Different anion (NO<sub>3</sub><sup>-</sup> and OAc<sup>-</sup>)-controlled construction of dysprosium clusters with different shapes.
Xie, Jia-Nan; Li, Yun-Lan; Wang, Hai-Ling; Xiao, Zi-Xin; Zhu, Zhong-Hong; Liang, Fu-Pei; Zou, Hua-Hong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5665–5675; doi:10.1039/d3dt03314g

data_7715178
_publ_section_title
;
 Different anion (NO<sub>3</sub><sup>-</sup> and
 OAc<sup>-</sup>)-controlled construction of dysprosium clusters with
 different shapes.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5665
_journal_page_last               5675
_journal_paper_doi               10.1039/d3dt03314g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C92 H76 Dy5 N9 O37, C2 H3 N, 0.5[2[CH3CN],20[H2O]]'
_chemical_formula_sum            'C94 H79 Dy5 N10 O37'
_chemical_formula_weight         2753.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-01-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2024-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                101.263(2)
_cell_angle_beta                 98.069(2)
_cell_angle_gamma                97.087(2)
_cell_formula_units_Z            2
_cell_length_a                   16.3885(3)
_cell_length_b                   16.4444(4)
_cell_length_c                   20.8387(5)
_cell_measurement_reflns_used    41691
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      76.3540
_cell_measurement_theta_min      2.7690
_cell_volume                     5387.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_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    -69.00  24.00   0.50    5.00    --  -47.39  74.00   8.00  186
  2  \w   -108.00 -25.00   0.50    5.00    --  -47.39 -74.00-119.00  166
  3  \w    -24.00  32.00   0.50    5.00    --   47.39 -74.00-119.00  112
  4  \w     59.00  93.00   0.50    5.00    --   47.39  74.00   8.00   68
  5  \w   -158.00 -73.00   0.50    5.00    --  -91.75 -74.00-119.00  170
  6  \w    -87.00 -62.00   0.50    5.00    --  -91.75  74.00   8.00   50
  7  \w     86.00 165.00   0.50    5.00    --  108.42  74.00   8.00  158
  8  \w     36.00  77.00   0.50    5.00    --  108.42 -74.00-119.00   82
  9  \w    -31.00   5.00   0.50    5.00    --  -47.39  37.00 -60.00   72
 10  \w   -117.00 -77.00   0.50    5.00    --  -47.39-125.00 -60.00   80
 11  \w    -13.00  26.00   0.50    5.00    --   47.39 -19.00-120.00   78
 12  \w     35.00  88.00   0.50    5.00    --   47.39-125.00 120.00  106
 13  \w    -48.00 -22.00   0.50    5.00    --  -91.75  45.00 -60.00   52
 14  \w    -51.00 -23.00   0.50    5.00    --  -91.75  45.00-180.00   56
 15  \w   -159.00-102.00   0.50    5.00    --  -91.75 -94.00 -60.00  114
 16  \w    -69.00 -27.00   0.50    5.00    --  -91.75  61.00-180.00   84
 17  \w    -56.00 -20.00   0.50    5.00    --  -91.75  61.00-150.00   72
 18  \w    -47.00 -21.00   0.50    5.00    --  -91.75  45.00-150.00   52
 19  \w   -154.00 -77.00   0.50    5.00    --  -91.75 -45.00 -60.00  154
 20  \w    -51.00 -21.00   0.50    5.00    --  -91.75  45.00  30.00   60
 21  \w   -158.00 -78.00   0.50    5.00    --  -91.75 -45.00  90.00  160
 22  \w     42.00  72.00   0.50    5.00    --  108.42 -77.00 120.00   60
 23  \w     38.00  68.00   0.50    5.00    --  108.42 -61.00  60.00   60
 24  \w     70.00 116.00   0.50    5.00    --  108.42-125.00  90.00   92
 25  \w     88.00 117.00   0.50    5.00    --  108.42-125.00  30.00   58
 26  \w     94.00 174.00   0.50    5.00    --  108.42  45.00 -30.00  160
 27  \w     48.00  82.00   0.50    5.00    --  108.42-125.00  30.00   68
 28  \w     40.00  65.00   0.50    5.00    --  108.42-125.00  90.00   50
 29  \w     67.00 106.00   0.50    5.00    --  108.42 -94.00 150.00   78
 30  \w     63.00 116.00   0.50    5.00    --  108.42-125.00 -30.00  106
 31  \w     70.00  98.00   0.50    5.00    --  108.42 -94.00  60.00   56
 32  \w     44.00  71.00   0.50    5.00    --  108.42 -61.00-120.00   54
 33  \w    115.00 178.00   0.50    5.00    --  108.42  30.00 120.00  126
 34  \w     89.00 115.00   0.50    5.00    --  108.42-125.00 -90.00   52
 35  \w     40.00  66.00   0.50    5.00    --  108.42 -94.00  60.00   52
 36  \w     39.00  96.00   0.50    5.00    --  108.42 -94.00-150.00  114
 37  \w    120.00 170.00   0.50    5.00    --  108.42 125.00 120.00  100
 38  \w     58.00 113.00   0.50    5.00    --  108.42-125.00 150.00  110
 39  \w     81.00 106.00   0.50    5.00    --  108.42 -77.00 120.00   50
 40  \w     36.00  69.00   0.50    5.00    --  108.42 -61.00  30.00   66
;
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61467
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         2.757
_exptl_absorpt_coefficient_mu    18.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
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    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             2678
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.273
_refine_diff_density_min         -2.049
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.000185(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         20117
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0702P)^2^+20.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18877
_reflns_number_total             20117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03314g2.cif
_cod_data_source_block           zhh-xjn-a661_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7715177--7715179.cif.'
_cod_database_code               7715178
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.253
_shelx_estimated_absorpt_t_min   0.132
_olex2_refinement_description
;
1. 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
2. Restrained distances
 O36-H36
 0.87 with sigma of 0.01
 O37-H37
 0.87 with sigma of 0.01
 C93-H37
 1.904676 with sigma of 0.02
 Dy2-H36
 3.060526 with sigma of 0.02
 Dy1-H37
 3.049147 with sigma of 0.02
 C94-H36
 1.909063 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N3(H3), C65(H65), C64(H64), C52(H52), C8(H8), C54(H54), C19(H19),
 C4(H4), C74(H74), C69(H69), C5(H5A), C79(H79), C17(H17), C72(H72), C39(H39),
 C35(H35), C27(H27), C18(H18), C63(H63), C3(H3A), C25(H25), C73(H73), C24(H24),
 C33(H33), C26(H26), C71(H71), C80(H80), C12(H12), C11(H11), C22(H22), C34(H34),
  C78(H78), C88(H88), C41(H41), C89(H89), C50(H50), C13(H13), C42(H42),
 C10(H10), C84(H84), C87(H87), C43(H43), C51(H51), C86(H86), C44(H44), C56(H56),
  C59(H59), C58(H58), C57(H57)
3.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C94(H94A,H94B,H94C), C15(H15A,H15B,H15C), C1(H1A,H1B,
 H1C), C29(H29A,H29B,H29C), C93(H93A,H93B,H93C), C46(H46A,H46B,H46C), C76(H76A,
 H76B,H76C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              59417
_shelx_fab_checksum              47198
_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
;