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_7711434
_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 H144 Cl N10 O80 Sm15, 11(Cl)'
_chemical_formula_sum            'C60 H144 Cl12 N10 O80 Sm15'
_chemical_formula_weight         4966.49
_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                   30.0081(9)
_cell_length_b                   12.3183(3)
_cell_length_c                   21.6051(6)
_cell_measurement_reflns_used    14292
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3080
_cell_measurement_theta_min      2.2280
_cell_volume                     7986.3(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -23.00  29.00   0.50    1.09    --    3.51  95.00 108.00  104
  2  \w     -8.00  37.00   0.50    1.09    --    3.51 -99.00-150.00   90
  3  \w    -17.00  12.00   0.50    1.09    --   -6.87 -99.00 -30.00   58
  4  \w    -24.00   2.00   0.50    1.09    --   -6.87 -95.00  -0.00   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      0.0134687000
_diffrn_orient_matrix_UB_12      0.0317390000
_diffrn_orient_matrix_UB_13      0.0200462000
_diffrn_orient_matrix_UB_21      -0.0154690000
_diffrn_orient_matrix_UB_22      0.0433183000
_diffrn_orient_matrix_UB_23      -0.0022576000
_diffrn_orient_matrix_UB_31      -0.0117600000
_diffrn_orient_matrix_UB_32      -0.0207614000
_diffrn_orient_matrix_UB_33      0.0258960000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33272
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.004
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.703
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27270
_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    2.065
_exptl_crystal_description       block
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.801
_refine_diff_density_min         -2.538
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         7533
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1122P)^2^+416.7511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5789
_reflns_number_total             7533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02712g2.cif
_cod_data_source_block           4
_cod_database_code               7711434
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
0105946b85ed2ab788c0885abac3a3e04700028ee52
;
_diffrn_oxdiff_digest_hkl
;
01d63481bec038b54e25336fbe3a903ce4d6dd
;
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H6 of O6, H8 of O8, H4 of O4, H5 of O5, H1 of O1, H3 of
  O3, H7 of O7, H2 of O2, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, H9 of O9, H11 of O11, H10 of O10, H21A of O21A, H21 of
  O21, H16A of O16A, H16 of O16
2. Restrained distances
 C14A-C16A
 1.5 with sigma of 0.02
 C18-C13A
 1.52 with sigma of 0.02
 C13A-N3A
 1.2 with sigma of 0.02
 C14A-C15A
 1.5 with sigma of 0.02
 O16A-C9A
 1.4 with sigma of 0.02
 C8A-O16A
 2.4 with sigma of 0.02
 O11-C4
 1.45 with sigma of 0.02
 C17-C14
 1.48 with sigma of 0.02
 C16-C17
 2.2 with sigma of 0.02
 C10A-C10
 2.2 with sigma of 0.02
 O16-C8
 2.2 with sigma of 0.02
 C10-C8 = C8-C9
 1.5 with sigma of 0.02
 C9-O16
 1.45 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C2-O9
 1.5 with sigma of 0.02
 O9-H9
 0.85 with sigma of 0.01
 O10-C1
 1.45 with sigma of 0.02
 O10-H10
 0.85 with sigma of 0.01
 C17A-O21A
 1.45 with sigma of 0.02
 C2-H9
 1.948792 with sigma of 0.02
 Sm1-H9
 3.088505 with sigma of 0.02
 C1-H10
 1.90845 with sigma of 0.02
 Sm1-H10
 3.128948 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3A \\sim C13A \\sim C18 \\sim O19A \\sim O20A: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
N3A \\sim C15A \\sim C16A \\sim C17A \\sim O21A \\sim O22 \\sim O23: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl8: within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
N2A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim O17 \\sim O18: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
N2A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim O16A \\sim O17: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
N2 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim O16 \\sim O17 \\sim O18: within
1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim O9 \\sim O10: within 1.7A with
sigma of 0.001 and sigma for terminal atoms of 0.002
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim O9 \\sim O10 \\sim O11: within
1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
N3 \\sim C12 \\sim C13 \\sim O14A \\sim C14 \\sim O15A \\sim C15 \\sim C16
\\sim C17 \\sim O21 \\sim O22 \\sim O23: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H1WA(0.5) H1WB(0.5) N1(0.5) H1A(0.5) C1(0.5) H1B(0.5) H1C(0.5)
 N2A(0.5) H2AA(0.5) N2(0.5) H2A(0.5) C2(0.5) H2B(0.5) H2C(0.5) N3(0.5) H3A(0.5)
 N3A(0.5) H3AA(0.5) C3(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 C7(0.5) H7A(0.5) H7B(0.5) C7A(0.5) H7AB(0.5) H7AA(0.5) C8A(0.5) C8(0.5)
 O9(0.5) H9(0.5) C9(0.5) H9A(0.5) H9B(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5)
 O10(0.5) H10(0.5) C10A(0.5) H10C(0.5) H10D(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 O11(0.5) H11(0.5) C11(0.5) H11A(0.5) H11B(0.5) C11A(0.5) H11C(0.5) H11D(0.5)
 O12(0.5) O13(0.5) C13A(0.5) H13C(0.5) H13D(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 O14(0.5) O14A(0.5) C14A(0.5) C14(0.5) O15(0.5) O15A(0.5) C15A(0.5) H15C(0.5)
 H15D(0.5) C15(0.5) H15A(0.5) H15B(0.5) O16A(0.5) H16A(0.5) O16(0.5) H16(0.5)
 C16(0.5) H16B(0.5) H16C(0.5) C16A(0.5) H16D(0.5) H16E(0.5) C17(0.5) H17A(0.5)
 H17B(0.5) C17A(0.5) H17C(0.5) H17D(0.5) O19(0.5) O19A(0.5) O20A(0.5) O20(0.5)
 O21(0.5) H21(0.5) O21A(0.5) H21A(0.5) Cl8(0.25)
5.a Riding coordinates:
 C5(H5A,H5B), C13A(H13C,H13D)
5.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.c Ternary CH refined with riding coordinates:
 O1(H1), O2(H2), N2A(H2AA), N2(H2A), O3(H3), N3(H3A), N3A(H3AA), O4(H4),
 O5(H5), O6(H6), O7(H7), O8(H8)
5.d Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2B,H2C), C4(H4A,H4B), C7(H7A,H7B), C7A(H7AB,H7AA), C9(H9A,
 H9B), C9A(H9AA,H9AB), C10A(H10C,H10D), C10(H10A,H10B), C11(H11A,H11B),
 C11A(H11C,H11D), C13(H13A,H13B), C15A(H15C,H15D), C15(H15A,H15B), C16(H16B,
 H16C), C16A(H16D,H16E), C17(H17A,H17B), C17A(H17C,H17D)
5.e Aromatic/amide H refined with riding coordinates:
 N1(H1A)
5.f Tetrahedral OH refined with riding coordinates:
 O16A(H16A), O16(H16), O21(H21), O21A(H21A)
5.g Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_shelx_res_checksum              97451
_shelx_hkl_checksum              68862
_shelx_fab_checksum              95105
_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 2.516
_oxdiff_exptl_absorpt_empirical_full_min 0.520