Terminal fluoride coordinated air-stable chiral dysprosium single-ion magnets
Wu, Jinjiang; Wang, Guo-Lu; Zhu, Zhenhua; Zhao, Chen; Li, Xiao-Lei; Zhang, Yi-Quan; Tang, Jinkui; Chemical Communications  (2022) –; doi:10.1039/D2CC02570A

data_7130198
_publ_section_title
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 Terminal fluoride coordinated air-stable chiral dysprosium single-ion
 magnets
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02570A
_journal_year                    2022
_chemical_formula_moiety
'C46 H44 Dy F2 N6 O, C24 H20 B, C H4 O, 2(H2 O)'
_chemical_formula_sum            'C71 H72 B Dy F2 N6 O4'
_chemical_formula_weight         1284.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
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_audit_update_record
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2022-01-18 deposited with the CCDC.	2022-06-07 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 96.2300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7090(5)
_cell_length_b                   23.6685(7)
_cell_length_c                   20.7456(6)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      24.980
_cell_measurement_theta_min      2.276
_cell_volume                     8156.0(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0668
_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       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83334
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.036
_diffrn_reflns_theta_max         25.036
_diffrn_reflns_theta_min         2.113
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1168 before and 0.0714 after correction.
The Ratio of minimum to maximum transmission is 0.8681.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.806
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 10447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.062(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1453
_refine_ls_number_reflns         28704
_refine_ls_number_restraints     496
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                25386
_reflns_number_total             28704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02570a2.cif
_cod_data_source_block           1
_cod_database_code               7130198
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.823
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C132-C88
 1.54 with sigma of 0.02
 C140-C104
 1.432 with sigma of 0.02
 H40-H14B
 2 with sigma of 0.02
 H2B-O2
 0.87 with sigma of 0.02
 O2-H2A
 0.87 with sigma of 0.02
 C114-C117
 1.45 with sigma of 0.02
 C114-C116 \\sim C114-C118
 with sigma of 0.02
 Dy1-H1A \\sim Dy1-H1B
 with sigma of 0.02
3. Rigid bond restraints
 C117, C118, C119, C120, C115, C116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C79, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C114 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim C115 \\sim C116: within
3.8A with sigma of 0.02 and sigma for terminal atoms of 0.01 within 3.8A
C93 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C121 \\sim
C133: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
C96 \\sim C109 \\sim C130 \\sim C111 \\sim C105 \\sim C107 \\sim C110: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C138 \\sim C139 \\sim C134 \\sim C135 \\sim C136 \\sim C137: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
5.a Everything fixed:
 C133, O3, H3A, O5, H5A, H5B, O6, H6A, H6B, O4, H4A, H4B, O8, H8A, H8B
5.b Riding coordinates:
 C127(H12A,H12B,H12C), C133(H13D,H13E,H13F), C142(H14G,H14H,H14I)
5.c Free rotating group:
 O1(H1A,H1B)
5.d Rotating group:
 O2(H2A,H2B)
5.e Ternary CH refined with riding coordinates:
 C13(H13), C36(H36), C39(H39), C40(H40), C43(H43), C60(H60), C74(H74), C93(H93)
5.f Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C15(H15), C16(H16),
 C18(H18), C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C41(H41),
 C42(H42), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52),
  C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C70(H70), C71(H71), C72(H72), C73(H73),
  C75(H75), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C89(H89), C90(H90), C91(H91),
  C92(H92), C95(H95), C97(H97), C99(H99), C100(H100), C102(H102), C103(H103),
 C105(H105), C106(H106), C108(H108), C109(H109), C111(H111), C112(H112),
 C115(H115), C116(H116), C119(H119), C120(H120), C123(H123), C124(H124),
 C125(H125), C126(H126), C128(H128), C129(H129), C130(H130), C131(H131),
 C134(H134), C135(H135), C136(H136), C137(H137), C139(H139)
5.g Fitted hexagon refined as free rotating group:
 C115(C116,C117,C118,C119,C120), C121(C122,C123,C124,C125,C126), C134(C135,
 C136,C137,C138,C139)
5.h Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C110(H11D,H11E,H11F), C113(H11A,H11B,H11C), C132(H13A,
 H13B,H13C), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F), C114(H11G,H11H,H11I)
5.i Idealised tetrahedral OH refined as rotating group:
 O7(H7A)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 1082 electrons were 
found in a volume of 2630\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
15[CH3OH] per Asymmetric Unit 
which account for 1080 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89981
_shelx_hkl_checksum              74519
_shelx_fab_checksum              48806
_olex2_submission_special_instructions 'No special instructions were received'