Two pairs of chiral lanthanide–oxo clusters Ln14 induced by amino acid derivatives
Lu, Tian-Qi; Yin, Jia-Jia; Chen, Cheng; Shi, Hai-Yan; Zheng, Jun; Liu, Zhengjie; Fang, Xiaolong; Zheng, Xiu-Ying; CrystEngComm 23 (2021) 6923–6929; doi:10.1039/D1CE00948F

data_7243419
_publ_section_title
;
 Two pairs of chiral lanthanide--oxo clusters Ln14 induced by amino acid
 derivatives
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              6923
_journal_page_last               6929
_journal_paper_doi               10.1039/D1CE00948F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C80 H112 Dy14 N16 O84, 6(Cl O4)'
_chemical_formula_sum            'C80 H318 Cl10 Dy14 N16 O191'
_chemical_formula_weight         7190.98
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-18 deposited with the CCDC.	2021-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.0353(11)
_cell_length_b                   31.0353(11)
_cell_length_c                   31.3981(12)
_cell_measurement_reflns_used    36660
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.77
_cell_measurement_theta_min      4.01
_cell_volume                     30242.3(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1250
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32609
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.708
_diffrn_reflns_theta_min         4.006
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    19.819
_exptl_absorpt_correction_T_max  0.0921
_exptl_absorpt_correction_T_min  0.0062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14128
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.673
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.228
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.108(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         13871
_refine_ls_number_restraints     544
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0976
_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^)+(0.1941P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2507
_refine_ls_wR_factor_ref         0.2673
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                11350
_reflns_number_total             13871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00948f2.cif
_cod_data_source_block           D-Dy14
_cod_depositor_comments
'Adding full bibliography for 7243416--7243419.cif.'
_cod_original_cell_volume        30242(2)
_cod_database_code               7243419
_shelx_shelxl_version_number     2018/3
_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
2. Restrained distances
 C10-C9 = O6-C9 = N2-C9 = C14-C15 = N3-C14 = O9-C14
 1.5 with sigma of 0.02
 O5-C6
 1.2 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 O5-O4
 2.2 with sigma of 0.02
3. Restrained planarity
 O4, O5, C6, C7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim O6 \\sim N2 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10:
within 1.7A with sigma of 0.0004 and sigma for terminal atoms of 0.0008
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1W)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O3W) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O19(0.5) O20(0.5) O21(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C17(H17)
6.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              68265
_shelx_hkl_checksum              41594
_shelx_fab_checksum              83703
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'