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_7709053
_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
'2(C82 H116 Cl4 Dy6 N16 O22), 2(C H4 O), 4(C2 H3 N), 7(H2 O), 4(Cl)'
_chemical_formula_sum            'C174 H266 Cl12 Dy12 N36 O53'
_chemical_formula_weight         6085.61
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.181(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   15.4667(3)
_cell_length_b                   26.7576(4)
_cell_length_c                   16.1721(4)
_cell_measurement_reflns_used    31294
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.5580
_cell_measurement_theta_min      2.3350
_cell_volume                     6152.5(2)
_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    'XT (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.812
_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    -31.00   4.00   0.50    6.00    --   10.14 -19.00 -60.00   70
  2  \w     -9.00  19.00   0.50    6.00    --   -9.28 -99.00 -90.00   56
  3  \w     12.00  60.00   0.50    6.00    --   10.14-117.00-147.00   96
  4  \w     35.00  60.00   0.50    6.00    --   10.14-161.00  61.00   50
  5  \w    -22.00  30.00   0.50    6.00    --   10.14 -99.00  60.00  104
  6  \w    -20.00  30.00   0.50    6.00    --   -9.28 -99.00  90.00  100
  7  \w    -70.00   3.00   0.50    6.00    --   10.14 -19.00 -90.00  146
;
_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      0.0003307000
_diffrn_orient_matrix_UB_12      -0.0062237000
_diffrn_orient_matrix_UB_13      0.0427915000
_diffrn_orient_matrix_UB_21      -0.0077368000
_diffrn_orient_matrix_UB_22      -0.0254532000
_diffrn_orient_matrix_UB_23      -0.0130672000
_diffrn_orient_matrix_UB_31      0.0492517000
_diffrn_orient_matrix_UB_32      -0.0039655000
_diffrn_orient_matrix_UB_33      0.0166858000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.812
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53113
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.648
_diffrn_reflns_theta_min         2.090
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59009
_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    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         15438
_refine_ls_number_restraints     1588
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+11.5859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12744
_reflns_number_total             15438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03137f2.cif
_cod_data_source_block           20201011-lfp-lj-4021
_cod_depositor_comments
'Adding full bibliography for 7709053--7709055.cif.'
_cod_database_code               7709053
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_digest_frames
;
01c09b0d4222403f8d46308d46235051b9000254f97
;
_diffrn_oxdiff_digest_hkl
;
01182b74182b9b4d999c1b310e67f80af992ae
;
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H,H)
  groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, H11 of O11, H12 of O12, All O(H,H) groups
2. Restrained distances
 O12-C46
 1.45 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 O11-H11
 0.85 with sigma of 0.01
 C47-C38 = C41-C38
 1.46 with sigma of 0.01
 N10-C1AA = N9-C42
 1.15 with sigma of 0.01
 C45-C1AA = C43-C42
 1.46 with sigma of 0.01
 C33-H11
 1.971364 with sigma of 0.02
 Dy2-H8
 2.917456 with sigma of 0.02
 Dy3-H11
 3.120902 with sigma of 0.02
 C12-H8
 1.902208 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. Others
 Sof(N10)=Sof(C1AA)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=1-FVAR(1)
 Sof(N9)=Sof(C42)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
 Sof(H38C)=Sof(H38D)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=1-FVAR(2)
 Sof(H38A)=Sof(H38B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(2)
 Fixed Sof: O12(0.5) H12(0.5) O13(0.5) H13A(0.5) H13B(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) O14(0.5) H14A(0.5) H14B(0.5) O15(0.25) H15A(0.25)
 H15B(0.25) O16(0.25) H16A(0.25) H16B(0.25) O17(0.25) H17A(0.25) H17B(0.25)
6.a Riding coordinates:
 O10(H10A,H10B), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C), O13(H13A,H13B),
 C47(H47A,H47B,H47C), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O17(H17A,
 H17B)
6.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3), N6(H6)
6.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C28(H28A,H28B), C38(H38A,H38B), C38(H38C,H38D), C40(H40A,H40B)
6.d Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C39(H39A,H39B,
 H39C), C43(H43A,H43B,H43C)
6.e Aromatic/amide H refined with riding coordinates:
 N3(H3A), N5(H5), C1(H1), C8(H8A), C11(H11A), C14(H14), C16(H16), C19(H19),
 C20(H20), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C31(H31), C35(H35)
6.f Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C46(H46A,H46B,H46C)
6.g Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_shelx_res_checksum              1035
_shelx_hkl_checksum              34015
_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 1.477
_oxdiff_exptl_absorpt_empirical_full_min 0.827