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_7715873
_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 H22.983 Eu N2 Na O13.491, 2.509(H2 O)'
_chemical_formula_sum            'C10 H28 Eu N2 Na O16'
_chemical_formula_weight         607.29
_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                   19.3808(9)
_cell_length_b                   35.2814(17)
_cell_length_c                   12.0315(6)
_cell_measurement_reflns_used    9146
_cell_measurement_temperature    100
_cell_measurement_theta_max      55.86
_cell_measurement_theta_min      3.12
_cell_volume                     8226.9(7)
_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 0.999
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35327
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         2.074
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.5128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1185 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.6828.
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    1.961
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             4864
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.606
_exptl_crystal_size_mid          0.522
_exptl_crystal_size_min          0.434
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(10)
_refine_ls_extinction_coef       0.00039(2)
_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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0162P)^2^+23.3911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0464
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                6407
_reflns_number_total             6527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00157e2.cif
_cod_data_source_block           mo_d8v5243_0ma
_cod_depositor_comments
'Adding full bibliography for 7715871--7715877.cif.'
_cod_database_code               7715873
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.982(10)
 0.018(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All H(H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 Na1-H7C \\sim Na1-H7D
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O3 \\sim H3A \\sim H3B: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
Uanis(O6) \\sim Ueq, : with sigma of 0.001 and sigma for terminal atoms of 0.002
Uiso(H6A) = Uiso(H10A)
5. Others
 Sof(O2)=Sof(H2A)=Sof(H2B)=Sof(O13)=Sof(H13A)=Sof(H13B)=1-FVAR(1)
 Sof(O18)=Sof(H18A)=Sof(H18B)=Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(1)
6.a Free rotating group:
 O17(H17A), O18(H18A,H18B), O7(H7C,H7D), O15(H15A,H15B), O2(H2A,H2B)
6.b Rotating group:
 O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B)
6.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C10(H10C,H10D), C5(H5A,H5B), C3(H3C,H3D), C7(H7A,H7B)
6.d Tetrahedral OH refined with riding coordinates:
 O3(H3A)
;
_shelx_res_checksum              39836
_olex2_submission_special_instructions 'No special instructions were received'