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_7711433
_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 H136 Cl Eu15 N10 O80, 2(N O3), 10(Cl)'
_chemical_formula_sum            'C60 H136 Cl11 Eu15 N12 O86'
_chemical_formula_weight         5071.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_Hall           '-P 2a 2a'
_space_group_name_H-M_alt        'P m m a'
_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            2
_cell_length_a                   29.9490(5)
_cell_length_b                   12.2649(2)
_cell_length_c                   21.5496(4)
_cell_measurement_reflns_used    15184
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.1370
_cell_measurement_theta_min      4.6630
_cell_volume                     7915.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -31.00  39.00   0.50    7.36    --    0.00  82.00 150.00  140
  2  \w    -35.00  25.00   0.50    7.36    --    0.00 -82.00 150.00  120
  3  \w    -15.00  15.00   0.50    7.36    --    0.00  82.00 -90.00   60
  4  \w     73.00 116.00   0.50   29.45    --  101.30 -57.00-150.00   86
  5  \w     90.00 179.00   0.50   29.45    --  101.30  38.00 -30.00  178
  6  \w    108.00 184.00   0.50   29.45    --  101.30  82.00-150.00  152
  7  \w     12.00  40.00   0.50   29.45    --  101.30 -57.00-150.00   56
  8  \w     42.00 132.00   0.50   29.45    --  101.30 -82.00  60.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0144682000
_diffrn_orient_matrix_UB_12      0.1024551000
_diffrn_orient_matrix_UB_13      0.0361738000
_diffrn_orient_matrix_UB_21      -0.0201588000
_diffrn_orient_matrix_UB_22      0.0484272000
_diffrn_orient_matrix_UB_23      -0.0596952000
_diffrn_orient_matrix_UB_31      -0.0450777000
_diffrn_orient_matrix_UB_32      -0.0543972000
_diffrn_orient_matrix_UB_33      0.0150876000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21655
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        59.988
_diffrn_reflns_theta_max         59.988
_diffrn_reflns_theta_min         4.103
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    44.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.819
_refine_diff_density_min         -2.872
_refine_diff_density_rms         0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         6296
_refine_ls_number_restraints     525
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.1036
_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^)+(0.1665P)^2^+458.8376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2711
_refine_ls_wR_factor_ref         0.2758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5686
_reflns_number_total             6296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02712g2.cif
_cod_data_source_block           3
_cod_database_code               7711433
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.85
_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, H16 of O16, H23 of O23, H19 of O19, H21 of O21, H18 of
  O18, H20 of O20, H22 of O22, H17 of O17, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, H7A of O7A, H7 of O7, H13 of O13, H1 of O1, H1A of O1A
2. Restrained distances
 C12-C5A
 1.48 with sigma of 0.02
 C9-O8
 1.4 with sigma of 0.02
 O7A-C7A
 2.3 with sigma of 0.02
 O14-C16
 1.4 with sigma of 0.02
 O1-C2
 1.4 with sigma of 0.02
 O7A-C8A
 1.45 with sigma of 0.02
 C11-C12
 1.48 with sigma of 0.02
 C11A-O11
 2 with sigma of 0.02
 C17-O11
 2.1 with sigma of 0.02
 C10A-C10
 2.2 with sigma of 0.02
 C1-C4
 1.5 with sigma of 0.02
 C3A-C2A
 2.3 with sigma of 0.02
 C8A-C7A
 1.48 with sigma of 0.02
 C9-C7
 1.5 with sigma of 0.02
 C7A-C9A
 1.5 with sigma of 0.02
 C8-O7
 1.45 with sigma of 0.02
 C10A-C7A
 1.45 with sigma of 0.02
 C14-O13
 1.45 with sigma of 0.02
 C9-C9A
 2.3 with sigma of 0.02
 C13-C15
 1.5 with sigma of 0.02
 N3-C13
 1.45 with sigma of 0.02
 C16-C13
 1.48 with sigma of 0.02
 O24A-N4
 1.15 with sigma of 0.02
 C7-C10
 1.5 with sigma of 0.02
 C7-C9
 1.5 with sigma of 0.02
 C10A-Eu1
 3.5 with sigma of 0.02
 C9A-O7A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O10 \\sim O4A \\sim O6 \\sim N1A \\sim C12 \\sim C11 \\sim C5A: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.002
O15 \\sim O14 \\sim O13 \\sim N3 \\sim C15 \\sim C13 \\sim C17 \\sim C14 \\sim
C16: within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
O9 \\sim O8 \\sim N2A \\sim C8A \\sim C9A \\sim C7A \\sim C10A \\sim Cl4:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
O14 \\sim O13 \\sim C13 \\sim C14 \\sim C16: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
O7A \\sim C8A \\sim C9A \\sim C7A \\sim C10A: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
O4 \\sim O5 \\sim N1 \\sim C6 \\sim C5: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.002
O25 \\sim O26 \\sim O24A: within 1.7A with sigma of 0.001 and sigma for
terminal atoms of 0.002
O25 \\sim O26 \\sim N4 \\sim O24A: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
O11 \\sim O12 \\sim O6A \\sim N2A \\sim N3 \\sim C18 \\sim C11A \\sim C17:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
O7 \\sim N2 \\sim C7 \\sim C9 \\sim C8 \\sim C10: within 1.7A with sigma of
0.001 and sigma for terminal atoms of 0.002
O2 \\sim O3 \\sim O1A \\sim C2A \\sim C3A \\sim C4A \\sim C1A: within 1.7A with
sigma of 0.001 and sigma for terminal atoms of 0.002
O2 \\sim O3 \\sim O1 \\sim N1 \\sim C3 \\sim C2 \\sim C1 \\sim C4: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Eu4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Eu3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(O24A) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O25)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Eu1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O7A) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O4(0.5) O4A(0.5) O12(0.5) O1(0.5) H1(0.5) O6(0.5) O6A(0.5)
 O1A(0.5) H1A(0.5) O7A(0.5) H7A(0.5) O13(0.5) H13(0.5) O7(0.5) H7(0.5) N1A(0.5)
 H1AA(0.5) N2A(0.5) H2A(0.5) N3(0.5) H3(0.5) N2(0.5) H2(0.5) N1(0.5) H1B(0.5)
 C15(0.5) H15A(0.5) H15B(0.5) C13(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) C11A(0.5)
 H11A(0.5) H11B(0.5) C7(0.5) C5(0.5) H5A(0.5) H5B(0.5) C2A(0.5) H2AA(0.5)
 H2AB(0.5) C11(0.5) H11C(0.5) H11D(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C17(0.5)
 H17A(0.5) H17B(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 C3A(0.5) H3AA(0.5) H3AB(0.5) C8(0.5) H8A(0.5) H8B(0.5) C7A(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C2(0.5) H2B(0.5) H2C(0.5)
 C16(0.5) H16A(0.5) H16B(0.5) C1(0.5) C10(0.5) H10A(0.5) H10B(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) C10A(0.5) H10C(0.5) H10D(0.5)
 C1A(0.5) O25(0.5) O26(0.25) O24(0.25)
5.a Riding coordinates:
 C11A(H11A,H11B), C17(H17A,H17B)
5.b Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.c Ternary CH refined with riding coordinates:
 O19(H19), O22(H22), O17(H17), O23(H23), O20(H20), O21(H21), O18(H18),
 O16(H16), N1A(H1AA), N3(H3), N2(H2), N1(H1B)
5.d Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C8A(H8AA,H8AB), C5(H5A,H5B), C2A(H2AA,H2AB), C11(H11C,H11D),
 C9A(H9AA,H9AB), C5A(H5AA,H5AB), C9(H9A,H9B), C3A(H3AA,H3AB), C8(H8A,H8B),
 C3(H3A,H3B), C14(H14A,H14B), C2(H2B,H2C), C16(H16A,H16B), C10(H10A,H10B),
 C4(H4A,H4B), C4A(H4AA,H4AB), C10A(H10C,H10D)
5.e Aromatic/amide H refined with riding coordinates:
 N2A(H2A)
5.f Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O7A(H7A), O13(H13), O7(H7)
5.g Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              58008
_shelx_hkl_checksum              81020
_shelx_fab_checksum              51846
_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 19.502
_oxdiff_exptl_absorpt_empirical_full_min 0.442