Structurally modulated single-ion magnets of mononuclear β-diketone dysprosium(III) complexes.
Kong, Ming; Feng, Xin; Li, Jing; Hu, Zhao-Bo; Wang, Jia; Song, Xiao-Jiao; Jing, Zhao-Yang; Zhang, Yi-Quan; Song, You; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14931–14940; doi:10.1039/d0dt02864a

data_7705585
_publ_section_title
;
 Structurally modulated single-ion magnets of mononuclear \b-diketone
 dysprosium(III) complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14931
_journal_page_last               14940
_journal_paper_doi               10.1039/d0dt02864a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C51 H28 Dy F9 N4 O6 S3, 0.5(C2 H6 O), 0.5(H2 O)'
_chemical_formula_sum            'C52 H32 Dy F9 N4 O7 S3'
_chemical_formula_weight         1254.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-01 deposited with the CCDC.	2020-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.986(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6667(12)
_cell_length_b                   19.2642(18)
_cell_length_c                   41.493(4)
_cell_measurement_reflns_used    7789
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      47.90
_cell_measurement_theta_min      3.45
_cell_volume                     10917.6(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      192.95
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            29955
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.879
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1203 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.6849.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         9395
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+127.9688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5359
_reflns_number_total             9395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02864a2.cif
_cod_data_source_block           m_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7705582--7705586.cif.'
_cod_original_cell_volume        10917.8(17)
_cod_database_code               7705585
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C49-C50
 1.43 with sigma of 0.02
 C49-C48 = C50-C49 = C51-C50 = C51-C3A = C48-C3A
 1.43 with sigma of 0.01
 S3-C51 = S3-C48 = S49A-C48 = S49A-C50
 1.65 with sigma of 0.01
 O7-H7A
 0.82 with sigma of 0.02
 C53-O8
 1.43 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
 H52A-H2
 2.2 with sigma of 0.02
 H52B-H2
 2.2 with sigma of 0.02
3. Restrained planarity
 C3A, C51, C48, S49A, C50
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C48 \\sim C49 \\sim C50 \\sim C51 \\sim S3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C49 \\sim S3 \\sim C48 \\sim C51 \\sim C50 \\sim C3A \\sim S49A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C2 \\sim C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C52 \\sim O8 \\sim C53: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C5 \\sim C10 \\sim C9 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C8 \\sim
C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C32 \\sim C33 \\sim C34 \\sim C35 \\sim S1: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(S3) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C49) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(S49A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C49, S3, C48, C51, C50, C3A, S49A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(H51A)=Sof(H50A)=Sof(C3A)=Sof(H3A)=Sof(S49A)=1-FVAR(1)
 Sof(C49)=Sof(H49)=Sof(S3)=Sof(H51)=Sof(H50)=FVAR(1)
 Fixed Sof: C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) O8(0.5) H8(0.5) H7B(0.5)
7.a Riding coordinates:
 O8(H8), O7(H7A,H7B)
7.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B)
7.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C27(H27), N2(H2), C46(H46), C38(H38), C51(H51), C51(H51A), C30(H30),
  C21(H21), C25(H25), C26(H26), C34(H34), C20(H20), C2(H2A), C41(H41), C1(H1),
 C19(H19), C33(H33), C11(H11), C43(H43), C35(H35), C3(H3), C4(H4), C42(H42),
 C12(H12), C14(H14), C13(H13), C10(H10), C50(H50), C50(H50A), C3A(H3A)
7.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              38792
_olex2_submission_special_instructions 'No special instructions were received'