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_7711435
_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 Ho15 N10 O80, 14(Cl)'
_chemical_formula_sum            'C60 H160 Cl15 Ho15 N10 O80'
_chemical_formula_weight         5307.67
_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             2022-01-12
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4098(3)
_cell_length_b                   29.7523(4)
_cell_length_c                   24.2371(4)
_cell_measurement_reflns_used    22368
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.5050
_cell_measurement_theta_min      2.9520
_cell_volume                     15438.8(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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.942
_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     37.00 103.00   0.50    0.36    --  104.12-111.00  23.00  132
  2  \w    121.00 170.00   0.50    0.36    --  104.12  86.00-134.00   98
  3  \w     92.00 170.00   0.50    0.36    --  104.12  39.00  35.00  156
  4  \w     18.00  43.00   0.50    0.09    --   45.82-125.00-180.00   50
  5  \w    -21.00  14.00   0.50    0.09    --  -45.82  19.00-180.00   70
  6  \w    -74.00 -43.00   0.50    0.36    -- -104.00  77.00-180.00   62
  7  \w    -42.00  16.00   0.50    0.09    --  -45.82  39.00  35.00  116
  8  \w    -58.00 -31.00   0.50    0.36    -- -104.00  61.00  30.00   54
  9  \w    -66.00 -41.00   0.50    0.36    -- -104.00  61.00  60.00   50
 10  \w    -69.00 -41.00   0.50    0.36    -- -104.00  61.00  90.00   56
 11  \w   -112.00 -72.00   0.50    0.36    -- -104.00 125.00 150.00   80
 12  \w    -68.00 -31.00   0.50    0.36    -- -104.00 125.00 150.00   74
 13  \w    -88.00 -35.00   0.50    0.09    --  -45.82 -39.00-118.00  106
;
_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      0.0267236000
_diffrn_orient_matrix_UB_12      -0.0448956000
_diffrn_orient_matrix_UB_13      0.0210863000
_diffrn_orient_matrix_UB_21      -0.0234165000
_diffrn_orient_matrix_UB_22      0.0110759000
_diffrn_orient_matrix_UB_23      0.0585660000
_diffrn_orient_matrix_UB_31      -0.0625578000
_diffrn_orient_matrix_UB_32      -0.0232886000
_diffrn_orient_matrix_UB_33      -0.0129451000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53272
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.751
_diffrn_reflns_theta_min         2.543
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17492
_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    2.283
_exptl_crystal_description       block
_exptl_crystal_F_000             9960
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.798
_refine_diff_density_min         -3.423
_refine_diff_density_rms         0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         15720
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0955
_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^)+(0.1820P)^2^+310.0208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2622
_refine_ls_wR_factor_ref         0.2857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12348
_reflns_number_total             15720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02712g2.cif
_cod_data_source_block           5
_cod_database_code               7711435
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
011a737294839c89e5268f1be8b2d4ba0e00035dafe
;
_diffrn_oxdiff_digest_hkl
;
013d446eb6b536e343a3ef0f0368505b5ab992
;
_reflns_odcompleteness_completeness 99.64
_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, H34 of O34, H35 of O35, H1 of O1, H24 of O24, H20 of O20,
   H8 of O8, H9 of O9, H5 of O5, H17 of O17, H7 of O7, H12 of O12, All N(H)
  groups
 At 1.5 times of:
  All O(H,H) groups, H33 of O33, H32 of O32, H31 of O31, H25 of O25, H28 of
  O28, H23 of O23, H27 of O27, H26 of O26, H29 of O29, H30 of O30, H21 of O21,
  H22 of O22, H11 of O11, H14 of O14
2. Restrained distances
 O11-H11
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 O21-H21
 0.87 with sigma of 0.01
 O25-H25
 0.87 with sigma of 0.01
 O26-H26
 0.87 with sigma of 0.01
 O28-H28
 0.87 with sigma of 0.01
 O29-H29
 0.87 with sigma of 0.01
 H24-O24
 0.9 with sigma of 0.02
 H24-C30
 2 with sigma of 0.02
 O23-H23
 0.87 with sigma of 0.01
 C26-H23
 1.874652 with sigma of 0.02
 C22-H25
 1.865107 with sigma of 0.02
 C25-H21
 1.9019 with sigma of 0.02
 C21-H28
 1.927606 with sigma of 0.02
 C16-H26
 1.914931 with sigma of 0.02
 C23-H29
 1.931584 with sigma of 0.02
 Ho7-H21
 3.008234 with sigma of 0.02
 Ho7-H25
 3.018335 with sigma of 0.02
 C13-H11
 1.894629 with sigma of 0.02
 Ho4-H26
 3.012827 with sigma of 0.02
 Ho5-H11
 3.039455 with sigma of 0.02
 Ho5-H28
 3.038243 with sigma of 0.02
 C11-H14
 1.887024 with sigma of 0.02
 Ho8-H29
 3.062816 with sigma of 0.02
 Ho8-H14
 3.002823 with sigma of 0.02
 Ho4-H23
 3.010038 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C24 \\sim C26 \\sim O30: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
N2 \\sim C17 \\sim C20 \\sim O22 \\sim O24 \\sim C28 \\sim C30 \\sim O33:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
C7 \\sim C11 \\sim O14 \\sim C23 \\sim C27 \\sim O29 \\sim O32: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Riding coordinates:
 C26(H26A,H26B)
4.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
4.c Ternary CH refined with riding coordinates:
 O1(H1), N1(H1A), N2(H2), N3(H3), N4(H4), O5(H5), N5(H5A), O7(H7), O8(H8),
 O9(H9), O12(H12), O17(H17), O20(H20), O34(H34), O35(H35)
4.d Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
4.e Tetrahedral OH refined with riding coordinates:
 O30(H30)
4.f Idealised tetrahedral OH refined as rotating group:
 O22(H22), O27(H27), O31(H31), O32(H32), O33(H33)
;
_shelx_res_checksum              77483
_shelx_hkl_checksum              60005
_shelx_fab_checksum              5718
_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 3.535
_oxdiff_exptl_absorpt_empirical_full_min 0.398