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_7057231
_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         'C45 H65 Dy N2 O6'
_chemical_formula_sum            'C45 H65 Dy N2 O6'
_chemical_formula_weight         892.49
_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                79.895(5)
_cell_angle_beta                 87.642(5)
_cell_angle_gamma                68.779(5)
_cell_formula_units_Z            2
_cell_length_a                   11.051(5)
_cell_length_b                   12.325(5)
_cell_length_c                   18.666(5)
_cell_measurement_reflns_used    7593
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5436
_cell_measurement_theta_min      3.2594
_cell_volume                     2332.5(16)
_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 0.997
_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  0.0240
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18706
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.266
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.692
_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    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10700
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0294P)^2^+0.7239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9309
_reflns_number_total             10700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00636a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7057229--7057232.cif.'
_cod_database_code               7057231
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.703
_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
 C13-C31 \\sim C33A-C13 \\sim C32-C13 \\sim C32A-C13 \\sim C33-C13 \\sim
C31A-C13
 with sigma of 0.02
 C18-C42A \\sim C42-C18 \\sim C43A-C18 \\sim C43-C18 \\sim C41A-C18 \\sim
C41-C18
 with sigma of 0.02
 C23-C53A \\sim C51-C23 \\sim C51A-C23 \\sim C53-C23 \\sim C52A-C23 \\sim
C52-C23
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C31, C33A, C32, C32A, C33, C31A, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42A, C42, C43A, C43, C41A, C41, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53A, C51, C51A, C53, C52A, C52, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C31A(0.5) H31D(0.5)
 H31E(0.5) H31F(0.5) C32A(0.5) H32D(0.5) H32E(0.5) H32F(0.5) C33A(0.5)
 H33D(0.5) H33E(0.5) H33F(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C41A(0.5)
 H41D(0.5) H41E(0.5) H41F(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5)
 C43A(0.5) H43D(0.5) H43E(0.5) H43F(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5)
 C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5)
 C51A(0.5) H51D(0.5) H51E(0.5) H51F(0.5) C52A(0.5) H52D(0.5) H52E(0.5)
 H52F(0.5) C53A(0.5) H53D(0.5) H53E(0.5) H53F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C20(H20), C25(H25)
5.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C31A(H31D,H31E,
 H31F), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C41A(H41D,H41E,H41F), C42A(H42D,H42E,H42F),
 C43A(H43D,H43E,H43F), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              25183
_olex2_submission_special_instructions 'No special instructions were received'