Structure and assembly mechanism of a centipede-shaped high-nuclear Dy14Cu12 heterometallic nanocluster
Yu, Shui; Hu, Huancheng; Qiu, Zhihui; Zhang, Yuzhen; Liu, Dongcheng; Liang, Yuning; Zou, Hua-Hong; Liang, Fu-Pei; Chen, Zilu; CrystEngComm 25 (2023) 114–121; doi:10.1039/D2CE01291J

data_7245826
_publ_section_title
;
 Structure and assembly mechanism of a centipede-shaped high-nuclear
 Dy14Cu12 heterometallic nanocluster
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              114
_journal_page_last               121
_journal_paper_doi               10.1039/D2CE01291J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C88 H108 Br8 Dy4 N8 Ni8 O36, 4(C2 H3 N), 3.25(C2 H6 O)'
_chemical_formula_sum            'C102.5 H139.5 Br8 Dy4 N12 Ni8 O39.25'
_chemical_formula_weight         3926.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc291tnv
_audit_creation_date             2022-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-30 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.0050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.4950(4)
_cell_length_b                   16.3703(2)
_cell_length_c                   60.2225(6)
_cell_measurement_reflns_used    34872
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.7230
_cell_measurement_theta_min      2.4530
_cell_volume                     28732.2(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            75343
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        62.881
_diffrn_reflns_theta_max         62.881
_diffrn_reflns_theta_min         2.421
_exptl_absorpt_coefficient_mu    15.219
_exptl_absorpt_correction_T_max  0.088
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       block
_exptl_crystal_F_000             15364
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.229
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1583
_refine_ls_number_reflns         22487
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0857P)^2^+758.2845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18971
_reflns_number_total             22487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01291j2.cif
_cod_data_source_block           20210427-czl-ys-zz-130
_cod_depositor_comments          'Adding full bibliography for 7245826.cif.'
_cod_original_cell_volume        28732.2(6)
_cod_original_formula_sum        'C102.50 H139.50 Br8 Dy4 N12 Ni8 O39.25'
_cod_database_code               7245826
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.194
_shelx_estimated_absorpt_t_min   0.115
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N11-C93
 1.16 with sigma of 0.01
 O43-C105
 1.48 with sigma of 0.01
 C105-C106
 1.54 with sigma of 0.01
 O43-C106
 2.6 with sigma of 0.02
 C93-C94
 1.46 with sigma of 0.01
 N11-C94
 2.64 with sigma of 0.02
 O39-C95
 1.46 with sigma of 0.01
 C95-C96
 1.53 with sigma of 0.01
 O39-C96
 2.62 with sigma of 0.01
 O40-C97
 1.46 with sigma of 0.01
 C97-C98
 1.53 with sigma of 0.01
 O40-C98
 2.62 with sigma of 0.02
 O41-C99
 1.46 with sigma of 0.01
 C99-C100
 1.5 with sigma of 0.01
 O41-C100
 2.5 with sigma of 0.02
 O42-C101
 1.46 with sigma of 0.01
 C101-C102
 1.5 with sigma of 0.01
 O42-C102
 2.5 with sigma of 0.02
 O45-C107
 1.46 with sigma of 0.01
 C108-C107
 1.52 with sigma of 0.01
 O45-C108
 2.5 with sigma of 0.02
 N12-C109
 1.18 with sigma of 0.01
 C109-C110
 1.48 with sigma of 0.01
 N12-C110
 2.68 with sigma of 0.02
 N13-C111
 1.16 with sigma of 0.01
 C111-C112
 1.46 with sigma of 0.01
 N13-C112
 2.62 with sigma of 0.02
3. Rigid bond restraints
 O43, C105, C106
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C94 \\sim C93 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C102 \\sim C101 \\sim C105 \\sim C106
\\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C112 \\sim C111: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O43 \\sim C105 \\sim C106: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O39 \\sim C95 \\sim C96: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O40 \\sim C97 \\sim C98: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O41 \\sim C99 \\sim C100: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O45 \\sim C107 \\sim C108: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C109 \\sim C110 \\sim N12: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(O43) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11) \\sim Ueq, Uanis(C93) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O41) \\sim Ueq, Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O42) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C100)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O45) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(N12) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O40)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=
 1-FVAR(1)
 Sof(O39)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=
 FVAR(1)
 Fixed Sof: C102(0.5) H10G(0.5) H10H(0.5) H10I(0.5) C101(0.5) H10J(0.5)
 H10K(0.5) O42(0.5) H42A(0.5) O43(0.25) H43A(0.25) C105(0.25) H10L(0.25)
 H10M(0.25) C106(0.25) H10N(0.25) H10O(0.25) H10P(0.25) O45(0.5) H45A(0.5)
 C107(0.5) H10Q(0.5) H10R(0.5) C108(0.5) H10S(0.5) H10T(0.5) H10U(0.5) N12(0.5)
 C109(0.5) C110(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C112(0.5) H11D(0.5)
 H11E(0.5) H11F(0.5) C111(0.5) N13(0.5)
6.a Riding coordinates:
 O17(H17), O18(H18), O19(H19), O20(H20), O21(H21), O22(H22), O23(H23),
 O24(H24), O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B),
 C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), N11(H39A),
 C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), O41(H41), C100(H10D,H10E,H10F),
 C102(H10G,H10H,H10I), O42(H42A), O43(H43A), C106(H10N,H10O,H10P), O45(H45A),
 C108(H10S,H10T,H10U), C110(H11A,H11B,H11C), C112(H11D,H11E,H11F)
6.b Ternary CH refined with riding coordinates:
 C9(H9), C19(H19A), C29(H29), C39(H39), C49(H49), C59(H59), C69(H69), C79(H79)
6.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C18(H18A,H18B), C28(H28C,H28D), C38(H38A,H38B), C48(H48A,H48B),
 C58(H58A,H58B), C68(H68A,H68B), C78(H78A,H78B), C95(H95A,H95B), C97(H97A,H97B),
  C99(H99A,H99B), C101(H10J,H10K), C105(H10L,H10M), C107(H10Q,H10R)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C12(H12), C13(H13), C15(H15), C17(H17A),
 C22(H22A), C23(H23A), C25(H25), C27(H27), C32(H32), C33(H33), C35(H35),
 C37(H37), C42(H42), C43(H43), C45(H45), C47(H47), C52(H52), C53(H53), C55(H55),
  C57(H57), C62(H62), C63(H63), C65(H65), C67(H67), C72(H72), C73(H73),
 C75(H75), C77(H77)
6.e Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C11(C12,C13,C14,C15,C16), C21(C22,C23,C24,C25,C26),
 C31(C32,C33,C34,C35,C36), C41(C42,C43,C44,C45,C46), C51(C52,C53,C54,C55,C56),
 C61(C62,C63,C64,C65,C66), C71(C72,C73,C74,C75,C76)
6.f Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C40(H40A,H40B,
 H40C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C70(H70A,H70B,H70C), C80(H80A,
 H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C),
 C88(H88A,H88B,H88C)
;
_shelx_res_checksum              40110
_shelx_hkl_checksum              90488
_olex2_submission_special_instructions 'No special instructions were received'