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_7126385
_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
'3(C6 H5 Cl), C58 H108 Al2 Dy0.2 N2 Y1.8, 2(Al C16 F36 O4)'
_chemical_formula_sum            'C108 H123 Al4 Cl3 Dy0.2 F72 N2 O8 Y1.8'
_chemical_formula_weight         3351.88
_chemical_name_systematic
'[Dy@Y(Cp*)2(Me3AlNEt3)]2[Al{OC(CF3)3}4]2(C6H5Cl)3'
_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             2019-10-06
_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                 98.2178(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.14639(9)
_cell_length_b                   30.4739(2)
_cell_length_c                   16.04187(10)
_cell_measurement_reflns_used    23047
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.0680
_cell_measurement_theta_min      3.0890
_cell_volume                     6844.57(8)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_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     17.00  89.00   1.00    1.00    --   44.70  10.00   0.00   72
  2  \w    -45.00 131.00   1.00    1.00    --   44.70  60.00 -90.00  176
  3  \w     58.00 197.00   1.00    2.00    --  108.20  30.00 -60.00  139
  4  \w     21.00  52.00   1.00    2.00    --  108.20  20.00 -30.00   31
  5  \w    106.00 197.00   1.00    2.00    --  108.20  20.00 -30.00   91
  6  \w     80.00 179.00   1.00    2.00    --  108.20  40.00 -60.00   99
  7  \w     22.00  52.00   1.00    2.00    --  108.20  30.00 -60.00   30
  8  \w    103.00 198.00   1.00    2.00    --  108.20  10.00 120.00   95
  9  \w     19.00 198.00   1.00    2.00    --  108.20  20.00 120.00  179
;
_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      0.0561527000
_diffrn_orient_matrix_UB_12      -0.0394841000
_diffrn_orient_matrix_UB_13      0.0414968000
_diffrn_orient_matrix_UB_21      -0.0892502000
_diffrn_orient_matrix_UB_22      -0.0151185000
_diffrn_orient_matrix_UB_23      0.0369466000
_diffrn_orient_matrix_UB_31      -0.0312713000
_diffrn_orient_matrix_UB_32      -0.0277440000
_diffrn_orient_matrix_UB_33      -0.0795592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41213
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.258
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.755
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.520
_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    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             3367
_exptl_crystal_recrystallization_method
'Crystallisation by layering a solution in chlorobenzene with hexane'
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1402
_refine_ls_number_reflns         13952
_refine_ls_number_restraints     3691
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+4.8920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12424
_reflns_number_total             13952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08945d2.cif
_cod_data_source_block           1-Dy@Y
_cod_depositor_comments
'Adding full bibliography for 7126383--7126388.cif.'
_cod_original_cell_volume        6844.58(8)
_cod_original_formula_sum        'C108 H123 Al4 Cl3 Dy0.20 F72 N2 O8 Y1.80'
_cod_database_code               7126385
_manchester_internal_coll_name   ldpm132
_manchester_internal_coll_client PE/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   PE
_manchester_internal_process_user PE
_manchester_internal_solution_user PE
_manchester_internal_refinement_user FO/PE
_manchester_internal_refinement_date 06/10/2019
_manchester_internal_validation_user FO
_manchester_internal_validation_date 06/10/2019
_manchester_internal_archive_date 06/10/2019
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.68
_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
 Cl2-C41 \\sim Cl2-C45
 with sigma of 0.02
3. Restrained planarity
 Cl2, C40, C41, C42, C43, C44, C45
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim
C23 \\sim C24 \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A
\\sim C21A \\sim C22A \\sim C23A \\sim C24A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Cl2 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O3A \\sim Al2 \\sim O2 \\sim O4 \\sim O1 \\sim O3 \\sim O1A \\sim C1_2 \\sim
C1_6 \\sim C1_4 \\sim C1_1 \\sim C1_5 \\sim C1A_7 \\sim C1_3 \\sim C2_2 \\sim
C3_2 \\sim C4_2 \\sim C2_6 \\sim C3_6 \\sim C4_6 \\sim C2_4 \\sim C3_4 \\sim
C4_4 \\sim C2_1 \\sim C3_1 \\sim C4_1 \\sim C2_5 \\sim C3_5 \\sim C4_5 \\sim
C2A_7 \\sim C3A_7 \\sim C4A_7 \\sim C2_3 \\sim C3_3 \\sim C4_3 \\sim F1_2 \\sim
F2_2 \\sim F3_2 \\sim F4_2 \\sim F5_2 \\sim F6_2 \\sim F7_2 \\sim F8_2 \\sim
F9_2 \\sim F1_6 \\sim F2_6 \\sim F3_6 \\sim F4_6 \\sim F5_6 \\sim F6_6 \\sim
F7_6 \\sim F8_6 \\sim F9_6 \\sim F1_4 \\sim F2_4 \\sim F3_4 \\sim F4_4 \\sim
F5_4 \\sim F6_4 \\sim F7_4 \\sim F8_4 \\sim F9_4 \\sim F1_1 \\sim F2_1 \\sim
F3_1 \\sim F4_1 \\sim F5_1 \\sim F6_1 \\sim F7_1 \\sim F8_1 \\sim F9_1 \\sim
F1_5 \\sim F2_5 \\sim F3_5 \\sim F4_5 \\sim F5_5 \\sim F6_5 \\sim F7_5 \\sim
F8_5 \\sim F9_5 \\sim F1A_7 \\sim F2A_7 \\sim F3A_7 \\sim F4A_7 \\sim F5A_7
\\sim F6A_7 \\sim F7A_7 \\sim F8A_7 \\sim F9A_7 \\sim F1_3 \\sim F2_3 \\sim
F3_3 \\sim F4_3 \\sim F5_3 \\sim F6_3 \\sim F7_3 \\sim F8_3 \\sim F9_3: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Dy1) = Uanis(Y1)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{F1_3, F2_3, F3_3, F4_3, F5_3, F6_3, F7_3, F8_3, F9_3, C1_3, C2_3, C3_3, C4_3}
{F1_4, F2_4, F3_4, F4_4, F5_4, F6_4, F7_4, F8_4, F9_4, C1_4, C2_4, C3_4, C4_4}
{F1_5, F2_5, F3_5, F4_5, F5_5, F6_5, F7_5, F8_5, F9_5, C1_5, C2_5, C3_5, C4_5}
{F1_6, F2_6, F3_6, F4_6, F5_6, F6_6, F7_6, F8_6, F9_6, C1_6, C2_6, C3_6, C4_6}
{F1_1, F2_1, F3_1, F4_1, F5_1, F6_1, F7_1, F8_1, F9_1, C1_1, C2_1, C3_1, C4_1}
as
{F1_2, F2_2, F3_2, F4_2, F5_2, F6_2, F7_2, F8_2, F9_2, C1_2, C2_2, C3_2, C4_2}
sigma for 1-2: 0.02 1-3: 0.04
7. Others
 Sof(C15A)=Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C15)=Sof(C16)=Sof(C17)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(1)
 Sof(O1A)=Sof(O3A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(F1)=Sof(F2)=
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(C1)=Sof(C2)=
 Sof(C3)=Sof(C4)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=
 Sof(F8)=Sof(F9)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=1-FVAR(2)
 Sof(O1)=Sof(O3)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=
 Sof(F8)=Sof(F9)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(F1)=Sof(F2)=Sof(F3)=
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(C1)=Sof(C2)=Sof(C3)=
 Sof(C4)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=
 Sof(F9)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=FVAR(2)
 Sof(Dy1)=1-FVAR(3)
 Sof(Y1)=FVAR(3)
 Fixed Sof: Cl2(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5)
 C45(0.5) H45(0.5) C40(0.5) C41(0.5) H41(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B)
8.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42), C43(H43),
 C44(H44), C45(H45), C41(H41)
8.c Fitted hexagon refined as free rotating group:
 C42(C43,C44,C45,C40,C41)
8.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F),
 C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F)
;
_shelx_res_checksum              22798
_shelx_hkl_checksum              57072
_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 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.839