#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:40:08 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179591 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/56/4505602.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_4505602
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Lanthanide Ion Complexes with 2-, 3-, or 4-Sulfobenzoate and
 Cucurbit[6]uril
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1632
_journal_paper_doi               10.1021/cg2016808
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C50 H74 La2 N26 O43 S2'
_chemical_formula_weight         2069.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 114.182(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.1305(5)
_cell_length_b                   17.3114(6)
_cell_length_c                   15.8534(5)
_cell_measurement_reflns_used    135165
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.69
_cell_volume                     3788.1(2)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and six ω scans with 2° steps (466 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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            135165
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.872
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         11548
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0385
_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)+(0.0706P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                9045
_reflns_number_total             11548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2016808_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4505602
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
La La 0.906994(9) 0.952550(8) 0.571869(10) 0.02034(6) Uani 1 1 d .
S1 S 0.98425(5) 0.76248(4) 0.49706(5) 0.02562(14) Uani 1 1 d .
O1 O 0.96423(13) 0.93993(10) 0.44261(12) 0.0231(4) Uani 1 1 d .
O2 O 1.00307(14) 0.92999(11) 0.32366(13) 0.0271(4) Uani 1 1 d .
O3 O 0.95352(13) 0.81284(11) 0.55434(13) 0.0268(4) Uani 1 1 d .
O4 O 0.98245(16) 0.68206(12) 0.52206(15) 0.0368(5) Uani 1 1 d .
O5 O 1.07603(13) 0.78606(12) 0.49680(13) 0.0301(4) Uani 1 1 d .
O6 O 0.75528(12) 0.91220(11) 0.43558(12) 0.0255(4) Uani 1 1 d .
O7 O 0.34047(13) 0.79896(12) 0.29663(14) 0.0330(4) Uani 1 1 d .
O8 O 0.80137(13) 0.86713(11) 0.62966(13) 0.0265(4) Uani 1 1 d .
O9 O 0.38567(13) 0.74659(12) 0.51706(15) 0.0349(5) Uani 1 1 d .
O10 O 0.74887(14) 1.01988(12) 0.77584(14) 0.0308(4) Uani 1 1 d .
O11 O 0.34480(13) 0.88982(12) 0.63888(14) 0.0329(4) Uani 1 1 d .
O12 O 1.09547(14) 0.92976(13) 0.68091(15) 0.0337(4) Uani 1 1 d .
O13 O 0.99591(16) 0.91349(13) 0.74674(14) 0.0381(5) Uani 1 1 d .
O14 O 1.1517(2) 0.91704(16) 0.83173(17) 0.0624(8) Uani 1 1 d .
O15 O 0.83461(13) 1.06601(11) 0.47032(13) 0.0269(4) Uani 1 1 d .
H15A H 0.8551 1.1065 0.4627 0.032 Uiso 1 1 d R
H15B H 0.7717 1.0741 0.4301 0.032 Uiso 1 1 d R
O16 O 0.79520(18) 1.02953(13) 0.62529(17) 0.0406(5) Uani 1 1 d .
H16A H 0.7746 1.0229 0.6703 0.049 Uiso 1 1 d R
H16B H 0.7918 1.0742 0.6142 0.049 Uiso 1 1 d R
O17 O 0.79789(15) 1.18974(13) 0.60511(14) 0.0372(5) Uani 1 1 d .
H17A H 0.8239 1.1893 0.5593 0.045 Uiso 1 1 d R
H17B H 0.7380 1.1955 0.5767 0.045 Uiso 1 1 d R
O18 O 0.2862(2) 0.60140(17) 0.4926(2) 0.0644(8) Uani 1 1 d .
H18A H 0.3185 0.6400 0.5158 0.077 Uiso 1 1 d R
H18B H 0.3192 0.5630 0.4817 0.077 Uiso 1 1 d R
O19 O 1.0541(4) 0.9269(6) 0.1558(7) 0.0412(16) Uani 0.50 1 d P
O20 O 1.0129(6) 0.9225(6) 0.1409(8) 0.064(2) Uani 0.50 1 d P
O21 O 0.9978(4) 0.5298(3) 0.5050(4) 0.0462(11) Uani 0.50 1 d P
O22 O 0.4234(6) 0.4910(5) 0.4906(5) 0.0323(17) Uani 0.25 1 d P
O23 O 0.3242(8) 0.4465(5) 0.4971(6) 0.042(2) Uani 0.25 1 d PU
O24 O 1.1902(4) 0.5047(3) 0.5627(4) 0.0587(14) Uani 0.50 1 d P
O25 O 1.1396(4) 0.5826(3) 0.5499(3) 0.0559(13) Uani 0.50 1 d P
O26 O 0.5682(6) 1.0278(6) 0.5319(6) 0.040(2) Uani 0.25 1 d PU
O27 O 0.5962(7) 0.9655(7) 0.5014(7) 0.059(3) Uani 0.25 1 d PU
N1 N 0.61651(15) 0.89653(13) 0.30371(15) 0.0252(4) Uani 1 1 d .
N2 N 0.66695(15) 0.79933(13) 0.40278(15) 0.0247(4) Uani 1 1 d .
N3 N 0.49860(15) 0.75659(14) 0.35019(16) 0.0285(5) Uani 1 1 d .
N4 N 0.44922(15) 0.84765(14) 0.24241(16) 0.0284(5) Uani 1 1 d .
N5 N 0.70461(15) 0.76109(13) 0.56109(16) 0.0259(5) Uani 1 1 d .
N6 N 0.69288(15) 0.81489(13) 0.68325(15) 0.0246(4) Uani 1 1 d .
N7 N 0.53190(15) 0.76104(14) 0.64380(16) 0.0276(5) Uani 1 1 d .
N8 N 0.53303(15) 0.72581(14) 0.50889(16) 0.0276(5) Uani 1 1 d .
N9 N 0.65868(15) 0.91210(14) 0.77444(16) 0.0265(5) Uani 1 1 d .
N10 N 0.61625(16) 1.02542(15) 0.81319(17) 0.0293(5) Uani 1 1 d .
N11 N 0.45010(16) 0.97600(15) 0.74510(16) 0.0277(5) Uani 1 1 d .
N12 N 0.49862(15) 0.85581(14) 0.73892(16) 0.0277(5) Uani 1 1 d .
N13 N 1.08247(19) 0.92086(15) 0.75392(18) 0.0369(6) Uani 1 1 d .
C1 C 0.95614(17) 0.90699(15) 0.36828(16) 0.0225(5) Uani 1 1 d .
C2 C 0.88859(17) 0.83997(16) 0.33116(17) 0.0237(5) Uani 1 1 d .
C3 C 0.89532(18) 0.77235(16) 0.38162(19) 0.0265(5) Uani 1 1 d .
C4 C 0.8333(2) 0.71066(18) 0.3400(2) 0.0347(7) Uani 1 1 d .
H4 H 0.8394 0.6650 0.3728 0.042 Uiso 1 1 calc R
C5 C 0.7633(2) 0.7165(2) 0.2511(2) 0.0426(8) Uani 1 1 d .
H5 H 0.7221 0.6751 0.2242 0.051 Uiso 1 1 calc R
C6 C 0.7545(2) 0.7842(2) 0.2018(2) 0.0386(7) Uani 1 1 d .
H6 H 0.7064 0.7887 0.1422 0.046 Uiso 1 1 calc R
C7 C 0.81719(19) 0.84573(19) 0.24111(19) 0.0315(6) Uani 1 1 d .
H7 H 0.8116 0.8908 0.2073 0.038 Uiso 1 1 calc R
C8 C 0.68536(17) 0.87310(15) 0.38562(18) 0.0228(5) Uani 1 1 d .
C9 C 0.54819(18) 0.83373(16) 0.25635(18) 0.0264(5) Uani 1 1 d .
H9 H 0.5528 0.8186 0.1987 0.032 Uiso 1 1 calc R
C10 C 0.58120(18) 0.76765(16) 0.32860(19) 0.0260(5) Uani 1 1 d .
H10 H 0.5965 0.7206 0.3029 0.031 Uiso 1 1 calc R
C11 C 0.42115(19) 0.80126(16) 0.29788(18) 0.0269(5) Uani 1 1 d .
C12 C 0.72908(18) 0.75537(15) 0.48296(18) 0.0246(5) Uani 1 1 d .
H12A H 0.7265 0.7014 0.4655 0.029 Uiso 1 1 calc R
H12B H 0.7953 0.7728 0.5014 0.029 Uiso 1 1 calc R
C13 C 0.49352(19) 0.69904(17) 0.4146(2) 0.0307(6) Uani 1 1 d .
H13A H 0.4264 0.6844 0.3968 0.037 Uiso 1 1 calc R
H13B H 0.5286 0.6533 0.4106 0.037 Uiso 1 1 calc R
C14 C 0.73818(18) 0.81959(16) 0.62475(18) 0.0251(5) Uani 1 1 d .
C15 C 0.63219(18) 0.71342(16) 0.57490(19) 0.0270(5) Uani 1 1 d .
H15 H 0.6497 0.6586 0.5802 0.032 Uiso 1 1 calc R
C16 C 0.63325(17) 0.74554(16) 0.66662(19) 0.0255(5) Uani 1 1 d .
H16 H 0.6604 0.7083 0.7173 0.031 Uiso 1 1 calc R
C17 C 0.47467(19) 0.74531(16) 0.5519(2) 0.0289(6) Uani 1 1 d .
C18 C 0.72765(17) 0.85596(17) 0.77040(18) 0.0264(5) Uani 1 1 d .
H18C H 0.7416 0.8190 0.8202 0.032 Uiso 1 1 calc R
H18D H 0.7876 0.8821 0.7797 0.032 Uiso 1 1 calc R
C19 C 0.49311(19) 0.77551(17) 0.7107(2) 0.0289(6) Uani 1 1 d .
H19A H 0.5279 0.7441 0.7650 0.035 Uiso 1 1 calc R
H19B H 0.4258 0.7594 0.6853 0.035 Uiso 1 1 calc R
C20 C 0.68127(19) 0.98830(17) 0.78604(18) 0.0276(6) Uani 1 1 d .
C21 C 0.58384(18) 0.89222(17) 0.80725(18) 0.0273(6) Uani 1 1 d .
H21 H 0.6105 0.8627 0.8650 0.033 Uiso 1 1 calc R
C22 C 0.54634(19) 0.97179(18) 0.82059(19) 0.0278(5) Uani 1 1 d .
H22 H 0.5431 0.9757 0.8809 0.033 Uiso 1 1 calc R
C23 C 0.42328(18) 0.90620(17) 0.70045(18) 0.0264(5) Uani 1 1 d .
C24 C 0.61897(19) 1.10673(17) 0.83183(18) 0.0300(6) Uani 1 1 d .
H24A H 0.6838 1.1257 0.8456 0.036 Uiso 1 1 calc R
H24B H 0.6065 1.1144 0.8866 0.036 Uiso 1 1 calc R
C25 C 0.37791(19) 1.03269(17) 0.7414(2) 0.0275(6) Uani 1 1 d .
H25A H 0.3140 1.0104 0.7089 0.033 Uiso 1 1 calc R
H25B H 0.3858 1.0443 0.8039 0.033 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
O15 La O6 70.11(6) . .
O15 La O1 75.60(6) . .
O6 La O1 77.08(6) . .
O15 La O16 68.13(7) . .
O6 La O16 86.25(7) . .
O1 La O16 143.43(7) . .
O15 La O3 137.80(6) . .
O6 La O3 80.79(6) . .
O1 La O3 68.42(6) . .
O16 La O3 140.88(6) . .
O15 La O8 120.30(6) . .
O6 La O8 70.72(6) . .
O1 La O8 134.13(6) . .
O16 La O8 66.07(7) . .
O3 La O8 74.81(6) . .
O15 La O2 76.93(7) . 3_776
O6 La O2 144.10(6) . 3_776
O1 La O2 108.42(6) . 3_776
O16 La O2 68.23(7) . 3_776
O3 La O2 134.80(6) . 3_776
O8 La O2 116.90(6) . 3_776
O15 La O13 141.70(7) . .
O6 La O13 136.54(6) . .
O1 La O13 129.27(6) . .
O16 La O13 84.65(8) . .
O3 La O13 80.04(7) . .
O8 La O13 66.75(6) . .
O2 La O13 67.93(7) 3_776 .
O15 La O12 126.91(6) . .
O6 La O12 149.65(6) . .
O1 La O12 83.33(6) . .
O16 La O12 122.34(8) . .
O3 La O12 70.47(6) . .
O8 La O12 109.42(6) . .
O2 La O12 64.46(7) 3_776 .
O13 La O12 48.25(7) . .
O15 La O1 63.56(6) . 3_776
O6 La O1 122.62(6) . 3_776
O1 La O1 60.48(7) . 3_776
O16 La O1 105.10(6) . 3_776
O3 La O1 113.00(5) . 3_776
O8 La O1 164.64(6) . 3_776
O2 La O1 48.03(5) 3_776 3_776
O13 La O1 100.77(6) . 3_776
O12 La O1 63.61(6) . 3_776
O5 S1 O4 113.35(12) . .
O5 S1 O3 112.45(12) . .
O4 S1 O3 110.82(12) . .
O5 S1 C3 106.96(12) . .
O4 S1 C3 106.37(13) . .
O3 S1 C3 106.37(12) . .
C1 O1 La 148.51(16) . .
C1 O1 La 91.64(14) . 3_776
La O1 La 119.52(7) . 3_776
C1 O2 La 99.03(15) . 3_776
S1 O3 La 143.01(11) . .
C8 O6 La 160.60(18) . .
C14 O8 La 157.48(18) . .
N13 O12 La 94.87(16) . .
N13 O13 La 97.58(16) . .
La O15 H15A 134.3 . .
La O15 H15B 129.0 . .
H15A O15 H15B 96.7 . .
La O16 H16A 133.7 . .
La O16 H16B 115.4 . .
H16A O16 H16B 106.9 . .
H17A O17 H17B 106.4 . .
H18A O18 H18B 114.6 . .
C8 N1 C25 123.6(2) . 3_676
C8 N1 C9 111.8(2) . .
C25 N1 C9 123.1(2) 3_676 .
C8 N2 C12 123.8(2) . .
C8 N2 C10 112.4(2) . .
C12 N2 C10 123.7(2) . .
C11 N3 C10 113.2(2) . .
C11 N3 C13 122.5(2) . .
C10 N3 C13 124.1(2) . .
C11 N4 C24 122.3(2) . 3_676
C11 N4 C9 112.1(2) . .
C24 N4 C9 124.6(2) 3_676 .
C14 N5 C12 122.5(2) . .
C14 N5 C15 112.4(2) . .
C12 N5 C15 124.5(2) . .
C14 N6 C18 122.2(2) . .
C14 N6 C16 111.9(2) . .
C18 N6 C16 122.2(2) . .
C17 N7 C19 123.1(2) . .
C17 N7 C16 111.6(2) . .
C19 N7 C16 124.2(2) . .
C17 N8 C13 121.4(2) . .
C17 N8 C15 111.5(2) . .
C13 N8 C15 124.6(2) . .
C20 N9 C18 120.9(2) . .
C20 N9 C21 111.6(2) . .
C18 N9 C21 122.2(2) . .
C20 N10 C24 123.8(2) . .
C20 N10 C22 111.3(2) . .
C24 N10 C22 124.9(2) . .
C23 N11 C25 121.0(2) . .
C23 N11 C22 111.3(2) . .
C25 N11 C22 123.3(2) . .
C23 N12 C21 112.4(2) . .
C23 N12 C19 122.8(2) . .
C21 N12 C19 124.7(2) . .
O14 N13 O12 122.0(3) . .
O14 N13 O13 119.9(3) . .
O12 N13 O13 118.1(2) . .
O2 C1 O1 121.3(2) . .
O2 C1 C2 118.5(2) . .
O1 C1 C2 120.2(2) . .
C7 C2 C3 119.3(3) . .
C7 C2 C1 117.6(2) . .
C3 C2 C1 123.1(2) . .
C4 C3 C2 119.5(3) . .
C4 C3 S1 119.4(2) . .
C2 C3 S1 121.0(2) . .
C5 C4 C3 121.0(3) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
C4 C5 C6 119.6(3) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
C5 C6 C7 120.3(3) . .
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 . .
C6 C7 C2 120.2(3) . .
C6 C7 H7 119.9 . .
C2 C7 H7 119.9 . .
O6 C8 N1 125.0(2) . .
O6 C8 N2 125.5(2) . .
N1 C8 N2 109.5(2) . .
N4 C9 N1 115.0(2) . .
N4 C9 C10 103.7(2) . .
N1 C9 C10 102.8(2) . .
N4 C9 H9 111.6 . .
N1 C9 H9 111.6 . .
C10 C9 H9 111.6 . .
N3 C10 N2 115.6(2) . .
N3 C10 C9 103.1(2) . .
N2 C10 C9 103.3(2) . .
N3 C10 H10 111.4 . .
N2 C10 H10 111.4 . .
C9 C10 H10 111.4 . .
O7 C11 N3 126.8(3) . .
O7 C11 N4 125.4(3) . .
N3 C11 N4 107.8(2) . .
N5 C12 N2 114.6(2) . .
N5 C12 H12A 108.6 . .
N2 C12 H12A 108.6 . .
N5 C12 H12B 108.6 . .
N2 C12 H12B 108.6 . .
H12A C12 H12B 107.6 . .
N8 C13 N3 113.0(2) . .
N8 C13 H13A 109.0 . .
N3 C13 H13A 109.0 . .
N8 C13 H13B 109.0 . .
N3 C13 H13B 109.0 . .
H13A C13 H13B 107.8 . .
O8 C14 N6 125.9(3) . .
O8 C14 N5 125.4(2) . .
N6 C14 N5 108.6(2) . .
N8 C15 N5 115.3(2) . .
N8 C15 C16 103.5(2) . .
N5 C15 C16 102.6(2) . .
N8 C15 H15 111.6 . .
N5 C15 H15 111.6 . .
C16 C15 H15 111.6 . .
N7 C16 N6 113.9(2) . .
N7 C16 C15 103.2(2) . .
N6 C16 C15 103.4(2) . .
N7 C16 H16 111.9 . .
N6 C16 H16 111.9 . .
C15 C16 H16 111.9 . .
O9 C17 N8 126.6(3) . .
O9 C17 N7 124.6(3) . .
N8 C17 N7 108.8(2) . .
N9 C18 N6 112.7(2) . .
N9 C18 H18C 109.1 . .
N6 C18 H18C 109.1 . .
N9 C18 H18D 109.1 . .
N6 C18 H18D 109.1 . .
H18C C18 H18D 107.8 . .
N7 C19 N12 114.0(2) . .
N7 C19 H19A 108.7 . .
N12 C19 H19A 108.7 . .
N7 C19 H19B 108.7 . .
N12 C19 H19B 108.8 . .
H19A C19 H19B 107.6 . .
O10 C20 N9 126.3(3) . .
O10 C20 N10 124.8(3) . .
N9 C20 N10 108.8(2) . .
N12 C21 N9 114.7(2) . .
N12 C21 C22 103.2(2) . .
N9 C21 C22 102.7(2) . .
N12 C21 H21 111.9 . .
N9 C21 H21 111.9 . .
C22 C21 H21 111.9 . .
N10 C22 N11 114.7(2) . .
N10 C22 C21 103.9(2) . .
N11 C22 C21 103.4(2) . .
N10 C22 H22 111.4 . .
N11 C22 H22 111.4 . .
C21 C22 H22 111.4 . .
O11 C23 N12 124.7(3) . .
O11 C23 N11 126.9(3) . .
N12 C23 N11 108.4(2) . .
N10 C24 N4 114.7(2) . 3_676
N10 C24 H24A 108.6 . .
N4 C24 H24A 108.6 3_676 .
N10 C24 H24B 108.6 . .
N4 C24 H24B 108.6 3_676 .
H24A C24 H24B 107.6 . .
N1 C25 N11 113.6(2) 3_676 .
N1 C25 H25A 108.8 3_676 .
N11 C25 H25A 108.8 . .
N1 C25 H25B 108.8 3_676 .
N11 C25 H25B 108.8 . .
H25A C25 H25B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La O15 2.4909(19) .
La O6 2.5224(18) .
La O1 2.5398(17) .
La O16 2.555(2) .
La O3 2.5657(18) .
La O8 2.6038(17) .
La O2 2.6236(19) 3_776
La O13 2.626(2) .
La O12 2.690(2) .
La O1 2.7713(18) 3_776
S1 O5 1.4489(19) .
S1 O4 1.451(2) .
S1 O3 1.4652(19) .
S1 C3 1.781(3) .
O1 C1 1.269(3) .
O1 La 2.7712(18) 3_776
O2 C1 1.255(3) .
O2 La 2.6235(19) 3_776
O6 C8 1.232(3) .
O7 C11 1.213(3) .
O8 C14 1.240(3) .
O9 C17 1.229(3) .
O10 C20 1.228(3) .
O11 C23 1.222(3) .
O12 N13 1.261(3) .
O13 N13 1.274(3) .
O14 N13 1.251(3) .
O15 H15A 0.7961 .
O15 H15B 0.9145 .
O16 H16A 0.8954 .
O16 H16B 0.7896 .
O17 H17A 0.9575 .
O17 H17B 0.8370 .
O18 H18A 0.8203 .
O18 H18B 0.8905 .
N1 C8 1.352(3) .
N1 C25 1.438(4) 3_676
N1 C9 1.476(3) .
N2 C8 1.358(3) .
N2 C12 1.449(3) .
N2 C10 1.455(3) .
N3 C11 1.365(4) .
N3 C10 1.437(3) .
N3 C13 1.451(4) .
N4 C11 1.380(4) .
N4 C24 1.442(4) 3_676
N4 C9 1.441(3) .
N5 C14 1.372(4) .
N5 C12 1.434(3) .
N5 C15 1.458(3) .
N6 C14 1.363(3) .
N6 C18 1.448(3) .
N6 C16 1.460(3) .
N7 C17 1.383(4) .
N7 C19 1.429(3) .
N7 C16 1.449(3) .
N8 C17 1.361(3) .
N8 C13 1.440(4) .
N8 C15 1.451(3) .
N9 C20 1.356(4) .
N9 C18 1.447(3) .
N9 C21 1.468(3) .
N10 C20 1.383(4) .
N10 C24 1.436(4) .
N10 C22 1.448(4) .
N11 C23 1.375(4) .
N11 C25 1.451(4) .
N11 C22 1.460(3) .
N12 C23 1.365(3) .
N12 C21 1.445(4) .
N12 C19 1.452(4) .
C1 C2 1.498(4) .
C2 C7 1.397(4) .
C2 C3 1.398(4) .
C3 C4 1.396(4) .
C4 C5 1.377(5) .
C4 H4 0.9300 .
C5 C6 1.385(5) .
C5 H5 0.9300 .
C6 C7 1.392(4) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C9 C10 1.550(4) .
C9 H9 0.9800 .
C10 H10 0.9800 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C15 C16 1.551(4) .
C15 H15 0.9800 .
C16 H16 0.9800 .
C18 H18C 0.9700 .
C18 H18D 0.9700 .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C21 C22 1.537(4) .
C21 H21 0.9800 .
C22 H22 0.9800 .
C24 N4 1.442(4) 3_676
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 N1 1.438(4) 3_676
C25 H25A 0.9700 .
C25 H25B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15A O5 0.80 2.10 2.843(3) 155.4 3_776
O15 H15B O11 0.91 1.76 2.665(3) 167.8 3_676
O16 H16A O10 0.90 1.87 2.754(3) 170.4 .
O16 H16B O17 0.79 2.01 2.794(3) 171.5 .
O17 H17A O5 0.96 2.09 2.992(3) 156.3 3_776
O17 H17B O9 0.84 2.11 2.876(3) 152.9 3_676
O18 H18A O9 0.82 2.10 2.873(4) 156.3 .
O18 H18B O22 0.89 1.97 2.832(8) 162.8 .
O18 H18B O23 0.89 2.03 2.738(8) 135.6 .
