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_7713423
_publ_section_title
;
 Peroxido-bridged chiral double-decker dysprosium macrocycles
;
_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), 5.5[CH3CN], 1[CH3OH]'
_chemical_formula_sum            'C180 H154.5 B2 Dy2 N17.5 O5'
_chemical_formula_weight         2989.32
_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
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7543(12)
_cell_length_b                   17.3502(7)
_cell_length_c                   62.722(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                     31528(2)
_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 0.994
_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  0.1338
_diffrn_reflns_av_unetI/netI     0.2373
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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            131144
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.066
_diffrn_reflns_theta_max         25.066
_diffrn_reflns_theta_min         1.902
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             12312
_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         5.411
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 7272 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.148(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2988
_refine_ls_number_reflns         54639
_refine_ls_number_restraints     3574
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2285
_refine_ls_R_factor_gt           0.1029
_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^)+(0.1856P)^2^+1.5920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2485
_refine_ls_wR_factor_ref         0.3448
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                24982
_reflns_number_total             54639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01540h2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C180 H154.50 B2 Dy2 N17.50 O5'
_cod_database_code               7713423
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C61-C102
 1.47 with sigma of 0.02
 C104-C109
 1.47 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C310) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C206) \\sim Ueq,
Uanis(C207) \\sim Ueq, Uanis(C229) \\sim Ueq, Uanis(C312) \\sim Ueq,
Uanis(C321) \\sim Ueq, Uanis(C227) \\sim Ueq, Uanis(C334) \\sim Ueq,
Uanis(C168) \\sim Ueq, Uanis(C171) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Y: Dy3(0.4272)
5.a Ternary CH refined with riding coordinates:
 C209(H209), C67(H67), C167(H167), C26(H26), C153(H153), C40(H40), C74(H74),
 C202(H202), C47(H47), C174(H174), C19(H19), C188(H188), C146(H146), C95(H95),
 C181(H181), C88(H88)
5.b Aromatic/amide H refined with riding coordinates:
 C143(H143), C81(H81), C35(H35), C54(H54), C80(H80), C79(H79), C78(H78),
 C77(H77), C76(H76), C197(H197), C201(H201), C199(H199), C336(H336), C164(H164),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C66(H66), C102(H102),
 C291(H291), C290(H290), C294(H294), C293(H293), C292(H292), C39(H39),
 C220(H220), C132(H132), C163(H163), C36(H36), C85(H85), C159(H159), C333(H333),
  C322(H322), C323(H323), C324(H324), C320(H320), C321(H321), C101(H101),
 C100(H100), C99(H99), C98(H98), C97(H97), C222(H222), C18(H18), C142(H142),
 C128(H128), C218(H218), C83(H83), C284(H284), C334(H334), C306(H306),
 C158(H158), C286(H286), C152(H152), C58(H58), C148(H148), C145(H145),
 C287(H287), C122(H122), C37(H37), C84(H84), C335(H335), C205(H205), C204(H204),
  C208(H208), C207(H207), C206(H206), C332(H332), C195(H195), C274(H274),
 C275(H275), C276(H276), C272(H272), C273(H273), C87(H87), C190(H190),
 C105(H105), C155(H155), C7(H7), C316(H316), C318(H318), C315(H315), C317(H317),
  C121(H121), C33(H33), C139(H139), C308(H308), C309(H309), C310(H310),
 C311(H311), C312(H312), C63(H63), C285(H285), C198(H198), C160(H160), C15(H15),
  C56(H56), C17(H17), C296(H296), C300(H300), C299(H299), C298(H298),
 C297(H297), C60(H60), C180(H180), C57(H57), C288(H288), C166(H166), C169(H169),
  C170(H170), C171(H171), C172(H172), C173(H173), C1(H1), C6(H6), C2(H2),
 C106(H106), C126(H126), C62(H62), C213(H213), C212(H212), C211(H211),
 C215(H215), C214(H214), C228(H228), C223(H223), C224(H224), C107(H107),
 C282(H282), C281(H281), C280(H280), C279(H279), C278(H278), C16(H16),
 C305(H305), C131(H131), C239(H239), C240(H240), C236(H236), C237(H237),
 C238(H238), C194(H194), C178(H178), C219(H219), C24(H24), C25(H25), C21(H21),
 C22(H22), C23(H23), C216(H216), C270(H270), C269(H269), C268(H268), C267(H267),
  C266(H266), C151(H151), C64(H64), C149(H149), C162(H162), C71(H71), C72(H72),
 C73(H73), C69(H69), C70(H70), C157(H157), C135(H135), C136(H136), C137(H137),
 C138(H138), C134(H134), C302(H302), C150(H150), C257(H257), C258(H258),
 C254(H254), C255(H255), C256(H256), C12(H12), C313(H313), C9(H9), C10(H10),
 C11(H11), C116(H116), C120(H120), C119(H119), C118(H118), C117(H117),
 C304(H304), C156(H156), C92(H92), C91(H91), C90(H90), C94(H94), C93(H93),
 C246(H246), C245(H245), C244(H244), C243(H243), C242(H242), C234(H234),
 C233(H233), C232(H232), C231(H231), C230(H230), C249(H249), C248(H248),
 C252(H252), C251(H251), C250(H250), C193(H193), C330(H330), C326(H326),
 C327(H327), C328(H328), C329(H329), C191(H191), C192(H192), C261(H261),
 C260(H260), C264(H264), C263(H263), C262(H262), C52(H52), C51(H51), C50(H50),
 C49(H49), C53(H53), C177(H177), C186(H186), C187(H187), C183(H183), C184(H184),
  C185(H185), C29(H29), C30(H30), C31(H31), C32(H32), C28(H28), C14(H14),
 C112(H112), C113(H113), C114(H114), C110(H110), C111(H111), C129(H129),
 C130(H130), C141(H141), C176(H176), C303(H303), C179(H179)
5.c Fitted hexagon refined as free rotating group:
 C75(C80,C79,C78,C77,C76), C41(C42,C43,C44,C45,C46), C291(C290,C289,C294,C293,
 C292), C322(C323,C324,C319,C320,C321), C101(C100,C99,C98,C97,C96), C205(C204,
 C203,C208,C207,C206), C274(C275,C276,C271,C272,C273), C7(C316,C318,C314,C315,
 C317), C307(C308,C309,C310,C311,C312), C296(C295,C300,C299,C298,C297),
 C169(C170,C171,C172,C173,C168), C1(C6,C5,C4,C3,C2), C213(C212,C211,C210,C215,
 C214), C225(C226,C227,C228,C223,C224), C277(C282,C281,C280,C279,C278),
 C239(C240,C235,C236,C237,C238), C24(C25,C20,C21,C22,C23), C265(C270,C269,C268,
 C267,C266), C71(C72,C73,C68,C69,C70), C135(C136,C137,C138,C133,C134),
 C257(C258,C253,C254,C255,C256), C12(C313,C8,C9,C10,C11), C116(C115,C120,C119,
 C118,C117), C92(C91,C90,C89,C94,C93), C246(C245,C244,C243,C242,C241),
 C229(C234,C233,C232,C231,C230), C249(C248,C247,C252,C251,C250), C330(C325,C326,
 C327,C328,C329), C261(C260,C259,C264,C263,C262), C52(C51,C50,C49,C48,C53),
 C186(C187,C182,C183,C184,C185), C29(C30,C31,C32,C27,C28), C112(C113,C114,C109,
 C110,C111)
;
_smtbx_masks_special_details
;
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              4149
_shelx_fab_checksum              46105
_olex2_submission_special_instructions 'No special instructions were received'