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_7045571
_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         'C34 H61 Dy O7, C7 H9 N'
_chemical_formula_sum            'C41 H70 Dy N O7'
_chemical_formula_weight         851.48
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-25
_audit_creation_method
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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                89.779(5)
_cell_angle_beta                 84.977(5)
_cell_angle_gamma                75.994(5)
_cell_formula_units_Z            2
_cell_length_a                   10.671(5)
_cell_length_b                   11.460(5)
_cell_length_c                   19.755(5)
_cell_measurement_reflns_used    8064
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4725
_cell_measurement_theta_min      3.5200
_cell_volume                     2334.6(16)
_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)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0742
_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       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19858
_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         27.500
_diffrn_reflns_theta_min         3.527
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.670
_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    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.850
_refine_diff_density_min         -3.235
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10702
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0657P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9164
_reflns_number_total             10702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04764a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045571--7045574.cif.'
_cod_database_code               7045571
_shelx_shelxl_version_number     2016/6
_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
 C19-C0AA \\sim C20-C19 \\sim C1AA-C19 \\sim C22-C19 \\sim C2AA-C19 \\sim
C21-C19
 with sigma of 0.02
3. Rigid bond restraints
 C20, C21, C22, C1AA, C0AA, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C22 \\sim C1AA \\sim C0AA \\sim C2AA: within 3.8A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C1AA, C20, C0AA, C21, C2AA, C22, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C1AA(0.5) H1AA(0.5)
 H1AB(0.5) H1AC(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)
7.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), 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), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C17(H17), C28(H28), C39(H39), C40(H40), C41(H41)
7.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C1AA(H1AA,H1AB,
 H1AC), C0AA(H0AA,H0AB,H0AC), C2AA(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              62788
_olex2_submission_special_instructions 'No special instructions were received'