#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:42:55 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263741 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/66/7706612.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_7706612
loop_
_publ_author_name
'Zhang, Jianfeng'
'Wenzel, Marco'
'Schnaars, Kathleen'
'Hennersdorf, Felix'
'Schwedtmann, Kai'
'März, Juliane'
'Rossberg, André'
'Kaden, Peter'
'Kraus, Florian'
'Stumpf, Thorsten'
'Weigand, Jan J.'
_publ_section_title
;
 Coordination of trivalent lanthanum and cerium, and tetravalent cerium
 and actinides (An = Th(IV), U(IV), Np(IV)) by a 4-phosphoryl
 1H-pyrazol-5-olate ligand in solution and the solid state.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3550
_journal_page_last               3558
_journal_paper_doi               10.1039/d1dt00365h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C68 H97 La N8 O16 P4, 0.75(C8 H12 N4), 3(H2 O)'
_chemical_formula_sum            'C74 H112 La N11 O19 P4'
_chemical_formula_weight         1722.53
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-06 deposited with the CCDC.	2021-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.80376(5)
_cell_length_b                   17.80376(5)
_cell_length_c                   13.75097(7)
_cell_measurement_reflns_used    31995
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      76.5650
_cell_measurement_theta_min      3.5020
_cell_volume                     4358.70(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -61.00  32.00   0.50    0.50    --  -38.50  57.00  60.00  186
  2  ω    -60.00 -33.00   0.50    0.50    --  -38.50  77.00-180.00   54
  3  ω    -15.00  26.00   0.50    0.50    --  -38.50  77.00-180.00   82
  4  ω     20.00  83.00   0.50    0.50    --   42.75  38.00-180.00  126
  5  ω     41.00  75.00   0.50    2.00    --  111.00 -45.00 -90.00   68
  6  ω     94.00 123.00   0.50    2.00    --  111.00 -45.00 -90.00   58
  7  ω    109.00 136.00   0.50    2.00    --  111.00 -77.00   0.00   54
  8  ω     96.00 121.00   0.50    2.00    --  111.00-125.00  30.00   50
  9  ω     78.00 105.00   0.50    2.00    --  111.00-125.00   0.00   54
 10  ω     64.00 101.00   0.50    2.00    --  111.00 -94.00  30.00   74
 11  ω     56.00  83.00   0.50    2.00    --  111.00-125.00  30.00   54
 12  ω     52.00  79.00   0.50    2.00    --  111.00-125.00  60.00   54
 13  ω     72.00 121.00   0.50    2.00    --  111.00-125.00 120.00   98
 14  ω     41.00 135.00   0.50    2.00    --  111.00 -45.00  30.00  188
 15  ω     61.00  88.00   0.50    2.00    --  111.00 -94.00-120.00   54
 16  ω     73.00 120.00   0.50    2.00    --  111.00-125.00-120.00   94
 17  ω     62.00  89.00   0.50    2.00    --  111.00 -61.00-150.00   54
 18  ω     53.00 115.00   0.50    2.00    --  111.00-125.00-180.00  124
 19  ω     53.00 121.00   0.50    2.00    --  111.00-125.00 -60.00  136
 20  ω     38.00  97.00   0.50    0.50    --   42.75-125.00-180.00  118
 21  ω     36.00  77.00   0.50    0.50    --   42.75-125.00 -90.00   82
 22  ω     37.00  84.00   0.50    2.00    --  111.00 -94.00-180.00   94
 23  ω     35.00 153.00   0.50    2.00    --  111.00 -15.00-120.00  236
 24  ω     39.00 107.00   0.50    2.00    --  111.00-125.00 -30.00  136
 25  ω     39.00  92.00   0.50    2.00    --  111.00 -94.00   0.00  106
 26  ω     31.00 154.00   0.50    2.00    --  111.00 -15.00   0.00  246
 27  ω     40.00 135.00   0.50    2.00    --  111.00 -45.00 150.00  190
 28  ω     30.00 109.00   0.50    2.00    --  111.00 -94.00  60.00  158
 29  ω     31.00 156.00   0.50    2.00    --  111.00 -15.00 120.00  250
 30  ω   -109.00 -12.00   0.50    0.50    --  -38.50 -57.00 -90.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0047782000
_diffrn_orient_matrix_UB_12      0.0270919000
_diffrn_orient_matrix_UB_13      0.1062664000
_diffrn_orient_matrix_UB_21      -0.0732933000
_diffrn_orient_matrix_UB_22      0.0423285000
_diffrn_orient_matrix_UB_23      -0.0235624000
_diffrn_orient_matrix_UB_31      -0.0459099000
_diffrn_orient_matrix_UB_32      -0.0702628000
_diffrn_orient_matrix_UB_33      0.0268405000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.693
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.058
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0326P)²+1.2051P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4556
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00365h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7706609--7706617.cif.'
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7706612
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C156 H192 La2 N22 O40 P8 '
_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.
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H5AA-N2
 2.1 with sigma of 0.02
 O5A-H5AB
 0.85 with sigma of 0.01
 H14A-O5B_$1
 -2 with sigma of 0.02
 H2-O5A
 1.96 with sigma of 0.01
 C18-H18C = C18-H18B = C18-H18A = N2-H2
 0.96 with sigma of 0.001
 H18C-H18B \\sim H18B-H18A \\sim H18C-H18A
 with sigma of 0.01
3. Same fragment restrains
{C23, C22, N5} sigma for 1-2: 0.02, 1-3: 0.02
{C21, C20, N4} sigma for 1-2: 0.02, 1-3: 0.02
as
{C18, C19, N3}
4. Others
 Fixed Sof: H18A(0.25) H18B(0.25) H18C(0.25) H2(0.25) N4(0.25) C20(0.25)
 C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25) C22(0.25) C23(0.25) H23A(0.25)
 H23B(0.25) H23C(0.25) N5(0.25) O5B(0.25) H5BA(0.25) H5BB(0.25) O5A(0.5)
 H5AA(0.5) H5AB(0.5)
5.a Free rotating group:
 O5B(H5BA,H5BB), O5A(H5AA,H5AB)
5.b Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C)
;
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.772
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -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
La1 La 0.750000 0.750000 0.62375(2) 0.01468(5) Uani 1 4 d S T P . .
P1 P 0.65372(2) 0.57742(2) 0.71935(2) 0.01885(7) Uani 1 1 d . . . . .
O1 O 0.74688(6) 0.63439(5) 0.52581(7) 0.0259(2) Uani 1 1 d . . . . .
O2 O 0.67129(5) 0.65897(5) 0.71923(6) 0.02121(18) Uani 1 1 d . . . . .
O3 O 0.69068(5) 0.53035(5) 0.80327(7) 0.02537(19) Uani 1 1 d . . . . .
O4 O 0.56740(5) 0.56230(5) 0.73852(7) 0.02258(18) Uani 1 1 d . . . . .
N1 N 0.73880(6) 0.51151(6) 0.47155(8) 0.0219(2) Uani 1 1 d . . . . .
N2 N 0.70860(6) 0.44337(6) 0.50168(9) 0.0255(2) Uani 1 1 d D . . . .
C1 C 0.72470(7) 0.56782(7) 0.53808(9) 0.0198(2) Uani 1 1 d . . . . .
C2 C 0.68347(7) 0.53284(7) 0.61379(9) 0.0206(2) Uani 1 1 d . . . . .
C3 C 0.67610(7) 0.45687(7) 0.58663(11) 0.0246(3) Uani 1 1 d . . . . .
C4 C 0.63825(9) 0.39570(8) 0.64179(13) 0.0357(3) Uani 1 1 d . . . . .
H4A H 0.585995 0.407602 0.649473 0.054 Uiso 1 1 calc GR . . . .
H4B H 0.661186 0.390754 0.704645 0.054 Uiso 1 1 calc GR . . . .
H4C H 0.643158 0.349289 0.606818 0.054 Uiso 1 1 calc GR . . . .
C5 C 0.77501(8) 0.51842(8) 0.38016(9) 0.0214(3) Uani 1 1 d . . . . .
C6 C 0.83504(8) 0.56827(8) 0.36964(10) 0.0256(3) Uani 1 1 d . . . . .
H6 H 0.850674 0.597618 0.421801 0.031 Uiso 1 1 calc R . . . .
C7 C 0.87110(8) 0.57347(8) 0.28035(10) 0.0286(3) Uani 1 1 d . . . . .
H7 H 0.910586 0.607209 0.273104 0.034 Uiso 1 1 calc R . . . .
C8 C 0.84969(8) 0.52957(8) 0.20157(10) 0.0300(3) Uani 1 1 d . . . . .
C9 C 0.78929(9) 0.48116(9) 0.21344(10) 0.0304(3) Uani 1 1 d . . . . .
H9 H 0.773774 0.451785 0.161250 0.037 Uiso 1 1 calc R . . . .
C10 C 0.75142(8) 0.47558(8) 0.30165(10) 0.0255(3) Uani 1 1 d . . . . .
H10 H 0.710591 0.443362 0.307922 0.031 Uiso 1 1 calc R . . . .
C11 C 0.89215(11) 0.53435(12) 0.10670(12) 0.0456(4) Uani 1 1 d . . . . .
H11A H 0.889648 0.584762 0.082144 0.068 Uiso 1 1 calc GR . . . .
H11B H 0.870101 0.500569 0.060376 0.068 Uiso 1 1 calc GR . . . .
H11C H 0.943681 0.520753 0.117282 0.068 Uiso 1 1 calc GR . . . .
C12 C 0.67677(9) 0.54941(9) 0.90563(11) 0.0326(3) Uani 1 1 d . . . . .
H12 H 0.628409 0.575299 0.911606 0.039 Uiso 1 1 calc R . . . .
C13 C 0.73899(10) 0.60031(11) 0.93976(13) 0.0460(4) Uani 1 1 d . . . . .
H13A H 0.786349 0.575096 0.932753 0.069 Uiso 1 1 calc GR . . . .
H13B H 0.731164 0.612906 1.006884 0.069 Uiso 1 1 calc GR . . . .
H13C H 0.739131 0.645365 0.901412 0.069 Uiso 1 1 calc GR . . . .
C14 C 0.67374(12) 0.47568(12) 0.95929(14) 0.0516(5) Uani 1 1 d . . . . .
H14A H 0.633197 0.445842 0.934253 0.077 Uiso 1 1 calc DGR . . . .
H14B H 0.665802 0.484895 1.027303 0.077 Uiso 1 1 calc GR . . . .
H14C H 0.720282 0.449314 0.950496 0.077 Uiso 1 1 calc GR . . . .
C15 C 0.50989(8) 0.61045(8) 0.69477(13) 0.0329(3) Uani 1 1 d . . . . .
H15 H 0.531459 0.659837 0.680263 0.039 Uiso 1 1 calc R . . . .
C16 C 0.48307(10) 0.57423(14) 0.60176(14) 0.0525(5) Uani 1 1 d . . . . .
H16A H 0.524882 0.567334 0.558586 0.079 Uiso 1 1 calc GR . . . .
H16B H 0.446369 0.605968 0.571308 0.079 Uiso 1 1 calc GR . . . .
H16C H 0.460917 0.526362 0.616245 0.079 Uiso 1 1 calc GR . . . .
C17 C 0.44853(9) 0.61876(11) 0.76944(14) 0.0453(4) Uani 1 1 d . . . . .
H17A H 0.427170 0.570406 0.783187 0.068 Uiso 1 1 calc GR . . . .
H17B H 0.410215 0.651536 0.744697 0.068 Uiso 1 1 calc GR . . . .
H17C H 0.469113 0.639647 0.828033 0.068 Uiso 1 1 calc GR . . . .
C18 C 0.750000 0.750000 0.3196(2) 0.0356(6) Uani 1 4 d DS T P . .
C19 C 0.750000 0.750000 0.2160(3) 0.0687(13) Uani 1 4 d DS T P . .
N3 N 0.750000 0.750000 0.1347(4) 0.178(4) Uani 1 4 d DS T P . .
H18A H 0.6984(14) 0.759(4) 0.336(8) 0.267 Uiso 0.25 1 d DR . . A -1
H18B H 0.782(3) 0.7898(19) 0.342(6) 0.267 Uiso 0.25 1 d DR . . B -1
H18C H 0.766(4) 0.7020(15) 0.343(6) 0.267 Uiso 0.25 1 d DR . . C -1
H2 H 0.722(6) 0.3945(19) 0.478(6) 0.267 Uiso 0.25 1 d DR . . D 2
N4 N 0.6678(6) 0.3079(5) 0.0565(8) 0.091(3) Uani 0.25 1 d D . . E -1
C20 C 0.7083(7) 0.2821(5) 0.1102(8) 0.062(3) Uani 0.25 1 d D . . E -1
C21 C 0.760(2) 0.247(4) 0.1745(9) 0.055(6) Uani 0.25 1 d D . . E -1
H21A H 0.764139 0.194778 0.158462 0.083 Uiso 0.25 1 calc GR . . E -1
H21B H 0.742395 0.252229 0.240141 0.083 Uiso 0.25 1 calc GR . . E -1
H21C H 0.808237 0.270614 0.168285 0.083 Uiso 0.25 1 calc GR . . E -1
C22 C 0.7665(6) 0.2892(5) 0.1006(7) 0.057(2) Uani 0.25 1 d D . . F -2
C23 C 0.731(3) 0.251(3) 0.179(2) 0.140(13) Uani 0.25 1 d D . . F -2
H23A H 0.697446 0.213588 0.154039 0.210 Uiso 0.25 1 calc GR . . F -2
H23B H 0.703257 0.286388 0.217728 0.210 Uiso 0.25 1 calc GR . . F -2
H23C H 0.768532 0.227297 0.218934 0.210 Uiso 0.25 1 calc GR . . F -2
N5 N 0.7906(5) 0.3299(4) 0.0451(7) 0.068(2) Uani 0.25 1 d D . . F -2
O5B O 0.8076(13) 0.1944(13) 0.4248(13) 0.034(3) Uani 0.25 1 d D . . G 2
H5BA H 0.802709 0.206688 0.365417 0.050 Uiso 0.25 1 d G . . G 2
H5BB H 0.848665 0.214703 0.442320 0.050 Uiso 0.25 1 d G . . G 2
O5A O 0.6888(7) 0.3004(6) 0.3999(6) 0.0306(13) Uani 0.5 1 d D . . H 1
H5AA H 0.690012 0.340696 0.433153 0.046 Uiso 0.5 1 d DG . . H 1
H5AB H 0.719441 0.271426 0.434663 0.046 Uiso 0.5 1 d DG . . H 1
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'
P P 0.2955 0.4335 '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
0 0 1 0.0771
0 0 -1 0.0771
1 -1 0 0.1283
-1 1 0 0.1283
1 1 0 0.0521
-1 -1 0 0.0521
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 O1 72.57(2) . 4_565 ?
O1 La1 O1 72.57(2) 4_565 2_665 ?
O1 La1 O1 113.63(4) . 2_665 ?
O1 La1 O1 72.57(2) . 3_655 ?
O1 La1 O1 113.63(4) 4_565 3_655 ?
O1 La1 O1 72.57(2) 3_655 2_665 ?
O1 La1 O2 74.57(3) 2_665 2_665 ?
O1 La1 O2 146.95(3) . 2_665 ?
O1 La1 O2 80.45(3) 4_565 . ?
O1 La1 O2 146.95(3) 4_565 3_655 ?
O1 La1 O2 146.95(3) 2_665 . ?
O1 La1 O2 80.45(3) . 3_655 ?
O1 La1 O2 74.57(3) . . ?
O1 La1 O2 80.45(3) 3_655 2_665 ?
O1 La1 O2 137.56(3) . 4_565 ?
O1 La1 O2 146.95(3) 3_655 4_565 ?
O1 La1 O2 137.56(3) 2_665 3_655 ?
O1 La1 O2 74.57(3) 3_655 3_655 ?
O1 La1 O2 137.56(3) 3_655 . ?
O1 La1 O2 80.45(3) 2_665 4_565 ?
O1 La1 O2 74.57(3) 4_565 4_565 ?
O1 La1 O2 137.56(3) 4_565 2_665 ?
O2 La1 O2 74.155(19) . 3_655 ?
O2 La1 O2 117.00(4) . 2_665 ?
O2 La1 O2 74.155(19) 2_665 4_565 ?
O2 La1 O2 74.155(19) 2_665 3_655 ?
O2 La1 O2 74.155(19) . 4_565 ?
O2 La1 O2 117.00(4) 3_655 4_565 ?
O2 P1 O3 115.73(5) . . ?
O2 P1 O4 111.78(5) . . ?
O2 P1 C2 112.43(6) . . ?
O3 P1 O4 101.17(5) . . ?
O3 P1 C2 104.03(6) . . ?
O4 P1 C2 110.95(6) . . ?
C1 O1 La1 136.08(8) . . ?
P1 O2 La1 138.46(5) . . ?
C12 O3 P1 120.67(9) . . ?
C15 O4 P1 120.73(8) . . ?
N2 N1 C5 121.05(11) . . ?
C1 N1 N2 111.46(10) . . ?
C1 N1 C5 127.39(11) . . ?
N1 N2 H2 126(5) . . ?
C3 N2 N1 105.86(10) . . ?
C3 N2 H2 125(5) . . ?
O1 C1 N1 122.49(11) . . ?
O1 C1 C2 132.33(12) . . ?
N1 C1 C2 105.18(10) . . ?
C1 C2 P1 124.80(10) . . ?
C3 C2 P1 129.17(10) . . ?
C3 C2 C1 105.97(11) . . ?
N2 C3 C2 111.52(11) . . ?
N2 C3 C4 120.93(12) . . ?
C2 C3 C4 127.55(13) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 119.66(12) . . ?
C10 C5 N1 120.31(12) . . ?
C10 C5 C6 120.04(12) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.19(13) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7 119.2 . . ?
C6 C7 C8 121.68(14) . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C11 120.31(15) . . ?
C9 C8 C7 118.06(13) . . ?
C9 C8 C11 121.63(15) . . ?
C8 C9 H9 119.3 . . ?
C8 C9 C10 121.49(13) . . ?
C10 C9 H9 119.3 . . ?
C5 C10 C9 119.51(13) . . ?
C5 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 H12 109.7 . . ?
O3 C12 C13 108.28(13) . . ?
O3 C12 C14 105.90(14) . . ?
C13 C12 H12 109.7 . . ?
C13 C12 C14 113.44(15) . . ?
C14 C12 H12 109.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C15 H15 109.6 . . ?
O4 C15 C16 108.60(13) . . ?
O4 C15 C17 106.52(13) . . ?
C16 C15 H15 109.6 . . ?
C17 C15 H15 109.6 . . ?
C17 C15 C16 112.96(13) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 H18A 103(7) . . ?
C19 C18 H18B 109(6) . . ?
C19 C18 H18C 110(5) . . ?
H18A C18 H18B 112(3) . . ?
H18A C18 H18C 112(3) . . ?
H18B C18 H18C 112(3) . . ?
N3 C19 C18 180.0 . . ?
N4 C20 C21 177(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C22 C23 169(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
H5BA O5B H5BB 104.6 . . ?
H5AA O5A H5AB 100.7 . . ?
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 O1 2.4603(9) . ?
La1 O1 2.4603(9) 3_655 ?
La1 O1 2.4603(9) 4_565 ?
La1 O1 2.4603(9) 2_665 ?
La1 O2 2.5127(9) . ?
La1 O2 2.5128(9) 4_565 ?
La1 O2 2.5128(9) 2_665 ?
La1 O2 2.5128(9) 3_655 ?
P1 O2 1.4853(9) . ?
P1 O3 1.5706(10) . ?
P1 O4 1.5824(9) . ?
P1 C2 1.7371(13) . ?
O1 C1 1.2608(15) . ?
O3 C12 1.4689(17) . ?
O4 C15 1.4648(16) . ?
N1 N2 1.3902(15) . ?
N1 C1 1.3802(16) . ?
N1 C5 1.4177(16) . ?
N2 C3 1.3256(19) . ?
N2 H2 0.9600(11) . ?
C1 C2 1.4179(17) . ?
C2 C3 1.4092(18) . ?
C3 C4 1.4884(19) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.397(2) . ?
C5 C10 1.3869(19) . ?
C6 H6 0.9300 . ?
C6 C7 1.3886(19) . ?
C7 H7 0.9300 . ?
C7 C8 1.389(2) . ?
C8 C9 1.388(2) . ?
C8 C11 1.510(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.391(2) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12 0.9800 . ?
C12 C13 1.506(2) . ?
C12 C14 1.507(2) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9800 . ?
C15 C16 1.510(3) . ?
C15 C17 1.507(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.425(5) . ?
C18 H18A 0.9600(11) . ?
C18 H18B 0.9600(11) . ?
C18 H18C 0.9600(10) . ?
C19 N3 1.117(6) . ?
N4 C20 1.131(11) . ?
C20 C21 1.419(14) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.425(14) . ?
C22 N5 1.137(11) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
O5B H5BA 0.8496 . ?
O5B H5BB 0.8498 . ?
O5A H5AA 0.8505 . ?
O5A H5AB 0.8901 . ?
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 C1 N1 -172.04(9) . . . . ?
La1 O1 C1 C2 8.0(2) . . . . ?
P1 O3 C12 C13 -93.94(13) . . . . ?
P1 O3 C12 C14 144.07(11) . . . . ?
P1 O4 C15 C16 95.33(13) . . . . ?
P1 O4 C15 C17 -142.72(11) . . . . ?
P1 C2 C3 N2 -177.57(11) . . . . ?
P1 C2 C3 C4 2.0(2) . . . . ?
O1 C1 C2 P1 -2.4(2) . . . . ?
O1 C1 C2 C3 -179.77(14) . . . . ?
O2 P1 O3 C12 57.98(11) . . . . ?
O2 P1 O4 C15 39.60(12) . . . . ?
O2 P1 C2 C1 4.27(14) . . . . ?
O2 P1 C2 C3 -179.04(12) . . . . ?
O3 P1 O2 La1 106.48(8) . . . . ?
O3 P1 O4 C15 163.35(11) . . . . ?
O3 P1 C2 C1 -121.70(11) . . . . ?
O3 P1 C2 C3 55.00(14) . . . . ?
O4 P1 O2 La1 -138.43(7) . . . . ?
O4 P1 O3 C12 -63.02(11) . . . . ?
O4 P1 C2 C1 130.28(11) . . . . ?
O4 P1 C2 C3 -53.03(14) . . . . ?
N1 N2 C3 C2 0.39(15) . . . . ?
N1 N2 C3 C4 -179.20(13) . . . . ?
N1 C1 C2 P1 177.56(10) . . . . ?
N1 C1 C2 C3 0.22(14) . . . . ?
N1 C5 C6 C7 178.69(12) . . . . ?
N1 C5 C10 C9 -177.75(12) . . . . ?
N2 N1 C1 O1 180.00(12) . . . . ?
N2 N1 C1 C2 0.01(14) . . . . ?
N2 N1 C5 C6 -147.25(13) . . . . ?
N2 N1 C5 C10 32.28(18) . . . . ?
C1 N1 N2 C3 -0.25(15) . . . . ?
C1 N1 C5 C6 36.62(19) . . . . ?
C1 N1 C5 C10 -143.85(13) . . . . ?
C1 C2 C3 N2 -0.39(16) . . . . ?
C1 C2 C3 C4 179.17(14) . . . . ?
C2 P1 O2 La1 -12.87(10) . . . . ?
C2 P1 O3 C12 -178.17(10) . . . . ?
C2 P1 O4 C15 -86.76(12) . . . . ?
C5 N1 N2 C3 -176.95(12) . . . . ?
C5 N1 C1 O1 -3.6(2) . . . . ?
C5 N1 C1 C2 176.45(12) . . . . ?
C5 C6 C7 C8 -0.9(2) . . . . ?
C6 C5 C10 C9 1.8(2) . . . . ?
C6 C7 C8 C9 1.7(2) . . . . ?
C6 C7 C8 C11 -177.48(14) . . . . ?
C7 C8 C9 C10 -0.8(2) . . . . ?
C8 C9 C10 C5 -1.0(2) . . . . ?
C10 C5 C6 C7 -0.8(2) . . . . ?
C11 C8 C9 C10 178.43(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
0.0023 0.0001 0.9998 0.1062 -0.0237 0.0267
-0.0023 -0.0001 -0.9998 -0.1062 0.0237 -0.0267
0.9962 -1.0019 -0.0004 -0.0319 -0.1154 0.0246
-0.9962 1.0019 0.0004 0.0319 0.1154 -0.0246
1.0014 0.9994 -0.0004 0.0222 -0.0311 -0.1162
-1.0014 -0.9994 0.0004 -0.0222 0.0311 0.1162
