#------------------------------------------------------------------------------
#$Date: 2019-11-23 15:58:00 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233914 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/93/4349385.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_4349385
loop_
_publ_author_name
'McLauchlan, Craig C.'
'Florián, Jan'
'Kissel, Daniel S.'
'Herlinger, Albert W.'
_publ_section_title
;
 Metal Ion Complexes of
 N,N'-Bis(2-Pyridylmethyl)-trans-1,2-Diaminocyclohexane-N,N'-Diacetic
 Acid, H₂bpcd: Lanthanide(III)-bpcd²⁻ Cationic
 Complexes.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3556
_journal_page_last               3567
_journal_paper_doi               10.1021/acs.inorgchem.6b03137
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety
;
C44 H56 La1.22 N8 O10, Na2.34, 2 H2 O, 2 P F6
;
_chemical_formula_sum            'C44 H60 F12 La1.22 N8 Na2.34 O12 P2'
_chemical_formula_weight         1406.20
_chemical_melting_point          ...3
_chemical_name_systematic
;
N,N'-bis(2-pyridylmethyl)-trans-1,2-diaminocyclohexane-N,N'-diacetato-
lanthanum(III) hexafluorophosphate hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.619(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3362(4)
_cell_length_b                   17.7054(6)
_cell_length_c                   15.0548(5)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.975
_cell_measurement_theta_min      2.238
_cell_volume                     2828.12(17)
_computing_cell_refinement       'SAINT v8.18C (Bruker AXS Inc.)'
_computing_data_collection       'Bruker Instrument Service v2011.12.3.0'
_computing_data_reduction        'SAINT v8.18C (Bruker AXS Inc.)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'EnCIFer 1.4 (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2010)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS'
_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  0.0504
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            105684
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.584
_diffrn_reflns_theta_min         1.847
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             1419
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.863
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8668
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      1.330
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          2.394
_refine_ls_shift/su_mean         0.075
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0667P)²+6.0852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6949
_reflns_number_total             8668
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b03137_si_002.cif
_cod_data_source_block           ccmisu209_0m_pl2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349385
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9895(3) 0.3035(2) 0.5910(2) 0.0291(7) Uani 1 1 d . . . . .
H1 H 0.9049 0.3208 0.5722 0.035 Uiso 1 1 calc R U . . .
C2 C 1.0113(4) 0.2316(2) 0.5650(3) 0.0322(7) Uani 1 1 d . . . . .
H2 H 0.9433 0.2004 0.5285 0.039 Uiso 1 1 calc R U . . .
C3 C 1.1349(4) 0.2058(2) 0.5936(3) 0.0358(8) Uani 1 1 d . . . . .
H3 H 1.1530 0.1563 0.5776 0.043 Uiso 1 1 calc R U . . .
C4 C 1.2315(4) 0.2536(2) 0.6457(3) 0.0321(7) Uani 1 1 d . . . . .
H4 H 1.3167 0.2372 0.6663 0.038 Uiso 1 1 calc R U . . .
C5 C 1.2021(3) 0.32603(19) 0.6676(2) 0.0271(6) Uani 1 1 d . . . . .
C6 C 1.3045(3) 0.38128(19) 0.7198(2) 0.0279(7) Uani 1 1 d . . . . .
H6A H 1.3196 0.3793 0.7886 0.034 Uiso 1 1 calc R U . . .
H6B H 1.3839 0.3677 0.7102 0.034 Uiso 1 1 calc R U . . .
C7 C 1.2522(3) 0.46385(19) 0.5821(2) 0.0244(6) Uani 1 1 d . . . . .
H7A H 1.2296 0.4136 0.5519 0.029 Uiso 1 1 calc R U . . .
H7B H 1.3336 0.4792 0.5772 0.029 Uiso 1 1 calc R U . . .
C8 C 1.1513(3) 0.52066(19) 0.5303(2) 0.0238(6) Uani 1 1 d . . . . .
C9 C 1.3569(3) 0.5202(2) 0.7352(2) 0.0281(6) Uani 1 1 d . . . . .
H9 H 1.3428 0.5642 0.6911 0.034 Uiso 1 1 calc R U . . .
C10 C 1.4950(3) 0.4964(2) 0.7618(3) 0.0317(7) Uani 1 1 d . . . . .
H10A H 1.5113 0.4519 0.8042 0.038 Uiso 1 1 calc R U . . .
H10B H 1.5108 0.4815 0.7036 0.038 Uiso 1 1 calc R U . . .
C11 C 1.5861(4) 0.5598(2) 0.8116(3) 0.0381(8) Uani 1 1 d . . . . .
H11A H 1.6742 0.5420 0.8288 0.046 Uiso 1 1 calc R U . . .
H11B H 1.5740 0.6036 0.7685 0.046 Uiso 1 1 calc R U . . .
C12 C 1.5612(4) 0.5830(3) 0.9001(3) 0.0409(9) Uani 1 1 d . . . . .
H12A H 1.6192 0.6244 0.9325 0.049 Uiso 1 1 calc R U . . .
H12B H 1.5769 0.5397 0.9443 0.049 Uiso 1 1 calc R U . . .
C13 C 1.4247(4) 0.6094(2) 0.8740(3) 0.0357(8) Uani 1 1 d . . . . .
H13A H 1.4106 0.6543 0.8323 0.043 Uiso 1 1 calc R U . . .
H13B H 1.4093 0.6244 0.9323 0.043 Uiso 1 1 calc R U . . .
C14 C 1.3313(3) 0.5471(2) 0.8229(2) 0.0298(7) Uani 1 1 d . . . . .
H14 H 1.3460 0.5033 0.8674 0.036 Uiso 1 1 calc R U . . .
C21 C 1.1645(4) 0.5661(2) 0.8852(2) 0.0304(7) Uani 1 1 d . . . . .
H21A H 1.0857 0.5943 0.8763 0.037 Uiso 1 1 calc R U . . .
H21B H 1.2329 0.5896 0.9385 0.037 Uiso 1 1 calc R U . . .
C22 C 1.1481(3) 0.4844(2) 0.9093(2) 0.0287(7) Uani 1 1 d . . . . .
C20 C 1.1697(4) 0.6480(2) 0.7580(3) 0.0319(7) Uani 1 1 d . . . . .
H20A H 1.2110 0.6547 0.7104 0.038 Uiso 1 1 calc R U . . .
H20B H 1.2067 0.6853 0.8093 0.038 Uiso 1 1 calc R U . . .
C19 C 1.0308(4) 0.6632(2) 0.7118(2) 0.0316(7) Uani 1 1 d . . . . .
C18 C 0.9898(5) 0.7370(2) 0.6875(3) 0.0395(9) Uani 1 1 d . . . . .
H18 H 1.0482 0.7776 0.7013 0.047 Uiso 1 1 calc R U . . .
C17 C 0.8633(5) 0.7497(3) 0.6434(3) 0.0467(11) Uani 1 1 d . . . . .
H17 H 0.8333 0.7994 0.6245 0.056 Uiso 1 1 calc R U . . .
C16 C 0.7791(4) 0.6899(3) 0.6263(3) 0.0481(11) Uani 1 1 d . . . . .
H16 H 0.6910 0.6981 0.5972 0.058 Uiso 1 1 calc R U . . .
C15 C 0.8268(4) 0.6179(3) 0.6526(3) 0.0402(9) Uani 1 1 d . . . . .
H15 H 0.7698 0.5767 0.6408 0.048 Uiso 1 1 calc R U . . .
La1 La 1.04322(3) 0.47857(2) 0.68813(2) 0.02366(10) Uani 0.61 1 d . . P A .
N1 N 1.0823(3) 0.35022(16) 0.64154(19) 0.0252(5) Uani 1 1 d . . . . .
N2 N 1.2655(3) 0.45873(16) 0.68330(19) 0.0243(5) Uani 1 1 d . . . . .
N4 N 1.1951(3) 0.57116(16) 0.7977(2) 0.0266(5) Uani 1 1 d . . . . .
N3 N 0.9507(3) 0.60444(18) 0.6940(2) 0.0313(6) Uani 1 1 d . . . . .
O1 O 1.0851(2) 0.54895(14) 0.57335(15) 0.0247(4) Uani 1 1 d . . . . .
O2 O 1.1371(2) 0.53405(15) 0.44489(16) 0.0283(5) Uani 1 1 d . . . . .
O3 O 1.1284(2) 0.43700(14) 0.84156(16) 0.0289(5) Uani 1 1 d . . . . .
O4 O 1.1496(3) 0.46901(17) 0.98997(18) 0.0390(6) Uani 1 1 d D . . . .
O5 O 0.8770(3) 0.43437(18) 0.73023(18) 0.0349(6) Uani 1 1 d D . . . .
H5A H 0.877(5) 0.421(3) 0.783(2) 0.052 Uiso 1 1 d D U . . .
H5B H 0.809(3) 0.419(3) 0.690(3) 0.052 Uiso 1 1 d D U . . .
O6 O 0.8824(5) 0.4107(2) 0.9065(3) 0.0693(12) Uani 1 1 d D . . . .
H6C H 0.854(5) 0.449(3) 0.925(5) 0.104 Uiso 1 1 d D U . . .
H6D H 0.965(2) 0.419(3) 0.931(5) 0.104 Uiso 1 1 d D U . . .
P1 P 0.61018(14) 0.24874(9) 0.41118(12) 0.0454(4) Uani 0.720(2) 1 d D U P A 1
F1 F 0.6346(5) 0.1601(3) 0.4080(3) 0.0777(15) Uani 0.720(2) 1 d D U P A 1
F2 F 0.6904(5) 0.2457(3) 0.5204(3) 0.0644(12) Uani 0.720(2) 1 d D U P A 1
F3 F 0.5860(8) 0.3354(3) 0.4121(5) 0.109(2) Uani 0.720(2) 1 d D U P A 1
F4 F 0.7364(5) 0.2617(4) 0.3870(4) 0.109(2) Uani 0.720(2) 1 d D U P A 1
F5 F 0.5335(6) 0.2508(3) 0.3033(4) 0.121(3) Uani 0.720(2) 1 d D U P A 1
F6 F 0.4866(5) 0.2253(4) 0.4266(7) 0.116(2) Uani 0.720(2) 1 d D U P A 1
Na1 Na 0.6425(7) 0.3760(6) 0.6336(7) 0.147(2) Uani 0.5762(18) 1 d . U P A 1
Na2 Na 0.5256(14) 0.3082(10) 0.6455(13) 0.133(3) Uani 0.2881(9) 1 d . U P A 1
Na3 Na 0.4930(17) 0.4470(12) 0.4798(14) 0.158(5) Uani 0.2881(9) 1 d . U P A 1
P1B P 0.659(15) 0.268(10) 0.711(12) 0.111(4) Uani 0.012(2) 1 d D U P B 2
F1B F 0.57(2) 0.341(13) 0.69(2) 0.106(6) Uani 0.012(2) 1 d D U P B 2
F2B F 0.77(2) 0.327(16) 0.71(2) 0.091(6) Uani 0.012(2) 1 d D U P B 2
F3B F 0.75(2) 0.197(13) 0.74(2) 0.094(8) Uani 0.012(2) 1 d D U P B 2
F4B F 0.68(3) 0.287(19) 0.832(15) 0.130(8) Uani 0.012(2) 1 d D U P B 2
F5B F 0.55(2) 0.212(17) 0.71(2) 0.119(9) Uani 0.012(2) 1 d D U P B 2
F6B F 0.62(3) 0.251(16) 0.599(14) 0.091(5) Uani 0.012(2) 1 d D U P B 2
P1C P 0.5876(5) 0.3349(4) 0.5105(5) 0.0753(16) Uani 0.268(2) 1 d D U P C 3
F1C F 0.4832(13) 0.3878(8) 0.4446(11) 0.089(4) Uani 0.268(2) 1 d D U P C 3
F2C F 0.6744(11) 0.3550(7) 0.4485(8) 0.070(3) Uani 0.268(2) 1 d D U P C 3
F3C F 0.6949(13) 0.2885(10) 0.5784(13) 0.106(4) Uani 0.268(2) 1 d D U P C 3
F4C F 0.6286(9) 0.4174(7) 0.5888(7) 0.063(3) Uani 0.268(2) 1 d D U P C 3
F5C F 0.4986(14) 0.3100(11) 0.5646(12) 0.111(4) Uani 0.268(2) 1 d D U P C 3
F6C F 0.5285(12) 0.2671(7) 0.4493(12) 0.084(3) Uani 0.268(2) 1 d D U P C 3
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'
F F 0.0171 0.0103 '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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
N1 C1 C2 123.1(3) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C1 C2 C3 118.5(3) . .
C1 C2 H2 120.7 . .
C3 C2 H2 120.7 . .
C4 C3 C2 118.8(3) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
C3 C4 C5 119.2(3) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
N1 C5 C4 121.7(3) . .
N1 C5 C6 117.3(3) . .
C4 C5 C6 121.0(3) . .
N2 C6 C5 109.3(3) . .
N2 C6 H6A 109.8 . .
C5 C6 H6A 109.8 . .
N2 C6 H6B 109.8 . .
C5 C6 H6B 109.8 . .
H6A C6 H6B 108.3 . .
N2 C7 C8 110.8(3) . .
N2 C7 H7A 109.5 . .
C8 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
O1 C8 O2 124.5(3) . .
O1 C8 C7 118.6(3) . .
O2 C8 C7 116.9(3) . .
O1 C8 La1 40.23(15) . .
O2 C8 La1 151.3(2) . .
C7 C8 La1 82.96(18) . .
N2 C9 C14 111.6(3) . .
N2 C9 C10 112.8(3) . .
C14 C9 C10 110.4(3) . .
N2 C9 H9 107.3 . .
C14 C9 H9 107.3 . .
C10 C9 H9 107.3 . .
C11 C10 C9 112.2(3) . .
C11 C10 H10A 109.2 . .
C9 C10 H10A 109.2 . .
C11 C10 H10B 109.2 . .
C9 C10 H10B 109.2 . .
H10A C10 H10B 107.9 . .
C12 C11 C10 109.1(3) . .
C12 C11 H11A 109.9 . .
C10 C11 H11A 109.9 . .
C12 C11 H11B 109.9 . .
C10 C11 H11B 109.8 . .
H11A C11 H11B 108.3 . .
C11 C12 C13 110.0(3) . .
C11 C12 H12A 109.7 . .
C13 C12 H12A 109.7 . .
C11 C12 H12B 109.7 . .
C13 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
C12 C13 C14 111.4(3) . .
C12 C13 H13A 109.3 . .
C14 C13 H13A 109.3 . .
C12 C13 H13B 109.3 . .
C14 C13 H13B 109.3 . .
H13A C13 H13B 108.0 . .
N4 C14 C9 111.1(3) . .
N4 C14 C13 112.6(3) . .
C9 C14 C13 110.6(3) . .
N4 C14 H14 107.4 . .
C9 C14 H14 107.4 . .
C13 C14 H14 107.4 . .
N4 C21 C22 110.9(3) . .
N4 C21 H21A 109.5 . .
C22 C21 H21A 109.5 . .
N4 C21 H21B 109.5 . .
C22 C21 H21B 109.5 . .
H21A C21 H21B 108.0 . .
O4 C22 O3 125.2(4) . .
O4 C22 C21 118.9(3) . .
O3 C22 C21 115.9(3) . .
O4 C22 La1 155.2(3) . .
O3 C22 La1 39.86(15) . .
C21 C22 La1 78.99(18) . .
N4 C20 C19 112.0(3) . .
N4 C20 H20A 109.2 . .
C19 C20 H20A 109.2 . .
N4 C20 H20B 109.2 . .
C19 C20 H20B 109.2 . .
H20A C20 H20B 107.9 . .
N3 C19 C18 122.3(4) . .
N3 C19 C20 118.6(3) . .
C18 C19 C20 119.1(4) . .
C17 C18 C19 118.5(4) . .
C17 C18 H18 120.7 . .
C19 C18 H18 120.7 . .
C18 C17 C16 119.9(4) . .
C18 C17 H17 120.1 . .
C16 C17 H17 120.1 . .
C15 C16 C17 118.4(4) . .
C15 C16 H16 120.8 . .
C17 C16 H16 120.8 . .
N3 C15 C16 122.3(5) . .
N3 C15 H15 118.8 . .
C16 C15 H15 118.8 . .
O3 La1 O1 143.45(9) . .
O3 La1 O2 140.56(9) . 3_766
O1 La1 O2 75.90(8) . 3_766
O3 La1 O5 73.19(9) . .
O1 La1 O5 141.70(9) . .
O2 La1 O5 69.50(9) 3_766 .
O3 La1 N1 86.36(9) . .
O1 La1 N1 100.35(9) . .
O2 La1 N1 81.79(9) 3_766 .
O5 La1 N1 90.65(10) . .
O3 La1 N3 106.65(9) . .
O1 La1 N3 75.09(9) . .
O2 La1 N3 82.06(10) 3_766 .
O5 La1 N3 84.21(11) . .
N1 La1 N3 163.84(10) . .
O3 La1 N4 66.48(9) . .
O1 La1 N4 82.32(9) . .
O2 La1 N4 145.04(9) 3_766 .
O5 La1 N4 118.16(9) . .
N1 La1 N4 129.44(9) . .
N3 La1 N4 65.95(10) . .
O3 La1 N2 85.15(9) . .
O1 La1 N2 65.87(8) . .
O2 La1 N2 122.57(8) 3_766 .
O5 La1 N2 149.13(10) . .
N1 La1 N2 65.77(9) . .
N3 La1 N2 123.74(10) . .
N4 La1 N2 69.98(9) . .
O3 La1 C22 20.97(9) . .
O1 La1 C22 132.77(9) . .
O2 La1 C22 144.66(9) 3_766 .
O5 La1 C22 76.17(9) . .
N1 La1 C22 107.17(9) . .
N3 La1 C22 86.51(9) . .
N4 La1 C22 50.55(9) . .
N2 La1 C22 91.47(9) . .
O3 La1 C8 134.87(9) . .
O1 La1 C8 20.55(8) . .
O2 La1 C8 80.12(8) 3_766 .
O5 La1 C8 149.38(9) . .
N1 La1 C8 81.11(9) . .
N3 La1 C8 95.57(9) . .
N4 La1 C8 88.99(9) . .
N2 La1 C8 50.19(8) . .
C22 La1 C8 134.44(9) . .
C5 N1 C1 118.6(3) . .
C5 N1 La1 118.4(2) . .
C1 N1 La1 123.1(2) . .
C7 N2 C6 110.2(3) . .
C7 N2 C9 106.9(3) . .
C6 N2 C9 114.3(2) . .
C7 N2 La1 105.97(18) . .
C6 N2 La1 106.5(2) . .
C9 N2 La1 112.7(2) . .
C20 N4 C21 110.1(3) . .
C20 N4 C14 113.4(3) . .
C21 N4 C14 107.4(3) . .
C20 N4 La1 110.1(2) . .
C21 N4 La1 102.9(2) . .
C14 N4 La1 112.4(2) . .
C15 N3 C19 118.6(3) . .
C15 N3 La1 122.0(3) . .
C19 N3 La1 116.0(2) . .
C8 O1 La1 119.2(2) . .
C8 O2 La1 128.4(2) . 3_766
C22 O3 La1 119.2(2) . .
La1 O5 Na1 135.2(2) . .
La1 O5 H5A 129(4) . .
Na1 O5 H5A 94(4) . .
La1 O5 H5B 122(4) . .
Na1 O5 H5B 13(4) . .
H5A O5 H5B 107(5) . .
H6C O6 H6D 101(3) . .
F5 P1 F6 87.7(4) . .
F5 P1 F3 87.2(4) . .
F6 P1 F3 95.2(4) . .
F5 P1 F2 178.8(4) . .
F6 P1 F2 93.1(4) . .
F3 P1 F2 93.6(3) . .
F5 P1 F1 91.8(3) . .
F6 P1 F1 85.2(4) . .
F3 P1 F1 178.8(4) . .
F2 P1 F1 87.4(2) . .
F5 P1 F4 88.6(4) . .
F6 P1 F4 171.7(5) . .
F3 P1 F4 92.0(4) . .
F2 P1 F4 90.5(3) . .
F1 P1 F4 87.5(4) . .
P1 F3 Na3 147.7(7) . .
P1 F5 Na2 141.6(6) . 4_565
Na2 Na1 Na3 97.6(7) . .
Na2 Na1 O5 142.2(7) . .
Na3 Na1 O5 119.0(6) . .
Na2 Na1 Na3 114.0(7) . 3_666
Na3 Na1 Na3 31.7(8) . 3_666
O5 Na1 Na3 95.4(4) . 3_666
Na2 Na1 H5B 147.0(18) . .
Na3 Na1 H5B 114.9(17) . .
O5 Na1 H5B 5.5(16) . .
Na3 Na1 H5B 93.0(17) 3_666 .
Na1 Na2 F5 124.2(8) . 4_566
Na1 Na2 Na3 50.2(6) . .
F5 Na2 Na3 157.6(8) 4_566 .
Na3 Na3 F3 147.8(15) 3_666 .
Na3 Na3 Na1 103.0(13) 3_666 .
F3 Na3 Na1 76.1(6) . .
Na3 Na3 Na2 118.9(14) 3_666 .
F3 Na3 Na2 77.6(6) . .
Na1 Na3 Na2 32.2(4) . .
Na3 Na3 Na1 45.3(9) 3_666 3_666
F3 Na3 Na1 129.1(7) . 3_666
Na1 Na3 Na1 148.3(8) . 3_666
Na2 Na3 Na1 151.4(8) . 3_666
F5B P1B F2B 177(2) . .
F5B P1B F1B 93(3) . .
F2B P1B F1B 85(3) . .
F5B P1B F3B 87(3) . .
F2B P1B F3B 94(3) . .
F1B P1B F3B 179(2) . .
F5B P1B F6B 85(2) . .
F2B P1B F6B 92(2) . .
F1B P1B F6B 89(3) . .
F3B P1B F6B 91(3) . .
F5B P1B F4B 90(2) . .
F2B P1B F4B 93(2) . .
F1B P1B F4B 86(3) . .
F3B P1B F4B 93(3) . .
F6B P1B F4B 173(2) . .
F6C P1C F3C 93.3(10) . .
F6C P1C F1C 90.8(8) . .
F3C P1C F1C 175.8(11) . .
F6C P1C F5C 82.2(10) . .
F3C P1C F5C 90.4(9) . .
F1C P1C F5C 90.9(9) . .
F6C P1C F2C 93.0(9) . .
F3C P1C F2C 90.1(8) . .
F1C P1C F2C 88.9(8) . .
F5C P1C F2C 175.2(10) . .
F6C P1C F4C 168.3(8) . .
F3C P1C F4C 92.1(9) . .
F1C P1C F4C 83.9(8) . .
F5C P1C F4C 87.4(8) . .
F2C P1C F4C 97.4(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.344(4) .
C1 C2 1.379(5) .
C1 H1 0.9500 .
C2 C3 1.391(6) .
C2 H2 0.9500 .
C3 C4 1.389(5) .
C3 H3 0.9500 .
C4 C5 1.393(5) .
C4 H4 0.9500 .
C5 N1 1.344(4) .
C5 C6 1.510(5) .
C6 N2 1.485(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 N2 1.480(4) .
C7 C8 1.516(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 O1 1.256(4) .
C8 O2 1.261(4) .
C8 La1 3.123(3) .
C9 N2 1.516(4) .
C9 C14 1.524(5) .
C9 C10 1.532(5) .
C9 H9 1.0000 .
C10 C11 1.531(5) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.513(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.530(6) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.535(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 N4 1.516(4) .
C14 H14 1.0000 .
C21 N4 1.478(4) .
C21 C22 1.519(5) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 O4 1.239(4) .
C22 O3 1.278(4) .
C22 La1 3.118(3) .
C20 N4 1.474(4) .
C20 C19 1.505(5) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C19 N3 1.344(5) .
C19 C18 1.393(5) .
C18 C17 1.370(7) .
C18 H18 0.9500 .
C17 C16 1.388(7) .
C17 H17 0.9500 .
C16 C15 1.387(6) .
C16 H16 0.9500 .
C15 N3 1.342(5) .
C15 H15 0.9500 .
La1 O3 2.289(2) .
La1 O1 2.311(2) .
La1 O2 2.314(2) 3_766
La1 O5 2.325(3) .
La1 N1 2.464(3) .
La1 N3 2.478(3) .
La1 N4 2.525(3) .
La1 N2 2.570(3) .
O2 La1 2.314(2) 3_766
O5 Na1 2.744(8) .
O5 H5A 0.838(19) .
O5 H5B 0.84(2) .
O6 H6C 0.84(2) .
O6 H6D 0.896(16) .
P1 F5 1.550(5) .
P1 F6 1.556(6) .
P1 F3 1.559(6) .
P1 F2 1.574(4) .
P1 F1 1.598(5) .
P1 F4 1.612(5) .
F3 Na3 2.61(2) .
F5 Na2 2.57(2) 4_565
Na1 Na2 1.843(18) .
Na1 Na3 2.66(2) .
Na1 Na3 3.64(2) 3_666
Na1 H5B 1.93(3) .
Na2 F5 2.57(2) 4_566
Na2 Na3 3.43(3) .
Na3 Na3 1.96(5) 3_666
Na3 Na1 3.64(2) 3_666
P1B F5B 1.57(8) .
P1B F2B 1.65(8) .
P1B F1B 1.61(4) .
P1B F3B 1.58(5) .
P1B F6B 1.61(7) .
P1B F4B 1.78(8) .
P1C F6C 1.518(12) .
P1C F3C 1.524(13) .
P1C F1C 1.560(12) .
P1C F5C 1.566(13) .
P1C F2C 1.616(11) .
P1C F4C 1.831(12) .
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_4
N1 C1 C2 C3 0.9(5) . .
C1 C2 C3 C4 -0.9(5) . .
C2 C3 C4 C5 -0.4(6) . .
C3 C4 C5 N1 1.7(5) . .
C3 C4 C5 C6 -176.8(3) . .
N1 C5 C6 N2 -34.3(4) . .
C4 C5 C6 N2 144.3(3) . .
N2 C7 C8 O1 -7.3(4) . .
N2 C7 C8 O2 175.2(3) . .
N2 C7 C8 La1 -26.7(2) . .
N2 C9 C10 C11 178.3(3) . .
C14 C9 C10 C11 -56.1(4) . .
C9 C10 C11 C12 58.4(4) . .
C10 C11 C12 C13 -58.7(4) . .
C11 C12 C13 C14 58.9(5) . .
N2 C9 C14 N4 -54.0(4) . .
C10 C9 C14 N4 179.8(3) . .
N2 C9 C14 C13 -179.8(3) . .
C10 C9 C14 C13 53.9(4) . .
C12 C13 C14 N4 178.9(3) . .
C12 C13 C14 C9 -56.2(4) . .
N4 C21 C22 O4 164.4(3) . .
N4 C21 C22 O3 -18.5(4) . .
N4 C21 C22 La1 -34.0(2) . .
N4 C20 C19 N3 -13.7(4) . .
N4 C20 C19 C18 167.4(3) . .
N3 C19 C18 C17 -0.5(6) . .
C20 C19 C18 C17 178.4(3) . .
C19 C18 C17 C16 1.8(6) . .
C18 C17 C16 C15 -1.7(6) . .
C17 C16 C15 N3 0.3(6) . .
C4 C5 N1 C1 -1.8(5) . .
C6 C5 N1 C1 176.8(3) . .
C4 C5 N1 La1 178.5(3) . .
C6 C5 N1 La1 -2.9(4) . .
C2 C1 N1 C5 0.5(5) . .
C2 C1 N1 La1 -179.9(2) . .
C8 C7 N2 C6 149.0(3) . .
C8 C7 N2 C9 -86.2(3) . .
C8 C7 N2 La1 34.2(3) . .
C5 C6 N2 C7 -63.8(4) . .
C5 C6 N2 C9 175.9(3) . .
C5 C6 N2 La1 50.8(3) . .
C14 C9 N2 C7 151.8(3) . .
C10 C9 N2 C7 -83.3(3) . .
C14 C9 N2 C6 -86.0(3) . .
C10 C9 N2 C6 38.9(4) . .
C14 C9 N2 La1 35.7(3) . .
C10 C9 N2 La1 160.6(2) . .
C19 C20 N4 C21 -73.8(4) . .
C19 C20 N4 C14 165.8(3) . .
C19 C20 N4 La1 39.0(3) . .
C22 C21 N4 C20 161.4(3) . .
C22 C21 N4 C14 -74.7(3) . .
C22 C21 N4 La1 44.1(3) . .
C9 C14 N4 C20 -80.9(4) . .
C13 C14 N4 C20 43.8(4) . .
C9 C14 N4 C21 157.2(3) . .
C13 C14 N4 C21 -78.1(4) . .
C9 C14 N4 La1 44.8(3) . .
C13 C14 N4 La1 169.4(2) . .
C16 C15 N3 C19 1.0(5) . .
C16 C15 N3 La1 -157.2(3) . .
C18 C19 N3 C15 -0.9(5) . .
C20 C19 N3 C15 -179.8(3) . .
C18 C19 N3 La1 158.6(3) . .
C20 C19 N3 La1 -20.3(4) . .
O2 C8 O1 La1 146.7(3) . .
C7 C8 O1 La1 -30.5(4) . .
O1 C8 O2 La1 -54.7(5) . 3_766
C7 C8 O2 La1 122.6(3) . 3_766
La1 C8 O2 La1 -7.1(7) . 3_766
O4 C22 O3 La1 152.7(3) . .
C21 C22 O3 La1 -24.2(4) . .
F5 P1 F3 Na3 121.4(11) . .
F6 P1 F3 Na3 33.9(11) . .
F2 P1 F3 Na3 -59.5(11) . .
F4 P1 F3 Na3 -150.2(11) . .
F6 P1 F5 Na2 -121.2(8) . 4_565
F3 P1 F5 Na2 143.5(9) . 4_565
F1 P1 F5 Na2 -36.0(8) . 4_565
F4 P1 F5 Na2 51.4(8) . 4_565
Na3 Na1 Na2 F5 -152.7(10) . 4_566
O5 Na1 Na2 F5 13.5(19) . 4_566
Na3 Na1 Na2 F5 -124.4(9) 3_666 4_566
O5 Na1 Na2 Na3 166.2(14) . .
Na3 Na1 Na2 Na3 28.3(9) 3_666 .
