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_7045574
_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         'C51 H73 Dy O7 P'
_chemical_formula_sum            'C51 H73 Dy O7 P'
_chemical_formula_weight         991.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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(5)
_cell_angle_beta                 104.739(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   11.474(5)
_cell_length_b                   21.516(5)
_cell_length_c                   22.125(5)
_cell_measurement_reflns_used    20272
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6146
_cell_measurement_theta_min      3.4130
_cell_volume                     5282(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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0322
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45629
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         3.420
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.728
_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             2064
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         12670
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0252P)^2^+6.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10317
_reflns_number_total             12670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04764a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045571--7045574.cif.'
_cod_database_code               7045574
_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, All O(H) groups
2. Restrained distances
 O7-H7A
 0.85 with sigma of 0.01
 P1-H7A
 1.941176 with sigma of 0.02
 Dy1-H7A
 2.367589 with sigma of 0.02
 C55-C0AA \\sim C56-C55 \\sim C1AA-C55 \\sim C57-C55 \\sim C2AA-C55 \\sim
C58-C55
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C55, C56, C57, C58, C0AA, C1AA, C2AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H6(0) H12(0) H18(0) H22(0) H24(0) H27(0) H29(0) H52(0) H54(0)
 C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5)
 C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(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)
5.a Me refined with riding coordinates:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29),
 C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C2AA(H2AA,H2AB,
 H2AC), C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              34691
_olex2_submission_special_instructions 'No special instructions were received'