Contrasting impact of coordination polyhedra and site symmetry on the electronic energy levels in nine-coordinated Eu(III) and Sm(III) crystals structures determined from single crystal luminescence spectra.
Mortensen, Sabina Svava; Nielsen, Villads R. M.; Sørensen, Thomas Just; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10079–10092; doi:10.1039/d4dt00157e

data_7715874
_publ_section_title
;
 Contrasting impact of coordination polyhedra and site symmetry on the
 electronic energy levels in nine-coordinated Eu(III) and Sm(III) crystals
 structures determined from single crystal luminescence spectra.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10079
_journal_page_last               10092
_journal_paper_doi               10.1039/d4dt00157e
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H23.113 N2 Na O13.557 Sm, 2.443(H2 O)'
_chemical_formula_sum            'C10 H28 N2 Na O16 Sm'
_chemical_formula_weight         605.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.459(3)
_cell_length_b                   35.397(6)
_cell_length_c                   12.032(2)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.23
_cell_measurement_theta_min      2.39
_cell_volume                     8288(2)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42482
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         2.071
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.6962.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             4848
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.024(10)
_refine_ls_extinction_coef       0.000101(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         8972
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+12.5418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                8445
_reflns_number_total             8972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00157e2.cif
_cod_data_source_block           mo_d8v5332_0ma
_cod_depositor_comments
'Adding full bibliography for 7715871--7715877.cif.'
_cod_database_code               7715874
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.283
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.976(10)
 0.024(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O16-H16B
 0.85 with sigma of 0.0002
 O13-H13C \\sim O13A-H13A
 with sigma of 0.02
 O13-H13D \\sim O13A-H13B
 with sigma of 0.02
 H13C-H13D \\sim H13A-H13B
 with sigma of 0.04
4. Others
 Sof(O2)=Sof(H2A)=Sof(H2B)=1-FVAR(1)
 Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Sof(O13A)=Sof(H13A)=Sof(H13B)=1-FVAR(2)
 Sof(O13)=Sof(H13C)=Sof(H13D)=FVAR(2)
5.a Free rotating group:
 O6(H6A,H6B), O12(H12A,H12B), O13(H13C,H13D), O7(H7C,H7D), O15(H15A,H15B),
 O2(H2A,H2B), O13A(H13A,H13B)
5.b Rotating group:
 O3(H3A,H3B)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C6(H6C,H6D), C4(H4A,H4B)
;
_shelx_res_checksum              82778
_olex2_submission_special_instructions 'No special instructions were received'