Combination of single-molecule magnet behaviour and luminescence properties in a new series of lanthanide complexes with tris(pyrazolyl)borate and oligo(β-diketonate) ligands.
Mikhalyova, Elena A.; Zeller, Matthias; Jasinski, Jerry P.; Butcher, Raymond J.; Carrella, Luca M.; Sedykh, Alexander E.; Gavrilenko, Konstantin S.; Smola, Sergey S.; Frasso, Michael; Cazorla, Sebastian Calderon; Perera, Kuluni; Shi, Anni; Ranjbar, Habib G.; Smith, Casey; Deac, Alexandru; Liu, Youlin; McGee, Sean M.; Dotsenko, Vladimir P.; Kumke, Michael U.; Müller-Buschbaum, Klaus; Rentschler, Eva; Addison, Anthony W.; Pavlishchuk, Vitaly V.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7774–7789; doi:10.1039/d0dt00600a

data_7704247
_publ_section_title
;
 Combination of single-molecule magnet behaviour and luminescence
 properties in a new series of lanthanide complexes with
 tris(pyrazolyl)borate and oligo(\b-diketonate) ligands.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7774
_journal_page_last               7789
_journal_paper_doi               10.1039/d0dt00600a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H31 B2 Dy N12 O2, 1(C7H16)'
_chemical_formula_sum            'C36 H47 B2 Dy N12 O2'
_chemical_formula_weight         863.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-03 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.121(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3834(5)
_cell_length_b                   23.2108(10)
_cell_length_c                   15.7395(7)
_cell_measurement_reflns_used    4159
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6090
_cell_measurement_theta_min      3.5720
_cell_volume                     3879.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0416
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega    3.00   30.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  -60.0000 27

  2 omega   11.00   55.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -       35.3572   77.0000  120.0000 44

  3 omega  102.00  128.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 26

  4 omega   92.00  156.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -90.0000 64

  5 omega   91.00  169.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -60.0000 78

  6 omega   99.00  132.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 33

  7 omega   52.00  107.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 55

  8 omega   63.00  100.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 37

  9 omega   84.00  109.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 25

 10 omega   56.00   83.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 27

 11 omega   43.00  110.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 67

 12 omega   42.00   91.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 49

 13 omega   40.00   87.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 47

 14 omega   29.00   74.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -       35.3572  -99.0000    0.0000 45

 15 omega   46.00   79.00   1.0000    5.5650
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 33

 16 omega  -63.00  -17.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000 -150.0000 46

 17 omega -103.00  -74.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000 -150.0000 29

 18 omega  -90.00  -41.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -      -33.5000 -178.0000  -90.0000 49

 19 omega -103.00  -19.00   1.0000    1.3900
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000  120.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku-OxfordDiffraction Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0313663000
_diffrn_orient_matrix_UB_12      -0.0635317000
_diffrn_orient_matrix_UB_13      -0.0107268000
_diffrn_orient_matrix_UB_21      -0.1399321000
_diffrn_orient_matrix_UB_22      -0.0159183000
_diffrn_orient_matrix_UB_23      -0.0263638000
_diffrn_orient_matrix_UB_31      -0.0208422000
_diffrn_orient_matrix_UB_32      0.0108468000
_diffrn_orient_matrix_UB_33      -0.1010255000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7719
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.623
_diffrn_reflns_theta_min         3.562
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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    1.479
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.803
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3433
_reflns_number_total             3690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00600a4.cif
_cod_data_source_block           ta-lm140616a
_cod_depositor_comments
'Adding full bibliography for 7704247--7704266.cif.'
_cod_database_code               7704247
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C36 H47 B2 Dy N12 O2'
_chemical_oxdiff_usercomment     'Addison's TA-LM140616a'
_shelx_estimated_absorpt_t_max   0.214
_shelx_estimated_absorpt_t_min   0.097
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 236 electrons were
found in a volume of 972 cubic Angstrom in two voids 
per unit cell.
This is consistent with the presence of 1[n-heptane] 
per Formula Unit which account for 232 electrons per 
unit cell. This material was recrystallised from 
n-heptane.
;
_shelx_res_checksum              48394
_shelx_fab_checksum              55556
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_special_instructions 'No special instructions were received'