Single-molecule magnet behavior in a mononuclear dysprosium(iii) complex with 1-methylimidazole
Yao, Binling; Gu, Bin; Su, Meihui; Li, Guoliang; Ma, Yue; Li, Licun; Wang, Qinglun; Cheng, Peng; Zhang, Xuan; RSC Adv. 7 (2017) 2766–; doi:10.1039/C6RA25038F

data_7227425
_publ_section_title
;
 Single-molecule magnet behavior in a mononuclear dysprosium(iii) complex
 with 1-methylimidazole
;
_journal_issue                   5
_journal_name_full               'RSC Adv.'
_journal_page_first              2766
_journal_paper_doi               10.1039/C6RA25038F
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C23 H15 Dy F18 N4 O6'
_chemical_formula_sum            'C23 H15 Dy F18 N4 O6'
_chemical_formula_weight         947.89
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-09 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.88(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.103(4)
_cell_length_b                   10.649(2)
_cell_length_c                   18.062(4)
_cell_measurement_reflns_used    5549
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9064
_cell_measurement_theta_min      2.2102
_cell_volume                     3535.7(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
scan:
    Number of images: 90
               Slice: -110.0000 - 70.0000
         Image width: 2.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9977
              2theta: -19.9451
scan:
    Number of images: 70
               Slice: -110.0000 - 30.0000
         Image width: 2.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9977
              2theta: -19.9451
scan:
    Number of images: 60
               Slice: -110.0000 - 10.0000
         Image width: 2.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9977
              2theta: -19.9451
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0490
_diffrn_orient_matrix_UB_12      0.0224
_diffrn_orient_matrix_UB_13      -0.0075
_diffrn_orient_matrix_UB_21      -0.0408
_diffrn_orient_matrix_UB_22      -0.0809
_diffrn_orient_matrix_UB_23      0.0247
_diffrn_orient_matrix_UB_31      -0.0227
_diffrn_orient_matrix_UB_32      0.0265
_diffrn_orient_matrix_UB_33      0.0495
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14331
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.098
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0041(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         3147
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2705
_reflns_number_total             3151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra25038f2.cif
_cod_data_source_block           r101025c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7227425
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.662
_diffrn_number_total             4438
_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
 F7-F8 = F7-F9 = F8-F9 = F7'-F8' = F8'-F9' = F7'-F9'
 2.13 with sigma of 0.01
 C6-F7 = C6-F8 = C6-F9 = C6-F7' = C6-F8' = C6-F9'
 1.34 with sigma of 0.01
 F4-F5 = F4-F6 = F5-F6 = F4'-F5' = F4'-F6' = F5'-F6'
 2.13 with sigma of 0.01
 C5-F4 = C5-F5 = C5-F6 = C5-F4' = C5-F5' = C5-F6'
 1.34 with sigma of 0.01
 F1-F2 = F1-F3 = F2-F3 = F1'-F2' = F1'-F3' = F2'-F3'
 2.13 with sigma of 0.01
 C1-F1 = C1-F2 = C1-F3 = C1-F1' = C1-F2' = C1-F3'
 1.34 with sigma of 0.01
3. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1') \\sim
Ueq, Uanis(F2') \\sim Ueq, Uanis(F3') \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4') \\sim
Ueq, Uanis(F5') \\sim Ueq, Uanis(F6') \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F7') \\sim
Ueq, Uanis(F8') \\sim Ueq, Uanis(F9') \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F7')=Sof(F8')=Sof(F9')=1-FVAR(3)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C11(H11)
6.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'