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_7710955
_publ_section_title
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 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_formula_moiety         'C30 H50 B2 Eu N6 O13 P2, Cl, 4.32(H2 O)'
_chemical_formula_sum            'C30 H58.64 B2 Cl Eu N6 O17.32 P2'
_chemical_formula_weight         1051.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                97.955(4)
_cell_angle_beta                 96.588(3)
_cell_angle_gamma                113.624(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8019(10)
_cell_length_b                   13.0077(13)
_cell_length_c                   16.9777(16)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.26
_cell_measurement_theta_min      2.40
_cell_volume                     2126.1(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 1.000
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            123351
_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         33.141
_diffrn_reflns_theta_min         1.745
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1153 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.8239.
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    1.643
_exptl_crystal_description       plate
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.608
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         16216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0213P)^2^+2.0104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14453
_reflns_number_total             16216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02172b5.cif
_cod_data_source_block           mo_d8v5039_0m_a
_cod_database_code               7710955
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(O17)=Sof(H17A)=Sof(H17B)=FVAR(2)
3.a Free rotating group:
 O16(H16C,H16D), O9(H9C,H9D), O7(H7D,H7E), O17(H17A,H17B)
3.b Rotating group:
 O12(H12A)
3.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C14(H14A,H14B),
 C16(H16A,H16B), C26(H26A,H26B), C28(H28A,H28B), C15(H15A,H15B), C2(H2A,H2B),
 C9(H9A,H9B), C5(H5A,H5B), C25(H25A,H25B), C27(H27A,H27B)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C20(H20), C24(H24), C17(H17), C21(H21), C11(H11A), C23(H23),
 C3(H3A), C13(H13A)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C29(H29A,H29B,H29C)
3.f Idealised tetrahedral OH refined as rotating group:
 O18(H18), O11(H11), O13(H13)
;
_shelx_res_checksum              98925
_olex2_submission_special_instructions 'No special instructions were received'