Assembly of pinwheel/twist shaped chiral lanthanide clusters with rotor structures by annular/linear growth mechanism and their magnetic properties
Long, Bing-Fan; Li, Yun-Lan; Zhu, Zhong-Hong; Wang, Hai-Ling; Liang, Fu-Pei; Zou, Hua-Hong; Dalton Transactions  (2022) –; doi:10.1039/D2DT02653H

data_7711548
_publ_section_title
;
 Assembly of pinwheel/twist shaped chiral lanthanide clusters with rotor
 structures by annular/linear growth mechanism and their magnetic
 properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02653H
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C64 H78 Dy8 N8 O37, 8(Cl), 7(H2 O), 2(C2 H6 O), 7[C2H6O], 7[H2O]'
_chemical_formula_sum            'C82 H160 Cl8 Dy8 N8 O60'
_chemical_formula_weight         3801.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-18 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1497(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.58205(16)
_cell_length_b                   18.45363(15)
_cell_length_c                   19.78771(14)
_cell_measurement_reflns_used    33983
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.3700
_cell_measurement_theta_min      2.2290
_cell_volume                     7145.45(10)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -32.00  36.00   0.50    0.80    --  -43.18  26.00 -78.00  136
  2  \w     18.00 122.00   0.50    0.80    --   43.18  26.00 -78.00  208
  3  \w     84.00 178.00   0.50    2.00    --  109.26  26.00 -78.00  188
  4  \w    143.00 174.00   0.50    2.00    --  109.26  45.00-150.00   62
  5  \w    134.00 173.00   0.50    2.00    --  109.26  61.00-180.00   78
  6  \w    150.00 178.00   0.50    2.00    --  109.26 125.00 -60.00   56
  7  \w     95.00 139.00   0.50    2.00    --  109.26  45.00-150.00   88
  8  \w     86.00 127.00   0.50    2.00    --  109.26  61.00-180.00   82
  9  \w     95.00 121.00   0.50    2.00    --  109.26 125.00 -60.00   52
 10  \w     95.00 153.00   0.50    2.00    --  109.26 125.00 -30.00  116
 11  \w     87.00 172.00   0.50    2.00    --  109.26  30.00  30.00  170
 12  \w     81.00 106.00   0.50    2.00    --  109.26 -77.00  30.00   50
 13  \w     77.00 108.00   0.50    2.00    --  109.26-108.00 -28.13   62
 14  \w     83.00 111.00   0.50    2.00    --  109.26-125.00   0.00   56
 15  \w     66.00 108.00   0.50    2.00    --  109.26-125.00  60.00   84
 16  \w     68.00 111.00   0.50    2.00    --  109.26-125.00  90.00   86
 17  \w     49.00  75.00   0.50    2.00    --  109.26-108.00 -28.13   52
 18  \w     46.00  94.00   0.50    2.00    --  109.26 -94.00 -90.00   96
 19  \w     68.00 105.00   0.50    2.00    --  109.26 -94.00-150.00   74
 20  \w     91.00 117.00   0.50    2.00    --  109.26-133.00-109.50   52
 21  \w     51.00  76.00   0.50    2.00    --  109.26-125.00  30.00   50
 22  \w     35.00  60.00   0.50    2.00    --  109.26 -77.00  30.00   50
 23  \w     41.00  67.00   0.50    2.00    --  109.26 -61.00  30.00   52
 24  \w     35.00  62.00   0.50    2.00    --  109.26 -61.00  60.00   54
 25  \w     48.00 108.00   0.50    2.00    --  109.26-113.00 144.41  120
 26  \w     39.00 108.00   0.50    2.00    --  109.26-125.00 150.00  138
 27  \w     36.00  87.00   0.50    2.00    --  109.26 -94.00 150.00  102
 28  \w     42.00  70.00   0.50    2.00    --  109.26-125.00   0.00   56
 29  \w     36.00  85.00   0.50    2.00    --  109.26 -94.00 -60.00   98
 30  \w     41.00  70.00   0.50    2.00    --  109.26-133.00-109.50   58
 31  \w     44.00  85.00   0.50    2.00    --  109.26 -94.00-120.00   82
 32  \w     37.00  65.00   0.50    2.00    --  109.26 -61.00-120.00   56
 33  \w     34.00  97.00   0.50    0.80    --   43.18-125.00 -30.00  126
 34  \w     -1.00  83.00   0.50    0.80    --   43.18 -99.00-120.00  168
 35  \w    -36.00  32.00   0.50    0.80    --   43.18 -26.00 117.00  136
 36  \w    -27.00  38.00   0.50    0.80    --  -43.18  19.00 150.00  130
 37  \w    -27.00  38.00   0.50    0.80    --  -43.18  19.00  90.00  130
 38  \w    -51.00 -16.00   0.50    2.00    --  -90.25  45.00  30.00   70
 39  \w    -51.00 -26.00   0.50    2.00    --  -90.25  45.00  90.00   50
 40  \w    -72.00  31.00   0.50    0.80    --  -43.18  77.00  90.00  206
 41  \w    -56.00 -20.00   0.50    2.00    --  -90.25 125.00 -30.00   72
 42  \w    -84.00 -57.00   0.50    2.00    --  -90.25 125.00 -30.00   54
 43  \w   -122.00 -17.00   0.50    0.80    --  -43.18 -26.00 117.00  210
 44  \w   -120.00 -72.00   0.50    2.00    --  -90.25 -62.00  22.49   96
 45  \w   -148.00 -94.00   0.50    2.00    --  -90.25 -94.00 150.00  108
 46  \w   -169.00 -64.00   0.50    2.00    --  -90.25 -26.00 117.00  210
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44229
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.234
_exptl_absorpt_coefficient_mu    24.033
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26483
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       block
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.896
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.077(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         12550
_refine_ls_number_restraints     1237
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1174P)^2^+136.1222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1766
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                12216
_reflns_number_total             12550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02653h2.cif
_cod_data_source_block           20210709-lfp-lbf-070604
_cod_database_code               7711548
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.161
_shelx_estimated_absorpt_t_min   0.134
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.923(9)
 0.077(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 H19B-H18A
 2.1 with sigma of 0.02
 H19A-H19A_$1
 2.1 with sigma of 0.02
 H19A_$1-H19A
 2.1 with sigma of 0.02
 Dy1-H17A \\sim Dy1-H17B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C6 \\sim C1 \\sim C5 \\sim C2 \\sim C4 \\sim C3: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C21 \\sim C20 \\sim C16 \\sim C18 \\sim C19 \\sim C17: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C26 \\sim C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C24 \\sim C10 \\sim
C15 \\sim C14 \\sim C13 \\sim C12 \\sim C11 \\sim C21 \\sim C16 \\sim C17 \\sim
C18 \\sim C19 \\sim C20 \\sim C22 \\sim C7 \\sim C9 \\sim C8 \\sim C6 \\sim C1
\\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C23 \\sim C31 \\sim C32 \\sim C35
\\sim C34: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
Uanis(O23) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C15, Dy4, O12, O8, O7, O16, O11, O33, Dy3, Dy2, C29, C30, O4, O14, O6, O15,
 N4, O10, O23, O3, O9, C28, C25, C14, C23, C35, N3, C24, Dy1, C27, C26, C13,
 C22, C34, O17, O18, O2, N2, C10, C12, C21, O5, C8, N1, C9, C11, C16, C20, C7,
 C17, C19, C6, O1, C18, C1, C5, C2, C4, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H32C)=Sof(H32D)=Sof(O25)=Sof(H25)=1-FVAR(1)
 Sof(O22)=Sof(H22A)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Fixed Sof: H21A(0.5) H21B(0.5)
7.a Riding coordinates:
 O14(H14A,H14B), O5(H5), O19(H19A,H19B), O18(H18A,H18B), O21(H21A,H21B),
 O20(H20A,H20B)
7.b Free rotating group:
 O17(H17A,H17B), O26(H26A,H26B)
7.c Rotating group:
 O16(H16A,H16B), O23(H23A,H23B)
7.d Ternary CH refined with riding coordinates:
 C22(H22), C7(H7)
7.e Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C32(H32C,H32D), C35(H35A,H35B)
7.f Aromatic/amide H refined with riding coordinates:
 N3(H3), C26(H26), C28(H28), C27(H27), C24(H24), N1(H1A), C13(H13), C12(H12),
 C11(H11), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C9(H9), C5(H5A),
 C1(H1B), C2(H2), C3(H3A), C4(H4)
7.g Fitted hexagon refined as free rotating group:
 C26(C25,C30,C29,C28,C27), C10(C15,C14,C13,C12,C11), C21(C16,C17,C18,C19,C20),
 C5(C6,C1,C2,C3,C4)
7.h Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C)
7.i Idealised tetrahedral OH refined as rotating group:
 O1(H1), O22(H22A), O25(H25)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 507 electrons were 
found in a volume of 2394\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 7[C2H6O], 7[H2O] per Formula Unit 
which account for 504 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85119
_shelx_hkl_checksum              16677
_shelx_fab_checksum              51799
_platon_squeeze_void_probe_radius 1.20
_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
;