#------------------------------------------------------------------------------
#$Date: 2023-11-22 12:08:01 +0200 (Wed, 22 Nov 2023) $
#$Revision: 287733 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/76/8107660.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_8107660
loop_
_publ_author_name
'Ying, Liu'
'Xi-Hai, Yan'
'Yuan-Fang, Wang'
'Xi-Shi, Tai'
_publ_section_title
;
 The crystal structure of catena-[diaqua-(4-acetylphenoxyacetato-κ 2
 O,O)-bis(4-acetylphenoxyacetato-κ 3
 O,O:O)-dihydrate-lanthanum(III)]--4,4′-bipyridine (2/1),
 C35H35NO14La
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1061
_journal_page_last               1063
_journal_paper_doi               10.1515/ncrs-2023-0301
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C30 H31 La O14, C5 H4 N'
_chemical_formula_sum            'C35 H35 La N O14'
_chemical_formula_weight         832.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                115.2310(10)
_cell_angle_beta                 97.4010(10)
_cell_angle_gamma                95.4830(10)
_cell_formula_units_Z            2
_cell_length_a                   9.06760(10)
_cell_length_b                   13.6139(2)
_cell_length_c                   15.5964(2)
_cell_measurement_reflns_used    14858
_cell_measurement_temperature    296.13(10)
_cell_measurement_theta_max      76.9300
_cell_measurement_theta_min      3.1820
_cell_volume                     1702.65(4)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.13(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 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     95.00 139.00   0.50    0.10    --  107.75  57.00-120.00   88
  2  ω    138.00 176.00   0.50    0.10    --  107.75  37.00 -30.00   76
  3  ω     98.00 124.00   0.50    0.10    --  107.75  37.00 -30.00   52
  4  ω    115.00 169.00   0.50    0.10    --  107.75  57.00  90.00  108
  5  ω    -40.00  18.00   0.50    0.05    --  -47.70  37.00 -60.00  116
  6  ω    -27.00  26.00   0.50    0.05    --  -47.70  19.00  90.00  106
  7  ω     -4.00  21.00   0.50    0.05    --  -47.70  19.00-150.00   50
  8  ω     83.00 112.00   0.50    0.10    --  107.75-125.00-120.00   58
  9  ω     70.00 110.00   0.50    0.10    --  107.75-125.00 -60.00   80
 10  ω     36.00  61.00   0.50    0.10    --  107.75-125.00 -60.00   50
 11  ω     79.00 112.00   0.50    0.10    --  107.75-125.00  60.00   66
 12  ω     80.00 112.00   0.50    0.10    --  107.75-125.00  90.00   64
 13  ω     37.00  66.00   0.50    0.10    --  107.75-125.00  90.00   58
 14  ω     35.00  87.00   0.50    0.10    --  107.75 -99.00  30.00  104
 15  ω     60.00 108.00   0.50    0.10    --  107.75-112.00 103.00   96
 16  ω     39.00  78.00   0.50    0.10    --  107.75 -99.00   0.00   78
 17  ω     35.00 106.00   0.50    0.10    --  107.75 -99.00 -60.00  142
 18  ω     38.00  64.00   0.50    0.05    --   47.70-112.00 103.00   52
 19  ω     76.00 101.00   0.50    0.10    --  107.75 -99.00 120.00   50
 20  ω     41.00  72.00   0.50    0.10    --  107.75 -99.00 120.00   62
 21  ω     36.00  67.00   0.50    0.10    --  107.75 -77.00 120.00   62
 22  ω     74.00  99.00   0.50    0.10    --  107.75 -77.00 120.00   50
 23  ω     40.00  65.00   0.50    0.10    --  107.75 -57.00   0.00   50
 24  ω     41.00  71.00   0.50    0.10    --  107.75 -77.00-180.00   60
 25  ω     76.00 101.00   0.50    0.10    --  107.75 -77.00-180.00   50
 26  ω     38.00  66.00   0.50    0.10    --  107.75 -57.00 -60.00   56
 27  ω     -4.00  25.00   0.50    0.05    --   47.70 -19.00  90.00   58
 28  ω     36.00  65.00   0.50    0.10    --  107.75 -57.00 120.00   58
 29  ω     35.00  65.00   0.50    0.10    --  107.75 -57.00 150.00   60
 30  ω    104.00 152.00   0.50    0.10    --  107.75 112.00-163.00   96
 31  ω     98.00 148.00   0.50    0.10    --  107.75 125.00 -30.00  100
 32  ω     95.00 146.00   0.50    0.10    --  107.75 125.00  90.00  102
 33  ω    -65.00 -14.00   0.50    0.10    --  -86.25  57.00  90.00  102
 34  ω    -41.00 -13.00   0.50    0.10    --  -86.25  37.00  60.00   56
 35  ω    -41.00 -16.00   0.50    0.10    --  -86.25  37.00 -30.00   50
 36  ω    -42.00 -15.00   0.50    0.10    --  -86.25  37.00-120.00   54
 37  ω    -82.00 -51.00   0.50    0.05    --  -47.70 112.00-163.00   62
 38  ω    -76.00 -51.00   0.50    0.10    --  -86.25 112.00-163.00   50
 39  ω    -83.00 -20.00   0.50    0.10    --  -86.25 125.00-150.00  126
 40  ω    -42.00  -4.00   0.50    0.05    --  -47.70 112.00-163.00   76
 41  ω   -121.00 -43.00   0.50    0.05    --  -47.70 -19.00 -90.00  156
 42  ω   -160.00-123.00   0.50    0.10    --  -86.25 -19.00 -30.00   74
 43  ω   -117.00 -90.00   0.50    0.10    --  -86.25 -19.00 -30.00   54
 44  ω   -154.00 -72.00   0.50    0.10    --  -86.25 -57.00 120.00  164
 45  ω   -107.00 -76.00   0.50    0.05    --  -47.70-125.00 -90.00   62
 46  ω   -126.00 -97.00   0.50    0.10    --  -86.25 -99.00-150.00   58
 47  ω   -136.00 -88.00   0.50    0.10    --  -86.25-112.00 103.00   96
;
_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      -0.0573278000
_diffrn_orient_matrix_UB_12      0.0068035000
_diffrn_orient_matrix_UB_13      -0.0943685000
_diffrn_orient_matrix_UB_21      0.0313264000
_diffrn_orient_matrix_UB_22      0.1267091000
_diffrn_orient_matrix_UB_23      0.0546648000
_diffrn_orient_matrix_UB_31      0.1610401000
_diffrn_orient_matrix_UB_32      0.0007435000
_diffrn_orient_matrix_UB_33      -0.0216348000
_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  0.0857
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20535
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.017
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         6027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0431
_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)+(0.0644P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5689
_reflns_number_total             6027
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0301_suppl_001.cif
_cod_data_source_block           5-1
_cod_database_code               8107660
_chemical_oxdiff_formula         'C H N O La'
_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   0.425
_shelx_estimated_absorpt_t_min   0.307
_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.a Rotating group:
 O13(H13A,H13B), O14(H14A,H14B)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C14(H14), C15(H15), C17(H17), C18(H18), C24(H24),
 C25(H25), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C)
;
_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 4.753
_oxdiff_exptl_absorpt_empirical_full_min 0.334
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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
C1 C -0.1419(5) 0.0841(4) 0.6624(3) 0.0348(10) Uani 1 1 d . . . . .
C2 C 0.4679(6) 0.4837(4) 0.0347(3) 0.0348(10) Uani 1 1 d . . . . .
C3 C -0.0142(5) 0.2351(4) 0.6426(3) 0.0332(10) Uani 1 1 d . . . . .
H3 H 0.035286 0.260429 0.605409 0.040 Uiso 1 1 calc R U . . .
C4 C -0.0382(5) 0.3086(4) 0.7318(3) 0.0283(9) Uani 1 1 d . . . . .
C5 C -0.1217(6) 0.2705(4) 0.7835(4) 0.0427(12) Uani 1 1 d . . . . .
H5 H -0.141810 0.319931 0.842141 0.051 Uiso 1 1 calc R U . . .
C6 C -0.1746(6) 0.1596(4) 0.7481(4) 0.0427(12) Uani 1 1 d . . . . .
H6 H -0.233106 0.135119 0.782157 0.051 Uiso 1 1 calc R U . . .
C7 C -0.1735(6) -0.0364(4) 0.6306(4) 0.0380(10) Uani 1 1 d . . . . .
C8 C -0.2797(8) -0.0798(5) 0.6772(6) 0.073(2) Uani 1 1 d . . . . .
H8A H -0.303688 -0.158576 0.641933 0.109 Uiso 1 1 calc R U . . .
H8B H -0.370546 -0.048920 0.676891 0.109 Uiso 1 1 calc R U . . .
H8C H -0.233076 -0.059750 0.742493 0.109 Uiso 1 1 calc R U . . .
C9 C 0.0941(5) 0.4635(3) 0.7237(3) 0.0273(8) Uani 1 1 d . . . . .
H9A H 0.162746 0.415548 0.691842 0.033 Uiso 1 1 calc R U . . .
H9B H 0.153561 0.534735 0.767867 0.033 Uiso 1 1 calc R U . . .
C10 C -0.0147(4) 0.4769(3) 0.6486(3) 0.0236(8) Uani 1 1 d . . . . .
C11 C 0.3149(4) 0.7031(3) 0.6507(3) 0.0255(8) Uani 1 1 d . . . . .
C12 C 0.3619(5) 0.8198(4) 0.7278(3) 0.0315(9) Uani 1 1 d . . . . .
H12A H 0.404309 0.865586 0.700465 0.038 Uiso 1 1 calc R U . . .
H12B H 0.274546 0.848268 0.752905 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5544(5) 0.9232(4) 0.8672(3) 0.0354(10) Uani 1 1 d . . . . .
C14 C 0.6763(7) 0.9180(4) 0.9272(4) 0.0494(13) Uani 1 1 d . . . . .
H14 H 0.694867 0.850324 0.923149 0.059 Uiso 1 1 calc R U . . .
C15 C 0.7706(6) 1.0141(5) 0.9933(4) 0.0483(12) Uani 1 1 d . . . . .
H15 H 0.851530 1.010169 1.034292 0.058 Uiso 1 1 calc R U . . .
C16 C 0.7469(5) 1.1165(4) 0.9999(3) 0.0392(11) Uani 1 1 d . . . . .
C17 C 0.6228(6) 1.1189(4) 0.9387(4) 0.0449(12) Uani 1 1 d . . . . .
H17 H 0.604634 1.186203 0.941519 0.054 Uiso 1 1 calc R U . . .
C18 C 0.5257(6) 1.0237(4) 0.8739(4) 0.0427(12) Uani 1 1 d . . . . .
H18 H 0.441600 1.027378 0.835137 0.051 Uiso 1 1 calc R U . . .
C19 C 0.9689(7) 1.2234(6) 1.1442(4) 0.0652(17) Uani 1 1 d . . . . .
H19A H 1.038169 1.291600 1.170830 0.098 Uiso 1 1 calc R U . . .
H19B H 1.022169 1.163024 1.116797 0.098 Uiso 1 1 calc R U . . .
H19C H 0.923193 1.217278 1.194315 0.098 Uiso 1 1 calc R U . . .
C20 C 0.8482(6) 1.2208(5) 1.0669(4) 0.0505(14) Uani 1 1 d . . . . .
C21 C 0.5401(4) 0.6472(3) 0.4444(3) 0.0243(8) Uani 1 1 d . . . . .
C22 C 0.4375(5) 0.7158(4) 0.4193(4) 0.0362(10) Uani 1 1 d . . . . .
H22A H 0.389577 0.675613 0.351858 0.043 Uiso 1 1 calc R U . . .
H22B H 0.358821 0.727068 0.457526 0.043 Uiso 1 1 calc R U . . .
C23 C 0.5870(5) 0.8301(4) 0.3677(3) 0.0316(10) Uani 1 1 d . . . . .
C24 C 0.6590(5) 0.9359(4) 0.3927(4) 0.0374(10) Uani 1 1 d . . . . .
H24 H 0.654183 0.993298 0.451763 0.045 Uiso 1 1 calc R U . . .
C25 C 0.7376(5) 0.9563(4) 0.3305(4) 0.0377(10) Uani 1 1 d . . . . .
H25 H 0.785780 1.027308 0.347961 0.045 Uiso 1 1 calc R U . . .
C26 C 0.7454(5) 0.8707(4) 0.2412(3) 0.0382(11) Uani 1 1 d . . . . .
C27 C 0.5931(6) 0.7442(4) 0.2798(4) 0.0409(11) Uani 1 1 d . . . . .
H27 H 0.545767 0.673054 0.262820 0.049 Uiso 1 1 calc R U . . .
C28 C 0.6716(6) 0.7664(5) 0.2173(4) 0.0438(12) Uani 1 1 d . . . . .
H28 H 0.674481 0.709240 0.157623 0.053 Uiso 1 1 calc R U . . .
C29 C 0.8324(6) 0.8961(5) 0.1766(4) 0.0470(13) Uani 1 1 d . . . . .
C30 C 0.8447(8) 0.8033(7) 0.0832(5) 0.0706(19) Uani 1 1 d . . . . .
H30A H 0.746886 0.774606 0.042242 0.106 Uiso 1 1 calc R U . . .
H30B H 0.882915 0.746109 0.095250 0.106 Uiso 1 1 calc R U . . .
H30C H 0.912125 0.829514 0.051957 0.106 Uiso 1 1 calc R U . . .
C31 C 0.2725(7) 0.4665(6) 0.1193(5) 0.0627(17) Uani 1 1 d . . . . .
H31 H 0.176248 0.478198 0.131182 0.075 Uiso 1 1 calc R U . . .
C32 C 0.3258(7) 0.4992(6) 0.0548(5) 0.0613(17) Uani 1 1 d . . . . .
H32 H 0.265793 0.531583 0.024849 0.074 Uiso 1 1 calc R U . . .
C33 C -0.0641(5) 0.1240(4) 0.6092(3) 0.0329(10) Uani 1 1 d . . . . .
H33 H -0.045413 0.074645 0.550041 0.039 Uiso 1 1 calc R U . . .
C34 C 0.5486(6) 0.4340(5) 0.0823(4) 0.0437(11) Uani 1 1 d . . . . .
H34 H 0.645012 0.421078 0.071762 0.052 Uiso 1 1 calc R U . . .
C35 C 0.4857(6) 0.4038(5) 0.1454(4) 0.0516(13) Uani 1 1 d . . . . .
H35 H 0.542294 0.370254 0.175865 0.062 Uiso 1 1 calc R U . . .
La1 La 0.24448(2) 0.47768(2) 0.48636(2) 0.01943(12) Uani 1 1 d . . . . .
N1 N 0.3492(6) 0.4198(4) 0.1654(3) 0.0498(11) Uani 1 1 d . . . . .
O1 O -0.1120(4) -0.0992(3) 0.5698(3) 0.0456(8) Uani 1 1 d . . . . .
O2 O 0.0200(4) 0.4187(2) 0.7774(2) 0.0334(7) Uani 1 1 d . . . . .
O3 O -0.1517(3) 0.4673(3) 0.6492(2) 0.0326(7) Uani 1 1 d . . . . .
O4 O 0.0399(3) 0.5028(3) 0.5891(2) 0.0299(6) Uani 1 1 d . . . . .
O5 O 0.2229(3) 0.6875(2) 0.5763(2) 0.0293(6) Uani 1 1 d . . . . .
O6 O 0.3696(3) 0.6257(2) 0.6599(2) 0.0290(6) Uani 1 1 d . . . . .
O7 O 0.4704(4) 0.8237(3) 0.8035(2) 0.0445(8) Uani 1 1 d . . . . .
O8 O 0.8368(6) 1.3057(4) 1.0591(4) 0.0827(16) Uani 1 1 d . . . . .
O9 O 0.4850(3) 0.5850(2) 0.4778(2) 0.0298(6) Uani 1 1 d . . . . .
O10 O 0.6731(3) 0.6523(3) 0.4340(3) 0.0376(7) Uani 1 1 d . . . . .
O11 O 0.5147(4) 0.8203(3) 0.4358(3) 0.0390(7) Uani 1 1 d . . . . .
O12 O 0.8896(5) 0.9897(4) 0.1976(3) 0.0627(11) Uani 1 1 d . . . . .
O13 O 0.0700(3) 0.2935(2) 0.4161(3) 0.0396(7) Uani 1 1 d . . . . .
H13A H -0.015205 0.302944 0.433903 0.059 Uiso 1 1 d R U . . .
H13B H 0.104598 0.253082 0.440932 0.059 Uiso 1 1 d R U . . .
O14 O 0.3182(3) 0.3605(3) 0.3231(2) 0.0341(7) Uani 1 1 d . . . . .
H14A H 0.412365 0.358901 0.331834 0.051 Uiso 1 1 d R U . . .
H14B H 0.306277 0.392443 0.286804 0.051 Uiso 1 1 d R 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'
La La -1.4094 9.0376 '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'
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
C6 C1 C7 122.4(4) . .
C6 C1 C33 118.2(4) . .
C33 C1 C7 119.1(4) . .
C32 C2 C2 122.8(5) . 2_665
C32 C2 C34 115.8(4) . .
C34 C2 C2 121.4(5) . 2_665
C4 C3 H3 120.2 . .
C33 C3 H3 120.2 . .
C33 C3 C4 119.6(4) . .
C3 C4 C5 119.5(4) . .
O2 C4 C3 125.1(4) . .
O2 C4 C5 115.3(4) . .
C4 C5 H5 119.9 . .
C6 C5 C4 120.2(4) . .
C6 C5 H5 119.9 . .
C1 C6 H6 119.5 . .
C5 C6 C1 120.9(4) . .
C5 C6 H6 119.5 . .
C1 C7 C8 118.7(4) . .
O1 C7 C1 121.3(4) . .
O1 C7 C8 120.0(4) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
H9A C9 H9B 107.8 . .
C10 C9 H9A 109.0 . .
C10 C9 H9B 109.0 . .
O2 C9 H9A 109.0 . .
O2 C9 H9B 109.0 . .
O2 C9 C10 112.9(3) . .
C9 C10 La1 174.3(3) . 2_566
O3 C10 C9 120.3(4) . .
O3 C10 La1 56.7(2) . 2_566
O3 C10 O4 121.8(4) . .
O4 C10 C9 117.8(4) . .
O4 C10 La1 65.1(2) . 2_566
O5 C11 C12 117.2(4) . .
O6 C11 C12 120.5(4) . .
O6 C11 O5 122.3(4) . .
C11 C12 H12A 109.7 . .
C11 C12 H12B 109.7 . .
H12A C12 H12B 108.2 . .
O7 C12 C11 110.0(4) . .
O7 C12 H12A 109.7 . .
O7 C12 H12B 109.7 . .
C18 C13 C14 120.2(4) . .
O7 C13 C14 114.9(4) . .
O7 C13 C18 124.9(4) . .
C13 C14 H14 120.2 . .
C13 C14 C15 119.7(5) . .
C15 C14 H14 120.2 . .
C14 C15 H15 119.3 . .
C14 C15 C16 121.4(4) . .
C16 C15 H15 119.3 . .
C15 C16 C20 123.2(5) . .
C17 C16 C15 117.5(4) . .
C17 C16 C20 119.3(5) . .
C16 C17 H17 119.2 . .
C18 C17 C16 121.6(5) . .
C18 C17 H17 119.2 . .
C13 C18 C17 119.6(4) . .
C13 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C20 C19 H19A 109.5 . .
C20 C19 H19B 109.5 . .
C20 C19 H19C 109.5 . .
C16 C20 C19 120.4(6) . .
O8 C20 C16 120.5(5) . .
O8 C20 C19 119.1(5) . .
C22 C21 La1 175.1(3) . 2_666
O9 C21 C22 117.2(3) . .
O9 C21 La1 62.4(2) . 2_666
O10 C21 C22 121.5(4) . .
O10 C21 La1 59.0(2) . 2_666
O10 C21 O9 121.3(4) . .
C21 C22 H22A 109.0 . .
C21 C22 H22B 109.0 . .
H22A C22 H22B 107.8 . .
O11 C22 C21 113.1(4) . .
O11 C22 H22A 109.0 . .
O11 C22 H22B 109.0 . .
C27 C23 C24 120.3(4) . .
O11 C23 C24 114.8(4) . .
O11 C23 C27 125.0(4) . .
C23 C24 H24 119.8 . .
C25 C24 C23 120.4(5) . .
C25 C24 H24 119.8 . .
C24 C25 H25 119.8 . .
C24 C25 C26 120.4(5) . .
C26 C25 H25 119.8 . .
C25 C26 C29 118.7(5) . .
C28 C26 C25 118.3(4) . .
C28 C26 C29 123.0(5) . .
C23 C27 H27 120.7 . .
C23 C27 C28 118.6(5) . .
C28 C27 H27 120.7 . .
C26 C28 C27 122.0(5) . .
C26 C28 H28 119.0 . .
C27 C28 H28 119.0 . .
C26 C29 C30 118.1(5) . .
O12 C29 C26 121.4(5) . .
O12 C29 C30 120.4(5) . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C32 C31 H31 117.8 . .
N1 C31 H31 117.8 . .
N1 C31 C32 124.4(5) . .
C2 C32 C31 120.0(5) . .
C2 C32 H32 120.0 . .
C31 C32 H32 120.0 . .
C1 C33 H33 119.3 . .
C3 C33 C1 121.3(4) . .
C3 C33 H33 119.3 . .
C2 C34 H34 120.0 . .
C35 C34 C2 120.0(5) . .
C35 C34 H34 120.0 . .
C34 C35 H35 118.0 . .
N1 C35 C34 124.1(5) . .
N1 C35 H35 118.0 . .
C10 La1 C21 159.22(10) 2_566 2_666
O3 La1 C10 23.49(10) 2_566 2_566
O3 La1 C21 146.72(9) 2_566 2_666
O3 La1 O4 47.83(8) 2_566 2_566
O3 La1 O5 74.66(10) 2_566 .
O3 La1 O6 121.42(10) 2_566 .
O3 La1 O9 127.64(8) 2_566 2_666
O3 La1 O10 158.03(11) 2_566 2_666
O4 La1 C10 24.36(10) 2_566 2_566
O4 La1 C10 84.91(10) . 2_566
O4 La1 C21 151.64(10) 2_566 2_666
O4 La1 C21 104.54(10) . 2_666
O4 La1 O3 107.01(9) . 2_566
O4 La1 O4 61.77(10) . 2_566
O4 La1 O5 69.84(9) . .
O4 La1 O6 73.59(9) . .
O4 La1 O9 125.27(9) . 2_666
O4 La1 O10 83.02(9) . 2_666
O4 La1 O14 145.76(10) . .
O5 La1 C10 73.27(9) . 2_566
O5 La1 C21 127.21(9) . 2_666
O5 La1 O4 73.87(9) . 2_566
O5 La1 O9 118.30(9) . 2_666
O5 La1 O10 127.29(10) . 2_666
O6 La1 C10 123.02(9) . 2_566
O6 La1 C21 77.69(9) . 2_666
O6 La1 O4 117.38(8) . 2_566
O6 La1 O5 49.88(9) . .
O6 La1 O9 75.71(9) . 2_666
O6 La1 O10 79.87(10) . 2_666
O9 La1 C10 149.45(9) 2_666 2_566
O9 La1 C10 99.51(10) . 2_566
O9 La1 C21 24.13(9) 2_666 2_666
O9 La1 C21 85.11(9) . 2_666
O9 La1 O3 77.45(9) . 2_566
O9 La1 O4 121.75(9) . 2_566
O9 La1 O4 140.27(10) . .
O9 La1 O4 166.88(10) 2_666 2_566
O9 La1 O5 73.75(9) . .
O9 La1 O6 71.04(9) . .
O9 La1 O9 61.45(10) . 2_666
O9 La1 O10 107.64(9) . 2_666
O9 La1 O14 73.01(10) . .
O10 La1 C10 149.50(10) 2_666 2_566
O10 La1 C21 23.39(10) 2_666 2_666
O10 La1 O4 130.50(9) 2_666 2_566
O10 La1 O9 47.49(8) 2_666 2_666
O13 La1 C10 82.90(11) . 2_566
O13 La1 C21 82.25(10) . 2_666
O13 La1 O3 96.80(11) . 2_566
O13 La1 O4 70.21(10) . 2_566
O13 La1 O4 73.29(10) . .
O13 La1 O5 137.33(9) . .
O13 La1 O6 135.13(11) . .
O13 La1 O9 100.22(9) . 2_666
O13 La1 O9 146.36(10) . .
O13 La1 O10 66.83(11) . 2_666
O13 La1 O14 74.43(11) . .
O14 La1 C10 80.07(10) . 2_566
O14 La1 C21 81.99(10) . 2_666
O14 La1 O3 65.94(10) . 2_566
O14 La1 O4 96.54(9) . 2_566
O14 La1 O5 132.66(10) . .
O14 La1 O6 139.82(9) . .
O14 La1 O9 71.75(9) . 2_666
O14 La1 O10 94.61(10) . 2_666
C31 N1 C35 115.6(4) . .
C4 O2 C9 117.2(3) . .
C10 O3 La1 99.8(2) . 2_566
C10 O4 La1 90.5(2) . 2_566
C10 O4 La1 145.6(3) . .
La1 O4 La1 118.23(10) . 2_566
C11 O5 La1 93.2(2) . .
C11 O6 La1 94.4(2) . .
C13 O7 C12 118.3(4) . .
C21 O9 La1 93.4(2) . 2_666
C21 O9 La1 145.9(3) . .
La1 O9 La1 118.55(10) . 2_666
C21 O10 La1 97.6(2) . 2_666
C23 O11 C22 120.3(4) . .
La1 O13 H13A 109.7 . .
La1 O13 H13B 109.6 . .
H13A O13 H13B 104.2 . .
La1 O14 H14A 109.4 . .
La1 O14 H14B 109.5 . .
H14A O14 H14B 104.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.385(7) .
C1 C7 1.482(7) .
C1 C33 1.394(7) .
C2 C2 1.494(9) 2_665
C2 C32 1.379(7) .
C2 C34 1.388(7) .
C3 H3 0.9300 .
C3 C4 1.385(6) .
C3 C33 1.379(7) .
C4 C5 1.391(7) .
C4 O2 1.369(5) .
C5 H5 0.9300 .
C5 C6 1.377(7) .
C6 H6 0.9300 .
C7 C8 1.497(7) .
C7 O1 1.215(6) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C10 1.517(5) .
C9 O2 1.422(5) .
C10 La1 3.062(4) 2_566
C10 O3 1.238(5) .
C10 O4 1.263(5) .
C11 C12 1.504(6) .
C11 O5 1.262(5) .
C11 O6 1.260(5) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 O7 1.415(5) .
C13 C14 1.381(7) .
C13 C18 1.379(7) .
C13 O7 1.365(6) .
C14 H14 0.9300 .
C14 C15 1.383(8) .
C15 H15 0.9300 .
C15 C16 1.394(8) .
C16 C17 1.391(7) .
C16 C20 1.480(7) .
C17 H17 0.9300 .
C17 C18 1.383(7) .
C18 H18 0.9300 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C19 C20 1.506(9) .
C20 O8 1.225(8) .
C21 C22 1.508(6) .
C21 La1 3.087(4) 2_666
C21 O9 1.264(5) .
C21 O10 1.236(5) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C22 O11 1.426(6) .
C23 C24 1.389(7) .
C23 C27 1.384(7) .
C23 O11 1.363(6) .
C24 H24 0.9300 .
C24 C25 1.376(7) .
C25 H25 0.9300 .
C25 C26 1.400(7) .
C26 C28 1.381(8) .
C26 C29 1.485(7) .
C27 H27 0.9300 .
C27 C28 1.392(8) .
C28 H28 0.9300 .
C29 C30 1.494(9) .
C29 O12 1.214(8) .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C31 H31 0.9300 .
C31 C32 1.382(8) .
C31 N1 1.323(7) .
C32 H32 0.9300 .
C33 H33 0.9300 .
C34 H34 0.9300 .
C34 C35 1.381(8) .
C35 H35 0.9300 .
C35 N1 1.329(7) .
La1 O3 2.598(3) 2_566
La1 O4 2.778(3) 2_566
La1 O4 2.558(3) .
La1 O5 2.632(3) .
La1 O6 2.607(3) .
La1 O9 2.741(3) 2_666
La1 O9 2.558(3) .
La1 O10 2.670(3) 2_666
La1 O13 2.539(3) .
La1 O14 2.579(3) .
O13 H13A 0.8564 .
O13 H13B 0.8566 .
O14 H14A 0.8515 .
O14 H14B 0.8506 .
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
C2 C2 C32 C31 179.6(7) 2_665 . . .
C2 C2 C34 C35 -179.4(6) 2_665 . . .
C2 C34 C35 N1 -0.5(9) . . . .
C3 C4 C5 C6 2.8(8) . . . .
C3 C4 O2 C9 8.7(6) . . . .
C4 C3 C33 C1 1.7(7) . . . .
C4 C5 C6 C1 2.1(9) . . . .
C5 C4 O2 C9 -174.2(4) . . . .
C6 C1 C7 C8 16.7(8) . . . .
C6 C1 C7 O1 -161.4(5) . . . .
C6 C1 C33 C3 3.0(7) . . . .
C7 C1 C6 C5 169.1(5) . . . .
C7 C1 C33 C3 -171.1(4) . . . .
C9 C10 O3 La1 174.2(3) . . . 2_566
C9 C10 O4 La1 -174.5(3) . . . 2_566
C9 C10 O4 La1 37.1(6) . . . .
C10 C9 O2 C4 74.5(4) . . . .
C11 C12 O7 C13 163.5(4) . . . .
C12 C11 O5 La1 173.3(3) . . . .
C12 C11 O6 La1 -173.1(3) . . . .
C13 C14 C15 C16 -1.1(9) . . . .
C14 C13 C18 C17 2.3(8) . . . .
C14 C13 O7 C12 -168.1(4) . . . .
C14 C15 C16 C17 1.3(8) . . . .
C14 C15 C16 C20 -177.5(6) . . . .
C15 C16 C17 C18 0.2(8) . . . .
C15 C16 C20 C19 -10.6(8) . . . .
C15 C16 C20 O8 168.1(6) . . . .
C16 C17 C18 C13 -2.0(8) . . . .
C17 C16 C20 C19 170.5(5) . . . .
C17 C16 C20 O8 -10.8(8) . . . .
C18 C13 C14 C15 -0.8(8) . . . .
C18 C13 O7 C12 11.5(7) . . . .
C20 C16 C17 C18 179.1(5) . . . .
C21 C22 O11 C23 84.0(5) . . . .
C22 C21 O9 La1 -174.5(3) . . . 2_666
C22 C21 O9 La1 25.0(7) . . . .
C22 C21 O10 La1 174.3(3) . . . 2_666
C23 C24 C25 C26 0.2(7) . . . .
C23 C27 C28 C26 1.2(8) . . . .
C24 C23 C27 C28 -0.5(7) . . . .
C24 C23 O11 C22 -179.4(4) . . . .
C24 C25 C26 C28 0.5(7) . . . .
C24 C25 C26 C29 -179.5(4) . . . .
C25 C26 C28 C27 -1.2(7) . . . .
C25 C26 C29 C30 177.7(5) . . . .
C25 C26 C29 O12 -3.8(7) . . . .
C27 C23 C24 C25 -0.2(7) . . . .
C27 C23 O11 C22 -0.1(7) . . . .
C28 C26 C29 C30 -2.3(7) . . . .
C28 C26 C29 O12 176.2(5) . . . .
C29 C26 C28 C27 178.8(5) . . . .
C32 C2 C34 C35 -0.2(8) . . . .
C32 C31 N1 C35 -0.6(11) . . . .
C33 C1 C6 C5 -4.9(8) . . . .
C33 C1 C7 C8 -169.4(6) . . . .
C33 C1 C7 O1 12.6(7) . . . .
C33 C3 C4 C5 -4.6(7) . . . .
C33 C3 C4 O2 172.4(4) . . . .
C34 C2 C32 C31 0.4(9) . . . .
C34 C35 N1 C31 0.8(9) . . . .
La1 C10 O4 La1 -148.4(5) 2_566 . . .
La1 C21 O9 La1 -160.5(5) 2_666 . . .
N1 C31 C32 C2 0.0(12) . . . .
O2 C4 C5 C6 -174.5(5) . . . .
O2 C9 C10 O3 11.8(5) . . . .
O2 C9 C10 O4 -171.3(3) . . . .
O3 C10 O4 La1 -146.1(4) . . . .
O3 C10 O4 La1 2.3(4) . . . 2_566
O4 C10 O3 La1 -2.5(4) . . . 2_566
O5 C11 C12 O7 -177.1(4) . . . .
O5 C11 O6 La1 4.7(4) . . . .
O6 C11 C12 O7 0.9(6) . . . .
O6 C11 O5 La1 -4.7(4) . . . .
O7 C13 C14 C15 178.9(5) . . . .
O7 C13 C18 C17 -177.3(5) . . . .
O9 C21 C22 O11 146.2(4) . . . .
O9 C21 O10 La1 -4.8(4) . . . 2_666
O10 C21 C22 O11 -32.9(6) . . . .
O10 C21 O9 La1 4.6(4) . . . 2_666
O10 C21 O9 La1 -155.8(3) . . . .
O11 C23 C24 C25 179.2(4) . . . .
O11 C23 C27 C28 -179.8(4) . . . .
