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_7713422
_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                   15.7450(3)
_cell_length_b                   16.3240(4)
_cell_length_c                   47.7781(12)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      24.939
_cell_measurement_theta_min      2.205
_cell_volume                     12280.0(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 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.994
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            83424
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.086
_diffrn_reflns_theta_min         2.113
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6303
_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 0.1060 before and 0.0721 after correction.
The Ratio of minimum to maximum transmission is 0.8458.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             5232
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.606
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 7773 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.010(4)
_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     1345
_refine_ls_number_reflns         21647
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0542P)^2^+22.3715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                18650
_reflns_number_total             21647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01540h2.cif
_cod_data_source_block           4
_cod_database_code               7713422
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Rigid bond restraints
 C119, C15, C121, C61, C123, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C8(H8), C12(H12), C32(H32), C34(H34), C52(H52), C62(H62), C64(H64), C124(H124)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C10(H10), C14(H14), C16(H16), C22(H22), C38(H38), C40(H40),
 C42(H42), C44(H44), C46(H46), C54(H54), C58(H58), C60(H60), C68(H68), C70(H70),
  C74(H74), C82(H82), C84(H84), C86(H86), C88(H88), C90(H90), C94(H94),
 C98(H98), C100(H100), C102(H102), C104(H104), C106(H106), C108(H108),
 C110(H110), C112(H112), C114(H114), C116(H116), C118(H118), C120(H120),
 C122(H122), C126(H126), C128(H128), C132(H132), C33(H33), C67(H67), C17(H17),
 C69(H69), C35(H35), C71(H71), C9(H9), C37(H37), C75(H75), C19(H19), C77(H77),
 C39(H39), C79(H79), C5(H5), C81(H81), C41(H41), C83(H83), C85(H85), C87(H87),
 C11(H11), C89(H89), C45(H45), C91(H91), 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), C107(H107), 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), C123(H123), C31(H31),
 C125(H125), C63(H63), C127(H127), C2(H2), C65(H65), C131(H131)
3.c Fitted hexagon refined as free rotating group:
 C119(C15,C121,C61,C123,C31), C63(C127,C2,C129,C65,C131)
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_smtbx_masks_special_details
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A solvent mask was calculated and 512 electrons were 
found in a volume of 2388\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6[CH3CN] per Formula Unit 
which account for 528 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24338
_shelx_fab_checksum              49996
_olex2_submission_special_instructions 'No special instructions were received'