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_7711551
_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
'C94 H88 Dy6 N12 O34, 7(H2 O), 4(C H4 O), 2(N O3), 9[CH4O], 7[H2O]'
_chemical_formula_sum            'C107 H168 Dy6 N14 O67'
_chemical_formula_weight         3697.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.41460(10)
_cell_length_b                   14.41460(10)
_cell_length_c                   71.4632(4)
_cell_measurement_reflns_used    26672
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6080
_cell_measurement_theta_min      2.4720
_cell_volume                     14848.67(17)
_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_detector_area_resol_mean 5.6
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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    -22.00  25.00   0.50    3.50    --   43.30 -19.00 -30.00   94
  2  \w     27.00  92.00   0.50    3.50    --   43.30-114.00-131.00  130
  3  \w     86.00 176.00   0.50   18.00    --  109.26  44.00-115.00  180
  4  \w     58.00 102.00   0.50   18.00    --  109.26 -94.00-120.00   88
  5  \w     35.00  60.00   0.50   18.00    --  109.26 -61.00-120.00   50
  6  \w     35.00 104.00   0.50   18.00    --  109.26 -77.00 -90.00  138
  7  \w     35.00  71.00   0.50   18.00    --  109.26 -61.00   0.00   72
  8  \w     36.00  85.00   0.50   18.00    --  109.26 -94.00  90.00   98
  9  \w    -38.00 -13.00   0.50    3.50    --  -43.30 125.00 -60.00   50
 10  \w    -26.00  35.00   0.50    3.50    --  -43.30  19.00-180.00  122
 11  \w   -156.00 -89.00   0.50   18.00    --  -90.25-114.00-131.00  134
;
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -88
_diffrn_reflns_number            49848
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.729
_diffrn_reflns_theta_min         2.473
_exptl_absorpt_coefficient_mu    16.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50372
_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    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             7360
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
TITL 20211020-lfp-lyl-P 41 21 2    R = 0.06
CELL   14.4146   14.4146   71.4632     90.00     90.00     90.00
SPGR P41212
C101 0.977 0.661 0.035 !       2.39 eA-3
Q102 0.642 0.672 0.905 !       2.32 eA-3
C103 0.452 0.508 0.220 !       2.26 eA-3
C104 0.542 0.215 0.191 !       2.23 eA-3
Q105 0.922 0.193 0.304 !       2.10 eA-3
C106 0.751 0.807 0.083 !       2.08 eA-3
Q107 0.433 0.307 0.445 !       2.07 eA-3
Q108 0.184 0.916 0.695 !       2.07 eA-3
C109 0.590 0.722 0.900 !       2.02 eA-3
C110 0.437 0.803 0.704 !       2.00 eA-3
C111 0.224 0.878 0.496 !       1.76 eA-3
Q112 0.550 0.382 0.277 !       1.63 eA-3
C113 0.614 0.863 0.995 !       1.60 eA-3
Q114 0.406 0.353 0.253 !       1.56 eA-3
C115 0.611 0.886 0.012 !       1.33 eA-3
Q116 0.484 0.704 0.826 !       1.32 eA-3
C117 0.892 0.614 0.989 !       1.30 eA-3
C118 0.311 0.138 0.451 !       1.28 eA-3
C119 0.911 0.348 0.287 !       1.26 eA-3
Q120 0.407 0.669 0.121 !       1.25 eA-3
C121 0.673 0.858 0.078 !       1.25 eA-3
C122 0.440 0.223 0.465 !       1.24 eA-3
C123 0.919 0.586 0.992 !       1.20 eA-3
Q124 0.407 0.377 0.452 !       1.19 eA-3
C125 0.612 0.213 0.184 !       1.19 eA-3
Q126 0.249 0.513 0.374 !       1.14 eA-3
C127 0.172 0.609 0.669 !       1.14 eA-3
C128 0.923 0.151 0.319 !       1.12 eA-3
C129 0.582 0.353 0.230 !       1.10 eA-3
C130 0.082 0.146 0.520 !       1.10 eA-3
Q131 0.418 0.356 0.618 !       1.09 eA-3
C132 0.471 0.538 0.719 !       1.08 eA-3
C133 0.246 0.887 0.699 !       1.03 eA-3
Q134 0.744 0.094 0.262 !       1.01 eA-3
Q135 0.080 0.841 0.484 !       1.01 eA-3
C136 0.854 0.887 0.984 !       1.00 eA-3
Q137 0.692 0.135 0.273 !       1.00 eA-3
C138 0.308 0.850 0.686 !       1.00 eA-3
C139 0.060 0.045 0.001 !       0.99 eA-3
Q140 0.242 0.382 0.415 !       0.97 eA-3
Q141 0.140 0.997 0.059 !       0.97 eA-3
Q142 0.726 0.188 0.977 !       0.95 eA-3
Q143 0.110 0.528 0.531 !       0.95 eA-3
C144 0.808 0.685 0.935 !       0.94 eA-3
Q145 0.301 0.825 0.746 !       0.91 eA-3
C146 0.794 0.307 0.196 !       0.89 eA-3
Q147 0.581 0.420 0.212 !       0.88 eA-3
Q148 0.255 0.200 0.495 !       0.86 eA-3
Q149 0.496 0.515 0.472 !       0.85 eA-3
C150 0.930 0.406 0.277 !       0.85 eA-3
Q151 0.424 0.704 0.688 !       0.82 eA-3
C152 0.887 0.891-0.001 !       0.79 eA-3
Q153 0.487 0.694 0.683 !       0.79 eA-3
C154 0.010 0.999 0.501 !       0.79 eA-3
Q155 0.443 0.193 0.222 !       0.79 eA-3
C156 0.390 0.890 0.728 !       0.78 eA-3
Q157 0.736 0.360 0.195 !       0.78 eA-3
C158 0.666 0.149 0.207 !       0.77 eA-3
Q159 0.290 0.576 0.812 !       0.76 eA-3
C160 0.901 0.555 0.990 !       0.75 eA-3
C161 0.140 0.668 0.684 !       0.75 eA-3
C162 0.423 0.680 0.743 !       0.74 eA-3
C163 0.253 0.169 0.429 !       0.74 eA-3
C164 0.568 0.939 0.981 !       0.74 eA-3
Q165 0.175 0.449 0.784 !       0.74 eA-3
C166 0.704 1.002 0.003 !       0.73 eA-3
Q167 0.544 0.511 0.610 !       0.73 eA-3
C168 0.765 0.815 0.019 !       0.71 eA-3
C169 0.737 0.390 0.248 !       0.71 eA-3
Q170 0.127 0.834 0.706 !       0.71 eA-3
Q171 0.629 0.440 0.578 !       0.71 eA-3
Q172 0.539 0.841 0.976 !       0.71 eA-3
C173 0.750 0.860 0.969 !       0.70 eA-3
C174 0.860 0.846-0.001 !       0.70 eA-3
C175 0.672 0.826 0.970 !       0.70 eA-3
Q176 0.108 0.021 0.871 !       0.69 eA-3
Q177 0.923 0.887 0.508 !       0.69 eA-3
Q178 0.203 1.000 0.643 !       0.69 eA-3
C179 0.279 0.992 0.586 !       0.68 eA-3
Q180 0.067 0.533 0.523 !       0.68 eA-3
C181 0.309 0.575 0.764 !       0.68 eA-3
Q182 0.772 0.905 0.035 !       0.67 eA-3
C183 0.531 0.512 0.742 !       0.67 eA-3
Q184 0.203 0.364 0.768 !       0.66 eA-3
Q185 0.748 0.700 0.262 !       0.66 eA-3
Q186 0.363 0.181 0.602 !       0.66 eA-3
C187 0.780 0.728 0.952 !       0.66 eA-3
Q188 0.099 0.862 0.419 !       0.66 eA-3
Q189 0.798 0.339 0.242 !       0.66 eA-3
C190 0.638 0.919 0.993 !       0.64 eA-3
Q191 0.738 0.676 0.117 !       0.64 eA-3
Q192 0.576 0.842 0.890 !       0.62 eA-3
Q193 0.281 0.019 0.721 !       0.62 eA-3
Q194 0.566 0.960 0.016 !       0.62 eA-3
C195 0.253 0.517 0.750 !       0.61 eA-3
Q196 0.391 0.369 0.375 !       0.60 eA-3
C197 0.775 0.669 0.949 !       0.60 eA-3
C198 0.703 0.345 0.263 !       0.60 eA-3
C199 0.761 0.878 0.020 !       0.60 eA-3
;
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 4765 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         14921
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0620P)^2^+10.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                12933
_reflns_number_total             14921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02653h2.cif
_cod_data_source_block           20211020-lfp-lyl-101903_sq
_cod_original_cell_volume        14848.7(2)
_cod_database_code               7711551
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.240
_shelx_estimated_absorpt_t_min   0.189
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O20-N7 = N7-O18
 1.25 with sigma of 0.02
 O19-N7 = N7-O20
 1.25 with sigma of 0.02
 O18-N7 = N7-O19
 1.25 with sigma of 0.02
 H15A-H23A
 2.1 with sigma of 0.01
 H24A_$1-H22A
 2.11 with sigma of 0.001
 H26A-H9
 2.1 with sigma of 0.01
 O18-O19
 2.165 with sigma of 0.04
 O19-O20
 2.165 with sigma of 0.04
 O20-O18
 2.165 with sigma of 0.04
 Dy1-H14A \\sim Dy1-H14B
 with sigma of 0.02
 O18-O20 \\sim O20-O19
 with sigma of 0.04
 N7-O18 \\sim N7-O20 \\sim N7-O19
 with sigma of 0.02
3. Restrained planarity
 N7, O19, O18, O20
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N7 \\sim O19 \\sim O18 \\sim O20: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O26) \\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O22) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O25(0.5) H25A(0.5) H25B(0.5)
 Fixed X: O23(0.31706) O26(0.56621)
 Fixed Y: O26(0.37594)
 Fixed Z: O26(0.315181)
6.a Riding coordinates:
 O14(H14A,H14B), O1(H1), O22(H22A), O25(H25A,H25B), O24(H24A,H24B), O26(H26A,
 H26B)
6.b Free rotating group:
 O23(H23A,H23B)
6.c Rotating group:
 O15(H15A,H15B), O17(H17A,H17B)
6.d Ternary CH refined with riding coordinates:
 C22(H22), C37(H37), C7(H7)
6.e Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C28(H28), C27(H27), C20(H20), C19(H19), C18(H18),
 C17(H17), C16(H16), C39(H39), C43(H43), C44(H44), C45(H45), C9(H9), C12(H12),
 C5(H5A), C4(H4), C3(H3), C2(H2), C1(H1A), C13(H13), C35(H35), C34(H34),
 C33(H33), C32(H32), C31(H31), C11(H11)
6.f Fitted hexagon refined as free rotating group:
 C26(C25,C30,C29,C28,C27), C21(C20,C19,C18,C17,C16), C40(C41,C42,C43,C44,C45),
 C6(C5,C4,C3,C2,C1), C36(C35,C34,C33,C32,C31)
6.g Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C48(H48A,H48B,
 H48C)
6.h Idealised tetrahedral OH refined as rotating group:
 O5(H5), O21(H21)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 929 electrons were 
found in a volume of 4379\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
9[CH4O], 7[H2O] per Asymmetric Unit 
which account for 928 electrons 
per unit cell.
;
_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
;