Slow magnetic relaxation and luminescence properties in neodymium(iii)-4,4,4-trifluoro-1-(2-naphthyl)butane-1,3-dionato complexes incorporating bipyridyl ligands
Vicente, Ramon; Tubau, Ànnia; Speed, Saskia; Mautner, Franz A.; Bierbaumer, Florian; Fischer, Roland C.; Massoud, Salah S.; New Journal of Chemistry 45 (2021) 14713–14723; doi:10.1039/D1NJ02583J

data_7060880
_publ_section_title
;
 Slow magnetic relaxation and luminescence properties in
 neodymium(iii)-4,4,4-trifluoro-1-(2-naphthyl)butane-1,3-dionato complexes
 incorporating bipyridyl ligands
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14713
_journal_page_last               14723
_journal_paper_doi               10.1039/D1NJ02583J
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C54 H32 F9 N2 Nd O6, 0.5[C2H6O]'
_chemical_formula_sum            'C55 H35 F9 N2 Nd O6.5'
_chemical_formula_weight         1143.09
_chemical_name_common            '[Nd(L)3(phen)]'
_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   geom
_audit_creation_date             2021-06-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.06.01 svn.r985b505f for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                88.967(2)
_cell_angle_beta                 82.251(3)
_cell_angle_gamma                72.708(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6987(4)
_cell_length_b                   12.5344(5)
_cell_length_c                   21.2378(9)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.40
_cell_volume                     2441.96(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37723
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        28.061
_diffrn_reflns_theta_max         28.061
_diffrn_reflns_theta_min         2.361
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  0.8967
_exptl_absorpt_correction_T_min  0.7245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11807
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.6600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9334
_reflns_number_total             11807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02583j2.cif
_cod_data_source_block           rf1614a
_cod_depositor_comments
'Adding full bibliography for 7060876--7060881.cif.'
_cod_original_formula_sum        'C55 H35 F9 N2 Nd O6.50'
_cod_database_code               7060880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.754
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O5-C30 \\sim O5-C30A
 with sigma of 0.02
 F9-C29 \\sim F9A-C29A
 with sigma of 0.02
 C30-C32 \\sim C30A-C32
 with sigma of 0.04
 C29-C31 \\sim C29A-C31A
 with sigma of 0.04
 F8-C30 \\sim F8A-C30A
 with sigma of 0.04
 F8-C29 \\sim F8A-C29A
 with sigma of 0.02
 F7-C29 \\sim F7A-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 F8-F7 \\sim F8A-F7A
 with sigma of 0.04
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 F7-C30 \\sim F7A-C30A
 with sigma of 0.04
 C31-C32 \\sim C31A-C32
 with sigma of 0.02
 O5-C29 \\sim O5-C29A
 with sigma of 0.04
 O5-C31 \\sim O5-C31A
 with sigma of 0.04
 F9-F8 \\sim F9A-F8A
 with sigma of 0.04
 F9-F7 \\sim F9A-F7A
 with sigma of 0.04
 F9-C30 \\sim F9A-C30A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F2) \\sim Ueq: with sigma of 0.009 and sigma for terminal atoms of 0.018
: with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Sof(F9A)=Sof(F8A)=Sof(F7A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=1-FVAR(1)
 Sof(F9)=Sof(F8)=Sof(F7)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(H31)=FVAR(1)
 Fixed Uiso: F9(0.03) F8(0.03) F7(0.03) C29(0.03) C30(0.03) C31(0.03) H31(0.03)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C8(H8), C10(H10), C11(H11), C14(H14), C13(H13),
 C17(H17), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
  C31(H31), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C50(H50), C51(H51), C52(H52), C53(H53),
  C54(H54), C31A(H31A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 30 electrons were 
found in a volume of 212\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 0.5[C2H6O] per Formula Unit 
which account for 26 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43718
_shelx_fab_checksum              59673
_olex2_submission_special_instructions 'No special instructions were received'