Bromine-bridged Dy2 single-molecule magnet: magnetic anisotropy driven by cis/trans stereoisomers
Li, Min; Wu, Haipeng; Xia, Zhengqiang; Montigaud, Vincent; Cador, Olivier; Le Guennic, Boris; Ke, Hongshan; Wang, Wenyuan; Xie, Gang; Chen, Sanping; Chemical Communications  (2019) –; doi:10.1039/C9CC07552F

data_7124481
_publ_section_title
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 Bromine-bridged Dy2 single-molecule magnet: magnetic anisotropy driven by
 cis/trans stereoisomers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07552F
_journal_year                    2019
_chemical_formula_moiety         'C72 H132 Br6 Dy2 O4 P4, C7 H8'
_chemical_formula_sum            'C86 H148 Br6 Dy2 O4 P4'
_chemical_formula_weight         2174.38
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-26 deposited with the CCDC.	2019-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                91.038(2)
_cell_angle_beta                 94.840(2)
_cell_angle_gamma                113.840(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4056(6)
_cell_length_b                   15.3549(6)
_cell_length_c                   24.7629(12)
_cell_measurement_reflns_used    9177
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.94
_cell_volume                     4638.1(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            123871
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.598
_diffrn_reflns_theta_min         2.848
_exptl_absorpt_coefficient_mu    4.297
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1045 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.6650. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.152
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         21374
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0256P)^2^+14.4994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16973
_reflns_number_total             21374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07552f2.cif
_cod_data_source_block           Dy2
_cod_database_code               7124481
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.605
_shelx_estimated_absorpt_t_min   0.529
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C77) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 C23, C22, C24, C19, C20, C21, C76, C75, C74, C73, C79, C78, C77
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C43(H43), C37(H37), C67(H67), C1(H1), C55(H55), C61(H61), C31(H31), C24(H24),
 C25(H25), C49(H49), C13(H13), C7(H7)
4.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C53(H53A,H53B), C52(H52A,H52B), C50(H50A,H50B), C51(H51A,
 H51B), C46(H46A,H46B), C45(H45A,H45B), C44(H44A,H44B), C48(H48A,H48B),
 C47(H47A,H47B), C56(H56A,H56B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C42(H42A,H42B), C41(H41A,H41B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,
 H70B), C71(H71A,H71B), C72(H72A,H72B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C57(H57A,H57B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
  C65(H65A,H65B), C66(H66A,H66B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C30(H30A,H30B), C29(H29A,H29B),
  C28(H28A,H28B), C27(H27A,H27B), C26(H26A,H26B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C18(H18A,H18B), C17(H17A,H17B),
 C16(H16A,H16B), C15(H15A,H15B), C14(H14A,H14B), C12(H12A,H12B), C11(H11A,H11B),
  C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B)
4.c Aromatic/amide H refined with riding coordinates:
 C77(H77), C78(H78), C79(H79), C76(H76), C75(H75)
4.d Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C)
;
_shelx_res_checksum              85441
_shelx_fab_checksum              91203
_olex2_submission_special_instructions 'No special instructions were received'