The pentagram-typed Ln15 (Ln=Dy, Tb, Eu, Sm, Ho) clusters with different anion templates: magnetic and luminescent properties
Zou, Ying; Lv, Wei; Xue, Zhe; Pan, Jie; Li, Xiao-Yu; Wang, Guo-Ming; Dalton Transactions  (2022) –; doi:10.1039/D2DT02712G

data_7711436
_publ_section_title
;
 The pentagram-typed Ln15 (Ln=Dy, Tb, Eu, Sm, Ho) clusters with different
 anion templates: magnetic and luminescent properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02712G
_journal_year                    2022
_chemical_formula_moiety         'C60 H140 Cl Dy15 N10 O80, 13(Cl)'
_chemical_formula_sum            'C60 H140 Cl14 Dy15 N10 O80'
_chemical_formula_weight         5215.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-22 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5433(3)
_cell_length_b                   29.8188(3)
_cell_length_c                   24.4709(4)
_cell_measurement_reflns_used    20791
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.3860
_cell_measurement_theta_min      2.5240
_cell_volume                     15720.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     46.00  92.00   0.50    1.77    --  104.12 -77.00  30.00   92
  2  \w     39.00  68.00   0.50    1.77    --  104.12 -61.00  60.00   58
  3  \w     44.00  71.00   0.50    1.77    --  104.12 -61.00  30.00   54
  4  \w    -15.00  27.00   0.50    0.44    --   45.94 -19.00 -30.00   84
  5  \w     46.00  71.00   0.50    1.77    --  104.12 -61.00-150.00   50
  6  \w     42.00  69.00   0.50    1.77    --  104.12 -61.00-120.00   54
  7  \w     56.00 113.00   0.50    1.77    --  104.12-149.00-167.00  114
  8  \w     39.00  97.00   0.50    1.77    --  104.12-124.00  -4.00  116
  9  \w    -40.00  23.00   0.50    0.44    --  -45.94  37.00-147.00  126
 10  \w    -62.00 -36.00   0.50    1.77    -- -104.00  61.00 -60.00   52
 11  \w    -24.00  19.00   0.50    0.44    --  -45.94  19.00   0.00   86
 12  \w    -69.00 -44.00   0.50    1.77    -- -104.00  61.00  30.00   50
 13  \w   -159.00 -94.00   0.50    1.77    -- -104.00 -37.00  57.00  130
 14  \w   -169.00-135.00   0.50    1.77    -- -104.00 -85.00-116.00   68
 15  \w   -112.00 -83.00   0.50    0.44    --  -45.94-125.00-150.00   58
 16  \w   -117.00 -92.00   0.50    0.44    --  -45.94-125.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0343590000
_diffrn_orient_matrix_UB_12      -0.0175198000
_diffrn_orient_matrix_UB_13      0.0508823000
_diffrn_orient_matrix_UB_21      -0.0530763000
_diffrn_orient_matrix_UB_22      0.0173785000
_diffrn_orient_matrix_UB_23      0.0365441000
_diffrn_orient_matrix_UB_31      -0.0335018000
_diffrn_orient_matrix_UB_32      -0.0453977000
_diffrn_orient_matrix_UB_33      -0.0057297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62120
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.686
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    40.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.204
_exptl_crystal_description       block
_exptl_crystal_F_000             9752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.628
_refine_diff_density_min         -4.399
_refine_diff_density_rms         0.550
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         16305
_refine_ls_number_restraints     376
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.1042
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2998
_refine_ls_wR_factor_ref         0.3186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12292
_reflns_number_total             16305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02712g2.cif
_cod_data_source_block           1
_cod_database_code               7711436
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
015e08c9a99065665c14e280cddc011f9c000277b73
;
_diffrn_oxdiff_digest_hkl
;
0100eaad46b985a476faaf1250f351c04dfcd5
;
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H46 of O46, H2 of O2, H16 of O16, H10 of O10, H8 of O8,
  H14 of O14, H28 of O28, H20 of O20, H24 of O24, H22 of O22, H30 of O30, All
  N(H) groups
 At 1.5 times of:
  H48 of O48, H50 of O50, H36 of O36, H52 of O52, H54 of O54, H56 of O56, H38
  of O38, H66 of O66, H68 of O68, H70 of O70, H58 of O58, H60 of O60, H62 of
  O62, H64 of O64
2. Restrained distances
 O36-H36
 0.85 with sigma of 0.01
 O38-H38
 0.85 with sigma of 0.01
 O48-H48
 0.85 with sigma of 0.01
 O50-H50
 0.85 with sigma of 0.01
 O52-H52
 0.85 with sigma of 0.01
 O54-H54
 0.85 with sigma of 0.01
 O60-H60
 0.85 with sigma of 0.01
 O70-C27
 1.4 with sigma of 0.02
 O56-H56
 0.85 with sigma of 0.01
 O58-H58
 0.85 with sigma of 0.01
 C4-H36
 1.880318 with sigma of 0.02
 Dy11-H36
 3.017246 with sigma of 0.02
 C6-H38
 1.907649 with sigma of 0.02
 Dy13-H38
 3.011882 with sigma of 0.02
 C18-H48
 1.91535 with sigma of 0.02
 Dy15-H48
 2.968821 with sigma of 0.02
 C17-H50
 1.959328 with sigma of 0.02
 Dy9-H50
 2.996305 with sigma of 0.02
 C26-H52
 1.890047 with sigma of 0.02
 Dy7-H52
 3.00404 with sigma of 0.02
 C23-H54
 1.885505 with sigma of 0.02
 Dy9-H54
 3.014421 with sigma of 0.02
 C22-H60
 1.853118 with sigma of 0.02
 Dy11-H60
 2.997874 with sigma of 0.02
 C24-H56
 1.870331 with sigma of 0.02
 Dy15-H56
 2.980574 with sigma of 0.02
 C30-H58
 1.856373 with sigma of 0.02
 Dy13-H58
 3.026866 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O66 \\sim O66 \\sim O68 \\sim O68: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O66 \\sim O66: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C21 \\sim C21 \\sim C28 \\sim O66 \\sim O66 \\sim O68: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C21 \\sim O66: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C12 \\sim C23 \\sim C27 \\sim O54 \\sim O70: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
N6 \\sim C16 \\sim C19 \\sim C26 \\sim C28 \\sim O68: within 1.7A with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O66) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O68)
\\sim Ueq, Uanis(O64) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O64) \\sim Ueq,
Uanis(O24) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O66) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O68)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(O66) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O68)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O66) \\sim Ueq, Uanis(O66) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O24) \\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(O16) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O30) \\sim Ueq,
Uanis(O32) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O3W)
\\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O42) \\sim Ueq,
Uanis(O4W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O46)
\\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O50) \\sim Ueq,
Uanis(O52) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O54) \\sim Ueq, Uanis(O56)
\\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O60) \\sim Ueq, Uanis(O62) \\sim Ueq,
Uanis(O64) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 O2(H2), N2(H2A), N4(H4), N6(H6), O8(H8), N8(H8A), O10(H10), N10(H10A),
 O14(H14), O16(H16), O20(H20), O22(H22), O24(H24), O28(H28), O30(H30)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C13(H13A,H13B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
4.c Aromatic/amide H refined with riding coordinates:
 O46(H46)
4.d Tetrahedral OH refined with riding coordinates:
 O62(H62), O66(H66), O68(H68)
4.e Idealised tetrahedral OH refined as rotating group:
 O64(H64), O70(H70)
;
_shelx_res_checksum              79778
_shelx_hkl_checksum              26178
_shelx_fab_checksum              38485
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.501
_oxdiff_exptl_absorpt_empirical_full_min 0.432