# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_20383
_database_code_depnum_ccdc_archive 'CCDC 1949330'
loop_
_audit_author_name
_audit_author_address
zhou
;Xiamen University
China
;
_audit_update_record             
;
2021-06-10 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_audit_creation_date             2021-06-04
_audit_creation_method           
;
Olex2 1.5-dev
(compiled 2021.06.01 svn.r985b505f for OlexSys, GUI svn.r6225)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H16 La N2 O10, Cl, 4(H2 O)'
_chemical_formula_sum            'C8 H24 Cl La N2 O14'
_chemical_formula_weight         546.65
_chemical_melting_point          ?
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'
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'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.8281(4)
_cell_length_b                   19.2494(8)
_cell_length_c                   22.4818(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3820.5(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3211
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.6210
_cell_measurement_theta_min      2.7070
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.527
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10788
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.019
_diffrn_reflns_theta_min         2.695
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  50.00   1.00   37.50    --  -22.85  19.00-180.00  120
  2  ω     65.00  99.00   1.00   37.50    --   24.26 178.00  90.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4057
_reflns_number_total             4800
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4800
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0340P)²+0.2005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0815
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O5W(H5WA,H5WB), O3W(H3WA,H3WB), O6W(H6WA,H6WB), O4W(H4WA,H4WB)
2.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C8(H8A,H8B), C6(H6A,H6B), C2(H2C,H2D), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
La1 La 0.25976(2) 0.32268(2) 0.25968(2) 0.01027(7) Uani 1 1 d . . . . .
Cl1 Cl -0.06849(9) 0.55702(4) 0.34127(4) 0.02282(18) Uani 1 1 d . . . . .
O7 O 0.0132(2) 0.75926(11) 0.21844(10) 0.0141(5) Uani 1 1 d . . . . .
O8 O -0.1908(2) 0.69353(11) 0.21080(11) 0.0191(5) Uani 1 1 d . . . . .
O5 O 0.0294(2) 0.39355(12) 0.23619(10) 0.0163(5) Uani 1 1 d . . . . .
O1W O 0.3266(2) 0.39810(11) 0.16074(10) 0.0182(5) Uani 1 1 d . . . . .
H1WA H 0.347227 0.441823 0.170111 0.027 Uiso 1 1 d R U . . .
H1WB H 0.246255 0.401970 0.137317 0.027 Uiso 1 1 d R U . . .
O6 O -0.1771(2) 0.45048(10) 0.21039(10) 0.0168(5) Uani 1 1 d . . . . .
O2 O 0.6635(2) 0.26385(12) 0.33363(10) 0.0189(5) Uani 1 1 d . . . . .
O2W O 0.1296(2) 0.35119(11) 0.36121(10) 0.0179(5) Uani 1 1 d . . . . .
H2WA H 0.047887 0.376888 0.355850 0.027 Uiso 1 1 d R U . . .
H2WB H 0.188231 0.378074 0.383110 0.027 Uiso 1 1 d R U . . .
O1 O 0.4179(2) 0.29054(12) 0.34665(11) 0.0221(5) Uani 1 1 d . . . . .
O5W O 1.2365(3) 0.05684(13) 0.39243(13) 0.0235(6) Uani 1 1 d G . . . .
H5WA H 1.326175 0.054454 0.378891 0.035 Uiso 1 1 d G U . . .
H5WB H 1.219892 0.016912 0.407118 0.035 Uiso 1 1 d G U . . .
N2 N -0.0390(3) 0.57377(11) 0.20475(12) 0.0120(5) Uani 1 1 d . . . . .
H2A H -0.106492 0.571189 0.174226 0.014 Uiso 1 1 calc R U . . .
H2B H -0.092676 0.574782 0.239309 0.014 Uiso 1 1 calc R U . . .
O3 O 0.8357(3) 0.06531(13) 0.45766(12) 0.0295(6) Uani 1 1 d . . . . .
O3W O 0.9571(3) 0.23403(15) 0.42448(13) 0.0326(6) Uani 1 1 d G . . . .
H3WA H 1.001732 0.263107 0.402117 0.049 Uiso 1 1 d G U . . .
H3WB H 1.028474 0.212291 0.441738 0.049 Uiso 1 1 d G U . . .
O4 O 0.7963(3) 0.07500(12) 0.55649(11) 0.0239(5) Uani 1 1 d . . . . .
O6W O 0.8880(3) -0.07265(12) 0.42805(12) 0.0265(6) Uani 1 1 d G . . . .
H6WA H 0.872496 -0.033370 0.444276 0.040 Uiso 1 1 d G U . . .
H6WB H 0.983370 -0.078208 0.429892 0.040 Uiso 1 1 d G U . . .
N1 N 0.6682(3) 0.17842(13) 0.43057(12) 0.0164(6) Uani 1 1 d . . . . .
H1A H 0.754319 0.201971 0.421189 0.020 Uiso 1 1 calc R U . . .
H1B H 0.662020 0.140649 0.406355 0.020 Uiso 1 1 calc R U . . .
O4W O 1.1918(4) 0.16094(14) 0.47545(13) 0.0346(6) Uani 1 1 d G . . . .
H4WA H 1.212160 0.135296 0.445715 0.052 Uiso 1 1 d G U . . .
H4WB H 1.178636 0.132583 0.503993 0.052 Uiso 1 1 d G U . . .
C7 C -0.0514(3) 0.70085(16) 0.21039(14) 0.0138(6) Uani 1 1 d . . . . .
C8 C 0.0481(3) 0.63908(14) 0.19926(16) 0.0173(7) Uani 1 1 d . . . . .
H8A H 0.092112 0.642284 0.158839 0.021 Uiso 1 1 calc R U . . .
H8B H 0.132504 0.638914 0.228272 0.021 Uiso 1 1 calc R U . . .
C5 C -0.0375(3) 0.44771(15) 0.21755(14) 0.0129(6) Uani 1 1 d . . . . .
C1 C 0.5403(3) 0.26231(16) 0.36104(14) 0.0140(6) Uani 1 1 d . . . . .
C6 C 0.0572(3) 0.51081(14) 0.20415(15) 0.0148(6) Uani 1 1 d . . . . .
H6A H 0.138429 0.515375 0.234265 0.018 Uiso 1 1 calc R U . . .
H6B H 0.105338 0.505644 0.164623 0.018 Uiso 1 1 calc R U . . .
C2 C 0.5344(4) 0.22415(18) 0.42038(15) 0.0198(7) Uani 1 1 d . . . . .
H2C H 0.528435 0.258690 0.452917 0.024 Uiso 1 1 calc R U . . .
H2D H 0.441237 0.195559 0.421816 0.024 Uiso 1 1 calc R U . . .
C3 C 0.7796(4) 0.09239(17) 0.50225(16) 0.0189(7) Uani 1 1 d . . . . .
C4 C 0.6760(4) 0.15507(17) 0.49389(15) 0.0209(7) Uani 1 1 d . . . . .
H4A H 0.572799 0.142979 0.507702 0.025 Uiso 1 1 calc R U . . .
H4B H 0.713323 0.193866 0.518800 0.025 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O7 2.523(2) 8_655 y
La1 O7 2.746(2) 3_545 y
La1 O8 2.644(2) 3_545 y
La1 O5 2.745(2) 6_656 y
La1 O5 2.505(2) . y
La1 O1W 2.721(2) . y
La1 O6 2.611(2) 6_656 y
La1 O2 2.531(2) 6_556 y
La1 O2W 2.614(2) . y
La1 O1 2.481(2) . y
La1 C7 3.055(3) 3_545 y
La1 C5 3.043(3) 6_656 y
O7 C7 1.274(4) . ?
O8 C7 1.239(4) . ?
O5 C5 1.269(4) . ?
O1W H1WA 0.8866 . ?
O1W H1WB 0.8867 . ?
O6 C5 1.245(4) . ?
O2 C1 1.251(4) . ?
O2W H2WA 0.8830 . ?
O2W H2WB 0.8821 . ?
O1 C1 1.252(4) . ?
O5W H5WA 0.8498 . ?
O5W H5WB 0.8491 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 C8 1.479(3) . ?
N2 C6 1.480(3) . ?
O3 C3 1.234(4) . ?
O3W H3WA 0.8494 . ?
O3W H3WB 0.8501 . ?
O4 C3 1.273(4) . ?
O6W H6WA 0.8506 . ?
O6W H6WB 0.8498 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.491(4) . ?
N1 C4 1.494(4) . ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8505 . ?
C7 C8 1.500(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C5 C6 1.505(4) . ?
C1 C2 1.524(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 C4 1.526(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?

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
O7 La1 O7 123.22(8) 8_655 3_545 y
O7 La1 O8 79.64(7) 8_655 3_545 y
O7 La1 O5 64.16(7) 8_655 6_656 y
O7 La1 O1W 77.61(7) 8_655 . y
O7 La1 O6 112.41(7) 8_655 6_656 y
O7 La1 O2 75.26(7) 8_655 6_556 y
O7 La1 O2W 140.50(7) 8_655 . y
O7 La1 C7 100.82(7) 8_655 3_545 y
O7 La1 C7 24.63(7) 3_545 3_545 y
O7 La1 C5 146.91(7) 3_545 6_656 y
O7 La1 C5 88.69(8) 8_655 6_656 y
O8 La1 O7 48.32(6) 3_545 3_545 y
O8 La1 O5 131.17(7) 3_545 6_656 y
O8 La1 O1W 139.18(7) 3_545 . y
O8 La1 C7 23.73(7) 3_545 3_545 y
O8 La1 C5 146.81(8) 3_545 6_656 y
O5 La1 O7 167.40(7) 6_656 3_545 y
O5 La1 O7 146.19(8) . 8_655 y
O5 La1 O7 64.36(7) . 3_545 y
O5 La1 O8 112.21(7) . 3_545 y
O5 La1 O5 116.13(8) . 6_656 y
O5 La1 O1W 73.34(7) . . y
O5 La1 O6 73.41(7) . 6_656 y
O5 La1 O2 78.25(7) . 6_556 y
O5 La1 O2W 73.31(7) . . y
O5 La1 C7 153.64(8) 6_656 3_545 y
O5 La1 C7 88.60(8) . 3_545 y
O5 La1 C5 94.72(8) . 6_656 y
O5 La1 C5 24.65(7) 6_656 6_656 y
O1W La1 O7 125.03(7) . 3_545 y
O1W La1 O5 64.81(7) . 6_656 y
O1W La1 C7 136.07(8) . 3_545 y
O1W La1 C5 65.66(8) . 6_656 y
O6 La1 O7 124.06(7) 6_656 3_545 y
O6 La1 O8 150.50(8) 6_656 3_545 y
O6 La1 O5 48.54(6) 6_656 6_656 y
O6 La1 O1W 70.23(7) 6_656 . y
O6 La1 O2W 70.78(7) 6_656 . y
O6 La1 C7 142.65(8) 6_656 3_545 y
O6 La1 C5 23.90(7) 6_656 6_656 y
O2 La1 O7 69.82(7) 6_556 3_545 y
O2 La1 O8 73.15(8) 6_556 3_545 y
O2 La1 O5 122.78(7) 6_556 6_656 y
O2 La1 O1W 68.53(7) 6_556 . y
O2 La1 O6 134.99(7) 6_556 6_656 y
O2 La1 O2W 132.09(7) 6_556 . y
O2 La1 C7 68.72(8) 6_556 3_545 y
O2 La1 C5 133.70(8) 6_556 6_656 y
O2W La1 O7 63.33(7) . 3_545 y
O2W La1 O8 82.94(7) . 3_545 y
O2W La1 O5 104.32(7) . 6_656 y
O2W La1 O1W 134.21(7) . . y
O2W La1 C7 72.79(8) . 3_545 y
O2W La1 C5 86.88(8) . 6_656 y
O1 La1 O7 104.00(7) . 3_545 y
O1 La1 O7 73.86(7) . 8_655 y
O1 La1 O8 72.38(7) . 3_545 y
O1 La1 O5 67.00(7) . 6_656 y
O1 La1 O5 139.35(8) . . y
O1 La1 O1W 130.93(7) . . y
O1 La1 O6 84.93(7) . 6_656 y
O1 La1 O2 136.94(7) . 6_556 y
O1 La1 O2W 67.14(7) . . y
O1 La1 C7 88.50(8) . 3_545 y
O1 La1 C5 74.55(8) . 6_656 y
C5 La1 C7 157.55(8) 6_656 3_545 y
La1 O7 La1 114.59(8) 8_665 3 ?
C7 O7 La1 91.42(17) . 3 ?
C7 O7 La1 146.62(19) . 8_665 ?
C7 O8 La1 97.10(18) . 3 ?
La1 O5 La1 115.23(8) . 6_556 ?
C5 O5 La1 153.4(2) . . ?
C5 O5 La1 90.94(18) . 6_556 ?
La1 O1W H1WA 110.9 . . ?
La1 O1W H1WB 110.9 . . ?
H1WA O1W H1WB 103.0 . . ?
C5 O6 La1 97.92(18) . 6_556 ?
C1 O2 La1 135.3(2) . 6_656 ?
La1 O2W H2WA 111.0 . . ?
La1 O2W H2WB 110.7 . . ?
H2WA O2W H2WB 103.1 . . ?
C1 O1 La1 142.9(2) . . ?
H5WA O5W H5WB 104.5 . . ?
H2A N2 H2B 107.7 . . ?
C8 N2 H2A 108.9 . . ?
C8 N2 H2B 108.9 . . ?
C8 N2 C6 113.3(2) . . ?
C6 N2 H2A 108.9 . . ?
C6 N2 H2B 108.9 . . ?
H3WA O3W H3WB 104.5 . . ?
H6WA O6W H6WB 104.5 . . ?
H1A N1 H1B 108.0 . . ?
C2 N1 H1A 109.4 . . ?
C2 N1 H1B 109.4 . . ?
C2 N1 C4 111.1(2) . . ?
C4 N1 H1A 109.4 . . ?
C4 N1 H1B 109.4 . . ?
H4WA O4W H4WB 104.5 . . ?
O7 C7 La1 63.95(15) . 3 ?
O7 C7 C8 117.4(3) . . ?
O8 C7 La1 59.17(16) . 3 ?
O8 C7 O7 123.0(3) . . ?
O8 C7 C8 119.6(3) . . ?
C8 C7 La1 176.5(2) . 3 ?
N2 C8 C7 110.8(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O5 C5 La1 64.41(16) . 6_556 ?
O5 C5 C6 118.1(3) . . ?
O6 C5 La1 58.18(16) . 6_556 ?
O6 C5 O5 122.6(3) . . ?
O6 C5 C6 119.3(3) . . ?
C6 C5 La1 177.2(2) . 6_556 ?
O2 C1 O1 127.8(3) . . ?
O2 C1 C2 118.2(3) . . ?
O1 C1 C2 114.0(3) . . ?
N2 C6 C5 109.9(2) . . ?
N2 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N1 C2 C1 113.1(3) . . ?
N1 C2 H2C 109.0 . . ?
N1 C2 H2D 109.0 . . ?
C1 C2 H2C 109.0 . . ?
C1 C2 H2D 109.0 . . ?
H2C C2 H2D 107.8 . . ?
O3 C3 O4 128.4(3) . . ?
O3 C3 C4 118.4(3) . . ?
O4 C3 C4 113.3(3) . . ?
N1 C4 C3 112.5(3) . . ?
N1 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O7 C7 La1 142.6(4) 8_665 . . 3 ?
La1 O7 C7 O8 146.9(3) 8_665 . . . ?
La1 O7 C7 O8 4.4(3) 3 . . . ?
La1 O7 C7 C8 -176.4(3) 3 . . . ?
La1 O7 C7 C8 -33.8(5) 8_665 . . . ?
La1 O8 C7 O7 -4.6(4) 3 . . . ?
La1 O8 C7 C8 176.2(3) 3 . . . ?
La1 O5 C5 La1 170.2(5) . . . 6_556 ?
La1 O5 C5 O6 171.9(3) . . . . ?
La1 O5 C5 O6 1.8(3) 6_556 . . . ?
La1 O5 C5 C6 -178.6(3) 6_556 . . . ?
La1 O5 C5 C6 -8.5(6) . . . . ?
La1 O6 C5 O5 -1.9(3) 6_556 . . . ?
La1 O6 C5 C6 178.5(2) 6_556 . . . ?
La1 O2 C1 O1 3.1(5) 6_656 . . . ?
La1 O2 C1 C2 -174.5(2) 6_656 . . . ?
La1 O1 C1 O2 34.3(6) . . . . ?
La1 O1 C1 C2 -147.9(3) . . . . ?
O7 C7 C8 N2 166.8(3) . . . . ?
O8 C7 C8 N2 -13.9(4) . . . . ?
O5 C5 C6 N2 -159.3(3) . . . . ?
O6 C5 C6 N2 20.3(4) . . . . ?
O2 C1 C2 N1 -14.5(4) . . . . ?
O1 C1 C2 N1 167.5(3) . . . . ?
O3 C3 C4 N1 -4.8(4) . . . . ?
O4 C3 C4 N1 175.1(3) . . . . ?
C8 N2 C6 C5 173.0(3) . . . . ?
C6 N2 C8 C7 -170.5(3) . . . . ?
C2 N1 C4 C3 162.7(3) . . . . ?
C4 N1 C2 C1 167.0(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_23406
_database_code_depnum_ccdc_archive 'CCDC 1949332'
loop_
_audit_author_name
_audit_author_address
zhou
;Xiamen university
China
;
_audit_update_record             
;
2021-08-05 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H28 La2 N4 O18, C2 H10 N2, 10[H2O]'
_chemical_formula_sum            'C22 H58 La2 N6 O28'
_chemical_formula_weight         1132.56

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   13.0217(4)
_cell_length_b                   13.1618(6)
_cell_length_c                   14.0976(7)
_cell_angle_alpha                114.764(5)
_cell_angle_beta                 92.033(3)
_cell_angle_gamma                103.503(4)
_cell_volume                     2108.89(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    4973
_cell_measurement_theta_min      2.8620
_cell_measurement_theta_max      27.6060

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             1140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.097
_shelx_estimated_absorpt_T_min   0.679
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15532
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.254
_diffrn_reflns_theta_max         28.577
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9381
_reflns_number_gt                7566
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9381
_refine_ls_number_parameters     441
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0853
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
La1 La 0.87264(2) 0.58860(2) 0.99522(2) 0.01833(7) Uani 1 1 d D . . . .
La2 La 0.42945(2) 0.52780(2) 0.64631(2) 0.01892(7) Uani 1 1 d D . . . .
O14 O 0.4257(2) 0.5438(3) 0.4694(2) 0.0239(6) Uani 1 1 d . . . . .
O1 O 1.0643(2) 0.5724(3) 0.9691(2) 0.0245(6) Uani 1 1 d . . . . .
O7 O 0.6868(2) 0.5349(3) 0.8928(2) 0.0290(7) Uani 1 1 d . . . . .
O8 O 0.5660(2) 0.5564(3) 0.7925(2) 0.0312(7) Uani 1 1 d . . . . .
O9 O 0.9930(2) 0.6902(3) 1.1761(2) 0.0304(7) Uani 1 1 d G . . . .
H9A H 1.039991 0.666355 1.197865 0.046 Uiso 1 1 d DG U . . .
H9B H 0.994516 0.754629 1.227607 0.046 Uiso 1 1 d DG U . . .
O18 O 0.5725(2) 0.7069(3) 0.6651(2) 0.0301(7) Uani 1 1 d G . . . .
H18A H 0.622332 0.705295 0.627667 0.045 Uiso 1 1 d DG U . . .
H18B H 0.598929 0.765478 0.724045 0.045 Uiso 1 1 d DG U . . .
O15 O 0.4919(3) 0.6657(3) 0.4035(2) 0.0348(8) Uani 1 1 d . . . . .
O2 O 1.2314(2) 0.6370(3) 1.0474(3) 0.0361(8) Uani 1 1 d . . . . .
O5 O 0.8391(2) 0.7827(3) 1.0723(2) 0.0301(7) Uani 1 1 d . . . . .
O16 O 0.3986(2) 0.6845(3) 0.8042(2) 0.0289(7) Uani 1 1 d . . . . .
O3 O 0.8841(3) 0.4474(3) 0.8116(2) 0.0334(8) Uani 1 1 d . . . . .
O12 O 0.3073(2) 0.3553(3) 0.4940(2) 0.0349(8) Uani 1 1 d . . . . .
O11 O 0.2480(2) 0.4104(3) 0.8694(2) 0.0332(8) Uani 1 1 d . . . . .
O10 O 0.3422(2) 0.4132(3) 0.7428(2) 0.0287(7) Uani 1 1 d . . . . .
O17 O 0.3504(3) 0.8415(3) 0.9039(2) 0.0380(8) Uani 1 1 d . . . . .
N2 N 0.8508(3) 0.6596(3) 0.8331(3) 0.0224(8) Uani 1 1 d . . . . .
N1 N 1.0403(3) 0.7851(3) 1.0134(3) 0.0240(8) Uani 1 1 d . . . . .
N4 N 0.2066(3) 0.4880(3) 0.6555(3) 0.0237(8) Uani 1 1 d . . . . .
N3 N 0.3379(3) 0.6923(3) 0.6193(3) 0.0252(8) Uani 1 1 d . . . . .
O6 O 0.8730(3) 0.9748(3) 1.1360(3) 0.0473(9) Uani 1 1 d . . . . .
O4 O 0.9070(3) 0.3963(3) 0.6438(3) 0.0526(10) Uani 1 1 d . . . . .
O13 O 0.1517(3) 0.2416(3) 0.3957(3) 0.0525(10) Uani 1 1 d . . . . .
N5 N 0.5057(3) 0.6633(4) 1.1766(3) 0.0383(10) Uani 1 1 d . . . . .
H5C H 0.449781 0.599358 1.150867 0.046 Uiso 1 1 calc R U . . .
H5D H 0.483420 0.726089 1.215216 0.046 Uiso 1 1 calc R U . . .
H5E H 0.554877 0.655472 1.217726 0.046 Uiso 1 1 calc R U . . .
C8 C 0.7425(3) 0.6777(4) 0.8297(3) 0.0288(10) Uani 1 1 d . . . . .
H8A H 0.723474 0.681191 0.763450 0.035 Uiso 1 1 calc R U . . .
H8B H 0.743338 0.752331 0.888221 0.035 Uiso 1 1 calc R U . . .
C17 C 0.3651(3) 0.7707(4) 0.8167(3) 0.0252(9) Uani 1 1 d . . . . .
C15 C 0.4383(3) 0.6406(4) 0.4664(3) 0.0263(10) Uani 1 1 d . . . . .
C14 C 0.1933(3) 0.4908(4) 0.7604(3) 0.0276(10) Uani 1 1 d . . . . .
H14A H 0.118991 0.451554 0.758941 0.033 Uiso 1 1 calc R U . . .
H14B H 0.208393 0.571873 0.813557 0.033 Uiso 1 1 calc R U . . .
C3 C 0.8846(3) 0.4615(4) 0.7280(3) 0.0295(10) Uani 1 1 d . . . . .
C2 C 1.1444(3) 0.7776(4) 1.0493(3) 0.0253(9) Uani 1 1 d . . . . .
H2A H 1.160999 0.822125 1.126292 0.030 Uiso 1 1 calc R U . . .
H2B H 1.199606 0.813288 1.018520 0.030 Uiso 1 1 calc R U . . .
C13 C 0.2658(3) 0.4330(4) 0.7920(3) 0.0221(9) Uani 1 1 d . . . . .
C7 C 0.6597(3) 0.5819(4) 0.8376(3) 0.0260(10) Uani 1 1 d . . . . .
C9 C 0.9313(3) 0.7701(4) 0.8567(3) 0.0286(10) Uani 1 1 d . . . . .
H9C H 0.906742 0.835044 0.905787 0.034 Uiso 1 1 calc R U . . .
H9D H 0.938147 0.778784 0.791249 0.034 Uiso 1 1 calc R U . . .
C1 C 1.1473(3) 0.6544(4) 1.0192(3) 0.0255(9) Uani 1 1 d . . . . .
C4 C 0.8584(4) 0.5674(5) 0.7301(3) 0.0359(12) Uani 1 1 d . . . . .
H4A H 0.912869 0.602670 0.698366 0.043 Uiso 1 1 calc R U . . .
H4B H 0.790069 0.541585 0.684184 0.043 Uiso 1 1 calc R U . . .
C16 C 0.3880(4) 0.7290(4) 0.5416(3) 0.0299(11) Uani 1 1 d . . . . .
H16A H 0.442885 0.803210 0.579712 0.036 Uiso 1 1 calc R U . . .
H16B H 0.333641 0.741351 0.500960 0.036 Uiso 1 1 calc R U . . .
N6 N 0.4636(4) 0.8147(4) 1.0626(3) 0.0472(11) Uani 1 1 d . . . . .
H6A H 0.416078 0.819393 1.017719 0.057 Uiso 1 1 calc R U . . .
H6B H 0.526590 0.866829 1.072905 0.057 Uiso 1 1 calc R U . . .
H6C H 0.439323 0.829868 1.124721 0.057 Uiso 1 1 calc R U . . .
C19 C 0.2251(3) 0.6267(4) 0.5746(3) 0.0295(10) Uani 1 1 d . . . . .
H19A H 0.222539 0.561097 0.506336 0.035 Uiso 1 1 calc R U . . .
H19B H 0.187875 0.677490 0.561780 0.035 Uiso 1 1 calc R U . . .
C6 C 0.9009(4) 0.8821(4) 1.0982(3) 0.0301(10) Uani 1 1 d . . . . .
C10 C 1.0397(3) 0.7759(5) 0.9045(4) 0.0318(11) Uani 1 1 d . . . . .
H10A H 1.060440 0.706045 0.859552 0.038 Uiso 1 1 calc R U . . .
H10B H 1.092790 0.843502 0.906421 0.038 Uiso 1 1 calc R U . . .
C11 C 0.2071(4) 0.3200(4) 0.4798(4) 0.0337(11) Uani 1 1 d . . . . .
C22 C 0.4779(4) 0.6981(5) 1.0179(3) 0.0378(12) Uani 1 1 d . . . . .
H22A H 0.505251 0.682979 0.950807 0.045 Uiso 1 1 calc R U . . .
H22B H 0.408009 0.641761 1.002398 0.045 Uiso 1 1 calc R U . . .
C12 C 0.1498(4) 0.3717(5) 0.5722(4) 0.0402(13) Uani 1 1 d . . . . .
H12A H 0.081469 0.375974 0.544789 0.048 Uiso 1 1 calc R U . . .
H12B H 0.133558 0.318126 0.604717 0.048 Uiso 1 1 calc R U . . .
C5 C 1.0172(4) 0.8929(4) 1.0844(4) 0.0326(11) Uani 1 1 d . . . . .
H5A H 1.040659 0.950835 1.057592 0.039 Uiso 1 1 calc R U . . .
H5B H 1.059599 0.922235 1.154014 0.039 Uiso 1 1 calc R U . . .
C20 C 0.1672(3) 0.5811(5) 0.6453(4) 0.0329(11) Uani 1 1 d . . . . .
H20A H 0.175485 0.645630 0.715587 0.039 Uiso 1 1 calc R U . . .
H20B H 0.090822 0.550250 0.616983 0.039 Uiso 1 1 calc R U . . .
C18 C 0.3476(4) 0.7949(4) 0.7218(3) 0.0322(11) Uani 1 1 d . . . . .
H18C H 0.282423 0.820410 0.724038 0.039 Uiso 1 1 calc R U . . .
H18D H 0.407544 0.858628 0.726662 0.039 Uiso 1 1 calc R U . . .
C21 C 0.5533(4) 0.6780(5) 1.0887(4) 0.0437(13) Uani 1 1 d . . . . .
H21A H 0.575550 0.608339 1.046082 0.052 Uiso 1 1 calc R U . . .
H21B H 0.617349 0.744196 1.117505 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O5 2.475(3) . ?
La1 O3 2.511(3) . ?
La1 O11 2.512(3) 2_667 ?
La1 O7 2.557(3) . ?
La1 O9 2.575(3) . ?
La1 O1 2.580(3) . ?
La1 O1 2.663(3) 2_767 ?
La1 O2 2.753(3) 2_767 ?
La1 N2 2.837(3) . ?
La1 N1 2.879(3) . ?
La1 C1 3.066(4) 2_767 ?
La2 O16 2.444(3) . ?
La2 O12 2.507(3) . ?
La2 O8 2.516(3) . ?
La2 O10 2.538(3) . ?
La2 O18 2.547(3) . ?
La2 O14 2.588(2) . ?
La2 O14 2.622(3) 2_666 ?
La2 O15 2.793(3) 2_666 ?
La2 N4 2.843(3) . ?
La2 N3 2.849(3) . ?
La2 C15 3.071(4) 2_666 ?
O14 C15 1.264(5) . ?
O1 C1 1.262(5) . ?
O7 C7 1.265(5) . ?
O8 C7 1.257(5) . ?
O9 H9A 0.8499 . ?
O9 H9B 0.8499 . ?
O18 H18A 0.8493 . ?
O18 H18B 0.8500 . ?
O15 C15 1.250(5) . ?
O2 C1 1.253(5) . ?
O5 C6 1.257(6) . ?
O16 C17 1.257(5) . ?
O3 C3 1.268(5) . ?
O12 C11 1.257(5) . ?
O11 C13 1.260(4) . ?
O10 C13 1.249(4) . ?
O17 C17 1.247(5) . ?
N2 C4 1.477(6) . ?
N2 C9 1.478(5) . ?
N2 C8 1.486(5) . ?
N1 C5 1.462(6) . ?
N1 C2 1.468(5) . ?
N1 C10 1.489(5) . ?
N4 C12 1.474(6) . ?
N4 C14 1.482(5) . ?
N4 C20 1.490(5) . ?
N3 C19 1.479(5) . ?
N3 C18 1.484(5) . ?
N3 C16 1.484(5) . ?
O6 C6 1.258(5) . ?
O4 C3 1.232(5) . ?
O13 C11 1.248(6) . ?
N5 C21 1.468(5) . ?
N5 H5C 0.9000 . ?
N5 H5D 0.9000 . ?
N5 H5E 0.9000 . ?
C8 C7 1.503(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C17 C18 1.520(5) . ?
C15 C16 1.509(6) . ?
C14 C13 1.502(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C3 C4 1.499(6) . ?
C2 C1 1.506(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C9 C10 1.514(6) . ?
C9 H9C 0.9800 . ?
C9 H9D 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
N6 C22 1.455(6) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N6 H6C 0.9000 . ?
C19 C20 1.505(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C6 C5 1.515(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.510(6) . ?
C22 C21 1.518(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 H18D 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?

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
O5 La1 O3 134.22(10) . . ?
O5 La1 O11 73.43(10) . 2_667 ?
O3 La1 O11 135.99(11) . 2_667 ?
O5 La1 O7 80.99(10) . . ?
O3 La1 O7 75.96(10) . . ?
O11 La1 O7 77.04(9) 2_667 . ?
O5 La1 O9 77.83(10) . . ?
O3 La1 O9 136.03(10) . . ?
O11 La1 O9 73.26(10) 2_667 . ?
O7 La1 O9 147.34(9) . . ?
O5 La1 O1 119.62(10) . . ?
O3 La1 O1 67.05(10) . . ?
O11 La1 O1 136.81(9) 2_667 . ?
O7 La1 O1 142.14(9) . . ?
O9 La1 O1 70.51(9) . . ?
O5 La1 O1 147.01(9) . 2_767 ?
O3 La1 O1 78.30(9) . 2_767 ?
O11 La1 O1 85.48(9) 2_667 2_767 ?
O7 La1 O1 119.21(9) . 2_767 ?
O9 La1 O1 71.85(9) . 2_767 ?
O1 La1 O1 61.51(10) . 2_767 ?
O5 La1 O2 138.49(9) . 2_767 ?
O3 La1 O2 68.11(10) . 2_767 ?
O11 La1 O2 70.64(10) 2_667 2_767 ?
O7 La1 O2 71.38(9) . 2_767 ?
O9 La1 O2 110.21(10) . 2_767 ?
O1 La1 O2 100.86(9) . 2_767 ?
O1 La1 O2 47.96(8) 2_767 2_767 ?
O5 La1 N2 70.97(10) . . ?
O3 La1 N2 63.29(10) . . ?
O11 La1 N2 128.17(9) 2_667 . ?
O7 La1 N2 61.28(9) . . ?
O9 La1 N2 131.56(11) . . ?
O1 La1 N2 93.84(9) . . ?
O1 La1 N2 140.59(9) 2_767 . ?
O2 La1 N2 117.80(10) 2_767 . ?
O5 La1 N1 61.86(10) . . ?
O3 La1 N1 98.62(10) . . ?
O11 La1 N1 125.17(11) 2_667 . ?
O7 La1 N1 121.88(9) . . ?
O9 La1 N1 67.91(10) . . ?
O1 La1 N1 58.95(9) . . ?
O1 La1 N1 115.79(9) 2_767 . ?
O2 La1 N1 159.59(9) 2_767 . ?
N2 La1 N1 64.94(10) . . ?
O5 La1 C1 153.11(10) . 2_767 ?
O3 La1 C1 68.83(10) . 2_767 ?
O11 La1 C1 79.75(10) 2_667 2_767 ?
O7 La1 C1 95.06(11) . 2_767 ?
O9 La1 C1 92.78(11) . 2_767 ?
O1 La1 C1 79.34(10) . 2_767 ?
O1 La1 C1 24.17(10) 2_767 2_767 ?
O2 La1 C1 24.11(10) 2_767 2_767 ?
N2 La1 C1 130.19(11) . 2_767 ?
N1 La1 C1 137.62(11) . 2_767 ?
O16 La2 O12 133.33(10) . . ?
O16 La2 O8 75.04(10) . . ?
O12 La2 O8 135.22(11) . . ?
O16 La2 O10 79.62(10) . . ?
O12 La2 O10 80.27(10) . . ?
O8 La2 O10 71.49(9) . . ?
O16 La2 O18 76.46(10) . . ?
O12 La2 O18 134.70(9) . . ?
O8 La2 O18 77.63(10) . . ?
O10 La2 O18 144.83(10) . . ?
O16 La2 O14 119.61(9) . . ?
O12 La2 O14 65.60(9) . . ?
O8 La2 O14 138.26(9) . . ?
O10 La2 O14 145.40(10) . . ?
O18 La2 O14 69.73(9) . . ?
O16 La2 O14 144.48(10) . 2_666 ?
O12 La2 O14 81.72(9) . 2_666 ?
O8 La2 O14 82.18(9) . 2_666 ?
O10 La2 O14 118.51(9) . 2_666 ?
O18 La2 O14 72.24(9) . 2_666 ?
O14 La2 O14 63.80(10) . 2_666 ?
O16 La2 O15 137.96(9) . 2_666 ?
O12 La2 O15 70.49(10) . 2_666 ?
O8 La2 O15 67.75(10) . 2_666 ?
O10 La2 O15 70.75(9) . 2_666 ?
O18 La2 O15 112.52(10) . 2_666 ?
O14 La2 O15 101.36(8) . 2_666 ?
O14 La2 O15 47.81(8) 2_666 2_666 ?
O16 La2 N4 70.43(10) . . ?
O12 La2 N4 63.03(10) . . ?
O8 La2 N4 123.82(9) . . ?
O10 La2 N4 59.85(9) . . ?
O18 La2 N4 131.84(10) . . ?
O14 La2 N4 97.55(9) . . ?
O14 La2 N4 144.70(10) 2_666 . ?
O15 La2 N4 115.54(10) 2_666 . ?
O16 La2 N3 61.98(9) . . ?
O12 La2 N3 94.47(11) . . ?
O8 La2 N3 129.73(11) . . ?
O10 La2 N3 120.86(9) . . ?
O18 La2 N3 68.41(10) . . ?
O14 La2 N3 59.54(9) . . ?
O14 La2 N3 118.80(8) 2_666 . ?
O15 La2 N3 160.04(9) 2_666 . ?
N4 La2 N3 65.48(10) . . ?
O16 La2 C15 150.88(10) . 2_666 ?
O12 La2 C15 72.35(11) . 2_666 ?
O8 La2 C15 76.09(10) . 2_666 ?
O10 La2 C15 94.73(10) . 2_666 ?
O18 La2 C15 93.80(11) . 2_666 ?
O14 La2 C15 80.77(10) . 2_666 ?
O14 La2 C15 24.04(9) 2_666 2_666 ?
O15 La2 C15 24.02(9) 2_666 2_666 ?
N4 La2 C15 131.03(12) . 2_666 ?
N3 La2 C15 139.86(10) . 2_666 ?
C15 O14 La2 121.7(2) . . ?
C15 O14 La2 98.3(2) . 2_666 ?
La2 O14 La2 116.20(10) . 2_666 ?
C1 O1 La1 123.8(3) . . ?
C1 O1 La1 96.1(2) . 2_767 ?
La1 O1 La1 118.49(10) . 2_767 ?
C7 O7 La1 125.8(3) . . ?
C7 O8 La2 153.9(3) . . ?
La1 O9 H9A 127.6 . . ?
La1 O9 H9B 127.9 . . ?
H9A O9 H9B 104.5 . . ?
La2 O18 H18A 124.4 . . ?
La2 O18 H18B 123.3 . . ?
H18A O18 H18B 104.6 . . ?
C15 O15 La2 90.5(3) . 2_666 ?
C1 O2 La1 92.1(3) . 2_767 ?
C6 O5 La1 130.7(3) . . ?
C17 O16 La2 131.9(3) . . ?
C3 O3 La1 128.8(3) . . ?
C11 O12 La2 128.9(3) . . ?
C13 O11 La1 146.6(3) . 2_667 ?
C13 O10 La2 123.9(3) . . ?
C4 N2 C9 110.7(3) . . ?
C4 N2 C8 109.1(4) . . ?
C9 N2 C8 108.9(3) . . ?
C4 N2 La1 110.3(2) . . ?
C9 N2 La1 111.3(2) . . ?
C8 N2 La1 106.4(2) . . ?
C5 N1 C2 111.9(3) . . ?
C5 N1 C10 110.6(3) . . ?
C2 N1 C10 108.7(3) . . ?
C5 N1 La1 109.7(2) . . ?
C2 N1 La1 110.5(2) . . ?
C10 N1 La1 105.4(3) . . ?
C12 N4 C14 109.3(4) . . ?
C12 N4 C20 111.7(4) . . ?
C14 N4 C20 110.0(3) . . ?
C12 N4 La2 109.2(2) . . ?
C14 N4 La2 105.9(2) . . ?
C20 N4 La2 110.5(2) . . ?
C19 N3 C18 111.8(3) . . ?
C19 N3 C16 108.6(3) . . ?
C18 N3 C16 110.5(4) . . ?
C19 N3 La2 103.9(3) . . ?
C18 N3 La2 110.8(2) . . ?
C16 N3 La2 111.1(2) . . ?
C21 N5 H5C 109.5 . . ?
C21 N5 H5D 109.5 . . ?
H5C N5 H5D 109.5 . . ?
C21 N5 H5E 109.5 . . ?
H5C N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?
N2 C8 C7 111.7(3) . . ?
N2 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
N2 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
O17 C17 O16 123.7(4) . . ?
O17 C17 C18 117.7(4) . . ?
O16 C17 C18 118.5(4) . . ?
O15 C15 O14 122.0(4) . . ?
O15 C15 C16 118.9(4) . . ?
O14 C15 C16 119.0(3) . . ?
O15 C15 La2 65.4(2) . 2_666 ?
O14 C15 La2 57.7(2) . 2_666 ?
C16 C15 La2 168.5(3) . 2_666 ?
N4 C14 C13 112.4(3) . . ?
N4 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
N4 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
O4 C3 O3 125.6(4) . . ?
O4 C3 C4 115.9(4) . . ?
O3 C3 C4 118.5(4) . . ?
N1 C2 C1 112.8(4) . . ?
N1 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
O10 C13 O11 123.5(4) . . ?
O10 C13 C14 118.6(3) . . ?
O11 C13 C14 117.9(3) . . ?
O8 C7 O7 123.6(4) . . ?
O8 C7 C8 117.9(4) . . ?
O7 C7 C8 118.4(4) . . ?
N2 C9 C10 112.5(4) . . ?
N2 C9 H9C 109.1 . . ?
C10 C9 H9C 109.1 . . ?
N2 C9 H9D 109.1 . . ?
C10 C9 H9D 109.1 . . ?
H9C C9 H9D 107.8 . . ?
O2 C1 O1 122.2(4) . . ?
O2 C1 C2 118.7(4) . . ?
O1 C1 C2 119.0(4) . . ?
O2 C1 La1 63.8(2) . 2_767 ?
O1 C1 La1 59.7(2) . 2_767 ?
C2 C1 La1 166.3(3) . 2_767 ?
N2 C4 C3 118.4(3) . . ?
N2 C4 H4A 107.7 . . ?
C3 C4 H4A 107.7 . . ?
N2 C4 H4B 107.7 . . ?
C3 C4 H4B 107.7 . . ?
H4A C4 H4B 107.1 . . ?
N3 C16 C15 112.6(4) . . ?
N3 C16 H16A 109.1 . . ?
C15 C16 H16A 109.1 . . ?
N3 C16 H16B 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C22 N6 H6A 109.5 . . ?
C22 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C22 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
N3 C19 C20 113.2(3) . . ?
N3 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
N3 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
O5 C6 O6 124.3(4) . . ?
O5 C6 C5 118.7(4) . . ?
O6 C6 C5 117.0(4) . . ?
N1 C10 C9 112.3(3) . . ?
N1 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
O13 C11 O12 124.5(4) . . ?
O13 C11 C12 117.5(4) . . ?
O12 C11 C12 118.0(4) . . ?
N6 C22 C21 114.3(4) . . ?
N6 C22 H22A 108.7 . . ?
C21 C22 H22A 108.7 . . ?
N6 C22 H22B 108.7 . . ?
C21 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
N4 C12 C11 116.5(4) . . ?
N4 C12 H12A 108.2 . . ?
C11 C12 H12A 108.2 . . ?
N4 C12 H12B 108.2 . . ?
C11 C12 H12B 108.2 . . ?
H12A C12 H12B 107.3 . . ?
N1 C5 C6 115.1(4) . . ?
N1 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
N1 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N4 C20 C19 113.1(3) . . ?
N4 C20 H20A 109.0 . . ?
C19 C20 H20A 109.0 . . ?
N4 C20 H20B 109.0 . . ?
C19 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N3 C18 C17 113.2(4) . . ?
N3 C18 H18C 108.9 . . ?
C17 C18 H18C 108.9 . . ?
N3 C18 H18D 108.9 . . ?
C17 C18 H18D 108.9 . . ?
H18C C18 H18D 107.7 . . ?
N5 C21 C22 113.4(4) . . ?
N5 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
N5 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?

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
C4 N2 C8 C7 75.5(4) . . . . ?
C9 N2 C8 C7 -163.5(3) . . . . ?
La1 N2 C8 C7 -43.5(4) . . . . ?
La2 O16 C17 O17 177.5(3) . . . . ?
La2 O16 C17 C18 -6.4(6) . . . . ?
La2 O15 C15 O14 -11.5(4) 2_666 . . . ?
La2 O15 C15 C16 168.0(4) 2_666 . . . ?
La2 O14 C15 O15 140.3(3) . . . . ?
La2 O14 C15 O15 12.4(4) 2_666 . . . ?
La2 O14 C15 C16 -39.2(5) . . . . ?
La2 O14 C15 C16 -167.1(3) 2_666 . . . ?
La2 O14 C15 La2 127.9(3) . . . 2_666 ?
C12 N4 C14 C13 78.4(5) . . . . ?
C20 N4 C14 C13 -158.6(4) . . . . ?
La2 N4 C14 C13 -39.2(4) . . . . ?
La1 O3 C3 O4 167.9(4) . . . . ?
La1 O3 C3 C4 -10.5(6) . . . . ?
C5 N1 C2 C1 149.4(4) . . . . ?
C10 N1 C2 C1 -88.3(4) . . . . ?
La1 N1 C2 C1 26.9(4) . . . . ?
La2 O10 C13 O11 -152.4(3) . . . . ?
La2 O10 C13 C14 25.2(5) . . . . ?
La1 O11 C13 O10 -177.9(3) 2_667 . . . ?
La1 O11 C13 C14 4.5(8) 2_667 . . . ?
N4 C14 C13 O10 15.4(6) . . . . ?
N4 C14 C13 O11 -166.9(4) . . . . ?
La2 O8 C7 O7 -147.2(5) . . . . ?
La2 O8 C7 C8 36.0(9) . . . . ?
La1 O7 C7 O8 -176.5(3) . . . . ?
La1 O7 C7 C8 0.3(5) . . . . ?
N2 C8 C7 O8 -149.9(4) . . . . ?
N2 C8 C7 O7 33.1(5) . . . . ?
C4 N2 C9 C10 -83.2(4) . . . . ?
C8 N2 C9 C10 156.8(3) . . . . ?
La1 N2 C9 C10 39.9(4) . . . . ?
La1 O2 C1 O1 -13.1(4) 2_767 . . . ?
La1 O2 C1 C2 164.8(3) 2_767 . . . ?
La1 O1 C1 O2 144.2(3) . . . . ?
La1 O1 C1 O2 13.7(4) 2_767 . . . ?
La1 O1 C1 C2 -33.8(5) . . . . ?
La1 O1 C1 C2 -164.3(3) 2_767 . . . ?
La1 O1 C1 La1 130.5(3) . . . 2_767 ?
N1 C2 C1 O2 -178.5(3) . . . . ?
N1 C2 C1 O1 -0.5(5) . . . . ?
N1 C2 C1 La1 -81.4(13) . . . 2_767 ?
C9 N2 C4 C3 118.6(4) . . . . ?
C8 N2 C4 C3 -121.5(4) . . . . ?
La1 N2 C4 C3 -5.0(5) . . . . ?
O4 C3 C4 N2 -168.7(4) . . . . ?
O3 C3 C4 N2 9.8(7) . . . . ?
C19 N3 C16 C15 -90.4(4) . . . . ?
C18 N3 C16 C15 146.6(4) . . . . ?
La2 N3 C16 C15 23.2(4) . . . . ?
O15 C15 C16 N3 -173.4(4) . . . . ?
O14 C15 C16 N3 6.2(6) . . . . ?
La2 C15 C16 N3 -64.0(16) 2_666 . . . ?
C18 N3 C19 C20 -60.0(5) . . . . ?
C16 N3 C19 C20 177.8(4) . . . . ?
La2 N3 C19 C20 59.5(4) . . . . ?
La1 O5 C6 O6 179.2(3) . . . . ?
La1 O5 C6 C5 -1.4(6) . . . . ?
C5 N1 C10 C9 -62.9(5) . . . . ?
C2 N1 C10 C9 174.0(4) . . . . ?
La1 N1 C10 C9 55.6(4) . . . . ?
N2 C9 C10 N1 -69.2(5) . . . . ?
La2 O12 C11 O13 170.7(4) . . . . ?
La2 O12 C11 C12 -12.3(6) . . . . ?
C14 N4 C12 C11 -137.3(4) . . . . ?
C20 N4 C12 C11 100.7(5) . . . . ?
La2 N4 C12 C11 -21.9(5) . . . . ?
O13 C11 C12 N4 -158.8(4) . . . . ?
O12 C11 C12 N4 24.0(7) . . . . ?
C2 N1 C5 C6 -144.6(4) . . . . ?
C10 N1 C5 C6 94.1(4) . . . . ?
La1 N1 C5 C6 -21.7(4) . . . . ?
O5 C6 C5 N1 17.8(6) . . . . ?
O6 C6 C5 N1 -162.8(4) . . . . ?
C12 N4 C20 C19 -88.5(4) . . . . ?
C14 N4 C20 C19 149.9(4) . . . . ?
La2 N4 C20 C19 33.3(4) . . . . ?
N3 C19 C20 N4 -68.0(5) . . . . ?
C19 N3 C18 C17 94.8(4) . . . . ?
C16 N3 C18 C17 -144.1(4) . . . . ?
La2 N3 C18 C17 -20.5(4) . . . . ?
O17 C17 C18 N3 -164.3(4) . . . . ?
O16 C17 C18 N3 19.3(6) . . . . ?
N6 C22 C21 N5 75.8(6) . . . . ?

_refine_diff_density_max         0.962
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.122



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1949331'
loop_
_audit_author_name
_audit_author_address
zhou
;Xiamen University
China
;
_audit_update_record             
;
2021-07-28 deposited with the CCDC.	2021-08-10 downloaded from the CCDC.
;
_audit_creation_date             2021-06-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H14 K2 La1 N2 O13'
_chemical_formula_sum            'C12 H14 K2 La1 N2 O13'
_chemical_formula_weight         611.37
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
K K 0.2009 0.2494 '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'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   12.3762(2)
_cell_length_b                   12.3762(2)
_cell_length_c                   12.3762(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1895.67(9)
_cell_formula_units_Z            3.99996
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1950
_cell_measurement_theta_min      3.2750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7973
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.659
_diffrn_reflns_theta_min         2.851
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00 -35.00   1.00    5.00    --  -22.85-178.00 150.00   58
  2  ω    -53.00  48.00   1.00    5.00    --  -22.85  38.00  30.00  101
  3  ω    -48.00   6.00   1.00    5.00    --  -22.85 -77.00  60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                1577
_reflns_number_total             1650
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 
;
 Flack x determined using 613 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0380
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0266P)²+5.1864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0802
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1WA(0.33333) H1WB(0.33333)
3.a Rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
La1 La 0.38408(3) 0.38408(3) 0.38408(3) 0.01616(16) Uani 1 3 d S T P . .
K1 K 0.80063(13) 0.69937(13) 0.30063(13) 0.0240(6) Uani 1 3 d S T P . .
K2 K 0.68745(15) 0.18745(15) 0.31255(15) 0.0378(8) Uani 1 3 d S T P . .
O3 O 0.4010(5) 0.2968(4) 0.1871(4) 0.0215(13) Uani 1 1 d . . . . .
O4 O 0.4082(4) 0.4758(4) 0.1939(4) 0.0239(12) Uani 1 1 d . . . . .
N2 N 0.4944(5) 0.5056(5) 0.0056(5) 0.0132(18) Uani 1 3 d S T P . .
O1 O 0.5846(4) 0.3919(5) 0.3401(4) 0.0251(12) Uani 1 1 d . . . . .
N1 N 0.5089(5) 0.5089(5) 0.5089(5) 0.020(2) Uani 1 3 d S T P . .
O2 O 0.7319(5) 0.4950(5) 0.3207(5) 0.0340(13) Uani 1 1 d . . . . .
C4 C 0.4196(5) 0.3887(7) 0.1452(5) 0.0214(13) Uani 1 1 d . . . . .
C3 C 0.4572(6) 0.3924(6) 0.0281(5) 0.0209(13) Uani 1 1 d . . . . .
H3A H 0.515966 0.341823 0.016840 0.025 Uiso 1 1 calc R U . . .
H3B H 0.398285 0.373225 -0.019920 0.025 Uiso 1 1 calc R U . . .
C2 C 0.6408(5) 0.4778(6) 0.3618(6) 0.0222(15) Uani 1 1 d . . . . .
C1 C 0.5931(6) 0.5571(6) 0.4406(6) 0.0245(16) Uani 1 1 d . . . . .
H1A H 0.650203 0.585089 0.486465 0.029 Uiso 1 1 calc R U . . .
H1B H 0.562501 0.617366 0.400962 0.029 Uiso 1 1 calc R U . . .
O1W O 0.8160(6) 0.3160(6) 0.1840(6) 0.059(4) Uani 1 3 d S T P . .
H1WA H 0.821746 0.379679 0.211693 0.088 Uiso 0.3333 1 d R U P . .
H1WB H 0.881010 0.291984 0.183312 0.088 Uiso 0.3333 1 d R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.674(5) . ?
La1 O3 2.674(5) 5 ?
La1 O3 2.674(5) 9 ?
La1 O4 2.630(5) 5 ?
La1 O4 2.630(5) . ?
La1 O4 2.630(5) 9 ?
La1 O1 2.542(5) . ?
La1 O1 2.542(5) 5 ?
La1 O1 2.542(5) 9 ?
La1 N1 2.675(10) . ?
La1 C4 2.989(6) . ?
La1 C4 2.989(6) 9 ?
K1 O3 2.775(6) 10_655 ?
K1 O3 2.775(6) 8_655 ?
K1 O3 2.775(6) 3_655 ?
K1 O2 2.680(6) . ?
K1 O2 2.681(6) 6_566 ?
K1 O2 2.681(6) 12_664 ?
K2 O4 2.875(6) 3_645 ?
K2 O4 2.875(6) 6_556 ?
K2 O4 2.875(6) 9 ?
K2 O1 2.853(6) 8_645 ?
K2 O1 2.853(6) . ?
K2 O1 2.853(6) 11_556 ?
K2 O1W 2.755(14) . ?
O3 C4 1.271(9) . ?
O4 C4 1.244(9) . ?
N2 C3 1.500(8) 10_655 ?
N2 C3 1.500(8) . ?
N2 C3 1.500(8) 7_564 ?
O1 C2 1.299(8) . ?
N1 C1 1.469(8) 9 ?
N1 C1 1.469(8) . ?
N1 C1 1.469(8) 5 ?
O2 C2 1.255(8) . ?
C4 C3 1.523(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 C1 1.505(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
O1W H1WA 0.86(9) 8_645 ?
O1W H1WA 0.8625 . ?
O1W H1WB 0.8579 . ?

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 74.6(2) 9 5 ?
O3 La1 O3 74.6(2) 5 . ?
O3 La1 O3 74.6(2) 9 . ?
O3 La1 C4 74.52(17) . 9 ?
O3 La1 C4 74.52(17) 5 . ?
O3 La1 C4 98.9(2) 9 . ?
O3 La1 C4 25.15(19) . . ?
O3 La1 C4 25.15(19) 9 9 ?
O3 La1 C4 98.9(2) 5 9 ?
O4 La1 O3 49.46(14) 9 9 ?
O4 La1 O3 49.46(13) . . ?
O4 La1 O3 120.62(17) . 9 ?
O4 La1 O3 120.62(17) 9 5 ?
O4 La1 O3 73.03(18) . 5 ?
O4 La1 O3 73.03(18) 5 9 ?
O4 La1 O3 73.03(18) 9 . ?
O4 La1 O3 120.62(17) 5 . ?
O4 La1 O3 49.46(14) 5 5 ?
O4 La1 O4 116.03(7) 5 9 ?
O4 La1 O4 116.03(7) . 9 ?
O4 La1 O4 116.03(7) . 5 ?
O4 La1 N1 101.65(11) . . ?
O4 La1 N1 101.65(11) 5 . ?
O4 La1 N1 101.65(11) 9 . ?
O4 La1 C4 24.52(18) 9 9 ?
O4 La1 C4 93.76(19) 9 . ?
O4 La1 C4 123.81(17) . 9 ?
O4 La1 C4 123.81(17) 5 . ?
O4 La1 C4 24.52(18) . . ?
O4 La1 C4 93.76(19) 5 9 ?
O1 La1 O3 116.46(19) . 9 ?
O1 La1 O3 75.15(17) 9 9 ?
O1 La1 O3 75.15(17) . . ?
O1 La1 O3 116.46(19) 9 5 ?
O1 La1 O3 143.14(18) 5 9 ?
O1 La1 O3 75.15(17) 5 5 ?
O1 La1 O3 143.14(18) . 5 ?
O1 La1 O3 143.14(18) 9 . ?
O1 La1 O3 116.46(19) 5 . ?
O1 La1 O4 164.07(16) 9 . ?
O1 La1 O4 164.07(16) . 5 ?
O1 La1 O4 71.42(18) 9 9 ?
O1 La1 O4 68.70(19) 5 . ?
O1 La1 O4 68.70(19) 9 5 ?
O1 La1 O4 71.41(18) . . ?
O1 La1 O4 164.07(16) 5 9 ?
O1 La1 O4 71.42(18) 5 5 ?
O1 La1 O4 68.70(19) . 9 ?
O1 La1 O1 100.38(15) 5 . ?
O1 La1 O1 100.38(15) 9 5 ?
O1 La1 O1 100.38(15) 9 . ?
O1 La1 N1 62.50(12) 5 . ?
O1 La1 N1 62.50(12) . . ?
O1 La1 N1 62.50(12) 9 . ?
O1 La1 C4 69.14(17) . . ?
O1 La1 C4 92.9(2) 5 . ?
O1 La1 C4 69.14(17) 9 9 ?
O1 La1 C4 164.5(2) 9 . ?
O1 La1 C4 92.9(2) . 9 ?
O1 La1 C4 164.5(2) 5 9 ?
N1 La1 O3 135.58(13) . 5 ?
N1 La1 O3 135.58(13) . 9 ?
N1 La1 O3 135.59(13) . . ?
N1 La1 C4 118.37(14) . 9 ?
N1 La1 C4 118.37(15) . . ?
C4 La1 C4 99.29(18) . 9 ?
O3 K1 La1 42.41(11) 3_655 3_655 ?
O3 K1 La1 42.41(11) 8_655 3_655 ?
O3 K1 La1 42.41(11) 10_655 3_655 ?
O3 K1 O3 71.47(18) 8_655 3_655 ?
O3 K1 O3 71.47(17) 10_655 8_655 ?
O3 K1 O3 71.47(18) 10_655 3_655 ?
O2 K1 La1 114.52(15) . 3_655 ?
O2 K1 La1 114.52(15) 12_664 3_655 ?
O2 K1 La1 114.52(15) 6_566 3_655 ?
O2 K1 O3 155.0(2) . 8_655 ?
O2 K1 O3 83.91(18) . 10_655 ?
O2 K1 O3 83.91(18) 12_664 8_655 ?
O2 K1 O3 96.86(17) 6_566 8_655 ?
O2 K1 O3 96.86(17) . 3_655 ?
O2 K1 O3 96.86(17) 12_664 10_655 ?
O2 K1 O3 83.91(18) 6_566 3_655 ?
O2 K1 O3 155.0(2) 6_566 10_655 ?
O2 K1 O3 155.0(2) 12_664 3_655 ?
O2 K1 O2 103.98(17) . 6_566 ?
O2 K1 O2 103.98(17) . 12_664 ?
O2 K1 O2 103.98(17) 6_566 12_664 ?
La1 K2 La1 112.52(3) 4_556 . ?
La1 K2 La1 112.52(3) 3_645 . ?
La1 K2 La1 112.52(3) 3_645 4_556 ?
O4 K2 La1 93.77(11) 6_556 . ?
O4 K2 La1 32.37(10) 6_556 4_556 ?
O4 K2 La1 98.77(12) 3_645 . ?
O4 K2 La1 93.77(11) 9 3_645 ?
O4 K2 La1 98.77(12) 6_556 3_645 ?
O4 K2 La1 32.37(10) 9 . ?
O4 K2 La1 93.77(11) 3_645 4_556 ?
O4 K2 La1 98.77(12) 9 4_556 ?
O4 K2 La1 32.37(10) 3_645 3_645 ?
O4 K2 O4 70.23(17) 3_645 9 ?
O4 K2 O4 70.23(17) 9 6_556 ?
O4 K2 O4 70.23(17) 3_645 6_556 ?
O1 K2 La1 135.00(11) 11_556 . ?
O1 K2 La1 30.25(11) 11_556 4_556 ?
O1 K2 La1 108.18(11) 8_645 . ?
O1 K2 La1 30.25(11) 8_645 3_645 ?
O1 K2 La1 135.00(11) . 3_645 ?
O1 K2 La1 30.25(11) . . ?
O1 K2 La1 108.18(11) 11_556 3_645 ?
O1 K2 La1 108.18(11) . 4_556 ?
O1 K2 La1 135.00(11) 8_645 4_556 ?
O1 K2 O4 105.58(16) . 6_556 ?
O1 K2 O4 61.28(15) 8_645 3_645 ?
O1 K2 O4 128.86(17) 11_556 9 ?
O1 K2 O4 128.86(17) 8_645 6_556 ?
O1 K2 O4 61.28(15) 11_556 6_556 ?
O1 K2 O4 105.58(16) 11_556 3_645 ?
O1 K2 O4 61.28(15) . 9 ?
O1 K2 O4 128.86(17) . 3_645 ?
O1 K2 O4 105.58(16) 8_645 9 ?
O1 K2 O1 116.65(7) . 8_645 ?
O1 K2 O1 116.65(7) 8_645 11_556 ?
O1 K2 O1 116.65(7) . 11_556 ?
O1W K2 La1 106.22(4) . . ?
O1W K2 La1 106.22(4) . 3_645 ?
O1W K2 La1 106.22(4) . 4_556 ?
O1W K2 O4 138.38(11) . 6_556 ?
O1W K2 O4 138.38(10) . 3_645 ?
O1W K2 O4 138.38(10) . 9 ?
O1W K2 O1 79.32(12) . 11_556 ?
O1W K2 O1 79.32(12) . . ?
O1W K2 O1 79.32(12) . 8_645 ?
La1 O3 K1 93.18(17) . 3_645 ?
C4 O3 La1 91.4(4) . . ?
C4 O3 K1 125.0(5) . 3_645 ?
La1 O4 K2 111.81(17) . 3_655 ?
C4 O4 La1 94.1(4) . . ?
C4 O4 K2 145.4(4) . 3_655 ?
C3 N2 C3 113.8(4) 7_564 . ?
C3 N2 C3 113.8(4) 10_655 7_564 ?
C3 N2 C3 113.8(4) 10_655 . ?
La1 O1 K2 115.3(2) . . ?
C2 O1 La1 120.6(4) . . ?
C2 O1 K2 120.8(4) . . ?
C1 N1 La1 108.2(5) . . ?
C1 N1 La1 108.2(5) 5 . ?
C1 N1 La1 108.2(5) 9 . ?
C1 N1 C1 110.7(5) . 9 ?
C1 N1 C1 110.7(5) 9 5 ?
C1 N1 C1 110.7(5) . 5 ?
C2 O2 K1 118.9(5) . . ?
O3 C4 La1 63.4(3) . . ?
O3 C4 C3 118.1(7) . . ?
O4 C4 La1 61.4(3) . . ?
O4 C4 O3 123.9(6) . . ?
O4 C4 C3 118.0(6) . . ?
C3 C4 La1 170.6(5) . . ?
N2 C3 C4 107.4(6) . . ?
N2 C3 H3A 110.2 . . ?
N2 C3 H3B 110.2 . . ?
C4 C3 H3A 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
O1 C2 C1 117.3(6) . . ?
O2 C2 O1 122.4(7) . . ?
O2 C2 C1 120.3(6) . . ?
N1 C1 C2 112.7(6) . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
K2 O1W H1WA 110(10) . 8_645 ?
K2 O1W H1WA 110.3 . . ?
K2 O1W H1WB 110.3 . . ?
H1WA O1W H1WA 108.7 . 8_645 ?
H1WA O1W H1WB 104.1 . . ?
H1WB O1W H1WA 113.1 . 8_645 ?

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
La1 O3 C4 O4 -10.9(7) . . . . ?
La1 O3 C4 C3 169.6(5) . . . . ?
La1 O4 C4 O3 11.2(8) . . . . ?
La1 O4 C4 C3 -169.4(5) . . . . ?
La1 O1 C2 O2 -163.6(5) . . . . ?
La1 O1 C2 C1 17.2(8) . . . . ?
La1 N1 C1 C2 -42.6(6) . . . . ?
K1 O3 C4 La1 94.9(4) 3_645 . . . ?
K1 O3 C4 O4 83.9(8) 3_645 . . . ?
K1 O3 C4 C3 -95.5(7) 3_645 . . . ?
K1 O2 C2 O1 154.0(5) . . . . ?
K1 O2 C2 C1 -26.8(9) . . . . ?
K2 O4 C4 La1 -139.6(8) 3_655 . . . ?
K2 O4 C4 O3 -128.4(7) 3_655 . . . ?
K2 O4 C4 C3 51.0(11) 3_655 . . . ?
K2 O1 C2 O2 37.8(9) . . . . ?
K2 O1 C2 C1 -141.4(5) . . . . ?
O3 C4 C3 N2 -168.8(6) . . . . ?
O4 C4 C3 N2 11.7(8) . . . . ?
O1 C2 C1 N1 19.9(9) . . . . ?
O2 C2 C1 N1 -159.3(7) . . . . ?
C3 N2 C3 C4 -145.6(7) 7_564 . . . ?
C3 N2 C3 C4 82.0(9) 10_655 . . . ?
C1 N1 C1 C2 -161.0(6) 5 . . . ?
C1 N1 C1 C2 75.9(10) 9 . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
