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_7715875
_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_formula_moiety         'C21 H17 Cs3 N3 O18 Sm, 3(H2 O)'
_chemical_formula_sum            'C21 H23 Cs3 N3 O21 Sm'
_chemical_formula_weight         1202.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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            4
_cell_length_a                   10.0017(13)
_cell_length_b                   18.033(3)
_cell_length_c                   18.530(3)
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    100
_cell_measurement_theta_max      45.28
_cell_measurement_theta_min      2.20
_cell_volume                     3342.1(9)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64847
_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         36.330
_diffrn_reflns_theta_min         2.198
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.067
_exptl_absorpt_correction_T_max  0.7492
_exptl_absorpt_correction_T_min  0.5940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1034 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.7928.
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    2.390
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.347
_refine_diff_density_min         -2.019
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.132(16)
_refine_ls_extinction_coef       0.00019(4)
_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   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         8116
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.711
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+10.9945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7616
_reflns_number_total             8116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00157e2.cif
_cod_data_source_block           mo_d8v5763_0ma
_cod_depositor_comments
'Adding full bibliography for 7715871--7715877.cif.'
_cod_original_cell_volume        3342.1(8)
_cod_database_code               7715875
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.494
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.868(16)
 0.132(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C6-H6 = C6-C2 = C6-C9
 0.4 with sigma of 0.02
 C2-C4 = C2-C6 = C2-H2
 0.4 with sigma of 0.02
 C9-C3
 0.4 with sigma of 0.02
 Cs1-O8 \\sim Cs1A-O8
 with sigma of 0.02
 Cs1-O12 \\sim Cs1A-O12
 with sigma of 0.02
4. Rigid bond restraints
 C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
6. Others
 Sof(Cs1A)=Sof(O1)=1-FVAR(1)
 Sof(Cs1)=Sof(O2)=FVAR(1)
 Fixed Sof: H11A(0.5) H11B(0.5)
7.a Free rotating group:
 O3(H3A,H3B), O11(H11A,H11B)
7.b Rotating group:
 O6(H6A,H6B), O12(H12A,H12B)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C2(H2), C5(H5)
;
_shelx_res_checksum              82553
_olex2_submission_special_instructions 'No special instructions were received'