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_7713420
_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
'C120 H94 Dy2 N12 O4, 2(C24 H20 B), 2(C2 H3 N), 1.5[CH3CN], 1[CH3OH], 2[CH3CN], 1.5[CH3CN]'
_chemical_formula_sum            'C183 H159 B2 Dy2 N19 O5'
_chemical_formula_weight         3050.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-26
_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                 103.2170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7238(10)
_cell_length_b                   17.4037(6)
_cell_length_c                   62.791(2)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    180.00
_cell_measurement_theta_max      22.625
_cell_measurement_theta_min      2.277
_cell_volume                     31621.6(18)
_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      180.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            160554
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.083
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         1.904
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.001
_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    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             12576
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.773
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 19349 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3496
_refine_ls_number_reflns         55747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+53.2736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                47044
_reflns_number_total             55747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01540h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        31621.5(19)
_cod_database_code               7713420
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.753
_olex2_refinement_description
;
1. Others
 Fixed Y: Dy1(0.601301)
2.a Ternary CH refined with riding coordinates:
 C40(H40), C47(H47), C209(H209), C167(H167), C67(H67), C202(H202), C74(H74),
 C26(H26), C153(H153), C146(H146), C174(H174), C181(H181), C19(H19), C95(H95),
 C88(H88), C188(H188)
2.b Aromatic/amide H refined with riding coordinates:
 C81(H81), C35(H35), C197(H197), C84(H84), C39(H39), C201(H201), C143(H143),
 C54(H54), C222(H222), C195(H195), C87(H87), C76(H76), C224(H224), C101(H101),
 C102(H102), C159(H159), C83(H83), C145(H145), C164(H164), C60(H60), C132(H132),
  C314(H314), C36(H36), C105(H105), C66(H66), C166(H166), C85(H85), C37(H37),
 C287(H287), C218(H218), C298(H298), C142(H142), C63(H63), C128(H128), C21(H21),
  C129(H129), C300(H300), C199(H199), C276(H276), C172(H172), C272(H272),
 C308(H308), C173(H173), C160(H160), C14(H14), C216(H216), C315(H315),
 C291(H291), C230(H230), C198(H198), C163(H163), C6(H6), C290(H290), C152(H152),
  C80(H80), C139(H139), C316(H316), C97(H97), C322(H322), C116(H116),
 C220(H220), C138(H138), C299(H299), C215(H215), C284(H284), C131(H131),
 C69(H69), C169(H169), C318(H318), C204(H204), C134(H134), C288(H288),
 C274(H274), C16(H16), C190(H190), C121(H121), C17(H17), C78(H78), C2(H2),
 C56(H56), C141(H141), C158(H158), C296(H296), C273(H273), C137(H137), C58(H58),
  C25(H25), C57(H57), C323(H323), C223(H223), C90(H90), C312(H312), C64(H64),
 C1(H1), C122(H122), C49(H49), C240(H240), C282(H282), C91(H91), C228(H228),
 C42(H42), C171(H171), C148(H148), C311(H311), C248(H248), C50(H50), C306(H306),
  C324(H324), C107(H107), C120(H120), C112(H112), C155(H155), C178(H178),
 C110(H110), C179(H179), C236(H236), C113(H113), C22(H22), C211(H211),
 C183(H183), C176(H176), C334(H334), C170(H170), C219(H219), C18(H18),
 C292(H292), C73(H73), C205(H205), C194(H194), C275(H275), C214(H214),
 C106(H106), C12(H12), C320(H320), C333(H333), C212(H212), C327(H327),
 C249(H249), C294(H294), C239(H239), C70(H70), C130(H130), C114(H114),
 C293(H293), C117(H117), C111(H111), C162(H162), C208(H208), C136(H136),
 C32(H32), C53(H53), C51(H51), C302(H302), C237(H237), C309(H309), C207(H207),
 C8(H8), C281(H281), C280(H280), C328(H328), C46(H46), C297(H297), C238(H238),
 C100(H100), C234(H234), C278(H278), C246(H246), C28(H28), C336(H336),
 C149(H149), C77(H77), C231(H231), C305(H305), C119(H119), C118(H118),
 C310(H310), C206(H206), C24(H24), C243(H243), C11(H11), C244(H244), C279(H279),
  C269(H269), C330(H330), C332(H332), C193(H193), C71(H71), C266(H266),
 C92(H92), C23(H23), C43(H43), C260(H260), C303(H303), C52(H52), C151(H151),
 C268(H268), C10(H10), C267(H267), C245(H245), C9(H9), C304(H304), C261(H261),
 C31(H31), C191(H191), C263(H263), C232(H232), C264(H264), C94(H94), C177(H177),
  C329(H329), C156(H156), C45(H45), C72(H72), C99(H99), C186(H186), C44(H44),
 C257(H257), C98(H98), C256(H256), C254(H254), C255(H255), C185(H185), C29(H29),
  C187(H187), C33(H33), C270(H270), C317(H317), C126(H126), C15(H15),
 C150(H150), C213(H213), C62(H62), C326(H326), C192(H192), C157(H157),
 C184(H184), C93(H93), C321(H321), C30(H30), C242(H242), C79(H79), C250(H250),
 C251(H251), C135(H135), C252(H252), C335(H335), C262(H262), C233(H233),
 C285(H285), C286(H286), C180(H180), C258(H258)
2.c Idealised Me refined as rotating group:
 C340(H34D,H34E,H34F), C342(H34A,H34B,H34C), C338(H33A,H33B,H33C), C344(H34G,
 H34H,H34I)
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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.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31060
_shelx_fab_checksum              26467
_olex2_submission_special_instructions 'No special instructions were received'