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_7711437
_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 H160 Cl N10 O80 Tb15, 4(N O3), 10(Cl)'
_chemical_formula_sum            'C60 H160 Cl11 N14 O92 Tb15'
_chemical_formula_weight         5323.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-13 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4425(2)
_cell_length_b                   21.4389(4)
_cell_length_c                   29.9936(4)
_cell_measurement_reflns_used    47838
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.0850
_cell_measurement_theta_min      2.0680
_cell_volume                     8641.2(2)
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.809
_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    -18.00  37.00   0.50    0.70    --    3.36 -99.00 -60.00  110
  2  \w     12.00  37.00   0.50    0.70    --    3.36 -99.00   0.00   50
  3  \w    -18.00  36.00   0.50    0.70    --    3.36 -99.00  30.00  108
  4  \w    -47.00 -17.00   0.50    0.70    --    3.36 -38.00-180.00   60
  5  \w     27.00  76.00   0.50    0.70    --    3.36  38.00-150.00   98
  6  \w    -18.00  27.00   0.50    0.70    --   -6.72 -99.00-180.00   90
  7  \w    -26.00  -1.00   0.50    0.70    --   -6.72  93.00 171.00   50
  8  \w    -17.00  14.00   0.50    0.70    --   -6.72 -99.00   0.00   62
  9  \w    -23.00   3.00   0.50    0.70    --   -6.72 -93.00  60.00   52
;
_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      0.0482022000
_diffrn_orient_matrix_UB_12      -0.0134165000
_diffrn_orient_matrix_UB_13      -0.0002997000
_diffrn_orient_matrix_UB_21      0.0203292000
_diffrn_orient_matrix_UB_22      0.0275004000
_diffrn_orient_matrix_UB_23      0.0097148000
_diffrn_orient_matrix_UB_31      -0.0070112000
_diffrn_orient_matrix_UB_32      -0.0125725000
_diffrn_orient_matrix_UB_33      0.0215705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            101277
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.033
_diffrn_reflns_theta_min         2.009
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51630
_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    2.046
_exptl_crystal_description       block
_exptl_crystal_F_000             5032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.043
_refine_diff_density_min         -2.052
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         22371
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0749P)^2^+136.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16981
_reflns_number_total             22371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02712g2.cif
_cod_data_source_block           2
_cod_database_code               7711437
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
013d8e6d62d1d78bb3916626468742121100033f96e
;
_diffrn_oxdiff_digest_hkl
;
01cabccf2eba385f1d91af686870b545a75341
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H23A,H23B} of O23, H10 of O10, H8 of O8, H3 of O3, H7 of
  O7, H5 of O5, H4 of O4, H6 of O6, H2 of O2, H9 of O9, H1 of O1, H33 of O33,
  H28 of O28, H29 of O29, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  H20 of O20, H18 of O18, H24 of O24, H14 of O14, H19 of O19, H13 of O13, H15
  of O15, H20A of O20A, {H2WA,H2WB} of O2W, {H4WA,H4WB} of O4W, {H5WA,H5WB} of
  O5W, {H3WA,H3WB} of O3W, {H1WA,H1WB} of O1W, H30 of O30, H25 of O25, H35 of
  O35, H34 of O34
2. Restrained distances
 O19-H19
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 O34-H34
 0.87 with sigma of 0.01
 O18-H18
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 C12-O35
 1.4 with sigma of 0.02
 C9-C12
 1.5 with sigma of 0.02
 O39-O40
 2.35 with sigma of 0.02
 O30-C22
 1.4 with sigma of 0.02
 C21-C22
 1.48 with sigma of 0.02
 O41-O39
 2.3 with sigma of 0.02
 O40-O41
 2.3 with sigma of 0.02
 O24-H24
 0.87 with sigma of 0.01
 O29-H29
 0.9 with sigma of 0.02
 C29-H19
 1.9305 with sigma of 0.02
 Tb6-H19
 3.082004 with sigma of 0.02
 C2-H13
 1.970854 with sigma of 0.02
 Tb7-H13
 3.054353 with sigma of 0.02
 C10-H34
 1.964678 with sigma of 0.02
 Tb8-H34
 3.16707 with sigma of 0.02
 C30-H18
 1.865558 with sigma of 0.02
 Tb6-H18
 3.035142 with sigma of 0.02
 C1-H14
 2.058886 with sigma of 0.02
 Tb7-H14
 2.999788 with sigma of 0.02
 C17-H24
 1.91566 with sigma of 0.02
 Tb2-H24
 3.066661 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N7 \\sim O39 \\sim O40 \\sim O41: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
N6 \\sim O36 \\sim O37 \\sim O38: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O30) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O41)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl6) \\sim Ueq, Uanis(Cl5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O20(0.5) H20(0.5) O20A(0.5) H20A(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
5.b Ternary CH refined with riding coordinates:
 O1(H1), N1(H1A), O2(H2), N2(H2A), O3(H3), N3(H3A), O4(H4), N4(H4A), O5(H5),
 N5(H5A), O6(H6), O7(H7), O8(H8), O9(H9), O10(H10), C28(H28A)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2B,H2C), C4(H4B,H4C), C5(H5B,H5C), C8(H8A,H8B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B),
 C17(H17A,H17B), C18(H18A,H18B), C20(H20B,H20C), C22(H22A,H22B), O23(H23A,H23B),
  C23(H23C,H23D), C24(H24A,H24B), C26(H26A,H26B), C29(H29A,H29B), C30(H30A,H30B)
5.d Aromatic/amide H refined with riding coordinates:
 O33(H33)
5.e Idealised tetrahedral OH refined as rotating group:
 O15(H15), O20(H20), O20A(H20A), O25(H25), O30(H30), O35(H35)
;
_shelx_res_checksum              93422
_shelx_hkl_checksum              3762
_shelx_fab_checksum              2982
_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 1.550
_oxdiff_exptl_absorpt_empirical_full_min 0.731