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_7243418
_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 N16 O84 Y14, 6(Cl O4)'
_chemical_formula_sum            'C80 H294 Cl10 N16 O179 Y14'
_chemical_formula_weight         5944.53
_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                   31.008(4)
_cell_length_b                   31.008(4)
_cell_length_c                   30.850(4)
_cell_measurement_reflns_used    66358
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.31
_cell_measurement_theta_min      3.50
_cell_volume                     29662(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.965
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            50227
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.785
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    5.167
_exptl_absorpt_correction_T_max  0.5384
_exptl_absorpt_correction_T_min  0.2595
_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    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             12136
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 4986 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.111(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         13571
_refine_ls_number_restraints     544
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0872P)^2^+36.3740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                11958
_reflns_number_total             13571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00948f2.cif
_cod_data_source_block           D-Y14
_cod_depositor_comments
'Adding full bibliography for 7243416--7243419.cif.'
_cod_original_cell_volume        29663(8)
_cod_database_code               7243418
_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 Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              58313
_shelx_hkl_checksum              91909
_shelx_fab_checksum              36980
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'