C32 C33 C34 . . 177.2(8)
C31 C32 C33 C34 . . -1.3(12)
C32 C33 C34 C35 . . -0.6(13)
C33 C34 C35 C36 . . 1.8(15)
C34 C35 C36 C31 . . -1.0(14)
C30 C31 C36 C35 . . -178.9(9)
C32 C31 C36 C35 . . -0.9(13)
C41 N1 C37 C38 . . 0.9(11)
Sm1 N1 C37 C38 . . 178.2(5)
N1 C37 C38 C39 . . -0.7(12)
C37 C38 C39 C40 . . -0.5(12)
C38 C39 C40 C41 . . 1.2(11)
C38 C39 C40 C47 . . -179.0(7)
C37 N1 C41 C40 . . -0.1(10)
Sm1 N1 C41 C40 . . -177.5(5)
C37 N1 C41 C42 . . 178.9(7)
Sm1 N1 C41 C42 . . 1.5(8)
C39 C40 C41 N1 . . -1.0(11)
C47 C40 C41 N1 . . 179.3(7)
C39 C40 C41 C42 . . -179.9(7)
C47 C40 C41 C42 . . 0.3(11)
C46 N2 C42 C43 . . -2.9(11)
Sm1 N2 C42 C43 . . 175.7(6)
C46 N2 C42 C41 . . 178.9(7)
Sm1 N2 C42 C41 . . -2.4(9)
N1 C41 C42 N2 . . 0.5(10)
C40 C41 C42 N2 . . 179.5(7)
N1 C41 C42 C43 . . -177.7(7)
C40 C41 C42 C43 . . 1.3(11)
N2 C42 C43 C44 . . 1.6(12)
C41 C42 C43 C44 . . 179.7(7)
N2 C42 C43 C48 . . 179.5(7)
C41 C42 C43 C48 . . -2.4(11)
C42 C43 C44 C45 . . 0.5(13)
C48 C43 C44 C45 . . -177.2(9)
C43 C44 C45 C46 . . -1.2(14)
C42 N2 C46 C45 . . 2.2(12)
Sm1 N2 C46 C45 . . -176.5(7)
C44 C45 C46 N2 . . -0.2(14)
C39 C40 C47 C48 . . 179.5(8)
C41 C40 C47 C48 . . -0.8(12)
C40 C47 C48 C43 . . -0.4(13)
C44 C43 C48 C47 . . 179.7(9)
C42 C43 C48 C47 . . 2.0(13)
C51 N3 C49 O7 . . 4.7(17)
C50 N3 C49 O7 . . -177.4(10)
