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_7711550
_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
'C60 H70 Dy8 N8 O37, 8(Cl), 5(H2 O), 2(C2 H6 O), 12[C2H6O], 10[H2O]'
_chemical_formula_sum            'C88 H184 Cl8 Dy8 N8 O66'
_chemical_formula_weight         3994.02
_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
_atom_sites_solution_primary     iterative
_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                 92.0950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.56100(10)
_cell_length_b                   18.40980(10)
_cell_length_c                   19.74860(10)
_cell_measurement_reflns_used    35867
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.6980
_cell_measurement_theta_min      3.2950
_cell_volume                     7107.00(6)
_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      100.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50425
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.051
_diffrn_reflns_theta_min         2.239
_exptl_absorpt_coefficient_mu    24.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37131
_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    1.866
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.019(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         14029
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0808P)^2^+24.6896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                13449
_reflns_number_total             14029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02653h2.cif
_cod_data_source_block           20210318-lfp-lbf-031503_sq_sq
_cod_database_code               7711550
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.159
_shelx_estimated_absorpt_t_min   0.122
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.981(5)
 0.019(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(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
 H16a-H22a
 2.1 with sigma of 0.01
 O23-C32 \\sim O24-C32
 with sigma of 0.02
 Dy3-H15a \\sim Dy3-H15b
 with sigma of 0.02
 Dy3-H16a \\sim Dy3-H16b
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim C7 \\sim C6 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C29 \\sim C26 \\sim C27 \\sim C28 \\sim C30 \\sim C25: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H32c)=Sof(H32d)=Sof(O23)=Sof(H23)=1-FVAR(1)
 Sof(O24)=Sof(H24a)=Sof(H32a)=Sof(H32b)=FVAR(1)
 Fixed Sof: H21a(0.5) H21b(0.5)
6.a Riding coordinates:
 O5(H5), O15(H15a,H15b), O21(H21a,H21b)
6.b Free rotating group:
 O16(H16a,H16b), O20(H20a,H20b), O22(H22a,H22b)
6.c Rotating group:
 O17(H17a,H17b), O18(H18a,H18b), O14(H14a,H14b)
6.d Ternary CH refined with riding coordinates:
 C22(H22), C7(H7)
6.e Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b), C32(H32c,H32d)
6.f Aromatic/amide H refined with riding coordinates:
 C30(H30), C28(H28), C29(H29), C24(H24), C13(H13), C12(H12), C11(H11), N1(H1a),
  C20(H20), C19(H19), C18(H18), C17(H17), C16(H16), C1(H1b), C2(H2), C3(H3),
 C4(H4), C5(H5a), C9(H9)
6.g Fitted hexagon refined as free rotating group:
 C30(C25,C26,C27,C28,C29), C10(C15,C14,C13,C12,C11), C21(C20,C19,C18,C17,C16),
 C6(C1,C2,C3,C4,C5)
6.h X=CH2 refined with riding coordinates:
 O19(H19a,H19b)
6.i Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c)
6.j Idealised tetrahedral OH refined as rotating group:
 O1(H1), O24(H24a), O23(H23)
;
_shelx_res_checksum              60284
_shelx_hkl_checksum              4974
_shelx_fab_checksum              6806
_platon_squeeze_special_details
;
A solvent mask was calculated and 822 electrons were 
found in a volume of 2619\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[C2H6O], 10[H2O] per Asymmetric Unit 
which account for 824 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'