#------------------------------------------------------------------------------
#$Date: 2025-07-06 17:06:59 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300709 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/01/7250139.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_7250139
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
'C12 H2 Cl4 La O9, 0.5(C14 H12 N2), 2(C3 H6 O), H2 O'
_chemical_formula_sum            'C25 H22 Cl4 La N O12'
_chemical_formula_weight         809.168
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                103.513(3)
_cell_angle_beta                 94.393(3)
_cell_angle_gamma                106.749(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7781(4)
_cell_length_b                   11.4423(4)
_cell_length_c                   12.9249(4)
_cell_measurement_reflns_used    11172
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9550
_cell_measurement_theta_min      4.3370
_cell_volume                     1466.26(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.80a 64-bit (release 13-01-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (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 0.9962
_diffrn_measured_fraction_theta_max 0.9248
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00   6.00   0.50    0.20    --   47.26 -60.00 -53.00   60
  2  ω    -22.00   5.00   0.50    0.20    --   47.26 -19.00 -60.00   54
  3  ω     35.00  62.00   0.50    0.20    --   47.26 -60.00 -53.00   54
  4  ω     57.00 106.00   0.50    0.40    --  105.30-125.00  30.00   98
  5  ω     84.00 110.00   0.50    0.40    --  105.30-125.00   0.00   52
  6  ω     40.00 110.00   0.50    0.40    --  105.30-125.00 -30.00  140
  7  ω     39.00 108.00   0.50    0.40    --  105.30-106.00-131.44  138
  8  ω     34.00  79.00   0.50    0.40    --  105.30 -94.00-180.00   90
  9  ω     36.00  67.00   0.50    0.40    --  105.30-125.00-180.00   62
 10  ω     34.00  81.00   0.50    0.20    --   47.26-125.00 -60.00   94
 11  ω     83.00 109.00   0.50    0.40    --  105.30-125.00-180.00   52
 12  ω     59.00 106.00   0.50    0.40    --  105.30-105.00 171.31   94
 13  ω     54.00 101.00   0.50    0.40    --  105.30 -94.00  60.00   94
 14  ω     74.00 105.00   0.50    0.40    --  105.30 -94.00   0.00   62
 15  ω     33.00  70.00   0.50    0.40    --  105.30 -61.00 -60.00   74
 16  ω     36.00  68.00   0.50    0.40    --  105.30 -60.00 -53.00   64
 17  ω    107.00 134.00   0.50    0.40    --  105.30  30.00-120.00   54
 18  ω    137.00 165.00   0.50    0.40    --  105.30  30.00-120.00   56
 19  ω     40.00  70.00   0.50    0.40    --  105.30 -61.00  90.00   60
 20  ω    101.00 174.00   0.50    0.40    --  105.30  60.00  85.00  146
 21  ω     32.00 117.00   0.50    0.20    --   47.26  60.00  85.00  170
 22  ω    -32.00  -7.00   0.50    0.20    --  -47.26  60.00  85.00   50
 23  ω    -62.00 -37.00   0.50    0.20    --  -47.26  60.00  85.00   50
 24  ω    -64.00 -21.00   0.50    0.40    --  -91.75  61.00 150.00   86
 25  ω    -29.00  27.00   0.50    0.20    --  -47.26  19.00-120.00  112
 26  ω    -66.00 -41.00   0.50    0.40    --  -91.75  61.00 -90.00   50
 27  ω    -48.00 -23.00   0.50    0.40    --  -91.75  45.00 -60.00   50
 28  ω    -69.00 -20.00   0.50    0.40    --  -91.75  60.00  85.00   98
 29  ω    -50.00 -21.00   0.50    0.40    --  -91.75  45.00  90.00   58
 30  ω   -120.00 -35.00   0.50    0.20    --  -47.26 -38.00  90.00  170
 31  ω    -62.00 -27.00   0.50    0.40    --  -91.75 125.00 -90.00   70
 32  ω    -83.00 -23.00   0.50    0.40    --  -91.75 125.00-150.00  120
 33  ω   -119.00 -38.00   0.50    0.20    --  -47.26 -60.00 -53.00  162
 34  ω   -162.00-109.00   0.50    0.40    --  -91.75 -60.00 -53.00  106
 35  ω   -159.00-126.00   0.50    0.40    --  -91.75 -45.00-150.00   66
 36  ω   -121.00 -88.00   0.50    0.40    --  -91.75 -45.00-150.00   66
 37  ω   -111.00 -83.00   0.50    0.40    --  -91.75 -15.00-180.00   56
 38  ω   -166.00-140.00   0.50    0.40    --  -91.75 -15.00-180.00   52
 39  ω   -163.00 -80.00   0.50    0.40    --  -91.75 -45.00   0.00  166
 40  ω   -154.00 -90.00   0.50    0.40    --  -91.75 -94.00  60.00  128
;
_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      -0.1157123000
_diffrn_orient_matrix_UB_12      -0.0939891000
_diffrn_orient_matrix_UB_13      -0.0844560000
_diffrn_orient_matrix_UB_21      0.0792772000
_diffrn_orient_matrix_UB_22      -0.0930550000
_diffrn_orient_matrix_UB_23      -0.0247818000
_diffrn_orient_matrix_UB_31      -0.0561431000
_diffrn_orient_matrix_UB_32      -0.0616759000
_diffrn_orient_matrix_UB_33      0.0874557000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.9962
_diffrn_reflns_Laue_measured_fraction_max 0.9248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17670
_diffrn_reflns_point_group_measured_fraction_full 0.9962
_diffrn_reflns_point_group_measured_fraction_max 0.9248
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.92
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.186
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
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    1.833
_exptl_crystal_description       prism
_exptl_crystal_F_000             800.000
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.7369
_refine_diff_density_min         -1.7232
_refine_diff_density_rms         0.1388
_refine_ls_d_res_high            0.7915
_refine_ls_d_res_low             12.4160
_refine_ls_goodness_of_fit_ref   1.0331
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5739
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.0206
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0750P)²+0.2416P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5383
_reflns_number_total             5739
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00026b2.cif
_cod_data_source_block           MF-1-33B_1-mask_avg_abs_a
_cod_depositor_comments
'Adding full bibliography for 7250132--7250140.cif.'
_cod_database_code               7250139
_chemical_oxdiff_formula         'C25 H22 Cl4 La N O12'
_chemical_oxdiff_usercomment     'solvent:acetone and water'
_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, All O(H,H) groups
2. Restrained distances
 C35-C36
 1.35 with sigma of 0.02
 C28-C35 = C36-C37
 1.43 with sigma of 0.02
 C32-C33
 1.51 with sigma of 0.02
 N30-C32 = N34-C33
 1.48 with sigma of 0.02
 O25-H25a = O25-H25b
 0.84 with sigma of 0.02
 H25a-H25b
 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
 C27-H27 = C31-H31
 0.95 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C29 \\sim C31 \\sim C28 \\sim C33 \\sim N34 \\sim N30 \\sim
C37 \\sim C32 \\sim C36 \\sim C35: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C28) = Uanis(N34)
Uanis(C33) = Uanis(C35)
Uanis(N30) = Uanis(C37)
Uanis(C32) = Uanis(C36)
4. Rigid body (RIGU) restrains
 C39, C40, O38, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C29, C31, C28, C33, N34, N30, C37, C32, C36, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C28(0.5) C33(0.5) H33a(0.5) H33b(0.5) N34(0.5) N30(0.5) C37(0.5)
 C32(0.5) H32a(0.5) H32b(0.5) C36(0.5) H36(0.5) C35(0.5) H35(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C33(H33a,H33b), C32(H32a,H32b)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C36(H36), C35(H35)
6.c Idealised Me refined as rotating group:
 C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C45(H45a,H45b,
 H45c)
;
_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 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.728
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z
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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
C2 C 0.6086(3) 0.4732(3) 0.5506(3) 0.0206(7) Uani 1.000000 . . . .
C3 C 0.5549(4) 0.4044(4) 0.4449(3) 0.0221(7) Uani 1.000000 . . . .
C4 C 0.4431(3) 0.4207(4) 0.3937(3) 0.0209(7) Uani 1.000000 . . . .
O5 O 0.3785(3) 0.3511(3) 0.3046(2) 0.0246(5) Uani 1.000000 . . . .
Cl6 Cl 0.61461(8) 0.28528(9) 0.38278(7) 0.02486(19) Uani 1.000000 . . . .
O7 O 0.5833(2) 0.4694(2) 0.8082(2) 0.0227(5) Uani 1.000000 . . . .
C8 C 0.5386(3) 0.4806(3) 0.8951(3) 0.0202(7) Uani 1.000000 . . . .
C9 C 0.4122(3) 0.4119(4) 0.9064(3) 0.0209(7) Uani 1.000000 . . . .
C10 C 0.3681(3) 0.4243(3) 1.0061(3) 0.0204(7) Uani 1.000000 . . . .
O11 O 0.2578(2) 0.3613(3) 1.0224(2) 0.0230(5) Uani 1.000000 . . . .
La1 La 0.811875(17) 0.602386(18) 0.788278(15) 0.01845(9) Uani 1.000000 . . . .
O1 O 0.6976(2) 0.4540(3) 0.6068(2) 0.0235(5) Uani 1.000000 . . . .
Cl12 Cl 0.31030(8) 0.30305(10) 0.79440(7) 0.0302(2) Uani 1.000000 . . . .
O13 O 1.0106(2) 0.7647(2) 0.9133(2) 0.0236(5) Uani 1.000000 . . . .
C14 C 1.0126(4) 0.8752(4) 0.9576(3) 0.0221(7) Uani 1.000000 . . . .
C15 C 1.1099(3) 0.9641(4) 1.0382(3) 0.0228(7) Uani 1.000000 . . . .
C16 C 1.1026(3) 1.0853(4) 1.0843(3) 0.0225(7) Uani 1.000000 . . . .
O17 O 1.1840(3) 1.1671(3) 1.1594(2) 0.0249(6) Uani 1.000000 . . . .
Cl18 Cl 1.24296(8) 0.92328(9) 1.08303(8) 0.0269(2) Uani 1.000000 . . . .
O19 O 0.9685(2) 0.4914(3) 0.7027(2) 0.0238(5) Uani 1.000000 . . . .
C20 C 0.9848(3) 0.4899(4) 0.6080(3) 0.0211(7) Uani 1.000000 . . . .
C21 C 1.0254(4) 0.3988(4) 0.5382(3) 0.0226(7) Uani 1.000000 . . . .
C22 C 1.0420(3) 0.4019(4) 0.4332(3) 0.0210(7) Uani 1.000000 . . . .
O23 O 1.0791(3) 0.3243(3) 0.3667(2) 0.0244(6) Uani 1.000000 . . . .
Cl24 Cl 1.05326(10) 0.27649(10) 0.58479(8) 0.0322(2) Uani 1.000000 . . . .
O25 O 0.8367(3) 0.4299(3) 0.8703(3) 0.0326(7) Uani 1.000000 D . . .
H25a H 0.782(4) 0.389(5) 0.901(4) 0.0489(10) Uiso 1.000000 DR . . .
H25b H 0.899(4) 0.402(5) 0.869(5) 0.0489(10) Uiso 1.000000 DR . . .
C26 C 0.2762(5) 0.1512(4) 0.4422(4) 0.0371(10) Uani 1.000000 . U . .
H26 H 0.2169(5) 0.1939(4) 0.4252(4) 0.0445(11) Uiso 1.000000 R . . .
C27 C 0.2710(6) 0.0379(5) 0.3763(4) 0.0458(12) Uani 1.000000 D U . .
H27 H 0.209(3) -0.002(5) 0.312(2) 0.0550(14) Uiso 1.000000 DR . . .
C29 C 0.4538(5) 0.0303(4) 0.4881(3) 0.0331(9) Uani 1.000000 . U . .
C31 C 0.3694(5) 0.2041(4) 0.5350(4) 0.0338(9) Uani 1.000000 D U . .
H31 H 0.371(4) 0.2864(17) 0.573(3) 0.0406(11) Uiso 1.000000 DR . . .
O38 O 0.2480(5) -0.0456(7) 0.6109(4) 0.0954(19) Uani 1.000000 . U . .
C39 C 0.2596(8) -0.0446(8) 0.7906(6) 0.0702(18) Uani 1.000000 . U . .
H39a H 0.201(3) -0.115(4) 0.812(3) 0.105(3) Uiso 1.000000 GR . . .
H39b H 0.343(3) -0.061(5) 0.7797(14) 0.105(3) Uiso 1.000000 GR . . .
H39c H 0.276(5) 0.034(2) 0.8474(13) 0.105(3) Uiso 1.000000 GR . . .
C40 C 0.1979(5) -0.0327(5) 0.6903(4) 0.0418(11) Uani 1.000000 . U . .
C41 C 0.0692(5) -0.0088(5) 0.6900(5) 0.0452(12) Uani 1.000000 . U . .
H41a H 0.045(2) 0.009(4) 0.6220(14) 0.0678(17) Uiso 1.000000 GR . . .
H41b H 0.0021(10) -0.0836(15) 0.698(3) 0.0678(17) Uiso 1.000000 GR . . .
H41c H 0.0760(12) 0.064(2) 0.750(2) 0.0678(17) Uiso 1.000000 GR . . .
O42 O 0.6335(3) 0.2946(3) 0.9537(2) 0.0311(6) Uani 1.000000 . . . .
C43 C 0.7426(4) 0.3684(5) 1.1352(4) 0.0370(10) Uani 1.000000 . . . .
H43a H 0.779(2) 0.3115(5) 1.165(2) 0.0555(15) Uiso 1.000000 GR . . .
H43b H 0.8106(16) 0.422(3) 1.1054(8) 0.0555(15) Uiso 1.000000 GR . . .
H43c H 0.7127(9) 0.421(3) 1.1924(15) 0.0555(15) Uiso 1.000000 GR . . .
C44 C 0.6295(4) 0.2918(4) 1.0481(4) 0.0284(8) Uani 1.000000 . . . .
C45 C 0.5117(4) 0.2093(5) 1.0781(4) 0.0360(10) Uani 1.000000 . . . .
H45a H 0.4393(11) 0.179(3) 1.0178(11) 0.0541(15) Uiso 1.000000 GR . . .
H45b H 0.5318(12) 0.1370(19) 1.095(3) 0.0541(15) Uiso 1.000000 GR . . .
H45c H 0.486(2) 0.2579(11) 1.1413(18) 0.0541(15) Uiso 1.000000 GR . . .
O46 O 1.0146(3) 0.3045(3) 0.8488(3) 0.0339(7) Uani 1.000000 D . . .
H46a H 1.078(4) 0.316(6) 0.896(3) 0.0509(10) Uiso 1.000000 DR . . .
H46b H 1.047(5) 0.326(6) 0.796(3) 0.0509(10) Uiso 1.000000 DR . . .
C28 C 0.3757(13) -0.0153(11) 0.3934(11) 0.0253(19) Uani 0.500000 D U P -1
C33 C 0.6832(9) 0.1687(8) 0.6514(7) 0.0276(13) Uani 0.500000 D U P -1
H33a H 0.7376(9) 0.1922(8) 0.7229(7) 0.0331(15) Uiso 0.500000 R . P -1
H33b H 0.7282(9) 0.2244(8) 0.6084(7) 0.0331(15) Uiso 0.500000 R . P -1
N34 N 0.6607(10) 0.0338(9) 0.5955(9) 0.0253(19) Uani 0.500000 D U P -1
N30 N 0.458(3) 0.149(4) 0.561(2) 0.0275(14) Uani 0.500000 D U P -1
C37 C 0.542(4) -0.140(5) 0.445(3) 0.0275(14) Uani 0.500000 D U P -1
C32 C 0.5481(14) 0.181(2) 0.6633(15) 0.021(2) Uani 0.500000 D U P -1
H32a H 0.5064(14) 0.125(2) 0.7073(15) 0.025(3) Uiso 0.500000 R . P -1
H32b H 0.5586(14) 0.269(2) 0.7035(15) 0.025(3) Uiso 0.500000 R . P -1
C36 C 0.4494(14) -0.2038(19) 0.3490(15) 0.021(2) Uani 0.500000 D U P -1
H36 H 0.4421(14) -0.2860(19) 0.3064(15) 0.025(3) Uiso 0.500000 R . P -1
C35 C 0.3737(9) -0.1355(8) 0.3249(7) 0.0276(13) Uani 0.500000 D U P -1
H35 H 0.3152(9) -0.1685(8) 0.2586(7) 0.0331(15) Uiso 0.500000 R . P -1
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 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Cl 0.36457 0.70364 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55740 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
La -1.36632 9.05284 20.57800 19.59900 11.37270 3.28719 2.94817 0.24448 18.77260
133.12399 2.14678 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -5 1 0.0230
3 5 -2 0.0297
0 0 8 0.0438
0 -1 -8 0.0461
6 -5 0 0.0319
-6 5 0 0.0092
3 -6 5 0.0361
3 3 -7 0.0514
2 -7 0 0.0271
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
C4 C2 C3 119.5(3) 2_666 . ?
O1 C2 C3 124.7(4) . . ?
O1 C2 C4 115.8(3) . 2_666 ?
C4 C3 C2 120.4(3) . . ?
Cl6 C3 C2 119.0(3) . . ?
Cl6 C3 C4 120.1(3) . . ?
C3 C4 C2 119.6(3) . 2_666 ?
O5 C4 C2 116.0(3) . 2_666 ?
O5 C4 C3 124.3(4) . . ?
La1 O5 C4 122.1(2) 2_666 . ?
La1 O7 C8 123.6(2) . . ?
C9 C8 O7 124.3(3) . . ?
C10 C8 O7 116.0(3) 2_667 . ?
C10 C8 C9 119.7(3) 2_667 . ?
C10 C9 C8 122.2(3) . . ?
Cl12 C9 C8 118.8(3) . . ?
Cl12 C9 C10 119.0(3) . . ?
C9 C10 C8 118.1(3) . 2_667 ?
O11 C10 C8 116.7(3) . 2_667 ?
O11 C10 C9 125.2(3) . . ?
La1 O11 C10 121.7(2) 2_667 . ?
O7 La1 O5 64.92(8) . 2_666 ?
O11 La1 O5 95.98(8) 2_667 2_666 ?
O11 La1 O7 61.83(8) 2_667 . ?
O1 La1 O5 62.67(8) . 2_666 ?
O1 La1 O7 70.94(8) . . ?
O1 La1 O11 132.77(8) . 2_667 ?
O13 La1 O5 126.13(9) . 2_666 ?
O13 La1 O7 136.39(8) . . ?
O13 La1 O11 74.67(8) . 2_667 ?
O13 La1 O1 152.38(8) . . ?
O17 La1 O5 64.27(8) 2_777 2_666 ?
O17 La1 O7 106.41(8) 2_777 . ?
O17 La1 O11 74.72(9) 2_777 2_667 ?
O17 La1 O1 121.56(9) 2_777 . ?
O17 La1 O13 62.07(8) 2_777 . ?
O19 La1 O5 128.51(8) . 2_666 ?
O19 La1 O7 119.51(8) . . ?
O19 La1 O11 133.05(8) . 2_667 ?
O19 La1 O1 70.95(8) . . ?
O19 La1 O13 87.50(8) . . ?
O19 La1 O17 133.45(9) . 2_777 ?
O23 La1 O5 80.95(9) 2_766 2_666 ?
O23 La1 O7 135.72(8) 2_766 . ?
O23 La1 O11 153.99(8) 2_766 2_667 ?
O23 La1 O1 68.56(8) 2_766 . ?
O23 La1 O13 86.26(9) 2_766 . ?
O23 La1 O17 80.81(8) 2_766 2_777 ?
O23 La1 O19 61.68(8) 2_766 . ?
O25 La1 O5 135.56(9) . 2_666 ?
O25 La1 O7 71.69(9) . . ?
O25 La1 O11 70.74(9) . 2_667 ?
O25 La1 O1 94.94(10) . . ?
O25 La1 O13 92.04(10) . . ?
O25 La1 O17 141.35(10) . 2_777 ?
O25 La1 O19 66.85(9) . . ?
O25 La1 O23 128.52(9) . 2_766 ?
La1 O1 C2 122.5(2) . . ?
C14 O13 La1 122.5(2) . . ?
C15 C14 O13 125.9(4) . . ?
C16 C14 O13 115.7(3) 2_777 . ?
C16 C14 C15 118.3(3) 2_777 . ?
C16 C15 C14 121.8(3) . . ?
Cl18 C15 C14 119.0(3) . . ?
Cl18 C15 C16 119.2(3) . . ?
C15 C16 C14 119.8(3) . 2_777 ?
O17 C16 C14 115.5(3) . 2_777 ?
O17 C16 C15 124.7(4) . . ?
C16 O17 La1 122.0(2) . 2_777 ?
C20 O19 La1 119.1(2) . . ?
C21 C20 O19 125.0(3) . . ?
C22 C20 O19 116.1(3) 2_766 . ?
C22 C20 C21 118.9(3) 2_766 . ?
C22 C21 C20 122.5(4) . . ?
Cl24 C21 C20 118.5(3) . . ?
Cl24 C21 C22 118.9(3) . . ?
C21 C22 C20 118.6(3) . 2_766 ?
O23 C22 C20 115.5(3) . 2_766 ?
O23 C22 C21 125.9(4) . . ?
C22 O23 La1 118.3(2) . 2_766 ?
H25a O25 La1 126(4) . . ?
H25b O25 La1 126(4) . . ?
H25b O25 H25a 108(4) . . ?
C27 C26 H26 120.4(3) . . ?
C31 C26 H26 120.4(3) . . ?
C31 C26 C27 119.2(4) . . ?
H27 C27 C26 122(4) . . ?
C28 C27 C26 119.4(7) . . ?
C28 C27 H27 117(4) . . ?
N34 C27 C26 122.2(6) 2_656 . ?
N34 C27 H27 115(4) 2_656 . ?
N34 C27 C28 17.5(7) 2_656 . ?
N34 C29 C28 17.4(7) 2_656 . ?
N30 C29 C28 121.2(12) . . ?
N30 C29 N34 117.7(11) . 2_656 ?
C37 C29 C28 121.2(16) 2_656 . ?
C37 C29 N34 117.8(14) 2_656 2_656 ?
C37 C29 N30 0(4) 2_656 . ?
H31 C31 C26 114(3) . . ?
N30 C31 C26 122.5(10) . . ?
N30 C31 H31 123(3) . . ?
C37 C31 C26 118.5(11) 2_656 . ?
C37 C31 H31 127(3) 2_656 . ?
C37 C31 N30 4.1(19) 2_656 . ?
H39b C39 H39a 109.5 . . ?
H39c C39 H39a 109.5 . . ?
H39c C39 H39b 109.5 . . ?
C40 C39 H39a 109.5 . . ?
C40 C39 H39b 109.5 . . ?
C40 C39 H39c 109.5 . . ?
C39 C40 O38 120.6(6) . . ?
C41 C40 O38 121.5(5) . . ?
C41 C40 C39 117.8(5) . . ?
H41a C41 C40 109.5 . . ?
H41b C41 C40 109.5 . . ?
H41b C41 H41a 109.5 . . ?
H41c C41 C40 109.5 . . ?
H41c C41 H41a 109.5 . . ?
H41c C41 H41b 109.5 . . ?
H43b C43 H43a 109.5 . . ?
H43c C43 H43a 109.5 . . ?
H43c C43 H43b 109.5 . . ?
C44 C43 H43a 109.5 . . ?
C44 C43 H43b 109.5 . . ?
C44 C43 H43c 109.5 . . ?
C43 C44 O42 121.6(4) . . ?
C45 C44 O42 120.4(4) . . ?
C45 C44 C43 118.0(4) . . ?
H45a C45 C44 109.5 . . ?
H45b C45 C44 109.5 . . ?
H45b C45 H45a 109.5 . . ?
H45c C45 C44 109.5 . . ?
H45c C45 H45a 109.5 . . ?
H45c C45 H45b 109.5 . . ?
H46b O46 H46a 107(4) . . ?
C29 C28 C27 118.0(8) . . ?
C35 C28 C27 121.0(11) . . ?
C35 C28 C29 118.7(12) . . ?
H33b C33 H33a 108.7 . . ?
N34 C33 H33a 110.6(6) . . ?
N34 C33 H33b 110.6(5) . . ?
C32 C33 H33a 110.6(8) . . ?
C32 C33 H33b 110.6(6) . . ?
C32 C33 N34 105.7(11) . . ?
C29 N34 C27 116.9(7) 2_656 2_656 ?
C33 N34 C27 124.8(10) . 2_656 ?
C33 N34 C29 117.8(9) . 2_656 ?
C31 N30 C29 117.5(13) . . ?
C32 N30 C29 113(3) . . ?
C32 N30 C31 129(2) . . ?
C31 C37 C29 121.6(16) 2_656 2_656 ?
C36 C37 C29 125(3) . 2_656 ?
C36 C37 C31 114(3) . 2_656 ?
N30 C32 C33 115.3(19) . . ?
H32a C32 C33 108.5(6) . . ?
H32a C32 N30 108(2) . . ?
H32b C32 C33 108.5(9) . . ?
H32b C32 N30 108.5(17) . . ?
H32b C32 H32a 107.5 . . ?
H36 C36 C37 123(2) . . ?
C35 C36 C37 113(3) . . ?
C35 C36 H36 123.5(10) . . ?
C36 C35 C28 124.2(13) . . ?
H35 C35 C28 117.9(7) . . ?
H35 C35 C36 117.9(10) . . ?
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 1.390(5) . ?
C2 C4 1.531(5) 2_666 ?
C2 O1 1.260(5) . ?
C3 C4 1.411(5) . ?
C3 Cl6 1.729(4) . ?
C4 O5 1.255(5) . ?
O5 La1 2.547(3) 2_666 ?
O7 C8 1.249(4) . ?
O7 La1 2.563(2) . ?
C8 C9 1.401(5) . ?
C8 C10 1.532(5) 2_667 ?
C9 C10 1.398(5) . ?
C9 Cl12 1.726(4) . ?
C10 O11 1.263(4) . ?
O11 La1 2.590(2) 2_667 ?
La1 O1 2.529(3) . ?
La1 O13 2.534(3) . ?
La1 O17 2.551(3) 2_777 ?
La1 O19 2.560(3) . ?
La1 O23 2.584(3) 2_766 ?
La1 O25 2.516(3) . ?
O13 C14 1.254(5) . ?
C14 C15 1.394(5) . ?
C14 C16 1.541(5) 2_777 ?
C15 C16 1.403(5) . ?
C15 Cl18 1.731(4) . ?
C16 O17 1.249(5) . ?
O19 C20 1.246(5) . ?
C20 C21 1.405(5) . ?
C20 C22 1.546(5) 2_766 ?
C21 C22 1.391(5) . ?
C21 Cl24 1.737(4) . ?
C22 O23 1.260(5) . ?
O25 H25a 0.832(18) . ?
O25 H25b 0.830(18) . ?
C26 H26 0.9500 . ?
C26 C27 1.358(7) . ?
C26 C31 1.393(7) . ?
C27 H27 0.9500(10) . ?
C27 C28 1.454(16) . ?
C27 N34 1.340(13) 2_656 ?
C29 C29 1.421(9) 2_656 ?
C29 C28 1.330(16) . ?
C29 N34 1.460(13) 2_656 ?
C29 N30 1.44(3) . ?
C29 C37 1.33(4) 2_656 ?
C31 H31 0.9500(10) . ?
C31 N30 1.35(3) . ?
C31 C37 1.41(4) 2_656 ?
O38 C40 1.195(6) . ?
C39 H39a 0.9800 . ?
C39 H39b 0.9800 . ?
C39 H39c 0.9800 . ?
C39 C40 1.464(9) . ?
C40 C41 1.489(7) . ?
C41 H41a 0.9800 . ?
C41 H41b 0.9800 . ?
C41 H41c 0.9800 . ?
O42 C44 1.231(5) . ?
C43 H43a 0.9800 . ?
C43 H43b 0.9800 . ?
C43 H43c 0.9800 . ?
C43 C44 1.495(6) . ?
C44 C45 1.486(6) . ?
C45 H45a 0.9800 . ?
C45 H45b 0.9800 . ?
C45 H45c 0.9800 . ?
O46 H46a 0.840(19) . ?
O46 H46b 0.843(18) . ?
C28 C35 1.445(12) . ?
C33 H33a 0.9900 . ?
C33 H33b 0.9900 . ?
C33 N34 1.483(11) . ?
C33 C32 1.517(14) . ?
N30 C32 1.485(15) . ?
C37 C36 1.428(16) . ?
C32 H32a 0.9900 . ?
C32 H32b 0.9900 . ?
C36 H36 0.9500 . ?
C36 C35 1.348(13) . ?
C35 H35 0.9500 . ?
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 8.0(3) . . . 2_666 ?
C2 C3 C4 O5 -170.0(3) . . . . ?
C2 C4 C3 C2 8.0(3) 2_666 . . . ?
C2 C4 C3 Cl6 -179.8(3) 2_666 . . . ?
C2 C4 O5 La1 -6.6(4) . 2_666 2_666 . ?
C3 C4 O5 La1 -175.3(3) . . . 2_666 ?
O7 C8 C9 C10 177.6(4) . . . . ?
O7 C8 C9 Cl12 0.7(4) . . . . ?
O7 C8 C10 C9 -177.7(3) . . 2_667 2_667 ?
O7 C8 C10 O11 3.7(4) . . 2_667 2_667 ?
C8 C9 C10 C8 1.7(4) . . . 2_667 ?
C8 C9 C10 O11 -176.7(4) . . . . ?
C8 C10 C9 C8 1.7(3) 2_667 . . . ?
C8 C10 C9 Cl12 178.6(3) 2_667 . . . ?
C8 C10 O11 La1 -2.6(4) . 2_667 2_667 . ?
C9 C10 O11 La1 -178.9(3) . . . 2_667 ?
La1 O13 C14 C15 170.5(3) . . . . ?
La1 O13 C14 C16 -10.9(3) . . . 2_777 ?
La1 O17 C16 C14 12.8(3) . 2_777 2_777 . ?
La1 O17 C16 C15 167.3(3) 2_777 . . . ?
La1 O19 C20 C21 -155.4(3) . . . . ?
La1 O19 C20 C22 24.9(2) . . . 2_766 ?
La1 O23 C22 C20 -23.2(2) . 2_766 2_766 . ?
La1 O23 C22 C21 -155.9(3) 2_766 . . . ?
O13 C14 C15 C16 -178.9(4) . . . . ?
O13 C14 C15 Cl18 0.7(4) . . . . ?
O13 C14 C16 C15 178.8(3) . . 2_777 2_777 ?
O13 C14 C16 O17 -1.3(4) . . 2_777 2_777 ?
C14 C15 C16 C14 -2.6(4) . . . 2_777 ?
C14 C15 C16 O17 177.2(4) . . . . ?
C14 C16 C15 C14 -2.6(3) 2_777 . . . ?
C14 C16 C15 Cl18 177.8(3) 2_777 . . . ?
O19 C20 C21 C22 -179.9(4) . . . . ?
O19 C20 C21 Cl24 1.1(4) . . . . ?
O19 C20 C22 C21 180.0(3) . . 2_766 2_766 ?
O19 C20 C22 O23 -0.9(4) . . 2_766 2_766 ?
C20 C21 C22 C20 0.2(4) . . . 2_766 ?
C20 C21 C22 O23 179.3(3) . . . . ?
C20 C22 C21 C20 0.2(3) 2_766 . . . ?
C20 C22 C21 Cl24 179.2(3) 2_766 . . . ?
C26 C27 C28 C29 17.4(6) . . . . ?
C26 C27 C28 C35 -179.9(8) . . . . ?
C26 C27 N34 C29 -21.8(7) . . 2_656 . ?
C26 C27 N34 C33 165.8(7) . . 2_656 2_656 ?
C26 C31 N30 C29 -0.2(5) . . . . ?
C26 C31 N30 C32 -169(2) . . . . ?
C26 C31 C37 C29 -0.6(5) . . 2_656 . ?
C26 C31 C37 C36 179(3) . . 2_656 2_656 ?
C27 C28 C29 C29 172.2(7) . . . 2_656 ?
C27 C28 C29 N34 67.6(17) . . . 2_656 ?
C27 C28 C29 N30 -16(3) . . . . ?
C27 C28 C29 C37 -16(3) . . . 2_656 ?
C27 C28 C35 C36 -164.7(11) . . . . ?
C27 N34 C29 C29 -169.1(6) . 2_656 . 2_656 ?
C27 N34 C29 C28 -83.6(18) . 2_656 . . ?
C27 N34 C29 N30 23(2) . 2_656 . . ?
C27 N34 C29 C37 22(3) . 2_656 . 2_656 ?
C27 N34 C33 C32 -135.1(10) 2_656 . . . ?
C29 C29 C28 C35 9.2(8) 2_656 . . . ?
C29 C29 N34 C33 -3.8(7) . 2_656 . . ?
C29 C29 N30 C31 180(3) 2_656 . . . ?
C29 C29 N30 C32 -10.0(9) 2_656 . . . ?
C29 C29 C37 C31 -180(3) . 2_656 . 2_656 ?
C29 C29 C37 C36 -0.3(11) . 2_656 . . ?
C29 C28 C35 C36 -2.2(14) . . . . ?
C29 N34 C33 C32 37.2(9) 2_656 . . . ?
C29 N30 C31 C37 -3(10) . . . 2_656 ?
C29 N30 C32 C33 48(4) . . . . ?
C29 C37 C31 N30 177(11) . 2_656 . . ?
C29 C37 C36 C35 7(6) 2_656 . . . ?
C31 N30 C32 C33 -143(4) . . . . ?
C31 C37 C36 C35 -174(3) 2_656 . . . ?
C28 C35 C36 C37 -6(3) . . . . ?
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O25 H25a 1 0.8400 0.0200 0.0085
O25 H25b 1 0.8400 0.0200 0.0102
H25a H25b 1 1.3400 0.0400 -0.0049
C27 H27 1 0.9500 0.0010 -0.0000
C31 H31 1 0.9500 0.0010 0.0000
O46 H46a 1 0.8400 0.0200 0.0005
O46 H46b 1 0.8400 0.0200 -0.0031
H46a H46b 1 1.3400 0.0400 -0.0112
C28 C35 1 1.4300 0.0200 -0.0148
N34 C33 1 1.4800 0.0200 -0.0029
N30 C32 1 1.4800 0.0200 -0.0047
C32 C33 1 1.5100 0.0200 -0.0075
C36 C37 1 1.4300 0.0200 0.0023
C35 C36 1 1.3500 0.0200 0.0018
loop_
_restr_U_similar_atom_site_label_1
_restr_U_similar_atom_site_label_2
_restr_U_similar_weight_param
C26 C27 0.0400
C26 C31 0.0400
C27 C28 0.0400
C29 C28 0.0400
C29 N30 0.0400
C31 N30 0.0400
C33 C32 0.0400
N30 C32 0.0400
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
-3.0370 -5.3038 0.5611 0.8025 0.2389 0.5467
3.1021 5.4133 -1.8363 -0.7126 -0.2123 -0.6686
0.0413 0.0985 8.0195 -0.6913 -0.2046 0.6930
-0.3410 -0.6213 -7.7478 0.7522 0.2228 -0.6201
6.3650 -4.8912 0.0905 -0.2844 0.9575 -0.0478
-6.4409 4.7131 0.2209 0.2837 -0.9547 0.0903
3.0179 -6.3291 5.3429 -0.2056 0.6958 0.6882
3.0360 3.1295 -7.1764 -0.0394 0.1273 -0.9911
2.2946 -7.2430 0.1100 0.4060 0.8532 0.3275
loop_
_restr_rigu_atom_site_label_1
_restr_rigu_atom_site_label_2
_restr_rigu_target_weight_param
_restr_rigu_u13_diff
_restr_rigu_u23_diff
_restr_rigu_u33_diff
C26 C27 0.004000 -0.002719 -0.007853 -0.004401
C26 C31 0.004000 -0.005868 0.005911 -0.003888
C26 C28 0.004000 -0.000392 0.000752 0.005213
C26 N30 0.004000 -0.008839 0.007540 0.005891
C27 C29 0.004000 -0.004035 0.002903 -0.003360
C27 C31 0.004000 -0.013502 0.014436 0.000739
C27 C28 0.004000 -0.002233 0.007515 0.002642
C29 C31 0.004000 0.002841 -0.001099 -0.000680
C29 C28 0.004000 -0.001217 0.002465 0.001137
C29 N30 0.004000 0.001882 0.000704 0.002266
C29 C32 0.004000 -0.005328 0.016176 0.002217
C31 N30 0.004000 -0.008136 0.001731 0.004850
C31 C32 0.004000 -0.003348 0.005621 0.014815
O38 C39 0.004000 0.001560 0.029666 -0.010494
O38 C40 0.004000 -0.007014 0.012554 -0.000474
O38 C41 0.004000 -0.020921 0.002382 -0.003067
C39 C40 0.004000 0.004664 -0.003736 0.005716
C39 C41 0.004000 0.011127 0.019771 0.004817
C40 C41 0.004000 -0.003368 -0.001862 0.000212
C28 N30 0.004000 -0.001121 0.002476 0.001832
C33 N30 0.004000 -0.001438 0.001136 -0.007475
C33 C32 0.004000 0.002745 0.000975 -0.000201
N30 C32 0.004000 0.002794 0.006059 -0.000489
