Investigation of magneto-structural correlation based on a series of seven-coordinated β-diketone Dy(iii) single-ion magnets with C<sub>2v</sub> and C<sub>3v</sub> local symmetry.
Yao, Xu; Yan, Pengfei; An, Guanghui; Li, Yuxin; Li, Weizuo; Li, Guangming; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3976–3984; doi:10.1039/c7dt04764a

data_7045573
_publ_section_title
;
 Investigation of magneto-structural correlation based on a series of
 seven-coordinated \b-diketone Dy(iii) single-ion magnets with
 C<sub>2v</sub> and C<sub>3v</sub> local symmetry.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3976
_journal_page_last               3984
_journal_paper_doi               10.1039/c7dt04764a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C39 H62 Dy N O7'
_chemical_formula_sum            'C39 H62 Dy N O7'
_chemical_formula_weight         819.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-01 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   10.061(5)
_cell_length_b                   18.089(5)
_cell_length_c                   23.985(5)
_cell_measurement_reflns_used    4311
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1354
_cell_measurement_theta_min      3.1391
_cell_volume                     4365(3)
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12576
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.145
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.745
_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    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 2707 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7551
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                6850
_reflns_number_total             7551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04764a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7045571--7045574.cif.'
_cod_database_code               7045573
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 C1-C31 \\sim C32-C1 \\sim C33-C1 \\sim C0AA-C1 \\sim C1AA-C1 \\sim C50-C1
 with sigma of 0.02
 C6-C37 \\sim C38-C6 \\sim C39-C6 \\sim C2AA-C6 \\sim C3AA-C6 \\sim C4AA-C6
 with sigma of 0.02
 C11-C34 \\sim C35-C11 \\sim C36-C11 \\sim C5AA-C11 \\sim C6AA-C11 \\sim C45-C11
 with sigma of 0.02
3. Rigid bond restraints
 C10, C28, C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C25, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C10 \\sim C28 \\sim C29 \\sim C30: within 3.8A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C15 \\sim C25 \\sim C26 \\sim C27: within 3.8A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C1, C31, C32, C33, C0AA, C1AA, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C37, C38, C39, C2AA, C3AA, C4AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C34, C35, C36, C5AA, C6AA, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. 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) C35(0.5) H35A(0.5)
 H35B(0.5) H35C(0.5) C36(0.5) H36A(0.5) H36B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5)
 C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
 C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C4AA(0.5) H4AA(0.5) H4AB(0.5)
 H4AC(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C5AA(0.5) H5AA(0.5)
 H5AB(0.5) H5AC(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) C45(0.5) H45A(0.5) H45B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C34(H34A,H34B), C6AA(H6AA,H6AB), C45(H45A,H45B)
7.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19)
7.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C50(H50A,H50B,H50C), C2AA(H2AA,
 H2AB,H2AC), C4AA(H4AA,H4AB,H4AC), C3AA(H3AA,H3AB,H3AC), C5AA(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              92339
_olex2_submission_special_instructions 'No special instructions were received'