Self-assembled lanthanide-based helixes: synthetic control of the helical handedness by chirality of the ligand.
Wu, Min-Yu; Xu, Jing-Xiang; Chen, Yi-Hsin; Lu, I-Chung; Han, Jeng-Liang; Lin, Po-Heng; Dalton transactions (Cambridge, England : 2003) 51 (2021) 69–73; doi:10.1039/d1dt03833h

data_7708946
_publ_section_title
;
 Self-assembled lanthanide-based helixes: synthetic control of the helical
 handedness by chirality of the ligand.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              69
_journal_page_last               73
_journal_paper_doi               10.1039/d1dt03833h
_journal_volume                  51
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H31 N9 O26 S3 Tb2, 3(H2 O)'
_chemical_formula_sum            'C30 H37 N9 O29 S3 Tb2'
_chemical_formula_weight         1401.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2021-10-19 deposited with the CCDC.	2021-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4028(7)
_cell_length_b                   17.0704(15)
_cell_length_c                   31.728(3)
_cell_measurement_reflns_used    9182
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.71
_cell_volume                     4551.0(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_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     0.71076
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            70190
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         2.471
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2760
_refine_diff_density_max         1.387
_refine_diff_density_min         -2.244
_refine_diff_density_rms         0.424
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.035(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.379
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         9307
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.378
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0501P)^2^+14.1284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9240
_reflns_number_total             9307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03833h2.cif
_cod_data_source_block           mo_wcl28_0m_pl
_cod_depositor_comments
'Adding full bibliography for 7708942--7708947.cif.'
_cod_database_code               7708946
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.965(15)
 0.035(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O16 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O3) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
4.a Free rotating group:
 O27(H27A,H27B), O28(H28C,H28D), O29(H29A,H29B)
4.b Rotating group:
 O18(H18A,H18B), O17(H17A,H17B), O6(H6A,H6B), O5(H5A,H5B), O4(H4A,H4B)
4.c Ternary CH refined with riding coordinates:
 N1(H1), N4(H4), N7(H7), C9(H9), C19(H19), C7(H7A), C17(H17), C27(H27), C29(H29)
4.d Secondary CH2 refined with riding coordinates:
 C18(H18C,H18D), C28(H28A,H28B), C8(H8A,H8B)
4.e Aromatic/amide H refined with riding coordinates:
 C5(H5), C25(H25), C3(H3), C15(H15), C23(H23), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'