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_7715177
_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         'C98 H88 Dy8 N10 O52, 0.5[12[CH3CN]2[H2O]]'
_chemical_formula_sum            'C98 H88 Dy8 N10 O52'
_chemical_formula_weight         3537.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-01-30
_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                90
_cell_angle_beta                 93.4290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.39970(10)
_cell_length_b                   27.4462(2)
_cell_length_c                   16.60710(10)
_cell_measurement_reflns_used    31195
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.3490
_cell_measurement_theta_min      3.1120
_cell_volume                     6096.67(7)
_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 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 0.998
_diffrn_measured_fraction_theta_max 0.956
_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    -63.00  31.00   0.50    1.50    --  -43.70  55.00 122.00  188
  2  \w   -117.00 -22.00   0.50    1.50    --  -43.70 -55.00 -20.00  190
  3  \w    -29.00  63.00   0.50    1.50    --   43.70 -55.00 -20.00  184
  4  \w   -170.00 -74.00   0.50    3.50    --  -96.00 -55.00 -20.00  192
  5  \w    -63.00 -22.00   0.50    3.50    --  -96.00  55.00 122.00   82
  6  \w     88.00 178.00   0.50    3.50    --  109.23  55.00 122.00  180
  7  \w     35.00  63.00   0.50    3.50    --  109.23 -55.00 -20.00   56
  8  \w    -36.00  27.00   0.50    1.50    --   43.70 -19.00-180.00  126
  9  \w     34.00  97.00   0.50    1.50    --   43.70-125.00-180.00  126
 10  \w    -71.00 -22.00   0.50    3.50    --  -96.00  61.00-150.00   98
 11  \w    -51.00 -20.00   0.50    3.50    --  -96.00  45.00  90.00   62
 12  \w    -51.00 -20.00   0.50    3.50    --  -96.00  45.00-120.00   62
 13  \w    -86.00 -22.00   0.50    3.50    --  -96.00 125.00-150.00  128
 14  \w    -51.00 -20.00   0.50    3.50    --  -96.00  45.00 -60.00   62
 15  \w   -170.00 -72.00   0.50    3.50    --  -96.00 -61.00 -60.00  196
 16  \w    -51.00 -20.00   0.50    3.50    --  -96.00  45.00 -30.00   62
 17  \w    -71.00 -22.00   0.50    3.50    --  -96.00  61.00-120.00   98
 18  \w    -51.00 -20.00   0.50    3.50    --  -96.00  45.00-150.00   62
 19  \w    -86.00 -22.00   0.50    3.50    --  -96.00 125.00-180.00  128
 20  \w     86.00 178.00   0.50    3.50    --  109.23  30.00 -90.00  184
 21  \w     95.00 178.00   0.50    3.50    --  109.23 125.00-180.00  166
 22  \w     36.00 105.00   0.50    3.50    --  109.23 -94.00 -30.00  138
 23  \w     36.00 105.00   0.50    3.50    --  109.23 -94.00 -60.00  138
 24  \w     35.00  60.00   0.50    3.50    --  109.23 -61.00-150.00   50
 25  \w     97.00 178.00   0.50    3.50    --  109.23 125.00 150.00  162
;
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.730
_diffrn_reflns_theta_min         3.114
_exptl_absorpt_coefficient_mu    26.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59441
_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    1.927
_exptl_crystal_description       block
_exptl_crystal_F_000             3380
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         12123
_refine_ls_number_restraints     1056
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0424P)^2^+31.9563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11624
_reflns_number_total             12123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03314g2.cif
_cod_data_source_block           xjn-20230607-14a2q8_auto
_cod_depositor_comments
'Adding full bibliography for 7715177--7715179.cif.'
_cod_database_code               7715177
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.258
_shelx_estimated_absorpt_t_min   0.226
_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,H) groups
2. Rigid bond restraints
 C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim C15 \\sim C22 \\sim C3 \\sim C6 \\sim C39 \\sim C5 \\sim C47 \\sim C4
\\sim C44 \\sim C41 \\sim C36 \\sim C46 \\sim C38 \\sim C2 \\sim C24 \\sim C23
\\sim C40 \\sim C10 \\sim C11 \\sim C42 \\sim C21 \\sim C48 \\sim C33 \\sim C30
\\sim C45 \\sim C7 \\sim C20 \\sim C34 \\sim C37 \\sim C14 \\sim C9 \\sim C13
\\sim C25 \\sim C16 \\sim C19 \\sim C17 \\sim C26 \\sim C1 \\sim C18 \\sim C43
\\sim C29 \\sim C12 \\sim C35 \\sim C27 \\sim C49 \\sim C28 \\sim C50 \\sim
C32: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C49) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C50) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) = Uanis(C7)
Uanis(C4) = Uanis(C40)
Uanis(C3) = Uanis(C11)
4.a Riding coordinates:
 O18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C5(H5), C44(H44), C36(H36), C24(H24), C40(H40), C42(H42),
 C21(H21), C7(H7), C20(H20), C37(H37), C14(H14), C13(H13), C19(H19), C26(H26),
 C43(H43), C12(H12), C35(H35), C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C1(H1A,H1B,
 H1C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C32(H32A,H32B,H32C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 290 electrons were
found in a volume of 1222\%A^3 in 1 void per unit cell.
This is consistent with the presence of 
1[6[CH3CN]1[H2O]] per Unit Cell 
which account for 49 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47730
_shelx_fab_checksum              89089
_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
;