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
Storm Thomsen, Maria; Parsons, Simon; Sørensen, Thomas Just; Dalton Transactions  (2022) –; doi:10.1039/D2DT02633C

data_7711386
_publ_section_title
;
 Invisible strings. The first single crystal of the cTSAP form of
 [Eu(DOTA)(H2O)]&#x2212; 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 Eu Gd N4 O13, 2.438(Cl), 2(H3.5 O2), H4 O2'
_chemical_formula_sum            'C16 H45 Cl2.44 Eu Gd N4 O19'
_chemical_formula_weight         993.18
_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                   8.8814(7)
_cell_length_b                   8.8814(7)
_cell_length_c                   41.505(5)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.23
_cell_measurement_theta_min      2.73
_cell_volume                     3273.9(5)
_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      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            46223
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.309
_diffrn_reflns_theta_min         2.345
_exptl_absorpt_coefficient_mu    4.186
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.3380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1640 before and 0.1045 after correction.
The Ratio of minimum to maximum transmission is 0.4524.
The \l/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    2.015
_exptl_crystal_description       plate
_exptl_crystal_F_000             1958
_exptl_crystal_size_max          0.748
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.704
_refine_diff_density_min         -3.181
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0289
_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/[\s^2^(Fo^2^)+(0.0370P)^2^+13.9852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3648
_reflns_number_total             4000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02633c4.cif
_cod_data_source_block           mo_d8v4791_0m_e
_cod_original_cell_volume        3273.9(6)
_cod_database_code               7711386
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.146
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(2)
 0.08(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: H1A(0.25) H1B(0.25) H4C(0.75) H5A(0.5) H5B(0.5)
5.a Free rotating group:
 O4(H4C,H4D), O5(H5A,H5B)
5.b Rotating group:
 O1(H1A,H1B), O2(H2C,H2D)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C4(H4A,H4B), C2(H2A,H2B)
;
_shelx_res_checksum              26617
_shelx_hkl_checksum              19579
_olex2_submission_special_instructions 'No special instructions were received'