# Electronic Supplementary Material (ESI) 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_exp_542
_database_code_depnum_ccdc_archive 'CCDC 2307060'
loop_
_audit_author_name
_audit_author_address
'Rebecca A. Musgrave'
;Kings College London
United Kingdom
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_audit_creation_date             2023-08-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H30 Co F3 N3 Na2 O9 S'
_chemical_formula_sum            'C30 H30 Co F3 N3 Na2 O9 S'
_chemical_formula_weight         770.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 H30 Co F3 N4 Na2 O9 S'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7547(5)
_cell_length_b                   13.2058(5)
_cell_length_c                   13.4600(4)
_cell_angle_alpha                104.532(3)
_cell_angle_beta                 106.887(3)
_cell_angle_gamma                105.274(3)
_cell_volume                     1803.25(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7704
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1540
_cell_measurement_theta_min      4.2180
_shelx_estimated_absorpt_T_max   0.611
_shelx_estimated_absorpt_T_min   0.220
_exptl_absorpt_coefficient_mu    5.115
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             790
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 8 0 0.0847
3 -8 0 0.0525
4 -7 -3 0.0824
-2 -7 6 0.1041
-5 1 7 0.1928
-2 2 -7 0.0869
4 0 4 0.1346
-3 1 -6 0.0679
-6 -2 0 0.1012
6 -6 1 0.1049
-7 5 1 0.1280
-1 7 -6 0.1194
-2 -6 7 0.1286
-5 7 2 0.1118
0 7 2 0.0624
-2 -7 1 0.0714
2 7 -1 0.1064
5 -4 5 0.1364
7 -2 0 0.1368
-4 7 -4 0.0997
4 -7 4 0.1111
1 -4 -6 0.0660
-1 -6 -3 0.0348
6 -3 3 0.1213
7 -3 2 0.1194
-1 8 1 0.0700

_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.107
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.5050 8.2542 0.1592 0.9102 -0.3221 0.2603
2.5139 -8.2506 -0.1735 -0.9107 0.3222 -0.2586
4.0579 -7.0565 -2.8806 -0.9388 0.3323 0.0906
-2.0989 -6.8854 5.8656 -0.4081 0.1442 -0.9015
-5.4952 1.0726 7.4241 0.5517 -0.1955 -0.8108
-1.5993 1.7885 -7.4809 -0.4461 -0.7280 0.5206
4.2099 0.2178 4.4454 0.5219 0.8521 -0.0397
-2.7801 0.9783 -6.4088 -0.4933 -0.8051 0.3294
-5.8322 -2.3321 0.1262 -0.4542 -0.7417 -0.4935
6.3078 -6.3037 0.8173 -0.4773 0.8787 0.0091
-7.0706 5.1856 0.9505 0.4635 -0.8532 -0.2393
-1.3850 7.3192 -6.0708 0.3305 -0.6088 0.7211
-1.7269 -5.9722 7.4175 -0.1621 0.2989 -0.9404
-5.4664 7.1000 1.5511 0.7908 -0.6065 -0.0824
0.3734 6.6278 1.9741 0.9575 0.1776 0.2275
-1.6429 -7.1149 0.6950 -0.8397 -0.1556 -0.5202
1.7631 7.1246 -0.9632 0.8230 0.1525 0.5471
4.7230 -4.4564 4.9416 0.0248 0.9582 -0.2850
7.1265 -1.9881 0.3766 0.0248 0.9488 0.3148
-3.9615 7.0593 -4.4901 0.3448 -0.8316 0.4355
4.3665 -6.9750 4.0835 -0.3547 0.8555 -0.3772
0.8890 -4.1998 -5.6974 -0.9308 -0.2758 0.2397
-0.7138 -5.8769 -2.8181 -0.9479 -0.2810 -0.1503
6.1840 -3.4050 2.8379 0.0260 0.9996 0.0090
6.7245 -2.7485 1.6586 0.0256 0.9868 0.1599
-1.3147 7.8820 0.7700 0.9540 -0.1255 0.2722

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.154
_diffrn_reflns_theta_min         3.671
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00  33.00   1.00    5.00    --  -33.50   0.00 -60.00  136
  2  ω     44.00  75.00   1.00    5.00    --   36.21 -99.00 -60.00   31
  3  ω     20.00 103.00   1.00    5.00    --   36.21  57.00 -30.00   83
  4  ω     69.00 104.00   1.00    5.00    --   36.21 178.00 -30.00   35
  5  ω     29.00  99.00   1.00    5.00    --   36.21  57.00 120.00   70
  6  ω     73.00  98.00   1.00    5.00    --   36.21 178.00 120.00   25
  7  ω      4.00  57.00   1.00    5.00    --   36.21 -99.00  60.00   53
  8  ω      2.00  51.00   1.00    5.00    --   36.21 -37.00-180.00   49
  9  ω    -33.00  -7.00   1.00    5.00    --   36.21 -37.00-180.00   26
 10  ω     23.00  75.00   1.00    5.00    --   36.21 -99.00 150.00   52
 11  ω    102.00 175.00   1.00   20.00    --  108.00  77.00  90.00   73
 12  ω     93.00 155.00   1.00   20.00    --  108.00  45.00   0.00   62
 13  ω     64.00 105.00   1.00   20.00    --  108.00-111.00  30.00   41
 14  ω    104.00 178.00   1.00   20.00    --  108.00 111.00-180.00   74
 15  ω     91.00 149.00   1.00   20.00    --  108.00  45.00 150.00   58
 16  ω     82.00 108.00   1.00   20.00    --  108.00 -30.00  90.00   26
 17  ω     38.00  64.00   1.00   20.00    --  108.00 -30.00  90.00   26
 18  ω     66.00 121.00   1.00   20.00    --  108.00 -45.00 -90.00   55
 19  ω     64.00 109.00   1.00   20.00    --  108.00-111.00-120.00   45
 20  ω     66.00 123.00   1.00   20.00    --  108.00 -45.00   0.00   57
 21  ω     79.00 107.00   1.00   20.00    --  108.00-111.00 120.00   28
 22  ω    110.00 177.00   1.00   20.00    --  108.00 111.00  30.00   67
 23  ω    114.00 146.00   1.00   20.00    --  108.00 111.00  60.00   32
 24  ω     43.00 116.00   1.00   20.00    --  108.00 -45.00 120.00   73
 25  ω     51.00 112.00   1.00   20.00    --  108.00 -77.00  90.00   61
 26  ω     92.00 160.00   1.00   20.00    --  108.00  45.00-120.00   68
 27  ω     52.00  96.00   1.00   20.00    --  108.00-111.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0322522000
_diffrn_orient_matrix_UB_12      0.1184988000
_diffrn_orient_matrix_UB_13      0.0810637000
_diffrn_orient_matrix_UB_21      0.1291457000
_diffrn_orient_matrix_UB_22      -0.0011646000
_diffrn_orient_matrix_UB_23      0.0694240000
_diffrn_orient_matrix_UB_31      0.0623647000
_diffrn_orient_matrix_UB_32      0.0518230000
_diffrn_orient_matrix_UB_33      -0.0705385000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6401
_reflns_number_total             6933
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²+1.3549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1085
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C18(H18), C22(H22), C16(H16), C10(H10), C8(H8), C17(H17),
 C26(H26), C9(H9), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.76295(3) 0.61712(3) 0.23095(3) 0.01787(10) Uani 1 1 d . . . . .
S1 S 0.29857(6) 0.32930(5) 0.33530(5) 0.02734(14) Uani 1 1 d . . . . .
Na03 Na 0.55927(10) 0.56488(8) 0.36453(8) 0.0272(2) Uani 1 1 d . . . . .
Na04 Na 0.86374(10) 0.68472(8) 0.51810(8) 0.0299(2) Uani 1 1 d . . . . .
O4 O 1.00547(17) 0.87955(14) 0.57843(14) 0.0253(4) Uani 1 1 d . . . . .
O3 O 0.89309(16) 0.73505(14) 0.37671(13) 0.0248(4) Uani 1 1 d . . . . .
O5 O 0.74400(16) 0.53316(13) 0.34754(13) 0.0229(3) Uani 1 1 d . . . . .
O1 O 0.61162(16) 0.65440(14) 0.25494(14) 0.0224(3) Uani 1 1 d . . . . .
O2 O 0.48489(17) 0.71950(16) 0.37102(15) 0.0287(4) Uani 1 1 d . . . . .
O6 O 0.85670(18) 0.50446(15) 0.53347(14) 0.0298(4) Uani 1 1 d . . . . .
N1 N 0.71731(19) 0.68050(17) 0.09768(16) 0.0229(4) Uani 1 1 d . . . . .
F3 F 0.3089(3) 0.1976(2) 0.16201(17) 0.0772(8) Uani 1 1 d . . . . .
N2 N 0.92548(19) 0.62598(16) 0.18551(16) 0.0206(4) Uani 1 1 d . . . . .
O9 O 0.3345(3) 0.3349(2) 0.44886(17) 0.0476(6) Uani 1 1 d . . . . .
N3 N 0.68005(19) 0.45321(17) 0.11326(16) 0.0224(4) Uani 1 1 d . . . . .
F2 F 0.2668(3) 0.11745(18) 0.2722(2) 0.0850(9) Uani 1 1 d . . . . .
O8 O 0.1638(2) 0.2972(2) 0.2804(2) 0.0535(6) Uani 1 1 d . . . . .
O7 O 0.3763(2) 0.42107(19) 0.3183(2) 0.0524(6) Uani 1 1 d . . . . .
F1 F 0.4558(3) 0.2267(3) 0.3127(2) 0.0880(9) Uani 1 1 d . . . . .
C14 C 1.0243(2) 0.7169(2) 0.22335(19) 0.0226(5) Uani 1 1 d . . . . .
H14 H 1.073457 0.723375 0.178767 0.027 Uiso 1 1 calc R U . . .
C20 C 1.0035(2) 0.80937(19) 0.39998(19) 0.0203(4) Uani 1 1 d . . . . .
C28 C 0.7476(2) 0.43388(19) 0.3392(2) 0.0213(5) Uani 1 1 d . . . . .
C15 C 1.0683(2) 0.80969(19) 0.32609(19) 0.0214(5) Uani 1 1 d . . . . .
C11 C 0.5110(2) 0.7793(2) 0.3052(2) 0.0248(5) Uani 1 1 d . . . . .
C6 C 0.6643(2) 0.7533(2) 0.09478(19) 0.0233(5) Uani 1 1 d . . . . .
H6 H 0.661323 0.782686 0.036892 0.028 Uiso 1 1 calc R U . . .
C12 C 0.5817(2) 0.73957(19) 0.24430(19) 0.0207(5) Uani 1 1 d . . . . .
C23 C 0.7026(2) 0.3449(2) 0.2368(2) 0.0249(5) Uani 1 1 d . . . . .
C18 C 1.1762(2) 0.9840(2) 0.5329(2) 0.0277(5) Uani 1 1 d . . . . .
H18 H 1.214421 1.042071 0.603841 0.033 Uiso 1 1 calc R U . . .
C27 C 0.8021(2) 0.4113(2) 0.4372(2) 0.0247(5) Uani 1 1 d . . . . .
C7 C 0.6085(2) 0.79507(19) 0.1711(2) 0.0229(5) Uani 1 1 d . . . . .
C22 C 0.6682(2) 0.3603(2) 0.1309(2) 0.0243(5) Uani 1 1 d . . . . .
H22 H 0.632779 0.294090 0.066898 0.029 Uiso 1 1 calc R U . . .
C19 C 1.0663(2) 0.89582(19) 0.50707(19) 0.0217(5) Uani 1 1 d . . . . .
C16 C 1.1804(2) 0.9011(2) 0.3536(2) 0.0271(5) Uani 1 1 d . . . . .
H16 H 1.221005 0.902653 0.302116 0.032 Uiso 1 1 calc R U . . .
C2 C 0.7709(2) 0.5296(2) -0.01035(19) 0.0247(5) Uani 1 1 d . . . . .
C10 C 0.4744(3) 0.8688(2) 0.2968(2) 0.0316(6) Uani 1 1 d . . . . .
H10 H 0.429165 0.894088 0.339682 0.038 Uiso 1 1 calc R U . . .
C8 C 0.5677(3) 0.8853(2) 0.1625(2) 0.0304(5) Uani 1 1 d . . . . .
H8 H 0.584982 0.920602 0.112363 0.036 Uiso 1 1 calc R U . . .
C4 C 0.8997(2) 0.5462(2) 0.07699(19) 0.0248(5) Uani 1 1 d . . . . .
H4A H 0.898469 0.473063 0.083852 0.030 Uiso 1 1 calc R U . . .
H4B H 0.969110 0.573969 0.051820 0.030 Uiso 1 1 calc R U . . .
C5 C 0.6576(2) 0.4462(2) -0.00191(19) 0.0257(5) Uani 1 1 d . . . . .
H5A H 0.579589 0.462042 -0.032441 0.031 Uiso 1 1 calc R U . . .
H5B H 0.643266 0.368875 -0.047356 0.031 Uiso 1 1 calc R U . . .
C17 C 1.2315(3) 0.9877(2) 0.4535(2) 0.0316(6) Uani 1 1 d . . . . .
H17 H 1.304683 1.050569 0.469282 0.038 Uiso 1 1 calc R U . . .
C3 C 0.7552(3) 0.6432(2) 0.0032(2) 0.0274(5) Uani 1 1 d . . . . .
H3A H 0.836806 0.700046 0.015099 0.033 Uiso 1 1 calc R U . . .
H3B H 0.689648 0.637223 -0.065905 0.033 Uiso 1 1 calc R U . . .
C1 C 0.7722(3) 0.4816(2) -0.1262(2) 0.0315(6) Uani 1 1 d . . . . .
H1A H 0.833269 0.538847 -0.138479 0.047 Uiso 1 1 calc R U . . .
H1B H 0.686806 0.459222 -0.182624 0.047 Uiso 1 1 calc R U . . .
H1C H 0.797429 0.415951 -0.131408 0.047 Uiso 1 1 calc R U . . .
C21 C 1.0565(3) 0.9648(2) 0.6857(2) 0.0287(5) Uani 1 1 d . . . . .
H21A H 1.001796 0.946249 0.726291 0.043 Uiso 1 1 calc R U . . .
H21B H 1.059911 1.037130 0.677548 0.043 Uiso 1 1 calc R U . . .
H21C H 1.142671 0.969566 0.726778 0.043 Uiso 1 1 calc R U . . .
C26 C 0.7998(3) 0.3052(2) 0.4328(2) 0.0316(6) Uani 1 1 d . . . . .
H26 H 0.835807 0.292434 0.499355 0.038 Uiso 1 1 calc R U . . .
C9 C 0.5038(3) 0.9224(2) 0.2250(3) 0.0353(6) Uani 1 1 d . . . . .
H9 H 0.479320 0.984559 0.219782 0.042 Uiso 1 1 calc R U . . .
C24 C 0.6987(3) 0.2364(2) 0.2346(2) 0.0336(6) Uani 1 1 d . . . . .
H24 H 0.663570 0.176265 0.165252 0.040 Uiso 1 1 calc R U . . .
C25 C 0.7448(3) 0.2166(2) 0.3309(3) 0.0363(6) Uani 1 1 d . . . . .
H25 H 0.739374 0.142815 0.328282 0.044 Uiso 1 1 calc R U . . .
C13 C 0.4056(3) 0.7463(3) 0.4278(3) 0.0414(7) Uani 1 1 d . . . . .
H13A H 0.323836 0.737783 0.373768 0.062 Uiso 1 1 calc R U . . .
H13B H 0.447740 0.824078 0.479933 0.062 Uiso 1 1 calc R U . . .
H13C H 0.390684 0.695654 0.468625 0.062 Uiso 1 1 calc R U . . .
C29 C 0.9251(3) 0.4905(3) 0.6334(2) 0.0365(6) Uani 1 1 d . . . . .
H29A H 0.987815 0.457667 0.621281 0.055 Uiso 1 1 calc R U . . .
H29B H 0.864990 0.440465 0.653358 0.055 Uiso 1 1 calc R U . . .
H29C H 0.969102 0.563673 0.693743 0.055 Uiso 1 1 calc R U . . .
C01F C 0.3338(3) 0.2103(3) 0.2670(3) 0.0420(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Na03 3.4197(10) . ?
Co1 Na04 3.4915(10) . ?
Co1 O3 2.0205(16) . ?
Co1 O5 2.1652(16) . ?
Co1 O1 2.0558(17) . ?
Co1 N1 2.153(2) . ?
Co1 N2 2.153(2) . ?
Co1 N3 2.101(2) . ?
S1 Na04 3.1230(12) 2_666 ?
S1 O9 1.440(2) . ?
S1 O8 1.430(2) . ?
S1 O7 1.426(2) . ?
S1 C01F 1.824(3) . ?
Na03 Na04 3.2653(15) . ?
Na03 O5 2.380(2) . ?
Na03 O1 2.2297(19) . ?
Na03 O2 2.416(2) . ?
Na03 O9 2.293(2) 2_666 ?
Na03 O7 2.257(2) . ?
Na04 O4 2.4418(19) . ?
Na04 O3 2.253(2) . ?
Na04 O5 2.3643(19) . ?
Na04 O6 2.423(2) . ?
Na04 O9 2.457(3) 2_666 ?
Na04 O8 2.783(3) 2_666 ?
Na04 C20 3.056(3) . ?
O4 C19 1.379(3) . ?
O4 C21 1.427(3) . ?
O3 C20 1.298(3) . ?
O5 C28 1.300(3) . ?
O1 C12 1.292(3) . ?
O2 C11 1.372(3) . ?
O2 C13 1.425(3) . ?
O6 C27 1.380(3) . ?
O6 C29 1.437(3) . ?
N1 C6 1.278(3) . ?
N1 C3 1.480(3) . ?
F3 C01F 1.314(4) . ?
N2 C14 1.290(3) . ?
N2 C4 1.462(3) . ?
N3 C22 1.287(3) . ?
N3 C5 1.469(3) . ?
F2 C01F 1.302(4) . ?
F1 C01F 1.318(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.443(3) . ?
C20 C15 1.418(3) . ?
C20 C19 1.428(3) . ?
C28 C23 1.412(3) . ?
C28 C27 1.431(3) . ?
C15 C16 1.409(3) . ?
C11 C12 1.431(3) . ?
C11 C10 1.379(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.445(4) . ?
C12 C7 1.424(3) . ?
C23 C22 1.446(4) . ?
C23 C24 1.415(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.374(3) . ?
C18 C17 1.408(4) . ?
C27 C26 1.380(4) . ?
C7 C8 1.414(3) . ?
C22 H22 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.369(4) . ?
C2 C4 1.544(3) . ?
C2 C5 1.542(3) . ?
C2 C3 1.531(3) . ?
C2 C1 1.535(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.401(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.366(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C17 H17 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C25 1.397(4) . ?
C9 H9 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.371(4) . ?
C25 H25 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Na03 Co1 Na04 56.38(3) . . ?
O3 Co1 Na03 87.90(5) . . ?
O3 Co1 Na04 37.49(5) . . ?
O3 Co1 O5 77.97(7) . . ?
O3 Co1 O1 93.97(7) . . ?
O3 Co1 N1 113.89(7) . . ?
O3 Co1 N2 84.22(7) . . ?
O3 Co1 N3 152.14(8) . . ?
O5 Co1 Na03 43.62(5) . . ?
O5 Co1 Na04 41.70(5) . . ?
O1 Co1 Na03 38.86(5) . . ?
O1 Co1 Na04 80.53(5) . . ?
O1 Co1 O5 82.33(7) . . ?
O1 Co1 N1 83.18(7) . . ?
O1 Co1 N2 160.06(7) . . ?
O1 Co1 N3 104.58(7) . . ?
N1 Co1 Na03 120.55(6) . . ?
N1 Co1 Na04 144.84(6) . . ?
N1 Co1 O5 161.88(7) . . ?
N2 Co1 Na03 159.94(6) . . ?
N2 Co1 Na04 108.56(5) . . ?
N2 Co1 O5 116.46(7) . . ?
N2 Co1 N1 79.48(8) . . ?
N3 Co1 Na03 93.62(6) . . ?
N3 Co1 Na04 125.03(6) . . ?
N3 Co1 O5 84.03(7) . . ?
N3 Co1 N1 89.17(8) . . ?
N3 Co1 N2 85.01(8) . . ?
O9 S1 Na04 49.91(11) . 2_666 ?
O9 S1 C01F 103.91(14) . . ?
O8 S1 Na04 63.03(11) . 2_666 ?
O8 S1 O9 112.32(16) . . ?
O8 S1 C01F 104.30(15) . . ?
O7 S1 Na04 132.82(11) . 2_666 ?
O7 S1 O9 114.94(16) . . ?
O7 S1 O8 115.97(17) . . ?
O7 S1 C01F 103.54(15) . . ?
C01F S1 Na04 122.91(11) . 2_666 ?
Na04 Na03 Co1 62.92(3) . . ?
O5 Na03 Co1 38.88(4) . . ?
O5 Na03 Na04 46.31(5) . . ?
O5 Na03 O2 134.44(7) . . ?
O1 Na03 Co1 35.34(5) . . ?
O1 Na03 Na04 83.77(5) . . ?
O1 Na03 O5 74.09(6) . . ?
O1 Na03 O2 67.88(7) . . ?
O1 Na03 O9 114.79(9) . 2_666 ?
O1 Na03 O7 126.61(9) . . ?
O2 Na03 Co1 101.04(5) . . ?
O2 Na03 Na04 104.22(6) . . ?
O9 Na03 Co1 109.41(7) 2_666 . ?
O9 Na03 Na04 48.69(7) 2_666 . ?
O9 Na03 O5 92.07(8) 2_666 . ?
O9 Na03 O2 82.18(8) 2_666 . ?
O7 Na03 Co1 132.26(8) . . ?
O7 Na03 Na04 146.28(8) . . ?
O7 Na03 O5 121.51(9) . . ?
O7 Na03 O2 101.37(9) . . ?
O7 Na03 O9 115.02(10) . 2_666 ?
S1 Na04 Co1 129.31(4) 2_666 . ?
S1 Na04 Na03 68.93(3) 2_666 . ?
Na03 Na04 Co1 60.70(2) . . ?
O4 Na04 Co1 99.36(5) . . ?
O4 Na04 S1 108.50(5) . 2_666 ?
O4 Na04 Na03 129.68(6) . . ?
O4 Na04 O9 113.52(8) . 2_666 ?
O4 Na04 O8 95.44(7) . 2_666 ?
O4 Na04 C20 48.78(6) . . ?
O3 Na04 Co1 33.07(4) . . ?
O3 Na04 S1 146.31(7) . 2_666 ?
O3 Na04 Na03 88.17(5) . . ?
O3 Na04 O4 67.04(6) . . ?
O3 Na04 O5 69.56(6) . . ?
O3 Na04 O6 123.48(8) . . ?
O3 Na04 O9 121.84(8) . 2_666 ?
O3 Na04 O8 159.38(8) . 2_666 ?
O3 Na04 C20 22.40(6) . . ?
O5 Na04 Co1 37.53(4) . . ?
O5 Na04 S1 106.77(6) . 2_666 ?
O5 Na04 Na03 46.70(5) . . ?
O5 Na04 O4 136.58(7) . . ?
O5 Na04 O6 66.96(6) . . ?
O5 Na04 O9 88.48(8) . 2_666 ?
O5 Na04 O8 126.77(7) . 2_666 ?
O5 Na04 C20 89.09(7) . . ?
O6 Na04 Co1 101.06(5) . . ?
O6 Na04 S1 81.21(5) . 2_666 ?
O6 Na04 Na03 87.32(6) . . ?
O6 Na04 O4 142.98(8) . . ?
O6 Na04 O9 91.31(8) . 2_666 ?
O6 Na04 O8 77.02(7) . 2_666 ?
O6 Na04 C20 127.32(8) . . ?
O9 Na04 Co1 103.28(6) 2_666 . ?
O9 Na04 S1 26.64(5) 2_666 2_666 ?
O9 Na04 Na03 44.52(6) 2_666 . ?
O9 Na04 O8 53.67(7) 2_666 2_666 ?
O9 Na04 C20 136.13(8) 2_666 . ?
O8 Na04 Co1 156.43(6) 2_666 . ?
O8 Na04 S1 27.25(5) 2_666 2_666 ?
O8 Na04 Na03 95.74(6) 2_666 . ?
O8 Na04 C20 144.02(7) 2_666 . ?
C20 Na04 Co1 54.70(5) . . ?
C20 Na04 S1 151.39(6) . 2_666 ?
C20 Na04 Na03 109.95(5) . . ?
C19 O4 Na04 111.93(13) . . ?
C19 O4 C21 117.25(19) . . ?
C21 O4 Na04 128.43(15) . . ?
Co1 O3 Na04 109.43(8) . . ?
C20 O3 Co1 130.88(15) . . ?
C20 O3 Na04 116.17(14) . . ?
Co1 O5 Na03 97.49(7) . . ?
Co1 O5 Na04 100.77(7) . . ?
Na04 O5 Na03 87.00(7) . . ?
C28 O5 Co1 126.16(15) . . ?
C28 O5 Na03 117.06(14) . . ?
C28 O5 Na04 119.84(15) . . ?
Co1 O1 Na03 105.80(7) . . ?
C12 O1 Co1 126.82(15) . . ?
C12 O1 Na03 123.38(15) . . ?
C11 O2 Na03 116.66(15) . . ?
C11 O2 C13 117.3(2) . . ?
C13 O2 Na03 125.67(17) . . ?
C27 O6 Na04 118.23(14) . . ?
C27 O6 C29 116.8(2) . . ?
C29 O6 Na04 124.05(17) . . ?
C6 N1 Co1 125.34(17) . . ?
C6 N1 C3 115.6(2) . . ?
C3 N1 Co1 118.93(15) . . ?
C14 N2 Co1 122.72(16) . . ?
C14 N2 C4 116.1(2) . . ?
C4 N2 Co1 115.77(15) . . ?
S1 O9 Na03 150.59(16) . 2_666 ?
S1 O9 Na04 103.46(13) . 2_666 ?
Na03 O9 Na04 86.79(8) 2_666 2_666 ?
C22 N3 Co1 127.99(17) . . ?
C22 N3 C5 115.8(2) . . ?
C5 N3 Co1 114.92(15) . . ?
S1 O8 Na04 89.72(12) . 2_666 ?
S1 O7 Na03 153.40(18) . . ?
N2 C14 H14 116.5 . . ?
N2 C14 C15 127.0(2) . . ?
C15 C14 H14 116.5 . . ?
O3 C20 Na04 41.43(11) . . ?
O3 C20 C15 124.2(2) . . ?
O3 C20 C19 118.9(2) . . ?
C15 C20 Na04 149.82(16) . . ?
C15 C20 C19 117.0(2) . . ?
C19 C20 Na04 83.43(14) . . ?
O5 C28 C23 123.6(2) . . ?
O5 C28 C27 119.8(2) . . ?
C23 C28 C27 116.6(2) . . ?
C20 C15 C14 121.7(2) . . ?
C16 C15 C14 118.3(2) . . ?
C16 C15 C20 119.9(2) . . ?
O2 C11 C12 113.0(2) . . ?
O2 C11 C10 124.8(2) . . ?
C10 C11 C12 122.1(2) . . ?
N1 C6 H6 116.9 . . ?
N1 C6 C7 126.2(2) . . ?
C7 C6 H6 116.9 . . ?
O1 C12 C11 119.0(2) . . ?
O1 C12 C7 124.6(2) . . ?
C7 C12 C11 116.3(2) . . ?
C28 C23 C22 123.0(2) . . ?
C28 C23 C24 120.3(2) . . ?
C24 C23 C22 116.5(2) . . ?
C19 C18 H18 120.3 . . ?
C19 C18 C17 119.5(2) . . ?
C17 C18 H18 120.3 . . ?
O6 C27 C28 113.9(2) . . ?
O6 C27 C26 124.4(2) . . ?
C26 C27 C28 121.7(2) . . ?
C12 C7 C6 121.3(2) . . ?
C8 C7 C6 118.0(2) . . ?
C8 C7 C12 120.4(2) . . ?
N3 C22 C23 127.6(2) . . ?
N3 C22 H22 116.2 . . ?
C23 C22 H22 116.2 . . ?
O4 C19 C20 112.8(2) . . ?
C18 C19 O4 125.4(2) . . ?
C18 C19 C20 121.8(2) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 C15 120.9(2) . . ?
C17 C16 H16 119.6 . . ?
C5 C2 C4 111.8(2) . . ?
C3 C2 C4 109.6(2) . . ?
C3 C2 C5 110.6(2) . . ?
C3 C2 C1 108.5(2) . . ?
C1 C2 C4 108.2(2) . . ?
C1 C2 C5 108.0(2) . . ?
C11 C10 H10 120.0 . . ?
C11 C10 C9 120.1(2) . . ?
C9 C10 H10 120.0 . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H8 119.4 . . ?
N2 C4 C2 111.6(2) . . ?
N2 C4 H4A 109.3 . . ?
N2 C4 H4B 109.3 . . ?
C2 C4 H4A 109.3 . . ?
C2 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
N3 C5 C2 112.00(19) . . ?
N3 C5 H5A 109.2 . . ?
N3 C5 H5B 109.2 . . ?
C2 C5 H5A 109.2 . . ?
C2 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C18 C17 H17 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
N1 C3 C2 111.9(2) . . ?
N1 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C26 H26 119.9 . . ?
C27 C26 C25 120.2(2) . . ?
C25 C26 H26 119.9 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9 120.0 . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.0(3) . . ?
C25 C24 H24 119.5 . . ?
C26 C25 H25 120.1 . . ?
C24 C25 C26 119.8(2) . . ?
C24 C25 H25 120.1 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O6 C29 H29A 109.5 . . ?
O6 C29 H29B 109.5 . . ?
O6 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F3 C01F S1 110.4(2) . . ?
F3 C01F F1 106.9(3) . . ?
F2 C01F S1 111.4(2) . . ?
F2 C01F F3 108.5(3) . . ?
F2 C01F F1 108.6(3) . . ?
F1 C01F S1 110.9(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O3 C20 Na04 -156.3(3) . . . . ?
Co1 O3 C20 C15 -12.2(3) . . . . ?
Co1 O3 C20 C19 169.00(16) . . . . ?
Co1 O5 C28 C23 -32.6(3) . . . . ?
Co1 O5 C28 C27 145.90(17) . . . . ?
Co1 O1 C12 C11 -154.41(16) . . . . ?
Co1 O1 C12 C7 28.8(3) . . . . ?
Co1 N1 C6 C7 -9.4(3) . . . . ?
Co1 N1 C3 C2 24.2(3) . . . . ?
Co1 N2 C14 C15 25.2(3) . . . . ?
Co1 N2 C4 C2 38.1(2) . . . . ?
Co1 N3 C22 C23 3.9(4) . . . . ?
Co1 N3 C5 C2 42.3(2) . . . . ?
Na03 O5 C28 C23 91.1(2) . . . . ?
Na03 O5 C28 C27 -90.4(2) . . . . ?
Na03 O1 C12 C11 -0.2(3) . . . . ?
Na03 O1 C12 C7 -176.92(16) . . . . ?
Na03 O2 C11 C12 -1.1(2) . . . . ?
Na03 O2 C11 C10 178.9(2) . . . . ?
Na04 S1 O9 Na03 -107.9(3) 2_666 . . 2_666 ?
Na04 S1 O7 Na03 82.1(4) 2_666 . . . ?
Na04 S1 C01F F3 131.0(2) 2_666 . . . ?
Na04 S1 C01F F2 10.4(3) 2_666 . . . ?
Na04 S1 C01F F1 -110.7(2) 2_666 . . . ?
Na04 O4 C19 C20 19.7(2) . . . . ?
Na04 O4 C19 C18 -160.0(2) . . . . ?
Na04 O3 C20 C15 144.09(19) . . . . ?
Na04 O3 C20 C19 -34.7(3) . . . . ?
Na04 O5 C28 C23 -165.90(18) . . . . ?
Na04 O5 C28 C27 12.6(3) . . . . ?
Na04 O6 C27 C28 -4.2(3) . . . . ?
Na04 O6 C27 C26 175.1(2) . . . . ?
Na04 C20 C15 C14 41.4(4) . . . . ?
Na04 C20 C15 C16 -137.0(3) . . . . ?
Na04 C20 C19 O4 -14.54(17) . . . . ?
Na04 C20 C19 C18 165.1(2) . . . . ?
O3 C20 C15 C14 -9.1(4) . . . . ?
O3 C20 C15 C16 172.4(2) . . . . ?
O3 C20 C19 O4 7.7(3) . . . . ?
O3 C20 C19 C18 -172.6(2) . . . . ?
O5 C28 C23 C22 10.9(4) . . . . ?
O5 C28 C23 C24 -174.1(2) . . . . ?
O5 C28 C27 O6 -5.2(3) . . . . ?
O5 C28 C27 C26 175.4(2) . . . . ?
O1 C12 C7 C6 5.0(3) . . . . ?
O1 C12 C7 C8 177.7(2) . . . . ?
O2 C11 C12 O1 0.9(3) . . . . ?
O2 C11 C12 C7 177.89(19) . . . . ?
O2 C11 C10 C9 -178.6(2) . . . . ?
O6 C27 C26 C25 -178.5(2) . . . . ?
N1 C6 C7 C12 -14.5(4) . . . . ?
N1 C6 C7 C8 172.7(2) . . . . ?
N2 C14 C15 C20 0.4(4) . . . . ?
N2 C14 C15 C16 178.9(2) . . . . ?
O9 S1 O8 Na04 8.08(14) . . . 2_666 ?
O9 S1 O7 Na03 24.6(4) . . . . ?
O9 S1 C01F F3 -178.0(3) . . . . ?
O9 S1 C01F F2 61.4(3) . . . . ?
O9 S1 C01F F1 -59.8(3) . . . . ?
O8 S1 O9 Na03 -117.3(3) . . . 2_666 ?
O8 S1 O9 Na04 -9.42(17) . . . 2_666 ?
O8 S1 O7 Na03 158.4(3) . . . . ?
O8 S1 C01F F3 64.1(3) . . . . ?
O8 S1 C01F F2 -56.5(3) . . . . ?
O8 S1 C01F F1 -177.6(3) . . . . ?
O7 S1 O9 Na03 18.2(4) . . . 2_666 ?
O7 S1 O9 Na04 126.05(15) . . . 2_666 ?
O7 S1 O8 Na04 -126.91(14) . . . 2_666 ?
O7 S1 C01F F3 -57.6(3) . . . . ?
O7 S1 C01F F2 -178.2(3) . . . . ?
O7 S1 C01F F1 60.6(3) . . . . ?
C14 N2 C4 C2 -116.8(2) . . . . ?
C14 C15 C16 C17 -175.3(2) . . . . ?
C20 C15 C16 C17 3.2(4) . . . . ?
C28 C23 C22 N3 4.7(4) . . . . ?
C28 C23 C24 C25 -3.7(4) . . . . ?
C28 C27 C26 C25 0.8(4) . . . . ?
C15 C20 C19 O4 -171.1(2) . . . . ?
C15 C20 C19 C18 8.5(3) . . . . ?
C15 C16 C17 C18 3.2(4) . . . . ?
C11 C12 C7 C6 -171.8(2) . . . . ?
C11 C12 C7 C8 0.9(3) . . . . ?
C11 C10 C9 C8 0.7(4) . . . . ?
C6 N1 C3 C2 -159.0(2) . . . . ?
C6 C7 C8 C9 174.0(2) . . . . ?
C12 C11 C10 C9 1.4(4) . . . . ?
C12 C7 C8 C9 1.1(4) . . . . ?
C23 C28 C27 O6 173.4(2) . . . . ?
C23 C28 C27 C26 -6.0(4) . . . . ?
C23 C24 C25 C26 -1.8(4) . . . . ?
C27 C28 C23 C22 -167.6(2) . . . . ?
C27 C28 C23 C24 7.4(4) . . . . ?
C27 C26 C25 C24 3.2(4) . . . . ?
C7 C8 C9 C10 -1.9(4) . . . . ?
C22 N3 C5 C2 -125.7(2) . . . . ?
C22 C23 C24 C25 171.6(3) . . . . ?
C19 C20 C15 C14 169.7(2) . . . . ?
C19 C20 C15 C16 -8.8(3) . . . . ?
C19 C18 C17 C16 -3.6(4) . . . . ?
C10 C11 C12 O1 -179.1(2) . . . . ?
C10 C11 C12 C7 -2.1(3) . . . . ?
C4 N2 C14 C15 178.2(2) . . . . ?
C4 C2 C5 N3 34.0(3) . . . . ?
C4 C2 C3 N1 -77.9(3) . . . . ?
C5 N3 C22 C23 170.0(2) . . . . ?
C5 C2 C4 N2 -81.3(3) . . . . ?
C5 C2 C3 N1 45.8(3) . . . . ?
C17 C18 C19 O4 177.1(2) . . . . ?
C17 C18 C19 C20 -2.4(4) . . . . ?
C3 N1 C6 C7 174.0(2) . . . . ?
C3 C2 C4 N2 41.8(3) . . . . ?
C3 C2 C5 N3 -88.5(2) . . . . ?
C1 C2 C4 N2 159.9(2) . . . . ?
C1 C2 C5 N3 153.0(2) . . . . ?
C1 C2 C3 N1 164.2(2) . . . . ?
C21 O4 C19 C20 -176.4(2) . . . . ?
C21 O4 C19 C18 4.0(3) . . . . ?
C24 C23 C22 N3 -170.4(3) . . . . ?
C13 O2 C11 C12 -174.8(2) . . . . ?
C13 O2 C11 C10 5.2(4) . . . . ?
C29 O6 C27 C28 -173.6(2) . . . . ?
C29 O6 C27 C26 5.8(4) . . . . ?
C01F S1 O9 Na03 130.6(3) . . . 2_666 ?
C01F S1 O9 Na04 -121.55(14) . . . 2_666 ?
C01F S1 O8 Na04 119.96(11) . . . 2_666 ?
C01F S1 O7 Na03 -88.0(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 87 electrons were 
found in a volume of 283Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C2H3N] per Asymmetric Unit 
which account for 44 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.089 0.000 0.000 282.7 86.7 '2 acetonitrile'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.837
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_603
_database_code_depnum_ccdc_archive 'CCDC 2336119'
loop_
_audit_author_name
_audit_author_address
'Rebecca Musgrave'
;Kings College London
United Kingdom
;
_audit_update_record             
;
2024-02-28 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_audit_creation_date             2024-02-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        exp_603
_chemical_formula_moiety         'C30 H30 F3 Mn N3 Na2 O9 S, 2[C2H3N]'
_chemical_formula_sum            'C34 H36 F3 Mn N5 Na2 O9 S'
_chemical_formula_weight         848.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         MnUC29H30N3O6I2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6556(5)
_cell_length_b                   13.3317(5)
_cell_length_c                   13.5391(6)
_cell_angle_alpha                104.826(4)
_cell_angle_beta                 106.697(4)
_cell_angle_gamma                105.433(4)
_cell_volume                     1812.26(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7299
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.0210
_cell_measurement_theta_min      4.1350
_shelx_estimated_absorpt_T_max   0.318
_shelx_estimated_absorpt_T_min   0.149
_exptl_absorpt_coefficient_mu    4.417
_exptl_absorpt_correction_T_max  0.146
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             874
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 2 -1 0.1540
-7 4 -2 0.1724
0 -8 6 0.2064
7 -4 1 0.2302
6 -5 2 0.2067
0 8 -6 0.2443
-4 7 -5 0.1712
-6 -3 4 0.3148
3 -7 5 0.1839
-3 5 -7 0.1673
-5 3 -4 0.1674
0 6 -8 0.2062
6 3 -4 0.3677
4 -4 6 0.1730
1 -6 8 0.1726
5 -3 4 0.2141
2 6 -8 0.2623
-6 3 -4 0.1754
0 -6 8 0.1832
1 -1 7 0.1512
0 -2 8 0.1479
-1 -2 9 0.1540
-3 0 -6 0.1887
-4 -1 -5 0.1923
1 2 -9 0.1934
3 0 6 0.2115
4 3 -8 0.2492
-1 1 -8 0.1853
-4 4 7 0.1531
-2 5 5 0.2000
4 -4 -7 0.1952
6 0 -7 0.2550
1 -5 -5 0.1865
-4 -5 0 0.2601
-6 1 7 0.2473
-5 3 7 0.1689
0 -5 -4 0.1903
4 -3 -7 0.1942
-5 7 1 0.1590
-2 9 -1 0.2560
-7 6 2 0.1533
7 -5 -2 0.2145
8 -2 -4 0.2669
4 -8 0 0.1873
3 -9 1 0.1815
-1 -8 3 0.2426
1 -4 8 0.1586
5 -2 5 0.2074

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.696
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.337
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.0000 2.0000 -1.0000 -0.0823 -0.3199 0.1024
-6.5785 4.4884 -1.8008 -0.2028 -0.8462 0.4927
0.1240 -7.6239 5.9778 0.1940 0.8080 0.5563
6.9041 -3.7224 1.1109 0.1879 0.7843 -0.5912
6.3633 -4.8795 2.1660 0.2098 0.8750 -0.4362
-0.4759 7.6725 -5.9232 -0.2000 -0.8331 -0.5156
-3.6286 7.2541 -4.7605 -0.2324 -0.9687 -0.0867
-6.0668 -3.1312 4.0711 -0.0036 -0.0166 0.9999
2.9678 -7.4834 5.1159 0.2292 0.9552 0.1872
-2.8157 4.8959 -6.7465 0.1823 -0.9828 -0.0302
-5.1455 3.0995 -4.4134 0.1673 -0.9012 0.3998
-0.3700 5.6964 -7.7267 0.1673 -0.9024 -0.3971
6.1239 3.0346 -3.8488 -0.0084 0.0437 -0.9990
4.2795 -3.9378 5.5115 -0.1777 0.9576 -0.2267
1.0276 -5.5626 7.5733 -0.1736 0.9365 0.3048
5.4532 -2.7236 3.9175 -0.1614 0.8692 -0.4674
1.7216 5.7501 -7.7109 0.1365 -0.7371 -0.6619
-5.6071 2.5134 -3.6395 0.1578 -0.8498 0.5029
0.0603 -5.7402 7.7728 -0.1637 0.8834 0.4391
1.3496 -0.6647 7.3657 -0.6473 0.7575 -0.0848
-0.4516 -1.6145 8.4512 -0.6346 0.7429 0.2128
-0.8607 -1.8129 8.5950 -0.6238 0.7302 0.2787
-2.7751 -0.1818 -5.9430 0.6133 -0.7177 0.3299
-3.7406 -0.8164 -4.6153 0.5619 -0.6574 0.5021
1.1854 1.9658 -8.6816 0.6130 -0.7176 -0.3306
2.7983 0.1964 5.9151 -0.6124 0.7166 -0.3340
3.5768 2.9443 -8.4446 0.4654 -0.5450 -0.6974
-0.7387 1.0009 -7.8172 0.6495 -0.7602 -0.0176
-3.6457 3.8161 6.6262 -0.9680 0.1273 0.2161
-1.5436 5.0376 5.2292 -0.9817 0.1290 -0.1400
3.6558 -3.8082 -6.6315 0.9676 -0.1273 -0.2180
6.1393 -0.4879 -6.9524 0.6378 -0.0841 -0.7656
0.7410 -5.3213 -4.5664 0.9564 -0.1257 0.2636
-3.5807 -5.2999 0.0996 0.5613 -0.0736 0.8243
-6.0658 0.6828 7.0113 -0.6637 0.0875 0.7429
-4.5037 3.0466 7.0045 -0.9172 0.1207 0.3798
0.1356 -5.4776 -4.0256 0.9277 -0.1219 0.3529
4.4195 -3.1320 -6.9744 0.9238 -0.1216 -0.3631
-5.3045 7.4515 0.7277 -0.7533 -0.6436 0.1354
-1.9172 8.6022 -1.4215 -0.7033 -0.6010 -0.3797
-6.5899 5.9403 1.8496 -0.6939 -0.5927 0.4088
6.9137 -5.2999 -2.2062 0.6600 0.5637 -0.4966
7.5014 -1.6465 -3.5637 0.4168 0.3558 -0.8365
4.0464 -8.1966 0.1611 0.7579 0.6476 0.0790
2.5439 -8.5710 1.0757 0.7258 0.6202 0.2976
-1.4909 -7.7096 2.9994 0.5034 0.4303 0.7493
1.3864 -3.7612 7.8018 -0.3795 0.9156 0.1330
4.6296 -1.5763 4.7253 -0.3433 0.8286 -0.4423

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12129
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.132
_diffrn_reflns_theta_min         3.653
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  17.00   1.00    6.61    --  -33.50  57.00 120.00   42
  2  ω   -106.00 -47.00   1.00    6.61    --  -33.50-178.00 120.00   59
  3  ω    -44.00 -17.00   1.00    6.61    --  -33.50 -57.00 150.00   27
  4  ω   -101.00 -63.00   1.00    6.61    --  -33.50 -57.00 150.00   38
  5  ω      2.00  74.00   1.00    6.61    --   36.21 -99.00   0.00   72
  6  ω     58.00  91.00   1.00    6.61    --   36.21-130.00 -78.00   33
  7  ω     37.00 103.00   1.00    6.61    --   36.21  57.00 -60.00   66
  8  ω      7.00 107.00   1.00    6.61    --   36.21  19.00  90.00  100
  9  ω    -31.00  53.00   1.00    6.61    --   36.21 -57.00 150.00   84
 10  ω      5.00  57.00   1.00    6.61    --   36.21 -77.00  90.00   52
 11  ω    151.00 176.00   1.00   26.44    --  108.00  45.00 -60.00   25
 12  ω     91.00 117.00   1.00   26.44    --  108.00  61.00  90.00   26
 13  ω    104.00 176.00   1.00   26.44    --  108.00  45.00 120.00   72
 14  ω     92.00 119.00   1.00   26.44    --  108.00  45.00 -60.00   27
 15  ω     43.00 106.00   1.00   26.44    --  108.00-111.00   0.00   63
 16  ω     44.00 124.00   1.00   26.44    --  108.00 -45.00 150.00   80
 17  ω     64.00 108.00   1.00   26.44    --  108.00-111.00 150.00   44
 18  ω    101.00 127.00   1.00   26.44    --  108.00 -77.00 150.00   26
 19  ω     42.00 118.00   1.00   26.44    --  108.00 -45.00  60.00   76
 20  ω     42.00  71.00   1.00   26.44    --  108.00 -94.00  30.00   29
 21  ω     77.00 103.00   1.00   26.44    --  108.00 -94.00  30.00   26
 22  ω     63.00 107.00   1.00   26.44    --  108.00-111.00-120.00   44
 23  ω     39.00 124.00   1.00   26.44    --  108.00 -30.00 -60.00   85
 24  ω     45.00  89.00   1.00   26.44    --  108.00 -94.00 -60.00   44
 25  ω     59.00 104.00   1.00   26.44    --  108.00 -61.00   0.00   45
 26  ω    148.00 173.00   1.00   26.44    --  108.00  61.00  90.00   25
 27  ω     52.00  77.00   1.00   26.44    --  108.00 -77.00 150.00   25
 28  ω     73.00 178.00   1.00   26.44    --  108.00  15.00-120.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0114227000
_diffrn_orient_matrix_UB_12      -0.0999692000
_diffrn_orient_matrix_UB_13      -0.0948026000
_diffrn_orient_matrix_UB_21      0.0793724000
_diffrn_orient_matrix_UB_22      -0.0381520000
_diffrn_orient_matrix_UB_23      0.0848596000
_diffrn_orient_matrix_UB_31      -0.1247841000
_diffrn_orient_matrix_UB_32      -0.0711382000
_diffrn_orient_matrix_UB_33      0.0049286000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6397
_reflns_number_total             6974
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6974
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0504
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0951P)²+0.3202P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1473
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid bond restraints
 S1, O7, O8, O9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18),
 C22(H22), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.23762(3) 0.38498(3) 0.76387(3) 0.03632(12) Uani 1 1 d . . . . .
S1 S 0.69950(6) 0.66826(6) 0.66136(5) 0.04469(16) Uani 1 1 d . U . . .
Na1 Na 0.13041(11) 0.31953(9) 0.47891(8) 0.0476(2) Uani 1 1 d . . . . .
Na2 Na 0.44516(10) 0.42758(9) 0.63187(9) 0.0456(2) Uani 1 1 d . . . . .
F1 F 0.6882(4) 0.7943(2) 0.8383(2) 0.0962(9) Uani 1 1 d . . . . .
F2 F 0.7369(4) 0.8809(2) 0.7361(3) 0.0985(9) Uani 1 1 d . . . . .
F3 F 0.5452(3) 0.7721(3) 0.6882(3) 0.1104(11) Uani 1 1 d . . . . .
O1 O 0.26683(17) 0.47403(15) 0.65358(14) 0.0409(4) Uani 1 1 d . . . . .
O2 O 0.1499(2) 0.49989(17) 0.46795(15) 0.0479(4) Uani 1 1 d . . . . .
O3 O 0.08658(18) 0.27509(16) 0.61548(15) 0.0440(4) Uani 1 1 d . . . . .
O4 O -0.01471(18) 0.12264(15) 0.42006(14) 0.0431(4) Uani 1 1 d . . . . .
O5 O 0.38850(17) 0.33732(16) 0.74005(15) 0.0429(4) Uani 1 1 d . . . . .
O6 O 0.51459(19) 0.26835(18) 0.62467(16) 0.0483(4) Uani 1 1 d . . . . .
O7 O 0.6233(3) 0.5766(2) 0.6760(2) 0.0718(6) Uani 1 1 d . U . . .
O8 O 0.8383(2) 0.7021(2) 0.7179(2) 0.0725(7) Uani 1 1 d . U . . .
O9 O 0.6670(3) 0.6692(2) 0.5518(2) 0.0690(6) Uani 1 1 d . U . . .
N1 N 0.3147(2) 0.55361(19) 0.88794(18) 0.0437(5) Uani 1 1 d . . . . .
N2 N 0.0688(2) 0.36404(19) 0.81896(17) 0.0409(4) Uani 1 1 d . . . . .
N3 N 0.2980(2) 0.32758(19) 0.91009(18) 0.0433(5) Uani 1 1 d . . . . .
C1 C 0.2285(3) 0.5174(3) 1.1285(2) 0.0506(6) Uani 1 1 d . . . . .
H1A H 0.316262 0.547371 1.184259 0.076 Uiso 1 1 calc R U . . .
H1B H 0.174108 0.457581 1.143073 0.076 Uiso 1 1 calc R U . . .
H1C H 0.193740 0.576926 1.131604 0.076 Uiso 1 1 calc R U . . .
C2 C 0.2308(3) 0.4705(2) 1.0127(2) 0.0433(5) Uani 1 1 d . . . . .
C3 C 0.3358(3) 0.5609(2) 1.0023(2) 0.0448(5) Uani 1 1 d . . . . .
H3A H 0.340220 0.635135 1.045007 0.054 Uiso 1 1 calc R U . . .
H3B H 0.420041 0.554866 1.035796 0.054 Uiso 1 1 calc R U . . .
C4 C 0.0944(2) 0.4418(2) 0.9276(2) 0.0435(5) Uani 1 1 d . . . . .
H4A H 0.029598 0.408818 0.955569 0.052 Uiso 1 1 calc R U . . .
H4B H 0.084849 0.511405 0.920159 0.052 Uiso 1 1 calc R U . . .
C5 C 0.2607(3) 0.3643(2) 1.0047(2) 0.0471(6) Uani 1 1 d . . . . .
H5A H 0.331527 0.378049 1.073896 0.057 Uiso 1 1 calc R U . . .
H5B H 0.183827 0.303984 0.997023 0.057 Uiso 1 1 calc R U . . .
C6 C 0.3278(3) 0.6444(2) 0.8697(2) 0.0459(5) Uani 1 1 d . . . . .
H6 H 0.361057 0.710410 0.933039 0.055 Uiso 1 1 calc R U . . .
C7 C 0.2981(3) 0.6591(2) 0.7636(2) 0.0445(5) Uani 1 1 d . . . . .
C8 C 0.2993(3) 0.7657(2) 0.7655(3) 0.0523(6) Uani 1 1 d . . . . .
H8 H 0.331730 0.825274 0.834476 0.063 Uiso 1 1 calc R U . . .
C9 C 0.2543(3) 0.7845(2) 0.6696(3) 0.0532(6) Uani 1 1 d . . . . .
H9 H 0.258697 0.857339 0.671989 0.064 Uiso 1 1 calc R U . . .
C10 C 0.2020(3) 0.6965(3) 0.5680(2) 0.0488(6) Uani 1 1 d . . . . .
H10 H 0.166007 0.708554 0.501638 0.059 Uiso 1 1 calc R U . . .
C11 C 0.2024(2) 0.5924(2) 0.5640(2) 0.0430(5) Uani 1 1 d . . . . .
C12 C 0.2580(2) 0.5712(2) 0.6619(2) 0.0400(5) Uani 1 1 d . . . . .
C13 C 0.0809(3) 0.5130(3) 0.3686(2) 0.0539(6) Uani 1 1 d . . . . .
H13A H 0.039923 0.440553 0.307709 0.081 Uiso 1 1 calc R U . . .
H13B H 0.140828 0.565378 0.350599 0.081 Uiso 1 1 calc R U . . .
H13C H 0.014713 0.541911 0.379539 0.081 Uiso 1 1 calc R U . . .
C14 C -0.0302(2) 0.2724(2) 0.7794(2) 0.0414(5) Uani 1 1 d . . . . .
H14 H -0.079122 0.262573 0.823879 0.050 Uiso 1 1 calc R U . . .
C15 C -0.0739(2) 0.1832(2) 0.6744(2) 0.0399(5) Uani 1 1 d . . . . .
C16 C -0.1800(2) 0.0858(2) 0.6486(2) 0.0446(5) Uani 1 1 d . . . . .
H16 H -0.217446 0.079639 0.701579 0.054 Uiso 1 1 calc R U . . .
C17 C -0.2295(3) 0.0006(2) 0.5489(2) 0.0490(6) Uani 1 1 d . . . . .
H17 H -0.299794 -0.064686 0.533725 0.059 Uiso 1 1 calc R U . . .
C18 C -0.1770(3) 0.0090(2) 0.4686(2) 0.0458(5) Uani 1 1 d . . . . .
H18 H -0.212812 -0.049626 0.398644 0.055 Uiso 1 1 calc R U . . .
C19 C -0.0725(2) 0.1033(2) 0.4921(2) 0.0399(5) Uani 1 1 d . . . . .
C20 C -0.0153(2) 0.1909(2) 0.5967(2) 0.0385(5) Uani 1 1 d . . . . .
C21 C -0.0601(3) 0.0355(2) 0.3153(2) 0.0472(6) Uani 1 1 d . . . . .
H21A H -0.149324 0.023692 0.272800 0.071 Uiso 1 1 calc R U . . .
H21B H -0.056056 -0.033432 0.326554 0.071 Uiso 1 1 calc R U . . .
H21C H -0.006037 0.056463 0.274761 0.071 Uiso 1 1 calc R U . . .
C22 C 0.3426(3) 0.2493(2) 0.9083(2) 0.0435(5) Uani 1 1 d . . . . .
H22 H 0.339737 0.217013 0.962891 0.052 Uiso 1 1 calc R U . . .
C23 C 0.3972(2) 0.2050(2) 0.8312(2) 0.0426(5) Uani 1 1 d . . . . .
C24 C 0.4376(3) 0.1160(2) 0.8415(2) 0.0497(6) Uani 1 1 d . . . . .
H24 H 0.421070 0.083441 0.893141 0.060 Uiso 1 1 calc R U . . .
C25 C 0.5002(3) 0.0757(3) 0.7785(3) 0.0556(7) Uani 1 1 d . . . . .
H25 H 0.524630 0.014409 0.785016 0.067 Uiso 1 1 calc R U . . .
C26 C 0.5278(3) 0.1256(3) 0.7043(3) 0.0519(6) Uani 1 1 d . . . . .
H26 H 0.572489 0.098882 0.661341 0.062 Uiso 1 1 calc R U . . .
C27 C 0.4907(2) 0.2127(2) 0.6934(2) 0.0442(5) Uani 1 1 d . . . . .
C28 C 0.4207(2) 0.2547(2) 0.7548(2) 0.0403(5) Uani 1 1 d . . . . .
C29 C 0.5907(3) 0.2372(3) 0.5656(3) 0.0630(8) Uani 1 1 d . . . . .
H29A H 0.544829 0.159710 0.514261 0.095 Uiso 1 1 calc R U . . .
H29B H 0.673047 0.244127 0.617925 0.095 Uiso 1 1 calc R U . . .
H29C H 0.606371 0.286161 0.524082 0.095 Uiso 1 1 calc R U . . .
C30 C 0.6676(4) 0.7863(3) 0.7365(3) 0.0600(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 Na1 3.4835(11) . ?
Mn1 Na2 3.4118(11) . ?
Mn1 O1 2.1771(18) . ?
Mn1 O3 2.0906(19) . ?
Mn1 O5 2.1014(18) . ?
Mn1 N1 2.193(2) . ?
Mn1 N2 2.272(2) . ?
Mn1 N3 2.294(2) . ?
S1 Na1 3.1168(12) 2_666 ?
S1 O7 1.403(3) . ?
S1 O8 1.459(3) . ?
S1 O9 1.426(2) . ?
S1 C30 1.833(3) . ?
Na1 Na2 3.3344(15) . ?
Na1 O1 2.443(2) . ?
Na1 O2 2.401(2) . ?
Na1 O3 2.230(2) . ?
Na1 O4 2.486(2) . ?
Na1 O8 2.746(3) 2_666 ?
Na1 O9 2.485(3) 2_666 ?
Na1 C20 3.126(3) . ?
Na2 O1 2.394(2) . ?
Na2 O5 2.250(2) . ?
Na2 O6 2.454(2) . ?
Na2 O7 2.258(3) . ?
Na2 O9 2.270(3) 2_666 ?
F1 C30 1.300(4) . ?
F2 C30 1.306(4) . ?
F3 C30 1.324(5) . ?
O1 C12 1.306(3) . ?
O2 C11 1.381(3) . ?
O2 C13 1.436(3) . ?
O3 C20 1.306(3) . ?
O4 C19 1.373(3) . ?
O4 C21 1.428(3) . ?
O5 C28 1.298(3) . ?
O6 C27 1.373(4) . ?
O6 C29 1.425(3) . ?
N1 C3 1.469(3) . ?
N1 C6 1.275(4) . ?
N2 C4 1.459(3) . ?
N2 C14 1.293(4) . ?
N3 C5 1.478(3) . ?
N3 C22 1.282(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.542(4) . ?
C2 C3 1.540(4) . ?
C2 C4 1.549(4) . ?
C2 C5 1.531(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6 0.9500 . ?
C6 C7 1.455(4) . ?
C7 C8 1.412(4) . ?
C7 C12 1.414(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.368(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.396(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.377(4) . ?
C11 C12 1.432(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14 0.9500 . ?
C14 C15 1.446(4) . ?
C15 C16 1.415(4) . ?
C15 C20 1.420(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.366(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.407(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(4) . ?
C19 C20 1.418(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.451(4) . ?
C23 C24 1.412(4) . ?
C23 C28 1.415(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.372(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.405(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.369(4) . ?
C27 C28 1.437(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Na2 Mn1 Na1 57.83(3) . . ?
O1 Mn1 Na1 44.02(5) . . ?
O1 Mn1 Na2 44.22(5) . . ?
O1 Mn1 N1 83.39(8) . . ?
O1 Mn1 N2 123.33(7) . . ?
O1 Mn1 N3 156.05(8) . . ?
O3 Mn1 Na1 37.65(5) . . ?
O3 Mn1 Na2 91.42(5) . . ?
O3 Mn1 O1 79.34(7) . . ?
O3 Mn1 O5 99.49(7) . . ?
O3 Mn1 N1 143.67(8) . . ?
O3 Mn1 N2 79.64(8) . . ?
O3 Mn1 N3 120.35(8) . . ?
O5 Mn1 Na1 82.68(5) . . ?
O5 Mn1 Na2 39.95(5) . . ?
O5 Mn1 O1 84.11(7) . . ?
O5 Mn1 N1 110.27(8) . . ?
O5 Mn1 N2 151.25(8) . . ?
O5 Mn1 N3 79.40(7) . . ?
N1 Mn1 Na1 125.31(6) . . ?
N1 Mn1 Na2 98.11(6) . . ?
N1 Mn1 N2 83.68(8) . . ?
N1 Mn1 N3 86.14(8) . . ?
N2 Mn1 Na1 110.31(6) . . ?
N2 Mn1 Na2 166.51(6) . . ?
N2 Mn1 N3 76.55(8) . . ?
N3 Mn1 Na1 147.82(6) . . ?
N3 Mn1 Na2 116.86(6) . . ?
O7 S1 Na1 130.71(12) . 2_666 ?
O7 S1 O8 115.56(19) . . ?
O7 S1 O9 117.21(18) . . ?
O7 S1 C30 103.98(16) . . ?
O8 S1 Na1 61.78(12) . 2_666 ?
O8 S1 C30 102.15(17) . . ?
O9 S1 Na1 51.19(12) . 2_666 ?
O9 S1 O8 111.46(18) . . ?
O9 S1 C30 104.21(15) . . ?
C30 S1 Na1 125.13(11) . 2_666 ?
S1 Na1 Mn1 126.61(4) 2_666 . ?
S1 Na1 Na2 66.81(3) 2_666 . ?
S1 Na1 C20 149.92(6) 2_666 . ?
Na2 Na1 Mn1 60.01(3) . . ?
O1 Na1 Mn1 38.27(4) . . ?
O1 Na1 S1 103.18(6) . 2_666 ?
O1 Na1 Na2 45.83(5) . . ?
O1 Na1 O4 136.73(7) . . ?
O1 Na1 O8 124.97(8) . 2_666 ?
O1 Na1 O9 85.89(8) . 2_666 ?
O1 Na1 C20 91.37(7) . . ?
O2 Na1 Mn1 100.90(6) . . ?
O2 Na1 S1 80.54(6) . 2_666 ?
O2 Na1 Na2 87.43(6) . . ?
O2 Na1 O1 66.30(7) . . ?
O2 Na1 O4 146.32(8) . . ?
O2 Na1 O8 77.84(8) . 2_666 ?
O2 Na1 O9 91.64(9) . 2_666 ?
O2 Na1 C20 129.54(8) . . ?
O3 Na1 Mn1 34.93(5) . . ?
O3 Na1 S1 149.41(7) . 2_666 ?
O3 Na1 Na2 91.05(6) . . ?
O3 Na1 O1 71.18(7) . . ?
O3 Na1 O2 120.97(8) . . ?
O3 Na1 O4 66.33(7) . . ?
O3 Na1 O8 160.65(9) . 2_666 ?
O3 Na1 O9 124.27(9) . 2_666 ?
O3 Na1 C20 20.73(7) . . ?
O4 Na1 Mn1 98.52(5) . . ?
O4 Na1 S1 108.99(6) . 2_666 ?
O4 Na1 Na2 126.20(6) . . ?
O4 Na1 O8 95.66(8) . 2_666 ?
O4 Na1 C20 47.47(6) . . ?
O8 Na1 Mn1 154.51(7) 2_666 . ?
O8 Na1 S1 27.92(5) 2_666 2_666 ?
O8 Na1 Na2 94.55(6) 2_666 . ?
O8 Na1 C20 143.03(8) 2_666 . ?
O9 Na1 Mn1 100.95(7) 2_666 . ?
O9 Na1 S1 26.55(6) 2_666 2_666 ?
O9 Na1 Na2 42.89(6) 2_666 . ?
O9 Na1 O4 111.35(9) 2_666 . ?
O9 Na1 O8 53.95(8) 2_666 2_666 ?
O9 Na1 C20 133.15(9) 2_666 . ?
C20 Na1 Mn1 55.65(5) . . ?
C20 Na1 Na2 109.17(6) . . ?
Na1 Na2 Mn1 62.16(3) . . ?
O1 Na2 Mn1 39.35(4) . . ?
O1 Na2 Na1 47.03(5) . . ?
O1 Na2 O6 136.80(8) . . ?
O5 Na2 Mn1 36.84(5) . . ?
O5 Na2 Na1 84.27(6) . . ?
O5 Na2 O1 76.15(7) . . ?
O5 Na2 O6 66.87(7) . . ?
O5 Na2 O7 128.95(10) . . ?
O5 Na2 O9 113.97(10) . 2_666 ?
O6 Na2 Mn1 101.69(6) . . ?
O6 Na2 Na1 105.98(6) . . ?
O7 Na2 Mn1 130.11(8) . . ?
O7 Na2 Na1 140.89(9) . . ?
O7 Na2 O1 114.19(10) . . ?
O7 Na2 O6 106.32(10) . . ?
O7 Na2 O9 115.31(11) . 2_666 ?
O9 Na2 Mn1 108.09(8) 2_666 . ?
O9 Na2 Na1 48.18(8) 2_666 . ?
O9 Na2 O1 92.04(9) 2_666 . ?
O9 Na2 O6 83.59(9) 2_666 . ?
Mn1 O1 Na1 97.72(7) . . ?
Mn1 O1 Na2 96.43(7) . . ?
Na2 O1 Na1 87.15(7) . . ?
C12 O1 Mn1 125.65(16) . . ?
C12 O1 Na1 117.12(15) . . ?
C12 O1 Na2 123.89(15) . . ?
C11 O2 Na1 119.51(15) . . ?
C11 O2 C13 116.6(2) . . ?
C13 O2 Na1 122.03(18) . . ?
Mn1 O3 Na1 107.41(8) . . ?
C20 O3 Mn1 130.45(16) . . ?
C20 O3 Na1 122.07(16) . . ?
C19 O4 Na1 113.74(15) . . ?
C19 O4 C21 117.4(2) . . ?
C21 O4 Na1 127.94(16) . . ?
Mn1 O5 Na2 103.21(8) . . ?
C28 O5 Mn1 129.91(16) . . ?
C28 O5 Na2 124.44(16) . . ?
C27 O6 Na2 116.87(16) . . ?
C27 O6 C29 117.1(2) . . ?
C29 O6 Na2 125.57(19) . . ?
S1 O7 Na2 155.7(2) . . ?
S1 O8 Na1 90.30(13) . 2_666 ?
S1 O9 Na1 102.25(15) . 2_666 ?
S1 O9 Na2 147.58(19) . 2_666 ?
Na2 O9 Na1 88.93(9) 2_666 2_666 ?
C3 N1 Mn1 116.12(17) . . ?
C6 N1 Mn1 126.78(19) . . ?
C6 N1 C3 116.5(2) . . ?
C4 N2 Mn1 116.12(16) . . ?
C14 N2 Mn1 123.61(17) . . ?
C14 N2 C4 116.7(2) . . ?
C5 N3 Mn1 119.44(16) . . ?
C22 N3 Mn1 124.15(18) . . ?
C22 N3 C5 115.2(2) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C4 107.0(2) . . ?
C3 C2 C1 107.4(2) . . ?
C3 C2 C4 112.9(2) . . ?
C5 C2 C1 107.4(2) . . ?
C5 C2 C3 111.9(2) . . ?
C5 C2 C4 110.0(2) . . ?
N1 C3 C2 114.0(2) . . ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N2 C4 C2 112.8(2) . . ?
N2 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C2 C4 H4A 109.0 . . ?
C2 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N3 C5 C2 112.3(2) . . ?
N3 C5 H5A 109.1 . . ?
N3 C5 H5B 109.1 . . ?
C2 C5 H5A 109.1 . . ?
C2 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
N1 C6 H6 116.1 . . ?
N1 C6 C7 127.9(2) . . ?
C7 C6 H6 116.1 . . ?
C8 C7 C6 115.9(2) . . ?
C8 C7 C12 120.3(3) . . ?
C12 C7 C6 123.5(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 120.9(3) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 119.9(3) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10 120.0 . . ?
O2 C11 C12 114.0(2) . . ?
C10 C11 O2 124.2(2) . . ?
C10 C11 C12 121.8(3) . . ?
O1 C12 C7 123.9(2) . . ?
O1 C12 C11 119.8(2) . . ?
C7 C12 C11 116.3(2) . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14 116.7 . . ?
N2 C14 C15 126.6(2) . . ?
C15 C14 H14 116.7 . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 C20 119.4(2) . . ?
C20 C15 C14 122.4(2) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 C15 121.2(2) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.7(2) . . ?
C19 C18 H18 120.2 . . ?
O4 C19 C18 125.2(2) . . ?
O4 C19 C20 113.5(2) . . ?
C18 C19 C20 121.3(2) . . ?
O3 C20 Na1 37.20(11) . . ?
O3 C20 C15 123.6(2) . . ?
O3 C20 C19 118.4(2) . . ?
C15 C20 Na1 153.90(18) . . ?
C19 C20 Na1 83.72(15) . . ?
C19 C20 C15 118.0(2) . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22 116.7 . . ?
N3 C22 C23 126.6(2) . . ?
C23 C22 H22 116.7 . . ?
C24 C23 C22 117.6(2) . . ?
C24 C23 C28 120.2(3) . . ?
C28 C23 C22 121.9(2) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 120.3 . . ?
C24 C25 C26 119.5(3) . . ?
C26 C25 H25 120.3 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.3(3) . . ?
C27 C26 H26 119.8 . . ?
O6 C27 C28 113.2(2) . . ?
C26 C27 O6 124.9(3) . . ?
C26 C27 C28 121.9(3) . . ?
O5 C28 C23 124.8(2) . . ?
O5 C28 C27 118.5(2) . . ?
C23 C28 C27 116.6(2) . . ?
O6 C29 H29A 109.5 . . ?
O6 C29 H29B 109.5 . . ?
O6 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F1 C30 S1 111.7(3) . . ?
F1 C30 F2 108.8(3) . . ?
F1 C30 F3 107.5(3) . . ?
F2 C30 S1 112.1(2) . . ?
F2 C30 F3 107.1(3) . . ?
F3 C30 S1 109.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O1 C12 C7 36.6(3) . . . . ?
Mn1 O1 C12 C11 -141.97(19) . . . . ?
Mn1 O3 C20 Na1 -176.9(3) . . . . ?
Mn1 O3 C20 C15 27.9(4) . . . . ?
Mn1 O3 C20 C19 -153.52(18) . . . . ?
Mn1 O5 C28 C23 -27.8(4) . . . . ?
Mn1 O5 C28 C27 155.28(18) . . . . ?
Mn1 N1 C3 C2 -38.6(3) . . . . ?
Mn1 N1 C6 C7 -1.5(4) . . . . ?
Mn1 N2 C4 C2 -36.6(3) . . . . ?
Mn1 N2 C14 C15 -21.9(4) . . . . ?
Mn1 N3 C5 C2 -22.0(3) . . . . ?
Mn1 N3 C22 C23 18.7(4) . . . . ?
Na1 S1 O7 Na2 -82.6(5) 2_666 . . . ?
Na1 S1 O9 Na2 107.8(3) 2_666 . . 2_666 ?
Na1 S1 C30 F1 -130.2(3) 2_666 . . . ?
Na1 S1 C30 F2 -7.7(4) 2_666 . . . ?
Na1 S1 C30 F3 110.9(3) 2_666 . . . ?
Na1 O1 C12 C7 160.21(19) . . . . ?
Na1 O1 C12 C11 -18.4(3) . . . . ?
Na1 O2 C11 C10 -170.7(2) . . . . ?
Na1 O2 C11 C12 8.9(3) . . . . ?
Na1 O3 C20 C15 -155.21(19) . . . . ?
Na1 O3 C20 C19 23.4(3) . . . . ?
Na1 O4 C19 C18 165.3(2) . . . . ?
Na1 O4 C19 C20 -14.5(2) . . . . ?
Na2 O1 C12 C7 -93.7(3) . . . . ?
Na2 O1 C12 C11 87.7(3) . . . . ?
Na2 O5 C28 C23 173.05(18) . . . . ?
Na2 O5 C28 C27 -3.9(3) . . . . ?
Na2 O6 C27 C26 -176.8(2) . . . . ?
Na2 O6 C27 C28 3.4(3) . . . . ?
O2 C11 C12 O1 6.6(3) . . . . ?
O2 C11 C12 C7 -172.1(2) . . . . ?
O4 C19 C20 Na1 10.56(18) . . . . ?
O4 C19 C20 O3 -3.4(3) . . . . ?
O4 C19 C20 C15 175.3(2) . . . . ?
O6 C27 C28 O5 -0.1(3) . . . . ?
O6 C27 C28 C23 -177.3(2) . . . . ?
O7 S1 O8 Na1 124.32(15) . . . 2_666 ?
O7 S1 O9 Na1 -121.85(17) . . . 2_666 ?
O7 S1 O9 Na2 -14.0(4) . . . 2_666 ?
O7 S1 C30 F1 54.3(3) . . . . ?
O7 S1 C30 F2 176.7(3) . . . . ?
O7 S1 C30 F3 -64.6(3) . . . . ?
O8 S1 O7 Na2 -156.3(4) . . . . ?
O8 S1 O9 Na1 14.48(18) . . . 2_666 ?
O8 S1 O9 Na2 122.3(3) . . . 2_666 ?
O8 S1 C30 F1 -66.3(3) . . . . ?
O8 S1 C30 F2 56.2(3) . . . . ?
O8 S1 C30 F3 174.8(3) . . . . ?
O9 S1 O7 Na2 -21.7(5) . . . . ?
O9 S1 O8 Na1 -12.78(16) . . . 2_666 ?
O9 S1 C30 F1 177.6(3) . . . . ?
O9 S1 C30 F2 -60.0(3) . . . . ?
O9 S1 C30 F3 58.7(3) . . . . ?
N1 C6 C7 C8 168.7(3) . . . . ?
N1 C6 C7 C12 -5.3(5) . . . . ?
N2 C14 C15 C16 176.0(2) . . . . ?
N2 C14 C15 C20 -4.8(4) . . . . ?
N3 C22 C23 C24 -178.2(3) . . . . ?
N3 C22 C23 C28 7.6(4) . . . . ?
C1 C2 C3 N1 -154.3(2) . . . . ?
C1 C2 C4 N2 -160.8(2) . . . . ?
C1 C2 C5 N3 -165.4(2) . . . . ?
C3 N1 C6 C7 -172.0(3) . . . . ?
C3 C2 C4 N2 81.3(3) . . . . ?
C3 C2 C5 N3 -47.8(3) . . . . ?
C4 N2 C14 C15 -179.7(2) . . . . ?
C4 C2 C3 N1 -36.6(3) . . . . ?
C4 C2 C5 N3 78.5(3) . . . . ?
C5 N3 C22 C23 -173.9(2) . . . . ?
C5 C2 C3 N1 88.2(3) . . . . ?
C5 C2 C4 N2 -44.5(3) . . . . ?
C6 N1 C3 C2 132.9(3) . . . . ?
C6 C7 C8 C9 -170.1(3) . . . . ?
C6 C7 C12 O1 -13.7(4) . . . . ?
C6 C7 C12 C11 165.0(2) . . . . ?
C7 C8 C9 C10 2.4(5) . . . . ?
C8 C7 C12 O1 172.6(2) . . . . ?
C8 C7 C12 C11 -8.7(4) . . . . ?
C8 C9 C10 C11 -3.8(5) . . . . ?
C9 C10 C11 O2 178.3(3) . . . . ?
C9 C10 C11 C12 -1.3(4) . . . . ?
C10 C11 C12 O1 -173.8(2) . . . . ?
C10 C11 C12 C7 7.5(4) . . . . ?
C12 C7 C8 C9 4.1(4) . . . . ?
C13 O2 C11 C10 -6.0(4) . . . . ?
C13 O2 C11 C12 173.7(2) . . . . ?
C14 N2 C4 C2 122.9(3) . . . . ?
C14 C15 C16 C17 177.2(2) . . . . ?
C14 C15 C20 Na1 -31.0(5) . . . . ?
C14 C15 C20 O3 4.2(4) . . . . ?
C14 C15 C20 C19 -174.4(2) . . . . ?
C15 C16 C17 C18 -1.1(4) . . . . ?
C16 C15 C20 Na1 148.2(3) . . . . ?
C16 C15 C20 O3 -176.6(2) . . . . ?
C16 C15 C20 C19 4.8(3) . . . . ?
C16 C17 C18 C19 1.5(4) . . . . ?
C17 C18 C19 O4 -178.4(2) . . . . ?
C17 C18 C19 C20 1.5(4) . . . . ?
C18 C19 C20 Na1 -169.3(2) . . . . ?
C18 C19 C20 O3 176.8(2) . . . . ?
C18 C19 C20 C15 -4.6(4) . . . . ?
C20 C15 C16 C17 -2.1(4) . . . . ?
C21 O4 C19 C18 -4.5(4) . . . . ?
C21 O4 C19 C20 175.7(2) . . . . ?
C22 N3 C5 C2 170.0(2) . . . . ?
C22 C23 C24 C25 -174.3(3) . . . . ?
C22 C23 C28 O5 -5.2(4) . . . . ?
C22 C23 C28 C27 171.8(2) . . . . ?
C23 C24 C25 C26 1.7(5) . . . . ?
C24 C23 C28 O5 -179.3(2) . . . . ?
C24 C23 C28 C27 -2.3(4) . . . . ?
C24 C25 C26 C27 -1.1(5) . . . . ?
C25 C26 C27 O6 179.0(3) . . . . ?
C25 C26 C27 C28 -1.3(4) . . . . ?
C26 C27 C28 O5 -179.9(2) . . . . ?
C26 C27 C28 C23 2.9(4) . . . . ?
C28 C23 C24 C25 0.1(4) . . . . ?
C29 O6 C27 C26 -4.1(4) . . . . ?
C29 O6 C27 C28 176.1(3) . . . . ?
C30 S1 O7 Na2 92.6(5) . . . . ?
C30 S1 O8 Na1 -123.54(12) . . . 2_666 ?
C30 S1 O9 Na1 123.92(15) . . . 2_666 ?
C30 S1 O9 Na2 -128.2(3) . . . 2_666 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.793 0.000 0.000 282.2 82.1 '4 acetonitrile'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_original_sample_id exp_603
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.758
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_548
_database_code_depnum_ccdc_archive 'CCDC 2307062'
loop_
_audit_author_name
_audit_author_address
'Rebecca A. Musgrave'
;Kings College London
United Kingdom
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_audit_creation_date             2023-08-22
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_chemical_formula_moiety         'C33 H33 F6 La Mn N4 O12 S2'
_chemical_formula_sum            'C33 H33 F6 La Mn N4 O12 S2'
_chemical_formula_weight         1049.616
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
La -1.32533 9.78168 20.57800 19.59900 11.37270 3.28719 2.94817 0.24448 18.77260
133.12399 2.14678001404
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Mn -0.54371 2.83629 11.28190 7.35730 3.01930 2.24410 5.34090 0.34320 17.86740
83.75430 1.089599967
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.33537 0.55136 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.07537 0.05506 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   16.0537(2)
_cell_length_b                   13.0153(2)
_cell_length_c                   19.0750(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.748(1)
_cell_angle_gamma                90
_cell_volume                     3928.06(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8588
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.0810
_cell_measurement_theta_min      4.1400
_exptl_absorpt_coefficient_mu    12.744
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             2098.393
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 -1 4 0.1700
7 -6 -4 0.1610
-3 7 6 0.2132
-9 2 -3 0.1682
3 -8 2 0.1954
-2 -7 -6 0.1781
-1 8 1 0.2389
-6 3 -8 0.1726
2 8 -2 0.2324
3 1 11 0.1782
-2 3 -11 0.1728
-3 -8 -2 0.1848
6 6 -6 0.1927
4 2 -12 0.1599
-6 -5 9 0.1619
-1 1 12 0.1441
-6 -7 3 0.1843
10 1 -1 0.1692
8 -3 -8 0.1512
-10 -2 0 0.1623
9 1 -7 0.1487
5 -3 -11 0.1308
-6 2 10 0.1666
-9 -1 7 0.1512
1 -8 2 0.1835
-1 -3 12 0.1659
3 7 -7 0.2153
1 4 -11 0.1660
-1 -1 -12 0.1931
-3 -6 9 0.1675
-4 -8 2 0.1782
-7 -5 6 0.1584
-5 -3 11 0.1533
6 3 -10 0.1536
3 0 -12 0.1663
6 0 -11 0.1516
8 4 -6 0.1626
-6 -5 -6 0.1854
-3 5 10 0.1838
10 -1 -7 0.1479
-9 1 7 0.1464
10 -1 1 0.1612
9 -4 -4 0.1547
5 -6 -7 0.1618
-7 5 6 0.1864
-8 -3 -5 0.1728
2 -8 -4 0.1761
7 -1 7 0.1697
-7 3 -6 0.1801
3 -2 11 0.1669
-1 -5 10 0.1660
-3 -8 4 0.1736
-8 0 10 0.1521

_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9794
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14963
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9794
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         71.97
_diffrn_reflns_theta_min         3.33
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9794
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00 -65.00   1.00    2.50    --  -33.50 -57.00 -30.00   28
  2  ω    -44.00 -19.00   1.00    2.50    --  -33.50 -57.00 -30.00   25
  3  ω   -104.00 -74.00   1.00    2.50    --  -33.50-178.00-150.00   30
  4  ω     23.00  58.00   1.00    2.50    --   36.21  57.00 120.00   35
  5  ω    -30.00  36.00   1.00    2.50    --   36.21 -19.00-150.00   66
  6  ω     35.00  75.00   1.00    2.50    --   36.21 -99.00   0.00   40
  7  ω     61.00 101.00   1.00    2.50    --   36.21  57.00 120.00   40
  8  ω     27.00  75.00   1.00    2.50    --   36.21 -99.00 150.00   48
  9  ω     72.00  99.00   1.00    2.50    --   36.21 178.00 -30.00   27
 10  ω     52.00 116.00   1.00   10.00    --  108.00 -45.00   0.00   64
 11  ω    109.00 172.00   1.00   10.00    --  108.00 111.00-180.00   63
 12  ω    106.00 176.00   1.00   10.00    --  108.00  77.00 -90.00   70
 13  ω     69.00 117.00   1.00   10.00    --  108.00 -45.00 150.00   48
 14  ω     39.00  90.00   1.00   10.00    --  108.00 -94.00-180.00   51
 15  ω    103.00 128.00   1.00   10.00    --  108.00 -30.00 150.00   25
 16  ω     40.00  66.00   1.00   10.00    --  108.00 -45.00 150.00   26
 17  ω     46.00  72.00   1.00   10.00    --  108.00 -30.00 150.00   26
 18  ω    105.00 176.00   1.00   10.00    --  108.00  45.00-120.00   71
 19  ω    107.00 172.00   1.00   10.00    --  108.00  30.00-180.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -19
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -13
_reflns_number_gt                6973
_reflns_number_total             7564
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.1310
_refine_diff_density_min         -1.5581
_refine_diff_density_rms         0.1207
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             13.2620
_refine_ls_goodness_of_fit_ref   1.0491
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.0491
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0585P)²+0.9443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0952
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18),
 C22(H22), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C13(H13a,H13b,H13c), C21(H21a,H21b,H21c), C29(H29a,H29b,
 H29c), C31(H31a,H31b,H31c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
La1 La 0.428022(10) 0.677283(14) 0.724951(8) 0.01758(7) Uani 1.000000 .
Mn1 Mn 0.32552(3) 0.58504(4) 0.56702(2) 0.01730(11) Uani 1.000000 .
S1 S 0.49495(5) 0.75280(6) 0.92625(4) 0.02124(16) Uani 1.000000 .
S2 S 0.62707(5) 0.74823(8) 0.71816(5) 0.02977(19) Uani 1.000000 .
F1 F 0.44514(17) 0.58303(17) 0.98036(13) 0.0398(5) Uani 1.000000 .
F2 F 0.34692(15) 0.6955(2) 0.95450(14) 0.0428(6) Uani 1.000000 .
F3 F 0.44295(18) 0.7151(2) 1.04682(12) 0.0453(6) Uani 1.000000 .
F4 F 0.6977(2) 0.8310(2) 0.61882(17) 0.0549(8) Uani 1.000000 .
F5 F 0.57879(18) 0.8993(3) 0.62897(17) 0.0596(8) Uani 1.000000 .
F6 F 0.6902(2) 0.9316(2) 0.70507(19) 0.0645(8) Uani 1.000000 .
O1 O 0.42882(14) 0.53454(18) 0.64562(12) 0.0222(5) Uani 1.000000 .
O2 O 0.53789(14) 0.52137(19) 0.76217(12) 0.0247(5) Uani 1.000000 .
O3 O 0.38831(15) 0.72860(18) 0.59788(12) 0.0223(5) Uani 1.000000 .
O4 O 0.41860(15) 0.87470(19) 0.69015(12) 0.0251(5) Uani 1.000000 .
O5 O 0.28659(14) 0.6239(2) 0.66740(12) 0.0241(5) Uani 1.000000 .
O6 O 0.28140(15) 0.7555(2) 0.76908(12) 0.0251(5) Uani 1.000000 .
O7 O 0.46017(16) 0.7178(2) 0.85497(12) 0.0274(5) Uani 1.000000 .
O8 O 0.47799(18) 0.8595(2) 0.93752(15) 0.0345(6) Uani 1.000000 .
O9 O 0.57874(16) 0.7162(2) 0.95240(14) 0.0331(6) Uani 1.000000 .
O10 O 0.57451(19) 0.6837(2) 0.66737(17) 0.0395(7) Uani 1.000000 .
O11 O 0.57757(17) 0.7882(3) 0.76900(14) 0.0391(7) Uani 1.000000 .
O12 O 0.70972(18) 0.7116(3) 0.74745(18) 0.0464(7) Uani 1.000000 .
N1 N 0.36676(18) 0.4582(2) 0.50634(15) 0.0262(6) Uani 1.000000 .
N2 N 0.27872(18) 0.6674(2) 0.46734(15) 0.0231(6) Uani 1.000000 .
N3 N 0.19746(18) 0.5206(2) 0.54547(14) 0.0229(6) Uani 1.000000 .
N4 N 0.3694(2) 0.5294(2) 0.80531(15) 0.0282(6) Uani 1.000000 .
C1 C 0.1821(2) 0.4415(3) 0.35222(18) 0.0314(8) Uani 1.000000 .
H1a H 0.1682(18) 0.3699(8) 0.3611(4) 0.0472(12) Uiso 1.000000 GR
H1b H 0.1300(11) 0.4798(16) 0.3354(9) 0.0472(12) Uiso 1.000000 GR
H1c H 0.2187(8) 0.444(2) 0.3160(6) 0.0472(12) Uiso 1.000000 GR
C2 C 0.2286(2) 0.4904(3) 0.42188(17) 0.0238(7) Uani 1.000000 .
C3 C 0.3191(2) 0.4482(3) 0.43308(19) 0.0319(8) Uani 1.000000 .
H3a H 0.3508(2) 0.4845(3) 0.40025(19) 0.0383(10) Uiso 1.000000 R
H3b H 0.3168(2) 0.3746(3) 0.41984(19) 0.0383(10) Uiso 1.000000 R
C4 C 0.2268(2) 0.6071(3) 0.40988(17) 0.0278(7) Uani 1.000000 .
H4a H 0.1675(2) 0.6309(3) 0.40467(17) 0.0333(9) Uiso 1.000000 R
H4b H 0.2469(2) 0.6216(3) 0.36458(17) 0.0333(9) Uiso 1.000000 R
C5 C 0.1789(2) 0.4590(3) 0.48004(18) 0.0292(8) Uani 1.000000 .
H5a H 0.1912(2) 0.3860(3) 0.49226(18) 0.0350(9) Uiso 1.000000 R
H5b H 0.1178(2) 0.4644(3) 0.46087(18) 0.0350(9) Uiso 1.000000 R
C6 C 0.4222(2) 0.3894(3) 0.5268(2) 0.0292(7) Uani 1.000000 .
H6 H 0.4270(2) 0.3360(3) 0.4938(2) 0.0350(9) Uiso 1.000000 R
C7 C 0.4792(2) 0.3832(3) 0.59492(19) 0.0257(7) Uani 1.000000 .
C8 C 0.5363(2) 0.3003(3) 0.6058(2) 0.0308(8) Uani 1.000000 .
H8 H 0.5346(2) 0.2498(3) 0.5696(2) 0.0370(9) Uiso 1.000000 R
C9 C 0.5947(2) 0.2903(3) 0.6674(2) 0.0323(8) Uani 1.000000 .
H9 H 0.6325(2) 0.2335(3) 0.6733(2) 0.0387(10) Uiso 1.000000 R
C10 C 0.5981(2) 0.3638(3) 0.72093(19) 0.0264(7) Uani 1.000000 .
H10 H 0.6388(2) 0.3583(3) 0.76314(19) 0.0317(8) Uiso 1.000000 R
C11 C 0.54191(19) 0.4445(3) 0.71207(17) 0.0220(6) Uani 1.000000 .
C12 C 0.48086(19) 0.4563(3) 0.64970(17) 0.0211(6) Uani 1.000000 .
C13 C 0.5960(3) 0.5143(3) 0.8277(2) 0.0372(9) Uani 1.000000 .
H13a H 0.6540(3) 0.517(3) 0.8180(3) 0.0558(13) Uiso 1.000000 GR
H13b H 0.5867(15) 0.5717(16) 0.8587(8) 0.0558(13) Uiso 1.000000 GR
H13c H 0.5872(15) 0.4492(13) 0.8513(9) 0.0558(13) Uiso 1.000000 GR
C14 C 0.2817(2) 0.7636(3) 0.45595(17) 0.0237(7) Uani 1.000000 .
H14 H 0.2557(2) 0.7868(3) 0.41024(17) 0.0284(8) Uiso 1.000000 R
C15 C 0.3208(2) 0.8420(3) 0.50541(18) 0.0238(7) Uani 1.000000 .
C16 C 0.3059(3) 0.9446(3) 0.4845(2) 0.0359(9) Uani 1.000000 .
H16 H 0.2785(3) 0.9588(3) 0.4374(2) 0.0431(10) Uiso 1.000000 R
C17 C 0.3297(3) 1.0255(3) 0.5302(2) 0.0406(9) Uani 1.000000 .
H17 H 0.3199(3) 1.0943(3) 0.5143(2) 0.0487(11) Uiso 1.000000 R
C18 C 0.3683(3) 1.0056(3) 0.5997(2) 0.0365(9) Uani 1.000000 .
H18 H 0.3835(3) 1.0604(3) 0.6322(2) 0.0438(10) Uiso 1.000000 R
C19 C 0.3843(2) 0.9045(3) 0.62103(18) 0.0247(7) Uani 1.000000 .
C20 C 0.3654(2) 0.8200(3) 0.57426(18) 0.0209(7) Uani 1.000000 .
C21 C 0.4408(3) 0.9573(3) 0.7405(2) 0.0318(8) Uani 1.000000 .
H21a H 0.3902(5) 0.9976(15) 0.7443(13) 0.0478(12) Uiso 1.000000 GR
H21b H 0.4644(19) 0.9286(3) 0.7871(4) 0.0478(12) Uiso 1.000000 GR
H21c H 0.4829(15) 1.0018(14) 0.7241(9) 0.0478(12) Uiso 1.000000 GR
C22 C 0.1341(2) 0.5538(3) 0.57152(17) 0.0221(6) Uani 1.000000 .
H22 H 0.0798(2) 0.5352(3) 0.54676(17) 0.0266(8) Uiso 1.000000 R
C23 C 0.1360(2) 0.6164(3) 0.63447(17) 0.0205(6) Uani 1.000000 .
C24 C 0.0576(2) 0.6464(3) 0.65135(19) 0.0258(7) Uani 1.000000 .
H24 H 0.0070(2) 0.6230(3) 0.62260(19) 0.0310(8) Uiso 1.000000 R
C25 C 0.0526(2) 0.7090(3) 0.7086(2) 0.0304(8) Uani 1.000000 .
H25 H -0.0011(2) 0.7266(3) 0.7197(2) 0.0365(9) Uiso 1.000000 R
C26 C 0.1262(2) 0.7467(3) 0.75036(19) 0.0273(7) Uani 1.000000 .
H26 H 0.1227(2) 0.7912(3) 0.78926(19) 0.0327(8) Uiso 1.000000 R
C27 C 0.2044(2) 0.7188(3) 0.73472(17) 0.0233(7) Uani 1.000000 .
C28 C 0.2110(2) 0.6502(3) 0.67805(16) 0.0195(6) Uani 1.000000 .
C29 C 0.2772(3) 0.8359(3) 0.8206(2) 0.0327(8) Uani 1.000000 .
H29a H 0.3346(3) 0.8578(18) 0.8411(13) 0.0491(13) Uiso 1.000000 GR
H29b H 0.2458(19) 0.8946(11) 0.7971(4) 0.0491(13) Uiso 1.000000 GR
H29c H 0.2485(19) 0.8101(8) 0.8584(10) 0.0491(13) Uiso 1.000000 GR
C30 C 0.3587(2) 0.4701(3) 0.84647(17) 0.0229(7) Uani 1.000000 .
C31 C 0.3459(3) 0.3950(3) 0.90013(19) 0.0319(8) Uani 1.000000 .
H31a H 0.2893(8) 0.3650(19) 0.8878(10) 0.0478(12) Uiso 1.000000 GR
H31b H 0.3884(13) 0.3405(14) 0.9022(12) 0.0478(12) Uiso 1.000000 GR
H31c H 0.351(2) 0.4287(6) 0.9466(4) 0.0478(12) Uiso 1.000000 GR
C32 C 0.4286(2) 0.6828(3) 0.97973(18) 0.0267(7) Uani 1.000000 .
C33 C 0.6486(2) 0.8583(3) 0.6648(2) 0.0344(8) Uani 1.000000 .


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 Mn1 3.3979(5) . ?
La1 S2 3.3496(8) . ?
La1 O1 2.398(2) . ?
La1 O2 2.703(2) . ?
La1 O3 2.491(2) . ?
La1 O4 2.652(3) . ?
La1 O5 2.449(2) . ?
La1 O6 2.821(2) . ?
La1 O7 2.502(2) . ?
La1 O10 2.760(3) . ?
La1 O11 2.805(3) . ?
La1 N4 2.726(3) . ?
Mn1 O1 2.142(2) . ?
Mn1 O3 2.157(2) . ?
Mn1 O5 2.172(2) . ?
Mn1 N1 2.182(3) . ?
Mn1 N2 2.201(3) . ?
Mn1 N3 2.194(3) . ?
S1 O7 1.453(2) . ?
S1 O8 1.438(3) . ?
S1 O9 1.435(3) . ?
S1 C32 1.836(4) . ?
S2 O10 1.442(3) . ?
S2 O11 1.450(3) . ?
S2 O12 1.431(3) . ?
S2 C33 1.824(4) . ?
F1 C32 1.326(4) . ?
F2 C32 1.328(5) . ?
F3 C32 1.329(4) . ?
F4 C33 1.323(5) . ?
F5 C33 1.322(5) . ?
F6 C33 1.332(5) . ?
O1 C12 1.311(4) . ?
O2 C11 1.392(4) . ?
O2 C13 1.431(4) . ?
O3 C20 1.303(4) . ?
O4 C19 1.395(4) . ?
O4 C21 1.445(4) . ?
O5 C28 1.310(4) . ?
O6 C27 1.383(4) . ?
O6 C29 1.444(4) . ?
N1 C3 1.481(4) . ?
N1 C6 1.277(5) . ?
N2 C4 1.485(4) . ?
N2 C14 1.272(5) . ?
N3 C5 1.471(4) . ?
N3 C22 1.280(5) . ?
N4 C30 1.134(5) . ?
C1 H1a 0.9800 . ?
C1 H1b 0.9800 . ?
C1 H1c 0.9800 . ?
C1 C2 1.547(4) . ?
C2 C3 1.534(5) . ?
C2 C4 1.535(5) . ?
C2 C5 1.529(5) . ?
C3 H3a 0.9900 . ?
C3 H3b 0.9900 . ?
C4 H4a 0.9900 . ?
C4 H4b 0.9900 . ?
C5 H5a 0.9900 . ?
C5 H5b 0.9900 . ?
C6 H6 0.9500 . ?
C6 C7 1.459(5) . ?
C7 C8 1.408(5) . ?
C7 C12 1.411(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.381(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.376(5) . ?
C11 C12 1.416(5) . ?
C13 H13a 0.9800 . ?
C13 H13b 0.9800 . ?
C13 H13c 0.9800 . ?
C14 H14 0.9500 . ?
C14 C15 1.458(5) . ?
C15 C16 1.402(5) . ?
C15 C20 1.415(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.388(5) . ?
C19 C20 1.416(5) . ?
C21 H21a 0.9800 . ?
C21 H21b 0.9800 . ?
C21 H21c 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.447(5) . ?
C23 C24 1.407(4) . ?
C23 C28 1.412(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.375(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.398(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(5) . ?
C27 C28 1.420(5) . ?
C29 H29a 0.9800 . ?
C29 H29b 0.9800 . ?
C29 H29c 0.9800 . ?
C30 C31 1.455(5) . ?
C31 H31a 0.9800 . ?
C31 H31b 0.9800 . ?
C31 H31c 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 La1 Mn1 112.647(17) . . ?
O1 La1 Mn1 38.76(5) . . ?
O1 La1 S2 94.71(6) . . ?
O2 La1 Mn1 99.45(5) . . ?
O2 La1 S2 68.46(6) . . ?
O2 La1 O1 60.73(7) . . ?
O3 La1 Mn1 39.31(6) . . ?
O3 La1 S2 88.69(6) . . ?
O3 La1 O1 67.76(8) . . ?
O3 La1 O2 120.33(7) . . ?
O4 La1 Mn1 97.00(5) . . ?
O4 La1 S2 74.79(6) . . ?
O4 La1 O1 126.80(7) . . ?
O4 La1 O2 143.14(7) . . ?
O4 La1 O3 60.14(7) . . ?
O5 La1 Mn1 39.59(5) . . ?
O5 La1 S2 151.50(5) . . ?
O5 La1 O1 66.49(8) . . ?
O5 La1 O2 114.77(8) . . ?
O5 La1 O3 64.83(8) . . ?
O5 La1 O4 98.81(8) . . ?
O6 La1 Mn1 95.10(5) . . ?
O6 La1 S2 139.61(6) . . ?
O6 La1 O1 124.20(7) . . ?
O6 La1 O2 137.13(7) . . ?
O6 La1 O3 96.00(7) . . ?
O6 La1 O4 73.13(7) . . ?
O6 La1 O5 58.60(7) . . ?
O7 La1 Mn1 160.19(6) . . ?
O7 La1 S2 86.69(6) . . ?
O7 La1 O1 140.05(8) . . ?
O7 La1 O2 83.22(8) . . ?
O7 La1 O3 152.10(9) . . ?
O7 La1 O4 92.14(8) . . ?
O7 La1 O5 121.60(8) . . ?
O7 La1 O6 70.77(7) . . ?
O10 La1 Mn1 88.58(7) . . ?
O10 La1 S2 24.99(6) . . ?
O10 La1 O1 71.12(8) . . ?
O10 La1 O2 64.24(8) . . ?
O10 La1 O3 72.52(9) . . ?
O10 La1 O4 83.53(8) . . ?
O10 La1 O5 128.17(8) . . ?
O10 La1 O6 156.64(8) . . ?
O10 La1 O7 109.96(9) . . ?
O11 La1 Mn1 135.13(5) . . ?
O11 La1 S2 25.33(6) . . ?
O11 La1 O1 119.47(8) . . ?
O11 La1 O2 79.65(9) . . ?
O11 La1 O3 102.63(8) . . ?
O11 La1 O4 65.55(9) . . ?
O11 La1 O5 164.05(9) . . ?
O11 La1 O6 116.10(8) . . ?
O11 La1 O7 64.68(8) . . ?
O11 La1 O10 50.21(9) . . ?
N4 La1 Mn1 95.02(6) . . ?
N4 La1 S2 129.71(7) . . ?
N4 La1 O1 81.19(9) . . ?
N4 La1 O2 66.06(9) . . ?
N4 La1 O3 132.91(8) . . ?
N4 La1 O4 144.55(9) . . ?
N4 La1 O5 70.72(9) . . ?
N4 La1 O6 72.68(9) . . ?
N4 La1 O7 67.94(9) . . ?
N4 La1 O10 130.07(9) . . ?
N4 La1 O11 123.66(9) . . ?
O1 Mn1 La1 44.48(6) . . ?
O3 Mn1 La1 47.02(6) . . ?
O3 Mn1 O1 78.71(9) . . ?
O5 Mn1 La1 45.94(6) . . ?
O5 Mn1 O1 76.04(9) . . ?
O5 Mn1 O3 75.43(9) . . ?
N1 Mn1 La1 126.34(8) . . ?
N1 Mn1 O1 82.57(10) . . ?
N1 Mn1 O3 129.06(10) . . ?
N1 Mn1 O5 143.35(11) . . ?
N2 Mn1 La1 129.56(8) . . ?
N2 Mn1 O1 149.84(10) . . ?
N2 Mn1 O3 83.63(10) . . ?
N2 Mn1 O5 122.74(10) . . ?
N2 Mn1 N1 90.01(11) . . ?
N3 Mn1 La1 126.80(7) . . ?
N3 Mn1 O1 127.14(10) . . ?
N3 Mn1 O3 139.64(10) . . ?
N3 Mn1 O5 81.60(9) . . ?
N3 Mn1 N1 88.30(11) . . ?
N3 Mn1 N2 81.51(11) . . ?
O8 S1 O7 112.96(16) . . ?
O9 S1 O7 114.23(16) . . ?
O9 S1 O8 117.32(17) . . ?
C32 S1 O7 101.38(15) . . ?
C32 S1 O8 104.68(17) . . ?
C32 S1 O9 103.89(17) . . ?
O10 S2 La1 53.98(12) . . ?
O11 S2 La1 55.85(13) . . ?
O11 S2 O10 109.49(18) . . ?
O12 S2 La1 136.09(15) . . ?
O12 S2 O10 117.8(2) . . ?
O12 S2 O11 115.79(18) . . ?
C33 S2 La1 120.67(13) . . ?
C33 S2 O10 103.12(19) . . ?
C33 S2 O11 105.6(2) . . ?
C33 S2 O12 103.22(19) . . ?
Mn1 O1 La1 96.76(9) . . ?
C12 O1 La1 129.5(2) . . ?
C12 O1 Mn1 133.6(2) . . ?
C11 O2 La1 117.57(18) . . ?
C13 O2 La1 125.3(2) . . ?
C13 O2 C11 117.0(3) . . ?
Mn1 O3 La1 93.67(9) . . ?
C20 O3 La1 126.3(2) . . ?
C20 O3 Mn1 127.2(2) . . ?
C19 O4 La1 120.2(2) . . ?
C21 O4 La1 123.9(2) . . ?
C21 O4 C19 115.7(3) . . ?
Mn1 O5 La1 94.47(8) . . ?
C28 O5 La1 132.1(2) . . ?
C28 O5 Mn1 127.6(2) . . ?
C27 O6 La1 117.28(19) . . ?
C29 O6 La1 127.0(2) . . ?
C29 O6 C27 115.6(3) . . ?
S1 O7 La1 167.34(16) . . ?
S2 O10 La1 101.03(15) . . ?
S2 O11 La1 98.82(16) . . ?
C3 N1 Mn1 114.4(2) . . ?
C6 N1 Mn1 128.8(2) . . ?
C6 N1 C3 116.7(3) . . ?
C4 N2 Mn1 116.5(2) . . ?
C14 N2 Mn1 127.5(2) . . ?
C14 N2 C4 115.3(3) . . ?
C5 N3 Mn1 114.6(2) . . ?
C22 N3 Mn1 125.4(2) . . ?
C22 N3 C5 116.9(3) . . ?
C30 N4 La1 167.6(3) . . ?
H1b C1 H1a 109.5 . . ?
H1c C1 H1a 109.5 . . ?
H1c C1 H1b 109.5 . . ?
C2 C1 H1a 109.5 . . ?
C2 C1 H1b 109.5 . . ?
C2 C1 H1c 109.5 . . ?
C3 C2 C1 106.3(3) . . ?
C4 C2 C1 106.5(3) . . ?
C4 C2 C3 111.6(3) . . ?
C5 C2 C1 106.1(3) . . ?
C5 C2 C3 113.7(3) . . ?
C5 C2 C4 112.0(3) . . ?
C2 C3 N1 115.2(3) . . ?
H3a C3 N1 108.5(2) . . ?
H3a C3 C2 108.5(2) . . ?
H3b C3 N1 108.5(2) . . ?
H3b C3 C2 108.5(2) . . ?
H3b C3 H3a 107.5 . . ?
C2 C4 N2 114.8(3) . . ?
H4a C4 N2 108.57(19) . . ?
H4a C4 C2 108.57(18) . . ?
H4b C4 N2 108.57(18) . . ?
H4b C4 C2 108.57(18) . . ?
H4b C4 H4a 107.5 . . ?
C2 C5 N3 114.4(3) . . ?
H5a C5 N3 108.7(2) . . ?
H5a C5 C2 108.7(2) . . ?
H5b C5 N3 108.65(19) . . ?
H5b C5 C2 108.65(18) . . ?
H5b C5 H5a 107.6 . . ?
H6 C6 N1 116.2(2) . . ?
C7 C6 N1 127.6(3) . . ?
C7 C6 H6 116.2(2) . . ?
C8 C7 C6 117.9(3) . . ?
C12 C7 C6 123.6(3) . . ?
C12 C7 C8 118.6(3) . . ?
H8 C8 C7 119.0(2) . . ?
C9 C8 C7 122.0(4) . . ?
C9 C8 H8 119.0(2) . . ?
H9 C9 C8 120.2(2) . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 H9 120.2(2) . . ?
H10 C10 C9 120.3(2) . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 H10 120.3(2) . . ?
C10 C11 O2 124.7(3) . . ?
C12 C11 O2 113.1(3) . . ?
C12 C11 C10 122.1(3) . . ?
C7 C12 O1 123.2(3) . . ?
C11 C12 O1 118.5(3) . . ?
C11 C12 C7 118.2(3) . . ?
H13a C13 O2 109.5 . . ?
H13b C13 O2 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 O2 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?
H14 C14 N2 116.5(2) . . ?
C15 C14 N2 127.1(3) . . ?
C15 C14 H14 116.46(19) . . ?
C16 C15 C14 116.7(3) . . ?
C20 C15 C14 123.6(3) . . ?
C20 C15 C16 119.5(3) . . ?
H16 C16 C15 118.9(2) . . ?
C17 C16 C15 122.1(3) . . ?
C17 C16 H16 118.9(2) . . ?
H17 C17 C16 120.3(2) . . ?
C18 C17 C16 119.4(4) . . ?
C18 C17 H17 120.3(2) . . ?
H18 C18 C17 120.4(2) . . ?
C19 C18 C17 119.2(4) . . ?
C19 C18 H18 120.4(2) . . ?
C18 C19 O4 124.4(3) . . ?
C20 C19 O4 112.8(3) . . ?
C20 C19 C18 122.8(3) . . ?
C15 C20 O3 125.1(3) . . ?
C19 C20 O3 118.3(3) . . ?
C19 C20 C15 116.6(3) . . ?
H21a C21 O4 109.5 . . ?
H21b C21 O4 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 O4 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H22 C22 N3 116.35(19) . . ?
C23 C22 N3 127.3(3) . . ?
C23 C22 H22 116.35(17) . . ?
C24 C23 C22 116.9(3) . . ?
C28 C23 C22 124.0(3) . . ?
C28 C23 C24 119.0(3) . . ?
H24 C24 C23 119.3(2) . . ?
C25 C24 C23 121.4(3) . . ?
C25 C24 H24 119.3(2) . . ?
H25 C25 C24 119.9(2) . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 H25 119.9(2) . . ?
H26 C26 C25 120.2(2) . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H26 120.2(2) . . ?
C26 C27 O6 125.3(3) . . ?
C28 C27 O6 113.7(3) . . ?
C28 C27 C26 121.0(3) . . ?
C23 C28 O5 123.2(3) . . ?
C27 C28 O5 118.2(3) . . ?
C27 C28 C23 118.6(3) . . ?
H29a C29 O6 109.5 . . ?
H29b C29 O6 109.5 . . ?
H29b C29 H29a 109.5 . . ?
H29c C29 O6 109.5 . . ?
H29c C29 H29a 109.5 . . ?
H29c C29 H29b 109.5 . . ?
C31 C30 N4 179.1(4) . . ?
H31a C31 C30 109.5 . . ?
H31b C31 C30 109.5 . . ?
H31b C31 H31a 109.5 . . ?
H31c C31 C30 109.5 . . ?
H31c C31 H31a 109.5 . . ?
H31c C31 H31b 109.5 . . ?
F1 C32 S1 110.9(3) . . ?
F2 C32 S1 111.5(2) . . ?
F2 C32 F1 108.0(3) . . ?
F3 C32 S1 110.9(3) . . ?
F3 C32 F1 107.4(3) . . ?
F3 C32 F2 108.0(3) . . ?
F4 C33 S2 110.4(3) . . ?
F5 C33 S2 112.4(3) . . ?
F5 C33 F4 108.3(4) . . ?
F6 C33 S2 111.4(3) . . ?
F6 C33 F4 106.1(3) . . ?
F6 C33 F5 107.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O1 C12 C7 -172.9(3) . . . . ?
La1 O1 C12 C11 7.0(3) . . . . ?
La1 O2 C11 C10 175.6(2) . . . . ?
La1 O2 C11 C12 -5.0(2) . . . . ?
La1 O3 C20 C15 -160.9(2) . . . . ?
La1 O3 C20 C19 17.4(3) . . . . ?
La1 O4 C19 C18 172.7(3) . . . . ?
La1 O4 C19 C20 -6.0(2) . . . . ?
La1 O5 C28 C23 174.5(3) . . . . ?
La1 O5 C28 C27 -3.2(3) . . . . ?
La1 O6 C27 C26 178.4(2) . . . . ?
La1 O6 C27 C28 -3.7(2) . . . . ?
La1 O7 S1 O8 78.1(8) . . . . ?
La1 O7 S1 O9 -59.3(8) . . . . ?
La1 O7 S1 C32 -170.4(8) . . . . ?
La1 O10 S2 O11 -6.5(2) . . . . ?
La1 O10 S2 O12 128.57(17) . . . . ?
La1 O10 S2 C33 -118.57(15) . . . . ?
La1 O11 S2 O10 6.39(19) . . . . ?
La1 O11 S2 O12 -129.73(18) . . . . ?
La1 O11 S2 C33 116.79(16) . . . . ?
Mn1 O1 C12 C7 1.9(3) . . . . ?
Mn1 O1 C12 C11 -178.2(3) . . . . ?
Mn1 O3 C20 C15 -29.8(3) . . . . ?
Mn1 O3 C20 C19 148.6(3) . . . . ?
Mn1 O5 C28 C23 28.7(3) . . . . ?
Mn1 O5 C28 C27 -149.1(3) . . . . ?
Mn1 N1 C3 C2 -26.5(3) . . . . ?
Mn1 N1 C6 C7 -6.6(4) . . . . ?
Mn1 N2 C4 C2 -12.5(2) . . . . ?
Mn1 N2 C14 C15 3.3(3) . . . . ?
Mn1 N3 C5 C2 -28.6(2) . . . . ?
Mn1 N3 C22 C23 -20.2(3) . . . . ?
O1 C12 C7 C6 3.0(4) . . . . ?
O1 C12 C7 C8 -178.0(3) . . . . ?
O1 C12 C11 O2 -0.3(3) . . . . ?
O1 C12 C11 C10 179.1(3) . . . . ?
O2 C11 C10 C9 178.6(3) . . . . ?
O2 C11 C12 C7 179.7(3) . . . . ?
O3 C20 C15 C14 11.1(4) . . . . ?
O3 C20 C15 C16 -174.8(4) . . . . ?
O3 C20 C19 O4 -6.1(3) . . . . ?
O3 C20 C19 C18 175.1(3) . . . . ?
O4 C19 C18 C17 -176.6(4) . . . . ?
O4 C19 C20 C15 172.4(3) . . . . ?
O5 C28 C23 C22 -3.3(4) . . . . ?
O5 C28 C23 C24 178.2(3) . . . . ?
O5 C28 C27 O6 4.4(3) . . . . ?
O5 C28 C27 C26 -177.7(3) . . . . ?
O6 C27 C26 C25 175.9(4) . . . . ?
O6 C27 C28 C23 -173.5(3) . . . . ?
N1 C3 C2 C1 -161.7(3) . . . . ?
N1 C3 C2 C4 82.5(4) . . . . ?
N1 C3 C2 C5 -45.3(4) . . . . ?
N1 C6 C7 C8 -179.4(4) . . . . ?
N1 C6 C7 C12 -0.4(5) . . . . ?
N2 C4 C2 C1 -172.0(3) . . . . ?
N2 C4 C2 C3 -56.3(3) . . . . ?
N2 C4 C2 C5 72.4(3) . . . . ?
N2 C14 C15 C16 -171.3(4) . . . . ?
N2 C14 C15 C20 3.0(4) . . . . ?
N3 C5 C2 C1 -163.2(3) . . . . ?
N3 C5 C2 C3 80.3(4) . . . . ?
N3 C5 C2 C4 -47.4(3) . . . . ?
N3 C22 C23 C24 177.9(4) . . . . ?
N3 C22 C23 C28 -0.6(4) . . . . ?
C6 C7 C8 C9 177.4(3) . . . . ?
C6 C7 C12 C11 -176.9(3) . . . . ?
C7 C8 C9 C10 -0.1(5) . . . . ?
C7 C12 C11 C10 -0.9(4) . . . . ?
C8 C9 C10 C11 1.2(4) . . . . ?
C9 C10 C11 C12 -0.7(4) . . . . ?
C14 C15 C16 C17 171.2(4) . . . . ?
C14 C15 C20 C19 -167.3(3) . . . . ?
C15 C16 C17 C18 -1.3(5) . . . . ?
C15 C20 C19 C18 -6.4(4) . . . . ?
C16 C17 C18 C19 2.0(5) . . . . ?
C17 C18 C19 C20 2.0(5) . . . . ?
C22 C23 C24 C25 -177.6(3) . . . . ?
C22 C23 C28 C27 174.4(3) . . . . ?
C23 C24 C25 C26 1.8(4) . . . . ?
C23 C28 C27 C26 4.5(4) . . . . ?
C24 C25 C26 C27 -1.4(4) . . . . ?
C25 C26 C27 C28 -1.8(4) . . . . ?


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

data_exp_3229
_database_code_depnum_ccdc_archive 'CCDC 2307061'
loop_
_audit_author_name
_audit_author_address
'Rebecca A. Musgrave'
;Kings College London
United Kingdom
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_exp_3229            
;
PROBLEM: Check Calcd Positive Resid. Density on       La1       1.60 eA-3
RESPONSE: There is no chemically sensible species corresponding to the residual density peak about the heavy metal lanthanum atom, and it may be a consequence of thermal restraints in the refinement.
;
# Added during the CSD deposition process: Friday 10 November 2023 11:11 AM
# end Validation Reply Form

_audit_creation_date             2023-11-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_formula_moiety         'C30 H30 F3 La N3 Na O9 S, C2 H3 N'
_chemical_formula_sum            'C32 H33 F3 La N4 Na O9 S'
_chemical_formula_weight         868.597
_chemical_oxdiff_formula         'C31 H33 F3 La N5 Na O9 S'
_chemical_oxdiff_usercomment     'TN022 MeCN Et2O'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.07537 0.05506 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
La -1.32533 9.78168 20.57800 19.59900 11.37270 3.28719 2.94817 0.24448 18.77260
133.12399 2.14678001404
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.33537 0.55136 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Na 0.13799 0.12245 4.76260 3.17360 1.26740 1.11280 3.28500 8.84220 0.31360
129.42400 0.675999999046
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   16.0670(1)
_cell_length_b                   13.0765(1)
_cell_length_c                   16.7696(1)
_cell_angle_alpha                90
_cell_angle_beta                 101.815(1)
_cell_angle_gamma                90
_cell_volume                     3448.65(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39389
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3290
_cell_measurement_theta_min      4.3450
_exptl_absorpt_coefficient_mu    10.929
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             1749.496
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 3 5 0.0632
5 -6 5 0.2479
-2 6 7 0.1113
-1 8 1 0.0812
2 7 5 0.1315
4 4 7 0.1923
4 8 -2 0.0858
8 5 1 0.1443
2 7 -6 0.0561
-3 7 -6 0.0656
6 5 -7 0.0645
10 0 -3 0.1616
9 3 -6 0.1055
8 0 -8 0.1033
9 -1 -7 0.1316
4 3 -10 0.0523
7 -5 -7 0.1658
0 -3 10 0.2089
0 3 -10 0.0476
-6 -4 -6 0.0768
-3 -7 -4 0.1241
1 -8 1 0.2224
-9 -1 -3 0.0600
-10 0 0 0.0555
-7 4 7 0.0809
-8 5 5 0.0696
-4 5 8 0.1010
-5 7 4 0.0771
-2 5 8 0.1250
3 -1 10 0.2193
3 8 1 0.1026
5 7 -4 0.0746
9 -1 2 0.2206
10 2 0 0.1774
-8 -3 7 0.0413
3 5 -9 0.0336
7 -1 -9 0.0934
0 0 -11 0.0459
0 -5 -9 0.0824
-5 -8 1 0.1321
3 -7 5 0.2258

_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-9.3941 3.0843 4.5384 0.3253 -0.7858 0.5260
5.1455 -5.8443 4.5682 -0.0176 0.0473 -0.9987
-1.7593 6.4253 7.0967 0.9535 -0.1763 0.2443
-0.9812 8.4321 0.8831 0.7011 0.1675 0.6931
2.2824 7.0340 4.9953 0.9558 0.2300 0.1833
4.4468 4.1044 7.1930 0.9303 0.2249 -0.2897
4.2857 7.7084 -1.7640 0.5908 0.6444 0.4854
7.6532 5.4098 0.8664 0.6747 0.7377 -0.0251
1.7906 7.0082 -6.1129 0.1734 0.5814 0.7949
-2.6473 6.5674 -5.6235 0.0632 0.2066 0.9764
6.0096 5.1094 -7.1775 0.0542 0.8834 0.4654
10.3781 0.2713 -3.2140 0.0549 0.9246 -0.3769
8.6567 3.3567 -6.0414 0.0600 0.9912 0.1178
8.2950 -0.0329 -8.2302 -0.3673 0.9298 -0.0226
9.0512 -1.2412 -6.9911 -0.3582 0.9055 -0.2277
4.3370 3.2602 -9.7126 -0.3080 0.7829 0.5406
6.8861 -4.7655 -6.7816 -0.6746 0.6159 -0.4069
-0.0429 -2.6981 10.1142 0.4859 -0.4465 -0.7514
-0.0834 2.8000 -10.0433 -0.4760 0.4376 0.7628
-5.6942 -4.2003 -5.9845 -0.8851 -0.3669 0.2864
-3.4848 -7.1957 -3.6382 -0.9043 -0.3760 -0.2023
1.1946 -8.3401 1.3038 -0.5373 -0.2249 -0.8128
-9.3083 -0.8755 -2.6903 -0.4844 -0.6541 0.5810
-10.1981 0.0924 -0.0506 -0.2476 -0.7841 0.5691
-7.4823 3.6374 7.4471 0.6171 -0.7221 0.3126
-7.8953 4.9128 4.9113 0.5320 -0.6234 0.5729
-3.8827 5.4537 7.9612 0.8844 -0.4026 0.2360
-5.1852 6.9274 4.2374 0.7109 -0.3245 0.6239
-1.5137 5.4631 8.3259 0.9688 -0.2318 0.0876
2.9585 -0.8389 9.5326 0.6661 -0.1334 -0.7339
2.7240 8.0921 1.0189 0.7750 0.4383 0.4552
4.6193 7.1132 -4.3850 0.3709 0.7430 0.5572
9.4372 -1.3759 2.1799 0.2750 0.6087 -0.7442
10.0182 1.6285 0.0031 0.3754 0.8279 -0.4167
-8.4021 -2.5256 7.2549 0.0957 -0.9871 -0.1282
3.0647 4.7389 -8.9251 -0.1684 0.7049 0.6890
6.8413 -1.3335 -9.3266 -0.5814 0.8136 0.0092
0.3305 0.3814 -10.7107 -0.7025 0.4143 0.5786
-0.3826 -4.6486 -8.8217 -0.9857 0.1291 0.1087
-4.7442 -7.5524 0.6435 -0.6673 -0.6355 -0.3884
2.8607 -7.0671 4.5203 -0.1736 -0.1676 -0.9705

_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9914
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59489
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9914
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.58
_diffrn_reflns_theta_min         3.47
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9914
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00  33.00   1.00    1.50    --  -42.37  75.00  36.00  108
  2  ω     97.00 136.00   1.00    6.00    --  103.86 -75.00 -90.00   39
  3  ω     29.00  73.00   1.00    6.00    --  103.86 -75.00 -90.00   44
  4  ω    115.00 140.00   1.00    6.00    --  103.86  75.00  36.00   25
  5  ω     -4.00  22.00   1.00    1.50    --   34.00  92.00 163.67   26
  6  ω     -3.00  22.00   1.00    1.50    --   34.00  90.00  28.46   25
  7  ω     -3.00  23.00   1.00    1.50    --   34.00  90.00 -34.54   26
  8  ω   -121.00 -10.00   1.00    1.50    --  -42.37 -19.00  30.00  111
  9  ω    -67.00  24.00   1.00    1.50    --  -42.37  38.00-150.00   91
 10  ω    -89.00 -18.00   1.00    1.50    --  -42.37 -38.00-150.00   71
 11  ω     -3.00  50.00   1.00    1.50    --   42.37 -75.00 -90.00   53
 12  ω     55.00  82.00   1.00    1.50    --   42.37  38.00 -90.00   27
 13  ω     35.00  85.00   1.00    1.50    --   42.37-125.00-180.00   50
 14  ω     19.00  47.00   1.00    1.50    --   42.37  38.00 -90.00   28
 15  ω     16.00  41.00   1.00    1.50    --   50.00  81.00  82.68   25
 16  ω     16.00  42.00   1.00    1.50    --   50.00  82.00   5.80   26
 17  ω     16.00  41.00   1.00    1.50    --   50.00  82.00 138.38   25
 18  ω     16.00  41.00   1.00    1.50    --   50.00  81.00-143.17   25
 19  ω     16.00  41.00   1.00    1.50    --   50.00  81.00 -83.09   25
 20  ω     31.00  57.00   1.00    1.50    --   62.00  71.00 176.92   26
 21  ω     35.00  68.00   1.00    1.50    --   66.00  71.00 -41.92   33
 22  ω     39.00  65.00   1.00    1.50    --   70.00  70.00-154.80   26
 23  ω     39.00  65.00   1.00    1.50    --   70.00  70.00  35.74   26
 24  ω     39.00  65.00   1.00    1.50    --   70.00  69.00 -67.53   26
 25  ω     39.00  65.00   1.00    1.50    --   70.00  71.00  95.98   26
 26  ω     39.00  65.00   1.00    1.50    --   70.00  71.00  -6.20   26
 27  ω     39.00  65.00   1.00    1.50    --   70.00  71.00-107.57   26
 28  ω     40.00  65.00   1.00    1.50    --   70.00  71.00 142.52   25
 29  ω     44.00  70.00   1.00    6.00    --   74.00  65.00  72.08   26
 30  ω     51.00  77.00   1.00    6.00    --   82.00  69.00 -36.23   26
 31  ω     51.00  99.00   1.00    6.00    --   82.00  71.00 154.05   48
 32  ω     54.00  81.00   1.00    6.00    --   82.00  62.00  94.82   27
 33  ω     51.00  77.00   1.00    6.00    --   82.00  69.00 -70.41   26
 34  ω     55.00  81.00   1.00    6.00    --   86.00  71.00 104.25   26
 35  ω     55.00  81.00   1.00    6.00    --   86.00  69.00 -15.47   26
 36  ω     56.00  83.00   1.00    6.00    --   86.00  67.00-146.62   27
 37  ω     62.00  89.00   1.00    6.00    --   90.00  62.00-169.83   27
 38  ω     59.00  85.00   1.00    6.00    --   90.00  71.00-116.52   26
 39  ω     64.00  90.00   1.00    6.00    --   94.00  67.00   2.23   26
 40  ω    104.00 130.00   1.00    6.00    --   94.00  67.00   2.23   26
 41  ω     74.00 102.00   1.00    6.00    --  103.86  67.00 -77.58   28
 42  ω    150.00 177.00   1.00    6.00    --  103.86  66.00 128.42   27
 43  ω    113.00 177.00   1.00    6.00    --  103.86  66.00 -60.44   64
 44  ω     75.00 109.00   1.00    6.00    --  103.86  66.00 128.42   34
 45  ω     74.00 105.00   1.00    6.00    --  103.86  66.00 -60.44   31
 46  ω     73.00 170.00   1.00    6.00    --  103.86  71.00-165.43   97
 47  ω     29.00 135.00   1.00    6.00    --  103.86 -77.00  90.00  106
 48  ω     75.00 177.00   1.00    6.00    --  103.86  60.00  80.37  102
 49  ω     75.00 173.00   1.00    6.00    --  103.86  61.00 150.00   98
 50  ω     74.00 136.00   1.00    6.00    --  103.86  63.00  23.49   62
 51  ω    114.00 176.00   1.00    6.00    --  103.86  61.00 120.00   62
 52  ω     31.00 113.00   1.00    6.00    --  103.86-125.00 -90.00   82
 53  ω     75.00 102.00   1.00    6.00    --  103.86  61.00 120.00   27
 54  ω     76.00 172.00   1.00    6.00    --  103.86  61.00-120.00   96
 55  ω     47.00 107.00   1.00    6.00    --  103.86-106.00 -23.52   60
 56  ω    114.00 176.00   1.00    6.00    --  103.86  61.00 -90.00   62
 57  ω     46.00 112.00   1.00    6.00    --  103.86-125.00  90.00   66
 58  ω     78.00 174.00   1.00    6.00    --  103.86  61.00 -30.00   96
 59  ω     78.00 104.00   1.00    6.00    --  103.86  61.00 -90.00   26
 60  ω     74.00 162.00   1.00    6.00    --  103.86  70.00  39.19   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0246463000
_diffrn_orient_matrix_UB_12      0.0787698000
_diffrn_orient_matrix_UB_13      0.0691546000
_diffrn_orient_matrix_UB_21      0.0773604000
_diffrn_orient_matrix_UB_22      0.0325502000
_diffrn_orient_matrix_UB_23      -0.0351379000
_diffrn_orient_matrix_UB_31      -0.0548016000
_diffrn_orient_matrix_UB_32      0.0813545000
_diffrn_orient_matrix_UB_33      -0.0528177000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -19
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -12
_reflns_number_gt                6650
_reflns_number_total             6788
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.3340
_refine_diff_density_min         -0.9522
_refine_diff_density_rms         0.0768
_refine_ls_d_res_high            0.8080
_refine_ls_d_res_low             12.7325
_refine_ls_goodness_of_fit_ref   1.0522
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6788
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0194
_refine_ls_restrained_S_all      1.0522
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²+1.3768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0508
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18),
 C22(H22), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C13(H13a,H13b,H13c), C21(H21a,H21b,H21c), C29(H29a,H29b,
 H29c), C32(H32a,H32b,H32c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
La1 La 0.610617(5) 0.530826(7) 0.498442(5) 0.00974(4) Uani 1.000000 .
S1 S 0.65828(3) 0.44208(3) 0.84651(3) 0.01682(9) Uani 1.000000 .
Na1 Na 0.52473(4) 0.48198(5) 0.69942(4) 0.01691(15) Uani 1.000000 .
F1 F 0.69105(13) 0.53479(12) 0.98789(10) 0.0579(5) Uani 1.000000 .
F2 F 0.56071(11) 0.49369(14) 0.94724(10) 0.0534(4) Uani 1.000000 .
F3 F 0.65196(11) 0.37888(11) 0.99353(8) 0.0437(3) Uani 1.000000 .
O1 O 0.61888(8) 0.54848(10) 0.35732(8) 0.0157(2) Uani 1.000000 .
O2 O 0.56607(8) 0.42802(11) 0.22961(8) 0.0227(3) Uani 1.000000 .
O3 O 0.54834(7) 0.40298(9) 0.58061(7) 0.0120(2) Uani 1.000000 .
O4 O 0.42110(7) 0.27050(9) 0.54251(7) 0.0152(2) Uani 1.000000 .
O5 O 0.50554(7) 0.59074(9) 0.58198(7) 0.0114(2) Uani 1.000000 .
O6 O 0.34786(7) 0.65625(9) 0.56843(8) 0.0153(2) Uani 1.000000 .
O7 O 0.74506(9) 0.40855(12) 0.86117(9) 0.0310(3) Uani 1.000000 .
O8 O 0.64176(9) 0.54073(10) 0.80780(9) 0.0222(3) Uani 1.000000 .
O9 O 0.59545(9) 0.36647(11) 0.81257(9) 0.0266(3) Uani 1.000000 .
N1 N 0.76764(9) 0.59511(11) 0.48301(9) 0.0160(3) Uani 1.000000 .
N2 N 0.73680(9) 0.42280(11) 0.59454(9) 0.0151(3) Uani 1.000000 .
N3 N 0.68381(9) 0.63291(11) 0.63678(9) 0.0135(3) Uani 1.000000 .
C1 C 0.92294(11) 0.59461(15) 0.68404(12) 0.0213(4) Uani 1.000000 .
H1a H 0.9268(3) 0.5646(10) 0.7382(3) 0.0319(6) Uiso 1.000000 GR
H1b H 0.96556(13) 0.5630(10) 0.6576(5) 0.0319(6) Uiso 1.000000 GR
H1c H 0.9334(4) 0.66837(15) 0.6893(8) 0.0319(6) Uiso 1.000000 GR
C3 C 0.82535(11) 0.64012(14) 0.55416(11) 0.0185(4) Uani 1.000000 .
H3a H 0.88239(11) 0.64841(14) 0.54125(11) 0.0222(4) Uiso 1.000000 R
H3b H 0.80424(11) 0.70899(14) 0.56449(11) 0.0222(4) Uiso 1.000000 R
C4 C 0.82546(11) 0.46044(13) 0.61455(12) 0.0179(4) Uani 1.000000 .
H4a H 0.85649(11) 0.42287(13) 0.66282(12) 0.0215(4) Uiso 1.000000 R
H4b H 0.85324(11) 0.44465(13) 0.56847(12) 0.0215(4) Uiso 1.000000 R
C5 C 0.77013(10) 0.61086(14) 0.68330(11) 0.0164(3) Uani 1.000000 .
H5a H 0.79282(10) 0.67331(14) 0.71346(11) 0.0197(4) Uiso 1.000000 R
H5b H 0.76616(10) 0.55723(14) 0.72402(11) 0.0197(4) Uiso 1.000000 R
C6 C 0.80056(11) 0.58585(15) 0.41964(12) 0.0211(4) Uani 1.000000 .
H6 H 0.85607(11) 0.61324(15) 0.42402(12) 0.0253(5) Uiso 1.000000 R
C7 C 0.76327(13) 0.53871(16) 0.34231(13) 0.0243(4) Uani 1.000000 .
C8 C 0.82117(15) 0.5073(2) 0.29443(16) 0.0411(6) Uani 1.000000 .
H8 H 0.87920(15) 0.5268(2) 0.30967(16) 0.0493(7) Uiso 1.000000 R
C9 C 0.79492(17) 0.4491(3) 0.22656(17) 0.0517(8) Uani 1.000000 .
H9 H 0.83464(17) 0.4282(3) 0.19490(17) 0.0621(9) Uiso 1.000000 R
C10 C 0.70946(15) 0.4201(2) 0.20334(14) 0.0386(6) Uani 1.000000 .
H10 H 0.69162(15) 0.3777(2) 0.15693(14) 0.0463(7) Uiso 1.000000 R
C11 C 0.65125(13) 0.45280(16) 0.24779(12) 0.0229(4) Uani 1.000000 .
C12 C 0.67570(12) 0.51578(15) 0.31804(11) 0.0183(4) Uani 1.000000 .
C13 C 0.54144(14) 0.34288(17) 0.17650(13) 0.0296(4) Uani 1.000000 .
H13a H 0.4814(3) 0.3270(8) 0.1743(8) 0.0444(7) Uiso 1.000000 GR
H13b H 0.5496(10) 0.3599(5) 0.1217(3) 0.0444(7) Uiso 1.000000 GR
H13c H 0.5764(7) 0.2834(4) 0.1971(6) 0.0444(7) Uiso 1.000000 GR
C2 C 0.83360(10) 0.57555(14) 0.63216(11) 0.0156(3) Uani 1.000000 .
C14 C 0.72752(11) 0.33233(14) 0.61985(11) 0.0155(3) Uani 1.000000 .
H14 H 0.77639(11) 0.30321(14) 0.65378(11) 0.0187(4) Uiso 1.000000 R
C15 C 0.65204(11) 0.26759(13) 0.60373(10) 0.0144(3) Uani 1.000000 .
C16 C 0.66813(11) 0.16185(14) 0.60624(11) 0.0181(4) Uani 1.000000 .
H16 H 0.72495(11) 0.13805(14) 0.62239(11) 0.0217(4) Uiso 1.000000 R
C17 C 0.60307(12) 0.09222(14) 0.58570(12) 0.0209(4) Uani 1.000000 .
H17 H 0.61507(12) 0.02105(14) 0.58647(12) 0.0251(5) Uiso 1.000000 R
C18 C 0.51945(12) 0.12678(14) 0.56377(11) 0.0189(4) Uani 1.000000 .
H18 H 0.47421(12) 0.07923(14) 0.54899(11) 0.0227(4) Uiso 1.000000 R
C19 C 0.50251(11) 0.23039(13) 0.56357(10) 0.0142(3) Uani 1.000000 .
C20 C 0.56768(10) 0.30430(13) 0.58273(10) 0.0121(3) Uani 1.000000 .
C21 C 0.35319(12) 0.19827(15) 0.53833(14) 0.0277(4) Uani 1.000000 .
H21a H 0.29931(19) 0.23497(15) 0.5343(10) 0.0415(7) Uiso 1.000000 GR
H21b H 0.3501(7) 0.1546(8) 0.4903(6) 0.0415(7) Uiso 1.000000 GR
H21c H 0.3637(5) 0.1558(8) 0.5875(5) 0.0415(7) Uiso 1.000000 GR
C22 C 0.65058(11) 0.71142(13) 0.66372(10) 0.0149(3) Uani 1.000000 .
H22 H 0.68820(11) 0.75148(13) 0.70254(10) 0.0179(4) Uiso 1.000000 R
C23 C 0.56318(11) 0.74771(13) 0.64307(10) 0.0139(3) Uani 1.000000 .
C24 C 0.54775(12) 0.84691(14) 0.66862(11) 0.0182(4) Uani 1.000000 .
H24 H 0.59438(12) 0.88902(14) 0.69255(11) 0.0219(4) Uiso 1.000000 R
C25 C 0.46638(12) 0.88416(14) 0.65963(12) 0.0214(4) Uani 1.000000 .
H25 H 0.45703(12) 0.95203(14) 0.67600(12) 0.0257(5) Uiso 1.000000 R
C26 C 0.39733(11) 0.82153(14) 0.62623(11) 0.0188(4) Uani 1.000000 .
H26 H 0.34089(11) 0.84646(14) 0.62063(11) 0.0225(4) Uiso 1.000000 R
C27 C 0.41134(10) 0.72406(14) 0.60158(10) 0.0141(3) Uani 1.000000 .
C28 C 0.49483(10) 0.68451(13) 0.60729(10) 0.0119(3) Uani 1.000000 .
C29 C 0.26283(11) 0.68887(15) 0.56993(12) 0.0205(4) Uani 1.000000 .
H29a H 0.2486(3) 0.7489(7) 0.5348(7) 0.0307(6) Uiso 1.000000 GR
H29b H 0.22290(14) 0.6334(4) 0.5501(8) 0.0307(6) Uiso 1.000000 GR
H29c H 0.2590(3) 0.7065(11) 0.62585(18) 0.0307(6) Uiso 1.000000 GR
C30 C 0.63949(15) 0.46376(15) 0.94896(14) 0.0270(5) Uani 1.000000 .
N4 N 0.04427(18) 0.7046(3) 0.5128(3) 0.0800(9) Uani 1.000000 .
C32 C 0.0926(2) 0.8100(3) 0.6431(3) 0.0766(11) Uani 1.000000 .
H32a H 0.1302(15) 0.8652(14) 0.6327(5) 0.1149(17) Uiso 1.000000 GR
H32b H 0.0428(2) 0.8393(19) 0.6602(11) 0.1149(17) Uiso 1.000000 GR
H32c H 0.1233(17) 0.7655(6) 0.6863(6) 0.1149(17) Uiso 1.000000 GR
C31 C 0.06543(18) 0.7515(3) 0.5703(3) 0.0611(9) Uani 1.000000 .


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 La1 3.65563(16) 3_666 ?
La1 Na1 3.5793(7) 3_666 ?
La1 O1 2.4083(12) . ?
La1 O3 2.7645(11) 3_666 ?
La1 O3 2.5019(11) . ?
La1 O4 2.7087(12) 3_666 ?
La1 O5 2.6074(11) 3_666 ?
La1 O5 2.5289(11) . ?
La1 O6 2.8273(12) 3_666 ?
La1 N1 2.7215(14) . ?
La1 N2 2.7138(15) . ?
La1 N3 2.7258(14) . ?
S1 Na1 2.9654(8) . ?
S1 O7 1.4341(14) . ?
S1 O8 1.4440(14) . ?
S1 O9 1.4440(14) . ?
S1 C30 1.826(2) . ?
Na1 O1 2.3428(14) 3_666 ?
Na1 O2 2.3751(14) 3_666 ?
Na1 O3 2.3431(13) . ?
Na1 O5 2.3973(13) . ?
Na1 O8 2.4557(16) . ?
Na1 O9 2.5081(16) . ?
Na1 C28 3.0541(18) . ?
F1 C30 1.324(3) . ?
F2 C30 1.319(3) . ?
F3 C30 1.330(2) . ?
O1 C12 1.302(2) . ?
O2 C11 1.379(2) . ?
O2 C13 1.430(2) . ?
O3 C20 1.326(2) . ?
O4 C19 1.386(2) . ?
O4 C21 1.434(2) . ?
O5 C28 1.320(2) . ?
O6 C27 1.380(2) . ?
O6 C29 1.4364(19) . ?
N1 C3 1.475(2) . ?
N1 C6 1.286(2) . ?
N2 C4 1.479(2) . ?
N2 C14 1.276(2) . ?
N3 C5 1.474(2) . ?
N3 C22 1.281(2) . ?
C1 H1a 0.9800 . ?
C1 H1b 0.9800 . ?
C1 H1c 0.9800 . ?
C1 C2 1.539(2) . ?
C3 H3a 0.9900 . ?
C3 H3b 0.9900 . ?
C3 C2 1.540(3) . ?
C4 H4a 0.9900 . ?
C4 H4b 0.9900 . ?
C4 C2 1.534(2) . ?
C5 H5a 0.9900 . ?
C5 H5b 0.9900 . ?
C5 C2 1.532(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.450(3) . ?
C7 C8 1.409(3) . ?
C7 C12 1.414(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.362(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.401(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(3) . ?
C11 C12 1.425(3) . ?
C13 H13a 0.9800 . ?
C13 H13b 0.9800 . ?
C13 H13c 0.9800 . ?
C14 H14 0.9500 . ?
C14 C15 1.458(2) . ?
C15 C16 1.406(2) . ?
C15 C20 1.413(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.376(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.394(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(2) . ?
C19 C20 1.413(2) . ?
C21 H21a 0.9800 . ?
C21 H21b 0.9800 . ?
C21 H21c 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.455(2) . ?
C23 C24 1.404(2) . ?
C23 C28 1.407(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.374(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.400(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.373(2) . ?
C27 C28 1.423(2) . ?
C29 H29a 0.9800 . ?
C29 H29b 0.9800 . ?
C29 H29c 0.9800 . ?
N4 C31 1.135(5) . ?
C32 H32a 0.9800 . ?
C32 H32b 0.9800 . ?
C32 H32c 0.9800 . ?
C32 C31 1.431(6) . ?

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 La1 Na1 40.43(3) . 3_666 ?
O3 La1 Na1 40.88(3) 3_666 3_666 ?
O3 La1 Na1 104.10(3) . 3_666 ?
O3 La1 O1 74.35(4) 3_666 . ?
O3 La1 O1 135.56(4) . . ?
O4 La1 Na1 76.28(3) 3_666 3_666 ?
O4 La1 O1 72.80(4) 3_666 . ?
O4 La1 O3 134.81(4) 3_666 . ?
O4 La1 O3 58.05(3) 3_666 3_666 ?
O5 La1 Na1 100.38(3) . 3_666 ?
O5 La1 Na1 42.04(3) 3_666 3_666 ?
O5 La1 O1 133.79(4) . . ?
O5 La1 O1 74.20(4) 3_666 . ?
O5 La1 O3 60.94(4) . . ?
O5 La1 O3 60.83(4) . 3_666 ?
O5 La1 O3 63.44(4) 3_666 . ?
O5 La1 O3 56.61(3) 3_666 3_666 ?
O5 La1 O4 74.40(4) . 3_666 ?
O5 La1 O4 112.09(4) 3_666 3_666 ?
O6 La1 Na1 74.91(3) 3_666 3_666 ?
O6 La1 O1 68.17(4) 3_666 . ?
O6 La1 O3 78.10(3) 3_666 . ?
O6 La1 O3 110.52(3) 3_666 3_666 ?
O6 La1 O4 140.96(4) 3_666 3_666 ?
O6 La1 O5 57.95(3) 3_666 3_666 ?
O6 La1 O5 136.58(3) 3_666 . ?
N1 La1 Na1 108.99(3) . 3_666 ?
N1 La1 O1 68.79(4) . . ?
N1 La1 O3 137.89(4) . . ?
N1 La1 O3 129.87(4) . 3_666 ?
N1 La1 O4 79.02(4) . 3_666 ?
N1 La1 O5 135.93(4) . 3_666 ?
N1 La1 O5 133.95(4) . . ?
N1 La1 O6 86.04(4) . 3_666 ?
N2 La1 Na1 139.85(3) . 3_666 ?
N2 La1 O1 116.66(4) . . ?
N2 La1 O3 162.21(4) . 3_666 ?
N2 La1 O3 70.09(4) . . ?
N2 La1 O4 136.78(4) . 3_666 ?
N2 La1 O5 109.55(4) . . ?
N2 La1 O5 111.00(4) . 3_666 ?
N2 La1 O6 64.97(4) . 3_666 ?
N2 La1 N1 67.84(4) . . ?
N3 La1 Na1 152.40(3) . 3_666 ?
N3 La1 O1 133.50(4) . . ?
N3 La1 O3 90.58(4) . . ?
N3 La1 O3 116.74(4) . 3_666 ?
N3 La1 O4 76.82(4) . 3_666 ?
N3 La1 O5 151.31(4) . 3_666 ?
N3 La1 O5 66.26(4) . . ?
N3 La1 O6 131.73(4) . 3_666 ?
N3 La1 N1 71.51(4) . . ?
N3 La1 N2 67.04(4) . . ?
O7 S1 Na1 135.15(7) . . ?
O8 S1 Na1 55.52(6) . . ?
O8 S1 O7 115.66(9) . . ?
O9 S1 Na1 57.61(6) . . ?
O9 S1 O7 115.78(9) . . ?
O9 S1 O8 112.66(8) . . ?
C30 S1 Na1 121.63(8) . . ?
C30 S1 O7 103.20(10) . . ?
C30 S1 O8 103.51(9) . . ?
C30 S1 O9 103.90(9) . . ?
S1 Na1 La1 164.09(3) . 3_666 ?
O1 Na1 La1 41.81(3) 3_666 3_666 ?
O1 Na1 S1 142.43(4) 3_666 . ?
O2 Na1 La1 99.72(4) 3_666 3_666 ?
O2 Na1 S1 94.84(4) 3_666 . ?
O2 Na1 O1 68.46(5) 3_666 3_666 ?
O3 Na1 La1 50.55(3) . 3_666 ?
O3 Na1 S1 114.47(4) . . ?
O3 Na1 O1 84.10(5) . 3_666 ?
O3 Na1 O2 150.18(5) . 3_666 ?
O5 Na1 La1 46.74(3) . 3_666 ?
O5 Na1 S1 137.49(4) . . ?
O5 Na1 O1 79.45(5) . 3_666 ?
O5 Na1 O2 97.40(5) . 3_666 ?
O5 Na1 O3 65.10(4) . . ?
O8 Na1 La1 158.21(4) . 3_666 ?
O8 Na1 S1 28.99(3) . . ?
O8 Na1 O1 153.51(5) . 3_666 ?
O8 Na1 O2 85.98(5) . 3_666 ?
O8 Na1 O3 122.31(5) . . ?
O8 Na1 O5 111.88(5) . . ?
O9 Na1 La1 140.21(4) . 3_666 ?
O9 Na1 S1 29.09(3) . . ?
O9 Na1 O1 117.44(5) . 3_666 ?
O9 Na1 O2 98.56(5) . 3_666 ?
O9 Na1 O3 104.52(5) . . ?
O9 Na1 O5 160.20(5) . . ?
O9 Na1 O8 57.91(5) . . ?
C28 Na1 La1 64.46(3) . 3_666 ?
C28 Na1 S1 125.83(4) . . ?
C28 Na1 O1 84.39(5) . 3_666 ?
C28 Na1 O2 76.98(5) . 3_666 ?
C28 Na1 O3 89.33(5) . . ?
C28 Na1 O5 24.44(4) . . ?
C28 Na1 O8 96.91(5) . . ?
C28 Na1 O9 154.81(5) . . ?
Na1 O1 La1 97.75(5) 3_666 . ?
C12 O1 La1 130.61(12) . . ?
C12 O1 Na1 118.21(12) . 3_666 ?
C11 O2 Na1 117.16(11) . 3_666 ?
C13 O2 Na1 125.30(12) . 3_666 ?
C13 O2 C11 117.16(15) . . ?
Na1 O3 La1 109.05(5) . . ?
Na1 O3 La1 88.58(4) . 3_666 ?
C20 O3 La1 123.17(10) . . ?
C20 O3 La1 120.39(10) . 3_666 ?
C20 O3 Na1 118.95(10) . . ?
C19 O4 La1 123.11(9) . 3_666 ?
C21 O4 La1 121.17(10) . 3_666 ?
C21 O4 C19 115.60(13) . . ?
Na1 O5 La1 106.45(4) . . ?
Na1 O5 La1 91.22(4) . 3_666 ?
C28 O5 La1 127.70(10) . . ?
C28 O5 La1 127.29(10) . 3_666 ?
C28 O5 Na1 106.87(9) . . ?
C27 O6 La1 120.06(9) . 3_666 ?
C29 O6 La1 124.50(10) . 3_666 ?
C29 O6 C27 115.43(13) . . ?
Na1 O8 S1 95.48(7) . . ?
Na1 O9 S1 93.31(7) . . ?
C3 N1 La1 119.18(10) . . ?
C6 N1 La1 126.55(12) . . ?
C6 N1 C3 114.16(15) . . ?
C4 N2 La1 121.94(11) . . ?
C14 N2 La1 123.79(12) . . ?
C14 N2 C4 113.94(15) . . ?
C5 N3 La1 123.36(10) . . ?
C22 N3 La1 123.65(11) . . ?
C22 N3 C5 112.65(14) . . ?
H1b C1 H1a 109.5 . . ?
H1c C1 H1a 109.5 . . ?
H1c C1 H1b 109.5 . . ?
C2 C1 H1a 109.5 . . ?
C2 C1 H1b 109.5 . . ?
C2 C1 H1c 109.5 . . ?
H3a C3 N1 108.87(9) . . ?
H3b C3 N1 108.87(9) . . ?
H3b C3 H3a 107.7 . . ?
C2 C3 N1 113.51(14) . . ?
C2 C3 H3a 108.87(9) . . ?
C2 C3 H3b 108.87(10) . . ?
H4a C4 N2 108.70(9) . . ?
H4b C4 N2 108.70(10) . . ?
H4b C4 H4a 107.6 . . ?
C2 C4 N2 114.22(14) . . ?
C2 C4 H4a 108.70(10) . . ?
C2 C4 H4b 108.70(10) . . ?
H5a C5 N3 108.49(9) . . ?
H5b C5 N3 108.49(9) . . ?
H5b C5 H5a 107.5 . . ?
C2 C5 N3 115.14(14) . . ?
C2 C5 H5a 108.49(9) . . ?
C2 C5 H5b 108.49(10) . . ?
H6 C6 N1 116.04(11) . . ?
C7 C6 N1 127.92(17) . . ?
C7 C6 H6 116.04(10) . . ?
C8 C7 C6 115.70(19) . . ?
C12 C7 C6 123.50(17) . . ?
C12 C7 C8 120.5(2) . . ?
H8 C8 C7 119.62(14) . . ?
C9 C8 C7 120.8(2) . . ?
C9 C8 H8 119.62(14) . . ?
H9 C9 C8 119.94(14) . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 H9 119.94(13) . . ?
H10 C10 C9 119.99(13) . . ?
C11 C10 C9 120.0(2) . . ?
C11 C10 H10 119.99(13) . . ?
C10 C11 O2 124.07(19) . . ?
C12 C11 O2 114.32(16) . . ?
C12 C11 C10 121.61(19) . . ?
C7 C12 O1 122.94(18) . . ?
C11 C12 O1 120.31(17) . . ?
C11 C12 C7 116.74(17) . . ?
H13a C13 O2 109.5 . . ?
H13b C13 O2 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 O2 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?
C3 C2 C1 107.43(14) . . ?
C4 C2 C1 107.49(14) . . ?
C4 C2 C3 112.67(15) . . ?
C5 C2 C1 106.59(14) . . ?
C5 C2 C3 111.03(14) . . ?
C5 C2 C4 111.30(14) . . ?
H14 C14 N2 115.62(10) . . ?
C15 C14 N2 128.77(16) . . ?
C15 C14 H14 115.62(9) . . ?
C16 C15 C14 115.13(15) . . ?
C20 C15 C14 124.61(15) . . ?
C20 C15 C16 120.19(16) . . ?
H16 C16 C15 119.41(10) . . ?
C17 C16 C15 121.18(17) . . ?
C17 C16 H16 119.41(11) . . ?
H17 C17 C16 120.22(11) . . ?
C18 C17 C16 119.57(17) . . ?
C18 C17 H17 120.22(11) . . ?
H18 C18 C17 120.09(11) . . ?
C19 C18 C17 119.83(17) . . ?
C19 C18 H18 120.09(11) . . ?
C18 C19 O4 123.15(15) . . ?
C20 C19 O4 114.57(14) . . ?
C20 C19 C18 122.26(16) . . ?
C15 C20 O3 123.01(15) . . ?
C19 C20 O3 120.06(15) . . ?
C19 C20 C15 116.92(15) . . ?
H21a C21 O4 109.5 . . ?
H21b C21 O4 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 O4 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H22 C22 N3 115.52(10) . . ?
C23 C22 N3 128.96(16) . . ?
C23 C22 H22 115.52(10) . . ?
C24 C23 C22 116.79(16) . . ?
C28 C23 C22 122.74(15) . . ?
C28 C23 C24 120.12(15) . . ?
H24 C24 C23 119.42(10) . . ?
C25 C24 C23 121.16(17) . . ?
C25 C24 H24 119.42(11) . . ?
H25 C25 C24 120.18(11) . . ?
C26 C25 C24 119.64(16) . . ?
C26 C25 H25 120.18(10) . . ?
H26 C26 C25 120.06(10) . . ?
C27 C26 C25 119.88(16) . . ?
C27 C26 H26 120.06(10) . . ?
C26 C27 O6 124.40(15) . . ?
C28 C27 O6 113.74(15) . . ?
C28 C27 C26 121.86(16) . . ?
O5 C28 Na1 48.69(7) . . ?
C23 C28 Na1 105.40(11) . . ?
C23 C28 O5 122.75(15) . . ?
C27 C28 Na1 113.44(11) . . ?
C27 C28 O5 119.95(15) . . ?
C27 C28 C23 117.26(15) . . ?
H29a C29 O6 109.5 . . ?
H29b C29 O6 109.5 . . ?
H29b C29 H29a 109.5 . . ?
H29c C29 O6 109.5 . . ?
H29c C29 H29a 109.5 . . ?
H29c C29 H29b 109.5 . . ?
F1 C30 S1 111.43(15) . . ?
F2 C30 S1 111.59(16) . . ?
F2 C30 F1 107.65(19) . . ?
F3 C30 S1 111.36(14) . . ?
F3 C30 F1 107.53(19) . . ?
F3 C30 F2 107.05(18) . . ?
H32b C32 H32a 109.5 . . ?
H32c C32 H32a 109.5 . . ?
H32c C32 H32b 109.5 . . ?
C31 C32 H32a 109.5 . . ?
C31 C32 H32b 109.5 . . ?
C31 C32 H32c 109.5 . . ?
C32 C31 N4 179.5(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O1 C12 C7 -55.09(16) . . . . ?
La1 O1 C12 C11 124.06(16) . . . . ?
La1 O3 C20 C15 163.97(11) 3_666 . . . ?
La1 O3 C20 C15 54.73(13) . . . . ?
La1 O3 C20 C19 -125.35(12) . . . . ?
La1 O3 C20 C19 -16.12(12) 3_666 . . . ?
La1 O4 C19 C18 -162.56(13) 3_666 . . . ?
La1 O4 C19 C20 15.69(11) 3_666 . . . ?
La1 O5 C28 Na1 105.01(15) 3_666 . . . ?
La1 O5 C28 Na1 -127.47(18) . . . . ?
La1 O5 C28 C23 -173.34(12) 3_666 . . . ?
La1 O5 C28 C23 -45.81(13) . . . . ?
La1 O5 C28 C27 136.51(13) . . . . ?
La1 O5 C28 C27 8.99(13) 3_666 . . . ?
La1 O6 C27 C26 171.57(12) 3_666 . . . ?
La1 O6 C27 C28 -7.53(11) 3_666 . . . ?
La1 N1 C3 C2 49.08(12) . . . . ?
La1 N1 C6 C7 -0.73(18) . . . . ?
La1 N2 C4 C2 40.38(12) . . . . ?
La1 N2 C14 C15 0.89(16) . . . . ?
La1 N3 C5 C2 32.60(12) . . . . ?
La1 N3 C22 C23 17.18(15) . . . . ?
Na1 O1 C12 C7 173.48(14) 3_666 . . . ?
Na1 O1 C12 C11 -7.36(14) 3_666 . . . ?
Na1 O2 C11 C10 -169.14(17) 3_666 . . . ?
Na1 O2 C11 C12 11.30(13) 3_666 . . . ?
Na1 O3 C20 C15 -89.08(12) . . . . ?
Na1 O3 C20 C19 90.84(12) . . . . ?
Na1 O5 C28 C23 81.66(11) . . . . ?
Na1 O5 C28 C27 -96.02(10) . . . . ?
Na1 C28 C23 C22 43.24(12) . . . . ?
Na1 C28 C23 C24 -129.72(11) . . . . ?
Na1 C28 C27 O6 -54.56(11) . . . . ?
Na1 C28 C27 C26 126.31(12) . . . . ?
O1 C12 C7 C6 10.5(2) . . . . ?
O1 C12 C7 C8 -175.6(2) . . . . ?
O1 C12 C11 O2 -2.8(2) . . . . ?
O1 C12 C11 C10 177.7(2) . . . . ?
O2 C11 C10 C9 -179.9(3) . . . . ?
O2 C11 C12 C7 176.45(17) . . . . ?
O3 C20 C15 C14 -4.5(2) . . . . ?
O3 C20 C15 C16 178.87(16) . . . . ?
O3 C20 C19 O4 0.79(17) . . . . ?
O3 C20 C19 C18 179.05(15) . . . . ?
O4 C19 C18 C17 -179.99(17) . . . . ?
O4 C19 C20 C15 -179.29(14) . . . . ?
O5 C28 C23 C22 -7.20(19) . . . . ?
O5 C28 C23 C24 179.85(16) . . . . ?
O5 C28 C27 O6 -0.05(16) . . . . ?
O5 C28 C27 C26 -179.18(15) . . . . ?
O6 C27 C26 C25 179.62(17) . . . . ?
O6 C27 C28 C23 -177.86(14) . . . . ?
N1 C3 C2 C1 150.47(15) . . . . ?
N1 C3 C2 C4 32.28(16) . . . . ?
N1 C3 C2 C5 -93.33(15) . . . . ?
N1 C6 C7 C8 -158.9(2) . . . . ?
N1 C6 C7 C12 15.3(3) . . . . ?
N2 C4 C2 C1 157.27(16) . . . . ?
N2 C4 C2 C3 -84.57(17) . . . . ?
N2 C4 C2 C5 40.90(17) . . . . ?
N2 C14 C15 C16 151.9(2) . . . . ?
N2 C14 C15 C20 -24.9(2) . . . . ?
N3 C5 C2 C1 159.76(16) . . . . ?
N3 C5 C2 C3 43.05(17) . . . . ?
N3 C5 C2 C4 -83.33(16) . . . . ?
N3 C22 C23 C24 -167.17(19) . . . . ?
N3 C22 C23 C28 19.7(2) . . . . ?
C6 C7 C8 C9 170.4(3) . . . . ?
C6 C7 C12 C11 -168.7(2) . . . . ?
C7 C8 C9 C10 0.2(4) . . . . ?
C7 C12 C11 C10 -3.1(2) . . . . ?
C8 C9 C10 C11 1.9(4) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C14 C15 C16 C17 -174.66(16) . . . . ?
C14 C15 C20 C19 175.62(17) . . . . ?
C15 C16 C17 C18 -1.5(2) . . . . ?
C15 C20 C19 C18 -1.03(19) . . . . ?
C16 C17 C18 C19 -0.6(2) . . . . ?
C17 C18 C19 C20 1.9(2) . . . . ?
C22 C23 C24 C25 -173.15(16) . . . . ?
C22 C23 C28 C27 170.54(16) . . . . ?
C23 C24 C25 C26 1.5(2) . . . . ?
C23 C28 C27 C26 3.02(19) . . . . ?
C24 C25 C26 C27 -1.0(2) . . . . ?
C25 C26 C27 C28 -1.4(2) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.343
_oxdiff_exptl_absorpt_empirical_full_min 0.550
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_3105
_database_code_depnum_ccdc_archive 'CCDC 2307063'
loop_
_audit_author_name
_audit_author_address
'Rebecca A. Musgrave'
;Kings College London
United Kingdom
;
_audit_update_record             
;
2023-11-10 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_audit_creation_date             2023-08-22
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_chemical_formula_moiety         'C33 H33 Co F6 La N4 O12 S2'
_chemical_formula_sum            'C33 H33 Co F6 La N4 O12 S2'
_chemical_formula_weight         1053.611
_chemical_oxdiff_formula         'C33 H33 Co F6 La N4 O12 S2'
_chemical_oxdiff_usercomment     TN001
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Co -2.41037 3.56694 12.28410 7.34090 4.00340 2.34880 4.27910 0.27840 13.53590
71.16920 1.01180005074
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.07537 0.05506 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
La -1.32533 9.78168 20.57800 19.59900 11.37270 3.28719 2.94817 0.24448 18.77260
133.12399 2.14678001404
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.33537 0.55136 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   13.4835(1)
_cell_length_b                   12.9504(1)
_cell_length_c                   22.0541(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.320(1)
_cell_angle_gamma                90
_cell_volume                     3844.55(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    43763
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.3060
_cell_measurement_theta_min      3.9580
_exptl_absorpt_coefficient_mu    13.729
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       block
_exptl_crystal_F_000             2099.288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 7 7 0.0816
2 8 -4 0.0832
6 5 -6 0.0906
6 -2 9 0.1057
-6 2 -9 0.1046
-6 2 10 0.1105
2 -6 -9 0.0710
0 -7 7 0.1015
1 0 -14 0.1251
-2 -6 -8 0.0769
-3 -6 8 0.1079
-5 -4 -9 0.0860
-7 -2 8 0.0914
-9 -1 -1 0.0945
8 -3 -5 0.0742
-2 8 -3 0.0878
1 7 8 0.0898
6 4 8 0.0797
8 3 -6 0.0850
8 3 3 0.0790
5 -3 -11 0.0884
7 -5 -3 0.0950
0 -7 -7 0.0653

_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.155
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.3589 7.0421 7.0089 -0.2104 -0.8834 -0.4187
1.7213 7.9748 -3.6797 0.1538 -0.9180 0.3656
5.9540 5.1392 -6.3338 0.6147 -0.5637 0.5517
6.0896 -2.0327 9.0933 0.7824 0.1755 -0.5975
-5.9035 2.0187 -9.4226 -0.7642 -0.1715 0.6217
-5.9479 2.0363 10.4622 -0.5825 -0.3152 -0.7493
1.8836 -6.4595 -8.7926 0.1388 0.8272 0.5445
0.4748 -7.1586 7.3996 0.1309 0.7947 -0.5927
1.2997 0.2529 -14.2557 0.0141 0.0715 0.9973
-1.9251 -6.4661 -8.3939 -0.2920 0.8254 0.4832
-2.9068 -6.3278 8.3926 -0.2464 0.6895 -0.6811
-5.4549 -3.5433 -8.9025 -0.7026 0.4832 0.5224
-7.2958 -1.6462 8.0710 -0.7550 0.1379 -0.6410
-8.5084 -1.4379 -1.4814 -0.9834 0.1813 0.0093
7.7438 -3.1274 -4.7400 0.8423 0.4035 0.3575
-1.9766 8.0231 -2.5746 -0.2579 -0.9313 0.2572
1.4345 6.6182 8.3604 0.2356 -0.8431 -0.4834
5.5202 4.3751 7.7074 0.6979 -0.5732 -0.4294
7.7157 2.7987 -5.5072 0.8259 -0.2926 0.4820
8.0309 2.6313 2.7410 0.9395 -0.3316 -0.0859
5.0998 -3.0773 -10.8560 0.4830 0.4413 0.7563
6.5290 -5.4597 -2.7065 0.7251 0.6652 0.1783
0.1990 -7.2007 -7.3852 -0.0394 0.9050 0.4236

_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.9999
_diffrn_reflns_Laue_measured_fraction_max 0.9896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71163
_diffrn_reflns_point_group_measured_fraction_full 0.9999
_diffrn_reflns_point_group_measured_fraction_max 0.9896
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         72.54
_diffrn_reflns_theta_min         3.75
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9896
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  -5.00   1.00    1.61    --   22.00 118.00-132.48   25
  2  ω   -115.00 -20.00   1.00    1.61    --  -42.37 -38.00   0.00   95
  3  ω    -87.00  -7.00   1.00    1.61    --  -42.37 125.00 -90.00   80
  4  ω   -115.00 -21.00   1.00    1.61    --  -42.37 -38.00  90.00   94
  5  ω   -111.00 -18.00   1.00    1.61    --  -42.37 -38.00-180.00   93
  6  ω   -116.00 -30.00   1.00    1.61    --  -42.37 -38.00 -90.00   86
  7  ω     27.00  98.00   1.00    1.61    --   42.37-125.00 150.00   71
  8  ω      8.00  33.00   1.00    1.61    --   42.37  83.00  46.93   25
  9  ω     16.00  41.00   1.00    1.61    --   50.00  81.00 -68.27   25
 10  ω     16.00  42.00   1.00    1.61    --   50.00  82.00  64.88   26
 11  ω     16.00  41.00   1.00    1.61    --   50.00  81.00   0.42   25
 12  ω     16.00  42.00   1.00    1.61    --   50.00  81.00-145.59   26
 13  ω     16.00  41.00   1.00    1.61    --   50.00  82.00 137.03   25
 14  ω     36.00  61.00   1.00    1.61    --   66.00  70.00 170.07   25
 15  ω     35.00  64.00   1.00    1.61    --   66.00  71.00  51.69   29
 16  ω     35.00  62.00   1.00    1.61    --   66.00  69.00  26.90   27
 17  ω     39.00  65.00   1.00    1.61    --   70.00  69.00-168.43   26
 18  ω     39.00  64.00   1.00    1.61    --   70.00  71.00  91.43   25
 19  ω    100.00 143.00   1.00    1.61    --   70.00  71.00 -91.52   43
 20  ω     40.00  65.00   1.00    1.61    --   70.00  71.00-153.39   25
 21  ω    106.00 132.00   1.00    1.61    --   70.00  71.00 -40.88   26
 22  ω    110.00 140.00   1.00    1.61    --   70.00  71.00-153.39   30
 23  ω     39.00  66.00   1.00    1.61    --   70.00  69.00 121.03   27
 24  ω     39.00  65.00   1.00    1.61    --   70.00  71.00 -40.88   26
 25  ω     98.00 143.00   1.00    1.61    --   70.00  66.00  -5.59   45
 26  ω     40.00  66.00   1.00    1.61    --   70.00  66.00  -5.59   26
 27  ω     39.00  65.00   1.00    1.61    --   70.00  71.00 -91.52   26
 28  ω     40.00  67.00   1.00    1.61    --   70.00  70.00 -69.74   27
 29  ω     44.00  71.00   1.00    6.43    --   74.00  66.00 147.25   27
 30  ω     43.00  69.00   1.00    6.43    --   74.00  69.00-118.36   26
 31  ω     48.00  74.00   1.00    6.43    --   78.00  68.00  -5.79   26
 32  ω     51.00  77.00   1.00    6.43    --   82.00  70.00  18.94   26
 33  ω     57.00  86.00   1.00    6.43    --   86.00  61.00  72.52   29
 34  ω     55.00  82.00   1.00    6.43    --   86.00  70.00 -67.16   27
 35  ω    113.00 139.00   1.00    6.43    --   86.00  70.00  32.61   26
 36  ω     55.00  81.00   1.00    6.43    --   86.00  70.00  32.61   26
 37  ω     59.00  85.00   1.00    6.43    --   90.00  70.00-116.78   26
 38  ω     61.00  87.00   1.00    6.43    --   90.00  63.00-141.49   26
 39  ω     59.00  85.00   1.00    6.43    --   90.00  71.00 161.07   26
 40  ω     94.00 167.00   1.00    6.43    --   94.00  71.00  88.84   73
 41  ω     63.00  89.00   1.00    6.43    --   94.00  71.00  88.84   26
 42  ω     64.00 167.00   1.00    6.43    --   94.00  64.00  -9.90  103
 43  ω    134.00 171.00   1.00    6.43    --   98.00  65.00 111.61   37
 44  ω     68.00  94.00   1.00    6.43    --   98.00  65.00 111.61   26
 45  ω     71.00 174.00   1.00    6.43    --  102.00  71.00 163.64  103
 46  ω    106.00 162.00   1.00    6.43    --  103.86  65.00-109.63   56
 47  ω     89.00 117.00   1.00    6.43    --  103.86 -61.00-150.00   28
 48  ω     74.00  99.00   1.00    6.43    --  103.86  65.00-109.63   25
 49  ω     33.00  64.00   1.00    6.43    --  103.86 -61.00-150.00   31
 50  ω     75.00 125.00   1.00    6.43    --  103.86  61.00 -30.00   50
 51  ω     75.00 172.00   1.00    6.43    --  103.86  71.00-155.95   97
 52  ω    148.00 174.00   1.00    6.43    --  103.86  61.00 -90.00   26
 53  ω     77.00 102.00   1.00    6.43    --  103.86  61.00 -90.00   25
 54  ω     80.00 106.00   1.00    6.43    --  103.86 -95.00  30.00   26
 55  ω     33.00  63.00   1.00    6.43    --  103.86 -95.00  30.00   30
 56  ω     75.00 153.00   1.00    6.43    --  103.86  61.00  30.00   78
 57  ω     29.00  71.00   1.00    6.43    --  103.86 -77.00-180.00   42
 58  ω    103.00 130.00   1.00    6.43    --  103.86 -61.00  30.00   27
 59  ω     37.00  73.00   1.00    6.43    --  103.86 -61.00  30.00   36
 60  ω     25.00 106.00   1.00    6.43    --  103.86 -95.00 -90.00   81
 61  ω     75.00 174.00   1.00    6.43    --  103.86  61.00 -60.00   99
 62  ω     32.00 106.00   1.00    6.43    --  103.86 -95.00 120.00   74
 63  ω     36.00 101.00   1.00    6.43    --  103.86 -95.00   0.00   65
 64  ω     75.00 141.00   1.00    6.43    --  103.86  61.00 137.17   66
 65  ω    111.00 175.00   1.00    6.43    --  103.86  61.00  60.00   64
 66  ω     76.00 108.00   1.00    6.43    --  103.86  61.00  60.00   32
 67  ω     48.00 108.00   1.00    6.43    --  103.86-109.00-124.81   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1141120000
_diffrn_orient_matrix_UB_12      -0.0010099000
_diffrn_orient_matrix_UB_13      0.0093976000
_diffrn_orient_matrix_UB_21      -0.0000675000
_diffrn_orient_matrix_UB_22      -0.1183804000
_diffrn_orient_matrix_UB_23      -0.0071219000
_diffrn_orient_matrix_UB_31      0.0088646000
_diffrn_orient_matrix_UB_32      0.0121243000
_diffrn_orient_matrix_UB_33      -0.0689378000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -13
_reflns_number_gt                7322
_reflns_number_total             7553
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.4819
_refine_diff_density_min         -0.9890
_refine_diff_density_rms         0.0803
_refine_ls_d_res_high            0.8081
_refine_ls_d_res_low             11.7925
_refine_ls_goodness_of_fit_ref   1.0503
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0218
_refine_ls_restrained_S_all      1.0503
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+3.0656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0546
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18),
 C22(H22), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C13(H13a,H13b,H13c), C21(H21a,H21b,H21c), C29(H29a,H29b,
 H29c), C33(H33a,H33b,H33c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
La1 La 0.735002(7) 0.719491(8) 0.393855(5) 0.01064(4) Uani 1.000000 .
Co1 Co 0.50352(2) 0.66194(2) 0.339351(14) 0.01003(7) Uani 1.000000 .
S1 S 0.78257(4) 0.75860(4) 0.57060(2) 0.01479(10) Uani 1.000000 .
S2 S 1.02062(3) 0.75293(4) 0.39370(2) 0.01824(10) Uani 1.000000 .
F1 F 0.84980(10) 0.56871(10) 0.57835(6) 0.0281(3) Uani 1.000000 .
F2 F 0.91689(12) 0.67266(12) 0.64433(7) 0.0394(4) Uani 1.000000 .
F3 F 0.95592(10) 0.68032(13) 0.55119(8) 0.0418(4) Uani 1.000000 .
F4 F 1.05474(14) 0.86186(16) 0.49267(7) 0.0532(5) Uani 1.000000 .
F5 F 1.03618(16) 0.95089(13) 0.41274(10) 0.0603(5) Uani 1.000000 .
F6 F 1.17131(12) 0.86443(18) 0.43122(10) 0.0629(6) Uani 1.000000 .
O1 O 0.61870(10) 0.58082(10) 0.38492(6) 0.0138(3) Uani 1.000000 .
O2 O 0.78610(10) 0.53595(10) 0.44184(7) 0.0158(3) Uani 1.000000 .
O3 O 0.62706(11) 0.72704(11) 0.30199(7) 0.0171(3) Uani 1.000000 .
O4 O 0.78501(11) 0.83000(12) 0.28814(7) 0.0223(3) Uani 1.000000 .
O5 O 0.55967(10) 0.77291(10) 0.40374(6) 0.0123(3) Uani 1.000000 .
O6 O 0.69840(10) 0.90857(11) 0.42847(7) 0.0176(3) Uani 1.000000 .
O7 O 0.74998(12) 0.73277(12) 0.50836(7) 0.0237(3) Uani 1.000000 .
O8 O 0.71101(13) 0.73475(13) 0.61391(8) 0.0281(4) Uani 1.000000 .
O9 O 0.83111(13) 0.85618(12) 0.57762(8) 0.0292(4) Uani 1.000000 .
O10 O 0.91519(11) 0.76446(12) 0.40477(8) 0.0213(3) Uani 1.000000 .
O11 O 1.06639(13) 0.66545(14) 0.42298(10) 0.0405(5) Uani 1.000000 .
O12 O 1.04387(14) 0.77127(16) 0.33252(9) 0.0364(4) Uani 1.000000 .
N1 N 0.41103(12) 0.54636(13) 0.37014(8) 0.0153(3) Uani 1.000000 .
N2 N 0.46560(12) 0.60864(13) 0.24987(8) 0.0157(3) Uani 1.000000 .
N3 N 0.37783(12) 0.75694(14) 0.32679(8) 0.0138(3) Uani 1.000000 .
N4 N 0.82952(14) 0.59972(14) 0.31392(9) 0.0216(4) Uani 1.000000 .
C1 C 0.18815(16) 0.5684(2) 0.25832(12) 0.0298(6) Uani 1.000000 .
H1a H 0.1857(4) 0.4937(3) 0.2513(8) 0.0447(8) Uiso 1.000000 GR
H1b H 0.1389(2) 0.5874(14) 0.2873(4) 0.0447(8) Uiso 1.000000 GR
H1c H 0.1734(6) 0.6047(11) 0.2198(5) 0.0447(8) Uiso 1.000000 GR
C2 C 0.29228(15) 0.59881(17) 0.28415(10) 0.0194(4) Uani 1.000000 .
C3 C 0.30619(15) 0.55212(18) 0.34767(10) 0.0208(4) Uani 1.000000 .
H3a H 0.27751(15) 0.48173(18) 0.34706(10) 0.0250(5) Uiso 1.000000 R
H3b H 0.26909(15) 0.59426(18) 0.37619(10) 0.0250(5) Uiso 1.000000 R
C4 C 0.36930(15) 0.55517(18) 0.24181(10) 0.0213(5) Uani 1.000000 .
H4a H 0.34347(15) 0.56245(18) 0.19908(10) 0.0256(5) Uiso 1.000000 R
H4b H 0.37902(15) 0.48067(18) 0.25027(10) 0.0256(5) Uiso 1.000000 R
C5 C 0.29612(16) 0.71734(16) 0.28627(10) 0.0194(5) Uani 1.000000 .
H5a H 0.23235(16) 0.74370(16) 0.30015(10) 0.0232(5) Uiso 1.000000 R
H5b H 0.30383(16) 0.74401(16) 0.24474(10) 0.0232(5) Uiso 1.000000 R
C6 C 0.43436(15) 0.46796(16) 0.40353(10) 0.0173(4) Uani 1.000000 .
H6 H 0.38244(15) 0.42045(16) 0.41025(10) 0.0207(5) Uiso 1.000000 R
C7 C 0.53091(15) 0.44373(15) 0.43214(9) 0.0149(4) Uani 1.000000 .
C8 C 0.53787(16) 0.35873(16) 0.47205(10) 0.0191(4) Uani 1.000000 .
H8 H 0.48013(16) 0.31900(16) 0.47834(10) 0.0230(5) Uiso 1.000000 R
C9 C 0.62622(17) 0.33203(16) 0.50206(10) 0.0207(4) Uani 1.000000 .
H9 H 0.62907(17) 0.27439(16) 0.52874(10) 0.0248(5) Uiso 1.000000 R
C10 C 0.71219(16) 0.38968(16) 0.49339(9) 0.0183(4) Uani 1.000000 .
H10 H 0.77344(16) 0.37190(16) 0.51424(9) 0.0220(5) Uiso 1.000000 R
C11 C 0.70654(15) 0.47259(15) 0.45415(9) 0.0136(4) Uani 1.000000 .
C12 C 0.61716(14) 0.50155(14) 0.42258(9) 0.0119(4) Uani 1.000000 .
C13 C 0.88276(15) 0.48744(17) 0.44544(11) 0.0208(4) Uani 1.000000 .
H13a H 0.8818(4) 0.4271(8) 0.4186(6) 0.0312(7) Uiso 1.000000 GR
H13b H 0.9327(2) 0.5368(4) 0.4328(7) 0.0312(7) Uiso 1.000000 GR
H13c H 0.8994(6) 0.4656(12) 0.48735(18) 0.0312(7) Uiso 1.000000 GR
C14 C 0.50829(15) 0.63066(16) 0.20114(9) 0.0165(4) Uani 1.000000 .
H14 H 0.47519(15) 0.60912(16) 0.16409(9) 0.0198(5) Uiso 1.000000 R
C15 C 0.60171(15) 0.68492(16) 0.19627(9) 0.0159(4) Uani 1.000000 .
C16 C 0.63895(18) 0.69407(18) 0.13828(10) 0.0237(5) Uani 1.000000 .
H16 H 0.60316(18) 0.66414(18) 0.10431(10) 0.0285(6) Uiso 1.000000 R
C17 C 0.7258(2) 0.7453(2) 0.12992(11) 0.0293(5) Uani 1.000000 .
H17 H 0.7506(2) 0.7484(2) 0.09052(11) 0.0352(6) Uiso 1.000000 R
C18 C 0.77854(19) 0.79330(18) 0.17873(12) 0.0267(5) Uani 1.000000 .
H18 H 0.83824(19) 0.82985(18) 0.17265(12) 0.0320(6) Uiso 1.000000 R
C19 C 0.74226(16) 0.78649(15) 0.23571(11) 0.0184(4) Uani 1.000000 .
C20 C 0.65463(15) 0.73072(15) 0.24597(9) 0.0135(4) Uani 1.000000 .
C21 C 0.86032(18) 0.9069(2) 0.28012(14) 0.0340(6) Uani 1.000000 .
H21a H 0.8789(11) 0.9392(11) 0.3193(2) 0.0510(9) Uiso 1.000000 GR
H21b H 0.9189(6) 0.8741(3) 0.2641(9) 0.0510(9) Uiso 1.000000 GR
H21c H 0.8345(5) 0.9596(9) 0.2515(7) 0.0510(9) Uiso 1.000000 GR
C22 C 0.36170(14) 0.84277(15) 0.35335(9) 0.0140(4) Uani 1.000000 .
H22 H 0.29566(14) 0.86855(15) 0.34963(9) 0.0167(5) Uiso 1.000000 R
C23 C 0.43387(15) 0.90461(15) 0.38850(9) 0.0139(4) Uani 1.000000 .
C24 C 0.40793(16) 1.00831(16) 0.39928(10) 0.0199(4) Uani 1.000000 .
H24 H 0.34131(16) 1.03012(16) 0.39073(10) 0.0239(5) Uiso 1.000000 R
C25 C 0.47693(18) 1.07818(17) 0.42185(11) 0.0251(5) Uani 1.000000 .
H25 H 0.45756(18) 1.14710(17) 0.42998(11) 0.0301(6) Uiso 1.000000 R
C26 C 0.57604(17) 1.04785(16) 0.43291(11) 0.0223(5) Uani 1.000000 .
H26 H 0.62493(17) 1.09654(16) 0.44679(11) 0.0267(6) Uiso 1.000000 R
C27 C 0.60165(15) 0.94619(15) 0.42335(9) 0.0148(4) Uani 1.000000 .
C28 C 0.53143(14) 0.87037(14) 0.40520(8) 0.0111(4) Uani 1.000000 .
C29 C 0.77311(17) 0.97655(17) 0.45549(12) 0.0253(5) Uani 1.000000 .
H29a H 0.7536(7) 0.9985(11) 0.4956(4) 0.0380(8) Uiso 1.000000 GR
H29b H 0.8368(3) 0.9401(5) 0.4597(8) 0.0380(8) Uiso 1.000000 GR
H29c H 0.7797(10) 1.0373(7) 0.4295(4) 0.0380(8) Uiso 1.000000 GR
C30 C 0.88125(16) 0.66515(17) 0.58694(10) 0.0207(4) Uani 1.000000 .
C31 C 1.07338(18) 0.8634(2) 0.43496(11) 0.0286(5) Uani 1.000000 .
C32 C 0.87122(16) 0.55414(17) 0.27943(10) 0.0211(5) Uani 1.000000 .
C33 C 0.9250(2) 0.4957(2) 0.23566(15) 0.0455(8) Uani 1.000000 .
H33a H 0.8781(3) 0.4537(14) 0.2106(7) 0.0683(12) Uiso 1.000000 GR
H33b H 0.9595(14) 0.5435(3) 0.2096(7) 0.0683(12) Uiso 1.000000 GR
H33c H 0.9736(12) 0.4506(14) 0.25722(15) 0.0683(12) Uiso 1.000000 GR


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 Co1 3.3627(3) . ?
La1 O1 2.3848(13) . ?
La1 O2 2.6758(13) . ?
La1 O3 2.4272(15) . ?
La1 O4 2.8497(15) . ?
La1 O5 2.4849(14) . ?
La1 O6 2.6203(14) . ?
La1 O7 2.5275(16) . ?
La1 O10 2.4964(14) . ?
La1 N4 2.7200(19) . ?
La1 C12 3.3180(19) . ?
Co1 O1 2.0844(13) . ?
Co1 O3 2.0794(14) . ?
Co1 O5 2.1286(14) . ?
Co1 N1 2.0867(17) . ?
Co1 N2 2.1249(17) . ?
Co1 N3 2.0995(17) . ?
S1 O7 1.4558(16) . ?
S1 O8 1.4302(17) . ?
S1 O9 1.4274(16) . ?
S1 C30 1.819(2) . ?
S2 O10 1.4640(15) . ?
S2 O11 1.4266(18) . ?
S2 O12 1.423(2) . ?
S2 C31 1.818(2) . ?
F1 C30 1.329(3) . ?
F2 C30 1.331(3) . ?
F3 C30 1.329(3) . ?
F4 C31 1.312(3) . ?
F5 C31 1.322(3) . ?
F6 C31 1.328(3) . ?
O1 C12 1.321(2) . ?
O2 C11 1.390(2) . ?
O2 C13 1.445(2) . ?
O3 C20 1.311(3) . ?
O4 C19 1.382(3) . ?
O4 C21 1.440(3) . ?
O5 C28 1.319(2) . ?
O6 C27 1.391(2) . ?
O6 C29 1.441(2) . ?
N1 C3 1.472(3) . ?
N1 C6 1.283(3) . ?
N2 C4 1.473(3) . ?
N2 C14 1.280(3) . ?
N3 C5 1.470(3) . ?
N3 C22 1.281(3) . ?
N4 C32 1.137(3) . ?
C1 H1a 0.9800 . ?
C1 H1b 0.9800 . ?
C1 H1c 0.9800 . ?
C1 C2 1.536(3) . ?
C2 C3 1.527(3) . ?
C2 C4 1.543(3) . ?
C2 C5 1.537(3) . ?
C3 H3a 0.9900 . ?
C3 H3b 0.9900 . ?
C4 H4a 0.9900 . ?
C4 H4b 0.9900 . ?
C5 H5a 0.9900 . ?
C5 H5b 0.9900 . ?
C6 H6 0.9500 . ?
C6 C7 1.448(3) . ?
C7 C8 1.409(3) . ?
C7 C12 1.409(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.373(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.401(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(3) . ?
C11 C12 1.407(3) . ?
C13 H13a 0.9800 . ?
C13 H13b 0.9800 . ?
C13 H13c 0.9800 . ?
C14 H14 0.9500 . ?
C14 C15 1.452(3) . ?
C15 C16 1.406(3) . ?
C15 C20 1.404(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.367(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.401(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.377(3) . ?
C19 C20 1.414(3) . ?
C21 H21a 0.9800 . ?
C21 H21b 0.9800 . ?
C21 H21c 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.450(3) . ?
C23 C24 1.411(3) . ?
C23 C28 1.417(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.370(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.401(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.380(3) . ?
C27 C28 1.406(3) . ?
C29 H29a 0.9800 . ?
C29 H29b 0.9800 . ?
C29 H29c 0.9800 . ?
C32 C33 1.453(3) . ?
C33 H33a 0.9800 . ?
C33 H33b 0.9800 . ?
C33 H33c 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 Co1 37.93(3) . . ?
O2 La1 Co1 99.03(3) . . ?
O2 La1 O1 61.10(4) . . ?
O3 La1 Co1 37.93(3) . . ?
O3 La1 O1 66.53(5) . . ?
O3 La1 O2 119.61(5) . . ?
O4 La1 Co1 94.45(3) . . ?
O4 La1 O1 119.75(5) . . ?
O4 La1 O2 134.59(4) . . ?
O4 La1 O3 57.02(4) . . ?
O5 La1 Co1 39.19(3) . . ?
O5 La1 O1 65.95(4) . . ?
O5 La1 O2 115.92(4) . . ?
O5 La1 O3 62.26(5) . . ?
O5 La1 O4 101.74(4) . . ?
O6 La1 Co1 97.16(3) . . ?
O6 La1 O1 126.43(4) . . ?
O6 La1 O2 139.77(5) . . ?
O6 La1 O3 95.26(5) . . ?
O6 La1 O4 80.01(5) . . ?
O6 La1 O5 61.19(4) . . ?
O7 La1 Co1 113.02(4) . . ?
O7 La1 O1 98.51(5) . . ?
O7 La1 O2 70.21(5) . . ?
O7 La1 O3 147.21(5) . . ?
O7 La1 O4 140.73(5) . . ?
O7 La1 O5 85.11(5) . . ?
O7 La1 O6 69.56(5) . . ?
O10 La1 Co1 164.62(4) . . ?
O10 La1 O1 144.61(5) . . ?
O10 La1 O2 86.69(5) . . ?
O10 La1 O3 127.18(5) . . ?
O10 La1 O4 71.74(5) . . ?
O10 La1 O5 148.44(5) . . ?
O10 La1 O6 87.28(5) . . ?
O10 La1 O7 82.34(5) . . ?
N4 La1 Co1 95.85(4) . . ?
N4 La1 O1 81.23(5) . . ?
N4 La1 O2 68.30(5) . . ?
N4 La1 O3 76.28(5) . . ?
N4 La1 O4 67.30(5) . . ?
N4 La1 O5 134.39(5) . . ?
N4 La1 O6 145.58(5) . . ?
N4 La1 O7 132.30(5) . . ?
N4 La1 O10 72.88(5) . . ?
C12 La1 Co1 55.59(3) . . ?
C12 La1 O1 19.15(5) . . ?
C12 La1 O2 44.28(4) . . ?
C12 La1 O3 85.59(5) . . ?
C12 La1 O4 136.23(5) . . ?
C12 La1 O5 75.61(4) . . ?
C12 La1 O6 129.71(5) . . ?
C12 La1 O7 83.02(5) . . ?
C12 La1 O10 130.86(5) . . ?
C12 La1 N4 83.47(5) . . ?
O1 Co1 La1 44.69(4) . . ?
O3 Co1 La1 45.85(4) . . ?
O3 Co1 O1 78.68(6) . . ?
O5 Co1 La1 47.54(4) . . ?
O5 Co1 O1 78.01(5) . . ?
O5 Co1 O3 74.24(6) . . ?
N1 Co1 La1 127.05(5) . . ?
N1 Co1 O1 85.66(6) . . ?
N1 Co1 O3 158.02(6) . . ?
N1 Co1 O5 117.60(6) . . ?
N2 Co1 La1 124.92(5) . . ?
N2 Co1 O1 114.61(6) . . ?
N2 Co1 O3 85.35(6) . . ?
N2 Co1 O5 153.65(6) . . ?
N2 Co1 N1 87.31(7) . . ?
N3 Co1 La1 129.99(5) . . ?
N3 Co1 O1 158.77(6) . . ?
N3 Co1 O3 111.66(6) . . ?
N3 Co1 O5 86.88(6) . . ?
N3 Co1 N1 88.30(7) . . ?
N3 Co1 N2 85.34(7) . . ?
O8 S1 O7 113.68(10) . . ?
O9 S1 O7 114.65(10) . . ?
O9 S1 O8 116.20(11) . . ?
C30 S1 O7 102.20(10) . . ?
C30 S1 O8 103.77(10) . . ?
C30 S1 O9 104.00(10) . . ?
O11 S2 O10 113.84(11) . . ?
O12 S2 O10 114.25(11) . . ?
O12 S2 O11 116.66(13) . . ?
C31 S2 O10 101.06(10) . . ?
C31 S2 O11 104.57(12) . . ?
C31 S2 O12 104.01(12) . . ?
Co1 O1 La1 97.37(5) . . ?
C12 O1 La1 124.56(12) . . ?
C12 O1 Co1 131.01(12) . . ?
C11 O2 La1 114.69(11) . . ?
C13 O2 La1 128.23(12) . . ?
C13 O2 C11 115.89(15) . . ?
Co1 O3 La1 96.22(6) . . ?
C20 O3 La1 126.79(12) . . ?
C20 O3 Co1 131.71(13) . . ?
C19 O4 La1 111.89(11) . . ?
C21 O4 La1 130.51(14) . . ?
C21 O4 C19 116.23(18) . . ?
Co1 O5 La1 93.27(5) . . ?
C28 O5 La1 123.09(12) . . ?
C28 O5 Co1 124.76(12) . . ?
C27 O6 La1 119.68(11) . . ?
C29 O6 La1 123.55(12) . . ?
C29 O6 C27 116.72(16) . . ?
S1 O7 La1 163.74(11) . . ?
S2 O10 La1 155.38(10) . . ?
C3 N1 Co1 115.75(13) . . ?
C6 N1 Co1 128.56(14) . . ?
C6 N1 C3 115.59(17) . . ?
C4 N2 Co1 115.33(13) . . ?
C14 N2 Co1 127.70(14) . . ?
C14 N2 C4 116.06(17) . . ?
C5 N3 Co1 116.52(13) . . ?
C22 N3 Co1 127.25(14) . . ?
C22 N3 C5 116.07(17) . . ?
C32 N4 La1 176.48(17) . . ?
H1b C1 H1a 109.5 . . ?
H1c C1 H1a 109.5 . . ?
H1c C1 H1b 109.5 . . ?
C2 C1 H1a 109.5 . . ?
C2 C1 H1b 109.5 . . ?
C2 C1 H1c 109.5 . . ?
C3 C2 C1 107.44(18) . . ?
C4 C2 C1 108.33(17) . . ?
C4 C2 C3 111.03(18) . . ?
C5 C2 C1 107.22(19) . . ?
C5 C2 C3 111.44(18) . . ?
C5 C2 C4 111.19(19) . . ?
C2 C3 N1 113.15(17) . . ?
H3a C3 N1 108.95(11) . . ?
H3a C3 C2 108.95(11) . . ?
H3b C3 N1 108.95(11) . . ?
H3b C3 C2 108.95(12) . . ?
H3b C3 H3a 107.8 . . ?
C2 C4 N2 111.97(16) . . ?
H4a C4 N2 109.22(11) . . ?
H4a C4 C2 109.22(12) . . ?
H4b C4 N2 109.22(11) . . ?
H4b C4 C2 109.22(13) . . ?
H4b C4 H4a 107.9 . . ?
C2 C5 N3 112.94(17) . . ?
H5a C5 N3 109.00(11) . . ?
H5a C5 C2 109.00(11) . . ?
H5b C5 N3 109.00(11) . . ?
H5b C5 C2 109.00(12) . . ?
H5b C5 H5a 107.8 . . ?
H6 C6 N1 116.35(11) . . ?
C7 C6 N1 127.31(18) . . ?
C7 C6 H6 116.35(11) . . ?
C8 C7 C6 117.85(18) . . ?
C12 C7 C6 123.28(18) . . ?
C12 C7 C8 118.87(19) . . ?
H8 C8 C7 119.26(12) . . ?
C9 C8 C7 121.49(19) . . ?
C9 C8 H8 119.26(12) . . ?
H9 C9 C8 119.95(12) . . ?
C10 C9 C8 120.10(19) . . ?
C10 C9 H9 119.95(12) . . ?
H10 C10 C9 120.51(12) . . ?
C11 C10 C9 119.0(2) . . ?
C11 C10 H10 120.51(12) . . ?
C10 C11 O2 124.56(18) . . ?
C12 C11 O2 113.25(17) . . ?
C12 C11 C10 122.19(19) . . ?
O1 C12 La1 36.29(8) . . ?
C7 C12 La1 152.75(13) . . ?
C7 C12 O1 123.36(18) . . ?
C11 C12 La1 85.14(11) . . ?
C11 C12 O1 118.28(17) . . ?
C11 C12 C7 118.36(18) . . ?
H13a C13 O2 109.5 . . ?
H13b C13 O2 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 O2 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?
H14 C14 N2 116.42(12) . . ?
C15 C14 N2 127.16(19) . . ?
C15 C14 H14 116.42(11) . . ?
C16 C15 C14 117.7(2) . . ?
C20 C15 C14 123.40(18) . . ?
C20 C15 C16 118.8(2) . . ?
H16 C16 C15 119.42(14) . . ?
C17 C16 C15 121.2(2) . . ?
C17 C16 H16 119.42(14) . . ?
H17 C17 C16 119.59(14) . . ?
C18 C17 C16 120.8(2) . . ?
C18 C17 H17 119.59(14) . . ?
H18 C18 C17 120.62(14) . . ?
C19 C18 C17 118.8(2) . . ?
C19 C18 H18 120.62(15) . . ?
C18 C19 O4 125.7(2) . . ?
C20 C19 O4 112.72(19) . . ?
C20 C19 C18 121.5(2) . . ?
C15 C20 O3 124.13(18) . . ?
C19 C20 O3 117.02(19) . . ?
C19 C20 C15 118.83(19) . . ?
H21a C21 O4 109.5 . . ?
H21b C21 O4 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 O4 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H22 C22 N3 116.66(11) . . ?
C23 C22 N3 126.68(18) . . ?
C23 C22 H22 116.66(11) . . ?
C24 C23 C22 116.78(18) . . ?
C28 C23 C22 123.41(18) . . ?
C28 C23 C24 119.30(19) . . ?
H24 C24 C23 119.34(12) . . ?
C25 C24 C23 121.3(2) . . ?
C25 C24 H24 119.34(13) . . ?
H25 C25 C24 120.04(13) . . ?
C26 C25 C24 119.9(2) . . ?
C26 C25 H25 120.04(13) . . ?
H26 C26 C25 120.48(13) . . ?
C27 C26 C25 119.0(2) . . ?
C27 C26 H26 120.48(13) . . ?
C26 C27 O6 124.28(18) . . ?
C28 C27 O6 113.05(17) . . ?
C28 C27 C26 122.63(19) . . ?
C23 C28 O5 123.93(17) . . ?
C27 C28 O5 118.97(17) . . ?
C27 C28 C23 117.09(17) . . ?
H29a C29 O6 109.5 . . ?
H29b C29 O6 109.5 . . ?
H29b C29 H29a 109.5 . . ?
H29c C29 O6 109.5 . . ?
H29c C29 H29a 109.5 . . ?
H29c C29 H29b 109.5 . . ?
F1 C30 S1 111.91(15) . . ?
F2 C30 S1 111.07(16) . . ?
F2 C30 F1 107.40(18) . . ?
F3 C30 S1 110.77(15) . . ?
F3 C30 F1 107.50(19) . . ?
F3 C30 F2 108.01(19) . . ?
F4 C31 S2 112.51(17) . . ?
F5 C31 S2 111.09(17) . . ?
F5 C31 F4 106.4(2) . . ?
F6 C31 S2 109.80(19) . . ?
F6 C31 F4 107.9(2) . . ?
F6 C31 F5 109.0(2) . . ?
C33 C32 N4 179.6(3) . . ?
H33a C33 C32 109.5 . . ?
H33b C33 C32 109.5 . . ?
H33b C33 H33a 109.5 . . ?
H33c C33 C32 109.5 . . ?
H33c C33 H33a 109.5 . . ?
H33c C33 H33b 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La1 O1 C12 C7 154.38(14) . . . . ?
La1 O1 C12 C11 -26.49(15) . . . . ?
La1 O2 C11 C10 -160.86(13) . . . . ?
La1 O2 C11 C12 18.71(12) . . . . ?
La1 O3 C20 C15 146.31(15) . . . . ?
La1 O3 C20 C19 -35.04(15) . . . . ?
La1 O4 C19 C18 -153.52(14) . . . . ?
La1 O4 C19 C20 25.76(12) . . . . ?
La1 O5 C28 C23 155.68(14) . . . . ?
La1 O5 C28 C27 -23.24(15) . . . . ?
La1 O6 C27 C26 -171.45(16) . . . . ?
La1 O6 C27 C28 6.50(13) . . . . ?
La1 O7 S1 O8 166.2(3) . . . . ?
La1 O7 S1 O9 29.2(4) . . . . ?
La1 O7 S1 C30 -82.6(3) . . . . ?
La1 O10 S2 O11 -72.3(3) . . . . ?
La1 O10 S2 O12 65.2(3) . . . . ?
La1 O10 S2 C31 176.2(2) . . . . ?
La1 C12 O1 Co1 -143.65(15) . . . . ?
La1 C12 C7 C6 31.4(3) . . . . ?
La1 C12 C7 C8 -147.8(3) . . . . ?
La1 C12 C11 O2 -13.64(10) . . . . ?
La1 C12 C11 C10 165.94(11) . . . . ?
Co1 O1 C12 C7 10.73(17) . . . . ?
Co1 O1 C12 C11 -170.14(16) . . . . ?
Co1 O3 C20 C15 -1.63(19) . . . . ?
Co1 O3 C20 C19 177.02(17) . . . . ?
Co1 O5 C28 C23 33.34(16) . . . . ?
Co1 O5 C28 C27 -145.58(15) . . . . ?
Co1 N1 C3 C2 31.10(14) . . . . ?
Co1 N1 C6 C7 4.8(2) . . . . ?
Co1 N2 C4 C2 32.53(15) . . . . ?
Co1 N2 C14 C15 10.0(2) . . . . ?
Co1 N3 C5 C2 27.65(15) . . . . ?
Co1 N3 C22 C23 13.7(2) . . . . ?
O1 C12 C7 C6 -2.6(2) . . . . ?
O1 C12 C7 C8 178.23(19) . . . . ?
O1 C12 C11 O2 1.72(19) . . . . ?
O1 C12 C11 C10 -178.70(17) . . . . ?
O2 C11 C10 C9 179.74(19) . . . . ?
O2 C11 C12 C7 -179.10(16) . . . . ?
O3 C20 C15 C14 2.0(2) . . . . ?
O3 C20 C15 C16 -179.9(2) . . . . ?
O3 C20 C19 O4 -0.59(19) . . . . ?
O3 C20 C19 C18 178.72(18) . . . . ?
O4 C19 C18 C17 -179.5(2) . . . . ?
O4 C19 C20 C15 178.13(16) . . . . ?
O5 C28 C23 C22 -16.8(2) . . . . ?
O5 C28 C23 C24 171.7(2) . . . . ?
O5 C28 C27 O6 9.7(2) . . . . ?
O5 C28 C27 C26 -172.28(19) . . . . ?
O6 C27 C26 C25 175.1(2) . . . . ?
O6 C27 C28 C23 -169.26(16) . . . . ?
N1 C3 C2 C1 161.79(19) . . . . ?
N1 C3 C2 C4 43.50(19) . . . . ?
N1 C3 C2 C5 -81.03(19) . . . . ?
N1 C6 C7 C8 173.7(2) . . . . ?
N1 C6 C7 C12 -5.4(3) . . . . ?
N2 C4 C2 C1 160.2(2) . . . . ?
N2 C4 C2 C3 -82.1(2) . . . . ?
N2 C4 C2 C5 42.6(2) . . . . ?
N2 C14 C15 C16 175.3(2) . . . . ?
N2 C14 C15 C20 -6.6(3) . . . . ?
N3 C5 C2 C1 161.97(19) . . . . ?
N3 C5 C2 C3 44.7(2) . . . . ?
N3 C5 C2 C4 -79.79(19) . . . . ?
N3 C22 C23 C24 162.8(2) . . . . ?
N3 C22 C23 C28 -8.9(3) . . . . ?
C6 C7 C8 C9 -178.51(19) . . . . ?
C6 C7 C12 C11 178.24(19) . . . . ?
C7 C8 C9 C10 0.0(2) . . . . ?
C7 C12 C11 C10 0.5(2) . . . . ?
C8 C9 C10 C11 -0.4(2) . . . . ?
C9 C10 C11 C12 0.2(2) . . . . ?
C14 C15 C16 C17 179.1(2) . . . . ?
C14 C15 C20 C19 -176.67(19) . . . . ?
C15 C16 C17 C18 -2.2(3) . . . . ?
C15 C20 C19 C18 -2.6(2) . . . . ?
C16 C17 C18 C19 1.1(3) . . . . ?
C17 C18 C19 C20 1.3(3) . . . . ?
C22 C23 C24 C25 -167.7(2) . . . . ?
C22 C23 C28 C27 162.1(2) . . . . ?
C23 C24 C25 C26 1.9(3) . . . . ?
C23 C28 C27 C26 8.7(2) . . . . ?
C24 C25 C26 C27 -2.9(3) . . . . ?
C25 C26 C27 C28 -2.6(3) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.873
_oxdiff_exptl_absorpt_empirical_full_min 0.723
