Regulating the magnetic dynamics of mononuclear β-diketone Dy(iii) single-molecule magnets through the substitution effect on capping N-donor coligands.
Xi, Jing; Ma, Xiufang; Cen, Peipei; Wu, Yuewei; Zhang, Yi-Quan; Guo, Yan; Yang, Jinhui; Chen, Lei; Liu, Xiangyu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2102–2111; doi:10.1039/d0dt03780j

data_7706391
_publ_section_title
;
 Regulating the magnetic dynamics of mononuclear \b-diketone Dy(iii)
 single-molecule magnets through the substitution effect on capping
 N-donor coligands.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2102
_journal_page_last               2111
_journal_paper_doi               10.1039/d0dt03780j
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C52 H31 Br Dy F9 N2 O6'
_chemical_formula_sum            'C52 H31 Br Dy F9 N2 O6'
_chemical_formula_weight         1193.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.699(5)
_cell_length_b                   11.435(3)
_cell_length_c                   20.275(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      2.65
_cell_volume                     4799(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43228
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_min         2.035
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 3264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         10550
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.5336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                8217
_reflns_number_total             10550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03780j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7706390--7706394.cif.'
_cod_original_cell_volume        4799.0(19)
_cod_database_code               7706391
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.755
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F3A-C1 \\sim F3-C1 \\sim F1A-C1 \\sim F1-C1 \\sim F2A-C1 \\sim F2-C1
 with sigma of 0.02
 F3A-F2A \\sim F3A-F1A \\sim F2A-F1A
 with sigma of 0.02
 F1A-C2 \\sim F3A-C2 \\sim F2A-C2
 with sigma of 0.02
 F3-F2 \\sim F3-F1 \\sim F2-F1
 with sigma of 0.02
 F3-C2 \\sim F2-C2 \\sim F1-C2
 with sigma of 0.02
 F9A-C29 \\sim F9-C29 \\sim F8A-C29 \\sim F8-C29 \\sim F7A-C29 \\sim F7-C29
 with sigma of 0.02
 F9A-F8A \\sim F9A-F7A \\sim F8A-F7A
 with sigma of 0.02
 F8A-C30 \\sim F7A-C30 \\sim F9A-C30
 with sigma of 0.02
 F9-F7 \\sim F8-F7 \\sim F9-F8
 with sigma of 0.02
 F9-C30 \\sim F8-C30 \\sim F7-C30
 with sigma of 0.02
 F6A-F4A \\sim F6A-F5A \\sim F5A-F4A
 with sigma of 0.02
 F6A-C16 \\sim F5A-C16 \\sim F4A-C16
 with sigma of 0.02
 F6-F5 \\sim F5-F4 \\sim F6-F4
 with sigma of 0.02
 F5-C16 \\sim F6-C16 \\sim F4-C16
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C4, C5, C6, C7, C8, C11, C12, C13, C14, C9, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1, F3, F2, F1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1, F3A, F2A, F1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F8A, C29, F9A, F7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C29, F7, F8, F9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C15, F6, F4, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F6A, C15, F5A, F4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F1A)=Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F9A)=Sof(F7A)=Sof(F8A)=1-FVAR(3)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C6(H6), C7(H7), C14(H14), C13(H13), C12(H12), C11(H11),
 C17(H17), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C31(H31), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C52(H52)
5.b Naphthalene refined as free rotating group:
 C10(C5,C6,C7,C8,C9,C14,C13,C12,C11)
;
_shelx_res_checksum              83170
_olex2_submission_special_instructions 'No special instructions were received'