Long Story Short: Donor Set Symmetry in Eu.DOTA Crystals Determines the Electronic Structure
Storm Thomsen, Maria; Andersen, Helene O. B.; Sørensen, Thomas Just; Dalton Transactions  (2022) –; doi:10.1039/D2DT02172B

data_7710956
_publ_section_title
;
 Long Story Short: Donor Set Symmetry in Eu.DOTA Crystals Determines the
 Electronic Structure
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02172B
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H28 Eu N4 O9, Cl, 2(H2 O)'
_chemical_formula_sum            'C16 H32 Cl Eu N4 O11'
_chemical_formula_weight         643.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-04 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1540(11)
_cell_length_b                   15.8407(17)
_cell_length_c                   15.8615(17)
_cell_measurement_reflns_used    9565
_cell_measurement_temperature    100
_cell_measurement_theta_max      41.14
_cell_measurement_theta_min      2.57
_cell_volume                     2300.0(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40965
_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         30.505
_diffrn_reflns_theta_min         2.569
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.907
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.5644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0876 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.7544.
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    1.859
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 3019 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0153
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0108P)^2^+0.1945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0378
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6924
_reflns_number_total             7028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02172b5.cif
_cod_data_source_block           d8v4348__ny0m
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H64 Cl2 Eu2 N8 O22'
_cod_original_formula_weight         1287.73
_cod_original_formula_moiety         '2(C16 H28 Eu N4 O9), 2(Cl), 4(H2 O)'
_cod_original_formula_units_Z            2
_cod_database_code               7710956
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.578
_shelx_estimated_absorpt_t_min   0.426
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O11(H11C,H11D), O3(H3A,H3B)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B),
 C16(H16A,H16B), C2(H2A,H2B), C9(H9A,H9B), C11(H11A,H11B), C3(H3C,H3D), C7(H7A,
 H7B), C15(H15A,H15B)
2.c Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_shelx_res_checksum              8637
_olex2_submission_special_instructions 'No special instructions were received'