Truncation reaction regulates the out-to-in growth mechanism to decrypt the formation of brucite-like dysprosium clusters.
Li, Yun-Lan; Wang, Hai-Ling; Zhu, Zhong-Hong; Li, Juan; Zou, Hua-Hong; Peng, Jin-Mei; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 51 (2021) 197–202; doi:10.1039/d1dt03137f

data_7709054
_publ_section_title
;
 Truncation reaction regulates the out-to-in growth mechanism to decrypt
 the formation of brucite-like dysprosium clusters.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              197
_journal_page_last               202
_journal_paper_doi               10.1039/d1dt03137f
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety
'C51 H64.69 Cl2.358 Dy7.997 N13.654 O28.95, 13[CH4O]'
_chemical_formula_sum            'C64 H116.69 Cl2.36 Dy8 N13.65 O41.95'
_chemical_formula_weight         3132.36
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-11-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-11-21 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   31.8024(5)
_cell_length_b                   31.8024(5)
_cell_length_c                   32.0143(7)
_cell_measurement_reflns_used    22141
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6310
_cell_measurement_theta_min      2.3010
_cell_volume                     28041.1(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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    'XT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -12.00  84.00   0.50   40.00    --   10.14  59.00-144.00  192
  2  \w    -23.00  16.00   0.50   40.00    --   10.14 -99.00  60.00   78
  3  \w    -23.00  29.00   0.50   40.00    --   -9.28 -99.00 150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            40405
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.334
_exptl_absorpt_coefficient_mu    6.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_description       block
_exptl_crystal_F_000             18000
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.516
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5506
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0421P)^2^+926.8146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4671
_reflns_number_total             5506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03137f2.cif
_cod_data_source_block           20201012-lfp-lj-460_sq
_cod_depositor_comments
'Adding full bibliography for 7709053--7709055.cif.'
_cod_original_cell_volume        28041.1(11)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7709054
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Shared sites
{Cl1, O12}
{Cl2, O13}
3. Restrained distances
 N5-O8 = N5-O11
 1.25 with sigma of 0.02
 N5-O10
 1.24 with sigma of 0.02
 N5-O8 \\sim N5-O10 \\sim N5-O11
 with sigma of 0.02
 O8-O10 \\sim O10-O11 \\sim O11-O8
 with sigma of 0.04
4. Restrained planarity
 N5, O8, O10, O11
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
N5 \\sim O8 \\sim O10 \\sim O11: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl1) = Uanis(O12)
Uanis(Cl2) = Uanis(O13)
6. Rigid body (RIGU) restrains
 N5, O8, O10, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O2)=Sof(N5)=Sof(O8)=Sof(O11)=1-FVAR(1)
 Sof(O6)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(O12)=Sof(H12A)=Sof(H12B)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
 Sof(H13A)=Sof(H13B)=1-FVAR(3)
 Sof(O13)=0.33333*(1-FVAR(4))
 Sof(Cl2)=0.33333*FVAR(4)
8.a Riding coordinates:
 O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B)
8.b Rotating group:
 O9(H9A,H9B)
8.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C14(H14A,H14B)
8.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C9(H9), C7(H7), C4(H4), C10(H10), C2(H2), C3(H3)
8.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              49582
_shelx_hkl_checksum              3216
_shelx_fab_checksum              64696
_platon_squeeze_special_details
;
A solvent mask was calculated and 2790 electrons were 
found in a volume of 8907\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 13[CH4O] per Formula Unit 
which account for 2808 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
;