# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_(detaH2)tfa2
_database_code_depnum_ccdc_archive 'CCDC 2347608'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 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         '2(C2 F3 O2), C4 H15 N3'
_chemical_formula_sum            'C8 H15 F6 N3 O4'
_chemical_formula_weight         331.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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                   9.799(2)
_cell_length_b                   10.499(2)
_cell_length_c                   14.933(3)
_cell_angle_alpha                69.922(4)
_cell_angle_beta                 76.226(5)
_cell_angle_gamma                72.531(4)
_cell_volume                     1360.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2578
_cell_measurement_theta_min      2.202
_cell_measurement_theta_max      29.547

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_F_000             680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    0.176
_shelx_estimated_absorpt_T_min   0.969
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7546
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10046
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.469
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_full        27.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             6426
_reflns_number_gt                3504
_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       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_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)+(0.0657P)²+0.7045P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6426
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1664
_refine_ls_wR_factor_gt          0.1297
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_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
O1 O 0.3247(2) 0.3053(2) 0.33726(17) 0.0312(6) Uani 1 1 d . . . . .
O2 O 0.5310(2) 0.3755(2) 0.28035(17) 0.0304(5) Uani 1 1 d . . . . .
O3 O 0.2680(2) 0.1606(2) 0.16520(17) 0.0334(6) Uani 1 1 d . . . . .
O4 O 0.0602(3) 0.2921(2) 0.10888(18) 0.0379(6) Uani 1 1 d . . . . .
O5 O 0.6287(2) 0.5291(2) 0.03149(16) 0.0266(5) Uani 1 1 d . . . . .
O6 O 0.7815(2) 0.5578(3) 0.10938(17) 0.0342(6) Uani 1 1 d . . . . .
O7 O 0.7822(2) 1.0686(2) 0.41572(16) 0.0294(5) Uani 1 1 d . . . . .
O8 O 1.0092(2) 1.0884(2) 0.35383(19) 0.0375(6) Uani 1 1 d . . . . .
N1 N 0.5062(3) 0.2784(3) 0.13168(18) 0.0228(6) Uani 1 1 d . . . . .
H11 H 0.4294(15) 0.2392(10) 0.1376(14) 0.034 Uiso 1 1 calc R U . . .
H12 H 0.5026(9) 0.3579(17) 0.0782(12) 0.034 Uiso 1 1 calc R U . . .
H13 H 0.4990(10) 0.3033(16) 0.1873(13) 0.034 Uiso 1 1 calc R U . . .
N2 N 0.5907(3) 0.0342(3) 0.28416(18) 0.0221(6) Uani 1 1 d . . . . .
H21 H 0.658(3) 0.0522(8) 0.3030(8) 0.026 Uiso 1 1 d R U . . .
N3 N 0.3018(3) 0.0258(3) 0.37732(19) 0.0240(6) Uani 1 1 d . . . . .
H31 H 0.2931(18) 0.0098(10) 0.4423(13) 0.036 Uiso 1 1 calc R U . . .
H32 H 0.2133(18) 0.0390(14) 0.3612(14) 0.036 Uiso 1 1 calc R U . . .
H33 H 0.3364(13) 0.1038(16) 0.3455(13) 0.036 Uiso 1 1 calc R U . . .
N4 N -0.0850(3) 0.4200(3) 0.94521(18) 0.0242(6) Uani 1 1 d . . . . .
H41 H -0.1787(19) 0.4433(18) 0.9697(13) 0.036 Uiso 1 1 calc R U . . .
H42 H -0.056(2) 0.4975(18) 0.9083(8) 0.036 Uiso 1 1 calc R U . . .
H43 H -0.032(2) 0.3761(12) 0.9934(13) 0.036 Uiso 1 1 calc R U . . .
N5 N -0.0436(3) 0.5148(3) 0.7371(2) 0.0283(6) Uani 1 1 d . . . . .
H51 H -0.094(2) 0.574(3) 0.7030(16) 0.034 Uiso 1 1 d R U . . .
N6 N 0.1803(3) 0.6426(3) 0.70963(19) 0.0254(6) Uani 1 1 d . . . . .
H61 H 0.113(2) 0.715(2) 0.7071(11) 0.038 Uiso 1 1 calc R U . . .
H62 H 0.2598(19) 0.664(2) 0.6985(10) 0.038 Uiso 1 1 calc R U . . .
H63 H 0.171(2) 0.5855(14) 0.7646(12) 0.038 Uiso 1 1 calc R U . . .
C1 C 0.6458(3) 0.1748(3) 0.1188(2) 0.0258(7) Uani 1 1 d . . . . .
H1A H 0.724099 0.203506 0.132659 0.031 Uiso 1 1 calc R U . . .
H1B H 0.669341 0.172569 0.051038 0.031 Uiso 1 1 calc R U . . .
C2 C 0.6376(3) 0.0313(3) 0.1848(2) 0.0253(7) Uani 1 1 d . . . . .
H2A H 0.568623 -0.002891 0.165340 0.030 Uiso 1 1 calc R U . . .
H2B H 0.733903 -0.033958 0.179265 0.030 Uiso 1 1 calc R U . . .
C3 C 0.5577(3) -0.0960(3) 0.3514(2) 0.0243(7) Uani 1 1 d . . . . .
H3A H 0.568949 -0.104100 0.417449 0.029 Uiso 1 1 calc R U . . .
H3B H 0.625660 -0.176932 0.332588 0.029 Uiso 1 1 calc R U . . .
C4 C 0.4033(3) -0.0960(3) 0.3497(2) 0.0259(7) Uani 1 1 d . . . . .
H4A H 0.393116 -0.091340 0.284156 0.031 Uiso 1 1 calc R U . . .
H4B H 0.380138 -0.183457 0.395175 0.031 Uiso 1 1 calc R U . . .
C5 C -0.0653(4) 0.3255(3) 0.8856(3) 0.0330(8) Uani 1 1 d . . . . .
H5A H -0.119036 0.252253 0.921011 0.040 Uiso 1 1 calc R U . . .
H5B H 0.038525 0.279141 0.873588 0.040 Uiso 1 1 calc R U . . .
C6 C -0.1192(4) 0.4064(4) 0.7909(2) 0.0336(8) Uani 1 1 d . . . . .
H6A H -0.105052 0.341961 0.752400 0.040 Uiso 1 1 calc R U . . .
H6B H -0.224144 0.448845 0.802936 0.040 Uiso 1 1 calc R U . . .
C7 C 0.0932(4) 0.4686(4) 0.6793(3) 0.0377(9) Uani 1 1 d . . . . .
H7A H 0.073959 0.441856 0.626958 0.045 Uiso 1 1 calc R U . . .
H7B H 0.152765 0.384971 0.720373 0.045 Uiso 1 1 calc R U . . .
C8 C 0.1752(4) 0.5790(4) 0.6367(3) 0.0359(8) Uani 1 1 d . . . . .
H8A H 0.275047 0.537972 0.610040 0.043 Uiso 1 1 calc R U . . .
H8B H 0.128645 0.652071 0.583114 0.043 Uiso 1 1 calc R U . . .
C9 C 0.4140(3) 0.3686(3) 0.3351(2) 0.0227(7) Uani 1 1 d . . . . .
C10 C 0.3756(4) 0.4499(4) 0.4082(2) 0.0340(8) Uani 1 1 d . . . . .
C11 C 0.1554(3) 0.1825(3) 0.1333(2) 0.0260(7) Uani 1 1 d . . . . .
C12 C 0.1276(3) 0.0544(3) 0.1186(3) 0.0293(8) Uani 1 1 d . . . . .
C13 C 0.6638(3) 0.5833(3) 0.0829(2) 0.0239(7) Uani 1 1 d . . . . .
C14 C 0.5464(4) 0.7019(3) 0.1126(2) 0.0291(7) Uani 1 1 d . . . . .
C15 C 0.9136(3) 1.0229(3) 0.3910(2) 0.0249(7) Uani 1 1 d . . . . .
C16 C 0.9605(3) 0.8641(3) 0.4054(2) 0.0297(8) Uani 1 1 d . . . . .
F1 F 0.4443(4) 0.3808(3) 0.48291(19) 0.0919(11) Uani 1 1 d . . . . .
F2 F 0.4079(3) 0.5715(2) 0.37451(17) 0.0658(8) Uani 1 1 d . . . . .
F3 F 0.2354(3) 0.4783(4) 0.4429(2) 0.1034(13) Uani 1 1 d . . . . .
F4 F 0.1949(2) -0.0669(2) 0.17267(18) 0.0528(6) Uani 1 1 d . . . . .
F5 F 0.1708(3) 0.0536(3) 0.02719(17) 0.0647(7) Uani 1 1 d . . . . .
F6 F -0.0113(2) 0.0531(2) 0.1376(2) 0.0648(8) Uani 1 1 d . . . . .
F7 F 0.4132(2) 0.6820(2) 0.12770(17) 0.0480(6) Uani 1 1 d . . . . .
F8 F 0.5643(2) 0.7202(2) 0.19255(15) 0.0483(6) Uani 1 1 d . . . . .
F9 F 0.5462(2) 0.8235(2) 0.04340(16) 0.0437(5) Uani 1 1 d . . . . .
F10 F 0.8986(2) 0.7919(2) 0.48932(16) 0.0489(6) Uani 1 1 d . . . . .
F11 F 0.9210(2) 0.8352(2) 0.33602(16) 0.0472(6) Uani 1 1 d . . . . .
F12 F 1.1025(2) 0.8129(2) 0.40142(17) 0.0457(6) 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 C9 1.236(4) . ?
O2 C9 1.245(4) . ?
O3 C11 1.233(4) . ?
O4 C11 1.248(4) . ?
O5 C13 1.254(4) . ?
O6 C13 1.233(4) . ?
O7 C15 1.244(4) . ?
O8 C15 1.239(4) . ?
N1 C1 1.489(4) . ?
N1 H11 0.934(17) . ?
N1 H12 0.934(17) . ?
N1 H13 0.934(17) . ?
N2 C2 1.453(4) . ?
N2 C3 1.467(4) . ?
N2 H21 0.87(3) . ?
N3 C4 1.483(4) . ?
N3 H31 0.913(17) . ?
N3 H32 0.913(17) . ?
N3 H33 0.913(17) . ?
N4 C5 1.491(4) . ?
N4 H41 0.897(18) . ?
N4 H42 0.897(18) . ?
N4 H43 0.897(18) . ?
N5 C6 1.444(4) . ?
N5 C7 1.458(4) . ?
N5 H51 0.78(4) . ?
N6 C8 1.476(4) . ?
N6 H61 0.837(17) . ?
N6 H62 0.837(18) . ?
N6 H63 0.837(17) . ?
C1 C2 1.505(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.519(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.503(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.484(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.521(4) . ?
C10 F2 1.307(4) . ?
C10 F1 1.316(4) . ?
C10 F3 1.329(4) . ?
C11 C12 1.543(4) . ?
C12 F4 1.324(4) . ?
C12 F6 1.325(4) . ?
C12 F5 1.331(4) . ?
C13 C14 1.532(4) . ?
C14 F8 1.331(4) . ?
C14 F7 1.337(4) . ?
C14 F9 1.339(4) . ?
C15 C16 1.542(4) . ?
C16 F12 1.328(4) . ?
C16 F10 1.332(4) . ?
C16 F11 1.339(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 N1 H11 109.5 . . ?
C1 N1 H12 109.5 . . ?
H11 N1 H12 109.5 . . ?
C1 N1 H13 109.5 . . ?
H11 N1 H13 109.5 . . ?
H12 N1 H13 109.5 . . ?
C2 N2 C3 114.2(2) . . ?
C2 N2 H21 108.6 . . ?
C3 N2 H21 108.8 . . ?
C4 N3 H31 109.5 . . ?
C4 N3 H32 109.5 . . ?
H31 N3 H32 109.5 . . ?
C4 N3 H33 109.5 . . ?
H31 N3 H33 109.5 . . ?
H32 N3 H33 109.5 . . ?
C5 N4 H41 109.5 . . ?
C5 N4 H42 109.5 . . ?
H41 N4 H42 109.5 . . ?
C5 N4 H43 109.5 . . ?
H41 N4 H43 109.5 . . ?
H42 N4 H43 109.5 . . ?
C6 N5 C7 114.5(3) . . ?
C6 N5 H51 108.6 . . ?
C7 N5 H51 108.6 . . ?
C8 N6 H61 109.5 . . ?
C8 N6 H62 109.5 . . ?
H61 N6 H62 109.5 . . ?
C8 N6 H63 109.5 . . ?
H61 N6 H63 109.5 . . ?
H62 N6 H63 109.5 . . ?
N1 C1 C2 111.0(2) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 110.5(2) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 109.3(2) . . ?
N2 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N3 C4 C3 109.7(2) . . ?
N3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N4 C5 C6 110.6(3) . . ?
N4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N5 C6 C5 111.2(3) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N5 C7 C8 112.0(3) . . ?
N5 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N5 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N6 C8 C7 111.1(3) . . ?
N6 C8 H8A 109.4 . . ?
C7 C8 H8A 109.4 . . ?
N6 C8 H8B 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O1 C9 O2 128.5(3) . . ?
O1 C9 C10 115.9(3) . . ?
O2 C9 C10 115.6(3) . . ?
F2 C10 F1 105.8(3) . . ?
F2 C10 F3 104.4(3) . . ?
F1 C10 F3 106.6(3) . . ?
F2 C10 C9 114.3(3) . . ?
F1 C10 C9 111.4(3) . . ?
F3 C10 C9 113.6(3) . . ?
O3 C11 O4 130.9(3) . . ?
O3 C11 C12 115.4(3) . . ?
O4 C11 C12 113.8(3) . . ?
F4 C12 F6 105.8(3) . . ?
F4 C12 F5 106.9(3) . . ?
F6 C12 F5 106.0(3) . . ?
F4 C12 C11 113.9(3) . . ?
F6 C12 C11 113.0(3) . . ?
F5 C12 C11 110.6(3) . . ?
O6 C13 O5 128.8(3) . . ?
O6 C13 C14 115.7(3) . . ?
O5 C13 C14 115.5(3) . . ?
F8 C14 F7 106.9(3) . . ?
F8 C14 F9 106.6(3) . . ?
F7 C14 F9 106.3(3) . . ?
F8 C14 C13 113.1(3) . . ?
F7 C14 C13 112.7(3) . . ?
F9 C14 C13 110.8(3) . . ?
O8 C15 O7 128.7(3) . . ?
O8 C15 C16 116.5(3) . . ?
O7 C15 C16 114.7(3) . . ?
F12 C16 F10 107.2(3) . . ?
F12 C16 F11 106.9(3) . . ?
F10 C16 F11 106.9(3) . . ?
F12 C16 C15 113.4(3) . . ?
F10 C16 C15 112.5(3) . . ?
F11 C16 C15 109.7(3) . . ?

_refine_diff_density_max         0.848
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.069



####################################################################### 
# 
# 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_Gdtfa3deta2
_database_code_depnum_ccdc_archive 'CCDC 2347609'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 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         'C14 H26 F9 Gd N6 O6, C3 H8 O'
_chemical_formula_sum            'C17 H34 F9 Gd N6 O7'
_chemical_formula_weight         762.75

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.294(7)
_cell_length_b                   12.580(5)
_cell_length_c                   24.686(10)
_cell_angle_alpha                90
_cell_angle_beta                 101.007(7)
_cell_angle_gamma                90
_cell_volume                     5577(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      4.462
_cell_measurement_theta_max      55.091

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_F_000             3032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.022
_exptl_absorpt_coefficient_mu    2.485
_shelx_estimated_absorpt_T_min   0.530
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3978
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6531
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.977
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6531
_reflns_number_gt                5991
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1521P)²+356.0354P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6531
_refine_ls_number_parameters     419
_refine_ls_number_restraints     166
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.1027
_refine_ls_wR_factor_ref         0.2919
_refine_ls_wR_factor_gt          0.2873
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.000
_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
Gd1 Gd 0.76988(4) 0.36039(6) 0.34862(3) 0.0193(2) Uani 1 1 d . . . . .
F1 F 0.9361(8) 0.4080(12) 0.5433(6) 0.067(4) Uani 1 1 d . . . . .
F2 F 0.9035(9) 0.5460(13) 0.4896(6) 0.073(5) Uani 1 1 d . . . . .
F3 F 0.8689(9) 0.5295(12) 0.5665(5) 0.058(4) Uani 1 1 d . . . . .
C4 C 0.872(3) 0.296(3) 0.1906(19) 0.035(6) Uani 0.536(18) 1 d . U P A 1
F4 F 0.8449(15) 0.293(2) 0.1349(10) 0.043(5) Uani 0.536(18) 1 d . U P A 1
F5 F 0.9231(12) 0.227(2) 0.2027(10) 0.046(5) Uani 0.536(18) 1 d . U P A 1
F6 F 0.9020(14) 0.392(2) 0.2041(11) 0.031(5) Uani 0.536(18) 1 d . U P A 1
C4A C 0.882(2) 0.302(3) 0.1985(13) 0.035(6) Uani 0.464(18) 1 d D U P A 2
F4A F 0.8757(16) 0.259(2) 0.1486(10) 0.041(6) Uani 0.464(18) 1 d D U P A 2
F5A F 0.9502(14) 0.281(2) 0.2260(10) 0.045(5) Uani 0.464(18) 1 d D U P A 2
F6A F 0.8785(17) 0.407(2) 0.1921(12) 0.033(5) Uani 0.464(18) 1 d D U P A 2
F7 F 0.5562(11) 0.5471(18) 0.2293(9) 0.061(4) Uani 0.616(16) 1 d D U P B 1
F8 F 0.5528(12) 0.3842(16) 0.2015(11) 0.060(4) Uani 0.616(16) 1 d D U P B 1
F9 F 0.5715(11) 0.5124(17) 0.1488(7) 0.043(5) Uani 0.616(16) 1 d D U P B 1
F7A F 0.5422(16) 0.424(3) 0.2120(15) 0.061(4) Uani 0.384(16) 1 d D U P B 2
F8A F 0.5988(18) 0.312(2) 0.1721(13) 0.061(5) Uani 0.384(16) 1 d D U P B 2
F9A F 0.5799(19) 0.462(3) 0.1375(11) 0.045(5) Uani 0.384(16) 1 d D U P B 2
O1 O 0.8053(7) 0.4074(11) 0.4442(4) 0.032(3) Uani 1 1 d . . . . .
O2 O 0.7765(7) 0.3698(11) 0.5264(5) 0.037(3) Uani 1 1 d . U . . .
O3 O 0.8260(6) 0.2982(9) 0.2745(5) 0.027(2) Uani 1 1 d D . . . .
O4 O 0.7503(12) 0.2355(19) 0.1958(8) 0.024(4) Uani 0.536(18) 1 d D U P A 1
C3 C 0.8035(16) 0.275(2) 0.2242(8) 0.019(5) Uani 0.536(18) 1 d D U P A 1
O4A O 0.7801(16) 0.194(2) 0.2052(11) 0.029(5) Uani 0.464(18) 1 d D U P A 2
C3A C 0.8244(18) 0.257(3) 0.2275(9) 0.020(5) Uani 0.464(18) 1 d D U P A 2
O5 O 0.6834(6) 0.4186(12) 0.2701(5) 0.036(3) Uani 1 1 d . . . . .
O6 O 0.7124(8) 0.5105(12) 0.1992(5) 0.042(3) Uani 1 1 d . . . . .
N1 N 0.8319(7) 0.5216(10) 0.3121(5) 0.020(2) Uani 1 1 d . . . . .
H1A H 0.828695 0.513113 0.275159 0.024 Uiso 1 1 calc R U . . .
H1B H 0.805121 0.580540 0.317106 0.024 Uiso 1 1 calc R U . . .
N2 N 0.9125(8) 0.3707(11) 0.3803(5) 0.026(3) Uani 1 1 d . U . . .
H2A H 0.920973 0.404739 0.417525 0.031 Uiso 1 1 calc R U . . .
N3 N 0.8262(7) 0.1903(11) 0.3964(6) 0.026(3) Uani 1 1 d . U . . .
H3A H 0.799041 0.170723 0.422030 0.031 Uiso 1 1 calc R U . . .
H3B H 0.822292 0.137352 0.370865 0.031 Uiso 1 1 calc R U . . .
N4 N 0.6938(8) 0.2007(12) 0.3033(6) 0.028(3) Uani 1 1 d . U . . .
H4A H 0.671226 0.219830 0.268563 0.033 Uiso 1 1 calc R U . . .
H4B H 0.725980 0.146916 0.300035 0.033 Uiso 1 1 calc R U . . .
N5 N 0.6559(8) 0.3106(12) 0.3939(6) 0.027(3) Uani 1 1 d . U . . .
H5A H 0.675214 0.262660 0.425693 0.032 Uiso 1 1 calc R U . . .
N6 N 0.6964(9) 0.5229(14) 0.3696(7) 0.039(4) Uani 1 1 d . . . . .
H6A H 0.722428 0.555948 0.400040 0.046 Uiso 1 1 calc R U . . .
H6B H 0.692406 0.569135 0.340857 0.046 Uiso 1 1 calc R U . . .
C1 C 0.8151(9) 0.4111(13) 0.4948(6) 0.028(3) Uani 1 1 d . U . . .
C2 C 0.8802(11) 0.4769(13) 0.5236(8) 0.035(4) Uani 1 1 d . . . . .
C5 C 0.6719(7) 0.4602(13) 0.2225(7) 0.031(4) Uani 1 1 d D . . . .
C6 C 0.5886(10) 0.4770(17) 0.2002(8) 0.034(5) Uani 0.616(16) 1 d D U P B 1
C6A C 0.6005(13) 0.414(2) 0.1866(10) 0.033(5) Uani 0.384(16) 1 d D U P B 2
C7 C 0.9109(9) 0.5421(14) 0.3372(7) 0.031(4) Uani 1 1 d . . . . .
H7A H 0.934002 0.587893 0.312472 0.037 Uiso 1 1 calc R U . . .
H7B H 0.914156 0.579226 0.372908 0.037 Uiso 1 1 calc R U . . .
C8 C 0.9505(9) 0.4400(12) 0.3457(7) 0.025(3) Uani 1 1 d . . . . .
H8A H 1.002812 0.451937 0.364292 0.030 Uiso 1 1 calc R U . . .
H8B H 0.950688 0.405508 0.309700 0.030 Uiso 1 1 calc R U . . .
C9 C 0.9457(10) 0.2655(17) 0.3888(8) 0.036(4) Uani 1 1 d . . . . .
H9A H 0.998463 0.271849 0.407465 0.044 Uiso 1 1 calc R U . . .
H9B H 0.944157 0.230277 0.352750 0.044 Uiso 1 1 calc R U . . .
C10 C 0.9040(10) 0.2003(15) 0.4234(8) 0.034(4) Uani 1 1 d . . . . .
H10A H 0.926767 0.128834 0.429221 0.041 Uiso 1 1 calc R U . . .
H10B H 0.907098 0.234389 0.459886 0.041 Uiso 1 1 calc R U . . .
C11 C 0.6371(11) 0.1599(15) 0.3320(7) 0.036(4) Uani 1 1 d . . . . .
H11A H 0.660627 0.112658 0.362415 0.043 Uiso 1 1 calc R U . . .
H11B H 0.600366 0.117614 0.306065 0.043 Uiso 1 1 calc R U . . .
C12 C 0.5988(9) 0.2481(16) 0.3545(7) 0.031(4) Uani 1 1 d . . . . .
H12A H 0.560518 0.219619 0.374030 0.037 Uiso 1 1 calc R U . . .
H12B H 0.573826 0.294564 0.324155 0.037 Uiso 1 1 calc R U . . .
C13 C 0.6250(9) 0.4041(14) 0.4165(7) 0.030(3) Uani 1 1 d . . . . .
H13A H 0.656079 0.421775 0.452740 0.036 Uiso 1 1 calc R U . . .
H13B H 0.574226 0.387280 0.422469 0.036 Uiso 1 1 calc R U . . .
C14 C 0.6213(11) 0.4987(18) 0.3792(9) 0.040(4) Uani 1 1 d . U . . .
H14A H 0.587617 0.483466 0.343619 0.048 Uiso 1 1 calc R U . . .
H14B H 0.601246 0.560616 0.396347 0.048 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
Gd1 O5 2.372(11) . ?
Gd1 O3 2.395(10) . ?
Gd1 O1 2.398(10) . ?
Gd1 N6 2.554(17) . ?
Gd1 N3 2.563(14) . ?
Gd1 N1 2.570(13) . ?
Gd1 N4 2.575(15) . ?
Gd1 N2 2.580(14) . ?
Gd1 N5 2.621(14) . ?
F1 C2 1.36(2) . ?
F2 C2 1.33(2) . ?
F3 C2 1.30(2) . ?
C4 F5 1.27(5) . ?
C4 F6 1.34(5) . ?
C4 F4 1.37(5) . ?
C4 C3 1.65(6) . ?
C4A F6A 1.33(2) . ?
C4A F5A 1.33(2) . ?
C4A F4A 1.33(2) . ?
C4A C3A 1.49(5) . ?
F7 C6 1.346(17) . ?
F8 C6 1.341(18) . ?
F9 C6 1.323(17) . ?
F7A C6A 1.342(19) . ?
F8A C6A 1.336(19) . ?
F9A C6A 1.342(19) . ?
O1 C1 1.228(19) . ?
O2 C1 1.26(2) . ?
O3 C3A 1.26(2) . ?
O3 C3 1.27(2) . ?
O4 C3 1.19(2) . ?
O4A C3A 1.19(2) . ?
O5 C5 1.27(2) . ?
O6 C5 1.20(2) . ?
N1 C7 1.48(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 C9 1.45(2) . ?
N2 C8 1.483(19) . ?
N2 H2A 1.0000 . ?
N3 C10 1.46(2) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N4 C11 1.46(2) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N5 C13 1.46(2) . ?
N5 C12 1.51(2) . ?
N5 H5A 1.0000 . ?
N6 C14 1.47(2) . ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
C1 C2 1.51(2) . ?
C5 C6 1.534(17) . ?
C5 C6A 1.544(18) . ?
C7 C8 1.47(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.49(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.48(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.50(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 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
O5 Gd1 O3 78.0(4) . . ?
O5 Gd1 O1 137.8(5) . . ?
O3 Gd1 O1 139.3(4) . . ?
O5 Gd1 N6 67.9(5) . . ?
O3 Gd1 N6 137.4(5) . . ?
O1 Gd1 N6 69.9(5) . . ?
O5 Gd1 N3 141.3(5) . . ?
O3 Gd1 N3 83.4(4) . . ?
O1 Gd1 N3 75.2(4) . . ?
N6 Gd1 N3 139.1(5) . . ?
O5 Gd1 N1 75.0(4) . . ?
O3 Gd1 N1 73.0(4) . . ?
O1 Gd1 N1 95.5(4) . . ?
N6 Gd1 N1 74.0(5) . . ?
N3 Gd1 N1 130.9(4) . . ?
O5 Gd1 N4 70.4(5) . . ?
O3 Gd1 N4 71.8(4) . . ?
O1 Gd1 N4 129.9(4) . . ?
N6 Gd1 N4 116.8(5) . . ?
N3 Gd1 N4 71.6(5) . . ?
N1 Gd1 N4 134.6(4) . . ?
O5 Gd1 N2 135.3(4) . . ?
O3 Gd1 N2 72.0(4) . . ?
O1 Gd1 N2 67.8(4) . . ?
N6 Gd1 N2 116.1(5) . . ?
N3 Gd1 N2 66.9(4) . . ?
N1 Gd1 N2 65.0(4) . . ?
N4 Gd1 N2 127.0(5) . . ?
O5 Gd1 N5 87.8(4) . . ?
O3 Gd1 N5 137.7(4) . . ?
O1 Gd1 N5 74.2(4) . . ?
N6 Gd1 N5 67.2(5) . . ?
N3 Gd1 N5 83.5(4) . . ?
N1 Gd1 N5 141.1(4) . . ?
N4 Gd1 N5 65.9(4) . . ?
N2 Gd1 N5 136.3(4) . . ?
F5 C4 F6 108(4) . . ?
F5 C4 F4 109(3) . . ?
F6 C4 F4 109(4) . . ?
F5 C4 C3 111(3) . . ?
F6 C4 C3 109(3) . . ?
F4 C4 C3 109(3) . . ?
F6A C4A F5A 106(3) . . ?
F6A C4A F4A 107(3) . . ?
F5A C4A F4A 107(3) . . ?
F6A C4A C3A 114(3) . . ?
F5A C4A C3A 111(3) . . ?
F4A C4A C3A 110(3) . . ?
C1 O1 Gd1 165.8(13) . . ?
C3A O3 Gd1 153.6(16) . . ?
C3 O3 Gd1 135.9(16) . . ?
O4 C3 O3 139(3) . . ?
O4 C3 C4 113(2) . . ?
O3 C3 C4 109(2) . . ?
O4A C3A O3 126(3) . . ?
O4A C3A C4A 121(2) . . ?
O3 C3A C4A 113(2) . . ?
C5 O5 Gd1 148.4(10) . . ?
C7 N1 Gd1 116.9(10) . . ?
C7 N1 H1A 108.1 . . ?
Gd1 N1 H1A 108.1 . . ?
C7 N1 H1B 108.1 . . ?
Gd1 N1 H1B 108.1 . . ?
H1A N1 H1B 107.3 . . ?
C9 N2 C8 113.0(13) . . ?
C9 N2 Gd1 111.6(11) . . ?
C8 N2 Gd1 114.4(9) . . ?
C9 N2 H2A 105.6 . . ?
C8 N2 H2A 105.6 . . ?
Gd1 N2 H2A 105.6 . . ?
C10 N3 Gd1 114.2(11) . . ?
C10 N3 H3A 108.7 . . ?
Gd1 N3 H3A 108.7 . . ?
C10 N3 H3B 108.7 . . ?
Gd1 N3 H3B 108.7 . . ?
H3A N3 H3B 107.6 . . ?
C11 N4 Gd1 116.1(10) . . ?
C11 N4 H4A 108.3 . . ?
Gd1 N4 H4A 108.3 . . ?
C11 N4 H4B 108.3 . . ?
Gd1 N4 H4B 108.3 . . ?
H4A N4 H4B 107.4 . . ?
C13 N5 C12 113.2(13) . . ?
C13 N5 Gd1 111.6(9) . . ?
C12 N5 Gd1 111.1(9) . . ?
C13 N5 H5A 106.8 . . ?
C12 N5 H5A 106.8 . . ?
Gd1 N5 H5A 106.8 . . ?
C14 N6 Gd1 114.3(13) . . ?
C14 N6 H6A 108.7 . . ?
Gd1 N6 H6A 108.7 . . ?
C14 N6 H6B 108.7 . . ?
Gd1 N6 H6B 108.7 . . ?
H6A N6 H6B 107.6 . . ?
O1 C1 O2 128.6(17) . . ?
O1 C1 C2 116.7(16) . . ?
O2 C1 C2 114.7(15) . . ?
F3 C2 F2 107.5(15) . . ?
F3 C2 F1 105.0(16) . . ?
F2 C2 F1 109.4(18) . . ?
F3 C2 C1 115.4(17) . . ?
F2 C2 C1 112.2(15) . . ?
F1 C2 C1 106.9(14) . . ?
O6 C5 O5 130.8(14) . . ?
O6 C5 C6 114.7(15) . . ?
O5 C5 C6 111.5(14) . . ?
O6 C5 C6A 117.0(16) . . ?
O5 C5 C6A 110.5(15) . . ?
F9 C6 F8 106.9(18) . . ?
F9 C6 F7 104.1(18) . . ?
F8 C6 F7 106.9(18) . . ?
F9 C6 C5 115.2(16) . . ?
F8 C6 C5 109.1(16) . . ?
F7 C6 C5 114.0(17) . . ?
F8A C6A F9A 102(2) . . ?
F8A C6A F7A 104(2) . . ?
F9A C6A F7A 106(2) . . ?
F8A C6A C5 119(2) . . ?
F9A C6A C5 114(2) . . ?
F7A C6A C5 111(2) . . ?
C8 C7 N1 108.8(13) . . ?
C8 C7 H7A 109.9 . . ?
N1 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
N1 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C7 C8 N2 108.9(13) . . ?
C7 C8 H8A 109.9 . . ?
N2 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
N2 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 C10 109.7(14) . . ?
N2 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N3 C10 C9 110.3(14) . . ?
N3 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N3 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N4 C11 C12 110.6(15) . . ?
N4 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 N5 108.3(14) . . ?
C11 C12 H12A 110.0 . . ?
N5 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
N5 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N5 C13 C14 112.3(14) . . ?
N5 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
N5 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
N6 C14 C13 109.2(16) . . ?
N6 C14 H14A 109.8 . . ?
C13 C14 H14A 109.8 . . ?
N6 C14 H14B 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?

_refine_diff_density_max         3.111
_refine_diff_density_min         -4.148
_refine_diff_density_rms         0.305

# start Validation Reply Form
_vrf_PLAT342_Gdtfa3deta2         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.028 Ang.
RESPONSE: The crystal is a very thin plate which combines non-merohedral 
and pseudo-merohedral twins with significant overlapping. 
;
# end Validation Reply Form






####################################################################### 
# 
# 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_Ybtfa3deta2
_database_code_depnum_ccdc_archive 'CCDC 2347610'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 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         'C12 H26 F6 N6 O4 Yb, C2 F3 O2'
_chemical_formula_sum            'C14 H26 F9 N6 O6 Yb'
_chemical_formula_weight         718.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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                   9.5390(7)
_cell_length_b                   28.4276(19)
_cell_length_c                   8.5495(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.018(2)
_cell_angle_gamma                90
_cell_volume                     2318.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      29.57

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_F_000             1404
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    4.150
_shelx_estimated_absorpt_T_min   0.645
_shelx_estimated_absorpt_T_max   0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6443
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19266
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.135
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        26.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5041
_reflns_number_gt                4746
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+35.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5041
_refine_ls_number_parameters     326
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1163
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_restrained_S_all      1.272
_refine_ls_shift/su_max          0.000
_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
Yb1 Yb 0.45998(6) 0.13533(2) 0.18248(6) 0.00956(10) Uani 1 1 d . . . . .
O1 O 0.2918(9) 0.1487(3) 0.0070(9) 0.0174(17) Uani 1 1 d . . . . .
O2 O 0.3410(9) 0.1828(3) -0.2246(9) 0.0237(19) Uani 1 1 d . . . . .
O3 O 0.6211(8) 0.1925(2) 0.1466(8) 0.0136(16) Uani 1 1 d . . . . .
O4 O 0.5499(10) 0.2583(3) 0.0278(9) 0.0212(17) Uani 1 1 d . . . . .
O5 O 0.3415(9) 0.0777(3) 0.6537(10) 0.024(2) Uani 1 1 d . . . . .
O6 O 0.3545(9) 0.0152(3) 0.8125(11) 0.0253(17) Uani 1 1 d . . . . .
N1 N 0.3488(10) 0.2075(3) 0.2791(10) 0.0136(19) Uani 1 1 d . . . . .
H1A H 0.414735 0.225010 0.329615 0.016 Uiso 1 1 calc R U . . .
H1B H 0.318600 0.224580 0.195533 0.016 Uiso 1 1 calc R U . . .
N2 N 0.2399(8) 0.1163(3) 0.3238(12) 0.0112(16) Uani 1 1 d . . . . .
H2A H 0.266082 0.107371 0.433149 0.013 Uiso 1 1 calc R U . . .
N3 N 0.3956(9) 0.0502(3) 0.1502(10) 0.0118(18) Uani 1 1 d . . . . .
H3A H 0.376778 0.044603 0.047460 0.014 Uiso 1 1 calc R U . . .
H3B H 0.470621 0.032161 0.177324 0.014 Uiso 1 1 calc R U . . .
N4 N 0.5679(9) 0.1156(3) -0.0753(10) 0.0109(18) Uani 1 1 d . U . . .
H4A H 0.502423 0.101082 -0.135658 0.013 Uiso 1 1 calc R U . . .
H4B H 0.592312 0.142875 -0.124069 0.013 Uiso 1 1 calc R U . . .
N5 N 0.6920(9) 0.0955(3) 0.2177(9) 0.0099(17) Uani 1 1 d . U . . .
H5A H 0.673089 0.061325 0.236396 0.012 Uiso 1 1 calc R U . . .
N6 N 0.5364(10) 0.1381(3) 0.4586(8) 0.0058(13) Uani 1 1 d . U . . .
H6A H 0.549926 0.168701 0.485772 0.007 Uiso 1 1 calc R U . . .
H6B H 0.465820 0.126685 0.519357 0.007 Uiso 1 1 calc R U . . .
C1 C 0.2605(12) 0.1651(4) -0.1280(13) 0.015(2) Uani 1 1 d . . . . .
C2 C 0.1021(13) 0.1646(4) -0.1586(14) 0.022(3) Uani 1 1 d . . . . .
C3 C 0.6308(12) 0.2342(4) 0.1042(12) 0.012(2) Uani 1 1 d . U . . .
C4 C 0.7710(11) 0.2600(4) 0.1502(10) 0.012(2) Uani 1 1 d . . . . .
C5 C 0.2975(13) 0.0420(4) 0.7207(11) 0.015(2) Uani 1 1 d . . . . .
C6 C 0.1418(12) 0.0293(3) 0.6855(17) 0.021(2) Uani 1 1 d . . . . .
C7 C 0.2292(12) 0.2002(4) 0.3861(13) 0.016(2) Uani 1 1 d . . . . .
H7A H 0.168213 0.228368 0.385830 0.019 Uiso 1 1 calc R U . . .
H7B H 0.264003 0.195291 0.493984 0.019 Uiso 1 1 calc R U . . .
C8 C 0.1462(11) 0.1576(3) 0.3336(14) 0.014(2) Uani 1 1 d . . . . .
H8A H 0.069702 0.151259 0.408971 0.017 Uiso 1 1 calc R U . . .
H8B H 0.103599 0.163759 0.229974 0.017 Uiso 1 1 calc R U . . .
C9 C 0.1720(12) 0.0752(4) 0.2519(14) 0.016(2) Uani 1 1 d . U . . .
H9A H 0.139277 0.083286 0.145350 0.019 Uiso 1 1 calc R U . . .
H9B H 0.089524 0.065733 0.314824 0.019 Uiso 1 1 calc R U . . .
C10 C 0.2741(11) 0.0355(4) 0.2439(13) 0.014(2) Uani 1 1 d . . . . .
H10A H 0.304922 0.026812 0.350616 0.017 Uiso 1 1 calc R U . . .
H10B H 0.229194 0.007706 0.195476 0.017 Uiso 1 1 calc R U . . .
C11 C 0.6914(12) 0.0855(4) -0.0655(12) 0.014(2) Uani 1 1 d . . . . .
H11A H 0.748073 0.088865 -0.161875 0.017 Uiso 1 1 calc R U . . .
H11B H 0.661969 0.052207 -0.056544 0.017 Uiso 1 1 calc R U . . .
C12 C 0.7783(12) 0.0990(4) 0.0748(12) 0.015(2) Uani 1 1 d . . . . .
H12A H 0.860309 0.077793 0.083401 0.018 Uiso 1 1 calc R U . . .
H12B H 0.813117 0.131592 0.062582 0.018 Uiso 1 1 calc R U . . .
C13 C 0.7641(11) 0.1141(4) 0.3596(11) 0.010(2) Uani 1 1 d . U . . .
H13A H 0.791952 0.147258 0.342005 0.011 Uiso 1 1 calc R U . . .
H13B H 0.849771 0.095552 0.380712 0.011 Uiso 1 1 calc R U . . .
C14 C 0.6676(11) 0.1112(4) 0.4957(12) 0.011(2) Uani 1 1 d . U . . .
H14A H 0.713208 0.124662 0.589541 0.013 Uiso 1 1 calc R U . . .
H14B H 0.644363 0.077901 0.517608 0.013 Uiso 1 1 calc R U . . .
F1 F 0.0689(8) 0.1768(3) -0.3045(10) 0.041(2) Uani 1 1 d . U . . .
F2 F 0.0486(10) 0.1219(2) -0.1335(8) 0.0337(17) Uani 1 1 d . . . . .
F3 F 0.0368(10) 0.1948(3) -0.0628(9) 0.0344(18) Uani 1 1 d . . . . .
F4 F 0.8221(8) 0.2845(2) 0.0326(8) 0.0246(16) Uani 1 1 d . . . . .
F5 F 0.7465(8) 0.2902(2) 0.2683(8) 0.0244(16) Uani 1 1 d . . . . .
F6 F 0.8695(6) 0.2305(2) 0.1989(9) 0.0212(14) Uani 1 1 d . . . . .
F7 F 0.0710(7) 0.0178(3) 0.8144(11) 0.0359(18) Uani 1 1 d . U . . .
F8 F 0.1374(9) -0.0092(2) 0.5909(10) 0.0339(19) Uani 1 1 d . . . . .
F9 F 0.0711(7) 0.0622(2) 0.6102(8) 0.0249(16) 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
Yb1 O1 2.229(8) . ?
Yb1 O3 2.259(7) . ?
Yb1 N1 2.454(8) . ?
Yb1 N2 2.482(9) . ?
Yb1 N6 2.472(7) . ?
Yb1 N4 2.496(8) . ?
Yb1 N5 2.505(9) . ?
Yb1 N3 2.513(8) . ?
O1 C1 1.281(13) . ?
O2 C1 1.235(13) . ?
O3 C3 1.242(12) . ?
O4 C3 1.221(13) . ?
O5 C5 1.238(13) . ?
O6 C5 1.222(13) . ?
N1 C7 1.477(14) . ?
N2 C9 1.471(13) . ?
N2 C8 1.478(12) . ?
N3 C10 1.469(12) . ?
N4 C11 1.459(13) . ?
N5 C13 1.491(12) . ?
N5 C12 1.477(12) . ?
N6 C14 1.500(13) . ?
C1 C2 1.533(16) . ?
C2 F1 1.333(14) . ?
C2 F2 1.334(14) . ?
C2 F3 1.339(14) . ?
C3 C4 1.574(14) . ?
C4 F4 1.318(11) . ?
C4 F6 1.325(12) . ?
C4 F5 1.346(11) . ?
C5 C6 1.558(16) . ?
C6 F9 1.320(13) . ?
C6 F7 1.333(15) . ?
C6 F8 1.362(13) . ?
C7 C8 1.515(14) . ?
C9 C10 1.492(14) . ?
C11 C12 1.508(15) . ?
C13 C14 1.486(14) . ?

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
O1 Yb1 O3 106.0(3) . . ?
O1 Yb1 N1 76.9(3) . . ?
O3 Yb1 N1 74.8(3) . . ?
O1 Yb1 N2 75.9(3) . . ?
O3 Yb1 N2 143.0(3) . . ?
N1 Yb1 N2 69.7(3) . . ?
O1 Yb1 N6 148.2(3) . . ?
O3 Yb1 N6 84.6(3) . . ?
N1 Yb1 N6 77.2(3) . . ?
N2 Yb1 N6 77.9(3) . . ?
O1 Yb1 N4 75.0(3) . . ?
O3 Yb1 N4 76.2(3) . . ?
N1 Yb1 N4 131.6(3) . . ?
N2 Yb1 N4 136.9(3) . . ?
N6 Yb1 N4 136.8(3) . . ?
O1 Yb1 N5 142.5(3) . . ?
O3 Yb1 N5 75.0(3) . . ?
N1 Yb1 N5 136.0(3) . . ?
N2 Yb1 N5 126.2(3) . . ?
N6 Yb1 N5 68.8(3) . . ?
N4 Yb1 N5 68.9(3) . . ?
O1 Yb1 N3 85.1(3) . . ?
O3 Yb1 N3 147.7(3) . . ?
N1 Yb1 N3 137.5(3) . . ?
N2 Yb1 N3 68.7(3) . . ?
N6 Yb1 N3 102.0(3) . . ?
N4 Yb1 N3 77.7(3) . . ?
N5 Yb1 N3 78.1(3) . . ?
C1 O1 Yb1 146.8(8) . . ?
C3 O3 Yb1 141.0(7) . . ?
C7 N1 Yb1 115.1(6) . . ?
C9 N2 C8 112.8(8) . . ?
C9 N2 Yb1 110.0(6) . . ?
C8 N2 Yb1 111.5(6) . . ?
C10 N3 Yb1 113.9(6) . . ?
C11 N4 Yb1 114.5(6) . . ?
C13 N5 C12 113.1(8) . . ?
C13 N5 Yb1 110.1(6) . . ?
C12 N5 Yb1 111.3(6) . . ?
C14 N6 Yb1 115.5(6) . . ?
O2 C1 O1 127.3(11) . . ?
O2 C1 C2 120.2(10) . . ?
O1 C1 C2 112.3(10) . . ?
F1 C2 F2 107.3(10) . . ?
F1 C2 F3 107.2(10) . . ?
F2 C2 F3 107.8(10) . . ?
F1 C2 C1 113.0(10) . . ?
F2 C2 C1 111.0(10) . . ?
F3 C2 C1 110.4(10) . . ?
O4 C3 O3 130.0(10) . . ?
O4 C3 C4 114.2(9) . . ?
O3 C3 C4 115.7(9) . . ?
F4 C4 F6 108.2(9) . . ?
F4 C4 F5 107.3(8) . . ?
F6 C4 F5 106.8(8) . . ?
F4 C4 C3 111.8(8) . . ?
F6 C4 C3 112.8(8) . . ?
F5 C4 C3 109.7(8) . . ?
O6 C5 O5 131.1(11) . . ?
O6 C5 C6 113.8(10) . . ?
O5 C5 C6 115.1(10) . . ?
F9 C6 F7 108.5(9) . . ?
F9 C6 F8 105.3(11) . . ?
F7 C6 F8 106.2(9) . . ?
F9 C6 C5 114.7(8) . . ?
F7 C6 C5 112.3(11) . . ?
F8 C6 C5 109.3(9) . . ?
N1 C7 C8 109.5(9) . . ?
N2 C8 C7 109.6(8) . . ?
N2 C9 C10 109.4(9) . . ?
N3 C10 C9 109.0(9) . . ?
N4 C11 C12 109.8(9) . . ?
N5 C12 C11 109.5(9) . . ?
N5 C13 C14 109.3(8) . . ?
C13 C14 N6 108.8(8) . . ?

_refine_diff_density_max         4.014
_refine_diff_density_min         -3.797
_refine_diff_density_rms         0.252



####################################################################### 
# 
# 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_Latfa3CH3CN
_database_code_depnum_ccdc_archive 'CCDC 2347611'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 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         'C8 H5 F9 La N O7'
_chemical_formula_sum            'C8 H5 F9 La N O7'
_chemical_formula_weight         537.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   12.4741(13)
_cell_length_b                   12.8468(12)
_cell_length_c                   9.7054(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.300(4)
_cell_angle_gamma                90
_cell_volume                     1530.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5202
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      34.06

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.331
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.039
_exptl_absorpt_coefficient_mu    2.929
_shelx_estimated_absorpt_T_min   0.541
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13695
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.295
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3685
_reflns_number_gt                3165
_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       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_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)+(0.0279P)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         3685
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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 0.62328(2) 0.36252(2) 0.52232(2) 0.01002(6) Uani 1 1 d . . . . .
N1 N 0.7970(2) 0.4742(2) 0.4651(3) 0.0216(6) Uani 1 1 d . . . . .
O1W O 0.49273(19) 0.36618(15) 0.6874(2) 0.0164(5) Uani 1 1 d . . . . .
H1W H 0.476319 0.308778 0.724596 0.025 Uiso 1 1 d R U . . .
H2W H 0.475139 0.418378 0.727586 0.025 Uiso 1 1 d R U . . .
O1 O 0.40196(18) 0.45207(16) 0.4098(2) 0.0148(4) Uani 1 1 d . . . . .
O2 O 0.44852(17) 0.28953(16) 0.3719(2) 0.0135(4) Uani 1 1 d . . . . .
O3 O 0.77227(19) 0.34782(17) 0.7272(2) 0.0171(5) Uani 1 1 d . . . . .
O4 O 0.72748(19) 0.25002(17) 0.8982(2) 0.0178(5) Uani 1 1 d . . . . .
O5 O 0.60004(19) 0.18393(17) 0.6109(2) 0.0166(5) Uani 1 1 d . . . . .
O6 O 0.59665(18) 0.06162(16) 0.7753(2) 0.0130(4) Uani 1 1 d . . . . .
C1 C 0.3835(3) 0.3632(2) 0.3598(3) 0.0130(6) Uani 1 1 d . . . . .
C2 C 0.2680(3) 0.3410(2) 0.2770(4) 0.0180(7) Uani 1 1 d . . . . .
C3 C 0.7904(3) 0.3030(2) 0.8421(3) 0.0141(6) Uani 1 1 d . . . . .
C4 C 0.9076(3) 0.3133(3) 0.9234(3) 0.0206(7) Uani 1 1 d . . . . .
C5 C 0.6132(2) 0.0956(2) 0.6604(3) 0.0116(6) Uani 1 1 d . . . . .
C6 C 0.6590(3) 0.0149(2) 0.5668(3) 0.0152(6) Uani 1 1 d . . . . .
C7 C 0.8540(3) 0.5195(3) 0.4084(3) 0.0221(7) Uani 1 1 d . . . . .
C8 C 0.9266(3) 0.5767(3) 0.3332(4) 0.0365(10) Uani 1 1 d . . . . .
H8A H 0.961500 0.633474 0.392183 0.055 Uiso 1 1 calc R U . . .
H8B H 0.884569 0.605447 0.246641 0.055 Uiso 1 1 calc R U . . .
H8C H 0.982611 0.529441 0.310354 0.055 Uiso 1 1 calc R U . . .
F1 F 0.21542(18) 0.42550(16) 0.2275(2) 0.0327(5) Uani 1 1 d . . . . .
F2 F 0.27144(18) 0.27631(18) 0.1709(2) 0.0377(6) Uani 1 1 d . . . . .
F3 F 0.20875(17) 0.29423(18) 0.3610(2) 0.0337(5) Uani 1 1 d . . . . .
F4 F 0.94673(17) 0.40924(18) 0.9167(2) 0.0308(5) Uani 1 1 d . . . . .
F5 F 0.91652(17) 0.28968(18) 1.0587(2) 0.0297(5) Uani 1 1 d . . . . .
F6 F 0.97336(18) 0.24887(19) 0.8696(2) 0.0339(5) Uani 1 1 d . . . . .
F7 F 0.60610(17) 0.01733(17) 0.4353(2) 0.0287(5) Uani 1 1 d . . . . .
F8 F 0.65606(19) -0.08236(15) 0.6129(2) 0.0289(5) Uani 1 1 d . . . . .
F9 F 0.76379(16) 0.03641(15) 0.5642(2) 0.0235(4) 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
La1 O4 2.407(2) 4_565 ?
La1 O3 2.474(2) . ?
La1 O1W 2.481(2) . ?
La1 O5 2.485(2) . ?
La1 O1 2.506(2) 3_666 ?
La1 O6 2.554(2) 4_565 ?
La1 O2 2.574(2) . ?
La1 N1 2.737(3) . ?
La1 O1 3.010(2) . ?
N1 C7 1.135(4) . ?
O1 C1 1.246(3) . ?
O2 C1 1.239(4) . ?
O3 C3 1.240(4) . ?
O4 C3 1.236(4) . ?
O5 C5 1.231(4) . ?
O6 C5 1.248(3) . ?
C1 C2 1.545(4) . ?
C2 F1 1.314(4) . ?
C2 F2 1.330(4) . ?
C2 F3 1.337(4) . ?
C3 C4 1.538(5) . ?
C4 F4 1.332(4) . ?
C4 F5 1.333(4) . ?
C4 F6 1.336(4) . ?
C5 C6 1.554(4) . ?
C6 F7 1.328(4) . ?
C6 F8 1.330(4) . ?
C6 F9 1.341(4) . ?
C7 C8 1.459(5) . ?

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
O4 La1 O3 87.77(8) 4_565 . ?
O4 La1 O1W 144.14(7) 4_565 . ?
O3 La1 O1W 88.17(8) . . ?
O4 La1 O5 74.07(7) 4_565 . ?
O3 La1 O5 76.63(7) . . ?
O1W La1 O5 70.33(7) . . ?
O4 La1 O1 143.81(7) 4_565 3_666 ?
O3 La1 O1 88.45(7) . 3_666 ?
O1W La1 O1 71.60(7) . 3_666 ?
O5 La1 O1 139.33(7) . 3_666 ?
O4 La1 O6 75.55(7) 4_565 4_565 ?
O3 La1 O6 137.42(7) . 4_565 ?
O1W La1 O6 127.50(7) . 4_565 ?
O5 La1 O6 132.33(7) . 4_565 ?
O1 La1 O6 83.27(7) 3_666 4_565 ?
O4 La1 O2 88.61(7) 4_565 . ?
O3 La1 O2 150.03(7) . . ?
O1W La1 O2 77.64(7) . . ?
O5 La1 O2 73.77(7) . . ?
O1 La1 O2 111.21(7) 3_666 . ?
O6 La1 O2 69.62(7) 4_565 . ?
O4 La1 N1 72.25(8) 4_565 . ?
O3 La1 N1 72.23(8) . . ?
O1W La1 N1 139.12(8) . . ?
O5 La1 N1 134.39(8) . . ?
O1 La1 N1 72.34(8) 3_666 . ?
O6 La1 N1 65.44(8) 4_565 . ?
O2 La1 N1 134.17(7) . . ?
O4 La1 O1 126.18(7) 4_565 . ?
O3 La1 O1 146.02(7) . . ?
O1W La1 O1 64.00(7) . . ?
O5 La1 O1 108.80(7) . . ?
O1 La1 O1 65.29(8) 3_666 . ?
O6 La1 O1 63.68(6) 4_565 . ?
O2 La1 O1 45.93(6) . . ?
N1 La1 O1 115.73(7) . . ?
C7 N1 La1 162.7(3) . . ?
La1 O1 La1 114.71(8) 3_666 . ?
C1 O2 La1 104.46(18) . . ?
C3 O3 La1 138.4(2) . . ?
C3 O4 La1 173.4(2) . 4_566 ?
C5 O5 La1 165.9(2) . . ?
C5 O6 La1 133.63(19) . 4_566 ?
O2 C1 O1 126.2(3) . . ?
O2 C1 C2 116.3(3) . . ?
O1 C1 C2 117.5(3) . . ?
O2 C1 La1 52.95(16) . . ?
O1 C1 La1 73.25(18) . . ?
C2 C1 La1 169.1(2) . . ?
F1 C2 F2 108.4(3) . . ?
F1 C2 F3 107.5(3) . . ?
F2 C2 F3 106.8(3) . . ?
F1 C2 C1 113.3(3) . . ?
F2 C2 C1 111.2(3) . . ?
F3 C2 C1 109.3(3) . . ?
O4 C3 O3 128.6(3) . . ?
O4 C3 C4 116.2(3) . . ?
O3 C3 C4 115.2(3) . . ?
F4 C4 F5 107.0(3) . . ?
F4 C4 F6 107.3(3) . . ?
F5 C4 F6 107.2(3) . . ?
F4 C4 C3 112.2(3) . . ?
F5 C4 C3 113.0(3) . . ?
F6 C4 C3 109.9(3) . . ?
O5 C5 O6 129.7(3) . . ?
O5 C5 C6 115.1(3) . . ?
O6 C5 C6 115.2(3) . . ?
F7 C6 F8 107.9(3) . . ?
F7 C6 F9 107.2(2) . . ?
F8 C6 F9 106.6(3) . . ?
F7 C6 C5 112.0(3) . . ?
F8 C6 C5 113.3(2) . . ?
F9 C6 C5 109.6(3) . . ?
N1 C7 C8 179.0(4) . . ?

_refine_diff_density_max         1.065
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.138



####################################################################### 
# 
# 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_Prtfa4detaH
_database_code_depnum_ccdc_archive 'CCDC 2347612'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C8 F12 Pr O8), C4 H15 N3'
_chemical_formula_sum            'C20 H15 F24 N3 O16 Pr2'
_chemical_formula_weight         1291.17

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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'

_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'

_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+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                   8.633(3)
_cell_length_b                   23.337(16)
_cell_length_c                   35.961(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7245(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    309
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      22.63

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_F_000             4944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    2.855
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5037
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36584
_diffrn_reflns_av_unetI/netI     0.2734
_diffrn_reflns_av_R_equivalents  0.3385
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.835
_diffrn_reflns_theta_max         27.226
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8052
_reflns_number_gt                2761
_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       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL XT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_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)] 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     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00056(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8052
_refine_ls_number_parameters     589
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.2241
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.2624
_refine_ls_wR_factor_gt          0.1709
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_restrained_S_all      0.918
_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
Pr1 Pr 0.68862(11) 0.73894(5) 0.21570(3) 0.0516(3) Uani 1 1 d . . . . .
Pr2 Pr 0.24983(13) 0.49697(5) 0.48334(3) 0.0495(3) Uani 1 1 d . . . . .
N1 N 0.2838(17) 0.5799(7) 0.3718(4) 0.058(4) Uani 1 1 d . . . . .
H1A H 0.330442 0.604206 0.388139 0.087 Uiso 1 1 calc R U . . .
H1B H 0.249323 0.548375 0.384178 0.087 Uiso 1 1 calc R U . . .
H1C H 0.202344 0.597963 0.360836 0.087 Uiso 1 1 calc R U . . .
N2 N 0.2951(19) 0.4687(7) 0.3474(4) 0.054(4) Uani 1 1 d . . . . .
H2 H 0.379451 0.453958 0.359147 0.065 Uiso 1 1 d R U . . .
N3 N 0.1967(18) 0.3687(7) 0.3900(5) 0.059(4) Uani 1 1 d . . . . .
H3A H 0.129094 0.355651 0.407448 0.088 Uiso 1 1 calc R U . . .
H3B H 0.259470 0.395718 0.400243 0.088 Uiso 1 1 calc R U . . .
H3C H 0.255186 0.339009 0.381475 0.088 Uiso 1 1 calc R U . . .
O1 O 0.6613(14) 0.7758(5) 0.1475(4) 0.053(3) Uani 1 1 d . . . . .
O2 O 0.6461(14) 0.6840(6) 0.1545(4) 0.057(4) Uani 1 1 d . . . . .
O3 O 0.7700(15) 0.6455(6) 0.2390(4) 0.062(4) Uani 1 1 d . . . . .
O4 O 0.9492(13) 0.6859(7) 0.2734(4) 0.061(4) Uani 1 1 d . . . . .
O5 O 0.5043(14) 0.8170(6) 0.2162(4) 0.057(3) Uani 1 1 d . . . . .
O6 O 0.3406(13) 0.8177(6) 0.2646(4) 0.061(4) Uani 1 1 d . . . . .
O7 O 0.9366(14) 0.7269(7) 0.1856(4) 0.073(5) Uani 1 1 d . . . . .
O8 O 1.1501(14) 0.7472(7) 0.2182(4) 0.067(4) Uani 1 1 d . . . . .
O9 O -0.1296(14) 0.4116(6) 0.5040(4) 0.057(4) Uani 1 1 d . . . . .
O10 O 0.0867(13) 0.4132(6) 0.4692(4) 0.053(4) Uani 1 1 d . . . . .
O11 O 0.3885(14) 0.4418(5) 0.4329(3) 0.048(3) Uani 1 1 d . . . . .
O12 O 0.5896(15) 0.4622(7) 0.4684(4) 0.060(4) Uani 1 1 d . . . . .
O13 O -0.1002(14) 0.5185(6) 0.4614(4) 0.053(4) Uani 1 1 d . . . . .
O14 O 0.1080(15) 0.5186(6) 0.4243(4) 0.058(4) Uani 1 1 d . . . . .
O15 O 0.5852(15) 0.4322(6) 0.5503(4) 0.058(4) Uani 1 1 d . . . . .
O16 O 0.3718(14) 0.4177(6) 0.5160(4) 0.052(3) Uani 1 1 d . . . . .
F1 F 0.6894(12) 0.7613(5) 0.0740(3) 0.060(3) Uani 1 1 d . . . . .
F2 F 0.4619(11) 0.7310(5) 0.0866(3) 0.068(3) Uani 1 1 d . . . . .
F3 F 0.6472(14) 0.6720(6) 0.0800(3) 0.073(4) Uani 1 1 d . . . . .
F4 F 0.924(3) 0.5473(7) 0.2611(5) 0.134(8) Uani 1 1 d . . . . .
F5 F 0.7627(17) 0.5741(9) 0.3017(6) 0.137(8) Uani 1 1 d . . . . .
F6 F 1.0035(12) 0.5887(5) 0.3090(3) 0.065(3) Uani 1 1 d . . . . .
F7 F 0.1724(15) 0.8885(8) 0.2168(5) 0.132(7) Uani 1 1 d . . . . .
F8 F 0.3746(17) 0.9056(6) 0.1865(4) 0.085(4) Uani 1 1 d . . . . .
F9 F 0.357(2) 0.9357(7) 0.2411(4) 0.113(6) Uani 1 1 d . . . . .
F10 F 1.0825(13) 0.7644(6) 0.1252(3) 0.071(3) Uani 1 1 d . . . . .
F11 F 1.2244(16) 0.6942(7) 0.1442(4) 0.093(5) Uani 1 1 d . . . . .
F12 F 1.2850(15) 0.7799(8) 0.1565(4) 0.112(6) Uani 1 1 d . . . . .
F13 F 0.1016(13) 0.3019(5) 0.4980(4) 0.074(4) Uani 1 1 d . . . . .
F14 F -0.0162(12) 0.3089(5) 0.4459(3) 0.060(3) Uani 1 1 d . . . . .
F15 F -0.1468(13) 0.3002(5) 0.4957(4) 0.072(4) Uani 1 1 d . . . . .
F16 F 0.7677(12) 0.4092(6) 0.4155(4) 0.074(4) Uani 1 1 d . . . . .
F17 F 0.6340(15) 0.3431(6) 0.4396(4) 0.087(4) Uani 1 1 d . . . . .
F18 F 0.5628(14) 0.3804(7) 0.3886(4) 0.094(5) Uani 1 1 d . . . . .
F19 F -0.2864(11) 0.5391(6) 0.4047(3) 0.070(4) Uani 1 1 d . . . . .
F20 F -0.1016(13) 0.5962(5) 0.3884(3) 0.067(3) Uani 1 1 d . . . . .
F21 F -0.1069(12) 0.5111(6) 0.3685(3) 0.066(3) Uani 1 1 d . . . . .
F22 F 0.5341(15) 0.3073(7) 0.5344(4) 0.089(4) Uani 1 1 d . . . . .
F23 F 0.5163(14) 0.3415(5) 0.5898(4) 0.078(4) Uani 1 1 d . . . . .
F24 F 0.3093(13) 0.3274(5) 0.5578(3) 0.070(3) Uani 1 1 d . . . . .
C1 C 0.645(2) 0.7269(10) 0.1357(6) 0.055(5) Uani 1 1 d . . . . .
C2 C 0.613(2) 0.7217(10) 0.0932(6) 0.059(5) Uani 1 1 d . U . . .
C3 C 0.872(2) 0.6444(10) 0.2632(5) 0.050(5) Uani 1 1 d . . . . .
C4 C 0.892(3) 0.5901(11) 0.2841(8) 0.075(7) Uani 1 1 d . . . . .
C5 C 0.395(2) 0.8368(10) 0.2352(7) 0.062(4) Uani 1 1 d . U . . .
C6 C 0.321(2) 0.8934(10) 0.2196(7) 0.063(4) Uani 1 1 d . U . . .
C7 C 1.073(2) 0.7388(9) 0.1896(5) 0.054(5) Uani 1 1 d . . . . .
C8 C 1.167(3) 0.7452(11) 0.1529(6) 0.069(6) Uani 1 1 d . U . . .
C9 C -0.024(2) 0.3901(10) 0.4854(6) 0.062(6) Uani 1 1 d . . . . .
C10 C -0.025(2) 0.3232(11) 0.4812(6) 0.061(6) Uani 1 1 d . . . . .
C11 C 0.529(2) 0.4352(9) 0.4404(6) 0.056(4) Uani 1 1 d . U . . .
C12 C 0.625(2) 0.3911(9) 0.4214(6) 0.058(4) Uani 1 1 d . U . . .
C13 C -0.0334(19) 0.5234(9) 0.4311(5) 0.048(4) Uani 1 1 d . U . . .
C14 C -0.134(2) 0.5433(9) 0.3980(6) 0.048(4) Uani 1 1 d . U . . .
C15 C 0.465(2) 0.4052(10) 0.5394(6) 0.058(6) Uani 1 1 d . . . . .
C16 C 0.462(2) 0.3434(10) 0.5556(6) 0.058(5) Uani 1 1 d . . . . .
C17 C 0.403(2) 0.5614(10) 0.3414(6) 0.070(7) Uani 1 1 d . . . . .
H17A H 0.420028 0.593422 0.323845 0.084 Uiso 1 1 calc R U . . .
H17B H 0.503259 0.552014 0.353266 0.084 Uiso 1 1 calc R U . . .
C18 C 0.346(3) 0.5116(8) 0.3212(6) 0.059(6) Uani 1 1 d . . . . .
H18A H 0.258837 0.522892 0.304873 0.071 Uiso 1 1 calc R U . . .
H18B H 0.429598 0.495752 0.305338 0.071 Uiso 1 1 calc R U . . .
C19 C 0.213(2) 0.4220(11) 0.3297(6) 0.073(7) Uani 1 1 d . . . . .
H19A H 0.287572 0.393777 0.319554 0.088 Uiso 1 1 calc R U . . .
H19B H 0.148694 0.436622 0.308989 0.088 Uiso 1 1 calc R U . . .
C20 C 0.111(2) 0.3938(10) 0.3591(7) 0.073(7) Uani 1 1 d . . . . .
H20A H 0.038253 0.422880 0.369109 0.088 Uiso 1 1 calc R U . . .
H20B H 0.048110 0.363455 0.347136 0.088 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
Pr1 O6 2.368(14) 6_656 ?
Pr1 O8 2.408(14) 6_556 ?
Pr1 O7 2.415(13) . ?
Pr1 O5 2.418(13) . ?
Pr1 O3 2.440(14) . ?
Pr1 O4 2.441(13) 6_556 ?
Pr1 O2 2.575(14) . ?
Pr1 O1 2.610(14) . ?
Pr1 C1 2.91(2) . ?
Pr2 O13 2.398(13) 5_566 ?
Pr2 O9 2.416(14) 5_566 ?
Pr2 O12 2.417(14) 5_666 ?
Pr2 O16 2.430(14) . ?
Pr2 O10 2.461(14) . ?
Pr2 O15 2.495(14) 5_666 ?
Pr2 O14 2.503(15) . ?
Pr2 O11 2.526(12) . ?
N1 C17 1.56(2) . ?
N2 C18 1.44(2) . ?
N2 C19 1.45(3) . ?
N3 C20 1.46(2) . ?
O1 C1 1.22(2) . ?
O2 C1 1.21(2) . ?
O3 C3 1.24(2) . ?
O4 C3 1.23(2) . ?
O5 C5 1.26(2) . ?
O6 C5 1.24(2) . ?
O7 C7 1.22(2) . ?
O8 C7 1.24(2) . ?
O9 C9 1.23(2) . ?
O10 C9 1.24(2) . ?
O11 C11 1.25(2) . ?
O12 C11 1.30(2) . ?
O13 C13 1.24(2) . ?
O14 C13 1.25(2) . ?
O15 C15 1.28(2) . ?
O16 C15 1.20(2) . ?
F1 C2 1.33(2) . ?
F2 C2 1.35(2) . ?
F3 C2 1.29(2) . ?
F4 C4 1.33(3) . ?
F5 C4 1.34(3) . ?
F6 C4 1.31(2) . ?
F7 C6 1.29(2) . ?
F8 C6 1.31(2) . ?
F9 C6 1.29(3) . ?
F10 C8 1.31(2) . ?
F11 C8 1.33(3) . ?
F12 C8 1.31(2) . ?
F13 C10 1.34(2) . ?
F14 C10 1.31(2) . ?
F15 C10 1.29(2) . ?
F16 C12 1.32(2) . ?
F17 C12 1.30(2) . ?
F18 C12 1.32(2) . ?
F19 C14 1.338(19) . ?
F20 C14 1.31(2) . ?
F21 C14 1.32(2) . ?
F22 C16 1.30(2) . ?
F23 C16 1.31(2) . ?
F24 C16 1.37(2) . ?
C1 C2 1.56(3) . ?
C3 C4 1.48(3) . ?
C5 C6 1.57(3) . ?
C7 C8 1.56(3) . ?
C9 C10 1.57(3) . ?
C11 C12 1.49(3) . ?
C13 C14 1.55(3) . ?
C15 C16 1.55(3) . ?
C17 C18 1.46(3) . ?
C19 C20 1.53(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
O6 Pr1 O8 73.7(5) 6_656 6_556 ?
O6 Pr1 O7 74.6(5) 6_656 . ?
O8 Pr1 O7 125.0(5) 6_556 . ?
O6 Pr1 O5 77.2(5) 6_656 . ?
O8 Pr1 O5 80.9(5) 6_556 . ?
O7 Pr1 O5 132.4(5) . . ?
O6 Pr1 O3 115.6(5) 6_656 . ?
O8 Pr1 O3 76.8(5) 6_556 . ?
O7 Pr1 O3 78.1(5) . . ?
O5 Pr1 O3 149.3(5) . . ?
O6 Pr1 O4 144.6(5) 6_656 6_556 ?
O8 Pr1 O4 76.4(5) 6_556 6_556 ?
O7 Pr1 O4 139.8(5) . 6_556 ?
O5 Pr1 O4 79.9(5) . 6_556 ?
O3 Pr1 O4 74.6(5) . 6_556 ?
O6 Pr1 O2 136.3(5) 6_656 . ?
O8 Pr1 O2 149.8(5) 6_556 . ?
O7 Pr1 O2 71.6(5) . . ?
O5 Pr1 O2 106.7(4) . . ?
O3 Pr1 O2 83.6(5) . . ?
O4 Pr1 O2 76.4(4) 6_556 . ?
O6 Pr1 O1 94.4(5) 6_656 . ?
O8 Pr1 O1 152.8(4) 6_556 . ?
O7 Pr1 O1 72.4(4) . . ?
O5 Pr1 O1 72.5(4) . . ?
O3 Pr1 O1 130.0(4) . . ?
O4 Pr1 O1 104.0(4) 6_556 . ?
O2 Pr1 O1 49.3(4) . . ?
O6 Pr1 C1 116.2(6) 6_656 . ?
O8 Pr1 C1 164.7(5) 6_556 . ?
O7 Pr1 C1 70.1(5) . . ?
O5 Pr1 C1 89.7(5) . . ?
O3 Pr1 C1 106.8(6) . . ?
O4 Pr1 C1 90.1(5) 6_556 . ?
O2 Pr1 C1 24.4(5) . . ?
O1 Pr1 C1 24.8(5) . . ?
O13 Pr2 O9 75.2(5) 5_566 5_566 ?
O13 Pr2 O12 76.9(4) 5_566 5_666 ?
O9 Pr2 O12 76.3(5) 5_566 5_666 ?
O13 Pr2 O16 73.6(4) 5_566 . ?
O9 Pr2 O16 140.1(5) 5_566 . ?
O12 Pr2 O16 72.8(5) 5_666 . ?
O13 Pr2 O10 75.1(4) 5_566 . ?
O9 Pr2 O10 119.6(4) 5_566 . ?
O12 Pr2 O10 142.1(5) 5_666 . ?
O16 Pr2 O10 75.1(4) . . ?
O13 Pr2 O15 144.0(5) 5_566 5_666 ?
O9 Pr2 O15 75.7(5) 5_566 5_666 ?
O12 Pr2 O15 76.1(5) 5_666 5_666 ?
O16 Pr2 O15 119.4(4) . 5_666 ?
O10 Pr2 O15 138.8(4) . 5_666 ?
O13 Pr2 O14 118.1(4) 5_566 . ?
O9 Pr2 O14 76.8(4) 5_566 . ?
O12 Pr2 O14 144.1(5) 5_666 . ?
O16 Pr2 O14 140.8(5) . . ?
O10 Pr2 O14 72.9(4) . . ?
O15 Pr2 O14 74.6(4) 5_666 . ?
O13 Pr2 O11 140.7(5) 5_566 . ?
O9 Pr2 O11 142.2(4) 5_566 . ?
O12 Pr2 O11 116.4(4) 5_666 . ?
O16 Pr2 O11 75.7(4) . . ?
O10 Pr2 O11 73.6(4) . . ?
O15 Pr2 O11 73.7(4) 5_666 . ?
O14 Pr2 O11 74.1(4) . . ?
C18 N2 C19 112.6(17) . . ?
C1 O1 Pr1 91.6(12) . . ?
C1 O2 Pr1 93.7(14) . . ?
C3 O3 Pr1 117.6(14) . . ?
C3 O4 Pr1 155.1(13) . 6_656 ?
C5 O5 Pr1 141.0(14) . . ?
C5 O6 Pr1 138.1(15) . 6_556 ?
C7 O7 Pr1 141.0(14) . . ?
C7 O8 Pr1 151.6(14) . 6_656 ?
C9 O9 Pr2 141.1(14) . 5_566 ?
C9 O10 Pr2 133.5(15) . . ?
C11 O11 Pr2 111.5(13) . . ?
C11 O12 Pr2 168.3(13) . 5_666 ?
C13 O13 Pr2 173.9(13) . 5_566 ?
C13 O14 Pr2 109.2(13) . . ?
C15 O15 Pr2 130.0(13) . 5_666 ?
C15 O16 Pr2 144.5(15) . . ?
O2 C1 O1 125(2) . . ?
O2 C1 C2 119(2) . . ?
O1 C1 C2 115.5(19) . . ?
O2 C1 Pr1 61.9(12) . . ?
O1 C1 Pr1 63.6(11) . . ?
C2 C1 Pr1 176.9(14) . . ?
F3 C2 F1 108.8(17) . . ?
F3 C2 F2 107.5(17) . . ?
F1 C2 F2 106.1(17) . . ?
F3 C2 C1 113.0(18) . . ?
F1 C2 C1 111.6(17) . . ?
F2 C2 C1 109.5(16) . . ?
O4 C3 O3 125(2) . . ?
O4 C3 C4 117.1(19) . . ?
O3 C3 C4 117(2) . . ?
F6 C4 F4 105(2) . . ?
F6 C4 F5 106(2) . . ?
F4 C4 F5 105(2) . . ?
F6 C4 C3 117(2) . . ?
F4 C4 C3 111(2) . . ?
F5 C4 C3 112(2) . . ?
O6 C5 O5 128(2) . . ?
O6 C5 C6 117(2) . . ?
O5 C5 C6 115(2) . . ?
F7 C6 F9 111(2) . . ?
F7 C6 F8 108(2) . . ?
F9 C6 F8 107.0(19) . . ?
F7 C6 C5 110.9(18) . . ?
F9 C6 C5 109.1(19) . . ?
F8 C6 C5 111.3(19) . . ?
O7 C7 O8 130.7(19) . . ?
O7 C7 C8 115.2(18) . . ?
O8 C7 C8 114.0(17) . . ?
F12 C8 F10 107(2) . . ?
F12 C8 F11 107(2) . . ?
F10 C8 F11 110(2) . . ?
F12 C8 C7 112.5(19) . . ?
F10 C8 C7 112.7(18) . . ?
F11 C8 C7 107.8(19) . . ?
O9 C9 O10 130(2) . . ?
O9 C9 C10 117.1(19) . . ?
O10 C9 C10 113(2) . . ?
F15 C10 F14 109.4(16) . . ?
F15 C10 F13 109.1(19) . . ?
F14 C10 F13 107.1(17) . . ?
F15 C10 C9 112.2(18) . . ?
F14 C10 C9 110.3(19) . . ?
F13 C10 C9 108.7(16) . . ?
O11 C11 O12 119.8(19) . . ?
O11 C11 C12 122(2) . . ?
O12 C11 C12 118.0(18) . . ?
F17 C12 F16 107.7(17) . . ?
F17 C12 F18 108(2) . . ?
F16 C12 F18 107.2(18) . . ?
F17 C12 C11 113.6(19) . . ?
F16 C12 C11 111.8(19) . . ?
F18 C12 C11 108.3(17) . . ?
O13 C13 O14 128.4(19) . . ?
O13 C13 C14 116.2(15) . . ?
O14 C13 C14 115.2(17) . . ?
F20 C14 F21 106.4(16) . . ?
F20 C14 F19 109.1(17) . . ?
F21 C14 F19 106.1(15) . . ?
F20 C14 C13 111.4(16) . . ?
F21 C14 C13 110.3(16) . . ?
F19 C14 C13 113.2(16) . . ?
O16 C15 O15 130(2) . . ?
O16 C15 C16 119(2) . . ?
O15 C15 C16 110.8(18) . . ?
F22 C16 F23 110.9(19) . . ?
F22 C16 F24 108.5(18) . . ?
F23 C16 F24 106.3(17) . . ?
F22 C16 C15 112.1(19) . . ?
F23 C16 C15 112.0(18) . . ?
F24 C16 C15 106.7(17) . . ?
C18 C17 N1 110.4(17) . . ?
N2 C18 C17 109.2(18) . . ?
N2 C19 C20 107.6(18) . . ?
N3 C20 C19 113.9(18) . . ?

_refine_diff_density_max         1.309
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.187

# start Validation Reply Form
_vrf_PLAT020_Prtfa4detaH         
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.338 Report
RESPONSE: The crystal a had tiny needele-like shape with a weak scattering
power. The data were collected at an exposition time of 60 seconds per frame.
The crystal was strongly affected by radiation damage during data acquisition. 
To achieve the required data completeness two independent diffraction
experiments were performed and the acquired datasets were combined.
;
_vrf_PLAT026_Prtfa4detaH         
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        34% Check
RESPONSE: Crystal had a weak scattering power, significant angular decay and
was affected by radiation damage.
;
_vrf_PLAT342_Prtfa4detaH         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: Weak scattering power of crystal and small number of intense 
reflection affected the precision of analysis.
;
# end Validation Reply Form




####################################################################### 
# 
# 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_Ndtfa4detaH
_database_code_depnum_ccdc_archive 'CCDC 2347613'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 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         '2(C8 F12 Nd O8), C4 H15 N3'
_chemical_formula_sum            'C20 H15 F24 N3 Nd2 O16'
_chemical_formula_weight         1297.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Nd Nd -0.1943 3.0179 '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'
H H 0.0000 0.0000 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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+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                   8.6514(16)
_cell_length_b                   23.450(5)
_cell_length_c                   35.880(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7279(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5015
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.92

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale violet'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.368
_exptl_crystal_F_000             4960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    3.017
_shelx_estimated_absorpt_T_min   0.508
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5406
_exptl_absorpt_correction_T_max  0.8763
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28710
_diffrn_reflns_av_unetI/netI     0.1429
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.827
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        26.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             7870
_reflns_number_gt                5110
_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       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_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)+(0.0250P)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         7870
_refine_ls_number_parameters     588
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1471
_refine_ls_wR_factor_gt          0.1220
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_restrained_S_all      0.951
_refine_ls_shift/su_max          0.002
_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
Nd1 Nd 0.31298(5) 0.76084(2) 0.21581(2) 0.01536(12) Uani 1 1 d . . . . .
Nd2 Nd 1.25000(5) 0.49698(2) 0.51654(2) 0.01319(12) Uani 1 1 d . . . . .
N1 N 0.2833(8) 0.4202(3) 0.12796(18) 0.0232(16) Uani 1 1 d . . . . .
H1A H 0.330470 0.404661 0.107691 0.035 Uiso 1 1 calc R U . . .
H1B H 0.230363 0.451973 0.120977 0.035 Uiso 1 1 calc R U . . .
H1C H 0.216533 0.394395 0.137949 0.035 Uiso 1 1 calc R U . . .
N2 N 0.2948(9) 0.5314(3) 0.15321(19) 0.0274(17) Uani 1 1 d . . . . .
H2 H 0.382034 0.546576 0.142696 0.041 Uiso 1 1 d R U . . .
N3 N 0.1957(8) 0.6321(3) 0.11036(17) 0.0223(15) Uani 1 1 d . . . . .
H3A H 0.130273 0.645665 0.092584 0.034 Uiso 1 1 calc R U . . .
H3B H 0.259218 0.605435 0.100155 0.034 Uiso 1 1 calc R U . . .
H3C H 0.253399 0.661361 0.119579 0.034 Uiso 1 1 calc R U . . .
O1 O 0.3389(7) 0.7228(2) 0.14820(15) 0.0226(13) Uani 1 1 d . . . . .
O2 O 0.3525(6) 0.8167(2) 0.15449(14) 0.0209(12) Uani 1 1 d . . . . .
O3 O 0.1628(6) 0.6807(2) 0.23565(14) 0.0203(12) Uani 1 1 d . . . . .
O5 O 0.5471(6) 0.8132(2) 0.22568(15) 0.0224(13) Uani 1 1 d . . . . .
O6 O 0.7306(7) 0.8536(3) 0.26068(17) 0.0299(15) Uani 1 1 d . . . . .
O7 O 0.3519(7) 0.7520(2) 0.28153(15) 0.0215(13) Uani 1 1 d . . . . .
O8 O 0.5642(7) 0.7734(3) 0.31411(16) 0.0270(14) Uani 1 1 d . . . . .
O9 O 1.3714(6) 0.5886(2) 0.50424(14) 0.0182(12) Uani 1 1 d . . . . .
O10 O 1.5889(6) 0.5862(2) 0.46898(14) 0.0176(12) Uani 1 1 d . . . . .
O12 O 1.0933(7) 0.5383(2) 0.46816(14) 0.0223(13) Uani 1 1 d . . . . .
O13 O 1.4018(7) 0.4822(2) 0.46178(14) 0.0200(13) Uani 1 1 d . . . . .
O14 O 1.6060(6) 0.4810(2) 0.42453(14) 0.0176(12) Uani 1 1 d . . . . .
O16 O 1.1293(6) 0.4172(2) 0.48414(14) 0.0189(12) Uani 1 1 d . . . . .
F1 F 0.3097(7) 0.7385(2) 0.07416(13) 0.0342(13) Uani 1 1 d . . . . .
F2 F 0.5382(6) 0.7689(2) 0.08660(14) 0.0312(12) Uani 1 1 d . . . . .
F3 F 0.3526(6) 0.8283(2) 0.08018(12) 0.0311(12) Uani 1 1 d . . . . .
F4 F 0.3273(8) 0.6115(3) 0.2831(2) 0.082(3) Uani 1 1 d . U . . .
F5 F 0.1424(10) 0.5645(3) 0.25892(18) 0.078(3) Uani 1 1 d . . . . .
F6 F 0.1251(8) 0.5935(3) 0.31344(15) 0.0518(17) Uani 1 1 d . . . . .
F7 F 0.4959(6) 0.9112(2) 0.19112(13) 0.0316(12) Uani 1 1 d . . . . .
F8 F 0.7369(7) 0.9245(3) 0.1982(2) 0.077(2) Uani 1 1 d . U . . .
F9 F 0.5767(11) 0.9520(3) 0.23933(19) 0.088(3) Uani 1 1 d . U . . .
F10 F 0.2157(8) 0.7193(4) 0.34326(17) 0.071(2) Uani 1 1 d . U . . .
F11 F 0.4182(7) 0.7370(2) 0.37495(13) 0.0375(14) Uani 1 1 d . . . . .
F12 F 0.2788(7) 0.8062(3) 0.35591(15) 0.0555(18) Uani 1 1 d . . . . .
F13 F 1.4834(6) 0.68964(19) 0.44531(12) 0.0253(11) Uani 1 1 d . . . . .
F14 F 1.6012(6) 0.6972(2) 0.49750(15) 0.0389(14) Uani 1 1 d . . . . .
F15 F 1.3536(6) 0.6995(2) 0.49581(14) 0.0334(13) Uani 1 1 d . . . . .
F16 F 1.2674(5) 0.5908(2) 0.41503(15) 0.0361(13) Uani 1 1 d . . . . .
F17 F 1.0601(6) 0.6207(3) 0.38864(15) 0.0514(18) Uani 1 1 d . . . . .
F18 F 1.1320(7) 0.6556(2) 0.43984(17) 0.0488(16) Uani 1 1 d . . . . .
F19 F 1.3942(6) 0.4890(2) 0.36803(12) 0.0271(12) Uani 1 1 d . . . . .
F20 F 1.3992(6) 0.4032(2) 0.38856(14) 0.0332(13) Uani 1 1 d . . . . .
F21 F 1.2164(5) 0.4597(3) 0.40467(13) 0.0326(13) Uani 1 1 d . . . . .
F22 F 0.9684(7) 0.3075(2) 0.46562(17) 0.0490(16) Uani 1 1 d . . . . .
F23 F 0.9827(7) 0.3410(2) 0.41042(15) 0.0449(16) Uani 1 1 d . . . . .
F24 F 1.1881(6) 0.3270(2) 0.44189(14) 0.0359(13) Uani 1 1 d . . . . .
C1 C 0.3537(9) 0.7719(3) 0.1351(2) 0.0175(17) Uani 1 1 d . . . . .
C2 C 0.3893(10) 0.7770(4) 0.0938(2) 0.0235(19) Uani 1 1 d . . . . .
C3 C 0.1049(9) 0.6633(3) 0.2652(2) 0.0203(18) Uani 1 1 d . . . . .
C4 C 0.1759(10) 0.6072(4) 0.2809(2) 0.0240(19) Uani 1 1 d . . . . .
C5 C 0.6284(10) 0.8541(3) 0.2363(2) 0.0192(17) Uani 1 1 d . U . . .
C6 C 0.6099(11) 0.9115(4) 0.2161(2) 0.030(2) Uani 1 1 d . . . . .
C7 C 0.4278(10) 0.7600(3) 0.3104(2) 0.0189(17) Uani 1 1 d . . . . .
C8 C 0.3339(11) 0.7548(4) 0.3468(2) 0.031(2) Uani 1 1 d . . . . .
C9 C 1.4776(9) 0.6096(3) 0.4855(2) 0.0179(17) Uani 1 1 d . . . . .
C10 C 1.4771(10) 0.6758(3) 0.4815(2) 0.0209(18) Uani 1 1 d . . . . .
C11 C 1.0278(9) 0.5635(3) 0.4423(2) 0.0159(16) Uani 1 1 d D . . . .
C12 C 1.1225(10) 0.6065(4) 0.4208(2) 0.028(2) Uani 1 1 d D . . . .
C13 C 1.4671(9) 0.4752(3) 0.43107(19) 0.0132(16) Uani 1 1 d . . . . .
C14 C 1.3662(9) 0.4570(4) 0.3982(2) 0.0211(18) Uani 1 1 d . . . . .
C15 C 1.0283(9) 0.4048(3) 0.4613(2) 0.0156(17) Uani 1 1 d . . . . .
C16 C 1.0429(10) 0.3447(4) 0.4444(2) 0.026(2) Uani 1 1 d . . . . .
C17 C 0.4028(10) 0.4359(4) 0.1564(2) 0.029(2) Uani 1 1 d . . . . .
H17A H 0.500960 0.445936 0.143829 0.034 Uiso 1 1 calc R U . . .
H17B H 0.422344 0.403137 0.173139 0.034 Uiso 1 1 calc R U . . .
C18 C 0.3449(11) 0.4862(4) 0.1788(3) 0.032(2) Uani 1 1 d . . . . .
H18A H 0.257225 0.474289 0.194687 0.039 Uiso 1 1 calc R U . . .
H18B H 0.428359 0.500656 0.195103 0.039 Uiso 1 1 calc R U . . .
C19 C 0.2066(11) 0.5773(4) 0.1694(2) 0.032(2) Uani 1 1 d . . . . .
H19A H 0.278193 0.605704 0.180306 0.038 Uiso 1 1 calc R U . . .
H19B H 0.140948 0.562168 0.189657 0.038 Uiso 1 1 calc R U . . .
C20 C 0.1057(10) 0.6062(4) 0.1407(2) 0.029(2) Uani 1 1 d . . . . .
H20A H 0.033425 0.577842 0.130013 0.035 Uiso 1 1 calc R U . . .
H20B H 0.043443 0.636158 0.153044 0.035 Uiso 1 1 calc R U . . .
O15 O 0.9133(6) 0.4322(2) 0.45065(13) 0.0162(11) Uani 1 1 d . . . . .
O11 O 0.8882(6) 0.5589(2) 0.43314(13) 0.0160(11) Uani 1 1 d . . . . .
O4 O -0.0027(6) 0.6828(2) 0.28391(15) 0.0224(13) 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
Nd1 O7 2.391(5) . ?
Nd1 O3 2.394(5) . ?
Nd1 O5 2.395(5) . ?
Nd1 O8 2.423(6) 6_556 ?
Nd1 O4 2.428(5) 6_656 ?
Nd1 O6 2.439(6) 6_556 ?
Nd1 O2 2.583(5) . ?
Nd1 O1 2.594(5) . ?
Nd2 O13 2.389(5) . ?
Nd2 O12 2.406(5) . ?
Nd2 O9 2.432(5) . ?
Nd2 O16 2.438(5) . ?
Nd2 O10 2.453(5) 5_866 ?
Nd2 O15 2.477(5) 5_766 ?
Nd2 O14 2.508(5) 5_866 ?
Nd2 O11 2.531(5) 5_766 ?
N1 C17 1.498(10) . ?
N2 C19 1.442(11) . ?
N2 C18 1.466(11) . ?
N3 C20 1.469(10) . ?
O1 C1 1.249(10) . ?
O2 C1 1.259(9) . ?
O3 C3 1.241(9) . ?
O5 C5 1.248(10) . ?
O6 C5 1.244(10) . ?
O7 C7 1.240(10) . ?
O8 C7 1.229(10) . ?
O9 C9 1.240(9) . ?
O10 C9 1.257(9) . ?
O12 C11 1.238(9) . ?
O13 C13 1.249(9) . ?
O14 C13 1.231(9) . ?
O16 C15 1.232(9) . ?
F1 C2 1.336(10) . ?
F2 C2 1.328(9) . ?
F3 C2 1.336(9) . ?
F4 C4 1.315(11) . ?
F5 C4 1.309(11) . ?
F6 C4 1.288(9) . ?
F7 C6 1.333(10) . ?
F8 C6 1.309(11) . ?
F9 C6 1.296(11) . ?
F10 C8 1.323(11) . ?
F11 C8 1.315(10) . ?
F12 C8 1.337(11) . ?
F13 C10 1.338(9) . ?
F14 C10 1.319(9) . ?
F15 C10 1.310(9) . ?
F16 C12 1.323(10) . ?
F17 C12 1.318(10) . ?
F18 C12 1.341(10) . ?
F19 C14 1.338(9) . ?
F20 C14 1.339(9) . ?
F21 C14 1.319(9) . ?
F22 C16 1.326(10) . ?
F23 C16 1.328(9) . ?
F24 C16 1.325(9) . ?
C1 C2 1.521(11) . ?
C3 O4 1.235(9) . ?
C3 C4 1.557(11) . ?
C5 C6 1.537(11) . ?
C7 C8 1.543(12) . ?
C9 C10 1.558(10) . ?
C11 O11 1.256(9) . ?
C11 C12 1.511(11) . ?
C13 C14 1.529(10) . ?
C15 O15 1.245(9) . ?
C15 C16 1.541(11) . ?
C17 C18 1.513(12) . ?
C19 C20 1.510(12) . ?

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 Nd1 O3 73.43(18) . . ?
O7 Nd1 O5 77.27(19) . . ?
O3 Nd1 O5 144.87(19) . . ?
O7 Nd1 O8 124.9(2) . 6_556 ?
O3 Nd1 O8 75.23(19) . 6_556 ?
O5 Nd1 O8 138.96(19) . 6_556 ?
O7 Nd1 O4 80.66(18) . 6_656 ?
O3 Nd1 O4 76.30(19) . 6_656 ?
O5 Nd1 O4 80.2(2) . 6_656 ?
O8 Nd1 O4 132.6(2) 6_556 6_656 ?
O7 Nd1 O6 77.16(19) . 6_556 ?
O3 Nd1 O6 116.0(2) . 6_556 ?
O5 Nd1 O6 74.9(2) . 6_556 ?
O8 Nd1 O6 77.6(2) 6_556 6_556 ?
O4 Nd1 O6 149.6(2) 6_656 6_556 ?
O7 Nd1 O2 149.95(18) . . ?
O3 Nd1 O2 136.32(17) . . ?
O5 Nd1 O2 75.76(18) . . ?
O8 Nd1 O2 71.25(18) 6_556 . ?
O4 Nd1 O2 107.38(18) 6_656 . ?
O6 Nd1 O2 83.19(19) 6_556 . ?
O7 Nd1 O1 151.65(18) . . ?
O3 Nd1 O1 93.16(18) . . ?
O5 Nd1 O1 103.96(18) . . ?
O8 Nd1 O1 72.80(19) 6_556 . ?
O4 Nd1 O1 71.81(18) 6_656 . ?
O6 Nd1 O1 130.93(19) 6_556 . ?
O2 Nd1 O1 50.66(17) . . ?
O13 Nd2 O12 76.97(19) . . ?
O13 Nd2 O9 75.00(18) . . ?
O12 Nd2 O9 75.90(19) . . ?
O13 Nd2 O16 74.46(18) . . ?
O12 Nd2 O16 73.97(18) . . ?
O9 Nd2 O16 140.95(17) . . ?
O13 Nd2 O10 75.33(17) . 5_866 ?
O12 Nd2 O10 142.48(17) . 5_866 ?
O9 Nd2 O10 119.73(18) . 5_866 ?
O16 Nd2 O10 74.56(18) . 5_866 ?
O13 Nd2 O15 143.27(17) . 5_766 ?
O12 Nd2 O15 75.62(17) . 5_766 ?
O9 Nd2 O15 74.96(17) . 5_766 ?
O16 Nd2 O15 119.77(18) . 5_766 ?
O10 Nd2 O15 139.13(16) 5_866 5_766 ?
O13 Nd2 O14 116.76(19) . 5_866 ?
O12 Nd2 O14 143.61(18) . 5_866 ?
O9 Nd2 O14 75.90(17) . 5_866 ?
O16 Nd2 O14 140.62(17) . 5_866 ?
O10 Nd2 O14 72.73(17) 5_866 5_866 ?
O15 Nd2 O14 75.20(17) 5_766 5_866 ?
O13 Nd2 O11 140.49(17) . 5_766 ?
O12 Nd2 O11 117.21(18) . 5_766 ?
O9 Nd2 O11 142.27(16) . 5_766 ?
O16 Nd2 O11 74.95(17) . 5_766 ?
O10 Nd2 O11 72.86(17) 5_866 5_766 ?
O15 Nd2 O11 74.85(17) 5_766 5_766 ?
O14 Nd2 O11 74.92(17) 5_866 5_766 ?
C19 N2 C18 116.4(7) . . ?
C1 O1 Nd1 92.5(5) . . ?
C1 O2 Nd1 92.8(5) . . ?
C3 O3 Nd1 136.9(5) . . ?
C5 O5 Nd1 156.3(5) . . ?
C5 O6 Nd1 117.3(5) . 6_656 ?
C7 O7 Nd1 152.2(6) . . ?
C7 O8 Nd1 140.7(5) . 6_656 ?
C9 O9 Nd2 140.3(5) . . ?
C9 O10 Nd2 133.0(5) . 5_866 ?
C11 O12 Nd2 172.4(6) . . ?
C13 O13 Nd2 173.4(5) . . ?
C13 O14 Nd2 110.3(4) . 5_866 ?
C15 O16 Nd2 143.3(5) . . ?
O1 C1 O2 124.1(7) . . ?
O1 C1 C2 117.4(7) . . ?
O2 C1 C2 118.3(7) . . ?
O1 C1 Nd1 62.3(4) . . ?
O2 C1 Nd1 61.8(4) . . ?
C2 C1 Nd1 175.2(6) . . ?
F2 C2 F3 106.8(7) . . ?
F2 C2 F1 107.6(7) . . ?
F3 C2 F1 107.1(7) . . ?
F2 C2 C1 111.9(7) . . ?
F3 C2 C1 112.2(7) . . ?
F1 C2 C1 110.9(7) . . ?
O4 C3 O3 130.3(8) . . ?
O4 C3 C4 114.4(7) . . ?
O3 C3 C4 115.3(7) . . ?
F6 C4 F5 106.3(8) . . ?
F6 C4 F4 107.8(8) . . ?
F5 C4 F4 108.3(8) . . ?
F6 C4 C3 113.8(7) . . ?
F5 C4 C3 110.0(7) . . ?
F4 C4 C3 110.5(7) . . ?
O6 C5 O5 127.5(7) . . ?
O6 C5 C6 114.4(7) . . ?
O5 C5 C6 118.0(7) . . ?
F9 C6 F8 109.2(9) . . ?
F9 C6 F7 105.8(8) . . ?
F8 C6 F7 107.0(7) . . ?
F9 C6 C5 111.3(7) . . ?
F8 C6 C5 110.4(8) . . ?
F7 C6 C5 112.9(7) . . ?
O8 C7 O7 129.7(8) . . ?
O8 C7 C8 115.7(7) . . ?
O7 C7 C8 114.5(8) . . ?
F11 C8 F10 107.6(8) . . ?
F11 C8 F12 107.1(7) . . ?
F10 C8 F12 108.3(9) . . ?
F11 C8 C7 112.6(8) . . ?
F10 C8 C7 112.1(7) . . ?
F12 C8 C7 108.8(8) . . ?
O9 C9 O10 130.5(7) . . ?
O9 C9 C10 116.4(7) . . ?
O10 C9 C10 113.1(7) . . ?
F15 C10 F14 109.3(7) . . ?
F15 C10 F13 108.1(6) . . ?
F14 C10 F13 107.2(7) . . ?
F15 C10 C9 112.9(7) . . ?
F14 C10 C9 109.7(6) . . ?
F13 C10 C9 109.4(6) . . ?
O12 C11 O11 126.6(7) . . ?
O12 C11 C12 116.9(7) . . ?
O11 C11 C12 116.4(7) . . ?
F17 C12 F16 108.7(7) . . ?
F17 C12 F18 104.7(8) . . ?
F16 C12 F18 105.1(7) . . ?
F17 C12 C11 113.1(7) . . ?
F16 C12 C11 114.1(7) . . ?
F18 C12 C11 110.4(7) . . ?
O14 C13 O13 126.5(7) . . ?
O14 C13 C14 116.1(7) . . ?
O13 C13 C14 117.4(7) . . ?
F21 C14 F20 107.4(7) . . ?
F21 C14 F19 107.1(7) . . ?
F20 C14 F19 106.4(6) . . ?
F21 C14 C13 114.3(6) . . ?
F20 C14 C13 109.9(7) . . ?
F19 C14 C13 111.4(7) . . ?
O16 C15 O15 130.5(7) . . ?
O16 C15 C16 114.8(7) . . ?
O15 C15 C16 114.7(7) . . ?
F24 C16 F22 107.1(7) . . ?
F24 C16 F23 106.8(7) . . ?
F22 C16 F23 107.0(7) . . ?
F24 C16 C15 113.0(7) . . ?
F22 C16 C15 109.6(7) . . ?
F23 C16 C15 112.9(7) . . ?
N1 C17 C18 108.9(7) . . ?
N2 C18 C17 109.2(7) . . ?
N2 C19 C20 111.6(7) . . ?
N3 C20 C19 112.6(7) . . ?
C15 O15 Nd2 131.0(5) . 5_766 ?
C11 O11 Nd2 108.2(4) . 5_766 ?
C3 O4 Nd1 140.9(5) . 6_556 ?

_refine_diff_density_max         1.220
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.195



####################################################################### 
# 
# 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_Latfa4detaH
_database_code_depnum_ccdc_archive 'CCDC 2347614'
loop_
_audit_author_name
_audit_author_address
'Dmitry Tsymbarenko'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2024-10-05 deposited with the CCDC.	2024-10-10 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         
'2(C16 F24 La2 O16), 2(C4 H15 N3), 5(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C50 H49 F48 La4 N11 O34'
_chemical_formula_weight         2815.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   8.783(3)
_cell_length_b                   23.995(8)
_cell_length_c                   21.910(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.324(12)
_cell_angle_gamma                90
_cell_volume                     4616(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2429
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      23.30

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_F_000             2716
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.993
_shelx_estimated_absorpt_T_min   0.703
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6035
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39845
_diffrn_reflns_av_unetI/netI     0.2257
_diffrn_reflns_av_R_equivalents  0.1671
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.697
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_point_group_measured_fraction_full 0.806
_reflns_number_total             16111
_reflns_number_gt                8668
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.567
_reflns_Friedel_fraction_max     0.593
_reflns_Friedel_fraction_full    0.604

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX4 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL XT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXTL-2013/1 (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL-2013/1 (Sheldrick, 2013)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         16111
_refine_ls_number_parameters     1330
_refine_ls_number_restraints     233
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.1839
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.002
_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 0.16210(14) 0.46633(7) 0.51977(6) 0.0202(3) Uani 1 1 d . . . . .
La2 La 0.66053(14) 0.46504(7) 0.46719(6) 0.0205(3) Uani 1 1 d . . . . .
La3 La 0.74760(14) 0.34069(7) 0.01802(6) 0.0190(3) Uani 1 1 d . . . . .
La4 La 0.25514(14) 0.33772(7) -0.03351(6) 0.0203(3) Uani 1 1 d . . . . .
O1 O 0.3032(19) 0.5168(7) 0.6092(8) 0.025(4) Uani 1 1 d . . . . .
O1W O -0.323(2) 0.4315(8) 0.1863(8) 0.046(5) Uani 1 1 d . . . . .
H1WA H -0.376514 0.431090 0.152144 0.069 Uiso 1 1 d R U . . .
H1WB H -0.238304 0.417690 0.173204 0.069 Uiso 1 1 d DR U . . .
O2 O 0.4924(19) 0.4947(8) 0.5493(7) 0.029(4) Uani 1 1 d . U . . .
O2W O 0.313(2) 0.8542(10) 0.7142(11) 0.088(10) Uani 1 1 d . . . . .
H2WA H 0.311442 0.873583 0.747482 0.132 Uiso 1 1 d DR U . . .
H2WB H 0.364142 0.875053 0.690562 0.132 Uiso 1 1 d R U . . .
O3 O 0.2678(18) 0.5541(8) 0.4753(8) 0.025(4) Uani 1 1 d . . . . .
O4 O 0.491(2) 0.5434(8) 0.4268(8) 0.029(4) Uani 1 1 d . U . . .
O5 O 0.3153(19) 0.4351(7) 0.4322(7) 0.026(4) Uani 1 1 d . . . . .
O6 O 0.5203(19) 0.4213(9) 0.3746(9) 0.035(5) Uani 1 1 d . . . . .
O7 O 0.322(2) 0.3879(7) 0.5612(8) 0.029(5) Uani 1 1 d . . . . .
O8 O 0.5441(17) 0.3793(7) 0.5108(8) 0.023(4) Uani 1 1 d . . . . .
O9 O 0.0365(19) 0.3779(8) 0.4809(9) 0.026(4) Uani 1 1 d . . . . .
O10 O -0.1819(18) 0.3851(7) 0.4275(8) 0.025(4) Uani 1 1 d . U . . .
O11 O -0.0017(19) 0.5479(8) 0.5559(8) 0.027(4) Uani 1 1 d . U . . .
O12 O -0.2216(18) 0.5569(8) 0.5028(8) 0.026(4) Uani 1 1 d . . . . .
O13 O -0.0195(18) 0.4924(7) 0.4333(8) 0.023(4) Uani 1 1 d . . . . .
O14 O -0.216(2) 0.5043(7) 0.3689(8) 0.025(4) Uani 1 1 d . . . . .
O15 O 0.8255(19) 0.4413(7) 0.5556(8) 0.030(4) Uani 1 1 d . . . . .
O16 O 1.0303(19) 0.4324(8) 0.6158(8) 0.024(4) Uani 1 1 d . . . . .
O17 O 0.633(2) 0.3049(8) 0.1200(9) 0.028(5) Uani 1 1 d . . . . .
O18 O 0.4402(19) 0.3173(7) 0.0542(7) 0.025(4) Uani 1 1 d . . . . .
O19 O 0.6412(19) 0.2501(8) -0.0121(8) 0.025(4) Uani 1 1 d . . . . .
O20 O 0.4132(18) 0.2564(8) -0.0645(8) 0.025(4) Uani 1 1 d . . . . .
O21 O 0.583(2) 0.3638(7) -0.0714(8) 0.025(4) Uani 1 1 d . . . . .
O22 O 0.3836(19) 0.3647(8) -0.1319(8) 0.028(4) Uani 1 1 d . . . . .
O23 O 0.5982(19) 0.4239(8) 0.0532(8) 0.025(4) Uani 1 1 d . . . . .
O24 O 0.3768(19) 0.4273(8) -0.0015(8) 0.029(4) Uani 1 1 d . . . . .
O25 O 0.8691(19) 0.4242(7) -0.0293(8) 0.025(4) Uani 1 1 d . . . . .
O26 O 1.0865(19) 0.4120(8) -0.0780(8) 0.026(4) Uani 1 1 d . . . . .
O27 O 0.9243(19) 0.2667(7) 0.0594(8) 0.022(4) Uani 1 1 d . . . . .
O28 O 1.1406(19) 0.2543(8) 0.0126(9) 0.028(5) Uani 1 1 d . . . . .
O29 O 0.9123(19) 0.3071(7) -0.0659(8) 0.025(4) Uani 1 1 d . . . . .
O30 O 1.1088(18) 0.2859(8) -0.1226(8) 0.028(5) Uani 1 1 d . . . . .
O31 O 0.109(2) 0.3742(8) 0.0515(8) 0.032(5) Uani 1 1 d . . . . .
O32 O -0.1034(19) 0.3884(7) 0.1050(8) 0.025(4) Uani 1 1 d . . . . .
N1 N -0.256(2) 0.7087(8) 0.2009(9) 0.019(4) Uani 1 1 d . U . . .
H1A H -0.213147 0.730996 0.172395 0.029 Uiso 1 1 calc R U . . .
H1B H -0.195623 0.708119 0.235191 0.029 Uiso 1 1 calc R U . . .
H1C H -0.265904 0.673540 0.185831 0.029 Uiso 1 1 calc R U . . .
N2 N -0.488(2) 0.6358(10) 0.2376(11) 0.042(6) Uani 1 1 d . . . . .
H2 H -0.553517 0.635168 0.205430 0.050 Uiso 1 1 d R U . . .
N3 N -0.356(2) 0.5276(9) 0.2522(10) 0.035(6) Uani 1 1 d . . . . .
H3A H -0.346656 0.491961 0.238591 0.052 Uiso 1 1 calc R U . . .
H3B H -0.320463 0.551585 0.223794 0.052 Uiso 1 1 calc R U . . .
H3C H -0.301759 0.531741 0.287776 0.052 Uiso 1 1 calc R U . . .
N4 N 0.214(3) 0.7548(9) 0.7671(10) 0.040(6) Uani 1 1 d . . . . .
H4A H 0.258475 0.788410 0.759692 0.061 Uiso 1 1 calc DR U . . .
H4B H 0.267029 0.737071 0.797548 0.061 Uiso 1 1 calc R U . . .
H4C H 0.215346 0.733712 0.732591 0.061 Uiso 1 1 calc DR U . . .
N5 N -0.018(4) 0.6812(15) 0.7358(17) 0.106(13) Uani 1 1 d D U . . .
H5 H -0.069944 0.708661 0.716777 0.127 Uiso 1 1 d DR U . . .
N6 N 0.128(3) 0.5856(13) 0.6842(11) 0.063(8) Uani 1 1 d . . . . .
H6A H 0.185403 0.554364 0.690527 0.094 Uiso 1 1 calc R U . . .
H6B H 0.099438 0.587668 0.644093 0.094 Uiso 1 1 calc R U . . .
H6C H 0.184318 0.616184 0.694555 0.094 Uiso 1 1 calc DR U . . .
N7 N -0.104(3) 0.7306(11) 0.3145(12) 0.055(7) Uani 1 1 d . . . . .
N8 N -0.168(2) 0.5911(11) 0.1620(11) 0.040(5) Uani 1 1 d . . . . .
N9 N 0.317(3) 0.6886(11) 0.6536(13) 0.054(8) Uani 1 1 d . . . . .
N10 N 0.334(3) 0.6427(13) 0.8063(13) 0.065(8) Uani 1 1 d . . . . .
N11 N 0.236(3) 0.4883(12) 0.7538(12) 0.049(7) Uani 1 1 d . . . . .
C1 C 0.437(3) 0.5167(10) 0.5941(12) 0.020(6) Uani 1 1 d . U . . .
C2 C 0.543(3) 0.5534(12) 0.6337(13) 0.030(6) Uani 1 1 d . U . . .
C3 C 0.382(3) 0.5691(11) 0.4493(11) 0.024(6) Uani 1 1 d . U . . .
C4 C 0.397(4) 0.6333(12) 0.4431(13) 0.035(7) Uani 1 1 d . . . . .
C5 C 0.379(3) 0.4204(10) 0.3860(12) 0.023(6) Uani 1 1 d . . . . .
C6 C 0.279(3) 0.3955(11) 0.3322(13) 0.033(7) Uani 1 1 d . . . . .
C7 C 0.447(2) 0.3661(9) 0.5477(10) 0.011(5) Uani 1 1 d . U . . .
C8 C 0.469(3) 0.3075(11) 0.5793(13) 0.027(6) Uani 1 1 d . U . . .
C9 C -0.060(2) 0.3641(10) 0.4451(11) 0.017(5) Uani 1 1 d . U . . .
C10 C -0.037(4) 0.3031(14) 0.4219(15) 0.046(8) Uani 1 1 d . . . . .
C11 C -0.107(3) 0.5748(9) 0.5295(11) 0.021(6) Uani 1 1 d . U . . .
C12 C -0.0911(16) 0.6372(6) 0.5295(7) 0.038(7) Uani 1 1 d D . . . .
C13 C -0.078(3) 0.5077(12) 0.3837(12) 0.026(7) Uani 1 1 d . . . . .
C14 C 0.023(3) 0.5346(14) 0.3369(15) 0.044(8) Uani 1 1 d . . . . .
C15 C 0.890(3) 0.4305(11) 0.6040(13) 0.029(6) Uani 1 1 d . U . . .
C16 C 0.789(3) 0.4095(11) 0.6562(14) 0.028(7) Uani 1 1 d . . . . .
C17 C 0.496(2) 0.2997(11) 0.1031(11) 0.019(5) Uani 1 1 d . U . . .
C18 C 0.386(3) 0.2723(13) 0.1467(14) 0.034(7) Uani 1 1 d . U . . .
C19 C 0.524(2) 0.2352(5) -0.0397(10) 0.030(7) Uani 1 1 d D . . . .
C20 C 0.5159(15) 0.1675(5) -0.0447(6) 0.042(8) Uani 1 1 d D U . . .
C21 C 0.515(3) 0.3704(11) -0.1226(11) 0.019(6) Uani 1 1 d . . . . .
C22 C 0.622(3) 0.3879(12) -0.1743(13) 0.033(7) Uani 1 1 d . . . . .
C23 C 0.481(3) 0.4451(10) 0.0327(12) 0.024(6) Uani 1 1 d . U . . .
C24 C 0.447(3) 0.5055(11) 0.0540(14) 0.027(6) Uani 1 1 d . . . . .
C25 C 0.974(3) 0.4356(12) -0.0657(11) 0.026(6) Uani 1 1 d . U . . .
C26 C 0.947(3) 0.4916(11) -0.0977(12) 0.028(6) Uani 1 1 d . U . . .
C27 C 1.027(3) 0.2398(12) 0.0384(12) 0.027(6) Uani 1 1 d . U . . .
C28 C 1.003(3) 0.1762(13) 0.0421(16) 0.042(8) Uani 1 1 d . . . . .
C29 C 0.975(3) 0.2859(12) -0.1095(12) 0.022(6) Uani 1 1 d . U . . .
C30 C 0.871(3) 0.2561(15) -0.1565(13) 0.037(8) Uani 1 1 d . . . . .
C31 C 0.032(3) 0.3892(10) 0.0994(11) 0.018(5) Uani 1 1 d . U . . .
C32 C 0.128(3) 0.4176(13) 0.1497(12) 0.029(7) Uani 1 1 d . U . . .
C33 C -0.409(3) 0.7309(13) 0.2161(13) 0.037(7) Uani 1 1 d . . . . .
H33A H -0.475243 0.731960 0.178880 0.044 Uiso 1 1 calc R U . . .
H33B H -0.399331 0.769310 0.232195 0.044 Uiso 1 1 calc R U . . .
C34 C -0.479(3) 0.6935(10) 0.2635(12) 0.032(6) Uani 1 1 d . U . . .
H34A H -0.415277 0.693588 0.301366 0.039 Uiso 1 1 calc R U . . .
H34B H -0.581978 0.706906 0.273383 0.039 Uiso 1 1 calc R U . . .
C35 C -0.542(3) 0.5964(12) 0.2849(12) 0.042(7) Uani 1 1 d . . . . .
H35A H -0.484182 0.602278 0.323753 0.051 Uiso 1 1 calc R U . . .
H35B H -0.651216 0.602691 0.292342 0.051 Uiso 1 1 calc R U . . .
C36 C -0.518(3) 0.5396(12) 0.2629(12) 0.035(7) Uani 1 1 d . . . . .
H36A H -0.577094 0.534281 0.224271 0.042 Uiso 1 1 calc R U . . .
H36B H -0.556950 0.512909 0.293176 0.042 Uiso 1 1 calc R U . . .
C37 C 0.054(3) 0.7636(13) 0.7857(13) 0.042(7) Uani 1 1 d . U . . .
H37A H -0.005193 0.782795 0.752921 0.050 Uiso 1 1 calc R U . . .
H37B H 0.050766 0.786432 0.823252 0.050 Uiso 1 1 calc R U . . .
C38 C -0.010(5) 0.7065(17) 0.7969(17) 0.096(14) Uani 1 1 d D U . . .
H38A H 0.057938 0.684774 0.824674 0.115 Uiso 1 1 calc R U . . .
H38B H -0.112208 0.708807 0.814726 0.115 Uiso 1 1 calc R U . . .
C39 C -0.110(4) 0.6336(15) 0.714(2) 0.108(15) Uani 1 1 d D U . . .
H39A H -0.140346 0.638395 0.670842 0.130 Uiso 1 1 calc R U . . .
H39B H -0.203201 0.629947 0.738631 0.130 Uiso 1 1 calc R U . . .
C40 C -0.010(3) 0.5831(16) 0.7226(19) 0.078(13) Uani 1 1 d . U . . .
H40A H 0.022112 0.580001 0.766039 0.094 Uiso 1 1 calc R U . . .
H40B H -0.069301 0.549290 0.711694 0.094 Uiso 1 1 calc R U . . .
C41 C -0.070(3) 0.7496(12) 0.3594(14) 0.041(7) Uani 1 1 d . U . . .
C42 C -0.018(3) 0.7740(12) 0.4180(11) 0.037(7) Uani 1 1 d . U . . .
H42A H 0.093989 0.773219 0.420539 0.056 Uiso 1 1 calc R U . . .
H42B H -0.058734 0.752334 0.451771 0.056 Uiso 1 1 calc DR U . . .
H42C H -0.053031 0.812613 0.420650 0.056 Uiso 1 1 calc DR U . . .
C43 C -0.138(3) 0.5682(12) 0.1151(13) 0.038(7) Uani 1 1 d . . . . .
C44 C -0.110(3) 0.5393(13) 0.0599(13) 0.040(8) Uani 1 1 d . . . . .
H44A H -0.010950 0.520926 0.062888 0.060 Uiso 1 1 calc R U . . .
H44B H -0.111074 0.565845 0.025837 0.060 Uiso 1 1 calc R U . . .
H44C H -0.190039 0.511282 0.052726 0.060 Uiso 1 1 calc R U . . .
C45 C 0.397(5) 0.7156(13) 0.6302(17) 0.064(12) Uani 1 1 d . . . . .
C46 C 0.492(3) 0.7515(13) 0.5869(15) 0.050(9) Uani 1 1 d . . . . .
H46A H 0.574451 0.728959 0.570585 0.075 Uiso 1 1 calc R U . . .
H46B H 0.534591 0.783329 0.609388 0.075 Uiso 1 1 calc R U . . .
H46C H 0.426358 0.764968 0.553166 0.075 Uiso 1 1 calc R U . . .
C47 C 0.372(4) 0.6067(15) 0.8321(15) 0.056(10) Uani 1 1 d . . . . .
C48 C 0.418(5) 0.5596(17) 0.8692(18) 0.087(14) Uani 1 1 d . . . . .
H48A H 0.338073 0.551188 0.898440 0.131 Uiso 1 1 calc R U . . .
H48B H 0.512753 0.568522 0.891457 0.131 Uiso 1 1 calc R U . . .
H48C H 0.433719 0.527127 0.843012 0.131 Uiso 1 1 calc R U . . .
C49 C 0.224(4) 0.4426(14) 0.7489(17) 0.048(9) Uani 1 1 d . . . . .
C50 C 0.185(4) 0.3853(13) 0.7437(17) 0.072(12) Uani 1 1 d . . . . .
H50A H 0.082729 0.379492 0.759488 0.109 Uiso 1 1 calc R U . . .
H50B H 0.258565 0.362906 0.767390 0.109 Uiso 1 1 calc R U . . .
H50C H 0.186668 0.374124 0.700741 0.109 Uiso 1 1 calc R U . . .
F1 F 0.6847(17) 0.5348(7) 0.6389(8) 0.036(4) Uani 1 1 d . . . . .
F2 F 0.4955(19) 0.5647(9) 0.6891(8) 0.069(6) Uani 1 1 d . U . . .
F3 F 0.562(2) 0.6038(7) 0.6068(10) 0.068(6) Uani 1 1 d . . . . .
F4 F 0.526(2) 0.6512(7) 0.4241(9) 0.050(5) Uani 1 1 d . . . . .
F5 F 0.285(2) 0.6525(7) 0.4046(8) 0.050(5) Uani 1 1 d . . . . .
F6 F 0.361(2) 0.6585(8) 0.4972(8) 0.068(6) Uani 1 1 d . . . . .
F7 F 0.1327(18) 0.4036(8) 0.3406(8) 0.042(5) Uani 1 1 d . . . . .
F8 F 0.3042(17) 0.3406(9) 0.3303(7) 0.050(4) Uani 1 1 d . . . . .
F9 F 0.3193(18) 0.4165(8) 0.2808(7) 0.051(5) Uani 1 1 d . . . . .
F10 F 0.4294(19) 0.3101(6) 0.6378(8) 0.045(4) Uani 1 1 d . . . . .
F11 F 0.3743(18) 0.2692(7) 0.5533(9) 0.050(5) Uani 1 1 d . . . . .
F12 F 0.6069(19) 0.2893(8) 0.5764(9) 0.056(6) Uani 1 1 d . . . . .
F13 F 0.1066(19) 0.2853(7) 0.4261(9) 0.053(5) Uani 1 1 d . . . . .
F14 F -0.130(2) 0.2675(7) 0.4501(8) 0.047(5) Uani 1 1 d . . . . .
F15 F -0.075(2) 0.2986(7) 0.3617(8) 0.056(5) Uani 1 1 d . . . . .
F16 F -0.2221(14) 0.6650(7) 0.5282(9) 0.089(9) Uani 1 1 d D . . . .
F17 F -0.009(2) 0.6550(8) 0.5775(8) 0.103(9) Uani 1 1 d D U . . .
F18 F -0.0165(19) 0.6513(7) 0.4796(8) 0.083(7) Uani 1 1 d D . . . .
F19 F 0.1720(17) 0.5264(7) 0.3469(8) 0.035(4) Uani 1 1 d . . . . .
F20 F -0.0075(19) 0.5181(10) 0.2804(8) 0.068(7) Uani 1 1 d . . . . .
F21 F 0.0078(19) 0.5898(8) 0.3359(9) 0.066(6) Uani 1 1 d . . . . .
F22 F 0.8251(17) 0.4389(6) 0.7078(6) 0.035(4) Uani 1 1 d . . . . .
F23 F 0.8271(17) 0.3560(6) 0.6703(7) 0.036(4) Uani 1 1 d . . . . .
F24 F 0.6433(17) 0.4134(8) 0.6466(8) 0.039(4) Uani 1 1 d . . . . .
F25 F 0.2467(17) 0.2927(7) 0.1452(8) 0.039(4) Uani 1 1 d . . . . .
F26 F 0.434(2) 0.2721(10) 0.2042(8) 0.073(7) Uani 1 1 d . . . . .
F27 F 0.373(2) 0.2179(7) 0.1274(9) 0.057(5) Uani 1 1 d . U . . .
F28 F 0.3847(19) 0.1508(7) -0.0702(10) 0.115(9) Uani 1 1 d D U . . .
F29 F 0.628(2) 0.1478(8) -0.0784(11) 0.143(12) Uani 1 1 d D U . . .
F30 F 0.528(3) 0.1440(7) 0.0101(7) 0.121(9) Uani 1 1 d D U . . .
F31 F 0.7678(17) 0.3841(8) -0.1629(8) 0.041(5) Uani 1 1 d . . . . .
F32 F 0.5915(17) 0.4434(7) -0.1869(8) 0.049(5) Uani 1 1 d . . . . .
F33 F 0.5815(17) 0.3623(7) -0.2247(7) 0.040(4) Uani 1 1 d . . . . .
F34 F 0.503(2) 0.5174(7) 0.1092(9) 0.058(6) Uani 1 1 d . . . . .
F35 F 0.539(2) 0.5384(7) 0.0213(9) 0.059(6) Uani 1 1 d . . . . .
F36 F 0.312(2) 0.5235(8) 0.0469(10) 0.068(6) Uani 1 1 d . . . . .
F37 F 0.8105(17) 0.5146(7) -0.0906(7) 0.041(4) Uani 1 1 d . . . . .
F38 F 1.046(2) 0.5308(7) -0.0791(9) 0.053(6) Uani 1 1 d . . . . .
F39 F 0.962(2) 0.4878(7) -0.1593(8) 0.049(5) Uani 1 1 d . . . . .
F40 F 1.126(2) 0.1487(8) 0.0606(12) 0.078(8) Uani 1 1 d . . . . .
F41 F 0.887(2) 0.1613(8) 0.0724(12) 0.083(8) Uani 1 1 d . . . . .
F42 F 0.973(3) 0.1566(8) -0.0139(11) 0.082(8) Uani 1 1 d . . . . .
F43 F 0.7252(17) 0.2596(7) -0.1461(8) 0.040(4) Uani 1 1 d . . . . .
F44 F 0.8953(17) 0.2754(8) -0.2126(6) 0.045(4) Uani 1 1 d . U . . .
F45 F 0.910(2) 0.2024(8) -0.1588(9) 0.055(5) Uani 1 1 d . . . . .
F46 F 0.0913(17) 0.3921(9) 0.2035(7) 0.057(6) Uani 1 1 d . . . . .
F47 F 0.093(2) 0.4705(9) 0.1558(9) 0.066(6) Uani 1 1 d . . . . .
F48 F 0.2776(16) 0.4130(7) 0.1466(7) 0.036(4) 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
La1 O5 2.485(16) . ?
La1 O7 2.505(19) . ?
La1 O3 2.508(18) . ?
La1 O13 2.527(16) . ?
La1 O9 2.530(19) . ?
La1 O16 2.559(16) 1_455 ?
La1 O11 2.565(18) . ?
La1 O1 2.594(17) . ?
La2 O2 2.459(16) . ?
La2 O15 2.459(17) . ?
La2 O8 2.498(16) . ?
La2 O10 2.531(16) 1_655 ?
La2 O4 2.545(17) . ?
La2 O12 2.550(17) 1_655 ?
La2 O6 2.572(18) . ?
La2 O14 2.609(17) 1_655 ?
La2 O13 2.996(17) 1_655 ?
La2 C13 3.14(3) 1_655 ?
La3 O19 2.451(18) . ?
La3 O21 2.472(17) . ?
La3 O29 2.500(17) . ?
La3 O25 2.507(17) . ?
La3 O27 2.514(17) . ?
La3 O23 2.520(18) . ?
La3 O32 2.558(17) 1_655 ?
La3 O17 2.616(19) . ?
La3 O18 2.887(17) . ?
La3 C17 3.09(2) . ?
La4 O31 2.446(19) . ?
La4 O28 2.467(17) 1_455 ?
La4 O24 2.493(18) . ?
La4 O20 2.498(16) . ?
La4 O26 2.501(18) 1_455 ?
La4 O18 2.536(16) . ?
La4 O22 2.540(17) . ?
La4 O30 2.626(18) 1_455 ?
La4 C21 3.13(2) . ?
O1 C1 1.23(3) . ?
O2 C1 1.22(3) . ?
O3 C3 1.22(3) . ?
O4 C3 1.25(3) . ?
O5 C5 1.22(3) . ?
O6 C5 1.27(3) . ?
O7 C7 1.26(3) . ?
O8 C7 1.23(2) . ?
O9 C9 1.19(3) . ?
O10 C9 1.24(3) . ?
O11 C11 1.26(3) . ?
O12 C11 1.23(3) . ?
O13 C13 1.25(3) . ?
O14 C13 1.25(3) . ?
O15 C15 1.22(3) . ?
O16 C15 1.26(3) . ?
O17 C17 1.26(3) . ?
O18 C17 1.24(3) . ?
O19 C19 1.24(3) . ?
O20 C19 1.21(3) . ?
O21 C21 1.27(3) . ?
O22 C21 1.17(3) . ?
O23 C23 1.22(3) . ?
O24 C23 1.25(3) . ?
O25 C25 1.27(3) . ?
O26 C25 1.17(3) . ?
O27 C27 1.21(3) . ?
O28 C27 1.21(3) . ?
O29 C29 1.22(3) . ?
O30 C29 1.22(3) . ?
O31 C31 1.31(3) . ?
O32 C31 1.20(3) . ?
N1 C33 1.49(3) . ?
N2 C35 1.49(3) . ?
N2 C34 1.50(3) . ?
N3 C36 1.47(3) . ?
N4 C37 1.49(3) . ?
N5 C38 1.469(7) . ?
N5 C39 1.471(7) . ?
N6 C40 1.49(4) . ?
N7 C41 1.12(4) . ?
N8 C43 1.20(3) . ?
N9 C45 1.09(4) . ?
N10 C47 1.08(4) . ?
N11 C49 1.11(3) . ?
C1 C2 1.54(3) . ?
C2 F2 1.32(3) . ?
C2 F1 1.33(3) . ?
C2 F3 1.36(3) . ?
C3 C4 1.55(4) . ?
C4 F4 1.29(3) . ?
C4 F5 1.36(3) . ?
C4 F6 1.37(3) . ?
C5 C6 1.58(4) . ?
C6 F9 1.29(3) . ?
C6 F7 1.31(3) . ?
C6 F8 1.34(3) . ?
C7 C8 1.58(3) . ?
C8 F12 1.29(3) . ?
C8 F10 1.34(3) . ?
C8 F11 1.36(3) . ?
C9 C10 1.56(4) . ?
C10 F13 1.33(3) . ?
C10 F14 1.35(3) . ?
C10 F15 1.36(3) . ?
C11 C12 1.50(3) . ?
C12 F17 1.329(7) . ?
C12 F16 1.330(7) . ?
C12 F18 1.332(7) . ?
C13 C14 1.52(4) . ?
C14 F20 1.32(4) . ?
C14 F21 1.33(4) . ?
C14 F19 1.34(3) . ?
C15 C16 1.55(4) . ?
C16 F24 1.29(3) . ?
C16 F23 1.36(3) . ?
C16 F22 1.37(3) . ?
C17 C18 1.52(3) . ?
C18 F25 1.31(3) . ?
C18 F26 1.32(3) . ?
C18 F27 1.38(4) . ?
C19 C20 1.629(8) . ?
C20 F29 1.330(4) . ?
C20 F30 1.330(4) . ?
C20 F28 1.331(4) . ?
C21 C22 1.55(3) . ?
C22 F33 1.30(3) . ?
C22 F31 1.31(3) . ?
C22 F32 1.38(3) . ?
C23 C24 1.55(4) . ?
C24 F36 1.27(3) . ?
C24 F34 1.33(3) . ?
C24 F35 1.35(3) . ?
C25 C26 1.53(4) . ?
C26 F37 1.33(3) . ?
C26 F38 1.34(3) . ?
C26 F39 1.36(3) . ?
C27 C28 1.54(4) . ?
C28 F41 1.28(3) . ?
C28 F40 1.32(4) . ?
C28 F42 1.34(4) . ?
C29 C30 1.54(4) . ?
C30 F43 1.31(3) . ?
C30 F45 1.33(3) . ?
C30 F44 1.34(3) . ?
C31 C32 1.53(3) . ?
C32 F47 1.31(4) . ?
C32 F48 1.32(3) . ?
C32 F46 1.37(3) . ?
C33 C34 1.51(4) . ?
C35 C36 1.46(4) . ?
C37 C38 1.50(5) . ?
C39 C40 1.51(5) . ?
C41 C42 1.48(4) . ?
C43 C44 1.42(4) . ?
C45 C46 1.54(5) . ?
C47 C48 1.45(5) . ?
C49 C50 1.42(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
O5 La1 O7 75.2(6) . . ?
O5 La1 O3 75.0(5) . . ?
O7 La1 O3 124.2(5) . . ?
O5 La1 O13 80.7(5) . . ?
O7 La1 O13 142.7(5) . . ?
O3 La1 O13 74.6(6) . . ?
O5 La1 O9 74.1(6) . . ?
O7 La1 O9 74.2(6) . . ?
O3 La1 O9 137.4(6) . . ?
O13 La1 O9 72.1(5) . . ?
O5 La1 O16 143.4(6) . 1_455 ?
O7 La1 O16 73.9(6) . 1_455 ?
O3 La1 O16 140.0(6) . 1_455 ?
O13 La1 O16 113.9(5) . 1_455 ?
O9 La1 O16 78.9(6) . 1_455 ?
O5 La1 O11 141.8(6) . . ?
O7 La1 O11 140.8(6) . . ?
O3 La1 O11 72.2(5) . . ?
O13 La1 O11 72.2(5) . . ?
O9 La1 O11 120.0(5) . . ?
O16 La1 O11 73.8(6) 1_455 . ?
O5 La1 O1 117.8(6) . . ?
O7 La1 O1 79.8(6) . . ?
O3 La1 O1 74.1(6) . . ?
O13 La1 O1 137.2(5) . . ?
O9 La1 O1 147.4(6) . . ?
O16 La1 O1 75.2(6) 1_455 . ?
O11 La1 O1 70.9(5) . . ?
O2 La2 O15 81.0(6) . . ?
O2 La2 O8 72.6(6) . . ?
O15 La2 O8 75.4(6) . . ?
O2 La2 O10 144.4(6) . 1_655 ?
O15 La2 O10 77.2(6) . 1_655 ?
O8 La2 O10 74.9(5) . 1_655 ?
O2 La2 O4 71.6(6) . . ?
O15 La2 O4 140.7(6) . . ?
O8 La2 O4 120.0(6) . . ?
O10 La2 O4 139.5(6) 1_655 . ?
O2 La2 O12 76.8(6) . 1_655 ?
O15 La2 O12 74.4(6) . 1_655 ?
O8 La2 O12 139.6(6) . 1_655 ?
O10 La2 O12 122.6(5) 1_655 1_655 ?
O4 La2 O12 72.4(6) . 1_655 ?
O2 La2 O6 114.2(6) . . ?
O15 La2 O6 142.2(6) . . ?
O8 La2 O6 76.9(6) . . ?
O10 La2 O6 71.1(6) 1_655 . ?
O4 La2 O6 76.2(6) . . ?
O12 La2 O6 141.0(6) 1_655 . ?
O2 La2 O14 140.1(6) . 1_655 ?
O15 La2 O14 119.0(6) . 1_655 ?
O8 La2 O14 142.6(5) . 1_655 ?
O10 La2 O14 75.5(5) 1_655 1_655 ?
O4 La2 O14 72.4(6) . 1_655 ?
O12 La2 O14 76.5(5) 1_655 1_655 ?
O6 La2 O14 72.4(6) . 1_655 ?
O2 La2 O13 134.5(5) . 1_655 ?
O15 La2 O13 73.0(5) . 1_655 ?
O8 La2 O13 132.1(5) . 1_655 ?
O10 La2 O13 63.7(5) 1_655 1_655 ?
O4 La2 O13 107.3(5) . 1_655 ?
O12 La2 O13 60.7(5) 1_655 1_655 ?
O6 La2 O13 109.2(5) . 1_655 ?
O14 La2 O13 46.1(5) 1_655 1_655 ?
O2 La2 C13 142.3(7) . 1_655 ?
O15 La2 C13 96.3(7) . 1_655 ?
O8 La2 C13 143.4(6) . 1_655 ?
O10 La2 C13 68.6(6) 1_655 1_655 ?
O4 La2 C13 89.2(7) . 1_655 ?
O12 La2 C13 66.4(6) 1_655 1_655 ?
O6 La2 C13 90.9(7) . 1_655 ?
O14 La2 C13 22.7(6) 1_655 1_655 ?
O13 La2 C13 23.3(6) 1_655 1_655 ?
O19 La3 O21 76.9(6) . . ?
O19 La3 O29 74.9(6) . . ?
O21 La3 O29 80.0(6) . . ?
O19 La3 O25 139.6(6) . . ?
O21 La3 O25 74.9(6) . . ?
O29 La3 O25 72.2(6) . . ?
O19 La3 O27 72.5(6) . . ?
O21 La3 O27 142.1(5) . . ?
O29 La3 O27 71.0(6) . . ?
O25 La3 O27 116.7(5) . . ?
O19 La3 O23 126.0(6) . . ?
O21 La3 O23 76.4(5) . . ?
O29 La3 O23 142.6(6) . . ?
O25 La3 O23 73.9(6) . . ?
O27 La3 O23 140.5(5) . . ?
O19 La3 O32 141.6(6) . 1_655 ?
O21 La3 O32 140.4(5) . 1_655 ?
O29 La3 O32 113.5(5) . 1_655 ?
O25 La3 O32 74.6(6) . 1_655 ?
O27 La3 O32 75.3(5) . 1_655 ?
O23 La3 O32 71.2(5) . 1_655 ?
O19 La3 O17 77.8(6) . . ?
O21 La3 O17 121.5(6) . . ?
O29 La3 O17 139.7(6) . . ?
O25 La3 O17 142.3(6) . . ?
O27 La3 O17 72.9(6) . . ?
O23 La3 O17 77.6(6) . . ?
O32 La3 O17 73.1(6) 1_655 . ?
O19 La3 O18 63.1(5) . . ?
O21 La3 O18 74.2(5) . . ?
O29 La3 O18 134.4(5) . . ?
O25 La3 O18 132.8(5) . . ?
O27 La3 O18 109.7(5) . . ?
O23 La3 O18 64.7(5) . . ?
O32 La3 O18 110.4(5) 1_655 . ?
O17 La3 O18 47.3(5) . . ?
O19 La3 C17 66.8(6) . . ?
O21 La3 C17 97.9(6) . . ?
O29 La3 C17 140.9(6) . . ?
O25 La3 C17 145.4(6) . . ?
O27 La3 C17 90.1(6) . . ?
O23 La3 C17 71.5(6) . . ?
O32 La3 C17 93.1(6) 1_655 . ?
O17 La3 C17 23.8(6) . . ?
O18 La3 C17 23.7(5) . . ?
O31 La4 O28 75.7(6) . 1_455 ?
O31 La4 O24 72.9(6) . . ?
O28 La4 O24 139.5(6) 1_455 . ?
O31 La4 O20 142.2(6) . . ?
O28 La4 O20 73.2(6) 1_455 . ?
O24 La4 O20 120.8(6) . . ?
O31 La4 O26 74.1(6) . 1_455 ?
O28 La4 O26 119.7(6) 1_455 1_455 ?
O24 La4 O26 75.0(6) . 1_455 ?
O20 La4 O26 141.1(6) . 1_455 ?
O31 La4 O18 80.2(6) . . ?
O28 La4 O18 78.0(6) 1_455 . ?
O24 La4 O18 72.0(6) . . ?
O20 La4 O18 72.8(5) . . ?
O26 La4 O18 142.8(6) 1_455 . ?
O31 La4 O22 143.6(6) . . ?
O28 La4 O22 138.4(6) 1_455 . ?
O24 La4 O22 79.8(6) . . ?
O20 La4 O22 73.1(6) . . ?
O26 La4 O22 76.0(6) 1_455 . ?
O18 La4 O22 113.8(6) . . ?
O31 La4 O30 118.6(6) . 1_455 ?
O28 La4 O30 73.9(6) 1_455 1_455 ?
O24 La4 O30 144.7(6) . 1_455 ?
O20 La4 O30 72.1(5) . 1_455 ?
O26 La4 O30 76.8(6) 1_455 1_455 ?
O18 La4 O30 140.0(5) . 1_455 ?
O22 La4 O30 73.1(6) . 1_455 ?
O31 La4 C21 141.8(6) . . ?
O28 La4 C21 140.1(6) 1_455 . ?
O24 La4 C21 69.3(6) . . ?
O20 La4 C21 67.0(6) . . ?
O26 La4 C21 90.7(6) 1_455 . ?
O18 La4 C21 93.3(6) . . ?
O22 La4 C21 20.6(6) . . ?
O30 La4 C21 90.4(6) 1_455 . ?
C1 O1 La1 103.8(15) . . ?
C1 O2 La2 165.3(17) . . ?
C3 O3 La1 138.2(17) . . ?
C3 O4 La2 132.5(17) . . ?
C5 O5 La1 174.4(17) . . ?
C5 O6 La2 107.6(16) . . ?
C7 O7 La1 135.4(16) . . ?
C7 O8 La2 139.5(15) . . ?
C9 O9 La1 139.0(17) . . ?
C9 O10 La2 132.7(17) . 1_455 ?
C11 O11 La1 131.4(16) . . ?
C11 O12 La2 140.4(17) . 1_455 ?
C13 O13 La1 165.4(18) . . ?
C13 O13 La2 84.7(16) . 1_455 ?
La1 O13 La2 109.8(6) . 1_455 ?
C13 O14 La2 103.2(16) . 1_455 ?
C15 O15 La2 171.3(19) . . ?
C15 O16 La1 107.6(17) . 1_655 ?
C17 O17 La3 99.5(16) . . ?
C17 O18 La4 162.3(17) . . ?
C17 O18 La3 87.2(14) . . ?
La4 O18 La3 110.0(6) . . ?
C19 O19 La3 134.1(14) . . ?
C19 O20 La4 130.5(14) . . ?
C21 O21 La3 169.9(17) . . ?
C21 O22 La4 109.6(17) . . ?
C23 O23 La3 131.0(18) . . ?
C23 O24 La4 140.3(17) . . ?
C25 O25 La3 139.2(18) . . ?
C25 O26 La4 138.4(18) . 1_655 ?
C27 O27 La3 134.4(18) . . ?
C27 O28 La4 140.7(18) . 1_655 ?
C29 O29 La3 170.6(17) . . ?
C29 O30 La4 106.4(17) . 1_655 ?
C31 O31 La4 174.8(16) . . ?
C31 O32 La3 115.0(17) . 1_455 ?
C35 N2 C34 110(2) . . ?
C38 N5 C39 129(4) . . ?
O2 C1 O1 128(2) . . ?
O2 C1 C2 117(2) . . ?
O1 C1 C2 115(2) . . ?
O2 C1 La1 74.5(14) . . ?
O1 C1 La1 53.8(12) . . ?
C2 C1 La1 165.3(18) . . ?
F2 C2 F1 108(2) . . ?
F2 C2 F3 105(2) . . ?
F1 C2 F3 102(2) . . ?
F2 C2 C1 116(2) . . ?
F1 C2 C1 114(2) . . ?
F3 C2 C1 110(2) . . ?
O3 C3 O4 133(3) . . ?
O3 C3 C4 114(3) . . ?
O4 C3 C4 113(2) . . ?
F4 C4 F5 108(2) . . ?
F4 C4 F6 111(3) . . ?
F5 C4 F6 102(2) . . ?
F4 C4 C3 116(3) . . ?
F5 C4 C3 109(2) . . ?
F6 C4 C3 110(2) . . ?
O5 C5 O6 129(2) . . ?
O5 C5 C6 118(2) . . ?
O6 C5 C6 113(2) . . ?
F9 C6 F7 111(2) . . ?
F9 C6 F8 108(2) . . ?
F7 C6 F8 108(2) . . ?
F9 C6 C5 110(2) . . ?
F7 C6 C5 112(2) . . ?
F8 C6 C5 108(2) . . ?
O8 C7 O7 132(2) . . ?
O8 C7 C8 116.2(19) . . ?
O7 C7 C8 111.4(19) . . ?
F12 C8 F10 109(2) . . ?
F12 C8 F11 109(2) . . ?
F10 C8 F11 105(2) . . ?
F12 C8 C7 113(2) . . ?
F10 C8 C7 110.3(19) . . ?
F11 C8 C7 111(2) . . ?
O9 C9 O10 134(2) . . ?
O9 C9 C10 112(2) . . ?
O10 C9 C10 113(2) . . ?
F13 C10 F14 110(3) . . ?
F13 C10 F15 105(3) . . ?
F14 C10 F15 105(2) . . ?
F13 C10 C9 114(2) . . ?
F14 C10 C9 111(2) . . ?
F15 C10 C9 111(3) . . ?
O12 C11 O11 129(2) . . ?
O12 C11 C12 115(2) . . ?
O11 C11 C12 116.1(19) . . ?
F17 C12 F16 107.8(7) . . ?
F17 C12 F18 107.5(7) . . ?
F16 C12 F18 107.2(7) . . ?
F17 C12 C11 111.8(15) . . ?
F16 C12 C11 114.6(14) . . ?
F18 C12 C11 107.5(14) . . ?
O14 C13 O13 126(2) . . ?
O14 C13 C14 116(2) . . ?
O13 C13 C14 118(3) . . ?
O14 C13 La2 54.1(13) . 1_455 ?
O13 C13 La2 71.9(15) . 1_455 ?
C14 C13 La2 168.8(19) . 1_455 ?
F20 C14 F21 105(3) . . ?
F20 C14 F19 107(2) . . ?
F21 C14 F19 104(3) . . ?
F20 C14 C13 113(3) . . ?
F21 C14 C13 112(3) . . ?
F19 C14 C13 114(2) . . ?
O15 C15 O16 127(3) . . ?
O15 C15 C16 117(2) . . ?
O16 C15 C16 116(2) . . ?
F24 C16 F23 110(2) . . ?
F24 C16 F22 108(2) . . ?
F23 C16 F22 104(2) . . ?
F24 C16 C15 116(2) . . ?
F23 C16 C15 109(2) . . ?
F22 C16 C15 108(2) . . ?
O18 C17 O17 125(2) . . ?
O18 C17 C18 116(2) . . ?
O17 C17 C18 119(2) . . ?
O18 C17 La3 69.1(13) . . ?
O17 C17 La3 56.7(12) . . ?
C18 C17 La3 172.1(18) . . ?
F25 C18 F26 108(3) . . ?
F25 C18 F27 106(2) . . ?
F26 C18 F27 108(2) . . ?
F25 C18 C17 115(2) . . ?
F26 C18 C17 114(2) . . ?
F27 C18 C17 105(2) . . ?
O20 C19 O19 138.5(16) . . ?
O20 C19 C20 110.8(14) . . ?
O19 C19 C20 110.7(14) . . ?
F29 C20 F30 107.7(4) . . ?
F29 C20 F28 107.6(4) . . ?
F30 C20 F28 107.6(4) . . ?
F29 C20 C19 111.2(5) . . ?
F30 C20 C19 111.1(5) . . ?
F28 C20 C19 111.3(5) . . ?
O22 C21 O21 126(2) . . ?
O22 C21 C22 121(2) . . ?
O21 C21 C22 113(2) . . ?
O22 C21 La4 49.8(13) . . ?
O21 C21 La4 75.8(14) . . ?
C22 C21 La4 170.7(17) . . ?
F33 C22 F31 112(2) . . ?
F33 C22 F32 104(2) . . ?
F31 C22 F32 107(2) . . ?
F33 C22 C21 110(2) . . ?
F31 C22 C21 117(2) . . ?
F32 C22 C21 107(2) . . ?
O23 C23 O24 133(3) . . ?
O23 C23 C24 116(2) . . ?
O24 C23 C24 111(2) . . ?
F36 C24 F34 111(3) . . ?
F36 C24 F35 108(2) . . ?
F34 C24 F35 98(2) . . ?
F36 C24 C23 118(3) . . ?
F34 C24 C23 114(2) . . ?
F35 C24 C23 105(2) . . ?
O26 C25 O25 132(3) . . ?
O26 C25 C26 116(2) . . ?
O25 C25 C26 112(2) . . ?
F37 C26 F38 105(2) . . ?
F37 C26 F39 105(2) . . ?
F38 C26 F39 106(2) . . ?
F37 C26 C25 116(2) . . ?
F38 C26 C25 113(2) . . ?
F39 C26 C25 112(2) . . ?
O27 C27 O28 131(3) . . ?
O27 C27 C28 114(2) . . ?
O28 C27 C28 115(2) . . ?
F41 C28 F40 111(3) . . ?
F41 C28 F42 103(3) . . ?
F40 C28 F42 105(3) . . ?
F41 C28 C27 114(2) . . ?
F40 C28 C27 114(3) . . ?
F42 C28 C27 109(3) . . ?
O30 C29 O29 130(3) . . ?
O30 C29 C30 114(2) . . ?
O29 C29 C30 117(2) . . ?
F43 C30 F45 109(3) . . ?
F43 C30 F44 108(3) . . ?
F45 C30 F44 105(2) . . ?
F43 C30 C29 115(2) . . ?
F45 C30 C29 109(2) . . ?
F44 C30 C29 111(2) . . ?
O32 C31 O31 128(2) . . ?
O32 C31 C32 118(2) . . ?
O31 C31 C32 114(2) . . ?
F47 C32 F48 109(2) . . ?
F47 C32 F46 106(2) . . ?
F48 C32 F46 105(2) . . ?
F47 C32 C31 112(2) . . ?
F48 C32 C31 117(2) . . ?
F46 C32 C31 106(2) . . ?
N1 C33 C34 109(2) . . ?
N2 C34 C33 108(2) . . ?
C36 C35 N2 108(2) . . ?
C35 C36 N3 112(2) . . ?
N4 C37 C38 106(3) . . ?
N5 C38 C37 104(3) . . ?
N5 C39 C40 106(3) . . ?
N6 C40 C39 112(3) . . ?
N7 C41 C42 177(4) . . ?
N8 C43 C44 177(3) . . ?
N9 C45 C46 170(4) . . ?
N10 C47 C48 177(4) . . ?
N11 C49 C50 171(4) . . ?

_refine_diff_density_max         2.060
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.207

# start Validation Reply Form
_vrf_PLAT342_Latfa4detaH         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04028 Ang.
RESPONSE: The crystal has very weak scattering power with no intense peaks
above 54degree of 2theta. Non-cetrosymmetric structure and small number
of intense peaks lead to reduced data-to-parameter ratio and to low bond
precision
;
_vrf_PLAT973_Latfa4detaH         
;
PROBLEM: Check Calcd Positive Resid. Density on       La3       1.92 eA-3
RESPONSE: Residual density peaks are Fourier riples originated from the
truncated diffraction data. 
;

_vrf_PLAT020_Latfa4detaH         
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.167 Report
RESPONSE: The crystal had tiny needele-like shape with weak scattering
power complicated by racemic twinning effect. The data were collected
at an exposition time of 90 sec per frame. The crystal was affected by 
radiation damage during data acquisition.
;

# end Validation Reply Form




