A double-dysprosocenium single-molecule magnet bound together with neutral ligands.
Evans, Peter; Reta, Daniel; Goodwin, Conrad A. P.; Ortu, Fabrizio; Chilton, Nicholas F.; Mills, David P.; Chemical communications (Cambridge, England) 56 (2020) 5677–5680; doi:10.1039/c9cc08945d

data_7126383
_publ_section_title
;
 A double-dysprosocenium single-molecule magnet bound together with
 neutral ligands.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5677
_journal_page_last               5680
_journal_paper_doi               10.1039/c9cc08945d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C58 H108 Al2 Dy2 N2, 3(C6 H5 Cl), 2(Al C16 F36 O4)'
_chemical_formula_sum            'C108 H123 Al4 Cl3 Dy2 F72 N2 O8'
_chemical_formula_weight         3484.35
_chemical_name_systematic        '[Dy(Cp*)2(Et3NAlMe3)][Al(OC(CF3)3)4]'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-06 deposited with the CCDC.	2020-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.720(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8684(3)
_cell_length_b                   30.4814(7)
_cell_length_c                   16.1283(5)
_cell_measurement_reflns_used    15048
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      75.8190
_cell_measurement_theta_min      3.0460
_cell_volume                     6756.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (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      100.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.936
_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     65.00  94.00   0.50    0.50    --   44.70  60.00 -30.00   58
  2  \w     42.00 133.00   0.50    0.50    --   44.70  40.00 -90.00  182
  3  \w    108.00 133.00   0.50    0.50    --   44.70  10.00 -90.00   50
  4  \w    -45.00 -18.00   0.50    0.50    --   44.70  60.00 -30.00   54
  5  \w    -44.00 134.00   0.50    0.50    --   44.70  60.00  30.00  356
  6  \w     38.00  65.00   0.50    2.00    --  108.20  50.00  90.00   54
  7  \w    149.00 174.00   0.50    2.00    --  108.20  50.00   0.00   50
  8  \w    112.00 197.00   0.50    2.00    --  108.20  50.00 -30.00  170
  9  \w    106.00 133.00   0.50    2.00    --  108.20  50.00  30.00   54
 10  \w     56.00  81.00   0.50    2.00    --  108.20  50.00  30.00   50
 11  \w    140.00 198.00   0.50    2.00    --  108.20  50.00  30.00  116
 12  \w    104.00 131.00   0.50    2.00    --  108.20  50.00   0.00   54
 13  \w    143.00 191.00   0.50    2.00    --  108.20  50.00  90.00   96
 14  \w     37.00 192.00   0.50    2.00    --  108.20   0.00  90.00  310
 15  \w     93.00 138.00   0.50    2.00    --  108.20  50.00  90.00   90
 16  \w     28.00  55.00   0.50    2.00    --  108.20  50.00   0.00   54
 17  \w     21.00 192.00   0.50    2.00    --  108.20  50.00  60.00  342
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0838093000
_diffrn_orient_matrix_UB_12      -0.0245157000
_diffrn_orient_matrix_UB_13      0.0532738000
_diffrn_orient_matrix_UB_21      0.0507032000
_diffrn_orient_matrix_UB_22      0.0440679000
_diffrn_orient_matrix_UB_23      0.0235728000
_diffrn_orient_matrix_UB_31      -0.0547340000
_diffrn_orient_matrix_UB_32      0.0034043000
_diffrn_orient_matrix_UB_33      0.0766931000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43524
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.046
_diffrn_reflns_theta_min         3.122
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    8.035
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.7b (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             3464
_exptl_crystal_recrystallization_method
'Crystallised by layering a solution in chlorobenzene with n-hexane'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.122
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         13559
_refine_ls_number_restraints     711
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+5.4596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10581
_reflns_number_total             13559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08945d2.cif
_cod_data_source_block           1-Dy
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126383--7126388.cif.
;
_cod_database_code               7126383
_manchester_internal_coll_name   ldpm116
_manchester_internal_coll_client PE/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 0.5s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   8/4/2019
_manchester_internal_process_user PE
_manchester_internal_process_date 9/4/2019
_manchester_internal_solution_user PE
_manchester_internal_solution_date 9/4/2019
_manchester_internal_refinement_user PE/FO
_manchester_internal_refinement_date 15/4/2019
_manchester_internal_validation_user FO
_manchester_internal_validation_date 15/04/2019
_manchester_internal_archive_date 15/04/2019
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C30 Dy Al2 O4 F26'
_reflns_odcompleteness_completeness 98.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C57-Cl2 \\sim Cl2-C53
 with sigma of 0.02
 F28-C43 \\sim F28A-C43A
 with sigma of 0.02
 F31-C44 \\sim F31A-C44A
 with sigma of 0.02
 F34-C45 \\sim F34A-C45A
 with sigma of 0.02
 C42-C45 \\sim C42-C45A
 with sigma of 0.02
 C42-C44 \\sim C42-C44A
 with sigma of 0.02
 C42-C43 \\sim C42-C43A
 with sigma of 0.02
 F28-C42 \\sim F28A-C42
 with sigma of 0.02
 F31-C42 \\sim F31A-C42
 with sigma of 0.02
 F34-C42 \\sim F34A-C42
 with sigma of 0.02
 F30-C43 \\sim F32-C43A
 with sigma of 0.02
 F30-F28 \\sim F32-F28A
 with sigma of 0.02
 F30-C42 \\sim F32-C42
 with sigma of 0.02
 F30-C43A \\sim F30-C43 \\sim F28-C43 \\sim F28A-C43A \\sim F29-C43 \\sim
F29-C45A \\sim F34A-C45A ~
 F36-C45A \\sim F36-C45 \\sim F34-C45 \\sim F35-C45 \\sim F35-C44A \\sim
F31A-C44A \\sim F33-C44A \\sim F33-
 C44 \\sim F31-C44 \\sim F32-C44 \\sim F32-C43A
 with sigma of 0.02
 F19-C39 \\sim F21-C39 \\sim F20-C39
 with sigma of 0.02
 F22-C40 \\sim F23-C40 \\sim F24-C40
 with sigma of 0.02
 F27-C41 \\sim F25-C41 \\sim F26-C41
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Al2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim C30 \\sim C34 \\sim C38 \\sim C42
\\sim C31 \\sim C32 \\sim C33 \\sim C35 \\sim C36 \\sim C37 \\sim C39 \\sim C40
\\sim C41 \\sim C43 \\sim C44 \\sim C45 \\sim C43A \\sim C44A \\sim C45A \\sim
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17
\\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim F25
\\sim F26 \\sim F27 \\sim F29 \\sim F30 \\sim F28 \\sim F32 \\sim F33 \\sim F31
\\sim F35 \\sim F36 \\sim F34 \\sim F28A \\sim F31A \\sim F34A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C57 \\sim C52 \\sim Cl2 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F28A)=Sof(F31A)=Sof(F34A)=Sof(C43A)=Sof(C44A)=Sof(C45A)=1-FVAR(1)
 Sof(F28)=Sof(F31)=Sof(F34)=Sof(C43)=Sof(C44)=Sof(C45)=FVAR(1)
 Fixed Sof: Cl2(0.5) C57(0.5) H57(0.5) C56(0.5) H56(0.5) C55(0.5) H55(0.5)
 C54(0.5) H54(0.5) C53(0.5) H53(0.5) C52(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C28(H28A,H28B)
5.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C57(H57), C56(H56),
 C55(H55), C54(H54), C53(H53)
5.c Fitted hexagon refined as free rotating group:
 C57(C56,C55,C54,C53,C52)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              69604
_shelx_hkl_checksum              57731
_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_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 3.316
_oxdiff_exptl_absorpt_empirical_full_min 0.507