Single-ion magnets with D4d symmetry based on electron-donating β-diketonate Dy(iii) complexes
Yao, Xu; Yan, Pengfei; An, Guanghui; Shi, Chao; Li, Yuxin; Li, Guangming; New Journal of Chemistry 42 (2018) 8438–; doi:10.1039/C8NJ00636A

data_7057229
_publ_section_title
;
 Single-ion magnets with D4d symmetry based on electron-donating
 \b-diketonate Dy(iii) complexes
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8438
_journal_paper_doi               10.1039/C8NJ00636A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C35 H63 Dy O8'
_chemical_formula_sum            'C35 H63 Dy O8'
_chemical_formula_weight         774.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-28 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                65.115(5)
_cell_angle_beta                 72.713(5)
_cell_angle_gamma                75.622(5)
_cell_formula_units_Z            2
_cell_length_a                   10.678(5)
_cell_length_b                   13.945(5)
_cell_length_c                   16.534(5)
_cell_measurement_reflns_used    6285
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6589
_cell_measurement_theta_min      3.0534
_cell_volume                     2110.8(14)
_computing_data_collection       'Bruker FRAMBO'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  MoK\a
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17638
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.059
_exptl_absorpt_coefficient_mu    1.810
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9689
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0477P)^2^+0.8670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8034
_reflns_number_total             9689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00636a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7057229--7057232.cif.'
_cod_database_code               7057229
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.671
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C21A \\sim C23-C3 \\sim C22-C3 \\sim C22A-C3 \\sim C23A-C3 \\sim C21-C3
 with sigma of 0.02
 C7-C25A \\sim C25-C7 \\sim C24A-C7 \\sim C26-C7 \\sim C26A-C7 \\sim C24-C7
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C21A, C23, C22A, C22, C23A, C21, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25A, C25, C24A, C26, C26A, C24, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C22A(0.5) H22D(0.5)
 H22E(0.5) H22F(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C21A(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C24A(0.5)
 H24D(0.5) H24E(0.5) H24F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5)
 C26A(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C21A(H21D,H21E,H21F),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C24A(H24D,H24E,
 H24F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C31A(H31A,H31B,H31C),
 C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              31316
_olex2_submission_special_instructions 'No special instructions were received'