#------------------------------------------------------------------------------
#$Date: 2020-10-06 14:24:54 +0300 (Tue, 06 Oct 2020) $
#$Revision: 258025 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/07/7240797.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_7240797
loop_
_publ_author_name
'Olyshevets, Iryna'
'Ovchynnikov, Vladimir'
'Kariaka, Nataliia'
'Dyakonenko, Viktoriya'
'Shishkina, Svitlana'
'Sliva, Tatiana'
'Ostrowska, Małgorzata'
'Jedyńczuk, Aleksandra'
'Gumienna-Kontecka, Elżbieta'
'Amirkhanov, Vladimir'
_publ_section_title
;
 Lanthanide complexes based on a new bis-chelating carbacylamidophosphate
 (CAPh) scorpionate-like ligand
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              24808
_journal_page_last               24816
_journal_paper_doi               10.1039/D0RA04714G
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C22 H36 N11 O19 P4 Tb, C3 H8 O'
_chemical_formula_sum            'C25 H44 N11 O20 P4 Tb'
_chemical_formula_weight         1101.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-16 deposited with the CCDC.	2020-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.506(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.134(2)
_cell_length_b                   17.152(2)
_cell_length_c                   19.453(3)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    110
_cell_measurement_theta_max      18.6650
_cell_measurement_theta_min      3.2450
_cell_volume                     4179.3(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    9.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   57.0000  150.0000 85

#__ type_ start__ end____ width___ exp.time_
  2 omega   -9.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -99.0000 -120.0000 78

#__ type_ start__ end____ width___ exp.time_
  3 omega   26.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -99.0000   30.0000 43

#__ type_ start__ end____ width___ exp.time_
  4 omega  -38.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000  -90.0000 49

#__ type_ start__ end____ width___ exp.time_
  5 omega   12.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega  -14.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645 -178.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
  8 omega   27.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -77.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
  9 omega   -4.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   19.0000   90.0000 103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0192364000
_diffrn_orient_matrix_UB_12      0.0071071000
_diffrn_orient_matrix_UB_13      -0.0375927000
_diffrn_orient_matrix_UB_21      -0.0442989000
_diffrn_orient_matrix_UB_22      -0.0246795000
_diffrn_orient_matrix_UB_23      -0.0024423000
_diffrn_orient_matrix_UB_31      -0.0294480000
_diffrn_orient_matrix_UB_32      0.0324787000
_diffrn_orient_matrix_UB_33      0.0063158000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1810
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.858
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0790
_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)+(0.0753P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.2067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4081
_reflns_number_total             7352
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ra04714g2.cif
_cod_data_source_block           kiev301_lt
_cod_depositor_comments
'Adding full bibliography for 7240795--7240798.cif.'
_cod_original_cell_volume        4179.6(12)
_cod_database_code               7240797
_shelx_shelxl_version_number     2018/1
_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   0.698
_shelx_estimated_absorpt_t_min   0.445
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -1(10)
 2(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 O10-C13B
 1.45 with sigma of 0.002
 O10-C13A
 1.45 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C13B) = Uanis(C13A)
Uanis(C25) = Uanis(C24)
5. Others
 Fixed Sof: C13A(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C13B(0.5) H13D(0.5)
 H13E(0.5) H13F(0.5)
6.a Ternary CH refined with riding coordinates:
 C23(H23)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N5(H5), N7(H7), N9(H9), N10(H10), C5(H5A), C6(H6), C7(H7A),
 C16(H16), C17(H17), C18(H18)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
6.d Idealised tetrahedral OH refined as rotating group:
 O20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Tb1 Tb 0.39196(5) 0.20773(3) 0.65651(3) 0.0336(2) Uani 1 1 d . . . . .
P1 P 0.4673(3) 0.36753(16) 0.76906(17) 0.0319(7) Uani 1 1 d . . . . .
P2 P 0.5030(3) 0.04011(16) 0.76432(17) 0.0334(7) Uani 1 1 d . . . . .
P3 P 0.5452(3) 0.1472(2) 0.5476(2) 0.0574(11) Uani 1 1 d . . . . .
P4 P 0.2078(3) 0.34581(17) 0.53981(19) 0.0379(8) Uani 1 1 d . . . . .
O1 O 0.4623(7) 0.3624(4) 0.8502(4) 0.039(2) Uani 1 1 d . . . . .
O2 O 0.4412(6) 0.4556(4) 0.7467(4) 0.0324(18) Uani 1 1 d . . . . .
O3 O 0.3816(7) 0.3137(4) 0.7271(4) 0.039(2) Uani 1 1 d . . . . .
O4 O 0.5667(6) 0.2273(4) 0.7349(4) 0.0311(18) Uani 1 1 d . . . . .
O5 O 0.6659(6) -0.0723(4) 0.7393(4) 0.0352(19) Uani 1 1 d . . . . .
O6 O 0.4530(7) -0.0414(4) 0.7384(4) 0.039(2) Uani 1 1 d . . . . .
O7 O 0.5452(7) 0.0290(4) 0.8464(4) 0.040(2) Uani 1 1 d . . . . .
O8 O 0.4282(7) 0.1052(4) 0.7393(4) 0.035(2) Uani 1 1 d . . . . .
O9 O 0.4889(8) 0.1292(6) 0.4660(5) 0.069(3) Uani 1 1 d . . . . .
O10 O 0.6370(8) 0.0854(6) 0.5681(6) 0.084(4) Uani 1 1 d D . . . .
O11 O 0.4732(7) 0.1312(4) 0.5913(4) 0.040(2) Uani 1 1 d . . . . .
O12 O 0.4757(7) 0.2964(4) 0.5961(4) 0.0349(19) Uani 1 1 d . . . . .
O13 O 0.1822(7) 0.5212(4) 0.5319(5) 0.045(2) Uani 1 1 d . . . . .
O14 O 0.2586(7) 0.2710(4) 0.5672(4) 0.042(2) Uani 1 1 d . . . . .
O15 O 0.1060(8) 0.3639(5) 0.5605(5) 0.056(3) Uani 1 1 d . . . . .
O16 O 0.1681(8) 0.3495(5) 0.4545(4) 0.052(2) Uani 1 1 d . . . . .
O17 O 0.2178(7) 0.1754(4) 0.6775(4) 0.040(2) Uani 1 1 d . . . . .
O18 O 0.0975(8) 0.0999(5) 0.6073(6) 0.064(3) Uani 1 1 d . . . . .
O19 O 0.2593(7) 0.1077(4) 0.5959(5) 0.042(2) Uani 1 1 d . . . . .
N1 N 0.5867(7) 0.3573(4) 0.7663(5) 0.024(2) Uani 1 1 d . . . . .
N2 N 0.7244(7) 0.2883(5) 0.7492(5) 0.033(2) Uani 1 1 d . . . . .
H2 H 0.757567 0.333134 0.761301 0.039 Uiso 1 1 calc R . . . .
N3 N 0.7522(8) 0.1564(5) 0.7324(5) 0.027(2) Uani 1 1 d . . . . .
N4 N 0.7753(8) 0.0215(5) 0.7238(5) 0.034(2) Uani 1 1 d . . . . .
H4 H 0.817921 -0.015608 0.717679 0.041 Uiso 1 1 calc R . . . .
N5 N 0.6115(8) 0.0529(4) 0.7404(5) 0.032(2) Uani 1 1 d . . . . .
H5 H 0.626083 0.101054 0.730964 0.038 Uiso 1 1 calc R . . . .
N6 N 0.6005(9) 0.2323(6) 0.5543(6) 0.046(3) Uani 1 1 d . . . . .
N7 N 0.6237(8) 0.3600(7) 0.5823(6) 0.050(3) Uani 1 1 d . . . . .
H7 H 0.689196 0.351978 0.580893 0.060 Uiso 1 1 calc R . . . .
N8 N 0.4918(8) 0.4543(5) 0.5839(5) 0.035(2) Uani 1 1 d . . . . .
N9 N 0.3580(9) 0.5444(5) 0.5740(5) 0.041(3) Uani 1 1 d . . . . .
H9 H 0.342436 0.593129 0.580855 0.049 Uiso 1 1 calc R . . . .
N10 N 0.2947(7) 0.4163(5) 0.5632(5) 0.033(2) Uani 1 1 d . . . . .
H10 H 0.361785 0.403318 0.583929 0.039 Uiso 1 1 calc R . . . .
N11 N 0.1892(9) 0.1276(6) 0.6269(7) 0.049(3) Uani 1 1 d . . . . .
C1 C 0.5308(11) 0.4112(6) 0.9041(7) 0.046(3) Uani 1 1 d . . . . .
H1A H 0.508190 0.465611 0.894805 0.069 Uiso 1 1 calc GR . . . .
H1B H 0.604436 0.405695 0.902692 0.069 Uiso 1 1 calc GR . . . .
H1C H 0.526842 0.395655 0.951686 0.069 Uiso 1 1 calc GR . . . .
C2 C 0.3365(9) 0.4868(7) 0.7453(7) 0.040(3) Uani 1 1 d . . . . .
H2A H 0.280885 0.463007 0.705487 0.061 Uiso 1 1 calc GR . . . .
H2B H 0.335893 0.543466 0.738575 0.061 Uiso 1 1 calc GR . . . .
H2C H 0.322843 0.474828 0.791010 0.061 Uiso 1 1 calc GR . . . .
C3 C 0.6204(9) 0.2889(6) 0.7492(5) 0.024(2) Uani 1 1 d . . . . .
C4 C 0.7880(10) 0.2296(6) 0.7336(6) 0.034(3) Uani 1 1 d . . . . .
C5 C 0.8822(9) 0.2487(6) 0.7204(6) 0.033(3) Uani 1 1 d . . . . .
H5A H 0.903829 0.301410 0.719693 0.040 Uiso 1 1 calc R . . . .
C6 C 0.9441(11) 0.1880(7) 0.7084(7) 0.043(3) Uani 1 1 d . . . . .
H6 H 1.010397 0.198713 0.700054 0.052 Uiso 1 1 calc R . . . .
C7 C 0.9093(10) 0.1116(6) 0.7084(6) 0.037(3) Uani 1 1 d . . . . .
H7A H 0.949769 0.069079 0.699199 0.044 Uiso 1 1 calc R . . . .
C8 C 0.8141(9) 0.1001(6) 0.7224(6) 0.029(3) Uani 1 1 d . . . . .
C9 C 0.6817(10) -0.0033(6) 0.7334(7) 0.036(3) Uani 1 1 d . . . . .
C10 C 0.4086(12) -0.0558(8) 0.6612(7) 0.057(4) Uani 1 1 d . . . . .
H10A H 0.439093 -0.018519 0.634631 0.085 Uiso 1 1 calc GR . . . .
H10B H 0.330900 -0.049403 0.646903 0.085 Uiso 1 1 calc GR . . . .
H10C H 0.426066 -0.108977 0.650312 0.085 Uiso 1 1 calc GR . . . .
C11 C 0.4719(11) 0.0338(7) 0.8907(7) 0.046(3) Uani 1 1 d . . . . .
H11A H 0.421204 -0.009639 0.878673 0.069 Uiso 1 1 calc GR . . . .
H11B H 0.432826 0.083275 0.881068 0.069 Uiso 1 1 calc GR . . . .
H11C H 0.513026 0.031059 0.941866 0.069 Uiso 1 1 calc GR . . . .
C12 C 0.3950(14) 0.1699(9) 0.4314(9) 0.080(5) Uani 1 1 d . . . . .
H12A H 0.380004 0.165426 0.379041 0.119 Uiso 1 1 calc GR . . . .
H12B H 0.403850 0.224972 0.445328 0.119 Uiso 1 1 calc GR . . . .
H12C H 0.335520 0.147772 0.445537 0.119 Uiso 1 1 calc GR . . . .
C13A C 0.633(3) 0.0102(9) 0.5335(15) 0.088(9) Uani 0.5 1 d D . P A 1
H13A H 0.595945 -0.027236 0.555593 0.133 Uiso 0.5 1 calc GR . P A 1
H13B H 0.705858 -0.008134 0.539511 0.133 Uiso 0.5 1 calc GR . P A 1
H13C H 0.594628 0.015150 0.482043 0.133 Uiso 0.5 1 calc GR . P A 1
C13B C 0.716(2) 0.0638(18) 0.5330(16) 0.088(9) Uani 0.5 1 d D . P A 2
H13D H 0.679694 0.041418 0.485537 0.133 Uiso 0.5 1 calc GR . P A 2
H13E H 0.764792 0.025204 0.562493 0.133 Uiso 0.5 1 calc GR . P A 2
H13F H 0.755994 0.110145 0.527144 0.133 Uiso 0.5 1 calc GR . P A 2
C14 C 0.5584(10) 0.2927(7) 0.5764(6) 0.040(3) Uani 1 1 d . . . . .
C15 C 0.5957(10) 0.4373(7) 0.5899(7) 0.041(3) Uani 1 1 d . . . . .
C16 C 0.6726(12) 0.4948(9) 0.5982(7) 0.054(4) Uani 1 1 d . . . . .
H16 H 0.743406 0.481936 0.599361 0.065 Uiso 1 1 calc R . . . .
C17 C 0.6442(13) 0.5703(9) 0.6046(7) 0.060(4) Uani 1 1 d . . . . .
H17 H 0.696853 0.610063 0.613551 0.072 Uiso 1 1 calc R . . . .
C18 C 0.5399(13) 0.5894(7) 0.5983(7) 0.052(4) Uani 1 1 d . . . . .
H18 H 0.519176 0.641780 0.602469 0.062 Uiso 1 1 calc R . . . .
C19 C 0.4663(11) 0.5288(7) 0.5857(7) 0.040(3) Uani 1 1 d . . . . .
C20 C 0.2718(10) 0.4940(6) 0.5533(7) 0.038(3) Uani 1 1 d . . . . .
C21 C 0.0888(13) 0.3346(7) 0.6240(8) 0.058(4) Uani 1 1 d . . . . .
H21A H 0.091146 0.277547 0.623512 0.086 Uiso 1 1 calc GR . . . .
H21B H 0.018718 0.351791 0.626330 0.086 Uiso 1 1 calc GR . . . .
H21C H 0.144501 0.354284 0.666120 0.086 Uiso 1 1 calc GR . . . .
C22 C 0.1070(11) 0.2882(6) 0.4138(6) 0.045(3) Uani 1 1 d . . . . .
H22A H 0.082075 0.303211 0.362807 0.068 Uiso 1 1 calc GR . . . .
H22B H 0.045477 0.277653 0.430902 0.068 Uiso 1 1 calc GR . . . .
H22C H 0.151237 0.241222 0.419243 0.068 Uiso 1 1 calc GR . . . .
O20 O 0.6741(11) 0.2890(6) 0.4414(7) 0.089(4) Uani 1 1 d . . . . .
H20 H 0.651926 0.262985 0.470543 0.133 Uiso 1 1 calc GR . . . .
C23 C 0.7523(13) 0.2469(9) 0.4228(8) 0.063(4) Uani 1 1 d . . . . .
H23 H 0.733399 0.190280 0.417148 0.075 Uiso 1 1 calc R . . . .
C24 C 0.7596(17) 0.2804(11) 0.3532(9) 0.100(5) Uani 1 1 d . . . . .
H24A H 0.687550 0.289978 0.320807 0.151 Uiso 1 1 calc GR . . . .
H24B H 0.796582 0.243438 0.330516 0.151 Uiso 1 1 calc GR . . . .
H24C H 0.799345 0.329534 0.362727 0.151 Uiso 1 1 calc GR . . . .
C25 C 0.8463(17) 0.2594(12) 0.4845(10) 0.100(5) Uani 1 1 d . . . . .
H25A H 0.826241 0.288894 0.521533 0.151 Uiso 1 1 calc GR . . . .
H25B H 0.899810 0.288745 0.469217 0.151 Uiso 1 1 calc GR . . . .
H25C H 0.876240 0.208899 0.504189 0.151 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
_geom_angle_publ_flag
O3 Tb1 O4 74.0(3) . . ?
O3 Tb1 O8 102.7(3) . . ?
O3 Tb1 O12 84.8(3) . . ?
O3 Tb1 O14 84.9(3) . . ?
O3 Tb1 O17 81.8(3) . . ?
O3 Tb1 O19 132.1(3) . . ?
O3 Tb1 N11 106.1(3) . . ?
O4 Tb1 O12 74.0(3) . . ?
O4 Tb1 O17 133.1(3) . . ?
O4 Tb1 O19 144.3(2) . . ?
O4 Tb1 N11 148.3(3) . . ?
O8 Tb1 O4 72.9(3) . . ?
O8 Tb1 O12 142.4(3) . . ?
O8 Tb1 O17 74.2(3) . . ?
O8 Tb1 O19 77.0(3) . . ?
O8 Tb1 N11 76.4(3) . . ?
O11 Tb1 O3 154.0(3) . . ?
O11 Tb1 O4 85.1(3) . . ?
O11 Tb1 O8 85.3(3) . . ?
O11 Tb1 O12 74.5(3) . . ?
O11 Tb1 O14 103.0(3) . . ?
O11 Tb1 O17 124.2(3) . . ?
O11 Tb1 O19 73.7(3) . . ?
O11 Tb1 N11 99.8(3) . . ?
O12 Tb1 O17 143.3(3) . . ?
O12 Tb1 O19 124.8(3) . . ?
O12 Tb1 N11 137.5(3) . . ?
O14 Tb1 O4 141.2(3) . . ?
O14 Tb1 O8 144.7(3) . . ?
O14 Tb1 O12 72.0(3) . . ?
O14 Tb1 O17 72.9(3) . . ?
O14 Tb1 O19 72.8(3) . . ?
O14 Tb1 N11 68.5(3) . . ?
O17 Tb1 N11 25.5(3) . . ?
O19 Tb1 O17 51.5(3) . . ?
O19 Tb1 N11 26.3(3) . . ?
O2 P1 O1 104.7(4) . . ?
O2 P1 N1 103.3(4) . . ?
O3 P1 O1 104.9(4) . . ?
O3 P1 O2 112.0(5) . . ?
O3 P1 N1 120.0(4) . . ?
N1 P1 O1 111.1(5) . . ?
O6 P2 N5 110.1(4) . . ?
O7 P2 O6 102.1(4) . . ?
O7 P2 N5 103.8(5) . . ?
O8 P2 O6 113.5(5) . . ?
O8 P2 O7 115.8(4) . . ?
O8 P2 N5 110.8(4) . . ?
O9 P3 N6 108.8(6) . . ?
O10 P3 O9 102.5(6) . . ?
O10 P3 N6 107.3(6) . . ?
O11 P3 O9 111.0(6) . . ?
O11 P3 O10 107.8(6) . . ?
O11 P3 N6 118.1(5) . . ?
O14 P4 O15 114.6(5) . . ?
O14 P4 O16 112.7(5) . . ?
O14 P4 N10 110.0(5) . . ?
O15 P4 O16 103.2(6) . . ?
O15 P4 N10 111.6(5) . . ?
O16 P4 N10 104.2(5) . . ?
C1 O1 P1 119.1(7) . . ?
C2 O2 P1 118.5(7) . . ?
P1 O3 Tb1 130.0(5) . . ?
C3 O4 Tb1 129.3(7) . . ?
C10 O6 P2 118.8(7) . . ?
C11 O7 P2 120.4(8) . . ?
P2 O8 Tb1 141.0(4) . . ?
C12 O9 P3 117.9(9) . . ?
C13A O10 P3 124.6(15) . . ?
C13B O10 P3 131.1(14) . . ?
P3 O11 Tb1 134.1(4) . . ?
C14 O12 Tb1 133.4(7) . . ?
P4 O14 Tb1 146.5(5) . . ?
C21 O15 P4 122.5(9) . . ?
C22 O16 P4 120.8(7) . . ?
N11 O17 Tb1 95.1(7) . . ?
N11 O19 Tb1 95.4(6) . . ?
C3 N1 P1 120.7(7) . . ?
C3 N2 H2 114.1 . . ?
C3 N2 C4 131.9(9) . . ?
C4 N2 H2 114.1 . . ?
C8 N3 C4 117.5(10) . . ?
C8 N4 H4 115.4 . . ?
C9 N4 H4 115.4 . . ?
C9 N4 C8 129.2(9) . . ?
P2 N5 H5 116.5 . . ?
C9 N5 P2 127.1(7) . . ?
C9 N5 H5 116.5 . . ?
C14 N6 P3 121.2(10) . . ?
C14 N7 H7 116.3 . . ?
C15 N7 H7 116.3 . . ?
C15 N7 C14 127.4(11) . . ?
C19 N8 C15 117.3(10) . . ?
C19 N9 H9 115.5 . . ?
C20 N9 H9 115.5 . . ?
C20 N9 C19 129.1(10) . . ?
P4 N10 H10 117.4 . . ?
C20 N10 P4 125.2(9) . . ?
C20 N10 H10 117.4 . . ?
O17 N11 Tb1 59.4(6) . . ?
O17 N11 O19 117.0(10) . . ?
O18 N11 Tb1 172.0(9) . . ?
O18 N11 O17 121.8(12) . . ?
O18 N11 O19 121.2(12) . . ?
O19 N11 Tb1 58.3(5) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O4 C3 N1 126.2(10) . . ?
O4 C3 N2 119.3(9) . . ?
N1 C3 N2 114.5(9) . . ?
N3 C4 N2 116.7(10) . . ?
N3 C4 C5 123.4(10) . . ?
C5 C4 N2 119.9(9) . . ?
C4 C5 H5A 121.3 . . ?
C4 C5 C6 117.5(10) . . ?
C6 C5 H5A 121.3 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0(12) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7A 121.4 . . ?
C8 C7 C6 117.1(11) . . ?
C8 C7 H7A 121.4 . . ?
N3 C8 N4 116.4(10) . . ?
N3 C8 C7 124.4(10) . . ?
C7 C8 N4 119.2(9) . . ?
O5 C9 N4 120.2(10) . . ?
O5 C9 N5 122.6(11) . . ?
N4 C9 N5 117.1(9) . . ?
O6 C10 H10A 109.5 . . ?
O6 C10 H10B 109.5 . . ?
O6 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C11 H11A 109.5 . . ?
O7 C11 H11B 109.5 . . ?
O7 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O9 C12 H12A 109.5 . . ?
O9 C12 H12B 109.5 . . ?
O9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O10 C13A H13A 109.5 . . ?
O10 C13A H13B 109.5 . . ?
O10 C13A H13C 109.5 . . ?
H13A C13A H13B 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
O10 C13B H13D 109.5 . . ?
O10 C13B H13E 109.5 . . ?
O10 C13B H13F 109.5 . . ?
H13D C13B H13E 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
O12 C14 N6 129.1(12) . . ?
O12 C14 N7 119.4(11) . . ?
N6 C14 N7 111.4(11) . . ?
N8 C15 N7 118.8(10) . . ?
N8 C15 C16 122.1(12) . . ?
C16 C15 N7 118.9(12) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 C15 118.5(14) . . ?
C17 C16 H16 120.8 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.6(13) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 121.4 . . ?
C17 C18 C19 117.3(13) . . ?
C19 C18 H18 121.4 . . ?
N8 C19 N9 115.8(10) . . ?
N8 C19 C18 123.9(13) . . ?
C18 C19 N9 120.3(11) . . ?
O13 C20 N9 118.8(10) . . ?
O13 C20 N10 124.9(11) . . ?
N10 C20 N9 116.2(11) . . ?
O15 C21 H21A 109.5 . . ?
O15 C21 H21B 109.5 . . ?
O15 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O16 C22 H22A 109.5 . . ?
O16 C22 H22B 109.5 . . ?
O16 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 O20 H20 109.5 . . ?
O20 C23 H23 110.8 . . ?
O20 C23 C24 106.8(13) . . ?
O20 C23 C25 102.6(13) . . ?
C24 C23 H23 110.8 . . ?
C25 C23 H23 110.8 . . ?
C25 C23 C24 114.8(16) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
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
Tb1 O3 2.307(7) . ?
Tb1 O4 2.366(8) . ?
Tb1 O8 2.335(7) . ?
Tb1 O11 2.298(6) . ?
Tb1 O12 2.384(7) . ?
Tb1 O14 2.331(8) . ?
Tb1 O17 2.504(8) . ?
Tb1 O19 2.476(8) . ?
Tb1 N11 2.897(10) . ?
P1 O1 1.602(8) . ?
P1 O2 1.582(7) . ?
P1 O3 1.494(9) . ?
P1 N1 1.595(9) . ?
P2 O6 1.562(8) . ?
P2 O7 1.537(8) . ?
P2 O8 1.470(8) . ?
P2 N5 1.642(9) . ?
P3 O9 1.567(10) . ?
P3 O10 1.565(10) . ?
P3 O11 1.475(8) . ?
P3 N6 1.618(11) . ?
P4 O14 1.470(8) . ?
P4 O15 1.540(9) . ?
P4 O16 1.584(8) . ?
P4 N10 1.632(9) . ?
O1 C1 1.428(14) . ?
O2 C2 1.469(13) . ?
O4 C3 1.254(12) . ?
O5 C9 1.213(11) . ?
O6 C10 1.459(14) . ?
O7 C11 1.475(12) . ?
O9 C12 1.400(17) . ?
O10 C13A 1.449(2) . ?
O10 C13B 1.449(2) . ?
O12 C14 1.256(13) . ?
O13 C20 1.217(14) . ?
O15 C21 1.412(14) . ?
O16 C22 1.412(13) . ?
O17 N11 1.250(13) . ?
O18 N11 1.243(13) . ?
O19 N11 1.289(13) . ?
N1 C3 1.332(12) . ?
N2 H2 0.8800 . ?
N2 C3 1.366(13) . ?
N2 C4 1.398(13) . ?
N3 C4 1.339(13) . ?
N3 C8 1.315(12) . ?
N4 H4 0.8800 . ?
N4 C8 1.444(12) . ?
N4 C9 1.366(14) . ?
N5 H5 0.8800 . ?
N5 C9 1.367(13) . ?
N6 C14 1.307(14) . ?
N7 H7 0.8800 . ?
N7 C14 1.422(16) . ?
N7 C15 1.395(15) . ?
N8 C15 1.365(15) . ?
N8 C19 1.324(14) . ?
N9 H9 0.8800 . ?
N9 C19 1.397(15) . ?
N9 C20 1.386(15) . ?
N10 H10 0.8800 . ?
N10 C20 1.366(13) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 C5 1.375(15) . ?
C5 H5A 0.9500 . ?
C5 C6 1.383(15) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(14) . ?
C7 H7A 0.9500 . ?
C7 C8 1.371(15) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C15 C16 1.386(17) . ?
C16 H16 0.9500 . ?
C16 C17 1.363(19) . ?
C17 H17 0.9500 . ?
C17 C18 1.38(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.390(17) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
O20 H20 0.8400 . ?
O20 C23 1.390(15) . ?
C23 H23 1.0000 . ?
C23 C24 1.500(19) . ?
C23 C25 1.46(2) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O5 0.88 1.91 2.765(11) 163.6 2_656 yes
N5 H5 N3 0.88 1.90 2.601(12) 135.1 . yes
N9 H9 O20 0.88 2.06 2.891(13) 155.9 3_666 yes
N10 H10 N8 0.88 1.92 2.581(13) 130.7 . yes
C13A H13A O9 0.98 2.05 2.88(3) 141.4 3_656 yes
O20 H20 N6 0.84 2.01 2.826(13) 162.7 . yes
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 -1(10)
2 2(10)
