Peroxido-bridged chiral double-decker dysprosium macrocycles
Zhao, Chen; Wang, Tingting; Liu, Xiaodong; Zhu, Zhenhua; Ying, Xu; Li, Xiao-Lei; Tang, Jinkui; Dalton Transactions  (2023) –; doi:10.1039/D3DT01540H

data_7713421
_publ_section_title
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 Peroxido-bridged chiral double-decker dysprosium macrocycles
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01540H
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C84 H68 Cl2 Dy2 N12 O2, 2(C24 H20 B), 6[CH3CN]'
_chemical_formula_sum            'C144 H126 B2 Cl2 Dy2 N18 O2'
_chemical_formula_weight         2558.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-20
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2023-07-07 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7298(3)
_cell_length_b                   16.3326(4)
_cell_length_c                   47.7251(10)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    180.00
_cell_measurement_theta_max      22.625
_cell_measurement_theta_min      2.277
_cell_volume                     12261.0(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            90517
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.053
_diffrn_reflns_theta_min         1.990
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1223 before and 0.0925 after correction.
The Ratio of minimum to maximum transmission is 0.8065.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       plate
_exptl_crystal_F_000             5232
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.119
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 6825 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         21667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0668P)^2^+8.8887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                17106
_reflns_number_total             21667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01540h2.cif
_cod_data_source_block           3
_cod_database_code               7713421
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.779
_olex2_refinement_description
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1.a Ternary CH refined with riding coordinates:
 C14(H14), C18(H18), C28(H28), C36(H36), C50(H50), C58(H58), C98(H98), C9(H9)
1.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C12(H12), C24(H24), C32(H32), C34(H34), C42(H42),
 C46(H46), C48(H48), C52(H52), C54(H54), C62(H62), C64(H64), C68(H68), C70(H70),
  C72(H72), C74(H74), C76(H76), C78(H78), C80(H80), C82(H82), C86(H86),
 C88(H88), C92(H92), C94(H94), C96(H96), C100(H100), C104(H104), C112(H112),
 C114(H114), C116(H116), C118(H118), C120(H120), C122(H122), C124(H124),
 C126(H126), C128(H128), C130(H130), C33(H33), C67(H67), C69(H69), C35(H35),
 C71(H71), C73(H73), C37(H37), C75(H75), C19(H19), C77(H77), C39(H39), C79(H79),
  C5(H5), C81(H81), C41(H41), C83(H83), C21(H21), C85(H85), C43(H43), C11(H11),
 C89(H89), C45(H45), C23(H23), C93(H93), C47(H47), C95(H95), C3(H3), C97(H97),
 C49(H49), C99(H99), C25(H25), C101(H101), C51(H51), C103(H103), C13(H13),
 C105(H105), C53(H53), C27(H27), C109(H109), C55(H55), C111(H111), C7(H7),
 C113(H113), C57(H57), C115(H115), C29(H29), C117(H117), C59(H59), C119(H119),
 C15(H15), C121(H121), C61(H61), C123(H123), C31(H31), C125(H125), C63(H63),
 C127(H127), C2(H2), C129(H129), C65(H65), C131(H131)
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_smtbx_masks_special_details
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A solvent mask was calculated and 1090 electrons were 
found in a volume of 7840\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6.5[CH3CN] per Asymmetric Unit 
which account for 1144 electrons 
per unit cell.
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34147
_shelx_fab_checksum              87480
_olex2_submission_special_instructions 'No special instructions were received'