# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2002456'
_audit_update_record             
;
2020-05-13 deposited with the CCDC.	2020-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F8 K La O8 P4'
_chemical_formula_weight         581.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.164(4)
_cell_length_b                   15.382(5)
_cell_length_c                   9.247(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.892(4)
_cell_angle_gamma                90
_cell_volume                     1383.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2395
_cell_measurement_theta_min      2.094
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   0.6717
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.979
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   face-indexed
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8371
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.094
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3131
_reflns_number_gt                2684
_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. 
  
 _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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0202P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3131
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0605
_refine_ls_wR_factor_gt          0.0576
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
K1 K 0.35340(10) 0.15123(6) 0.44067(11) 0.0329(2) Uani 1 1 d . . . A 1
La1 La 0.71823(2) 0.58360(2) 0.50957(2) 0.01624(7) Uani 1 1 d . . . B 1
P1 P 0.38020(10) 0.54909(7) 0.19831(12) 0.0218(2) Uani 1 1 d . . . B 1
P2 P 0.58785(10) 0.34494(7) 0.41184(13) 0.0238(2) Uani 1 1 d . . . A 1
P3 P 1.07842(11) 0.51637(7) 0.72481(12) 0.0245(2) Uani 1 1 d . . . B 1
P4 P 0.86990(11) 0.77250(7) 0.35322(12) 0.0264(2) Uani 1 1 d . . . B 1
O1 O 0.5152(3) 0.58876(16) 0.2704(3) 0.0267(6) Uani 1 1 d . . . B 1
O2 O 0.4602(3) 0.31345(17) 0.4381(3) 0.0267(6) Uani 1 1 d . . . A 1
O3 O 0.3371(3) 0.46744(17) 0.2527(3) 0.0275(6) Uani 1 1 d . . . B 1
O4 O 0.9354(3) 0.51199(18) 0.6306(3) 0.0325(7) Uani 1 1 d . . . B 1
O5 O 0.7587(3) 0.72102(17) 0.3822(3) 0.0323(7) Uani 1 1 d . . . B 1
O6 O 1.1826(3) 0.45488(18) 0.7035(3) 0.0278(6) Uani 1 1 d . . . . .
O7 O 0.6383(3) 0.43173(17) 0.4651(3) 0.0319(7) Uani 1 1 d . . . . .
F1 F 0.3720(3) 0.53629(18) 0.0294(3) 0.0457(7) Uani 1 1 d . . . B 1
F2 F 0.2675(3) 0.61727(17) 0.1798(3) 0.0478(7) Uani 1 1 d . . . B 1
F3 F 0.5733(3) 0.33821(18) 0.2418(3) 0.0541(8) Uani 1 1 d . . . A 1
F4 F 1.0803(3) 0.5118(2) 0.8906(3) 0.0599(9) Uani 1 1 d . . . B 1
F5 F 0.6999(3) 0.27765(17) 0.4707(4) 0.0564(9) Uani 1 1 d . . . . .
F6 F 1.1325(3) 0.60846(17) 0.7211(4) 0.0690(11) Uani 1 1 d . . . . .
F7 F 1.0015(3) 0.7208(2) 0.3966(4) 0.0652(10) Uani 1 1 d . . . . .
F8 F 0.9059(4) 0.84529(19) 0.4727(3) 0.0752(11) Uani 1 1 d . . . . .
O8 O 0.8485(3) 0.81044(18) 0.2034(3) 0.0321(7) 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
K1 O2 2.724(3) . ?
K1 O1 2.834(3) 2_645 ?
K1 O6 2.877(3) 4_465 ?
K1 F8 2.970(4) 3_666 ?
K1 O5 2.988(3) 3_666 ?
K1 F1 2.990(3) 4_566 ?
K1 F3 3.026(3) 4_566 ?
K1 O5 3.064(3) 2_645 ?
K1 O8 3.224(3) 2_645 ?
K1 F1 3.247(3) 2_645 ?
K1 P4 3.5259(16) 2_645 ?
K1 P4 3.5600(17) 3_666 ?
La1 O4 2.430(3) . ?
La1 O7 2.469(3) . ?
La1 O8 2.498(3) 4_576 ?
La1 O5 2.511(3) . ?
La1 O6 2.531(3) 3_766 ?
La1 O3 2.546(3) 3_666 ?
La1 O1 2.550(3) . ?
La1 O2 2.557(3) 3_666 ?
P1 O3 1.466(3) . ?
P1 O1 1.473(3) . ?
P1 F2 1.526(3) . ?
P1 F1 1.552(3) . ?
P2 O7 1.463(3) . ?
P2 O2 1.470(3) . ?
P2 F5 1.518(3) . ?
P2 F3 1.539(3) . ?
P3 O4 1.463(3) . ?
P3 O6 1.475(3) . ?
P3 F6 1.523(3) . ?
P3 F4 1.529(3) . ?
P4 O8 1.460(3) . ?
P4 O5 1.467(3) . ?
P4 F7 1.507(3) . ?
P4 F8 1.540(3) . ?

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 K1 O1 92.06(8) . 2_645 ?
O2 K1 O6 131.83(9) . 4_465 ?
O1 K1 O6 65.38(8) 2_645 4_465 ?
O2 K1 F8 111.89(8) . 3_666 ?
O1 K1 F8 145.56(9) 2_645 3_666 ?
O6 K1 F8 80.18(8) 4_465 3_666 ?
O2 K1 O5 67.57(8) . 3_666 ?
O1 K1 O5 158.69(8) 2_645 3_666 ?
O6 K1 O5 123.32(9) 4_465 3_666 ?
F8 K1 O5 47.98(8) 3_666 3_666 ?
O2 K1 F1 153.19(9) . 4_566 ?
O1 K1 F1 81.78(8) 2_645 4_566 ?
O6 K1 F1 68.77(8) 4_465 4_566 ?
F8 K1 F1 86.20(8) 3_666 4_566 ?
O5 K1 F1 119.20(8) 3_666 4_566 ?
O2 K1 F3 76.66(8) . 4_566 ?
O1 K1 F3 106.39(9) 2_645 4_566 ?
O6 K1 F3 148.50(8) 4_465 4_566 ?
F8 K1 F3 103.10(9) 3_666 4_566 ?
O5 K1 F3 75.96(8) 3_666 4_566 ?
F1 K1 F3 80.11(8) 4_566 4_566 ?
O2 K1 O5 72.96(8) . 2_645 ?
O1 K1 O5 64.14(8) 2_645 2_645 ?
O6 K1 O5 58.99(8) 4_465 2_645 ?
F8 K1 O5 98.56(9) 3_666 2_645 ?
O5 K1 O5 102.17(6) 3_666 2_645 ?
F1 K1 O5 125.55(8) 4_566 2_645 ?
F3 K1 O5 147.56(8) 4_566 2_645 ?
O2 K1 O8 60.52(8) . 2_645 ?
O1 K1 O8 110.10(8) 2_645 2_645 ?
O6 K1 O8 86.86(8) 4_465 2_645 ?
F8 K1 O8 65.77(8) 3_666 2_645 ?
O5 K1 O8 55.16(8) 3_666 2_645 ?
F1 K1 O8 145.92(8) 4_566 2_645 ?
F3 K1 O8 123.41(8) 4_566 2_645 ?
O5 K1 O8 47.11(7) 2_645 2_645 ?
O2 K1 F1 99.49(8) . 2_645 ?
O1 K1 F1 46.26(7) 2_645 2_645 ?
O6 K1 F1 93.98(8) 4_465 2_645 ?
F8 K1 F1 142.66(9) 3_666 2_645 ?
O5 K1 F1 140.05(8) 3_666 2_645 ?
F1 K1 F1 57.79(9) 4_566 2_645 ?
F3 K1 F1 64.17(7) 4_566 2_645 ?
O5 K1 F1 109.93(7) 2_645 2_645 ?
O8 K1 F1 151.27(8) 2_645 2_645 ?
O2 K1 P4 71.19(7) . 2_645 ?
O1 K1 P4 88.58(7) 2_645 2_645 ?
O6 K1 P4 66.54(7) 4_465 2_645 ?
F8 K1 P4 77.02(8) 3_666 2_645 ?
O5 K1 P4 79.16(7) 3_666 2_645 ?
F1 K1 P4 134.21(6) 4_566 2_645 ?
F3 K1 P4 144.95(6) 4_566 2_645 ?
O5 K1 P4 24.46(5) 2_645 2_645 ?
O8 K1 P4 24.46(5) 2_645 2_645 ?
F1 K1 P4 134.32(6) 2_645 2_645 ?
O2 K1 P4 91.16(6) . 3_666 ?
O1 K1 P4 169.04(7) 2_645 3_666 ?
O6 K1 P4 104.93(7) 4_465 3_666 ?
F8 K1 P4 25.28(6) 3_666 3_666 ?
O5 K1 P4 23.91(5) 3_666 3_666 ?
F1 K1 P4 99.81(6) 4_566 3_666 ?
F3 K1 P4 84.54(6) 4_566 3_666 ?
O5 K1 P4 106.97(6) 2_645 3_666 ?
O8 K1 P4 62.79(6) 2_645 3_666 ?
F1 K1 P4 143.10(6) 2_645 3_666 ?
P4 K1 P4 82.56(4) 2_645 3_666 ?
O4 La1 O7 81.88(10) . . ?
O4 La1 O8 75.19(10) . 4_576 ?
O7 La1 O8 144.80(10) . 4_576 ?
O4 La1 O5 110.30(10) . . ?
O7 La1 O5 144.03(10) . . ?
O8 La1 O5 70.28(10) 4_576 . ?
O4 La1 O6 74.82(9) . 3_766 ?
O7 La1 O6 80.52(10) . 3_766 ?
O8 La1 O6 117.60(9) 4_576 3_766 ?
O5 La1 O6 71.04(9) . 3_766 ?
O4 La1 O3 82.06(10) . 3_666 ?
O7 La1 O3 72.99(9) . 3_666 ?
O8 La1 O3 77.62(9) 4_576 3_666 ?
O5 La1 O3 140.52(9) . 3_666 ?
O6 La1 O3 146.93(9) 3_766 3_666 ?
O4 La1 O1 144.24(9) . . ?
O7 La1 O1 74.97(9) . . ?
O8 La1 O1 136.75(9) 4_576 . ?
O5 La1 O1 76.62(9) . . ?
O6 La1 O1 74.76(9) 3_766 . ?
O3 La1 O1 115.61(9) 3_666 . ?
O4 La1 O2 142.47(9) . 3_666 ?
O7 La1 O2 113.60(9) . 3_666 ?
O8 La1 O2 73.58(9) 4_576 3_666 ?
O5 La1 O2 77.83(9) . 3_666 ?
O6 La1 O2 139.20(9) 3_766 3_666 ?
O3 La1 O2 71.40(9) 3_666 3_666 ?
O1 La1 O2 72.85(9) . 3_666 ?
O4 La1 K1 116.56(7) . 2_655 ?
O7 La1 K1 96.71(7) . 2_655 ?
O8 La1 K1 117.30(7) 4_576 2_655 ?
O5 La1 K1 47.36(7) . 2_655 ?
O6 La1 K1 43.13(6) 3_766 2_655 ?
O3 La1 K1 157.83(7) 3_666 2_655 ?
O1 La1 K1 42.23(6) . 2_655 ?
O2 La1 K1 96.16(7) 3_666 2_655 ?
O4 La1 K1 123.65(7) . 3_666 ?
O7 La1 K1 151.62(7) . 3_666 ?
O8 La1 K1 50.15(7) 4_576 3_666 ?
O5 La1 K1 44.75(7) . 3_666 ?
O6 La1 K1 115.74(6) 3_766 3_666 ?
O3 La1 K1 96.68(6) 3_666 3_666 ?
O1 La1 K1 86.69(6) . 3_666 ?
O2 La1 K1 38.87(6) 3_666 3_666 ?
K1 La1 K1 83.145(18) 2_655 3_666 ?
O3 P1 O1 122.11(17) . . ?
O3 P1 F2 109.74(16) . . ?
O1 P1 F2 109.66(17) . . ?
O3 P1 F1 107.61(16) . . ?
O1 P1 F1 106.17(16) . . ?
F2 P1 F1 98.96(16) . . ?
O3 P1 K1 144.19(12) . 2_655 ?
O1 P1 K1 45.25(11) . 2_655 ?
F2 P1 K1 105.84(11) . 2_655 ?
F1 P1 K1 62.04(10) . 2_655 ?
O3 P1 K1 63.44(12) . 4_565 ?
O1 P1 K1 120.02(12) . 4_565 ?
F2 P1 K1 124.35(13) . 4_565 ?
F1 P1 K1 45.85(11) . 4_565 ?
K1 P1 K1 93.01(4) 2_655 4_565 ?
O7 P2 O2 118.99(17) . . ?
O7 P2 F5 110.40(17) . . ?
O2 P2 F5 108.82(16) . . ?
O7 P2 F3 109.00(17) . . ?
O2 P2 F3 108.61(16) . . ?
F5 P2 F3 99.19(18) . . ?
O4 P3 O6 121.20(17) . . ?
O4 P3 F6 109.39(17) . . ?
O6 P3 F6 108.41(17) . . ?
O4 P3 F4 108.43(17) . . ?
O6 P3 F4 107.71(16) . . ?
F6 P3 F4 99.5(2) . . ?
O8 P4 O5 118.59(18) . . ?
O8 P4 F7 109.87(17) . . ?
O5 P4 F7 109.73(17) . . ?
O8 P4 F8 109.19(18) . . ?
O5 P4 F8 107.26(19) . . ?
F7 P4 F8 100.7(2) . . ?
O8 P4 K1 66.11(12) . 2_655 ?
O5 P4 K1 59.85(13) . 2_655 ?
F7 P4 K1 104.39(15) . 2_655 ?
F8 P4 K1 154.55(16) . 2_655 ?
O8 P4 K1 115.70(12) . 3_666 ?
O5 P4 K1 55.61(12) . 3_666 ?
F7 P4 K1 133.32(14) . 3_666 ?
F8 P4 K1 55.42(15) . 3_666 ?
K1 P4 K1 102.67(5) 2_655 3_666 ?
P1 O1 La1 142.43(16) . . ?
P1 O1 K1 113.09(15) . 2_655 ?
La1 O1 K1 100.56(9) . 2_655 ?
P2 O2 La1 122.40(15) . 3_666 ?
P2 O2 K1 132.56(15) . . ?
La1 O2 K1 105.04(9) 3_666 . ?
P1 O3 La1 136.31(16) . 3_666 ?
P3 O4 La1 149.98(18) . . ?
P4 O5 La1 141.24(17) . . ?
P4 O5 K1 100.47(14) . 3_666 ?
La1 O5 K1 98.98(10) . 3_666 ?
P4 O5 K1 95.69(14) . 2_655 ?
La1 O5 K1 95.56(9) . 2_655 ?
K1 O5 K1 132.19(11) 3_666 2_655 ?
P3 O6 La1 135.87(16) . 3_766 ?
P3 O6 K1 124.04(15) . 4_666 ?
La1 O6 K1 99.91(9) 3_766 4_666 ?
P2 O7 La1 170.3(2) . . ?
P1 F1 K1 112.27(13) . 4_565 ?
P1 F1 K1 92.98(11) . 2_655 ?
K1 F1 K1 122.21(9) 4_565 2_655 ?
P2 F3 K1 139.68(16) . 4_565 ?
P4 F8 K1 99.31(16) . 3_666 ?
P4 O8 La1 147.49(17) . 4_575 ?
P4 O8 K1 89.43(13) . 2_655 ?
La1 O8 K1 93.34(9) 4_575 2_655 ?

_refine_diff_density_max         0.537
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.131

####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 2002457'
_audit_update_record             
;
2020-07-12 deposited with the CCDC.	2020-07-22 downloaded from the CCDC.
;
_audit_creation_date             2020-07-12
_audit_creation_method           
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r1) 
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F8 La O8 P4, H4 N'
_chemical_formula_sum            'F8 H4 La N O8 P4'
_chemical_formula_weight         560.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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                   10.190(4)
_cell_length_b                   15.511(6)
_cell_length_c                   9.228(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.583(5)
_cell_angle_gamma                90
_cell_volume                     1397.8(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3513
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   0.712
_shelx_estimated_absorpt_T_min   0.560
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5215
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_process_details   
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1182 before and 0.0476 after correction. 
The Ratio of minimum to maximum transmission is 0.6994. 
The λ/2 correction factor is Not present. 
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_min   0.5215
_exptl_transmission_factor_max   0.7456
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8510
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         2.464
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2714
_reflns_number_total             3153
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0076(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+1.1861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0793
_refine_special_details          ?
_olex2_refinement_description    
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All N(H,H,H,H) groups 
2. Restrained distances 
 N1-H1A = N1-H1B = N1-H1C = N1-H1D 
 0.9 with sigma of 0.02 
 H1A-H1B = H1A-H1C = H1A-H1D = H1B-H1C = H1B-H1D = H1C-H1D 
 1.35 with sigma of 0.02 
 N1-H1A \\sim N1-H1B \\sim N1-H1C \\sim N1-H1D 
 with sigma of 0.02 
 H1A-H1B \\sim H1B-H1C \\sim H1C-H1D \\sim H1D-H1A \\sim H1B-H1D \\sim H1A-H1C 
 with sigma of 0.04 
3. Uiso/Uaniso restraints and constraints 
N1 \\sim H1A \\sim H1B \\sim H1C \\sim H1D: within 1.7A with sigma of 0.04 and 
sigma for terminal atoms of 0.08 
Uanis(F7) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.01 
Uanis(F8) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.004 
4. Rigid body (RIGU) restrains 
 N1, H1A, H1B, H1C, H1D 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 H1D, H1A, N1, H1B, H1C 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
;
_atom_sites_solution_hydrogens   difmap
_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 0.72062(2) 1.08222(2) 0.01651(3) 0.01923(11) Uani 1 1 d . . . . .
P1 P 0.58984(11) 0.84557(7) -0.08348(13) 0.0254(3) Uani 1 1 d . . . . .
P2 P 0.38505(12) 1.05349(7) -0.29898(13) 0.0257(2) Uani 1 1 d . . . . .
P3 P 1.08027(11) 1.01713(8) 0.22823(13) 0.0293(3) Uani 1 1 d . . . . .
P4 P 0.88395(12) 1.23436(7) 0.35236(13) 0.0294(3) Uani 1 1 d . . . . .
O1 O 0.3392(3) 0.97018(19) -0.2543(3) 0.0302(7) Uani 1 1 d . . . . .
O2 O 0.5202(3) 1.08943(19) -0.2225(4) 0.0317(7) Uani 1 1 d . . . . .
O3 O 1.1866(3) 0.9607(2) 0.1995(3) 0.0328(7) Uani 1 1 d . . . . .
O4 O 0.4585(3) 0.81561(19) -0.0658(4) 0.0317(7) Uani 1 1 d . . . . .
O5 O 0.7782(4) 1.2845(2) 0.3952(4) 0.0427(9) Uani 1 1 d . . . . .
O6 O 0.8440(3) 1.1854(2) 0.2136(4) 0.0502(10) Uani 1 1 d . . . . .
O7 O 0.6388(3) 0.93175(18) -0.0285(4) 0.0332(7) Uani 1 1 d . . . . .
O8 O 0.9391(3) 1.0129(2) 0.1351(4) 0.0362(8) Uani 1 1 d . . . . .
F1 F 0.5842(3) 0.8378(2) -0.2508(3) 0.0539(8) Uani 1 1 d . . . . .
F2 F 0.2746(3) 1.12176(19) -0.3089(4) 0.0479(8) Uani 1 1 d . . . . .
F3 F 0.3762(3) 1.0468(2) -0.4693(3) 0.0474(8) Uani 1 1 d . . . . .
F4 F 0.6999(3) 0.7786(2) -0.0163(4) 0.0562(9) Uani 1 1 d . . . . .
F5 F 1.0829(4) 1.0048(3) 0.3923(3) 0.0755(12) Uani 1 1 d . . . . .
F6 F 1.1313(4) 1.1093(2) 0.2347(6) 0.0833(14) Uani 1 1 d . . . . .
F7 F 1.0019(3) 1.2914(3) 0.3547(6) 0.0889(14) Uani 1 1 d . U . . .
F8 F 0.9531(5) 1.1742(3) 0.4811(5) 0.1049(15) Uani 1 1 d . U . . .
N1 N 0.3469(4) 0.8527(2) -0.5461(5) 0.0371(9) Uani 1 1 d D U . . .
H1A H 0.308(4) 0.8899(19) -0.611(3) 0.045 Uiso 1 1 d DR U . . .
H1B H 0.392(3) 0.877(2) -0.467(3) 0.045 Uiso 1 1 d DR U . . .
H1C H 0.284(3) 0.822(2) -0.529(4) 0.045 Uiso 1 1 d DR U . . .
H1D H 0.398(3) 0.821(2) -0.580(4) 0.045 Uiso 1 1 d DR 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 O1 2.571(3) 3_675 ?
La1 O2 2.545(3) . ?
La1 O3 2.527(3) 3_775 ?
La1 O4 2.554(3) 3_675 ?
La1 O5 2.499(3) 4_585 ?
La1 O6 2.478(3) . ?
La1 O7 2.473(3) . ?
La1 O8 2.433(3) . ?
P1 O4 1.469(3) . ?
P1 O7 1.466(3) . ?
P1 F1 1.534(3) . ?
P1 F4 1.524(3) . ?
P2 O1 1.472(3) . ?
P2 O2 1.466(3) . ?
P2 F2 1.529(3) . ?
P2 F3 1.552(3) . ?
P3 O3 1.475(3) . ?
P3 O8 1.451(3) . ?
P3 F5 1.519(3) . ?
P3 F6 1.517(4) . ?
P4 O5 1.471(3) . ?
P4 O6 1.444(3) . ?
P4 F7 1.488(4) . ?
P4 F8 1.517(4) . ?
O1 La1 2.571(3) 3_675 ?
O3 La1 2.527(3) 3_775 ?
O4 La1 2.554(3) 3_675 ?
O5 La1 2.499(3) 4_586 ?
N1 H1A 0.847(11) . ?
N1 H1B 0.834(11) . ?
N1 H1C 0.848(11) . ?
N1 H1D 0.840(11) . ?

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 O1 115.24(10) . 3_675 ?
O2 La1 O4 71.92(11) . 3_675 ?
O3 La1 O1 145.42(11) 3_775 3_675 ?
O3 La1 O2 73.51(11) 3_775 . ?
O3 La1 O4 138.68(10) 3_775 3_675 ?
O4 La1 O1 71.85(10) 3_675 3_675 ?
O5 La1 O1 141.90(11) 4_585 3_675 ?
O5 La1 O2 78.95(11) 4_585 . ?
O5 La1 O3 71.08(11) 4_585 3_775 ?
O5 La1 O4 80.66(11) 4_585 3_675 ?
O6 La1 O1 76.81(12) . 3_675 ?
O6 La1 O2 136.14(12) . . ?
O6 La1 O3 121.56(11) . 3_775 ?
O6 La1 O4 72.98(11) . 3_675 ?
O6 La1 O5 70.13(13) . 4_585 ?
O7 La1 O1 72.21(10) . 3_675 ?
O7 La1 O2 75.36(10) . . ?
O7 La1 O3 78.65(11) . 3_775 ?
O7 La1 O4 113.05(11) . 3_675 ?
O7 La1 O5 144.71(12) . 4_585 ?
O7 La1 O6 143.94(13) . . ?
O8 La1 O1 83.45(11) . 3_675 ?
O8 La1 O2 144.51(11) . . ?
O8 La1 O3 74.83(10) . 3_775 ?
O8 La1 O4 143.39(11) . 3_675 ?
O8 La1 O5 105.39(12) . 4_585 ?
O8 La1 O6 75.40(12) . . ?
O8 La1 O7 83.10(12) . . ?
O4 P1 F1 108.26(19) . . ?
O4 P1 F4 109.10(19) . . ?
O7 P1 O4 118.75(19) . . ?
O7 P1 F1 109.36(19) . . ?
O7 P1 F4 110.0(2) . . ?
F4 P1 F1 99.6(2) . . ?
O1 P2 F2 109.74(18) . . ?
O1 P2 F3 107.03(18) . . ?
O2 P2 O1 121.89(19) . . ?
O2 P2 F2 109.84(19) . . ?
O2 P2 F3 106.76(18) . . ?
F2 P2 F3 99.04(19) . . ?
O3 P3 F5 107.4(2) . . ?
O3 P3 F6 107.8(2) . . ?
O8 P3 O3 121.43(19) . . ?
O8 P3 F5 108.5(2) . . ?
O8 P3 F6 109.7(2) . . ?
F6 P3 F5 99.9(3) . . ?
O5 P4 F7 109.4(2) . . ?
O5 P4 F8 109.1(2) . . ?
O6 P4 O5 118.3(2) . . ?
O6 P4 F7 110.4(2) . . ?
O6 P4 F8 108.7(3) . . ?
F7 P4 F8 99.3(3) . . ?
P2 O1 La1 133.45(18) . 3_675 ?
P2 O2 La1 144.25(18) . . ?
P3 O3 La1 139.24(18) . 3_775 ?
P1 O4 La1 122.91(17) . 3_675 ?
P4 O5 La1 147.2(2) . 4_586 ?
P4 O6 La1 161.1(2) . . ?
P1 O7 La1 169.7(2) . . ?
P3 O8 La1 150.6(2) . . ?
H1A N1 H1B 110(2) . . ?
H1A N1 H1C 106.3(19) . . ?
H1A N1 H1D 110(2) . . ?
H1B N1 H1C 110(2) . . ?
H1B N1 H1D 110(2) . . ?
H1C N1 H1D 110(2) . . ?

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
N1 H1A O3 0.847(11) 2.132(14) 2.966(5) 168(4) 1_454
N1 H1B O1 0.834(11) 2.61(3) 3.271(5) 137(3) .
N1 H1B F1 0.834(11) 2.44(3) 3.093(5) 136(3) .
N1 H1C O5 0.848(11) 2.26(2) 3.017(5) 149(3) 3_675
N1 H1D O2 0.840(11) 2.60(4) 2.975(5) 108(3) 3_674
N1 H1D O4 0.840(11) 2.20(3) 2.874(5) 137(3) 4_575

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
O1 P2 O2 La1 -18.8(4) . . . . ?
O2 P2 O1 La1 67.6(3) . . . 3_675 ?
O3 P3 O8 La1 -147.2(4) . . . . ?
O4 P1 O7 La1 -120.9(12) . . . . ?
O5 P4 O6 La1 -54.3(8) . . . . ?
O6 P4 O5 La1 -145.2(4) . . . 4_586 ?
O7 P1 O4 La1 18.3(3) . . . 3_675 ?
O8 P3 O3 La1 51.9(4) . . . 3_775 ?
F1 P1 O4 La1 -107.1(2) . . . 3_675 ?
F1 P1 O7 La1 3.9(13) . . . . ?
F2 P2 O1 La1 -62.8(3) . . . 3_675 ?
F2 P2 O2 La1 111.5(3) . . . . ?
F3 P2 O1 La1 -169.4(2) . . . 3_675 ?
F3 P2 O2 La1 -142.0(3) . . . . ?
F4 P1 O4 La1 145.4(2) . . . 3_675 ?
F4 P1 O7 La1 112.4(12) . . . . ?
F5 P3 O3 La1 177.5(3) . . . 3_775 ?
F5 P3 O8 La1 87.7(5) . . . . ?
F6 P3 O3 La1 -75.7(4) . . . 3_775 ?
F6 P3 O8 La1 -20.5(5) . . . . ?
F7 P4 O5 La1 -17.8(5) . . . 4_586 ?
F7 P4 O6 La1 178.7(7) . . . . ?
F8 P4 O5 La1 89.9(5) . . . 4_586 ?
F8 P4 O6 La1 70.8(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
