LnDOTA puppeteering: removing the water molecule and imposing tetragonal symmetry.
Manvell, Anna Schannong; Pfleger, Rouven; Bonde, Niels Andreas; Briganti, Matteo; Mattei, Carlo Andrea; Nannestad, Theis Brock; Weihe, Høgni; Powell, Annie K.; Ollivier, Jacques; Bendix, Jesper; Perfetti, Mauro; Chemical science 15 (2023) 113–123; doi:10.1039/d3sc03928e

data_1570548
_publ_section_title
;
 LnDOTA puppeteering: removing the water molecule and imposing tetragonal
 symmetry.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              113
_journal_page_last               123
_journal_paper_doi               10.1039/d3sc03928e
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C16 H24 N4 O8 Yb, 3(C4 H12 N), 2(Cl), 6(H2 O)'
_chemical_formula_sum            'C28 H72 Cl2 N7 O14 Yb'
_chemical_formula_weight         974.87
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_Hall           'P 4 -2ab'
_space_group_name_H-M_alt        'P 4 b m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-13 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3928(6)
_cell_length_b                   17.3928(6)
_cell_length_c                   6.7688(3)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.99
_cell_measurement_theta_min      2.34
_cell_volume                     2047.63(13)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      100(2)
_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       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            41527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.085
_diffrn_reflns_theta_min         2.342
_exptl_absorpt_coefficient_mu    2.482
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5748
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0956 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.7698.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       needle
_exptl_crystal_F_000             1010
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.369(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2374
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0150
_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^)+(0.0124P)^2^+1.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0328
_refine_ls_wR_factor_ref         0.0344
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2055
_reflns_number_total             2374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03928e2.cif
_cod_data_source_block           mo_D8V4611_0m_d_AL_DSR
_cod_depositor_comments
'Adding full bibliography for 1570548--1570554.cif.'
_cod_original_cell_volume        2047.63(17)
_cod_database_code               1570548
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              622