Dinuclear lanthanide‒lithium complexes based on fluorinated β-diketonate with acetal group: magnetism and effect of crystal packing on mechanoluminescence
Bazhin, Denis N.; Kudyakova, Yulia S.; Bogomyakov, Artem S.; Slepukhin, Pavel A.; Kim, Grigory A.; Burgart, Yanina V.; Saloutin, Victor I.; Inorganic Chemistry Frontiers 6 (2019) 40–; doi:10.1039/C8QI00772A

data_4349903
_publ_section_title
;
 Dinuclear lanthanide--lithium complexes based on fluorinated
 \b-diketonate with acetal group: magnetism and effect of crystal packing
 on mechanoluminescence
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              40
_journal_paper_doi               10.1039/C8QI00772A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C32 H42 Dy F12 Li O17'
_chemical_formula_sum            'C32 H42 Dy F12 Li O17'
_chemical_formula_weight         1096.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-09
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2018-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1377(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0892(3)
_cell_length_b                   11.9719(2)
_cell_length_c                   22.2112(5)
_cell_measurement_reflns_used    9571
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.5130
_cell_measurement_theta_min      2.4060
_cell_volume                     4532.35(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 15.9555
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details
;
  1 omega  -68.00  -35.00   1.0000   19.2600
omega____ theta____ kappa____ phi______ frames
    -      -20.7924 -178.0000  -30.0000 33

  2 omega  -25.00    0.00   1.0000   19.2600
omega____ theta____ kappa____ phi______ frames
    -      -20.7924  -99.0000  120.0000 25

  3 omega  -25.00    0.00   1.0000   19.2600
omega____ theta____ kappa____ phi______ frames
    -      -20.7924  -99.0000  -60.0000 25

  4 omega    0.00   91.00   1.0000   19.2600
omega____ theta____ kappa____ phi______ frames
    -       23.2924   38.0000  -60.0000 91

  5 omega  -46.00   44.00   1.0000   19.2600
omega____ theta____ kappa____ phi______ frames
    -       23.2924  -38.0000  120.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0356457000
_diffrn_orient_matrix_UB_12      0.0223428000
_diffrn_orient_matrix_UB_13      0.0132120000
_diffrn_orient_matrix_UB_21      -0.0015483000
_diffrn_orient_matrix_UB_22      0.0429832000
_diffrn_orient_matrix_UB_23      -0.0220423000
_diffrn_orient_matrix_UB_31      -0.0214141000
_diffrn_orient_matrix_UB_32      0.0341427000
_diffrn_orient_matrix_UB_33      0.0190837000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26513
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.90
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            '? colourless'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2188
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         12473
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                9424
_reflns_number_total             12473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi00772a5.cif
_cod_data_source_block           exp_1000
_cod_original_cell_volume        4532.35(16)
_cod_database_code               4349903
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22