Ancillary ligand modulated stereoselective self-assembly of triple-stranded Eu(iii) helicate featuring circularly polarized luminescence
Yao, Zhiwei; Zhou, Yanyan; Gao, Ting; Yan, Pengfei; Li, Hongfeng; RSC Advances 11 (2021) 10524–10531; doi:10.1039/D1RA01583D

data_7242391
_publ_section_title
;
 Ancillary ligand modulated stereoselective self-assembly of
 triple-stranded Eu(iii) helicate featuring circularly polarized
 luminescence
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              10524
_journal_page_last               10531
_journal_paper_doi               10.1039/D1RA01583D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C84 H46 Eu2 F18 N4 O12 S3, 1.5(C7 H8)'
_chemical_formula_sum            'C94.5 H58 Eu2 F18 N4 O12 S3'
_chemical_formula_weight         2183.55
_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.	2021-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                105.518(3)
_cell_angle_beta                 96.587(3)
_cell_angle_gamma                118.352(4)
_cell_formula_units_Z            2
_cell_length_a                   17.5629(7)
_cell_length_b                   18.0137(7)
_cell_length_c                   18.8460(6)
_cell_measurement_reflns_used    11118
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5581
_cell_measurement_theta_min      3.0091
_cell_volume                     4846.0(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -55.00  -17.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1312  -19.0000  -90.0000 38

  2 omega  -26.00   52.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1312  -57.0000  120.0000 78

  3 omega  -25.00   72.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       23.1312  -99.0000   90.0000 97

  4 omega  -25.00   21.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1468  -99.0000  -90.0000 46

  5 omega  -49.00  -22.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1468   19.0000   30.0000 27

  6 omega    7.00   36.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1468   19.0000   30.0000 29

  7 omega  -97.00  -15.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1468  -57.0000  -30.0000 82

  8 omega  -97.00    2.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1468  -57.0000 -150.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0314173000
_diffrn_orient_matrix_UB_12      -0.0308917000
_diffrn_orient_matrix_UB_13      -0.0364626000
_diffrn_orient_matrix_UB_21      -0.0361269000
_diffrn_orient_matrix_UB_22      -0.0071858000
_diffrn_orient_matrix_UB_23      0.0163910000
_diffrn_orient_matrix_UB_31      -0.0003613000
_diffrn_orient_matrix_UB_32      0.0361967000
_diffrn_orient_matrix_UB_33      -0.0079075000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34920
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.015
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2170
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         17033
_refine_ls_number_restraints     442
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+3.3751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12464
_reflns_number_total             17033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra01583d2.cif
_cod_data_source_block           c
_cod_original_formula_sum        'C94.50 H58 Eu2 F18 N4 O12 S3'
_cod_database_code               7242391
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C96-C95
 2.4 with sigma of 0.02
 C92-C95
 2.4 with sigma of 0.02
 C94-C92
 1.5 with sigma of 0.02
 C105-C99 \\sim C99-C101
 with sigma of 0.02
 F11-F12 \\sim F12-F10 \\sim F11-F10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C100) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C104) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C96)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F10A) \\sim Ueq,
Uanis(C6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C99, C100, C101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F10, F10A, F11, F11A, F12, F12A, C6, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(C6A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C6)=FVAR(1)
 Fixed Sof: C85(0.5) H85(0.5) C86(0.5) C87(0.5) H87(0.5) C88(0.5) H88(0.5)
 C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5) C90(0.5) H90(0.5) C91(0.5) H91(0.5)
 C93(0.5) C96(0.5) H96(0.5) C98(0.5) H98(0.5) C97(0.5) H97(0.5) C94(0.5)
 H94(0.5) C92(0.5) H92(0.5) C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5) C99(0.5)
 H99A(0.5) H99B(0.5) H99C(0.5) C104(0.5) H104(0.5) C103(0.5) H103(0.5)
 C105(0.5) H105(0.5) C100(0.5) C101(0.5) H101(0.5) C102(0.5) H102(0.5)
6.a Riding coordinates:
 C99(H99A,H99B,H99C)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C34(H34), C35(H35), C37(H37), C39(H39), C40(H40), C43(H43), C44(H44), C47(H47),
  C48(H48), C50(H50), C51(H51), C55(H55), C64(H64), C65(H65), C66(H66),
 C69(H69), C71(H71), C74(H74), C75(H75), C76(H76), C79(H79), C80(H80), C84(H84),
  C85(H85), C87(H87), C88(H88), C90(H90), C91(H91), C96(H96), C98(H98),
 C97(H97), C94(H94), C92(H92), C104(H104), C103(H103), C105(H105), C101(H101),
 C102(H102)
6.c Fitted hexagon refined as free rotating group:
 C93(C96,C98,C97,C94,C92), C104(C103,C105,C100,C101,C102)
6.d Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C95(H95A,H95B,H95C)
;
_shelx_res_checksum              44759
_olex2_submission_special_instructions 'No special instructions were received'