Fulvalene as a platform for the synthesis of a dimetallic dysprosocenium single-molecule magnet.
He, Mian; Guo, Fu-Sheng; Tang, Jinkui; Mansikkamäki, Akseli; Layfield, Richard A.; Chemical science 11 (2020) 5745–5752; doi:10.1039/d0sc02033h

data_1558078
_publ_section_title
;
 Fulvalene as a platform for the synthesis of a dimetallic dysprosocenium
 single-molecule magnet.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              5745
_journal_page_last               5752
_journal_paper_doi               10.1039/d0sc02033h
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C46 H74 B Dy2, B C24 F20'
_chemical_formula_sum            'C70 H74 B2 Dy2 F20'
_chemical_formula_weight         1641.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-26 deposited with the CCDC.	2020-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.812(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1029(5)
_cell_length_b                   20.9327(4)
_cell_length_c                   19.4229(5)
_cell_measurement_reflns_used    19764
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.0720
_cell_measurement_theta_min      2.6450
_cell_volume                     6833.2(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_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     16.00  84.00   1.00    3.44    --    5.00  60.00-120.00   68
  2  \w    -82.00  -1.00   1.00    3.44    --    5.00  60.00-120.00   81
  3  \w    -62.00 -30.00   1.00    3.44    --  -89.00  60.00  60.00   32
  4  \w   -177.00 -62.00   1.00    3.44    --  -89.00  60.00 120.00  115
  5  \w   -170.00-135.00   1.00    3.44    --  -89.00  43.00-150.00   35
  6  \w    -96.00 -55.00   1.00    3.44    --  -89.00  43.00-150.00   41
  7  \w    -88.00 -30.00   1.00    3.44    --  -89.00  57.00-120.00   58
  8  \w    -81.00  -1.00   1.00    3.44    --  -89.00  60.00 -30.00   80
  9  \w    -62.00  -1.00   1.00    3.44    --  -89.00  43.00 120.00   61
 10  \w    -47.00  -1.00   1.00    3.44    --  -89.00  60.00 120.00   46
 11  \w   -163.00-132.00   1.00    3.44    --  -89.00  14.00 -30.00   31
 12  \w    -85.00 -58.00   1.00    3.44    --  -89.00  14.00 -30.00   27
 13  \w    -41.00 -16.00   1.00    3.44    --  -89.00  14.00 -30.00   25
 14  \w   -145.00-112.00   1.00    3.44    --  -89.00  60.00  30.00   33
 15  \w   -177.00-145.00   1.00    3.44    --  -89.00  60.00 -30.00   32
 16  \w   -176.00-135.00   1.00    3.44    --  -89.00  57.00-120.00   41
 17  \w   -175.00-150.00   1.00    3.44    --  -89.00  43.00 120.00   25
 18  \w   -131.00 -90.00   1.00    3.44    --  -89.00  43.00 120.00   41
 19  \w   -177.00-124.00   1.00    3.44    --  -89.00  60.00  60.00   53
 20  \w   -177.00-150.00   1.00    3.44    --  -89.00  29.00  30.00   27
 21  \w    -92.00 -65.00   1.00    3.44    --  -89.00  29.00  30.00   27
 22  \w   -132.00   0.00   1.00    3.44    --  -89.00  57.00 -60.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072849000
_diffrn_orient_matrix_UB_12      0.0696643000
_diffrn_orient_matrix_UB_13      -0.0219200000
_diffrn_orient_matrix_UB_21      0.0840657000
_diffrn_orient_matrix_UB_22      -0.0143147000
_diffrn_orient_matrix_UB_23      0.0013259000
_diffrn_orient_matrix_UB_31      -0.0357090000
_diffrn_orient_matrix_UB_32      -0.0187765000
_diffrn_orient_matrix_UB_33      -0.0826054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55944
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.381
_diffrn_reflns_theta_max         67.381
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.397
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78492
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.422
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1112
_refine_ls_number_reflns         12172
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0685P)^2^+36.2734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10648
_reflns_number_total             12172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02033h2.cif
_cod_data_source_block           exp_379
_cod_depositor_comments
;Adding full bibliography for 1558076--1558078.cif.

 Adding full bibliography for 1558076--1558078.cif.
;
_cod_database_code               1558078
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H100 Dy3 B3 F20'
_shelx_estimated_absorpt_t_max   0.370
_shelx_estimated_absorpt_t_min   0.191
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1A
 1.19 with sigma of 0.01
 B1-H1B
 1.19 with sigma of 0.01
 B1-H1C
 1.19 with sigma of 0.01
 B1-H1D
 1.19 with sigma of 0.01
 C43-C38 \\sim C43A-C38A
 with sigma of 0.02
 C46-C41 \\sim C46A-C41A
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C39-C44 \\sim C39A-C44A
 with sigma of 0.02
 C45-C40 \\sim C45A-C40A
 with sigma of 0.02
 C42-C37 \\sim C42A-C37A
 with sigma of 0.02
 C38-C37 \\sim C38A-C37A
 with sigma of 0.02
 C37-C41 \\sim C37A-C41A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 Dy2-C43 \\sim Dy2-C43A
 with sigma of 0.04
 Dy2-C46 \\sim Dy2-C46A
 with sigma of 0.04
 Dy2-C39 \\sim Dy2-C39A
 with sigma of 0.04
 Dy2-C45 \\sim Dy2-C45A
 with sigma of 0.04
 Dy2-C42 \\sim Dy2-C42A
 with sigma of 0.04
 Dy2-C38 \\sim Dy2-C38A
 with sigma of 0.04
 Dy2-C37 \\sim Dy2-C37A
 with sigma of 0.04
 Dy2-C40 \\sim Dy2-C40A
 with sigma of 0.04
 Dy2-C41 \\sim Dy2-C41A
 with sigma of 0.04
 Dy2-C44 \\sim Dy2-C44A
 with sigma of 0.04
 C43-C39 \\sim C43A-C39A
 with sigma of 0.04
 C43-C37 \\sim C43A-C37A
 with sigma of 0.04
 C46-C37 \\sim C46A-C37A
 with sigma of 0.04
 C46-C40 \\sim C46A-C40A
 with sigma of 0.04
 C39-C45 \\sim C39A-C45A
 with sigma of 0.04
 C39-C37 \\sim C39A-C37A
 with sigma of 0.04
 C39-C41 \\sim C39A-C41A
 with sigma of 0.04
 C45-C41 \\sim C45A-C41A
 with sigma of 0.04
 C42-C38 \\sim C42A-C38A
 with sigma of 0.04
 C42-C41 \\sim C42A-C41A
 with sigma of 0.04
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 C38-C41 \\sim C38A-C41A
 with sigma of 0.04
 C38-C44 \\sim C38A-C44A
 with sigma of 0.04
 C37-C40 \\sim C37A-C40A
 with sigma of 0.04
 C40-C44 \\sim C40A-C44A
 with sigma of 0.04
 C19-C21 \\sim C19-C21A
 with sigma of 0.02
 C19-C20 \\sim C19-C20A
 with sigma of 0.02
 C19-C22 \\sim C19-C22A
 with sigma of 0.02
 F15-C60 \\sim F15A-C60A
 with sigma of 0.02
 F11-C64 \\sim F11A-C64A
 with sigma of 0.02
 F14-C61 \\sim F14A-C61A
 with sigma of 0.02
 F13-C62 \\sim F13A-C62A
 with sigma of 0.02
 F12-C63 \\sim F12A-C63A
 with sigma of 0.02
 C64-C59 \\sim C64A-C59A
 with sigma of 0.02
 C64-C63 \\sim C64A-C63A
 with sigma of 0.02
 C60-C59 \\sim C60A-C59A
 with sigma of 0.02
 C60-C61 \\sim C60A-C61A
 with sigma of 0.02
 C59-B2 \\sim C59A-B2
 with sigma of 0.02
 C62-C61 \\sim C62A-C61A
 with sigma of 0.02
 C62-C63 \\sim C62A-C63A
 with sigma of 0.02
 F15-C59 \\sim F15A-C59A
 with sigma of 0.04
 F15-C61 \\sim F15A-C61A
 with sigma of 0.04
 F11-C59 \\sim F11A-C59A
 with sigma of 0.04
 F11-C63 \\sim F11A-C63A
 with sigma of 0.04
 F14-C60 \\sim F14A-C60A
 with sigma of 0.04
 F14-C62 \\sim F14A-C62A
 with sigma of 0.04
 F13-C61 \\sim F13A-C61A
 with sigma of 0.04
 F13-C63 \\sim F13A-C63A
 with sigma of 0.04
 F12-C64 \\sim F12A-C64A
 with sigma of 0.04
 F12-C62 \\sim F12A-C62A
 with sigma of 0.04
 C64-C60 \\sim C64A-C60A
 with sigma of 0.04
 C64-C62 \\sim C64A-C62A
 with sigma of 0.04
 C64-B2 \\sim C64A-B2
 with sigma of 0.04
 C60-C62 \\sim C60A-C62A
 with sigma of 0.04
 C60-B2 \\sim C60A-B2
 with sigma of 0.04
 C59-C61 \\sim C59A-C61A
 with sigma of 0.04
 C59-C63 \\sim C59A-C63A
 with sigma of 0.04
 C61-C63 \\sim C61A-C63A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C43, C43A, C38, C38A, C37, C42, C42A, C37A, C41, C46, C41A, C46A, C40, C45,
 C40A, C45A, C39, C44, C39A, C44A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C21A, C20, C20A, C22, C22A, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F11, F11A, F12, F12A, F13, F13A, F14, F14A, F15, F15A, C59, C59A, C60, C60A,
 C61A, C61, C62, C62A, C63A, C63, C64, C64A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C46A)=Sof(H46D)=
 Sof(H46E)=Sof(H46F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C40A)=
 Sof(C39A)=Sof(C38A)=Sof(C37A)=Sof(C41A)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C39)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C38)=Sof(C37)=Sof(C40)=Sof(C41)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=FVAR(1)
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Sof(F11A)=Sof(C64A)=Sof(C63A)=Sof(F12A)=Sof(F13A)=Sof(C62A)=Sof(C61A)=
 Sof(F14A)=Sof(C60A)=Sof(C59A)=Sof(F15A)=1-FVAR(3)
 Sof(F15)=Sof(F11)=Sof(F14)=Sof(F13)=Sof(F12)=Sof(C64)=Sof(C60)=Sof(C59)=
 Sof(C62)=Sof(C61)=Sof(C63)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C3(H3), C8(H8)
5.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C15(H15A,H15B,H15C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C18(H18A,
 H18B,H18C), C12(H12A,H12B,H12C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C),
 C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C43(H43A,H43B,H43C), C46(H46A,
 H46B,H46C), C45(H45A,H45B,H45C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C44A(H44D,H44E,H44F), C43A(H43D,H43E,H43F), C42A(H42D,H42E,H42F), C46A(H46D,
 H46E,H46F), C45A(H45D,H45E,H45F), C21A(H21D,H21E,H21F), C20A(H20D,H20E,H20F),
 C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              87111
_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 1.309
_oxdiff_exptl_absorpt_empirical_full_min 0.706