Asymmetric induction in quadruple-stranded europium(III) helicates and circularly polarized luminescence.
Wang, Yunlu; Zhou, Yanyan; Yao, Zhiwei; Huang, Wenru; Gao, Ting; Yan, Pengfei; Li, Hongfeng; Dalton transactions (Cambridge, England : 2003) 51 (2022) 10973–10982; doi:10.1039/d2dt01379g

data_7710524
_publ_section_title
;
 Asymmetric induction in quadruple-stranded europium(III) helicates and
 circularly polarized luminescence.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10973
_journal_page_last               10982
_journal_paper_doi               10.1039/d2dt01379g
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety
'C80 H40 Eu2 F24 O16 S4, C H Cl3, 2(C3 H6 O), 2(C6 H16 N)'
_chemical_formula_sum            'C99 H85 Cl3 Eu2 F24 N2 O18 S4'
_chemical_formula_weight         2585.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2022-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                86.179(2)
_cell_angle_beta                 72.372(2)
_cell_angle_gamma                73.179(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7543(4)
_cell_length_b                   17.2189(4)
_cell_length_c                   22.8872(6)
_cell_measurement_reflns_used    3596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     5303.0(2)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47110
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         30.140
_diffrn_reflns_theta_min         3.044
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  0.8965
_exptl_absorpt_correction_T_min  0.6127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2588
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         26419
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+9.5123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20885
_reflns_number_total             26419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01379g2.cif
_cod_data_source_block           c
_cod_depositor_comments
'Adding full bibliography for 7710524--7710527.cif.'
_cod_database_code               7710524
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. 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 C(H,H,H) groups
2. Restrained distances
 Cl1-C81
 1.7 with sigma of 0.02
 C90-C91
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F12) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl1, Cl1', Cl2, Cl2', Cl3, Cl3', C81, C81'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C88, C89, C90, C91, C92, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C81)=Sof(H81)=1-FVAR(1)
 Sof(Cl1')=Sof(Cl2')=Sof(Cl3')=Sof(C81')=Sof(H81')=FVAR(1)
6.a Riding coordinates:
 C94(H94A,H94B,H94C), C95(H95A,H95B,H95C)
6.b Ternary CH refined with riding coordinates:
 C81(H81), C81'(H81'), N1(H1), N2(H2)
6.c Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C84(H84A,H84B), C86(H86A,H86B), C88(H88A,H88B), C90(H90A,
 H90B), C93(H93A,H93B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15),
 C16(H16), C18(H18), C23(H23), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32),
  C33(H33), C35(H35), C36(H36), C37(H37), C43(H43), C46(H46), C47(H47),
 C49(H49), C50(H50), C52(H52), C53(H53), C55(H55), C56(H56), C58(H58), C63(H63),
  C66(H66), C67(H67), C69(H69), C70(H70), C72(H72), C73(H73), C75(H75),
 C76(H76), C78(H78)
6.e Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C83(H83A,H83B,H83C), C85(H85A,H85B,
 H85C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C92(H92A,
 H92B,H92C)
;
_shelx_res_checksum              18079
_shelx_hkl_checksum              72685
_olex2_submission_special_instructions 'No special instructions were received'