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_7710038
_publ_section_title
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 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
'C42 H52 Dy O8 P3, 3(I), C28 H28 O2 P2, H2 O, C2 H6 O'
_chemical_formula_sum            'C72 H88 Dy I3 O12 P5'
_chemical_formula_weight         1843.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-05 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.264(2)
_cell_angle_beta                 98.186(2)
_cell_angle_gamma                102.180(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6227(5)
_cell_length_b                   13.5467(5)
_cell_length_c                   23.6777(11)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.361
_cell_measurement_theta_min      2.494
_cell_volume                     3825.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v2016.1-0'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      119.99
_diffrn_detector                 'Bruker PHOTON 100 CMOS detector'
_diffrn_detector_type            'CMOS active pixel sensor detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 QUEST'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66147
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'I\mS microfocus'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'I\mS microfocus'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.348
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1126 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.8700.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         14046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+2.6283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12007
_reflns_number_total             14046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01107g2.cif
_cod_data_source_block           C72H88DyI3O12P5
_cod_database_code               7710038
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C69(H69A,H69B), C70(H70A,H70B),
 C72(H72A,H72B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68)
2.c Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C)
;
_shelx_res_checksum              20679
_olex2_submission_special_instructions 'No special instructions were received'