Subcomponent self-assembly of circular helical Dy6(L)6 and bipyramid Dy12(L)8 architectures directed via second-order template effects
Li, Xiao-Lei; Zhao, Lang; Wu, Jianfeng; Shi, Wei; Struch, Niklas; Lützen, Arne; Powell, Annie K.; Cheng, Peng; Tang, Jinkui; Chemical Science  (2022) –; doi:10.1039/D2SC03156F

data_1567485
_publ_section_title
;
 Subcomponent self-assembly of circular helical Dy6(L)6 and bipyramid
 Dy12(L)8 architectures directed via second-order template effects
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03156F
_journal_year                    2022
_chemical_formula_moiety
'C127 H146 Dy6 N40 O48, C6 H15 N, 7(C H4 O), 3(C H3 O), 2(N O3), 11(O)'
_chemical_formula_sum            'C143 H198 Dy6 N43 O75'
_chemical_formula_weight         4694.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2022-07-15 deposited with the CCDC.	2022-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.666(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.480(3)
_cell_length_b                   23.024(3)
_cell_length_c                   39.629(4)
_cell_measurement_reflns_used    9369
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.37
_cell_volume                     23247(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            143251
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.073
_diffrn_reflns_theta_min         1.294
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.986
_exptl_absorpt_correction_T_max  0.672
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             9412
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.197
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2451
_refine_ls_number_reflns         45888
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+79.3048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28717
_reflns_number_total             45888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03156f2.cif
_cod_data_source_block           Dy6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1567485
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H19A of O19, H12M of O12, H6 of O6, H27 of O27, H42 of O42,
   H46 of O46, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H7 of O7, H52A of O52, H61 of O61, H62 of O62, H63A of
  O63, H71 of O71, H73A of O73, H81 of O81, All O(H,H) groups
2. Restrained distances
 C133-O81
 1.43 with sigma of 0.02
 C144-O76
 1.43 with sigma of 0.02
 C134-O52
 1.43 with sigma of 0.02
 C135-O71
 1.43 with sigma of 0.02
 C143-O74
 1.43 with sigma of 0.02
 C137-O61
 1.43 with sigma of 0.02
 C139-O73
 1.43 with sigma of 0.02
 C138-O64
 1.43 with sigma of 0.02
 O7-H7
 0.85 with sigma of 0.01
 C146-H7
 1.991958 with sigma of 0.02
 Dy1-H7
 2.914892 with sigma of 0.02
3. Rigid bond restraints
 O42, C145
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, C146
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C146) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C144)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C100)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C133) \\sim Ueq, Uanis(C134) \\sim Ueq, Uanis(C135) \\sim Ueq,
Uanis(C143) \\sim Ueq, Uanis(C144) \\sim Ueq, Uanis(C145) \\sim Ueq,
Uanis(C146) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N41) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O11) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O35) \\sim Ueq,
Uanis(O70) \\sim Ueq, Uanis(O71) \\sim Ueq, Uanis(O72) \\sim Ueq, Uanis(O73)
\\sim Ueq, Uanis(O74) \\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O76) \\sim Ueq,
Uanis(O77) \\sim Ueq, Uanis(O78) \\sim Ueq, Uanis(O79) \\sim Ueq, Uanis(O80)
\\sim Ueq, Uanis(O81) \\sim Ueq, Uanis(O82) \\sim Ueq, Uanis(O83) \\sim Ueq,
Uanis(O53) \\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O61) \\sim Ueq, Uanis(O67)
\\sim Ueq, Uanis(O68) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a Rotating group:
 O13(H13H,H13I), O18(H18A,H18B), O31(H31A,H31B), O36(H36B,H36C), O37(H37A,H37B)
5.b Secondary CH2 refined with riding coordinates:
 C121(H12N,H12O), C123(H12S,H12T), C125(H12X,H12Y)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C23(H23), C24(H24), C25(H25), C28(H28), C30(H30), C32(H32),
  C33(H33), C35(H35), C36(H36), C37(H37), C43(H43), C44(H44), C45(H45),
 C48(H48), C50(H50), C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C63(H63),
  C64(H64), C65(H65), C68(H68), C70(H70), C72(H72), C73(H73), C75(H75),
 C76(H76), C77(H77), C83(H83), C84(H84), C85(H85), C88(H88), C90(H90), C92(H92),
  C93(H93), C95(H95), C96(H96), C97(H97), C103(H103), C104(H104), C105(H105),
 C108(H108), C110(H110), C112(H112), C113(H113), C115(H115), C116(H116),
 C117(H117), N2(H2), N5(H5A), N10(H10G), N13(H13G), N16(H16A), N19(H19),
 N22(H22), N26(H26), N30(H30A), N33(H33A), N36(H36A), N39(H39), O6(H6),
 O12(H12M), O19(H19A), O27(H27), O42(H42), O46(H46)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C80(H80A,
 H80B,H80C), C81(H81A,H81B,H81C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C120(H12A,H12B,H12C), C122(H12P,H12Q,H12R), C124(H12U,H12V,H12W), C126(H12Z,H,
 HA), C127(H12D,H12E,H12F), C128(H12G,H12H,H12I), C129(H12J,H12K,H12L),
 C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C133(H13J,H13K,H13L), C134(H13M,
 H13N,H13O), C135(H13P,H13Q,H13R), C136(H13S,H13T,H13U), C137(H13V,H13W,H13X),
 C138(H13Z,HB,HC), C139(H13Y,HD,HE), C140(H14G,H14H,H14I), C143(H14J,H14K,H14L),
  C144(H14M,H14N,H14O), C145(H14A,H14B,H14C), C146(H14D,H14E,H14F)
5.e Idealised tetrahedral OH refined as rotating group:
 O52(H52A), O61(H61), O62(H62), O63(H63A), O71(H71), O73(H73A), O81(H81)
;
_shelx_res_checksum              289
_shelx_fab_checksum              66582
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'