Trigonal bipyramidal CoDy<sub>3</sub> cluster exhibiting single-molecule magnet behavior.
Lun, Hui-Jie; Kong, Xiang-Jian; Long, La-Sheng; Zheng, Lan-Sun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2421–2425; doi:10.1039/c9dt04600c

data_7703483
_publ_section_title
;
 Trigonal bipyramidal CoDy<sub>3</sub> cluster exhibiting single-molecule
 magnet behavior.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2421
_journal_page_last               2425
_journal_paper_doi               10.1039/c9dt04600c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H38 Co2 Dy3 N4 Na O32, H2 O'
_chemical_formula_sum            'C18 H40 Co2 Dy3 N4 Na O33'
_chemical_formula_weight         1468.89
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-21 deposited with the CCDC.	2020-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.3027(2)
_cell_length_b                   25.3027(2)
_cell_length_c                   25.8582(3)
_cell_measurement_reflns_used    10927
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9450
_cell_measurement_theta_min      3.4920
_cell_volume                     16555.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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    -68.00  23.00   1.00    4.00    --  -46.75  72.00 -50.00   91
  2  \w   -118.00 -79.00   1.00    4.00    --  -46.75-125.00 -60.00   39
  3  \w   -158.00-131.00   1.00   12.00    --  -88.50-118.00 105.00   27
  4  \w     35.00  78.00   1.00   12.00    --  107.31-125.00  60.00   43
  5  \w     38.00  85.00   1.00   12.00    --  107.31 -94.00   0.00   47
  6  \w     93.00 178.00   1.00   12.00    --  107.31  45.00  60.00   85
  7  \w     86.00 177.00   1.00   12.00    --  107.31  72.00 -50.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517302000
_diffrn_orient_matrix_UB_12      -0.0244312000
_diffrn_orient_matrix_UB_13      -0.0204587000
_diffrn_orient_matrix_UB_21      -0.0311276000
_diffrn_orient_matrix_UB_22      -0.0279987000
_diffrn_orient_matrix_UB_23      -0.0432578000
_diffrn_orient_matrix_UB_31      0.0081514000
_diffrn_orient_matrix_UB_32      0.0482044000
_diffrn_orient_matrix_UB_33      -0.0354714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22488
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.991
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    35.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'greenish violet'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_description       block
_exptl_crystal_F_000             11248
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Flack x determined using 2770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(4)
_refine_ls_extinction_coef       0.0000048(18)
_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   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     733
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+257.9985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.859
_reflns_Friedel_fraction_max     0.845
_reflns_number_gt                6755
_reflns_number_total             7245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04600c2.cif
_cod_data_source_block           exp_3468
_cod_depositor_comments          'Adding full bibliography for 7703483.cif.'
_cod_database_code               7703483
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C8-C9
 1.48 with sigma of 0.02
 C15-C14
 1.48 with sigma of 0.02
 C15-C14 \\sim C9-C8 \\sim C3-C2 \\sim C6-C5 \\sim C18-C17 \\sim C12-C11
 with sigma of 0.01
 C11-C10 \\sim C14-C13 \\sim C17-C16 \\sim C5-C4 \\sim C2-C1 \\sim C8-C7
 with sigma of 0.01
 C11-C10 \\sim C12-C11
 with sigma of 0.005
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2W
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.001
O2W: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: O29'(0.5) O30'(0.5) N4'(0.5) N4(0.5) O29(0.5) O30(0.5)
6.a Free rotating group:
 O2W(H2WA,H2WB)
6.b Rotating group:
 O1W(H1WA,H1WB)
6.c Ternary CH refined with riding coordinates:
 O4(H4), O6(H6), O1(H1), O5(H5), O2(H2), O3(H3)
6.d Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C2(H2A,H2B), C14(H14A,H14B), C5(H5A,H5B), C11(H11A,H11B),
 C8(H8A,H8B)
6.e Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C18(H18A,H18B,H18C), C3(H3A,H3B,H3C), C15(H15A,H15B,H15C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C)
;
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.763