#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325279.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_4325279
loop_
_publ_author_name
'Tereza Peristeraki'
'Marianna Samios'
'Milosz Siczek'
'Tadeusz Lis'
'Constantinos J. Milios'
_publ_contact_author_email       komil@chemistry.uoc.gr
_publ_contact_author_name        'Constantinos Milios'
_publ_section_title
;
 Artificial Amino Acids in Nickel(II) and Nickel(II)/Lanthanide(III)
 Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5175
_journal_page_last               5185
_journal_paper_doi               10.1021/ic2004744
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C48 H96 La N12 Ni6 O24, 3(N O3), 5.5(H2 O)'
_chemical_formula_sum            'C48 H107 La N15 Ni6 O38.5'
_chemical_formula_weight         2001.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.557(5)
_cell_length_b                   17.905(5)
_cell_length_c                   14.130(4)
_cell_measurement_reflns_used    29807
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.88
_cell_volume                     4189(2)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM4 CCD κ-geometry diffractometer'
_diffrn_measurement_method       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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51641
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.909
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       needle
_exptl_crystal_F_000             2066
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.13
_refine_diff_density_min         -1.03
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5256
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0835P)²+3.1252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                4458
_reflns_number_total             5256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2004744_si_001_3.cif
_cod_data_source_block           complex_2
_cod_original_formula_sum        'C48 H107 La N15 Ni6 O38.50'
_cod_database_code               4325279
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
La La 0.5000 0.5000 0.5000 0.02251(11) Uani 1 4 d S . .
Ni1 Ni 0.5000 0.5000 0.23891(3) 0.02740(14) Uani 1 2 d S . .
Ni2 Ni 0.27752(3) 0.51134(3) 0.5000 0.02642(14) Uani 1 2 d S . .
Ni3 Ni 0.5070(4) 0.70694(8) 0.5000 0.0251(3) Uani 0.74(3) 2 d SP . .
Ni31 Ni 0.5243(10) 0.7069(2) 0.5000 0.0197(12) Uiso 0.26(3) 2 d SP . .
O11 O 0.36198(13) 0.50714(10) 0.39613(14) 0.0265(4) Uani 1 1 d . . .
O21 O 0.37592(16) 0.50610(12) 0.23923(16) 0.0394(5) Uani 1 1 d . . .
N11 N 0.19822(18) 0.51419(18) 0.3887(2) 0.0434(6) Uani 1 1 d . . .
H11A H 0.1647 0.4747 0.3923 0.052 Uiso 1 1 calc R . .
H11B H 0.1681 0.5560 0.3923 0.052 Uiso 1 1 calc R . .
C11 C 0.33434(19) 0.50816(14) 0.31211(19) 0.0290(5) Uani 1 1 d . . .
C21 C 0.24185(19) 0.51264(18) 0.2960(2) 0.0361(6) Uani 1 1 d . . .
C31 C 0.2245(2) 0.5841(3) 0.2411(3) 0.0614(11) Uani 1 1 d . . .
H31A H 0.2413 0.6264 0.2778 0.092 Uiso 1 1 calc R . .
H31B H 0.1676 0.5875 0.2286 0.092 Uiso 1 1 calc R . .
H31C H 0.2535 0.5833 0.1824 0.092 Uiso 1 1 calc R . .
C41 C 0.2163(2) 0.4446(3) 0.2401(3) 0.0618(11) Uani 1 1 d . . .
H41A H 0.1590 0.4462 0.2295 0.093 Uiso 1 1 calc R . .
H41B H 0.2297 0.4003 0.2749 0.093 Uiso 1 1 calc R . .
H41C H 0.2439 0.4441 0.1803 0.093 Uiso 1 1 calc R . .
O12 O 0.50471(10) 0.58323(12) 0.33683(14) 0.0281(4) Uani 1 1 d . . .
O22 O 0.51219(15) 0.70721(13) 0.35289(17) 0.0399(5) Uani 1 1 d . . .
N12 N 0.50555(15) 0.5873(2) 0.14610(19) 0.0402(6) Uani 1 1 d . . .
H12A H 0.5496 0.5821 0.1093 0.048 Uiso 1 1 calc R . .
H12B H 0.4618 0.5862 0.1083 0.048 Uiso 1 1 calc R . .
C12 C 0.50836(16) 0.64850(18) 0.3038(2) 0.0311(6) Uani 1 1 d . . .
C22 C 0.50916(18) 0.66006(19) 0.1947(2) 0.0371(7) Uani 1 1 d . . .
C32 C 0.5868(3) 0.7005(3) 0.1682(3) 0.0647(12) Uani 1 1 d . . .
H32A H 0.6324 0.6700 0.1848 0.097 Uiso 1 1 calc R . .
H32B H 0.5897 0.7470 0.2018 0.097 Uiso 1 1 calc R . .
H32C H 0.5874 0.7099 0.1013 0.097 Uiso 1 1 calc R . .
C42 C 0.4348(3) 0.7063(3) 0.1687(3) 0.0661(12) Uani 1 1 d . . .
H42A H 0.3868 0.6794 0.1859 0.099 Uiso 1 1 calc R . .
H42B H 0.4346 0.7156 0.1017 0.099 Uiso 1 1 calc R . .
H42C H 0.4362 0.7530 0.2020 0.099 Uiso 1 1 calc R . .
O13 O 0.59564(17) 0.62454(14) 0.5000 0.0277(5) Uani 1 2 d S . .
O23 O 0.72849(19) 0.60366(16) 0.5000 0.0380(7) Uani 1 2 d S . .
N13 N 0.6118(3) 0.7740(2) 0.5000 0.0676(15) Uani 1 2 d S . .
H13A H 0.6107 0.8035 0.4485 0.081 Uiso 1 1 d R . .
C13 C 0.6684(2) 0.6460(2) 0.5000 0.0305(8) Uani 1 2 d S . .
C23 C 0.6872(3) 0.7304(2) 0.5000 0.0388(9) Uani 1 2 d S . .
C33 C 0.7345(4) 0.7489(3) 0.4124(4) 0.093(2) Uani 1 1 d . . .
H33A H 0.7029 0.7370 0.3575 0.140 Uiso 1 1 calc R . .
H33B H 0.7835 0.7202 0.4116 0.140 Uiso 1 1 calc R . .
H33C H 0.7475 0.8011 0.4122 0.140 Uiso 1 1 calc R . .
O14 O 0.41837(16) 0.63352(14) 0.5000 0.0264(5) Uani 1 2 d S . .
O24 O 0.28386(18) 0.62644(17) 0.5000 0.0383(7) Uani 1 2 d S . .
N14 N 0.4194(3) 0.78427(19) 0.5000 0.0461(9) Uani 1 2 d S . .
H14A H 0.4240 0.8135 0.5515 0.055 Uiso 1 1 d R . .
C14 C 0.3487(2) 0.6624(2) 0.5000 0.0301(8) Uani 1 2 d S . .
C24 C 0.3387(3) 0.7485(2) 0.5000 0.0434(10) Uani 1 2 d S . .
C34 C 0.2948(4) 0.7713(3) 0.4123(4) 0.096(2) Uani 1 1 d . . .
H34A H 0.3247 0.7551 0.3578 0.143 Uiso 1 1 calc R . .
H34B H 0.2894 0.8246 0.4110 0.143 Uiso 1 1 calc R . .
H34C H 0.2422 0.7487 0.4117 0.143 Uiso 1 1 calc R . .
N15 N 0.6734(4) 0.4913(3) 0.0000 0.0542(11) Uiso 0.3333 2 d SP . .
O15 O 0.6493(13) 0.5555(9) 0.0000 0.074(4) Uiso 0.3333 2 d SP A 1
O25 O 0.6190(12) 0.4439(12) 0.0000 0.080(4) Uiso 0.3333 2 d SP A 1
O35 O 0.7461(12) 0.4629(12) 0.0000 0.086(5) Uiso 0.3333 2 d SP A 1
N17 N 0.6734(4) 0.4913(3) 0.0000 0.0542(11) Uiso 0.3333 2 d SP A 2
O17 O 0.6590(14) 0.4211(9) 0.0000 0.078(4) Uiso 0.3333 2 d SP A 2
O27 O 0.6089(10) 0.5274(11) 0.0000 0.067(4) Uiso 0.3333 2 d SP A 2
O37 O 0.7449(9) 0.5183(9) 0.0000 0.061(3) Uiso 0.3333 2 d SP A 2
N18 N 0.6734(4) 0.4913(3) 0.0000 0.0542(11) Uiso 0.3333 2 d SP A 3
O18 O 0.5954(9) 0.4880(9) 0.0000 0.053(3) Uiso 0.3333 2 d SP A 3
O28 O 0.7109(14) 0.4334(11) 0.0000 0.084(5) Uiso 0.3333 2 d SP A 3
O38 O 0.7037(13) 0.5516(10) 0.0000 0.081(4) Uiso 0.3333 2 d SP A 3
N16 N 0.0147(12) 0.3981(16) 0.4513(16) 0.127(10) Uiso 0.25 1 d PD . .
O16 O -0.0025(10) 0.4189(15) 0.3664(14) 0.084(6) Uiso 0.25 1 d PD . .
O26 O 0.0809(13) 0.3860(11) 0.5000 0.080(5) Uiso 0.25 2 d SPD . .
O36 O -0.0505(17) 0.3762(18) 0.5000 0.129(9) Uiso 0.25 2 d SPD . .
O1W O 0.5080(4) 0.8634(5) 0.3212(6) 0.085(2) Uiso 0.50 1 d P . .
O2W O 0.4944(9) 0.9209(16) 0.3771(15) 0.104(7) Uiso 0.25 1 d P . .
O3W O 0.5000 1.0000 0.383(2) 0.104(9) Uiso 0.25 2 d SP . .
O4W O 0.6098(6) 0.9484(6) 0.4720(7) 0.106(5) Uani 0.40 1 d P . .
O5W O 0.620(2) 1.041(2) 0.5000 0.123(13) Uiso 0.20 2 d SP . .
O6W O -0.0032(10) 0.4315(13) 0.3350(17) 0.088(6) Uiso 0.25 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'
Ni Ni 0.3393 1.1124 '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
O11 La O11 65.34(9) 5_666 2_665
O11 La O11 114.66(9) 5_666 6_556
O11 La O11 180.00(5) 2_665 6_556
O11 La O11 180.0 5_666 .
O11 La O11 114.66(9) 2_665 .
O11 La O11 65.34(9) 6_556 .
O11 La O13 116.63(6) 5_666 5_666
O11 La O13 116.63(6) 2_665 5_666
O11 La O13 63.37(6) 6_556 5_666
O11 La O13 63.36(6) . 5_666
O11 La O13 63.37(6) 5_666 .
O11 La O13 63.37(6) 2_665 .
O11 La O13 116.63(6) 6_556 .
O11 La O13 116.64(6) . .
O13 La O13 180.0 5_666 .
O11 La O14 117.04(6) 5_666 .
O11 La O14 117.04(6) 2_665 .
O11 La O14 62.96(6) 6_556 .
O11 La O14 62.96(6) . .
O13 La O14 115.14(9) 5_666 .
O13 La O14 64.86(9) . .
O11 La O14 62.96(6) 5_666 5_666
O11 La O14 62.96(6) 2_665 5_666
O11 La O14 117.04(6) 6_556 5_666
O11 La O14 117.04(6) . 5_666
O13 La O14 64.86(9) 5_666 5_666
O13 La O14 115.14(9) . 5_666
O14 La O14 180.0 . 5_666
O11 La O12 117.05(6) 5_666 .
O11 La O12 63.16(6) 2_665 .
O11 La O12 116.84(6) 6_556 .
O11 La O12 62.95(6) . .
O13 La O12 117.31(5) 5_666 .
O13 La O12 62.69(5) . .
O14 La O12 62.72(5) . .
O14 La O12 117.28(5) 5_666 .
O11 La O12 63.16(6) 5_666 6_556
O11 La O12 117.05(6) 2_665 6_556
O11 La O12 62.95(6) 6_556 6_556
O11 La O12 116.84(6) . 6_556
O13 La O12 117.31(5) 5_666 6_556
O13 La O12 62.69(5) . 6_556
O14 La O12 62.72(5) . 6_556
O14 La O12 117.28(5) 5_666 6_556
O12 La O12 114.17(9) . 6_556
O11 La O12 116.84(6) 5_666 2_665
O11 La O12 62.95(6) 2_665 2_665
O11 La O12 117.05(6) 6_556 2_665
O11 La O12 63.16(6) . 2_665
O13 La O12 62.68(5) 5_666 2_665
O13 La O12 117.32(5) . 2_665
O14 La O12 117.28(5) . 2_665
O14 La O12 62.72(5) 5_666 2_665
O12 La O12 65.83(9) . 2_665
O12 La O12 180.0 6_556 2_665
O11 La O12 62.95(6) 5_666 5_666
O11 La O12 116.84(6) 2_665 5_666
O11 La O12 63.16(6) 6_556 5_666
O11 La O12 117.05(6) . 5_666
O13 La O12 62.68(5) 5_666 5_666
O13 La O12 117.32(5) . 5_666
O14 La O12 117.28(5) . 5_666
O14 La O12 62.72(5) 5_666 5_666
O12 La O12 180.0 . 5_666
O12 La O12 65.83(9) 6_556 5_666
O12 La O12 114.17(9) 2_665 5_666
O12 Ni1 O12 94.33(12) . 2_665
O12 Ni1 N12 82.80(11) . .
O12 Ni1 N12 177.11(11) 2_665 .
O12 Ni1 N12 177.11(11) . 2_665
O12 Ni1 N12 82.79(11) 2_665 2_665
N12 Ni1 N12 100.08(19) . 2_665
O12 Ni1 O21 89.95(8) . 2_665
O12 Ni1 O21 89.88(8) 2_665 2_665
N12 Ni1 O21 89.83(9) . 2_665
N12 Ni1 O21 90.32(10) 2_665 2_665
O12 Ni1 O21 89.88(8) . .
O12 Ni1 O21 89.95(8) 2_665 .
N12 Ni1 O21 90.32(10) . .
N12 Ni1 O21 89.84(9) 2_665 .
O21 Ni1 O21 179.75(13) 2_665 .
O11 Ni2 O11 92.69(12) . 6_556
O11 Ni2 N11 83.54(10) . .
O11 Ni2 N11 176.18(10) 6_556 .
O11 Ni2 N11 176.19(10) . 6_556
O11 Ni2 N11 83.54(10) 6_556 6_556
N11 Ni2 N11 100.23(17) . 6_556
O11 Ni2 O23 89.78(8) . 5_666
O11 Ni2 O23 89.78(8) 6_556 5_666
N11 Ni2 O23 89.65(11) . 5_666
N11 Ni2 O23 89.65(11) 6_556 5_666
O11 Ni2 O24 90.11(8) . .
O11 Ni2 O24 90.11(8) 6_556 .
N11 Ni2 O24 90.45(11) . .
N11 Ni2 O24 90.45(11) 6_556 .
O23 Ni2 O24 179.85(14) 5_666 .
O14 Ni3 N14 85.5(3) . .
O14 Ni3 O22 91.84(15) . 6_556
N14 Ni3 O22 91.60(14) . 6_556
O14 Ni3 O22 91.84(15) . .
N14 Ni3 O22 91.60(14) . .
O22 Ni3 O22 175.3(4) 6_556 .
O14 Ni3 O13 93.00(13) . .
N14 Ni3 O13 178.5(3) . .
O22 Ni3 O13 88.44(15) 6_556 .
O22 Ni3 O13 88.44(15) . .
O14 Ni3 N13 172.8(3) . .
N14 Ni3 N13 101.67(19) . .
O22 Ni3 N13 87.99(17) 6_556 .
O22 Ni3 N13 87.99(17) . .
O13 Ni3 N13 79.8(3) . .
N13 Ni31 O13 91.0(7) . .
N13 Ni31 O22 94.2(3) . 6_556
O13 Ni31 O22 93.6(3) . 6_556
N13 Ni31 O22 94.2(3) . .
O13 Ni31 O22 93.6(3) . .
O22 Ni31 O22 168.9(9) 6_556 .
N13 Ni31 O14 177.2(6) . .
O13 Ni31 O14 91.8(2) . .
O22 Ni31 O14 85.7(4) 6_556 .
O22 Ni31 O14 85.7(4) . .
N13 Ni31 N14 101.8(3) . .
O13 Ni31 N14 167.2(7) . .
O22 Ni31 N14 85.6(4) 6_556 .
O22 Ni31 N14 85.6(4) . .
O14 Ni31 N14 75.4(5) . .
C11 O11 Ni2 115.25(19) . .
C11 O11 La 143.76(19) . .
Ni2 O11 La 100.98(8) . .
C11 O21 Ni1 123.9(2) . .
C21 N11 Ni2 111.2(2) . .
C21 N11 H11A 109.4 . .
Ni2 N11 H11A 109.4 . .
C21 N11 H11B 109.4 . .
Ni2 N11 H11B 109.4 . .
H11A N11 H11B 108.0 . .
O21 C11 O11 125.1(3) . .
O21 C11 C21 115.4(3) . .
O11 C11 C21 119.5(2) . .
N11 C21 C41 109.7(3) . .
N11 C21 C31 109.8(3) . .
C41 C21 C31 110.9(3) . .
N11 C21 C11 110.4(2) . .
C41 C21 C11 108.2(3) . .
C31 C21 C11 107.7(3) . .
C21 C31 H31A 109.5 . .
C21 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C21 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C21 C41 H41A 109.5 . .
C21 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C21 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C12 O12 Ni1 115.44(19) . .
C12 O12 La 144.64(19) . .
Ni1 O12 La 99.92(9) . .
C12 O22 Ni3 123.1(2) . .
C12 O22 Ni31 123.4(2) . .
C22 N12 Ni1 112.26(19) . .
C22 N12 H12A 109.2 . .
Ni1 N12 H12A 109.2 . .
C22 N12 H12B 109.2 . .
Ni1 N12 H12B 109.2 . .
H12A N12 H12B 107.9 . .
O12 C12 O22 124.9(3) . .
O12 C12 C22 119.4(3) . .
O22 C12 C22 115.7(3) . .
N12 C22 C32 109.9(3) . .
N12 C22 C42 109.5(3) . .
C32 C22 C42 111.3(4) . .
N12 C22 C12 110.1(3) . .
C32 C22 C12 108.3(3) . .
C42 C22 C12 107.7(3) . .
C22 C32 H32A 109.5 . .
C22 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C22 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C22 C42 H42A 109.5 . .
C22 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C22 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C13 O13 Ni31 110.9(4) . .
C13 O13 Ni3 117.1(3) . .
C13 O13 La 143.1(2) . .
Ni31 O13 La 105.9(4) . .
Ni3 O13 La 99.78(17) . .
C13 O23 Ni2 124.6(3) . 5_666
C23 N13 Ni31 108.4(4) . .
C23 N13 Ni3 113.4(3) . .
C23 N13 H13A 109.2 . .
Ni31 N13 H13A 111.1 . .
Ni3 N13 H13A 108.5 . .
O23 C13 O13 124.9(4) . .
O23 C13 C23 115.7(4) . .
O13 C13 C23 119.4(3) . .
N13 C23 C33 109.0(3) . 6_556
N13 C23 C33 109.0(3) . .
C33 C23 C33 111.0(6) 6_556 .
N13 C23 C13 110.3(3) . .
C33 C23 C13 108.7(3) 6_556 .
C33 C23 C13 108.7(3) . .
C23 C33 H33A 109.5 . .
C23 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C23 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C14 O14 Ni3 114.1(3) . .
C14 O14 Ni31 119.1(4) . .
C14 O14 La 143.6(2) . .
Ni3 O14 La 102.36(17) . .
Ni31 O14 La 97.4(3) . .
C14 O24 Ni2 123.8(3) . .
C24 N14 Ni3 110.7(3) . .
C24 N14 Ni31 115.8(4) . .
C24 N14 H14A 109.2 . .
Ni3 N14 H14A 109.8 . .
Ni31 N14 H14A 107.2 . .
O24 C14 O14 125.0(4) . .
O24 C14 C24 114.8(3) . .
O14 C14 C24 120.2(4) . .
N14 C24 C34 108.7(3) . 6_556
N14 C24 C34 108.7(3) . .
C34 C24 C34 112.2(6) 6_556 .
N14 C24 C14 109.5(3) . .
C34 C24 C14 108.9(3) 6_556 .
C34 C24 C14 108.9(3) . .
C24 C34 H34A 109.5 . .
C24 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C24 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
O38 N15 O28 124.2(17) . .
O28 N15 O15 168.3(16) . .
O38 N15 O25 158.1(15) . .
O28 N15 O25 77.7(13) . .
O15 N15 O25 114.0(15) . .
O38 N15 O35 88.0(14) . .
O15 N15 O35 132.1(14) . .
O25 N15 O35 113.8(14) . .
O27 N15 O35 171.8(14) . .
O37 N15 O35 45.2(11) . .
O17 N15 O35 77.8(12) . .
O18 N15 O35 154.5(12) . .
O16 N16 O26 136(2) . .
O16 N16 O36 112.7(17) . .
O26 N16 O36 111(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La O11 2.719(2) 5_666
La O11 2.719(2) 2_665
La O11 2.719(2) 6_556
La O11 2.719(2) .
La O13 2.735(3) 5_666
La O13 2.735(3) .
La O14 2.746(3) .
La O14 2.746(3) 5_666
La O12 2.746(2) .
La O12 2.746(2) 6_556
La O12 2.746(2) 2_665
La O12 2.746(2) 5_666
Ni1 O12 2.035(2) .
Ni1 O12 2.035(2) 2_665
Ni1 N12 2.042(3) .
Ni1 N12 2.042(3) 2_665
Ni1 O21 2.057(3) 2_665
Ni1 O21 2.057(3) .
Ni2 O11 2.029(2) .
Ni2 O11 2.029(2) 6_556
Ni2 N11 2.049(3) .
Ni2 N11 2.049(3) 6_556
Ni2 O23 2.062(3) 5_666
Ni2 O24 2.063(3) .
Ni3 O14 1.971(6) .
Ni3 N14 2.006(6) .
Ni3 O22 2.080(2) 6_556
Ni3 O22 2.080(2) .
Ni3 O13 2.081(5) .
Ni3 N13 2.109(7) .
Ni31 N13 1.881(13) .
Ni31 O13 1.889(11) .
Ni31 O22 2.088(3) 6_556
Ni31 O22 2.088(3) .
Ni31 O14 2.192(13) .
Ni31 N14 2.222(13) .
O11 C11 1.272(3) .
O21 C11 1.239(4) .
N11 C21 1.496(4) .
N11 H11A 0.9000 .
N11 H11B 0.9000 .
C11 C21 1.550(4) .
C21 C41 1.513(5) .
C21 C31 1.523(5) .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C41 H41A 0.9600 .
C41 H41B 0.9600 .
C41 H41C 0.9600 .
O12 C12 1.260(4) .
O22 C12 1.261(4) .
N12 C22 1.475(5) .
N12 H12A 0.9000 .
N12 H12B 0.9000 .
C12 C22 1.555(4) .
C22 C32 1.523(5) .
C22 C42 1.530(5) .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C42 H42A 0.9600 .
C42 H42B 0.9600 .
C42 H42C 0.9600 .
O13 C13 1.264(5) .
O23 C13 1.252(5) .
O23 Ni2 2.062(3) 5_666
N13 C23 1.472(6) .
N13 H13A 0.9000 .
C13 C23 1.543(5) .
C23 C33 1.501(5) 6_556
C23 C33 1.501(5) .
C33 H33A 0.9600 .
C33 H33B 0.9600 .
C33 H33C 0.9600 .
O14 C14 1.264(5) .
O24 C14 1.251(5) .
N14 C24 1.482(6) .
N14 H14A 0.9000 .
C14 C24 1.551(6) .
C24 C34 1.493(5) 6_556
C24 C34 1.493(5) .
C34 H34A 0.9600 .
C34 H34B 0.9600 .
C34 H34C 0.9600 .
N15 O38 1.191(18) .
N15 O28 1.208(18) .
N15 O15 1.217(16) .
N15 O25 1.238(17) .
N15 O27 1.248(16) .
N15 O37 1.278(16) .
N15 O17 1.279(17) .
N15 O18 1.293(15) .
N15 O35 1.305(19) .
N16 O16 1.288(17) .
N16 O26 1.313(17) .
N16 O36 1.339(18) .
N16 N16 1.38(5) 6_556
N16 O6W 1.77(3) .
O26 N16 1.313(17) 6_556
O36 N16 1.339(18) 6_556
O1W O2W 1.32(3) .
O2W O3W 1.42(3) .
O3W O2W 1.42(3) 2_675
O4W O4W 0.79(2) 6_556
O4W O5W 1.72(4) .
O5W O4W 1.72(4) 6_556
