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_7045572
_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         'C38 H63 Dy N O7'
_chemical_formula_sum            'C38 H63 Dy N O7'
_chemical_formula_weight         808.39
_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             2018-01-29
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.102(5)
_cell_length_b                   17.263(5)
_cell_length_c                   24.347(5)
_cell_measurement_reflns_used    3255
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3637
_cell_measurement_theta_min      3.2087
_cell_volume                     4246(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  0.0316
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11202
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.215
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.655
_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    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.501
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6279
_reflns_number_total             7122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04764a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7045571--7045574.cif.'
_cod_database_code               7045572
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56(2)
 0.44(2)
2. 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
3. Restrained distances
 H3-H3AA
 2.45 with sigma of 0.01
 C5-C34 \\sim C35-C5 \\sim C36-C5 \\sim C3AA-C5 \\sim C4AA-C5 \\sim C6-C5
 with sigma of 0.02
 C10-C40 \\sim C41-C10 \\sim C42-C10 \\sim C5AA-C10 \\sim C6AA-C10 \\sim
C7AA-C10
 with sigma of 0.02
 C46-C43 \\sim C44-C46 \\sim C45-C46 \\sim C8AA-C46 \\sim C9AA-C46 \\sim
C0BA-C46
 with sigma of 0.02
 C31-C32 \\sim C32-C33 \\sim C33-C31
 with sigma of 0.02
 C1-C31 \\sim C1-C32 \\sim C1-C33 \\sim C1-C0AA \\sim C1-C1AA \\sim C1-C2AA
 with sigma of 0.02
 C0AA-C1AA \\sim C1AA-C2AA \\sim C2AA-C0AA
 with sigma of 0.02
4. Rigid bond restraints
 C2AA, C1AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C2AA \\sim C1AA: within 2.8A with sigma of 0.014 and sigma for terminal atoms
of 0.028
6. Rigid body (RIGU) restrains
 C5, C34, C35, C36, C3AA, C4AA, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C40, C41, C42, C5AA, C6AA, C7AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, C44, C43, C45, C8AA, C9AA, C0BA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C31, C32, C33, C0AA, C1AA, C2AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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) C34(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C36(0.5) H36A(0.5)
 H36B(0.5) H36C(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(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) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) H45C(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C2AA(0.5)
 H2AA(0.5) H2AB(0.5) H2AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) H6C(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) C6AA(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5)
 C5AA(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) C7AA(0.5) H7AA(0.5) H7AB(0.5)
 H7AC(0.5) C0BA(0.5) H0BA(0.5) H0BB(0.5) H0BC(0.5) C9AA(0.5) H9AA(0.5)
 H9AB(0.5) H9AC(0.5) C8AA(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C30(H30)
8.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C0AA(H0AA,H0AB,H0AC), C2AA(H2AA,H2AB,H2AC), C1AA(H1AA,H1AB,H1AC), C6(H6A,H6B,
 H6C), C4AA(H4AA,H4AB,H4AC), C3AA(H3AA,H3AB,H3AC), C6AA(H6AA,H6AB,H6AC),
 C5AA(H5AA,H5AB,H5AC), C7AA(H7AA,H7AB,H7AC), C0BA(H0BA,H0BB,H0BC), C9AA(H9AA,
 H9AB,H9AC), C8AA(H8AA,H8AB,H8AC)
9.the hydrogen atom of t-Bu in which be split into two PARTS  The  DAMP Command was used to solve non-convergence.
;
_shelx_res_checksum              4376
_olex2_submission_special_instructions 'No special instructions were received'