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_7130199
_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_absolute_configuration ad
_chemical_formula_moiety         'C46 H44 Dy F2 N6 O, C24 H20 B, 2(C H4 O)'
_chemical_formula_sum            'C72 H72 B Dy F2 N6 O3'
_chemical_formula_weight         1280.66
_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
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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                 96.1420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7039(4)
_cell_length_b                   23.7837(7)
_cell_length_c                   20.8546(6)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      25.011
_cell_measurement_theta_min      2.379
_cell_volume                     8237.6(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84217
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.106
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1097 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.7555.
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    1.033
_exptl_crystal_description       block
_exptl_crystal_F_000             2636
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 12041 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.073(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1500
_refine_ls_number_reflns         28919
_refine_ls_number_restraints     632
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+4.1312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                26868
_reflns_number_total             28919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02570a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7130199
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
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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
 C139-C101
 1.532 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C102 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C139:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C119 \\sim C120 \\sim C121 \\sim C122 \\sim C117 \\sim C118 \\sim C136: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C51 \\sim C58 \\sim C105 \\sim C88 \\sim C132 \\sim C129 \\sim C138: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C47 \\sim C63 \\sim C113 \\sim C126 \\sim C131 \\sim C104 \\sim C140: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C108 \\sim C109 \\sim C110 \\sim C111 \\sim C106 \\sim C107 \\sim C134: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(Dy1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Everything fixed:
 O4, H4A
4.b Riding coordinates:
 C138(H13G,H13H,H13I), C139(H13M,H13N,H13O), C1(H1C,H1D,H1E)
4.c Rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
4.d Ternary CH refined with riding coordinates:
 C19(H19), C29(H29), C45(H45), C46(H46), C61(H61), C68(H68), C82(H82), C93(H93)
4.e Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C27(H27), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36),
 C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C48(H48), C49(H49), C50(H50),
  C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60),
 C62(H62), C63(H63), C64(H64), C67(H67), C69(H69), C70(H70), C71(H71), C72(H72),
  C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C80(H80), C81(H81),
 C83(H83), C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91),
  C92(H92), C94(H94), C95(H95), C97(H97), C98(H98), C99(H99), C100(H100),
 C103(H103), C105(H105), C106(H106), C109(H109), C110(H110), C111(H111),
 C112(H112), C113(H113), C114(H114), C115(H115), C117(H117), C120(H120),
 C121(H121), C122(H122), C123(H123), C125(H125), C126(H126), C127(H127),
 C128(H128), C131(H131), C132(H132), C133(H133), C135(H135), C137(H137)
4.f Fitted hexagon refined as free rotating group:
 C97(C98,C99,C100,C101,C102), C106(C107,C108,C109,C110,C111), C117(C118,C119,
 C120,C121,C122)
4.g Idealised Me refined as rotating group:
 C116(H11A,H11B,H11C), C130(H13A,H13B,H13C), C134(H13J,H13K,H13L), C136(H13D,
 H13E,H13F), C140(H14D,H14E,H14F), C141(H14A,H14B,H14C), C142(H14G,H14H,H14I),
 C143(H14J,H14K,H14L), C144(H14M,H14N,H14O)
4.h Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O6(H6), O3(H3)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 562 electrons were 
found in a volume of 2784\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
7.5[CH3OH] per Asymmetric Unit 
which account for 540 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25199
_shelx_hkl_checksum              75958
_shelx_fab_checksum              67495
_olex2_submission_special_instructions 'No special instructions were received'