Air-stable chiral double-decker Dy(III) macrocycle with fluoride ion as sole axial ligand
Liu, Xiaodong; Zhao, Chen; Wu, Jinjiang; Zhu, Zhenhua; Tang, Jinkui; Dalton Transactions  (2022) –; doi:10.1039/D2DT02902B

data_7711492
_publ_section_title
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 Air-stable chiral double-decker Dy(III) macrocycle with fluoride ion as
 sole axial ligand
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02902B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C84 H68 Dy2 F4 N12, 3(C H2 Cl2), 2(C24 H20 B)'
_chemical_formula_sum            'C135 H114 B2 Cl6 Dy2 F4 N12'
_chemical_formula_weight         2539.70
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2022-10-01 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2406(6)
_cell_length_b                   25.9357(10)
_cell_length_c                   27.5500(12)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      24.907
_cell_measurement_theta_min      2.475
_cell_volume                     12318.9(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0935
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            80204
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.032
_diffrn_reflns_theta_max         25.032
_diffrn_reflns_theta_min         1.965
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0807 after correction.
The Ratio of minimum to maximum transmission is 0.8626.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             5152
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 6278 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1460
_refine_ls_number_reflns         21727
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0492P)^2^+4.6705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                16908
_reflns_number_total             21727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02902b2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7711492
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl10-C7
 1.77 with sigma of 0.02
 Cl6-C7
 1.78 with sigma of 0.02
 Cl6-C7 = Cl10-C7
 1.771 with sigma of 0.01
 Cl6-Cl10
 2.916 with sigma of 0.03
 Cl6-Cl10
 2.92 with sigma of 0.04
 Cl10-C7 \\sim Cl-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl6 \\sim Cl10 \\sim C7: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Cl6, Cl10, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H45)=Sof(H47)=Sof(Cl)=1-FVAR(1)
 Sof(Cl10)=Sof(H43)=Sof(H44)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C11(H11), C15(H15), C18(H18), C21(H21), C23(H23), C40(H40)
6.b Secondary CH2 refined with riding coordinates:
 C121(H26,H27), C137(H36,H37), C7(H43,H44), C7(H45,H47)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C134(H134), C135(H135), C10(H10), C14(H14), C19(H19), C24(H24),
 C25(H25), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H), C37(HA), C38(H38), C39(H39), C41(H41), C42(H42), C45(HB), C46(H46),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(HC), C55(HD), C56(H56),
 C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(HE), C63(HF), C64(H64),
 C65(H65), C66(H66), C67(HG), C68(HH), C69(H69), C70(H70), C71(H71), C72(HI),
 C74(H74), C76(HJ), C77(HK), C78(H78), C79(HL), C80(H80), C82(H82), C83(H83),
 C84(HM), C85(HN), C86(HO), C87(HP), C88(H88), C89(HQ), C90(HR), C92(HS),
 C93(HT), C94(HU), C96(H96), C97(H97), C98(H98), C99(HV), C100(HW), C101(H101),
 C102(HX), C103(HY), C104(HZ), C105(H3), C106(H4), C107(H107), C108(H5),
 C109(H109), C110(H7), C111(H8), C112(H112), C113(H9), C114(H114), C115(H12),
 C116(H13), C117(H16), C118(H17), C119(H20), C120(H22), C122(H30), C123(H123),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132)
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_smtbx_masks_special_details
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A solvent mask was calculated and 300 electrons were 
found in a volume of 1216\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] and 2[H2O] per Asymmetric Unit 
which account for 208 electrons 
per unit cell.
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29814
_shelx_fab_checksum              12311
_olex2_submission_special_instructions 'No special instructions were received'