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_7709055
_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         '4(C62 H84 Dy7 N17 O35), 8(Cl)'
_chemical_formula_sum            'C260 H388 Cl8 Dy28 N74 O157'
_chemical_formula_weight         11896.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-11-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-21 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4542(18)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   24.1218(4)
_cell_length_b                   19.51008(19)
_cell_length_c                   22.0893(3)
_cell_measurement_reflns_used    13383
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1290
_cell_measurement_theta_min      2.9400
_cell_volume                     10019.8(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.939
_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    -14.00  58.00   0.50    2.50    --   46.87 -53.00  -6.00  144
  2  \w     44.00  70.00   0.50    8.00    --  108.56 -61.00 120.00   52
  3  \w     40.00  71.00   0.50    8.00    --  108.56 -61.00  30.00   62
  4  \w     36.00  61.00   0.50    8.00    --  108.56 -61.00   0.00   50
  5  \w     43.00 104.00   0.50    8.00    --  108.56 -94.00 -60.00  122
  6  \w     77.00 105.00   0.50    8.00    --  108.56 -77.00 -60.00   56
  7  \w     36.00  62.00   0.50    8.00    --  108.56 -61.00-150.00   52
  8  \w     37.00  63.00   0.50    8.00    --  108.56 -61.00-120.00   52
  9  \w     36.00  69.00   0.50    8.00    --  108.56 -77.00 -60.00   66
 10  \w     38.00  65.00   0.50    8.00    --  108.56 -61.00 -30.00   54
 11  \w     39.00  69.00   0.50    8.00    --  108.56 -61.00 -60.00   60
 12  \w     97.00 139.00   0.50    8.00    --  108.56  45.00  60.00   84
 13  \w    141.00 173.00   0.50    8.00    --  108.56  45.00  60.00   64
 14  \w    140.00 177.00   0.50    8.00    --  108.56  45.00  90.00   74
 15  \w     95.00 121.00   0.50    8.00    --  108.56  53.00 138.00   52
 16  \w    104.00 129.00   0.50    8.00    --  108.56  45.00  90.00   50
 17  \w     52.00  77.00   0.50    2.50    --   46.87  53.00 138.00   50
 18  \w    -60.00  25.00   0.50    2.50    --  -46.87  53.00 138.00  170
 19  \w    -55.00 -15.00   0.50    8.00    --  -88.50  53.00 138.00   80
 20  \w    -50.00 -16.00   0.50    8.00    --  -88.50  45.00 120.00   68
 21  \w    -49.00 -16.00   0.50    8.00    --  -88.50  45.00  60.00   66
 22  \w    -51.00 -26.00   0.50    8.00    --  -88.50  45.00 -60.00   50
 23  \w    -66.00 -21.00   0.50    8.00    --  -88.50  61.00 -60.00   90
 24  \w    -55.00 -18.00   0.50    8.00    --  -88.50 125.00-150.00   74
 25  \w    -86.00 -60.00   0.50    8.00    --  -88.50 125.00-150.00   52
 26  \w   -119.00 -36.00   0.50    2.50    --  -46.87 -53.00  -6.00  166
 27  \w   -115.00 -86.00   0.50    2.50    --  -46.87-125.00 150.00   58
 28  \w   -160.00 -90.00   0.50    8.00    --  -88.50 -53.00  -6.00  140
 29  \w   -116.00 -91.00   0.50    2.50    --  -46.87-125.00-150.00   50
 30  \w   -157.00 -98.00   0.50    8.00    --  -88.50 -94.00  90.00  118
;
_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      -0.0026192000
_diffrn_orient_matrix_UB_12      0.0208210000
_diffrn_orient_matrix_UB_13      -0.0679796000
_diffrn_orient_matrix_UB_21      0.0532705000
_diffrn_orient_matrix_UB_22      0.0458727000
_diffrn_orient_matrix_UB_23      0.0242715000
_diffrn_orient_matrix_UB_31      0.0393000000
_diffrn_orient_matrix_UB_32      -0.0608188000
_diffrn_orient_matrix_UB_33      -0.0049739000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37561
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.182
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    28.640
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60748
_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            yellow
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_description       block
_exptl_crystal_F_000             5706
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.717
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9976
_refine_ls_number_restraints     1481
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0655P)^2^+99.5197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7939
_reflns_number_total             9976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03137f2.cif
_cod_data_source_block           20200711-lfp-lj-404
_cod_depositor_comments
'Adding full bibliography for 7709053--7709055.cif.'
_cod_original_cell_volume        10019.7(3)
_cod_database_code               7709055
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Dy Cl'
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.489
_diffrn_oxdiff_digest_frames
;
017a23af0f65f6609904cd0249a4c1e80a00026448d
;
_diffrn_oxdiff_digest_hkl
;
01ae87a65a0078709f72ebf0d3c67feca10dab
;
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H3 of O3, H2 of O2, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H11 of O11, H12 of O12, All O(H,H) groups
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 O12-H12
 0.85 with sigma of 0.01
 C30-H11
 1.856027 with sigma of 0.02
 Dy4-H11
 2.850602 with sigma of 0.02
 Dy3-H12
 2.971193 with sigma of 0.02
 C31-H12
 1.924662 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Riding coordinates:
 C31(H31A,H31B,H31C), O23(H23A,H23B)
5.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3), C12(H12A)
5.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C26(H26A,H26B)
5.d Aromatic/amide H refined with riding coordinates:
 N6(H6), C1(H1), C2(H2A), C7(H7), C10(H10), C11(H11A), C13(H13), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
5.e Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              54088
_shelx_hkl_checksum              73608
_shelx_fab_checksum              98122
_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 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.766