#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:57:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179086 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/48/4304899.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_4304899
loop_
_publ_author_name
'Shanmugaperumal Kannan'
'Morgan A. Moody'
'Charles L. Barnes'
'Paul B. Duval'
_publ_section_title
;
Lanthanum(III) and Uranyl(VI) Diglycolamide Complexes: Synthetic Precursors
and Structural Studies Involving Nitrate Complexation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4691
_journal_page_last               4695
_journal_paper_doi               10.1021/ic7025076
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '3(C20 H40 N2 O3)La+, N6O18La-, 4(C2H4Cl2)'
_chemical_formula_sum            'C68 H136 Cl8 La2 N12 O27'
_chemical_formula_weight         2115.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.4936(3)
_cell_length_b                   14.4936(3)
_cell_length_c                   82.795(3)
_cell_measurement_reflns_used    13382
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.5
_cell_volume                     15062.2(7)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       105
_diffrn_reflns_limit_l_min       -106
_diffrn_reflns_number            33839
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6564
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7425
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0373
_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)+(0.0485P)²+14.2641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                5465
_reflns_number_total             7425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7025076-file009.cif
_cod_data_source_block           Kannan27
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4304899
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'
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
La1 La 0.6667 0.3333 0.062268(4) 0.02824(11) Uani 1 3 d S . .
Cl1 Cl 1.14984(19) 0.77639(19) -0.01692(2) 0.0999(6) Uani 1 1 d . . .
O1 O 0.4627(2) 0.2536(2) 0.06206(4) 0.0334(6) Uani 1 1 d . . .
N1 N 0.4037(3) 0.0568(3) 0.09309(4) 0.0328(7) Uani 1 1 d . . .
C1 C 0.3890(3) 0.1662(3) 0.07188(5) 0.0370(10) Uani 1 1 d . . .
H1A H 0.3401 0.1052 0.0650 0.044 Uiso 1 1 calc R . .
H1B H 0.3461 0.1876 0.0786 0.044 Uiso 1 1 calc R . .
La2 La 0.0000 0.0000 0.050022(4) 0.03085(11) Uani 1 3 d S . .
Cl2 Cl 0.9414(2) 0.7952(2) -0.02772(3) 0.1298(9) Uani 1 1 d . . .
O2 O 0.5530(2) 0.1834(2) 0.08096(3) 0.0371(7) Uani 1 1 d . . .
N2 N 0.4549(3) 0.4148(3) 0.02954(4) 0.0369(8) Uani 1 1 d . . .
C2 C 0.4544(3) 0.1362(3) 0.08251(5) 0.0334(9) Uani 1 1 d . . .
Cl3 Cl 0.6667 0.3333 0.16642(7) 0.213(4) Uani 1 3 d S . .
O3 O 0.5863(2) 0.4027(2) 0.04247(3) 0.0371(6) Uani 1 1 d . . .
N3 N 0.1519(3) 0.1927(3) 0.07103(5) 0.0392(9) Uani 1 1 d . . .
C3 C 0.2875(3) 0.0038(3) 0.09604(5) 0.0381(9) Uani 1 1 d . . .
H3A H 0.2580 -0.0743 0.0959 0.046 Uiso 1 1 calc R . .
H3B H 0.2540 0.0216 0.0871 0.046 Uiso 1 1 calc R . .
Cl4 Cl 0.6667 0.3333 0.11516(5) 0.150(2) Uani 1 3 d S . .
O4 O 0.1336(2) 0.0993(3) 0.07410(4) 0.0415(7) Uani 1 1 d . . .
N4 N 0.1871(3) 0.0437(4) 0.02748(5) 0.0470(10) Uani 1 1 d . . .
C4 C 0.2569(4) 0.0347(4) 0.11199(5) 0.0454(11) Uani 1 1 d . . .
H4 H 0.2898 0.0153 0.1210 0.054 Uiso 1 1 calc R . .
O5 O 0.1002(3) 0.2028(3) 0.05949(4) 0.0462(7) Uani 1 1 d . . .
C5 C 0.1354(4) -0.0312(5) 0.11379(7) 0.0675(16) Uani 1 1 d . . .
H5A H 0.1144 -0.0154 0.1242 0.101 Uiso 1 1 calc R . .
H5B H 0.1125 -0.1072 0.1132 0.101 Uiso 1 1 calc R . .
H5C H 0.1016 -0.0131 0.1051 0.101 Uiso 1 1 calc R . .
O6 O 0.2160(3) 0.2698(3) 0.07885(4) 0.0552(9) Uani 1 1 d . . .
C6 C 0.2970(5) 0.1518(4) 0.11288(6) 0.0633(14) Uani 1 1 d . . .
H6A H 0.2653 0.1724 0.1041 0.095 Uiso 1 1 calc R . .
H6B H 0.3747 0.1909 0.1118 0.095 Uiso 1 1 calc R . .
H6C H 0.2773 0.1689 0.1233 0.095 Uiso 1 1 calc R . .
O7 O 0.1971(3) 0.0974(2) 0.04023(4) 0.0484(8) Uani 1 1 d . . .
C7 C 0.4663(4) 0.0257(3) 0.10337(5) 0.0393(10) Uani 1 1 d . . .
H7A H 0.4251 -0.0079 0.1133 0.047 Uiso 1 1 calc R . .
H7B H 0.5327 0.0907 0.1066 0.047 Uiso 1 1 calc R . .
O8 O 0.0962(3) -0.0349(3) 0.02455(4) 0.0469(8) Uani 1 1 d . . .
C8 C 0.4953(4) -0.0507(4) 0.09544(6) 0.0495(12) Uani 1 1 d . . .
H8 H 0.5420 -0.0136 0.0859 0.059 Uiso 1 1 calc R . .
O9 O 0.2636(3) 0.0687(4) 0.01853(5) 0.0788(13) Uani 1 1 d . . .
C9 C 0.5577(5) -0.0790(5) 0.10707(7) 0.0674(16) Uani 1 1 d . . .
H9A H 0.5122 -0.1187 0.1162 0.101 Uiso 1 1 calc R . .
H9B H 0.6197 -0.0136 0.1110 0.101 Uiso 1 1 calc R . .
H9C H 0.5816 -0.1231 0.1015 0.101 Uiso 1 1 calc R . .
C10 C 0.3992(5) -0.1517(5) 0.08943(8) 0.0672(16) Uani 1 1 d . . .
H10A H 0.4228 -0.1973 0.0843 0.101 Uiso 1 1 calc R . .
H10B H 0.3602 -0.1336 0.0816 0.101 Uiso 1 1 calc R . .
H10C H 0.3525 -0.1897 0.0986 0.101 Uiso 1 1 calc R . .
C11 C 0.4090(3) 0.2891(3) 0.05175(6) 0.0428(10) Uani 1 1 d . . .
H11A H 0.3721 0.3183 0.0582 0.051 Uiso 1 1 calc R . .
H11B H 0.3551 0.2288 0.0453 0.051 Uiso 1 1 calc R . .
C12 C 0.4892(4) 0.3738(4) 0.04079(5) 0.0382(11) Uani 1 1 d . . .
C13 C 0.3409(3) 0.3833(3) 0.02771(6) 0.0429(11) Uani 1 1 d . . .
H13A H 0.2972 0.3169 0.0339 0.052 Uiso 1 1 calc R . .
H13B H 0.3210 0.3674 0.0162 0.052 Uiso 1 1 calc R . .
C14 C 0.3135(4) 0.4660(4) 0.03329(6) 0.0523(12) Uani 1 1 d . . .
H14 H 0.3538 0.5309 0.0264 0.063 Uiso 1 1 calc R . .
C15 C 0.3428(5) 0.4980(4) 0.05071(6) 0.0568(13) Uani 1 1 d . . .
H15A H 0.3356 0.5603 0.0531 0.085 Uiso 1 1 calc R . .
H15B H 0.4166 0.5156 0.0526 0.085 Uiso 1 1 calc R . .
H15C H 0.2952 0.4388 0.0578 0.085 Uiso 1 1 calc R . .
C16 C 0.1948(5) 0.4230(5) 0.03064(8) 0.0648(16) Uani 1 1 d . . .
H16A H 0.1771 0.4029 0.0193 0.097 Uiso 1 1 calc R . .
H16B H 0.1772 0.4782 0.0334 0.097 Uiso 1 1 calc R . .
H16C H 0.1537 0.3604 0.0375 0.097 Uiso 1 1 calc R . .
C17 C 0.5320(4) 0.4974(3) 0.01862(5) 0.0435(11) Uani 1 1 d . . .
H17A H 0.5993 0.5414 0.0246 0.052 Uiso 1 1 calc R . .
H17B H 0.5040 0.5446 0.0154 0.052 Uiso 1 1 calc R . .
C18 C 0.5563(8) 0.4549(7) 0.00357(9) 0.122(4) Uani 1 1 d . . .
H18 H 0.6091 0.4365 0.0081 0.147 Uiso 1 1 calc R . .
C19 C 0.4910(8) 0.3642(6) -0.00374(10) 0.131(4) Uani 1 1 d . . .
H19A H 0.4732 0.3047 0.0036 0.197 Uiso 1 1 calc R . .
H19B H 0.5256 0.3567 -0.0134 0.197 Uiso 1 1 calc R . .
H19C H 0.4256 0.3640 -0.0068 0.197 Uiso 1 1 calc R . .
C20 C 0.6305(6) 0.5499(6) -0.00715(7) 0.111(3) Uani 1 1 d . . .
H20A H 0.6553 0.5248 -0.0162 0.166 Uiso 1 1 calc R . .
H20B H 0.6918 0.6013 -0.0008 0.166 Uiso 1 1 calc R . .
H20C H 0.5917 0.5843 -0.0113 0.166 Uiso 1 1 calc R . .
C21 C 1.1209(6) 0.8742(6) -0.01131(9) 0.085(2) Uani 1 1 d . . .
H21A H 1.1562 0.9050 -0.0009 0.102 Uiso 1 1 calc R . .
H21B H 1.1511 0.9318 -0.0195 0.102 Uiso 1 1 calc R . .
C22 C 1.0089(6) 0.8363(6) -0.00972(8) 0.0829(19) Uani 1 1 d . . .
H22A H 0.9990 0.8940 -0.0052 0.100 Uiso 1 1 calc R . .
H22B H 0.9778 0.7761 -0.0020 0.100 Uiso 1 1 calc R . .
C23 C 0.6667 0.3333 0.1462 0.100 Uiso 1 3 d S . .
C24 C 0.6976 0.3924 0.1348 0.100 Uiso 0.33 1 d P . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O3 La1 O3 81.54(11) 2_655 3_665 ?
O3 La1 O3 81.54(11) 2_655 . ?
O3 La1 O3 81.54(11) 3_665 . ?
O3 La1 O2 121.28(9) 2_655 2_655 ?
O3 La1 O2 81.17(10) 3_665 2_655 ?
O3 La1 O2 148.61(9) . 2_655 ?
O3 La1 O2 81.17(10) 2_655 . ?
O3 La1 O2 148.61(9) 3_665 . ?
O3 La1 O2 121.28(10) . . ?
O2 La1 O2 85.73(10) 2_655 . ?
O3 La1 O2 148.61(10) 2_655 3_665 ?
O3 La1 O2 121.28(10) 3_665 3_665 ?
O3 La1 O2 81.17(10) . 3_665 ?
O2 La1 O2 85.73(10) 2_655 3_665 ?
O2 La1 O2 85.73(10) . 3_665 ?
O3 La1 O1 60.99(9) 2_655 2_655 ?
O3 La1 O1 74.49(9) 3_665 2_655 ?
O3 La1 O1 137.65(10) . 2_655 ?
O2 La1 O1 60.35(9) 2_655 2_655 ?
O2 La1 O1 74.23(9) . 2_655 ?
O2 La1 O1 141.18(10) 3_665 2_655 ?
O3 La1 O1 137.65(10) 2_655 3_665 ?
O3 La1 O1 60.99(9) 3_665 3_665 ?
O3 La1 O1 74.49(9) . 3_665 ?
O2 La1 O1 74.23(9) 2_655 3_665 ?
O2 La1 O1 141.18(10) . 3_665 ?
O2 La1 O1 60.35(9) 3_665 3_665 ?
O1 La1 O1 119.995(2) 2_655 3_665 ?
O3 La1 O1 74.49(9) 2_655 . ?
O3 La1 O1 137.65(10) 3_665 . ?
O3 La1 O1 60.99(9) . . ?
O2 La1 O1 141.18(10) 2_655 . ?
O2 La1 O1 60.35(9) . . ?
O2 La1 O1 74.23(9) 3_665 . ?
O1 La1 O1 119.995(2) 2_655 . ?
O1 La1 O1 119.995(2) 3_665 . ?
C11 O1 C1 111.2(3) . . ?
C11 O1 La1 123.8(2) . . ?
C1 O1 La1 125.0(2) . . ?
C2 N1 C7 119.1(3) . . ?
C2 N1 C3 123.2(3) . . ?
C7 N1 C3 117.5(3) . . ?
O1 C1 C2 106.7(3) . . ?
O1 C1 H1A 110.4 . . ?
C2 C1 H1A 110.4 . . ?
O1 C1 H1B 110.4 . . ?
C2 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
O7 La2 O7 110.77(7) 3 . ?
O7 La2 O7 110.77(7) 3 2 ?
O7 La2 O7 110.77(7) . 2 ?
O7 La2 O4 133.24(10) 3 . ?
O7 La2 O4 68.51(10) . . ?
O7 La2 O4 112.61(10) 2 . ?
O7 La2 O4 112.61(10) 3 2 ?
O7 La2 O4 133.24(10) . 2 ?
O7 La2 O4 68.51(10) 2 2 ?
O4 La2 O4 69.48(11) . 2 ?
O7 La2 O4 68.51(10) 3 3 ?
O7 La2 O4 112.61(10) . 3 ?
O7 La2 O4 133.24(10) 2 3 ?
O4 La2 O4 69.48(11) . 3 ?
O4 La2 O4 69.48(11) 2 3 ?
O7 La2 O5 178.72(11) 3 . ?
O7 La2 O5 69.42(10) . . ?
O7 La2 O5 68.07(10) 2 . ?
O4 La2 O5 48.04(10) . . ?
O4 La2 O5 67.60(10) 2 . ?
O4 La2 O5 112.64(10) 3 . ?
O7 La2 O5 68.07(10) 3 2 ?
O7 La2 O5 178.72(11) . 2 ?
O7 La2 O5 69.42(10) 2 2 ?
O4 La2 O5 112.64(10) . 2 ?
O4 La2 O5 48.04(10) 2 2 ?
O4 La2 O5 67.60(10) 3 2 ?
O5 La2 O5 111.72(6) . 2 ?
O7 La2 O5 69.42(10) 3 3 ?
O7 La2 O5 68.07(10) . 3 ?
O7 La2 O5 178.72(11) 2 3 ?
O4 La2 O5 67.60(10) . 3 ?
O4 La2 O5 112.64(10) 2 3 ?
O4 La2 O5 48.04(10) 3 3 ?
O5 La2 O5 111.72(6) . 3 ?
O5 La2 O5 111.72(6) 2 3 ?
O7 La2 O8 48.07(10) 3 3 ?
O7 La2 O8 109.47(11) . 3 ?
O7 La2 O8 66.95(11) 2 3 ?
O4 La2 O8 177.76(11) . 3 ?
O4 La2 O8 112.03(10) 2 3 ?
O4 La2 O8 112.50(10) 3 3 ?
O5 La2 O8 130.65(10) . 3 ?
O5 La2 O8 69.38(10) 2 3 ?
O5 La2 O8 112.78(11) 3 3 ?
O7 La2 O8 109.47(11) 3 2 ?
O7 La2 O8 66.95(11) . 2 ?
O7 La2 O8 48.07(10) 2 2 ?
O4 La2 O8 112.03(10) . 2 ?
O4 La2 O8 112.50(10) 2 2 ?
O4 La2 O8 177.76(10) 3 2 ?
O5 La2 O8 69.38(10) . 2 ?
O5 La2 O8 112.78(11) 2 2 ?
O5 La2 O8 130.65(10) 3 2 ?
O8 La2 O8 65.95(12) 3 2 ?
O7 La2 O8 66.95(11) 3 . ?
O7 La2 O8 48.07(10) . . ?
O7 La2 O8 109.47(11) 2 . ?
O4 La2 O8 112.50(10) . . ?
O4 La2 O8 177.76(10) 2 . ?
O4 La2 O8 112.03(10) 3 . ?
O5 La2 O8 112.78(11) . . ?
O5 La2 O8 130.65(10) 2 . ?
O5 La2 O8 69.38(10) 3 . ?
O8 La2 O8 65.95(12) 3 . ?
O8 La2 O8 65.95(12) 2 . ?
C2 O2 La1 128.2(3) . . ?
C12 N2 C17 119.5(4) . . ?
C12 N2 C13 122.8(4) . . ?
C17 N2 C13 117.6(3) . . ?
O2 C2 N1 121.8(4) . . ?
O2 C2 C1 119.7(4) . . ?
N1 C2 C1 118.4(4) . . ?
C12 O3 La1 127.4(3) . . ?
O6 N3 O5 121.2(4) . . ?
O6 N3 O4 121.8(4) . . ?
O5 N3 O4 117.0(4) . . ?
N1 C3 C4 114.3(3) . . ?
N1 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C24 Cl4 C24 42.12(10) 3_665 . ?
C24 Cl4 C24 42.12(10) 3_665 2_655 ?
C24 Cl4 C24 42.12(10) . 2_655 ?
N3 O4 La2 97.8(2) . . ?
O9 N4 O8 122.2(4) . . ?
O9 N4 O7 120.6(4) . . ?
O8 N4 O7 117.2(4) . . ?
C6 C4 C3 111.7(4) . . ?
C6 C4 C5 112.1(4) . . ?
C3 C4 C5 108.2(4) . . ?
C6 C4 H4 108.3 . . ?
C3 C4 H4 108.3 . . ?
C5 C4 H4 108.3 . . ?
N3 O5 La2 97.0(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 O7 La2 99.7(3) . . ?
N1 C7 C8 114.3(4) . . ?
N1 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N4 O8 La2 94.9(2) . . ?
C9 C8 C10 109.4(5) . . ?
C9 C8 C7 110.1(4) . . ?
C10 C8 C7 113.1(4) . . ?
C9 C8 H8 108.0 . . ?
C10 C8 H8 108.0 . . ?
C7 C8 H8 108.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C12 108.7(3) . . ?
O1 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O1 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
O3 C12 N2 122.3(4) . . ?
O3 C12 C11 119.0(4) . . ?
N2 C12 C11 118.7(4) . . ?
N2 C13 C14 114.8(4) . . ?
N2 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
N2 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C15 C14 C13 113.0(4) . . ?
C15 C14 C16 110.5(5) . . ?
C13 C14 C16 108.8(4) . . ?
C15 C14 H14 108.1 . . ?
C13 C14 H14 108.1 . . ?
C16 C14 H14 108.1 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 C18 114.4(4) . . ?
N2 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N2 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C19 C18 C17 126.0(7) . . ?
C19 C18 C20 117.4(7) . . ?
C17 C18 C20 108.3(6) . . ?
C19 C18 H18 99.7 . . ?
C17 C18 H18 99.7 . . ?
C20 C18 H18 99.7 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 Cl1 113.7(5) . . ?
C22 C21 H21A 108.8 . . ?
Cl1 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
Cl1 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 Cl2 113.1(5) . . ?
C21 C22 H22A 109.0 . . ?
Cl2 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
Cl2 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C24 64.7 3_665 . ?
C24 C23 C24 64.7 3_665 2_655 ?
C24 C23 C24 64.7 . 2_655 ?
C24 C23 Cl3 141.840(1) 3_665 . ?
C24 C23 Cl3 141.840(1) . . ?
C24 C23 Cl3 141.840(1) 2_655 . ?
C23 C24 C24 57.7 . 2_655 ?
C23 C24 C24 57.7 . 3_665 ?
C24 C24 C24 60.0 2_655 3_665 ?
C23 C24 Cl4 117.33(6) . . ?
C24 C24 Cl4 68.94(5) 2_655 . ?
C24 C24 Cl4 68.94(5) 3_665 . ?
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
La1 O3 2.496(3) 2_655 ?
La1 O3 2.496(3) 3_665 ?
La1 O3 2.496(3) . ?
La1 O2 2.501(3) 2_655 ?
La1 O2 2.501(3) . ?
La1 O2 2.501(3) 3_665 ?
La1 O1 2.580(3) 2_655 ?
La1 O1 2.580(3) 3_665 ?
La1 O1 2.580(3) . ?
Cl1 C21 1.730(8) . ?
O1 C11 1.413(5) . ?
O1 C1 1.433(5) . ?
N1 C2 1.336(5) . ?
N1 C7 1.469(5) . ?
N1 C3 1.481(5) . ?
C1 C2 1.509(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
La2 O7 2.603(3) 3 ?
La2 O7 2.603(3) . ?
La2 O7 2.603(3) 2 ?
La2 O4 2.647(3) . ?
La2 O4 2.647(3) 2 ?
La2 O4 2.647(3) 3 ?
La2 O5 2.663(3) . ?
La2 O5 2.663(3) 2 ?
La2 O5 2.663(3) 3 ?
La2 O8 2.711(3) 3 ?
La2 O8 2.711(3) 2 ?
La2 O8 2.711(3) . ?
Cl2 C22 1.718(7) . ?
O2 C2 1.244(5) . ?
N2 C12 1.328(5) . ?
N2 C17 1.471(6) . ?
N2 C13 1.485(6) . ?
Cl3 C23 1.674(5) . ?
O3 C12 1.258(5) . ?
N3 O6 1.222(5) . ?
N3 O5 1.267(5) . ?
N3 O4 1.267(5) . ?
C3 C4 1.530(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
Cl4 C24 1.787(4) 3_665 ?
Cl4 C24 1.787(4) . ?
Cl4 C24 1.787(4) 2_655 ?
N4 O9 1.227(5) . ?
N4 O8 1.261(5) . ?
N4 O7 1.276(5) . ?
C4 C6 1.495(7) . ?
C4 C5 1.534(7) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.516(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.512(7) . ?
C8 C10 1.514(8) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.502(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C13 C14 1.511(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.510(7) . ?
C14 C16 1.524(7) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.508(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.321(10) . ?
C18 C20 1.536(10) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.436(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.2004 3_665 ?
C23 C24 1.2004 . ?
C23 C24 1.2004 2_655 ?
C24 C24 1.2846 2_655 ?
C24 C24 1.2846 3_665 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 La1 O1 C11 -91.0(3) 2_655 . . . ?
O3 La1 O1 C11 -33.0(4) 3_665 . . . ?
O3 La1 O1 C11 -2.2(3) . . . . ?
O2 La1 O1 C11 148.1(3) 2_655 . . . ?
O2 La1 O1 C11 -180(53) . . . . ?
O2 La1 O1 C11 86.4(3) 3_665 . . . ?
O1 La1 O1 C11 -133.1(3) 2_655 . . . ?
O1 La1 O1 C11 45.5(4) 3_665 . . . ?
O3 La1 O1 C1 87.1(3) 2_655 . . . ?
O3 La1 O1 C1 145.0(3) 3_665 . . . ?
O3 La1 O1 C1 175.9(3) . . . . ?
O2 La1 O1 C1 -33.9(4) 2_655 . . . ?
O2 La1 O1 C1 -1.5(3) . . . . ?
O2 La1 O1 C1 -95.6(3) 3_665 . . . ?
O1 La1 O1 C1 44.9(4) 2_655 . . . ?
O1 La1 O1 C1 -136.4(3) 3_665 . . . ?
C11 O1 C1 C2 -179.1(3) . . . . ?
La1 O1 C1 C2 2.7(5) . . . . ?
O3 La1 O2 C2 -77.5(3) 2_655 . . . ?
O3 La1 O2 C2 -134.8(3) 3_665 . . . ?
O3 La1 O2 C2 -3.1(4) . . . . ?
O2 La1 O2 C2 159.9(3) 2_655 . . . ?
O2 La1 O2 C2 73.9(4) 3_665 . . . ?
O1 La1 O2 C2 -139.7(3) 2_655 . . . ?
O1 La1 O2 C2 101.7(3) 3_665 . . . ?
O1 La1 O2 C2 -0.4(3) . . . . ?
La1 O2 C2 N1 -179.9(3) . . . . ?
La1 O2 C2 C1 2.0(5) . . . . ?
C7 N1 C2 O2 1.1(6) . . . . ?
C3 N1 C2 O2 175.7(4) . . . . ?
C7 N1 C2 C1 179.2(4) . . . . ?
C3 N1 C2 C1 -6.2(6) . . . . ?
O1 C1 C2 O2 -2.8(5) . . . . ?
O1 C1 C2 N1 179.0(3) . . . . ?
O3 La1 O3 C12 77.5(4) 2_655 . . . ?
O3 La1 O3 C12 160.1(3) 3_665 . . . ?
O2 La1 O3 C12 -142.7(3) 2_655 . . . ?
O2 La1 O3 C12 3.3(4) . . . . ?
O2 La1 O3 C12 -76.2(4) 3_665 . . . ?
O1 La1 O3 C12 104.5(4) 2_655 . . . ?
O1 La1 O3 C12 -137.7(4) 3_665 . . . ?
O1 La1 O3 C12 0.6(3) . . . . ?
C2 N1 C3 C4 -105.5(5) . . . . ?
C7 N1 C3 C4 69.2(5) . . . . ?
O6 N3 O4 La2 -176.3(3) . . . . ?
O5 N3 O4 La2 4.1(4) . . . . ?
O7 La2 O4 N3 177.6(2) 3 . . . ?
O7 La2 O4 N3 78.8(2) . . . . ?
O7 La2 O4 N3 -25.6(3) 2 . . . ?
O4 La2 O4 N3 -80.2(3) 2 . . . ?
O4 La2 O4 N3 -155.1(3) 3 . . . ?
O5 La2 O4 N3 -2.3(2) . . . . ?
O5 La2 O4 N3 -101.8(2) 2 . . . ?
O5 La2 O4 N3 153.1(3) 3 . . . ?
O8 La2 O4 N3 53(3) 3 . . . ?
O8 La2 O4 N3 26.7(3) 2 . . . ?
O8 La2 O4 N3 98.7(2) . . . . ?
N1 C3 C4 C6 59.6(5) . . . . ?
N1 C3 C4 C5 -176.6(4) . . . . ?
O6 N3 O5 La2 176.3(3) . . . . ?
O4 N3 O5 La2 -4.0(4) . . . . ?
O7 La2 O5 N3 -176(85) 3 . . . ?
O7 La2 O5 N3 -76.8(3) . . . . ?
O7 La2 O5 N3 159.2(3) 2 . . . ?
O4 La2 O5 N3 2.3(2) . . . . ?
O4 La2 O5 N3 84.3(2) 2 . . . ?
O4 La2 O5 N3 29.9(3) 3 . . . ?
O5 La2 O5 N3 103.8(2) 2 . . . ?
O5 La2 O5 N3 -22.2(3) 3 . . . ?
O8 La2 O5 N3 -175.3(2) 3 . . . ?
O8 La2 O5 N3 -149.0(3) 2 . . . ?
O8 La2 O5 N3 -98.1(2) . . . . ?
O9 N4 O7 La2 176.0(4) . . . . ?
O8 N4 O7 La2 -3.9(4) . . . . ?
O7 La2 O7 N4 27.5(3) 3 . . . ?
O7 La2 O7 N4 -95.8(2) 2 . . . ?
O4 La2 O7 N4 157.2(3) . . . . ?
O4 La2 O7 N4 -175.4(2) 2 . . . ?
O4 La2 O7 N4 102.1(3) 3 . . . ?
O5 La2 O7 N4 -151.1(3) . . . . ?
O5 La2 O7 N4 3(6) 2 . . . ?
O5 La2 O7 N4 83.6(3) 3 . . . ?
O8 La2 O7 N4 -23.9(3) 3 . . . ?
O8 La2 O7 N4 -75.6(3) 2 . . . ?
O8 La2 O7 N4 2.1(2) . . . . ?
C2 N1 C7 C8 -83.5(5) . . . . ?
C3 N1 C7 C8 101.5(4) . . . . ?
O9 N4 O8 La2 -176.1(4) . . . . ?
O7 N4 O8 La2 3.7(4) . . . . ?
O7 La2 O8 N4 -156.3(3) 3 . . . ?
O7 La2 O8 N4 -2.1(2) . . . . ?
O7 La2 O8 N4 98.7(3) 2 . . . ?
O4 La2 O8 N4 -27.3(3) . . . . ?
O4 La2 O8 N4 125(3) 2 . . . ?
O4 La2 O8 N4 -103.3(3) 3 . . . ?
O5 La2 O8 N4 25.0(3) . . . . ?
O5 La2 O8 N4 177.9(2) 2 . . . ?
O5 La2 O8 N4 -80.7(3) 3 . . . ?
O8 La2 O8 N4 150.9(3) 3 . . . ?
O8 La2 O8 N4 77.7(3) 2 . . . ?
N1 C7 C8 C9 -179.1(4) . . . . ?
N1 C7 C8 C10 -56.3(5) . . . . ?
C1 O1 C11 C12 -175.1(4) . . . . ?
La1 O1 C11 C12 3.2(5) . . . . ?
La1 O3 C12 N2 -178.4(3) . . . . ?
La1 O3 C12 C11 0.8(6) . . . . ?
C17 N2 C12 O3 -0.4(7) . . . . ?
C13 N2 C12 O3 -178.4(4) . . . . ?
C17 N2 C12 C11 -179.7(4) . . . . ?
C13 N2 C12 C11 2.4(6) . . . . ?
O1 C11 C12 O3 -2.5(6) . . . . ?
O1 C11 C12 N2 176.8(4) . . . . ?
C12 N2 C13 C14 106.7(5) . . . . ?
C17 N2 C13 C14 -71.3(5) . . . . ?
N2 C13 C14 C15 -57.1(6) . . . . ?
N2 C13 C14 C16 179.8(4) . . . . ?
C12 N2 C17 C18 88.4(7) . . . . ?
C13 N2 C17 C18 -93.6(7) . . . . ?
N2 C17 C18 C19 28.7(15) . . . . ?
N2 C17 C18 C20 175.6(6) . . . . ?
Cl1 C21 C22 Cl2 -65.8(7) . . . . ?
C24 C23 C24 C24 72.6 3_665 . . 2_655 ?
Cl3 C23 C24 C24 -143.7 . . . 2_655 ?
C24 C23 C24 C24 -72.6 2_655 . . 3_665 ?
Cl3 C23 C24 C24 143.7 . . . 3_665 ?
C24 C23 C24 Cl4 36.3 3_665 . . . ?
C24 C23 C24 Cl4 -36.3 2_655 . . . ?
Cl3 C23 C24 Cl4 180.0 . . . . ?
C24 Cl4 C24 C23 -32.397(12) 3_665 . . . ?
C24 Cl4 C24 C23 32.397(12) 2_655 . . . ?
C24 Cl4 C24 C24 -64.79(2) 3_665 . . 2_655 ?
C24 Cl4 C24 C24 64.79(2) 2_655 . . 3_665 ?
