Synthesis and multifunctional sensing of axially chiral tetranuclear europium clusters
Cui, Dongxu; Zhao, Hong-Lei; Kou, Jun-Ning; Sun, Chun-Yi; Wang, Xinlong; Su, Zhong-Min; CrystEngComm  (2022) –; doi:10.1039/D1CE01554K

data_7244253
_publ_section_title
;
 Synthesis and multifunctional sensing of axially chiral tetranuclear
 europium clusters
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01554K
_journal_year                    2022
_chemical_formula_moiety
'C174 H131 Cl2 Eu4 O44 P8, 2(Cl), 3[CH3CH2OH]'
_chemical_formula_sum            'C176 H158 Cl4 Eu4 O51 P8'
_chemical_formula_weight         4086.41
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-14
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-30 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                108.665(3)
_cell_angle_beta                 107.697(3)
_cell_angle_gamma                97.375(3)
_cell_formula_units_Z            1
_cell_length_a                   13.7311(9)
_cell_length_b                   18.3631(12)
_cell_length_c                   20.1893(13)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     4448.8(5)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      293.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    '0.5 mm double- pinhole'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            63762
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        44.972
_diffrn_reflns_theta_max         44.972
_diffrn_reflns_theta_min         2.483
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.856
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2062
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.886
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.171(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2035
_refine_ls_number_reflns         13352
_refine_ls_number_restraints     6590
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+74.7861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                10565
_reflns_number_total             13352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01554k2.cif
_cod_data_source_block           s
_cod_database_code               7244253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.829(11)
 0.171(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O9-P3
 1.47 with sigma of 0.02
 Cl2-Eu3
 2.8 with sigma of 0.02
 Cl2-Eu4
 2.8 with sigma of 0.02
 C112-C111 = C113-C112 = C114-C113 = C115-C114 = C116-C115 = C117-C116 = C118-
 C117 = C119-C118 = C120-C119 = C120-C111 = C120-C115
 1.38 with sigma of 0.01
 C170-C169 = C164-C163 = C162-C161 = C168-C167 = C166-C165 = C174-C173 = C172-
 C171
 1.45 with sigma of 0.01
 P8-O30 = P3-O9
 1.55 with sigma of 0.01
 O40-C175
 1.4 with sigma of 0.01
 C175-C176
 1.45 with sigma of 0.01
 C168-C167 \\sim C166-C165 \\sim C172-C171 \\sim C174-C173 \\sim C170-C169
\\sim C162-C161 \\sim C164-
 C163
 with sigma of 0.02
 O34-C163 \\sim O33-C161 \\sim O36-C167 \\sim O35-C165 \\sim O39-C171 \\sim
O38-C173 \\sim O37-C169
 with sigma of 0.02
 C111-C101 \\sim C131-C121 \\sim C151-C145 \\sim C11-C1 \\sim C31-C21 \\sim
C72-C61 \\sim C51-C42 ~
 C91-C81
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C22 \\sim C21 \\sim C30 \\sim C25 \\sim C24
\\sim C23 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C42
\\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50
\\sim C41 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C72 \\sim C73 \\sim C74
\\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C71 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C90 \\sim C89 \\sim C88 \\sim C87
\\sim C86 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118
\\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125
\\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132
\\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C139
\\sim C140 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146 \\sim C147
\\sim C148 \\sim C149 \\sim C150 \\sim C141 \\sim C151 \\sim C152 \\sim C153
\\sim C154 \\sim C155 \\sim C156 \\sim C157 \\sim C158 \\sim C159 \\sim C160
\\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167
\\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim C174
\\sim C176 \\sim C175 \\sim O1 \\sim O1W \\sim O2 \\sim O2W \\sim O3 \\sim O3W
\\sim O4 \\sim O40 \\sim O5 \\sim O4W \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim
O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17 \\sim
O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim
O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim
O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.03 within 3.8A
Uanis(P3) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(Cl1) \\sim Ueq, Uanis(P3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
5. Others
 Fixed Sof: Cl2(0.5) Cl2A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C161(H16A,H16B), C163(H16F,H16G), C165(H16K,H16L), C167(H16P,H16Q), C169(H16U,
 H16V), C171(H17D,H17E), C173(H17I,H17J), C175(H17Q,H17R)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C24(H24), C23(H23), C26(H26), C27(H27), C28(H28),
  C29(H29), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39),
 C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C41(H41), C53(H53), C54(H54),
  C56(H56), C57(H57), C58(H58), C59(H59), C63(H63), C64(H64), C66(H66),
 C67(H67), C68(H68), C69(H69), C74(H74), C75(H75), C78(H78), C79(H79), C80(H80),
  C71(H71), C83(H83), C84(H84), C89(H89), C88(H88), C87(H87), C86(H86),
 C93(H93), C94(H94), C96(H96), C97(H97), C98(H98), C99(H99), C103(H103),
 C104(H104), C106(H106), C107(H107), C108(H108), C109(H109), C113(H113),
 C114(H114), C116(H116), C117(H117), C118(H118), C119(H119), C123(H123),
 C124(H124), C126(H126), C127(H127), C128(H128), C129(H129), C133(H133),
 C134(H134), C136(H136), C137(H137), C138(H138), C139(H139), C142(H142),
 C143(H143), C148(H148), C149(H149), C150(H150), C141(H141), C153(H153),
 C154(H154), C156(H156), C157(H157), C158(H158), C159(H159)
6.c Fitted hexagon refined as free rotating group:
 C22(C21,C30,C25,C24,C23)
6.d Naphthalene refined as free rotating group:
 C42(C43,C44,C45,C46,C47,C48,C49,C50,C41), C72(C73,C74,C75,C76,C77,C78,C79,C80,
 C71), C81(C82,C83,C84,C85,C90,C89,C88,C87,C86), C142(C143,C144,C145,C146,C147,
 C148,C149,C150,C141)
6.e Idealised Me refined as rotating group:
 C162(H16C,H16D,H16E), C164(H16H,H16I,H16J), C166(H16M,H16N,H16O), C168(H16R,
 H16S,H16T), C170(H17A,H17B,H17C), C172(H17F,H17G,H17H), C174(H17K,H17L,H17M),
 C176(H17N,H17O,H17P)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              59589
_shelx_hkl_checksum              1900
_shelx_fab_checksum              59009
_olex2_submission_special_instructions 'No special instructions were received'