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_7711549
_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 H92 Dy6 N12 O34, 2(N O3), 2(C H4 O), 11[CH4O], 15[H2O]'
_chemical_formula_sum            'C107 H174 Dy6 N14 O68'
_chemical_formula_weight         3719.59
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.40060(10)
_cell_length_b                   14.40060(10)
_cell_length_c                   71.4120(5)
_cell_measurement_reflns_used    28284
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9430
_cell_measurement_theta_min      3.1240
_cell_volume                     14809.23(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.979
_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    -97.00 -13.00   0.25    4.00    --  -43.18 -12.00 103.00  336
  2  \w   -127.00-102.00   0.25   14.00    --  -90.25 -12.00 103.00  100
  3  \w    105.00 142.00   0.25   14.00    --  109.26  12.00 -84.00  148
  4  \w     50.00 100.00   0.25   14.00    --  109.26  12.00 -84.00  200
  5  \w    -85.00 -13.00   0.25    4.00    --  -43.18 125.00   0.00  288
  6  \w    -31.00  -6.00   0.25    4.00    --   43.18 -12.00 103.00  100
  7  \w    -51.00 -14.00   0.25   14.00    --  -90.25  45.00-180.00  148
  8  \w    -51.00 -14.00   0.25   14.00    --  -90.25  45.00  60.00  148
  9  \w     35.00  71.00   0.25   14.00    --  109.26 -61.00  60.00  144
 10  \w     71.00 111.00   0.25   14.00    --  109.26-125.00  30.00  160
 11  \w     35.00  69.00   0.25   14.00    --  109.26 -61.00-150.00  136
 12  \w     37.00  63.00   0.25   14.00    --  109.26 -94.00 -30.00  104
 13  \w     38.00  99.00   0.25   14.00    --  109.26-125.00   0.00  244
 14  \w     35.00  69.00   0.25   14.00    --  109.26 -61.00 -30.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0415875000
_diffrn_orient_matrix_UB_12      -0.0972233000
_diffrn_orient_matrix_UB_13      -0.0033024000
_diffrn_orient_matrix_UB_21      -0.0984735000
_diffrn_orient_matrix_UB_22      -0.0416672000
_diffrn_orient_matrix_UB_23      -0.0005128000
_diffrn_orient_matrix_UB_31      -0.0041697000
_diffrn_orient_matrix_UB_32      0.0160578000
_diffrn_orient_matrix_UB_33      -0.0213096000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -88
_diffrn_reflns_number            52013
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.826
_diffrn_reflns_theta_min         2.475
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             7416
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         14821
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+10.0654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                12624
_reflns_number_total             14821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02653h2.cif
_cod_data_source_block           20221013-lfp-lbf-101212_auto
_cod_original_cell_volume        14809.2(2)
_cod_database_code               7711549
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Dy '
_shelx_estimated_absorpt_t_max   0.239
_shelx_estimated_absorpt_t_min   0.203
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.985(5)
 0.015(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(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
 O5-H5
 0.87 with sigma of 0.01
 O16-H16
 0.87 with sigma of 0.01
 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
 O21-C48
 1.3 with sigma of 0.02
 C22-H5
 1.913578 with sigma of 0.02
 C47-H16
 1.919339 with sigma of 0.02
 Dy3-H16
 2.996415 with sigma of 0.02
 Dy1-H5
 3.076928 with sigma of 0.02
 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
 O18-O20 \\sim O20-O19
 with sigma of 0.04
 N7-O18 \\sim N7-O20 \\sim N7-O19
 with sigma of 0.02
4. Restrained planarity
 N7, O19, O18, O20
 with sigma of 0.1
5. 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(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O18)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Riding coordinates:
 N1(H1)
6.b Rotating group:
 O15(H15A,H15B), O17(H17A,H17B)
6.c Ternary CH refined with riding coordinates:
 C37(H37), C7(H7)
6.d Aromatic/amide H refined with riding coordinates:
 N5(H5A), C24(H24), C26(H26), C27(H27), C13(H13), C28(H28), C41(H41), C9(H9),
 C39(H39), C43(H43), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C12(H12),
  C16(H16A), C1(H1B), C42(H42), C17(H17), C11(H11), C19(H19), C18(H18), C5(H5B),
  C20(H20), C4(H4), C3(H3), C2(H2)
6.e Fitted hexagon refined as free rotating group:
 C31(C32,C33,C34,C35,C36)
6.f Tetrahedral OH refined with riding coordinates:
 O21(H21)
6.g X=CH2 refined with riding coordinates:
 O14(H14A,H14B)
6.h Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
6.i Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              29319
_shelx_hkl_checksum              31946
_shelx_fab_checksum              47549
_platon_squeeze_special_details
;
A solvent mask was calculated and 1395 electrons were 
found in a volume of 4989\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
11[CH4O], 15[H2O] per Asymmetric Unit 
which account for 1392 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
;
_oxdiff_exptl_absorpt_empirical_full_max 39.595
_oxdiff_exptl_absorpt_empirical_full_min 0.376