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_1567486
_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         'C224 H222 Dy12 N50 Na4 O84, 10(O)'
_chemical_formula_sum            'C224 H222 Dy12 N50 Na4 O94'
_chemical_formula_weight         7160.46
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.0539(6)
_cell_length_b                   32.0539(6)
_cell_length_c                   56.6487(17)
_cell_measurement_reflns_used    7692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.131
_cell_measurement_theta_min      2.22
_cell_volume                     58204(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            68692
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         2.890
_exptl_absorpt_coefficient_mu    3.134
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       Block
_exptl_crystal_F_000             28032
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         4.229
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         17461
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1296P)^2^+1049.6730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8479
_reflns_number_total             17461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03156f2.cif
_cod_data_source_block           Dy12Na4
_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_original_cell_volume        58204(3)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               1567486
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.510
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O23-O25
 2.7 with sigma of 0.01
 C52-N13
 1.15 with sigma of 0.01
 C52-C53
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H53A(0.5) H53B(0.5) H53C(0.5)
5.a Riding coordinates:
 O10(H10A,H10B), N2(H2), N5(H5), N8(H8), N11(H11)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5A), C8(H8A), C12(H12), C13(H13), C14(H14), C17(H17),
 C20(H20), C21(H21), C22(H22), C25(H25), C27(H27), C28(H28), C31(H31), C32(H32),
  C33(H33), C36(H36), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45)
5.c Idealised Me refined with riding coordinates and stretchable bonds:
 C53(H53A,H53B,H53C)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10C,H10D,H10E), C18(H18A,H18B,H18C), C29(H29A,H29B,
 H29C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C57(H57A,
 H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'