The influence of organic bases and substituted groups on coordination structures affording two mononuclear Dy(iii) single-molecule magnets (SMMs) and a novel Dy(iii)‒K(i) compound with unusually coordinated fluorine atoms
Shen, Nan; Liang, Jing; Qu, Xiaoni; Liu, Sha; Zhu, Lin; Zhang, Sheng; Chen, Ling; Zhang, Jiangwei; Hu, Dengwei; Yin, Bing; CrystEngComm 23 (2021) 4013–4027; doi:10.1039/D1CE00431J

data_7242717
_publ_section_title
;
 The influence of organic bases and substituted groups on coordination
 structures affording two mononuclear Dy(iii) single-molecule magnets
 (SMMs) and a novel Dy(iii)--K(i) compound with unusually coordinated
 fluorine atoms
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4013
_journal_page_last               4027
_journal_paper_doi               10.1039/D1CE00431J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C88 H66 Dy2 F24 K O16, C5 H6 N'
_chemical_formula_sum            'C93 H72 Dy2 F24 K N O16'
_chemical_formula_weight         2279.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                78.309(8)
_cell_angle_beta                 76.098(8)
_cell_angle_gamma                65.756(9)
_cell_formula_units_Z            1
_cell_length_a                   12.7036(11)
_cell_length_b                   12.9201(12)
_cell_length_c                   16.3475(15)
_cell_measurement_reflns_used    3247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.7830
_cell_measurement_theta_min      3.8690
_cell_volume                     2358.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  64.00   1.00    1.00    --    0.00  57.00  30.00   63
  2  \w      7.00  71.00   1.00    1.00    --    0.00  57.00 -60.00   64
  3  \w     30.00 129.00   1.00    1.00    --   56.49  45.00-150.00   99
  4  \w     90.00 121.00   1.00    1.00    --  112.98  77.00-120.00   31
  5  \w    109.00 136.00   1.00    1.00    --  112.98  63.00-120.00   27
  6  \w    151.00 178.00   1.00    1.00    --  112.98  63.00-120.00   27
  7  \w    138.00 165.00   1.00    1.00    --  112.98 111.00 -30.00   27
  8  \w    109.00 136.00   1.00    1.00    --  112.98 111.00 -30.00   27
  9  \w    106.00 150.00   1.00    1.00    --  112.98 111.00  60.00   44
 10  \w     82.00 133.00   1.00    1.00    --  112.98 178.00 150.00   51
 11  \w     40.00 175.00   1.00    1.00    --  112.98  12.00 150.00  135
 12  \w     80.00 116.00   1.00    1.00    --  112.98-111.00   0.00   36
 13  \w     51.00 145.00   1.00    1.00    --  112.98 -37.00  90.00   94
 14  \w     50.00 107.00   1.00    1.00    --  112.98-111.00 -60.00   57
 15  \w     91.00 116.00   1.00    1.00    --  112.98-111.00-180.00   25
 16  \w     48.00 139.00   1.00    1.00    --  112.98 -63.00 -90.00   91
 17  \w     42.00 155.00   1.00    1.00    --  112.98 -25.00-120.00  113
 18  \w     41.00  95.00   1.00    1.00    --  112.98 -50.00  90.00   54
 19  \w     46.00 153.00   1.00    1.00    --  112.98 -91.00 120.00  107
 20  \w     20.00 114.00   1.00    1.00    --   56.49-125.00  60.00   94
 21  \w     18.00  74.00   1.00    1.00    --   56.49-125.00 -30.00   56
 22  \w    -12.00  77.00   1.00    1.00    --   56.49 -61.00  60.00   89
 23  \w    -21.00   6.00   1.00    1.00    --    0.00  57.00 -60.00   27
 24  \w    -80.00 -46.00   1.00    1.00    --    0.00 178.00  90.00   34
 25  \w    -81.00 -12.00   1.00    1.00    --  -56.49  61.00 -90.00   69
 26  \w   -122.00 -85.00   1.00    1.00    --  -56.49 -94.00 -30.00   37
 27  \w   -122.00 -56.00   1.00    1.00    --  -56.49 -61.00 -30.00   66
 28  \w   -103.00 -76.00   1.00    1.00    --  -56.49-125.00-120.00   27
 29  \w   -107.00 -82.00   1.00    1.00    --  -56.49 -94.00-180.00   25
 30  \w   -119.00 -86.00   1.00    1.00    --  -56.49 -94.00 120.00   33
 31  \w     73.00 149.00   1.00    1.00    --  112.98 178.00-180.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1136510000
_diffrn_orient_matrix_UB_12      0.0307631000
_diffrn_orient_matrix_UB_13      -0.0338940000
_diffrn_orient_matrix_UB_21      0.0645033000
_diffrn_orient_matrix_UB_22      -0.0959229000
_diffrn_orient_matrix_UB_23      -0.0579428000
_diffrn_orient_matrix_UB_31      -0.0343044000
_diffrn_orient_matrix_UB_32      -0.0848103000
_diffrn_orient_matrix_UB_33      0.0710735000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.1332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15364
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.250
_diffrn_reflns_theta_max         67.250
_diffrn_reflns_theta_min         3.778
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         8444
_refine_ls_number_restraints     1950
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+2.1877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5320
_reflns_number_total             8444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00431j2.cif
_cod_data_source_block           exp_8457
_cod_depositor_comments
'Adding full bibliography for 7242716--7242718.cif.'
_cod_database_code               7242717
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.509
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Shared sites
{N1A, C1B}
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
Uanis(N1A) = Uanis(C1B)
Uanis(C1B) = Uanis(N1A)
4. Others
 Fixed Sof: C1B(0.5) H1B(0.5) H45A(0.5) H45(0.5) H46A(0.5) H46(0.5) N1A(0.5)
 H1A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C17(H17), C18(H18), C20(H20),
 C21(H21), C25(H25), C28(H28), C29(H29), C31(H31), C32(H32), C36(H36), C39(H39),
  C40(H40), C42(H42), C43(H43), C1B(H1B), C45(H45A), C45(H45), C46(H46A),
 C46(H46), N1A(H1A)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              19187
_shelx_hkl_checksum              72817
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.376
_oxdiff_exptl_absorpt_empirical_full_min 0.494