Opening Magnetic Hysteresis via Improving Planarity of Equatorial Coordination by Hydrogen Bonding
Qu, Yun-Xia; Ruan, Ze-Yu; Lyu, Bang-Heng; Chen, Yan-Cong; Huang, Guo-Zhang; Liu, Jun-Liang; Tong, Ming-Liang; Dalton Transactions  (2022) –; doi:10.1039/D2DT01107G

data_7710039
_publ_section_title
;
 Opening Magnetic Hysteresis via Improving Planarity of Equatorial
 Coordination by Hydrogen Bonding
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01107G
_journal_year                    2022
_chemical_formula_moiety
'C28 H38 Dy O7 P2, 3(I), 2(C18 H15 O P), 0.5(C2 H6 O), 0.5(H2 O)'
_chemical_formula_sum            'C65 H72 Dy I3 O10 P4'
_chemical_formula_weight         1680.30
_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             2021-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-12 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.623(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2644(5)
_cell_length_b                   23.3768(11)
_cell_length_c                   15.1012(7)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.476
_cell_measurement_theta_min      2.349
_cell_volume                     3521.6(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            77697
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.538
_diffrn_reflns_theta_min         2.220
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.519
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1433 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.6398.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1654
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.788
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.025(7)
_refine_ls_extinction_coef       0.00280(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         16091
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+2.6896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                15583
_reflns_number_total             16091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01107g2.cif
_cod_data_source_block           DyChain
_cod_database_code               7710039
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.590
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.975(7)
 0.025(7)
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, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C65-O10
 1.42 with sigma of 0.005
 C65-C66
 1.51 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O10 \\sim C65 \\sim C66: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(I3B)=1-FVAR(1)
 Sof(I3A)=FVAR(1)
 Fixed Sof: O10(0.5) H10A(0.5) C65(0.5) H65A(0.5) H65B(0.5) C66(0.5) H66A(0.5)
 H66B(0.5) H66C(0.5) O11(0.5) H11A(0.5) H11B(0.5)
6.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O10(H10A), O11(H11A,H11B)
6.b Rotating group:
 O5(H5A,H5B)
6.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C65(H65A,H65B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C28(H28),
  C27(H27), C26(H26), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
 C52(H52), C58(H58), C57(H57), C56(H56), C55(H55), C54(H54), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64)
6.e Fitted hexagon refined as free rotating group:
 C24(C23,C28,C27,C26,C25), C53(C58,C57,C56,C55,C54)
6.f Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C)
;
_shelx_res_checksum              80675
_olex2_submission_special_instructions 'No special instructions were received'