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_4349904
_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_absolute_configuration ad
_chemical_formula_moiety         'C33 H44 Dy F12 Li O17'
_chemical_formula_sum            'C33 H44 Dy F12 Li O17'
_chemical_formula_weight         1110.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-08
_audit_creation_method
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  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                 94.512(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3203(4)
_cell_length_b                   12.2197(4)
_cell_length_c                   15.8773(5)
_cell_measurement_reflns_used    4148
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.1060
_cell_measurement_theta_min      2.3630
_cell_volume                     2382.93(13)
_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
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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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_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 0.9832
_diffrn_measured_fraction_theta_max 0.5327
_diffrn_measurement_details
;
  1 omega  -79.00  -44.00   1.0000    3.0200
omega____ theta____ kappa____ phi______ frames
    -      -20.9487 -178.0000 -180.0000 35

  2 omega    2.00   92.00   1.0000    3.0200
omega____ theta____ kappa____ phi______ frames
    -       23.4487   57.0000   30.0000 90

  3 omega   52.00   99.00   1.0000    3.0200
omega____ theta____ kappa____ phi______ frames
    -       23.4487  178.0000  -30.0000 47

  4 omega  -41.00    9.00   1.0000    3.0200
omega____ theta____ kappa____ phi______ frames
    -       23.4487  -77.0000   90.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0210510000
_diffrn_orient_matrix_UB_12      0.0001723000
_diffrn_orient_matrix_UB_13      0.0403171000
_diffrn_orient_matrix_UB_21      -0.0392593000
_diffrn_orient_matrix_UB_22      -0.0397153000
_diffrn_orient_matrix_UB_23      -0.0141293000
_diffrn_orient_matrix_UB_31      0.0368458000
_diffrn_orient_matrix_UB_32      -0.0422770000
_diffrn_orient_matrix_UB_33      0.0134712000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11726
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.92
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73263
_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    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1110
_exptl_crystal_preparation
'Magnetic properties,Luminescent,Triboluminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.180
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         8042
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                6984
_reflns_number_total             8042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi00772a5.cif
_cod_data_source_block           exp_1006
_cod_original_cell_volume        2382.94(14)
_cod_database_code               4349904
_reflns_odcompleteness_completeness 98.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_date_sample_data_collection 1465896448.17
_olex2_submission_special_instructions 'No special instructions were received'