#------------------------------------------------------------------------------
#$Date: 2022-10-01 01:56:53 +0300 (Sat, 01 Oct 2022) $
#$Revision: 278293 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/13/7711387.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_7711387
loop_
_publ_author_name
'Storm Thomsen, Maria'
'Parsons, Simon'
'Sørensen, Thomas Just'
_publ_section_title
;
 Invisible strings. The first single crystal of the cTSAP form of
 [Eu(DOTA)(H2O)]− has an electronic structure similar to one of the
 reported cSAP forms
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02633C
_journal_year                    2022
_chemical_formula_moiety
'C16 H34 Eu0.963 N4 O13 Y, 2.523(Cl), H4 O2, 2(H3.401 O2)'
_chemical_formula_sum            'C16 H44.8 Cl2.52 Eu0.96 N4 O19 Y'
_chemical_formula_weight         921.95
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-11 deposited with the CCDC.	2022-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8351(6)
_cell_length_b                   8.8351(6)
_cell_length_c                   41.578(4)
_cell_measurement_reflns_used    9577
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.13
_cell_measurement_theta_min      2.36
_cell_volume                     3245.5(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            80579
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.987
_diffrn_reflns_theta_min         1.959
_exptl_absorpt_coefficient_mu    3.912
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1361 before and 0.1083 after correction.
The Ratio of minimum to maximum transmission is 0.7068.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       plate
_exptl_crystal_F_000             1853
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.726
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.022(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0237
_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)+(0.0292P)²+4.1084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.654
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2486
_reflns_number_total             2613
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02633c4.cif
_cod_data_source_block           d8v4600_4mmm_e
_cod_original_cell_volume        3245.5(6)
_cod_original_formula_sum        'C16 H44.80 Cl2.52 Eu0.96 N4 O19 Y'
_cod_database_code               7711387
_shelx_shelxl_version_number     2018/3
_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   0.878
_shelx_estimated_absorpt_t_min   0.333
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.978(13)
 0.022(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H10A(0.25) H10B(0.25)
4.a Free rotating group:
 O1(H1A,H1B), O12(H12A,H12B)
4.b Rotating group:
 O10(H10A,H10B), O27(H27A,H27B)
4.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C28(H28A,H28B), C27(H27C,H27D)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+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
Eu1 Eu 1.000000 1.000000 0.61902(2) 0.00423(8) Uani 0.963(2) 4 d S T . . .
Y1 Y 0.500000 0.500000 0.57165(2) 0.00525(13) Uani 1 4 d S T P . .
Cl2 Cl 1.000000 1.000000 0.80368(3) 0.0161(3) Uani 1 4 d S T P . .
O1 O 0.000000 0.500000 0.56398(8) 0.0219(6) Uani 1 2 d GS T P . .
H1A H 0.002365 0.587781 0.573535 0.033 Uiso 0.5 1 d G U P . .
H1B H -0.075054 0.452714 0.573106 0.033 Uiso 0.5 1 d G U P . .
O10 O 1.000000 1.000000 0.56072(9) 0.0164(8) Uani 1 4 d S T P . .
H10A H 1.060088 1.075952 0.552442 0.025 Uiso 0.25 1 d R U P . .
H10B H 0.906195 1.023979 0.552442 0.025 Uiso 0.25 1 d R U P . .
O12 O 0.7170(3) 0.9996(8) 0.75483(6) 0.0335(6) Uani 1 1 d G . . . .
H12A H 0.787321 1.005531 0.769408 0.050 Uiso 1 1 d G U . . .
H12B H 0.656261 1.087845 0.753993 0.050 Uiso 0.70(9) 1 d G U . . .
N7 N 0.8941(3) 0.7876(3) 0.65800(6) 0.0070(5) Uani 1 1 d . . . . .
O26 O 0.6002(3) 0.7033(3) 0.59996(6) 0.0119(5) Uani 1 1 d . . . . .
O27 O 0.2865(3) 0.4394(3) 0.53995(6) 0.0149(5) Uani 1 1 d . . . . .
H27A H 0.199697 0.452766 0.550801 0.022 Uiso 1 1 d R U . . .
H27B H 0.283130 0.340310 0.535044 0.022 Uiso 1 1 d R U . . .
C14 C 1.0191(4) 0.6995(3) 0.67291(7) 0.0085(7) Uani 1 1 d . . . . .
H14A H 1.059530 0.626666 0.656983 0.010 Uiso 1 1 calc R U . . .
H14B H 0.978886 0.640975 0.691335 0.010 Uiso 1 1 calc R U . . .
C28 C 0.7998(4) 0.6859(4) 0.63827(8) 0.0093(6) Uani 1 1 d . . . . .
H28A H 0.726530 0.633493 0.652421 0.011 Uiso 1 1 calc R U . . .
H28B H 0.865499 0.607968 0.628385 0.011 Uiso 1 1 calc R U . . .
O25 O 0.7610(3) 0.8960(3) 0.60249(6) 0.0117(5) Uani 1 1 d . . . . .
C19 C 0.7136(4) 0.7675(3) 0.61185(8) 0.0088(6) Uani 1 1 d . . . . .
C27 C 0.8012(3) 0.8538(3) 0.68446(7) 0.0088(6) Uani 1 1 d . . . . .
H27C H 0.869444 0.893074 0.701410 0.011 Uiso 1 1 calc R U . . .
H27D H 0.738034 0.773232 0.694129 0.011 Uiso 1 1 calc R U . . .
Cl1 Cl 0.8364(7) 1.1636(7) 0.500000 0.0215(13) Uani 0.56(2) 2 d S T . A 1
Cl1A Cl 0.792(3) 1.208(3) 0.500000 0.043(3) Uani 0.20(2) 2 d S T . B 2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'
Y Y -2.7962 3.5667 '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
0.00 -1.00 0.00 0.1800
0.00 1.00 0.00 0.1320
0.00 0.00 1.00 0.0120
0.00 0.00 -1.00 0.0170
2.00 0.00 -1.00 0.1510
-2.00 0.00 1.00 0.1530
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
O10 Eu1 N7 127.70(6) . 2_775 ?
O10 Eu1 N7 127.70(6) . 4_575 ?
O10 Eu1 N7 127.70(6) . 3_755 ?
O10 Eu1 N7 127.70(6) . . ?
N7 Eu1 N7 104.60(11) 2_775 . ?
N7 Eu1 N7 104.60(11) 3_755 4_575 ?
N7 Eu1 N7 68.04(6) 3_755 . ?
N7 Eu1 N7 68.04(6) 4_575 . ?
N7 Eu1 N7 68.04(6) 2_775 3_755 ?
N7 Eu1 N7 68.04(6) 2_775 4_575 ?
O25 Eu1 O10 73.39(6) 3_755 . ?
O25 Eu1 O10 73.39(6) 2_775 . ?
O25 Eu1 O10 73.39(6) 4_575 . ?
O25 Eu1 O10 73.39(6) . . ?
O25 Eu1 N7 131.45(8) 3_755 2_775 ?
O25 Eu1 N7 71.80(8) . 4_575 ?
O25 Eu1 N7 66.04(8) 2_775 2_775 ?
O25 Eu1 N7 131.45(8) 4_575 . ?
O25 Eu1 N7 71.80(8) 2_775 3_755 ?
O25 Eu1 N7 131.46(8) . 3_755 ?
O25 Eu1 N7 131.45(8) 2_775 4_575 ?
O25 Eu1 N7 71.80(8) 3_755 . ?
O25 Eu1 N7 66.04(8) . . ?
O25 Eu1 N7 71.80(8) 4_575 2_775 ?
O25 Eu1 N7 139.09(8) 3_755 4_575 ?
O25 Eu1 N7 139.09(8) . 2_775 ?
O25 Eu1 N7 66.04(8) 3_755 3_755 ?
O25 Eu1 N7 66.04(8) 4_575 4_575 ?
O25 Eu1 N7 139.09(8) 2_775 . ?
O25 Eu1 N7 139.09(8) 4_575 3_755 ?
O25 Eu1 O25 85.31(3) 4_575 . ?
O25 Eu1 O25 146.78(12) 3_755 4_575 ?
O25 Eu1 O25 85.31(3) 3_755 . ?
O25 Eu1 O25 85.31(3) 2_775 4_575 ?
O25 Eu1 O25 85.31(3) 2_775 3_755 ?
O25 Eu1 O25 146.78(12) 2_775 . ?
O26 Y1 O26 119.12(13) . 2_665 ?
O26 Y1 O26 119.12(13) 4_565 3_655 ?
O26 Y1 O26 75.13(6) . 3_655 ?
O26 Y1 O26 75.13(6) . 4_565 ?
O26 Y1 O26 75.13(6) 4_565 2_665 ?
O26 Y1 O26 75.13(6) 2_665 3_655 ?
O26 Y1 O27 139.65(9) 4_565 4_565 ?
O26 Y1 O27 144.47(9) . 3_655 ?
O26 Y1 O27 75.61(9) 3_655 . ?
O26 Y1 O27 75.62(9) . 4_565 ?
O26 Y1 O27 78.65(9) 2_665 . ?
O26 Y1 O27 139.65(9) 3_655 3_655 ?
O26 Y1 O27 78.65(9) 3_655 4_565 ?
O26 Y1 O27 75.62(9) 4_565 2_665 ?
O26 Y1 O27 144.47(9) 3_655 2_665 ?
O26 Y1 O27 78.65(9) 4_565 3_655 ?
O26 Y1 O27 144.47(9) 4_565 . ?
O26 Y1 O27 75.62(9) 2_665 3_655 ?
O26 Y1 O27 78.65(9) . 2_665 ?
O26 Y1 O27 139.65(9) . . ?
O26 Y1 O27 139.65(8) 2_665 2_665 ?
O26 Y1 O27 144.47(9) 2_665 4_565 ?
O27 Y1 O27 112.17(13) . 2_665 ?
O27 Y1 O27 112.17(13) 3_655 4_565 ?
O27 Y1 O27 71.86(6) . 3_655 ?
O27 Y1 O27 71.86(6) . 4_565 ?
O27 Y1 O27 71.86(6) 3_655 2_665 ?
O27 Y1 O27 71.86(6) 2_665 4_565 ?
H1A O1 H1A 125.7 . 2_565 ?
H1A O1 H1B 49.9 . 2_565 ?
H1A O1 H1B 104.3 . . ?
H1A O1 H1B 104.3 2_565 2_565 ?
H1B O1 H1A 49.9 . 2_565 ?
H1B O1 H1B 128.3 . 2_565 ?
Eu1 O10 H10A 111.9 . . ?
Eu1 O10 H10B 111.9 . . ?
H10A O10 H10B 102.2 . . ?
H12A O12 H12B 112.3 . . ?
C14 N7 Eu1 111.32(19) . . ?
C14 N7 C27 107.8(2) . . ?
C28 N7 Eu1 106.89(18) . . ?
C28 N7 C14 109.4(2) . . ?
C28 N7 C27 109.8(3) . . ?
C27 N7 Eu1 111.56(17) . . ?
C19 O26 Y1 148.7(2) . . ?
Y1 O27 H27A 111.9 . . ?
Y1 O27 H27B 111.9 . . ?
H27A O27 H27B 102.3 . . ?
N7 C14 H14A 109.3 . . ?
N7 C14 H14B 109.3 . . ?
N7 C14 C27 111.8(2) . 3_755 ?
H14A C14 H14B 107.9 . . ?
C27 C14 H14A 109.3 3_755 . ?
C27 C14 H14B 109.3 3_755 . ?
N7 C28 H28A 108.9 . . ?
N7 C28 H28B 108.9 . . ?
N7 C28 C19 113.4(3) . . ?
H28A C28 H28B 107.7 . . ?
C19 C28 H28A 108.9 . . ?
C19 C28 H28B 108.9 . . ?
C19 O25 Eu1 122.9(2) . . ?
O26 C19 C28 118.1(3) . . ?
O26 C19 O25 123.2(3) . . ?
O25 C19 C28 118.7(3) . . ?
N7 C27 C14 112.5(2) . 4_575 ?
N7 C27 H27C 109.1 . . ?
N7 C27 H27D 109.1 . . ?
C14 C27 H27C 109.1 4_575 . ?
C14 C27 H27D 109.1 4_575 . ?
H27C C27 H27D 107.8 . . ?
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
Eu1 O10 2.424(4) . ?
Eu1 N7 2.650(3) . ?
Eu1 N7 2.650(3) 2_775 ?
Eu1 N7 2.650(3) 4_575 ?
Eu1 N7 2.650(3) 3_755 ?
Eu1 O25 2.403(2) . ?
Eu1 O25 2.403(2) 3_755 ?
Eu1 O25 2.403(2) 4_575 ?
Eu1 O25 2.403(2) 2_775 ?
Y1 O26 2.323(2) 2_665 ?
Y1 O26 2.323(2) 4_565 ?
Y1 O26 2.323(2) . ?
Y1 O26 2.323(2) 3_655 ?
Y1 O27 2.362(3) . ?
Y1 O27 2.362(3) 4_565 ?
Y1 O27 2.362(3) 3_655 ?
Y1 O27 2.362(3) 2_665 ?
O1 H1A 0.8717 . ?
O1 H1A 0.87(8) 2_565 ?
O1 H1B 0.87(9) 2_565 ?
O1 H1B 0.8708 . ?
O10 H10A 0.9223 . ?
O10 H10B 0.9221 . ?
O12 H12A 0.8698 . ?
O12 H12B 0.9473 . ?
N7 C14 1.487(4) . ?
N7 C28 1.474(4) . ?
N7 C27 1.492(4) . ?
O26 C19 1.253(4) . ?
O27 H27A 0.8978 . ?
O27 H27B 0.8996 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C27 1.516(4) 3_755 ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C19 1.519(4) . ?
O25 C19 1.271(4) . ?
C27 H27C 0.9900 . ?
C27 H27D 0.9900 . ?
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
Eu1 N7 C14 C27 44.0(3) . . . 3_755 ?
Eu1 N7 C28 C19 -35.3(3) . . . . ?
Eu1 N7 C27 C14 40.9(3) . . . 4_575 ?
Eu1 O25 C19 O26 -169.6(2) . . . . ?
Eu1 O25 C19 C28 9.2(4) . . . . ?
Y1 O26 C19 C28 -62.3(5) . . . . ?
Y1 O26 C19 O25 116.5(4) . . . . ?
N7 C28 C19 O26 -159.9(3) . . . . ?
N7 C28 C19 O25 21.3(4) . . . . ?
C14 N7 C28 C19 -156.0(3) . . . . ?
C14 N7 C27 C14 163.4(3) . . . 4_575 ?
C28 N7 C14 C27 161.9(3) . . . 3_755 ?
C28 N7 C27 C14 -77.4(3) . . . 4_575 ?
C27 N7 C14 C27 -78.7(3) . . . 3_755 ?
C27 N7 C28 C19 85.8(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.978(13)
2 0.022(13)
