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_7126386
_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 N2 Y2, 3(C6 H5 Cl), 2(Al C16 F36 O4)'
_chemical_formula_sum            'C108 H123 Al4 Cl3 F72 N2 O8 Y2'
_chemical_formula_weight         3337.17
_chemical_name_systematic
'[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                 98.4210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1215(2)
_cell_length_b                   30.3026(3)
_cell_length_c                   16.0232(2)
_cell_measurement_reflns_used    13426
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      75.3110
_cell_measurement_theta_min      3.0990
_cell_volume                     6782.70(15)
_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      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_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     29.00 121.00   1.00    1.00    --   44.80  20.00 -90.00   92
  2  \w    -19.00  14.00   1.00    1.00    --   44.80  20.00 -90.00   33
  3  \w    -44.00 133.00   1.00    1.00    --   44.80  10.00 120.00  177
  4  \w     93.00 118.00   1.00    1.00    --   44.80   0.00 -30.00   25
  5  \w     62.00 197.00   1.00    2.00    --  108.20  30.00-150.00  135
  6  \w     67.00 191.00   1.00    2.00    --  108.20  30.00  60.00  124
  7  \w    164.00 191.00   1.00    2.00    --  108.20  50.00 -60.00   27
  8  \w     19.00  48.00   1.00    2.00    --  108.20  20.00-120.00   29
  9  \w     22.00  48.00   1.00    2.00    --  108.20  30.00-150.00   26
 10  \w     71.00 105.00   1.00    2.00    --  108.20  20.00-120.00   34
 11  \w    130.00 198.00   1.00    2.00    --  108.20  20.00-120.00   68
 12  \w     65.00 188.00   1.00    2.00    --  108.20  20.00  90.00  123
 13  \w     99.00 126.00   1.00    2.00    --  108.20  50.00 -60.00   27
;
_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      -0.0315759000
_diffrn_orient_matrix_UB_12      -0.0258748000
_diffrn_orient_matrix_UB_13      0.0739750000
_diffrn_orient_matrix_UB_21      -0.0970625000
_diffrn_orient_matrix_UB_22      0.0240783000
_diffrn_orient_matrix_UB_23      -0.0137431000
_diffrn_orient_matrix_UB_31      -0.0417954000
_diffrn_orient_matrix_UB_32      -0.0365266000
_diffrn_orient_matrix_UB_33      -0.0615436000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39863
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.187
_diffrn_reflns_theta_min         3.484
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.321
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.625
_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            yellow
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       plate
_exptl_crystal_F_000             3356
_exptl_crystal_recrystallization_method
'Crystallised from layering a solution in chlorobenzene with n-hexane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1518
_refine_ls_number_reflns         13759
_refine_ls_number_restraints     4829
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1557P)^2^+5.8006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10853
_reflns_number_total             13759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08945d2.cif
_cod_data_source_block           1-Y
_cod_depositor_comments
'Adding full bibliography for 7126383--7126388.cif.'
_cod_database_code               7126386
_manchester_internal_coll_name   ldpm130
_manchester_internal_coll_client PE/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1s
_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         C108Al4Cl3Y2F72N2O8
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.619
_reflns_odcompleteness_completeness 99.80
_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
 F2_7-C2_7
 1.3 with sigma of 0.02
 F3_6-C2_6
 1.32 with sigma of 0.02
 C2_6-C1_6
 1.32 with sigma of 0.02
 F1_6-F3_6
 2.2 with sigma of 0.02
 F3_6-F2_6
 2.2 with sigma of 0.02
 F2_6-F1_6
 2.2 with sigma of 0.02
 Cl2-C41 \\sim Cl2-C45
 with sigma of 0.02
 Al1-O1_2 \\sim Al1-O1_7 \\sim Al1-O1_3 \\sim Al1-O1_8 \\sim Al1-O1_4 \\sim
Al1-O1_6 \\sim Al1-O1_5 ~
 Al1-O1_1
 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
C40 \\sim C43 \\sim C44 \\sim C42 \\sim C45 \\sim C41 \\sim Cl2: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
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
Al1 \\sim O1_5 \\sim C4_7 \\sim O1_6 \\sim O1_1 \\sim O1_4 \\sim O1_3 \\sim
O1_2 \\sim O1_8 \\sim C1_5 \\sim C1_7 \\sim C1_6 \\sim C1_1 \\sim C1_4 \\sim
C1_3 \\sim C1_2 \\sim C1_8 \\sim C2_5 \\sim C3_5 \\sim C4_5 \\sim O1_7 \\sim
C2_7 \\sim C3_7 \\sim C2_6 \\sim C3_6 \\sim C4_6 \\sim C2_1 \\sim C3_1 \\sim
C4_1 \\sim C2_4 \\sim C3_4 \\sim C4_4 \\sim C2_3 \\sim C3_3 \\sim C4_3 \\sim
C2_2 \\sim C3_2 \\sim C4_2 \\sim C2_8 \\sim C3_8 \\sim C4_8 \\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 F7_7 \\sim F8_7 \\sim F9_7 \\sim F1_7 \\sim F2_7 \\sim F3_7 \\sim
F4_7 \\sim F5_7 \\sim F6_7 \\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_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_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_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 \\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_8 \\sim
F2_8 \\sim F3_8 \\sim F4_8 \\sim F5_8 \\sim F6_8 \\sim F7_8 \\sim F8_8 \\sim
F9_8: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(F7_2) \\sim Ueq, Uanis(F8_2) \\sim Ueq, Uanis(F9_2) \\sim Ueq,
Uanis(C4_2) \\sim Ueq, Uanis(F7_7) \\sim Ueq, Uanis(F8_7) \\sim Ueq,
Uanis(F9_7) \\sim Ueq, Uanis(O1_7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
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_2, F2_2, F3_2, F4_2, F5_2, F6_2, F7_2, F8_2, F9_2, O1_2, C1_2, C2_2, C3_2,
C4_2}
{F1_3, F2_3, F3_3, F4_3, F5_3, F6_3, F7_3, F8_3, F9_3, O1_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, O1_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, O1_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, O1_6, C1_6, C2_6, C3_6,
C4_6}
{F1_7, F2_7, F3_7, F4_7, F5_7, F6_7, F7_7, F8_7, F9_7, O1_7, C1_7, C2_7, C3_7,
C4_7}
{F1_8, F2_8, F3_8, F4_8, F5_8, F6_8, F7_8, F8_8, F9_8, O1_8, C1_8, C2_8, C3_8,
C4_8}
as
{F1_1, F2_1, F3_1, F4_1, F5_1, F6_1, F7_1, F8_1, F9_1, O1_1, C1_1, C2_1, C3_1,
C4_1} 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(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(O1)=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(O1)=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(O1)=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(O1)=Sof(C1)=Sof(C2)=
 Sof(C3)=Sof(C4)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=
 Sof(O1)=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(O1)=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(O1)=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(O1)=Sof(C1)=Sof(C2)=
 Sof(C3)=Sof(C4)=FVAR(2)
 Fixed Sof: Cl2(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) C42(0.5) H42(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B)
8.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), 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)
8.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44),
 C45(H45), C41(H41), C42(H42)
8.d Fitted hexagon refined as free rotating group:
 C43(C44,C45,C40,C41,C42)
8.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              88660
_shelx_hkl_checksum              77350
_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 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.841