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_7715179
_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
'C167 H171 Dy14 N7 O91, 7(H2 O), 23[C2H3N], 23[H2O], 1[C2H3N], 1[H2O], 0.75[]'
_chemical_formula_sum            'C215 H305 Dy14 N31 O122'
_chemical_formula_weight         7550.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-01-03
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.12.20 svn.rf89b8cd1 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2024-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3873(3)
_cell_length_b                   27.8871(5)
_cell_length_c                   38.2827(5)
_cell_measurement_reflns_used    92635
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      59.9100
_cell_measurement_theta_min      1.9020
_cell_volume                     28152.1(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (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      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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    -30.00  36.00   0.50    0.75    --   -1.09 -94.00 -76.00  132
  2  \w    -38.00  30.00   0.50    0.75    --   -1.09  94.00  33.00  136
  3  \w     84.00 149.00   0.50    3.80    --   75.54  94.00  33.00  130
  4  \w      2.00 106.00   0.50    3.80    --   75.54 -94.00 -76.00  208
  5  \w   -151.00 -84.00   0.50    3.80    --  -77.72 -94.00 -76.00  134
  6  \w   -106.00  -4.00   0.50    3.80    --  -77.72  94.00  33.00  204
  7  \w     -8.00  37.00   0.50    0.75    --   -1.09 -99.00 150.00   90
  8  \w     -8.00  37.00   0.50    0.75    --   -1.09 -99.00  30.00   90
  9  \w     -8.00  37.00   0.50    0.75    --   -1.09 -99.00-120.00   90
 10  \w     -8.00  37.00   0.50    0.75    --   -1.09 -99.00-150.00   90
 11  \w     -8.00  37.00   0.50    0.75    --   -1.09 -99.00-180.00   90
 12  \w     -8.00  37.00   0.50    0.75    --   -1.09 -99.00 120.00   90
 13  \w      1.00  96.00   0.50    3.80    --   75.54 -57.00-180.00  190
 14  \w     79.00 147.00   0.50    3.80    --   75.54 125.00 120.00  136
 15  \w     79.00 147.00   0.50    3.80    --   75.54 125.00  60.00  136
 16  \w     47.00 150.00   0.50    3.80    --   75.54  77.00 -60.00  206
 17  \w     53.00 150.00   0.50    3.80    --   75.54  57.00   0.00  194
 18  \w   -151.00-103.00   0.50    3.80    --  -77.72 -99.00-120.00   96
 19  \w   -145.00-119.00   0.50    3.80    --  -77.72 -99.00-180.00   52
 20  \w    -31.00  -1.00   0.50    3.80    --  -77.72  38.00-120.00   60
 21  \w    -70.00 -45.00   0.50    3.80    --  -77.72  38.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.2983
_diffrn_reflns_av_unetI/netI     0.1457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            290267
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.199
_diffrn_reflns_theta_min         2.008
_exptl_absorpt_coefficient_mu    19.748
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (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    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             14848
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         8.978
_refine_diff_density_min         -6.647
_refine_diff_density_rms         0.554
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.695
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2764
_refine_ls_number_reflns         62206
_refine_ls_number_restraints     4517
_refine_ls_restrained_S_all      1.682
_refine_ls_R_factor_all          0.2147
_refine_ls_R_factor_gt           0.1815
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4466
_refine_ls_wR_factor_ref         0.4694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                41408
_reflns_number_total             62206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03314g2.cif
_cod_data_source_block           cgh-dy_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7715177--7715179.cif.'
_cod_database_code               7715179
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.243
_shelx_estimated_absorpt_t_min   0.243
_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 C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H95B-O94
 1 with sigma of 0.1
 H89A-O95
 1 with sigma of 0.1
 O65-H89B
 1 with sigma of 0.1
 H93B-O31
 1 with sigma of 0.1
 H93A-O92
 1 with sigma of 0.1
 H94A-O93
 1 with sigma of 0.1
 H90B-O89
 1 with sigma of 0.1
 H94B-O40
 1 with sigma of 0.1
 O64-C04W \\sim O64A-C3
 with sigma of 0.02
 O60-C04O \\sim O60A-C1
 with sigma of 0.02
 O51-C07F \\sim O51A-C07G
 with sigma of 0.02
 C04W-C066 \\sim C3-C4
 with sigma of 0.02
 N5-C059 \\sim N5A-C0
 with sigma of 0.02
 N5-C082 \\sim N5A-C7
 with sigma of 0.02
 C059-C06W \\sim C0-C5
 with sigma of 0.02
 O46-C07S \\sim O46A-C07T
 with sigma of 0.02
 O46-C07R \\sim O46A-C9
 with sigma of 0.02
 C066-C07W \\sim C4-C07X
 with sigma of 0.02
 C06W-C07W \\sim C5-C07X
 with sigma of 0.02
 C082-C69 \\sim C7-C69A
 with sigma of 0.02
 C235-C07R \\sim C2-C9
 with sigma of 0.02
 C235-CXF \\sim C2-CXG
 with sigma of 0.02
 C07R-C07F \\sim C9-C07G
 with sigma of 0.02
 C07F-C69 \\sim C07G-C69A
 with sigma of 0.02
 C69-CXE \\sim C69A-C8
 with sigma of 0.02
 CXE-CXF \\sim C8-CXG
 with sigma of 0.02
 O64-C066 \\sim O64A-C4
 with sigma of 0.04
 O51-C07R \\sim O51A-C9
 with sigma of 0.04
 O51-C69 \\sim O51A-C69A
 with sigma of 0.04
 C04O-C04W \\sim C1-C3
 with sigma of 0.04
 C04O-C059 \\sim C1-C0
 with sigma of 0.04
 C04W-C059 \\sim C3-C0
 with sigma of 0.04
 C04W-C07W \\sim C3-C07X
 with sigma of 0.04
 N5-C06W \\sim N5A-C5
 with sigma of 0.04
 N5-C69 \\sim N5A-C69A
 with sigma of 0.04
 C059-C07W \\sim C0-C07X
 with sigma of 0.04
 C059-C082 \\sim C0-C7
 with sigma of 0.04
 O46-C235 \\sim O46A-C2
 with sigma of 0.04
 O46-C07F \\sim O46A-C07G
 with sigma of 0.04
 C066-C06W \\sim C4-C5
 with sigma of 0.04
 C07S-C07R \\sim C07T-C9
 with sigma of 0.04
 C082-C07F \\sim C7-C07G
 with sigma of 0.04
 C082-CXE \\sim C7-C8
 with sigma of 0.04
 C235-C07F \\sim C2-C07G
 with sigma of 0.04
 C235-CXE \\sim C2-C8
 with sigma of 0.04
 C07R-C69 \\sim C9-C69A
 with sigma of 0.04
 C07R-CXF \\sim C9-CXG
 with sigma of 0.04
 C07F-CXE \\sim C07G-C8
 with sigma of 0.04
 C69-CXF \\sim C69A-CXG
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C5 \\sim C2 \\sim C9 \\sim CXG \\sim C07G \\sim O46A \\sim C8 \\sim C69A \\sim
O51A \\sim C07T \\sim C7 \\sim N5A \\sim C0 \\sim C1 \\sim C3 \\sim C07X \\sim
O55A \\sim O60A \\sim C4 \\sim O64A \\sim C059 \\sim C04O \\sim O60 \\sim C03X
\\sim C04W \\sim C066 \\sim O64 \\sim N5 \\sim C06W \\sim C07W \\sim C06V \\sim
C082 \\sim C69 \\sim C07F \\sim CXE \\sim O51 \\sim C07R \\sim CXF \\sim O46
\\sim C235 \\sim C07S: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(C04Y) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(C053) \\sim Ueq, Uanis(C04D)
\\sim Ueq, Uanis(C04F) \\sim Ueq, Uanis(C068) \\sim Ueq, Uanis(O34) \\sim Ueq,
Uanis(C06X) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C07Q) \\sim Ueq, Uanis(C040)
\\sim Ueq, Uanis(C055) \\sim Ueq, Uanis(C05H) \\sim Ueq, Uanis(C05N) \\sim Ueq,
Uanis(C076) \\sim Ueq, Uanis(C05U) \\sim Ueq, Uanis(C05W) \\sim Ueq,
Uanis(C06L) \\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O45)
\\sim Ueq, Uanis(C074) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C03M) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Dy1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Sof(HH)=Sof(HI)=Sof(HJ)=Sof(C2)=Sof(H2A)=Sof(C9)=Sof(C07G)=Sof(C69A)=Sof(C8)=
 Sof(H8A)=Sof(CXG)=Sof(HXG)=Sof(C1)=Sof(O60A)=Sof(C3)=Sof(C0)=Sof(C4)=Sof(H4A)=
 Sof(O64A)=Sof(N5A)=Sof(C5)=Sof(H5A)=Sof(C07X)=Sof(H14)=Sof(C7)=Sof(H7A)=
 Sof(O51A)=Sof(O46A)=Sof(C07T)=Sof(H15)=Sof(HP)=Sof(HQ)=1-FVAR(1)
 Sof(O64)=Sof(O60)=Sof(O51)=Sof(C04O)=Sof(C04W)=Sof(N5)=Sof(C059)=Sof(O46)=
 Sof(C066)=Sof(H066)=Sof(H8)=Sof(HK)=Sof(HL)=Sof(C06W)=Sof(H9)=Sof(C07S)=
 Sof(H11)=Sof(HN)=Sof(HO)=Sof(C07W)=Sof(H13)=Sof(C082)=Sof(H082)=Sof(C235)=
 Sof(H235)=Sof(C07R)=Sof(C07F)=Sof(C69)=Sof(CXE)=Sof(HXE)=Sof(CXF)=Sof(HXF)=
 FVAR(1)
6.a Riding coordinates:
 O91(H91A,H91B), O90(H90A,H90B), O93(H93A,H93B), O94(H94A,H94B), O95(H95A,
 H95B), O92(H92A,H92B), O89(H89A,H89B)
6.b Me refined with riding coordinates:
 C06V(HH,HI,HJ), C06V(H8,HK,HL)
6.c Aromatic/amide H refined with riding coordinates:
 C03E(H03G), C03M(H03M), C03S(H03U), C03V(H03V), C048(H048), C04I(H04M),
 C04L(H04Q), C04V(H04V), C04Y(H04Y), C05C(H05D), C05E(H05E), C05F(H05F),
 C05H(H05J), C05V(H05Z), C064(H064), C066(H066), C068(H068), C06E(H06S),
 C06F(H06T), C06G(H06U), C06L(H06), C06M(H2), C06N(H3), C06P(H4), C06R(H5),
 C06T(H6), C06U(H7), C06W(H9), C06X(H10), C076(H076), C079(H079), C07B(H07M),
 C07D(H07N), C07K(H07R), C07M(H07V), C07N(H07W), C07P(H07Z), C07Q(H07),
 C07U(H12), C07W(H13), C082(H082), C087(H087), C088(H088), C87(H87), C73(H73),
 C235(H235), CXE(HXE), CXF(HXF), C2(H2A), C8(H8A), CXG(HXG), C4(H4A), C5(H5A),
 C07X(H14), C7(H7A)
6.d Fitted hexagon refined as free rotating group:
 C235(C07R,C07F,C69,CXE,CXF), C2(C9,C07G,C69A,C8,CXG)
6.e Idealised Me refined as rotating group:
 C03B(H03A,H03B,H03C), C03C(H03D,H03E,H03F), C03I(H03H,H03I,H03J), C03N(H03K,
 H03L,H03N), C03P(H03O,H03P,H03Q), C03Q(H03R,H03S,H03T), C040(H04A,H04B,H04C),
 C043(H04D,H04E,H04F), C045(H04G,H04H,H04I), C049(H04J,H04K,H04L), C04K(H04N,
 H04O,H04P), C04Q(H04R,H04S,H04T), C058(H05A,H05B,H05C), C05G(H05G,H05H,H05I),
 C05J(H05K,H05L,H05M), C05K(H05N,H05O,H05P), C05M(H05Q,H05R,H05S), C05O(H05T,
 H05U,H05V), C05S(H05W,H05X,H05Y), C05X(H05,H,HA), C05Y(H1,HB,HC), C061(H06A,
 H06B,H06C), C062(H06D,H06E,H06F), C065(H06G,H06H,H06I), C069(H06J,H06K,H06L),
 C06A(H06M,H06N,H06O), C06C(H06P,H06Q,H06R), C06I(H06V,H06W,H06X), C06J(H06Y,HD,
 HE), C06K(H06Z,HF,HG), C070(H07A,H07B,H07C), C073(H07D,H07E,H07F), C074(H07G,
 H07H,H07I), C077(H07J,H07K,H07L), C07J(H07O,H07P,H07Q), C07L(H07S,H07T,H07U),
 C07O(H07X,H07Y,HM), C07S(H11,HN,HO), C08J(H08A,H08B,H08C), C60(H60A,H60B,H60C),
  C07T(H15,HP,HQ)
;
_shelx_res_checksum              80551
_shelx_fab_checksum              42406
_platon_squeeze_special_details
;
A solvent mask was calculated and 3063 electrons were 
found in a volume of 10935\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 23[C2H3N], 23[H2O],
1[C2H3N], 1[H2O], per Asymmetric Unit which account for 3072
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
;