#------------------------------------------------------------------------------
#$Date: 2025-07-06 17:06:59 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300709 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/01/7250136.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7250136
loop_
_publ_author_name
'Feng, Yuying'
'Hua, Carol'
'van Koeverden, Martin P.'
_publ_section_title
;
 The effect of viologen counterions on the topologies of
 La(iii)--tetraoxolene metal--organic frameworks
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2559
_journal_page_last               2569
_journal_paper_doi               10.1039/D5CE00026B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C15 Cl5 La O10, C12 H12 N2, 3(H2 O)'
_chemical_formula_sum            'C27 H18 Cl5 La N2 O13'
_chemical_formula_weight         894.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.089(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7957(3)
_cell_length_b                   26.3110(5)
_cell_length_c                   10.5813(3)
_cell_measurement_reflns_used    12510
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.1670
_cell_measurement_theta_min      3.3460
_cell_volume                     3121.67(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     47.00  81.00   0.50    0.20    --  111.50-125.00  30.00   68
  2  ω     86.00 111.00   0.50    0.20    --  111.50-125.00  30.00   50
  3  ω     34.00  93.00   0.50    0.10    --   48.11-125.00 -30.00  118
  4  ω     41.00  85.00   0.50    0.10    --   48.11-125.00 -90.00   88
  5  ω     43.00 110.00   0.50    0.20    --  111.50-125.00-180.00  134
  6  ω     76.00 106.00   0.50    0.20    --  111.50-102.00 -55.35   60
  7  ω     58.00 107.00   0.50    0.20    --  111.50-125.00   0.00   98
  8  ω     82.00 107.00   0.50    0.20    --  111.50-102.00  30.22   50
  9  ω     46.00  72.00   0.50    0.20    --  111.50-102.00 -55.35   52
 10  ω     43.00  78.00   0.50    0.20    --  111.50-102.00  30.22   70
 11  ω     45.00 100.00   0.50    0.20    --  111.50 -94.00  30.00  110
 12  ω     77.00 106.00   0.50    0.20    --  111.50-103.00  84.75   58
 13  ω     48.00  73.00   0.50    0.20    --  111.50-103.00  84.75   50
 14  ω     58.00 107.00   0.50    0.20    --  111.50-112.00 177.42   98
 15  ω     77.00 102.00   0.50    0.20    --  111.50 -94.00 -30.00   50
 16  ω     42.00  70.00   0.50    0.20    --  111.50 -94.00 -30.00   56
 17  ω     53.00  95.00   0.50    0.20    --  111.50 -94.00 -90.00   84
 18  ω     41.00  67.00   0.50    0.20    --  111.50 -94.00-120.00   52
 19  ω     51.00 105.00   0.50    0.20    --  111.50 -94.00-150.00  108
 20  ω     79.00 105.00   0.50    0.20    --  111.50 -94.00-180.00   52
 21  ω     42.00  73.00   0.50    0.20    --  111.50 -94.00-180.00   62
 22  ω     76.00 102.00   0.50    0.20    --  111.50 -94.00-120.00   52
 23  ω     81.00 106.00   0.50    0.20    --  111.50 -93.00  71.15   50
 24  ω     79.00 104.00   0.50    0.20    --  111.50 -94.00 150.00   50
 25  ω     40.00  66.00   0.50    0.20    --  111.50 -93.00  71.15   52
 26  ω     -1.00  27.00   0.50    0.10    --   48.11 -19.00 -90.00   56
 27  ω     53.00  86.00   0.50    0.20    --  111.50 -77.00  60.00   66
 28  ω     41.00  69.00   0.50    0.20    --  111.50 -77.00  90.00   56
 29  ω     40.00  65.00   0.50    0.20    --  111.50 -61.00  90.00   50
 30  ω     40.00  65.00   0.50    0.20    --  111.50 -61.00  60.00   50
 31  ω     40.00  68.00   0.50    0.20    --  111.50 -61.00-120.00   56
 32  ω     40.00  69.00   0.50    0.20    --  111.50 -77.00-180.00   58
 33  ω     45.00  71.00   0.50    0.20    --  111.50 -61.00-150.00   52
 34  ω     41.00  67.00   0.50    0.20    --  111.50 -61.00 -90.00   52
 35  ω     43.00  71.00   0.50    0.20    --  111.50 -61.00 -60.00   56
 36  ω    102.00 153.00   0.50    0.20    --  111.50  15.00  30.00  102
 37  ω     99.00 146.00   0.50    0.20    --  111.50  61.00  90.00   94
 38  ω    102.00 140.00   0.50    0.20    --  111.50  45.00-120.00   76
 39  ω    101.00 151.00   0.50    0.20    --  111.50  30.00-180.00  100
 40  ω    118.00 144.00   0.50    0.20    --  111.50  61.00-180.00   52
 41  ω    149.00 178.00   0.50    0.20    --  111.50  61.00-180.00   58
 42  ω    149.00 176.00   0.50    0.20    --  111.50  45.00-120.00   54
 43  ω    104.00 177.00   0.50    0.20    --  111.50  30.00-120.00  146
 44  ω    115.00 178.00   0.50    0.20    --  111.50  15.00 -60.00  126
 45  ω    103.00 162.00   0.50    0.20    --  111.50  15.00 -30.00  118
 46  ω    102.00 164.00   0.50    0.20    --  111.50  30.00  60.00  124
 47  ω    109.00 167.00   0.50    0.20    --  111.50  30.00 150.00  116
 48  ω    -68.00  22.00   0.50    0.10    --  -48.11  77.00  90.00  180
 49  ω    -44.00  24.00   0.50    0.10    --  -48.11  38.00  60.00  136
 50  ω    -28.00  23.00   0.50    0.10    --  -48.11  19.00 150.00  102
 51  ω    -51.00 -26.00   0.50    0.20    --  -90.00  45.00 -60.00   50
 52  ω    -41.00  24.00   0.50    0.10    --  -48.11  38.00-180.00  130
 53  ω   -155.00 -86.00   0.50    0.20    --  -90.00 -30.00-150.00  138
 54  ω    -53.00 -13.00   0.50    0.10    --  -48.11 125.00-120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0778618000
_diffrn_orient_matrix_UB_12      0.0279002000
_diffrn_orient_matrix_UB_13      -0.1248101000
_diffrn_orient_matrix_UB_21      0.0862003000
_diffrn_orient_matrix_UB_22      0.0455481000
_diffrn_orient_matrix_UB_23      0.0331674000
_diffrn_orient_matrix_UB_31      0.0734325000
_diffrn_orient_matrix_UB_32      -0.0239763000
_diffrn_orient_matrix_UB_33      -0.0823017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            45204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.871
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.151
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.116
_refine_diff_density_min         -2.502
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0494
_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)+(0.0656P)²+8.2914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5754
_reflns_number_total             6725
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           mf-1-15b_2_1-mask_smrt_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250136
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H18 N2 O13 Cl5 La '
_chemical_oxdiff_usercomment     'Purple plate in oil'
_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.
;
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.255
_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 O(H,H) groups
2. Restrained distances
 O45-H45A = O45-H45B
 0.84 with sigma of 0.02
 H45A-H45B
 1.34 with sigma of 0.04
 O46-H46A = O46-H46B
 0.84 with sigma of 0.02
 H46A-H46B
 1.34 with sigma of 0.04
 O47-H47A = O47-H47B
 0.84 with sigma of 0.02
 H47A-H47B
 1.34 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41)
;
_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 1.580
_oxdiff_exptl_absorpt_empirical_full_min 0.683
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C2 C 0.5559(5) 0.4512(2) 1.0019(6) 0.0222(11) Uani 1 1 d . . . . .
C3 C 0.4808(5) 0.4584(2) 1.0788(6) 0.0205(11) Uani 1 1 d . . . . .
C4 C 0.4179(5) 0.5035(2) 1.0782(5) 0.0203(11) Uani 1 1 d . . . . .
O5 O 0.3419(3) 0.51129(15) 1.1363(4) 0.0193(8) Uani 1 1 d . . . . .
Cl6 Cl 0.45876(12) 0.40792(5) 1.17610(14) 0.0234(3) Uani 1 1 d . . . . .
O7 O 0.8993(3) 0.43130(15) 0.8106(4) 0.0203(8) Uani 1 1 d . . . . .
C8 C 0.9504(5) 0.4644(2) 0.8948(6) 0.0181(10) Uani 1 1 d . . . . .
C9 C 1.0280(5) 0.5014(2) 0.8766(5) 0.0175(10) Uani 1 1 d . . . . .
C10 C 1.0785(5) 0.5383(2) 0.9738(5) 0.0172(10) Uani 1 1 d . . . . .
O11 O 1.1439(3) 0.57354(14) 0.9629(4) 0.0197(8) Uani 1 1 d . . . . .
Cl12 Cl 1.05107(12) 0.50636(5) 0.72222(13) 0.0232(3) Uani 1 1 d . . . . .
La1 La 0.70515(3) 0.39107(2) 0.81410(3) 0.01457(11) Uani 1 1 d . . . . .
O1 O 0.6040(4) 0.40960(14) 0.9896(4) 0.0207(8) Uani 1 1 d . . . . .
O13 O 0.6940(4) 0.44225(15) 0.6075(4) 0.0217(8) Uani 1 1 d . . . . .
C14 C 0.6062(5) 0.4704(2) 0.5525(5) 0.0178(10) Uani 1 1 d . . . . .
C15 C 0.6039(5) 0.5075(2) 0.4577(6) 0.0202(11) Uani 1 1 d . . . . .
C16 C 0.5048(5) 0.5385(2) 0.4033(6) 0.0207(11) Uani 1 1 d . . . . .
O17 O 0.4977(4) 0.57263(14) 0.3193(4) 0.0207(8) Uani 1 1 d . . . . .
Cl18 Cl 0.72926(11) 0.51624(5) 0.40755(14) 0.0220(3) Uani 1 1 d . . . . .
C19 C 0.8348(5) 0.2595(2) 0.5798(6) 0.0198(11) Uani 1 1 d . . . . .
C20 C 0.7773(5) 0.2188(2) 0.5006(6) 0.0198(11) Uani 1 1 d . . . . .
C21 C 0.6416(5) 0.2216(2) 0.4387(6) 0.0228(11) Uani 1 1 d . . . . .
C22 C 0.5801(5) 0.2622(2) 0.4715(6) 0.0261(12) Uani 1 1 d . . . . .
C23 C 0.6360(5) 0.2999(2) 0.5621(6) 0.0209(11) Uani 1 1 d . . . . .
C24 C 0.7733(5) 0.2986(2) 0.6217(6) 0.0202(11) Uani 1 1 d . . . . .
O25 O 0.8273(4) 0.18002(14) 0.4747(4) 0.0209(8) Uani 1 1 d . . . . .
O26 O 0.5951(4) 0.18600(15) 0.3602(4) 0.0226(8) Uani 1 1 d . . . . .
O27 O 0.5853(4) 0.33586(15) 0.6006(4) 0.0243(8) Uani 1 1 d . . . . .
O28 O 0.8201(4) 0.33261(15) 0.7012(4) 0.0214(8) Uani 1 1 d . . . . .
Cl29 Cl 0.99040(12) 0.25941(5) 0.64130(14) 0.0237(3) Uani 1 1 d . . . . .
Cl30 Cl 0.42658(14) 0.26455(6) 0.39689(19) 0.0409(4) Uani 1 1 d . . . . .
N31 N 0.0236(4) 0.35168(18) 0.3945(5) 0.0212(9) Uani 1 1 d . . . . .
C32 C -0.0719(5) 0.3512(2) 0.2866(6) 0.0243(12) Uani 1 1 d . . . . .
H32 H -0.065847 0.336743 0.206673 0.029 Uiso 1 1 calc R U . . .
C33 C -0.1796(5) 0.3711(2) 0.2886(6) 0.0221(11) Uani 1 1 d . . . . .
H33 H -0.247341 0.370352 0.211235 0.026 Uiso 1 1 calc R U . . .
C34 C -0.1869(5) 0.3924(2) 0.4059(6) 0.0229(12) Uani 1 1 d . . . . .
H34 H -0.260517 0.405330 0.411141 0.027 Uiso 1 1 calc R U . . .
C35 C -0.0841(5) 0.3945(2) 0.5163(6) 0.0213(11) Uani 1 1 d . . . . .
H35 H -0.086708 0.411143 0.595078 0.026 Uiso 1 1 calc R U . . .
C36 C 0.0207(5) 0.3729(2) 0.5120(6) 0.0192(11) Uani 1 1 d . . . . .
C37 C 0.1288(5) 0.3693(2) 0.6298(6) 0.0201(11) Uani 1 1 d . . . . .
C38 C 0.1245(6) 0.3757(2) 0.7572(6) 0.0247(12) Uani 1 1 d . . . . .
H38 H 0.050665 0.382443 0.772386 0.030 Uiso 1 1 calc R U . . .
C39 C 0.2289(6) 0.3721(2) 0.8636(7) 0.0285(13) Uani 1 1 d . . . . .
H39 H 0.227295 0.378218 0.951506 0.034 Uiso 1 1 calc R U . . .
C40 C 0.3350(6) 0.3597(2) 0.8417(6) 0.0278(13) Uani 1 1 d . . . . .
H40 H 0.406286 0.356488 0.914206 0.033 Uiso 1 1 calc R U . . .
C41 C 0.3358(5) 0.3522(2) 0.7126(6) 0.0230(11) Uani 1 1 d . . . . .
H41 H 0.407451 0.342496 0.695979 0.028 Uiso 1 1 calc R U . . .
N42 N 0.2355(4) 0.35849(18) 0.6113(5) 0.0216(10) Uani 1 1 d . . . . .
C43 C 0.2412(6) 0.3557(3) 0.4746(6) 0.0276(13) Uani 1 1 d . . . . .
H43A H 0.316108 0.338958 0.474012 0.033 Uiso 1 1 calc R U . . .
H43B H 0.239641 0.390398 0.437737 0.033 Uiso 1 1 calc R U . . .
C44 C 0.1346(6) 0.3255(2) 0.3909(7) 0.0296(13) Uani 1 1 d . . . . .
H44A H 0.136326 0.323249 0.298160 0.035 Uiso 1 1 calc R U . . .
H44B H 0.137121 0.290614 0.426633 0.035 Uiso 1 1 calc R U . . .
O45 O 0.7895(5) 0.5607(2) 0.7543(6) 0.0423(12) Uani 1 1 d D . . . .
H45A H 0.750(8) 0.549(3) 0.802(9) 0.063 Uiso 1 1 d D U . . .
H45B H 0.819(9) 0.535(2) 0.728(10) 0.063 Uiso 1 1 d D U . . .
O46 O 0.9054(5) 0.6411(2) 0.9194(6) 0.0452(13) Uani 1 1 d D . . . .
H46A H 0.899(8) 0.612(2) 0.883(10) 0.068 Uiso 1 1 d D U . . .
H46B H 0.979(3) 0.646(4) 0.954(10) 0.068 Uiso 1 1 d D U . . .
O47 O 0.7666(6) 0.7322(3) 0.9083(8) 0.0615(17) Uani 1 1 d D . . . .
H47A H 0.807(8) 0.705(2) 0.920(13) 0.092 Uiso 1 1 d D U . . .
H47B H 0.694(3) 0.723(4) 0.891(14) 0.092 Uiso 1 1 d D U . . .
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'
N N 0.0311 0.0180 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 11 0 0.0393
5 -11 0 0.0245
2 2 -7 0.0748
-3 -1 7 0.0471
-5 -13 -1 0.0301
6 -10 -2 0.0318
4 -11 2 0.0257
-5 11 -1 0.0412
-6 10 3 0.0403
-2 -14 -3 0.0347
-7 -6 3 0.0306
2 14 3 0.0395
-2 15 -2 0.0449
4 4 -6 0.0664
5 12 0 0.0274
6 10 -1 0.0317
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
C3 C2 C4 119.1(5) . 3_667 ?
O1 C2 C3 124.8(5) . . ?
O1 C2 C4 116.1(5) . 3_667 ?
C2 C3 C4 123.2(5) . . ?
C2 C3 Cl6 118.6(4) . . ?
C4 C3 Cl6 118.1(4) . . ?
C3 C4 C2 117.4(5) . 3_667 ?
O5 C4 C2 116.0(5) . 3_667 ?
O5 C4 C3 126.6(5) . . ?
C4 O5 La1 118.1(4) . 3_667 ?
C8 O7 La1 121.0(3) . . ?
O7 C8 C9 125.3(5) . . ?
O7 C8 C10 114.8(5) . 3_767 ?
C9 C8 C10 119.9(5) . 3_767 ?
C8 C9 C10 122.0(5) . . ?
C8 C9 Cl12 118.9(4) . . ?
C10 C9 Cl12 118.8(4) . . ?
C9 C10 C8 118.1(5) . 3_767 ?
O11 C10 C8 116.1(5) . 3_767 ?
O11 C10 C9 125.8(5) . . ?
C10 O11 La1 116.6(3) . 3_767 ?
O7 La1 O5 81.23(12) . 3_667 ?
O7 La1 O11 60.31(12) . 3_767 ?
O7 La1 O1 124.13(13) . . ?
O7 La1 O13 64.59(13) . . ?
O7 La1 O17 122.10(12) . 3_666 ?
O7 La1 O25 89.43(12) . 4_566 ?
O7 La1 O26 148.86(13) . 4_566 ?
O7 La1 O27 117.09(12) . . ?
O7 La1 O28 68.56(12) . . ?
O11 La1 O5 67.40(12) 3_767 3_667 ?
O11 La1 O27 166.52(12) 3_767 . ?
O1 La1 O5 60.49(12) . 3_667 ?
O1 La1 O11 67.69(12) . 3_767 ?
O1 La1 O17 76.16(13) . 3_666 ?
O1 La1 O25 87.25(12) . 4_566 ?
O1 La1 O27 118.22(13) . . ?
O1 La1 O28 152.32(12) . . ?
O13 La1 O5 72.84(12) . 3_667 ?
O13 La1 O11 114.99(13) . 3_767 ?
O13 La1 O1 128.04(12) . . ?
O13 La1 O17 62.37(12) . 3_666 ?
O13 La1 O25 143.56(12) . 4_566 ?
O13 La1 O27 71.92(13) . . ?
O13 La1 O28 79.13(12) . . ?
O17 La1 O5 62.64(12) 3_666 3_667 ?
O17 La1 O11 128.07(12) 3_666 3_767 ?
O17 La1 O25 148.46(12) 3_666 4_566 ?
O17 La1 O27 65.16(12) 3_666 . ?
O17 La1 O28 120.28(13) 3_666 . ?
O25 La1 O5 130.63(12) 4_566 3_667 ?
O25 La1 O11 65.97(12) 4_566 3_767 ?
O25 La1 O27 101.41(12) 4_566 . ?
O26 La1 O5 124.91(12) 4_566 3_667 ?
O26 La1 O11 110.67(12) 4_566 3_767 ?
O26 La1 O1 68.23(13) 4_566 . ?
O26 La1 O13 134.26(13) 4_566 . ?
O26 La1 O17 87.58(13) 4_566 3_666 ?
O26 La1 O25 61.20(12) 4_566 4_566 ?
O26 La1 O27 64.05(13) 4_566 . ?
O26 La1 O28 89.20(13) 4_566 . ?
O27 La1 O5 126.03(12) . 3_667 ?
O28 La1 O5 145.46(12) . 3_667 ?
O28 La1 O11 108.56(12) . 3_767 ?
O28 La1 O25 67.28(12) . 4_566 ?
O28 La1 O27 60.19(12) . . ?
C2 O1 La1 124.8(4) . . ?
C14 O13 La1 121.7(3) . . ?
O13 C14 C15 125.0(5) . . ?
O13 C14 C16 115.2(5) . 3_666 ?
C15 C14 C16 119.8(5) . 3_666 ?
C14 C15 C16 122.2(5) . . ?
C14 C15 Cl18 119.0(4) . . ?
C16 C15 Cl18 118.7(4) . . ?
C15 C16 C14 118.0(5) . 3_666 ?
O17 C16 C14 116.8(5) . 3_666 ?
O17 C16 C15 125.2(5) . . ?
C16 O17 La1 120.4(4) . 3_666 ?
C20 C19 C24 123.2(5) . . ?
C20 C19 Cl29 118.7(4) . . ?
C24 C19 Cl29 117.9(4) . . ?
C19 C20 C21 117.9(5) . . ?
O25 C20 C19 125.6(5) . . ?
O25 C20 C21 116.5(5) . . ?
C22 C21 C20 119.0(5) . . ?
O26 C21 C20 115.5(5) . . ?
O26 C21 C22 125.5(6) . . ?
C21 C22 Cl30 117.6(5) . . ?
C23 C22 C21 123.0(6) . . ?
C23 C22 Cl30 119.5(5) . . ?
C22 C23 C24 118.6(5) . . ?
O27 C23 C22 126.0(6) . . ?
O27 C23 C24 115.4(5) . . ?
C19 C24 C23 117.7(5) . . ?
O28 C24 C19 125.4(5) . . ?
O28 C24 C23 116.9(5) . . ?
C20 O25 La1 121.3(4) . 4_565 ?
C21 O26 La1 125.3(4) . 4_565 ?
C23 O27 La1 120.1(4) . . ?
C24 O28 La1 124.1(4) . . ?
C32 N31 C36 121.9(5) . . ?
C32 N31 C44 119.3(5) . . ?
C36 N31 C44 118.7(5) . . ?
N31 C32 H32 119.3 . . ?
N31 C32 C33 121.4(5) . . ?
C33 C32 H32 119.3 . . ?
C32 C33 H33 120.7 . . ?
C32 C33 C34 118.7(6) . . ?
C34 C33 H33 120.7 . . ?
C33 C34 H34 120.5 . . ?
C33 C34 C35 119.0(5) . . ?
C35 C34 H34 120.5 . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.7(6) . . ?
C36 C35 H35 119.6 . . ?
N31 C36 C35 118.3(5) . . ?
N31 C36 C37 118.6(5) . . ?
C35 C36 C37 123.0(5) . . ?
C38 C37 C36 122.1(5) . . ?
N42 C37 C36 118.9(5) . . ?
N42 C37 C38 118.9(5) . . ?
C37 C38 H38 120.3 . . ?
C37 C38 C39 119.5(6) . . ?
C39 C38 H38 120.3 . . ?
C38 C39 H39 119.9 . . ?
C40 C39 C38 120.1(6) . . ?
C40 C39 H39 119.9 . . ?
C39 C40 H40 120.5 . . ?
C39 C40 C41 119.0(6) . . ?
C41 C40 H40 120.5 . . ?
C40 C41 H41 120.1 . . ?
N42 C41 C40 119.8(6) . . ?
N42 C41 H41 120.1 . . ?
C37 N42 C43 118.5(5) . . ?
C41 N42 C37 122.5(5) . . ?
C41 N42 C43 118.9(5) . . ?
N42 C43 H43A 110.0 . . ?
N42 C43 H43B 110.0 . . ?
N42 C43 C44 108.5(5) . . ?
H43A C43 H43B 108.4 . . ?
C44 C43 H43A 110.0 . . ?
C44 C43 H43B 110.0 . . ?
N31 C44 C43 108.6(5) . . ?
N31 C44 H44A 110.0 . . ?
N31 C44 H44B 110.0 . . ?
C43 C44 H44A 110.0 . . ?
C43 C44 H44B 110.0 . . ?
H44A C44 H44B 108.4 . . ?
H45A O45 H45B 106(5) . . ?
H46A O46 H46B 107(5) . . ?
H47A O47 H47B 105(5) . . ?
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
C2 C3 1.389(8) . ?
C2 C4 1.549(8) 3_667 ?
C2 O1 1.257(7) . ?
C3 C4 1.399(8) . ?
C3 Cl6 1.748(6) . ?
C4 O5 1.251(7) . ?
O5 La1 2.714(4) 3_667 ?
O7 C8 1.256(7) . ?
O7 La1 2.534(4) . ?
C8 C9 1.392(7) . ?
C8 C10 1.533(7) 3_767 ?
C9 C10 1.404(8) . ?
C9 Cl12 1.742(5) . ?
C10 O11 1.235(7) . ?
O11 La1 2.645(4) 3_767 ?
La1 O1 2.547(4) . ?
La1 O13 2.536(4) . ?
La1 O17 2.556(4) 3_666 ?
La1 O25 2.635(4) 4_566 ?
La1 O26 2.535(4) 4_566 ?
La1 O27 2.689(4) . ?
La1 O28 2.576(4) . ?
O13 C14 1.260(7) . ?
C14 C15 1.393(8) . ?
C14 C16 1.538(7) 3_666 ?
C15 C16 1.395(8) . ?
C15 Cl18 1.735(6) . ?
C16 O17 1.249(7) . ?
C19 C20 1.398(8) . ?
C19 C24 1.406(8) . ?
C19 Cl29 1.747(6) . ?
C20 C21 1.532(8) . ?
C20 O25 1.251(7) . ?
C21 C22 1.395(8) . ?
C21 O26 1.259(7) . ?
C22 C23 1.393(8) . ?
C22 Cl30 1.737(6) . ?
C23 C24 1.545(8) . ?
C23 O27 1.254(7) . ?
C24 O28 1.235(7) . ?
N31 C32 1.331(8) . ?
N31 C36 1.373(7) . ?
N31 C44 1.490(7) . ?
C32 H32 0.9500 . ?
C32 C33 1.381(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.388(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.400(9) . ?
C35 H35 0.9500 . ?
C35 C36 1.374(8) . ?
C36 C37 1.484(8) . ?
C37 C38 1.375(8) . ?
C37 N42 1.363(7) . ?
C38 H38 0.9500 . ?
C38 C39 1.391(9) . ?
C39 H39 0.9500 . ?
C39 C40 1.380(9) . ?
C40 H40 0.9500 . ?
C40 C41 1.384(9) . ?
C41 H41 0.9500 . ?
C41 N42 1.337(8) . ?
N42 C43 1.470(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.518(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
O45 H45A 0.84(2) . ?
O45 H45B 0.85(2) . ?
O46 H46A 0.85(2) . ?
O46 H46B 0.85(2) . ?
O47 H47A 0.85(2) . ?
O47 H47B 0.86(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
C2 C3 C4 C2 -6.2(9) . . . 3_667 ?
C2 C3 C4 O5 173.9(6) . . . . ?
C2 C4 O5 La1 -20.8(6) 3_667 . . 3_667 ?
C3 C2 O1 La1 166.6(4) . . . . ?
C3 C4 O5 La1 159.1(5) . . . 3_667 ?
C4 C2 C3 C4 6.3(10) 3_667 . . . ?
C4 C2 C3 Cl6 -176.4(4) 3_667 . . . ?
C4 C2 O1 La1 -12.1(7) 3_667 . . . ?
Cl6 C3 C4 C2 176.5(4) . . . 3_667 ?
Cl6 C3 C4 O5 -3.4(8) . . . . ?
O7 C8 C9 C10 177.7(5) . . . . ?
O7 C8 C9 Cl12 4.5(8) . . . . ?
C8 C9 C10 C8 2.3(9) . . . 3_767 ?
C8 C9 C10 O11 -176.8(5) . . . . ?
C8 C10 O11 La1 27.3(6) 3_767 . . 3_767 ?
C9 C10 O11 La1 -153.6(5) . . . 3_767 ?
C10 C8 C9 C10 -2.3(9) 3_767 . . . ?
C10 C8 C9 Cl12 -175.6(4) 3_767 . . . ?
Cl12 C9 C10 C8 175.5(4) . . . 3_767 ?
Cl12 C9 C10 O11 -3.6(8) . . . . ?
La1 O7 C8 C9 -154.9(4) . . . . ?
La1 O7 C8 C10 25.1(6) . . . 3_767 ?
La1 O13 C14 C15 165.6(4) . . . . ?
La1 O13 C14 C16 -14.6(6) . . . 3_666 ?
O1 C2 C3 C4 -172.3(6) . . . . ?
O1 C2 C3 Cl6 5.0(8) . . . . ?
O13 C14 C15 C16 -178.1(5) . . . . ?
O13 C14 C15 Cl18 0.7(8) . . . . ?
C14 C15 C16 C14 -2.0(9) . . . 3_666 ?
C14 C15 C16 O17 179.2(5) . . . . ?
C14 C16 O17 La1 -15.3(6) 3_666 . . 3_666 ?
C15 C16 O17 La1 163.5(4) . . . 3_666 ?
C16 C14 C15 C16 2.1(9) 3_666 . . . ?
C16 C14 C15 Cl18 -179.1(4) 3_666 . . . ?
Cl18 C15 C16 C14 179.1(4) . . . 3_666 ?
Cl18 C15 C16 O17 0.4(8) . . . . ?
C19 C20 C21 C22 -4.8(8) . . . . ?
C19 C20 C21 O26 174.8(5) . . . . ?
C19 C20 O25 La1 -177.2(4) . . . 4_565 ?
C19 C24 O28 La1 -165.9(4) . . . . ?
C20 C19 C24 C23 -8.0(8) . . . . ?
C20 C19 C24 O28 173.0(5) . . . . ?
C20 C21 C22 C23 -2.3(9) . . . . ?
C20 C21 C22 Cl30 178.9(4) . . . . ?
C20 C21 O26 La1 5.2(7) . . . 4_565 ?
C21 C20 O25 La1 2.4(6) . . . 4_565 ?
C21 C22 C23 C24 4.3(9) . . . . ?
C21 C22 C23 O27 -176.3(6) . . . . ?
C22 C21 O26 La1 -175.2(5) . . . 4_565 ?
C22 C23 C24 C19 0.6(8) . . . . ?
C22 C23 C24 O28 179.7(5) . . . . ?
C22 C23 O27 La1 166.4(5) . . . . ?
C23 C24 O28 La1 15.1(7) . . . . ?
C24 C19 C20 C21 10.0(8) . . . . ?
C24 C19 C20 O25 -170.4(5) . . . . ?
C24 C23 O27 La1 -14.2(6) . . . . ?
O25 C20 C21 C22 175.5(5) . . . . ?
O25 C20 C21 O26 -4.8(7) . . . . ?
O26 C21 C22 C23 178.2(6) . . . . ?
O26 C21 C22 Cl30 -0.7(9) . . . . ?
O27 C23 C24 C19 -178.9(5) . . . . ?
O27 C23 C24 O28 0.3(7) . . . . ?
Cl29 C19 C20 C21 -175.3(4) . . . . ?
Cl29 C19 C20 O25 4.3(8) . . . . ?
Cl29 C19 C24 C23 177.3(4) . . . . ?
Cl29 C19 C24 O28 -1.8(8) . . . . ?
Cl30 C22 C23 C24 -176.9(4) . . . . ?
Cl30 C22 C23 O27 2.5(9) . . . . ?
N31 C32 C33 C34 0.5(9) . . . . ?
N31 C36 C37 C38 -160.7(5) . . . . ?
N31 C36 C37 N42 18.0(7) . . . . ?
C32 N31 C36 C35 -0.8(8) . . . . ?
C32 N31 C36 C37 176.6(5) . . . . ?
C32 N31 C44 C43 144.9(6) . . . . ?
C32 C33 C34 C35 2.3(8) . . . . ?
C33 C34 C35 C36 -4.4(8) . . . . ?
C34 C35 C36 N31 3.7(8) . . . . ?
C34 C35 C36 C37 -173.6(5) . . . . ?
C35 C36 C37 C38 16.5(8) . . . . ?
C35 C36 C37 N42 -164.7(5) . . . . ?
C36 N31 C32 C33 -1.2(9) . . . . ?
C36 N31 C44 C43 -39.2(7) . . . . ?
C36 C37 C38 C39 -179.7(5) . . . . ?
C36 C37 N42 C41 -176.6(5) . . . . ?
C36 C37 N42 C43 6.0(7) . . . . ?
C37 C38 C39 C40 -3.3(9) . . . . ?
C37 N42 C43 C44 -44.7(7) . . . . ?
C38 C37 N42 C41 2.2(8) . . . . ?
C38 C37 N42 C43 -175.2(5) . . . . ?
C38 C39 C40 C41 1.5(9) . . . . ?
C39 C40 C41 N42 2.1(9) . . . . ?
C40 C41 N42 C37 -4.0(8) . . . . ?
C40 C41 N42 C43 173.4(5) . . . . ?
C41 N42 C43 C44 137.8(5) . . . . ?
N42 C37 C38 C39 1.5(8) . . . . ?
N42 C43 C44 N31 59.4(7) . . . . ?
C44 N31 C32 C33 174.5(6) . . . . ?
C44 N31 C36 C35 -176.6(5) . . . . ?
C44 N31 C36 C37 0.8(8) . . . . ?
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
-5.5304 11.4135 0.3978 0.6994 0.0563 -0.7125
5.3505 -11.4981 0.0745 -0.7467 -0.0600 0.6625
2.3197 1.8273 -6.8303 0.7229 0.0566 0.6887
-2.8797 -0.6489 6.8477 -0.6486 -0.0507 -0.7595
-4.6491 -12.6736 -0.5670 0.0792 -0.9968 0.0091
5.9934 -10.4611 -2.3530 -0.4648 -0.0379 0.8846
4.4792 -11.3394 1.7886 -0.8884 -0.0711 0.4536
-4.6886 11.4340 -1.4337 0.8630 0.0691 -0.5004
-6.0331 9.5897 3.3163 0.3234 0.0267 -0.9459
-2.0327 -14.3555 -2.5196 0.0722 -0.9127 0.4023
-7.1214 -6.0942 2.5642 0.0644 -0.8064 -0.5879
1.6884 14.4028 2.7317 -0.0706 0.8922 -0.4462
-1.7219 14.9638 -2.3032 0.8390 0.4568 -0.2957
4.0189 4.3345 -6.4259 0.6100 0.3307 0.7201
5.1144 12.0468 0.1340 -0.0788 0.9940 0.0757
6.2786 9.6622 -1.1610 -0.0744 0.9428 0.3249
