# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_co513
_database_code_depnum_ccdc_archive 'CCDC 1547498'
_audit_update_record             
;
2017-06-27 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_co513               
;
PROBLEM: Short Inter D-H..H-D       H2     ..  H5A     ..       2.01 Ang.
RESPONSE: Hydrogens H2, H5A and H5B are all involved in strong, linear hydrogen bonds, and therefore, while the H2-H5A/H5B distances are short, I believe these hydrogen atoms are in the correct locations.
;
_vrf_PLAT417_co513_2             
;
PROBLEM: Short Inter D-H..H-D       H2     ..  H5B     ..       2.05 Ang.
RESPONSE: Hydrogens H2, H5A and H5B are all involved in strong, linear hydrogen bonds, and therefore, while the H2-H5A/H5B distances are short, I believe these hydrogen atoms are in the correct locations.
;
# Added during the CSD deposition process: Tuesday 27 June 2017 11:09 PM
# end Validation Reply Form

_audit_creation_date             2017-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H26 N4 O8, 2(H2 O), 4(Cl)'
_chemical_formula_sum            'C20 H30 Cl4 N4 O10'
_chemical_formula_weight         628.28
_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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   9.8590(11)
_cell_length_b                   6.1687(8)
_cell_length_c                   22.747(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.898(4)
_cell_angle_gamma                90
_cell_volume                     1353.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.822
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1322 before and 0.0455 after correction. The Ratio of minimum to maximum transmission is 0.8439. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13409
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.871
_diffrn_reflns_theta_min         1.830
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2561
_reflns_number_total             3187
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0423
_refine_ls_restrained_S_all      1.026
_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)+(0.0588P)²+0.7715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
O1 O 0.12207(15) 0.8981(2) 0.23106(6) 0.0234(3) Uani 1 1 d . . . . .
O2 O 0.31162(16) 0.7881(3) 0.19764(7) 0.0271(4) Uani 1 1 d . . . . .
H2 H 0.286(4) 0.914(6) 0.1701(16) 0.070(11) Uiso 1 1 d . . . . .
O3 O 0.23761(16) 0.9740(3) 0.49459(7) 0.0265(4) Uani 1 1 d . . . . .
O4 O 0.42490(17) 0.8043(3) 0.54885(7) 0.0313(4) Uani 1 1 d . . . . .
H4 H 0.453(3) 0.943(5) 0.5616(13) 0.050(9) Uiso 1 1 d . . . . .
N1 N 0.16338(17) 0.5738(3) 0.31412(7) 0.0173(4) Uani 1 1 d . . . . .
H1 H 0.096(3) 0.686(5) 0.3161(11) 0.032(7) Uiso 1 1 d . . . . .
N2 N 0.12067(17) 0.5969(3) 0.44804(7) 0.0169(4) Uani 1 1 d . . . . .
H2A H 0.108(3) 0.727(5) 0.4274(11) 0.029(7) Uiso 1 1 d . . . . .
C1 C 0.2178(2) 0.7736(4) 0.23089(9) 0.0202(4) Uani 1 1 d . . . . .
C2 C 0.24166(19) 0.5803(3) 0.27226(9) 0.0184(4) Uani 1 1 d . . . . .
C3 C 0.3379(2) 0.4195(4) 0.26977(10) 0.0216(4) Uani 1 1 d . . . . .
H3 H 0.392439 0.423061 0.239870 0.026 Uiso 1 1 calc R . . . .
C4 C 0.3539(2) 0.2527(4) 0.31161(10) 0.0233(5) Uani 1 1 d . . . . .
H4A H 0.419139 0.140322 0.310497 0.028 Uiso 1 1 calc R . . . .
C5 C 0.2733(2) 0.2516(3) 0.35521(10) 0.0206(4) Uani 1 1 d . . . . .
H5 H 0.283653 0.138303 0.384067 0.025 Uiso 1 1 calc R . . . .
C6 C 0.1784(2) 0.4155(3) 0.35647(9) 0.0172(4) Uani 1 1 d . . . . .
C7 C 0.0872(2) 0.4159(3) 0.40223(9) 0.0176(4) Uani 1 1 d . . . . .
H7A H 0.097206 0.275067 0.423581 0.021 Uiso 1 1 calc R . . . .
H7B H -0.010732 0.429811 0.381005 0.021 Uiso 1 1 calc R . . . .
C8 C 0.2661(2) 0.5875(3) 0.48428(9) 0.0205(4) Uani 1 1 d . . . . .
H8A H 0.330265 0.540660 0.458537 0.025 Uiso 1 1 calc R . . . .
H8B H 0.271725 0.481614 0.517395 0.025 Uiso 1 1 calc R . . . .
C9 C 0.3067(2) 0.8126(4) 0.50984(9) 0.0227(5) Uani 1 1 d . . . . .
C10 C 0.0132(2) 0.6104(3) 0.48697(9) 0.0202(4) Uani 1 1 d . . . . .
H10A H -0.074674 0.666769 0.462656 0.024 Uiso 1 1 calc R . . . .
H10B H 0.045460 0.713589 0.520261 0.024 Uiso 1 1 calc R . . . .
O5 O 0.26238(17) 1.1069(3) 0.12633(7) 0.0257(4) Uani 1 1 d . . . . .
H5A H 0.211(3) 1.200(5) 0.1362(12) 0.031(7) Uiso 1 1 d . . . . .
H5B H 0.336(4) 1.168(6) 0.1204(14) 0.057(10) Uiso 1 1 d . . . . .
Cl1 Cl -0.02706(5) 0.92395(8) 0.35780(2) 0.02095(14) Uani 1 1 d . . . . .
Cl2 Cl 0.53452(5) 1.21269(9) 0.60912(2) 0.02517(15) Uani 1 1 d . . . . .


_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
O1 C1 1.217(3) . ?
O2 H2 1.00(4) . ?
O2 C1 1.313(3) . ?
O3 C9 1.216(3) . ?
O4 H4 0.93(3) . ?
O4 C9 1.312(2) . ?
N1 H1 0.97(3) . ?
N1 C2 1.344(3) . ?
N1 C6 1.358(3) . ?
N2 H2A 0.93(3) . ?
N2 C7 1.516(3) . ?
N2 C8 1.500(3) . ?
N2 C10 1.517(3) . ?
C1 C2 1.508(3) . ?
C2 C3 1.382(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(3) . ?
C4 H4A 0.9500 . ?
C4 C5 1.392(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(3) . ?
C6 C7 1.510(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.527(3) . ?
C10 C10 1.530(4) 3_566 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O5 H5A 0.83(3) . ?
O5 H5B 0.86(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O2 H2 107(2) . . ?
C9 O4 H4 109.8(19) . . ?
C2 N1 H1 121.0(15) . . ?
C2 N1 C6 121.93(18) . . ?
C6 N1 H1 117.1(15) . . ?
C7 N2 H2A 107.6(16) . . ?
C7 N2 C10 111.25(15) . . ?
C8 N2 H2A 109.1(16) . . ?
C8 N2 C7 113.41(16) . . ?
C8 N2 C10 112.61(15) . . ?
C10 N2 H2A 102.1(15) . . ?
O1 C1 O2 126.7(2) . . ?
O1 C1 C2 121.21(19) . . ?
O2 C1 C2 112.05(18) . . ?
N1 C2 C1 115.28(18) . . ?
N1 C2 C3 120.50(19) . . ?
C3 C2 C1 124.21(18) . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.02(19) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4A 120.3 . . ?
C3 C4 C5 119.4(2) . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 H5 120.0 . . ?
N1 C6 C5 119.12(18) . . ?
N1 C6 C7 119.64(18) . . ?
C5 C6 C7 121.18(18) . . ?
N2 C7 H7A 108.9 . . ?
N2 C7 H7B 108.9 . . ?
C6 C7 N2 113.49(16) . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
N2 C8 H8A 110.0 . . ?
N2 C8 H8B 110.0 . . ?
N2 C8 C9 108.69(17) . . ?
H8A C8 H8B 108.3 . . ?
C9 C8 H8A 110.0 . . ?
C9 C8 H8B 110.0 . . ?
O3 C9 O4 126.3(2) . . ?
O3 C9 C8 123.26(18) . . ?
O4 C9 C8 110.42(19) . . ?
N2 C10 C10 111.9(2) . 3_566 ?
N2 C10 H10A 109.2 . . ?
N2 C10 H10B 109.2 . . ?
C10 C10 H10A 109.2 3_566 . ?
C10 C10 H10B 109.2 3_566 . ?
H10A C10 H10B 107.9 . . ?
H5A O5 H5B 109(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O5 1.00(4) 1.54(4) 2.532(2) 174(3) .
O4 H4 Cl2 0.93(3) 2.06(3) 2.9637(18) 166(3) .
N1 H1 Cl1 0.97(3) 2.23(3) 3.1537(18) 158(2) .
N2 H2A Cl1 0.93(3) 2.21(3) 3.0286(18) 147(2) .
O5 H5A Cl1 0.83(3) 2.31(3) 3.1117(18) 165(3) 2
O5 H5B Cl2 0.86(4) 2.15(4) 3.0038(18) 173(3) 4_585
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_co525_sq
_database_code_depnum_ccdc_archive 'CCDC 1559002'
_audit_update_record             
;
2017-06-27 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_mo_co525_sq         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.934 Note
RESPONSE: This was a weakly scattering crystal, no discernible data was available beyond 0.93 Angstroms.
;
_vrf_PLAT213_mo_co525_sq         
;
PROBLEM: Atom O6              has ADP max/min Ratio .....        5.3 prolat
RESPONSE: This is the best data set we could produce, based on the twinning present in the crystal. This resulted in a number of NPD atoms, which was only resolved through the use of the RIGU/SIMU/ISOR commands. The atoms are no longer NPD, however a few still have irregular ADPs.
;
_vrf_PLAT213_mo_co525_sq_2       
;
PROBLEM: Atom N4              has ADP max/min Ratio .....        5.3 prolat
RESPONSE: This is the best data set we could produce, based on the twinning present in the crystal. This resulted in a number of NPD atoms, which was only resolved through the use of the RIGU/SIMU/ISOR commands. The atoms are no longer NPD, however a few still have irregular ADPs.
;
_vrf_PLAT213_mo_co525_sq_3       
;
PROBLEM: Atom C7              has ADP max/min Ratio .....        6.0 prolat
RESPONSE: Author Response: This is the best data set we could produce, based on the twinning present in the crystal. This resulted in a number of NPD atoms, which was only resolved through the use of the RIGU/SIMU/ISOR commands. The atoms are no longer NPD, however a few still have irregular ADPs.
;
_vrf_PLAT308_mo_co525_sq         
;
PROBLEM: Single Bonded Metal Atom in Structure  (Unusual)        La3 Check
RESPONSE: La3 and La3A bridge symmetry equivalent La-Octa complexes. These La atoms are coordinated to acid groups and solvent water molecules.
;
_vrf_PLAT308_mo_co525_sq_2       
;
PROBLEM: Single Bonded Metal Atom in Structure  (Unusual)       La3A Check
RESPONSE: La3 and La3A bridge symmetry equivalent La-Octa complexes. These La atoms are coordinated to acid groups and solvent water molecules.
;
_vrf_PLAT213_mo_co525_sq_4       
;
PROBLEM: Atom O11             has ADP max/min Ratio .....        4.1 prolat
RESPONSE: This is the best data set we could produce, based on the twinning present in the crystal. This resulted in a number of NPD atoms, which was only resolved through the use of the RIGU/SIMU/ISOR commands. The atoms are no longer NPD, however a few still have irregular ADPs.
;
_vrf_PLAT213_mo_co525_sq_5       
;
PROBLEM: Atom N6              has ADP max/min Ratio .....        4.1 prolat
RESPONSE: This is the best data set we could produce, based on the twinning present in the crystal. This resulted in a number of NPD atoms, which was only resolved through the use of the RIGU/SIMU/ISOR commands. The atoms are no longer NPD, however a few still have irregular ADPs.
;
_vrf_PLAT213_mo_co525_sq_6       
;
PROBLEM: Atom C12             has ADP max/min Ratio .....        4.7 prolat
RESPONSE: This is the best data set we could produce, based on the twinning present in the crystal. This resulted in a number of NPD atoms, which was only resolved through the use of the RIGU/SIMU/ISOR commands. The atoms are no longer NPD, however a few still have irregular ADPs.
;
# Added during the CSD deposition process: Tuesday 27 June 2017 11:09 PM
# end Validation Reply Form

_audit_creation_date             2017-06-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H46.3 La2.5 N8 Na0.5 O21.15, 5(H2 O)'
_chemical_formula_sum            'C40 H56.29 La2.50 N8 Na0.50 O26.15'
_chemical_formula_weight         1426.39
_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'
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'
Na Na 0.0362 0.0249 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.703(3)
_cell_length_b                   16.076(6)
_cell_length_c                   20.536(7)
_cell_angle_alpha                82.406(5)
_cell_angle_beta                 84.822(5)
_cell_angle_gamma                90.092(4)
_cell_volume                     2835.9(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5987
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 2:
 wR2(int) was 0.0728 before and 0.0624 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 26539 reflections, Rint = 0.0648
 (12126 with I > 3sig(I), Rint = 0.0529)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       blade
_exptl_crystal_F_000             1419
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8861
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.283
_diffrn_reflns_theta_min         1.278
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7402
_reflns_number_total             8861
_reflns_special_details          
;
 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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.956
_refine_diff_density_min         -2.278
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         8861
_refine_ls_number_restraints     1541
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0786
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1002P)²+69.4212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2130
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.3837(15)
 0.6163(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O1A-H1AA = O1A-H1AB
 0.84 with sigma of 0.01
 O1B-H1BA = O1B-H1BB
 0.84 with sigma of 0.01
 O1C-H1CA = O1C-H1CB
 0.84 with sigma of 0.01
 H1AB-La3A
 -3 with sigma of 0.01
 H1AA-La3A
 -3 with sigma of 0.01
 H1BB-La3
 -3 with sigma of 0.01
 H1BA-La3
 -3 with sigma of 0.01
 H1CB-La3A
 -3 with sigma of 0.01
 H1CA-La3A
 -3 with sigma of 0.01
 H1AA-H1AB
 1.33 with sigma of 0.02
 H1BA-H1BB
 1.33 with sigma of 0.02
 H1CA-H1CB
 1.33 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(Na1) \\sim Ueq, Uanis(Na1A) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(C25) \\sim Ueq, Uanis(O1C) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
Uanis(O1C) \\sim Ueq: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(O17A) = Uanis(O17)
Uanis(O18A) = Uanis(O18)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O17A)=Sof(O18A)=1-FVAR(1)
 Sof(O17)=Sof(O18)=FVAR(1)
 Sof(La3A)=0.5*(1-FVAR(3))
 Sof(La3)=0.5*FVAR(3)
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=FVAR(3)
 Sof(O1C)=Sof(H1CA)=Sof(H1CB)=FVAR(4)
 Fixed Sof: Na1(0.25) Na1A(0.25) O1A(0.33333) H1AA(0.33333) H1AB(0.33333)
7.a Free rotating group:
 O23(H23A,H23B), O24(H24A,H24B), O25(H25A,H25B), O26(H26A,H26B), O1A(H1AA,
 H1AB), O1B(H1BA,H1BB), O1C(H1CA,H1CB), O10(H10C,H10D), O22(H22A,H22B)
7.b Rotating group:
 O9(H9A,H9B), O20(H20A,H20B), O19(H19A,H19B)
7.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C34(H34A,H34B)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24),
 C25(H25), C36(H36), C37(H37), C38(H38)
7.e Fitted hexagon refined as free rotating group:
 N1(C2,C3,C4,C5,C6), N4(C15,C16,C17,C18,C19), N5(C22,C23,C24,C25,C26), N8(C35,
 C36,C37,C38,C39)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.56221(7) 1.25975(3) 0.74305(3) 0.01133(12) Uani 1 1 d . U . . .
La2 La 0.93814(7) 1.17276(3) 0.25893(3) 0.01160(12) Uani 1 1 d . U . . .
La3 La 0.9773(3) 1.01710(11) 0.50881(11) 0.0310(6) Uani 0.3538(16) 1 d D U P A
1
La3A La 0.8857(7) 1.0263(3) 0.50052(19) 0.0351(12) Uani 0.1462(16) 1 d D U P A
2
Na1 Na 0.687(3) 1.2318(15) 0.4455(12) 0.059(4) Uani 0.25 1 d . U P A 2
Na1A Na 0.719(4) 1.2737(16) 0.4407(13) 0.065(5) Uani 0.25 1 d . U P A 1
O1 O 0.4400(14) 1.2976(8) 0.5294(5) 0.081(3) Uani 1 1 d . U . . .
O2 O 0.5499(9) 1.2592(5) 0.6198(4) 0.0272(17) Uani 1 1 d . U . . .
O3 O 0.1793(8) 1.2850(5) 0.9084(4) 0.0206(17) Uani 1 1 d . U . . .
O4 O 0.3941(8) 1.2439(4) 0.8523(4) 0.0155(15) Uani 1 1 d . U . . .
O5 O 1.0471(9) 1.3601(5) 0.6893(4) 0.0311(19) Uani 1 1 d . U . . .
O6 O 0.7888(8) 1.3622(4) 0.7001(4) 0.0203(16) Uani 1 1 d . U . . .
O7 O 0.5470(10) 0.9727(4) 0.7432(4) 0.0288(17) Uani 1 1 d . U . . .
O8 O 0.4841(8) 1.1097(4) 0.7370(4) 0.0211(16) Uani 1 1 d . U . . .
O9 O 0.2724(8) 1.2480(5) 0.7202(4) 0.0212(17) Uani 1 1 d . U . . .
H9A H 0.217134 1.221750 0.755257 0.032 Uiso 1 1 d GR . . . .
H9B H 0.262019 1.219538 0.686679 0.032 Uiso 1 1 d GR . . . .
O11 O 0.9486(9) 0.8864(4) 0.2588(4) 0.0270(18) Uani 1 1 d . U . . .
O12 O 1.0132(8) 1.0197(5) 0.2674(4) 0.0214(15) Uani 1 1 d . U . . .
O13 O 0.4563(9) 1.2483(6) 0.3160(5) 0.046(2) Uani 1 1 d . U . . .
O14 O 0.7141(8) 1.2587(5) 0.3042(4) 0.0262(15) Uani 1 1 d . U . . .
O15 O 1.3149(8) 1.2559(5) 0.0941(4) 0.0206(17) Uani 1 1 d . U . . .
O16 O 1.0978(8) 1.1956(4) 0.1482(4) 0.0155(14) Uani 1 1 d . U . . .
O17 O 1.065(3) 1.1505(14) 0.4796(11) 0.046(2) Uani 0.405(15) 1 d . U P A 1
O17A O 1.151(2) 1.1283(9) 0.4588(8) 0.046(2) Uani 0.595(15) 1 d . U P A 2
O18 O 0.951(3) 1.1374(12) 0.3822(10) 0.0303(16) Uani 0.405(15) 1 d . U P A 1
O18A O 0.9814(18) 1.1257(9) 0.3855(7) 0.0303(16) Uani 0.595(15) 1 d . U P A 2
O20 O 1.2327(8) 1.1543(5) 0.2762(4) 0.0239(17) Uani 1 1 d . U . . .
H20A H 1.252695 1.164333 0.316751 0.036 Uiso 1 1 d GR . . . .
H20B H 1.292737 1.189731 0.246862 0.036 Uiso 1 1 d GR . . . .
N1 N 0.4699(6) 1.4004(3) 0.6694(2) 0.0182(16) Uani 1 1 d . U . . .
C2 C 0.4317(8) 1.3901(4) 0.6067(3) 0.030(2) Uani 1 1 d G U . . .
C3 C 0.3684(11) 1.4562(5) 0.5676(3) 0.043(3) Uani 1 1 d G U . . .
H3 H 0.342285 1.449208 0.524727 0.052 Uiso 1 1 calc R . . . .
C4 C 0.3432(11) 1.5326(4) 0.5913(4) 0.051(3) Uani 1 1 d G U . . .
H4 H 0.299881 1.577756 0.564671 0.062 Uiso 1 1 calc R . . . .
C5 C 0.3813(10) 1.5429(3) 0.6541(4) 0.033(2) Uani 1 1 d G U . . .
H5 H 0.364133 1.595040 0.670329 0.039 Uiso 1 1 calc R . . . .
C6 C 0.4447(8) 1.4768(3) 0.6931(3) 0.0176(18) Uani 1 1 d G U . . .
N2 N 0.4812(9) 1.4024(5) 0.8050(4) 0.0152(15) Uani 1 1 d . U . . .
N3 N 0.7679(10) 1.3021(5) 0.8307(5) 0.0192(15) Uani 1 1 d . U . . .
N4 N 0.6693(5) 1.1364(3) 0.8287(2) 0.0150(15) Uani 1 1 d . U . . .
C15 C 0.7544(6) 1.1529(3) 0.8798(3) 0.0200(18) Uani 1 1 d G U . . .
C16 C 0.8161(8) 1.0871(4) 0.9197(3) 0.021(2) Uani 1 1 d G U . . .
H16 H 0.874175 1.098330 0.954602 0.025 Uiso 1 1 calc R . . . .
C17 C 0.7927(8) 1.0048(3) 0.9085(3) 0.023(2) Uani 1 1 d G U . . .
H17 H 0.834905 0.959798 0.935756 0.028 Uiso 1 1 calc R . . . .
C18 C 0.7077(8) 0.9883(3) 0.8574(3) 0.0186(19) Uani 1 1 d G U . . .
H18 H 0.691763 0.932083 0.849719 0.022 Uiso 1 1 calc R . . . .
C19 C 0.6460(6) 1.0542(3) 0.8175(3) 0.0191(18) Uani 1 1 d G U . . .
N5 N 0.8292(5) 1.0794(3) 0.1735(2) 0.0152(15) Uani 1 1 d . U . . .
C22 C 0.8548(6) 0.9935(3) 0.1840(3) 0.0123(15) Uani 1 1 d G U . . .
C23 C 0.7952(8) 0.9412(3) 0.1435(3) 0.0184(19) Uani 1 1 d G U . . .
H23 H 0.812637 0.882502 0.150661 0.022 Uiso 1 1 calc R . . . .
C24 C 0.7099(8) 0.9747(4) 0.0924(3) 0.022(2) Uani 1 1 d G U . . .
H24 H 0.669163 0.938949 0.064717 0.026 Uiso 1 1 calc R . . . .
C25 C 0.6843(7) 1.0606(4) 0.0819(3) 0.0179(18) Uani 1 1 d G U . . .
H25 H 0.626094 1.083482 0.047034 0.022 Uiso 1 1 calc R . . . .
C26 C 0.7440(6) 1.1129(3) 0.1225(2) 0.0166(17) Uani 1 1 d G U . . .
N6 N 0.7331(9) 1.2441(5) 0.1730(5) 0.0183(15) Uani 1 1 d . U . . .
N7 N 1.0137(9) 1.3376(5) 0.1970(4) 0.0167(15) Uani 1 1 d . U . . .
N8 N 1.0436(6) 1.2885(3) 0.3315(2) 0.0201(16) Uani 1 1 d . U . . .
C35 C 1.0634(7) 1.3731(3) 0.3072(3) 0.0161(18) Uani 1 1 d G U . . .
C36 C 1.1419(9) 1.4258(3) 0.3418(4) 0.030(2) Uani 1 1 d G U . . .
H36 H 1.155496 1.483563 0.325149 0.037 Uiso 1 1 calc R . . . .
C37 C 1.2007(10) 1.3939(5) 0.4006(4) 0.040(3) Uani 1 1 d G U . . .
H37 H 1.254355 1.429876 0.424184 0.048 Uiso 1 1 calc R . . . .
C38 C 1.1808(10) 1.3093(5) 0.4249(3) 0.040(3) Uani 1 1 d G U . . .
H38 H 1.220969 1.287487 0.465091 0.048 Uiso 1 1 calc R . . . .
C39 C 1.1023(8) 1.2566(3) 0.3904(3) 0.031(2) Uani 1 1 d G U . . .
C1 C 0.4776(16) 1.3126(8) 0.5824(6) 0.037(2) Uani 1 1 d . U . . .
C7 C 0.4953(11) 1.4822(6) 0.7555(5) 0.0133(17) Uani 1 1 d . U . . .
H7A H 0.436161 1.526711 0.775125 0.016 Uiso 1 1 calc R . . . .
H7B H 0.605033 1.500285 0.749222 0.016 Uiso 1 1 calc R . . . .
C8 C 0.3196(13) 1.3875(6) 0.8276(5) 0.017(2) Uani 1 1 d . U . . .
H8A H 0.257507 1.393567 0.789161 0.021 Uiso 1 1 calc R . . . .
H8B H 0.284272 1.429724 0.856416 0.021 Uiso 1 1 calc R . . . .
C9 C 0.2952(12) 1.2985(6) 0.8660(5) 0.0162(19) Uani 1 1 d . U . . .
C10 C 0.5730(11) 1.4101(6) 0.8607(5) 0.0189(19) Uani 1 1 d . U . . .
H10A H 0.528972 1.372250 0.899902 0.023 Uiso 1 1 calc R . . . .
H10B H 0.566968 1.468352 0.871413 0.023 Uiso 1 1 calc R . . . .
C11 C 0.7423(11) 1.3882(6) 0.8452(5) 0.017(2) Uani 1 1 d . U . . .
H11A H 0.786169 1.427607 0.806905 0.020 Uiso 1 1 calc R . . . .
H11B H 0.799463 1.396937 0.883382 0.020 Uiso 1 1 calc R . . . .
C12 C 0.9185(11) 1.3019(6) 0.7923(6) 0.018(2) Uani 1 1 d . U . . .
H12A H 0.950855 1.243148 0.790773 0.021 Uiso 1 1 calc R . . . .
H12B H 0.995753 1.329954 0.814840 0.021 Uiso 1 1 calc R . . . .
C13 C 0.9162(12) 1.3446(7) 0.7245(6) 0.026(2) Uani 1 1 d . U . . .
C14 C 0.7630(12) 1.2426(7) 0.8916(5) 0.020(2) Uani 1 1 d . U . . .
H14A H 0.672156 1.254702 0.921270 0.024 Uiso 1 1 calc R . . . .
H14B H 0.856463 1.250973 0.914201 0.024 Uiso 1 1 calc R . . . .
C20 C 0.5527(14) 1.0462(6) 0.7624(5) 0.0180(16) Uani 1 1 d . U . . .
C21 C 0.9479(13) 0.9636(5) 0.2395(5) 0.0164(15) Uani 1 1 d . U . . .
C27 C 0.7312(13) 1.2079(7) 0.1125(6) 0.024(2) Uani 1 1 d . U . . .
H27A H 0.818091 1.231920 0.081173 0.029 Uiso 1 1 calc R . . . .
H27B H 0.634175 1.223291 0.092489 0.029 Uiso 1 1 calc R . . . .
C28 C 0.5783(12) 1.2264(7) 0.2127(6) 0.0206(19) Uani 1 1 d . U . . .
H28A H 0.549682 1.166695 0.213339 0.025 Uiso 1 1 calc R . . . .
H28B H 0.498607 1.261038 0.191004 0.025 Uiso 1 1 calc R . . . .
C29 C 0.5816(12) 1.2455(7) 0.2834(6) 0.026(2) Uani 1 1 d . U . . .
C30 C 0.7524(13) 1.3372(6) 0.1589(6) 0.023(2) Uani 1 1 d . U . . .
H30A H 0.713782 1.362782 0.198465 0.028 Uiso 1 1 calc R . . . .
H30B H 0.690252 1.358942 0.122449 0.028 Uiso 1 1 calc R . . . .
C31 C 0.9197(11) 1.3623(6) 0.1402(5) 0.017(2) Uani 1 1 d . U . . .
H31A H 0.960180 1.334568 0.102036 0.021 Uiso 1 1 calc R . . . .
H31B H 0.927895 1.423781 0.127044 0.021 Uiso 1 1 calc R . . . .
C32 C 1.1803(12) 1.3323(6) 0.1719(5) 0.0170(18) Uani 1 1 d . U . . .
H32A H 1.245432 1.326965 0.209341 0.020 Uiso 1 1 calc R . . . .
H32B H 1.212327 1.384076 0.142009 0.020 Uiso 1 1 calc R . . . .
C33 C 1.2015(11) 1.2566(6) 0.1351(5) 0.0141(18) Uani 1 1 d . U . . .
C34 C 1.0002(11) 1.3998(6) 0.2451(5) 0.0170(18) Uani 1 1 d . U . . .
H34A H 1.053286 1.452433 0.224368 0.020 Uiso 1 1 calc R . . . .
H34B H 0.889731 1.412534 0.254312 0.020 Uiso 1 1 calc R . . . .
C40 C 1.0672(18) 1.1680(8) 0.4128(7) 0.0423(19) Uani 1 1 d . U . . .
O23 O 0.4709(8) 1.4017(4) 0.0424(4) 0.038(2) Uani 1 1 d . U . . .
H23A H 0.426443 1.365004 0.071603 0.057 Uiso 1 1 d G . . . .
H23B H 0.522708 1.377424 0.013334 0.057 Uiso 1 1 d G . . . .
O24 O 0.7507(7) 1.4765(4) 0.0016(4) 0.027(2) Uani 1 1 d . U . . .
H24A H 0.696884 1.463879 -0.028456 0.041 Uiso 1 1 d G . . . .
H24B H 0.821186 1.511421 -0.015457 0.041 Uiso 1 1 d G . . . .
O25 O 1.0255(10) 1.4143(5) 0.9593(4) 0.038(2) Uani 1 1 d . U . . .
H25A H 1.075519 1.391510 0.929027 0.056 Uiso 1 1 d G . . . .
H25B H 0.993452 1.376577 0.990676 0.056 Uiso 1 1 d G . . . .
O26 O 1.0424(9) 1.1699(5) 0.0125(4) 0.032(2) Uani 1 1 d . U . . .
H26A H 1.001923 1.210726 -0.010213 0.048 Uiso 1 1 d G . . . .
H26B H 1.044699 1.180272 0.051899 0.048 Uiso 1 1 d G . . . .
O1A O 0.7988(19) 1.0150(15) 0.6194(3) 0.061(8) Uani 0.3333 1 d D U P A 2
H1AA H 0.858229 1.028511 0.646934 0.091 Uiso 0.3333 1 d DG . P A 2
H1AB H 0.706950 1.028411 0.632155 0.091 Uiso 0.3333 1 d DG . P A 2
O1B O 1.125(2) 1.0717(9) 0.6002(4) 0.058(6) Uani 0.50(2) 1 d D U P A 1
H1BA H 1.068639 1.064909 0.636444 0.087 Uiso 0.50(2) 1 d DG . P A 1
H1BB H 1.189263 1.111642 0.601633 0.087 Uiso 0.50(2) 1 d DG . P A 1
O1C O 1.045(3) 0.9605(8) 0.4047(5) 0.040(4) Uani 0.315(19) 1 d D U P A 2
H1CA H 0.981874 0.932379 0.387005 0.060 Uiso 0.315(19) 1 d DG . P A 2
H1CB H 1.131090 0.963063 0.380709 0.060 Uiso 0.315(19) 1 d DG . P A 2
O10 O 0.7948(8) 1.1812(5) 0.6879(4) 0.0240(17) Uani 1 1 d . U . B -1
H10C H 0.886229 1.148258 0.690432 0.00(2) Uiso 1 1 d G . . B -1
H10D H 0.829623 1.234201 0.664146 0.01(2) Uiso 1 1 d G . . B -1
O22 O 0.4536(10) 1.1748(5) 0.9882(4) 0.034(2) Uani 1 1 d . U . . .
H22A H 0.422896 1.201744 0.952210 0.051 Uiso 1 1 d G . . . .
H22B H 0.402453 1.191742 1.022250 0.051 Uiso 1 1 d G . . . .
O19 O 0.7028(9) 1.0754(5) 0.3161(4) 0.0277(18) Uani 1 1 d . U . . .
H19A H 0.737065 1.027118 0.337442 0.042 Uiso 1 1 d GR . . . .
H19B H 0.640604 1.062037 0.285996 0.042 Uiso 1 1 d GR . . . .


_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 O2 2.544(8) . ?
La1 O4 2.549(7) . ?
La1 O6 2.583(7) . ?
La1 O8 2.527(7) . ?
La1 O9 2.618(7) . ?
La1 N1 2.714(5) . ?
La1 N2 2.827(8) . ?
La1 N3 2.794(9) . ?
La1 N4 2.696(4) . ?
La1 O10 2.635(7) . ?
La2 O12 2.534(7) . ?
La2 O14 2.568(7) . ?
La2 O16 2.539(7) . ?
La2 O18 2.53(2) . ?
La2 O18A 2.669(15) . ?
La2 O20 2.631(7) . ?
La2 N5 2.687(4) . ?
La2 N6 2.767(9) . ?
La2 N7 2.833(8) . ?
La2 N8 2.739(5) . ?
La2 O19 2.663(7) . ?
La3 La3 0.786(4) 2_776 ?
La3 O17 2.26(2) . ?
La3 O17 2.69(2) 2_776 ?
La3 C40 2.972(13) . ?
La3 O1B 2.612(13) . ?
La3 O1B 3.008(12) 2_776 ?
La3A La3A 2.162(12) 2_776 ?
La3A Na1 3.82(3) . ?
La3A O17A 2.526(15) 2_776 ?
La3A O17A 2.833(17) . ?
La3A O18A 2.733(14) . ?
La3A C40 3.052(14) . ?
La3A O1A 2.473(7) . ?
La3A O1C 2.642(15) . ?
La3A O1C 2.124(15) 2_776 ?
Na1 O1 2.92(3) . ?
Na1 O14 2.86(3) . ?
Na1A O1 2.95(3) . ?
Na1A O14 2.85(3) . ?
O1 C1 1.220(17) . ?
O2 C1 1.279(15) . ?
O3 C9 1.270(12) . ?
O4 C9 1.271(12) . ?
O5 C13 1.298(13) . ?
O6 C13 1.275(13) . ?
O7 C20 1.298(12) . ?
O8 C20 1.260(12) . ?
O11 C21 1.253(11) . ?
O12 C21 1.288(13) . ?
O13 C29 1.232(14) . ?
O14 C29 1.292(14) . ?
O15 C33 1.239(12) . ?
O16 C33 1.316(12) . ?
O17 C40 1.36(3) . ?
O17A C40 1.34(2) . ?
O18 C40 1.36(3) . ?
O18A C40 1.23(2) . ?
N1 C2 1.3900 . ?
N1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 C1 1.445(14) . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.405(12) . ?
N2 C7 1.524(12) . ?
N2 C8 1.449(14) . ?
N2 C10 1.471(14) . ?
N3 C11 1.467(14) . ?
N3 C12 1.467(13) . ?
N3 C14 1.468(13) . ?
N4 C15 1.3900 . ?
N4 C19 1.3900 . ?
C15 C16 1.3900 . ?
C15 C14 1.496(12) . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.468(12) . ?
N5 C22 1.3900 . ?
N5 C26 1.3900 . ?
C22 C23 1.3900 . ?
C22 C21 1.485(11) . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C26 C27 1.519(11) . ?
N6 C27 1.442(15) . ?
N6 C28 1.515(13) . ?
N6 C30 1.493(13) . ?
N7 C31 1.497(14) . ?
N7 C32 1.501(13) . ?
N7 C34 1.493(14) . ?
N8 C35 1.3900 . ?
N8 C39 1.3900 . ?
C35 C36 1.3900 . ?
C35 C34 1.447(12) . ?
C36 C37 1.3900 . ?
C37 C38 1.3900 . ?
C38 C39 1.3900 . ?
C39 C40 1.461(13) . ?
C8 C9 1.545(13) . ?
C10 C11 1.530(14) . ?
C12 C13 1.470(16) . ?
C28 C29 1.526(17) . ?
C30 C31 1.512(14) . ?
C32 C33 1.519(14) . ?
O1A O1C 1.44(3) 2_776 ?

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
O2 La1 O4 142.2(2) . . ?
O2 La1 O6 81.1(2) . . ?
O2 La1 O9 71.6(2) . . ?
O2 La1 N1 61.1(2) . . ?
O2 La1 N2 121.8(2) . . ?
O2 La1 N3 139.5(3) . . ?
O2 La1 N4 126.7(2) . . ?
O2 La1 O10 66.9(2) . . ?
O4 La1 O6 130.2(2) . . ?
O4 La1 O9 70.8(2) . . ?
O4 La1 N1 107.07(19) . . ?
O4 La1 N2 59.7(2) . . ?
O4 La1 N3 77.7(2) . . ?
O4 La1 N4 69.64(18) . . ?
O4 La1 O10 137.6(2) . . ?
O6 La1 O9 135.5(2) . . ?
O6 La1 N1 67.60(19) . . ?
O6 La1 N2 77.7(2) . . ?
O6 La1 N3 60.6(3) . . ?
O6 La1 N4 107.74(19) . . ?
O6 La1 O10 68.9(2) . . ?
O8 La1 O2 77.7(2) . . ?
O8 La1 O4 85.6(2) . . ?
O8 La1 O6 138.8(2) . . ?
O8 La1 O9 68.5(2) . . ?
O8 La1 N1 127.5(2) . . ?
O8 La1 N2 143.3(2) . . ?
O8 La1 N3 122.5(2) . . ?
O8 La1 N4 61.2(2) . . ?
O8 La1 O10 70.3(2) . . ?
O9 La1 N1 68.58(19) . . ?
O9 La1 N2 87.5(2) . . ?
O9 La1 N3 145.9(3) . . ?
O9 La1 N4 116.69(19) . . ?
O9 La1 O10 126.1(2) . . ?
N1 La1 N2 60.7(2) . . ?
N1 La1 N3 110.0(2) . . ?
N3 La1 N2 65.0(3) . . ?
N4 La1 N1 171.05(15) . . ?
N4 La1 N2 111.4(2) . . ?
N4 La1 N3 61.4(2) . . ?
O10 La1 N1 115.3(2) . . ?
O10 La1 N2 144.0(2) . . ?
O10 La1 N3 86.3(3) . . ?
O10 La1 N4 68.2(2) . . ?
O12 La2 O14 137.0(2) . . ?
O12 La2 O16 87.8(2) . . ?
O12 La2 O18A 74.0(4) . . ?
O12 La2 O20 68.8(2) . . ?
O12 La2 N5 62.1(2) . . ?
O12 La2 N6 123.2(3) . . ?
O12 La2 N7 145.3(2) . . ?
O12 La2 N8 125.8(2) . . ?
O12 La2 O19 69.8(2) . . ?
O14 La2 O18A 85.1(4) . . ?
O14 La2 O20 136.5(3) . . ?
O14 La2 N5 108.0(2) . . ?
O14 La2 N6 61.3(3) . . ?
O14 La2 N7 77.5(2) . . ?
O14 La2 N8 69.3(2) . . ?
O14 La2 O19 68.0(2) . . ?
O16 La2 O14 129.8(2) . . ?
O16 La2 O18A 138.3(4) . . ?
O16 La2 O20 70.1(2) . . ?
O16 La2 N5 68.80(18) . . ?
O16 La2 N6 76.3(2) . . ?
O16 La2 N7 59.8(2) . . ?
O16 La2 N8 106.09(19) . . ?
O16 La2 O19 137.6(2) . . ?
O18 La2 O12 79.0(5) . . ?
O18 La2 O14 78.4(5) . . ?
O18 La2 O16 144.3(5) . . ?
O18 La2 O20 74.2(5) . . ?
O18 La2 N5 129.2(5) . . ?
O18 La2 N6 138.2(5) . . ?
O18 La2 N7 119.5(5) . . ?
O18 La2 N8 59.2(5) . . ?
O18 La2 O19 67.6(5) . . ?
O18A La2 N5 127.8(3) . . ?
O18A La2 N6 144.8(4) . . ?
O18A La2 N7 121.2(4) . . ?
O18A La2 N8 60.8(3) . . ?
O20 La2 O18A 68.4(4) . . ?
O20 La2 N5 115.4(2) . . ?
O20 La2 N6 144.0(2) . . ?
O20 La2 N7 87.4(2) . . ?
O20 La2 N8 67.8(2) . . ?
O20 La2 O19 127.6(2) . . ?
N5 La2 N6 61.2(2) . . ?
N5 La2 N7 111.0(2) . . ?
N5 La2 N8 171.21(13) . . ?
N6 La2 N7 64.2(2) . . ?
N8 La2 N6 111.1(2) . . ?
N8 La2 N7 60.5(2) . . ?
O19 La2 O18A 70.5(4) . . ?
O19 La2 N5 68.9(2) . . ?
O19 La2 N6 86.4(3) . . ?
O19 La2 N7 142.7(2) . . ?
O19 La2 N8 116.3(2) . . ?
La3 La3 O17 115.6(8) 2_776 . ?
La3 La3 O17 49.2(6) 2_776 2_776 ?
La3 La3 C40 99.4(4) 2_776 . ?
La3 La3 O1B 53.0(5) 2_776 2_776 ?
La3 La3 O1B 113.1(5) 2_776 . ?
O17 La3 O17 164.8(2) . 2_776 ?
O17 La3 C40 25.9(7) . . ?
O17 La3 C40 143.3(6) 2_776 . ?
O17 La3 O1B 56.8(6) 2_776 2_776 ?
O17 La3 O1B 67.6(7) . . ?
O17 La3 O1B 116.3(6) . 2_776 ?
C40 La3 O1B 90.5(4) . 2_776 ?
O1B La3 O17 115.7(6) . 2_776 ?
O1B La3 C40 92.2(4) . . ?
O1B La3 O1B 166.10(10) . 2_776 ?
La3A La3A Na1 139.9(5) 2_776 . ?
La3A La3A O17A 58.9(4) 2_776 . ?
La3A La3A O18A 88.2(4) 2_776 . ?
La3A La3A C40 80.3(4) 2_776 . ?
La3A La3A O1A 103.4(5) 2_776 . ?
La3A La3A O1C 51.3(5) 2_776 . ?
O17A La3A Na1 81.3(5) . . ?
O17A La3A Na1 145.6(6) 2_776 . ?
O17A La3A O17A 132.8(4) 2_776 . ?
O17A La3A O18A 137.9(5) 2_776 . ?
O17A La3A C40 149.7(5) 2_776 . ?
O17A La3A C40 26.1(4) . . ?
O17A La3A O1C 79.3(5) 2_776 . ?
O18A La3A Na1 58.1(5) . . ?
O18A La3A O17A 46.7(5) . . ?
O18A La3A C40 23.7(4) . . ?
C40 La3A Na1 60.1(5) . . ?
O1A La3A Na1 97.6(6) . . ?
O1A La3A O17A 115.5(6) . . ?
O1A La3A O18A 148.6(7) . . ?
O1A La3A C40 129.1(6) . . ?
O1A La3A O1C 147.6(6) . . ?
O1C La3A Na1 104.9(6) 2_776 . ?
O1C La3A Na1 114.8(5) . . ?
O1C La3A O17A 71.8(6) . . ?
O1C La3A O17A 82.1(7) 2_776 . ?
O1C La3A O18A 125.8(6) 2_776 . ?
O1C La3A O18A 60.3(4) . . ?
O1C La3A C40 72.1(4) . . ?
O1C La3A C40 102.1(6) 2_776 . ?
O1C La3A O1A 35.4(8) 2_776 . ?
O1C La3A O1C 127.4(4) 2_776 . ?
O1 Na1 La3A 121.6(8) . . ?
O14 Na1 La3A 108.0(7) . . ?
O14 Na1 O1 124.7(10) . . ?
O14 Na1A O1 123.9(12) . . ?
C1 O1 Na1 114.5(11) . . ?
C1 O1 Na1A 109.7(11) . . ?
C1 O2 La1 125.0(7) . . ?
C9 O4 La1 121.8(6) . . ?
C13 O6 La1 115.5(6) . . ?
C20 O8 La1 124.5(7) . . ?
C21 O12 La2 124.9(6) . . ?
La2 O14 Na1 110.0(6) . . ?
La2 O14 Na1A 113.5(7) . . ?
C29 O14 La2 115.6(7) . . ?
C29 O14 Na1 109.3(9) . . ?
C29 O14 Na1A 117.2(10) . . ?
C33 O16 La2 120.5(6) . . ?
La3 O17 La3 15.2(2) . 2_776 ?
C40 O17 La3 107.7(14) . . ?
C40 O17 La3 98.6(13) . 2_776 ?
La3A O17A La3A 47.2(4) 2_776 . ?
C40 O17A La3A 86.1(10) . . ?
C40 O17A La3A 121.8(11) . 2_776 ?
C40 O18 La2 121.0(13) . . ?
La2 O18A La3A 147.2(6) . . ?
C40 O18A La2 119.1(10) . . ?
C40 O18A La3A 92.9(10) . . ?
C2 N1 La1 115.6(2) . . ?
C2 N1 C6 120.0 . . ?
C6 N1 La1 124.1(2) . . ?
N1 C2 C3 120.0 . . ?
N1 C2 C1 116.8(6) . . ?
C3 C2 C1 122.8(6) . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
N1 C6 C7 115.5(5) . . ?
C5 C6 N1 120.0 . . ?
C5 C6 C7 124.4(5) . . ?
C7 N2 La1 111.0(6) . . ?
C8 N2 La1 103.3(6) . . ?
C8 N2 C7 108.5(7) . . ?
C8 N2 C10 111.0(8) . . ?
C10 N2 La1 112.0(6) . . ?
C10 N2 C7 110.7(8) . . ?
C11 N3 La1 110.6(6) . . ?
C11 N3 C14 111.2(9) . . ?
C12 N3 La1 103.2(6) . . ?
C12 N3 C11 107.0(8) . . ?
C12 N3 C14 111.4(8) . . ?
C14 N3 La1 113.0(6) . . ?
C15 N4 La1 122.3(2) . . ?
C15 N4 C19 120.0 . . ?
C19 N4 La1 117.5(2) . . ?
N4 C15 C14 116.3(5) . . ?
C16 C15 N4 120.0 . . ?
C16 C15 C14 123.5(5) . . ?
C15 C16 C17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C17 C18 C19 120.0 . . ?
N4 C19 C20 114.0(5) . . ?
C18 C19 N4 120.0 . . ?
C18 C19 C20 126.0(5) . . ?
C22 N5 La2 117.2(2) . . ?
C22 N5 C26 120.0 . . ?
C26 N5 La2 122.8(2) . . ?
N5 C22 C23 120.0 . . ?
N5 C22 C21 116.1(4) . . ?
C23 C22 C21 123.9(4) . . ?
C24 C23 C22 120.0 . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C26 120.0 . . ?
N5 C26 C27 115.8(5) . . ?
C25 C26 N5 120.0 . . ?
C25 C26 C27 124.0(5) . . ?
C27 N6 La2 115.2(6) . . ?
C27 N6 C28 108.5(8) . . ?
C27 N6 C30 110.6(9) . . ?
C28 N6 La2 102.6(6) . . ?
C30 N6 La2 112.2(6) . . ?
C30 N6 C28 107.1(8) . . ?
C31 N7 La2 111.5(6) . . ?
C31 N7 C32 109.5(8) . . ?
C32 N7 La2 103.8(5) . . ?
C34 N7 La2 111.7(6) . . ?
C34 N7 C31 111.6(8) . . ?
C34 N7 C32 108.5(8) . . ?
C35 N8 La2 122.9(2) . . ?
C35 N8 C39 120.0 . . ?
C39 N8 La2 116.2(2) . . ?
N8 C35 C36 120.0 . . ?
N8 C35 C34 115.7(5) . . ?
C36 C35 C34 124.3(5) . . ?
C35 C36 C37 120.0 . . ?
C38 C37 C36 120.0 . . ?
C37 C38 C39 120.0 . . ?
N8 C39 C40 115.1(6) . . ?
C38 C39 N8 120.0 . . ?
C38 C39 C40 124.8(6) . . ?
O1 C1 O2 121.7(13) . . ?
O1 C1 C2 120.0(12) . . ?
O2 C1 C2 118.2(10) . . ?
C6 C7 N2 116.6(8) . . ?
N2 C8 C9 110.4(8) . . ?
O3 C9 O4 124.9(9) . . ?
O3 C9 C8 118.4(9) . . ?
O4 C9 C8 116.7(9) . . ?
N2 C10 C11 112.0(9) . . ?
N3 C11 C10 114.8(8) . . ?
N3 C12 C13 112.7(9) . . ?
O5 C13 C12 118.2(9) . . ?
O6 C13 O5 121.0(11) . . ?
O6 C13 C12 120.8(9) . . ?
N3 C14 C15 113.2(8) . . ?
O7 C20 C19 116.6(8) . . ?
O8 C20 O7 124.3(10) . . ?
O8 C20 C19 119.1(8) . . ?
O11 C21 O12 124.4(10) . . ?
O11 C21 C22 118.0(9) . . ?
O12 C21 C22 117.4(7) . . ?
N6 C27 C26 113.0(8) . . ?
N6 C28 C29 111.9(9) . . ?
O13 C29 O14 124.9(11) . . ?
O13 C29 C28 116.9(10) . . ?
O14 C29 C28 118.1(9) . . ?
N6 C30 C31 111.3(8) . . ?
N7 C31 C30 110.4(9) . . ?
N7 C32 C33 109.1(8) . . ?
O15 C33 O16 123.6(9) . . ?
O15 C33 C32 118.2(9) . . ?
O16 C33 C32 118.2(8) . . ?
C35 C34 N7 115.0(8) . . ?
O17 C40 La3 46.4(10) . . ?
O17 C40 C39 111.4(13) . . ?
O17A C40 La3A 67.8(9) . . ?
O17A C40 C39 117.6(12) . . ?
O18 C40 La3 80.4(10) . . ?
O18 C40 O17 118.7(17) . . ?
O18 C40 C39 113.1(13) . . ?
O18A C40 La3A 63.4(9) . . ?
O18A C40 O17A 118.3(13) . . ?
O18A C40 C39 123.3(12) . . ?
C39 C40 La3 156.9(8) . . ?
C39 C40 La3A 152.6(9) . . ?
O1C O1A La3A 58.9(6) 2_776 . ?
La3 O1B La3 13.90(10) . 2_776 ?
La3A O1C La3A 52.6(4) 2_776 . ?
O1A O1C La3A 123.7(11) 2_776 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O23 H23A O15 0.85 1.98 2.745(10) 148.8 1_455
O24 H24B O25 0.85 2.27 2.857(11) 126.0 2_786
O25 H25A O3 0.85 2.01 2.746(11) 143.7 1_655
O26 H26B O16 0.85 2.12 2.950(11) 167.9 .
O1A H1AA O12 0.85 2.22 2.955(15) 144.6 2_776
O10 H10C O11 0.96 1.89 2.739(11) 145.8 2_776
O10 H10D O6 0.96 2.29 2.954(10) 125.3 .
O22 H22A O4 0.87 2.11 2.955(11) 163.4 .
O22 H22B O15 0.87 2.01 2.858(11) 166.3 1_456
O19 H19B O7 0.90 1.90 2.744(12) 155.2 2_676

# SQUEEZE RESULTS (Version =  21116)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 117 51 ' '
2 0.479 0.084 0.586 18 7 ' '
3 0.521 0.916 0.414 18 8 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.3837(15)
2 0.6163(15)

