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_7124482
_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 Gd2 O4 P4, C7 H8'
_chemical_formula_sum            'C86 H148 Br6 Gd2 O4 P4'
_chemical_formula_weight         2163.88
_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                90.982(12)
_cell_angle_beta                 94.971(12)
_cell_angle_gamma                113.756(11)
_cell_formula_units_Z            2
_cell_length_a                   13.453(5)
_cell_length_b                   15.414(6)
_cell_length_c                   24.917(10)
_cell_measurement_reflns_used    9657
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.321
_cell_measurement_theta_min      2.215
_cell_volume                     4704(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      152.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66353
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1000 before and 0.0671 after correction. The Ratio of minimum to maximum transmission is 0.6073. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.738
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         19017
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0433P)^2^+12.7567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15035
_reflns_number_total             19017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07552f2.cif
_cod_data_source_block           Gd2
_cod_database_code               7124482
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.620
_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. Rigid bond restraints
 O2, P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C25(H25), C7(H7), C37(H37), C19(H19), C1(H1), C31(H31), C13(H13), C55(H55),
 C67(H67), C43(H43), C61(H61), C49(H49)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C54(H54A,H54B), C65(H65A,H65B), C56(H56A,H56B), C60(H60A,H60B),
 C30(H30A,H30B), C62(H62A,H62B), C34(H34A,H34B), C20(H20A,H20B), C50(H50A,H50B),
  C27(H27A,H27B), C48(H48A,H48B), C18(H18A,H18B), C69(H69A,H69B), C68(H68A,
 H68B), C53(H53A,H53B), C32(H32A,H32B), C22(H22A,H22B), C33(H33A,H33B),
 C59(H59A,H59B), C29(H29A,H29B), C44(H44A,H44B), C70(H70A,H70B), C35(H35A,H35B),
  C2(H2A,H2B), C57(H57A,H57B), C23(H23A,H23B), C66(H66A,H66B), C51(H51A,H51B),
 C12(H12A,H12B), C72(H72A,H72B), C63(H63A,H63B), C21(H21A,H21B), C26(H26A,H26B),
  C58(H58A,H58B), C64(H64A,H64B), C8(H8A,H8B), C24(H24A,H24B), C38(H38A,H38B),
 C45(H45A,H45B), C14(H14A,H14B), C9(H9A,H9B), C36(H36A,H36B), C28(H28A,H28B),
 C46(H46A,H46B), C47(H47A,H47B), C42(H42A,H42B), C3(H3A,H3B), C71(H71A,H71B),
 C17(H17A,H17B), C52(H52A,H52B), C15(H15A,H15B), C40(H40A,H40B), C5(H5A,H5B),
 C39(H39A,H39B), C4(H4A,H4B), C10(H10A,H10B), C41(H41A,H41B), C11(H11A,H11B),
 C16(H16A,H16B)
3.c Aromatic/amide H refined with riding coordinates:
 C02H(H02H), C02K(H02K), C02N(H02N), C02P(H02P), C02Q(H02Q)
3.d Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              87948
_shelx_fab_checksum              24675
_olex2_submission_special_instructions 'No special instructions were received'