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_7057230
_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         'C51 H68 Dy N4 O6'
_chemical_formula_sum            'C51 H68 Dy N4 O6'
_chemical_formula_weight         995.59
_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                96.749(5)
_cell_angle_beta                 102.977(5)
_cell_angle_gamma                110.251(5)
_cell_formula_units_Z            2
_cell_length_a                   10.928(5)
_cell_length_b                   12.363(5)
_cell_length_c                   21.554(5)
_cell_measurement_reflns_used    4828
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4769
_cell_measurement_theta_min      3.0630
_cell_volume                     2600.8(17)
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.1026
_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       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21896
_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         27.500
_diffrn_reflns_theta_min         3.069
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.837
_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_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         11926
_refine_ls_number_restraints     424
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.9416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7057
_reflns_number_total             11926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00636a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7057229--7057232.cif.'
_cod_database_code               7057230
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C43A \\sim C43-C21 \\sim C42A-C21 \\sim C41-C21 \\sim C41A-C21 \\sim
C42-C21
 with sigma of 0.02
 C30-C54A \\sim C54-C30 \\sim C56A-C30 \\sim C55-C30 \\sim C55A-C30 \\sim
C56-C30
 with sigma of 0.02
3. Rigid bond restraints
 C16, H16, C17, C18, C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43A, C43, C42A, C41, C41A, C42, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54A, C54, C56A, C55, C55A, C56, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C16 \\sim H16 \\sim C17 \\sim C18 \\sim C22 \\sim C23: within 3.8A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C43A \\sim C43 \\sim C42A \\sim C41 \\sim C41A \\sim C42 \\sim C21: within 3.8A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C54A \\sim C54 \\sim C56A \\sim C55 \\sim C55A \\sim C56 \\sim C30: within 3.8A
with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C43A, C43, C42A, C41, C41A, C42, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54A, C54, C56A, C55, C55A, C56, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: 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) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5)
 H55A(0.5) H55B(0.5) H55C(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C54A(0.5)
 H54D(0.5) H54E(0.5) H54F(0.5) C55A(0.5) H55D(0.5) H55E(0.5) H55F(0.5)
 C56A(0.5) H56D(0.5) H56E(0.5) H56F(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C18(H18), C23(H23), C28(H28), C33(H33), N4(H4)
7.b Idealised Me refined as rotating group:
 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), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F),
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              55976
_olex2_submission_special_instructions 'No special instructions were received'